Preparation method of polyester filament with deodorizing function

Abstract

The present invention relates to a preparation method of polyester filaments with a deodorizing function. A solvent-free two-component deodorizing finishing agent is placed in an oil bath tank and kept at 40 - 50 °C to make the viscosity 200 - 400 mPa·s. After passing through the spinning process of melting polyester raw materials - metering - spinning - cooling - passing through the oil bath tank - stretching - heat curing - winding and forming, the product is obtained. The solvent-free two-component deodorizing finishing agent is obtained by uniformly mixing component A and component B at room temperature. Component A is a deodorizing modifier and a bio-based macromolecular polyol after vacuum dehydration, and component B is a curing agent and a catalyst. The synthesis method of the deodorizing modifier is as follows: by mass, 90 - 95 parts of epoxy-modified montmorillonite, 5 - 10 parts of zinc ricinoleate and 200 parts of ethanol are mixed, and the pH value of the system is adjusted to 3 - 4, and the reaction is carried out at 40 - 50 °C to obtain the deodorizing modifier. The present invention endows the polyester filaments with efficient and long-lasting deodorizing functions.

Description

Technical Field

[0001] The present invention belongs to the technical field of functional fibers and relates to a method for preparing polyester filaments with a deodorizing function. Background Art

[0002] Polyester fabrics have been widely used in the fields of clothing, home fabrics, etc. in recent years due to their excellent properties such as firmness, durability, wrinkle resistance, non-ironing, elasticity, and good chemical resistance. With the continuous expansion of the application fields of polyester fabrics and the continuous improvement of consumers' living quality, polyester products with excellent deodorizing functions have begun to be favored by people. Odors are usually caused by nitrogen- and sulfur-containing molecules, namely amines, ammonia, mercaptans, thioesters, hydrogen sulfide, low-molecular-weight organic acids, etc.

[0003] Chinese Patent CN102182062 discloses a moisture-absorbing and deodorizing polyester knitted fabric, which includes a base fabric made of polyester, and a zeolite powder layer is printed on the surface of the base fabric; the composition and weight ratio of the zeolite powder layer are: 47-50% acrylic composite resin, 28-30% 5-50μm synthetic zeolite powder, 20-24% ethyl acetate, and 0.5% leveling agent. The moisture-absorbing and deodorizing polyester knitted fabric of this patent prints the zeolite layer on polyester with a light fastness greater than 6 and a color fastness to high-temperature washing at 60°C greater than 4 through screen printing technology. It not only retains the original advantages of polyester such as high light fastness and high-temperature washing color fastness, but also can absorb moisture and deodorize; it also has the advantages of simple process, etc. However, the above method imparts deodorizing properties by physically mixing zeolite, and the large introduction of physical fillers easily affects the hand feeling of the fabric.

[0004] In contrast, using zinc ricinoleate as a deodorizing material is more superior. Zinc ricinoleate contains active zinc atoms, and the zinc atoms can form very strong chemical bonds with nitrogen and sulfur atoms in the odor, thus completely eliminating the odor, and it has no effect on fragrance components such as esters, aldehydes or aromatics. In addition, zinc ricinoleate is safe and environmentally friendly and can be widely used in clothing, homes, and other relatively crowded enclosed places.

[0005] Patent CN201610653393.5 discloses an antibacterial and deodorant spray for textiles, which includes the following components: α-ethynyl ketone, isopropyl myristate, tributyl acetylcitrate, tridecanoic acid, grapefruit seed extract, sodium bicarbonate, polyglyceryl-3-caprate, sucrose cocoate, zinc ricinoleate, dodecyl methacrylate, isothiazolinone, water-soluble plant essence, Tween 80, propylene glycol, vegetable glycerin, deionized water; it is non-toxic, colorless, non-irritating, non-corrosive, has good stability, is safe and reliable, has broad-spectrum antibacterial and high-efficiency deodorant functions, is easy to use, and especially has remarkable deodorant and antibacterial effects after being used on special uniforms, such as the uniforms of sanitation workers, medical staff, and corpse handlers. However, this patent is a physical adsorption of the spray, which requires repeated use and does not have persistence.

[0006] Therefore, it is of great significance to study a preparation method of polyester filaments with deodorant function to solve the problems existing in the prior art. Summary of the Invention

[0007] The purpose of the present invention is to solve the problems existing in the prior art and provide a preparation method of polyester filaments with deodorant function.

[0008] To achieve the above purpose, the technical scheme adopted by the present invention is as follows:

[0009] A preparation method of polyester filaments with deodorant function, put the solvent-free two-component deodorant finishing agent in an oil bath tank, keep it at 40~50°C to make the viscosity 200~400 mPa·s (the solvent-free two-component finishing agent usually has a relatively high viscosity, and it needs to be kept warm during use to ensure the fluidity of the finishing agent), and then obtain the polyester filaments with deodorant function through the spinning process of molten polyester raw material - metering - spinning - cooling - passing through the oil bath tank - stretching - heat curing - winding and forming; although the stretching process also heats, due to the relatively fast stretching speed, only a small part of the solvent-free two-component deodorant finishing agent on the fiber will be cured after stretching, and the curing is incomplete, so further heat curing is required;

[0010] The solvent-free two-component deodorant finishing agent is obtained by mixing component A and component B evenly at room temperature;

[0011] Component A is a deodorant modifier and a bio-based macromolecular polyol after vacuum dehydration, and component B is a curing agent and a catalyst;

[0012] By mass, the dosage of each material in the solvent-free two-component deodorant finishing agent is: 2~5 parts of deodorant modifier, 55~70 parts of bio-based macromolecular polyol after vacuum dehydration, 3~5 parts of curing agent, and 0.1~0.3 parts of catalyst;

[0013] The synthesis method of the deodorant modifier is as follows: by mass parts, 90-95 parts of epoxy-modified montmorillonite, 5-10 parts of zinc ricinoleate and 200 parts of ethanol are mixed, and the pH value of the system is adjusted to 3-4, so that the molar ratio of hydroxyl groups to epoxy groups ranges from 1.5-2:0.75-1, and the reaction is carried out at 40-50 °C to obtain the deodorant modifier;

[0014] The synthesis method of epoxy-modified montmorillonite is: a silane coupling agent containing epoxy groups is mixed with montmorillonite, and hydrolysis and condensation reaction are carried out under acidic conditions to obtain epoxy-modified montmorillonite.

[0015] As a preferred technical solution:

[0016] For the preparation method of a polyester filament with deodorant function as described above, after passing through the oil bath tank, there is also an oiling process, and stretching is carried out after oiling.

[0017] For the preparation method of a polyester filament with deodorant function as described above, the content of the solvent-free two-component deodorant finishing agent after the cooled tow passes through the oil bath tank is 0.8-1.2 wt%.

[0018] For the preparation method of a polyester filament with deodorant function as described above, the spinning process parameters are: spinning temperature (i.e., the temperature of the molten polyester raw material) 300-320 °C, cooling air blowing temperature 18-28 °C, cooling air blowing speed 0.3-0.6 m / s, stretching temperature 130-160 °C, stretching ratio 4-6 times, heat curing temperature 90-110 °C, heat curing time 2-3 s.

[0019] For the preparation method of a polyester filament with deodorant function as described above, the bio-based macromolecular polyol is polytrimethylene ether glycol or succinic acid-based polymer polyol, and the number average molecular weight of the bio-based macromolecular polyol is 1000-3000.

[0020] For the preparation method of a polyester filament with deodorant function as described above, the curing agent is one or more of hexamethylene diisocyanate trimer and isophorone diisocyanate trimer.

[0021] For the preparation method of a polyester filament with deodorant function as described above, the catalyst is bismuth neodecanoate or bismuth isooctanoate.

