阅读说明：本技术 一种水性仿涂层高弹挺括整理剂及制备方法 (Waterborne imitation coating high-elasticity stiff and smooth finishing agent and preparation method thereof ) 是由 荣星 陈龙 唐丽 陈剑冰 孙海娥 盛艳霞 于 2020-12-10 设计创作，主要内容包括：本发明公开了一种水性仿涂层高弹挺括整理剂及制备方法,涉及纺织面料后整理技术领域,所述整理剂由如下重量份数的原料制备而成：乳液A 50-60份、乳液B 100-120份、阳离子型封端异氰酸酯交联剂5-10份。一种水性仿涂层高弹挺括整理剂的制备方法通过高摩尔质量的环氧改性聚有机硅氧烷乳液A,由氨基聚醚改性聚有机硅氧烷与聚硅酸乙酯交联剂制备成的乳液B与封端异氰酸酯交联剂的合理复配,对面料进行浸轧整理,可以使面料的弹性及挺括性明显提升,达到涂层工艺的效果。得到的整理剂柔软性好、抗皱效果佳、耐洗性能优异,且水性环保,可以满足出口环保要求。(The invention discloses a waterborne imitation coating high-elastic stiff and smooth finishing agent and a preparation method thereof, and relates to the technical field of textile fabric after-finishing, wherein the finishing agent is prepared from the following raw materials in parts by weight: 50-60 parts of emulsion A, 120 parts of emulsion B100-120 parts and 5-10 parts of cationic blocked isocyanate crosslinking agent. According to the preparation method of the waterborne imitation coating high-elasticity stiff and smooth finishing agent, the epoxy modified polysiloxane emulsion A with high molar mass, the emulsion B prepared from the amino polyether modified polysiloxane and the ethyl polysilicate crosslinking agent and the blocked isocyanate crosslinking agent are reasonably compounded to perform padding finishing on the fabric, so that the elasticity and the stiff and smooth performance of the fabric can be obviously improved, and the effect of a coating process is achieved. The obtained finishing agent has good softness, good crease-resistant effect, excellent washing resistance and water-based environmental protection, and can meet the export environmental protection requirement.)

1. The water-based imitation coating high-elasticity stiff and smooth finishing agent is characterized by being prepared from the following raw materials in parts by weight: 50-60 parts of emulsion A, 120 parts of emulsion B100 and 5-10 parts of cationic blocked isocyanate crosslinking agent;

the emulsion A is prepared from the following raw materials in parts by weight: 150 parts of octamethylcyclotetrasiloxane 100-one, 3-7 parts of silane coupling agent, 3-6 parts of quaternary ammonium type cationic surfactant, 101-2 parts of peregal O-101, 0.1-0.15 part of potassium hydroxide and 350 parts of deionized water 220-one;

the emulsion B is prepared from the following raw materials in parts by weight: 150 parts of double-end epoxy silicone oil 100-containing materials, 3-10 parts of polyetheramine, 25-40 parts of ethylene glycol monobutyl ether, 21-40 parts of isomeric tridecanol polyoxyethylene ether, 401-2 parts of poly ethyl silicate, 1-2 parts of glacial acetic acid and 430 parts of softened water 254-containing materials.

2. The finishing agent of claim 1, wherein the silane coupling agent is an epoxy-containing silane coupling agent; the epoxy-containing silane coupling agent is one of gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, beta- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane and beta- (3, 4-epoxycyclohexyl) ethyltriethoxysilane.

3. The finish of claim 1, wherein the quaternary cationic surfactant is cetyltrimethylammonium chloride or octadecyltrimethylammonium chloride.

4. The finishing agent according to claim 1, wherein the number average molecular weight of the double-ended epoxy silicone oil is 8000-10000; the double-end epoxy silicone oil is selected from one of 622V150 and 622V300 products of Jiangxi Star fire organic silicon company Limited.

5. The finish of claim 1, wherein the polyetheramine has a number average molecular weight of 200-400; the polyether amine is selected from one of Henschel Melamine products D-230 and ED-410.

6. The finish of claim 1, wherein the isomeric tridecanol polyoxyethylene ether is one or both of isomeric tridecanol polyoxyethylene (5) ether, isomeric tridecanol polyoxyethylene (7) ether, and isomeric tridecanol polyoxyethylene (9) ether.

7. The finish of claim 1, wherein the cationic blocked isocyanate crosslinker is selected from Y-203B, a product of addia chemical limited.

8. The finish of claim 1, wherein the finish has technical specifications of: appearance: white emulsion, solid content: 30 plus or minus 2%, pH value: 7 ± 1, ionic: yang.

