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Preparation method of viscosity reducing type polycarboxylic acid water reducing agent

A technology of viscous polycarboxylic acid and water reducing agent, which is applied in the field of concrete admixtures and can solve the problems of the structure and molecular weight of the polycarboxylic acid water reducing agent.

Active Publication Date: 2018-07-10
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation of hyperbranched polycarboxylate superplasticizers by atom transfer radical polymerization or chain transfer agents is similar to the method of using cross-linked monomers. It is difficult to control the structure and molecular weight of polycarboxylate superplasticizers. Industrial production poses great challenges

Method used

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  • Preparation method of viscosity reducing type polycarboxylic acid water reducing agent
  • Preparation method of viscosity reducing type polycarboxylic acid water reducing agent
  • Preparation method of viscosity reducing type polycarboxylic acid water reducing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Preparation of aminated polyether with a molecular weight of 635.

[0064] Chlorinated polyether preparation:

[0065] Initiator allyl alcohol, catalyst DMC. Weigh 100 parts of allyl alcohol and 1.1 parts of catalyst DMC, 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 20 parts of propylene oxide was passed into the reaction kettle. When the pressure in the reaction kettle dropped and the temperature rose, it indicated that the polymerization reaction started. When the pressure of the reactor no longer decreases, feed 411 parts of ethylene oxide into the reactor; when the pressure in the reactor no longer decreases, continue to feed 159 parts of epichlorohydrin into the reactor, and maintain the reactor during the feeding process. The temperature is between 110-130°C and the pressure is between 0.2-0.4MPa. After the feeding of epichlorohydrin is com...

Embodiment 2

[0081] Addition reaction of aminated polyether M1 with methyl acrylate.

[0082] Weigh 300 parts of aminated polyether M1 and 93 parts of catalyst NKC-93, put the above materials into the reactor and replace the reactor with nitrogen for 3 times to empty the air in the reactor. Keep the temperature of the reaction kettle at 50°C to prevent the aminated polyether from solidifying and separating out. Weigh 325 parts of methyl acrylate, add all of them into the reaction kettle within 30 minutes, and continue to fully stir at this temperature for 30 minutes. Then the pressure of the reactor was increased to 0.1 MPa, and the reaction was continued for 5 hours at 50°C. After the reaction, the catalyst NKC-9 is separated from the reaction material through a filter device and recycled for use; the remaining reaction material is passed through a vacuum distillation device to remove volatile substances in the material to obtain brown-yellow polycarboxylate group-containing The comonom...

Embodiment 3

[0096] Synthesis of polyether with a molecular weight of 1100.

[0097] The initiator is allyl alcohol, and the catalyst is potassium tert-butoxide. Weigh 100 parts of allyl alcohol and 1.5 parts of potassium tert-butoxide, put the above materials into the reactor, and evacuate the reactor to -0.1MPa at room temperature. Then the temperature of the reaction kettle was raised to 80° C., and 20 parts of ethylene oxide was introduced into the reaction kettle. After the pressure in the reaction kettle dropped and the temperature rose, it indicated that the polymerization reaction started. Continue to feed 1780 parts of ethylene oxide into the reactor. During the feeding process, keep the temperature of the reactor between 120-130°C and the pressure between 0.2-0.4MPa. After the addition of ethylene oxide is completed, keep the temperature at 100°C for 1h about. When the pressure of the reactor no longer decreases, reduce the temperature of the reactor to about 80°C, open the ven...

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Abstract

The invention provides a preparation method of a viscosity reducing type polycarboxylic acid water reducing agent. The obtained water reducing agent is good in viscosity reducing effect, excellent inwater reducing performance, outstanding in moisture retention performance and better in peaceability. The preparation method of the viscosity reducing type polycarboxylic acid water reducing agent comprises the following steps of (1), preparation of a comonomer of a polycarboxylic acid group structure, wherein firstly, chlorinated polyether of a specific structure and an aminating agent of a specific structure are subjected to an amination reaction to obtain aminated polyether, and after purification, aminated polyether and unsaturated carboxylic acid ester of a specific structure are subjected to an addition reaction of a C=C double bond under the action of a catalyst to synthesize a comonomer having the comonomer of the polycarboxylic acid group structure; (2) polymerization, wherein thecomonomer of the polycarboxylic acid group structure, unsaturated polyether and an unsaturated carboxylic acid monomer are subjected to a radical polymerization reaction according to a molar ratio of(0.1-0.5):1:(3-8) to obtain the polycarboxylic acid water reducing agent.

Description

technical field [0001] The invention relates to a preparation method of a viscosity-reducing polycarboxylate water reducer, which belongs to the technical field of concrete admixtures. Background technique [0002] With the rapid development of my country's economic construction, the use of concrete is increasing at a rate of more than ten percent per year. At the same time, the level of concrete application technology is also developing. Among the numerous concrete admixtures, the water reducer is currently the most widely studied and used admixture. Water reducing agent is essentially a surfactant, which mainly improves the fluidity of concrete, controls the setting or hardening time, and improves the strength of concrete. [0003] Polycarboxylate superplasticizer is a high-performance superplasticizer, its molecular structure is mainly composed of polyether macromonomer and unsaturated carboxylic acid molecules through free radical polymerization. Carboxylic acid functi...

Claims

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Application Information

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IPC IPC(8): C08F290/06C08F283/06C08F220/06C08F222/02C08F222/06C08F222/04C08G65/28C04B24/26C04B103/30
CPCC04B24/2658C04B24/267C04B2103/0059C04B2103/302C08F283/065C08F290/062C08G65/2609C08G65/2663C08F220/06C08F222/02C08F222/06C08F222/04
Inventor 王涛范士敏亓帅冉千平杨勇马建峰曹攀攀刘加平
Owner JIANGSU SOBUTE NEW MATERIALS
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