A method for preparing a high compatibility silicone softener

Abstract

The application discloses a preparation method of a high-compatibility organic silicon softener. The method comprises the following steps: a. under the protection of nitrogen, sodium methoxide is used as a catalyst to react hydroxyl silicone oil with bio-based fatty acid ester to obtain an organic phase product; b. nano silicon dioxide is added into the product obtained in the step a, the nano silicon dioxide is uniformly dispersed under the assistance of ultrasonic waves, polyether amine and water are added, a microemulsion is formed through high-speed shearing emulsification, and polyaspartic acid sodium is added and uniformly mixed to obtain the high-compatibility organic silicon softener. The application realizes effective preparation of the high-performance and high-compatibility fabric softener, and meets the production requirement.

Description

Technical Field

[0001] This invention relates to the field of fabric softener technology, and more specifically, to a method for preparing a highly compatible organosilicon softener. Background Technology

[0002] Existing silicone softeners (such as dimethyl silicone oil) mostly rely on physical adsorption to reach the fiber surface, making it difficult to penetrate deep into the fiber. This results in a general lack of compatibility in textile processing. Particularly in the treatment of natural fibers such as cotton and linen, the lack of strong interaction between the fiber's hydroxyl groups and silicone oil molecules leads to easy migration and shedding of the softener, significantly reducing wash resistance and hand feel durability. These compatibility issues between existing silicone softeners and fibers limit their application, making it difficult to meet the demands of modern textile multifunctionality and efficient production. Summary of the Invention

[0003] The purpose of this invention is to overcome the shortcomings of the prior art and provide a method for preparing a highly compatible organosilicon softener.

[0004] To achieve the above objectives, the present invention adopts the following technical solution:

[0005] A method for preparing a highly compatible organosilicon softener includes the following steps:

[0006] a. Under nitrogen protection, sodium methoxide is used as a catalyst to react hydroxyl silicone oil with bio-based fatty acid esters to obtain organic phase products;

[0007] b. Add nano-silica to the product obtained in step a, disperse it evenly under ultrasonic assistance, add polyetheramine and water, emulsify at high speed to form a microemulsion, then add sodium polyaspartate, mix evenly to obtain a highly compatible organosilicon softener.

[0008] The present invention is further configured such that the molar ratio of hydroxyl silicone oil to bio-based fatty acid ester is 1:1.2-1:1.6, and the bio-based fatty acid ester is ethyl lactate.

[0009] The present invention is further configured such that the amount of catalyst used is 1-2% of the mass of hydroxyl silicone oil.

[0010] The present invention is further configured such that the amount of nano-silica used is 1-2% of the mass of the bio-based fatty acid ester.

[0011] The present invention is further configured such that the amount of polyetheramine used is 1 / 10 to 3 / 20 of the mass of the bio-based fatty acid ester.

[0012] The present invention is further configured such that the mass ratio of polyetheramine to water in step b is 1:3-6.

[0013] The present invention is further configured such that the amount of sodium polyaspartate is 1-2% of the mass of the bio-based fatty acid ester.

[0014] The present invention is further configured such that step a specifically comprises: under nitrogen protection, adding hydroxyl silicone oil and bio-based fatty acid ester to the reactor and stirring and mixing at 80-100°C, adding sodium methoxide catalyst and continuing stirring and heating to 100-120°C for reaction, removing ethanol byproducts during the reaction, cooling to room temperature after the reaction, adding sodium carbonate to adjust the pH of the system to 7, adding saturated brine to wash the reaction solution, allowing it to stand and separate into layers, and separating the organic phase.

[0015] The present invention is further configured such that the reaction time at 100-120℃ is 4-6h.

[0016] In summary, the present invention has the following beneficial effects:

[0017] This invention improves the interaction between silicone softeners and natural fibers such as cotton and linen by reacting hydroxyl silicone oil with bio-based fatty acid esters, utilizing the dual effects of hydroxyl and ester groups. This improves compatibility, and further enhances the bonding between silicone softeners and fabrics through modification with nano-silica and sodium polyaspartate, thereby improving the fabric's wash resistance. This invention achieves the effective preparation of highly compatible softeners that can meet production needs. Detailed Implementation

[0018] The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0019] The preparation method of the highly compatible organosilicon softener of the present invention includes the following steps:

[0020] a. Modified silicone oil is prepared by reacting hydroxyl silicone oil with bio-based fatty acid esters under nitrogen protection and using p-toluenesulfonic acid as a catalyst. Specifically, under nitrogen protection, hydroxyl silicone oil and bio-based fatty acid esters (preferably ethyl lactate, with a molar ratio of hydroxyl silicone oil to bio-based fatty acid ester of 1:1.2-1.6) are added to a reactor and stirred at 80-100℃ for 30 min. Then, p-toluenesulfonic acid (catalyst amount is 1-2% of the mass of hydroxyl silicone oil) is added, and stirring is continued and the temperature is raised to 100-120℃ for 4-6 h. During the reaction, ethanol byproducts are removed. After the reaction, the mixture is cooled to room temperature, sodium carbonate is added to adjust the pH of the system to 7, saturated brine is added to wash the reaction solution, and the mixture is allowed to stand and separate into layers to separate the organic phase.

