Preparation method of polyester yarn with deodorization function

Abstract

The invention relates to a preparation method of polyester yarn with a deodorization function, which comprises the following steps: putting a solvent-free bi-component deodorization finishing agent into an oil bath tank, and keeping the temperature at 40-50 DEG C to enable the viscosity to be 200-400 mPa.s; a product is prepared by a spinning process of melting a polyester raw material, metering, spinning, cooling, passing through an oil bath tank, stretching, thermocuring and winding and forming. The solvent-free bi-component deodorization finishing agent is obtained by uniformly mixing a component A and a component B at room temperature, the component A is a deodorization modifier and bio-based macromolecular polyol subjected to vacuum dehydration, and the component B is a curing agent and a catalyst; the synthesis method of the deodorizing modifier comprises the following steps: mixing 90-95 parts by mass of epoxy modified montmorillonite, 5-10 parts by mass of zinc diricinoleate and 200 parts by mass of ethanol, adjusting the pH value of the system to 3-4, and reacting at 40-50 DEG C to obtain the deodorizing modifier. According to the invention, the polyester yarn is endowed with an efficient and lasting deodorization function.

Description

Technical Field

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

[0002] Polyester fabrics have been widely used in clothing, home furnishings and other fields in recent years due to their excellent properties such as durability, wrinkle resistance, elasticity and good chemical resistance. With the continuous expansion of the application field of polyester fabrics and the continuous improvement of consumers' quality of life, polyester products with excellent deodorizing function have begun to gain people's favor. Odors are usually caused by nitrogen- and sulfur-containing molecules, namely amines, ammonia, thiols, 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 artificial zeolite powder, 20-24% ethyl acetate, and 0.5% leveling agent. The moisture-absorbing and deodorizing polyester knitted fabric of the patent uses screen printing technology to print the zeolite layer on polyester with a light fastness greater than level 6 and a 60°C high-temperature water washing color fastness greater than level 4. It not only retains the original advantages of polyester such as high light fastness and high-temperature water washing color fastness, but also can absorb moisture and deodorize; it also has the advantages of simple process. However, the above method imparts deodorizing properties by physically mixing zeolite, and the large amount of physical fillers introduced easily affects the feel of the fabric.

[0004] In contrast, the use of zinc ricinoleate as a deodorant material is more advantageous. Zinc ricinoleate contains active zinc atoms, which can form strong chemical bonds with nitrogen and sulfur atoms in the odor to completely eliminate the odor, and has no effect on fragrance ingredients 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 closed places with dense crowds of people.

[0005] Patent CN201610653393.5 discloses an antibacterial deodorant spray for textiles, including the following ingredients: α-acetylenic ketone, isopropyl myristate, tributyl acetyl citrate, tridecanoic acid, grapefruit seed extract, sodium bicarbonate, polyglycerol-3-decanoate, sucrose cocoate, zinc ricinoleate, dodecyl methacrylate, isothiazolinone, water-soluble plant essence, Tween 80, propylene glycol, vegetable glycerin, deionized water; non-toxic, colorless, non-irritating, non-corrosive, stable, safe and reliable, with broad-spectrum antibacterial and high-efficiency deodorizing functions, easy to use, especially for special uniforms, such as sanitation workers' uniforms, medical staff uniforms and corpse movers' uniforms, the deodorizing and antibacterial effects are significant after use. However, the patent is a spray physical adsorption, which needs to be used repeatedly and is not durable.

[0006] Therefore, it is of great significance to study a method for preparing polyester yarn with deodorizing function to solve the problems existing in the prior art. Summary of the invention

[0007] The purpose of the invention is to solve the problems existing in the prior art and provide a method for preparing polyester yarn with deodorizing function.

