CN115874304A - Preparation method of antistatic textile fabric - Google Patents

Abstract

The application relates to textile fabrics, a preparation method of antistatic textile fabrics, comprising the following steps, first modifying graphene oxide with dodecyltrimethylammonium chloride, and then coupling the graphene oxide with a silane coupling agent Silica, finally reduced to graphene with sodium citrate, then graphene and ethylene glycol compounded to obtain an antistatic agent slurry, added to the raw materials for polymerization, and finally esterified and polycondensed to obtain antistatic polyester chips , and then make antistatic fibers, and then blend the prepared antistatic fibers into yarns, and make antistatic textile fabrics according to the conventional weft knitting process, so that the textile fabrics have good antistatic properties, and antistatic after washing The ingredients are not easy to fall off and have permanent antistatic properties.

Description

A kind of preparation method of antistatic textile fabric

technical field

The invention relates to the field of textile fabrics, in particular to a method for preparing antistatic textile fabrics.

Background technique

With the advancement of technology and the development of society, people have higher and higher requirements for the quality of life, especially for the environment of daily life. As a result, high-tech products continue to enter the textile industry. The functional finishing of textiles continues to increase, and the added value of textiles is increased by endowing these special functions to textiles, thereby improving people's living environment and meeting people's growing material needs.

Chemical fibers, especially synthetic fibers, have many excellent characteristics compared with natural fibers, such as they can obtain special performance and aesthetic properties in fiber production and processing, and are low in price, high in manufacturability, good in strength and toughness, etc. , has been rapidly developed and widely used. Synthetic fibers have many advantages, but there are also many disadvantages that cannot be ignored, such as easy to accumulate charges and generate static electricity. The various impacts of static electricity on human society are well known, and it will affect the accuracy of electronic products; it will cause discharge phenomena in petrochemical industry operations And cause explosion or combustion; human body charged with static electricity will also cause adverse effects such as easy dust collection, uncomfortable wearing, and electric shock. In view of the above reasons, it is necessary to improve the antistatic performance of the fabric.

For knitted fabric products, antistatic functional products can be obtained by various methods. One of the simplest methods is to carry out antistatic treatment on the surface of fibers or fiber products, and the antistatic agents used are mainly surfactants. The principle of action is: the hydrophobic end of the surfactant molecule is adsorbed on the surface of the fiber, and the hydrophilic end points to the space to form a polar surface, which absorbs water molecules in the air, improves the hygroscopicity of the fiber, reduces the resistivity of the fiber surface, and accelerates the charge escape. Dispersion, so as to achieve antistatic effect. However, the antistatic effect of this method is difficult to last. As time goes by, the surfactant will gradually volatilize, and the fabric will lose its antistatic property after several washings.

Another antistatic method is to use graft modification, blending or copolymerization to introduce hydrophilic monomers or polymers into fiber-forming polymers during polymerization or spinning of synthetic fibers, or to use composite spinning methods , to make a composite fiber with a hydrophilic outer layer to improve the hygroscopicity of the fiber, reduce the surface specific resistance of the fiber, and obtain antistatic properties. However, this method still reduces the surface specific resistance of the fiber by increasing the hydrophilicity of the fiber, and accelerates the charge dissipation, so it is difficult to exert the antistatic effect in an environment with low relative humidity.

Chinese patent publication number: CN108611848A A production method of antistatic breathable fabrics discloses "a production method of antistatic breathable fabrics. It solves the technical problems of existing waterproof and breathable fabrics without corresponding production methods and complicated production. This antistatic The production method of the electrostatic breathable fabric is characterized in that it comprises the following steps: a. Weaving: weaving the warp and weft into the required fabric, the warp is woven from flax fiber, viscose fiber and linen fiber, and the weft is made of polyester Ester fiber, yarn fiber and mercerized cotton fiber are blended and woven; b, making antistatic finishing solution: by weight percentage, 6% antistatic agent, 2.5% binding agent, 12% ethanol and 70- Put 90% of the water into the blender and stir to prepare the antistatic finishing solution; c, padding: dip the fabric in the antistatic finishing solution; d, rinse: rinse the fabric in cold water and dry it ; e, setting: Put the fabric into the setting machine to set the shape, and you can get the antistatic breathable fabric.”