9. A process for the preparation of a finish according to any of claims 1 to 8, characterized in that it comprises the following steps:

s1: fully and uniformly stirring 100-150 parts of octamethylcyclotetrasiloxane, 3-7 parts of silane coupling agent containing epoxy group, 3-6 parts of quaternary ammonium cationic surfactant, 1-2 parts of peregal O-10 and 220-350 parts of deionized water, preparing the obtained mixed solution into emulsion once or twice in a high-pressure homogenizer, adding the emulsion into a reactor provided with a condenser and a stirring device, adding 0.1-0.15 part of potassium hydroxide, reacting at 80-85 ℃ for 5-6 hours, reducing the temperature to room temperature within 3 hours, and neutralizing the pH value of the emulsion to 6 by using glacial acetic acid with the concentration of more than 99% to obtain emulsion A;

s2: adding 100-150 parts of double-end epoxy silicone oil, 3-10 parts of polyether amine and 25-40 parts of ethylene glycol monobutyl ether into a closed reaction kettle with a reflux and cooling device, heating to 112 ℃ within 2 hours under the stirring condition, and carrying out reflux and heat preservation within the temperature range for 5-6 hours to carry out copolymerization reaction to obtain amino polyether modified polysiloxane;

s3: putting the amino polyether modified polyorganosiloxane obtained in the step S2 into an emulsifying kettle, cooling to room temperature, adding 21-40 parts of isomeric tridecanol polyoxyethylene ether, 1-2 parts of ethyl polysilicate 40 and 1-2 parts of glacial acetic acid, slowly adding 430 parts of softened water 254-containing chitosan for several times, stirring and emulsifying to obtain emulsion B;

s4: and (2) mixing and uniformly stirring 50-60 parts of emulsion A, 100-120 parts of emulsion B and 5-10 parts of cationic blocked isocyanate crosslinking agent to obtain the finishing agent.

10. The method of claim 9, wherein the high pressure homogenizer at step S1 has an operating pressure of 30 Mpa.

Technical Field

The invention relates to the technical field of textile fabric after-finishing, in particular to a water-based imitation coating high-elasticity stiff and smooth finishing agent and a preparation method thereof.

Background

The high-elasticity stiff and smooth finishing agent of the fabric on the market at present is mostly finished by solvent type organic silicon high-elasticity coating glue, and is very popular with customers due to the unique hand feeling style of excellent high elasticity, stiffness and smoothness. But the defects that the special hand feeling and style of the coated fabric are seriously reduced after the coated fabric is washed by water, 70-80 percent of the solvent glue is solvent toluene, and the toluene is baked away after the coating, so that the resource waste is caused, the environment is polluted, and if the operation is improper, fire or explosion is easy to occur, so that the loss of personnel and property is caused.

The patent publication No. CN102926212A discloses a water-based high-elasticity coating adhesive for cotton and linen fabrics and a preparation method thereof. The coating adhesive is composed of high-molar-mass modified polysiloxane, polyurethane resin, a cross-linking agent and a catalyst, and the fabric is finished by a coating method, so that the coated cotton and linen fabric has high resilience and wrinkle resistance.

Disclosure of Invention

Therefore, the invention provides a waterborne imitation coating high-elasticity stiff and smooth finishing agent and a preparation method thereof, and aims to solve the problems that the coated fabric is seriously reduced in unique hand feeling and style after being washed, is not environment-friendly, is limited in application range and the like in the high-elasticity stiff and smooth finishing agent in the existing market.

In order to achieve the above purpose, the invention provides the following technical scheme:

according to the first aspect of the invention, the waterborne imitation coating high-elasticity stiff and smooth finishing agent is prepared from the following raw materials in parts by weight: 50-60 parts of emulsion A, 120 parts of emulsion B100 and 5-10 parts of cationic blocked isocyanate crosslinking agent;

the emulsion A is prepared from the following raw materials in parts by weight: 150 parts of octamethylcyclotetrasiloxane 100-one, 3-7 parts of silane coupling agent, 3-6 parts of quaternary ammonium type cationic surfactant, 101-2 parts of peregal O-101, 0.1-0.15 part of potassium hydroxide and 350 parts of deionized water 220-one;

the emulsion B is prepared from the following raw materials in parts by weight: 150 parts of double-end epoxy silicone oil 100-containing materials, 3-10 parts of polyetheramine, 25-40 parts of ethylene glycol monobutyl ether, 21-40 parts of isomeric tridecanol polyoxyethylene ether, 401-2 parts of poly ethyl silicate, 1-2 parts of glacial acetic acid and 430 parts of softened water 254-containing materials.

Further, the silane coupling agent is a silane coupling agent containing an epoxy group; the epoxy-containing silane coupling agent is one of gamma-glycidoxypropyltrimethoxysilane, gamma-glycidoxypropyltriethoxysilane, beta- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane and beta- (3, 4-epoxycyclohexyl) ethyltriethoxysilane.

Further, the quaternary ammonium type cationic surfactant is hexadecyl trimethyl ammonium chloride or octadecyl trimethyl ammonium chloride.

Further, the number average molecular weight of the double-end epoxy silicone oil is 8000-; the double-end epoxy silicone oil is selected from one of 622V150 and 622V300 products of Jiangxi Star fire organic silicon company Limited.

Further, the number average molecular weight of the polyetheramine is 200-400; the polyether amine is selected from one of Henschel Melamine products D-230 and ED-410.

