Super cool polyester fiber and preparation method thereof
By using the ratio of modified guar gum and cool particles in polyester fiber, the super cool guar gum and mechanical properties of the fiber are improved, and the problem of poor mechanical properties of the existing fibers is solved, achieving better use effects.
Patent Information
- Application Number
- CN202510234317.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-28
- Publication Date
- 2025-05-06
AI Technical Summary
The existing cool-sensing polyester fibers have poor performance in mechanical properties and have a short service life, making it difficult to have excellent super cool-sensing sensibility while maintaining good mechanical properties.
The ratio of 60-80 parts of polyester, 6-10 parts of modified guar gum, 3-7 parts of cold-sensing particles and 400-550 parts of N,N-dimethylformamide is adopted. The anti-static, super cool-sensing and mechanical properties of the fiber are improved by the synthesis method of modified guar gum and cold-sensing particles.
It achieves that polyester fibers have excellent super cool sensibility and anti-static properties while maintaining good mechanical properties, extending their service life.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of textiles, and in particular relates to a super cool polyester fiber and a preparation method thereof. Background Art
[0002] With the improvement of people's living standards and the increasing demand for comfortable wear, the research and development and application of functional fibers have become an important development direction of the textile industry. As the most widely used chemical fiber, polyester fiber has good fiber-forming properties, high strength, light resistance, heat resistance, acid and alkali resistance, and good processability and easy spinning. With the rise of global temperatures and the hot summer, cool polyester fiber came into being. As a new type of functional fiber, cool polyester fiber has a significant cooling effect and a comfortable wearing experience, and has broad application prospects.
[0003] In a hot environment, people hope to lower their body temperature and improve comfort by wearing clothes with cooling function. Although traditional polyester fiber has good physical properties and processing performance, it still lacks in cooling performance. Therefore, the development of polyester fiber with super cooling function has become an important topic in the textile industry.
[0004] Chinese patent CN 118546500 A provides a cool polyester masterbatch, fiber and preparation method thereof, wherein the cool polyester masterbatch comprises modified polyester and a plant-based cool agent, wherein the plant-based cool agent is a mixture obtained by condensation of an ester of a mint extract and dihydroxyethyl terephthalate. Although this invention improves the coolness of the polyester fiber to a certain extent, the mechanical properties of the polyester fiber are unsatisfactory and the service life is short.
[0005] Therefore, there is an urgent need for a super cool polyester fiber that can make the polyester fiber have excellent super cool properties while maintaining good mechanical properties. Summary of the invention
[0006] In view of the existing technical problems, the purpose of the present invention is to provide a super cool polyester fiber and a preparation method thereof. The polyester fiber of the present invention has excellent antistatic properties, super cool properties and mechanical properties.
[0007] In order to achieve the above object, the technical solution adopted by the present invention is as follows:
[0008] On one hand, the present invention provides a super cool polyester fiber, which comprises the following raw materials by weight: 60-80 parts of polyester, 6-10 parts of modified guar gum, 3-7 parts of cool particles, and 400-550 parts of N,N-dimethylformamide.
[0009] The reaction mechanism and effects of the present invention are as follows:
[0010] 1. Guar gum is a natural polysaccharide with good biodegradability. On the one hand, guar gum has excellent thickening and stability, and can provide a stable solution environment during the fiber production process to ensure the uniformity and consistency of polyester fibers. On the other hand, guar gum contains a large number of hydrophilic groups and has good hygroscopicity. It can absorb moisture on the fiber surface and further enhance the cooling effect of polyester fibers. At the same time, the effect of moisture on the steady-state cooling of the fabric is greater than the thermal conductivity of the fiber. The better the hygroscopicity of the fabric, the better its steady-state cooling effect. However, the high temperature resistance of guar gum is average.
[0011] The invention uses guar gum and N-ethyl-3-hydroxy-N,N-dimethylaniline chloride to react to prepare modified guar gum. A quaternary ammonium salt structure and a benzene ring structure are introduced into the guar gum. The quaternary ammonium salt group is a cationic group with a positive charge, which can interact with the negative charge on the surface of an object, thereby effectively reducing the static electricity on the surface of the object, further improving the antistatic performance of the cool polyester fiber, thereby improving the comfort and durability of the fiber; in addition, the benzene ring structure has high chemical stability and strong π-π interaction, can interact with the benzene ring structure or other aromatic ring structures in the polyester fiber, enhance the affinity between the modified guar gum and the polyester fiber, thereby improving the stability and uniformity of the fiber, and at the same time, the benzene ring structure helps to improve the high temperature resistance of the modified guar gum, so that it can still maintain good performance in a high temperature environment, and is suitable for various processing techniques.
[0012] 2. Inorganic powders are prone to uneven dispersion in polyester systems. Aluminum nitride, boron nitride and silicon nitride are all functional fillers with high specific surface area and good thermal conductivity. The present invention uses inorganic powders, lauryl hydroxysulfonyl betaine and a dispersant to prepare cooling particles, which improves its dispersion performance in the polyester system, thereby improving the cooling coefficient of the polyester fiber; at the same time, lauryl hydroxysulfonyl betaine has good hydrophilicity, anti-fouling and antistatic properties. In addition, inorganic powders have the characteristics of high strength and low density. Introducing them into polyester fibers can toughen and strengthen the fibers and improve the mechanical properties of the polyester fibers.
[0013] In some embodiments, the method for preparing the modified guar gum comprises the following steps:
[0014] S1. Mix guar gum and solvent, stir for 30-60 min at 20-35 ° C, adjust the pH value to 10.5-11.5, stir and react for 20-35 min to obtain a liquid;
[0015] S2. The liquid obtained in step S1 and N-ethyl-3-hydroxy-N,N-dimethylaniline chloride are mixed, heated to 60-75° C., stirred for reaction for 2-3 hours, washed, and dried to obtain modified guar gum.
[0016] In some embodiments, the solvent in step S1 is a combination of anhydrous ethanol and deionized water.
[0017] In some embodiments, the mass ratio of guar gum to solvent in step S1 is 1:(3.5-5.5).
[0018] In some embodiments, the mass ratio of guar gum to N-ethyl-3-hydroxy-N,N-dimethylaniline chloride in the liquid is 1:(0.1-0.3).
[0019] In some embodiments, the method for preparing the cooling particles comprises the following steps:
[0020] The inorganic powder, deionized water, lauryl hydroxysulfobetaine and a dispersant are mixed, ball-milled, washed and dried to obtain cooling particles.
[0021] Preferably, the dispersant is any one or more of sodium hexametaphosphate, sodium pyrophosphate, and sodium tripolyphosphate.
[0022] Further preferably, the mass ratio of the inorganic powder to the dispersant is 10:(0.015-0.035).
[0023] In some embodiments, the inorganic powder is any one or more of aluminum nitride, boron nitride and silicon nitride.
[0024] In some embodiments, the particle size D50 of the inorganic powder is 100-500 nm.
[0025] In some embodiments, the mass ratio of the inorganic powder to lauryl hydroxysulfobetaine is 10:(0.1-0.4).
[0026] Another aspect of the present invention provides a method for preparing super cool polyester fiber, comprising the following steps:
[0027] Q1. Mix polyester, modified guar gum, cooling particles, and N,N-dimethylformamide, and stir to obtain a spinning solution;
[0028] Q2. The spinning solution obtained in step Q1 is wet-spun and dried at 50-70°C for 8-10 hours under vacuum conditions to obtain polyester fibers.
