CN110904530B - A kind of anti-pilling elastic fiber material and preparation method thereof - Google Patents

Abstract

The invention relates to an anti-pilling elastic fiber material and a preparation method thereof, belonging to the technical field of textile fabrics. In the technical scheme of the present invention, the technical scheme of the present invention adopts the nano-gel material to cooperate with the fibroin dialysate, which effectively improves the bonding fastness of the fiber and the finishing agent, and reduces the directional friction effect of the polyester fiber during use. It can further improve the directional friction effect of polyester fiber in the process of use, and further improve the anti-pilling performance of the material by forming a film by using silk fibroin as the finishing agent material, and at the same time, the low-temperature sol coating can first improve the structure of the material. Anti-pilling At the same time, the polyester fiber is rapidly cooled, so that the prepared polyester fiber has good stability, good elasticity and excellent mechanical properties.

Description

A kind of anti-pilling elastic fiber material and preparation method thereof

technical field

The invention relates to an anti-pilling elastic fiber material and a preparation method thereof, belonging to the technical field of textile fabrics.

Background technique

The elastic polyester fiber family includes elastic yarn, PBT fiber, PTT fiber, polyether fiber, composite polyester fiber (PET/PTT, PET/PBT, modified PET/conventional PET, etc.). Although both belong to the polyester family, their elastic mechanisms are different from each other. Usually pre-oriented yarn or fully drawn yarn and other raw yarn are processed into a small spring-like crimped wire through twisting deformation or twisting and shaping-untwisting process. The elasticity of this kind of silk is not strong, the tension should be small when processing at high temperature, and the time should not be long, because as the spring shape becomes loose or disappears, the elasticity of the textile will be greatly reduced. The macromolecular chain in the crystal region of the PBT polymer is a plane zigzag shape, which is not fully unfolded. In each PBT macromolecular repeating unit, there are 4 methylene flexible groups. The lattice structure of PBT polymer will undergo reversible conversion from a crystal form to p crystal form. This reversible structural change endows PBT fibers with excellent elastic properties. In addition, PBT can also be used in other fields, such as nano-coating materials obtained by compounding with inorganic oxides. Compared with the even number of methylene units in the chemical structure of PET and PBT, PTT exists between terephthalic acid units. With 3 methylene groups, the odd number of methylene units in this chemical structure will produce an "odd carbon effect" between the macromolecular chains,

However, in the existing polyester fiber polyester fiber fabric, the end of the fiber yarn is exposed to the cloth surface due to friction during use, and the formed hairiness is entangled with each other to form a hair ball, and the hair ball will not fall off, affecting the appearance of the clothing, and it is easy to Contamination of dust reduces the use value of the fabric, so it is necessary to produce a polyester fiber elastic material with excellent anti-pilling properties.

SUMMARY OF THE INVENTION

The purpose of the present invention is to provide an anti-pilling elastic fiber material and a preparation method thereof to solve the problems in the prior art.

To achieve the above object, the present invention provides the following technical solutions:

An anti-pilling elastic fiber material is prepared by spinning and drawing modified polyester, and then finishing with a finishing agent at a low temperature. The modified polyester is made of purified terephthalic acid and ethylene glycol. The raw material is prepared by adding deionized water, carbon nanotubes, tetrabutyl titanate and catalyst through vacuum polycondensation. The finishing agent is ethanol, calcium chloride and degummed silk, which are dissolved and then dialyzed, and nano titanium dioxide sol and sodium sulfite are added. Then, it is prepared by dispersing and grinding, and the low temperature finishing temperature is 0-5°C.

The preparation steps of the modified polyester are as follows: S1: take deionized water, carbon nanotubes and tetrabutyl titanate respectively, stir and mix them and place them in a three-necked flask, program the temperature for heating and keep the temperature for reaction to obtain a modified slurry; S2: then Take the catalyst, ethylene glycol, modified slurry and purified terephthalic acid respectively and put them in the reaction kettle, stir and mix and pass nitrogen to remove air, and then under nitrogen atmosphere, vacuumize and then pass nitrogen to pressurize, and pump after heat preservation reaction. Vacuum treatment, thermal insulation polycondensation, standing and cooling to room temperature to obtain modified polyester particles.

