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Title:
MELALEUCA ALTERIFOLIA PLANT BASED ANTIMICROBIAL FINISH ON FABRICS AND METHOD THEREOF
Document Type and Number:
WIPO Patent Application WO/2022/003731
Kind Code:
A1
Abstract:
The present invention relates to an anti-microbial finish on the fabrics. The present invention particularly relates to an antimicrobial microencapsulated fabric finish composition comprising Melaleuca alterifolia oil or tea tree oil. The invention relates to microcapsules of Melaleuca alterifolila microcapsules with Melamine as coat. Further the invention relates to method of finishing of fabric with antimicrobial composition of tea tree oil microcapsules, to provide a durable and anti-microbial fabric, wherein the fabric is preferably terry towel and woven plain fabrics like sheetings and bed linen.

Inventors:
DEVARAJ VIKRAM KRISHNA (IN)
Application Number:
PCT/IN2021/050650
Publication Date:
January 06, 2022
Filing Date:
July 03, 2021
Export Citation:
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Assignee:
DEVARAJ VIKRAM KRISHNA (IN)
International Classes:
A61K36/61; D06M13/224
Foreign References:
DE102007010109A12008-09-04
US20100119461A12010-05-13
Other References:
SATHIANARAYANAN, M P ET AL.: "Antibacterial finish for cotton fabric from herbal products", INDIAN JOURNAL OF FIBRE & TEXTILE RESEARCH, vol. 35, pages 50 - 58, XP055227205
Attorney, Agent or Firm:
RAVINDRAN, Sudhir Raja et al. (IN)
Download PDF:
Claims:
I CLAIM:

1. An antimicrobial microencapsulated fabric finish composition, comprising of: microcapsules of Melaleuca alterifolia (tea tree oil) and melamine in the ratio of 1:4 and 2:5 by volume.

2. The antimicrobial microencapsulated fabric finish composition as claimed in claim 1, wherein the Melaleuca alterifolia (tea tree oil) comprises of the core and is of 100% concentration with terpen-4-ol as the anti-microbial ingredient.

3. The antimicrobial microencapsulated fabric finish composition as claimed in claim 1, wherein the microcapsules have a particles size in range of 5-30pm.

4. The antimicrobial microencapsulated fabric finish composition as claimed in claim 1, wherein the microcapsule composition for application comprises a solution of microcapsules and binder in the ratio of 1:1 (2% w/v) in deionized water.

5. The antimicrobial microencapsulated fabric finish composition as claimed in claim 1, wherein the binder is selected from polyurethane, melamine, acrylic styrene copolymer, polyvinyl alcohol, acrylic polymer, and polyethylene.

6. The antimicrobial microencapsulated fabric finish composition as claimed in claim 1, wherein the binder is a salt of polyacrylic acid.

7. A method of coating a fabric with microencapsulated Melaleuca alterifolia oil antimicrobial composition, comprising steps: dissolving antimicrobial composition of microencapsulated Melaleuca alterifolia oil or tea tree oil in deionized water (2% w/v) and dissolving binder (AGL 502) in water 2% w/v solution at 70°C; addition of this antimicrobial composition to dosing tank and dosing for a period of 20 min at a pH of 6-6.5 for exhaustion of the binder causing fixation of the tea tree oil microcapsules to the fabric; raising the temperature to 60°C; application of hydrophilic softener added to final bath at 40 °C at pH 5 - 6.0 for complete exhaustion and run for 30 min; unloading of the treated fabric from dyeing machine and loaded in the hydro extractor to take excess moisture out; passing the fabric through rope opener; and drying the fabric in a drying chamber at 100 -120 °C till the fabric is completely dry, wherein curing of Melamine is devoid of high temperature (160-180°C).

8. The method of coating a fabric with microencapsulated Melaleuca alterifolia oil antimicrobial composition as claimed in claim 7, wherein the concentration of the microencapsulated Melaleuca alterifolia oil or tea tree oil for antimicrobial activity is 2% by weight of fabric.

9. The method of coating a fabric with microencapsulated Melaleuca alterifolia oil antimicrobial composition as claimed in claim 7, wherein the softener is cationic and silicone based softener.

