Preparation method and application of polycarboxylate water reducer containing phosphate group

A phosphate-based, polycarboxylic acid technology, applied in the field of concrete admixtures, can solve the problems of cumbersome steps, poor slump retention, difficult process control and the like

Active Publication Date: 2016-03-23
JIANGSU SOBUTE NEW MATERIALS +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] Chinese patent document CN104311752A reports a preparation method of a polycarboxylate water reducer. Some unsaturated phosphine-containing and silicon-containing monomers are added to the raw materials for synthesizing the water reducer, thereby introducing some phosphine-containing monomers into the molecular chain of the water reducer. , containing silicon groups, to prepare a polycarboxylate water reducer with high water reducing rate, good slump retention, and conducive to the early stre

Method used

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  • Preparation method and application of polycarboxylate water reducer containing phosphate group
  • Preparation method and application of polycarboxylate water reducer containing phosphate group
  • Preparation method and application of polycarboxylate water reducer containing phosphate group

Examples

Experimental program
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Effect test

Embodiment 1

[0059] Synthesis of methyl-terminated polyether with a molecular weight of 2006.

[0060] Polyether preparation:

[0061] The initiator is allyl alcohol, and the catalyst is sodium methoxide. Weigh 58g (1mol) of allyl alcohol and 3g of sodium methoxide, put the above materials into the reactor, and vacuumize the reactor to -0.1MPa at room temperature. Then the temperature of the reaction kettle was raised to 100° C., and 50 g of ethylene oxide was introduced into the reaction kettle. When the pressure in the reaction kettle dropped and the temperature rose, it indicated that the polymerization reaction started. Continue to feed 1892g of ethylene oxide into the reactor. During the feeding process, keep the temperature of the reactor between 100-120°C and the pressure between 0.2-0.4MPa. After the addition of ethylene oxide is completed, keep the temperature at 100°C for about 1h . When the pressure of the reactor no longer decreases, reduce the temperature of the reactor to ...

Embodiment 2

[0072] Synthesis of a methyl-terminated block polyether with a molecular weight of 4800.

[0073] Polyether preparation:

[0074] Initiator 10-undecenol, catalyst sodium hydride (60%). Weigh 85 g (0.5 mol) of 10-undecenol and 2 g of sodium hydride, put the above materials into the reactor, and vacuumize the reactor to -0.1 MPa at room temperature. Then the temperature of the reaction kettle is raised to 100°C, and 82.86g of epoxycyclohexane is passed into the reaction kettle. When the pressure in the reaction kettle drops and the temperature rises, it indicates that the polymerization reaction starts. The internal pressure no longer drops. Then continuously feed 2232.14g of ethylene oxide into the reactor, keep the temperature of the reactor between 100-120°C and the pressure between 0.2-0.4MPa during the feeding process, and keep the temperature at 100°C after the feeding of ethylene oxide is completed About 1h. When the pressure of the reactor is no longer reduced, reduc...

Embodiment 3

[0081] Synthesis of polycarboxylate superplasticizer prepolymer:

[0082] Add 200g (0.1mol) of unsaturated polyether M1, 21.5g (0.25mol) of methyl acrylate, 0.058g (0.001mol) of allyl alcohol into a glass reaction flask equipped with a thermometer, stirrer, and peristaltic pump feeding system , while adding 44g of petroleum ether, heating up to 30°C to dissolve while stirring, then adding 1.15g (0.007mol) of azobisisobutyronitrile, and stirring evenly. Then weigh 0.14g (0.0018mol) of mercaptoethanol, add it to 22g of petroleum ether, stir to make a uniform solution, and use the peristaltic pump feeding system to drop it into the reaction bottle at a constant speed. The dropping time is 2h, and the dropping is completed. After incubation, the reaction was carried out for 2 hours. Tested by GPC, the molecular weight is 25000, and the molecular weight distribution is 1.71.

[0083] Phosphorylation modification:

[0084] Weigh 0.12g (0.00102mol) of 85% phosphoric acid and 0.22g...

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Abstract

The invention provides a preparation method and application of a polycarboxylate water reducer containing a phosphate group. According to the preparation method, the defects that the structure and the molecular weight of the water reducer cannot be accurately controlled due to the chain transfer action of the phosphate group can be overcome. The preparation method comprises the steps that an unsaturated polyether macromonomer, unsaturated carboxylic ester and unsaturated alcohol are subjected to a copolymerization reaction in organic solvent to obtain a polycarboxylate water reducer pre-polymer; phosphorylated modification is performed on the polycarboxylate water reducer pre-polymer; on the condition that an acid aqueous solution exists, a carboxylic ester group on a product obtained after phosphorylated modification is hydrolyzed, and the organic solvent is removed; neutralization is performed to obtain the polycarboxylate water reducer containing the phosphate group; the unsaturated polyether macromonomer does not contain hydroxyl, phosphorylated modification is achieved through the step that an alcoholic hydroxyl group in the polycarboxylate water reducer pre-polymer and a phosphate esterification reagent are subjected to an esterification reaction, and the using amount of the phosphate esterification reagent is sufficient to completely esterify the alcoholic hydroxyl group in the polycarboxylate water reducer pre-polymer.

Description

technical field [0001] The invention relates to a preparation method and application of a phosphate group-containing polycarboxylate water reducer, belonging to the technical field of concrete admixtures. Background technique [0002] The addition of chemical admixtures can greatly improve the durability, workability, applicability, economy and strength of concrete, and provide a strong guarantee for the quality of large-scale projects. Therefore, its wide application is known as the successor to reinforced concrete and prestressed concrete. The 3rd major breakthrough in concrete technology after concrete. [0003] Polycarboxylate superplasticizer has become the most important product in the current concrete admixture market due to its advantages such as low dosage, high water reducing rate, good slump retention, strong molecular structure adjustability, and environmental protection. With the scarcity of natural high-quality sandstone and other material resources and the de...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F220/14C08F216/08C08F216/04C08F220/18C08F220/28C08G65/327C04B24/32C04B103/30
CPCC04B24/32C08F283/06C08G65/327C04B2103/302C08F220/18C08F220/1802C08F220/1804C08F216/08C08F220/281C04B24/246
Inventor 王涛范士敏冉千平亓帅杨勇马建峰宋峰岩
Owner JIANGSU SOBUTE NEW MATERIALS
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