阅读说明：本技术 一种含氟固色剂及其制备方法 (Fluorine-containing color fixing agent and preparation method thereof ) 是由 魏焕曹 许兆坤 于 2019-12-05 设计创作，主要内容包括：本发明公开一种含氟固色剂及其制备方法,由以下重量百分含量的组分组成：40～60％二甲基二烯丙基氯化铵、5～25％二烯丙基胺盐、1～5％烯丙基全氟辛基醚或酯、0.5～1％过氧化物和去离子水余量；本发明含氟固色剂为黄色粘稠状,相对于现有的固色剂,本发明的固色剂稳定性更好,能与硅油等多种整理剂同溶；且在织物水洗、干擦、湿擦及日晒牢度都有了明显的提升。本发明的含氟固色剂的制备过程简单、便捷,提供了一种性能更优异的固色剂选择。(The invention discloses a fluorine-containing color fixing agent and a preparation method thereof, wherein the fluorine-containing color fixing agent comprises the following components in percentage by weight: 40-60% of dimethyldiallylammonium chloride, 5-25% of diallylamine salt, 1-5% of allyl perfluorooctyl ether or ester, 0.5-1% of peroxide and the balance of deionized water; compared with the existing color fixing agent, the fluorine-containing color fixing agent has better stability and can be dissolved with various finishing agents such as silicone oil and the like; and the fastness to washing, dry wiping, wet wiping and sunlight of the fabric is obviously improved. The fluorine-containing color fixing agent disclosed by the invention is simple and convenient in preparation process, and provides a color fixing agent with more excellent performance.)

1. The fluorine-containing color fixing agent is characterized by comprising the following components in percentage by weight: 40-60% of dimethyldiallylammonium chloride, 5-25% of diallylamine salt, 1-5% of allyl perfluorooctyl ether or ester, 0.5-1% of peroxide and the balance of deionized water.

2. The fixing agent according to claim 1, wherein the diallylamine salt is the hydrochloride or sulfate salt thereof.

3. The fixing agent according to claim 1, wherein the peroxide is at least one of ammonium persulfate, sodium persulfate, benzoyl peroxide, azobisisobutyronitrile.

4. The fixing agent according to claim 1, wherein the allyl perfluorooctyl ether or perfluorooctanol acrylate is obtained by substitution reaction of perfluorooctanol with acryloyl chloride or esterification reaction with acrylic acid.

5. The fixing agent according to claim 4, wherein the allyl perfluorooctyl ether is prepared by the following process: adding perfluorooctanol and triethylamine into a four-neck flask, uniformly mixing, dropwise adding acryloyl chloride with the same molar weight as that of the perfluorooctanol, dropwise adding at a speed to keep the reaction temperature below 20 ℃, and reacting at the temperature below 20 ℃ for 60min after the addition is finished to obtain the allyl perfluorooctyl ether.

6. The fixing agent according to claim 4, wherein the perfluorooctanol acrylate is prepared by the following method: adding perfluorooctanol, p-toluenesulfonic acid, a polymerization inhibitor and acrylic acid with the same molar weight as that of the perfluorooctanol into a four-neck flask, uniformly mixing, heating to 160-180 ℃, stopping heating until no water is evaporated, and continuously stirring to room temperature to obtain the perfluorooctanol acrylate.

7. The fixing agent according to claim 6, wherein the polymerization inhibitor is hydroquinone.

8. A process for the preparation of a fixing agent according to any of claims 1 to 7, characterized in that the process is as follows: uniformly mixing dimethyl diallyl ammonium chloride, diallyl amine salt, allyl perfluorooctyl ether or ester and water; heating to 80-90 ℃, and stirring for 30-60 minutes under heat preservation; and (3) dropwise adding peroxide, continuing to polymerize at the temperature of 80-90 ℃, keeping the temperature for 120 minutes, and cooling to room temperature to obtain the fluorine-containing color fixing agent.

Technical Field

The invention belongs to the field of textile auxiliary agents, relates to a color fixing agent, and particularly relates to a fluorine-containing color fixing agent and a preparation method thereof.

Background

The color fixing agent is one of important auxiliaries in the printing and dyeing industry, and can be used for improving the color fastness of the dye on fabrics to wet treatment. The insoluble color substance can be formed on the fabric with the dye, thereby improving the washing fastness and the perspiration fastness of the color and sometimes also improving the light fastness of the color. Therefore, when cellulosic fiber fabrics are dyed in deep colors (dye concentration > 1%), color fixing treatment is required to be carried out on the cellulosic fiber fabrics so as to obtain various fastness indexes of washing, dry wiping, wet wiping and the like which are accepted by customers.