[0021] b. Add 1-2% nano-silica (by mass of bio-based fatty acid ester) to the organic phase and disperse it evenly under ultrasonic assistance. Add polyetheramine and water (polyetheramine accounts for 1 / 10-3 / 20 of the mass of bio-based fatty acid ester, and the mass ratio of polyetheramine to water is 1:3-6). Emulsify by high-speed shearing to form a microemulsion. Add 1-2% sodium polyaspartate (by mass of bio-based fatty acid ester) and mix evenly to obtain an organosilicon softener that is highly compatible with cotton fibers.

[0022] Example 1

[0023] a. Under nitrogen protection, hydroxyl silicone oil and ethyl lactate (molar ratio of hydroxyl silicone oil to ethyl lactate is 1:1.3) are added to the reactor and stirred at 95°C for 30 min. Then, 0.9% of the mass of hydroxyl silicone oil catalyst p-toluenesulfonic acid is added, and stirring is continued until the temperature is raised to 110°C for 6 h. During the reaction, ethanol byproducts are removed. After the reaction, the mixture is cooled to room temperature, sodium carbonate is added to adjust the pH of the system to 7, saturated brine is added to wash the reaction solution, and the mixture is allowed to stand and separate into layers to separate the organic phase.

[0024] b. Add 1.3% of nano-silica (based on the mass of bio-based fatty acid ester) to the organic phase and disperse it evenly under ultrasonic assistance. Add polyetheramine and water (polyetheramine accounts for 3 / 20 of the mass of ethyl lactate, and the mass ratio of polyetheramine to water is 1:5). Emulsify by high-speed shearing to form a microemulsion. Add 1.6% of sodium polyaspartate (based on the mass of ethyl lactate) and mix evenly to obtain a highly compatible organosilicon softener.

[0025] Comparative Example 1

[0026] The softener was prepared according to Example 1, but without the addition of nano-silica.

[0027] Comparative Example 2

[0028] The softener was prepared according to Example 1, but without the addition of polyetheramine.

[0029] Comparative Example 3

[0030] The softener was prepared according to Example 1, but without the addition of sodium polyaspartate.

[0031] Comparative Example 4

[0032] The softener was prepared according to Example 1, but sodium polyaspartate was replaced by an equal mass of acrylic acid-acrylamide copolymer.

[0033] The softeners prepared in Example 1 and Comparative Examples 1-4 were used to treat cotton fabrics (the treatment process was: two dips and two nips (70% pick-up) → pre-drying (105℃, 2 min) → baking (150℃, 2 min)). The performance test results are shown in Table 1 (initially, the cotton fabric treated with the softener retained 51.2% of its breaking strength after 250 washes).

[0034]

[0035] The above description is merely a preferred embodiment of the present invention. The scope of protection of the present invention is not limited to the above embodiments. All technical solutions falling within the scope of the present invention's concept are within the scope of protection of the present invention. It should be noted that for those skilled in the art, any improvements and modifications made without departing from the principles of the present invention should also be considered within the scope of protection of the present invention.

Claims

1. A method for preparing a highly compatible organosilicon softener, characterized in that, Includes the following steps: a. Under nitrogen protection, p-toluenesulfonic acid is used as a catalyst to react hydroxyl silicone oil with bio-based fatty acid ester to obtain an organic phase product, wherein the bio-based fatty acid ester is ethyl lactate. Step a specifically involves: under nitrogen protection, adding hydroxyl silicone oil and ethyl lactate to the reactor and stirring at 95°C, adding 0.9% (by weight of) p-toluenesulfonic acid catalyst and continuing stirring and heating to 110°C for 6 hours, removing ethanol byproducts during the reaction, cooling to room temperature after the reaction, adding sodium carbonate to adjust the pH of the system to 7, adding saturated brine to wash the reaction solution, allowing it to stand and separate into layers, and separating the organic phase; the molar ratio of hydroxyl silicone oil to ethyl lactate is 1:1.

3. b. Add 1.3% of the bio-based fatty acid ester mass of nano-silica to the organic phase, disperse it evenly under ultrasonic assistance, add polyetheramine and water, emulsify to form a microemulsion, then add 1.6% of the ethyl lactate mass of sodium polyaspartate, mix evenly to obtain a highly compatible organosilicon softener; the polyetheramine accounts for 3 / 20 of the ethyl lactate mass, and the mass ratio of polyetheramine to water is 1:5.

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