A nylon fabric anti-yellowing agent and its preparation method and application
By using maleic anhydride and dimethylhydrazine-based nylon fabric anti-heat yellowing agent, the problem of nylon fiber yellowing in high temperature is solved, the low-cost and efficient anti-heat yellowing effect is achieved, and the product is improved Security.
Patent Information
- Application Number
- CN202211673688.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2022-12-26
- Publication Date
- 2025-02-25
- Estimated Expiration
- 2042-12-26
AI Technical Summary
Nylon fibers are prone to yellowing during high temperature treatment. The existing anti-heat yellowing agents are costly and have poor performance. They contain ADH and will absorb formaldehyde, which is not conducive to human health.
A nylon fabric anti-heat yellowing agent prepared in a 1:1 molar ratio using maleic anhydride and dimethylhydrazine as materials. This agent does not adsorb formaldehyde and organizes the nylon fabric through the rolling-baking-baking process.
It achieves the effect of nylon fabrics not yellowing under high temperature treatment, while reducing raw material costs, avoiding formaldehyde adsorption, and improving product safety and market prospects.
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Abstract
Description
Technical Field
[0001] The invention belongs to the field of textiles, and specifically relates to a nylon fabric dyeing and finishing auxiliary agent and application thereof, and in particular to a nylon fabric anti-heat yellowing agent and a preparation method and application thereof. Background Art
[0002] Nylon is an important textile raw material and is widely used in textile and other industrial fields. However, nylon fiber also has some shortcomings, such as poor heat resistance and easy yellowing under light and heat. Fiber fabrics such as white textiles and dyed textiles can be processed into various clothing and are deeply favored by consumers.
[0003] From the molecular structure of nylon, it has many amide groups, which give this fiber many excellent physical and mechanical properties, including good wear resistance, fatigue resistance and resilience. At present, this fiber has been widely used in stockings, stretch knitted outerwear, thin seamless underwear, high-end swimsuits, sportswear and suit linings, etc., and is favored by consumers. However, when the fiber is treated at high temperature, the terminal amino group is easily oxidized and yellowing occurs, affecting the final performance of the fabric. Therefore, for white and light-colored fiber fabrics that need to be treated at high temperature (such as heat setting), heat-resistant yellowing treatment should be carried out. However, the existing domestic heat-resistant yellowing agent formula has a high raw material cost and poor product performance. Although the product containing ADH (adipic acid dihydrazide) has good performance, it adsorbs formaldehyde and is not conducive to human health. Most manufacturers use imported products, and it is difficult for domestic products to reach the effect level of imported products. Summary of the invention
[0004] In view of the above technical problems, the first object of the present invention is to provide a nylon fabric anti-heat yellowing agent, which will not absorb methanol after finishing the nylon fabric and also has the effect of anti-heat yellowing.
[0005] The second purpose of the present invention is to provide a method for preparing a nylon fabric anti-yellowing agent, which has low raw material cost, a simple synthesis route, high efficiency, does not require any catalyst, does not produce any pollutants, has low formula cost, has no special requirements for equipment, has a simple manufacturing process, and is easy to realize industrialization.
[0006] The third object of the present invention is to provide a nylon fabric anti-yellowing agent for use in finishing nylon fabrics, and the finished nylon fabrics have the advantages of being able to maintain whiteness and brightness and being friendly to the human body and the environment.
[0007] To achieve the above object, the technical solution of the present invention is:
[0008] A nylon fabric anti-yellowing agent, wherein the structure of the nylon fabric anti-yellowing agent has the following groups:
[0009]
[0010] Wherein, the nylon fabric anti-heat yellowing agent does not absorb formaldehyde.
[0011] Preferably, the nitrogen of the hydrazide group in the chemical formula of the nylon fabric anti-yellowing agent is connected to two methyl end caps.
