阅读说明：本技术 一种用于棉织物的亲水有机硅整理剂及其制备方法 (Hydrophilic organic silicon finishing agent for cotton fabric and preparation method thereof ) 是由 甘宏宇 张金龙 张桃勇 施可可 方颂 沈涛 于 2020-07-03 设计创作，主要内容包括：本发明公开了一种用于棉织物的亲水有机硅整理剂及其制备方法,涉及纺织助剂的技术领域,所述有机硅整理剂由包括以下重量百分比的组分制备得到：一氯单体15%～25%、二氯单体5%～10%、三氯单体2.5%～5%、交联性单体0.5%～1%、环保溶剂5%～10%、混合乳化剂2.5%～5%、pH=4～4.5的去离子水余量。本发明具有提供一种亲水性能更好的纺织整理剂优点。(The invention discloses a hydrophilic organic silicon finishing agent for cotton fabrics and a preparation method thereof, and relates to the technical field of textile auxiliaries, wherein the organic silicon finishing agent is prepared from the following components in percentage by weight: 15-25% of monochloro monomer, 5-10% of dichloro monomer, 2.5-5% of trichloro monomer, 0.5-1% of crosslinking monomer, 5-10% of environment-friendly solvent, 2.5-5% of mixed emulsifier and the balance of deionized water with pH = 4-4.5. The invention has the advantage of providing the textile finishing agent with better hydrophilic property.)

1. The hydrophilic organic silicon finishing agent for the cotton fabric is characterized by being prepared from the following components in percentage by weight:

adjusting the pH of the deionized water by adopting acetic acid;

wherein the structural formula of the monochloro monomer is shown as a formula (a);

the structural formula of the dichloro monomer is shown as a formula (b);

the structural formula of the trichloro monomer is shown as a formula (c);

wherein the content of the first and second substances,

r is:

4≤a≤6,8≤b≤10,8≤n≤10,5≤x≤10，30≤y≤60。

2. the hydrophilic silicone finishing agent for cotton fabrics according to claim 1, characterized in that: the crosslinking monomer is vinyl silicone oil with the molecular weight of 1000-2000, and the environment-friendly solvent is 1, 4-pentanediol.

3. The hydrophilic silicone finishing agent for cotton fabrics according to claim 1, characterized in that: the monochloro monomer, the dichloro monomer and the trichloro monomer are prepared from the following components in percentage by weight:

the alkaline catalyst is one or more of sodium bicarbonate, sodium carbonate or monoethanolamine;

the end epoxy group-terminated silicone oil has a structural formula as follows:

the structural formula of the polyether amine is as follows:

4. a hydrophilic silicone finish for cotton fabric according to claim 3, characterized in that: the epoxy-terminated silicone oil is epoxy-terminated silicone oil with the molecular weight of 2218-2774, and the polyether amine is polyether amine with the molecular weight of 364-654.

5. A hydrophilic silicone finish for cotton fabric according to claim 3, characterized in that: the monochloro monomer, the dichloro monomer and the trichloro monomer are prepared by the following steps:

step a: preparing an intermediate A with the molecular weight of 5000-7000;

step b: controlling the pH value of the intermediate A to be 8-8.5 by using an alkaline catalyst at the temperature of 0-10 ℃, and reacting the intermediate A with cyanuric chloride to obtain a crude monochloro monomer; controlling the pH value of the intermediate A to be 8.6-9.0 by using an alkaline catalyst at the temperature of 30-40 ℃, and reacting the intermediate A with cyanuric chloride to obtain a crude dichloro monomer; controlling the pH value of the intermediate A to be 9.5-10.5 by using an alkaline catalyst amine at the temperature of 70-80 ℃, and reacting the intermediate A with cyanuric chloride to obtain a crude trichloromonomer;

step c: then purifying the obtained crude monochloro monomer, dichloro monomer and trichloro monomer in a solution of ethanol and water for many times, removing impurities, and finally distilling to obtain pure monochloro monomer, dichloro monomer and trichloro monomer.

6. The hydrophilic silicone finishing agent for cotton fabrics according to claim 5, characterized in that: the preparation method of the intermediate A comprises the following steps:

step a: adding epoxy-terminated silicone oil and polyether amine into isopropanol in proportion, and stirring and mixing uniformly;

step b: controlling the temperature to be 80-90 ℃, and carrying out reflux reaction for 5-7 h to obtain the amino-terminated block silicone oil;

step c: adding octamethylcyclotetrasiloxane and 6-8 ppm chloroplatinic acid into the amino-terminated block silicone oil obtained in the step b according to a ratio, and uniformly stirring;

step d: controlling the temperature to be 90-100 ℃, and carrying out chain extension reaction for 4-6 hours to obtain an intermediate A;

step e: and d, adding polyethylene glycol into the intermediate A in the step d, and distilling off the isopropanol serving as a solvent at 50-60 ℃.

