阅读说明：本技术 一种水溶剂聚丙烯酸树脂及其制备方法 (Hydrosolvent polyacrylic resin and preparation method thereof ) 是由 刘坤 崔进 赵明喜 韩冬 于 2020-12-22 设计创作，主要内容包括：本发明公开了一种水性溶剂丙烯酸树脂,其原料按质量百分比包括：丙烯酸60-80％,氢氧化钾20-30％,引发剂0.01-0.5％,交联剂1-10％,水10-30％。本发明公开了上述水性溶剂聚丙烯酸树脂的制备方法,包括如下步骤：将丙烯酸、水、交联剂加入反应釜中搅拌,搅拌温度为15-25℃,然后持续通入氮气；向上述所得体系中滴加氢氧化钾,滴加过程中维持温度小于30℃；降至15-20℃,加入引发剂搅拌均匀；将上述所得体系微波加热10-120min,微波功率为120-140W,接着微波加热20-35min,微波功率为900-1100W,粉碎得到水性溶剂聚丙烯酸树脂。(The invention discloses an aqueous solvent acrylic resin, which comprises the following raw materials in percentage by mass: 60-80% of acrylic acid, 20-30% of potassium hydroxide, 0.01-0.5% of initiator, 1-10% of cross-linking agent and 10-30% of water. The invention discloses a preparation method of the water-based solvent polyacrylic resin, which comprises the following steps: adding acrylic acid, water and a cross-linking agent into a reaction kettle, stirring at the temperature of 15-25 ℃, and then continuously introducing nitrogen; dropwise adding potassium hydroxide into the obtained system, and maintaining the temperature to be less than 30 ℃ in the dropwise adding process; cooling to 15-20 deg.C, adding initiator, and stirring; the obtained system is heated by microwave for 10-120min with the microwave power of 120-.)

1. The acrylic resin as the aqueous solvent is characterized by comprising the following raw materials in percentage by mass:

2. the aqueous solvent polyacrylic resin of claim 1, wherein the initiator comprises: azodiisobutyronitrile, potassium persulfate.

3. The aqueous solvent polyacrylic resin as claimed in claim 2, wherein the mass ratio of azodiisobutyronitrile to potassium persulfate is 1-10: 1-10.

4. The aqueous solvent polyacrylic resin of claim 1, wherein the cross-linking agent is pentaerythritol.

5. A method for preparing the aqueous solvent polyacrylic resin according to any one of claims 1 to 4, comprising the steps of:

s1, adding acrylic acid, water and a cross-linking agent into a reaction kettle, stirring at the temperature of 15-25 ℃, and then continuously introducing nitrogen;

s2, dropwise adding potassium hydroxide into the system obtained in the S1, and maintaining the temperature to be lower than 30 ℃ in the dropwise adding process; cooling to 15-20 deg.C, adding initiator, and stirring;

s3, microwave heating the system obtained in S3 for 10-120min with the microwave power of 120-140W, then microwave heating for 20-35min with the microwave power of 900-1100W, and crushing to obtain the polyacrylic resin of the aqueous solvent.

6. The method for preparing polyacrylic resin as aqueous solvent according to claim 5, wherein the reaction vessel in S1 is a glass-lined reaction vessel.

7. The method for preparing polyacrylic resin as aqueous solvent according to claim 5, wherein in S2, the temperature is reduced to 20 ℃, and the initiator is added and stirred uniformly.

8. The method for preparing polyacrylic resin as aqueous solvent according to claim 5, wherein in S3, the heating is performed with microwave power of 130W for 2h, and then the heating is performed with microwave power of 1000W for 20 min.

Technical Field

The invention relates to the technical field of daily chemicals, in particular to hydrosolvent polyacrylic resin and a preparation method thereof.

Background

Carbomer, also known as carbopol, is a high molecular polymer formed by crosslinking acrylic acid and allyl sucrose, was produced by the American Goodrich company at first, and is currently imported into the pharmacopoeias of America, English and the like, and is already imported and carried by the pharmacopoeias of China in 2000 edition. Carbomer is a multipurpose polymer material and pharmaceutic adjuvant, is widely applied to the development and production of medicines and cosmetics at home and abroad, and has wide application prospect.

