Method for preparing tobias acid by effective components extracted from waste water of tobias acid production

A technology for the production of waste water and active ingredients, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems affecting the quality of tunic acid products, the increase of impurity content, and the accumulation of impurities in the stripping solution, etc.

Inactive Publication Date: 2008-08-27
WUXI HUASHENG ENVIRONMENT PROTECTION TECH
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  • Abstract
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Problems solved by technology

However, the main disadvantage of this method is that the harmful impurities in the stripping solution will be discharged together with the mother liquor of tunic acid, and after the subsequent extraction-stripping process, they will enter the stri...

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  • Method for preparing tobias acid by effective components extracted from waste water of tobias acid production
  • Method for preparing tobias acid by effective components extracted from waste water of tobias acid production

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Embodiment 1

[0027] 1000 milliliters of stripping solution was cooled to 0° C. and kept for 12 hours, then 105 grams of Glauber’s salt was filtered off to obtain 900 milliliters of denitrification solution, which was distilled in a retort to remove 450 milliliters of water. The room temperature was naturally cooled to 22° C., and filtered to obtain 150 grams of filter cake with a water content of 20%. After the filter cake is mixed with ammonia, it is transferred to a 1000ml autoclave for ammoniation, the temperature is raised to 160°C, and the temperature is kept for 8 hours. The ammonia is discharged and the temperature is lowered to 100°C. 1:1 hydrochloric acid acid analysis to PH=1~2. Filtration and washing resulted in fine granular tunic acid crystals. After drying, 72 g of the product was obtained with a purity of 99.21% (as determined by HPLC).

[0028] Implementation column 2:

[0029] Take 1000 ml of back-extraction solution, cool to ~2°C, keep warm for 3 hours, filter out 120 g...

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Abstract

The invention relates to a method for extracting effective component from the waste water of the mother liquor of tobias acid production to produce tobias acid, belonging to the waste pollutant resource utilization technique of environment protection field. The invention resolves the problems of prior art which simply refluxes strip liquor as impurity accumulation to affect product quality. The method comprises cooling strip liquor to -2DEG C and 20DEG C in a kettle with a jacket, keeping the temperature for 3-12h, filtering out mirabilite, concentrating the denitration liquid in a distiller, discharging steam, evaporating out 35-50% of water content, reducing temperature, precipitating at least 95% organic crystal at 35-50DEG C, centrifugally filtering to obtain hydroxyl sodium tobias acid and some wet product of sodium tobias acid, dissolving the wet product and processing ammonia complex, feeding into an ammoniation reactor for ammoniation, increasing temperature to 140-160DEG C, keeping temperature for 6-8h, discharging ammonia, reducing temperature to 100-110DEG C, transferring ammoniation liquid into am acid precipitation kettle, processing acid precipitation via hydrochloride (or dilute sulfuric acid) at 75-100DEG C until pH is 1-2, filtering and washing to obtain tobias acid particle crystals, centrifugally processing to obtain tobias acid wet product, and drying to obtain final product whose purity is higher than 97.00-99.00% (tested by HPLC).

Description

technical field [0001] The invention relates to a method of extracting effective components from the waste water of the production mother liquor of Tubic acid to prepare Tubic acid, which belongs to the recycling technology of waste pollutants in the field of environmental protection. Background technique [0002] The production of tunic acid discharges a large amount of wastewater, which has high COD, dark color, high salt content, and complex components. The technology of extraction treatment has been very mature. The essence of this technology is to remove almost all colored substances and most of the organic matter in wastewater And a part of the inorganic matter is extracted; then after back extraction, it is transferred to the back extraction liquid. Although the back-extraction liquid contains available toborate and hydroxytomolate, its color is darker and the impurity content is higher. However, in the prior art, the stripping liquid is disposed of without any treat...

Claims

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Application Information

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IPC IPC(8): C07C309/46C07C303/44
Inventor 周春华
Owner WUXI HUASHENG ENVIRONMENT PROTECTION TECH
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