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

[0009] A method for preparing polyester yarn with deodorizing function, wherein a solvent-free two-component deodorizing finishing agent is placed in an oil bath, kept warm at 40-50°C to make the viscosity 200-400 mPa·s (the solvent-free two-component finishing agent usually has a large viscosity, and the two components need to be kept warm during use to ensure the fluidity of the finishing agent), and the polyester yarn with deodorizing function is prepared after a spinning process of melting polyester raw material - metering - spinning - cooling - passing through an oil bath - stretching - thermal curing - winding and forming; although heating is also performed during the stretching process, due to the high stretching speed, only a small part of the solvent-free two-component deodorizing finishing agent on the fiber after stretching will be cured, and the curing is incomplete, so further thermal curing is required;

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

[0011] 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;

[0012] The amount of each material in the solvent-free two-component deodorizing finishing agent is as follows: 2-5 parts of deodorizing 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: after mixing 90-95 parts of epoxy-modified montmorillonite, 5-10 parts of zinc ricinoleate and 200 parts of ethanol by weight, the pH value of the system is adjusted to 3-4, so that the molar ratio of hydroxyl group to epoxy group is in the range of 1.5-2:0.75-1, and reacting at 40-50° C. to obtain the deodorant modifier;

[0014] 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.

[0015] As the preferred technical solution:

[0016] The method for preparing the polyester yarn with deodorizing function as described above further comprises the step of oiling after passing through the oil bath, and then stretching is performed after oiling.

[0017] In the above-mentioned method for preparing polyester yarn with deodorizing function, the content of solvent-free two-component deodorizing finishing agent in the cooled yarn bundle after passing through the oil bath is 0.8-1.2wt%.

[0018] The method for preparing a polyester yarn with a deodorizing function as described above has the following spinning process parameters: spinning temperature (i.e., the temperature of the molten polyester raw material) 300~320°C, cooling blowing temperature 18~28°C, cooling blowing speed 0.3~0.6m / s, stretching temperature 130~160°C, stretching multiple 4~6 times, thermal curing temperature 90~110°C, and thermal curing time 2~3s.

[0019] In the method for preparing polyester yarn with deodorizing 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] In the above-mentioned method for preparing polyester yarn with deodorizing function, the curing agent is one or more of hexamethylene diisocyanate trimer and isophorone diisocyanate trimer.

[0021] In the method for preparing polyester yarn with deodorizing function as described above, the catalyst is bismuth neodecanoate or bismuth isooctanoate.

[0022] The preparation method of the polyester yarn with deodorizing function as described above, the specific synthesis process of epoxy-modified montmorillonite is as follows: by weight, first, 90 parts of ethanol and 10 parts of water are added to a reaction bottle, 1-2 parts of formic acid are added to adjust the pH value of the solution to 2-3, and then 5 parts of epoxy-containing silane coupling agent are added, and hydrolyzed for 2-3 hours, and finally 10-20 parts of montmorillonite are added to the hydrolyzed system, and reflux reaction is carried out at a temperature of 50-60°C for 10-12 hours, and the product is washed with ethanol 3-5 times, filtered and dried to obtain epoxy-modified montmorillonite.

[0023] In the method for preparing the polyester yarn with deodorizing function as described above, the epoxy-containing silane coupling agent is γ-(2,3-epoxypropoxy)propyltrimethoxysilane.

[0024] According to the method for preparing a polyester yarn with a deodorizing function as described above, the deodorizing rate of the polyester yarn with a deodorizing function is above 85%, and after being washed with water according to GB / T 8629-2017, the deodorizing rate is still higher than 80%.

[0025] Principle of the invention:

[0026] The present invention covalently intercalates zinc ricinoleate into montmorillonite with a high specific surface area, introduces it into a solvent-free two-component polyurethane coating system, and uniformly coats, solidifies and wraps the solvent-free two-component deodorant finishing agent with a deodorizing function on the surface of polyester filaments, which can give polyester fabrics an efficient deodorizing function from the source of the fabric, that is, the "fiber" level; the high specific surface area of ​​the montmorillonite after intercalation modification and the zinc ricinoleate grafted thereon synergistically give the polyester filaments an efficient and lasting deodorizing function. Specifically, the present invention retains the negative and positive charges on the montmorillonite on the one hand, and retains its efficient adsorption; at the same time, the reactivity of the hydroxyl group on the montmorillonite is utilized, the grafting coupling agent is used as a bridge, and then the zinc ricinoleate with a deodorizing function is grafted, and at the same time, a hydroxyl group on the castor oil is retained, so that such a large deodorizing molecule can be covalently bonded to the coating, improving the deodorizing stability and long-term performance.

