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Polyethylene glycol methyl ether maleate, and preparation method and application thereof

A technology of polyethylene glycol monomethyl ether and maleic acid, which is applied in the field of concrete admixture synthesis, can solve the problems of cumbersome post-processing such as storage, recycling, and discharge, large equipment investment, and high risk, and it is easy to achieve reaction conditions The effect of control, less investment in equipment, and less by-products

Inactive Publication Date: 2014-02-19
GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ma Baoguo and others used toluene as the water-carrying agent to synthesize dipolyethylene glycol monomethyl ether maleate. This method introduces toluene, and the macromonomer cannot be directly used in the preparation of water-soluble superdispersion, and the solvent is toxic and volatile. , the risk is high, so the equipment investment is large, and the post-processing such as storage, recycling, and discharge is cumbersome

Method used

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  • Polyethylene glycol methyl ether maleate, and preparation method and application thereof
  • Polyethylene glycol methyl ether maleate, and preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Add 50 g of polyethylene glycol monomethyl ether with a molecular weight of 1000 and 2.131 g of maleic anhydride into a three-necked flask, heat up to 60° C., melt, and add polymerization inhibitor p-benzoquinone 0.104 g, hydroquinone monomethyl ether 0.104 g, Hydroquinone 0.104g, catalyst p-toluenesulfonic acid 2.09g, after stirring evenly, pass nitrogen, react at 90 ° C for 2 hours, so that most of the reaction products form maleic acid monopolyethylene glycol monomethyl ether ester, and then heat up to 140 ℃, constant temperature stirring reaction for 7.5h, that is, bis(polyethylene glycol monomethyl ether) maleate is obtained. Denoted as MADMPEG-1.

Embodiment 2

[0036] 50g of the monomer polyethylene glycol monomethyl ether with a molecular weight of 350 and 4.245g of maleic anhydride were added to the three-necked flask, the temperature was raised to 60°C, melted, 1.08g of the polymerization inhibitor hydroquinone and 1.627g of the catalyst concentrated sulfuric acid were added, and the mixture was stirred. After homogeneous, pass nitrogen and react at 90 °C for 2 hours, so that most of the reaction products form maleic acid monopolyethylene glycol monomethyl ether ester, then heat up to 145 °C, and stir at constant temperature for 4 hours to obtain bis-polyethylene maleate. Glycol monomethyl ether ester, denoted as MADMPEG-2.

Embodiment 3

[0038] 50g of the monomer polyethylene glycol monomethyl ether with a molecular weight of 500 and 3.502g of maleic anhydride were added to the three-necked flask, the temperature was raised to 60°C, melted, and the polymerization inhibitor hydroquinone 0.54g, p-benzoquinone 0.53g, and a catalyst were added. 1.87g of p-toluenesulfonic acid, after stirring evenly, pass nitrogen, and react at 90 °C for 2 hours, so that most of the reaction products form maleic acid monopolyethylene glycol monomethyl ether ester, then the temperature is raised to 150 °C, and the reaction is stirred at a constant temperature for 5 hours. That is, bis-polyethylene glycol monomethyl ether maleate is obtained, which is designated as MADMPEG-3.

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Abstract

The invention belongs to the concrete additive synthesis field, and concretely discloses a polyethylene glycol methyl ether maleate used for synthesizing a hyper-dispersant, and a preparation method and an application thereof. The preparation method concretely comprises the following steps: adding maleic anhydride and polyethylene glycol monomethyl ether into a reactor, heating to 60DEG C, and carrying out melt mixing; adding a polymerization inhibitor and a catalyst, uniformly stirring, letting in nitrogen, reacting at 90DEG C for 2h to generate an intermediate polyethylene glycol monomethyl ether maleate; and heating to 140-180DEG C, and carrying out a constant temperature stirring reaction for 4-10h to obtain the polyethylene glycol methyl ether maleate. The polyethylene glycol methyl ether maleate prepared through the method can be used for synthesizing hyper-dispersants. The preparation method has the advantages of easy operation, no need of a water carrying agent, simple reaction technology, high esterification rate, few byproudcts, no need of post-tretmetn, realization of the implementation of the reactions under normal pressure, mild reaction conditions, less apparatus investment and low energy consumption.

Description

technical field [0001] The invention belongs to the field of concrete admixture synthesis, in particular to a maleic acid bis(polyethylene glycol monomethyl ether) ester used for synthesizing a hyperdispersant and a preparation method and application thereof. Background technique [0002] At present, the molecular structure of concrete hyperdispersant is mostly composed of the main chain containing carboxyl structure and the long side chain containing active functional macromonomers. There are many reports on maleic anhydride as a raw material for the synthesis of esterification active macromonomers for concrete hyperdispersants, among which the synthesis of maleic anhydride monopolyethylene glycol monomethyl ether ester is the most common. The Chinese invention patent with the application number of 201010515271.2 uses toluenesulfonic acid as a catalyst and an inert gas as a water-carrying agent to synthesize polyethylene glycol monomethyl ether maleic acid active macromonom...

Claims

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Application Information

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IPC IPC(8): C08G65/48C04B24/32
Inventor 廖兵刘海露庞浩郑景新黄健恒程劲松梁潇
Owner GUANGZHOU CHEM CO LTD CHINESE ACADEMY OF SCI
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