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Method for improving sulfonation process of naphthalene-based water reducer

A naphthalene-based water reducer and sulfonation technology, which is applied in the field of improving the sulfonation process of naphthalene-based water reducers, can solve the problems of low sulfonation rate, waste of energy, and waste, so as to increase the degree of sulfonation and reduce production costs , the effect of reducing the content

Inactive Publication Date: 2012-10-24
JIANGSU NIGAO SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method has serious defects. During the sulfonation reaction of naphthalene-based water reducers, at a temperature of 160-165°C, the molar ratio of naphthalene to concentrated sulfuric acid is 1:1.3-1.45. After 2.5-4h of sulfonation, industrial naphthalene is Sulfonation into naphthalenesulfonic acid and water mainly composed of β-naphthalenesulfonic acid and supplemented by α-naphthalenesulfonic acid. Due to the reversibility of the reaction, water is formed in the reaction. The existence of water will affect the deviation of the chemical balance, so that The reaction balance shifts in the opposite direction, so that the sulfonation reaction cannot continue, resulting in a low sulfonation rate. At the same time, the free naphthalene without sulfonation after sulfonation of industrial naphthalene directly enters the condensation stage, and the final neutralization discharge is mixed into the water reducer , not only wasting energy, but also absorbing a small amount of water reducing agent, which affects the performance of the product. The most important thing is that free naphthalene itself has certain toxicity, which is not conducive to the protection of the environment.
To solve this problem, in the prior art, steam is passed into the material being sulfonated to blow out industrial naphthalene, but even so, it still needs to go through collection, separation and post-processing procedures, the process is complicated and the waste is serious

Method used

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  • Method for improving sulfonation process of naphthalene-based water reducer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Measure 1.2 tons of industrial naphthalene into the reactor, heat up to 120°C, start to add 1.3 tons of 98% concentrated sulfuric acid dropwise, and finish the dropwise addition in half an hour. Start the negative pressure device every 0.5h, control the pressure in the kettle to 0.07MP, and the extraction time is 8 minutes. At the same time, turn on the steam valve of the heat exchanger to melt the volatilized industrial naphthalene, ensure the smooth flow of gas in the whole extraction device, and extract the reaction kettle. The gas is treated with more than two alkali sprays in the spray tower, then enters the liquid alkali sealing tank for neutralization treatment, and is finally discharged. After the sulfonation is completed, the dry powder product is obtained by hydrolysis, condensation and neutralization, and the sulfonation rate is 95.50%.

Embodiment 2

[0015] Measure 1.2 tons of industrial naphthalene into the reactor, heat up to 120°C, start to add 1.3 tons of 98% concentrated sulfuric acid dropwise, and finish the dropwise addition in half an hour. Start the negative pressure device every 0.5 hours, control the pressure in the kettle to 0.08 MP, and the extraction time is 6 minutes. At the same time, start the steam valve of the heat exchanger to melt the volatilized industrial naphthalene, so as to ensure the smooth flow of gas in the entire extraction device. After the sulfonation is completed, the dry powder product is obtained by hydrolysis, condensation and neutralization, and the detected sulfonation rate is 96.20%.

Embodiment 3

[0017] Measure 1.2 tons of industrial naphthalene into the reactor, heat up to 120°C, start to add 1.3 tons of 98% concentrated sulfuric acid dropwise, and finish the dropwise addition in half an hour. Start the negative pressure device every 0.5 hours, control the pressure in the kettle to 0.09 MP, and the extraction time is 5 minutes. At the same time, start the steam valve of the heat exchanger to melt the volatilized industrial naphthalene, so as to ensure the smooth flow of gas in the entire extraction device. After the sulfonation is completed, the dry powder product is obtained by hydrolysis, condensation and neutralization, and the sulfonation rate is 96.50%.

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Abstract

The invention relates to a method for improving the sulfonation process of a naphthalene-based water reducer, characterized by cascading a heat exchanger and a vacuum-pumping device to the cover of a reaction vessel, sulfonating the naphthalene-based water reducer for 0.5-1h, then generating negative pressure by extracting the gas of the reaction vessel every 0.5 h to bring out the moisture generated by the reaction; simultaneously letting in steam to the air inlet of the heat exchanger while extracting to let the industrial naphthalene volatilized and crystallized in the extracting process melt and relux to the sulfonation system and circulate continuously to be sulfonated, after finishing the sulfonation reaction, conducting hydrolysis, condensation and neutralization to obtain a powder product. According to the invention, the content of the toxic raw material industrial naphthalene in the water reducer is reduced, the production cost is reduced, the pollution of the materials to the environment is eliminated, and the method is easy to operate, and the operation is convenient.

Description

technical field [0001] The invention relates to a naphthalene-based water-reducer used in concrete, in particular to a method for improving the sulfonation process of the naphthalene-based water-reducer. Background technique [0002] Due to the needs of industrial development, people have put forward higher and higher requirements for the performance of concrete, and a necessary condition for realizing high-performance concrete is the use of high-efficiency water reducing agent, which can not only improve construction conditions, but also increase the compressive strength of concrete , but also can enhance the performance of concrete such as frost resistance and impermeability, and is considered to be the fifth component necessary for concrete. At present, most of the high-efficiency water reducers used in China are naphthalene-based water reducers, accounting for more than 60% of the market. [0003] The production method of naphthalene-based water reducer is relatively ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C309/35C07C303/06C04B24/20C04B103/30
Inventor 王文军金卫民蒋长清钱超成立强吴益
Owner JIANGSU NIGAO SCI & TECH
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