CROSS-REFERENCE TO RELATED APPLICATIONS

[0001] This application claims priority to U.S. Application No. 17/966,622 filed October 14, 2022, and to U.S. Provisional Application No. 63/333,428 filed April 21 , 2022, the entirety of each of which is incorporated herein by reference.

FIELD OF THE DISCLOSURE

[0002] The present disclosure is related to processes for making synthetic hair made out of plant fibers. Accordingly, the disclosure is related to the fields of chemistry and chemical engineering.

BACKGROUND

[0003] Many women desire protective hairstyles such as braids and twists. To create this hairstyle, additional hair is needed to give the illusion of longer hair. Synthetic braiding hair is the material used to create the desired protective style. Unfortunately, synthetic braiding hair has a rough texture and contains chemical smells. Synthetic hair is also commonly made from plastics such as acrylic or nylon, whereas many users prefer natural products. Additionally, synthetic braiding hair can cause irritation to the scalp of the users. The irritation can include itchiness, redness, burning, bumps, and in some cases, it can cause hair loss.

[0004] There is a need for braiding hair that is safe for women with sensitive scalps.

SUMMARY

[0005] Described herein are methods of making synthetic hair from plant fiber. The method comprises providing a plant fiber, degumming the plant fiber, and dyeing the plant fiber. In some embodiments, the plant fiber is banana fiber. In some aspects, the method further comprises conditioning the plant fiber after degumming the plant fiber. In some additional aspects, the method further comprises neutralizing the plant fiber after dyeing the plant fiber. In still further aspects, the method further comprises rinsing and scouring the plant fiber after dyeing the plant fiber. In still further aspects, the method further comprises detangling, combing, and/or braiding the banana fiber after dyeing the banana fiber

[0006] In some embodiments, the degumming comprises soaking the plant fiber in an alkaline hydrogen peroxide solution. In some aspects, the alkaline hydrogen peroxide solution comprises a base, magnesium sulfate, and hydrogen peroxide.

[0007] In some embodiments, the dyeing is accomplished with a dye solution comprising dye, a salt, and soda ash.

[0008] In some embodiments, the method further comprises soaking the banana fiber in an alkaline pre-soak solution prior to degumming the banana fiber. In some aspects, the alkaline pre-soak solution comprises water and a strong base. In still further aspects, the alkaline pre-soak solution may comprise an enzyme, such as pectinase.

[0009] In some embodiments, the method further comprises soaking the plant fiber in an acid solution prior to degumming the plant fiber. In some aspects, the acid solution comprises a strong acid or an organic acid.

[0010] Further described herein are methods of degumming banana fiber. The methods generally comprise providing banana fiber and soaking the banana fiber in a degumming solution. Generally, the degumming solution comprises a base, magnesium sulfate, and hydrogen peroxide. In some embodiments, the method further comprises soaking the banana fiber in an alkaline pre-soak solution and rinsing the banana fiber prior to soaking the banana fiber in the degumming solution.

[0011] Further described herein are methods of dyeing banana fiber. The methods generally comprise soaking the banana fiber in a dye solution. Generally, the dye solution comprises a dye, a non-iodized salt, and soda ash. In some embodiments, the dye comprises a reactive dye powder.

[0012] Further described herein are synthetic hair compositions that are made using any of the methods described herein. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] FIGS. 1A-1 B show FTIR spectra for degummed banana fibers prepared before treatment with cetrimonium bromide (CTAB) (FIG. 1A) and after treatment with CTAB (FIG. 1 B).

[0014] FIGS. 2A-2F show Pareto charts depicting the analysis of the DOE degumming experimental data, as described in Example 2. FIG. 2A shows the factors affecting color. FIG. 2B shows the factors affecting texture. FIG. 2C shows the factors affecting density. FIG. 2D shows the factors affecting the concentration of cellulose. FIG. 2E shows the factors affecting the concentration of xylan. FIG. 2F shows the factors affecting the concentration of lignin.

[0015] FIGS. 3A-3E shows photographs of the bundles tested in the multifactor degumming experiment described in Example 5. FIG. 3A shows a picture of sample A. FIG. 3B shows a picture of sample B. FIG. 3C shows a picture of sample C. FIG. 3D shows a picture of sample D. FIG. 3E shows a picture of sample E.

[0016] FIGS. 4A-4E shows photographs of the bundles tested in the stabilizer and pre-soak evaluation described in Example 7. FIG. 4A shows a picture of sample A. FIG. 4B shows a picture of sample B. FIG. 4C shows a picture of sample C. FIG. 4D shows a picture of sample D. FIG. 4E shows a picture of sample E.

[0017] FIGS. 5A-5E shows photographs of the bundles tested in the enzyme evaluation described in Example 8. FIG. 5A shows a picture of sample A. FIG. 5B shows a picture of sample B. FIG. 50 shows a picture of sample C. FIG. 5D shows a picture of sample D. FIG. 5E shows a picture of sample E.

[0018] FIGS. 6A-6F show chromatograms of a glycosyl linkage analysis of treated banana fiber, untreated banana fiber, and dust samples from both. All times shown are in minutes. FIG. 6A shows a chromatogram of untreated banana fiber. FIG. 6B shows a chromatogram of partially methylated alditol acetates generated from an untreated banana fiber dust sample. FIG. 6C shows a chromatogram of partially methylated alditol acetates generated from a degummed banana fiber sample. FIG. 6D shows a chromatogram of partially methylated alditol acetates generated from a degummed banana fiber dust sample. FIG. 6E shows a chromatogram of partially methylated alditol acetates generated from a degummed and dyed banana fiber sample. FIG. 6F shows a chromatogram of partially methylated alditol acetates generated from a degummed and dyed banana fiber dust sample.

[0019] FIGS. 7A-7I show ¹ H-NMR spectra of several samples. FIGS. 7Aand 7B show the spectra of raw untreated banana fiber in ionic liquid at 70°C. FIGS. 7C and 7D show the spectra of degummed banana fiber in ionic liquid at 70°C. FIGS. 7E and 7F show the spectra of degummed and dyed banana fiber in ionic liquid at 70°C. FIG. 7G shows the spectra of an untreated banana fiber dust sample in ionic liquid at 70°C. FIG. 7H shows the spectra of a degummed banana fiber dust sample in ionic liquid at 70°C. FIG. 7I shows the spectra of a degummed and dyed banana fiber dust sample in ionic liquid at 70°C.

[0020] FIGS. 8A-8M show chromatograms of a TMS glycosyl composition analysis. All times shown are in minutes. FIG. 8A shows a chromatogram of the TMS standards by the TMS method. FIG. 8B shows a chromatogram of an O-acetylated raw untreated banana fiber. FIG. 8C shows a chromatogram of an O-acetylated raw untreated banana fiber dust sample. FIG. 8D shows a chromatogram of an O-acetylated degummed banana fiber. FIG. 8E shows a chromatogram of an O-acetylated degummed banana fiber dust sample. FIG. 8F shows a chromatogram of an O-acetylated dyed and degummed banana fiber. FIG. 8G shows a chromatogram of an O-acetylated dyed and degummed banana fiber dust sample. FIG. 8H shows a chromatogram of a non-acetylated raw untreated banana fiber. FIG. 8I shows a chromatogram of a non-acetylated raw untreated banana fiber dust sample. FIG. 8J shows a chromatogram of a non-acetylated degummed banana fiber. FIG. 8K shows a chromatogram of a non-acetylated degummed banana fiber dust sample. FIG. 8L shows a chromatogram of a non-acetylated dyed and degummed banana fiber. FIG. 8M shows a chromatogram of a non-acetylated dyed and degummed banana fiber dust sample.

DETAILED DESCRIPTION

[0021] Provided herein are methods of making synthetic hair from plant fibers. Plant fibers provide an environmentally-friendly alternative to other synthetic hair products, which generally include plastics. The hair can be braided without causing itchiness or irritation to the scalp of a user. The methods generally include providing plant fibers such as banana fiber, degumming the plant fibers, and dyeing the plant fibers. The methods may further include softening the plant fibers and texturing the plant fibers. The plant fiber may be provided in bundles of varying sizes.

[0022] Preferably, the plant fiber comprises banana fiber. Banana fiber is generally produced from the stems and stalks of the banana tree. The fibers can be collected by stripping apart sheaths of banana stem with a knife, retting, combing, or by chemical extraction. Many species and varieties of banana are used to produce banana fiber, and any may be used for the methods described herein. Additionally, it is envisioned that other cellulosic plant fibers, such as sisal and pineapple, could be used instead of banana fiber to achieve similar results.

[0023] Degumming the plant fiber may be accomplished by any degumming methods known in the art, including steam explosion, soaking the plant fiber in an alkaline solution followed by soaking the plant fiber in an aqueous alkaline hydrogen peroxide solution, soaking the plant fiber in a solution comprising a degumming enzyme, alcohol hydrolysis and combinations thereof. Preferably, the degumming is accomplished by soaking the plant fiber in an aqueous alkaline solution (also referred to herein as an “alkaline pre-soak”) followed by soaking in an alkaline hydrogen peroxide solution.

[0024] The alkaline pre-soak solution comprises a base (such as a strong base) and water as a solvent. The base may comprise sodium hydroxide, lithium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide, ammonium hydroxide, sodium carbonate, or combinations thereof. Preferably, the base comprises sodium hydroxide. The base may have a concentration in the alkaline pre-soak solution of about 0.1 wt% to about 5 wt%; for example, about 0.1 wt% to about 0.5 wt%, about 0.1 wt% to about 1 wt%, about 0.1 wt% to about 2 wt%, about 0.1 wt% to about 3 wt%, about 0.1 wt% to about 4 wt%, about 0.5 wt% to about 1 wt%, about 0.5 wt% to about 2 wt%, about 0.5 wt% to about 3 wt%, about 0.5 wt% to about 4 wt%, or about 0.5 wt% to about 5 wt%. Preferably, the base may have a concentration of about 1 wt%.

[0025] The alkaline pre-soak solution may have a pH from about 7 to about 11 ; for example, from about 7 to about 8, about 7 to about 9, about 7 to about 10, about 8 to about 9, about 8 to about 10, about 8 to about 11 , about 9 to about 10, about 9 to about 11 , or about 10 to about 11. Preferably, the alkaline hydrogen peroxide solution has a pH of about 9 to about 11 ; for example, about 9.0, 9.1 , 9.2, 9.3, 9.4, 9.5, 9.6, 9.7, 9.8, 9.9, 10.0, 10.1 , 10.2, 10.3, 10.4, 10.5, 10.6, 10.7, 10.8, 10.9, or about 11.0. The alkaline pre-soak solution may have a temperature of about 40°C to about 60°C, such as about 40°C, 45°C, 50°C, 55°C, or about 60°C.

