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Preparation method of polycarboxylic acids high efficiency water reducer

A high-efficiency water-reducing agent and polycarboxylic acid-based technology, applied in the field of chemical preparation, can solve the problems that cannot meet the needs of the development of high-performance concrete, and achieve the effects of increased water-reducing rate, simplified production process, and long release time

Inactive Publication Date: 2011-04-20
ANHUI ZHONGTIE ENGINEER MATERIAL SCI & TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 exploring polycarboxylate-based water reducers through molecular approaches, relevant academic papers and research literature published in China, And according to the published Chinese patent literature, most of the domestic development of polycarboxylate superplasticizer products is in the laboratory stage, and there are still very few manufacturers that actually form products, which is far from meeting the needs of the development of high-performance concrete.

Method used

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

Examples

Experimental program
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Effect test

Embodiment 1

[0017] Preparation of polycarboxylic acid water reducing agent:

[0018] The first step, the esterification reaction: Take 300g (0.1mol) of MPEG (molecular weight 3000) and put it into a 1000ml four-necked flask equipped with a breakpoint thermometer, condenser, and stirrer. When the reaction temperature reaches about 70℃, add resistance Polymerizing agent hydroquinone and hydroquinone monomethyl ether each 0.4g, stir well, then add 57.6g (0.8mol) of acrylic acid, continue to heat up to 90℃, add 4.29g of catalyst concentrated sulfuric acid, and pass nitrogen as The water-carrying agent is reacted at 120°C for 10 hours to obtain the esterified macromonomer, namely methoxy polyethylene glycol monomethyl ether acrylate.

[0019] The second step, polymerization reaction: add a proper amount of distilled water into a 1000ml four-necked flask equipped with a breakpoint thermometer, a condenser, and a stirrer, and then pass in nitrogen. At 85°C, use a constant flow pump to dropwise add 66...

Embodiment 2

[0022] The industrial production of the esterified 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.

[0025] (3) Weigh 990kg of methoxy polyethylene glycol monomethyl ether (MPEG) and put it into the reactor. When the temperature rises to about 70℃, add the inhibitor hydroquinone and hydroquinone monomethyl ether. 2.64kg, stir evenly, and add 190.1kg of acrylic acid.

[0026] (4) When the temperature is raised to 90°C, add 14.16kg of concentrated sulfuric acid as a catalyst, and pass in nitrogen as a water-carrying agent. After reacting at 120°C for 10 hours, an esterified macromonomer, methoxy polyethylene glycol monomethyl ether acrylic acid, is obtained. ester.

[0027] (5) The prepared esteri...

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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 series superplasticizer. Background technique [0002] Polycarboxylic acid high-performance water-reducing agent has many unique properties such as low content, high dispersibility, small slump loss, large freedom of molecular structure, and easy modification. In the past ten years in China, the main products for the research and development of new superplasticizers and superplasticizers are naphthalenesulfonate methane condensate and sulfamate condensate, and the research on polycarboxylic acid-based water reducers Whether in terms of raw material selection, production technology or performance improvement, it started late. Although domestic researchers have achieved certain results in exploring polycarboxylic acid-based water-reducing agent products through molecular channels, from relevant academic papers and research documents published...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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