The specific preparation steps of a preparation method of an anti-pilling elastic fiber material are as follows: (1) respectively taking ethanol solution, calcium chloride and degummed silk and placing them in a conical flask, stirring and mixing and collecting a mixed solution; Put it in a dialysis bag, collect the dialysis modification solution through dialysis treatment, add tetrabutyl titanate to the acetic acid solution, stir and mix to obtain a nanosol solution, and then take the nanosol solution, the dialysis modification solution and the sodium sulfite solution respectively and place them in the solution. In a mortar, grind and disperse and collect the dispersing slurry, process the dispersing slurry through a screen, collect the mixed slurry, and let it stand for aging to obtain a sol-modified liquid; (2) take deionized water, carbon nanotubes, and Butyl ester, stirred and mixed and placed in a three-necked flask, heated with a programmed temperature and heat preservation reaction, to obtain a modified slurry, and then separately took the catalyst, ethylene glycol, modified slurry, and purified terephthalic acid and placed them in the reaction kettle, and stirred and mixed. And pass nitrogen to remove air, then in nitrogen atmosphere, vacuumize and then pressurize with nitrogen, vacuumize after heat preservation reaction, heat preservation polycondensation, stand and cool to room temperature to obtain modified polyester particles; through low temperature and long time drying, The moisture content of the slices is lower, which is beneficial to the temperature control of the spinning process; (3) the modified polyester particles are dried at low temperature, and the dried modified polyester particles are collected, and the dried modified polyester particles are sliced and placed in the spinning process. In the device, adjusting the spinning temperature, pulling and stretching, collecting the spinning fibers, finishing the spinning fibers with a sol-modified liquid at a low temperature, drying them to a constant weight, and letting them stand to cool to room temperature to prepare the said spinning fibers. For the anti-pilling elastic fiber material, the low temperature finishing temperature is 0-5°C. The polyester fiber is rapidly cooled, the molten melt will be rapidly cooled, the internal microcrystalline structure will be changed, the strength of a single fiber will be increased, the strength of the resulting fiber web will also be increased, and other qualities will also be increased. There are corresponding improvements, so that the prepared polyester fiber has good stability, good elasticity and excellent mechanical properties.

The catalyst is ethylene glycol titanium.

In the vacuum treatment, the thermal insulation polycondensation is carried out at 220-250° C. for 25-30 minutes, vacuuming to 40-50 Pa, and thermal insulation polycondensation for 2-3 hours.

The traction ratio of the traction stretching treatment is 3.2 to 3.5; the stretching ratio is optimized and the stretching rate is improved. In the process of improving the traction, the orientation time of the macromolecules under the action of the stretching tension is shortened, and it is too late to fully orientate, resulting in a decrease in the strength of the thread. , the phenomenon of elongation and growth, and then the spinning fiber is treated by high-speed air cooling to cool down the polyester fiber rapidly, reducing the de-stretching, de-orientation and de-crystallization movement of macromolecules in the solution that occur in the traditional mesh curtain under high temperature and no tension. , so that the prepared polyester fiber has good stability, good elasticity and excellent mechanical properties.

The spinning temperature is 280-285°C; the spinning temperature is optimized to make the spinning fiber structure excellent.

Compared with the prior art, the beneficial effects of the present invention are: (1) The technical solution of the present invention adopts nano-gel material to cooperate with the fibroin dialysate, and due to the good film-forming property of fibroin on the fiber surface, the membrane is repaired; Destroys the polyester fiber surface of the scale layer, making the fiber surface smoother, and the coefficient of friction in the forward and reverse directions is significantly reduced, which greatly reduces the directional friction effect on the fiber surface, and improves the pilling performance of clothing fiber materials. The function of the material is to form crystalline TiO ₂ at a lower temperature through the spontaneous crystallization of inorganic products, so the present invention uses nano-titania gel as the matrix gel material, and the surface of the fiber material contains C=O, - OC=O, -COH, -COOH, CH2-OH groups are combined, and the groups and the titanium dioxide finishing solution have a chemical reaction in the active group, thereby effectively improving the bonding fastness of the fiber and the finishing agent, and effectively improving the finishing agent material and fiber. The bonding strength between the two, and then repair the polyester fiber material through fibroin to reduce the directional friction effect of the polyester fiber during use, so that it can further improve the directional friction effect of the polyester fiber during use. Protein is a finishing agent material, which further improves the anti-pilling performance of the material by forming a film;