[0026] The alkaline pre-soak solution may further comprise an enzyme. The enzyme may comprise pectinase, polygalacturonase, lignin peroxidase, amylase, one or more xylanases, or combinations thereof. The enzyme may have a concentration in the alkaline soak from about 0.1 wt% to about 0.2 wt%; for example, about 0.1 wt%, about 0.11 wt%, about 0.12 wt%, about 0.13 wt%, about 0.14 wt%, about 0.15 wt%, about 0.16 wt%, about 0.17 wt%, about 0.18 wt%, about 0.19 wt%, or about 0.2 wt%. Preferably, the enzyme has a concentration in the alkaline soak from about 0.15 wt% to about 0.2 wt%, or more preferably about 0.14 wt% to about 0.18 wt%. In an exemplary embodiment, the enzyme has a concentration in the alkaline soak of about 0.16 wt%.

[0027] The enzyme may have an enzymatic activity in the alkaline soak from about 50 units per gram (U/g) of plant fiber to about 150 U/g; for example, about 50 U/g to about 75 U/g, about 50 U/g to about 100 U/g, about 50 U/g to about 125 U/g, about 75 U/g to about 100 U/g, about 75 U/g to about 125 U/g, about 75 U/g to about 150 U/g, about 100 U/g to about 125 U/g, about 100 U/g to about 150 U/g, or about 125 U/g to about 150 U/g. Preferably, the enzyme may have an enzymatic activity in the alkaline soak of about 75 U/g to about 125 U/g, or more preferably about 75 U/g to about 100 U/g.

[0028] The alkaline hydrogen peroxide solution may comprise hydrogen peroxide, a base, and water as a solvent. The base may comprise sodium hydroxide, lithium hydroxide, potassium hydroxide, rubidium hydroxide, cesium hydroxide, ammonium hydroxide, sodium carbonate, or combinations thereof. Preferably, the base comprises sodium hydroxide. The base may have a concentration in the alkaline hydrogen peroxide solution from about 0.1 wt% to about 5 wt%; for example, about 0.1 wt% to about 0.5 wt%, about 0.1 wt% to about 1 wt%, about 0.1 wt% to about 2 wt%, about 0.1 wt% to about 3 wt%, about 0.1 wt% to about 4 wt%, about 0.5 wt% to about 1 wt%, about 0.5 wt% to about 2 wt%, about 0.5 wt% to about 3 wt%, about 0.5 wt% to about 4 wt%, or about 0.5 wt% to about 5 wt%. Preferably, the base may have a concentration of about 1 wt%. [0029] In another embodiment, the molarity of the base in the alkaline hydrogen peroxide presoak solution may be from about 1 M to about 6 M; for example, the molarity of the base in the alkaline hydrogen peroxide presoak solution may be from about 1 M to about 2 M, about 1 M to about 3 M, about 1 M to about 4 M, about 1 M to about 5 M, about 1 M to about 6 M, about 2 M to about 6 M, about 3 M to about 6 M, about 4 M to about 6 M, about 5 M to about 6 M, about 2 M to about 4 M, about 2 M to about 5 M, about 3 M to about 4 M, or about 3 M to about 5 M.

[0030] The alkaline hydrogen peroxide solution may have a hydrogen peroxide concentration from about 1 wt% to about 10 wt%. Preferably, the alkaline hydrogen peroxide solution may have a hydrogen peroxide concentration of about 5 wt%.

[0031] Preferably, the alkaline hydrogen peroxide solution further comprises a stabilizer. The stabilizer functions to stabilize the hydrogen peroxide, which otherwise would degrade rapidly. The stabilizer may comprise a sulfate salt such as magnesium sulfate, calcium sulfate, strontium sulfate, barium sulfate, lithium sulfate, sodium sulfate, potassium sulfate, ammonium iron sulfate, or combinations thereof. Alternatively, or additionally, the stabilizer may comprise a citrate salt, such as sodium citrate, lithium citrate, potassium citrate, magnesium citrate, calcium citrate, strontium citrate, barium citrate, or combinations thereof. Preferably, the stabilizer comprises magnesium sulfate, sodium citrate, or ammonium iron sulfate. The stabilizer may have a concentration in the alkaline hydrogen peroxide solution from about 0.1 wt% to about 1 wt %; for example, about 0.1 wt%, about 0.2 wt%, about 0.3 wt%, about 0.4 wt%, about 0.5 wt%, about 0.6 wt%, about 0.7 wt%, about 0.8 wt%, about 0.9 wt%, or about 1 wt%. Preferably, the stabilizer has a concentration in the alkaline hydrogen peroxide solution from about 0.1 wt% to about 0.5 wt%, or more preferably about 0.1 wt% to about 0.25 wt%.

[0032] The alkaline hydrogen peroxide solution may have a pH from about 7 to about 11 ; for example, from about 7 to about 8, about 7 to about 9, about 7 to about 10, about 8 to about 9, about 8 to about 10, about 8 to about 11 , about 9 to about 10, about 9 to about 11 , or about 10 to about 11. Preferably, the alkaline hydrogen peroxide solution has a pH of about 9 to about 11 ; for example, about 9.0, 9.1 , 9.2, 9.3, 9.4, 9.5, 9.6, 9.7, 9.8, 9.9, 10.0, 10.1 , 10.2, 10.3, 10.4, 10.5, 10.6, 10.7, 10.8, 10.9, or about 11.0. [0033] The plant fiber may be soaked in the alkaline hydrogen peroxide solution for a period from about 2 minutes to about 10 minutes, such as from about 2 minutes to about 3 minutes, about 2 minutes to about 4 minutes, about 3 minutes to about

5 minutes, about 4 minutes to about 5 minutes, about 5 minutes to about 7 minutes, about

6 minutes to about 8 minutes, about 7 minutes to about 9 minutes or 8 minutes to about 10 minutes. Preferably, the plant fiber is soaked in the alkaline hydrogen peroxide solution for a period of about 3 minutes.

[0034] The alkaline hydrogen peroxide solution may have a temperature from about 75°C to about 100°C; for example, about 75°C, 80°C, 85°C, 90°C, 95°C, or about 100°C. In some embodiments, the alkaline hydrogen peroxide solution may have a temperature from about 75°C to about 80°C, about 75°C to about 85°C, about 75°C to about 90°C, about 75°C to about 95°C, about 80°C to about 100°C, about 85°C to about 100°C, about 90°C to about 100°C, or about 95°C to about 100°C.

[0035] It has been found that as the temperature of the alkaline hydrogen peroxide solution increases, the time the plant fiber must soak to complete the degumming decreases. For example, at 100°C plant fiber should soak for about 2 minutes; whereas at 75°C, plant fiber should soak for about 10 minutes to complete the degumming.

[0036] Optionally, the plant fiber may be soaked in boiling water before and/or after the alkaline hydrogen peroxide soak. The plant fiber may be soaked in boiling water for about 15 minutes. Preferably, the plant fiber is soaked in boiling water only before the alkaline hydrogen peroxide soak, as it was surprisingly discovered that doing so helped to comb dust off of the plant fiber.

[0037] Prior to degumming the plant fiber, the plant fiber may optionally be soaked in an acid pre-soak solution. The acid pre-soak solution may comprise an acid such as a strong acid, an organic acid, or a combination thereof. The strong acid may comprise sulfuric acid, hydrochloric acid, chloric acid, hydrobromic acid, nitric acid, hydroiodic acid, perchloric acid, or combinations thereof. The organic acid may comprise acetic acid, formic acid, glycolic acid, lactic acid, citric acid, oxalic acid, uric acid, malic acid, tartaric acid, and combinations thereof. The plant fiber may soak in the acid presoak solution from about 20 minutes to about 2 hours; for example, about 20 minutes, 30 minutes, 40 minutes, 50 minutes, 1 hour, 1.25 hours, 1.5 hours, 1.75 hours, or about 2 hours. In exemplary embodiments, the plant fiber is soaked for about 1 hour in the acid pre-soak solution.

[0038] The acid may have a concentration in the pre-soak solution from about 0. 1 wt% to about 1 wt%, such as from about 0.1 wt% to about 0.25 wt%, about 0.1 wt% to about 0.5 wt%, about 0.1 wt% to about 0.75 wt%, or from about 0.1 wt% to about 1 wt%. In some examples, the acid may have a concentration of about 0.1 wt%, 0.2 wt%, 0.3 wt%, 0.4 wt%, 0.5 wt%, 0.6 wt%, 0.7 wt%, 0.8 wt%, 0.9 wt% or about 1 wt%.

[0039] The acid pre-soak solution may have a pH from about 1 to about 3.5; for example, about 1.1 , 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1 , 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8, 2.9, 3.0, 3.1 , 3.2, 3.3, 3.4 or about 3.5. In some embodiments, the acid pre-soak solution may have a pH from about 1 to about 3, or more preferably from about 1.5 to about 2.5, or even more preferably of about 2.

[0040] The acid pre-soak solution may have a temperature from about 50°C to about 75°C; for example, about 50°C, 55°C, 60°C, 65°C, 70°C, or about 75°C. In some embodiments, the acid pre-soak solution may have a temperature from about 50°C to about 55°C, about 50°C to about 60°C, about 50°C to about 65°C, about 50°C to about 70°C, or about 55°C to about 75°C, about 60°C to about 75°C, about 65°C to about 75°C, or about 70°C to about 75°C.

[0041] Optionally, the plant fibers may be soaked in boiling water before the acid pre-soak. The plant fibers may be soaked in boiling water for about 15 minutes.

[0042] After degumming, the plant fibers are rinsed in a cold water bath before dyeing. The dye solution comprises a dye and water, and may further comprise a salt and soda ash.

[0043] The dye may comprise a dye powder such as a reactive dye powder, a disperse dye powder, a direct dye powder, a basic dye powder, an acid dye powder, or a combination thereof. Alternatively, the dye may comprise a permanent hair dye. A permanent hair dye operates by oxidation of precursor materials such as paraphenylenediamine (PPD), meta-phenylenediamine (MPD), para-aminophenol (PAP), and/ or resorcinol with the aid of an oxidant (e.g., hydrogen peroxide) and a base (e.g., ammonium hydroxide). [0044] Preferably, the dye powder is operable to permanently dye the fibers. Preferably, reactive dye powders are used for colors such as black, red, yellow, and blue. Alternatively, or additionally, the dye may comprise p-phenylenediamine or m- phenylenediamine for a black dye. The dye powder may have a concentration in the dye solution from about 0.001 wt% to about 1 .00 wt%, such as from about 0.001 wt% to about 0.005 wt%, about 0.001 wt% to about 0.01 wt%, about 0.001 wt% to about 0.05 wt%, about 0.001 wt% to about 0.1 wt%, about 0.001 wt% to about 0.5 wt%, about 0.005 wt% to about 1 wt%, about 0.01 wt% to about 1 wt%, about 0.05 wt% to about 1 wt%, about 0.1 wt% to about 1 wt%, or from about 0.5 wt% to about 1 wt%.

