Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of low-residual-monomer N-vinyl butyl lactam homopolymer K90 aqueous solution

A vinylbutyrolactam and homopolymer technology, which is applied in the field of preparation of low-residue mono-N-vinylbutyrolactam homopolymer K90 aqueous solution, can solve the problem of high residual raw materials, and achieves simple preparation, ingenious design and suitable The effect of large-scale promotion and application

Active Publication Date: 2012-08-15
SHANGHAI YUKING WATER SOLUBLE MATERIAL TECH
View PDF2 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Since the viscosity of homopoly N-vinyl butyrolactam K90 is higher than that of other low molecular weight homopoly N-vinyl butyrolactams, the residual raw materials in the reaction are relatively high, and the elimination of residual raw materials is currently a bottleneck, and K value easily degradable

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of low-residual-monomer N-vinyl butyl lactam homopolymer K90 aqueous solution
  • Preparation method of low-residual-monomer N-vinyl butyl lactam homopolymer K90 aqueous solution
  • Preparation method of low-residual-monomer N-vinyl butyl lactam homopolymer K90 aqueous solution

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] In this experiment, the reaction concentration is 18% by weight of N-vinylbutyrolactam monomer aqueous solution, and the total weight of initiator added is: 0.32% (relative to the mass ratio of monomer N-vinylbutyrolactam). Add 287 parts of water as a reaction solvent to a reaction vessel equipped with a gas inlet, a condenser, and a thermometer, introduce nitrogen while stirring, and exhaust the air in the reaction vessel to form a nitrogen atmosphere. Next, after heating with an oil bath so that the internal temperature of the reaction vessel reached 70°C, 63 parts of N-vinylbutyrolactam and 0.08 parts of initiator produced by Shanghai Yuang Chemical Technology Development Co., Ltd. were added. Azobisisobutyronitrile / azobisisoheptanonitrile=5 / 5 composition. After 1h, add 0.06 part of initiator again, continue to react after 0.5h, continue to add 0.04 part of initiator, after 0.5h, add 0.02 part of initiator, after continuing to react for 1.5h, add malonic acid / Mix h...

Embodiment 2

[0084] The difference from Example 1 is that the total weight of the initiator added is: 0.01% (relative to the mass ratio of monomer NVP); an oil bath is used to heat the internal temperature of the reaction vessel to 90°C; the initiator is composed of azobisisobutyl Nitrile / Azobisisoheptanonitrile=7 / 3 composition; add 0.003 parts of initiator for the first time, after 1h, add 0.0012 parts of initiator, continue to react for 0.5h, continue to add 0.0006 parts of initiator, 0.5h Finally, add 0.0012 parts of initiator, and continue the polymerization reaction for 0.5h after adding the initiator; the mixed acid for the first time is a mixed acid in equal proportions of malonic acid / hydrochloric acid, and the pH is adjusted to be 7, and the mixed acid for the second time is sulfuric acid / hydrochloric acid =8 / 2 mixed acid, adjust the pH to 5, and the interval between two acid additions is 1h. Prepare the N-vinylbutyrolactam concentration in the reaction liquid of PVPK90 polymer to...

Embodiment 3

[0086] The difference from Example 1 is that the total weight of the added initiator is: 3% (relative to the mass ratio of monomer NVP); an oil bath is used to heat the internal temperature of the reaction vessel to 55°C; the initiator is composed of azobisisobutyl Nitrile / Azobisisoheptanonitrile=3 / 7 composition; add 1.134 parts of initiator for the first time, 1h later, add 0.378 parts of initiator, continue to react for 0.5h, continue to add 0.189 parts of initiator, 0.5h Finally, add 0.378 parts of initiator, and continue the polymerization reaction for 2 hours after adding the initiator; the mixed acid for the first time is a mixed acid of sulfuric acid / hydrochloric acid=3 / 7, adjust the pH to 5, and the mixed acid for the second time is malonic acid / sulfuric acid = 1 / 9 mixed acid, adjust the pH to 2, and the interval between two acid additions is 5h. An aqueous solution with a PVPK90 concentration of 18% was prepared, the residual N-vinylbutyrolactam concentration was 7....

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a preparation method of low-residual-monomer N-vinyl butyl lactam homopolymer K90 aqueous solution. The preparation method comprises the following steps that: in the existence of inert gas and at a polymerization temperature ranging from 55 DEG C to 90 DEG C, a raw material, namely 10-35wt% N-vinyl butyl lactam monomer aqueous solution is stirred and reacted for 2.5 hours to 4.5 hours; during the period, an initiator is added in the raw material in batches, wherein the initiator is a mixture of azodiisobutyronitrile and azo-bis-iso-heptonitrile, and the total quantity of the initiator equals to 0.01% to 3% of the mass of N-vinyl butyl lactam monomers; and when a system K value reaches 90 to 102, the raw material with the initiator is kept at a temperature of 95 DEG C overnight to eliminate residual monomers, and in the process, mixed acid is added into the raw material with the initiator in batches to adjust the pH value to 2.0 to 7.0, thus obtaining the colorless transparent product, wherein the mixed acid is formed by mixing at least two acid selected from malonic acid, sulfuric acid and hydrochloric acid, and 10-35wt% product having the residual monomers below 10ppm and the stable K value being from 90 to 102. According to the invention, the design is ingenious, the preparation is simple, the residual monomers of the prepared N-vinyl butyl lactam homopolymer K90 aqueous solution are below 10ppm, the product is colorless, the K value of the product is stable, and thus the product is applicable to large-scale promotion and application.

Description

technical field [0001] The invention relates to the technical field of compound preparation, in particular to the technical field of N-vinylbutyrolactam homopolymer preparation, in particular to a preparation method of a low-residue mono-N-vinylbutyrolactam homopolymer K90 aqueous solution. Background technique [0002] Homopoly N-vinyl butyrolactam is a non-ionic water-soluble polymer compound. Homopoly N-vinyl butyrolactam is easily soluble in water, alcohols, amines and halogenated hydrocarbons, and can be mixed with almost all other Compounding of cationic, anionic and nonionic cosmetic polymers. It has excellent solubility, biocompatibility, physiological inertness, film-forming property, and membrane body protection ability. Homopolymer N-vinylbutyrolactam K90 is the most distinctive and widely used fine chemical variety among N-vinylamide homopolymers, so it has a wide range of uses. Application of homopoly N-vinyl butyrolactam K90 in daily chemical industry: In dai...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C08F126/10C08F6/10
CPCC08F26/10C08F126/10C08F6/003C08F4/04C08F2/10C08L39/06C08F6/10
Inventor 王宇吴美玲陈占
Owner SHANGHAI YUKING WATER SOLUBLE MATERIAL TECH
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com