10. The method of coating a fabric with microencapsulated Melaleuca alterifolia oil antimicrobial composition as claimed in claim 7, wherein the pH is maintained by addition of Glacial acetic acid (0.1 gpl) and Core alkali remover 0.2 gpl).

Description:
MELALEUCA ALTERIFOLIA PLANT BASED ANTIMICROBIAL FINISH ON

FABRICS AND METHOD THEREOF

FIELD OF THE INVENTION:

The present invention relates to the field of textiles. More particularly, relates to a durable anti microbial finish on the fabrics. The present invention particularly relates to an anti-microbial composition of tea tree oil extract and provided as an anti-microbial durable finish coat on the fabrics such as terry towels and woven plain fabrics. The present invention also relates to a method for fabric finish with antimicrobial composition of tea tree oil to provide a durable and antimicrobial fabric such as terry towel and plain woven fabrics.

BACKGROUND OF THE INVENTION

Certain investigations on medicinal plants provide a clue that herbal drugs can be effectively utilized for identifying their additive or potentiating effects in appropriate areas. The present invention goes by this approach and seeks to explore the synergistic / potentiating or additive effects of medicinal plants to address the issue of bacterial resistance.

The tea tree oil is distilled from the leaves of the Melaleuca alternifolia plant is known since ages for its health care benefits. The oil possesses antibacterial, anti-inflammatory, anti-viral and anti-fungal properties. A person can treat acne, athlete’s foot, contact dermatitis or head lice using tea tree oil mostly from leaves.

Tea tree oil comes from the leaves of Melaleuca alternifolia, a small tree native to Queensland and New South Wales, Australia.

Although Melaleuca alternifolia is known as the tea tree, it should not be confused with the plant that produces leaves used to make black, green and oolong tea.

Tea tree oil has been used as a traditional medicine by Aborigines for centuries. These native Australians crush tea tree leaves to extract the oil, which is then inhaled to treat coughs and colds or applied directly to the skin for healing.

Today, tea tree oil is widely available as a 100% undiluted or “neat” oil. Diluted forms are also available, ranging from 5 - 50% strength in products designed for the skin. Tea tree oil contains a number of compounds, including terpinen-4-ol, which has been shown to kill certain bacteria, viruses and fungi.

Terpinen-4-ol also appears to increase the activity of your white blood cells, which help fight germs and other foreign invaders. These germ fighting properties make tea tree oil a valued natural remedy for treating bacterial and fungal skin conditions, preventing infection and promoting healing.

Tea tree oil is distilled from the leaves of the Melaleuca alternifolia plant, found in Australia.

The oil possesses anti-bacterial, anti-inflammatory, anti- viral and anti-fungal properties. A person can treat acne, athlete’s foot, contact dermatitis or head lice using tea tree oil. The oil has been used for almost 100 years as a healing treatment in Australia, particularly for skin conditions. Today, it is used for a number of conditions. Tea tree oil is probably best known for its anti-bacterial activity.

CN102517914A discloses preparation method with towel that purifies skin by adding tea tree ethereal oil is put into polyurethane, add water, microencapsule solution, dispersant, adhesive, softener and applied on the yarn. Process. Tea Tree oil treated yam is dried at 80 - 100 Deg C at 3 - 5 min followed by curing at 140 - 160 Deg Celsius. Cotton Fiber is put into plasma processing to handle 1 - 7min under the condition of 0 -0.078Mpa in vacuum. Micro encapsule is applied in yarn stage and woven as terry towels.

EP2898774A1 discloses Composition of treatment of textile materials comprising Active Components. Quartenary ammonium compound comprising hydroxypropyltrimonium + X moiety and a carbohydrate moiety. Synthetic organic chemical. Not Ecofriendly.

CN105544230B discloses a method of using tea tree ethereal oil microcapsulation flavoring on the textile Key active components. Composition of both cyclodextrin / tea tree oil.

CN10314731 IB discloses Tea Tree oil microcapsule antibacterial health care fiber and preparation method thereof. The preparation method comprises the following steps of 1, preparing tea tree oil emulsified dispersion liquid; 2, preparing a mixed dispersion system of core materials and wall materials; 3, enabling the mixed dispersion system of the core materials and the wall materials to be subject to complex coacervation reaction; 4, preparing tea tree oil microcapsule dispersion liquid; 5, preparing tea tree oil microcapsule antibacterial healthcare fiber finishing agent; and 6, preparing antibacterial healthcare fabrics which load tea tree oil microcapsules: using the prepared tea tree oil microcapsule antibacterial healthcare fiber finishing agent for the pretreatment or post-treatment of the fabrics to obtain the antibacterial healthcare fabrics which load the tea tree oil microcapsules.