Chinese Patent Publication No.: CN114606634A An antistatic knitted fabric and its preparation method discloses that "the present invention belongs to the technical field of printing and dyeing textiles, and specifically relates to an antistatic knitted fabric and its preparation method. Among the products developed by the present invention, conductive polyester is used The fiber, the conductive polyester fiber includes conductive short filaments with a mass fraction of 3-5%; the conductive polyester fibers are conductive polyester fibers with a fineness of 45-80dtex; the aspect ratio of the conductive short filaments is 20:1-30:1; the length distribution range of the short conductive fibers is 10-20mm; the specifications of the knitted fabric are: horizontal density: along the direction of the course, the number of wales within 5cm is 80-85 Longitudinal density: along the coil wale direction, the number of coil courses in 5cm is 120-130. In addition, microcrystalline wax and lubricant are also included, and conductive polyester fiber and viscose fiber are twisted into composite fibers. The product obtained in the present invention It has excellent antistatic properties.” In this invention, conductive agents such as microcrystalline wax and lubricants are applied to the fiber surface, and after repeated washing, the antistatic components will fall off, resulting in a decrease in antistatic properties. However, the way of post-finishing adopted is to attach the antistatic agent to the surface of the fiber. After washing with water, the antistatic component is easy to fall off, and the fiber loses its antistatic property.

Chinese patent publication number: CN216864454U anti-static low-elastic polyester fabric discloses that "the utility model is aimed at the lack of antistatic performance of the existing anti-static low-elastic polyester fabric, which cannot be compared with inelastic polyester fabric, and designs a Anti-static low-elastic polyester fabric with improved resistivity of the fabric itself and improved spray coating structure, including: low-elastic silk thread and metal low-elastic silk thread as the diameter line, unstretched silk thread as the weft thread, interwoven to form the main fabric layer; Both sides of the fabric layer are sprayed with surfactants, and the overall antistatic effect is improved through the surfactants; the metal low-stretch yarn is a low-stretch yarn made of short metal yarns and pre-oriented yarns mixed with false twist; the low-elastic yarns The use ratio of metal low elastic wire is 17:1 to 33:5." This utility model invention improves the resistivity of the fabric itself and improves the antistatic low elastic polyester fabric of the spray coating structure. The coating is easy to wear after repeated friction It falls off, and the metal has low elasticity, and the hand feel is not as good as no metal fiber.

Most of the current antistatic fabrics achieve the purpose of antistatic directly by coating a layer of hydrophilic antistatic treatment agent on the surface of the fabric or by blending with a single conductive fiber. However, such antistatic fabrics are antistatic The effect is poor, and it cannot be used for a long time. After long-term use or repeated cleaning, the antistatic treatment agent on the surface of the fabric will fall off, thereby losing the antistatic effect. To enhance the antistatic effect of the fabric from the material, it is impossible to achieve the purpose of making the antistatic treatment solution fully adhere to the surface of each fiber by first performing antistatic soaking treatment on the non-conductive basic fiber, and then performing blended weaving. It is realized that by adding a viscous agent in the antistatic treatment liquid, the adhesion of the treatment liquid is greatly enhanced, so that the use of antistatic fabrics is very unfavorable.

Contents of the invention

The object of the present invention is to provide a method for preparing antistatic textile fabrics to solve the problems raised in the above-mentioned background technology.

The invention provides the following technical scheme: a preparation method of an antistatic textile fabric, comprising the following steps,

S1: Dissolve graphene oxide in water, ultrasonically disperse to obtain graphene oxide hydrosol, then add dodecyltrimethylammonium chloride to graphene oxide hydrosol, stir at constant temperature, then filter, wash and dry to obtain modified After the graphene oxide;

S2: Dissolve the modified graphene oxide in water, ultrasonically disperse to obtain the modified graphene oxide hydrosol, then add KH-560 and nano-silica to the modified graphene oxide hydrosol, and keep the temperature constant Stir, then filter, wash and dry to obtain a mixture M;

S3: dissolving sodium citrate in water, adding the mixture M obtained in step S2, stirring at a constant temperature, then filtering, washing and drying to obtain an antistatic agent;

S4: Mix and stir the antistatic agent and ethylene glycol, disperse evenly, and obtain the antistatic agent slurry;

S5: dissolving tetrabutyl titanate in ethylene glycol and stirring evenly to obtain a catalyst slurry; then adding the catalyst slurry to terephthalic acid and ethylene glycol and stirring evenly to obtain a polymerization reaction raw material;

S6: Add the antistatic agent slurry to the polymerization reaction raw materials, stir evenly, and put it into the polyester reactor;

S7: After the polymerization reaction is completed, the material is discharged and then dried and pelletized to obtain antistatic polyester chips;

S8: Melt-spinning antistatic polyester chips, and then forming antistatic fibers through fiber forming, drawing and orientation of nascent fibers, heat setting and winding of fibers; blending the obtained antistatic fibers into yarns, according to Antistatic textile fabrics are made by conventional weft knitting process.

Preferably, the specific process of step S1 is, by weight component, 5-10 parts of graphene oxide are dissolved in 1000-1500 parts of water, ultrasonically dispersed for 2-3h to obtain graphene oxide hydrosol, and then to graphene oxide Add 1-2 parts of dodecyltrimethylammonium chloride to the hydrosol, stir at a constant temperature of 50-60°C, then filter, wash with water 2-3 times, and vacuum dry at 80-100°C for 16-18h to obtain the modified of graphene oxide. Dodecyltrimethylammonium chloride has antistatic properties, which can effectively increase the degree of exfoliation of graphene oxide, improve the antistatic properties of graphene oxide, and increase the functional groups on graphene oxide, which is beneficial to subsequent contact with B combination of diols.

Preferably, the specific process of step S2 is, in terms of weight components, dissolving 10-15 parts of modified graphene oxide in 1200-1500 parts of water, and ultrasonically dispersing for 2-3 hours to obtain modified graphene oxide water sol, then add 20-30 parts of KH-560 and 25-30 parts of nano-silica to the modified graphene oxide hydrosol, stir at 50-60°C for 2-3 hours, then filter and wash with water 2-3 times , 80-100°C vacuum drying for 10-12h to obtain the mixture M. Nano-silica has water absorption, forms bound water, improves the hygroscopicity of the fiber, thereby improving the conductivity of the fiber and improving the antistatic property of the fabric.

Preferably, the specific process of step S3 is, based on weight components, dissolving 5-10 parts of sodium citrate in water, adding 5-10 parts of the mixture M obtained in step S2, stirring at a constant temperature of 80-100 ° C for 1-2 h, and then Filter, wash with water 2-3 times and vacuum dry for 10-15 hours to obtain the antistatic agent. Reduction of graphene oxide with sodium citrate.

Preferably, the specific process of step S4 is, based on weight components, mixing and stirring 20-30 parts of antistatic agent and 100 parts of ethylene glycol for 2-3 hours, then raising the temperature to 80-90 ° C and continuing stirring for 2-3 hours, Disperse evenly to obtain antistatic agent slurry. Since S2 has modified graphene and coupled nano-silica, a large number of hydroxyl groups and amino groups remain on the surface of graphene, which are chemically bonded with ethylene glycol to form an antistatic agent slurry, which is beneficial to subsequent antistatic agents. Participate in the polycondensation reaction, doped into the polyester polymer chain to form a stable antistatic property.

Preferably, the specific process of step S5 is, based on weight components, dissolving 1-2 parts of tetrabutyl titanate in 500-600 parts of ethylene glycol, stirring evenly to obtain a catalyst slurry, and then adding the catalyst slurry to Add 1,000-1,500 parts of ethylene glycol and 4,000-5,000 parts of terephthalic acid, and stir evenly to obtain polymerization raw materials. The raw material for polymerization reaction is prepared by adopting titanium series catalyst, terephthalic acid and ethylene glycol.

Preferably, the specific process of step S6 is, based on weight components, adding 10-20 parts of antistatic slurry to 100 parts of polymerization reaction raw materials, stirring evenly, and adding them into the reaction kettle from the feed port. Adding too much antistatic slurry will affect the spinnability of polyester, and adding too little antistatic agent slurry will reduce the antistatic performance of polyester.

Preferably, the specific process of step S7 is to carry out the esterification reaction at a temperature of 230-240°C and a pressure of 0.2-0.3MPa. When the effluent value reaches the theoretical value, carry out the polycondensation reaction and raise the temperature to 275-280°C. Simultaneously evacuate to an absolute pressure of ≤150Pa, and the polycondensation reaction time is 60-90 minutes. After the polycondensation reaction is completed, the material is discharged and then dried and pelletized to obtain antistatic polyester chips. After polycondensation and esterification, the antistatic agent is incorporated into polyethylene terephthalate, so that the polyester chips obtain antistatic properties.

Preferably, it is applied in the field of medical protective clothing. Increase the antistatic performance of protective clothing.

Compared with the prior art, the beneficial effects achieved by the present invention are:

1. The antistatic agent is dissolved in the polyester, so that the polyester chips have permanent antistatic properties, and the antistatic components are not easy to fall off.

2. Nano-silica can improve the spinnability of the fiber, improve the hygroscopicity, and produce antistatic effect synergistically with the antistatic agent.

3. Use dodecyltrimethylammonium chloride to modify graphene. Dodecyltrimethylammonium chloride not only has antistatic properties, but also improves the peeling degree of graphene oxide sheets and improves electrical conductivity. Thereby improving the antistatic properties of textile fabrics.

Description of drawings

The accompanying drawings are used to provide a further understanding of the present invention, and constitute a part of the description, and are used together with the embodiments of the present invention to explain the present invention, and do not constitute a limitation to the present invention. In the attached picture:

Fig. 1 is a diagram showing the results of the antistatic test of the prepared antistatic textile fabrics in Examples 1-3 and Comparative Examples 1-3 of the present invention.

Detailed ways

Example 1

S1: Calculated by weight components, dissolve 5 parts of graphene oxide in 1000 parts of water, ultrasonically disperse for 2 hours to obtain graphene oxide hydrosol, and then add 1 part of dodecyltrimethyl chloride to the graphene oxide hydrosol ammonium chloride, stirred at a constant temperature of 50°C, then filtered, washed twice with water, and vacuum-dried at 80°C for 16 hours to obtain modified graphene oxide.

S2: Dissolve 10 parts of modified graphene oxide in 1200 parts of water, ultrasonically disperse for 2 hours to obtain modified graphene oxide hydrosol, and then add 20 parts of KH-560 to the modified graphene oxide hydrosol and 25 parts of nano-silica, stirred at 50°C for 2h, then filtered, washed twice with water, and vacuum-dried at 80°C for 10h to obtain a mixture M.

S3: Dissolve 5 parts of sodium citrate in water, add 5 parts of the mixture M obtained in step S2, stir at 80°C for 1 hour, then filter, wash twice with water, and dry in vacuum for 10 hours to obtain an antistatic agent.

S4: Mix and stir 20 parts of antistatic agent and 100 parts of ethylene glycol for 2 hours, then raise the temperature to 80° C. and continue stirring for 2 hours, and disperse evenly to obtain antistatic agent slurry.

S5: Dissolve 1 part of tetrabutyl titanate in 500 parts of ethylene glycol, stir evenly to prepare a catalyst slurry, then add the catalyst slurry to 1000 parts of ethylene glycol and 4000 parts of terephthalic acid, stir evenly, and prepare The raw materials for the polymerization reaction were obtained.

S6: Add 10 parts of antistatic slurry to 100 parts of polymerization reaction raw materials, stir evenly, and add into the reaction kettle from the feeding port.

S7: Carry out the esterification reaction at a temperature of 230°C and a pressure of 0.2MPa. When the effluent value reaches the theoretical value, carry out a polycondensation reaction, raise the temperature to 275°C, and at the same time evacuate to an absolute pressure of ≤150Pa, and the polycondensation reaction time is 60min After the polycondensation reaction is completed, the material is discharged and then dried and pelletized to obtain antistatic polyester chips.

S8: Melt-spinning antistatic polyester chips, and then forming antistatic fibers through fiber forming, drawing and orientation of nascent fibers, heat setting and winding of fibers; blending the obtained antistatic fibers into yarns, according to Antistatic textile fabrics are made by conventional weft knitting process.

Example 2

S1: Calculated by weight components, dissolve 10 parts of graphene oxide in 1500 parts of water, ultrasonically disperse for 3 hours to obtain graphene oxide hydrosol, and then add 2 parts of dodecyltrimethyl chloride to the graphene oxide hydrosol ammonium chloride, stirred at a constant temperature of 60°C, then filtered, washed with water three times, and vacuum-dried at 100°C for 18 hours to obtain modified graphene oxide.

S2: Dissolve 15 parts of modified graphene oxide in 1500 parts of water, ultrasonically disperse for 3 hours to obtain modified graphene oxide hydrosol, and then add 30 parts of KH-560 to the modified graphene oxide hydrosol and 30 parts of nano-silica, stirred at 60°C for 3 hours, then filtered, washed with water three times, and vacuum-dried at 100°C for 12 hours to obtain a mixture M.

S3: Dissolve 10 parts of sodium citrate in water, add 10 parts of the mixture M obtained in step S2, stir at 100°C for 2 hours, then filter, wash with water three times and dry in vacuum for 15 hours to obtain an antistatic agent.

S4: 30 parts of antistatic agent and 100 parts of ethylene glycol were mixed and stirred for 3 hours, then heated to 90° C. and stirred for 3 hours, and dispersed uniformly to obtain an antistatic agent slurry.

S5: Dissolve 1-2 parts of tetrabutyl titanate in 600 parts of ethylene glycol, stir evenly to prepare a catalyst slurry, then add the catalyst slurry to 1500 parts of ethylene glycol and 5000 parts of terephthalic acid, and stir evenly , to obtain the raw materials for the polymerization reaction.

S6: Add 20 parts of antistatic slurry to 100 parts of polymerization reaction raw materials, stir evenly, and add into the reaction kettle from the feed port.

S7: Carry out the esterification reaction at a temperature of 240°C and a pressure of 0.3MPa. When the effluent value reaches the theoretical value, carry out the polycondensation reaction, raise the temperature to 280°C, and at the same time evacuate to an absolute pressure of ≤150Pa, and the polycondensation reaction time is 90min After the polycondensation reaction is completed, the material is discharged and then dried and pelletized to obtain antistatic polyester chips.

