Preparation method and application of polycarboxylate superplasticizer containing phosphate groups

A technology of polycarboxylic acid and water-reducing agent, applied in the field of concrete admixtures, can solve the problems of inability to accurately control the structure and molecular weight of the water-reducing agent, complicated steps, low water-reducing rate, etc.

Active Publication Date: 2016-05-25
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 strength

Method used

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  • Preparation method and application of polycarboxylate superplasticizer containing phosphate groups
  • Preparation method and application of polycarboxylate superplasticizer containing phosphate groups
  • Preparation method and application of polycarboxylate superplasticizer containing phosphate groups

Examples

Experimental program
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Effect test

Embodiment 1

[0055] Synthesis of methyl terminated polyether M1 with a molecular weight of 2006.

[0056] Polyether preparation:

[0057] Starter allyl alcohol, catalyst sodium methoxide. Weigh 58 g (1 mol) of allyl alcohol and 3 g of sodium methoxide, add the above-mentioned materials into the reaction vessel, and vacuum the reaction vessel to -0.1 MPa at room temperature. Then the reactor was heated to 100°C, and 50 g of ethylene oxide was introduced into the reactor. When the pressure in the reactor dropped and the temperature rose, the polymerization reaction started. Continue to feed 1892g of ethylene oxide into the reactor. During the feeding process, maintain the temperature of the reactor at 100~120℃ and the pressure between 0.2~0.4MPa. After the ethylene oxide feed is finished, keep the temperature at 100℃ for about 1h. . When the pressure of the reactor no longer decreases, reduce the temperature of the reactor to about 80℃, open the vent valve to reduce the pressure in the reactor...

Embodiment 2

[0068] Synthesis of methyl-terminated block polyether M2 with a molecular weight of 4800.

[0069] Polyether preparation:

[0070] Starter 3-methyl-3-buten-1-ol, catalyst sodium hydride (60%). Weigh 48 g (0.5 mol) of 3-methyl-3-buten-1-ol and 2 g of sodium hydride, put the above materials into the reaction vessel, and evacuate the reaction vessel to -0.1 MPa at room temperature. Then the reactor was heated to 100°C, and 43.7g of propylene oxide was introduced into the reactor. When the pressure in the reactor dropped and the temperature rose, the polymerization reaction started. Keep the reaction at 100-120°C until the pressure in the reactor No more decline. Then, 1658.3g of ethylene oxide was continuously fed into the reaction kettle. During the feeding process, the temperature of the reaction kettle was maintained at 100-120℃ and the pressure at 0.2-0.4MPa. After the feeding of ethylene oxide, the temperature was kept at 100℃. About 1h. When the pressure of the reaction kett...

Embodiment 3

[0077] For phosphorylation reagents containing phosphorous acid groups, we use the Mannich reaction in organic chemistry to achieve. Take the Mannich reaction of ethylenediamine as an example: take 0.15g (0.0025mol) of ethylenediamine and add 1.23g Phosphorous acid (0.015mol), 0.52g (0.005mol) of hydrochloric acid with a mass fraction of 35% are placed in a 50ml three-necked flask, and the reaction mixture is heated to 100°C for 5h. Subsequently, 0.67 g (0.00825 mol) of 37% formaldehyde aqueous solution was added, and the mixture was heated and refluxed for 24 hours (the molar ratio of ethylenediamine, formaldehyde, and phosphorous acid was 1:3.3:6). After the reaction, keep the reaction temperature, add 0.94g (0.0075mol) 32% NaOH solution to the reaction system to neutralize the excess free phosphorous acid into monosodium phosphite, and neutralize the hydrochloric acid in the reaction system into chlorination The sodium salt was then extracted with 50ml of cold dichloromethan...

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Abstract

The invention provides a preparation method and application of a polycarboxylate superplasticizer containing phosphate groups. The preparation method can overcome the defect that due to the chain transfer effect of the phosphate groups, the structure and molecular weight of the superplasticizer can not be accurately controlled. The preparation method includes the steps that firstly, unsaturated polyether macromonomers and unsaturated anhydride are subjected to a solution copolymerization reaction in an organic solvent to obtain a polycarboxylate superplasticizer prepolymer; then, the polycarboxylate superplasticizer prepolymer is subjected to phosphorylation modification to obtain the polycarboxylate superplasticizer, wherein the unsaturated polyether macromonomers do not contain OH, phosphorylation modification refers to that anhydride groups in the polycarboxylate superplasticizer prepolymer and a phosphorylation reagent are subjected to an amidation reaction to obtain the polycarboxylate superplasticizer containing the phosphate groups, molecules of the phosphorylation reagent contain one or more phosphate groups and amino capable of participating in the amidation reaction, and the molar ratio of unsaturated anhydride participating in the solution copolymerization reaction to the phosphorylation reagent is 1:(0.01-0.5).

Description

Technical field [0001] The invention relates to a preparation method and application of a polycarboxylic acid water reducer containing phosphoric acid groups, and belongs 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 following reinforced concrete and prestressed concrete. The third major breakthrough in concrete technology after concrete. [0003] Polycarboxylic acid water-reducing agent has become the most important product in the concrete admixture market due to its advantages such as low dosage, high water-reducing rate, good slump retention, strong molecular structure adjustment, and environmental protection. With the scarcity of natural high-quality sand and gravel and the development of green bu...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F222/06C08F222/04C08F8/40C08F2/06C04B24/32
CPCY02P20/582C08F8/40C04B24/32C04B2103/302C04B2103/408C08F2/06C08F283/065C08F222/06C08F222/04
Inventor 范士敏亓帅王涛冉千平马建峰舒鑫宋峰岩
Owner JIANGSU SOBUTE NEW MATERIALS
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