Highly-efficient polyether-modified sulfamate water-reducing agent, and preparation method and application thereof

A technology of sulfamate and high-efficiency water reducer, which is applied in the field of polyether modified sulfamate high-efficiency water reducer, can solve the problems of no change of water reducer, high dosage, large collapse loss, etc. Dispersion retention performance, effect of improving dispersion performance

Active Publication Date: 2018-07-06
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although many researchers have modified the sulfamate superplasticizer, which can improve the dispersion and slump retention of the sulfamate superplasticizer, it is mainly through the introduction of other The adsorption group does not change the dispersion mechanism of the water reducing agent, mainly relying on electrostatic repulsion to disperse, so it cannot fundamentally solve the problems of low water reducing rate, high dosage, large collapse loss, etc.

Method used

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  • Highly-efficient polyether-modified sulfamate water-reducing agent, and preparation method and application thereof
  • Highly-efficient polyether-modified sulfamate water-reducing agent, and preparation method and application thereof
  • Highly-efficient polyether-modified sulfamate water-reducing agent, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Weigh 0.08mol sodium 4-aminobenzenesulfonate and 0.02mol sodium 4-hydroxybenzenesulfonate, place them in a 500mL three-neck flask equipped with a stirring paddle and a reflux condenser, add 0.1mol polyether PH-1, 0.1mol water Salicylic acid, 0.1mol urea, and 0.12mol phenol were heated up to 80°C to dissolve them all, and 20.6g of concentrated sulfuric acid (10wt% of the total amount of monomers) was added while stirring, and 0.52mol of formaldehyde was added dropwise within 20 minutes. React at 90°C for 5 hours to obtain the molecular backbone of the sulfamate superplasticizer. Then add 60g of xylene into the flask, slowly add 10g of concentrated sulfuric acid, install a water separator, raise the temperature to 130°C, and perform the esterification reaction for 4 hours. After no water evaporates, turn off the stirring and heating, stop the reaction, and recover the fraction Aqueous xylene in the water container. After the reaction was completed, it was neutralized wit...

Embodiment 2

[0057] Weigh 0.09mol sodium 4-aminobenzenesulfonate and 0.01mol sodium 4-hydroxybenzenesulfonate, place them in a 500mL three-necked flask equipped with a stirring paddle and a reflux condenser, add 0.08mol polyether PH-2, 0.1mol salicylic acid , 0.01mol urea and 0.19mol hydroquinone, be warmed up to 85 ℃ and make it all dissolve, add vitriol oil 11.73g (5wt% of monomer total amount) while stirring, after slowly adding 0.504mol formaldehyde dropwise in 20min, in React at a constant temperature of 90°C for 4 hours to obtain the molecular backbone of the sulfamate superplasticizer. Then add 60g of toluene to the flask, slowly add 20g of p-toluenesulfonic acid, install a water separator, raise the temperature to 120°C, and carry out the esterification reaction for 5 hours. After no water evaporates, stop the reaction and recover the water-carrying agent toluene . After the reaction was completed, it was neutralized with 30% NaOH solution, and 250 g of water was added to obtain a...

Embodiment 3

[0059] Weigh 0.048mol sodium 4-aminobenzenesulfonate, 0.032mol sodium 2-aminobenzenesulfonate, and 0.04mol sodium 4-hydroxybenzenesulfonate, place them in a 500mL three-necked flask equipped with a stirring paddle and a reflux condenser, and add 0.05 mol polyether PH-3, 0.1mol salicylic acid, 0.1mol urea and 0.1mol phenol, be heated up to 100 ℃ and make it all dissolve, add 28.4g p-toluenesulfonic acid (15wt% of monomer total amount) while stirring ), slowly add 0.52mol formaldehyde dropwise within 20min, and react at a constant temperature of 110°C for 5h to obtain the molecular backbone of the sulfamate superplasticizer. Then add 50g of benzene in the flask, slowly add 10g of phosphoric acid (mass fraction greater than 85%), install a water separator, raise the temperature to 120°C, and perform the esterification reaction for 4 hours. After no water evaporates, stop the reaction and recover the water agent benzene. After the reaction was completed, it was neutralized with N...

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Abstract

The invention provides a highly-efficient polyether-modified sulfamate water-reducing agent, and a preparation method thereof and application thereof. The main molecular chain of a sulfamate water-reducing agent is grafted with a polyether side chain, so the sulfamate water-reducing agent is improved in dispersion effect on cement particles and has enhanced slump loss resistance. The preparation method comprises the following steps: (1) with hydroxy-containing polyether of a specific structure as a solvent, subjecting aminobenzenesulfonate, hydroxybenzenesulfonate, salicylic acid, a phenol compound, urea and an aldehyde compound to a condensation reaction under the action of an acidic condensation catalyst so as to obtain a carboxyl-containing sulfamate water-reducing agent intermediate; and (2) subjecting the hydroxyl-containing polyether and the carboxyl-containing sulfamate water-reducing agent intermediate to an esterification reaction in the presence of a water-carrying agent andan esterification catalyst, removing the water-removing agent, and adding alkali for neutralization so as to obtain the highly-efficient polyether-modified sulfamate water-reducing agent. The preparedpolyether-modified sulfamate water-reducing agent has a molecular weight of 24,000 to 38,000.

Description

technical field [0001] The invention relates to a polyether modified sulfamate high-efficiency water reducer, its preparation method and application, and belongs to the technical field of concrete admixtures. Background technique [0002] As a building material, concrete is widely used in many fields. With the development of concrete, it also promotes the rapid development of concrete admixture technology. Concrete admixture is one of the indispensable components in modern concrete and a part of concrete modification. important methods and techniques. Commonly used admixtures mainly include water reducing agents, retarders, air-entraining agents, early strength agents, antifreeze agents, expansion agents, etc., and water reducing agents are the most important components. At present, the types of high-efficiency water reducers in China mainly include: sulfamate high-efficiency water reducer, naphthalene sulfonate high-efficiency water-reducer, melamine sulfonate high-efficie...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/00C08G14/08C08G14/12C04B24/22C04B103/30
CPCC04B24/22C04B2103/302C08G14/08C08G14/12C08G81/00
Inventor 马建峰王兵冉千平王涛齐帅范士敏杨勇刘加平
Owner JIANGSU SOBUTE NEW MATERIALS
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