TECHNICAL FIELD

The invention provides a process developed and optimized for the production of polyacrylate fibers from acrylic fibers for the related technical field. The invention relates to the optimization of the reaction conditions and parameters of the process steps in the existing processes for the production of polyacrylate fiber products. In the polyacrylate production process of the invention, it is possible to increase the production capacity, low cycle costenergy consumption, and efficiency increase by finding the ideal reaction conditions and parameters. In addition, thanks to the improvements made in the production process of the invention, it is possible to obtain an environmentally friendly and sustainable polyacrylate fiber during the production of polyacrylate fiber by reducing the consumption of the water used, reducing the resulting carbon footprint and minimizing the production of waste-by- product.

The invention mainly belongs to the field of textile and is related to the creation of an efficient process by optimizing the reaction environment conditions and parameters for the production of polyacrylate fibers, which are included as raw materials in the production of textile products with many different functions, and the industrial applicability of the said process.

BACKGROUND

Acrylic fiber is obtained in various thicknesses and intersecting morphologies as a result of converting the homopolymer or copolymer containing 85% or more by weight of acrylonitrile monomer into solution form with the help of at least one solvent and then applying the wet/dry methods known in the art from these solutions. Additional methods may be developed or chemicals may be added in order to improve their chemical-physical properties and performances in order to obtain an acrylic fiber product suitable for the needs and sector of the consumer during the process steps applied. Acrylic fiber is a type of fiber frequently used in the technical field related to its ability to be washed as a synthetic fiber and not to maintain its shape, to provide resistance to moth, oil and chemicals, to be painted in colors, to have high fastness properties to sunlight and heat as a synthetic fiber. Thanks to its components, polyacrylate fibers are resistant to heat and flame, have low heat transfer coefficient, high thermal insulation and hygroscopic properties, as well as high odor adsorption thanks to their chemical resistance against acidic and basic, pH balance-buffer and acidic, cationic and reactive paint systems. Thanks to the mentioned features, polyacrylate fibers are a type of fiber that is frequently used in the related technical field. Polyacrylate fibers are obtained from acrylic fibers by methods known in the art. The said production method comprises the following process steps:

Chemical crosslinking reaction of acrylic fibers;

The use of multi amine functional chemicals used as crosslinkers in the said process step requires high safety and process control due to their corrosive chemical effect, carcinogenic, skin itchy, sensitive effect, environmental aqueous toxic effect and strong reductive, extremely explosive and combustible properties.

Hydrolysis reaction of nitrile groups within the fiber with metal alkali salts;

As is known, this process step is essentially two-step as joining and elimination reaction mechanisms. It has been found in the related technical field that nitrile groups, -CONHs,- COO-M ⁺ conversion, do not occur at 100% efficiency in this process step, and this negative situation affects process parameters and conditions and thus product quality.

Subjecting the obtained fibers to neutralization reaction;

Carboxylate salts of strong basic character are obtained as a result of the application of the previous process step. In order for the neutralization process in question to be carried out at high efficiency, the most appropriate acid selection and process step conditions need to be optimized.

Performing polyvalent metal complex formation processes as the final process step;

In this process step, it is critical to select the appropriate solvent of metal organic-inorganic salts and to determine the process step conditions that will provide the desired ionization amount, and to determine the parameters that form the chelate complex coordination bond of metal ions. In the present art, the production of polyacrylate fibers is performed by applying the four above-mentioned independent reactions. The processes of the present art applied for the production of the said polyacrylate fibers are discontinuous and inefficient production methods due to their long reaction times, complex reaction mechanisms and precision production process steps. This negative situation encountered in the present art causes high production costs, time, energy and water losses for polyacrylate fibers. A production method in which high-efficiency and continuous industrial productions are carried out instead of all these negative production processes and existing disadvantages are eliminated has become a must for the related technical field.

WO 2008/128660 A1 relates to the production method for the production of low-toxic and smoke-emission, uniformly dyed fireproof polyacrylate fibers. The production method of the invention comprises the following process steps;

Hydrazine solution in a concentration of 15% by weight is used as a crosslinker of acrylic fibers and this crosslinking process is carried out for 5 hours at 105°C temperatures,

The next treatment step is neutralization with sodium hydroxide solution at a concentration of 5% by weight, the said treatment step being carried out for 2 hours at temperatures of 100°C,

Subsequently, the neutralization process is carried out with a 5% by weight concentration of sulfuric acid solution, the said process step is carried out at a temperature of 60°C for 1 hour,

The final process step is the process of complexing with a solution handled from a mixture of zinc acetate and acetic acid, the said process step being carried out at a temperature of 100°C for 1 hour.

