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Preparation method of monomer-terminated amine ether for synthesizing early-strength polycarboxylate superplasticizer

A technology of capping amine ether and polycarboxylic acid, which is applied in the field of polycarboxylate superplasticizer monomer polyether synthesis, can solve the problems of large air-entraining volume, achieve the effects of reducing air-entraining volume, excellent product performance, and wide application range

Active Publication Date: 2019-05-21
FUSHUN DONGKE FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the present invention is to provide a method for preparing monomer-terminated amine ethers for synthesizing early-strength polycarboxylate superplasticizers. The monomer-terminated amine ethers prepared by the method can effectively overcome the disadvantages of existing monomer polyethers. At the same time, the polycarboxylate water reducer synthesized by the monomer-terminated amine ether can also effectively solve the problem of large air-entraining capacity of the existing water reducer itself

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] ①Synthesis of crude block monomer amine ether: Add 110g of N-methallylamine and 1.34g of catalyst KOH to 1# reactor (2L), and the catalyst accounts for 0.09% of the total feed. Use high-purity N2 to replace the air in the reactor three times, keep the nitrogen pressure in the reactor at 0.3-0.5 MPa, raise the temperature to 95° C., and feed 42.3 g of ethylene oxide. After the reaction is initiated successfully, set the reaction temperature T=110-130°C, keep the temperature and under the condition of reaction pressure P<0.8MPa, continuously feed the first stage of ethylene oxide 643.1g into the reaction kettle, the first stage The amount of ethylene oxide (comprising the amount of initiation) that passes into the section is 76% of the total feed amount of ethylene oxide, and slaking is carried out after the feeding is completed; in the reactor, feed propylene oxide 528.8g continuously, The mass ratio of propane to ethylene oxide is 1:1.6, and after the feed is completed,...

Embodiment 2

[0028] ①Synthesis of crude block monomer amine ether: Add 95g of N-methallylamine and 1.72g of catalyst KOH to 1# reactor (2L), and the catalyst accounts for 0.11% of the total feed. Use high-purity N2 to replace the air in the reactor three times, keep the nitrogen pressure in the reactor at 0.3-0.5 MPa, raise the temperature to 95° C., and feed 49.1 g of ethylene oxide. After the reaction is initiated successfully, set the reaction temperature T=110-130°C, keep the temperature and under the condition of reaction pressure P<0.8MPa, continuously feed the first stage of ethylene oxide 785.3g into the reaction kettle, the first stage The amount of ethylene oxide (comprising the amount of initiation) that passes into the section is 80% of the total feed amount of ethylene oxide, and is matured after the feeding is completed; then continuously feeds 490.8g of propylene oxide in the reactor, The mass ratio of propane to ethylene oxide is 1:2, after the feeding is completed, it is m...

Embodiment 3

[0032] ①Synthesis of crude block monomer amine ether: Add 100g of N-methallylamine and 2.1g of catalyst KOH to 1# reactor (2L), and the catalyst accounts for 0.12% of the total feed. Use high-purity N2 to replace the air in the reactor three times, keep the nitrogen pressure in the reactor at 0.3-0.5 MPa, raise the temperature to 95° C., and feed 58.9 g of ethylene oxide. After the reaction is initiated successfully, set the reaction temperature T=110-130°C, keep the temperature and under the condition of reaction pressure P<0.8MPa, continuously feed the first stage of ethylene oxide 1001.8g into the reactor, the first stage The amount of ethylene oxide (comprising the amount of initiation) that passes into the section is 85% of the total feed amount of ethylene oxide, and aging is carried out after the feeding is completed; The mass ratio of propane to ethylene oxide is 1:2.5, and after the feeding is completed, it is matured; finally, 176.8 g of the second stage of ethylene ...

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Abstract

The invention discloses a preparation method of monomer-terminated amine ether for synthesizing an early-strength polycarboxylate superplasticizer. The method comprises the following steps: (1) synthesizing block monomer amine ether; (2) refining the block amine ether; and (3) preparing monomer-terminated amine ether. The method provided by the invention has simple process control, stable productstructure and excellent product performance. In the method, a one-step synthesis method different from conventional synthesis methods of alcohols, amine initiators and epoxides is adopted, and throughsynthesis and refining of EO-PO-EO type specific block amine ether and a key technology for terminating amine ether, nitrogen element is introduced into a final polycarboxylate superplasticizer and aprimary hydroxyl group is eliminated through terminating. The polycarboxylate superplasticizer synthesized by the method not only improves an early strength function, but also appropriately reduces an air entraining content, thus further expanding the application of the polycarboxylate superplasticizer in the field of concrete.

Description

1. Technical field [0001] The invention belongs to the technical field of synthesis of polycarboxylate superplasticizer monomer polyether, and in particular relates to a method for preparing monomer-terminated amine ether for synthesizing early-strength polycarboxylate superplasticizer. 2. Background technology [0002] High-performance polycarboxylate superplasticizer is the third generation of high-performance superplasticizer. Compared with the previous two generations of superplasticizers, it has the characteristics of low dosage, high water-reducing rate, no segregation and high slump retention. Specify the admixture. Monomer polyether is the main raw material for the synthesis of high-efficiency polycarboxylate superplasticizers, which are usually synthesized from unsaturated alcohols as initiators, such as propenyl alcohol and its homologues, prenyl alcohol, unsaturated six-carbon alcohol ether, etc. As a result, monomer polyethers synthesized from the above raw mate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/331C08G65/26C08G65/30
Inventor 徐仕睿刘勇李鹏刘威
Owner FUSHUN DONGKE FINE CHEM
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