[0045] The dye solution may further comprise a salt. The salt may comprise a chloride salt, such as sodium chloride, potassium chloride, lithium chloride, calcium chloride, magnesium chloride, strontium chloride, barium chloride, or combinations thereof. The salt may comprise a carbonate salt, such as sodium carbonate (also referred to herein as soda ash), lithium carbonate, potassium carbonate, magnesium carbonate, calcium carbonate, strontium carbonate, barium carbonate, or combinations thereof. The salt may comprise a sulfate salt, such as sodium sulfate, lithium sulfate, potassium sulfate, calcium sulfate, magnesium sulfate, strontium sulfate, barium sulfate, or combinations thereof. Preferably, the salt is a non-iodized salt. The salt may have a concentration in the dye solution from about 5 wt% to about 15 wt%; for example, about 5 wt% to about 10 wt%, or about 10 wt% to about 15 wt%, about 5 wt%, about 6 wt%, about 7 wt%, about 8 wt%, about 9 wt%, about 10 wt%, about 11 wt%, about 12 wt%, about 13 wt%, about 14 wt%, or about 15 wt%.

[0046] The dye solution may further comprise soda ash. The soda ash may be present in a concentration from about 0.5 wt% to about 1.5 wt%; for example, about 0.5 wt%, about 0.6 wt%, about 0.7 wt%, about 0.8 wt%, about 0.9 wt%, about 1 wt%, about 1.1 wt%, about 1 .2 wt%, about 1 .3 wt%, about 1 .4 wt%, and about 1 .5 wt%.

[0047] The dye solution may further comprise an organic acid to neutralize the dye solution and/or adjust the pH of the dye solution. The organic acid may comprise acetic acid, citric acid, formic acid, glycolic acid, lactic acid, oxalic acid, uric acid, malic acid, tartaric acid, and combinations thereof. Preferably, the organic acid comprises acetic acid. The organic acid may have a concentration in the dye solution from about 0.1 wt% to about 1 wt%, such as from about 0.1 wt% to about 0.25 wt%, about 0.1 wt% to about 0.5 wt%, about 0.1 wt% to about 0.75 wt%, about 0.25 wt% to about 1 wt%, about 0.5 wt% to about 1 wt%, or about 0.75 wt%. Preferably, the concentration of the organic acid in the solution is from about 0.1 wt% to about 0.5 wt%, or more preferably about 0.25 wt%.

[0048] The dye solution may have a pH from about 9 to about 11 , such as about 9.0, 9.1 , 9.2, 9.3, 9.4, 9.5, 9.6, 9.7, 9.8, 9.9, 10.0, 10.1 , 10.2, 10.3, 10.4, 10.5, 10.6, 10.7, 10.8, 10.9, or about 11.0. Preferably, the dye solution has a pH of about 9.5 to about 10.5, or even more preferably of about 10.

[0049] After dyeing, the dyed banana fiber may be scoured, softened, sealed, detangled, combed, dried, and/or conditioned. These steps may be performed to improve the appearance and texture of the final synthetic hair product. These steps may be performed in the following order: scouring, softening, conditioning, detangling sealing, and drying; however, this order of performance is not required.

[0050] The scouring may be performed to clean the dyed banana fiber and remove impurities, leftover dye, etc. The scouring may be accomplished by scrubbing the dyed banana fiber with a scouring solution comprising a detergent (such as a commercial liquid detergent), sodium laureth sulfate, cocamidopropyl betaine, Synthrapol®, and combinations thereof.

[0051] The detergent may have a concentration in the scouring solution of about 0.01 wt% to about 1 wt%, such as from 0.01 wt% to about 0.05 wt%, about 0.01 wt% to about 0.1 wt%, about 0.01 wt% to about 0.5 wt%, about 0.05 wt% to about 1 wt%, about 0.1 wt% to about 1 wt%, or about 0.5 wt% to about 1 wt%.

[0052] The sodium laureth sulfate may have a concentration in the scouring solution of about 0.01 wt% to about 0.05 wt%, or more preferably about 0.03 wt%.

[0053] The cocamidopropyl betaine may have a concentration in the scouring solution of about 0.005 wt% to about 0.05 wt%, or more preferably of about 0.01 wt%.

[0054] The softening may be performed to improve the texture of the dyed plant fiber, and to eliminate color bleeding or transfer after dyeing. The softening may accomplished by soaking the dyed banana fiber in a softening solution comprising a softening agent. The softening agent may comprise a conditioning agent such as dicetyldimonium chloride (trade name Quaternium-31 ), or may comprise butyric acid, polyquaternium-10 (a polymeric quaternary ammonium salt of hydroxyethyl cellulose), behentrimonium chloride, barley quat (a quaternary ammonium compound derived from hydrolyzed proteins sourced from barley), cetrimonium bromide, or combinations thereof. In an alternative embodiment, the softening agent may include Milsoft®. Preferably, the softening agent comprises dicetyldimonium chloride.

[0055] The softening agent may have a concentration in the softening solution from about 0.5 wt% to about 5 wt%. In some aspects, the softening agent may have a concentration in the softening solution from about 0.5 wt% to about 1 wt%, about 0.5 wt% to about 1.5 wt%, about 0.5 wt% to about 2 wt%, about 0.5 wt% to about 2.5 wt%, about 0.5 wt% to about 3 wt%, about 0.5 wt% to about 3.5 wt%, about 0.5 wt% to about 4 wt%, about 0.5 wt% to about 4.5 wt%, about 0.5 wt% to about 5 wt%, about 1 wt% to about 5 wt%, about 1 .5 wt% to about 5 wt%, about 2 wt% to about 5 wt%, about 2.5 wt% to about 5 wt%, about 3 wt% to about 5 wt%, about 3.5 wt% to about 5 wt%, about 4 wt% to about 5 wt%, or about 4.5 wt% to about 5 wt%. In some examples, the softening agent may have a concentration in the softening solution in an amount of about 0.5 wt%, 0.75 wt%, 1 wt%, 1 .25 wt%, 1 .5 wt%, 1 .75 wt%, 2 wt%, 2.25 wt%, 2.5 wt%, 2.75 wt%, 3 wt%, 3.25 wt%, 3.5 wt%, 3.75 wt%, 4 wt%, 4.25 wt%, 4.5 wt%, 4.75 wt%, or about 5 wt%. In a preferred embodiment, the softening agent may have a concentration in the softening solution of about 1 wt%.

[0056] The sealing may be performed to trap moisture in the dyed banana fiber to prevent the banana fiber from drying out. The sealing may be accomplished by soaking the dyed banana fiber in a sealing solution. The sealing solution may comprise a solvent or carrier such as an isoalkane, such as a C10 isoalkane, a Cn isoalkane, a C12 isoalkane, or a C13 isoalkane. Isoalkanes for use in the solvent or carrier may include isobutane, isopentane, isohexane, isoheptane, isooctane, isononane, isodecane, isoundecane, isododecane, and other isoalkanes and combinations thereof. Preferably, the isoalkane comprises isododecane.

[0057] The sealing solution may further comprise one or more emollients. The one or more emollients may comprise isopropyl palmitate, a vegetable oil, squalene, neopentyl glycol diheptanoate, cyclopentasiloxane, diheptyl succinate, carpyloyl glycerine, sebacid acid copolymer, dimethicone, and combinations thereof. The vegetable oil may comprise canola oil, corn oil, cottonseed oil, grapeseed oil, olive oil, palm oil, rapeseed oil, soybean oil, safflower oil, peanut oil, sesame oil, rice bran oil, almond oil, brazil nut oil, cashew oil, hazelnut oil, pecan oil, pine nut oil, pistachio oil, walnut oil, pumpkin seed oil, or other vegetable oils known in the art. Preferably, the vegetable oil comprises grapeseed oil.

[0058] The emollient may be present in the sealing solution in a concentration from about 10 wt% to about 100 wt%, such as from about 10 wt% to about 25 wt%, about 10 wt% to about 50 wt%, about 10 wt% to about 75 wt%, about 10 wt% to about 100 wt%, about 25 wt% to about 100 wt%, about 50 wt% to about 100 wt%, or about 75 wt% to about 100 wt%. In some examples, the emollient may be present in the sealing solution in a concentration of about 10 wt%, 15 wt%, 20 wt%, 25 wt%, 30 wt%, 35 wt%, 40 wt%, 45 wt%, 50 wt%, 55 wt%, 60 wt%, 65 wt%, 70 wt%, 75 wt%, 80 wt%, 85 wt%, 90 wt%, 95 wt%, or about 100 wt%. Preferably, the emollient is present in the sealing solution in an amount from about 25 wt% to about 75 wt%, or more preferably from about 45 wt% to about 65 wt%.

[0059] The conditioning may be performed to further improve the texture and appearance of the dyed banana fiber. The conditioning may be accomplished by soaking the banana fiber in a conditioning solution and massaging the banana fiber in the conditioning solution. The conditioning solution may comprise water and a conditioning agent. The conditioning agent may comprise a commercial hair conditioner.

[0060] The conditioning solution may further comprise a humectant. The humectant may comprise glycerin, propanediol, urea, hyaluronic acid, salicylic acid, glycolic acid, lactic acid, propylene glycol, honey, sorbitol, aloe vera, castor oil, sugar alcohols, or other humectants known in the art and combinations thereof. Preferably, the humectant comprises glycerin.

[0061] The humectant may have a concentration in the conditioning solution from about 25 wt% to about 100 wt%. In some aspects, the humectant may have a concentration in the conditioning solution from about 25 wt% to about 30 wt%, about 25 wt% to about 40 wt%, about 25 wt% to about 50 wt%, about 25 wt% to about 60 wt%, about 25 wt% to about 70 wt%, about 25 wt% to about 80 wt%, about 25 wt% to about 90 wt%, about 25 wt% to about 100 wt%, about 30 wt% to about 100 wt%, about 40 wt% to about 100 wt%, about 50 wt% to about 100 wt%, about 60 wt% to about 100 wt%, about 70 wt% to about 100 wt%, about 80 wt% to about 100 wt%, or about 90 wt% to about 100 wt%. In some examples, the humectant may have a concentration in the conditioning solution of about 25 wt%, 30 wt%, 35 wt%, 40 wt%, 45 wt%, 50 wt%, 55 wt%, 60 wt%, 65 wt%, 70 wt%, 75 wt%, 80 wt%, 85 wt%, 90 wt%, 95 wt%, or about 100 wt%. In a preferred embodiment the humectant may have a concentration in the conditioning solution of about 45 wt%.

