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Preparation method of polyvinylpyrrolidone

A technology for polyvinylpyrrolidone and vinylpyrrolidone, which is applied in the field of polymer material preparation, can solve the problems that the content of heavy metal ions cannot meet the application standard of polyvinylpyrrolidone, the residual monomer content of polyvinylpyrrolidone is high, and the heavy metal ions are difficult to remove, and the like. Good chromaticity and solubility, improved reaction conversion rate and low production cost

Active Publication Date: 2014-04-16
SICHUAN CHEM IND HLDG GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] ZL200810218921.X discloses a method for preparing low-molecular-weight polyvinylpyrrolidone. The method uses azobisisobutyronitrile or benzoyl peroxide as an initiator, and ferric chloride or copper chloride as a catalyst to prepare low-molecular-weight polyvinylpyrrolidone. Polyvinylpyrrolidone, but the polyvinylpyrrolidone obtained by this method has a high residual monomer content, and because ferric chloride or copper chloride is used as a catalyst, it is difficult to remove heavy metal ions in the product, and its heavy metal ion content cannot meet the requirements of polyvinylpyrrolidone. Application standards in cosmetics and pharmaceuticals
The patent application whose publication number is CN1015087152A discloses a preparation method of polyvinylpyrrolidone, and the initiator used is an azo compound or an organic peroxide. In this method, the initiator is added into the reactor in two or more times, and the polymerization In the later stage of the reaction, the conversion efficiency is low and the reaction time is long

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Measure 30 parts by weight (300g) of N-vinylpyrrolidone, 60 parts by weight (600g) of deionized water, and 3 parts by weight (30g) of a composite initiator. The composite initiator consists of dimethyl azobisisobutyrate, di Composed of tert-butyl and cyclohexanone peroxide, the mass ratio of dimethyl azobisisobutyrate, di-tert-butyl peroxide and cyclohexanone peroxide is 1:2:2.

[0022] The processing step of preparing polyvinylpyrrolidone is as follows:

[0023] (1) Add deionized water into the reactor at one time and start stirring, replace the air in the reactor with nitrogen, then add the composite initiator into the reactor under the protection of nitrogen and mix well;

[0024] (2) When the mixture formed in step (1) is heated to 60°C under the protection of nitrogen, add N-vinylpyrrolidone dropwise to the reaction kettle at a rate of 2.5g / min. After the addition of N-vinylpyrrolidone is completed , carry out the polymerization reaction at 90 ℃, the reaction time...

Embodiment 2

[0028] Measure 30 parts by weight (300g) of N-vinylpyrrolidone, 60 parts by weight (600g) of deionized water, and 3 parts by weight (30g) of a composite initiator. The composite initiator consists of azobisisobutyronitrile and tert-butyl peroxybenzoate Ester composition, the mass ratio of azobisisobutyronitrile to tert-butyl peroxybenzoate is 3:1.

[0029] The processing step of preparing polyvinylpyrrolidone is as follows:

[0030] (1) Add deionized water into the reactor at one time and start stirring, replace the air in the reactor with nitrogen, then add the composite initiator into the reactor under the protection of nitrogen and mix well;

[0031] (2) When the mixture formed in step (1) is heated to 60°C under the protection of nitrogen, add N-vinylpyrrolidone dropwise to the reaction kettle at a rate of 2.5g / min. After the addition of N-vinylpyrrolidone is completed , carry out the polymerization reaction at 80 ℃, the reaction time is 4 hours;

[0032] (3) After the r...

Embodiment 3

[0035] Measure 30 parts by weight (300g) of N-vinylpyrrolidone, 60 parts by weight (600g) of deionized water, and 3 parts by weight (30g) of a composite initiator. The composite initiator consists of azobisisobutyronitrile, tert-butyl peroxybenzoate It is composed of ester and benzoyl peroxide, and the mass ratio of azobisisobutyronitrile, tert-butyl peroxybenzoate and benzoyl peroxide is 3:2:1.

[0036] The processing step of preparing polyvinylpyrrolidone is as follows:

[0037] (1) Add deionized water into the reactor at one time and start stirring, replace the air in the reactor with nitrogen, then add the composite initiator into the reactor under the protection of nitrogen and mix well;

[0038] (2) When the mixture formed in step (1) is heated to 60°C under the protection of nitrogen, add N-vinylpyrrolidone dropwise to the reaction kettle at a rate of 1.7g / min. After the addition of N-vinylpyrrolidone is completed , carry out the polymerization reaction at 70°C, and th...

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PUM

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Abstract

The invention relates to a preparation method of polyvinylpyrrolidone. The method uses the following components by weight as raw materials: 30 parts of N-vinylpyrrolidone, 60-90 parts of solvent and 1-3 parts of compound initiator. The process comprises the following steps in sequence: (1) adding the solvent into a reaction vessel, stirring, and then adding the compound initiator into the reaction vessel under the protection of nitrogen and uniformly mixing to obtain a mixed solution; (2) heating the mixed solution prepared in step (1) to 60 DEG C under the protection of nitrogen, dipping N-vinylpyrrolidone into the reaction vessel, and carrying out polymerization at 60-90 DEG C for 4-6h after the addition of N-vinylpyrrolidone; (3) after the reaction time is expired, stopping stirring to obtain a reaction solution, and drying the reaction solution by spray drying or by drum frying, and crushing to form powder, wherein the compound initiator comprises two or more initiators with 1-2h difference of half life at 60-90 DEG C.

Description

technical field [0001] The invention belongs to the field of preparation methods of polymer materials, and in particular relates to a preparation method of polyvinylpyrrolidone. Background technique [0002] Polyvinylpyrrolidone (abbreviated as PVP in English) is a water-soluble white resinous solid formed by the homopolymerization of N-vinylpyrrolidone. The molecular formula is (C 6 h 9 NO) X , according to different molecular weights, there are K15, K30, K60, K90 and other types. PVP is an important fine chemical product with excellent performance and high added value. Its molecule contains a relatively polar lactam group and has the ability of a polar group. It is soluble in both water and alcohol, Polar organic solvents such as carboxylic acid, alcohol amine, halogenated hydrocarbon, etc., the chemical properties of PVP solid and its aqueous solution are very stable. PVP can form a film in water, methanol, ethanol, chloroform or dichloroethane, and the formed film is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F126/10C08F4/34C08F4/04
Inventor 魏先全赵世比刘明刚吴勇周珂阳杨东刘孔满徐家富张利周志明
Owner SICHUAN CHEM IND HLDG GRP