Process of preparing oxyalkylene-base unsaturated ester polymer

A polyoxyalkylene-based, unsaturated technology, applied in the field of preparing polyoxyalkylene-based unsaturated esters, can solve the problems of unfavorable industrial production and long reaction time, and achieve easy control of synthesis conditions, save reaction time, and facilitate industrial production Effect

Inactive Publication Date: 2007-12-19
SHENZHEN OCEANPOWER NEW MATERIALS TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] This shows that the reaction time of the above polyoxyalkylene-based unsaturated ester macromonomer is long, which is very unfavorable to suitability for industrialized production.

Method used

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  • Process of preparing oxyalkylene-base unsaturated ester polymer
  • Process of preparing oxyalkylene-base unsaturated ester polymer
  • Process of preparing oxyalkylene-base unsaturated ester polymer

Examples

Experimental program
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Effect test

Embodiment 1

[0032]Add 90 g of xylene solution dissolved with 1 g of sodium methoxide into the reactor, and after evacuating the reactor, replace it with nitrogen for no less than 2 times, draw in 50 g of methanol under negative pressure, raise the temperature to 135°C, and pass through ethylene oxide, Keep the reaction at 135°C and 0.05Mpa pressure for 1 hour, then cool the reaction mixture to room temperature, add 1.5g of sodium hydroxide to the reaction vessel, raise the temperature to 110°C, and keep the pressure at 20mmHg for 1.5 hours to dehydrate. Then the nitrogen pressure was increased to 0.5Mpa, and a solution of 100g methacryloyl chloride and 60g xylene was added to the mixture four times within 1 hour and stirred, and a solution of 25g methacryloyl chloride and 15g xylene was added each time. After 4 hours from the start of the reaction, when the alkalinity of the mixture decreased to a stable value, the mixture was neutralized with glacial acetic acid, and after the by-product ...

Embodiment 2

[0034] Add 90 g of xylene solution dissolved with 1 g of potassium methylate into the reactor, and after evacuating the reactor, replace it with nitrogen for no less than 2 times, draw in 50 g of methanol under negative pressure, raise the temperature to 135°C, and pass through ethylene oxide, Keep the reaction at 135°C and 0.05Mpa pressure for 1 hour, then cool the reaction mixture to room temperature, add 1.5g of potassium hydroxide to the reaction vessel, raise the temperature to 110°C, and keep the pressure at 20mmHg for 1.5 hours to dehydrate. Then the nitrogen pressure was increased to 0.5Mpa, and a solution of 100g of methacryloyl chloride and 60g of xylene was added to the mixture four times within 1 hour and stirred, and a solution of 25g of acryloyl chloride and 15g of xylene was added each time. After 4 hours from the start of the reaction, when the alkalinity of the mixture decreased to a stable value, the mixture was neutralized with glacial acetic acid, and after ...

Embodiment 3

[0036] Add 90 g of xylene solution in which 1 g of sodium ethoxide is dissolved in the reactor. After evacuating the reactor, replace it with nitrogen for no less than 2 times, draw in 50 g of ethanol under negative pressure, raise the temperature to 135 ° C, and pass through ethylene oxide. Keep the reaction at 135°C and 0.05Mpa pressure for 1 hour, then cool the reaction mixture to room temperature, add 1.5g of sodium hydroxide to the reaction vessel, raise the temperature to 110°C, and keep the pressure at 20mmHg for 1.5 hours to dehydrate. Then the nitrogen pressure was increased to 0.5Mpa, and a solution of 100g methyl methacrylate and 60g xylene was added to the mixture in four times within 1 hour and stirred, and each addition of 25g methyl methacrylate and 15g xylene solution. After 4 hours from the start of the reaction, when the alkalinity of the mixture decreased to a stable value, the mixture was neutralized with glacial acetic acid, and after the by-product salts ...

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Abstract

The present invention discloses process of preparing polyoxyalkylene-base unsaturated ester. The process is a one-step active anionic polymerization process including three steps of dewatering the reactant with molecular sieve, reaction and separating side product. The polyoxyalkylene-base unsaturated ester has controllable molecular weight for different requirements, and the process has easy control in the synthesis condition, easy application in industrial production and short reaction period. The polyoxyalkylene-base unsaturated ester may be copolymerized with hydrophilic and lipophilic monomer to form amphiphilic graft copolymer with polyoxyalkylene-base long branched chain, with the ratio between the hydrophilic groups and the lipophilic groups being adjustable for obtain products with different performances.

Description

【Technical field】 [0001] The invention relates to a method for preparing polyoxyalkylene-based unsaturated esters, in particular to a method for synthesizing polyoxyalkylene-based unsaturated esters through living anion polymerization in one step. 【Background technique】 [0002] The discovery of living polymerization provides the necessary means for polymer synthesis technology to move from the realm of freedom to the realm of necessity, and what modern polymer chemistry is pursuing is how to realize the designability of molecular structure through living polymerization. Macromonomers (oligomers with polymerizable double bonds at the ends of molecular chains) have a clear molecular structure and polymerizability, and in the design of macromolecules, two completely opposite properties can be synthesized to synthesize many compounds with predetermined structures . As a kind of macromonomer, polyoxyalkylene-based unsaturated ester macromonomer is necessary for the preparation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/26
Inventor 苏花平何唯平
Owner SHENZHEN OCEANPOWER NEW MATERIALS TECH
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