Controllable method for preparing methoxy polyethylene glycol methacrylate-styrene polymer under condition of high vacuum degree

A technology of polyethylene glycol methacrylate and methoxypolyethylene glycol, which is applied in the direction of organic chemistry, can solve the problems of difficult extraction, difficult catalyst recovery, limited entrainment effect, etc., and achieves mild reaction conditions and high reaction temperature. Low, cost reduction effect

Inactive Publication Date: 2008-12-31
SOUTHEAST UNIV
View PDF5 Cites 6 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Propose to adopt solid acid to do catalyst among CN101092478A, replace homogeneous catalyst, although overcome the problem of catalyst recovery difficulty, still adopt azeotropic solvents such as hexanaphthene to carry water
The method of passing nitrogen has a limited entrainment effect on water, and can only take away part of the water; although in patent CN101117378A, the method of nitrogen passing and vacuuming is combined, but the highest vacuum proposed i

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
  • Controllable method for preparing methoxy polyethylene glycol methacrylate-styrene polymer under condition of high vacuum degree

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Add 30.2000g of methoxypolyethylene glycol (the degree of polymerization n is 13) into the reaction kettle, add catalyst 4-(dimethylamino)pyridine 1.0351g under stirring, heat to dissolve, weigh 0.0086g of polymerization inhibitor and dissolve in 4.3045 In 1 g of methacrylic acid, connect constant pressure drop liquid and controllable vacuuming device, control the vacuum at 0.095MPa, raise the temperature to 63°C, add methacrylic acid dropwise within 3 hours, react for 5 hours, and cool down to obtain methoxy Polyethylene glycol methacrylate.

Embodiment 2

[0021] Add 50.3000g of methoxypolyethylene glycol (the degree of polymerization n is 45) in the reaction kettle, add the catalyst 4-(dimethylamino)pyridine 2.1239g under stirring, heat to dissolve, weigh 0.0084g of polymerization inhibitor and dissolve in 2.7979 In 1 g of methacrylic acid, connect constant pressure drop liquid and controllable vacuuming device, control the vacuum at 0.097MPa, raise the temperature to 50°C, add methacrylic acid dropwise within 2 hours, react for 5.5 hours, and cool down to obtain methoxy Polyethylene glycol methacrylate.

Embodiment 3

[0023] Add 110.8000g of methoxypolyethylene glycol (polymerization degree n is 100) in the reaction kettle, add catalyst 4-(dimethylamino)pyridine 5.7014g under stirring, heat to dissolve, weigh 0.0129g of polymerization inhibitor and dissolve in 3.2284 In 1 g of methacrylic acid, connect constant pressure drop liquid and controllable vacuuming device, control the vacuum at 0.099MPa, raise the temperature to 30°C, add methacrylic acid dropwise within 2.5 hours, react for 6 hours, and cool down to obtain methoxy Polyethylene glycol methacrylate.

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

Disclosed is a method for preparing methoxy polyethylene glycol methacrylate-styrene polymer under high controllable vacuum degree, relating to the technical field of the synthesis of organic macromolecule through chemical esterification. The method takes methoxy polyethylene glycol at certain polymerization degree and methacrylic acid as raw materials, 4-dimethylaminopyridine as catalyzer and at least one of nitroxyl radical piperidone, toluquinone and hydroquinone as retardant. When the reaction begins, the methacrylic acid in which the retardant is dissolved is added into the reaction kettle drop by drop within 1-3 hours, and water produced in the esterification process is brought away through specific controllable vacuum degree, thus pushing the reaction equation forward towards the positive direction; wherein the specific vacuum degree and the reaction temperature are key factors for controlling the esterification rate and the reaction temperature depends on the vacuum degree of the system. The invention prepares methoxy polyethylene glycol methacrylate-styrene polymer through controllable vacuum degree mode and is moderate in reaction conditions and does not use organic solvent, thus avoiding the step of post processing.

Description

technical field [0001] The invention relates to the field of organic polymer chemistry, in particular to an esterification method for preparing methoxypolyethylene glycol methacrylate under controllable high vacuum. Background technique [0002] Polycarboxylate water reducer is a new type of high-efficiency water reducer and a core technical material in the preparation of high performance concrete. Compared with the first two generations of lignosulfonate ordinary water reducers and the second generation of high-efficiency water reducers represented by naphthalene and melamine, polycarboxylate high-performance water reducers have hyperdispersibility and can prevent Concrete loses slump over time, does not cause obvious retardation, and has the characteristics of low dosage, high water-reducing performance, and environmental protection. The performance of the water reducer can be adjusted through molecular design, selection of monomer type and ratio, polymerization process c...

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
IPC IPC(8): C08G65/48C08G65/332C07C69/54
Inventor 肖国民周金能许泽宁
Owner SOUTHEAST UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap