Method for preparing polycarboxylic acid water reducer macromer

A technology of water reducing agent and macromonomer, which is applied in the field of preparation of polycarboxylate water reducing agent intermediates, can solve the problems of complex reaction equipment and unstable reaction system, and achieve simple reaction equipment, stable reaction, and esterification rate. high effect

Inactive Publication Date: 2010-12-01
浙江五龙新材股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the reaction conditions described in the invention are gentle, no organic solvent is used, and the step of post-treatment is exempted, the reaction equipment is more complicated, and the reaction principle is to take the water generated by unreacted methacrylic acid, so there is methacrylic acid recovery problem; at the same time, in the reaction process, methacrylic acid is constantly drawn out, and the reaction system is not stable

Method used

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  • Method for preparing polycarboxylic acid water reducer macromer

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In the reactor with good airtightness, under the condition of constant stirring, add 1000Kg of molecular weight 1000 polyethylene glycol monomethyl ether, 1.22Kg of hydroquinone, 1.22Kg of phenothiazine, and 350Kg of methacrylic acid. 15-30min, then slowly add 20Kg of concentrated sulfuric acid, and start to heat up. When the temperature reaches 100℃, close all the vent valves of the reactor and blow in nitrogen to keep the pressure in the reactor at 0.1Mpa. Continue to heat up to 125-130°C and keep it at this temperature for 6 hours. After the reaction is completed, polyethylene glycol monomethyl ether methacrylate, which is a macromonomer of polycarboxylic acid water reducing agent, is obtained. After the reaction, the measured esterification rate was 98.76%.

Embodiment 2

[0024] In a relatively tightly sealed reaction vessel, under the condition of constant stirring, add 1000Kg of molecular weight of 1000 polyethylene glycol monomethyl ether, 1.75Kg of hydroquinone, 290Kg of acrylic acid, and stir for 15-30min, and then slowly add concentrated Sulfuric acid 9.7Kg, p-toluenesulfonic acid 9.7Kg, and start to heat up. When the temperature reaches 100°C, close all vent valves of the reactor and blow in nitrogen to keep the pressure in the reactor at 0.2Mpa. Continue to heat up to 125-130°C and keep it at this temperature for 6 hours. After the reaction is completed, polyethylene glycol monomethyl ether acrylate, which is a macromonomer of polycarboxylic acid water reducing agent, is obtained. After the reaction, the measured esterification rate was 99.36%.

Embodiment 3

[0026] In a relatively tightly sealed reactor, under the condition of constant stirring, add 1000Kg of molecular weight 1000 polyethylene glycol monomethyl ether, 1.85Kg of p-benzoquinone, and 330Kg of methacrylic acid, stir for 15-30min, and then slowly add Concentrated sulfuric acid was 21.5Kg and started to heat up. When the temperature reached 100°C, all vent valves of the reactor were closed, and carbon dioxide gas was introduced to keep the pressure in the reactor at 0.1Mpa. Continue to heat up to 125-130°C and keep it at this temperature for 6 hours. After the reaction is completed, polyethylene glycol monomethyl ether methacrylate, which is a macromonomer of polycarboxylic acid water reducing agent, is obtained. After the reaction, the measured esterification rate was 98.97%.

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Abstract

The invention discloses a method for preparing a polycarboxylic acid water reducer intermediate, namely the method for preparing polyethylene glycol monomethyl ether methacrylate or polyethylene glycol monomethyl ether acrylate, in particular the method for preparing a polycarboxylic acid water reducer macromer. The method for preparing the polycarboxylic acid water reducer macromer comprises the following steps of: putting polyethylene glycol monomethyl ether, methacrylic acid or acrylic acid into a reaction kettle; adding a polymerization inhibitor and a catalyst into the reaction kettle, stirring and heating the mixture; raising the temperature of esterificatin reaction, then introducing inert gas into the reaction kettle, and keeping certain pressure in the reaction kettle; and then preserving the heat for hours to obtain the polyethylene glycol monomethyl ether methacrylate or the polyethylene glycol monomethyl ether acrylate. The invention mainly aims to provide the simple and fast method for preparing the polycarboxylic acid water reducer macromer so as to overcome the defects of the conventional production technique and process of the macromer.

Description

Technical field [0001] The present invention is a preparation method of polycarboxylic acid water reducing agent intermediate, namely the preparation method of polyethylene glycol monomethyl ether methacrylate or polyethylene glycol monomethyl ether acrylate, that is, polycarboxylic acid reducing agent Preparation method of aqueous macromonomer. Background technique [0002] Polycarboxylate water reducer is a new type of concrete additive. It not only has higher concrete water reduction rate and better concrete fluidity, but the most important thing is the slump of fresh concrete mixed with polycarboxylate water reducer. The drop loss is small, the strength of the formed concrete is higher, the later drying shrinkage of the concrete is relatively small, and the corrosion resistance, aging resistance and other aspects have superior performance. At the same time, in the production process of polycarboxylic acid water reducing agent, its molecular structure has strong designability...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/48C04B24/32C04B103/30
Inventor 张建锋王家丰宋永良李秋平李洪涛丁继英
Owner 浙江五龙新材股份有限公司
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