(2) In the technical scheme of the present invention, by adding carbon nanotube material, in the preparation process of the polyurethane material, since carbon nanotubes have greater rigidity, the introduction of carbon nanotubes into the polyester molecular chain can improve the rigidity of the molecular chain and reduce the matrix. The free volume of the polyester is reduced, thereby reducing the gap between the molecular chains, blocking the penetration of small molecules, improving the structural strength and mechanical properties of the polyester material, and then the molten high-viscosity polyester particles prepared by polycondensation are used as polyester elastic yarn products. Low cost, can improve the elasticity and feel of polyester fabrics, the product is resistant to chlorine bleaching, and has excellent chemical stability;

(3) Through low-temperature sol coating, the structure and anti-pilling properties of the material are first improved, and at the same time, the polyester fiber is rapidly cooled, so that the molten melt will be rapidly cooled, the internal microcrystalline structure will be changed, and the strength of a single fiber will be With the increase, the strength of the obtained fiber web will also increase, and other qualities will also be improved accordingly, so that the prepared polyester fiber has good stability, good elasticity and excellent mechanical properties.

Detailed ways

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. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

In parts by weight, weigh 25 to 30 parts by mass of 15% ethanol solution, 3 to 5 parts of calcium chloride and 3 to 5 parts of degummed silk and place them in a conical flask, stir and mix and collect the mixed solution, The mixed solution was placed in a dialysis bag, respectively placed in a dialysis bag with a molecular weight of 3500, 7000 and 14000 for dialysis treatment, and the dialysis modified liquid was collected; at a mass ratio of 1:20, tetrabutyl titanate was added to the mass parts 50% acetic acid solution, stir and mix to obtain nano sol solution, in parts by weight, weigh 45-50 parts of nano-sol solution, 25-30 parts of dialysis modified solution and 6-8 parts of 5% sodium sulfite solution by mass respectively Put it in a mortar, grind and disperse and collect the dispersing slurry, pass the dispersing slurry through a 0.25-0.28 μm screen, filter and collect the mixed slurry, and let it stand for 6-8 hours to obtain a modified sol solution; by weight In total, weigh 45-50 parts of deionized water, 6-8 parts of carbon nanotubes, and 10-15 parts of tetrabutyl titanate respectively, stir and mix and place them in a three-necked flask, and heat up to 150- 160 ° C, heat preservation reaction for 3 to 5 hours, to obtain modified slurry; in parts by weight, weigh 1 to 2 parts of catalyst, 10 to 20 parts of ethylene glycol, 6 to 8 parts of modified slurry, and 35 to 40 parts of refined The terephthalic acid was placed in the reaction kettle, stirred and mixed, and the air was removed by passing nitrogen gas, and the nitrogen feeding rate was controlled to be 45-50 mL/min. min, pass nitrogen into the reaction kettle, pass nitrogen to pressurize to 2～3kPa, then heat the reaction at 220～250℃ for 25～30min, evacuate to 40～50Pa, heat preservation and polycondensation for 2～3h, stand and cool to room temperature , to obtain modified polyester particles; after the modified polyester particles are kept at 100-110 ℃ for 6-8 hours, the dried modified polyester particles are collected, and the dried modified polyester particles are sliced and placed in a spinning In the spinning device, the spinning temperature of the spinning device is controlled to be 280-285 ℃, and the drawing and drawing ratio is 3.2-3.5 for drawing and drawing and collecting the spinning fibers. The anti-pilling elastic fiber material can be prepared by cooling in the sol-modified liquid for 3-5 s at ℃, drying to constant weight at 100-110 ℃, and cooling to room temperature.