In the present invention, highly complex and controllable process steps are applied for obtaining polyacrylate fiber in desired properties, while the said process steps have long reaction times. In the present invention, a period of at least 9 hours is required to obtain polyacrylate fibers. It is clear that a production method with such high reaction times will require high energy, effort and water requirements, resulting in a high cost and control capability requirement for the production of polyacrylate fibers.

The invention with patent number EP 1788145 A1 relates to fiber with high flame retardant and moisture absorbing properties and to the production thereof. Following process steps are applied in respect of obtaining fibers having the said properties: A hydrazine solution is used for crosslinking the fibers, and wherein the said crosslinking solution contains a 30% by weight hydrazine solution, the process step being carried out at a temperature of 98°C for 3 hours,

For the hydrolysis process, a sodium hydroxide solution with a concentration of 3% by weight is used, the said process step being carried out at a temperature of 92°C and for a period of 5 hours,

A nitric acid solution with a concentration of 6% by weight is used for the neutralization process, the said process step is carried out at a temperature of 60°C and for a period of 2 hours,

For the complexation process, a concentration of 15% by weight of magnesium nitrate solution is used, the said process step is carried out at temperatures of 60°C and for 2 hours.

For the production of fibers of the properties desired in the present invention, it is necessary to apply the mentioned reaction process steps at the specified temperatures and components for at least 12 hours.

The invention EP 1026309 A2 relates to the obtaining of fibers that can be used as raw materials or fillers in clothing, upholstery, transport and construction with flame retardant properties. The following process steps are applied to obtain the said fibers:

A hydrazine solution is used for crosslinking the fibers, and wherein the crosslinker solution comprises the use of 35 % by weight hydrazine solution, the process step being carried out at a temperature of 120°C for 2 hours.

A concentration of 32% by weight of sodium hydroxide solution is used for the hydrolysis process, the said process step being carried out at a temperature of 120°C and for a period of 0,5 hours,

A nitric acid solution with a concentration of 5.8% by weight is used for the neutralization process, the said process step is carried out at a temperature of 65°C and for 2 hours,

For the complexing process, a zinc sulfate solution with a concentration of 13% by weight is used, the said process step is carried out at temperatures of 120°C and for a period of 20 minutes.

For the production of fibers of the characteristics desired in the present invention, it is necessary to apply the reaction process steps at the specified temperatures and with the components for at least 5 hours. The production of polyacrylate fibers by methods known in the present art is carried out as a result of the application of process steps for periods of 5-24 hours. The fact that polyacrylate fiber production process times are so high causes high energy, water and chemical input consumption, low process efficiency, work density and excessive personnel requirements. For this reason, studies, research and development processes have become imperative in order for the polyacrylate fiber production process to be more environmentally friendly and to reduce unit production costs.

BRIEF DESCRIPTION OF THE INVENTION

The present invention provides a method in which the process steps for the production of polyacrylate fibers are optimized and improved in order to eliminate the known negativities in the related technical field and to provide additional advantages to the technical field. In the invention, it is aimed to obtain a more environmentally friendly, high-throughput, controllable and continuous industrial process for the production of polyacrylate fibers.

Thanks to the method of the invention applied for the production of polyacrylate fibers, technical solutions and advantages will be provided for the related technical field:

Producing a higher amount of polyacrylate fiber in the unit time,

Decreasing energy consumption,

Reducing the need for personnel,

Reducing water, chemical input consumption,

Reducing the carbon footprint during production,

Providing a continuous industrial process,

Using chemicals that are less harmful to health, safety and the environment

As a benefit to all of this, the invention sets forth a method for the production of polyacrylate fiber at lower costs and with more environmentally friendly methods.

The present invention is to set forth a polyacrylate fiber production method in which reaction times are shortened by performing optimizations in the reaction medium and parameters in the production of polyacrylate fiber known in the art. DETAILED DESCRIPTION OF THE INVENTION

The subject of the invention is a method developed for the production of polyacrylate fibers and the parameters are optimized, and it is explained with examples that do not have any limiting effect only for a better understanding of the subject.