[0027] Beneficial effects:

[0028] (1) The present invention provides a method for preparing polyester yarn with deodorizing function, wherein zinc ricinoleate is covalently intercalated into montmorillonite with a high specific surface area, introduced into a solvent-free two-component deodorizing finishing agent system, and a polyurethane coating with deodorizing function is uniformly coated, cured and wrapped on the surface of the polyester yarn, thereby giving the polyester fabric an efficient deodorizing function from the source of the fabric, that is, the "fiber" level; the high specific surface area of ​​the montmorillonite after intercalation modification and the zinc ricinoleate grafted thereon synergistically give the polyester yarn an efficient and lasting deodorizing function;

[0029] (2) The method for preparing a polyester yarn with a deodorizing function of the present invention uses zinc ricinoleate as a deodorizing modifying component, which is safe and non-toxic; and uses a solvent-free two-component deodorizing finishing agent as a finishing agent coating matrix, which is green and sustainable. The obtained polyester yarn with a deodorizing function is an environmentally friendly product and meets the sustainable development requirements of the industry;

[0030] (3) The method for preparing polyester yarn with deodorizing function of the present invention selects the organic chemical molecule zinc ricinoleate as the deodorizing modifier, which does not simply adsorb the odor, but can completely eliminate the odor molecules; it effectively solves the problems of simple adsorption of physical deodorizing materials, incomplete deodorization and affecting the feel of the fabric. DETAILED DESCRIPTION

[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 are not intended 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 fall within the scope limited by the appended claims of the application equally.

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

[0033] Deodorization rate: The experiment was carried out in accordance with QB / T2761-2006 standard.

[0034] The sources of the montmorillonite of the present invention are: manufacturer: Zhejiang Huate New Materials Co., Ltd., brand: DK32B; succinic acid-based polymer polyol comes from BioAmber Company, brand: SA-PEP.

[0035] Example 1

[0036] A method for preparing polyester yarn with deodorizing function, the specific steps are as follows:

[0037] (1) First, 90 parts of ethanol and 10 parts of water were added to a reaction bottle by weight, 1 part of formic acid was added to adjust the pH value of the solution to 2, and then 5 parts of γ-(2,3-epoxypropoxy)propyltrimethoxysilane were added and hydrolyzed for 2 hours. Finally, 10 parts of montmorillonite were added to the hydrolyzed system, and refluxed at 50°C for 10 hours. The product was washed with ethanol three times, filtered and dried to obtain epoxy-modified montmorillonite.

[0038] (2) 90 parts by mass of epoxy-modified montmorillonite, 5 parts by mass of zinc ricinoleate and 200 parts by mass of ethanol were mixed, phosphoric acid was added to adjust the pH value of the system to 3, and the mixture was reacted at 40° C. for 4 h to obtain a deodorant modifier;

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

[0040] (4) placing the solvent-free two-component deodorizing finishing agent in an oil bath and keeping it at 40°C to make the viscosity 200 mPa·s, and then undergoing a spinning process of melting polyester raw material - metering - spinning - cooling - passing through an oil bath - oiling - stretching - heat curing - winding to obtain polyester yarn with deodorizing function;

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

[0042] Among them, the content of the solvent-free two-component deodorizing finishing agent in the cooled tow after passing through the oil bath is 0.8 wt%.

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

[0044] Comparative Example 1

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

[0046] The deodorization rate of the prepared polyester yarn is 38%, and after washing according to GB / T 8629-2017, the deodorization rate is 32%.

[0047] By comparing Comparative Example 1 with Example 1, it can be found that the deodorization rate is significantly reduced. This is because without the intercalation modification of the silane coupling agent, the montmorillonite cannot be fully stripped, and it is difficult to exert the capture and adsorption effect of the high specific area layer on odor.

[0048] Comparative Example 2

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

[0050] The deodorization rate of the prepared polyester yarn is 82%, and after washing according to GB / T 8629-2017, the deodorization rate is 80%.

