Preparation method of polycarboxylate water reducer with intensively-distributed carboxyl groups and high water reduction performance, product thereof, and application of product

A technology of polycarboxylate and water reducer, which is applied in the field of preparation of polycarboxylate water reducer, can solve the problem of uncontrollable arrangement and distribution of carboxyl groups and polyether side chains, and achieve good application prospects

Active Publication Date: 2015-11-11
SHANGHAI TAIJIE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the prior art, most of the literature reports on the synthesis of polycarboxylate superplasticizers using unsaturated alcohol polyethers as raw materials are one-step methods, that is, under certain reaction conditions, unsaturated alcohol polyethers and unsaturated carboxylic acids are directly copolymerized by free radicals. Reaction, synthesis of polycarboxylate water reducer, this type of method can not control the arrangement and distribution of carboxyl and polyether side chains, only the proportion of functional groups can be controlled, and the unsuitable distribution and arrangement of carboxyl and polyether side chains may bring polycarboxylate Negative Effects on Superplasticizer Performance

Method used

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preparation example Construction

[0027] In the first aspect, the present invention provides a method for preparing a polycarboxylate water-reducer with concentrated carboxyl distribution and high water-reducing performance, comprising the following steps:

[0028] (1) Add a certain amount of low molecular weight unsaturated carboxylic acid compounds into the reaction vessel, and add a certain amount of catalyst, react for 15min to 90min, and complete the polymerization reaction to obtain an unsaturated carboxylic acid polymer with a number average molecular weight range of 600 ~3000;

[0029] (2) Add the unsaturated carboxylic acid polymer, unsaturated polyether monomer and unsaturated sulfonate or polyether monomer unsaturated carboxylic acid ester prepared in step (1) to the reaction vessel, add distilled water, and mechanically stir , fully dissolved to form a clear solution, adding the initiator, adding the chain transfer agent aqueous solution dropwise at a constant rate, the dropping time is controlled ...

Embodiment 1

[0047] Add 500 g of acrylic acid and 5.0 g of hydrogen peroxide into the reaction vessel, and react at 50° C. for 30 min to prepare a carboxylic acid polymer through polymerization. Add 2000g isopentenol polyoxyethylene ether (TPEG, molecular weight 2400) and 20g sodium methacrylate sulfonate at one time, add 2000g distilled water, stir mechanically at a reaction temperature of 60°C, fully dissolve to form a clear solution, add the initiator 25.0 g of ammonium sulfate, 10 g of chain transfer agent mercaptoacetic acid was added dropwise at a constant rate, the dropping time was controlled at 150 min, and the reaction was continued for 60 min after the dropping was completed, and the reaction was stopped. Add 30% NaOH aqueous solution to neutralize to pH 5-7, add distilled water to adjust the solid content to 30%, and obtain a polycarboxylate water reducer with concentrated carboxyl groups and high water reducing performance.

Embodiment 2

[0049] Add 500 g of methacrylic acid and 6.0 g of hydrogen peroxide into the reaction vessel, and react at 55° C. for 30 minutes to prepare a carboxylic acid polymer through polymerization. Add 2000g isopentenol polyoxyethylene ether (TPEG, molecular weight 2400) and 20g sodium methacrylate sulfonate at one time, add 2000g distilled water, stir mechanically at a reaction temperature of 60°C, fully dissolve to form a clear solution, add the initiator 25.0 g of ammonium sulfate, 10 g of chain transfer agent mercaptoacetic acid was added dropwise at a constant rate, the dropping time was controlled at 150 min, and the reaction was continued for 60 min after the dropping was completed, and the reaction was stopped. Add 30% NaOH aqueous solution to neutralize to pH 5-7, add distilled water to adjust the solid content to 30%, and obtain a polycarboxylate water reducer with concentrated carboxyl groups and high water reducing performance.

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Abstract

The invention provides a preparation method of a polycarboxylate water reducer with intensively-distributed carboxyl groups and high water reduction performance. The preparation method comprises the following steps: adding a low molecular weight unsaturated carboxylic acid compound, adding a catalyst, and reacting to obtain an unsaturated carboxylic acid polymer; adding the unsaturated carboxylic acid polymer, an unsaturated polyether monomer and an unsaturated sulfonate or polyether monomer unsaturated carboxylate, adding distilled water, mechanically stirring for fully dissolving to form a clarified solution, adding an initiator, adding an aqueous solution of a chain transferring agent in a dropwise manner at a constant speed, continuously reacting after the dropwise addition ends, and stopping the reaction to obtain polycarboxylic acid with intensively-distributed carboxyl groups; and adding an alkali solution to the polycarboxylic acid with intensively-distributed carboxyl groups, neutralizing to the pH value of 5-7, and adding water to dilute in order to obtain the product. The invention also provides the polycarboxylate water reducer prepared through the method, and an application of the polycarboxylate water reducer in concrete. The polycarboxylate water reducer has better initial fluidity and ageing fluidity than common polycarboxylate water reducers, and has very good application prospect.

Description

technical field [0001] The invention belongs to the field of concrete admixtures, and in particular relates to a preparation method, product and application of a polycarboxylate water-reducer with concentrated carboxyl groups and high water-reducing performance. Background technique [0002] Polycarboxylate superplasticizer, also known as superplasticizer, was first patented by Kao Corporation of Japan in the 1980s. After rapid development, it has basically replaced naphthalene-based superplasticizers in developed countries such as Europe, America and Japan. And aliphatic superplasticizers, the market share of domestic polycarboxylate superplasticizers has exceeded 50%, and is expected to reach 80% of the total amount of concrete admixtures within a few years. [0003] Polycarboxylate water reducers are divided into ester monomer water reducers and ether monomer water reducers. Among them, the raw materials used in ether monomer water reducers are unsaturated alcohol polyeth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F291/06C08F228/02C08F2/38C04B24/16C04B103/30
Inventor 朱伟亮邵越峰邵田云
Owner SHANGHAI TAIJIE CHEM
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