A nylon softener and a method for preparing the same

Abstract

This application relates to the technical field of textile auxiliary agent synthesis, and in particular to a nylon softener and its preparation method, which is prepared from the following components by weight percentage: 10%-20% nylon silicone oil, 0.3%-1.0% pH adjuster, 1.0%-3.0% anti-coagulation agent, and deionized water to make up the balance to 100%. This application improves the bonding strength between the prepared nylon softener and nylon fabrics by modifying the nylon silicone oil with an organic amine similar in structure to nylon fibers, while also increasing the absorption rate of the nylon softener by the nylon fibers. Furthermore, the nylon softener exhibits good stability and dispersibility, resulting in better softness properties for novel nylon fabrics.

Description

Technical Field

[0001] This application relates to the technical field of textile auxiliary agent synthesis, and in particular to a nylon softener and its preparation method. Background Technology

[0002] Silicone softeners can impart softness, smoothness, fluffiness, elasticity, and hydrophilicity to fabrics, improving their quality. Therefore, they are widely used in fabric hand finishing. Nylon has high strength, light weight, high abrasion resistance, good resilience, and better moisture absorption than polyester, making it widely used in sportswear, fitness apparel, and mountaineering clothing. However, with the diversification of nylon fiber structure and fabric weaving, the processing difficulty of some nylon fabrics in terms of hand feel is also increasing. For example, nylon single-hole yarn, nylon twill, and nylon blends of multiple fibers are difficult to soften, affecting wearing comfort and seriously restricting the development of the industry.

[0003] The invention patent with publication number CN113373696A discloses a softener for bamboo fiber fabrics and its preparation method. The steps include: (1) reacting low molecular weight polyether epoxy silicone oil with tetramethylhexanediamine, polyetheramine EA600 and polyetheramine AM2200 respectively to obtain A1, A2 and A3; (2) reacting medium molecular weight polyether epoxy silicone oil with polyetheramine EA220, polyetheramine EA600 and polyetheramine EA900 respectively to obtain B1, B2 and B3; (3) reacting high molecular weight polyether epoxy silicone oil with diethanolamine, polyetheramine EA1200 and polyetheramine AM2200 respectively to obtain C1, C2 and C3; (4) mixing A1, A2, A3, B1, B2, B3, C1, C2 and C3 with an emulsifier and then adding a modified piperazine-based silicone oil emulsion and an additive.

[0004] The softener prepared by the method disclosed in this invention patent has the problem of poor softening effect on relatively new nylon fabrics. Summary of the Invention

[0005] The technical problem to be solved by the present invention is to provide a nylon softener and its preparation method, which improves the bonding force between the prepared nylon softener and nylon fabric by modifying nylon silicone oil with an organic amine similar in structure to nylon fiber. At the same time, the nylon fiber has a high absorption rate of the nylon softener, and the nylon softener has good stability and dispersibility, and has good softness performance for new nylon fabrics.

[0006] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:

[0007] A nylon softener, said nylon softener being prepared from components comprising the following in weight percentages:

[0008]

[0009] The isoelectric point of nylon fibers is 5.0-6.0. When the solution pH is lower than the isoelectric point, the nylon fibers carry a positive charge. Since the nylon silicone oil also carries a positive charge, like charges repel each other, causing the nylon silicone oil and nylon fibers to bind only through intermolecular attraction such as van der Waals forces or hydrogen bonds. The binding force is weak, thus reducing the softening effect of the nylon silicone oil on the nylon fibers. When the solution pH is higher than the isoelectric point of the nylon fibers, the nylon silicone oil is not easy to emulsify and has poor subsequent storage stability. By adopting the above technical solution, by adding a pH adjuster to the nylon silicone oil, the pH of the nylon softener prepared in this application is maintained near the isoelectric point of the nylon fibers, so that the nylon softener prepared in this application has a good softening effect and is also easy to store.

[0010] In this invention, the pH adjuster is composed of a mixture of acetic acid, diethanolamine, and triethanolamine, wherein the mass ratio of acetic acid, diethanolamine, and triethanolamine is (5-6):(1-2):(1-2).

[0011] By adopting the above technical solution, acetic acid, diethanolamine, and triethanolamine are mixed in proportion to form a relatively stable buffer system, which keeps the pH value of the nylon softener at 5.0-6.0, close to the isoelectric point of nylon fibers. This facilitates the adsorption of silicone oil onto the surface of nylon fibers and improves the utilization rate of silicone oil.

[0012] In this invention, the anti-coagulation agent is isomeric alcohol polyoxyethylene ether silane, wherein the carbon chain length of the isomeric alcohol in the isomeric alcohol polyoxyethylene ether silane is one or a combination of C10 and C13.

[0013] By adopting the above technical solution, isomeric alcohol polyoxyethylene ether silane, because it contains silicon atoms, can be tightly adsorbed on the surface of silicone oil according to the principle of like dissolves like, so that the nylon softener forms a stable system. At the same time, due to its large molecular weight and good dispersibility, it forms a strong barrier between silicone oil and other impurities, preventing demulsification and aggregation, and preventing silicone oil stains from being formed on the fabric.

[0014] In this invention, the nylon silicone oil is prepared from components comprising the following weight percentages:

[0015] End-cap epoxy silicone oil 50%-60%

[0016] Organic amines 3.0%-5.0%

[0017] Isopropanol 30%-50%.

[0018] By adopting the above technical solution, grafting organic amines onto end-epoxy silicone oil can improve the adsorption of nylon silicone oil on nylon fibers, thereby improving the wash resistance of nylon softener.

[0019] In this invention, the organic amine is one or a combination of 1,5-pentanediamine, 1,6-hexanediamine, and 1,7-heptanediamine.

[0020] By adopting the above technical solution, adding one or more of 1,5-pentanediamine, 1,6-hexanediamine, and 1,7-heptanediamine to nylon silicone oil results in the presence of structural segments similar to nylon fibers in the silicone oil. Based on the principle of like dissolves like, this increases the affinity between silicone oil molecules and nylon fibers, thereby increasing the absorption rate of silicone oil molecules.

[0021] In this invention, the nylon silicone oil is prepared through the following steps:

[0022] A1: In a nitrogen atmosphere, add terminal epoxy silicone oil, organic amine and isopropanol into the reactor, stir continuously and heat, slowly raising the temperature to 78-82℃.

[0023] A2: Maintain the reactor temperature between 78-82℃ for 1-2 hours to allow the material inside the reactor to transform into a transparent fluid;

[0024] A3: Continue to maintain the temperature of the material in the reactor at 78-82℃ for 6-8 hours to obtain nylon silicone oil.

[0025] By adopting the above technical solution, nitrogen is used to fill the reaction vessel, reducing the degree of oxidation of the epoxy silicone oil and organic amines during high-temperature heating, thereby improving the quality of the final synthesized nylon silicone oil.

[0026] The preparation method of the nylon softener in this invention includes the following steps:

[0027] B1: Add nylon silicone oil to the reactor and stir continuously for 5-10 minutes;

[0028] B2: After mixing the pH adjuster and deionized water evenly, add the pH adjuster and water mixture into the reaction vessel of step B1 and stir continuously for 20-30 minutes.

[0029] B3: Slowly add the remaining deionized water to the reactor from step B2 over a period of 1-2 hours.

[0030] B4: After the deionized water is added, add the anti-coagulation agent to the reactor in step B3 and stir for 10-20 minutes to obtain the nylon softener.

[0031] By adopting the above technical solution and through long-term stirring, the various materials of the nylon softener are fully mixed, and the addition of pH adjuster and anti-coagulation agent helps to maintain the stability of the entire system.

[0032] In this invention, the mass ratio of pH adjuster to deionized water in step B2 is 1:(10-20).

[0033] By adopting the above technical solution, when the pH adjuster is directly added to the reactor, the high concentration can easily lead to the destruction of the stable system. Diluting the pH adjuster with deionized water in advance can reduce the occurrence of this phenomenon.

[0034] More specifically, the preparation method described in this invention is recommended to be carried out according to the following steps: Nitrogen gas is continuously purged into reactor A for 5-10 minutes to replace the original air in reactor A, creating a nitrogen environment. After closing the nitrogen pipeline, 50-60 parts by mass of terminal epoxy silicone oil, 30-40 parts by mass of isopropanol, and 3-5 parts by mass of organic amine are added to reactor A. The mixture is continuously stirred and heated. Within 1-2 hours, the temperature of reactor A and the materials inside reactor A is slowly raised to 78-82°C. Stirring is then continued, and the temperature inside reactor A is maintained at 78-82°C for 1-2 hours. After the material in reactor A has transformed into a transparent fluid, reactor A is kept at 78-82℃ for 6-8 hours to obtain nylon silicone oil. 10-20 parts of the nylon silicone oil are added to reactor B and stirred continuously for 5-10 minutes. 3-20 parts of deionized water and 0.3-1 parts of pH adjuster are mixed evenly, and the mixture of pH adjuster and water is added to reactor B. The remaining deionized water is slowly added to reactor B over 1-2 hours. After the deionized water is completely added, an anti-coagulation agent is added to reactor B and stirred continuously for 10-20 minutes to obtain nylon softener.