[0022] A preparation method of a polyester filament with a deodorizing function as described above. The specific synthesis process of the epoxy-modified montmorillonite is as follows: By mass, first add 90 parts of ethanol and 10 parts of water into a reaction flask, add 1 - 2 parts of formic acid to adjust the pH value of the solution to 2 - 3, then add 5 parts of a silane coupling agent containing epoxy groups, hydrolyze for 2 - 3 h, and finally add 10 - 20 parts of montmorillonite to the hydrolyzed system, reflux and react at a temperature of 50 - 60 °C for 10 - 12 h. The product is successively washed with ethanol 3 - 5 times, filtered, and dried to obtain the epoxy-modified montmorillonite.

[0023] A preparation method of a polyester filament with a deodorizing function as described above. The silane coupling agent containing epoxy groups is γ-(2,3-epoxypropoxy)propyltrimethoxysilane.

[0024] A preparation method of a polyester filament with a deodorizing function as described above. The deodorization rate of the polyester filament with a deodorizing function is above 85%. After being washed according to GB / T 8629 - 2017, the deodorization rate is still higher than 80%.

[0025] Principle of the invention:

[0026] In the present invention, zinc ricinoleate is covalently intercalated into montmorillonite with a high specific surface area and introduced into a solvent-free two-component polyurethane coating system. The solvent-free two-component deodorizing finishing agent with a deodorizing function is uniformly coated and cured to wrap on the surface of the polyester filament, which can endow the polyester fabric with an efficient deodorizing function from the source of the fabric, that is, at the "fiber" level; the high specific surface area after the intercalation modification of montmorillonite and the zinc ricinoleate grafted thereon synergistically endow the polyester filament with efficient and long-lasting deodorizing functions. Specifically, on the one hand, the present invention retains the negative and positive charges on the montmorillonite and its high adsorption efficiency; at the same time, using the reactivity of the hydroxyl groups on the montmorillonite, a coupling agent is grafted as a bridge, and then zinc ricinoleate with a deodorizing function is grafted. At the same time, one hydroxyl group on the ricinoleic acid is retained, so that such a large deodorizing molecule can be covalently bound to the coating, improving the deodorization stability and long-term performance.

[0027] Beneficial effects:

[0028] (1) In the preparation method of a polyester filament with a deodorizing function of the present invention, zinc ricinoleate is covalently intercalated into montmorillonite with a high specific surface area and introduced into a solvent-free two-component deodorizing finishing agent system. The polyurethane coating with a deodorizing function is uniformly coated and cured to wrap on the surface of the polyester filament, which can endow the polyester fabric with an efficient deodorizing function from the source of the fabric, that is, at the "fiber" level; the high specific surface area after the intercalation modification of montmorillonite and the zinc ricinoleate grafted thereon synergistically endow the polyester filament with efficient and long-lasting deodorizing functions;

[0029] (2) The preparation method of a polyester filament with deodorizing function according to the present invention selects zinc ricinoleate as the deodorizing modification component, which is safe and non-toxic; selects a solvent-free two-component deodorizing finishing agent as the finishing agent coating matrix, which is green and sustainable. The obtained polyester filament with deodorizing function is an environmental protection product, meeting the requirements of the sustainable development of the industry.

[0030] (3) The preparation method of a polyester filament with deodorizing function according to the present invention selects the organic chemical molecule zinc ricinoleate as the deodorizing modifier, which does not simply adsorb odors, but can completely eliminate odor molecules; effectively solves the problems of simple adsorption of physical deodorizing materials, incomplete deodorization, and affecting the hand feeling of fabrics. Specific embodiments

[0031] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and not to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of this application.

[0032] The test methods related to the performance indicators of the present invention are as follows:

[0033] Deodorization rate: Experiments are carried out in accordance with the standard of QB / T2761-2006.

[0034] The source of montmorillonite in the present invention: Manufacturer: Zhejiang Huate New Materials Co., Ltd., Brand: DK32B; Succinic acid-based polymer polyol is from BioAmber, Brand: SA-PEP.