In the invention, optimization processes are applied in all process steps for the production of high efficiency polyacrylate fibers where existing disadvantages are eliminated and optimization processes are applied in all process steps. Accordingly, the production method of the invention comprises the following process steps: i. Performing crosslinking of acrylic fibers with at least one crosslinker, ii. Subjecting acrylic fiber fibers subjected to crosslinking process to hydrolysis reaction with at least one metal alkali salt, iii.After the process step ii, the fibers are subjected to a neutralization reaction with at least one acid, iv.The fibers obtained as a result of the neutralization process form a complex with at least one metal salt.

In the production method process step i) of the invention, it is ensured that the polymer nitrile (-CN) groups forming acrylic fibers are crosslinked with the functional groups within the crosslinking chemical compounds and retain their fiber form and properties in the subsequent reaction stages.

The hydrazine compound can be used as a crosslinker in the production method i) process step of the invention.

As is known in the art, the hydrazine chemical has environmental and biological disadvantages. Due to the known disadvantages of the hydrazine chemical in the art, chemical compounds with at least two or more amine chemical functional groups of at least 3, 4, 5, or more than 5 can also be used as crosslinkers in the production method of the invention.

The crosslinker may include at least one amine functional group within it. The said crosslinker may be tertiary in structure provided that it contains at least two amine groups or at least two amine groups with at least two or more than 3, 4, 5, or more than 5 amine chemical functional groups, each amine group may be primary, secondary, tertiary chemical structure, or at least two amine groups with at least two primary or secondary structure. Other chemical structures may include more than two secondary amine groups, or 3, 4, or 5, as well as two or more amine groups, each of which is primary or secondary. The multi amine has a functional, 2HN-R-NH2 structure; R may be an alkyl group or an aryl group, or may include more than one of a heteroaryl groups. In some chemical structures, the alkyl, aryl or heteroalkyl group may be straight-chained, branched, cyclic or have more than one of these structures. The R groups are ether, diethers and polyether (((CH2CH2)O) _n (CH2CH2) and n=1 , 2, 3, 4, 5 or more than 5, polyethoethers ((CH2CR2)S)O(CH2CH2) n= 1 , 2, 3, 4, 5 or more than 5, polyamines (CH2CH2)NX )n(CH2CH2) each X independently is H or alkyl or aryl or another suitable group and n= 1 , 2, 3, 4, 5 or more than 5. The R groups can be dyes having a chemical group that absorbs light in the visible range (400-700 nm) to give the fiber a desired color. R groups may also be selected from flame retardant or flame retardant phosphorus chemical functional groups. These may be groups containing trialkylphosphine, trialkylphosphite, trialkylphosphate, trialkylphosphonate, trialkylphosphoramide, hexaalkylcyclotripolyphosphazine or another phosphorus.

The polyacrylate production method of the invention may comprise chemical compounds having the following formulas as crosslinkers:

NH2-(CH2) _n -NH2, wherein n is one of the values 0, 2, 4, 6, 8, NH2-(CH2) _n -NH-(CH2) _n -NH-(CH ₂ ) _n -NH2 wherein n is one of the values 0, 2, 4, 6, 8, NH2-(CH2) _n -N-(-(CH2) _n -NH2))(CH ₂ ) _n -NH2 wherein n is one of the values 0, 2, 4, 6, 8, NH2-(CH2) _n -R-(CH2) _n -NH-(CH ₂ ) _n -NH2 wherein n is one of the values 0, 2, 4, 6, 8, while R includes one of the groups CH, C.

In the production method of the invention, at least one crosslinker comprising the amine functional group can be used as a crosslinker.

Multiple chemical compounds may be used as crosslinkers in the production method of the invention. At least one of the crosslinkers that may be used in the present invention is a chemical compound containing an amine group.

In the invention, there is preferably a use of a crosslinker and the said crosslinker comprises at least one amine group within its body. The preferred embodiment of the invention is that the crosslinker to be used as the crosslinker in the production step i) comprises more than one amine functional group within it. The crosslinker may contain 2, 3, 4 or 5 amine groups.