[0035] The beneficial effects of the synthesis method described in this invention are mainly as follows: when preparing nylon softener, nylon silicone oil is modified by using organic amines. The organic amines used have a similar carbon chain structure to those in nylon fibers. The organic amines are incorporated into the nylon silicone oil chain segments. According to the principle of "like dissolves like," the organic amines help to improve the bonding force between nylon silicone oil and nylon fabric, and also improve the absorption rate of nylon softener by nylon fibers. Traditional softeners generally use isomeric alcohol polyoxyethylene ether as an anti-agglomeration agent. In this application, isomeric alcohol polyoxyethylene ether silane is used instead of isomeric alcohol polyoxyethylene ether. Since isomeric alcohol polyoxyethylene ether silane and silicone oil both contain silicon atoms, it is easier to adsorb onto the surface of silicone oil molecules than isomeric alcohol polyoxyethylene ether, thereby improving the dispersibility of silicone oil molecules, reducing aggregation, and making it easier for nylon softener to disperse on the surface of nylon fibers. Detailed Implementation

[0036] The present invention will be further described below through specific embodiments, but the scope of protection of the present invention is not limited thereto.

[0037] Example 1:

[0038] Nitrogen gas was continuously purged into reactor A for 10 minutes to replace the existing air, creating a nitrogen environment. After shutting off the nitrogen supply, 50g of epoxy silicone oil, 47g of isopropanol, and 3g of 1,6-hexanediamine were added to reactor A. The mixture was continuously stirred and heated, slowly raising the temperature of reactor A and its contents to 80°C over one hour. Stirring was continued, and the temperature was maintained at 80°C for 2 hours. Once the material in reactor A had transformed into a transparent fluid, reactor A was maintained at 80°C for another 6 hours to obtain nylon silicone oil. 20g of this nylon silicone oil was added to reactor B, and the mixture was stirred continuously for 10 minutes. Acetic acid, diethanolamine, and triethanolamine were then mixed in a 5:1:1 mass ratio to obtain... To obtain the pH adjuster, mix 10g of deionized water and 1g of pH adjuster evenly. Add the mixture of pH adjuster and water to reactor B. Continue to slowly add 68g of deionized water to reactor B over a period of 1 hour. After the deionized water has been added, mix isomeric alcohol polyoxyethylene ether silane with a carbon chain length of C10 and isomeric alcohol polyoxyethylene ether silane with a carbon chain length of C13 in a 1:1 mass ratio to obtain an anti-coagulation agent. Add 1g of anti-coagulation agent to reactor B and stir continuously for 10 minutes to obtain nylon softener.

[0039] The difference between Examples 2-3 and Comparative Examples 1-2 and Example 1 lies in the type of organic amine added in step A1, as shown in the table below:

[0040]

[0041] The difference between Examples 4-5 and Example 1 lies in the anti-coagulation agent added in step B4, as shown in the table below:

[0042]

[0043] The difference between Examples 6-7 and Comparative Example 3 and Example 1 lies in the amount of pH adjuster added in step B2, as shown in the table below:

[0044] Example 1 Example 6 Example 7 Comparative Example 3 Comparative Example 4 pH adjuster 1g 0.6g 0.3g 0 2

[0045] Comparative Example 5 is a commercially available conventional silicone oil softener.

[0046] Detection methods

[0047] Feel Evaluation

[0048] Fabric: Nylon monofilament fabric

[0049] Process: one dip and one roll, 75% slurry yield, 160℃, machine speed 1m / min.

[0050] Evaluation method: Five people with experience in tactile evaluation were selected to blindly touch the treated fabric sample and score it, with a minimum score of 1 point and a maximum score of 10 points. The lowest and highest scores were removed, and the average score was taken. The test results are shown in the table below:

[0051]

[0052] Conclusion: Data from Examples 1 and Comparative Example 5 in the table above show that the nylon softener prepared by the method described in this invention exhibits significantly higher softening properties for nylon fabrics than commercially available softeners. This indicates that the softening properties of the nylon softener prepared by the method described in this invention meet market requirements, and the hand feel gradually improves with increasing dosage. Using isomeric alcohol polyoxyethylene ether silane instead of traditional isomeric alcohol polyoxyethylene ether as an anti-coagulation agent can significantly improve the softening properties of the nylon softener. Data from Examples 1 and Comparative Example 6 in the table above show that the addition of organic amines during the preparation of nylon silicone oil in the method described in this invention can immediately provide the softening properties of the nylon softener. Data from Examples 1-3 and Comparative Examples 1-2 in the table above show that 1,5-pentanediamine, 1,6-hexanediamine, and 1,7-heptanediamine provide better softening properties.

