Preparation method of mud resisting and slump retaining type phosphate group containing polycarboxylate superplasticizer

A technology of phosphate-based polycarboxylic acid and water-reducing agent, applied in the field of polycarboxylate water-reducing agent for cement concrete, can solve the problem that the structure and molecular weight of the water-reducing agent cannot be accurately controlled, which is unfavorable for large-scale production and application, and production technology. complex problems, to achieve the effect of ensuring slump loss, reducing sensitivity, and enriching sources

Active Publication Date: 2016-10-12
JIANGSU CHINA RAILWAY ARIT NEW MATEIRALS CO LTD
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Problems solved by technology

[0004] Chinese patent document CN 105418857A reports a preparation method of a phosphate-based polycarboxylate water reducer, which is to firstly carry out copolymerization of unsaturated polyether macromonomer, unsaturated carboxylic acid ester, and unsaturated alcohol in an organic solvent The polycarboxylate superplasticizer prepolymer is obtained by reaction, and then the polycarboxylate superplasticizer prepolymer is phosphorylated and modified, and then in the presence of an acidic aqueous solution, the carboxylate group on the phosphorylated modified product is Hydrolyze the mass, remove the organic solvent, and finally neutralize to obtain the polycarboxylate water reducer containing phosphate groups, but the production process of this invention is complicated, the conversion rate is n...

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  • Preparation method of mud resisting and slump retaining type phosphate group containing polycarboxylate superplasticizer
  • Preparation method of mud resisting and slump retaining type phosphate group containing polycarboxylate superplasticizer

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Embodiment 1

[0029] 1) Preparation of polycarboxylate superplasticizer prepolymer containing halogen: 1mol 3-bromopropene, 1mol acrylic acid and 5mol methallyl polyethylene glycol (300g / mol) in 0.05mol hydrogen peroxide, 0.1 Under the action of mol of molasses and 0.05mol of 2-mercaptopropionic acid, carry out free radical polymerization at 20°C for 5 hours to obtain bromine-containing polycarboxylate superplasticizer prepolymer;

[0030]2) Preparation of mud-resistant and slump-resistant phosphate-based polycarboxylate superplasticizer: 1 mol of bromine-containing polycarboxylate superplasticizer prepolymer and 3 mol of trimethyl phosphite were subjected to Arbuzov reaction at 80°C to obtain A phosphate-based copolymerization product; the pH value of the copolymerization product is adjusted to 6.5 with lye, and water is added to obtain a polycarboxylate water reducer with a mass concentration of 10%;

Embodiment 2

[0032] 1) Preparation of polycarboxylate superplasticizer prepolymer containing halogen: 1mol p-chloromethylstyrene, 0.1mol sodium methacrylate and 1.2mol allyl polyethylene glycol (800g / mol) in 0.01mol Under the action of ammonium persulfate, 0.03mol sodium metabisulfite and 0.005mol sodium methacryl sulfonate, keep at 50°C for free radical polymerization for 3 hours to obtain bromine-containing polycarboxylate superplasticizer prepolymer;

[0033] 2) Preparation of anti-mud and slump-containing phosphate-based polycarboxylate superplasticizer: Arbuzov reaction of 1 mol polycarboxylate superplasticizer prepolymer containing bromine and 4 monomethyl phosphite at 85°C to obtain phosphoric acid The copolymerization product of ester group; the pH value of the copolymerization product is adjusted to 7 with lye, and water is added to obtain a polycarboxylate water reducer with a mass concentration of 5%;

Embodiment 3

[0035] 1) Preparation of polycarboxylate superplasticizer prepolymer containing halogen: 1mol 3-chloro-2-methyl-1-propene, 1mol potassium methacrylate and 10mol methoxypolyethylene glycol acrylate (2000g / mol) Under the action of 0.1mol sodium persulfate, 0.2mol sodium ascorbate and 0.1mol mercaptoacetic acid, keep at 25°C for free radical polymerization for 3.5h to obtain a polycarboxylate superplasticizer prepolymer containing chlorine;

[0036] 2) Preparation of mud-resistant and slump-resistant polycarboxylate-based polycarboxylate superplasticizer: 1 mol of chlorine-containing polycarboxylate superplasticizer prepolymer and 5 mol of triethyl phosphite were subjected to Arbuzov reaction at 90°C to obtain phosphoric acid-containing A copolymerization product of ester groups; the pH value of the copolymerization product is adjusted to 6.5 with lye, and water is added to obtain a polycarboxylate water reducer with a mass concentration of 50%;

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Abstract

The invention discloses a preparation method of a mud resisting and slump retaining type phosphate group containing polycarboxylate superplasticizer. The preparation method comprises the following specific steps that 1, a halogen containing polycarboxylate superplasticizer prepolymer is prepared, wherein halogen containing unsaturated monomers, halogen containing unsaturated acid small monomers and halogen containing unsaturated polyether macromonomers or unsaturated ester macromonomers are subjected to an oxidation-reduction radical polymerization reaction to obtain the halogen containing polycarboxylate superplasticizer prepolymer; 2, the halogen containing polycarboxylate superplasticizer prepolymer and alkyl phosphate are subjected to an Arbuzov reaction to obtain a phosphate group containing copolymerization product, the pH value is adjusted after reacting is completed, water is added, and then the polycarboxylate superplasticizer is obtained. The mud resisting and slump retaining type phosphate group containing polycarboxylate superplasticizer prepared through the method has the advantages of being low in mixing amount, high in water reducing ratio, long in slump retaining time and high in mud resisting property, can avoid the adverse effect brought by mud containing aggregate in concrete and is simple in synthesis process, easy to control and low in production cost.

Description

technical field [0001] The invention relates to the technical field of a polycarboxylate water-reducer for cement concrete, in particular to a preparation method of a mud-resisting slump-retaining polycarboxylate-containing polycarboxylate water-reducer. Background technique [0002] Polycarboxylate superplasticizers are more and more widely used in concrete engineering because of their excellent properties such as low dosage, high water reducing rate, good slump retention, strong molecular structure adjustability, and environmental protection. However, a large number of engineering examples and studies have shown that compared with traditional naphthalene-based, melamine-based and sulfamic acid-based water-reducers, polycarboxylate-based water-reducers are more sensitive to the clay content of aggregates. The mud in the mixture will absorb the polycarboxylate superplasticizer. With the increase of the mud content, the water reducing and dispersing ability of the polycarboxy...

Claims

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Application Information

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IPC IPC(8): C08F283/06C08F220/56C08F238/00C08F220/06C08F214/16C08F8/40C04B24/26C04B103/30
CPCC04B24/2694C04B2103/302C08F8/40C08F283/065C08F214/16C08F220/06C08F238/00C08F220/56
Inventor 李梦婷王毅姜海东王高明郑春扬郭兆来
Owner JIANGSU CHINA RAILWAY ARIT NEW MATEIRALS CO LTD
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