CN105220500A discloses preparation method of novel tea tree essential oil microencapsules finishing agent and application thereof. No durability mentioned. Its preparation method comprises following operating procedure: the first step: prepare tea tree ethereal oil microcapsules; Second step: prepare tea tree ethereal oil microcapsule dressing agent. It discloses the application of tea tree ethereal oil microcapsules dressing liquid in the post finishing process of textiles simultaneously.

CN1060494059A discloses a fabric Antibacterial finishing agent and preparation method thereof. Key active components: Chitosan 5 -8 %, 13 to 15 % sodium Alginate 0.5 % to 1.0 % Nickel Salt, 5 to 8% of tea tree oil essential 3 to 6 parts of poly ethylene glycol and 50 - 70 % water. This is a mixture of Tea tree oil and Synthetic product with heavy metal like Nickel. This is a combination of inorganic and synthetic organic based.

CN105926271A discloses a fabric Antibacterial finishing agent and preparation method thereof Key active components chitin - 5 - 8 %, nickel salt 0.5 - 1.0 % tea tree oil - 5 -8 5 %, poly ethylene glycol 3 - 6 % water 50 - 70 % This composition is synthetic organic and having inorganic based heavy metal.

CN103643491A discloses a method for functionality finishing fabric by adopting natural extract. Tea tree washing, drying and smashing the tea tree fruits dissolving the tree fruit powder into a solvent.

US2004/0115233A1 discloses a composition of improving skin environment clothes thereof. Key active components: Tea tree oil, lemon scented tea tree oil and gama linolenic acid and Beta linolenic acid. This is a combination of Natural and Organic based components.

US9719058B2 Fragrant oil encapsulation. The invention relates to microcapsules having a particle size distribution that has at least two maxima, wherein the main maximum of the particle size lies in the range of 5 to 100 pm and wherein the volume assumed by the microcapsules that have a particle size less than ¼ of the particle size of the main maximum is greater than approximately 20% of the total volume of the microcapsules.

CN107620145 Kind of super abrasive antibacterial quilt Raw material composition Tencel -40 - 50 % , Calcium carbonate 56 , wheat talk 15 20, silk 30 35, lignocellulose 56, paraffin 46, ginger 23, tea tree oil 0.4 and 0.5 soya bean fiber 89. This claim is a combination of more natural fibers and inorganic chemical blends. Tencel fiber has natuarl antimicribial activity.

CN1461214A Compositions for improving the skin environment and clothes thereof. Active raw material composition: Tea tree oil, gamma Linolenic acid or alpha -linolenic acid selected from terpinene -4-alcohol, citral etc Combination of synthetic and Tea tree oil.

CN104179016B A kind of fabric antibiosis composite dope and preparartion. Fabric antibiosis and composite dope made up of following parts. Poly ester resin, 4 -5 parts silver nano Zinc oxide and 0.5 part jade powder form Surface coating comprises of 10 -15 parts PVA, 10 -15 % tea tree oil, 8 -9 part Zinc sulphide, 1-5 butadiene styrene, 1 - 1.3 lipid poly ester, 1 -4 4 part contain magnesium aluminium oxide .All are synthetic with metal based inorganic components.

CN110885717 Natural antibacterial detergent for lady clothes. Raw material composition: Lemon grass essential oil and lauryl arginine ester hydrochloride. Ratio is 0.09; 0.05; 0.2. This is a combination of natural and synthetic products.

US2017/0275472al antimicrobial coating for long term disinfection of surfaces. Key active components. Combination of inorganic and organic components Inorganic components. Components selected from group consisting of chlorine dioxide, hydrogen peroxide, peroxy acids, alcoholic components etc inorganic materials selected from metal oxides, metal complexes Organic materials like poly vinyl alcohol, Ethylene glycol, propylene glycol, glycerol diproylene, glycol etc . In addition tea tree oil is added as natural antimicrobial component with metal oxide component etc.

