Branching polyether macromonomer and preparation method thereof

A branched polyether and macromonomer technology, applied in the field of reactive polyether synthesis, can solve problems such as limited effect and steric hindrance to be further improved, and achieves improved steric hindrance, high yield, and avoidance of steric hindrance. Effects of Environmental Pollution

Inactive Publication Date: 2012-05-02
JIANGSU SUBOTE MATERIAL +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the polyether with double branched chain structure has a limited effect in polycarboxylate water reducers, and the steric hindrance needs to be further improved.

Method used

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  • Branching polyether macromonomer and preparation method thereof
  • Branching polyether macromonomer and preparation method thereof
  • Branching polyether macromonomer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a flask with a reflux condenser, a thermometer and a stirrer, add 60.5g of allylamine, place the flask in a water bath at 30°C, stir to keep the temperature constant, then slowly add 74.2g of glycidol dropwise to the flask for 4 hours , After the dropwise addition, continue to keep stirring for 2h, and the reaction ends. Then the temperature of the water bath was raised to 60°C, and the excess allylamine was removed from the product by distillation under reduced pressure, and the product was recovered, and the product remaining in the flask was the intermediate.

[0028] Put 121g of the intermediate synthesized above into a 2L dry stainless steel autoclave, add 0.09g of sodium metal, stir to dissolve, and seal the autoclave. Replace the air in the kettle with nitrogen three times, then evacuate the reactor to below -0.09MPa, turn on the heating, raise the temperature to 120°C, and keep the reactor continuously vacuumed for 30 minutes, then stop, and then continue to ...

Embodiment 2

[0031] In the flask with reflux condenser, thermometer and stirrer, add 71.9g of allylamine, place the flask in a 45°C water bath, stir and keep constant temperature, then slowly add 78.5g of glycidol dropwise to the flask for 6h , After the dropwise addition, continue to insulate and stir for 3h, and the reaction ends. Then the temperature of the water bath was raised to 60°C, and the excess allylamine was removed from the product by distillation under reduced pressure, and the product was recovered, and the product remaining in the flask was the intermediate.

[0032] Put 98g of the above synthesized intermediate in a 2L dry stainless steel autoclave, add 4.9g of potassium hydroxide, stir to dissolve, and seal the autoclave. Replace the air in the kettle with nitrogen three times, then evacuate the reactor to below -0.09MPa, turn on the heating, raise the temperature to 130°C, and keep the reactor continuously vacuumed for 30 minutes, then stop, and then continue to slowly f...

Embodiment 3

[0034] In a flask with a reflux condenser, a thermometer and a stirrer, add 67.3g of allylamine, place the flask in a water bath at 50°C, stir to keep the temperature constant, then slowly add 79.2g of glycidol dropwise to the flask for 8h , After the dropwise addition, continue to insulate and stir for 4h, and the reaction ends. Then the temperature of the water bath was raised to 60°C, and the excess allylamine was removed from the product by distillation under reduced pressure, and the product was recovered, and the product remaining in the flask was the intermediate.

[0035]Put 54g of the intermediate synthesized above into a 2L dry stainless steel autoclave, add 0.56g of sodium hydride, stir to dissolve, and seal the autoclave. Replace the air in the kettle with nitrogen three times, then evacuate the reactor to below -0.09MPa, turn on the heating, raise the temperature to 110°C, and keep the reactor continuously vacuumed for 30 minutes, then stop, and then continue to s...

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Abstract

The invention provides a branching polyether macromonomer and a preparation method thereof. The structural formula of the branching polyether macromonomer is shown as a formula (I), and the preparation method comprises the following steps of: directly performing quantitative ring-opening addition reaction on allylamine used as a raw material and glycidol to obtain an intermedium of which the tail end contains double hydroxy groups, adding an alkoxylation catalyst by taking the intermedium as initiator, and performing alkoxylation reaction by taking an epoxy compound as a raw material to prepare the branching polyether macromonomer. The preparation method is easy to operate, the branching polyether macromonomer is high in yield, and organic solvents are not used, so environmental pollution is avoided.

Description

technical field [0001] The invention relates to a method for preparing a branched polyether macromonomer, which belongs to the technical field of reactive polyether synthesis. Background technique [0002] In the molecular structure of reactive polyether, one end is an unsaturated double bond with polymerization activity, and the other end is a long polyether chain. Under this condition, it is induced to generate free radicals, and undergoes free radical copolymerization with other unsaturated monomers to form a copolymer with a comb structure. Such comb copolymers are widely used as concrete superplasticizers, flocculants, scale inhibitors, pigment and coating dispersants, detergents, thickeners, etc., especially as superplasticizers for concrete. The performance advantage is obvious and comprehensive, and it has qualitatively improved the comprehensive performance of concrete. [0003] At present, concrete superplasticizers are mainly prepared by copolymerizing reactive ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08F283/06C04B24/16C04B103/32
Inventor 冉千平杨勇刘加平缪昌文张志勇乔敏
Owner JIANGSU SUBOTE MATERIAL
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