阅读说明：本技术 一种改性硅油柔软剂及其制备方法 (Modified silicone oil softening agent and preparation method thereof ) 是由 钟晓扬 陈耀武 王春正 徐杰 于 2020-08-08 设计创作，主要内容包括：本发明适用于纺织技术领域,提供了一种改性硅油柔软剂及其制备方法,该改性硅油柔软剂,包含A组分和B组分,其中,A组分为乙烯基硅油和含氢量为0.15％～0.2％的端基含氢硅油的混合物,B组分为氨基硅油、C<Sub>10</Sub>～C<Sub>20</Sub>的高级脂肪酸和蔗糖聚酯乳液的混合物。通过上述组分的科学复配得到改性硅油柔软剂,不仅具有优异的亲水性能、耐黄变性能,而且将该柔软剂应用于高档纺织物或浅色系列的纺织物后整理,可以赋予整理后的纺织物更加爽滑、亲肤的质感,并提升织物的耐洗性。(The invention is suitable for the technical field of spinning and provides a modified silicone oil softener and a preparation method thereof, wherein the modified silicone oil softener comprises a component A and a component B, wherein the component A is a mixture of vinyl silicone oil and terminal group hydrogen-containing silicone oil with the hydrogen content of 0.15-0.2%, and the component B is amino silicone oil and C 10 ～C 20 And a mixture of a higher fatty acid and a sucrose polyester emulsion. The modified silicone oil softening agent is obtained by scientific compounding of the components, has excellent hydrophilic performance and yellowing resistance, and is applied to high-grade textiles or light-color series textile fabric finishingAnd the finished textile fabric can be endowed with more smooth and skin-friendly texture, and the washability of the textile fabric is improved.)

1. The modified silicone oil softener is characterized by comprising a component A and a component B;

the component A comprises the following components in parts by weight: 80-100 parts of vinyl silicone oil and 50-80 parts of terminal group hydrogen-containing silicone oil with the hydrogen content of 0.15-0.2%;

the component B comprises: 90-110 parts of amino silicone oil and C₁₀～C₂₀11-15 parts of higher fatty acid and 12-23 parts of sucrose polyester emulsion.

2. The modified silicone oil softener according to claim 1, wherein the mixing mass ratio of the component A to the component B is 1: (1-2).

3. The modified silicone oil softener according to claim 1, wherein the terminal hydrogen-containing silicone oil having a hydrogen content of 0.15% to 0.2% is prepared by the following method:

weighing 250-300 parts by weight of octamethylcyclotetrasiloxane, placing in a container, slowly adding 7-10 parts by weight of concentrated sulfuric acid while stirring, heating to 50-55 ℃, reacting for 1-2 hours under heat preservation, adding 20-25 parts by weight of tetramethyldisiloxane into the container, and continuing to react for 5-6 hours to obtain a reaction solution;

standing and layering after the reaction liquid is cooled, and separating to obtain upper silicone oil;

and adjusting the pH value of the upper layer silicon oil to 5.5-6, stirring, standing and settling, filtering, and removing oligomers in the upper layer silicon oil under reduced pressure to obtain the clarified terminal group hydrogen-containing silicon oil with the hydrogen content of 0.15-0.2%.

4. The modified silicone oil softener of claim 1 wherein said sucrose polyester emulsion is prepared by the following method:

under the condition of constant temperature, uniformly stirring and mixing the composite emulsifier and the sucrose polyester to obtain an oil phase;

slowly adding deionized water into the oil phase while stirring, and stirring for 10-20 minutes at the rotating speed of 8000-10000 r/min to obtain the oil-in-water sucrose polyester emulsion.

5. The modified silicone oil softener according to claim 1 or 4, wherein said B component is prepared by the following steps:

mixing amino silicone oil with C₁₀～C₂₀Stirring the higher fatty acid at room temperature for 1.5-2 hours under the protection of inert gas to obtain a reaction product;

sequentially using polyether and deionized water to prepare an emulsion with the viscosity of 2000-3000 mPa & s from the reaction product;

and adding the sucrose polyester emulsion into the emulsion, and stirring and mixing uniformly to obtain the component B.

6. The modified silicone oil softener of claim 1 wherein C is₁₀～C₂₀The higher fatty acid of (b) is any one or more of undecanoic acid, lauric acid, oleic acid and stearic acid.

7. The modified silicone oil softener according to claim 1, wherein the mixing mass ratio of the vinyl silicone oil in the component A to the terminal group hydrogen-containing silicone oil with a hydrogen content of 0.15% to 0.2% is 5: 4.

8. The modified silicone oil softener according to claim 1, wherein the viscosity of said vinyl silicone oil is 9000 to 10000 mPas.

9. The modified silicone oil softener according to claim 1, wherein the mixing mass ratio of the component a to the component B is 1: 1.5.

