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Preparation method of vinyl pyrrolidone-dimethylamino ethyl methacrylate copolymer

A technology of dimethylamino ethyl methacrylate and vinyl pyrrolidone is applied in the field of preparation of vinyl pyrrolidone-dimethylamino ethyl methacrylate copolymer, and can solve the problems of high toxicity of acetone, hydrolysis of molecular chain, unenvironmental protection, etc. problem, to achieve the effect of less toxicity, less side reaction products, and better cost

Inactive Publication Date: 2019-04-26
HUANGSHAN BONSUN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the existing preparation process, during the synthesis of vinylpyrrolidone-dimethylaminoethyl methacrylate copolymer, acetone or dichloromethane is usually used as a solvent in the reaction process. Acetone is highly toxic, not environmentally friendly, and harmful to the human body. Harmful; Not only that, in the existing preparation technology disclosed today, its product viscosity is in the range of 10000mPa.s~50000Pa.s, and sulfuric acid is usually added to terminate the reaction in the process of eliminating residual single (new polymerization process to synthesize NVP and DMAEMA cation Research on copolymer PVP-Q[J]. Fine and Specialty Chemicals, 2012, 20(2):32-35.), for high viscosity products, it is difficult to prepare due to process equipment and other reasons, and the addition of sulfuric acid will cause Its molecular chain is hydrolyzed, the viscosity decreases sharply, and it will cause redness or yellowing of the product, and it will produce burnt odor

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of preparation method of vinylpyrrolidone-dimethylaminoethyl methacrylate copolymer, its difference is that, described preparation method comprises the following steps:

[0020] Step 1: Add dimethylaminoethyl methacrylate and diethyl sulfate to an ethanol solvent to obtain a quaternization reaction system, and obtain a pre-polymer quaternary ammonium salt after the reaction; the dimethylaminoethyl methacrylate and sulfuric acid The mass ratio of diethyl ester is 1:1.1; The quality sum of the dimethylaminoethyl methacrylate and diethyl sulfate accounts for 25% of the quality of the quaternization reaction system; the reaction time is 30 hours, and the reaction temperature is 0°C.

[0021] Step 2: adding the prepolymer quaternary ammonium salt, N-vinylpyrrolidone and initiator into water to react to obtain a polymerization system; in step 2, the quality of the initiator is the same as that of N-vinylpyrrolidone and dimethyl methacrylate The mass ratio of amino eth...

Embodiment 2

[0025] A kind of preparation method of vinylpyrrolidone-dimethylaminoethyl methacrylate copolymer, its difference is that, described preparation method comprises the following steps:

[0026] Step 1: Add dimethylaminoethyl methacrylate and diethyl sulfate to an ethanol solvent to obtain a quaternization reaction system, and obtain a pre-polymer quaternary ammonium salt after the reaction; the dimethylaminoethyl methacrylate and sulfuric acid The mass ratio of diethyl ester is 1:1.1; the mass sum of the dimethylaminoethyl methacrylate and diethyl sulfate accounts for 15% of the mass of the quaternization reaction system, and the reaction time of the first step is 24 Hours, the reaction temperature is 5°C;

[0027] Step 2: adding the pre-polymer quaternary ammonium salt, N-vinylpyrrolidone and initiator into water to react to obtain a polymerization reaction system; the quality of the initiator is the same as that of N-vinylpyrrolidone, dimethylaminoethyl methacrylate and The m...

Embodiment 3

[0031] A kind of preparation method of vinylpyrrolidone-dimethylaminoethyl methacrylate copolymer, its difference is that, described preparation method comprises the following steps:

[0032] Step 1: Add dimethylaminoethyl methacrylate and diethyl sulfate to an ethanol solvent to obtain a quaternization reaction system, and obtain a pre-polymer quaternary ammonium salt after the reaction; the dimethylaminoethyl methacrylate and sulfuric acid The mass ratio of diethyl ester is 1:1.1; The quality sum of described dimethylaminoethyl methacrylate and diethyl sulfate accounts for 18% of the quality of the quaternization reaction system; The reaction time is 30 hours, and the reaction temperature is 0°C.

[0033] Step 2: adding the pre-polymer quaternary ammonium salt, N-vinylpyrrolidone and initiator into water to react to obtain a polymerization reaction system; the quality of the initiator is the same as that of N-vinylpyrrolidone, dimethylaminoethyl methacrylate and The mass ra...

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PUM

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Abstract

The invention provides a preparation method of a vinyl pyrrolidone-dimethylamino ethyl methacrylate copolymer. The preparation method comprises the following steps: step one, adding dimethylaminoethylmethacrylate and diethyl sulfate into an ethyl alcohol solvent to obtain a quaternarization system, and reacting to obtain a pre-polymer quaternary ammonium salt; step two, adding the pre-polymer quaternary ammonium salt, N-vinyl pyrrolidone and an initiator into water for reacting to obtain a polymerization reaction system; and step three, adding the initiator into the polymerization reaction system for eliminating residual monomers so as to obtain the product. The preparation method has the beneficial effects that the product with the viscosity range of 5000 mPa.s to 150000 mPa.s can be produced, the yield can be 99.5%, the residual rate of monomers is below 0.02%, the product is colorless, transparent and free of peculiar smell, ethyl alcohol and water are taken as solvents, the initiator can preferably participate in the reaction, the cost is lower, few side reaction products are generated, and compared with acetone and methylene dichloride commonly used in the field, the productis low in toxicity and more environmentally-friendly.

Description

technical field [0001] The invention belongs to the field of polymer chemical industry, and in particular relates to a preparation method of vinylpyrrolidone-dimethylaminoethyl methacrylate copolymer. Background technique [0002] Vinylpyrrolidone-dimethylaminoethyl methacrylate copolymer (also known as PVP-Q cationic copolymer) is a common product in the field of fine chemicals. It is used as a conditioning agent in long-lasting curling liquid, conditioning shampoo, and cleaning and conditioning varieties , as a film-forming agent in styling products, has affinity for hair, provides conditioning and firming effects, accumulates very little, makes hair easier to comb, shiny, smooth, and easy to style. It can be used with anionic, non-ionic and Amphoteric surfactant compatibility, non-irritating to eyes and skin. [0003] In the existing preparation process, during the synthesis of vinylpyrrolidone-dimethylaminoethyl methacrylate copolymer, acetone or dichloromethane is usua...

Claims

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Application Information

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IPC IPC(8): C08F226/10C08F220/34
CPCC08F220/34C08F226/10
Inventor 程跃光戴微张敏敏吴璟汪菲
Owner HUANGSHAN BONSUN PHARMA
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