[0029] In some embodiments, the process parameters of the wet spinning in step Q2 are as follows: immersing the spinneret in deionized water, pouring the spinning solution into a liquid container for wet spinning, and transporting the spinning solution in the liquid container to the spinneret assembly through a peristaltic pump at a transport speed of 0.58-0.62 mL / min. The outer diameter of the spinneret hole on the spinneret is 1.2-1.4 mm, and the inner diameter is 0.6-0.8 mm. The spinning solution is extruded through the spinneret hole to form a hollow spinning stream. At the same time, another peristaltic pump transports deionized water into the interior of the hollow spinning stream at a transport speed of 0.8-1.0 mL / min. The inner and outer surfaces of the hollow spinning stream are in contact with the deionized water at the same time. Under the action of double diffusion, the hollow spinning stream is solidified into polyester fiber.
[0030] Compared with the prior art, the present invention has the following beneficial effects:
[0031] 1. The polyester fiber of the present invention has excellent antistatic properties, super cool feeling and mechanical properties.
[0032] 2. The modified guar gum of the present invention enables the guar gum to maintain good performance under high temperature environment. On the one hand, the modified guar gum can not only improve the cooling effect of polyester fiber, but also improve the uniformity of polyester fiber; on the other hand, the quaternary ammonium salt structure introduced into the guar gum can improve the antistatic performance of the cooling polyester fiber; in addition, the introduction of the benzene ring structure can enhance the affinity between the modified guar gum and the polyester fiber, thereby improving the stability of the fiber.
[0033] 3. The present invention uses inorganic powder, lauryl hydroxysulfonyl betaine and a dispersant to prepare cooling particles, thereby improving the dispersion performance in the polyester system, thereby improving the cooling coefficient of the polyester fiber, and at the same time, it can also play a role in toughening and strengthening the polyester fiber, thereby improving the mechanical properties of the polyester fiber. DETAILED DESCRIPTION
[0034] The present invention will be described below in conjunction with specific embodiments. It should be noted that the following embodiments are examples of the present invention and are only used to illustrate the present invention, rather than to limit the present invention. Other combinations and various modifications within the concept of the present invention may be performed without departing from the spirit or scope of the present invention.
[0035] According to the ratios of the raw materials and the preparation methods specified in the following examples and comparative examples, various polyester fibers were produced.
[0036] In order to facilitate those skilled in the art to implement the present invention, some raw material manufacturers of the embodiments and comparative examples are described as follows:
[0037] Polyethylene terephthalate: purchased from Guangdong Pengcheng Shihai New Materials Co., Ltd.; model: PET-P1000;
[0038] Boron nitride: particle size D50 is 200nm;
[0039] Other raw materials are not specially specified and can be purchased from the market.
[0040] Preparation Example 1
[0041] The preparation method of modified guar gum A comprises the following steps:
[0042] S1. 140 g of guar gum, 630 g of anhydrous ethanol and 180 g of deionized water were mixed and stirred at 30 ° C for 45 min, the pH value was adjusted to 11.0 with a molar concentration of 1 mol / L of sodium hydroxide aqueous solution, and the reaction was stirred for 30 min to obtain a liquid;
[0043] S2. Mix all the liquid obtained in step S1 and 28 g of N-ethyl-3-hydroxy-N,N-dimethylaniline chloride, heat to 70°C, stir and react for 2.5 hours, wash with anhydrous ethanol three times, and dry at 75°C for 16 hours under vacuum conditions to obtain modified guar gum A.
[0044] Preparation Example 2
[0045] The preparation method of modified guar gum B is the same as that of Preparation Example 1, except that the added amount of N-ethyl-3-hydroxy-N,N-dimethylaniline chloride is 11.2 g.
[0046] Preparation Example 3
[0047] The preparation method of cooling particles A comprises the following steps:
[0048] 20 g of boron nitride, 120 mL of deionized water, 0.5 g of lauryl hydroxysulfobetaine, and 50 mg of sodium hexametaphosphate were mixed, wet-milled for 3 h, washed with deionized water 3 times, and dried at 80° C. for 16 h under vacuum conditions to obtain cooling particles A.