[0035] Example 1

[0036] The preparation method of a polyester filament with deodorizing function is as follows:

[0037] (1) By mass, first add 90 parts of ethanol and 10 parts of water into a reaction flask, add 1 part of formic acid to adjust the pH value of the solution to 2, then add 5 parts of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, hydrolyze for 2 h, and finally add 10 parts of montmorillonite to the hydrolyzed system, reflux and react at 50 °C for 10 h. The product is washed with ethanol 3 times, filtered and dried in sequence to obtain epoxy-modified montmorillonite.

[0038] (2) By mass, mix 90 parts of epoxy-modified montmorillonite, 5 parts of zinc ricinoleate and 200 parts of ethanol, add phosphoric acid to adjust the pH value of the system to 3, and react at 40 °C for 4 h to obtain a deodorizing modifier.

[0039] (3) By mass parts, 2 parts of deodorant modifier, 55 parts of polytrimethylene ether glycol after vacuum dehydration (number average molecular weight is 1000), 3 parts of hexamethylene diisocyanate trimer and 0.1 part of bismuth neodecanoate are mixed evenly at room temperature to obtain a solvent-free two-component deodorant finishing agent;

[0040] (4) The solvent-free two-component deodorant finishing agent is placed in an oil bath tank and kept at 40 °C to make the viscosity 200 mPa·s. After the spinning process of molten polyester raw material - metering - spinning - cooling - passing through the oil bath tank - oiling - stretching - thermal curing - winding and forming, polyester filaments with deodorant function are obtained;

[0041] The spinning process parameters are: spinning temperature 300 °C, cooling air blowing temperature 18 °C, cooling air blowing speed 0.3 m / s, stretching temperature 130 °C, stretching ratio 4 times, thermal curing temperature 90 °C, thermal curing time 2 s;

[0042] Among them, the content of the solvent-free two-component deodorant finishing agent after the cooled filament bundle passes through the oil bath tank is 0.8 wt%.

[0043] The deodorization rate of the finally obtained polyester filaments with deodorant function is 85%. After washing according to GB / T 8629-2017, the deodorization rate is 81%.

[0044] Comparative Example 1

[0045] A method for preparing polyester filaments is basically the same as that in Example 1, except that: the operation in step (1) is omitted, and the epoxy-modified montmorillonite in step (2) is replaced by montmorillonite.

[0046] The deodorization rate of the obtained polyester filaments is 38%. After washing according to GB / T 8629-2017, the deodorization rate is 32%.

[0047] Comparing Comparative Example 1 with Example 1, it can be found that the deodorization rate drops significantly. This is because without intercalation modification by silane coupling agent, it is impossible to fully exfoliate the montmorillonite, and it is difficult to exert the capture and adsorption effect of the high specific surface area lamellae on the odor.

[0048] Comparative Example 2

[0049] A method for preparing polyester filaments is basically the same as that in Example 1, except that: the mass parts of the epoxy-modified montmorillonite in step (2) is 88 parts.

[0050] The deodorization rate of the obtained polyester filaments is 82%. After washing according to GB / T 8629-2017, the deodorization rate is 80%.

[0051] Comparing Comparative Example 2 with Example 1, it can be found that the deodorization rate decreased slightly. This is because in step (2), after reducing the amount of epoxy-modified montmorillonite, zinc ricinoleate was in excess. As a result, the deodorization modifier formed was a mixture of zinc ricinoleate and zinc ricinoleate-grafted epoxy-modified montmorillonite. When 2 parts of the deodorization modifier were used in step (3), the content of ricinoleate-grafted epoxy-modified montmorillonite in Comparative Example 2 was lower than that in Example 1, resulting in an impure deodorization modifier. Since ricinoleate-grafted epoxy-modified montmorillonite plays a key role in deodorization, the performance decreased.

