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Preparation method of amine-ester slow-setting polycarboxylic acid type water-reducer

A slow-coagulation carboxylic acid and water-reducing agent technology, which is applied in the field of polycarboxylic acid-based water-reducing agents, can solve the problems of complicated process methods, difficult realization, and easy thermal polymerization, etc., and achieve abundant raw material sources, rapid response, and easy engineering operation Effect

Inactive Publication Date: 2015-09-30
JIANGSU CHINA RAILWAY ARIT NEW MATEIRALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Raw material problem: macromonomer materials such as allyl polyoxyethylene ether and methoxy polyethylene glycol unsaturated carboxylate for the production of polycarboxylate water reducers, there are no such intermediate products in China
(Meth)acrylic acid has a low boiling point and is easy to thermally polymerize. It may self-polymerize or copolymerize with esterified macromonomers during the preparation of macromonomers. The esterified mixture is prone to partial polymerization or polymerization under conditions triggered by heat or other factors. Overall implosion polymerization, there is a contradiction between high temperature esterification and high temperature polymerization
[0006] Synthesis process problem: Most domestic polycarboxylate water reducers are in the experimental research stage, and there is no mature production process that can be referred to. The process methods provided by foreign patent documents are too complicated, and there are too many influencing factors, such as polymerization in a solvent-free system , or polymerization in low boiling point solvents or aqueous solutions, all require extremely strict feeding methods, solvent recovery and nitrogen protection reaction measures, etc., which are not easy to achieve in actual tests and production

Method used

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  • Preparation method of amine-ester slow-setting polycarboxylic acid type water-reducer
  • Preparation method of amine-ester slow-setting polycarboxylic acid type water-reducer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1) Preparation of hydroxyl-containing copolymerization product: 10 mol 2-methallyl alcohol, 9 mol acrylic acid and 1 mol sodium methoxyallyl sulfonate at 6°C in 1 mol benzoyl peroxide, 2 mol ferrous pyrophosphate, 0.01 mol Oxidation-reduction radical polymerization was carried out under the action of thioglycolic acid for 30 minutes to obtain a copolymer product with a molecular weight of 2000;

[0031] 2) Preparation of polyethylene glycol monomethyl ether monoisocyanate: Add 10 mol of polyethylene glycol monomethyl ether with a molecular weight of 400 to 10.5 mol excess toluene diisocyanate (TDI) at 0°C under a nitrogen atmosphere. - under the effect of dimethylcyclohexylamine, reaction under reduced pressure distillation obtains polyethylene glycol monomethyl ether monoisocyanate after reaction 10min;

[0032]3) Preparation of urethane type retarding water reducer: add 10 mol of hydroxyl-containing copolymerization product to 10 mol polyethylene glycol monomethyl eth...

Embodiment 2

[0034] 1) Preparation of hydroxyl-containing copolymerization product: 10 mol hydroxyethyl acrylate, 1 mol methacrylic acid and 1 mol potassium allyl sulfonate were mixed at 45°C in 0.9 mol benzoyl peroxide, 1.8 mol N,N-diethylaniline, Under the action of 0.1mol 2-mercaptopropionic acid, oxidation-reduction radical polymerization was carried out for 40 minutes to obtain a copolymer product with a molecular weight of 2500;

[0035] 2) Preparation of polyethylene glycol monomethyl ether monoisocyanate: Add 10 mol of polyethylene glycol monomethyl ether with a molecular weight of 450 to 10.1 mol of excess hexamethylene diisocyanate (HDI) at 8°C under a nitrogen atmosphere. Under the effect of mol bis(2-dimethylaminoethyl) ether, reaction under the effect of 40min underpressure distillation obtains polyethylene glycol monomethyl ether monoisocyanate;

[0036] 3) Preparation of urethane-type retarding water reducer: add 10mol of hydroxyl-containing copolymer product to 20mol of pol...

Embodiment 3

[0038] 1) Preparation of hydroxyl-containing copolymer products: 10mol hydroxyethyl methacrylate, 5mol sodium acrylate at 45°C in 0.8mol hydrogen peroxide, 1.6mol ferrous sulfate, 0.05mol 3-mercaptopropionic acid for oxidation-reduction freedom Based polymerization reaction 50min obtains the copolymerization product that molecular weight is 3000;

[0039] 2) Preparation of polyethylene glycol monomethyl ether monoisocyanate: 10 mol of polyethylene glycol monomethyl ether with a molecular weight of 500 was added to 10.2 mol of excess isophorone diisocyanate (IPDI) under an argon atmosphere at 6°C. Under the action of 0.07mol N,N,N',N'-tetramethylalkylenediamine, reacted for 30min and then distilled under reduced pressure to obtain polyethylene glycol monomethyl ether monoisocyanate;

[0040] 3) Preparation of urethane-type retarding water reducer: 10 mol of hydroxyl-containing copolymerization product obtained in step 1) was added to 20 mol of polyethylene glycol monomethyl eth...

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Abstract

The invention discloses a preparation method of an amine-ester slow-setting polycarboxylic acid type water-reducer. The preparation method comprises the following concrete steps: 1) a unsaturated acid monomer and a hydroxyl-containing unsaturated monomer are subjected to a normal temperature oxidation-reduction free radical polymerization reaction under the action of an initiator, a reducing agent and a chain transfer agent to obtain a hydroxyl-containing copolymerization product; 2) excessive diisocyanate is added into methoxypolyethylene glycol to react under the action of a catalyst so as to obtain methoxypolyethylene glycol monoisocyanate; and 3) the hydroxyl-containing copolymerization product obtained in the step 1) is added into the methoxypolyethylene glycol monoisocyanate obtained in the step 2) to react, and then pH value is adjusted by alkali neutralization so as to obtain the amine-ester slow-setting polycarboxylic acid type water-reducer. According to the method, product performance is adjusted by controlling molecular structure / molecular weight of the hydroxyl-containing copolymerization product and molecular weight of methoxy polyethylene glycol / type of diisocyanate. Reaction efficiency is greatly raised, and reaction time is shortened. In addition, no organic solvent is used; the water-reducer is nontoxic and pollution-free; and operation is simple. The product performance is stable.

Description

technical field [0001] The present invention relates to the technical field of polycarboxylate water-reducer for cement concrete, in particular to the preparation of a urethane-type slow-coagulation carboxylic acid-based water-reducer using isocyanate and hydroxyl urethane reaction and free radical polymerization method. Background technique [0002] The application of polycarboxylate high-efficiency water reducer in concrete is more and more extensive. Its performance advantages bring great convenience to the quality control of concrete. However, there is also the problem of excessive slump loss of concrete mixture. question. With the variation of raw materials of modern concrete, it has added a lot of difficulty to the quality control of concrete mixture. At present, ordinary polycarboxylate superplasticizers are difficult to maintain good workability and slump retention of concrete mixtures in a short period of time. The slow-release polycarboxylate high-efficiency wat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/02C08G65/48C08F220/06C08F216/04C08F228/02C08F220/28C08F212/14C08F216/08C04B24/28
Inventor 钱珊珊石宇丁蓓王毅姜海东郑春扬
Owner JIANGSU CHINA RAILWAY ARIT NEW MATEIRALS CO LTD
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