[0062] It is to be understood that this disclosure is not limited to the particular methods, compositions, or materials specified herein but is extended to equivalents thereof as would be recognized by those ordinarily skilled in the relevant arts. It should also be understood that terminology employed herein is used for the purpose of describing particular embodiments only and is not intended to be limiting.

[0063] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the art to which the disclosure belongs. Although any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the subject matter of the present disclosure, preferred methods and materials are described. For the purposes of the present disclosure, the following terms are defined below.

[0064] As used herein, the term “about” is used to provide flexibility to a numerical range endpoint by providing that a given value may be “a little above” or “a little below” the endpoint. For example, the endpoint may be within 10%, 8%, 5%, 3%, 2%, or 1 % of the listed value. Further, for the sake of convenience and brevity, a numerical range of “about 50 mg/mL to about 80 mg/mL” should also be understood to provide support for the range of “50 mg/mL to 80 mg/mL”

[0065] As used herein, “comprises,” “comprising,” “containing,” and “having” and the like can have the meaning ascribed to them in U.S. Patent Law and can mean “includes,” “including,” and the like, and are generally interpreted to be open ended terms. The terms “consisting of” or “consists of” are closed terms, and include only the components, structures, steps, or the like specifically listed in conjunction with such terms, as well as that which is in accordance with U.S. Patent law. “Consisting essentially of” or “consists essentially of” have the meaning generally ascribed to them by U.S. Patent law. In particular, such terms are generally closed terms, with the exception of allowing inclusion of additional items, materials, components, steps, or elements, that do not materially affect the basic and novel characteristics or function of the item(s) used in connection therewith. For example, trace elements present in a composition, but not affecting the composition’s nature or characteristics would be permissible if present under the “consisting essentially of” language, even though not expressly recited in a list of items following such terminology. In this specification when using an open ended term, like “comprising” or “including,” it is understood that direct support should be afforded also to “consisting essentially of” language as well as “consisting of” language as if stated explicitly and vice versa.

[0066] Concentrations, amounts, and other numerical data may be expressed or presented herein in a range format. It is to be understood that such a range format is used merely for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. As an illustration, a numerical range of “about 2 to about 50” should be interpreted to include not only the explicitly recited values of 2 to 50, but also include all individual values and sub-ranges within the indicated range. Thus, included in this numerical range are individual values such as 2, 2.4, 3, 3.7, 4, 5.5, 10, 10.1 , 14, 15, 15.98, 20, 20.13, 23, 25.06, 30, 35.1 , 38.0, 40, 44, 44.6, 45, 48, and sub-ranges such as from 1 -3, from 2-4, from 5-10, from 5-20, from 5-25, from 5-30, from 5-35, from 5-40, from 5-50, from 2-10, from 2-20, from 2-30, from 2-40, from 2-50, etc. This same principle applies to ranges reciting only one numerical value as a minimum or a maximum. Furthermore, such an interpretation should apply regardless of the breadth of the range or the characteristics being described. EXEMPLARY EMBODIMENTS

[0067] Embodiment 1 : A method of making synthetic hair from plant fiber, the method comprising: providing a plant fiber; degumming the plant fiber; and dyeing the plant fiber.

[0068] Embodiment 2: The method of embodiment 1 , wherein the plant fiber is banana fiber.

[0069] Embodiment 3: The method of embodiment 1 or embodiment 2, wherein the degumming comprises soaking the plant fiber in an alkaline hydrogen peroxide solution.

[0070] Embodiment 4: The method of embodiment 3, wherein the alkaline hydrogen peroxide solution comprises a base, magnesium sulfate, and hydrogen peroxide.

[0071] Embodiment 5: The method of any one of embodiments 1 -4, further comprising soaking the banana fiber in an alkaline pre-soak solution prior to degumming the banana fiber.

[0072] Embodiment 6: The method of embodiment 5, wherein the alkaline pre-soak solution comprises water and a strong base.

[0073] Embodiment 7: The method of embodiment 6, wherein the alkaline pre-soak solution further comprises an enzyme.

[0074] Embodiment 8: The method of embodiment 7, wherein the enzyme comprises pectinase.

[0075] Embodiment 9: The method of any one of embodiments 1 -8, further comprising soaking the plant fiber in an acid solution prior to degumming the plant fiber.

[0076] Embodiment 10: The method of embodiment 9, wherein the acid solution comprises a strong acid or an organic acid.

[0077] Embodiment 11 : The method of any one of embodiments 1 -10, wherein the dyeing is accomplished with a dye solution comprising dye, a salt, and soda ash.

[0078] Embodiment 12: The method of any one of embodiments 1 -11 , further comprising conditioning the plant fiber after degumming the plant fiber, wherein the conditioning comprises soaking the plant fiber in a conditioning solution. [0079] Embodiment 13: The method of embodiment 12, wherein the conditioning solution comprises water, a conditioning agent, and optionally a humectant.

[0080] Embodiment 14: The method of embodiment 13, wherein the conditioning solution comprises a humectant, and the humectant is selected from the group consisting of glycerin, propanediol, urea, hyaluronic acid, salicylic acid, glycolic acid, lactic acid, propylene glycol, honey, sorbitol, aloe vera, castor oil, sugar alcohols, and combinations thereof.

[0081] Embodiment 15: The method of embodiment 13 or embodiment 14, wherein the humectant has a concentration in the conditioning solution of about 45 wt%.

[0082] Embodiment 16: The method of any one of embodiments 1 -15, further comprising neutralizing the plant fiber.

[0083] Embodiment 17: The method of any one of embodiments 1 -16, further comprising rinsing and scouring the plant fiber after dyeing the plant fiber.

[0084] Embodiment 18: The method of embodiment 17, wherein the scouring is accomplished by scrubbing the plant fiber with a scouring solution comprising a detergent.

[0085] Embodiment 19: The method of embodiment 18, wherein the detergent comprises sodium laureth sulfate, cocam idopropyl betaine, and combinations thereof.

[0086] Embodiment 20: The method of embodiment 18 or embodiment 19, wherein the detergent has a concentration in the scouring solution from about 0.01 wt% to about 1 wt%.

[0087] Embodiment 21 : The method of any one of embodiments 1 -20, further comprising detangling, combing, and/or braiding the plant fiber after dyeing the plant fiber.

[0088] Embodiment 22: A method of degumming banana fiber, the method comprising: providing banana fiber; and soaking the banana fiber in a degumming solution, the degumming solution comprising: a base; magnesium sulfate; and hydrogen peroxide. [0089] Embodiment 23: The method of embodiment 22, further comprising soaking the banana fiber in an alkaline pre-soak solution and rinsing the banana fiber prior to soaking the banana fiber in the degumming solution.

[0090] Embodiment 24: The method of embodiment 22 or embodiment 23, wherein the method further comprises soaking the banana fiber in an alkaline hydrogen peroxide solution before soaking the banana fiber in the degumming solution.

[0091] Embodiment 25: The method of embodiment 24, wherein the alkaline hydrogen peroxide solution comprises a base, magnesium sulfate, and hydrogen peroxide.

[0092] Embodiment 26: The method of embodiment 23, wherein the alkaline pre-soak solution comprises water and a strong base.

[0093] Embodiment 27: The method of embodiment 26, wherein the alkaline pre-soak solution further comprises an enzyme.

[0094] Embodiment 28: The method of embodiment 27, wherein the enzyme comprises pectinase.

[0095] Embodiment 29: The method of any one of embodiments 22-28, further comprising soaking the banana fiber in an acid solution prior to degumming the banana fiber.

[0096] Embodiment 30: The method of embodiment 29, wherein the acid solution comprises a strong acid or an organic acid.

[0097] Embodiment 31 : The method of any one of embodiments 22-30, further comprising dyeing the banana fiber, wherein the dyeing is accomplished with a dye solution comprising dye, a salt, and soda ash.

[0098] Embodiment 32: The method of any one of embodiments 22-31 , further comprising conditioning the banana fiber after degumming the banana fiber, wherein the conditioning comprises soaking the banana fiber in a conditioning solution.

[0099] Embodiment 33: The method of embodiment 32, wherein the conditioning solution comprises water, a conditioning agent, and optionally a humectant.

[0100] Embodiment 34: The method of embodiment 33, wherein the conditioning solution comprises a humectant, and the humectant is selected from the group consisting of glycerin, propanediol, urea, hyaluronic acid, salicylic acid, glycolic acid, lactic acid, propylene glycol, honey, sorbitol, aloe vera, castor oil, sugar alcohols, and combinations thereof.

[0101] Embodiment 35: The method of embodiment 33 or embodiment 34, wherein the humectant has a concentration in the conditioning solution of about 45 wt%.

[0102] Embodiment 36: The method of any one of embodiments 22-35, further comprising neutralizing the banana fiber

[0103] Embodiment 37: The method of any one of embodiments 22-36, further comprising rinsing and scouring the banana fiber after dyeing the banana fiber.

[0104] Embodiment 38: The method of embodiment 37, wherein the scouring is accomplished by scrubbing the banana fiber with a scouring solution comprising a detergent.

[0105] Embodiment 39: The method of embodiment 38, wherein the detergent comprises sodium laureth sulfate, cocam idopropyl betaine, and combinations thereof.

[0106] Embodiment 40: The method of embodiment 38 or embodiment 39, wherein the detergent has a concentration in the scouring solution from about 0.01 wt% to about 1 wt%.

[0107] Embodiment 41 : The method of any one of claims 22-40, further comprising detangling, combing, and/or braiding the banana fiber after dyeing the banana fiber.

[0108] Embodiment 42: A method of dyeing banana fiber, the method comprising soaking the banana fiber in a dye solution comprising: a dye; non-iodized salt; and soda ash.

[0109] Embodiment 43: The method of claim 42, wherein the dye comprises a reactive dye powder.

[0110] Embodiment 44: A synthetic hair composition comprising banana fiber made by the method of any one of the previous claims.

