Preparation method of polycarboxylic acids high efficiency water reducer

A high-efficiency water-reducing agent and a polycarboxylic acid-based technology, which is applied in the field of chemical preparation, can solve problems such as the inability to meet the needs of the development of high-performance concrete, and achieve the effects of improving the water-reducing rate, simplifying the production process, and enhancing the slump retention performance.

Inactive Publication Date: 2009-09-16
ANHUI ZHONGTIE ENGINEER MATERIAL SCI & TECH CO LTD
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Problems solved by technology

In the past ten years in China, the main products of research and development of new high-efficiency water reducers and superplasticizers are naphthalenesulfonate formazan condensates and sulfamate condensates, etc., while the research on polycarboxylate water reducers Whether it is in terms of raw material selection, production technology or performance improvement, it started late. Although domestic researchers have achieved certain results in explorin

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  • Preparation method of polycarboxylic acids high efficiency water reducer
  • Preparation method of polycarboxylic acids high efficiency water reducer

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Effect test

Embodiment 1

[0017] Preparation of polycarboxylate water reducer:

[0018] The first step, esterification reaction: take 300g (0.1mol) of MPEG (molecular weight 3000), put it into a 1000ml four-necked flask equipped with a breakpoint thermometer, a condenser tube, and a stirrer, and add a resistor when the reaction temperature reaches about 70°C. Polymerizing agent hydroquinone and hydroquinone monomethyl ether each 0.4g, stir evenly, then add 57.6g (0.8mol) of acrylic acid, when the temperature continues to rise to 90°C, add catalyst concentrated sulfuric acid 4.29g, and pass through nitrogen as Water-carrying agent, after reacting at 120°C for 10 hours, the esterified macromer is methoxy polyethylene glycol monomethyl ether acrylate.

[0019] The second step, polymerization reaction: Add appropriate amount of distilled water in a 1000ml four-neck flask equipped with a breakpoint thermometer, a condensing device, and a stirrer, feed nitrogen, and at 85°C, use a constant flow pump to dropw...

Embodiment 2

[0022] The industrialized production of esterification macromonomer of the present invention is as follows:

[0023] (1) Detection of main raw materials: determination of MPEG hydroxyl value, determination of acrylic acid purity

[0024] (2) The operation of production equipment: including the calibration of thermometers, temperature control equipment, and the sealing of pipelines and reactors, etc.

[0025] (3) Weigh 990kg of methoxypolyethylene glycol monomethyl ether (MPEG), put it into the reaction kettle, and when the temperature rises to about 70°C, add the polymerization inhibitor hydroquinone and hydroquinone monomethyl ether respectively. 2.64kg, stir evenly, and add 190.1kg of acrylic acid.

[0026] (4) When the temperature rises to 90°C, add 14.16 kg of concentrated sulfuric acid as a catalyst, and pass nitrogen gas as a water-carrying agent, and react at 120°C for 10 hours to obtain an esterified macromonomer, namely methoxypolyethylene glycol monomethyl ether acr...

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Abstract

The invention discloses a preparation method of polycarboxylic acids high efficiency water reducer, which includes steps of firstly synthesizing methoxypoly(ethylene glycol) monomethyl ether acrylate large monomer from methoxypoly(ethylene glycol) monomethyl ether and crylic acid which are used as raw materials, then copolymerizing the esterified large monomer and the acrylic acid to prepare the polycarboxylic acids high efficiency water reducer. In the synthesis of the esterified large monomer, hydroquinones and hydroquinone monomethyl ether are employed to coordinatedly blocking polymerization, thereby reducing failure ratio of unsaturated double bond, increasing effective content of the synthesized water reducer, increasing concrete water reducing ratio, and increasing slump retaining performance.

Description

technical field [0001] The invention belongs to a chemical preparation method, in particular to a preparation method of a polycarboxylic acid-based high-efficiency water reducer. Background technique [0002] Polycarboxylate high-performance water reducer has many unique properties such as low dosage, high dispersibility, small slump loss, large degree of freedom in molecular structure, and easy modification. In the past ten years in China, the main products of research and development of new high-efficiency water reducers and superplasticizers are naphthalenesulfonate formazan condensate and sulfamate condensate, etc., while the research on polycarboxylate water reducer Whether it is in terms of raw material selection, production process or performance improvement, it started late. Although domestic researchers have achieved certain results in exploring polycarboxylate water reducer products through molecular approaches, relevant academic papers and research literature publ...

Claims

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Application Information

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IPC IPC(8): C08F299/02C04B24/26C04B103/30
Inventor 黄玉华江常青汪志勇黄海周春娥
Owner ANHUI ZHONGTIE ENGINEER MATERIAL SCI & TECH CO LTD
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