[0053] Stability test

[0054] The finished softeners from each example and comparative example were prepared into a 50 g / L mixture. 100 g of each example and comparative example was placed in separate steel cups. 5 g of 0.2 g / L Disperse Red 3B, 5 g of 5.0 g / L Glauber's salt, and 5 g of 5.0 g / L soda ash were added to each cup. The mixtures were kept at 50°C for 30 minutes, 60 minutes, and 90 minutes, and the presence of flocculent matter was observed to determine the stability of each mixture. The test results are shown in the table below.

[0055]

[0056] Conclusion: As can be seen from the data in Example 1 and Comparative Example 3 above, the preparation method of the present invention can significantly improve the stability of nylon softener by adding a pH adjuster during the preparation process. As can be seen from the data in Example 1, Examples 6-7 and Comparative Example 4 above, when the amount of pH adjuster added is less than 1%, the stability of nylon softener is better as the amount of pH adjuster added increases. When the amount of pH adjuster added is greater than 1%, the effect of increasing the stability of nylon softener is not obvious. The amount of pH adjuster added is more suitable between 0.3% and 1%.

[0057] Conclusion: As can be seen from the data in Example 1 and Comparative Example 5 above, the preparation method of the present invention, in the process of preparing nylon softener, uses isomeric alcohol polyoxyethylene ether silane instead of traditional isomeric alcohol polyoxyethylene ether as an anti-coagulation agent, which can significantly improve the dispersibility and stability of nylon softener. As can be seen from the data in Example 1 and Examples 4-5 above, the effect of mixing isomeric alcohol polyoxyethylene ether silane with a carbon chain length of C10 and isomeric alcohol polyoxyethylene ether silane with a carbon chain length of C13 in a mass ratio of 1:1 is better.

[0058] Conclusion: As can be seen from the data of Example 1 and Comparative Example 6 in the table above, the preparation method of the present invention can improve the dispersibility and stability of nylon softener by adding organic amines during the preparation of nylon silicone oil. As can be seen from the data of Examples 1-3 and Comparative Examples 1-2 in the table above, when the structure of the added organic amine is close to that of hexamethylenediamine, it is similar to the structure of nylon fiber and has good stability. When the carbon chain length of the organic amine is less than five or greater than seven, the stability of the nylon softener decreases. Therefore, 1,5-pentanediamine, 1,6-hexamethylenediamine, and 1,7-heptanediamine are preferred organic amines.

[0059] The above are all preferred embodiments of this application, and are not intended to limit the scope of protection of this application. Therefore, all equivalent changes made in accordance with the structure, shape and principle of this application should be covered within the scope of protection of this application.

Claims

1. A nylon softener, characterized in that, The nylon softener is prepared from the following components in weight percentages: 10%-20% nylon silicone oil pH adjuster 0.3%-1.0%, Anti-coagulant 1.0%-3.0% The remaining deionized water level should be replenished to 100%. The anti-coagulation agent is composed of isomeric alcohol polyoxyethylene ether silane with a carbon chain length of C10 and isomeric alcohol polyoxyethylene ether silane with a carbon chain length of C13 in a 1:1 mass ratio. The pH adjuster is composed of acetic acid, diethanolamine, and triethanolamine, wherein the mass ratio of acetic acid, diethanolamine, and triethanolamine is (5-6):(1-2):(1-2). The nylon silicone oil is prepared from components comprising the following weight percentages: End-cap epoxy silicone oil 50%-60%; Organic amines: 3.0%-5.0%; Isopropanol 30%-50%; The organic amine is one or a combination of 1,5-pentanediamine, 1,6-hexanediamine, and 1,7-heptanediamine.

2. The nylon softener according to claim 1, characterized in that: The nylon silicone oil is prepared by the following steps: A1: In a nitrogen atmosphere, add terminal epoxy silicone oil, organic amine and isopropanol into the reactor, stir continuously and heat, slowly raising the temperature to 78-82℃. A2: Maintain the reactor temperature between 78-82℃ for 1-2 hours to allow the material inside the reactor to transform into a transparent fluid; A3: Continue to maintain the temperature of the material in the reactor at 78-82℃ for 6-8 hours to obtain nylon silicone oil.

3. A method for preparing a nylon softener as described in any one of claims 1 to 2, characterized in that, Includes the following steps: B1: Add nylon silicone oil to the reactor and stir continuously for 5-10 minutes; B2: After mixing the pH adjuster and deionized water evenly, add the pH adjuster and water mixture into the reaction vessel of step B1 and stir continuously for 20-30 minutes. B3: Slowly add the remaining deionized water to the reactor from step B2 over a period of 1-2 hours. B4: After the deionized water is added, add the anti-coagulation agent to the reactor in step B3 and stir for 10-20 minutes to obtain the nylon softener.

4. The method for preparing a nylon softener according to claim 3, characterized in that: In step B2, the mass ratio of pH adjuster to deionized water is 1:(10-20).

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