The most particular embodiment of the invention may include at least one, in certain proportions mixtures of hydrazine, hexamethylene diamine, diethylene triamine, tetraethylene triamine, tetraethylene pentamine, Bis-hexamethylene diamine, tris(2-aminoethyl)amine compounds, or all of them as crosslinkers.

The crosslinking process in the process step i) is carried out under reflux conditions at boiling temperature. The temperature of the process in question is between 100°C and 110°C. The said process temperature is preferably one of 100°C, 105°C, 106°C, 107°C, 108°C, 109°C and 110°C.

The process step i) is one of crosslinking: acrylic fiber ratio, by weight, of 1 : 1 , 1 : 25, 1 :50, 1 :100, 1 :200, 1 :300 in crosslinking.

The crosslinker in the process step i) is used to form a solution in at least one solvent. The amine group capable of solvent crosslinking may be an organic solvent. The solvent contains at least one of the organic solvents: water, methanol, ethanol, isopropanol, acetone, dimethylsulfoxide, dimethylfomiamide, dimethylacetamide. Preferably water is used as the solvent, preferably there is at least one organic solvent in the water. Preferably, there is at least one organic solvent dissolved in water in the range of 10% to 50% by weight. In the most preferred embodiment, only water is present as the solvent. The crosslinker used in the process step i) is preferably contained in the solvent at a value in the range of 20% to 60% by weight. Preferably, the crosslinker:solvent ratio is in the range of 35% to 50%.

The mixing process i) is preferably carried out in the process step. The said mixing is preferably in the range of 100 to 500 rpm. The mixing process is preferably in the range of 200 rpm to 400 rpm.

In the process step i) of the invention, the crosslinking ratio:acrylic fiber is 4.6% (w/w) by weight. This value is considered to be the value realized by the necessary crosslinking in the state of the art. In the present invention, the crosslinking ratio:acrylic fiber realized in the process step i) is at least 4.6% (w/w) by weight. The reaction time of the process step i) takes place in the range of 10 minutes to 45 minutes with the optimization and development processes.

The reaction time of the processing step i) is preferably in the range of 15 minutes to 30 minutes with the optimization and development processes carried out.

As is known in the art, in process step ii), the polymer nitrile (-CN) groups forming the remaining acrylic fiber, which are not included in the crosslinking, as a result of process step i), undergo conversion to CONH2, COOM functional groups of nitrile groups by two-stage adhesion and elimination reactions in the presence of metal alkali. The said process step ii) is carried out under reflux reaction conditions. Preferably, the process step ii) is carried out at a value in the temperature range of 100 to 110°C. The temperature of said process step ii) is preferably one of 100°C, 105°C, 106°C, 107°C, 108°C, 109°C and 110°C.

The reactions mentioned in the process step ii) are preferably carried out by mixing with at least one mixer. The said mixing is preferably carried out in the range of from 200 to 400 rpm.

The metal alkali salt mentioned in the process step ii) is at least one of the compounds of calcium hydroxide, magnesium hydroxide, calcium hydroxide, sodium hydroxide, calcium nitrate, magnesium nitrate, potassium nitrate, sodium nitrate.

The metal alkali salt used in the process step ii) is in the range of 8% to 20% by weight in at least one solvent. At least one of water, methanol, ethanol, isopropanol, solvents can be used as the solvent mentioned herein. Water is used as the said solvent, if preferred, at least one organic solvent may be present in the water. Preferably, the process step ii) comprises at least one solvent dissolved in water at a value in the range of 10% to 50% by weight.

In the most preferred embodiment, water is used as the solvent in the process step ii).

The processing step ii) is preferably carried out over a time period of 10 to 30 minutes.

The amount of the metal alkali salt in the process step ii) is one of 1 :1 , 1 :10, 1 :25, 1 :50, 1 :100 by weight metal alkali salt:f iber. Preferably, at least one acid is used for the neutralization process in the process step iii). Preferably, the pH of the acid to be used is expected to have a value in the range from 1 to 5. Preferably, the acid to be used is expected to have a pH value of 3 and below. If preferred, the acid may be a mixture. At least one of the said acid mixtures is organic acid. Preferably, the organic acid in the acid mixture is at least 50% by weight.