[0012] A method for preparing the above-mentioned nylon fabric anti-yellowing agent comprises the following steps:
[0013] Place maleic anhydride and unsymmetrical dimethylhydrazine in pure water, stir and dissolve, then react at a temperature of 30-45° C. for 1-2 hours. The reaction temperature should not be too high, as too high a temperature may cause the appearance of impurities. After the reaction is completed, cool to room temperature (room temperature in the present invention refers to a temperature range of 20-30° C.), adjust the product concentration by weight with pure water, and obtain a nylon fabric anti-heat yellowing agent.
[0014] Wherein, the molar concentration of maleic anhydride and UDMH is 1:1-3, preferably 1:1.
[0015] If the concentration of the raw material solution is too high, impurities may appear. Therefore, the maleic anhydride and unsymmetrical dimethylhydrazine are placed in pure water with a weight of 2-4 times the weight of the monomers and stirred and dissolved.
[0016] Preferably, for the purpose of anti-yellowing effect and cost calculation, the product concentration is adjusted to 20-30% by weight with purified water.
[0017] The nylon fabric anti-heat yellowing agent is the above-mentioned nylon fabric anti-heat yellowing agent or is obtained by the above-mentioned preparation method of the nylon fabric anti-heat yellowing agent. The nylon fabric anti-heat yellowing agent adopts a pad-bake-cook process to perform anti-heat yellowing finishing on nylon fabric.
[0018] The pad-bake-baking process is as follows: after the nylon fabric is dipped in the anti-yellowing agent finishing liquid, it is pre-baked at 100-110° C. for 2-4 minutes, and then baked at a temperature of 185-200° C. for 30-120 seconds.
[0019] After padding, the liquid carrying rate of the nylon fabric is 45-60%.
[0020] Due to the adoption of the above technical solution, the present invention has the following advantages and positive effects compared with the prior art:
[0021] (1) The nylon anti-yellowing agent of the present invention has a simple synthesis route, high efficiency, does not require any catalyst, does not produce any pollutants, has a low formulation cost, has no special requirements for equipment, has a simple manufacturing process, is easy to mass produce, and realizes industrialization.
[0022] (2) The nylon anti-yellowing agent of the present invention is prepared by using maleic anhydride and unsymmetrical dimethyl hydrazine as materials in a 1:1 molar ratio, and the product has a novel structure, a single component, and stable performance. In particular, by using unsymmetrical dimethyl hydrazine as a raw material, the active hydrogen on the hydrazide group of the synthesized anti-yellowing agent is blocked with a dimethyl group, and the finished nylon fabric will not absorb surrounding formaldehyde during use and storage, thereby improving the safety of the product. In addition, the carboxylic acid-containing structure puts the finished nylon fabric in an acidic atmosphere, and together with the hydrazide structure, has a synergistic anti-yellowing effect.
[0023] (3) The nylon anti-yellowing agent of the present invention has good water solubility, good effect, high product quality, and can well maintain the whiteness and brightness of nylon fabric after finishing, which is friendly to the human body and the environment and has broad market prospects. DETAILED DESCRIPTION
[0024] The following is a further detailed description of the nylon fabric anti-yellowing agent, preparation method and application proposed by the present invention in conjunction with specific embodiments. The advantages and features of the present invention will become more apparent from the following description.
[0025] Example 1
[0026] Maleic anhydride and unsymmetrical dimethylhydrazine in a molar ratio of 1:1 were placed in pure water twice the weight of the monomers, stirred and dissolved, and then reacted at 35°C for 1.5 hours to obtain the product. After the reaction was completed, the product was cooled to room temperature.
[0027] After removal of solvent and purification, the product was used 1 H NMR and HR-MS were used to verify the results: 1 H NMR (500MHz, Chloroform-d) δ10.81 (s, 1H), 7.45 (d, 1H), 7.07 (s, 1H), 6.91 (d, 1H); 2.77 (s, 6H).C6H 10 N2O3HR-MS detection value: 158.1562; calculated value: 158.1552. This indicates that the obtained product structure has The two chemical bonds of the nitrogen of the hydrazide group connect the two methyl end caps.
[0028] The product was adjusted with water to a product content of 20% by weight to obtain a nylon fabric anti-yellowing agent.
