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Preparation method for comb-shaped copolymer cement dispersant, monomer used therein and prepared comb-shaped copolymer cement dispersant

A technology of cement dispersant and comb copolymerization, which is applied in the field of preparation of comb copolymer cement dispersant, which can solve the problems of cumbersome steps, environmental pollution and increased cost

Inactive Publication Date: 2011-07-06
JIANGSU SUBOTE MATERIAL +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The steps of this preparation method are cumbersome, and it needs to be esterified first to prepare the active polyether macromonomer, and then to carry out copolymerization
A large amount of organic solvent toluene is used in the esterification, which not only increases the cost, but also causes pollution to the environment; in addition, the esterification with polyethylene glycol and acrylic acid in the preparation process will generate a large amount of by-product polyethylene glycol diacrylate, Seriously affect the quality of subsequent polymerization reactions

Method used

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  • Preparation method for comb-shaped copolymer cement dispersant, monomer used therein and prepared comb-shaped copolymer cement dispersant
  • Preparation method for comb-shaped copolymer cement dispersant, monomer used therein and prepared comb-shaped copolymer cement dispersant
  • Preparation method for comb-shaped copolymer cement dispersant, monomer used therein and prepared comb-shaped copolymer cement dispersant

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Experimental program
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preparation example Construction

[0055] Preparation of branched living macromonomer

[0056] 58g of allyl alcohol is placed in a four-necked flask with a reflux condenser, a thermometer, a nitrogen conduit and a stirrer, 23g of sodium metal is added, and nitrogen bubbling is continuously carried out in the reaction flask, stirred at normal temperature until dissolved, and then Raise the temperature to 120°C, slowly add 74g of glycidol dropwise for 6 hours, keep it warm for 2 hours, and cool to obtain Intermediate 1.

[0057] 33g of intermediate 1 was placed in a 2L dry stainless steel autoclave, and the autoclave was sealed. After evacuating the reactor, replace the air in the reactor with nitrogen three times, raise the temperature to 120°C, and keep the reactor continuously vacuumed for 30 minutes, then stop, then continuously and slowly feed 990g of ethylene oxide, keeping the temperature at 120°C and the pressure of 0.2MPa , react until the pressure no longer drops, evacuate to -0.08MPa, maintain for 30m...

Embodiment 1

[0084] In a 1L glass reactor equipped with a thermometer, stirrer, dropping funnel and nitrogen conduit, add 300g of water, add 200g of branched active macromonomer 1, stir and heat up to dissolve, and purge the reaction vessel with nitrogen, and heat up to 90°C , and then 17.4g maleic acid, 0.22g 3-mercaptopropionic acid and 80g water were mixed and stirred to make a uniform aqueous monomer solution, which was added dropwise to the reactor at a constant speed for 4 hours, while 80g was added dropwise at a constant speed The initiator aqueous solution containing 1.62g of potassium persulfate, the dropping time is 4.5h, after the whole solution is added dropwise, continue to keep warm for 8h, then cool down to 50°C, add sodium hydroxide to neutralize to pH=7.5, and the obtained solid content is 32.2 % transparent liquid, the molecular weight of the copolymer is 37,600, and the conversion rate of branched active macromonomer 1 is 90.2%.

Embodiment 2

[0086]In a 1L glass reactor equipped with a thermometer, a stirrer, a dropping funnel and a nitrogen conduit, add 200g of water, add 200g of branched active macromonomer 2, stir and heat up to dissolve, and purge the reaction vessel with nitrogen, and heat up to 95°C , and then 24.8g of acrylic acid, 1.61g of 2-mercaptopropionic acid and 80g of water were mixed and stirred to form a uniform monomer aqueous solution, which was added dropwise to the reactor at a constant speed for 2 hours, and 50g containing 4.33 The initiator aqueous solution of g ammonium persulfate, the dropping time is 2.5h, continue to keep warm for 4h after the whole solution is added dropwise, then cool down to 50°C, add potassium hydroxide to neutralize to pH=7.5, and obtain a solid content of 42.5%. Transparent liquid, the molecular weight of the copolymer is 22,300, and the conversion rate of branched active macromonomer 2 is 93.3%.

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Abstract

The invention relates to a preparation method for a comb-shaped copolymer cement dispersant, a monomer used in the comb-shaped copolymer cement dispersant and the prepared comb-shaped copolymer cement dispersant. The preparation method for the comb-shaped copolymer cement dispersant comprises the following steps: a monomer (a) and a monomer (b) are subjected to free-radical copolymerization in aqueous medium, wherein the monomer (a) is expressed with a general formula (I), and the monomer (b) is expressed with a general formula (II); and the mol ratio of the monomer (a) and the monomer (b) is preferably 1:(1 to 10). The structure formula of the comb-shaped copolymer cement dispersant obtained by the preparation method is shown in (VI). The new monomer (a) is introduced in the comb-shaped copolymer cement dispersant, and the molecular structure of the monomer (a) has an unsaturated reactive double bond and two branching polyoxyalkylene long chains, so that the steric hindrance among cement particles can be greatly enhanced, and the dispersion stability of cement can be enhanced. The preparation method for the comb-shaped copolymer cement dispersant is simple and convenient for production operation, and meanwhile, the prepared comb-shaped copolymer cement dispersant has the advantages of low dosage, good dispersivity, high water-reducing rate, small slump loss and low gas content.

Description

technical field [0001] The invention relates to a preparation method of a comb-shaped copolymer cement dispersant, monomers used and the obtained comb-shaped copolymer cement dispersant, belonging to the technical field of concrete admixtures. Background technique [0002] In recent years, comb-shaped polymer copolymers have been widely used as cement dispersants, becoming the third generation of high-performance concrete water reducers after lignosulfonate and naphthalene sulfonate. The new generation of comb-shaped copolymer cement dispersant has strong adjustable chemical structure, low dosage, high water reducing rate, good fluidity and fluidity retention of fresh concrete, low shrinkage, and significant reinforcement effect. The performance has been improved qualitatively and has been successfully applied to many major projects. [0003] Comb copolymer cement dispersant is mainly prepared by free radical copolymerization of unsaturated carboxylic acid and unsaturated r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F283/06C08G65/28C07C43/178C04B24/26C04B103/40C04B103/30
Inventor 杨勇冉千平刘加平缪昌文张志勇乔敏毛永琳
Owner JIANGSU SUBOTE MATERIAL
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