At least one of the group of propionic acid, acetic acid, sulfuric acid, hydrochloric acid, phosphoric acid, nitric acid, phosphoric acid, benzoic acid, nitric acid is used as acid for the neutralization process in the process step iii).

Preferably, an acid is used as the acid in the process of neutralization of the process step iii).

The concentration of the acid preferably used in the process of neutralization of the process step iii) is in the range of 10%-20% by weight.

In the process step neutralization process iii), the acrylic fiber: acid ratio is in the range of 1 :1 to 1 :150,

The neutralization process is carried out at a value in the range of temperatures of 40°C to 60°C. Preferably, the neutralization process is carried out at one of the temperatures of 45°C, 50°C, 55°C and 60°C.

Chlorides, acetates, sulfates, phosphates, carbonates of metals with an ion value of +2 or +3 and included in the 4th and 5th periods of the periodic table can be used as metal salts in the process step iv). Preferably, the salt of more than one metal may be used as the metal salt.

At least one of the chlorides, acetates or carbonates of the transition metals preferably having an ion value of (+2) is used as the metal salt in the process step iv).

Preferably, chlorides, acetates, bromides or carbonates containing zinc metal are used as the metal salt in process step iv).

In the process step iv), the metal salt is used at a value in the range of 8% to 20% by weight.

The ratio of acrylic fiber:metal salt in the process step iv) is in the range of 1 :1 to 1 :150. In the invention, the process step iv) is carried out at a value in the range of 90 to 100°C temperatures.

In the invention, the process step iv) is carried out at a value in the range of 15 to 30 minutes.

Thanks to the application of the production process steps mentioned in the invention, polyacrylate fiber production can be carried out for a period of between 60 minutes and 120 minutes.

In the invention, the term "tow" is a term given to the fiber form of the infinite filament.

The production of polyacrylate in the current art is carried out with a technology that includes successive complex process steps in reactor-boiler with discontinuous process systems, with low production amount and process efficiency, at high costs, at very long times (production process steps available in the art are between 6 hours and 36 hours) that are not intended for reuse after use of waste and by-products. Another innovative aspect of the invention is that thanks to the optimizations carried out in the production process steps, the production is carried out in a progressive series of successive bath systems. Accordingly, in the invention, in line with the optimized parameters of polyacrylate fiber production, the process and production technology have been developed by modification of the tow band as a continuous in a progressive series successive bathing system, and technical solutions and advantages are presented for the related technical field.

Thanks to the polyacrylate fiber production of the invention, the following additives emerge for the related technical field:

• Providing continuous industrial production process,

• Obtaining polyacrylate fiber for a long time in large quantities,

• Using chemicals that are less harmful to health, safety and the environment

• Decreasing energy consumption,

• Reducing the need for personnel,

• Reducing water, chemical input consumption,

• Reducing the carbon footprint during production.

In the present art, polyacrylate production takes about 5 hours to complete the longest process step with a technology that includes sequential complex crosslinking, hydrolysis, neutralization, metal complexation process steps in the reactor-boiler with discontinuous batch process systems, while the shortest process step takes about 1 hour. Accordingly, in the current production methods in the technical field, it is not possible to make continuous production in bathrooms with a duration of 1 to 5 hours.

The present production methods in the art require the design of a bath in which 300 m of fibers can fit for a production with an input speed of 1 m/min as a continuous if the i) process step is carried out for 5 hours and around. The investment cost of the bath with the said configuration is not possible industrially. In the invention, the process comprising sequential complex crosslinking, hydrolysis, neutralization, metal complexation process steps forming the production of polyacrylate fibers can be carried out as a continuous production of the fiber tow band in each step in a serial successive bathing system, subject to the process in the bath. In the production process of the invention, the optimization of each successive chemical process step was studied, and thus shorter process times were obtained, as well as bathroom dimensions suitable for sustainable production, tow band number and fiber extraction ratio were taken into consideration. In this way, the production process of polyacrylate fiber, which can be produced on an industrial scale, is ensured.

As with the WO 2008/128660 A1 and EP1026309 A2 patents, the polyacrylate production processes in the present art are carried out over long periods of time, such as an average of 9 hours. With the optimization of the invention and the improved polyacrylate production method, the process times were reduced to 1 hour and the industrial production capacity was reached. The processes of the invention can produce 9 tons of fiber instead of 1 ton of fiber, unlike the production processes in the present art, with their duration and consumption. Thanks to the production method of the invention, an efficient production process is put forward along with shortening the process production time, developing the continuous production method instead of discontinuous production, less energy consumption and low cycle costs.