The current color fixing agent of the copolymer taking dimethyl diallyl ammonium chloride and diallylamine as main bodies can only improve the washing fastness and the dry rubbing fastness, has no effect on the wet rubbing fastness, and simultaneously influences the light fastness for improving the wet rubbing fastness of dyed fabrics; in addition, at present, polyurethane wet rubbing fastness improving agents are mainly used, but the wet rubbing fastness improving agents generally have the problems of poor stability, easiness in emulsion breaking and failure, incapability of being dissolved with silicone oil and the like. Therefore, it is necessary to develop a fixing agent with better stability and better fixing effect compared with the existing fixing agent.

Disclosure of Invention

The invention aims to provide the fluorine-containing color fixing agent which has better fabric washing, dry wiping, wet wiping and light fastness and can be used together with various after-finishes aiming at the defects of the prior art.

In order to achieve the purpose, the invention adopts the technical scheme that: a fluorine-containing color fixing agent comprises the following components in percentage by weight: 40-60% of dimethyldiallylammonium chloride, 5-25% of diallylamine salt, 1-5% of allyl perfluorooctyl ether or ester, 0.5-1% of peroxide and the balance of deionized water.

In a preferred embodiment of the present invention, the diallylamine salt is a hydrochloride or sulfate thereof.

In a preferred embodiment of the present invention, the peroxide is at least one of ammonium persulfate, sodium persulfate, benzoyl peroxide, and azobisisobutyronitrile.

As a preferred embodiment of the invention, the allyl perfluorooctyl ether or perfluorooctanol acrylate is prepared by a substitution reaction of perfluorooctanol and acryloyl chloride or an esterification reaction of perfluorooctanol and acrylic acid.

Further, the preparation method of the allyl perfluorooctyl ether comprises the following steps: adding perfluorooctanol and triethylamine into a four-neck flask, wherein the molar ratio of the perfluorooctanol to the triethylamine is 10:1, uniformly mixing, dropwise adding acryloyl chloride with the same molar weight as that of the perfluorooctanol, keeping the reaction temperature below 20 ℃ at the dropwise adding speed, and reacting for 60min at the temperature below 20 ℃ after the addition is finished to obtain the allyl perfluorooctyl ether.

Further, the preparation method of the perfluorooctanol acrylate comprises the following steps: adding perfluorooctanol, p-toluenesulfonic acid, a polymerization inhibitor and acrylic acid with the same molar weight as the perfluorooctanol into a four-neck flask, wherein the molar ratio of the perfluorooctanol to the p-toluenesulfonic acid to the polymerization inhibitor is 1000: 100: 1, uniformly mixing, heating to 160-180 ℃, stopping heating until no water is evaporated, and continuously stirring to room temperature to obtain the perfluorooctanol acrylate.

As a preferred embodiment of the present invention, the polymerization inhibitor is hydroquinone.

The invention also provides a preparation method of the color fixing agent, which comprises the following steps: uniformly mixing dimethyl diallyl ammonium chloride, diallyl amine salt, allyl perfluorooctyl ether or ester and water; heating to 80-90 ℃, and stirring for 30-60 minutes under heat preservation; and (3) dropwise adding peroxide, continuing to polymerize at the temperature of 80-90 ℃, keeping the temperature for 120 minutes, and cooling to room temperature to obtain the fluorine-containing color fixing agent.

The invention provides a fluorine-containing color fixing agent which is in a yellow-brown sticky state, the color fixing agent prepared under the interaction of all components does not contain formaldehyde, is environment-friendly and pollution-free, and compared with the existing color fixing agent, the color fixing agent disclosed by the invention has the advantages that as the carbon chain contains fluorine elements, the surface tension of the solution is low, the solution is easy to permeate and diffuse into the interior of a fabric, and the color fixing agent is better combined with a dye. Can be used together with various finishing agents such as silicone oil and the like; the fastness of the fabric to washing, dry wiping, wet wiping and sunlight is obviously improved. The fluorine-containing color fixing agent disclosed by the invention is simple and convenient in preparation process, provides a color fixing agent with more excellent performance, and has a wide market prospect.

Detailed Description

To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.