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Preparation method of polyester type pure solid polycarboxylic acid high-performance water reducing agent

A pure solid, polycarboxylic acid technology, applied in the field of polycarboxylate high-performance water reducers, can solve the problems of inability to fully realize solid polyester type water reducers, enrich the preparation methods of synthetic polycarboxylates, etc., and achieve good market competition force and application prospects, avoiding the reduction of separation and concentration efficiency, and reducing the effect of transportation costs

Active Publication Date: 2013-04-03
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polymerization step in this method adopts the bulk polymerization method, and the whole process does not use water as a solvent or medium, which effectively improves the problem that in the past, the aqueous solution system was usually used for polymerization and then concentrated and separated, but the solid polyester water reducer could not be fully realized. , which enriches the preparation method of synthetic polycarboxylate high-performance water reducer

Method used

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  • Preparation method of polyester type pure solid polycarboxylic acid high-performance water reducing agent
  • Preparation method of polyester type pure solid polycarboxylic acid high-performance water reducing agent
  • Preparation method of polyester type pure solid polycarboxylic acid high-performance water reducing agent

Examples

Experimental program
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Effect test

Embodiment 1

[0023] First, add 100g of methoxypolyethylene glycol (molecular weight: 2500) into the reactor, raise the temperature to 50°C, and when the methoxypolyethylene glycol is in liquid state, add 0.07g of hydroquinone, 14.41g of acrylic acid, 1.5g of p-toluenesulfonic acid, and the stirring time between each addition is 20 minutes. When the temperature rises to 80°C, add 17.16g of cyclohexane, and continue to heat up to 105°C for esterification reaction. The water obtained from the reaction was separated, and after 6 hours of reaction, the cyclohexane was removed by vacuuming to obtain the esterification reaction product; the esterification reaction product was added to the reactor, the temperature was raised to 50°C, and 2.76g of mercapto groups were added to the reactor in turn. Acetic acid, 4.32g of acrylic acid, 0.48g of dibenzoyl peroxide, and the stirring time between each addition is 20 minutes, continue to heat up to 95°C for bulk polymerization, react for 4 hours, stop the ...

Embodiment 2

[0025] After the cement dispersant with a mass fraction of 35% obtained in Example 1 was stored at 6°C for 30 days, its implementation effect was measured.

Embodiment 3

[0027] First, 50g of polyethylene glycol (molecular weight: 500) was added to the reactor, and the temperature was raised to 70°C. When the polyethylene glycol was in a liquid state, 0.65g of phenothiazine, 12.91g of methacrylic acid, 5g of Phosphoric acid, and the stirring time between each feeding is 5 minutes. When the temperature rises to 100°C, 18.87g toluene is added, and the temperature is continued to rise to 110°C to carry out the esterification reaction. Vacuumize the toluene to get the esterification reaction product; put the esterification reaction product into the reactor, heat up to 70°C, add 0.53g of mercaptopropionic acid, 4.8g of acrylic acid, 32.67g of maleic anhydride, 1.64g of azobisisobutyronitrile, and the stirring time between each addition is 5 minutes, continue to heat up to 75°C for bulk polymerization, react for 8 hours, stop the reaction, cool to 25°C, and obtain 106.66g of polyester-type pure The solid reaction product was finally diluted with 130....

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Abstract

The invention discloses a preparation method of a polyester type pure solid polycarboxylic acid high-performance water reducing agent, belonging to the field of water reducing agents. According to the invention, by taking a (methyl) acrylic acid monomer and a polyethylene glycol compound as reactants, a polymerizable macromonomer is prepared through esterification reaction under the effect of a catalyst, and the polymerizable macromonomer conducts a free radical bulk polymerization reaction with an unsaturated carboxylic acid monomer and a chain transfer agent under the effect of an initiator in an environment without any solvent to obtain the polyester type pure solid polycarboxylic acid high-performance water reducing agent. The method disclosed by the invention has strong process controllability, high degree of polymerization and low cost and prevents environmental pollution; a completely anhydrous polyester type pure solid polycarboxylic acid high-performance water reducing agent is prepared through esterification reaction and bulk polymerization, which has neat cement paste liquidity and holding ability, cement adaptability and concrete application performance similar to a traditional solution method; meanwhile, since the polymer product is an anhydrous pure solid, a solution with any concentration can be prepared according to actual needs; and without the after-treatment processes such as heating and drying, solvent separation and the like, the transportation is more convenient, and good market competitiveness and application prospects are realized.

Description

technical field [0001] The invention relates to the technical field of a polycarboxylate high-performance water-reducer for cement concrete, in particular to a polyester-type pure solid anhydrous polycarboxylate high-performance water-reducer synthesized by the copolymerization reaction of polyethylene glycol compounds. The specific preparation method of the agent. Background technique [0002] The rapid growth of my country's national economy has brought new opportunities for the further development of the construction industry. At the same time, the green and high-performance concrete has put forward higher requirements for various components of concrete, especially admixtures. Polycarboxylate superplasticizer, the third-generation product of superplasticizer, plays an important role in the entire field of concrete admixtures. With the continuous expansion of its dosage and application range, it is necessary to further improve its application convenience under the premise ...

Claims

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Application Information

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IPC IPC(8): C08F290/06C08F220/06C08F222/02C08F222/06C08F2/38C04B24/28C04B103/30
Inventor 刘晓王子明朱洁梁旭李慧群周姮路芳卢子臣
Owner BEIJING UNIV OF TECH
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