[0029] Example 2
[0030] The product in this example is adjusted to a product content of 30% by weight with purified water, and the rest is the same as in Example 1.
[0031] Example 3
[0032] Maleic anhydride and unsymmetrical dimethylhydrazine in a molar ratio of 1:1 were placed in pure water 3 times the weight of the monomers, stirred and dissolved, and then reacted at 45°C for 1 hour to obtain the product. After the reaction was completed, the product was cooled to room temperature.
[0033] After removal of solvent and purification, the product was used 1 H NMR and HR-MS were used to verify the results: 1 H NMR (500MHz, Chloroform-d) δ10.82 (s, 1H), 7.46 (d, 1H), 7.08 (s, 1H), 6.90 (d, 1H); 2.76 (s, 6H).C6H 10 N2O3HR-MS detection value: 158.1548; calculated value: 158.1552. This indicates that the obtained product structure has The two chemical bonds of the nitrogen of the hydrazide group connect the two methyl end caps.
[0034] The product was adjusted with water to a product content of 20% by weight to obtain a nylon fabric anti-yellowing agent.
[0035] Example 4
[0036] In this embodiment, maleic anhydride and unsymmetrical dimethylhydrazine in a molar ratio of 1:1 are placed in pure water twice the weight of the monomers, and the rest is the same as in Embodiment 3.
[0037] Example 5
[0038] Maleic anhydride and unsymmetrical dimethylhydrazine in a molar ratio of 1:1 were placed in pure water twice the weight of the monomers, stirred and dissolved, and then reacted at 30°C for 2 hours to obtain the product. After the reaction was completed, the product was cooled to room temperature.
[0039] After removal of solvent and purification, the product was used 1 H NMR and HR-MS were used to verify the results: 1 H NMR (500MHz, Chloroform-d) δ10.83 (s, 1H), 7.47 (d, 1H), 7.05 (s, 1H), 6.93 (d, 1H); 2.76 (s, 6H).C6H 10 N2O3HR-MS detection value: 158.1549; calculated value: 158.1552. This indicates that the obtained product structure has The two chemical bonds of the nitrogen of the hydrazide group connect the two methyl end caps.
[0040] The product was adjusted with water to a product content of 20% by weight to obtain a nylon fabric anti-yellowing agent.
[0041] 1. Thermal yellowing resistance test
[0042] The following is an experimental example of the effect of finishing nylon with the nylon fabric anti-yellowing agent obtained in the above five embodiments. Taking white nylon woven fabric as an example, the white nylon woven fabric was subjected to a heat yellowing resistance test after high-temperature baking.
[0043] Finishing process 1: The white nylon woven fabric was twice dipped and twice rolled in 30 g / L of the nylon fabric anti-heat yellowing agent finishing liquid of Example 1-5 (liquid carrying rate 55%), pre-baked at 110°C for 2 minutes in a heat setting machine and then baked at 185°C for 120s, and finally the whiteness of the white nylon fabric treated with and without the anti-heat yellowing agent was tested.
[0044] Finishing process 2: The white nylon woven fabric was twice dipped and twice rolled in 30 g / L of the nylon fabric anti-heat yellowing agent finishing liquid of Example 1-5 (liquid carrying rate 55%), pre-baked at 110°C for 2 minutes in a heat setting machine and then baked at 195°C for 60s, and finally the whiteness of the white nylon fabric treated with and without the anti-heat yellowing agent was tested.
[0045] Fabric whiteness test: Datacolor 750 colorimeter was used to test the whiteness of the original and finished fabrics. According to GB 8424.2-2001 Textile color fastness test - Instrumental evaluation method for relative whiteness, the sample was folded into 4 layers, and different points were measured 4 times to take the average value.