Carbomer is white, loose powder, has strong hygroscopicity, and is soluble in water, ethanol and glycerol. Depending on the structure of the polymer monomers, there are two general categories from the solvent selection: one is water soluble carbomer and one is alcohol (lipid) soluble carbomer.

At present, carbomer is polymerized in environment-friendly systems such as ethyl acetate, cyclohexane, toluene and the like, and organic solvents used in the production process are low in recovery rate, complex in hazard treatment and high in cost, and have certain risk in large-scale production.

Disclosure of Invention

Based on the technical problems in the background art, the invention provides a hydrosolvent polyacrylic resin and a preparation method thereof.

The invention provides an aqueous solvent acrylic resin which comprises the following raw materials in percentage by mass:

preferably, the initiator comprises: azodiisobutyronitrile, potassium persulfate.

Preferably, the mass ratio of the azodiisobutyronitrile to the potassium persulfate is 1-10: 1-10.

Preferably, the crosslinking agent is pentaerythritol.

The preparation method of the water-based solvent polyacrylic resin comprises the following steps:

s1, adding acrylic acid, water and a cross-linking agent into a reaction kettle, stirring at the temperature of 15-25 ℃, and then continuously introducing nitrogen;

s2, dropwise adding potassium hydroxide into the system obtained in the S1, and maintaining the temperature to be lower than 30 ℃ in the dropwise adding process; cooling to 15-20 deg.C, adding initiator, and stirring;

s3, microwave heating the system obtained in S3 for 10-120min with the microwave power of 120-140W, then microwave heating for 20-35min with the microwave power of 900-1100W, and crushing to obtain the polyacrylic resin of the aqueous solvent.

Preferably, the reaction kettle in S1 is a glass lining reaction kettle.

Preferably, in S2, the temperature is reduced to 20 ℃, and the initiator is added and stirred uniformly.

Preferably, in S3, microwave heating is carried out for 2h with microwave power of 130W, and then microwave heating is carried out for 20min with microwave power of 1000W.

According to the invention, water is used as a solvent, organic solvents such as ethyl acetate, toluene, cyclohexane and the like are not used for synthesizing the polyacrylic resin, microwave heating is adopted in the synthesis process, no waste water, waste gas and waste residue are generated in the whole production process, and the process is environment-friendly and pollution-free.

Detailed Description

The technical solution of the present invention will be described in detail below with reference to specific examples.

Example 1

Adding 100g of acrylic acid solution with the mass fraction of 30% into a four-neck flask, stirring, slowly dropwise adding 85g of potassium hydroxide solution with the mass fraction of 40%, controlling the temperature to be less than 40 ℃, introducing nitrogen to drive oxygen for 30min, adding 1g of pentaerythritol, 0.2g of azodiisobutyronitrile and 0.1g of potassium persulfate, uniformly stirring, pouring into a glass tray, putting into a microwave oven, performing 130W microwave treatment for 20min, performing 1000W microwave treatment for 30min, cooling to room temperature, taking out and crushing to obtain about 58g of finished product.

And (3) implementing a second step:

adding 200g of 30% acrylic acid solution into a four-neck flask, stirring, slowly dropwise adding 155g of 40% potassium hydroxide solution, controlling the temperature to be less than 40 ℃, introducing nitrogen to drive oxygen for 30min, adding 10g of pentaerythritol, 0.5g of azodiisobutyronitrile and 3g of potassium persulfate, uniformly stirring, pouring into a glass tray, putting into a microwave oven, performing microwave treatment at 130W for 10min, performing microwave treatment at 1000W for 35min, cooling to room temperature, taking out and crushing to obtain about 108g of a finished product.

The viscosity of the resulting crosslinked polyacrylic resin was characterized: 0.5g of the above-mentioned crosslinked polyacrylic resin was added to 99.5g of water, and the viscosity was measured at 25 ℃ as follows:

the viscosity was measured to be 101250cps using an NDJ-8 type viscometer using a No. 4 spindle.

The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.