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Preparation method of phosphate water reducer with amide structure

A phosphoric acid-based, water-reducing agent technology, which is applied in the synthesis and application of phosphoric-acid-based water-reducing agents, can solve problems such as low clay sensitivity, and achieve the effects of simple preparation process, simple synthesis method, and excellent clay tolerance.

Active Publication Date: 2018-04-27
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent document CN103596993A discloses a copolymer with geminal bisphosphate groups, which is less sensitive to clay than polycarboxylate water reducers

Method used

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  • Preparation method of phosphate water reducer with amide structure
  • Preparation method of phosphate water reducer with amide structure
  • Preparation method of phosphate water reducer with amide structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Preparation of ethylene oxide polyether:

[0046] The initiator is allyl alcohol, and the catalyst is potassium tert-butoxide. Weigh 58 parts of allyl alcohol and 0.9 part of potassium tert-butoxide, 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 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 910 parts of ethylene oxide into the reaction kettle. During the feeding process, keep the temperature of the reaction kettle between 120-130°C and the pressure between 0.2-0.4MPa. After the addition of ethylene oxide, keep the temperature at 100°C for 1h about. Until the pressure of the reactor no longer decreases, reduce the temperature of the reactor to about 80°C, open the vent valve to re...

Embodiment 2

[0054] Preparation of ethylene oxide, propylene oxide block polyether:

[0055] Initiator hydroxyethyl vinyl ether, catalyst potassium tert-butoxide. Weigh 88 parts of hydroxyethyl vinyl ether and 4.4 parts of potassium tert-butoxide, 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 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 1595 parts of ethylene oxide in the reactor, until the pressure in the reactor no longer drops, 283 parts of propylene oxide in the reactor. During the feeding process, the temperature of the reactor is maintained between 110-115°C and the pressure is between 0.3-0.5MPa. After all the alkylene oxide is fed, the temperature is kept at 100°C for about 1 hour. Until th...

Embodiment 3

[0062] Synthesis of prepolymers containing carboxylic acid groups:

[0063] In the reaction kettle equipped with a temperature measuring device, a stirring device, a titration device and a nitrogen gas introduction pipe, add 500 parts of unsaturated polyether monomer P1, and add 381 parts of solvent water at the same time, purging the reactor with nitrogen while stirring, and Raise the temperature to 70°C and stir well, then add 3.4 parts of hydrogen peroxide (mass concentration: 30%). Then mix 72 parts of acrylic acid, 2.6 parts of L-ascorbic acid, 4.1 parts of thioglycolic acid, and 763 parts of water, stir to form a uniform aqueous solution, and drop it into the reactor for 3.5 hours. 1.5h, cooled to room temperature. The sample was tested by GPC to have a molecular weight of 5720 and a molecular weight distribution of 1.50.

[0064] Synthesis of Phosphate-based Water Reducer:

[0065] Add 31.3 parts of concentrated sulfuric acid and 54.1 parts of ethylenediamine to the ...

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Abstract

The invention discloses a preparation method of a phosphate water reducer with an amide structure. The preparation method includes the steps: under certain reaction conditions, carrying out a free radical polymerization reaction of an unsaturated polyether monomer and an unsaturated carboxylic monomer to polymerize to obtain a carboxylic group-containing prepolymer; adding an amination reagent into the prepared carboxylic group-containing prepolymer, undergoing an amidation reaction, then adding phosphorous acid and an aldehyde monomer, and carrying out a Mannich reaction to obtain the phosphate water reducer containing the amide structure. According to the preparation method, the amide structure is introduced, the amidation reaction of the carboxylic group-containing prepolymer and the organic polyamine monomer is carried out, the synthesis method is simple, expensive amino-terminated polyether is not needed, and the synthesis cost is greatly reduced; while the amide structure is formed, the connection of the organic polyamine monomer and a polymer chain is completed indirectly, a traditional method of firstly synthesis of chlorinated polyether and then amination is avoided, and the introduction of chloride ions is avoided.

Description

technical field [0001] The invention belongs to the field of concrete admixture preparation, in particular to the synthesis and application of a phosphoric acid-based water reducer containing an amide structure. Background technique [0002] With the rapid development of the construction industry, concrete technology is constantly developing in the direction of high workability, high strength, high durability or special performance. As an essential material and core technology for modern concrete preparation, water reducer products are facing new challenges, and it is even more urgent to research and develop water reducer materials with new structures and characteristic properties. [0003] In recent years, polycarboxylate superplasticizer has become the mainstream of research in the industry due to its advantages such as low dosage, high water reducing rate, and good cement adaptability. However, theoretical research and engineering applications have shown that polycarboxy...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F220/06C08F222/02C08F222/06C08F8/40C08F8/32C04B24/26C04B103/30
CPCC04B24/246C04B2103/302C08F8/40C08F283/065C08F220/06C08F222/02C08F222/06C08F8/32
Inventor 韩正亓帅王兵冉千平王涛马建峰范士敏
Owner JIANGSU SOBUTE NEW MATERIALS
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