WO2013159216A1 Coatings, coated surface, and method of production thereof. Combination of inorganic and organic components Key composition of antimicrobial surface. Copper or copper alloy metal oxides of Silver ions, Zinc ions etc and organic polymer containing antimicrobial components like tea tree oil, quaternary ammonium components, benzimidazoles, isothiazolinones etc. This is a combination of inorganic and synthetic organic based. All metal based components are non bio degradable.

WO20 11/081899A1 Antimicrobial surface and surface coatings. Key active components. An antimicrobial surface and surface coatings include an antimicrobial surface on an object. The antimicrobial material includes a metallic material, an epoxy resin, an epoxy hardener, and a surfactant. Antimicrobial component is derived from metal oxides of copper, Zinc, Nickel etc., with epoxy resin and hardener.

Fabric controlled release technology. Key active components: Tea tree oil, insect Repellent Wizard protects LE plus Lemon eucalyptus 1 % to 5 %.

“Ecofriendly antimicrobial finishing of textile using bioactive agents based on natural products” Indian Journal of Fibre and Textile Research 34(3):295-304 by Mangala Joshi discloses Combination of tea tree oil and Terpinen. No details on application methods and durability.

OBJECTS OF THE INVENTION

It is the primary object of the present invention to provide a fabric with anti-microbial property using 100% natural tea tree oil prepared by microencapsulation.

It is another object of the present invention to provide a method for fabric finish with the microencapsulated antimicrobial composition, wherein the tea tree extract is preferably prepared from leaves.

It is another object of the present invention to provide a fabric with insecticidal and mosquito repellent property.

It is another object of the present invention to provide an antimicrobial finish on the fabric.

It is another object of the present invention to provide an antimicrobial finish on the fabric, wherein the fabric is preferably terry towel, woven plain fabrics such as sheet and bed linens and the like.

It is another object of the present invention to provide a durable anti -microbial composition as fabric finish comprising of tea tree extract. SUMMARY OF THE INVENTION

One or more of the problems of the conventional prior arts may be overcome by various embodiments of the present invention.

It is the primary aspect of the present invention to provide an antimicrobial microencapsulated fabric finish composition, comprising of: Melaleuca alterifolia (tea tree oil) and melamine in the ratio of 1:4 and 2:5 by volume.

It is another aspect of the present invention to provide antimicrobial microencapsulated fabric finish composition, wherein the Melaleuca alterifolia (tea tree oil) comprises of the core and is of 100% concentration with terpen-4-ol as the anti-microbial ingredient.

It is another aspect of the present invention to provide antimicrobial microencapsulated fabric finish composition, wherein the microcapsules have a particles size in range of 5-30pm.

It is another aspect of the present invention to provide antimicrobial microencapsulated fabric finish composition, wherein the microcapsule composition for application comprises a solution of microcapsules and binder in the ratio of 1:1 (2% w/v) in deionized water.

It is another aspect of the present invention to provide antimicrobial microencapsulated fabric finish composition, wherein the binder is selected from polyurethane, melamine, acrylic styrene copolymer, polyvinyl alcohol, acrylic polymer, and polyethylene.

It is another aspect of the present invention to provide antimicrobial microencapsulated fabric finish composition, wherein the binder is a salt of polyacrylic acid.

It is yet another aspect of the present invention to provide a method of coating a fabric with microencapsulated Melaleuca alterifolia oil antimicrobial composition, comprising steps: dissolving antimicrobial composition of microencapsulated Melaleuca alterifolia oil or tea tree oil in deionized water (2% w/v) and dissolving binder (AGL 502) in water 2% w/v solution at 70°C; addition of this antimicrobial composition to dosing tank and dosing for a period of 20 min at a pH of 6-6.5 for exhaustion of the binder causing fixation of the tea tree oil microcapsules to the fabric; raising the temperature to 60°C; application of hydrophilic softener added to final bath at 40 °C at pH 5 - 6.0 for complete exhaustion and run for 30 min; unloading of the treated fabric from dyeing machine and loaded in the hydro extractor to take excess moisture out; passing the fabric through rope opener; and drying the fabric in a drying chamber at 100 -120 °C till the fabric is completely dry, wherein curing of Melamine is devoid of high temperature (160-180°C).

