Production method of extracting active ingredient from wastewater of producing tobias acid

An active ingredient, the technology of torezic acid, which is applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problems of product quality decline and the color deepening of torrentic acid products, so as to achieve good quality and less environmental pollution , the effect of high yield

Inactive Publication Date: 2011-09-07
TIANJIN NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to solve the problem that the above-mentioned simple reuse of the stripping solution causes the color of the Tobacic acid product to deepen and the quality of the product to decline, and to provide a preparation method for extracting active ingredients from the wastewater producing Tobacic acid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1000 ml of back-extraction solution was cooled to 0° C., kept at a temperature of 24 hours, and 105 grams of Glauber’s salt were filtered off to obtain 900 ml of denitrification solution. The denitration solution was concentrated under reduced pressure and vacuum in a distillation bottle, and 450 ml of water was distilled off. Room temperature was naturally cooled to 22°C. Filter to obtain filter cake 150 grams, water content 20%. After the filter cake is mixed with ammonia, it is transferred to a 1000 ml autoclave for ammoniation, the temperature is raised to 160°C, and the temperature is kept for 8 hours, and the temperature is lowered to 100°C after the ammonia is discharged. The ammoniated solution was transferred to a 1000 ml three-necked flask, and acidified with 1:1 hydrochloric acid at 75°C-80°C until pH=1-2. After filtering and washing, the pale yellow fine granular tunic acid crystals were obtained, and after drying, 72 g of the product was obtained, with a ...

Embodiment 2

[0023] Strip 1000 ml, cool to -10°C, keep warm for 12 hours, and filter out 120 grams of Glauber's salt. The denitrification mother liquor was concentrated under reduced pressure and vacuum in a distillation flask, and 500 ml of water was distilled off. Room temperature was naturally cooled to 25°C. Filter to obtain filter cake 157 grams, water content 20%. After the filter cake is mixed with ammonia, it is transferred to a 1000 ml autoclave for ammoniation, the temperature is raised to 160°C, and the temperature is kept for 8 hours, and the temperature is lowered to 100°C after the ammonia is discharged. The ammoniated solution was transferred to a 1000 ml three-neck flask, and acidified with 1:1 hydrochloric acid at 80°C until pH = 1-2. Filtration and washing resulted in pale pink fine granule tunic acid crystals, and after drying, 75 g of the product was obtained with a purity of 99.3% (as determined by HPLC).

Embodiment 3

[0025] Strip 1000 milliliters, cool to -5°C, keep warm for 24 hours, filter out 110 grams of Glauber's salt. The denitration mother liquor was concentrated under reduced pressure and vacuum in a distillation flask, and 450 ml of water was distilled off. Room temperature was naturally cooled to 20°C. Filter to obtain filter cake 155 grams, water content 21%. After the filter cake is mixed with ammonia, it is transferred to a 1000 ml autoclave for ammoniation, the temperature is raised to 160°C, and the temperature is kept for 8 hours, and the temperature is lowered to 100°C after the ammonia is discharged. The ammoniated solution was transferred to a 1000 ml three-neck flask, and acidified with 1:1 hydrochloric acid at 80°C until pH=2. Filtration and washing resulted in pale yellow fine granule tunic acid crystals. After drying, 70 g of the product was obtained with a purity of 99.5% (as determined by HPLC). Example 4 Comparative Example

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Abstract

The present invention discloses a method for extracting effective component from the production waste water of Tobias acid to produce Tobias acid further, which comprises processing extraction and back extraction on the waste water of Tobias acid production, freezing and desalting strip liquor to obtain denitration liquid, evaporating, concentrating, freezing and crystallizing denitration liquid, separating to obtain mixture salt, using ammoniation and acid out processes to obtain Tobias acid with purity higher than 99.0%. The inventive preparation method has simple and reliable process, high yield, and non environment pollution, which eliminates foreigner material accumulation caused by simply recovering strip liquor to avoid affecting product quality. Each cubic meter of strip liquor can produce 60-70kg Tobias acid which purity is higher than 99%, to reduce cost, improve yield, and support simple and reliable method for further advanced treatment of waste water.

Description

technical field [0001] The invention belongs to the technical field of production of chemical intermediates, and relates to a technical method for recycling waste pollutants in the production of tunic acid. More specifically, it is a preparation method for extracting active ingredients from waste water producing tunic acid. 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 is mainly to obtain 2-naphthol-1-sulfonic acid by sulfonating 2-naphthol with chlorosulfonic acid; , and then in the presence of acidic ammonium sulfite, feed liquid ammonia in the autoclave for ammoniation reaction, and convert it into 2-amino-1-naphthalenesulfonate sodium; then acidify, precipitate crystals, and filter to obtain Tuo’s acid. A large amount of wastewater will be discharged in the ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C309/47C07C303/44
Inventor 王宝丰
Owner TIANJIN NORMAL UNIVERSITY
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