[0052] Example 2

[0053] A method for preparing polyester filaments with deodorizing function, the specific steps are as follows:

[0054] (1) By mass, first add 90 parts of ethanol and 10 parts of water to a reaction flask, add 2 parts of formic acid to adjust the pH value of the solution to 3, then add 5 parts of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, and hydrolyze for 3 h. Finally, add 20 parts of montmorillonite to the hydrolyzed system, and reflux and react at 60 °C for 12 h. The product is washed 5 times with ethanol, filtered, and dried to obtain epoxy-modified montmorillonite;

[0055] (2) By mass, mix 95 parts of epoxy-modified montmorillonite, 10 parts of zinc ricinoleate, and 200 parts of ethanol, add phosphoric acid to adjust the pH value of the system to 4, and react at 50 °C for 5 h to obtain a deodorization modifier;

[0056] (3) By mass, mix 4 parts of the deodorization modifier, 60 parts of vacuum-dehydrated polytetramethylene ether glycol (number-average molecular weight of 2000), 4 parts of isophorone diisocyanate trimer, and 0.2 parts of bismuth neodecanoate at room temperature to obtain a solvent-free two-component deodorization finishing agent;

[0057] (4) Place the solvent-free two-component deodorization finishing agent in an oil bath tank, keep it at 45 °C to make the viscosity 300 mPa·s, and then obtain polyester filaments with deodorizing function through a spinning process of melting polyester raw materials - metering - spinning - cooling - passing through the oil bath tank - oiling - stretching - heat curing - winding and forming;

[0058] The spinning process parameters are: spinning temperature 310 °C, cooling air blowing temperature 23 °C, cooling air blowing speed 0.5 m / s, stretching temperature 150 °C, stretching ratio 5 times, heat curing temperature 100 °C, and heat curing time 3 s;

[0059] Among them, the content of the solvent-free two-component deodorization finishing agent after the cooled filament bundle passes through the oil bath tank is 1.0 wt%.

[0060] The deodorization rate of the finally prepared polyester filament with deodorizing function is 86%. After washing according to GB / T 8629-2017, the deodorization rate is 82%.

[0061] Example 3

[0062] A preparation method of a polyester filament with deodorizing function, the specific steps are as follows:

[0063] (1) By mass, first add 90 parts of ethanol and 10 parts of water into a reaction flask, add 2 parts of formic acid to adjust the pH value of the solution to 3, then add 5 parts of γ-(2,3-epoxypropoxy)propyltrimethoxysilane, hydrolyze for 3 h, and finally add 20 parts of montmorillonite to the hydrolyzed system, and reflux and react at 55 °C for 12 h. The product is washed with ethanol 5 times, filtered and dried in sequence to obtain epoxy-modified montmorillonite;

[0064] (2) By mass, mix 95 parts of epoxy-modified montmorillonite, 10 parts of zinc ricinoleate and 200 parts of ethanol, then add phosphoric acid to adjust the pH value of the system to 4, and react at 50 °C for 5 h to obtain a deodorizing modifier;

[0065] (3) By mass, mix 5 parts of deodorizing modifier, 70 parts of vacuum-dehydrated succinic acid-based polymer polyol (number-average molecular weight is 3000), 5 parts of isophorone diisocyanate trimer and 0.3 parts of bismuth isooctanoate evenly at room temperature to obtain a solvent-free two-component deodorizing finishing agent;

[0066] (4) Place the solvent-free two-component deodorizing finishing agent in an oil bath tank, keep it at 50 °C to make the viscosity 400 mPa·s. After the spinning process of melting polyester raw material - metering - spinning - cooling - passing through the oil bath tank - oiling - stretching - thermal curing - winding and forming, the polyester filament with deodorizing function is obtained;

[0067] The spinning process parameters are: spinning temperature 320 °C, cooling air blowing temperature 28 °C, cooling air blowing speed 0.6 m / s, stretching temperature 160 °C, stretching multiple 6 times, thermal curing temperature 110 °C, thermal curing time 3 s;

[0068] Among them, the content of the solvent-free two-component deodorizing finishing agent after the cooled filament bundle passes through the oil bath tank is 1.2 wt%.

[0069] The deodorization rate of the finally prepared polyester filament with deodorizing function is 88%. After washing according to GB / T 8629-2017, the deodorization rate is 83%.

Claims

1. A method for preparing polyester yarn with deodorizing function, characterized in that: The solvent-free two-component deodorizing finishing agent is placed in an oil bath, kept at 40-50°C to make the viscosity 200-400mPa·s, and the polyester yarn with deodorizing function is obtained after the spinning process of melting polyester raw material - metering - spinning - cooling - passing through the oil bath - stretching - heat curing - winding and forming; The solvent-free two-component deodorizing finishing agent is obtained by mixing component A and component B evenly at room temperature; Component A is a deodorizing modifier and a bio-based macromolecular polyol after vacuum dehydration, and component B is a curing agent and a catalyst; The amount of each material in the solvent-free two-component deodorizing finishing agent is as follows: 2 to 5 parts of deodorizing modifier, 55 to 70 parts of bio-based macromolecular polyol after vacuum dehydration, 3 to 5 parts of curing agent, and 0.1 to 0.3 parts of catalyst; The deodorant modifier is synthesized by mixing 90-95 parts of epoxy-modified montmorillonite, 5-10 parts of zinc ricinoleate and 200 parts of ethanol by weight, adjusting the pH value of the system to 3-4, and reacting at 40-50° C. to obtain the deodorant modifier; The synthesis method of epoxy-modified montmorillonite is as follows: a silane coupling agent containing an epoxy group is mixed with montmorillonite, and the epoxy-modified montmorillonite is obtained by hydrolysis and condensation reaction under acidic conditions.

2. The method for preparing a polyester yarn with deodorizing function according to claim 1, characterized in that: After the oil bath, there is also an oiling process, and then stretching is carried out.

3. The method for preparing a polyester yarn with deodorizing function according to claim 1 or 2, characterized in that: The content of the solvent-free two-component deodorizing finishing agent in the cooled tow after passing through the oil bath is 0.8-1.2 wt %.

4. The method for preparing a polyester yarn with a deodorizing function according to claim 1, characterized in that: The spinning process parameters are: spinning temperature 300-320°C, cooling blowing temperature 18-28°C, cooling blowing speed 0.3-0.6 m / s, stretching temperature 130-160°C, stretching multiple 4-6 times, thermal curing temperature 90-110°C, and thermal curing time 2-3s.

5. The method for preparing a polyester yarn with a deodorizing function according to claim 1, characterized in that: The bio-based macromolecular polyol is polytrimethylene ether glycol or succinic acid-based polymer polyol, and the number average molecular weight of the bio-based macromolecular polyol is 1000-3000.

6. The method for preparing a polyester yarn with a deodorizing function according to claim 1, characterized in that: The curing agent is one or more of hexamethylene diisocyanate trimer and isophorone diisocyanate trimer.

7. The method for preparing a polyester yarn with a deodorizing function according to claim 1, characterized in that: The catalyst is bismuth neodecanoate or bismuth isooctanoate.

8. The method for preparing a polyester yarn with a deodorizing function according to claim 1, characterized in that: The specific synthesis process of epoxy-modified montmorillonite is as follows: by weight, first add 90 parts of ethanol and 10 parts of water into a reaction bottle, add 1-2 parts of formic acid to adjust the pH value of the solution to 2-3, then add 5 parts of epoxy-containing silane coupling agent, hydrolyze for 2-3 hours, Finally, 10 to 20 parts of montmorillonite are added to the hydrolyzed system, and the reaction is refluxed at 50 to 60° C. for 10 to 12 hours. The product is washed with ethanol for 3 to 5 times, filtered and dried to obtain epoxy-modified montmorillonite.

9. The method for preparing a polyester yarn with a deodorizing function according to claim 8, characterized in that: The epoxy-containing silane coupling agent is γ-(2,3-epoxypropoxy)propyltrimethoxysilane.

10. The method for preparing polyester yarn with deodorizing function according to claim 1, characterized in that: The deodorization rate of polyester yarn with deodorizing function is above 85%. After washing according to GB / T 8629-2017, the deodorization rate is still higher than 80%.