7. A process for the preparation of a silicone finish for cotton fabric according to claim 1, characterized in that: the method comprises the following steps: and mixing the pure monochloro product, the dichlorine product and the trichloro product according to a ratio, adding vinyl silicone oil with the molecular weight of 1000-2000, an environment-friendly solvent 1, 4-pentanediol and a mixed emulsifier, and uniformly stirring to obtain the high-hydrophilicity organic silicon finishing agent with excellent performance.

Technical Field

The invention relates to the technical field of textile auxiliary agents, in particular to a hydrophilic organic silicon finishing agent for cotton fabrics and a preparation method thereof.

Background

Textile auxiliaries are chemicals which are necessary in the production and processing of textiles. The textile auxiliary agent has an indispensable important role in improving the product quality and the added value of the textile, can endow the textile with various special functions and styles, such as softness, crease resistance, shrinkproof property, water resistance, antibiosis, antistatic property, flame retardance and the like, can improve the dyeing and finishing process, and plays roles in saving energy and reducing the processing cost. Textile auxiliaries are crucial to increasing the overall level of the textile industry and their role in the textile industry chain.

The organic silicon finishing agent is used as a special function finishing of fabric fabrics, is more and more popular with consumers, and as the consumption level of the consumers is continuously improved and the consumption demand is continuously increased, the organic silicon finishing agent is used as a fabric processing unit, the hand feeling research of the fabrics is also more and more emphasized, and the hand feeling characteristic meeting the requirements of the consumers is continuously promoted.

However, the common defects of the current organic silicon finishing agent for cotton fabrics are that the washing fastness is poor and the hydrophilicity is lost too much because customers pursue hand feeling, which is mainly caused by that the reaction groups of the organic silicon finishing agent and cotton fibers are not firm enough, the hand feeling is obviously reduced after ten times of conventional washing, and in addition, the hydrophilic groups of the cotton fabrics are sealed by the organic silicon finishing agent and lose the effect.

Disclosure of Invention

Aiming at the defects in the prior art, the invention aims to provide a hydrophilic organic silicon finishing agent for cotton fabrics and a preparation method thereof, wherein the finishing agent is required to have high adsorption capacity and good washability on the cotton fabrics, and the high hydrophilic performance of the cotton fabrics is not lost while the fabrics are endowed with good soft, smooth, fluffy and other handfeels.

The above object of the present invention is achieved by the following technical solutions:

a hydrophilic organic silicon finishing agent for cotton fabrics is prepared from the following components in percentage by weight:

wherein the structural formula of the monochloro monomer is shown as a formula (a);

the structural formula of the dichloro monomer is shown as a formula (b);

the structural formula of the trichloro monomer is shown as a formula (c);

wherein the content of the first and second substances,

r is:

4≤a≤6,8≤b≤10,8≤n≤10,5≤x≤10，30≤y≤60。

by adopting the technical scheme, on one hand, the prepared organic silicon finishing agent has a bridge structure of cyanuric chloride and an excellent plane configuration, so that the organic silicon finishing agent has more excellent smoothness; on the other hand, the organic silicon structure contains various reaction groups, particularly chlorine reaction groups, so that the organic silicon structure can better react with cotton fabrics, and meanwhile, the molecular weight difference of the monochloro monomer, the dichloro monomer and the trichloro monomer is large, so that the organic silicon finishing agent can act on different layers of the cotton fabrics in the middle and outside.

The invention is further configured to: the crosslinking monomer is vinyl silicone oil with the molecular weight of 1000-2000, and the environment-friendly solvent is 1, 4-pentanediol.

By adopting the technical scheme, the vinyl silicone oil with the molecular weight of 1000-2000 has good compatibility with other components, and the molecular weight of the product obtained after crosslinking is more appropriate, so that the finishing effect of the obtained organic silicon finishing agent cloth is more facilitated.

The invention is further configured to: the monochloro monomer, the dichloro monomer and the trichloro monomer are prepared from the following components in percentage by weight:

the alkaline catalyst is one or more of sodium bicarbonate, sodium carbonate or monoethanolamine;

the end epoxy group-terminated silicone oil has a structural formula as follows:

the structural formula of the polyether amine is as follows:

the invention is further configured to: the epoxy-terminated silicone oil is epoxy-terminated silicone oil with the molecular weight of 2218-2774, and the polyether amine is polyether amine with the molecular weight of 364-654.

By adopting the technical scheme, the molecular weights of the epoxy-terminated silicone oil and the polyether amine are controlled so as to control the molecular weight of the final product to be proper, the hydrophilic effect is easily lost when the molecular weight is too large, and the hand feeling is seriously influenced when the molecular weight is too small.

The invention is further configured to: the monochloro monomer, the dichloro monomer and the trichloro monomer are prepared by the following steps:

step a: preparing an intermediate A with the molecular weight of 5000-7000;

step b: controlling the pH value of the intermediate A to be 8-8.5 by using an alkaline catalyst at the temperature of 0-10 ℃, and reacting the intermediate A with cyanuric chloride to obtain a crude monochloro monomer; controlling the pH value of the intermediate A to be 8.6-9.0 by using an alkaline catalyst at the temperature of 30-40 ℃, and reacting the intermediate A with cyanuric chloride to obtain a crude dichloro monomer; controlling the pH value of the intermediate A to be 9.5-10.5 by using an alkaline catalyst at the temperature of 70-80 ℃, and reacting the intermediate A with cyanuric chloride to obtain a crude trichloromonomer;

step c: then purifying the obtained crude monochloro monomer, dichloro monomer and trichloro monomer in a solution of ethanol and water for many times, removing impurities, and finally distilling to obtain pure monochloro monomer, dichloro monomer and trichloro monomer.

By adopting the technical scheme, the cyanuric chloride contains active chloride ions, the two ends of the intermediate A contain reactive amino, the chlorine ions of the cyanuric chloride and the amino of the amino-terminated polyether silicone oil are easy to undergo condensation reaction under the alkaline condition, the next hydrogen chloride is removed in the reaction process, and the hydrogen chloride is neutralized by alkali to perform forward reaction, so that the required product is promoted to be obtained. The reaction is carried out at different alkalinity and different temperature to obtain different substituted condensation compounds. The bridge structure of cyanuric chloride has excellent planar configuration and thus excellent smoothness. The molecular weight difference of the monochloro monomer, the dichloro monomer and the trichloro monomer is large, so that the monochloro monomer, the dichloro monomer and the trichloro monomer can act on different layers of the inner layer, the middle layer and the outer layer of the cotton fabric, and the excellent smooth and soft effect on the cotton fabric is achieved.

The invention is further configured to: the preparation method of the intermediate A comprises the following steps:

step a: adding epoxy-terminated silicone oil and polyether amine into isopropanol in proportion, and stirring and mixing uniformly;

step b: controlling the temperature to be 80-90 ℃, and carrying out reflux reaction for 5-7 h to obtain the amino-terminated block silicone oil;

step c: adding octamethylcyclotetrasiloxane and chloroplatinic acid serving as a catalyst into the amino-terminated block silicone oil obtained in the step b in proportion, and uniformly stirring;

step d: controlling the temperature to be 90-100 ℃, and carrying out chain extension reaction for 4-6 hours to obtain an intermediate A;

step e: and d, adding polyethylene glycol into the intermediate A in the step d, and distilling off the isopropanol serving as a solvent at 50-60 ℃.

By adopting the technical scheme, the epoxy-terminated silicone oil reacts with the polyether amine to generate condensation reaction of epoxy groups and amino groups, and the octamethylcyclotetrasiloxane is added to carry out chain extension under the action of a solvent and a catalyst, wherein the reaction is as follows:

the silicon semi-structural groups in the molecular structure are increased, so that the effect of being smoother and softer is achieved.

A preparation method of a hydrophilic organic silicon finishing agent for cotton fabrics comprises the following steps:

and mixing the pure monochloro product, the dichlorine product and the trichloro product according to a ratio, adding the crosslinking monomer, the environment-friendly solvent 1, 4-pentanediol and the mixed emulsifier, and uniformly stirring to obtain the high-hydrophilic organic silicon finishing agent with excellent performance.

Compared with the prior art, the invention has the beneficial effects that:

1. the organic silicon finishing agent containing the amino polysiloxane chain segment can endow the cotton fabric with excellent washing resistance, softness, smoothness, fluffiness and other handfeels, and also contains a chlorine group which preferentially reacts with the cotton fabric, so that more amino and hydroxyl groups can be reserved, and more polyoxyethylene ether chain segments, amino and hydroxyl groups are exposed on the surface of the fabric to play a role in high hydrophilicity.

2. The requirements of fabrics with different colors and different dyeing depths can be met through compounding monochloro, dichloro, trichloro and cross-linking agent monomers in different proportions, and fabric hand feeling finishing effects with different styles can be derived.

Detailed Description

The present invention will be described in detail with reference to examples.