10. The method for preparing the modified silicone oil softener according to any one of claims 1 to 9, comprising the steps of:

mixing the component A and the component B according to a mixing mass ratio of 1: (1-2) stirring and mixing, and homogenizing for 10-15 minutes at the rotating speed of 5000-8000 r/min to obtain the modified silicone oil softener.

Technical Field

The invention belongs to the technical field of spinning, and particularly relates to a modified silicone oil softening agent and a preparation method thereof.

Background

Softeners are chemical aids that impart a soft, smooth feel to fabrics. The fabric treated by the softening agent has an adsorption layer formed on the surface of the fiber, the dynamic and static friction coefficient of the fiber is reduced, the friction resistance among yarns is reduced, and the fabric becomes soft.

The organosilicon softener has the characteristics of high cost performance, good flexibility and the like, and is widely applied to the textile industry. However, the conventional silicone softener has poor performance in yellowing resistance and the like, thereby limiting the application of the silicone softener to high-grade textiles and light-colored fabrics.

Disclosure of Invention

The embodiment of the invention provides a modified silicone oil softener, aiming at solving the problem of poor yellowing resistance of the existing silicone softener.

The embodiment of the invention is realized in such a way that the modified silicone oil softener comprises a component A and a component B;

the component A comprises the following components in parts by weight: 80-100 parts of vinyl silicone oil and 50-80 parts of terminal group hydrogen-containing silicone oil with the hydrogen content of 0.15-0.2%; the component B comprises: 90-110 parts of amino silicone oil and C₁₀～C₂₀11-15 parts of higher fatty acid and 12-23 parts of sucrose polyester emulsion.

The embodiment of the invention also provides a preparation method of the modified silicone oil softener, which comprises the following steps:

mixing the component A and the component B according to a mixing mass ratio of 1: (1-2) stirring and mixing, and homogenizing for 10-15 minutes at the rotating speed of 5000-8000 r/min to obtain the modified silicone oil softener.

The modified silicone oil softener provided by the embodiment of the invention comprises a component A and a component B, wherein the component A is a mixture of vinyl silicone oil and terminal group hydrogen-containing silicone oil with the hydrogen content of 0.15-0.2%, and the component B is amino silicone oil and C₁₀～C₂₀And a mixture of a higher fatty acid and a sucrose polyester emulsion. Through scientific compounding of the componentsThe obtained modified silicone oil softening agent has excellent hydrophilic performance and yellowing resistance, and can be applied to the after-finishing of high-grade textiles or light-color series textiles, so that the finished textiles can have smooth and skin-friendly texture, and the washability of the textiles is improved.

Detailed Description

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

The modified silicone oil softener provided by the embodiment of the invention comprises a component A and a component B, wherein the component A is a mixture of vinyl silicone oil and terminal group hydrogen-containing silicone oil with the hydrogen content of 0.15-0.2%, and the component B is amino silicone oil and C₁₀～C₂₀And a mixture of a higher fatty acid and a sucrose polyester emulsion. The modified silicone oil softener is obtained by scientific compounding of the components, has excellent hydrophilic performance and yellowing resistance, and can be applied to the after-finishing of high-grade textiles or light-color series textiles, so that the finished textiles can be more smooth and skin-friendly, and the washability and resilience of the textiles are improved.

The embodiment of the invention provides a modified silicone oil softening agent which is characterized by comprising a component A and a component B; the component A comprises the following components in parts by weight: 80-100 parts of vinyl silicone oil and 50-80 parts of terminal group hydrogen-containing silicone oil with the hydrogen content of 0.15-0.2%; the component B comprises: 90-110 parts of amino silicone oil and C₁₀～C₂₀11-15 parts of higher fatty acid and 12-23 parts of sucrose polyester emulsion.

In the preferred embodiment of the invention, the vinyl silicone oil with the viscosity of 9000-10000 mPas is adopted, the vinyl content of the product is about 3.0 moL%, the volatile matter is low, no yellowing occurs, and the quality is very stable. The vinyl silicone oil used in the examples of the present invention is commercially available, for example, from Dow Corning, USA.

In the embodiment of the invention, the terminal group hydrogen-containing silicone oil with the hydrogen content of 0.15-0.2% is prepared by the following method:

step 101, weighing 250-300 parts by weight of octamethylcyclotetrasiloxane, placing the octamethylcyclotetrasiloxane in a container, slowly adding 7-10 parts by weight of concentrated sulfuric acid while stirring, heating to 50-55 ℃, reacting for 1-2 hours under heat preservation, adding 20-25 parts by weight of tetramethyldisiloxane in the container, and continuing to react for 5-6 hours to obtain a reaction solution.

In the embodiment of the invention, the concentrated sulfuric acid with the concentration of 98% is adopted. Octamethylcyclotetrasiloxane, tetramethyldisiloxane and the like are commercially available as raw materials, and octamethylcyclotetrasiloxane and tetramethyldisiloxane are available from Shanghai Dongti chemical import and export Co., Ltd; concentrated sulfuric acid was purchased from Guangzhou chemical reagent works.

