Preparation method and application of polycarboxylate water reducer containing phosphate groups

A phosphate-based, polycarboxylic acid technology, 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, cumbersome steps, and low water-reducing rate.

Active Publication Date: 2017-10-10
JIANGSU SOBUTE NEW MATERIALS +1
View PDF12 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] Chinese patent document CN 104311752 A 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 Containing phosphine and silicon groups, a polycarboxylate superplasticizer with high water reducing rate, good slump retention, and early strength development of concrete is prepared to overcome the ubiquity of polycarboxylate superplasticizers in machine-made sand. Problems of low water reducing rate and poor slump retention
Therefore, in the copolymerization reaction of water reducer involving unsaturated monomers containing phosphoric acid groups, there is the possibility of changes in the structure and molecular weight of the water reducer, and the structure and molecular weight of the water reducer cannot be accurately controlled. To optimize the water reducing agent of the group, the steps are cumbersome and the process control is difficult

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method and application of polycarboxylate water reducer containing phosphate groups
  • Preparation method and application of polycarboxylate water reducer containing phosphate groups
  • Preparation method and application of polycarboxylate water reducer containing phosphate groups

Examples

Experimental program
Comparison scheme
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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

PropertyMeasurementUnit
particle diameteraaaaaaaaaa
molecular weight distributionaaaaaaaaaa
molecular weight distributionaaaaaaaaaa
Login to view more

Abstract

The invention provides a preparation method and application of a polycarboxylate water-reducer containing phosphate groups. The preparation method can avoid the disadvantage that the structure and molecular weight of the water-reducer cannot be accurately controlled due to the chain transfer effect of the phosphoric acid group. . The preparation method is to first carry out copolymerization reaction of unsaturated polyether macromonomer, unsaturated carboxylic acid ester, and unsaturated alcohol in an organic solvent to obtain a polycarboxylate water-reducer prepolymer, and then make the polycarboxylate water-reducer The prepolymer is phosphorylated and modified, and then in the presence of an acidic aqueous solution, the carboxylate group on the phosphorylated and modified product is hydrolyzed, and the organic solvent is removed, and finally neutralized to obtain the phosphate group-containing Polycarboxylate superplasticizer, in which the unsaturated polyether macromonomer does not contain hydroxyl groups; phosphorylation modification is to esterify the alcoholic hydroxyl groups in the polycarboxylate superplasticizer prepolymer with phosphoric acid esterification reagents Reaction; the amount of the phosphoric acid esterification reagent is enough to completely esterify the alcoholic hydroxyl group in the polycarboxylate superplasticizer prepolymer.

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
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
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap