阅读说明：本技术 一种抗静电功能纺织纤维的制备工艺 (Preparation process of textile fiber with antistatic function ) 是由 金桃勇 许秋梅 于 2020-06-11 设计创作，主要内容包括：本发明公开一种抗静电功能纺织纤维的制备工艺,称取如下重量份原料：35-50份丙烯腈,10-15份2-甲基-2-丁烯腈,0.5-1.5份过硫酸钠,2-3.5份亚硫酸钠,55-70份正丁醇,25-35份抗静电剂；该具有抗静电功能的纺织纤维,通过熔融纺织制备出纤维,通过高温使得制备出的纤维干燥致密化,进而能够将抗静电剂包缠在纤维的微孔中,进而赋予纤维永久的抗静电性能,而且能够提高该纤维的力学性能；该抗静电剂不带电荷且极性小,在水中不离解成离子,无法通过自身导电泄露电荷,所以能够起到抗静电效果,而且该抗静电剂结构稳定,既具有优异的抗静电性能,又具有良好的稳定性。(The invention discloses a preparation process of antistatic functional textile fiber, which comprises the following raw materials in parts by weight: 35-50 parts of acrylonitrile, 10-15 parts of 2-methyl-2-butenenitrile, 0.5-1.5 parts of sodium persulfate, 2-3.5 parts of sodium sulfite, 55-70 parts of n-butyl alcohol and 25-35 parts of antistatic agent; the textile fiber with the antistatic function is prepared by melt spinning, and the prepared fiber is dried and densified through high temperature, so that an antistatic agent can be wrapped in micropores of the fiber, the fiber is endowed with permanent antistatic performance, and the mechanical performance of the fiber can be improved; the antistatic agent is uncharged and small in polarity, does not dissociate into ions in water, cannot conduct electricity through the antistatic agent and leak the charges, so that an antistatic effect can be achieved, and the antistatic agent is stable in structure, has excellent antistatic performance and good stability.)

1. A preparation process of antistatic functional textile fiber is characterized by comprising the following steps:

step S1, weighing the following raw materials in parts by weight: 35-50 parts of acrylonitrile, 10-15 parts of 2-methyl-2-butenenitrile, 0.5-1.5 parts of sodium persulfate, 2-3.5 parts of sodium sulfite, 55-70 parts of n-butyl alcohol and 25-35 parts of antistatic agent;

step S2, adding deionized water into a reaction kettle, heating to 40-45 ℃, sequentially adding acrylonitrile and 2-methyl-2-butenenitrile, heating to 65-75 ℃, adding sodium persulfate, performing magnetic stirring at the rotating speed of 150r/min, stirring for 15min, adding n-butanol, continuing stirring for 2-3h to obtain a mixture, filtering, washing, transferring to a vacuum oven, and drying at 80-90 ℃ for 10h to obtain polyacrylonitrile resin;

and S3, uniformly mixing the polyacrylonitrile resin prepared in the step S2 and an antistatic agent, blending, extruding and granulating by using a double-screw extruder to prepare antistatic master batches, drying the antistatic master batches at the temperature of 110-120 ℃ for 6-10h, feeding the dried antistatic master batches into a feeder of a spinning machine for melt spinning, and controlling the spinning speed to be 2500m/min and the initial pressure of a spinning assembly to be 8MPa to prepare the antistatic functional textile fiber.

2. The preparation process of the antistatic functional textile fiber according to claim 1, wherein the antistatic agent is prepared from the following raw materials in parts by weight: 50-80 parts of 25% formaldehyde solution, 10-20 parts of hexamethylenetetramine, 4-6 parts of urea, 35-50 parts of ethylene oxide, 3.5-5 parts of 10% diluted hydrochloric acid and 0.5-2.0 parts of potassium carbonate.

3. The process for preparing antistatic functional textile fiber according to claim 1, wherein the antistatic agent is prepared by the following method:

(1) adding 25% of formaldehyde solution and hexamethylenetetramine into a three-neck flask, heating in a water bath at 45 ℃, magnetically stirring for 30-40min, adding urea, stirring for 10min at the rotating speed of 120r/min, then heating to 85-95 ℃, adding urea again, stirring at the rotating speed of 250r/min, reacting for 60-80min at the temperature, and then adjusting the pH value by using 10% of sodium hydroxide solution until the pH value is 8 to prepare resin A;

(2) and (2) adding the resin A prepared in the step (1) into a beaker filled with deionized water, heating to 75-80 ℃, magnetically stirring at the rotating speed of 120r/min for 30-45min, adding ethylene oxide and potassium carbonate, continuously stirring for 10min, adding 10% dilute hydrochloric acid, heating to 100 ℃, magnetically stirring for 3h, transferring to a vacuum drying oven, and drying until the solvent is completely evaporated to prepare the antistatic agent.

4. The process for preparing antistatic functional textile fiber according to claim 3, wherein the weight ratio of the first and second urea additions in step (2) is 1: 2.