S8: Melt-spinning antistatic polyester chips, and then forming antistatic fibers through fiber forming, drawing and orientation of nascent fibers, heat setting and winding of fibers; blending the obtained antistatic fibers into yarns, according to Antistatic textile fabrics are made by conventional weft knitting process.

Example 3

S1: Calculated by weight components, dissolve 7.5 parts of graphene oxide in 1350 parts of water, ultrasonically disperse for 2.5 hours to obtain graphene oxide hydrosol, and then add 1.5 parts of dodecyltrimethyl to the graphene oxide hydrosol ammonium chloride, stirred at a constant temperature of 55°C, then filtered, washed twice with water, and vacuum-dried at 90°C for 17 hours to obtain modified graphene oxide.

S2: 12.5 parts of modified graphene oxide were dissolved in 1350 parts of water, ultrasonically dispersed for 2.5h to obtain modified graphene oxide hydrosol, and then 25 parts of KH- 560 and 27.5 parts of nano-silica, stirred at a constant temperature of 55°C for 2.5h, then filtered, washed twice with water, and vacuum-dried at 90°C for 11h to obtain a mixture M.

S3: Dissolve 7.5 parts of sodium citrate in water, add 7.5 parts of the mixture M obtained in step S2, stir at 90°C for 1.5 minutes, then filter, wash twice with water, and dry in vacuum for 13.5 hours to obtain an antistatic agent.

S4: 25 parts of antistatic agent and 100 parts of ethylene glycol were mixed and stirred for 2.5 hours, then heated to 85° C. and stirred for 2.5 hours, and dispersed uniformly to obtain antistatic agent slurry.

S5: Dissolve 1-2 parts of tetrabutyl titanate in 550 parts of ethylene glycol, stir evenly to prepare a catalyst slurry, then add the catalyst slurry to 1350 parts of ethylene glycol and 4500 parts of terephthalic acid, and stir evenly , to obtain the raw materials for the polymerization reaction.

S6: Add 15 parts of antistatic slurry to 100 parts of polymerization reaction raw materials, stir evenly, and add into the reaction kettle from the feed port.

S7: Carry out the esterification reaction at a temperature of 235°C and a pressure of 0.25MPa. When the effluent value reaches the theoretical value, carry out a polycondensation reaction, raise the temperature to 277.5°C, and at the same time evacuate to an absolute pressure of ≤150Pa, and the polycondensation reaction time is 75min After the polycondensation reaction is completed, the material is discharged and then dried and pelletized to obtain antistatic polyester chips.

S8: Melt-spinning antistatic polyester chips, and then forming antistatic fibers through fiber forming, drawing and orientation of nascent fibers, heat setting and winding of fibers; blending the obtained antistatic fibers into yarns, according to Antistatic textile fabrics are made by conventional weft knitting process.

Example 4

S1: Calculated by weight components, dissolve 8 parts of graphene oxide in 1100 parts of water, ultrasonically disperse for 2 hours to obtain graphene oxide hydrosol, and then add 1 part of dodecyltrimethyl chloride to the graphene oxide hydrosol ammonium chloride, stirred at a constant temperature of 50°C, then filtered, washed with water three times, and vacuum-dried at 80°C for 17 hours to obtain modified graphene oxide.

S2: Dissolve 10 parts of modified graphene oxide in 1200 parts of water, ultrasonically disperse for 2 hours to obtain modified graphene oxide hydrosol, and then add 20 parts of KH-560 to the modified graphene oxide hydrosol and 25 parts of nano-silica, stirred at 50°C for 2 hours, then filtered, washed twice with water, and vacuum-dried at 85°C for 11 hours to obtain a mixture M.

S3: Dissolve 7 parts of sodium citrate in water, add 7 parts of the mixture M obtained in step S2, stir at 85°C for 1 hour, then filter, wash twice with water, and dry in vacuum for 10 hours to obtain an antistatic agent.

S4: 28 parts of antistatic agent and 100 parts of ethylene glycol were mixed and stirred for 2 hours, then heated to 80° C. and stirred for 2 hours, and dispersed uniformly to obtain antistatic agent slurry.

S5: Dissolve 1 part of tetrabutyl titanate in 500 parts of ethylene glycol, stir evenly to prepare a catalyst slurry, then add the catalyst slurry to 1000 parts of ethylene glycol and 4000 parts of terephthalic acid, stir evenly, and prepare The raw materials for the polymerization reaction were obtained.

S6: Add 18 parts of antistatic slurry to 100 parts of polymerization raw materials, stir evenly, and add to the reaction kettle from the feed port.

S7: Carry out the esterification reaction at a temperature of 230°C and a pressure of 0.2MPa. When the effluent value reaches the theoretical value, carry out a polycondensation reaction, raise the temperature to 275°C, and at the same time evacuate to an absolute pressure of ≤150Pa, and the polycondensation reaction time is 60min After the polycondensation reaction is completed, the material is discharged and then dried and pelletized to obtain antistatic polyester chips.

S8: Melt-spinning antistatic polyester chips, and then forming antistatic fibers through fiber forming, drawing and orientation of nascent fibers, heat setting and winding of fibers; blending the obtained antistatic fibers into yarns, according to Antistatic textile fabrics are made by conventional weft knitting process.

Comparative example 1

S1: Calculated by weight components, dissolve 5 parts of graphene oxide in 1000 parts of water, ultrasonically disperse for 2 hours to obtain graphene oxide hydrosol, and then add 1 part of dodecyltrimethyl chloride to the graphene oxide hydrosol ammonium chloride, stirred at a constant temperature of 50°C, then filtered, washed twice with water, and vacuum-dried at 80°C for 16 hours to obtain modified graphene oxide.

S2: 5 parts of sodium citrate are dissolved in water, and 5 parts of modified graphene oxide are added. Stir at 80°C for 1 hour, then filter, wash twice with water, and dry in vacuum for 10 hours to obtain an antistatic agent.

S3: 20 parts of antistatic agent and 100 parts of ethylene glycol were mixed and stirred for 2 hours, then heated to 80° C. and stirred for 2 hours, and dispersed evenly to obtain an antistatic agent slurry.

S4: Dissolve 1 part of tetrabutyl titanate in 500 parts of ethylene glycol, stir evenly to prepare a catalyst slurry, then add the catalyst slurry to 1000 parts of ethylene glycol and 4000 parts of terephthalic acid, stir evenly, and prepare The raw materials for the polymerization reaction were obtained.

S5: Add 10 parts of antistatic slurry to 100 parts of polymerization reaction raw materials, stir evenly, and add into the reaction kettle from the feeding port.

S6: Carry out the esterification reaction at a temperature of 230°C and a pressure of 0.2MPa. When the effluent value reaches the theoretical value, carry out the polycondensation reaction, raise the temperature to 275°C, and at the same time evacuate to an absolute pressure of ≤150Pa, and the polycondensation reaction time is 60min After the polycondensation reaction is completed, the material is discharged and then dried and pelletized to obtain antistatic polyester chips.

S7: Melt-spinning antistatic polyester chips, and then forming antistatic fibers through fiber forming, drawing and orientation of nascent fibers, heat setting and winding of fibers; blending the obtained antistatic fibers into yarns, according to Antistatic textile fabrics are made by conventional weft knitting process.

Compared with Example 1, Comparative Example 1 omits S2 in Example 1, and the rest of the steps are the same.

Comparative example 2

S1: Calculated by weight components, dissolve 5 parts of graphene oxide in 1000 parts of water, ultrasonically disperse for 2 hours to obtain graphene oxide hydrosol, and then add 1 part of dodecyltrimethyl chloride to the graphene oxide hydrosol ammonium chloride, stirred at a constant temperature of 50°C, then filtered, washed twice with water, and vacuum-dried at 80°C for 16 hours to obtain modified graphene oxide.

S2: Dissolve 10 parts of modified graphene oxide in 1200 parts of water, ultrasonically disperse for 2 hours to obtain modified graphene oxide hydrosol, and then add 20 parts of KH-560 to the modified graphene oxide hydrosol and 25 parts of nano-silica, stirred at 50°C for 2h, then filtered, washed twice with water, and vacuum-dried at 80°C for 10h to obtain a mixture M.

S3: Dissolve 5 parts of sodium citrate in water, add 5 parts of the mixture M obtained in step S2, stir at 80°C for 1 hour, then filter, wash twice with water, and dry in vacuum for 10 hours to obtain an antistatic agent.

S4: Mix and stir 20 parts of antistatic agent and 100 parts of ethylene glycol for 2 hours, then raise the temperature to 80° C. and continue stirring for 2 hours, and disperse evenly to obtain antistatic agent slurry.

S5: Dissolve 1 part of tetrabutyl titanate in 500 parts of ethylene glycol, stir evenly to prepare a catalyst slurry, then add the catalyst slurry to 1000 parts of ethylene glycol and 4000 parts of terephthalic acid, stir evenly, and prepare The raw materials for the polymerization reaction were obtained.

S6: Add 5 parts of antistatic slurry to 100 parts of polymerization reaction raw materials, stir evenly, and add to the reaction kettle from the feed port.

S7: Carry out the esterification reaction at a temperature of 230°C and a pressure of 0.2MPa. When the effluent value reaches the theoretical value, carry out a polycondensation reaction, raise the temperature to 275°C, and at the same time evacuate to an absolute pressure of ≤150Pa, and the polycondensation reaction time is 60min After the polycondensation reaction is completed, the material is discharged and then dried and pelletized to obtain antistatic polyester chips.