Example 1

In parts by weight, 25 parts by mass of 15% ethanol solution, 3 parts of calcium chloride and 3 parts of degummed silk were weighed and placed in a conical flask, stirred and collected to obtain a mixed solution, and the mixed solution was placed in a conical flask. The dialysis bags were placed in the dialysis bags with molecular weights of 3500, 7000 and 14000 in turn for dialysis treatment, and the dialysis modified liquid was collected; at a mass ratio of 1:20, tetrabutyl titanate was added to a 50% acetic acid solution in parts by mass. , stir and mix to obtain the nano-sol liquid, in parts by weight, weigh 45 parts of the nano-sol liquid, 25 parts of the dialysis modified liquid and 6 parts of the 5% sodium sulfite solution by mass and place them in a mortar, grind and disperse and collect the dispersed slurry , pass the dispersing slurry through a 0.25 μm screen, filter and collect the mixed slurry, and let it stand for 6 hours to obtain a modified sol solution; in parts by weight, weigh 45 parts of deionized water and 6 parts of carbon nanotubes respectively. , 10 parts of tetrabutyl titanate, stirred and mixed, placed in a three-necked flask, heated to 150 °C at a temperature of 5 °C/min, and kept for reaction for 3 h to obtain a modified slurry; in parts by weight, weigh 1 part of the catalyst respectively. , 10 parts of ethylene glycol, 6 parts of modified slurry, and 35 parts of purified terephthalic acid were placed in the reaction kettle, stirred and mixed and passed nitrogen to remove air. Evacuate to 450Pa, then press 45mL/min, pass nitrogen into the reaction kettle, pass nitrogen and pressurize to 2kPa, then heat the reaction at 220 ° C for 25min, evacuate to 40Pa, heat preservation and polycondensation for 2 ~ 3h, stand to cool to room temperature to obtain modified polyester particles; after the modified polyester particles were kept at 100 °C for 6 hours, the dried modified polyester particles were collected, and the dried modified polyester particles were sliced and placed in a spinning device In the process, the spinning temperature of the spinning device was controlled to be 280°C, and the spun fibers were collected by drawing and drawing at a draw ratio of 3.2, and the spinning fibers were cooled in a sol-modified solution at 0°C at a rate of 10 m/s. After treatment for 3 s, drying at 100° C. to constant weight, and cooling to room temperature, the anti-pilling elastic fiber material can be prepared.

Example 2

In parts by weight, 27 parts by mass of 15% ethanol solution, 4 parts of calcium chloride and 4 parts of degummed silk were weighed and placed in a conical flask, stirred and mixed to collect a mixed solution, and the mixed solution was placed in a conical flask. The dialysis bags were placed in the dialysis bags with molecular weights of 3500, 7000 and 14000 in turn for dialysis treatment, and the dialysis modified liquid was collected; at a mass ratio of 1:20, tetrabutyl titanate was added to a 50% acetic acid solution in parts by mass. , stir and mix to obtain nano-sol liquid, in parts by weight, weigh 47 parts of nano-sol liquid, 27 parts of dialysis modified liquid and 7 parts of 5% sodium sulfite solution by mass and place them in a mortar, grind and disperse and collect the dispersed slurry , pass the dispersed slurry through a 0.27 μm screen, filter and collect the mixed slurry, let it stand for 7 hours to obtain a sol modified liquid; in parts by weight, weigh 47 parts of deionized water and 7 parts of carbon nanotubes respectively. , 12 parts of tetrabutyl titanate, stirred and mixed and placed in a three-necked flask, heated to 155°C at a temperature of 5°C/min, kept for 4h and reacted to obtain a modified slurry; in parts by weight, weigh 1 part of catalyst respectively , 15 parts of ethylene glycol, 7 parts of modified slurry, and 37 parts of purified terephthalic acid were placed in the reaction kettle, stirred and mixed and passed nitrogen to remove air, and the nitrogen feeding rate was controlled to be 47 mL/min, and then under nitrogen atmosphere, Evacuate to 475Pa, then press 47mL/min, pass nitrogen into the reaction kettle, pass nitrogen and pressurize to 2kPa, then heat the reaction at 235°C for 27min, evacuate to 42Pa, heat preservation and polycondensation for 2h, stand and cool to room temperature , to obtain modified polyester particles; after the modified polyester particles were kept at 105 °C for 7 hours, the dried modified polyester particles were collected, and the dried modified polyester particles were sliced and placed in a spinning device, The spinning temperature of the spinning device was controlled to be 282°C, and the spun fibers were collected by drawing and drawing at a draw ratio of 3.4. The spinning fibers were cooled in a sol-modified solution at 3°C for 4s at a rate of 10 m/s. After that, it is dried to constant weight at 105° C., and cooled to room temperature by standing to prepare the anti-pilling elastic fiber material.

