阅读说明：本技术 一种聚丙烯酸酯硬挺整理剂的制备方法 (Preparation method of polyacrylate stiffening finishing agent ) 是由 王春梅 陈何卿 华学铭 缪勤华 于 2019-09-30 设计创作，主要内容包括：本发明涉及高分子聚合物技术领域,尤其涉及一种聚丙烯酸酯硬挺整理剂的制备方法,以纳米SiO<Sub>2</Sub>代替传统乳化剂,由甲基丙烯酸甲酯为硬单体,丙烯酸丁酯为软单体,双丙酮丙烯酰胺和丙烯酸为功能单体,过硫酸铵-亚硫酸氢钠为引发剂,聚合制得环保型无甲醛硬挺整理剂；本发明制备的聚丙烯酸酯硬挺整理剂不使用乳化剂,可减少乳化剂带来的弊端,对环境友好,同时整理后织物硬挺度高,断裂强力提高,耐水洗性好,且具备一定的拒水性能。(The invention relates to the technical field of high molecular polymers, in particular to a preparation method of a polyacrylate stiffening finishing agent prepared from nano SiO 2 Instead of the traditional emulsifier, methyl methacrylate is taken as a hard monomer, butyl acrylate is taken as a soft monomer, diacetone acrylamide and acrylic acid are taken as functional monomers, ammonium persulfate-sodium bisulfite is taken as an initiator, and the ring is prepared by polymerizationThe shape-preserving formaldehyde-free stiffening finishing agent; the polyacrylate stiffening finishing agent prepared by the invention does not use an emulsifier, can reduce the defects caused by the emulsifier, is environment-friendly, and simultaneously has high stiffness of the finished fabric, improved breaking strength, good water washing resistance and certain water repellency.)

1. Polyacrylate stiffening agentThe preparation method of the physical agent is characterized by comprising the following steps: with nano SiO₂The preparation method of the polyacrylic acid stiffening finishing agent comprises the following steps:

(1) preparing emulsion by mixing 1-1.5 parts of nano SiO₂Mixing the powder with 30-35 parts of deionized water, and performing ultrasonic dispersion to obtain uniform nano SiO₂An aqueous dispersion; uniformly mixing 10-15 parts of soft monomer and 15-20 parts of hard monomer to prepare soft and hard mixed monomer, and quickly dripping 1/5 soft and hard mixed monomer into nano SiO₂Stirring and pre-emulsifying in water dispersion liquid at the speed of 1000-;

(2) emulsion polymerization, namely placing a reaction container containing the emulsion prepared in the step (1) in a water bath kettle to raise the temperature, starting to dropwise add an initiator solution prepared by mixing 0.2-0.4 part of ammonium persulfate, 0.1-0.2 part of sodium bisulfite and 15-25 parts of deionized water when the temperature in the reaction container rises to 70 ℃, stirring at the speed of 300-350r/min, and after the polymerization reaction starts, simultaneously dropwise adding the remaining 4/5 soft and hard mixed monomers and a functional monomer solution prepared by mixing 0.5-1.0 part of diacetone acrylamide, 0.5-1.0 part of acrylic acid and 10-15 parts of deionized water for 1-2h, wherein the reaction temperature is 70-75 ℃;

(3) in the heat preservation stage, after all the monomers and the initiator are dripped, the temperature is raised to 80-90 ℃, and the heat is preserved for 0.5-1 h;

(4) discharging, cooling, filtering, discharging, and adjusting the pH value to be neutral by using ammonia water to obtain a polyacrylate stiffening finishing agent;

wherein, the parts are all parts by mass.

2. The preparation method of polyacrylate stiffening finishing agent according to claim 1, wherein in the step (1), nano SiO₂The particle size is 20-40 nm.

3. The preparation method of the polyacrylate stiffening finishing agent according to claim 1, wherein the ultrasonic power for ultrasonic dispersion in the preparation of the emulsion in the step (1) is 75W, the frequency is 20kHz, and the ultrasonic time is 10-15 min.

4. The preparation method of the polyacrylate stiffening finishing agent according to claim 1, wherein in the step (2), during emulsion polymerization, the functional monomer accounts for 3-5% of the total monomer amount, and the mass ratio of diacetone acrylamide to acrylic acid is 1: 1; the initiator accounts for 1-2% of the total monomer amount, and the mass ratio of ammonium persulfate to sodium bisulfite is 2: 1.

