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
2 Cites 2 Cited by

AI-Extracted 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 react...
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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.

Technology Topic

DichloromethaneResidual monomer +13

Examples

  • Experimental program(4)
  • Comparison scheme(1)
  • Effect test(1)

Example Embodiment

[0018] Example one
[0019] A preparation method of vinylpyrrolidone-dimethylamino ethyl methacrylate copolymer, the difference is that the preparation method includes the following steps:
[0020] Step 1: Add dimethylaminoethyl methacrylate and diethyl sulfate into an ethanol solvent to obtain a quaternization reaction system, and obtain a prepolymer quaternary ammonium salt after the reaction; the dimethylaminoethyl methacrylate and sulfuric acid The mass ratio of diethyl ester is 1:1.1; the sum of the masses of the dimethylaminoethyl methacrylate and diethyl sulfate accounts for 25% of the mass of the quaternization reaction system; the reaction time is 30 hours, and the reaction temperature It is 0°C.
[0021] Step 2: Add the prepolymer quaternary ammonium salt, N-vinylpyrrolidone and initiator into water to react to obtain a polymerization reaction system; in Step 2, the quality of the initiator is the same as that of N-vinylpyrrolidone and dimethyl methacrylate. The ratio of the total mass of ethyl aminoethyl sulfate to diethyl sulfate is 1:500, the reaction time of the second step is 8 hours, and the reaction temperature is 75°C.
[0022] Step 3: Add an initiator to the polymerization reaction system to eliminate residual monomers to obtain a product. After the polymerization reaction system is heated to 90°C, the initiator is added for a reaction time of 2 hours. The quality of the initiator added is The quality of the initiator added in the second step is the same.
[0023] The initiator of step two and step three is azobisisobutyronitrile.

Example Embodiment

[0024] Example two
[0025] A preparation method of vinylpyrrolidone-dimethylamino ethyl methacrylate copolymer, the difference is that the preparation method includes the following steps:
[0026] Step 1: Add dimethylaminoethyl methacrylate and diethyl sulfate into an ethanol solvent to obtain a quaternization reaction system, and obtain a prepolymer quaternary ammonium salt after the reaction; the dimethylaminoethyl methacrylate and sulfuric acid The mass ratio of diethyl ester is 1:1.1; the sum of the masses of the dimethylaminoethyl methacrylate and diethyl sulfate accounts for 15% of the mass of the quaternization reaction system, and the reaction time of step one is 24 Hours, the reaction temperature is 5℃;
[0027] Step 2: Add 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 combined with N-vinylpyrrolidone, dimethylaminoethyl methacrylate and The ratio of the total mass of diethyl sulfate is 1:1000, the reaction time is 6 hours, and the reaction temperature is 75°C.
[0028] Step 3: After the polymerization reaction system is heated to 80° C., an initiator is added for a reaction time of 2 hours, wherein the added quality of the initiator is the same as that of the initiator added in the second step.
[0029] The initiator of step two and step three is azobisisoheptonitrile.

Example Embodiment

[0030] Example three
[0031] A preparation method of vinylpyrrolidone-dimethylamino ethyl methacrylate copolymer, the difference is that the preparation method includes the following steps:
[0032] Step 1: Add dimethylaminoethyl methacrylate and diethyl sulfate into an ethanol solvent to obtain a quaternization reaction system, and obtain a prepolymer quaternary ammonium salt after the reaction; the dimethylaminoethyl methacrylate and sulfuric acid The mass ratio of diethyl ester is 1:1.1; the sum of the masses of the dimethylaminoethyl methacrylate and diethyl sulfate accounts for 18% of the mass of the quaternization reaction system; the reaction time is 30 hours, and the reaction temperature It is 0°C.
[0033] Step 2: Add 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 combined with N-vinylpyrrolidone, dimethylaminoethyl methacrylate and The ratio of the total mass of diethyl sulfate is 1:1000, the reaction time is 6 hours, and the reaction temperature is 70°C.
[0034] Step 3: After the polymerization reaction system is heated to 95°C, an initiator is added for a reaction time of 2 hours, wherein the added quality of the initiator is the same as that of the initiator added in the second step.
[0035] The initiator in step two and step three is a peroxide type initiator which is benzoyl peroxide.
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Description & Claims & Application Information

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