Example 3

In parts by weight, 30 parts by mass of 15% ethanol solution, 5 parts of calcium chloride and 5 parts of degummed silk were weighed and placed in a conical flask, stirred and mixed to collect a mixed solution, and the mixed solution was placed in a conical flask. The dialysis bags were placed in the dialysis bags with molecular weights of 3500, 7000 and 14000 in turn for dialysis treatment, and the dialysis modified liquid was collected; at a mass ratio of 1:20, tetrabutyl titanate was added to a 50% acetic acid solution in parts by mass. , stir and mix to obtain the nano-sol liquid, in parts by weight, weigh 50 parts of the nano-sol liquid, 30 parts of the dialysis modified liquid and 8 parts of the 5% sodium sulfite solution in a mortar, grind and disperse and collect the dispersed slurry , pass the dispersed slurry through a 0.28 μm screen, filter and collect the mixed slurry, let it stand for 8 hours, and obtain a sol modified liquid; in parts by weight, weigh 50 parts of deionized water and 8 parts of carbon nanotubes respectively. , 15 parts of tetrabutyl titanate, stirred and mixed and placed in a three-necked flask, heated to 160 °C at a temperature of 5 °C/min, and incubated for 5 h to obtain a modified slurry; in parts by weight, weigh 2 parts of the catalyst respectively. , 20 parts of ethylene glycol, 8 parts of modified slurry, and 40 parts of purified terephthalic acid were placed in the reaction kettle, stirred and mixed and passed nitrogen to remove air, and the nitrogen feeding rate was controlled to be 50mL/min, and then under nitrogen atmosphere, Evacuate to 500Pa, then press 50mL/min, pass nitrogen into the reaction kettle, pass nitrogen and pressurize to 3kPa, then keep the reaction at 250℃ for 30min, evacuate to 50Pa, heat preservation and polycondensation for 3h, stand and cool to room temperature , to obtain modified polyester particles; after the modified polyester particles were kept at 110 °C for 8 hours, the dried modified polyester particles were collected, and the dried modified polyester particles were sliced and placed in a spinning device, The spinning temperature of the spinning device was controlled to be 285 °C, and the spun fibers were collected by pulling and drawing at a draw ratio of 3.5. The spinning fibers were cooled in a sol-modified solution at 5 °C for 5 s at a rate of 10 m/s. Then, it is dried at 110° C. to constant weight, and cooled to room temperature by standing to prepare the anti-pilling elastic fiber material.

Example 4

In parts by weight, 27 parts by mass of 15% ethanol solution, 4 parts of calcium chloride and 4 parts of degummed silk were weighed and placed in a conical flask, stirred and mixed to collect a mixed solution, and the mixed solution was placed in a conical flask. The dialysis bags were placed in the dialysis bags with molecular weights of 3500, 7000 and 14000 in turn for dialysis treatment, and the dialysis modified liquid was collected; at a mass ratio of 1:20, tetrabutyl titanate was added to a 50% acetic acid solution in parts by mass. , stir and mix to obtain nano-sol liquid, in parts by weight, weigh 47 parts of nano-sol liquid, 27 parts of dialysis modified liquid and 7 parts of 5% sodium sulfite solution by mass and place them in a mortar, grind and disperse and collect the dispersed slurry , pass the dispersing slurry through a 0.27 μm screen, filter and collect the mixed slurry, let it stand for 7 hours, and obtain a sol modified liquid; in parts by weight, weigh 1 part of catalyst, 12 parts of ethylene glycol, 37 parts of ethylene glycol Parts of purified terephthalic acid were placed in the reactor, stirred and mixed, and the air was purged with nitrogen, and the nitrogen feeding rate was controlled to be 47 mL/min. Put it into the reaction kettle, pressurize it with nitrogen to 2kPa, then keep the reaction at 235℃ for 27min, evacuate to 45Pa, heat preservation and polycondensation for 2h, stand and cool to room temperature to obtain modified polyester particles; After being kept at 105 °C for 7 hours, the dry modified polyester particles were collected, and the dried modified polyester particles were sliced and placed in a spinning device, and the spinning temperature of the spinning device was controlled to be 282 °C. At a draw ratio of 3.4, the spun fibers were collected by pulling and stretching. The spun fibers were cooled in a sol-modified solution at 3 °C for 4 s at a rate of 10 m/s, and then dried to constant weight at 100-110 °C. The anti-pilling elastic fiber material can be prepared by standing and cooling to room temperature.