Further, the isomeric tridecanol polyoxyethylene ether is one or two of isomeric tridecanol polyoxyethylene (5) ether, isomeric tridecanol polyoxyethylene (7) ether and isomeric tridecanol polyoxyethylene (9) ether.

Further, the cationic blocked isocyanate crosslinking agent is selected from Y-203B which is a product of Adia chemical industry Co.

Further, the technical indexes of the finishing agent are as follows: appearance: white emulsion, solid content: 30 plus or minus 2%, pH value: 7 ± 1, ionic: yang.

According to a second aspect of the present invention, the above-mentioned method for preparing a finishing agent comprises the steps of:

s1: fully and uniformly stirring 100-150 parts of octamethylcyclotetrasiloxane, 3-7 parts of silane coupling agent containing epoxy group, 3-6 parts of quaternary ammonium cationic surfactant, 1-2 parts of peregal O-10 and 220-350 parts of deionized water, preparing the obtained mixed solution into emulsion once or twice in a high-pressure homogenizer, adding the emulsion into a reactor provided with a condenser and a stirring device, adding 0.1-0.15 part of potassium hydroxide, reacting at 80-85 ℃ for 5-6 hours, reducing the temperature to room temperature within 3 hours, and neutralizing the pH value of the emulsion to 6 by using glacial acetic acid with the concentration of more than 99% to obtain emulsion A;

s2: adding 100-150 parts of double-end epoxy silicone oil, 3-10 parts of polyether amine and 25-40 parts of ethylene glycol monobutyl ether into a closed reaction kettle with a reflux and cooling device, heating to 112 ℃ within 2 hours under the stirring condition, and carrying out reflux and heat preservation within the temperature range for 5-6 hours to carry out copolymerization reaction to obtain amino polyether modified polysiloxane;

s3: putting the amino polyether modified polyorganosiloxane obtained in the step S2 into an emulsifying kettle, cooling to room temperature, adding 21-40 parts of isomeric tridecanol polyoxyethylene ether, 1-2 parts of ethyl polysilicate 40 and 1-2 parts of glacial acetic acid, slowly adding 430 parts of softened water 254-containing chitosan for several times, stirring and emulsifying to obtain emulsion B;

s4: and (2) mixing and uniformly stirring 50-60 parts of emulsion A, 100-120 parts of emulsion B and 5-10 parts of cationic blocked isocyanate crosslinking agent to obtain the finishing agent.

Further, in step S1, the working pressure of the high pressure homogenizer is 30 MPa.

The invention has the following advantages:

the preparation method of the waterborne imitation coating high-elasticity stiff and smooth finishing agent adopts a special emulsion polymerization method, and the trialkoxysilane coupling agent containing epoxy groups reacts with an organic silicon intermediate to prepare the epoxy modified polysiloxane with high molar mass, the polysiloxane structure on the main chain of the epoxy modified polysiloxane can enable the fabric to generate smooth hand feeling, the alkoxy groups, the epoxy groups and the hydroxyl groups introduced on the side chain are active groups, and under the heating condition, the active groups contained in different molecular chains can react with each other to form a reticular crosslinking system, so that the self-crosslinking performance of the product is improved, and the elasticity and the wrinkle resistance of the finished fabric are effectively improved.

The invention relates to a preparation method of a water-based imitation coating high-elasticity stiff and smooth finishing agent, which simultaneously adopts a bulk polymerization method to synthesize amino polyether modified polysiloxane, in the structure, amino and polyether groups are uniformly distributed on the main chain of polymer molecules, the existence of the polyether groups enables methyl groups on the main chain of the molecules to be irregularly spaced, the methyl groups are not regularly arranged on the surface of a fabric, the smoothness of the fabric is reduced, the bulkiness and the stiff and smooth performance are improved, the amino groups are at the ends of the molecular chains and have small steric hindrance, and the amino groups can be easily subjected to ring-opening reaction with epoxy groups in a mixed epoxy modified polysiloxane structure under the heating condition to form a more three-dimensional crosslinked film, so that the elasticity of the finished fabric is further improved.

According to the preparation method of the water-based imitation coating high-elasticity stiff and smooth finishing agent, the polyethyl silicate is added in the emulsification process, the polyethyl silicate is a cross-linking agent of the amino silicone oil, and the amino polyether modified polysiloxane is also one of the amino silicone oil. On one hand, ethoxy in the poly (ethyl silicate) can react with amino in molecules to further solidify into a net-shaped structure film to increase elasticity, and on the other hand, the ethoxy can also react with hydroxyl or amino on fibers to form chemical bonding, so that an auxiliary effect is achieved on the washing durability of the finished fabric.

According to the preparation method of the water-based imitation coating high-elasticity stiff and smooth finishing agent, the cationic blocked isocyanate crosslinking agent is added in the preparation process, and the NCO group which is deblocked under the heating condition can react with the hydroxyl and the amino on the modified polysiloxane molecule to form crosslinking, and can also react with the hydroxyl and the amino on the natural fiber fabric and the carboxyl and the amido on the synthetic fiber fabric to generate crosslinking reaction, so that the adhesive force of the modified polysiloxane on the fabric is remarkably improved, and the washing durability of the finished fabric is improved.

In conclusion, the elasticity and the stiffness of the fabric can be obviously improved by padding and finishing the fabric through reasonable compounding of the epoxy modified polysiloxane, the amino polyether modified polysiloxane, the polyethyl silicate cross-linking agent and the blocked isocyanate cross-linking agent with high molar mass, so that the effect of the coating process is achieved. The obtained finishing agent has good softness, good crease-resistant effect, excellent washing resistance and water-based environmental protection, and can meet the export environmental protection requirement.

Detailed Description

The present invention is described in terms of particular embodiments, other advantages and features of the invention will become apparent to those skilled in the art from the following disclosure, and it is to be understood that the described embodiments are merely exemplary of the invention and that it is not intended to limit the invention to the particular embodiments disclosed. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1

The water-based imitation coating high-elasticity stiff and smooth finishing agent is prepared from the following raw materials in parts by weight: 50 parts of emulsion A, 100 parts of emulsion B and 5 parts of cationic blocked isocyanate crosslinking agent; the cationic blocked isocyanate crosslinking agent is selected from Y-203B which is a product of Adia chemical company Limited.

The emulsion A is prepared from the following raw materials in parts by weight: 100 parts of octamethylcyclotetrasiloxane, 3 parts of silane coupling agent, 3 parts of quaternary ammonium cationic surfactant, 0.1 part of peregal O-101, 0.1 part of potassium hydroxide and 220 parts of deionized water; the silane coupling agent is gamma-glycidoxypropyltrimethoxysilane; the quaternary ammonium type cationic surfactant is hexadecyl trimethyl ammonium chloride.

The emulsion B is prepared from the following raw materials in parts by weight: 100 parts of epoxy-terminated silicone oil, 3.2 parts of polyether amine, 25 parts of ethylene glycol monobutyl ether, 21 parts of isomeric tridecanol polyoxyethylene ether, 401 parts of polyethyl silicate, 1 part of glacial acetic acid and 290 parts of softened water. The number average molecular weight of the double-end epoxy silicone oil is 8000, and the double-end epoxy silicone oil is selected from 622V150 which is a product of Jiangxi Star fire organosilicon Limited company; the number average molecular weight of the polyether amine is 200, and the polyether amine is selected from a Henschel Melamine product D-230; the isomeric tridecanol polyoxyethylene ether is isomeric tridecanol polyoxyethylene (7) ether.

The preparation method of the finishing agent comprises the following steps:

s1: fully and uniformly stirring 100 parts of octamethylcyclotetrasiloxane, 3 parts of gamma-glycidoxypropyltrimethoxysilane, 3 parts of hexadecyltrimethylammonium chloride, 1 part of peregal O-10 and 220 parts of deionized water, enabling the obtained mixed solution to pass through a 30Mpa high-pressure homogenizer to prepare emulsion, adding the emulsion into a reactor provided with a condenser and a stirring device, adding 0.1 part of potassium hydroxide, reacting at 80 ℃ for 6 hours, cooling to room temperature within 3 hours, and neutralizing with more than 99% of glacial acetic acid until the pH value of the emulsion is 6 to obtain emulsion A (epoxy modified polyorganosiloxane emulsion);

s2: adding 100 parts of double-end epoxy silicone oil, 3.2 parts of polyether amine and 25 parts of ethylene glycol monobutyl ether into a closed reaction kettle with a reflux and cooling device, heating to 112 ℃ within 2 hours under the stirring condition, and carrying out reflux and heat preservation within the temperature range for 5 hours to carry out copolymerization reaction to obtain amino polyether modified polysiloxane;

s3: putting the amino polyether modified polyorganosiloxane obtained in the step S2 into an emulsifying kettle, cooling to room temperature, adding 21 parts of isomeric tridecanol polyoxyethylene (7) ether, 1 part of ethyl polysilicate 40 and 1 part of glacial acetic acid, slowly adding 290 parts of softened water in portions, stirring and emulsifying to obtain emulsion B;

s4: and mixing and stirring uniformly 50 parts of emulsion A, 100 parts of emulsion B and 5 parts of cationic blocked isocyanate crosslinking agent to obtain the finishing agent.

The technical indexes of the finishing agent are as follows: appearance: white emulsion, solid content: 29.8%, pH: 7.0, ionic: yang.

Example 2

The water-based imitation coating high-elasticity stiff and smooth finishing agent is prepared from the following raw materials in parts by weight: 60 parts of emulsion A, 100 parts of emulsion B and 8 parts of cationic blocked isocyanate crosslinking agent; the cationic blocked isocyanate crosslinking agent is selected from Y-203B which is a product of Adia chemical company Limited.