In the current production methods, boiler paints are produced for approximately 9 hours at flote ratios of 1 :4 to 1 :6, and for the production of 1 ton of fiber, approximately 5 tons of water are used for each process step, resulting in a total water consumption of 25 tons. In addition, with the addition of washing process steps, this value approaches 30 tons. Unfortunately, these amounts of water used in the production methods in the current art cannot be recycled and are disposed of as waste. The present invention theoretically does not consume water except for a quantity of water evaporated by the moisture and process loss-leakages of the fiber tow belt in the continuous production system, and the production is carried out by chemical addition as the chemical is consumed. In the current production methods, it is seen that the polyacrylate fiber, which is produced with 30 tons of water consumption, is made at 1 -2 tons of water consumption with the present invention.

Table 1. Technical properties of polyacrylate fibers obtained by the production method of the present invention

In the polyacrylate fiber production processes of the invention, the carbon footprint of the process also allows to improve due to the decrease in water consumption, decrease in energy consumption and increase in production capacity.

When the current production methods and the production method of the invention are compared, there is an improvement in many different points such as production cost, duration, carbon footprint, etc.

The polymer forming the fiber is an acrylonitrile polymer, which may comprise monomer units in a polymer chemical structure (CR1R2-CR3CN)- also comprising nitrile-functional monomer units. Here, the structures R1, R2 and R3 may be H, alkyl (methyl, ethyl, propyl), aryl (phenyl). However, R1 and R2 can both be H, as well as R3, methyl, and H. These polymeric chemical structures (meth) may be acrylate, alkyl vinyl ether or other types of comonomer units, or may be polyacrylonitrile and polymethacrylonil, acrylonitrile-vinylester copolymer and acrylonitrile polymer mixtures formed by them. If the acrylonitrile polymer is a copolymer, such as a copolymer (terpolymer, block), the above-mentioned chemical (CR1R2-CR3CN) - structure of at least about 50% or more or even 60%, 70%, 80% or 90% or even 100% monomer units.

The fibers developed by the present invention production technology may be short fibers (e.g., about 1 mm to about 1 cm long) or may be in the form of long fibers (e.g., about 1 cm to about 1 m or longer). At the same time, the diameter of the fiber may be between approximately 0.7-50 dtex. If the diameter of the thin fibers in the fiber is <3 dtex, they can facilitate the penetration of chemicals into the fiber and polymer during crosslinking, hydrolysis, neutralization, metal complex bonding, If the diameter of the thick fibers in the fiber is >7 dtex, chemical reactions can occur in an inhomogeneous manner in the entire fiber. However, the small size of the pore structure of the fiber, the crystalline structure and degree of the polymer forming the fiber, the orientation of the polymer chains may facilitate or make it difficult to penetrate the chemical processes that take place at each stage, depending on whether they are more or less. In fact, core-shell structures can be formed by polymer modification formed close to the outer layer of the fibers. In such cases, it is obtained by modification with the outer layer properties of the obtained fibers and fibers, and the modified fiber can provide flame and heat resistant, antifungal or antimicrobial performance, low heat transfer coefficient, high thermal insulation and hygroscopic properties, pH balance buffer feature and performance against acidic and basic.

The polyacrylate fibers may be obtained from the acrylic fibers' hole, yarn, filament yarn, woven-nonwoven fabrics and from the mixture of at least one, two or more, as may be obtained from the different forms of staple fibers, tows, tops, bumps. Further, in textile applications of acrylic, the fabric may be a piece of clothing, e.g. a sock or an underwear or an upper garment, a blanket, e.g. a fire blanket, a curtain, a fibrous mat, a rug, a carpet.

