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Method for preparing concrete superplasticizer by utilizing synthesized aspirin waste liquor

A technology of high-efficiency water-reducing agent and aspirin, which is applied in the field of preparing high-efficiency water-reducing agent for concrete, can solve environmental pollution and other problems, and achieve the effect of solving environmental pollution problems, high water-reducing rate, and not easy to bleed

Inactive Publication Date: 2012-06-20
TIANJIN VOCATIONAL INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Another object of the present invention is to provide a new approach for comprehensive utilization of synthetic aspirin waste liquid to solve the problem of environmental pollution in the aspirin production process

Method used

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  • Method for preparing concrete superplasticizer by utilizing synthesized aspirin waste liquor
  • Method for preparing concrete superplasticizer by utilizing synthesized aspirin waste liquor
  • Method for preparing concrete superplasticizer by utilizing synthesized aspirin waste liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Add 133g (1.3mol) of chemically pure acetic anhydride to a 500ml four-necked flask equipped with a stirrer, a thermometer and a reflux condenser, add 0.5ml of concentrated sulfuric acid, heat on a water bath at 80°C, and add chemically pure water in batches under stirring 138g (1.0mol) of citric acid, maintain the reaction temperature at 80-85°C, and continue to stir and react for 60 minutes after the addition is complete. The reaction solution was cooled to 40°C, 5.4g of distilled water was added to decompose excess acetic anhydride, further cooled to 10°C for crystallization, the aspirin crystals were separated by filtration, washed with a small amount of water to obtain 153g of aspirin products (after drying), and the synthesis yield was 85%. Reaction mother liquor is about 124g. Distill the reaction mother liquor with a rotary thin film evaporator at -0.8Mpa vacuum, reclaim about 86.4g of acetic acid, and reclaim about 30g of phenolic residue.

Embodiment 2

[0046] In a four-necked flask equipped with a thermometer, a stirrer, a dropping funnel and a reflux condenser, add 30 g of recovered phenolic residues, add 100 g of deionized water, and adjust the pH of the solution to 10-11 with 30% sodium hydroxide to make most of the residues Dissolve and remove the insoluble residue by filtration to obtain the sodium salt solution of the phenolic residue. Add 15.0 g of p-aminobenzenesulfonic acid to the solution, stir until it is completely dissolved, adjust the pH to 8.0-8.5 with 30% sodium hydroxide solution, and start to add 30.4 g of 37% formaldehyde solution dropwise when the temperature is raised to 90-95°C. After the addition, carry out the condensation reaction at reflux temperature for 6 hours, then adjust the pH to 10-11 with 30% sodium hydroxide solution, continue the reflux condensation for 1 hour, then add 1.0 g of urea to completely convert the residual formaldehyde, concentrate in vacuo, and cool to obtain 40% amino aromati...

Embodiment 3

[0049] In a four-necked flask equipped with a thermometer, a stirrer, a dropping funnel, and a reflux condenser, add 15 g of recovered phenolic residues, add 100 g of deionized water, and adjust the pH of the solution to 10-11 with 30% sodium hydroxide to make most of the residues Dissolve and remove the insoluble residue by filtration to obtain the sodium salt solution of the phenolic residue. Add 10 g of phenol to the solution, add 15 g (0.15 mol) of p-aminobenzenesulfonic acid, stir until completely dissolved, adjust the pH to 8.0-8.5 with 30% sodium hydroxide solution, and start adding 37 % formaldehyde aqueous solution 30.4g, after the dropwise addition, carry out condensation reaction at reflux temperature for 6 hours, then adjust pH 10-11 with 30% sodium hydroxide solution, continue reflux condensation for 1 hour, then add 1.0g urea to completely convert residual formaldehyde , concentrated in vacuo, and cooled to obtain a 40% aminoarene sulfonate high-efficiency water ...

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Abstract

The invention relates to a method for preparing an amino aromatic sulfonic acid concrete superplasticizer by utilizing synthesized aspirin waste liquor to partially or completely substitute phenol so as to be condensed with sulfanilic acid and formaldehyde. The preparation method comprises the following steps of: distilling the synthesized aspirin reaction waste liquor and recovering solvent acetic acid so as to obtain phenol residue; adding sulfanilic acid or a mixture of sulfanilic acid and phenol into a phenol residue sodium salt solution, and then stirring until the substances are completely dissolved; dropwise adding a 37% by mass of formaldehyde aqueous solution under the conditions that the pH value of a reaction liquid is 8.0-8.5 and the temperature is 90-95 DEG C; carrying out a condensation reaction for 3-6 hours at the reflux temperature, and carrying out reflux condensation for 1 hour at the pH of 10-11; adding a small amount of urea so that the content of free formaldehyde is less than 0.5%; and concentrating the reaction liquid in vacuum, and cooling to obtain a 40% by mass of amino aromatic sulfonic acid concrete superplasticizer liquid. The invention provides a comprehensive utilization method of synthesized aspirin waste liquor; and by using the method, the pollution generated in the aspirin production process is reduced, raw material cost is low, and application prospect is wide.

Description

technical field [0001] The invention relates to a method for preparing a high-efficiency water reducer for concrete, in particular to a method for preparing an aminoarylsulfonic acid high-efficiency water reducer by using synthetic aspirin waste liquid to partially or completely replace phenol, and belongs to the field of fine chemicals and chemical building materials. Background technique [0002] Amino aromatic sulfonic acid series high-efficiency water reducer for concrete is mainly formed by condensation of phenol, p-aminobenzenesulfonic acid and formaldehyde. Because of its simple production process, good dispersion of cement particles and high water reducing rate, the prepared concrete Due to the advantages of high strength, good durability, and small loss of slump over time, technology development and application research have attracted attention in recent years. With the rapid development of construction and chemical building materials industry, amino aromatic sulfon...

Claims

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Application Information

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IPC IPC(8): C08G14/073C04B24/22C04B103/30
Inventor 李建生何北菁吕英芳温景汀杨菲刘钰朱亚楠梁鑫莲
Owner TIANJIN VOCATIONAL INST
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