[0049] Preparation Example 4
[0050] The preparation method of cooling particles B is the same as that of Preparation Example 3, except that the amount of lauryl hydroxysulfobetaine added is 0.16 g.
[0051] Preparation Example 5
[0052] The preparation method of cooling particles C is the same as that of Preparation Example 3, except that sodium hexametaphosphate is not added.
[0053] Example 1
[0054] A super cool polyester fiber comprises the following raw materials in parts by weight: 70 parts of polyethylene terephthalate, 8 parts of modified guar gum A, 5 parts of cool particles A, and 480 parts of N,N-dimethylformamide.
[0055] The method for preparing the polyester fiber of this embodiment comprises the following steps:
[0056] Q1. Polyethylene terephthalate, modified guar gum A, cooling particles A, and N,N-dimethylformamide are mixed and stirred to obtain a spinning solution;
[0057] Q2. The spinning solution obtained in step Q1 is wet-spun, and dried at 80°C for 9h under vacuum conditions to obtain polyester fibers; wherein the process parameters of the wet spinning are as follows: the spinneret is immersed in deionized water, the spinning solution is poured into a liquid container for wet spinning, the spinning solution in the liquid container is transported to the spinneret assembly by a peristaltic pump at a transport speed of 0.60mL / min, the outer diameter of the spinneret hole on the spinneret is 1.3mm, and the inner diameter is 0.7mm. The spinning solution is extruded through the spinneret hole to form a hollow spinning stream. At the same time, another peristaltic pump transports deionized water into the hollow spinning stream at a transport speed of 0.9mL / min. The inner and outer surfaces of the hollow spinning stream are in contact with the deionized water at the same time. Under the action of double diffusion, the hollow spinning stream is solidified into polyester fibers.
[0058] Example 2
[0059] A super cool polyester fiber comprises the following raw materials in parts by weight: 60 parts of polyethylene terephthalate, 6 parts of modified guar gum A, 3 parts of cool particles A, and 400 parts of N,N-dimethylformamide.
[0060] The method for preparing the polyester fiber of this embodiment comprises the following steps:
[0061] Q1. Polyethylene terephthalate, modified guar gum A, cooling particles A, and N,N-dimethylformamide are mixed and stirred to obtain a spinning solution;
[0062] Q2. The spinning solution obtained in step Q1 is wet-spun, and dried at 90°C for 8h under vacuum conditions to obtain polyester fibers; wherein the process parameters of the wet spinning are as follows: the spinneret is immersed in deionized water, the spinning solution is poured into a liquid container for wet spinning, the spinning solution in the liquid container is transported to the spinneret assembly by a peristaltic pump at a transport speed of 0.58mL / min, the outer diameter of the spinneret hole on the spinneret is 1.2mm, and the inner diameter is 0.6mm. The spinning solution is extruded through the spinneret hole to form a hollow spinning stream. At the same time, another peristaltic pump transports deionized water into the hollow spinning stream at a transport speed of 0.8mL / min. The inner and outer surfaces of the hollow spinning stream are in contact with the deionized water at the same time. Under the action of double diffusion, the hollow spinning stream is solidified into polyester fibers.
[0063] Example 3
[0064] A super cool polyester fiber comprises the following raw materials in parts by weight: 80 parts of polyethylene terephthalate, 10 parts of modified guar gum A, 7 parts of cool particles A, and 550 parts of N,N-dimethylformamide.
[0065] The method for preparing the polyester fiber of this embodiment comprises the following steps:
[0066] Q1. Polyethylene terephthalate, modified guar gum A, cooling particles A, and N,N-dimethylformamide are mixed and stirred to obtain a spinning solution;
[0067] Q2. The spinning solution obtained in step Q1 is wet-spun, and dried at 60°C for 10 hours under vacuum conditions to obtain polyester fibers; wherein the process parameters of the wet spinning are as follows: the spinneret is immersed in deionized water, the spinning solution is poured into a liquid container for wet spinning, the spinning solution in the liquid container is transported to the spinneret assembly by a peristaltic pump, and the transport speed is 0.62 mL / min. The outer diameter of the spinneret hole on the spinneret is 1.4 mm, and the inner diameter is 0.8 mm. The spinning solution is extruded through the spinneret hole to form a hollow spinning stream. At the same time, another peristaltic pump transports deionized water into the hollow spinning stream at a transport speed of 1.0 mL / min. The inner and outer surfaces of the hollow spinning stream are in contact with the deionized water at the same time. Under the action of double diffusion, the hollow spinning stream is solidified into polyester fibers.
[0068] Example 4
[0069] A super cool polyester fiber and a preparation method thereof. The specific implementation manner is the same as that of Example 1, except that an equal amount of modified guar gum B is used to replace modified guar gum A.
[0070] Example 5
[0071] A super cool polyester fiber and a preparation method thereof. The specific implementation method is the same as that of Example 1, except that an equal amount of cool particles B is used to replace cool particles A.
[0072] Example 6
[0073] A super cool polyester fiber and a preparation method thereof. The specific implementation method is the same as that of Example 1, except that an equal amount of cool particles C is used to replace cool particles A.
[0074] Comparative Example 1
[0075] A super cool polyester fiber and a preparation method thereof. The specific implementation manner is the same as that of Example 1, except that an equal amount of guar gum is used to replace modified guar gum A.
[0076] Comparative Example 2
[0077] A super cool polyester fiber and a preparation method thereof. The specific implementation manner is the same as that of Example 1, except that an equal amount of boron nitride is used to replace the cool particles A.
[0078] Effect evaluation:
[0079] The polyester fibers prepared in the above Examples 1-6 and Comparative Examples 1-2 were tested, and the specific results are shown in Table 1-2.
[0080] Performance Test:
[0081] (1) Cooling coefficient: The cooling coefficient is measured in accordance with the national standard GB / T 35263-2017 Testing and evaluation of instantaneous cooling properties of textiles;
[0082] (2) Elongation at break: The test was conducted in accordance with GB / T 14337-2022 Test Method for Tensile Strength of Chemical Staple Fibers. The mechanical properties of single polyester fiber were tested using a fiber strength and elongation tester. The applied tension was 0.15 cN / dtex, the stretching rate was 20 mm / min, the clamping distance was 20 mm, and the draft ratio was 1.6 times.
[0083] Table 1
[0084]
[0085]
[0086] The results in Table 1 show that the polyester fibers of Examples 1 to 3 have excellent super cooling properties and elongation at break.
[0087] When preparing modified guar gum, Example 4 changes the mass ratio of guar gum and N-ethyl-3-hydroxy-N,N-dimethylaniline chloride compared to Example 1, the benzene ring structure on the modified guar gum is reduced, the stability and uniformity of the polyester fiber are reduced, and the super coolness and elongation at break of the polyester fiber are reduced.
[0088] When preparing the cooling particles, Example 5 changes the mass ratio of the inorganic powder to lauryl hydroxysulfobetaine compared to Example 1, and Example 6 does not add a dispersant compared to Example 1, both of which reduce the dispersibility of the inorganic powder, thereby reducing the super cooling property and elongation at break of the polyester fiber.
[0089] Compared with Example 1, Comparative Example 1 uses an equal amount of guar gum to replace modified guar gum A, and the quaternary ammonium salt and benzene ring structure on the guar gum are reduced. Comparative Example 2 uses an equal amount of boron nitride to replace the cooling particles A. Boron nitride is easy to agglomerate, both of which will reduce the super cooling property and elongation at break of the polyester fiber.
[0090] (3) Antistatic property: The polyester fiber was woven into a polyester fiber fabric by a textile machine, and the charge surface density of Examples 1 to 3 and Comparative Example 1 was tested with reference to GB / T 12703 Textile Electrostatic Test Method.