EXAMPLES

[0111] Examples have been set forth below for the purpose of illustration and to describe certain specific embodiments of the disclosure. However, the scope of the claims is not to be in any way limited by the examples set forth herein. Various changes and modifications to the disclosed embodiments will be apparent to those skilled in the art and such changes and modifications including, without limitation, those relating to the chemical structures, substituents, derivatives, formulations, or methods of the disclosure may be made without departing from the spirit of the disclosure and the scope of the appended claims.

Example 1 : Exemplary process for preparing Black hair bundles

[0112] Black hair bundles were prepared using the methods described herein. First, banana fibers were separated into 156 g bundles and secured with a hair tie composed of banana fiber. A single batch consisted of 7 x 156 g bundles.

[0113] Next, an alkaline pre-soak solution was prepared. The alkaline solution was prepared in a brew kettle by combining 52.5 g of sodium hydroxide pellets with 21 liters of tap water. The solution was mixed well until all solids dissolved. The pH of the solution was tested, with a target pH between 11 and 12. The solution was then allowed to heat to a temperature of 100 °C. After reaching the desired temperature, 7 bundles were loaded into the kettle and allowed to process for 60 minutes. After 60 minutes, the pH of the solution was reduced to 7. The pH was adjusted by adding concentrated sulfuric acid dropwise to the solution. The bundles were then allowed to soak for an additional 30 min. After 30 minutes, the bundles were removed from the kettle, rinsed under cool water, and set aside for the next step.

[0114] Next, an alkaline hydrogen peroxide solution was prepared. To prepare the solution, 13 liters of tap water was added into a brew kettle. Next, 33 g of magnesium sulfate hepta-hydrate and 133 g of sodium carbonate was added into the kettle and mixed until all solids dissolved. The solution was then allowed to heat to a temperature of 90 °C. After reaching the desired temperature, the 7 bundles from above were loaded into the kettle. 662 g of 30 % hydrogen peroxide was added into the kettle and the bundles were allowed to soak for 3 min. After 3 min, the bundles were removed from the kettle, rinsed under cool water, and set aside until they were ready to be dyed.

[0115] To prepare the dye bath, 13 liters of tap water was added into a brew kettle. Next, 1324 g of sodium chloride was added into the kettle and mixed well until all of the solids dissolved. The kettle was then allowed to heat to 60 °C. Once the salt was fully dissolved, 81.90 g black dye, 32.76 g red dye, and 49.14 g yellow dye was added into the kettle and mixed well until all of the solids were dissolved. Next, the 7 bundles from above were loaded into the kettle and allowed to soak for approximately 10 min. 132 g of sodium carbonate was weighed into a separate beaker. A portion of the dye solution was drained from the kettle into the beaker and this solution was mixed well to dissolve all solids. The sodium carbonate solution was then poured into the kettle and the bundles were gently mixed and allowed to soak for 60 minutes. After 60 minutes, the kettle was drained and the bundles were removed and rinsed under cool water.

[0116] A neutralization bath was then prepared in a brew kettle by combining 13 liters of tap water with 119 g of vinegar. The kettle was then allowed to heat to 50 °C. Next, the 7 bundles from above were loaded into the kettle and allowed to process for 10 minutes. During this time, a shampoo bath was prepared by combining 13 liters of hot tap water, 18 g sodium carbonate, 3.31 g sodium laureth sulfate, and 0.66 g cocamidopropyl betaine into a separate container. After processing in the neutralization bath for 10 minutes, the bundles were removed and loaded into the shampoo bath. Bundles were gently massaged for 10 minutes in the bath and then rinsed under cool tap water.

[0117] Next a softening solution was prepared in a brew kettle by combining 13 liters of tap water with 35 g Milsoft. The solution was mixed well and allowed to heat to a temperature of 60 °C. The 7 bundles from above were loaded into the kettle and allowed to process for 10 min. After 10 minutes, the bundles were removed and rinsed under cool tap water until the water ran clear. Each bundle was gently squeezed to remove excess water and then set aside until ready to be detangled.

[0118] The bundles were soaked in a bucket containing hot water (130°F) for about 1 hour prior to detangling. One bundle at a time was removed from the bucket, gently squeezed to remove excess water, and hung on a rack. 50 g of glycerin was applied directly onto each bundle and massaged into the fiber. Combing tools were used to begin detangling the bundles. Once the bundles were combed through, each bundle was flipped to the opposite side. An additional 50 g of glycerin was applied to each bundle. The bundles were detangled using combing tools once again. 20 sprays of a sealant was sprayed into each bundle and massaged through. Once seven bundles have been detangled, the entire batch is allowed to dry in an oven at about 75°C for no more than about 1 hour Once dried, the bundles were removed an hung on racks.

Example 2: Surface Modification of Natural Fibers for Improved Texture

[0119] The goal of this project was to improve texture of banana fibers via surface modification. To achieve this goal, the project had two main objectives: (1 ) chemical treatment for surface modification of banana fibers; and (2) characterization of treated banana fibers.

[0120] Previously degummed banana fibers were treated with a variety of chemicals to screen for the best option to use in surface modification. Compounds with a high affinity to banana fiber surfaces may react via hydrogen bonding or electrostatic interactions. The following modifying agents were initially evaluated: cetrimonium bromide (CTAB), tween 80, sodium dodecyl sulfate (SDS), gelatin, and polyethylenimine (PEI). In this screening experiment, CTAB represented a cationic surfactant with a positive charge, tween 80 represented a nonionic surfactant with no charge, SDS represented an anionic surfactant with negative charge, gelatin and PEI each represented polymers. Samples of degummed banana fibers were surface treated by soaking in solutions of their respective modifiers and characterized by FT-IR.

[0121] Next, epoxytrimethylammonium chloride (ETMAC) was used to pretreat freshly degummed fibers prior to soaking the fibers in modifying agents. ETMAC was expected to bond covalently to the fibers allowing for a more stable reaction between the banana fibers and the modifying agents. For this experiment, butyric acid (BA), benzenesulfonic acid (BSA), and dodecylbenzenesulfonic acid (DBSA) were also evaluated as surface modifiers. Fibers that had been treated with ETMAC exhibited a more “frayed” appearance compared to fibers that had not been treated with ETMAC. Soaking the fibers for 1-2 hours in the modifying agents produced fibers with brighter and more smooth surfaces, while fibers that had been soaking for 22 hours were too dry. Butyric acid was the best candidate in improving the feel of smoothness with the fibers, while CTAB worked the best on the overall surface modification. FIGS. 1A and 1 B show exemplary FTIR spectra obtained from a bundle before and after treatment with CTAB. The fiber analyzed in FIGS. 1 A and 1 B was sample 10 from the experiment described in Example 3 below. As can be seen from the FTIR spectra, a peak at around 1245 cm’ ¹ appears, likely due to stretching of C-N in the CTAB.

[0122] Lastly, surface coating with biopolymers such as gelatin, gluten, and gum arabic was evaluated to determine their impact on the texture of banana fibers. Previously degummed banana fibers were first allowed to soak in 1 wt% glycerin overnight before spray coating with either gelatin, gluten, or gum arabic. The fibers were allowed to dry at 40 °C and were characterized by FTIR. Polymer coating improved the flexibility of the fibers but there remains opportunity for optimizing the polymer choice. In the future, a two-step schema should be used to produce the desired texture of banana fiber Step 1 - Modification with small non-polymeric compounds with an oily moiety and high affinity to fiber surfaces. Step 2- Polymeric coating by physical or chemical reactions to overcome the natural rough texture of the banana fibers while also maintaining its flexibility.

Example 3: Degumming DOE Evaluation

[0123] The purpose of this study is to evaluate the relationships of several processing variables on the properties of de-gummed banana fiber.

[0124] A design of experiments (DOE) was used to manipulate the following 8 variables and determine their effect on the response variable of fiber dusting: sulfuric acid concentration, pre-soak time, pre-soak temperature, sodium hydroxide concentration, hydrogen peroxide concentration, magnesium sulfate concentration, AHP bath temperature, and AHP bath time. The dusting is suspected to be undissolved lignin. In respect of time and resources, a 1/16 fractional factorial screening DOE was used to complete a total of 16 experiments.

[0125] The low and high values for each factor in the DOE are listed in Table

1. Table 1 : Low and high values for factors impacting degumming properties.

[0126] Method: Sixteen 30 g raw banana fiber bundles were weighed, rinsed, and finger detangled prior to starting the degumming process. The degumming process was completed in multiple phases including an acid pre-soak (phase I) and an alkaline hydrogen peroxide orAHP treatment (phase II).

[0127] In phase 1, 1000 mL of tap water was transferred into a glass beaker. An appropriate amount of sulfuric acid solution was added to the beaker as described in Table 2 below. The solution was heated on a hot plate to the appropriate temperatrue described in Table 2. Once the final temperature was reached, a 30 g banana fiber bundle was loaded and allowed to soak for the appropriate time as described in Table 2. Fibers were removed from the beaker, rinsed under lukewarm tap water, and set aside for phase II.

[0128] In phase II, 1000 mL of tap water was transferred to a glass beaker. The appropriate amount of magnesium sulfate was weighed into the beaker per Table 2. The appropriate amount of sodium hydroxide was weighed into the beaker as described in Table 2. An appropriate amount of hydrogen peroxide solution (30%) was transferred into the beaker as described in Table 2. The solution was heated on a hot plate to the appropriate temperature. Once the final temperature was reached, pre-soaked fibers were added and allowed to soak for the appropriate time as described in Table 2 below. Fibers were then removed from the beaker, rinsed under lukewarm tap water, and set aside to be labeled for testing.

Table 2: Partial factorial design with a total of 16 trials

[0129] Each sample was analyzed to obtain FTIR spectra, linear densities, fiber characterization and content, and for color and texture. Color and texture were measured subjectively using the scale in Table 3. Table 3: Subjective measurements of color and texture.

[0130] The final results are shown in Table 4.

Table 4: Summary of DOE results.

[0131] MiniTab software was used to analyze DOE data using the response factors of color, texture, linear density, cellulose content, lignin content, and xylan content. The results are shown in FIGS. 2A-2F.

[0132] Conclusion: Human hair has an average linear density of 0.0065 g/m or 6.5 tex. The DOE samples tested have linear density values that range from 1 - 13 tex. The degumming process had a significant impact on the linear densities. Additional treatments such as dyeing and softening are likely to impact linear density values as well.

[0133] High cellulose content (>75%) is a result of over-processed bundles. The acid pre-soak temperature was the major factor impacting cellulose content. The ideal cellulose content appears to be between 40-65%; therefore, by adjusting the temperature of the acid pre-soak, the desired cellulose levels may be achieved.

