Method for preparing polycarboxylate water-reducer by grafting cationic side chain with modified isocyanate of main chain

A technology of isocyanate and cation, applied in the field of cationic side chain polycarboxylate water reducer

Active Publication Date: 2019-03-22
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, this requires a fundamental innovation in the molecular structure of the synthesized polycarboxylate superplasticizer. It does not stick to the traditional synthesis method, and innovatively uses amide-modified isocyanate, high-valent cerium salt to trigger long chain polycations, and isocyanate bonding. The synthetic routes and characteristics of branch-reaction polycation side chains and polyether side chains not only have the composite performance of water-reducing slump-resistance-mud, but are also beneficial to industrial production and popularization and application. There are no reports on this aspect at home and abroad.

Method used

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  • Method for preparing polycarboxylate water-reducer by grafting cationic side chain with modified isocyanate of main chain
  • Method for preparing polycarboxylate water-reducer by grafting cationic side chain with modified isocyanate of main chain
  • Method for preparing polycarboxylate water-reducer by grafting cationic side chain with modified isocyanate of main chain

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] First, 4.8 g of acrylic acid, 3.87 g of fumaric acid, 1.07 g of acrylamide, 17.53 g of water, 1.57 g of mercaptoacetic acid, and 31.09 g of potassium persulfate aqueous solution with a mass fraction of 2% were sequentially added to the reactor, and stirring was performed at each feeding interval. The time was 15 minutes, and the temperature was raised to 55 ° C to carry out the polymerization reaction, and the reaction was carried out for 6 hours to obtain an aqueous solution of polycarboxylic acid-amide; The mixed solution of g sodium hydroxide, stirred for 5 minutes, and reacted at a constant temperature of 35°C for 1.5 hours to obtain polycarboxylic acid-isocyanate; 88.26g of methacryloyloxyethyldimethylbutyl was added to another reactor Ammonium bromide and 0.53 n-amyl alcohol were added, and 799.1 g of water was added to prepare an aqueous solution with a mass concentration of 10%. The reactor was filled with nitrogen for 4 times and deoxygenated for 15 minutes, the...

Embodiment 2

[0031] After the polycarboxylate water-reducing agent solution with a mass fraction of 50% obtained in Example 1 was stored at 6° C. for 20 days, its implementation effect was measured.

Embodiment 3

[0033] First, 0.66g of acrylic acid, 11.83g of itaconic acid, 1.85g of acrylamide, 28.6558g of water, 2.39g of sodium methacrylate sulfonate, 30g of 1% aqueous sodium persulfate solution were added to the reactor in sequence, and each time The feeding interval was stirred for 20 minutes, and the temperature was raised to 75 ° C to carry out the polymerization reaction, and the reaction was carried out for 4 hours to obtain an aqueous solution of polycarboxylic acid-amide; The mixed solution of sodium hypochlorite and 1.04g of sodium hydroxide was stirred for 12 minutes, and then reacted at a constant temperature of 50°C for 1 hour to obtain polycarboxylic acid-isocyanate; in another reactor, 73.56g of dimethyldiallyl chloride was added. Ammonium and 0.96 n-butanol, and then add 894.28 g of water to prepare an aqueous solution with a mass concentration of 7.69%. The reactor is filled with nitrogen for 5 times and deoxygenated for 10 minutes, and then sealed. Add 4.99 g of cerium...

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Abstract

The invention relates to a method for preparing a polycarboxylate superplasticizer with a main chain modified isocyanate grafted positive ion side chain and belongs to the field of the superplasticizer. The method comprises the following steps: by taking unsaturated carboxylic acid and unsaturated amide monomer as reactants, acquiring a polycarboxylic acid-amide main chain through free radical polymerization; further modifying the amide group on the main chain as isocyanate group; by taking unsaturated positive ion quaternary ammonium salt monomer as the reactant, performing free radical polymerization under an oxidation-reduction initiating system composed of high-price cerate and alcohol, thereby acquiring an end hydroxy positive ion side chain; performing grafting reaction on polycarboxylic acid main chain containing isocyanate with the end hydroxy positive ion side chain and the polyethylene glycol compound. The method has the advantages of simple and controllable process, low cost, energy-saving effect, high efficiency, polyethylene glycol and no pollution; the main chain modified isocyanate is grafted with the positive ion side chain and the polyether side chain according to a molecular structure design method; the double modification for main chain and side chain of molecule is successfully realized; the water-reducing collapse-protecting property and the capacity of restraining clay side effect are better than those of the common polycarboxylate superplasticizer.

Description

technical field [0001] The invention relates to the technical field of a cationic side-chain polycarboxylate water-reducing agent for concrete, in particular to a method of using unsaturated carboxylic acid monomers and unsaturated amide monomers to first polymerize the main chain to modify isocyanate groups and then polymerize them A specific preparation method for synthesizing a cationic side chain type polycarboxylate water-reducing agent by cationic side chain and then main side chain branching reaction. Background technique [0002] As an important component of concrete, polycarboxylate superplasticizer has increasingly become the focus of research due to its advantages of low dosage, high water reduction rate, and large degree of freedom in molecular design. Workability, strength, durability, etc., have become the most important member of the concrete chemical admixture family. However, concrete raw materials have an important influence on the application performance ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G81/02C08F220/06C08F222/02C08F220/56C08F228/02C08F222/06C08F8/06C08F120/34C08F126/02C08F4/40C04B24/26C04B103/30
CPCC04B24/2652C04B2103/302C08F4/40C08F8/06C08F120/34C08F126/02C08F220/06C08F220/56C08F222/02C08G81/025C08F228/02C08F222/06
Inventor 刘晓管佳男王子明庞晓凡申和庆薛龙
Owner BEIJING UNIV OF TECH
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