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A kind of preparation method of polyphosphate ester superplasticizer

A technology of polyphosphate ester and water reducer, which is applied in the field of preparation of polyphosphate ester water reducer, can solve the problems of hindering the adsorption of water reducer and cement, the volatile environment of carboxylic acid, and the limitation of work performance, etc. Harsh, inexpensive, low-cost-to-produce effects

Inactive Publication Date: 2018-03-09
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The unreacted small monomer organic carboxylic acid in the polycarboxylate superplasticizer is volatile and will cause environmental pollution; the side chain of the electrically neutral polyvinyl alcohol unit in its molecular structure will hinder the adsorption of the superplasticizer and cement, which It will cause part of the polycarboxylate superplasticizer to be free in the concrete, which limits its working performance

Method used

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  • A kind of preparation method of polyphosphate ester superplasticizer
  • A kind of preparation method of polyphosphate ester superplasticizer

Examples

Experimental program
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Effect test

Embodiment 1

[0018] In the preparation of the polyphosphate water reducer in this example: the molar ratio of isopentenol polyoxyethylene ether to pyrophosphoric acid is 1:1, the phosphating reaction temperature is 80°C, and the reaction time is 12h; the free radical homopolymerization temperature The temperature is 80°C, the mass of the initiator ammonium persulfate is 2% of the mass of the monomer, the mass of the regulator mercaptopropionic acid is 1% of the mass of the monomer, the dropping time is 2h, and the temperature is kept for 1h. The specific preparation process is:

[0019] Accurately weigh 24g of prenol polyoxyethylene ether (Mn=2400) and 1.98g of pyrophosphoric acid in a 100mL three-necked flask, fix them in an oil bath at 80°C, blow in nitrogen gas for 30min, and then react in a closed and constant temperature for 12h, and the reaction ends Then add 10g deionized water;

[0020] Weigh 0.48g of ammonium persulfate and 0.24g of mercaptopropionic acid and dissolve them in 10g...

Embodiment 2

[0026] In the preparation of the polyphosphate water reducer in this example: the molar ratio of isopentenol polyoxyethylene ether to pyrophosphoric acid is 1:1, the phosphating reaction temperature is 80°C, the reaction time is 12h, and the free radical polymerization temperature is 80°C, the mass of the initiator ammonium persulfate is 1% of the mass of the monomer, the mass of the regulator mercaptopropionic acid is 1% of the mass of the monomer, the dropping time is 2h, and the temperature is kept for 1h. The specific preparation process is:

[0027] Accurately weigh 24g of prenol polyoxyethylene ether (Mn=2400) and 1.98g of pyrophosphoric acid in a 100mL three-necked flask, fix them in an oil bath at 80°C, blow in nitrogen gas for 30min, and then react in a closed and constant temperature for 12h, and the reaction ends Then add 10g deionized water;

[0028] Weigh 0.24g of ammonium persulfate and 0.24g of mercaptopropionic acid and dissolve them in 10g of deionized water....

Embodiment 3

[0034] In the preparation of polyphosphate water reducer in this example: the molar ratio of isopentenol polyoxyethylene ether and pyrophosphoric acid is 1:1, the phosphating reaction temperature is 80°C, and the reaction time is 12h; the free radical polymerization temperature is 80°C, the mass of the initiator ammonium persulfate is 1% of the mass of the monomer, the mass of the regulator mercaptopropionic acid is 0.8% of the mass of the monomer, the dropping time is 2h, and the temperature is kept for 1h. The specific preparation process is:

[0035] Accurately weigh 24g of prenol polyoxyethylene ether (Mn=2400) and 1.98g of pyrophosphoric acid in a 100mL three-necked flask, fix them in an oil bath at 80°C, blow in nitrogen gas for 30min, and then react in a closed and constant temperature for 12h, and the reaction ends Then add 10g deionized water;

[0036] Weigh 0.24g of ammonium persulfate and 0.192g of mercaptopropionic acid and dissolve them in 10g of deionized water....

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Abstract

The invention discloses a preparation method for a polyphosphate water-reducing agent. The preparation method is characterized by comprising the following steps: subjecting isoamylenol polyoxyethylene ether and pyrophosphoric acid to a phosphate esterification reaction so as to obtain isoamylenol polyoxyethylene ether phosphate monomer; and then with ammonium persulfate as an initiator and mercaptopropionic acid as a conditioning agent, carrying out free radical homopolymerization in an aqueous solution so as to obtain the polyphosphate water-reducing agent. The preparation method is simple; a single, cheap and low-cost raw material is used in the method; and the obtained polyphosphate water-reducing agent is nonvolatile and basically nontoxic, and has good biodegradability, a water-reducing rate and slump loss resistance.

Description

technical field [0001] The invention relates to a preparation method of a high-performance concrete admixture, in particular to a preparation method of a polyphosphate water reducer. Background technique [0002] In today's concrete engineering, admixtures have become an indispensable part, and among admixtures, water reducers are the most important. This is because the water reducer can significantly improve the fluidity of concrete at low dosage, reduce the amount of water and increase the strength of concrete. The development of water reducers has been developed to the third generation of polycarboxylate water reducers, and the synthesis of polycarboxylate water reducers requires at least two basic monomers: one of the monomers is called a small monomer, which provides carboxyl groups to make Water reducers can be adsorbed on the surface of cement, especially acrylic acid is the most common. Another monomer is called a macromonomer, and the side chain with polyvinyl alco...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F299/02C08G65/327C04B24/26C04B103/30
CPCC04B24/246C04B2103/302C08F299/022C08G65/327
Inventor 王文平邢国兵
Owner HEFEI UNIV OF TECH
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