Example 5

In parts by weight, weigh 1 part of catalyst, 12 parts of ethylene glycol, and 37 parts of purified terephthalic acid, respectively, and place them in the reaction kettle, stir and mix and pass nitrogen to remove air, and control the feeding rate of nitrogen to be 47 mL/min, Under a nitrogen atmosphere, vacuumize to 475Pa, then press 47mL/min, pass nitrogen into the reaction kettle, pass nitrogen and pressurize to 2kPa, then heat the reaction at 235 ° C for 27min, vacuum to 45Pa, heat preservation polycondensation for 2h , cooled to room temperature, and the modified polyester particles were obtained; after the modified polyester particles were kept at 105 °C for 7 hours, the dried modified polyester particles were collected, and the dried modified polyester particles were sliced and placed on the In the spinning device, the spinning temperature of the spinning device is controlled to be 282°C, and the spun fibers are collected by drawing and drawing at a draw ratio of 3.4, and then dried to a constant weight at 100-110°C, and left to cool. When the temperature reaches room temperature, the anti-pilling elastic fiber material can be prepared.

It will be apparent to those skilled in the art that the present invention is not limited to the details of the above-described exemplary embodiments, but that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments are to be regarded in all respects as illustrative and not restrictive, and the scope of the invention is to be defined by the appended claims rather than the foregoing description, which are therefore intended to fall within the scope of the claims. All changes within the meaning and scope of the equivalents of , are included in the present invention. Any signs in the claims should not be construed as limiting the involved claim.

The performance tests were carried out on Example 1, Example 2, Example 3, Example 4 and Example 5. The Example 4 is a composite polyester fiber prepared without adding carbon nanotubes, and Example 5 is a composite polyester fiber without the use of low temperature. Finishing the polyester fiber prepared by the technical scheme, and specifically testing its mechanical strength:

Mechanical property test: YG061 electronic yarn tenacity tester. The setting of parameters refers to the standard of GB/T14344-2003 "Test method for tensile properties of synthetic fiber filaments". The test was carried out under constant temperature and humidity conditions, the temperature was (20.0±2.0)°C, and the relative humidity was (65±2)%.

The specific test results are shown in Table 1.

Table 1 Performance comparison table

(1) Comparing Example 1, Example 2, Example 3, Example 4 and Example 5 of the present invention, the breaking strength and breaking productivity of Example 5 are far smaller than those of Example 1, Example 2 and Example 5 3. Explain that in the technical solution of the present invention, the low-temperature sol coating is used to improve the structural anti-pilling performance of the material, and at the same time, the polyester fiber is rapidly cooled, so that the molten melt will be rapidly cooled, and the internal microcrystalline structure will be changed. The strength of the fibers will increase, the strength of the resulting fiber web will also increase, and other qualities will also be improved accordingly, so that the prepared polyester fibers have good stability, good elasticity and excellent mechanical properties.

(2) Comparing Example 1, Example 2, Example 3, Example 4 and Example 5 of the present invention, the elongation at break and the breaking strength in Example 4 are significantly decreased, which is due to the addition of carbon nanometers. The tube material makes the polyurethane material in the preparation process, due to the large rigidity of carbon nanotubes, the introduction of carbon nanotubes into the polyester molecular chain can improve the rigidity of the molecular chain and reduce the free volume of the matrix, thereby reducing the gap between the molecular chains. To block the penetration of small molecules and improve the structural strength and mechanical properties of polyester materials, the molten high-viscosity polyester particles prepared by polycondensation are used as polyester elastic yarn products. The production cost is low, and it can improve the elasticity and feel of polyester fabrics. Chlorine bleach, excellent chemical stability.