Polyacrylate fiber can be produced starting from the form of acrylic fiber prepared with appropriate heat, light, stabilizer, antimicrobial, antiviral, antiodor, biocidal additives, conductivity enhancers, antioxidants, pigments, plasticizers, and some additives that provide antifungal. The said additives can be made into polyacrylate products by known methods, e.g., dissolving the polymer in a solvent, combining the solution with the additive, producing the fiber by wet gravity technology. The obtained fibers were obtained from polyacrylate fibers with the production technology detailed in the invention. The polyacrylate obtained may be in the form of fibers, yarns, fabrics. The products obtained from this can be used in many application areas in the textile sector, such as protective clothing, public transport textile products, filtration, fireproof blanket, upholstery, clothing (socks, underwear), outdoor and indoor textile applications, etc.

The polyacrylate fibers can be prepared by mixing with one or two or more of the appropriate solutions of heat, light, stabilizer, antimicrobial, antiviral, antiodor, biocidal additives, conductivity enhancers, antioxidants, pigments, plasticizers, and some antifungal additives in the metal complex step, which is the last step of the known process steps, and can be produced by drying or fixing the fibers by a heat treatment. The said additives can be made into polyacrylate products by known methods, dissolving the additives in a suitable solvent, combining the solution with the additive, or producing the fiber by wet shooting technology. The polyacrylate obtained may be in the form of fibers, yarns, fabrics. Protective clothing, public transport textile products, filtration, fireproof blankets, upholstery, clothing (socks, underwear), outdoor and indoor textile products can be obtained from the polyacrylate fibers obtained.

Additional chemical compounds may be used during the production of the polyacrylate fibers of the invention to increase the chemical and physical properties of the polyacrylate fibers to be obtained, such as non-flammability, strength, and humidity.

As is known from the invention with patent number JP 5056358, the dyeing processes of polyacrylate fibers can be carried out with cationic dyeing systems due to the carboxylate and carboxylic acid chemical functional groups they have, but the desired technical characteristics are not provided in the dyeing fastness and industrial applications of polyacrylate fibers after the processes carried out in this way. It has been determined by the present inventors that polyacrylate fiber, reagent and pigment dyeing systems can demonstrate superior performances in applicability and dyeing fastness.

The scope of protection of the invention is specified in the attached claims and cannot be limited to those explained for sampling purposes in this detailed description. It is evident that a person skilled in the art may exhibit similar embodiments in light of above-mentioned facts without drifting apart from the main theme of the invention. Tests

For the production of polyacrylate fibers, the process steps known in the art are applied.

These process steps are provided below: i. Performing crosslinking of acrylic fibers with at least one crosslinker, ii. Subjecting acrylic fiber fibers subjected to crosslinking process to hydrolysis reaction with at least one metal alkali salt, iii. After the process step ii, the fibers are subjected to a neutralization reaction with at least one acid, iv. The fibers obtained as a result of the neutralization process form a complex with at least one metal salt.

These process steps are tested by applying the development and optimization processes of the present invention. The results obtained are shared under this heading.

Hydrazine solution is used in the tests as a crosslinker in the process step i).

Hydrazine chemical was used for fiber crosslinking, and concentration NIR spectroscopy on the fiber was analyzed after application to the solution and fiber. For analysis in the solution, 0-80% reference solutions with known concentration were prepared and spectroscopic calibration was prepared. The prepared calibration correlation R2=98. For the analysis of crosslinked hydrazine on the fiber surface, solutions with a known concentration of 0-80% were prepared and applied separately at 107°C for 180 minutes. The obtained fibers were dried and analyzed in NIR spectroscopy and the calibration graph was prepared in the reliability range (R2 >97%).

- Investigation of hydrazine-fiber crosslinking ratio

In these tests, 30 g acrylic fibers were prepared by crosslinking at a concentration of 15% by weight with hydrazine solution at 200 rpm mixing medium at 107°C for varying periods of time specified in the table. After each process step, the fiber form is washed with fiber water and the chemical residues are removed and dried overnight in the incubator under 60°C temperature conditions. As can be seen in detail in Table 2, it was found that 4.6% hydrazine was attached to the fiber with nitrogen elemental analysis and gravimetric calculations by taking the fiber in 180 minutes.

Table 2. Investigation of hydrazine-fiber crosslinking ratio

Crosslinking of acrylic fibers with hydrazine solution process step

In order to investigate the relationship between hydrazine concentration and reaction time in acrylic fiber, 30 g of acrylic fiber was carried out at the concentrations specified in Table 2, at a temperature of 107°C at 200 rpm mixing medium. After each process step, the fiber was washed with water and the chemical residues were removed and dried overnight in the oven under 60°C temperature conditions. Then, the amount of crosslinking on the fiber surface was analyzed in the calibration standard ranges prepared by NIR spectroscopy. Based on the fact that the hydrazine solution forms a 4.6% (w/w) crosslinking on the fiber, the required time is given in Table 3.