5. The process for preparing textile fiber with antistatic function as claimed in claim 3, wherein the vacuum degree of the vacuum drying oven in step (2) is controlled to be-0.09 MPa and the temperature is controlled to be 100 ℃ and 110 ℃.

Technical Field

The invention belongs to the technical field of textile fiber preparation, and particularly relates to a preparation process of textile fiber with an antistatic function.

Background

The antistatic problem is a persistent problem faced by chemical fiber fabrics, some solutions are provided at present, for example, the solutions are from the origin of fibers, conductive fibers can be prepared, for example, the conductive fibers are prepared by adopting a high-addition and composite spinning technology, the used conductive powder is ATO, AZO, ITO, conductive carbon black and the like, the resistance of the fibers can reach 106 ohms or even lower, the antistatic requirement of the fabrics can be completely met, and the antistatic conductive fiber fabric has wide application in some safety fields at present. However, such fibers also have irreparable disadvantages: firstly, the cost is too high; secondly, the mechanical property of the fiber is poor; thirdly, the diameter of the fiber is too thick; fourth, the color difference of the fibers. At present, more fabrics in the market adopt antistatic after-finishing to realize the antistatic function of the fabrics, and compared with the mode of using conductive fibers, the mode has the advantages of lower cost and obvious effect, thereby being used by most fabric manufacturers.

The Chinese invention patent CN107022805B discloses a preparation method of an in-situ polymerization composite conductive/antistatic fiber, which comprises the steps of surface modification of nano conductive powder, preparation of an antistatic master batch, drying the antistatic master batch at the temperature of 100-180 ℃ for 2-8 hours, uniformly mixing the antistatic master batch and basic resin slices, and then carrying out melt spinning at the spinning speed of 600-3000m/min and the initial pressure of a spinning component of 8-16MPa to obtain the in-situ polymerization composite conductive/antistatic fiber. The invention adopts a brand new antistatic mechanism to prepare new antistatic fiber, has permanent antistatic function, mechanical property can reach the standard of common fiber, completely meets various weaving requirements, has the cost equivalent to that of antistatic after finishing, is only one fourth of the cost of using white conductive fiber, reduces pollution, can expand the export of textiles and improves the added value of the textiles.

Disclosure of Invention

In order to overcome the technical problems, the invention provides a preparation process of antistatic functional textile fibers.

The technical problems to be solved by the invention are as follows:

urea and formaldehyde form hydroxymethyl derivatives (methylol ureas) during the reaction, but the formed hydroxymethyl derivatives (methylol ureas) undergo condensation reactions.

The fiber is prepared through melt spinning, and the prepared fiber is dried and densified through high temperature, so that the antistatic agent can be wrapped in micropores of the fiber, the permanent antistatic performance is given to the fiber, and the mechanical performance of the fiber can be improved.

The purpose of the invention can be realized by the following technical scheme:

a preparation process of antistatic functional textile fiber comprises the following steps:

step S1, weighing the following raw materials in parts by weight: 35-50 parts of acrylonitrile, 10-15 parts of 2-methyl-2-butenenitrile, 0.5-1.5 parts of sodium persulfate, 2-3.5 parts of sodium sulfite, 55-70 parts of n-butyl alcohol and 25-35 parts of antistatic agent;

step S2, adding deionized water into a reaction kettle, heating to 40-45 ℃, sequentially adding acrylonitrile and 2-methyl-2-butenenitrile, heating to 65-75 ℃, adding sodium persulfate, performing magnetic stirring at the rotating speed of 150r/min, stirring for 15min, adding n-butanol, continuing stirring for 2-3h to obtain a mixture, filtering, washing, transferring to a vacuum oven, and drying at 80-90 ℃ for 10h to obtain polyacrylonitrile resin;

and S3, uniformly mixing the polyacrylonitrile resin prepared in the step S2 and an antistatic agent, blending, extruding and granulating by using a double-screw extruder to prepare antistatic master batches, drying the antistatic master batches at the temperature of 110-120 ℃ for 6-10h, feeding the dried antistatic master batches into a feeder of a spinning machine for melt spinning, and controlling the spinning speed to be 2500m/min and the initial pressure of a spinning assembly to be 8MPa to prepare the antistatic functional textile fiber.

Firstly, acrylonitrile, 2-methyl-2-butenenitrile and other raw materials are used for preparing polyacrylonitrile resin, in the preparation step S3, the polyacrylonitrile resin and the antistatic agent are uniformly mixed, then extrusion, granulation and spinning are carried out, the textile fiber with the antistatic function is prepared, in the process, the fiber is prepared through melt spinning, the prepared fiber is dried and densified through high temperature, and then the antistatic agent can be wrapped in micropores of the fiber, so that the fiber is endowed with permanent antistatic performance.

Further, the antistatic agent is prepared from the following raw materials in parts by weight: 50-80 parts of 25% formaldehyde solution, 10-20 parts of hexamethylenetetramine, 4-6 parts of urea, 35-50 parts of ethylene oxide, 3.5-5 parts of 10% diluted hydrochloric acid and 0.5-2.0 parts of potassium carbonate.