It is another aspect of the present invention to provide a method of coating a fabric with microencapsulated Melaleuca alterifolia oil antimicrobial composition, wherein the concentration of the microencapsulated Melaleuca alterifolia oil or tea tree oil for antimicrobial activity is 2% by weight of fabric.

It is another aspect of the present invention to provide a method of coating a fabric with microencapsulated Melaleuca alterifolia oil antimicrobial composition, wherein the softener is cationic and silicone based softener.

It is another aspect of the present invention to provide a method of coating a fabric with microencapsulated Melaleuca alterifolia oil antimicrobial composition, wherein the pH is maintained by addition of Glacial acetic acid (0.1 gpl) and Core alkali remover 0.2 gpl).

DETAILED DESCRIPTION OF THE INVENTION

Biological source: Melaleuca alterifolia oil or Tea tree oil is acquired from Auxilla Technologies private ltd, Corporate office. Dhanalakshmi Industrial estate Gokul Nagar, Thane 400601, Maharashtra.

One aspect of the present invention generally relates to fabric finishing. More particularly, it relates to microencapsulated antimicrobial fabric finish comprising of tea tree extract which is a 100% concentrate. The active ingredient of the tea tree oil responsible for the anti-microbial activity is terpine-4-ol.

According to the present invention the microencapsulated fabric finish agent comprises of tea tree extract which is a 100% concentrate and has the active ingredient as terpine-4-ol. The shell material or the microencapsulating agent is melamine. The microcapsules are comprising of central core of pure 100% tea tree oil extract and the coating of melamine in the w/v ratio of 1:4. In another embodiment the tea tree oil comprises the core and the melamine as the coating in the ratio of 2:5 % w/v. Both have proven efficacy.

Another embodiment of the present invention relates to a process of producing a fabric finish with antimicrobial composition comprising of the steps:

1. DESIZING:

Desizing is the process of removing the sizing chemicals like Starch, PVA etc., from the fabric by treating with Enzyme at 60 Deg C for 30 min. This is needed to ensure complete removal of sizing chemicals as the presence of residual sizing chemical will tent to reduce absorbency and color yield. Chemicals used Desizing are Enzyme and Wetting agent.

2. SCOURING

This is the process of removing all natural impurities present in the cotton like oil, wax, heavy metals and natural colors.

Caustic Soda, hydrogen peroxide, wetting agent, dispersing agent are added and treated at 98 Deg C for 30 min followed by hot wash at 80 Deg C and Neutralization with Acetic and Peroxide Killer to kill the residual peroxide. Now the fabric is free from Sizing chemicals and with better whiteness and absorbancy.

3. DYEING.

Reactive dyes are used for colouring. Quantity of dyes used depends on the depth of the shade and is usually taken on the weight of the fabric. Dissolved dyes in the bath will have negative charge like cotton fabric, hence dyes will get repelled. Electrolyte like sodium chloride or Sodium sulfate is added to the dye bath to make the exhaust into cotton.

After exhaustion of dyestuff into fabric, alkali like soda ash is added to the dye bath for the dyes to react with cellulose (Hydroxyl group) by chemical reaction forming covalent bond.

4. AFTER TREATMENT

80 to 85 % of dyestuff will react with cotton and remaining 15 - 20 % will react with Hydoxyl group water. This un reacted 15 -20 % dyes will be removed from the fabric by means of subsequent washing/ renationalisation/ soaping/ Hot washing to ensure no more colour bleeding at 70°C in the final hot wash followed by neutralization · 5. APPLICATION OF TEA TREE OIL EXTRACT ON TO FABRIC (FINISHING) Microencapsulated Tea Tree oil 2.0 % w/v, and Binder 2.0 % w/v are taken and dissolved at 70°C for homogenization in solvent, herein the solvent is deionized water. This results in a dispersion of microcapsules in water and stabilized by the binder, it is a homogenous dispersion of microcapsules comprising Melaleuca alterifolia oil. The microcapsules have a core of 100% cone tea tree oil with Melamine coating (1:4 and 2:5 ratio by weight) The average particle size of the microcapsules is 5-30 microns in the dispersion. The binder is chosen from polyurethane, melamine, acrylic styrene copolymer, polyvinyl alcohol, acrylic polymer, and polyethylene. For exemplary purpose the present invention used AGL 502 a salt of poly acrylic acid.