S8: Melt-spinning antistatic polyester chips, and then forming antistatic fibers through fiber forming, drawing and orientation of nascent fibers, heat setting and winding of fibers; blending the obtained antistatic fibers into yarns, according to Antistatic textile fabrics are made by conventional weft knitting process.

Compared with Example 1 in Comparative Example 2, in S6, 5 parts of the antistatic agent slurry was added, and the rest of the steps were the same.

Comparative example 3

S1: Calculated by weight components, dissolve 5 parts of graphene oxide in 1000 parts of water, ultrasonically disperse for 2 hours to obtain graphene oxide hydrosol, and then add 1 part of dodecyltrimethyl chloride to the graphene oxide hydrosol ammonium chloride, stirred at a constant temperature of 50°C, then filtered, washed twice with water, and vacuum-dried at 80°C for 16 hours to obtain modified graphene oxide.

S2: Dissolve 10 parts of modified graphene oxide in 1200 parts of water, ultrasonically disperse for 2 hours to obtain modified graphene oxide hydrosol, and then add 20 parts of KH-560 to the modified graphene oxide hydrosol and 25 parts of nano-silica, stirred at 50°C for 2h, then filtered, washed twice with water, and vacuum-dried at 80°C for 10h to obtain a mixture M.

S3: Dissolve 5 parts of sodium citrate in water, add 5 parts of the mixture M obtained in step S2, stir at 80°C for 1 hour, then filter, wash twice with water, and dry in vacuum for 10 hours to obtain an antistatic agent.

S4: Mix and stir 20 parts of antistatic agent and 100 parts of ethylene glycol for 2 hours, then raise the temperature to 80° C. and continue stirring for 2 hours, and disperse evenly to obtain antistatic agent slurry.

S5: Dissolve 1 part of tetrabutyl titanate in 500 parts of ethylene glycol, stir evenly to prepare a catalyst slurry, then add the catalyst slurry to 1000 parts of ethylene glycol and 4000 parts of terephthalic acid, stir evenly, and prepare The raw materials for the polymerization reaction were obtained.

S6: Add 25 parts of antistatic slurry to 100 parts of polymerization reaction raw materials, stir evenly, and add to the reaction kettle from the feed port.

S7: Carry out the esterification reaction at a temperature of 230°C and a pressure of 0.2MPa. When the effluent value reaches the theoretical value, carry out a polycondensation reaction, raise the temperature to 275°C, and at the same time evacuate to an absolute pressure of ≤150Pa, and the polycondensation reaction time is 60min After the polycondensation reaction is completed, the material is discharged and then dried and pelletized to obtain antistatic polyester chips.

S8: Melt-spinning antistatic polyester chips, and then forming antistatic fibers through fiber forming, drawing and orientation of nascent fibers, heat setting and winding of fibers; blending the obtained antistatic fibers into yarns, according to Antistatic textile fabrics are made by conventional weft knitting process.

Compared with Example 1 in Comparative Example 3, in S6, 25 parts of the antistatic agent slurry was added, and the rest of the steps were the same.

Embodiment 1-3, comparative example 1-3, carry out antistatic test to the prepared antistatic textile fabric.

It can be seen that Example 4 is the best ratio, and Comparative Example 1, due to the lack of coupled nano-silica, leads to a decrease in the hygroscopicity of the fabric and a high resistivity, resulting in a decrease in the antistatic property of the fabric. In Comparative Example 2, due to the low proportion of antistatic liquid added, the antistatic property of the fabric was insufficient. In Comparative Example 3, due to the addition of too much antistatic liquid, impurities in the molecular chain of polyethylene terephthalate were excessive, and the spinnability decreased. , cannot be used for textiles.

Finally, it should be noted that: the above is only a preferred embodiment of the present invention, and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, for those skilled in the art, it still The technical solutions recorded in the foregoing embodiments may be modified, or some technical features thereof may be equivalently replaced. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included within the protection scope of the present invention.