Further, the antistatic agent is prepared by the following method:

(1) adding 25 mass percent of formaldehyde solution and hexamethylenetetramine into a three-neck flask, heating in a water bath at 45 ℃ and magnetically stirring for 30-40min, adding urea, stirring for 10min at the rotating speed of 120r/min, then heating to 85-95 ℃, adding urea again, stirring at the rotating speed of 250r/min, reacting for 60-80min at the temperature, and then adjusting the pH value with 10 mass percent of sodium hydroxide solution until the pH value is 8 to prepare resin A;

(2) and (2) adding the resin A prepared in the step (1) into a beaker filled with deionized water, heating to 75-80 ℃, magnetically stirring at the rotating speed of 120r/min for 30-45min, adding ethylene oxide and potassium carbonate, continuously stirring for 10min, adding dilute hydrochloric acid with the mass fraction of 10%, heating to 100 ℃, magnetically stirring for 3h, transferring to a vacuum drying oven, and drying until the solvent is completely evaporated to prepare the antistatic agent.

Mixing a formaldehyde solution and hexamethylenetetramine in the step (1), and then adding urea twice, wherein in the reaction process, formaldehyde can perform an addition reaction with amino, namely a hydroxymethylation reaction of the amino to form a hydroxymethyl derivative, and the pH value is adjusted to 8 so as to ensure that the urea and the formaldehyde form the hydroxymethyl derivative (hydroxymethyl urea) and prevent the hydroxymethyl derivative from performing a condensation reaction, so that a resin A is finally prepared, the use amounts of the formaldehyde and the urea are controlled, the reaction process can be accelerated, the resin A has no time adjustment structure in the reaction process, and microspheres with smooth surfaces are further formed, so that the structure is stable, and the stability of the resin A is enhanced; and then step (2) mixing the resin A with ethylene oxide to prepare the antistatic agent, wherein the antistatic agent is actually a polyoxyethylene type nonionic antistatic agent, has no electric charge and small polarity, is not dissociated into ions in water, and cannot leak electric charge through self conduction, so that an antistatic effect can be achieved, 10% dilute hydrochloric acid is added in the reaction process of the resin A and the ethylene oxide, the hydrochloric acid can perform affinity addition on the ethylene oxide to generate a catalytic action, and further the reaction process is accelerated, and the prepared resin A reacts with the ethylene oxide, so that the prepared antistatic agent is stable in structure, has excellent antistatic performance and good stability.

Further, the weight ratio of the urea added for the first time and the urea added for the second time in the step (2) is 1: 2.

Further, in the step (2), the vacuum degree of the vacuum drying oven is controlled to be-0.09 MPa, and the temperature is controlled to be 100-.

The invention has the beneficial effects that:

(1) in the preparation process of the antistatic textile fiber, firstly, polyacrylonitrile resin is prepared from raw materials such as acrylonitrile, 2-methyl-2-butenenitrile and the like, the polyacrylonitrile resin and an antistatic agent are uniformly mixed in the preparation step S3, and then the mixture is extruded, granulated and spun to prepare the antistatic textile fiber;

(2) the invention also prepares an antistatic agent, in the preparation process, the formaldehyde solution and hexamethylenetetramine are mixed in the step (1), then urea is added in twice, in the reaction process, firstly, formaldehyde can generate addition reaction with amino, namely, hydroxymethylation reaction of amino to form hydroxymethyl derivatives, and the pH value is adjusted to 8 so as to ensure that urea and formaldehyde form hydroxymethyl derivatives (hydroxymethyl urea) and prevent the hydroxymethyl derivatives from generating condensation reaction, so that the resin A is finally prepared, the use amounts of formaldehyde and urea are controlled, the reaction process can be accelerated, so that the resin A has no time adjustment structure in the reaction process, and further microspheres with smooth surfaces are formed, the structure is stable, and the stability performance of the resin A is enhanced; then, the resin A is mixed with ethylene oxide in the step (2) to prepare an antistatic agent, the antistatic agent is actually a polyoxyethylene type nonionic antistatic agent, the antistatic agent is uncharged and small in polarity, ions are not dissociated in water, and charges cannot be leaked through self conduction, so that an antistatic effect can be achieved, 10% dilute hydrochloric acid is added in the reaction process of the resin A and the ethylene oxide, the hydrochloric acid can perform affinity addition on the ethylene oxide to generate a catalytic action, the reaction process is further accelerated, and the prepared resin A and the ethylene oxide react, so that the prepared antistatic agent is stable in structure, has excellent antistatic performance and good stability; the technical problem that the hydroxymethyl derivative (hydroxymethyl urea) is formed in the reaction process of urea and formaldehyde, but the formed hydroxymethyl derivative (hydroxymethyl urea) can undergo condensation reaction is solved.

Drawings

In order to facilitate understanding for those skilled in the art, the present invention will be further described with reference to the accompanying drawings.

FIG. 1 is a reaction scheme of step (2) of the antistatic agent preparation process.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.