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Organic monomer for synthesizing amphoteric polycarboxylic superplasticizer and preparation method

A high-efficiency water reducer and polycarboxylic acid technology, which is applied in the preparation of organic compounds, preparation of amino hydroxyl compounds, organic chemistry, etc., can solve the problems of high synthesis cost and difficult industrialization

Active Publication Date: 2016-05-04
LIMING VOCATIONAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The main problem in the synthesis of existing amphoteric polycarboxylate superplasticizers is that it has been difficult to realize industrialization due to the high cost of synthesis

Method used

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  • Organic monomer for synthesizing amphoteric polycarboxylic superplasticizer and preparation method
  • Organic monomer for synthesizing amphoteric polycarboxylic superplasticizer and preparation method
  • Organic monomer for synthesizing amphoteric polycarboxylic superplasticizer and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Preparation of dimethylaminoethyl acrylate intermediate

[0023] Using one-time feeding method, add ethyl acrylate, N,N-dimethylaminoethanol, polymerization inhibitor and catalyst into a three-neck round bottom flask, turn on the stirring device, slowly heat up, condense and reflux for collection. During the preparation process, maintain the reaction temperature in the round bottom flask at 110°C to 130°C, control the temperature at the top of the fractionating column at 85°C to 95°C, and the reflux ratio to be 1:1 to 1:6, and the ethanol generated by the transesterification reaction and Ethyl acrylate azeotrope was distilled out of the system. After 4-8 hours of the transesterification reaction, stop the reaction to obtain the crude product of dimethylaminoethyl acrylate. The obtained crude product is subjected to sedimentation and vacuum distillation to obtain the dimethylaminoethyl acrylate intermediate for future use.

[0024] Preferably, the molar ratio of et...

Embodiment 2

[0035] It is basically the same as Example 1, the difference is:

[0036] Preferably, the molar ratio of ethyl acrylate to N,N-dimethylaminoethanol in the step (1) is 1:1.

[0037] Preferably, the polymerization inhibitor in the step (1) is a phenothiazine polymerization inhibitor, and the amount of the polymerization inhibitor is 0.2% of the total mass of ethyl acrylate and N,N-dimethylaminoethanol.

[0038] Preferably, the catalyst in the step (1) is a sodium methoxide catalyst, and the catalyst dosage is 1.0% of the total mass of ethyl acrylate and N,N-dimethylaminoethanol.

[0039] Preferably, the molar ratio of water to dimethylaminoethyl acrylate intermediate in the step (2) is 1.5:1.

[0040] Preferably, the polymerization inhibitor in the step (2) is a phenothiazine polymerization inhibitor, and the amount of the polymerization inhibitor is 0.25% of the mass of the dimethylaminoethyl acrylate intermediate.

Embodiment 3

[0042] Basically the same as Example 1, the difference is:

[0043] Preferably, the molar ratio of ethyl acrylate to N,N-dimethylaminoethanol in the step (1) is 1:1.

[0044] Preferably, the polymerization inhibitor in the step (1) is a 2,2,6,6-tetramethylpiperidine oxide polymerization inhibitor, and the amount of the polymerization inhibitor is ethyl acrylate and N,N-dimethylamino 0.3% of the total mass of ethanol.

[0045] Preferably, the catalyst in the step (1) is a tetrabutyl titanate catalyst, and the amount of the catalyst is 1.5% of the total mass of ethyl acrylate and N,N-dimethylaminoethanol.

[0046] Preferably, the molar ratio of water to dimethylaminoethyl acrylate intermediate in the step (2) is 2.0:1.

[0047] Preferably, the polymerization inhibitor in the step (2) is a hydroquinone polymerization inhibitor, and the polymerization inhibitor consumption is 0.5% of the mass of the dimethylaminoethyl acrylate intermediate.

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Abstract

The invention discloses an organic monomer for synthesizing an amphoteric polycarboxylic superplasticizer, which has a molecular structure shown in the description. The invention further discloses a preparation method of the organic monomer for synthesizing the amphoteric polycarboxylic superplasticizer and comprises the following steps: preparing a dimethylaminoethyl acrylate intermediate and a cationic active organic monomer; adopting one-time charging at the normal temperature; and selecting a reasonable type of catalyst to prepare the organic monomer. The method has reduced cost, plays an important part in process simplification, and has characteristics of high reaction conversion rate, high yield, and high purity. Compared with an anionic polycarboxylic superplasticizer sold in the market, under a condition of a relatively low mixing amount, the amphoteric polycarboxylic superplasticizer enables neat cement paste or concrete to have excellent performance of good water reduction, high dispersion, good plasticity preservation, and high early-stage compressive strength.

Description

technical field [0001] The invention belongs to the technical field of synthesizing active organic monomers of polycarboxylic acid high-efficiency water reducers, and specifically relates to an organic monomer used for synthesizing amphoteric polycarboxylate high-efficiency water reducers. The preparation method of the organic monomer of type polycarboxylate high-efficiency water reducer. Background technique [0002] With the rapid advancement of my country's urbanization, the establishment of the Asian Infrastructure Investment Bank and the continuous implementation of the "Belt and Road" strategy, it is bound to promote the modernization of infrastructure projects. Since most of the different environments and different infrastructure projects use concrete as the engineering structure material, this will speed up the progress of concrete technology. Today, polycarboxylate superplasticizers are an essential and important component of concrete. The research and development ...

Claims

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Application Information

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IPC IPC(8): C07C219/08C07C213/08C04B24/26C04B103/30
CPCC04B24/2647C04B2103/302C07C213/06C07C213/08C07C219/08
Inventor 陈宝璠卓玲
Owner LIMING VOCATIONAL UNIV
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