[0134] Xylan (hemicellulose) content was most impacted by acid pre-soak time and temperature. High temperatures during this step may result in lower xylan content. Therefore, the temperature and soak time during this step may be adjusted to achieve the desired xylan levels, i.e., less than 15%.

[0135] Lignin content was most impacted by sodium hydroxide concentration; therefore the pH at the AHP step may be adjusted to achieve the desired lignin levels, i.e., less than 10%.

Example 4: Boiling after AHP Treatment

[0136] The effect of adding a boiling step after the AHP treatment (instead of before the acid pre-soak) and increasing the sodium hydroxide concentration in the AHP treatment to 0.4% was evaluated. A 156 g bundle was prepared. The bundle was placed in an acid pre-soak solution at a pH of 1.17 and a temperature of 50°C for two hours. The AHP soak was then performed at a pH of 11 .25 at a temperature of 75°C for 10 minutes. The bundle was then placed in boiling water for 15 minutes. The bundle was then rinsed, shampooed, conditioned, and detangled. The bundle was allowed to dry in an oven for 1 hour at 75°C, and then finished air drying overnight. The bundle was then evaluated for quality control.

[0137] The additional boiling step after the AHP soak appeared to slightly decrease the brightness of the fibers. Therefore, it was recommended to perform the boiling step before the acid pre-soak solution.

Example 5: Multifactor Degumming Experiment

[0138] Several factors were tested in an attempt to improve the degumming process. The sample and the description of the factor tested are shown in Table 5.

Table 5: Factors tested in degumming process. [0139] Each bundle weighed 25 g and was cut to a length of 30 cm. The acid pre-soak was conducted with a 0.4% sulfuric acid solution at a 100°C for 25 minutes for Samples A-D. Sample E was soaked in tap water at 100°C for 25 minutes.

[0140] Next, Sample C was soaked in an alkaline solution comprising 0.25% NaOH at 100 °C for 15 minutes. Samples A, B, D, and E were not soaked in an alkaline solution.

[0141] Samples A and C-E were soaked in an alkaline hydrogen peroxide solution that contained 0.25% NaOH and 1.30% H2O2 at 100°C for 2 minutes. Sample B was soaked in a solution containing 0.25% NaOH and 5% H2O2 at 100°C for 2 minutes.

[0142] After the alkaline hydrogen peroxide soak, Sample D was boiled in tap water at 100°C for 2 minutes.

[0143] Each bundle was then rinsed, shampooed, conditioned, and detangled. The bundles were dried in the oven for 1 hour at 75°C, and then air dried overnight.

[0144] The bundles are shown in FIGS. 3A-3E. Sample B showed improved softness and brightness as compared to the control sample; however, Samples C-E all showed a decrease in brightness. The level of dusting of each sample was comparable to the control.

Example 6: Acid Pre-Soak Evaluation

[0145] Different acids were tested for use in the acid pre-soak solution as alternatives to sulfuric acid. The acid pre-soak was conducted with 100 g of banana fiber. Sulfuric acid was replaced with acetic acid at a concentration of 7.33% to achieve a pH of 3.0. The temperature of the pre-soak solution was decreased to 60°C and the soak time was increased to 60 minutes. After the acid pre-soak, the fiber underwent an alkaline hydrogen peroxide soak, rinse, shampoo, conditioning, and detangling as described herein. The banana fiber was then allowed to dry in a drying oven for 3.5 hours at 75°C.

[0146] The fiber that underwent an acetic acid pre-soak showed an increase in dusting compared to previous samples. However, there was a noticeable decrease in the shedding of shorter fiber strands and fiber breakage. [0147] In an additional experiment, sulfuric acid was used but at a lower concentration (0.01 wt%) to give a pH of about 3.25. Three 50 g bundles were soaked at 75°C for 1 hour, 2 hours, and three hours. After the acid pre-soak, the bundles underwent an alkaline hydrogen peroxide soak, rinse, shampoo, conditioning, and detangling as described herein. The bundles were then allowed to dry in a drying oven for 3.5 hours at 75°C.

[0148] The reduced concentration of sulfuric acid resulted in insufficient degumming of the banana fiber, and the dried fibers appeared dustier. Additionally, longer pre-soak times did not improve the degumming.

Example 7: Stabilizer and Acid Pre-Soak Evaluation

[0149] Magnesium sulfate (MgSC ) is used as an alkaline-peroxide stabilizing agent to slow down the degradation of peroxide and to prevent the formation of free radicals. The purpose of this experiment is to evaluate the impact of increasing MgSC concentration to 0.25%. In addition, this experiment will also evaluate the impact of replacing NaOH with Na2COs, replacing the acid pre-soak with an alkaline step that is neutralized with sulfuric acid after an initial 1 hour soak time, and replacing sulfuric acid with glycolic acid.

[0150] Five 25 g bundles of banana fiber were prepared according to the conditions outlined in Table 6. The bundles were then rinsed, shampooed, softened, conditioned, and dried.

Table 6: Sample preparation for stabilizer and acid pre-soak evaluation

[0151] The bundles are shown in FIGS. 4A-4E. All samples passed quality control testing. Dusting was not completely eliminated from any sample, although samples C and D appeared to have fewer dust particles remaining on the fibers compared to the other samples.

[0152] Next, alkali solutions were prepared to determine whether other alkali solutions could improve dusting in the fibers. Three alkali solutions were tested: ammonium hydroxide, sodium hydroxide, and sodium carbonate.

[0153] Sample A was treated by first preparing 100 mL of a solution of 1 % ammonium hydroxide having a pH of 11.3. The solution was heated to 75°C. 0.1 g of dust from banana fibers was transferred into the solution and allowed to soak for 1 hour. After 1 hour, the dust particles had not dissolved in the solution. An additional 200 mL of water and 16 mL of 28% ammonium hydroxide was added to the solution. The solution was then heated to 100°C for another hour. Significant dust particles still remained in the solution.

[0154] Sample B was treated by first preparing 100 mL of a solution of 1 % sodium hydroxide having a pH of 11.6. The solution was heated to 75°C. 0.1 g of dust from banana fibers was transferred into the solution and allowed to soak for 1 hour. After 1 hour, the dust particles had not dissolved in the solution. An additional 200 mL of water and 4 g of sodium hydroxide was added to the solution. The solution was then heated to 100°C for another hour. After 1 hour, there was a significant reduction in the amount of dust particles in the solution.

[0155] Sample C was treated by first preparing 100 mL of a solution of 1 % sodium carbonate having a pH of 10.8. The solution was heated to 75°C. 0.1 g of dust from banana fibers was transferred into the solution and allowed to soak for 1 hour. After 1 hour, the dust particles had not dissolved in the solution. An additional 200 mL of water and 4 g of sodium carbonate was added to the solution. The solution was then heated to 100°C for another hour. Significant dust particles still remained in the solution.

[0156] Thus it was concluded that boiling the dust particles in a solution of sodium hydroxide was able to remove most dust particles.

Example 8: Enzyme Evaluation

[0157] The use of enzymes to degum banana fibers was evaluated. Preparation of Samples A-E is shown in Table 7.

Table 7: Sample preparation for enzyme evaluation

[0158] A glycine-NaOH buffer was prepared. Te a 1000 mL volumetric flask, 3.75 g of glycine and 1 .28 g of sodium hydroxide were added, followed by about 800 mL of distilled water. The final pH was adjusted to about 10.0. Additional distilled water was added to bring the solution to 1000 mL.

[0159] Enzyme-1 (alkaline pectinase, 600 U/mL) was prepared by adding 1 mL of alkaline pectinase (60,000 U/mL) to a 100 mL volumetric flask, followed by 80 mL of distilled water. The solution was mixed well, and then distilled water was added to bring the solution to 100 mL.

[0160] Enzyme-2 (alkaline pectinase, 1200 U/mL) was prepared by adding 2 mL of alkaline pectinase (60,000 U/mL) to a 100 mL volumetric flask, followed by 80 mL of distilled water. The solution was mixed well, and then distilled water was added to bring the solution to 100 mL.

[0161] Enzyme-3 (alkaline pectinase, 96 U/mL) was prepared by adding 8 mL of Enzyme-2 to a 100 mL volumetric flask, followed by 80 mL of distilled water. The solution was mixed well, and then distilled water was added to bring the solution to 100 mL.

[0162] Sample A was prepared by weighing 50 g of banana fibers and loading the fibers into a beaker containing 1000 mL of the buffer solution. The buffer solution was then heated to 50°C. Next, 8 mL of Enzyme-1 was added to the beaker. The fibers soaked for 120 min. The pH was measured to be 9.6 throughout the 120 minutes. The fibers were removed and rinsed under lukewarm tap water Then the fibers were loaded into a beaker containing 950 mL of distilled water, 50 mL of hydrogen peroxide, 10 g of soda ash, 2.5 g of magnesium sulfate at a temperature of 90°C. The fibers were soaked for three minutes before rinsing under lukewarm tap water. The fibers were shampooed using a solution containing about 600 mL of tap water, 1 g of commercial dish detergent, and 1 g of soda ash for 10 minutes at a temperature of 60°C. The fibers were rinsed under lukewarm tap water. The fibers were then softened using a solution containing about 600 mL of tap water and 4.25 g of Milsoft for 10 minutes at a temperature of 60°C before rinsing the fibers under lukewarm tap water. The fibers were then conditioned, detangled, and dried in an oven.

[0163] Sample B was prepared by weighing 50 g of banana fibers and loading the fibers into a beaker containing 1000 mL of the buffer solution. The buffer solution was then heated to 50°C. Next, 8 mL of Enzyme-1 was added to the beaker. The fibers soaked for 180 min. The pH was measured to be 9.6 throughout the 180 minutes. The fibers were removed and rinsed under lukewarm tap water. Then the fibers were loaded into a beaker containing 950 mL of distilled water, 50 mL of hydrogen peroxide, 10 g of soda ash, 2.5 g of magnesium sulfate at a temperature of 90°C. The fibers were soaked for three minutes before rinsing under lukewarm tap water. The fibers were shampooed using a commercial laundry detergent. The fibers were rinsed under lukewarm tap water. The fibers were then dried in an oven.