This dispersion is added to the dyeing machine through dosing tank (Eg. vol 200 Its to 8001ts of main tank) and dosed over a period of 20 min at pH 6.0-6.5 with glacial acetic acid ( 0.1 gpl ) and Core alkali remover 0.2 gpl ) for exhaustion and binder will fix the tea tree extract micro encapsulation on the fabric. Fabric is preferably terry towel and woven plain fabrics like sheetings and bed linen.

The temperature is raised to 60°C and run for 30 min and drained the bath. This process of application tea tree extract will not affect the absorbency which is key for terry fabric. Treated fabric is dried at 100 - 120 °C and no high temperature curing is required (160 - 180 degree Celsius) for achieving durability.

FINISHING MECHANISM:

Three finishing mechanisms may be recognized based on the antimicrobial function performed by the particular finish on the textile. These mechanisms include control-release, regeneration and barrier-block. The first two finishing mechanism having problems in usage. The problems with control release mechanism are its durability after laundering and leaching of antimicrobial from fabric which can come in contact with wearer’s skin. These agents have the potential to affect the normal skin, which could lead to extreme skin irritation and allergy issues. This leachate will cause serious issues in sewage waste water treatment causing harmful effects microorganisms. These problems can occur with the fabric using a regenerate mechanism by fixing on the surface of the fiber by binder.

Microencapsulated Tea tree oil exhibits good antimicrobial property and durability upto 100 HL. Tea tree oil starts coming out from the fabric surface gradually while rubbing due to melamine as outer shell in the microencapsulation which is highly durable to heat, boil resistant and moisture resistance. Other agents require chlorine bleach to activate its antimicrobial properties after laundering. Chlorine bleach not only damages the cotton fabric but is also harmful for human skin. Barrier- block mechanism does not pose the problems associated with other two methods. These agents are bonded on fabric surface and do not leach, thereby killing the bacteria that come in contact with the fabric. The result of the present invention, Antimicrobial property of towels, woven plain fabric treated with Extract of leaves of Tea tree oil (natural composition), is extremely good and durable up to 100 HL.

Example 1: Table 1: Standard Operating Procedure for Terry fabric with microencapsulated Teatree oil finish.

Example 2

Preparation of Tea Tree Extract Microencapsulation for application 1. Fabric weight 400 kgs. 2. Tea Tree oil extract required 2% on the weight of the fabric (8 kgs)

3. Taken 50 Its of water at 60°C and added gradually Tea tree oil microcapsules and mixed for 5 mins.

4. Taken 50 Its of water at 70°C and added gradually binder and mixed for 5 mins.

5. The mixture of microcapsules and binder is filtered and ready for application. The average particle size of the microcapsules is 5-30 microns.

For exemplary purpose the binder is AGL 502 which is salt of polyacrylic acid. It is used in ratio of 1 : 1 with Tea tree oil. Table 2: Drying Parameters after application of Tea tree oil microcapsules as anti-microbial finish. ANTIMICROBIAL EFFICACY OF THE TEA TREE OIL MICROCAPSULE FABRIC FINISH

1. Evaluation of Antimicrobial activity by AATCC 100-2012 Test inoculum:

1. Staphylococcus aureus ATCC 6538 (2.00 x 10 5 CfU/ml)

2. Klebsiella pneumoniae ATCC 4352 (2.10 x 10 5 CfU/ml) Additional Test Information:

1. Sample s2e: 48 mm discs

2. No. of swatches used: 2

3. Method of Sterilization of sample: Free steaming

4. Inoculum Canier: Phosphate Buffered water 5. Neutraliser: DE Broflf

Table 3: Antimicrobial test results.

1. CFU: Colony Forming Unit = No. of microorganisms 2. Percentage Reduction of Microorganisms (R) = 100 (B -Ai B) Results:

Towel labelled as Treated with tea tree oil 20 HIL sample Shade; Mocha has shown 99.31% and 99.05% antimicrobial activity towards Staphyloeoccus aureus and Klebsiella pneumonia respectively when analyzed as per AATCC 100 - 2012 test Method.