[0091] Table 2
[0092] Serial number <![CDATA[Surface charge density / μc·m -2 > Example 1 0.56 Example 2 0.51 Example 3 0.58 Comparative Example 1 0.69
[0093] It can be seen from the results in Table 2 that the cool polyester fibers prepared in Examples 1-3 of the present invention have good antistatic properties.
[0094] The above is only a preferred embodiment of the present invention and does not constitute any form of limitation to the present application. Although the present application is disclosed as above in the preferred embodiment, it is not intended to limit the present application. Any technician familiar with the profession, without departing from the scope of the technical solution of the present application, using the technical content disclosed above to make slight changes or modifications are equivalent to equivalent implementation cases. However, any simple modifications, equivalent changes and modifications made to the above embodiments based on the technical essence of the present invention without departing from the content of the technical solution of the present invention are still within the scope of the technical solution.
Claims
1. A super cool polyester fiber, characterized in that: The polyester fiber comprises the following raw materials by weight: 60-80 parts of polyester, 6-10 parts of modified guar gum, 3-7 parts of cooling particles, and 400-550 parts of N,N-dimethylformamide.
2. The super cool polyester fiber according to claim 1, characterized in that: The preparation method of the modified guar gum comprises the following steps: S1. Mix guar gum and solvent, stir for 30-60 min at 20-35 ° C, adjust the pH value to 10.5-11.5, stir and react for 20-35 min to obtain a liquid; S2. The liquid obtained in step S1 and N-ethyl-3-hydroxy-N,N-dimethylaniline chloride are mixed, heated to 60-75° C., stirred for reaction for 2-3 hours, washed, and dried to obtain modified guar gum.
3. The super cool polyester fiber according to claim 2, characterized in that: The solvent in step S1 is a composition of anhydrous ethanol and deionized water.
4. The super cool polyester fiber according to claim 2, characterized in that: The mass ratio of guar gum to N-ethyl-3-hydroxy-N,N-dimethylaniline chloride in the liquid is 1:(0.1-0.3).
5. The super cool polyester fiber according to claim 1, characterized in that: The preparation method of the cooling particles comprises the following steps: The inorganic powder, deionized water, lauryl hydroxysulfobetaine and a dispersant are mixed, ball-milled, washed and dried to obtain cooling particles.
6. The super cool polyester fiber according to claim 5, characterized in that: The inorganic powder is any one or more of aluminum nitride, boron nitride and silicon nitride.
7. The super cool polyester fiber according to claim 5, characterized in that: The particle size D50 of the inorganic powder is 100-500nm.
8. The super cool polyester fiber according to claim 5, characterized in that: The mass ratio of the inorganic powder to lauryl hydroxysulfobetaine is 10:(0.1-0.4).
9. A method for preparing the super cool polyester fiber according to any one of claims 1 to 8, characterized in that: The following steps are included: Q1. Mix polyester, modified guar gum, cooling particles, and N,N-dimethylformamide, and stir to obtain a spinning solution; Q2. The spinning solution obtained in step Q1 is wet-spun and dried at 60-90°C for 8-10 hours under vacuum conditions to obtain polyester fibers.
10. The method for preparing a super cool polyester fiber according to claim 9, characterized in that: The process parameters of the wet spinning described in step Q2 are as follows: immersing the spinneret in deionized water, pouring the spinning solution into a liquid container for wet spinning, and conveying the spinning solution in the liquid container to the spinneret assembly through a peristaltic pump at a conveying speed of 0.58-0.62 mL / min. The outer diameter of the spinneret hole on the spinneret is 1.2-1.4 mm, and the inner diameter is 0.6-0.8 mm. The spinning solution is extruded through the spinneret hole to form a hollow spinning stream. At the same time, another peristaltic pump conveys deionized water into the hollow spinning stream at a conveying speed of 0.8-1.0 mL / min. The inner and outer surfaces of the hollow spinning stream are in contact with the deionized water at the same time. Under the action of double diffusion, the hollow spinning stream is solidified into polyester fiber.
Citation Information
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