[0164] Sample C was prepared by weighing 5 g of banana fibers and loading the fibers into a beaker containing 95 mL of the buffer solution. The buffer solution was then heated to 50°C. Next, 5 mL of Enzyme-3 was added to the beaker. The fibers soaked for 60 min. The pH was measured to be 9.6 throughout the 60 minutes. The fibers were removed and rinsed under lukewarm tap water. Then the fibers were loaded into a beaker containing 95 mL of tap water, 5 mL of hydrogen peroxide, 1 g of soda ash, 0.25 g of magnesium sulfate at a temperature of 90°C. The fibers were soaked for three minutes before rinsing under lukewarm tap water. The fibers were shampooed using 1 g of commercial dish detergent. The fibers were rinsed under lukewarm tap water and dried in an oven. [0165] Sample D was prepared by weighing 5 g of banana fibers and loading the fibers into a beaker containing 90 mL of the buffer solution. The buffer solution was then heated to 50°C. Next, 10 mL of Enzyme-3 was added to the beaker. The fibers soaked for 60 min. The pH was measured to be 9.6 throughout the 60 minutes. The fibers were removed and rinsed under lukewarm tap water. Then the fibers were loaded into a beaker containing 95 mL of distilled water, 5 mL of hydrogen peroxide, 1 g of soda ash, 0.25 g of magnesium sulfate at a temperature of 90°C. The fibers were soaked for three minutes before rinsing under lukewarm tap water. The fibers were shampooed using a commercial dish detergent. The fibers were rinsed under lukewarm tap water and dried in an oven.

[0166] Sample E was prepared by weighing 5 g of banana fibers and loading the fibers into a beaker containing 85 mL of the buffer solution. The buffer solution was then heated to 50°C. Next, 15 mL of Enzyme-3 was added to the beaker. The fibers soaked for 60 min. The pH was measured to be 9.6 throughout the 60 minutes. The fibers were removed and rinsed under lukewarm tap water. Then the fibers were loaded into a beaker containing 95 mL of distilled water, 5 mL of hydrogen peroxide, 1 g of soda ash, 0.25 g of magnesium sulfate at a temperature of 90°C. The fibers were soaked for three minutes before rinsing under lukewarm tap water. The fibers were shampooed using a commercial dish detergent. The fibers were rinsed under lukewarm tap water and dried in an oven.

[0167] The Bundles are shown in FIGS. 5A-5E. Processing the raw banana fibers with alkaline pectinase + alkaline peroxide sufficiently degummed and softened the fibers. However, excessive dusting was still present. Additional evaluation is required to determine if combining alkaline peroxidase with additional enzymes such as lignin peroxidase or polygalacturonase will completely eliminate dusting.

Example 9: Sealing Evaluation

[0168] The sealing of the banana fibers was evaluated to improve the performance of the synthetic hair and to eliminate dusting. It was believed that adding glycerin or other humectants to the fibers reduced friction and improved the softness of the fibers. [0169] About 15 swatches of degummed banana fibers were weighed (about 25 g damp weight). The bundles were folded in half and secured with a hair tie to form fanned swatches. Glycerin was applied to each swatch in the amounts shown in Table 8 below.

Table 8: Sample preparation for sealing evaluation

[0170] Each swatch was then sealed with a commercial detangling spray and allowed to air dry overnight. Each bundle was then evaluated for quality control.

[0171] Sample C showed the most favorable characteristics, having the least amount of shedding and the most “bounce-back”; i.e., decreased stiffness and increased flexibility and softness.

[0172] Next, three 156 g degummed bundles were prepared and towel dried. Glycerin and the emergency detangling spray were added in the amounts shown in Table 9. Each bundle was then dried in a convection oven at 75°C for 150 minutes. The bundles were then allowed to air dry over the weekend, and were evaluated for quality control.

Table 9: Sample preparation for follow-up sealing evaluation

[0173] Although all samples passed quality inspection, Sample Ayielded the best results, having increased softness, increased flexibility, and decreased shedding of shorter fiber strands.

Example 10: Sealant

[0174] Sealants were tested to replace the commercial detangling solution used. The sealant was prepared according to Table 10.

Table 10: Sample preparation for sealant evaluation

[0175] The commercial sealant #1 was combined with grapeseed oil and mixed well, followed by isopropyl palmitate, commercial sealant #2, and isododecane which were mixed well. The solution was heated in a water bath at a temperature of about 70-80°C and stirred to mix thoroughly. The mixture was slightly cloudy, possibly due to the grapeseed oil.

[0176] A 3 g sample of banana fiber was rinsed under lukewarm water and allowed to soak in a jar of water. The sample was removed and excess water was squeezed out. 1.5 g of glycerin was added to the sample and combed through, followed by 0.5 g of sealant mixture. The sample was dried in an oven at 75°C for 30 minutes.

[0177] Meanwhile, eight 10 g samples of banana fiber were prepared and rinsed under lukewarm water, then allowed to soak in a jar of water. The samples were removed from the jar and excess water was squeezed out. Glycerin and the sealant mixture were applied according to Table 11 . Each sample was then dried in a convection oven at 75°C for 30 minutes. The samples were then evaluated for quality control.

Table 11 : Application of Sealant

[0178] Fully saturating the fibers with high concentrations of glycerin and sealant prior to drying them offered the best results. High concentrations of glycerin without any sealant (sample E) resulted in a sticky texture. Applying sealant without any glycerin (Sample D) did not result in the desired levels of softness and flexibility.

Example 11 : Softening Process

[0179] The recommended softening schema post-shampoo involves treatment with a cationic surfactant, followed by treatment with a humectant, followed by treatment with a sealant. The scope of this project was to identify the best cationic surfactant intended to replace Milsoft as the softening agent. Additionally, it was desired to improve the long-term flexibility of the fibers and to decrease their stiffness by optimizing the humectants and polymers used in the formulation.

[0180] First, an experiment was conducted to evaluate the impact of treating blonde, and black dyed bundles with different types of cationic surfactants. Black bundles were separated into 30 g sample sizes. 350 g of water was weighed into a beaker and heated. 3.5 g of each surfactant listed in Table 12 was weighed and dissolved in water. Each bundle was allowed to soak in the surfactant solution for 30 minutes, after which the sample was removed and squeezed to remove excess water. The samples were then allowed to dry overnight.

Table 12: Black Bundle Softeners

[0181] The same process was repeated for blonde bundles. The materials are shown in Table 13.

Table 13: Blonde Bundle Softeners

[0182] Judging softness based on the damp feel of each bundle, samples C and E for black produced the best results and samples C and E for blonde produced the best results. Based on the air-dried feel of each bundle, samples C, E, and F produced the best results for black and samples C, D, and E produced the best results for blonde.

[0183] A second experiment was conducted to evaluate the impact of treating blonde and black dyed bundles with different types of cationic surfactants in combination with a humectant and sealant. First, black and blonde bundles were separated into 25 g samples. 300 g of water was weighed into a beaker and heated to 75°C. The surfactant (softener) was weighed into a beaker and dissolved in water. The samples were allowed to soak in the surfactant solution for 30 minutes. The samples were removed from the solution and squeezed to remove excess water. The humectant was then applied to each sample. The samples were detangled and allowed to dry. Table 14 shows the surfactant and humectant used in each sample.

Table 14: Black Bundle Humectants [0184] The process was repeated for the blonde bundles. The humectants are shown in Table 15.

Table 15: Blonde Bundle Humectants

[0185] Judging softness based on the damp feel of each bundle, samples L, M, and N for black produced the best results and samples L, M, and N for blonde produced the best results. Based on the air-dried feel of each bundle, samples L and N produced the best results for black. Sample M had a noticeable white residue once dried. Samples L, M, and N produce the best results for blonde based on air-dried feel of the samples. Therefore, it was determined that soaking bundles in a solution of 5% quaternium-31 immediately after the shampoo step produced the best results.

[0186] A third experiment was conducted to evaluate the impact of treating full-sized blonde, and black dyed bundles with different concentrations of Quaternium-31 surfactant. 1500 g of water were weighed into a beaker and heated to 60°C. The Quaternium-31 was weighed and dissolved into the water. Bundles were allowed to soak in the surfactant solution for 30 minutes. The bundles were then removed and squeezed to remove excess water. 50 g of glycerin was then applied to each bundle. The bundles were detangled and 10 g of sealant was applied to each bundle. The bundles dried in an oven at 80°C for 30 minutes. A description of each sample is provided in Table 16.

Table 16: Softening Optimization

[0187] Higher concentrations of Quaternium-31 produced softer and more manageable the bundle. Although 5% quat- 31 produced the softest bundles, using Quaternium-31 at a level as low as 1 % produced bundles with sufficient softness.

[0188] A fourth experiment was conducted to evaluate the performance of bundles treated with Quaternium-31 (dicetyldimonium chloride). Bundles prepared using the Quaternium-31 were formed into 4 braids and installed into a mannequin’s hair. After the braids were installed, the braids were dipped in hot water and a commercial mousse was applied. The results are described in Table 17.

Table 17: Performance of Braids without applying Quaternium-31. [0189] Three 10 g samples of blonde bundles were prepared. The bundles were shampooed and conditioned according to Table 18 below. The samples were dried in a convection oven at 80°C for about 25 minutes.

Table 18: Performance of bundles after shampoo and conditioning.

[0190] Next, three 10 g black samples were prepared and braided. A chlorine bath including water and 3 ppm chlorine was prepared with a pH of 7.2 to simulate use of the hair in a swimming pool. Each sample was tested in a different chlorine bath. The first sample was used as a control. The second sample was added to the chlorine bath, which was heated to a temperature of 25°C. The sample soaked in the bath for 30 minutes. The sample was removed from the bath and blotted with a paper towel. The third sample followed the same procedure, except that the chlorine bath was heated to a temperature of 37°C. The results are shown in Table 19. Table 19: Chlorine evaluation

[0191] It was concluded that dipping braids in hot water after braiding caused the ends to dry out and become hard, while applying a mousse helped to tame the fly-aways and keep the braids conditioned. Chlorine had no impact on the color ofJET braids and there was no color bleeding or transfer from wet braids. Therefore, activities such as swimming are not expected to impact the quality of the braided styles. The blonde swatches had a great wet feel after shampoo with excellent slip and more manageable wet combing compared to the control, however it became hard and dried out after drying in the oven. The swatches remained soft and smooth after applying a conditioner immediately after shampooing and applying a sealant when the swatches were nearly dried. Therefore, it was recommended to apply a conditioner and hair oil to bundles if the customer wishes to shampoo or re-use their bundles. Example 12: Characterization of banana fiber hair extensions at different stages via glycosyl composition with and without acetylation, glycosyl uronic acid linkage and ¹ H-NMR

[0192] An experiment was conducted to determine the cause of dust buildup observed in the product. This work was supported by GlycoMIP, a National Science Foundation Materials Innovation Platform funded through Cooperative Agreement DMR- 1933525.

[0193] Banana fibers were cut with scissors and placed in a mortar and pestle. Liquid nitrogen was added, and the sample was ground. The ground sample was then placed in a ceramic bead microtube and placed in a bead ruptorwith 500pl of water. The processed sample was then frozen and lyophilized.

