Method for preparing refined tobias acid from tobias acid wastewater

A technology of tunic acid and waste water, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of long production cycle, high investment, and huge equipment, so as to save time, reduce ammonia nitrogen content, and reduce The effect of processing difficulty

Active Publication Date: 2013-09-11
山西翔宇化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the disadvantages of huge equipm

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Concentrated hydrochloric acid was added to the back-extraction of Tuo's acid, the pH was adjusted to 1.0, and centrifugal filtration was performed to obtain the back-extraction of Tuo's acid. Add 100g of tunic acid stripping material to 500mL of water, raise the temperature to 75°C and add 125mL of sodium hydroxide aqueous solution (concentration of 10% by weight), the pH of the solution is 2.5, keep the temperature at 80~85°C for 5 minutes, carry out hot filtration, The insoluble residue was filtered off. Cool the mother liquor at room temperature to 30°C, add 105mL hydrochloric acid (10% by weight concentration) within half an hour under vigorous stirring to adjust the pH to 1.5, perform centrifugal filtration, beat the filter cake with 500mL ethanol, filter, and dry the filter cake The purity of the dried vested finished product tunic acid is 97.2%, and ethanol can continue to be used mechanically.

Embodiment 2

[0030] Concentrated hydrochloric acid was added to the back-extraction of Tuo's acid, the pH was adjusted to 1.0, and centrifugal filtration was performed to obtain the back-extraction of Tuo's acid. Add 100g of tunic acid stripping material to 500mL of water, raise the temperature to 60°C and add 125mL of potassium hydroxide aqueous solution (concentration of 12% by weight), the pH of the solution is 2.5, keep the temperature at 80~85°C for 10 minutes, carry out hot filtration, The insoluble residue was filtered off. Cool the mother liquor at room temperature to 30°C, add 105mL of hydrochloric acid (10% by weight) within half an hour under vigorous stirring to adjust the pH to 1.5, perform centrifugal filtration, beat the filter cake with 700mL of ethanol, filter, and dry the filter cake The purity of the dried vested finished product tunic acid is 98.4%, and ethanol can continue to be used mechanically.

Embodiment 3

[0032] Concentrated sulfuric acid was added to the back-extraction of Tuo's acid to adjust the pH to 1.0, and centrifugal filtration was performed to obtain the back-extraction of Tuo's acid. Add 100g of tunic acid stripping material to 400mL of water, raise the temperature to 90°C and add 125mL of sodium hydroxide aqueous solution (concentration of 15% by weight), the pH of the solution is 2.5, keep the temperature at 80~85°C for 8 minutes, carry out hot filtration, The insoluble residue was filtered off. Cool the mother liquor at room temperature to 30°C, add 50mL of dilute sulfuric acid (10% by weight) within half an hour under vigorous stirring to adjust the pH to 1.5, perform centrifugal filtration, beat the filter cake with 600mL of ethanol, filter, and filter the cake The finished product tunic acid obtained by drying has a purity of 97.8%, and ethanol can continue to be used mechanically.

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Abstract

The invention relates to a production method of refined tobias acid from a tobias acid stripping solution after performing extraction-stripping in tobias acid wastewater. The invention aims at providing a method for preparing the refined tobias acid from the tobias acid wastewater, which can reduce consumption of energy and materials and also reduces the content of ammonia nitrogen and the content of strong cancerogenic substance, namely 2-naphthylamine in the wastewater. The adopted technical scheme is as follows: the method comprises the following steps of: performing acidolysis and centrifugal separation on the striping solution obtained by performing extraction-stripping on the wastewater for producing the tobias acid, and abandoning filtrate to obtain a tobias acid stripping material; heating the tobias acid stripping material, performing alkali dissolution, and then performing hot filtration to obtain a stripping material alkaline solution; performing cooling, crystallization, secondary acidolysis and centrifugal filtration on the stripping material alkaline solution to obtain a tobias acid wet product; and beating and washing the tobias acid wet product with ethanol, and performing centrifugal filtration and drying to obtain the tobias acid with the purity of not less than 97.0%. The production method disclosed by the invention can be widely applied in the technical field of preparation of the refined tobias acid from the tobias acid wastewater.

Description

technical field [0001] The invention relates to a method for refining and utilizing the waste pollutants in the production of torezic acid, specifically, after extracting and back-extracting from torezic acid waste water, refining torezic acid from the back-extraction liquid of torezic acid method. Background technique [0002] Tuccinic acid is an azo dye intermediate, mainly used in the manufacture of J acid and Lithol red R and other dye products. The chemical name is: 2-amino-1-naphthalenesulfonic acid. At present, the production method of Tuo's acid mainly is, 2-naphthol is obtained 2-naphthol-1 sulfonic acid through chlorosulfonic acid sulfonation; After alkali neutralization, obtain 2-naphthol-1 sulfonic acid sodium, then In the presence of acidic ammonium sulfite, feed liquid ammonia in the autoclave for ammoniation reaction, and convert it into 2-amino-1-naphthalenesulfonic acid. After acidification, crystallization is precipitated, and tunic acid is obtained by f...

Claims

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Application Information

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IPC IPC(8): C07C309/47C07C303/44
Inventor 刘云龙吴永廷张兴会
Owner 山西翔宇化工有限公司
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