Technical Field

The invention relates to the technical field of high molecular polymers, in particular to a preparation method of a polyacrylate stiffening finishing agent.

Background

The stiffening agent is a textile printing and dyeing auxiliary which is widely applied. The stiffening finishing has the advantages of improving the appearance of the fabric, endowing the fabric with stiffening feeling, thickness, elasticity, plump hand feeling and the like, and is widely applied to processing of textiles such as lining cloth, luggage cloth, advertising cloth, tents and the like.

Many types of stiffening agents are available in the market at present, and urea-formaldehyde resin, cyanic aldehyde resin, polyacrylate and the like are commonly used. The polyacrylate stiffening finishing agent is different from aldehyde-containing resin, the finishing agent does not have the problem of formaldehyde release, and has the advantages of excellent stability, good dispersibility, good self-crosslinking property, no yellowing at high temperature and the like while the stiffness of the fabric is improved, however, in the traditional emulsion polymerization process of polyacrylate, the used surfactant can influence the electrical property, the optical property, the surface property, the water resistance and other properties of polyacrylate, so the development and application prospect of emulsion polyacrylate is limited.

Disclosure of Invention

The invention aims to solve the defects in the prior art, and provides the preparation method of the polyacrylate stiffening finishing agent.

In order to achieve the purpose, the invention adopts the following technical scheme: a process for preparing the polyacrylate-type stiffening agent from nano SiO₂The preparation method of the polyacrylic acid stiffening finishing agent comprises the following steps:

(1) preparing emulsion by mixing 1.0-1.5 parts of nano SiO₂Mixing the powder with 30-35 parts of deionized water, and performing ultrasonic dispersion to obtain uniform nano SiO₂An aqueous dispersion; uniformly mixing 10-15 parts of soft monomer and 15-20 parts of hard monomer to prepare soft and hard mixed monomer, and quickly dripping 1/5 soft and hard mixed monomer into nano SiO₂Stirring and pre-emulsifying in water dispersion liquid at the speed of 1000-;

(2) emulsion polymerization, namely placing a reaction container containing the emulsion prepared in the step (1) in a water bath kettle to raise the temperature, starting to dropwise add an initiator solution prepared by mixing 0.2-0.4 part of ammonium persulfate, 0.1-0.2 part of sodium bisulfite and 15-25 parts of deionized water when the temperature in the reaction container rises to 70 ℃, stirring at the speed of 300-350r/min, and after the polymerization reaction starts, simultaneously dropwise adding the remaining 4/5 soft and hard mixed monomers and a functional monomer solution prepared by mixing 0.5-1.0 part of diacetone acrylamide, 0.5-1.0 part of acrylic acid and 10-15 parts of deionized water for 1-2h, wherein the reaction temperature is 70-75 ℃;

(3) in the heat preservation stage, after all the monomers and the initiator are dripped, the temperature is raised to 80-90 ℃, and the heat is preserved for 0.5-1 h;

(4) discharging, cooling, filtering, discharging, and adjusting the pH value to be neutral by using ammonia water to obtain a polyacrylate stiffening finishing agent;

wherein, the parts are all parts by mass.

Preferably, the step (1) is performed by using nano SiO₂The particle size is 20-40nm, the ultrasonic power of an ultrasonic processor is 75W, the frequency is 20kHz, and the ultrasonic time is 10-15 min.

Preferably, during the emulsion polymerization in the step (2), the functional monomer accounts for 3-5% of the total monomer amount, and the mass ratio of diacetone acrylamide to acrylic acid is 1: 1; the initiator accounts for 1-2% of the total monomer amount, and the mass ratio of ammonium persulfate to sodium bisulfite is 2: 1.

The invention has the following beneficial effects: the invention uses nano SiO₂The environment-friendly formaldehyde-free polyacrylate stiffening finishing agent is prepared by polymerization by using methyl methacrylate as a hard monomer, butyl acrylate as a soft monomer, diacetone acrylamide and acrylic acid as functional monomers and ammonium persulfate-sodium bisulfite as an initiating system instead of a traditional emulsifier; the polyacrylate stiffening finishing agent prepared by the invention does not use an emulsifier, can reduce the defects caused by the emulsifier, is environment-friendly, and simultaneously has high stiffness of the finished fabric, improved breaking strength, good water washing resistance and certain water repellency.

Detailed Description

The technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments.