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Solid superacid catalyzed esterification synthesis of methoxy polyethylene glycol methacrylic acid ester

A technology of methoxy polyethylene glycol and monomethacrylate, which is applied in the field of synthesis of methoxy polyethylene glycol methacrylate and can solve the problems of difficult separation of products, dark color of products and the like

Inactive Publication Date: 2012-02-08
湖北鑫汇生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Japanese Patent Laid-Open No. 2000-233956 utilizes p-toluene sulfonate to synthesize methoxypolyethylene glycol methacrylate as a macromer for preparing polycarboxylic acid water reducer, but p-toluene sulfonate results in a product with a darker color. And it is not easy to separate from the product and other shortcomings; CN00103594.0 introduces a preparation method of polycarboxylate water reducer, the macromonomer used in the synthesis of water reducer adopts methyl polyoxyethylene ether, methyl methacrylate, p-phenylene Diphenol and p-toluenesulfonic acid are prepared at 85±3°C; Xi Qiang et al. published patent CN 101434465A utilizes polyethylene glycol monomethyl ether and maleic anhydride, uses p-toluenesulfonic acid as a catalyst, and feeds nitrogen at 80 React at ~90°C to obtain a macromonomer; in the published patent CN 101544729A such as Li Jinbiao, allyl polyethylene glycol and acrylic acid are used to prepare allyl polyethylene glycol acrylate, and are used to prepare monomers for water reducers; while using solid super acid SO 4 2- / ZrO 2 Esterification of methoxypolyethylene glycol monomethacrylate as a macromonomer for the synthesis of polycarboxylate superplasticizers has not been reported at home and abroad

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Install a stirring device, a condenser, a water separator and a thermometer on a 250ml three-necked flask. Add the methacrylic acid of 1.1mol, the methoxy polyethylene glycol (molecular weight 400) of 1.0mol, the solid superacid SO of 3.0% (relative to the quality of total feeding) 4 2- / ZrO 2 Catalyst, 20% (relative to the quality of the total feed) of water-carrying agent cyclohexane, 0.5% (relative to the quality of methacrylic acid) of hydroquinone, carry out air bath heating with an electric kettle, and start stirring. From the water-carrying agent and the water generated by the reactant to azeotrope, react at a temperature of 85°C for 20 hours. Under normal pressure, the water is removed by azeotropy through the water separator, and the water agent is returned to the three-necked bottle for recycling. The esterified product is filtered to separate the solid superacid SO 4 2- / ZrO 2 Catalyst, filtrate recovers hexanaphthene through vacuum distillation and can...

Embodiment 2

[0033] Install a stirring device, a condenser, a water separator and a thermometer on a 250ml three-necked flask. Add the methacrylic acid of 1.2mol, the methoxypolyethylene glycol (molecular weight 2000) of 1.0mol, the solid superacid SO of 1.5% (relative to the quality of total charging) 4 2- / ZrO 2 Catalyst, 80% (relative to the quality of total feeding) water-carrying agent xylene, 0.25% (relative to the quality of methacrylic acid feeding) of hydroquinone, carry out air bath heating with electric kettle, start stirring. From the azeotropic start of the water-carrying agent and the water generated by the reactants, the reaction was carried out at a temperature of 135° C. for 12 hours. Under normal pressure, the water is removed by azeotropy through the water separator, and the water agent is returned to the three-necked bottle for recycling. The esterified product is filtered to separate the solid superacid SO 4 2- / ZrO 2 Catalyst, filtrate reclaims xylene through va...

Embodiment 3

[0036] Install a stirring device, a condenser, a water separator and a thermometer on a 250ml three-necked flask. Add the methacrylic acid of 1.5mol, the methoxypolyethylene glycol (molecular weight 4000) of 1.0mol, the solid superacid SO of 5.0% (relative to the quality of total charging) 4 2- / ZrO 2 Catalyst, 80% (relative to the quality of total feeding) of water-carrying agent toluene, 0.2% (relative to the quality of methacrylic acid feeding) of hydroquinone, carry out air bath heating with electric kettle, start stirring. From the azeotropic start of the water-carrying agent and the water generated by the reactants, the reaction was carried out at a temperature of 145° C. for 6 hours. Under normal pressure, the water is removed by azeotropy through the water separator, and the water agent is returned to the three-necked bottle for recycling. The esterified product is filtered to separate the solid superacid SO 4 2- / ZrO 2 Catalyst, filtrate reclaims toluene through...

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PUM

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Abstract

The invention discloses a solid superacid catalyzed esterification synthesis method of methoxy polyethylene glycol methacrylic acid ester. Methoxy polyethylene glycol and methacrylic acid are treated with a esterification reaction under conditions of solid superacid catalyst SO4<2-> / ZrO2, polymerization inhibitor and water carrying agent. After the reaction, the solid superacid is removed by filtering separation; a filtrate is treated with reduced pressure distillation to recover the water carrying agent. Obtained high purity methoxy polyethylene glycol mono methacrylic acid ester is a macromonomer methoxy polyethylene glycol mono methacrylic acid ester for synthesizing polycarboxylic water carrying agent. The recovered water carrying agent and solid superacid SO4<2-> / ZrO2 can be reused. A conversion based on methoxy polyethylene glycol reaches higher than 98.2%, and an ester yield is higher than 98%.

Description

technical field [0001] The invention relates to the field of fine chemicals, and relates to a method for synthesizing methoxy polyethylene glycol methacrylate (MPEGMA). The synthesized macromonomer is used in the synthesis of polycarboxylate water reducer. Background technique [0002] At present, esters of synthetic methoxypolyethylene glycol systems are widely used in polycarboxylate superplasticizer products. Japanese Patent Laid-Open No. 2000-233956 utilizes p-toluene sulfonate to synthesize methoxypolyethylene glycol methacrylate as a macromer for preparing polycarboxylic acid water reducer, but p-toluene sulfonate results in a product with a darker color. And it is not easy to separate from the product and other shortcomings; CN00103594.0 introduces a preparation method of polycarboxylate water reducer, the macromonomer used in the synthesis of water reducer adopts methyl polyoxyethylene ether, methyl methacrylate, p-phenylene Diphenol and p-toluenesulfonic acid are ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48C07C69/54C07C67/08C08F290/06C04B24/26C04B103/30
Inventor 廖国胜李厚祥
Owner 湖北鑫汇生物科技有限公司
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