And step 102, standing and layering after the reaction liquid is cooled, and separating to obtain upper silicone oil.

In the embodiment of the invention, the reaction solution can be placed at room temperature for slow cooling and placed still to be completely divided into an upper layer of a silicon oil layer and a lower layer of a sulfuric acid layer. The upper silicone oil layer was separated by a separatory funnel.

103, adjusting the pH value of the upper layer silicone oil to 5.5-6, stirring, standing for settling, filtering, and removing oligomers in the upper layer silicone oil under reduced pressure to obtain the clarified terminal group hydrogen-containing silicone oil with the hydrogen content of 0.15% -0.2%.

In the embodiment of the invention, the pH value of the upper layer silicon oil is adjusted to 5.5-6 by adopting anhydrous sodium carbonate.

Through a great deal of research, the modified silicone oil softener has excellent yellowing resistance and hydrophilic performance when the mixing mass ratio of the vinyl silicone oil in the component A to the terminal group hydrogen-containing silicone oil with the hydrogen content of 0.15-0.2% is (8-10) to (5-8). Most preferably, the mixing mass ratio of the vinyl silicone oil to the terminal group hydrogen-containing silicone oil with the hydrogen content of 0.15-0.2% is 5: 4.

In the embodiment of the invention, the sucrose polyester emulsion is prepared by the following method: under the condition of constant temperature, uniformly stirring and mixing the composite emulsifier and the sucrose polyester to obtain an oil phase; slowly adding deionized water into the oil phase while stirring, and stirring for 10-20 minutes at the rotating speed of 8000-10000 r/min to obtain the oil-in-water sucrose polyester emulsion.

The composite emulsifier is a mixture of glycerol stearate, fatty alcohol-polyoxyethylene ether and tween in a mass ratio of 2:5: 3. Sucrose polyester crude oil available from Procter & gamble is used.

By a phase inversion emulsification method, deionized water is added into an oil phase obtained by mixing a composite emulsifier and sucrose polyester under a constant temperature condition, so that the water-in-oil type emulsion is gradually converted into an oil-in-water type emulsion, and the oil-in-water type sucrose polyester emulsion with good hydrophilic property and good stability is obtained.

In the embodiment of the invention, the component B is prepared by the following steps:

step 201, amino silicone oil and C₁₀～C₂₀The higher fatty acid is stirred for 1.5 to 2 hours at room temperature under the protection of inert gas, and a reaction product is obtained.

In the embodiment of the invention, C₁₀～C₂₀The higher fatty acid of (b) is any one or more of undecanoic acid, lauric acid, oleic acid and stearic acid. Multiple experimental studies prove that C₂The following fatty acids are easily volatilized by heating at 150 ℃ and C₃～C₉The fatty acid(s) will cause the softening agent to impart a smoothness and reduced softening performance to the fabric, and therefore C is preferred in the present invention₁₀～C₂₀The higher fatty acid and the amino silicone oil are mixed to modify the amino silicone oil to obtain a reaction product. Preferred amino silicone oils with C₁₀～C₂₀The mixing mass ratio of the higher fatty acid(s) is 1: 0.5-1.

202, sequentially using polyether and deionized water to prepare the reaction product into an emulsion with the viscosity of 2000-3000 mPa & s.

In the embodiment of the invention, polyether is adopted to prepare a reaction product into a high-viscosity system, and deionized water is added to prepare the system into an emulsion with the viscosity of 2000-3000 mPa & s.

Step 203, adding the prepared sucrose polyester emulsion into the emulsion, and stirring and mixing uniformly to obtain the component B.

In the embodiment of the invention, the mixing mass ratio of the component A to the component B is 1: (1-2). More preferably, the mixing mass ratio of the component A to the component B is 1: 1.5. Test research shows that when the mixing mass ratio of the component A to the component B is 1: (1-2), the prepared compound modified silicone oil softener has excellent hydrophilicity and yellowing resistance, is applied to the after-finishing of high-grade textiles or light-color series textiles, can endow the finished textiles with smoother and skin-friendly texture, and improves the washability and rebound resilience of the textiles.

The embodiment of the invention also provides a preparation method of the modified silicone oil softener, which comprises the following steps:

mixing the component A and the component B according to a mixing mass ratio of 1: (1-2) stirring and mixing, and homogenizing for 10-15 minutes at the rotating speed of 5000-8000 r/min to obtain the modified silicone oil softener.

Examples of certain embodiments of the invention are given below, which are not intended to limit the scope of the invention.

In addition, it should be noted that the numerical values given in the following examples are as precise as possible, but those skilled in the art will understand that each numerical value should be understood as a divisor rather than an absolutely exact numerical value due to measurement errors and experimental operational problems that cannot be avoided. For example, with respect to the weight values of the components in the modified silicone oil softener of each example, it should be understood that it may have an error of ± 2% or ± 1%, due to an error of a weighing instrument.