[0194] Uronic Acid Glycosyl Linkage Analysis: Glycosyl linkage analysis was performed by combined gas chromatography-mass spectrometry (GC/MS) of the partially methylated alditol acetates (PMAAs) derivatives produced from the samples. The procedure is a slight modification of the one described by Willis et al. (2013) PNAS, 110 (19) 7868-7873, incorporated by reference herein.

[0195] First, to improve the solubility of the samples, they were dissolved in 1-Ethyl-3-methylimidazolium acetate [Emim][Ac] and acetylated using acetic anhydride and 1 -methyl imidazole. The samples were then extracted with dichloromethane (DCM), and the dried samples were dissolved in dimethyl sulfoxide (DMSO). Methylation of the samples using dimsyl potassium base was performed. The samples were again extracted with dichloromethane, and the carboxylic acid methyl esters were reduced using lithium aluminum deuteride in THF (80 °C, 8 h). Dialysis (1 kDa MWCO in 0.1 % acetic acid, 4 °C for 3 days) was used to desalt the samples after reduction. The samples were then frozen and lyophilized. The dried sample was then redissolved in DMSO for 3 days.

[0196] The sodium hydroxide base was prepared according to the protocol described byAnumula et al. (1992) Analytical Biochemistry, 203 (1 ) 101 -108, incorporated herein by reference. Briefly, to NaOH (50 % w/w, 100 pL) was added of methanol (200 pL, MeOH), and the mixture was vortexed. Then DMSO (2 mL) was added, and the base solution was vortexed and centrifuged. The supernatant solution was removed and fresh DMSO was added. This was repeated 5 times. After the final extraction, DMSO (2 mL) was added to the NaOH pellet, and the solution was vortexed. Of this final base solution, 300 pL was added to the sample, and the mixture was magnetically stirred for 15 min. Then, iodomethane (70 pL) was added, and the sample was stirred at room temperature for 20 min. A second round of base (15 min) and then iodomethane (25 min) was added, the sample was then dissolved in DCM and washed 5 times with 2 mL of water. The water was removed, remaining DCM dried off under a stream of nitrogen, and the sample was frozen and lyophilized, after which a third round of base (15 min) and iodomethane (25 min) treatment was performed. Finally, the sample was washed with DCM and water 5 times, the water was removed, the remaining DCM was dried off under a stream of nitrogen, and the residue was lyophilized.

[0197] The permethylated materials were hydrolyzed with 2 M TFA for 2 h at 121 °C and dried down with isopropanol under a stream of nitrogen. The samples were then reduced with NaBD4 in nanopure water overnight, neutralized with glacial acetic acid, and dried with methanol. Finally, the samples were O-acetylated using acetic anhydride (250 pL) and concentrated trifluoroacetic acid (TFA, 250 pL) at 50 °C for 20 min. The samples were dried under a stream of nitrogen, reconstituted in dichloromethane, and washed with nanopure water before injection into GC-MS.

[0198] The resulting PMAAs were analyzed on an Agilent 7890A GC interfaced to a 5975C MSD; separation was performed on a Supelco 2331 fused silica capillary column (30 m x 0.25 mm ID) with a temperature gradient detailed in Table 20. The method is a derivation of the linkage method detailed by Heiss et al.

Table 20: Temperature program for the GC-MS analysis for the PMAA and AA method [0199] 1 -Dimensional 1 H-NMR Spectroscopy: A portion of 3.0 - 4.0 mg of each sample was weighed, dried, and suspended in 600 pL DMSO-d6/pyridinium chloride-d6 (1 %, w/v). Samples were heated at 40 °C for 2 h and each of the supernatant transferred into a 5-mm NMR tube. Liquid ¹ H-NMR data were obtained at 70 °C on a Varian VNMRS spectrometer (1 H, 599.66 MHz). ¹ H-NMR parameters: 60 s relaxation delay, 8992.8 Hz spectral width, 15323 data points and 64 transients with total recycle delay of 2.7 s between each transient. Prior to the Fourier transformation, the data were apodized with an exponential decay function with line broadening of 0.5 Hz, 90° sine square, and zero-filled to 64k points. The baselines were corrected automatically by subtracting a 3rd-order polynomial. The spectra were processed and analyzed with MestreNova (version *64).

[0200] O-acetylation for detection of cellulose: The samples (310 pg-380 pg) were dissolved in [Emim][Ac] with stirring, for three days. The following day, the sample was acetylated with acetic anhydride and 1 -methylimidazole for 10 minutes. Water (1 ml) was added to the sample. The samples were then placed in a 1000-Da dialysis bag and dialyzed against water for 3 days, the water being replaced every 8 h. The sample was then transferred to a new screw-top glass tube and placed on dry ice and lyophilized. The sample was then derivatized by the TMS method described below.

[0201] Glycosyl composition analysis by GC-MS of TMS-derivatized methyl glycosides: Glycosyl composition analysis was performed by combined gas chromatography-mass spectrometry (GC-MS) of the per-O-trimethylsilyl (TMS) derivatives of the monosaccharide methyl glycosides produced from the sample by acidic methanolysis as described previously by Santander et al. (2013) Microbiology 159:1471 , incorporated by reference herein.

[0202] Briefly, the dry sample (290-380 pg) was heated with methanolic HCI in a sealed screw-top glass test tube for 16 h at 80 °C. After cooling and removal of the solvent under a stream of nitrogen, the samples were re-N-acetylated and dried again. The sample was then derivatized with Tri-Sil® (Thermo) at 80 °C for 30 min. GC-MS analysis of the TMS methyl glycosides was performed on an Agilent 7890A GC interfaced to a 5975C MSD, using an Supelco Equity-1 fused silica capillary column (30 m x 0.25 mm ID). The GC temperature conditions are listed below in Table 21.

Table 21 : Temperature program for the GC-MS analysis for the TMS method

Results

[0203] Uronic Acid Glycosyl Linkage Analysis: The chromatograms of the glycosyl linkage analysis are shown in FIGS. 6A-6F, and the results are listed in Table 22. The major linkage in all the samples is 4-linked glucose, but some minor linkages coming from xylose, arabinose, galactose, and mannose were also detected.

[0204] Most of the 4-linked glucose likely originated from cellulose and possibly starch. The 4,6-linked glucose residues could be from hemicellulose or starch. Since xyloglucan is low in monocots (such as banana), most of the 4,6-Glc residues are likely from starch. These residues were elevated in all dust samples, suggesting a higher proportion of starch in the dust samples. The other linkage residues that were detected were probably from other hemicelluloses, such as xylan, arabinogalactan, and mannan.

[0205] The relative increase of 4-linked glucose moving from less to more processed samples. The reason for the increasing percentage of 4-linked glucose may be the result of partial extraction of hemicellulose from the fibers, leaving the insoluble cellulose behind. The dust samples are higher in arabinose and xylose when compared to the regular fibers suggesting that the dust is indeed from arabinoxylan, the major hemicellulose of monocot such as banana plant. Thus, the dusting could be the result of the disintegration of hemicellulose and starch. Table 22: Relative percentage of each detected linkage in the Banana Fiber and Dust samples.

[0206] 1 -Dimensional ¹ H-NMR Spectroscopy: The NMR spectra of the 3 samples are shown in FIGS. 7A-7I. The fiber samples were not totally soluble in the ionic liquid, DMSO-de/pyridinium chloride-de. Therefore, only soluble materials were detectable as shown in the ¹ H-NMR spectra. In summary, all samples contained carbohydrate protons and aliphatic protons. The 3 samples have ¹ H chemical shifts corresponding to anomeric protons of cellulose and/or [3-xylopyranose (H 1 at ~ 4.3 - 4.6 ppm) and of starch or a-arabinofuranose (H1 at ~ 4.9 - 5.3 ppm). Together with the linkage analysis, the NMR spectra indicate the presence of cellulose, arabinoxylan and starch in the samples. Consistent with the fiber processing steps, treated samples degummed and degummed and dyed have less arabinoxylan and starch-like signals, compared to the untreated raw banana sample. The dyed and degummed sample contains strong signals at the sugar ring proton region that may originate from the dye treatment.

[0207] It was noted that the dust samples were more readily resuspended and less sticky in the ionic liquid compared to the fiber samples, consistent with a higher presence of hemicellulose. The fact that the starch content decreased, but the 4-linked glucose increased with more processing suggests that the enrichment of cellulose is larger than what the linkage analysis indicated.

[0208] The Degummed and Dyed Banana Fiber sample contained a large set of peaks that were labeled "non-carbohydrate". These signals were likely from glycerol. However, glycerol could not be detected in the linkage analysis.

[0209] TMS Glycosyl composition analysis: The chromatograms of the TMS glycosyl composition analysis are shown in FIGS. 8A-8M, and the results are listed in Tables 23-24. FIGS. 8B-8G are for the O-acetylation results and FIGS. 8H-8M are for the regular TMS analysis without acetylation. The O-acetylation increased the solubility of cellulose in samples, leading to higher glucose and lower arabinose and xylose percentages. Because glucose comes from both starch and cellulose, these results were difficult to interpret. Between the dust samples and fiber samples after O-acetylation, the dust samples contained higher levels of arabinose and uronic acids. In the Raw Dust sample, the relative proportions of xylose decreased, while those of glucose increased relative to the Raw sample. In the Dyed Dust sample, xylose slightly increased, and glucose decreased when compared to the Dyed Fiber sample; however, the dyed fiber sample had an abnormally high glycerol peak that may have interfered with the results.

[0210] In the regular TMS results without O-acetylation, cellulose was essentially not detected, and this enabled assessment how much of the glucose came from starch. The glucose and thus starch in the Raw Dust sample was much higher than in all the other samples, indicating that the dust coming from the raw untreated fiber consisted mostly of starch, whereas the dust from the degummed and from the dyed and degummed fibers had a higher hemicellulose content.

Table 23: Quantitation and mole percentage of monosaccharides present in the 0- acetylated Banana Fiber samples.

Table 24: Quantitation and mole percentage of monosaccharides present in the non-acetylated

Banana Fiber samples.

Conclusion

[0211] The data indicate that the dusting comes mainly from the presence of starch and hemicellulose in the fiber samples. These polysaccharides possess less physical strength than cellulose and can more easily disintegrate. The degumming and dyeing processes likely remove some of the starch and hemicellulose, so that the samples thus treated produce less dust.

[0212] Having described the invention in detail, it will be apparent that modifications and variations are possible without departing from the scope of the invention defined in the appended claims.