(3) By observing the directional friction coefficient of Example 5 and other examples, the friction coefficient of Example 5 was significantly increased, indicating that the nanogel material was used to cooperate with the fibroin dialysate, thereby reducing the use process of polyester fibers. The directional friction effect existing in the polyester fiber makes it possible to further improve the directional friction effect of polyester fibers during use. The technical scheme of further improving the anti-pilling performance of the material by forming a film by using silk fibroin as the finishing agent material is established.

Claims (7)

1. The anti-pilling elastic fiber material is characterized by being prepared by stretching a modified polyester spinning material and then carrying out low-temperature finishing by using a finishing agent, wherein the modified polyester is prepared by taking purified terephthalic acid and ethylene glycol as raw materials, adding deionized water, carbon nano tubes, tetrabutyl titanate and a catalyst and carrying out vacuum polycondensation, the finishing agent is prepared by dissolving ethanol, calcium chloride and degummed silk and then carrying out dialysis treatment, adding nano titanium dioxide sol and sodium sulfite and then dispersing and grinding, and the low-temperature finishing temperature is 0-5 ℃.

2. The anti-pilling spandex material of claim 1, wherein the modified polyester is prepared by the steps of:

s1: respectively taking deionized water, carbon nano tubes and tetrabutyl titanate, stirring and mixing, placing in a three-neck flask, heating by a programmed temperature and reacting while keeping the temperature to obtain modified slurry;

s2: and respectively putting the catalyst, ethylene glycol, the modified slurry and the purified terephthalic acid into a reaction kettle, stirring and mixing, introducing nitrogen to remove air, vacuumizing and pressurizing by introducing nitrogen again in the nitrogen atmosphere, carrying out heat preservation reaction and vacuumizing treatment, carrying out heat preservation polycondensation, standing and cooling to room temperature to obtain the modified polyester particles.

3. The preparation method of the anti-pilling elastic fiber material is characterized by comprising the following specific preparation steps:

(1) respectively placing ethanol solution, calcium chloride and degummed silk into a triangular flask, stirring, mixing and collecting to obtain mixed dissolved solution, placing the mixed dissolved solution into a dialysis bag, performing dialysis treatment to obtain dialysis modified solution, adding tetrabutyl titanate into acetic acid solution, stirring and mixing to obtain nano sol solution, then respectively placing the nano sol solution, the dialysis modified solution and sodium sulfite solution into a mortar, grinding, dispersing and collecting dispersed slurry, passing the dispersed slurry through a screen, collecting the mixed slurry, standing and aging to obtain sol modified solution;

(2) respectively taking deionized water, carbon nano tubes and tetrabutyl titanate, stirring, mixing, placing in a three-neck flask, heating by temperature programming, carrying out heat preservation reaction to obtain modified slurry, then respectively taking a catalyst, ethylene glycol, the modified slurry and purified terephthalic acid, placing in a reaction kettle, stirring, mixing, introducing nitrogen to remove air, vacuumizing and then pressurizing by nitrogen under the atmosphere of nitrogen, carrying out heat preservation reaction, carrying out vacuum treatment, carrying out heat preservation polycondensation, standing and cooling to room temperature to obtain modified polyester particles;

(3) drying the modified polyester particles at low temperature, collecting the dried modified polyester particles, slicing the dried modified polyester particles, placing the slices in a spinning device, adjusting the spinning temperature, carrying out traction and stretching treatment, collecting spinning fibers, carrying out low-temperature finishing on the spinning fibers by using a sol modification solution, drying the spinning fibers to constant weight, standing and cooling the spinning fibers to room temperature to obtain the anti-pilling elastic fiber material, wherein the low-temperature finishing temperature is 0-5 ℃.

4. The anti-pilling spandex material of claim 1 or claim 2, wherein the catalyst is titanium glycol.

5. The preparation method of the anti-pilling spandex material as claimed in claim 3, wherein the vacuum treatment and the thermal polycondensation in the step (2) are carried out for 25-30 min at 220-250 ℃, and the vacuum treatment and the thermal polycondensation are carried out for 2-3 h under the condition of vacuum pumping to 40-50 Pa.

6. The preparation method of the anti-pilling spandex material as claimed in claim 3, wherein the draw ratio of the drawing and stretching treatment in the step (3) is 3.2-3.5.

7. The method for preparing the anti-pilling spandex material as claimed in claim 3, wherein the spinning temperature in the step (3) is 280-285 ℃.