The emulsion A is prepared from the following raw materials in parts by weight: 120 parts of octamethylcyclotetrasiloxane, 5 parts of silane coupling agent, 5 parts of quaternary ammonium cationic surfactant, 0.12 part of peregal O-101, 0.12 part of potassium hydroxide and 300 parts of deionized water; the silane coupling agent is gamma-glycidoxypropyltriethoxysilane; the quaternary ammonium type cationic surfactant is octadecyl trimethyl ammonium chloride.

The emulsion B is prepared from the following raw materials in parts by weight: 150 parts of epoxy-terminated silicone oil, 9 parts of polyether amine, 40 parts of ethylene glycol monobutyl ether, 40 parts of isomeric tridecanol polyoxyethylene ether, 402 parts of poly ethyl silicate, 2 parts of glacial acetic acid and 430 parts of softened water. The number average molecular weight of the double-end epoxy silicone oil is 8000, and the double-end epoxy silicone oil is selected from 622V150 which is a product of Jiangxi Star fire organosilicon Limited company; the number average molecular weight of the polyether amine is 400, and the polyether amine is selected from a Henschel Michael polyether amine product ED-410; the isomeric tridecanol polyoxyethylene ether is isomeric tridecanol polyoxyethylene (5) ether and isomeric tridecanol polyoxyethylene (7) ether.

The preparation method of the finishing agent comprises the following steps:

s1: fully and uniformly stirring 120 parts of octamethylcyclotetrasiloxane, 5 parts of gamma-glycidoxypropyltriethoxysilane, 5 parts of octadecyl trimethyl ammonium chloride, 1 part of peregal O-10 and 300 parts of deionized water, preparing the mixed solution into emulsion twice in a high-pressure homogenizer of 30Mpa, adding the emulsion into a reactor provided with a condenser and a stirring device, adding 0.12 part of potassium hydroxide, reacting at 85 ℃ for 5 hours, cooling to room temperature within 3 hours, and neutralizing with more than 99% of glacial acetic acid until the pH value of the emulsion is 6 to obtain emulsion A (epoxy modified polyorganosiloxane emulsion);

s2: adding 150 parts of double-end epoxy silicone oil, 9 parts of polyether amine and 40 parts of ethylene glycol monobutyl ether into a closed reaction kettle with a reflux and cooling device, heating to 110-112 ℃ within 2 hours under the stirring condition, carrying out reflux and heat preservation within the temperature range for 6 hours, and carrying out copolymerization reaction to obtain amino polyether modified polysiloxane;

s3: putting the amino polyether modified polyorganosiloxane obtained in the step S2 into an emulsifying kettle, cooling to room temperature, adding 20 parts of isomeric tridecanol polyoxyethylene (5) ether, 20 parts of isomeric tridecanol polyoxyethylene (7) ether, 2 parts of polyethyl silicate 40 and 2 parts of glacial acetic acid, slowly adding 430 parts of softened water in portions, stirring and emulsifying to obtain emulsion B;

s4: and mixing and stirring 60 parts of emulsion A, 100 parts of emulsion B and 8 parts of cationic blocked isocyanate crosslinking agent uniformly to obtain the finishing agent.

The technical indexes of the finishing agent are as follows: appearance: white emulsion, solid content: 30.1%, pH: 6.5, ionic: yang.

Example 3

The water-based imitation coating high-elasticity stiff and smooth finishing agent is prepared from the following raw materials in parts by weight: 50 parts of emulsion A, 120 parts of emulsion B and 10 parts of cationic blocked isocyanate crosslinking agent; the cationic blocked isocyanate crosslinking agent is selected from Y-203B which is a product of Adia chemical company Limited.

The emulsion A is prepared from the following raw materials in parts by weight: 150 parts of octamethylcyclotetrasiloxane, 5 parts of silane coupling agent, 5 parts of quaternary ammonium cationic surfactant, 0.15 part of peregal O-102 part, 0.15 part of potassium hydroxide and 350 parts of deionized water; the silane coupling agent is beta- (3, 4-epoxy cyclohexyl) ethyl trimethoxy silane; the quaternary ammonium type cationic surfactant is octadecyl trimethyl ammonium chloride.

The emulsion B is prepared from the following raw materials in parts by weight: 150 parts of epoxy-terminated silicone oil, 7.2 parts of polyether amine, 38 parts of ethylene glycol monobutyl ether, 26 parts of isomeric tridecanol polyoxyethylene ether, 402 parts of polyethyl silicate, 1.5 parts of glacial acetic acid and 390 parts of softened water. The number average molecular weight of the double-end epoxy silicone oil is 10000, and the double-end epoxy silicone oil is selected from 622V300 which is a product of Jiangxi Star fire organosilicon Limited company; the number average molecular weight of the polyether amine is 400, and the polyether amine is selected from a Henschel Michael polyether amine product ED-410; the isomeric tridecanol polyoxyethylene ether is isomeric tridecanol polyoxyethylene (5) ether and isomeric tridecanol polyoxyethylene (9) ether.