[0046] Table 1 Changes in whiteness values of nylon fabrics treated with and without heat-resistant yellowing agents
[0047] Finishing agent As is Not used Example 1 Example 2 Example 3 Example 4 Example 5 Finishing process 1 77.1 60.2 74.3 75.6 74.8 74.9 75.1 Finishing process 2 77.1 59.9 74.2 75.4 74.7 74.7 74.8
[0048] It can be seen from Table 1 above that the addition of the nylon heat-resistant yellowing agent that does not absorb formaldehyde in the embodiment can effectively improve the high-temperature yellowing phenomenon of nylon fabrics. The reason is that the heat-resistant yellowing agent in the embodiment covers the surface of nylon, blocking the relevant active groups in the fiber from contacting and reacting with oxygen, nitrogen dioxide, etc. in the air during high-temperature processing, thereby preventing the fabric from yellowing; and secondly, the chemical structure of the anti-yellowing agent in the embodiment contains carboxylic acid and hydrazide groups. The carboxylic acid-containing structure puts the nylon fabric in an acidic atmosphere after finishing, and has a synergistic anti-yellowing effect together with the hydrazide structure.
[0049] 2. Formaldehyde adsorption test
[0050] A 500 ppm formaldehyde solution was prepared and placed at the bottom of the sealed dryer. The sample was placed on the upper part of the partition. The whole was placed in a 30°C oven for 3.5 hours. The formaldehyde concentration in the air of the sealed dryer was tested using an air formaldehyde test kit, which was about 1.5 mg / m 3 , far exceeding the national standard indoor air formaldehyde concentration limit of 0.1mg / m 3 At such a high concentration, the difference in formaldehyde adsorption by nylon after treatment with different thermal yellowing agents can be more clearly seen.
[0051] Table 2 Adsorption of formaldehyde by nylon fabrics treated with anti-yellowing agent and untreated nylon fabrics at higher concentrations
[0052]
[0053] It can be seen from the above two tables that the nylon heat-resistant yellowing agent that does not absorb formaldehyde according to the embodiment of the present invention can effectively reduce the adsorption of formaldehyde in the surrounding environment by the fabric compared with the commonly used high-temperature heat-resistant yellowing agent ADH on the market. The reason is that the active hydrogen on the hydrazide group of the heat-resistant yellowing agent in the embodiment of the present invention is blocked with a dimethyl group, and the finished nylon fabric will not absorb the surrounding formaldehyde during use and storage, thereby improving the safety of the product.
[0054] The above is a detailed description of the implementation of the present invention in conjunction with specific embodiments, but the present invention is not limited to the above implementation. Even if various changes are made to the present invention, if these changes fall within the scope of the claims of the present invention and their equivalents, they still fall within the protection scope of the present invention.
Claims
1. An application of a nylon fabric anti-yellowing agent, characterized in that: The structure of the nylon fabric anti-yellowing agent has the following structure: Wherein, the nylon fabric anti-heat yellowing agent does not absorb formaldehyde, and the nylon fabric anti-heat yellowing agent adopts a pad-bake-cook process to perform anti-heat yellowing finishing on the nylon fabric; The preparation method of the nylon fabric anti-yellowing agent comprises: Maleic anhydride and unsymmetrical dimethylhydrazine with a molar concentration of 1:1 are placed in pure water, stirred and dissolved, and then reacted at a temperature of 30-45°C for 1-2 hours. After the reaction is completed, the mixture is cooled to 20-30°C, and then the concentration of the product is adjusted to 20-30% with pure water.
2. The use of the nylon fabric anti-yellowing agent according to claim 1, characterized in that: The maleic anhydride and unsymmetrical dimethylhydrazine are placed in pure water 2-4 times the weight of the monomers and stirred and dissolved.
3. The use of the nylon fabric anti-yellowing agent according to claim 1, characterized in that: The pad-bake-baking process is as follows: after the nylon fabric is dipped in the anti-yellowing agent finishing liquid, it is pre-baked at 100-110° C. for 2-4 minutes, and then baked at a temperature of 185-200° C. for 30-120 seconds. After padding, the liquid carrying rate of the nylon fabric is 45-60%.
Citation Information
Patent Citations
Process for the enhancement of thermostability
CN101426973A
Method for preventing formaldehyde in polyamide underwear from exceeding standard
CN108457081A