Claims (9)

1. A preparation method of an antistatic textile fabric is characterized by comprising the following steps: comprises the following steps of (a) carrying out,

s1: dissolving graphene oxide in water, performing ultrasonic dispersion to obtain graphene oxide hydrosol, adding dodecyl trimethyl ammonium chloride into the graphene oxide hydrosol, stirring at a constant temperature, filtering, washing and drying to obtain modified graphene oxide;

s2: dissolving the modified graphene oxide in water, performing ultrasonic dispersion to obtain a modified graphene oxide hydrosol, adding KH-560 and nano silicon dioxide into the modified graphene oxide hydrosol, stirring at a constant temperature, filtering, washing with water, and drying to obtain a mixture M;

s3: dissolving sodium citrate in water, adding the mixture M obtained in the step S2, stirring at constant temperature, filtering, washing with water and drying to obtain the antistatic agent;

s4: mixing and stirring the antistatic agent and glycol, and uniformly dispersing to obtain antistatic agent slurry;

s5: dissolving tetrabutyl titanate in ethylene glycol, and uniformly stirring to prepare catalyst slurry; adding the catalyst slurry into terephthalic acid and ethylene glycol, and uniformly stirring to obtain a polymerization reaction raw material;

s6: adding the antistatic agent slurry into a polymerization reaction raw material, uniformly stirring, and putting into a polyester reaction kettle;

s7: after the polymerization reaction is finished, discharging, and then drying and dicing to obtain antistatic polyester chips;

s8: carrying out melt spinning on the antistatic polyester chip, and then carrying out fiber forming, primary fiber drafting orientation, fiber heat setting and winding to prepare antistatic fiber; and (3) blending the prepared antistatic fibers into yarns, and preparing the antistatic woven fabric according to a conventional weft knitting weaving process.

2. The method for preparing an antistatic textile fabric according to claim 1, characterized in that: the specific process of the step S1 comprises the steps of dissolving 5-10 parts of graphene oxide in 1000-1500 parts of water by weight, ultrasonically dispersing for 2-3 hours to obtain graphene oxide hydrosol, adding 1-2 parts of dodecyl trimethyl ammonium chloride into the graphene oxide hydrosol, stirring at a constant temperature of 50-60 ℃, filtering, washing for 2-3 times by using water, and vacuum drying at a temperature of 80-100 ℃ for 16-18 hours to obtain the modified graphene oxide.

3. The method for preparing an antistatic textile fabric according to claim 1, characterized in that: the specific process of the step S2 comprises the steps of dissolving 10-15 parts of modified graphene oxide in 1200-1500 parts of water by weight, carrying out ultrasonic dispersion for 2-3 hours to obtain modified graphene oxide hydrosol, adding 20-30 parts of KH-560 and 25-30 parts of nano silicon dioxide into the modified graphene oxide hydrosol, stirring at the constant temperature of 50-60 ℃ for 2-3 hours, filtering, washing for 2-3 times, and carrying out vacuum drying at the temperature of 80-100 ℃ for 10-12 hours to obtain a mixture M.

4. The method for preparing an antistatic textile fabric according to claim 1, characterized in that: and the specific process of the step S3 comprises the steps of dissolving 5-10 parts by weight of sodium citrate in water, adding 5-10 parts by weight of the mixture M obtained in the step S2, stirring at a constant temperature of 80-100 ℃ for 1-2h, filtering, washing with water for 2-3 times, and drying in vacuum for 10-15h to obtain the antistatic agent.

5. The method for preparing an antistatic textile fabric according to claim 1, characterized in that: and the specific process of the step S4 is that 20-30 parts of antistatic agent and 100 parts of glycol are mixed and stirred for 2-3h according to the weight components, then the temperature is raised to 80-90 ℃, the stirring is continued for 2-3h, and the antistatic agent slurry is uniformly dispersed, so that the antistatic agent slurry is obtained.

6. The method for preparing an antistatic textile fabric according to claim 1, characterized in that: and the specific process of the step S5 is that 1-2 parts of tetrabutyl titanate is dissolved in 500-600 parts of ethylene glycol by weight, the mixture is uniformly stirred to prepare catalyst slurry, and then the catalyst slurry is added into 1000-1500 parts of ethylene glycol and 4000-5000 parts of terephthalic acid, and the mixture is uniformly stirred to prepare the polymerization reaction raw material.

7. The method for preparing an antistatic textile fabric according to claim 1, characterized in that: the specific process of the step S6 is that 10 to 20 parts of antistatic slurry is added into 100 parts of polymerization reaction raw materials by weight, is uniformly stirred and is added into the reaction kettle from a feed inlet.

8. The method for preparing an antistatic textile fabric according to claim 1, characterized in that: and the specific process of the step S7 is that esterification reaction is carried out under the conditions that the temperature is 230-240 ℃ and the pressure is 0.2-0.3MPa, when the water outlet value reaches a theoretical value, polycondensation reaction is carried out, the temperature is increased to 275-280 ℃, meanwhile, vacuum pumping is carried out until the absolute pressure is less than or equal to 150Pa, the polycondensation reaction time is 60-90min, and after the polycondensation reaction is finished, discharging, drying and pelletizing are carried out, so that the antistatic polyester slice is obtained.

9. The method for preparing an antistatic textile fabric according to claim 1, characterized in that: is applied to the field of medical protective clothing.

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