Table 3. Investigation of crosslinking reaction conditions and parameters with hydrazine solution

In the test studies, it has been determined that acrylic fibers do not provide the desired physical properties when the crosslinker has a concentration value of 60% or more by weight in the solution.

Table 4. Investigation of crosslinking reaction conditions and parameters with DMA solution

Subjecting acrylic fiber fibers subjected to crosslinking process to hydrolysis reaction with at least one metal alkali salt,

Hydrolysis reaction was carried out with sodium hydroxide, a metal alkaline salt, at a temperature of 105°C in a 200 rpm mixing medium at the concentration specified in Table 5 of 30,5 g fiber crosslinked at 4.6% by weight. The hydrolysis mechanism is realized in two stages, the first stage is understood by dark red color transformation, while the second stage is determined by the complete light yellow color of the fiber color. The completion of the reaction at this stage was detected by the time completing the two-color transformation. The obtained fiber was washed with warm water after each process step and its chemical residues were removed and dried overnight under 60°C temperature incubator conditions.

Table 5. Investigation of hydrolysis reaction conditions and parameters with sodium hydroxide solution In the test studies, it has been determined that acrylic fibers do not provide the desired physical properties when the metal alkali salt has a concentration of 30% or more by weight in the solution.

Being subjected to a neutralization reaction with at least one acid

Neutralization of the polyacrylate transformed from acrylic fiber with acetic acid was carried out with acetic acid, which is a weak organic acid, at a temperature of 56°C in a 200 rpm mixing medium at the concentrations specified in Table 6. Neutralization of the fiber is determined by monitoring the peak of the COONa chemical functional group at a wide and widespread wavelength of 2900-3600 cm' ¹ with FT-IR spectroscopy. The obtained fiber was washed with water and the acid chemical residues were removed and dried overnight under 60°C temperature incubator conditions and examined with FT-IR. The neutralization of the acetic acid concentration over different times is provided in Table 6.

Table 6. Neutralization reaction neutralization conditions and parameters with acetic acid solution

In the test studies, it has been determined that acrylic fibers do not provide the desired physical properties when the acid has a concentration of 30% or more by weight in the solution.

Complexation of the obtained fibers with at least one metal salt

Polyvalent fiber can be obtained by binding metal ions by preparing polycarboxylic fiber with carboxylic acid chemical group by neutralizing sodium polyacrylate fiber. In this process step, zinc ions were bound to the polymer with the chelate complex coordination bond at the zinc concentrations specified in Table 7 by adding acid to increase water and ionization as the appropriate solvent of metal organic-inorganic salts, at a mixing ratio of 200 rpm, at a temperature of 60°C, and at different times by adjusting the solution to the pH 4,5-5 range in the presence of weak acid. The obtained fiber was washed with water to ensure that the excess zinc ion and acetate residues were not removed by washing from the fiber and it was examined by drying at 60°C incubator temperature.

Table 7. Complexing reaction conditions and parameters with zinc acetate solution

In the test studies, it has been determined that acrylic fibers do not provide the desired physical properties when the metal salt has a concentration of 30% or more by weight in the solution.

Table 8. Technical properties of polyacrylate fibers obtained by the production method of the present invention

Polyacrylate fiber has the physical properties of 12-35 cN/tex strength in the range of 0.7-45 dtex fiber thickness when the process steps given as the production method of the invention are produced by applying chemical treatment as a continuous in the successive sequential bath system with chemical solution in 10 m/min and 0.01 m/min of a fiber tow band.

However, polyacrylate fibers may have low thermal conductivity, moisture retention properties of 10% or more, with a combustion resistance in the range of 30-40% L.O.I. In textile applications of acrylic obtained from at least one, two or more mixtures of cotton, cellulose, polyester, nylon, fiber, yarn, fabric, piece of clothing, socks or underwear or upper clothing, a blanket and fire blanket, curtain, fiber mat, rug, carpet can be obtained from polyacrylate fiber and filament yarn.