The preparation method of the finishing agent comprises the following steps:

s1: 150 parts of octamethylcyclotetrasiloxane, 6 parts of beta- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, 5 parts of octadecyl trimethyl ammonium chloride, 2 parts of peregal O-10 and 350 parts of deionized water are fully and uniformly stirred, the mixed solution is made into emulsion once in a high-pressure homogenizer of 30Mpa, then the emulsion is added into a reactor provided with a condenser and a stirring device, 0.15 part of potassium hydroxide is added, the reaction is carried out for 6 hours at 85 ℃, the temperature is reduced to room temperature within 3 hours, and then more than 99 percent of glacial acetic acid is used for neutralizing the pH value of the emulsion to be 6, thus obtaining emulsion A (epoxy modified polyorganosiloxane emulsion);

s2: adding 150 parts of double-end epoxy silicone oil with the average molecular weight of 10000, 7.2 parts of polyether amine with the average molecular weight of 400 and 38 parts of ethylene glycol monobutyl ether into a closed reaction kettle with a reflux and cooling device, heating to 110-112 ℃ within 2 hours under the stirring condition, carrying out reflux and heat preservation within the temperature range for 6 hours, and carrying out copolymerization reaction to obtain amino polyether modified polysiloxane;

s3: putting the amino polyether modified polyorganosiloxane obtained in the step S2 into an emulsifying kettle, cooling to room temperature, adding 20 parts of isomeric tridecanol polyoxyethylene (5) ether, 6 parts of isomeric tridecanol polyoxyethylene (9) ether, 2 parts of polyethyl silicate 40 and 1.5 parts of glacial acetic acid, slowly adding 390 parts of softened water in portions, stirring and emulsifying to obtain emulsion B;

s4: and mixing and stirring uniformly 50 parts of emulsion A, 120 parts of emulsion B and 10 parts of cationic blocked isocyanate crosslinking agent to obtain the finishing agent.

The technical indexes of the finishing agent are as follows: appearance: white emulsion, solid content: 30.6%, pH: 7.0 Ionic Properties: yang.

Example 4

The water-based imitation coating high-elasticity stiff and smooth finishing agent is prepared from the following raw materials in parts by weight: 55 parts of emulsion A, 120 parts of emulsion B and 7 parts of cationic blocked isocyanate crosslinking agent; the cationic blocked isocyanate crosslinking agent is selected from Y-203B which is a product of Adia chemical company Limited.

The emulsion A is prepared from the following raw materials in parts by weight: 150 parts of octamethylcyclotetrasiloxane, 4 parts of silane coupling agent, 5 parts of quaternary ammonium cationic surfactant, 0.15 part of peregal O-101, 0.15 part of potassium hydroxide and 350 parts of deionized water; the silane coupling agent is gamma-glycidoxypropyltriethoxysilane; the quaternary ammonium type cationic surfactant is hexadecyl trimethyl ammonium chloride.

The emulsion B is prepared from the following raw materials in parts by weight: 120 parts of epoxy-terminated silicone oil, 3.2 parts of polyether amine, 30 parts of ethylene glycol monobutyl ether, 30 parts of isomeric tridecanol polyoxyethylene ether, 401 parts of poly ethyl silicate, 1 part of glacial acetic acid and 325 parts of softened water. The number average molecular weight of the double-end epoxy silicone oil is 10000, and the double-end epoxy silicone oil is selected from 622V300 which is a product of Jiangxi Star fire organosilicon Limited company; the number average molecular weight of the polyether amine is 200, and the polyether amine is selected from a Henschel Melamine product D-230; the isomeric tridecanol polyoxyethylene ether is isomeric tridecanol polyoxyethylene (7) ether and isomeric tridecanol polyoxyethylene (9) ether.

The preparation method of the finishing agent comprises the following steps:

s1: fully and uniformly stirring 150 parts of octamethylcyclotetrasiloxane, 4 parts of gamma-glycidoxypropyltriethoxysilane, 5 parts of hexadecyltrimethylammonium chloride, 1 part of peregal O-10 and 350 parts of deionized water, making the mixed solution into emulsion once in a 30Mpa high-pressure homogenizer, adding the emulsion into a reactor provided with a condenser and a stirring device, adding 0.15 part of potassium hydroxide, reacting at 80 ℃ for 5 hours, cooling to room temperature within 3 hours, and neutralizing with more than 99% of glacial acetic acid until the pH value of the emulsion is 6 to obtain emulsion A (epoxy modified polyorganosiloxane emulsion);

s2: adding 120 parts of double-end epoxy silicone oil with the average molecular weight of 10000, 3.2 parts of polyether amine with the average molecular weight of 200 and 30 parts of ethylene glycol monobutyl ether into a closed reaction kettle with a reflux and cooling device, heating to 110-112 ℃ within 2 hours under the stirring condition, carrying out reflux and heat preservation within the temperature range for 5 hours, and carrying out copolymerization reaction to obtain amino polyether modified polysiloxane;

s3: putting the amino polyether modified polyorganosiloxane obtained in the step S2 into an emulsifying kettle, cooling to room temperature, adding 20 parts of isomeric tridecanol polyoxyethylene (7) ether, 10 parts of isomeric tridecanol polyoxyethylene (9) ether, 1 part of polyethyl silicate 40 and 1 part of glacial acetic acid, slowly adding 325 parts of softened water in portions, stirring and emulsifying to obtain emulsion B;

s5: and mixing and stirring 55 parts of emulsion A, 120 parts of emulsion B and 7 parts of cationic blocked isocyanate crosslinking agent uniformly to obtain the finishing agent.

The technical indexes of the finishing agent are as follows: appearance: white emulsion, solid content: 30.5%, pH: 7.5, ionic property: yang.

Example 5

The water-based imitation coating high-elasticity stiff and smooth finishing agent is prepared from the following raw materials in parts by weight: 60 parts of emulsion A, 105 parts of emulsion B and 6 parts of cationic blocked isocyanate crosslinking agent; the cationic blocked isocyanate crosslinking agent is selected from Y-203B which is a product of Adia chemical company Limited.

The emulsion A is prepared from the following raw materials in parts by weight: 140 parts of octamethylcyclotetrasiloxane, 6 parts of silane coupling agent, 3 parts of quaternary ammonium cationic surfactant, 0.15 part of peregal O-102, 0.15 part of potassium hydroxide and 320 parts of deionized water; the silane coupling agent is beta- (3, 4-epoxy cyclohexyl) ethyl triethoxysilane; the quaternary ammonium type cationic surfactant is octadecyl trimethyl ammonium chloride.

The emulsion B is prepared from the following raw materials in parts by weight: 120 parts of epoxy-terminated silicone oil, 7.5 parts of polyether amine, 31 parts of ethylene glycol monobutyl ether, 25 parts of isomeric tridecanol polyoxyethylene ether, 401 parts of polyethyl silicate, 2 parts of glacial acetic acid and 293 parts of softened water. The number average molecular weight of the double-end epoxy silicone oil is 8000, and the double-end epoxy silicone oil is selected from 622V150 which is a product of Jiangxi Star fire organosilicon Limited company; the number average molecular weight of the polyether amine is 400, and the polyether amine is selected from a Henschel Michael polyether amine product ED-410; the isomeric tridecanol polyoxyethylene ether is isomeric tridecanol polyoxyethylene (5) ether and isomeric tridecanol polyoxyethylene (7) ether.

The preparation method of the finishing agent comprises the following steps:

s1: fully and uniformly stirring 140 parts of octamethylcyclotetrasiloxane, 6 parts of beta- (3, 4-epoxycyclohexyl) ethyltriethoxysilane, 3 parts of octadecyl trimethyl ammonium chloride, 2 parts of peregal O-10 and 320 parts of deionized water, making the mixed solution into emulsion once in a high-pressure homogenizer of 30Mpa, adding the emulsion into a reactor provided with a condenser and a stirring device, adding 0.15 part of potassium hydroxide, reacting at 85 ℃ for 6 hours, cooling to room temperature within 3 hours, and neutralizing with glacial acetic acid of more than 99% until the pH value of the emulsion is 6 to obtain emulsion A (epoxy modified polyorganosiloxane emulsion);

s2: adding 120 parts of double-end epoxy silicone oil with the average molecular weight of 8000, 7.5 parts of polyether amine with the average molecular weight of 400 and 31 parts of ethylene glycol monobutyl ether into a closed reaction kettle with a reflux and cooling device, heating to 110-112 ℃ within 2 hours under the stirring condition, carrying out reflux and heat preservation within the temperature range for 6 hours, and carrying out copolymerization reaction to obtain amino polyether modified polysiloxane;

s3: putting the amino polyether modified polyorganosiloxane obtained in the step S2 into an emulsifying kettle, cooling to room temperature, adding 10 parts of isomeric tridecanol polyoxyethylene (5) ether, 15 parts of isomeric tridecanol polyoxyethylene (7) ether, 1 part of polyethyl silicate 40 and 2 parts of glacial acetic acid, slowly adding 293 parts of softened water in portions, stirring and emulsifying to obtain emulsion B;

s4: and mixing and stirring 60 parts of emulsion A, 105 parts of emulsion B and 6 parts of cationic blocked isocyanate crosslinking agent uniformly to obtain the finishing agent.

The technical indexes of the finishing agent are as follows: appearance: white emulsion, solid content: 31.9%, pH: 7.0, ionic: yang.

Example 6

The water-based imitation coating high-elasticity stiff and smooth finishing agent is prepared from the following raw materials in parts by weight: 50 parts of emulsion A, 115 parts of emulsion B and 7 parts of cationic blocked isocyanate crosslinking agent; the cationic blocked isocyanate crosslinking agent is selected from Y-203B which is a product of Adia chemical company Limited.

The emulsion A is prepared from the following raw materials in parts by weight: 130 parts of octamethylcyclotetrasiloxane, 5.2 parts of silane coupling agent, 4 parts of quaternary ammonium cationic surfactant, 102 parts of peregal O-L, 0.13 part of potassium hydroxide and 300 parts of deionized water; the silane coupling agent is gamma-glycidoxypropyltriethoxysilane; the quaternary ammonium type cationic surfactant is hexadecyl trimethyl ammonium chloride.

