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Preparation method and use of micromolecule water reducer with delayed coagulation and slump retaining properties

A small-molecule water-reducing agent technology, applied in the field of preparation of small-molecule water-reducing agents, can solve problems such as high cost and poor economy, and achieve the effects of low production energy consumption, low raw material cost, and excellent concrete workability

Active Publication Date: 2018-07-03
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are two main ways to obtain the amino polyether used in polyether derivatives. One is to aminate after chlorination of methoxy polyether. This method will introduce chloride ions, and the concrete industry has strict regulations on the content of chloride ions. The second method is the direct amination of methoxypolyether. At present, only a few companies have mastered the industrialized method, resulting in higher cost and poor economy of aminated methoxypolyether.

Method used

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  • Preparation method and use of micromolecule water reducer with delayed coagulation and slump retaining properties
  • Preparation method and use of micromolecule water reducer with delayed coagulation and slump retaining properties
  • Preparation method and use of micromolecule water reducer with delayed coagulation and slump retaining properties

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0065] (1) Amination reaction

[0066]Put 59.11g (1.0mol) of propylamine, 87.82g (1.02mol) of methyl acrylate and 0.68g of NKC-9 in a 250ml reaction bottle, raise the temperature to 40°C, stir and react for 1h, after the reaction is completed, remove the excess by vacuuming and vacuuming The methyl acrylate is removed by filtration to obtain an organic amine intermediate with a carboxylate group structure. By controlling the amount of organic amine and unsaturated carboxylic acid ester to be close to equimolar, a secondary amine intermediate formed by only one amino hydrogen participating in the addition reaction is obtained. The nucleophilic activity of the amine is greatly reduced and cannot continue to react with a slight excess of unsaturated carboxylate, so only one amino hydrogen may participate in the addition reaction.

[0067] (2) phosphorylation reaction

[0068] Put 145.20g (1.0mol) of the above-mentioned organic amine intermediate and 82.82g (1.01mol) of phosphor...

Embodiment 2

[0072] (1) Amination reaction

[0073] Put 269.51g (1.0mol) of octadecylamine, 87.82g (1.02mol) of methyl acrylate and 2.89g of NKC-9 in a 500ml reaction bottle, raise the temperature to 80°C, stir and react for 4h, after the reaction is completed, vacuumize and evaporate Excess methyl acrylate is removed, and insoluble matter is removed by filtration to obtain an organic amine intermediate with a carboxylate group structure. By controlling the amine and the unsaturated carboxylic acid ester to be close to equimolar amounts, a secondary amine intermediate formed by only one amino hydrogen participating in the addition reaction is obtained. The nucleophilic activity is greatly reduced and cannot continue to react with a slight excess of unsaturated carboxylic acid esters, so only one amino hydrogen may participate in the addition reaction.

[0074] (2) phosphorylation reaction

[0075] Put 355.60g (1.0mol) of the above-mentioned organic amine intermediate and 82.82g (1.01mol)...

Embodiment 3

[0079] (1) Amination reaction

[0080] Put 93.13g (1.0mol) of aniline, 103.12g (1.03mol) of 2-methyl methacrylate and 0.95g NKC-9 in a 500ml reaction bottle, raise the temperature to 80°C, stir and react for 6h, and vacuumize under reduced pressure after the reaction is completed The excess 2-methyl methacrylate was evaporated, and the insoluble matter was removed by filtration to obtain an organic amine intermediate with a carboxylate group structure. By controlling the amine and the unsaturated carboxylic acid ester to be close to equimolar amounts, a secondary amine intermediate formed by only one amino hydrogen participating in the addition reaction is obtained. The nucleophilic activity is greatly reduced and cannot continue to react with a slight excess of unsaturated carboxylic acid esters, so only one amino hydrogen may participate in the addition reaction.

[0081] (2) phosphorylation reaction

[0082] Put 193.25g (1.0mol) of the above-mentioned organic amine interm...

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Abstract

The invention provides a preparation method and use of a micromolecule water reducer with delayed coagulation and slump retaining properties. The preparation method has the beneficial effects that a preparation method is strong in adjustability and high in cost performance, a preparation process is simple, the prepared micromolecule water reducer has excellent slump retaining property, delayed coagulation property and clay tolerance. The preparation method comprises the following steps: (1) carrying out amination reaction: carrying out C=C double bond Michael addition reaction by virtue of organic amine with a specific structure and unsaturated carboxylate with a specific structure, and purifying, so as to obtain an organic amine intermediate with an amino hydrogen and carboxylic ester group structure; (2) carrying out Mannich reaction by virtue of the organic amine intermediate, formaldehyde and phosphorous acid, and purifying, so as to obtain phosphorylated organic amine intermediate; and (3) carrying out condensation reaction by virtue of carboxyl of the phosphorylated organic amine intermediate and polyether with a specific structure and a terminal OH or a terminal NH2 so as toconvert carboxyl into an ester group or acylamino, and alkalizing for neutralization so as to obtain the micromolecule water reducer with the delayed coagulation and slump retaining properties.

Description

technical field [0001] The invention relates to a preparation method and application of a small-molecule water-reducing agent with retarding and slump-retaining properties, and belongs to the technical field of concrete admixtures. Background technique [0002] As a building material, concrete is widely used in many fields. Concrete admixture is an essential component of concrete, which can adjust and improve the working performance of concrete materials, and plays a central role in concrete production technology. Water reducer is one of the largest and most widely used concrete admixtures. [0003] As the third generation of high-performance water reducer, polycarboxylate water reducer is mainly composed of unsaturated carboxylic acid and unsaturated polyether macromonomer through free radical polymerization to obtain a comb-shaped polymer. The acid adsorption groups provide electrostatic repulsion, and the polyether side chains provide effective steric hindrance. Compare...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/335C04B24/32C04B103/22C04B103/30
CPCC04B24/32C04B2103/22C04B2103/302C04B2103/308C08G65/3356C08G2650/04C08G2650/38C08G2650/50
Inventor 亓帅冉千平王涛舒鑫马建峰范士敏杨勇刘加平
Owner JIANGSU SOBUTE NEW MATERIALS
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