[0051] By comparing Comparative Example 2 with Example 1, it can be found that the deodorization rate is slightly reduced. This is because in step (2), after reducing the number of epoxy-modified montmorillonite, the amount of zinc ricinoleate is excessive, and the resulting deodorant is a mixture of zinc ricinoleate and zinc ricinoleate grafted modified epoxy-modified montmorillonite. When 2 parts of the deodorant are used in step (3), the content of castor oil grafted modified epoxy montmorillonite in Comparative Example 2 is lower than that in Example 1, resulting in the deodorant being impure. Castor oil grafted modified epoxy montmorillonite plays a key role in deodorization, so the performance is reduced.

[0052] Example 2

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

[0054] (1) First, 90 parts of ethanol and 10 parts of water were added to a reaction bottle by weight, 2 parts of formic acid were added to adjust the pH value of the solution to 3, and then 5 parts of γ-(2,3-epoxypropoxy)propyltrimethoxysilane were added and hydrolyzed for 3 hours. Finally, 20 parts of montmorillonite were added to the hydrolyzed system, and refluxed at 60°C for 12 hours. The product was washed with ethanol 5 times, filtered and dried to obtain epoxy-modified montmorillonite.

[0055] (2) 95 parts by mass of epoxy-modified montmorillonite, 10 parts by mass of zinc ricinoleate and 200 parts by mass of ethanol were mixed, phosphoric acid was added to adjust the pH value of the system to 4, and the mixture was reacted at 50° C. for 5 h to obtain a deodorant modifier;

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

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

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

[0059] Among them, the content of the solvent-free two-component deodorizing finishing agent in the cooled tow after passing through the oil bath is 1.0 wt%.

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

[0061] Example 3

[0062] A method for preparing polyester yarn with deodorizing function, the specific steps are as follows:

[0063] (1) First, 90 parts of ethanol and 10 parts of water were added to a reaction bottle by weight, 2 parts of formic acid were added to adjust the pH value of the solution to 3, and then 5 parts of γ-(2,3-epoxypropoxy)propyltrimethoxysilane were added and hydrolyzed for 3 hours. Finally, 20 parts of montmorillonite were added to the hydrolyzed system, and refluxed at 55°C for 12 hours. The product was washed with ethanol 5 times, filtered and dried to obtain epoxy-modified montmorillonite.

[0064] (2) 95 parts by mass of epoxy-modified montmorillonite, 10 parts by mass of zinc ricinoleate and 200 parts by mass of ethanol were mixed, phosphoric acid was added to adjust the pH value of the system to 4, and the mixture was reacted at 50° C. for 5 h to obtain a deodorant modifier;

[0065] (3) 5 parts by weight of a deodorant modifier, 70 parts by weight of a succinic acid-based polymer polyol (number average molecular weight of 3000) after vacuum dehydration, 5 parts by weight of isophorone diisocyanate trimer and 0.3 parts by weight of bismuth isooctanoate were mixed uniformly at room temperature to obtain a solvent-free two-component deodorant finishing agent;

[0066] (4) placing the solvent-free two-component deodorizing finishing agent in an oil bath and maintaining the temperature at 50°C to make the viscosity 400 mPa·s, and then undergoing a spinning process of melting polyester raw material - metering - spinning - cooling - passing through an oil bath - oiling - stretching - heat curing - winding to obtain polyester yarn with deodorizing function;

[0067] The spinning process parameters are as follows: 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, heat curing temperature 110°C, heat curing time 3 s;

[0068] Among them, the content of the solvent-free two-component deodorizing finishing agent in the cooled tow after passing through the oil bath is 1.2 wt%.

[0069] The deodorization rate of the polyester yarn with deodorization function finally obtained is 88%, and 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 200-400 mPa·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: 2-5 parts of deodorizing 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; 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 solvent-free two-component deodorizing finishing agent in the cooled tow after passing through the oil bath is 0.8~1.2wt%.

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℃, cooling blowing temperature 18~28℃, cooling blowing speed 0.3~0.6m / s, stretching temperature 130~160℃, stretching multiple 4~6 times, thermal curing temperature 90~110℃, 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 mass, 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, and finally add 10-20 parts of montmorillonite to the hydrolyzed system, reflux at 50-60°C for 10-12 hours, and the product is washed with ethanol 3-5 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%.