The emulsion B is prepared from the following raw materials in parts by weight: 100 parts of epoxy-terminated silicone oil, 3 parts of polyether amine, 28 parts of ethylene glycol monobutyl ether, 28 parts of isomeric tridecanol polyoxyethylene ether, 401 parts of poly ethyl silicate, 1.5 parts of glacial acetic acid and 271 parts of softened water. The number average molecular weight of the double-end epoxy silicone oil is 10000, and the double-end epoxy silicone oil is selected from 622V300 which is a product of Jiangxi Star fire organosilicon Limited company; the number average molecular weight of the polyether amine is 400, and the polyether amine is selected from a Henschel Michael polyether amine product ED-410; the isomeric tridecanol polyoxyethylene ether is isomeric tridecanol polyoxyethylene (7) ether.

The preparation method of the finishing agent comprises the following steps:

s1: fully and uniformly stirring 130 parts of octamethylcyclotetrasiloxane, 5.2 parts of gamma-glycidoxypropyltriethoxysilane, 4 parts of hexadecyltrimethylammonium chloride, 2 parts of peregal O-10 and 300 parts of deionized water, making the mixed solution into emulsion once in a 30Mpa high-pressure homogenizer, adding the emulsion into a reactor provided with a condenser and a stirring device, adding 0.13 part of potassium hydroxide, reacting at 80 ℃ for 5.5 hours, cooling to room temperature within 3 hours, and neutralizing with more than 99% of glacial acetic acid until the pH value of the emulsion is 6 to obtain emulsion A (epoxy modified polyorganosiloxane emulsion);

s2: adding 110 parts of double-end epoxy silicone oil with the average molecular weight of 10000, 3 parts of polyether amine with the average molecular weight of 200 and 28 parts of ethylene glycol monobutyl ether into a closed reaction kettle with a reflux and cooling device, heating to 110-112 ℃ within 2 hours under the stirring condition, refluxing and preserving heat within the temperature range for 5 hours, and carrying out copolymerization reaction to obtain amino polyether modified polysiloxane;

s3: putting the amino polyether modified polyorganosiloxane obtained in the step S2 into an emulsifying kettle, cooling to room temperature, adding 28 parts of isomeric tridecanol polyoxyethylene (7) ether, 1 part of ethyl polysilicate 40 and 1.5 parts of glacial acetic acid, slowly adding 271 parts of softened water in portions, stirring and emulsifying to obtain emulsion B;

s4: and mixing and stirring uniformly 50 parts of emulsion A, 115 parts of emulsion B and 7 parts of cationic blocked isocyanate crosslinking agent to obtain the finishing agent.

The technical indexes of the finishing agent are as follows: appearance: white emulsion, solid content: 32.0%, pH: 6.5, ionic: yang.

Comparative example

The product is Liaoning sidereal fine chemical industry Co., Ltd solvent type high elastic coating glue FS-950B.

Examples of the experiments

The finishing agents obtained in examples 1 to 6 were padded on pure cotton fabrics with the specification of 60 × 60 and 90 × 88 and nylon cotton fabrics with the specification of 70D nylon × 21S cotton, and the finishing process was as follows: the using amount of the finishing agent is 100 g/L, the mangle rolling rate is 60-70%, the drying is carried out at the temperature of 100 ℃, and the baking is carried out for 1min at the temperature of 170 ℃.

The comparative example is subjected to coating finishing on the same fabric, and the coating weight is controlled to be 18-20 g/m²Oven drying at 100 deg.C, and baking at 170 deg.C for 1 min.

The stiffness and the smoothness of the fabric are evaluated by using a bending length index, and the bending length is measured according to GB/T18318.1-2009 part 1 of the determination of the bending performance of the textile: testing by the inclined plane method; the elasticity of the fabric is evaluated by the wrinkle recovery angle which is tested according to GB/T3819-1997 method for measuring the recovery angle of the crease of the textile fabric; the water washing was tested according to GB/T8629-:

table 1 test results of the finishes obtained in examples 1 to 6 and of the coating glues of the comparative examples on pure cotton face fabric are compared in the table:

table 3 comparison of the results of the tests on brocade cotton face fabric with the finishes obtained in examples 1 to 6 and the coating glues of the comparative examples:

as can be seen from the results in tables 1 and 2, the fabric finished with the finish of the examples of the present invention has a smaller bending length than the comparative examples, indicating better softness than the comparative examples; the wrinkle recovery angle is close to the comparative example, which shows that the wrinkle-resistant effect of the imitation coating can be achieved. Although the wrinkle recovery angle of the fabric coated with the comparative example was similar to that of the example before washing, the wrinkle recovery angle was significantly reduced after 5 times of washing, indicating that the comparative example was not good in washing fastness and the example was excellent in washing fastness.

Although the invention has been described in detail above with reference to a general description and specific examples, it will be apparent to one skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.