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Method for preparing polycarboxylate superplasticizer with main chain modified isocyanate grafted positive ion side chain

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

Active Publication Date: 2016-11-09
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 superplasticizer with main chain modified isocyanate grafted positive ion side chain
  • Method for preparing polycarboxylate superplasticizer with main chain modified isocyanate grafted positive ion side chain
  • Method for preparing polycarboxylate superplasticizer with main chain modified isocyanate grafted positive ion side chain

Examples

Experimental program
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Effect test

Embodiment 1

[0029] First, 4.8g of acrylic acid, 3.87g of fumaric acid, 1.07g of acrylamide, 17.53g of water, 1.57g of mercaptoacetic acid, and 31.09g of a 2% potassium persulfate aqueous solution were successively added to the reactor, and each feeding interval was stirred. The time is 15 minutes, and the temperature is raised to 55°C for polymerization reaction, and the reaction is 6 hours to obtain the aqueous solution of polycarboxylic acid-amide; the aqueous solution of the obtained product polycarboxylic acid-amide is vacuumed to remove the moisture in the system, and 3.13 g of sodium hypochlorite and 0.6 The mixed solution of sodium hydroxide was 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 methacryloyloxyethyl dimethyl butyl Ammonium bromide and 0.53 n-pentanol, then add 799.1g water and be mixed with the aqueous solution that mass concentration is 10%, the reactor is filled with nitrogen and i...

Embodiment 2

[0031] After the polycarboxylate superplasticizer 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 add 0.66g acrylic acid, 11.83g itaconic acid, 1.85g acrylamide, 28.6558g water, 2.39g sodium methylpropene sulfonate, 30g mass fraction in the reactor successively and be 1% sodium persulfate aqueous solution, and each time Stir for 20 minutes between additions, heat up to 75°C for polymerization reaction, and react for 4 hours to obtain an aqueous solution of polycarboxylic acid-amide; vacuumize the aqueous solution of the obtained product polycarboxylic acid-amide to remove moisture in the system, and add 5.81g The mixed solution of sodium hypochlorite and 1.04g sodium hydroxide was stirred for 12 minutes, and reacted at a constant temperature of 50°C for 1 hour to obtain polycarboxylic acid-isocyanate; in another reactor, 73.56g dimethyldiallyl chloride was added Ammonium and 0.96 n-butanol, then add 894.28g of water to prepare an aqueous solution with a mass concentration of 7.69%. The reactor is filled with nitrogen for 5 times to remove oxygen and then sealed...

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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 type polycarboxylate water reducer for concrete, in particular to a kind of polycarboxylate water reducer which uses unsaturated carboxylic acid monomer and unsaturated amide monomer to first polymerize the main chain and then polymerize the modified isocyanate group A specific preparation method for synthesizing a cationic side chain type polycarboxylate water reducer by cationic side chain and then main side chain grafting reaction. Background technique [0002] As an important component in concrete, polycarboxylate superplasticizer has increasingly become the focus of research due to its low dosage, high water reducing rate, and large degree of freedom in molecular design. At the same time, it can also improve the concrete Workability, strength, durability, etc., have become the most important member of the family of concrete chemical admixtures. However, concrete raw materials h...

Claims

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Application Information

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Patent Type & Authority Applications(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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