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Aryl sulfonic acid intermediate and preparation method and application thereof in synthesis of low-temperature-sensitive admixture for concrete

A technology of aryl sulfonic acid and intermediates, applied in the field of concrete admixtures, can solve the problems of low application environmental sensitivity and low water reduction efficiency, achieve the effect of low dosage and solve sensitivity problems

Active Publication Date: 2020-07-31
JIANGSU SOBUTE NEW MATERIALS +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The water reducing efficiency of these two types of water reducing agents is significantly lower than that of the third-generation water reducing agent comb-type polycarboxylate water reducing agent. Therefore, it is necessary to develop a water reducing agent that is less sensitive to the application environment and has better dispersion performance. Significance

Method used

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  • Aryl sulfonic acid intermediate and preparation method and application thereof in synthesis of low-temperature-sensitive admixture for concrete
  • Aryl sulfonic acid intermediate and preparation method and application thereof in synthesis of low-temperature-sensitive admixture for concrete
  • Aryl sulfonic acid intermediate and preparation method and application thereof in synthesis of low-temperature-sensitive admixture for concrete

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] Example 1 (b / a=1 / 3, c / a=0.8, d / b=1.0)

[0072] (1) In a 2000ml four-neck flask equipped with electromechanical stirring and constant temperature heating oil bath, add polyether F-1 (Mw=1174, 0.5mol) 587g, formaldehyde aqueous solution 32.8g (0.4mol, 37.5% aqueous solution), Sulfuric acid (concentration 98%) 11.74g, ethylene glycol dimethyl ether 30g, the temperature was raised to 100°C for precondensation reaction for 5h to obtain a prepolymerization mixture, which was tested by GPC and had a molecular weight of 6328;

[0073] (2) Add 301.5 g of sulfonic acid monomer G-1 (Mw=201, 1.5 mol) to the above prepolymerization mixture, add 121.5 g (1.5 mol, 37.5% aqueous solution) of formaldehyde solution, and raise the temperature to 105° C. for 6 h. The reaction is cooled to room temperature, neutralized with 30% lye until the pH is about 10, and the reaction is continued at 110° C. for 0.5-1 hour to remove unreacted formaldehyde. The reaction was cooled to room temperature ...

Embodiment 2

[0074] Example 2 (b / a=1 / 1, c / a=1.0, d / b=1.0)

[0075] (1) In a 2000ml four-necked flask equipped with electric mechanical stirring and constant temperature heating oil bath, add 587g of polyether F-2 (Mw=1174, 0.5mol), 41g of formaldehyde aqueous solution (0.5mol, 37.5% aqueous solution), sulfuric acid (concentration 98%) 11.74g, ethylene glycol dimethyl ether 30g, heat up to 100°C for pre-condensation reaction for 5h to obtain a pre-polymerization mixture, the molecular weight is 4780 by GPC test;

[0076] (2) Add 100.5 g of sulfonic acid monomer G-1 (Mw=201, 0.5 mol) to the above prepolymerization mixture, add 40.5 g of formaldehyde aqueous solution (0.5 mol, 37.5% aqueous solution), and heat up to 105° C. for 6 hours. The reaction is cooled to room temperature, neutralized with 30% lye until the pH is about 10, and the reaction is continued at 110° C. for 0.5-1 hour to remove unreacted formaldehyde. The reaction was cooled to room temperature and diluted with water to a so...

Embodiment 3

[0077] Embodiment 3 (b / a=1 / 2, c / a=1.0, d / b=1.0)

[0078] (1) In a 2000ml four-necked flask equipped with electric mechanical stirring and constant temperature heating oil bath, add 587g of polyether F-2 (Mw=1174, 0.5mol), 41g of formaldehyde aqueous solution (0.5mol, 37.5% aqueous solution), sulfuric acid (concentration 98%) 11.74g, ethylene glycol dimethyl ether 30g, heated up to 100°C for pre-condensation reaction for 5h to obtain a pre-polymerization mixture, tested by GPC, the molecular weight was 5125;

[0079] (2) Add 201 g of sulfonic acid monomer G-1 (Mw=201, 1.0 mol) to the above prepolymerization mixture, add 81 g of formaldehyde aqueous solution (1.0 mol, 37.5% aqueous solution), and heat up to 105° C. for 6 h. The reaction is cooled to room temperature, neutralized with 30% lye until the pH is about 10, and the reaction is continued at 110° C. for 0.5-1 hour to remove unreacted formaldehyde. The reaction was cooled to room temperature and diluted with water to a s...

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Abstract

The invention discloses an aryl sulfonic acid intermediate, and a preparation method and application thereof in the synthesis of a low-temperature-sensitive admixture. The aryl sulfonic acid intermediate introduces an aromatic ring and a sulfonic acid adsorption group into a main chain of a macromolecule of the low-temperature-sensitive admixture for concrete. An aromatic ring main chain and a polyether macro-monomer side chain, which are linked by urea bonds, are introduced into the low-temperature-sensitive admixture at the same time. The water reducer is high in water reducing rate and lowin sensitivity to the environment temperature, and has very important significance in expanding the application environment of water reducers.

Description

technical field [0001] The invention relates to an aryl sulfonic acid intermediate and a preparation method thereof, and its application in synthesizing a low-temperature-sensitive admixture for concrete, belonging to the technical field of concrete admixtures. Background technique [0002] Water reducers are also called dispersants or plasticizers, and they get their name because they can reduce the water consumption of freshly mixed concrete when used. In the field of modern concrete technology, water reducing agent is one of the admixtures to improve the rheological properties of concrete, and has been regarded as the fifth component of concrete besides cement, sand, stone and water. [0003] With the rapid improvement of my country's economic strength, the construction of high-speed railways, highways, hydropower, nuclear power, large bridges and other projects has brought new opportunities for the development of high-performance concrete, but at the same time it is also...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/334C08G65/26C04B24/16
CPCC08G65/3346C08G65/2618C04B24/16Y02W30/91
Inventor 马建峰冉千平刘加平王涛王兵亓帅韩正范士敏
Owner JIANGSU SOBUTE NEW MATERIALS
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