Method for recycling oxytetracycline hydrochloride from oxytetracycline hydrochloride crystallization mother liquid

A technology of oxytetracycline hydrochloride and crystallization mother liquor, applied in the separation/purification of carboxylic acid amide, organic chemistry, etc., can solve the problems of difficult biodegradation methods, large solvents, and difficult handling, and achieve high tolerance and high recovery rate , the effect of easy operation

Active Publication Date: 2017-08-04
扬州联博药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The waste liquid produced in the production of oxytetracycline hydrochloride generally has a large amount of solvent (generally, the amount of waste liquid is more than 5 times that of oxytetracycline hydrochloride production), and the high acidity and antibiotic components make it difficult to carry out biodegradation methods. industrial wastewater that is difficult to treat

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] 1000L oxytetracycline hydrochloride crystallization mother liquor, pH=0.68, add 100L of 2M ammonia / methanol solution, pH=2.01, filter with filter cloth, cool to 20°C, press into ultrafiltration system, operating pressure 0.3MPa, get 900L without Methanol solution of oxytetracycline and 180L concentrate. The pH of the concentrated solution was adjusted with 2M ammonia / methanol solution, and 9.3 kg of oxytetracycline was obtained by crystallization. After crystallization, 200 L of concentrated liquid mother liquor was obtained, which was used as alkaline solution to neutralize the oxytetracycline crystallization mother liquor for recycling treatment. The recovery rate of oxytetracycline was 93%. Add the recovered oxytetracycline into 45L of anhydrous methanol, add 0.8kg of calcium chloride to aid dissolution, filter, add 3.6L of 30% methanol hydrochloride, and crystallize to obtain 9.71kg of recovered oxytetracycline hydrochloride with a purity of 95.9%.

Embodiment 2

[0023] Add 500L oxytetracycline hydrochloride crystallization mother liquor, add 500L concentrated liquid mother liquor, add 2M ammonia / methanol solution, pH=2.01, filter with filter cloth, cool to 20°C, press into ultrafiltration system, operating pressure 0.28MPa, get 960L Oxytetracycline in methanol and 100L concentrate. The pH of the concentrated solution was adjusted with 2M ammonia / methanol solution, and 4.8 kg of oxytetracycline was obtained by crystallization. After crystallization, 110 L of concentrated liquid mother liquor was obtained, which was used as alkaline solution to neutralize the oxytetracycline crystallization mother liquor for recycling treatment. The recovery rate of oxytetracycline was 96%. Add the recovered oxytetracycline into 24L of anhydrous methanol, add 0.4kg of calcium chloride to aid dissolution, filter, add 1.8L of 30% methanol hydrochloride, and crystallize to obtain 4.91kg of recovered oxytetracycline hydrochloride with a purity of 97.2%.

Embodiment 3

[0025] Add 500L oxytetracycline hydrochloride crystallization mother liquor, add 500L concentrated liquid mother liquor, add 5% sodium hydroxide methanol solution, pH=2.00, filter with filter cloth, cool to 20°C, press into ultrafiltration system, operating pressure 0.30MPa, get 1020L methanol without oxytetracycline and 135L concentrate. Use 5% sodium hydroxide methanol solution to adjust the pH of the concentrate, and crystallize to obtain 4.7 kg of oxytetracycline. After crystallization, 150 L of concentrate mother liquor is obtained, which is used as lye to neutralize the mother liquor of oxytetracycline crystallization for recycling treatment. The recovery rate of oxytetracycline was 94%. Add the recovered oxytetracycline into 24L of anhydrous methanol, add 0.4kg of calcium chloride to aid dissolution, filter, add 1.8L of 30% methanol hydrochloride, and crystallize to obtain 4.76kg of recovered oxytetracycline hydrochloride with a purity of 96.5%.

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Abstract

The invention discloses a method for recycling oxytetracycline hydrochloride from oxytetracycline hydrochloride crystallization mother liquid. The method comprises the following steps: (1) adjusting the pH value of oxytetracycline hydrochloride mother liquid, and filtering to remove insoluble impurities; (2) separating treated filtrate by virtue of an ultrafiltration system so as to obtain a concentrated solution rich in oxytetracycline hydrochloride and an alcohol solution containing a small amount of calcium salt, and recycling methanol from the alcohol solution; (3) carrying out alkalization crystallization on the concentrated solution obtained through ultrafiltration, adding an alkalization reagent during alkalization so as to adjust the pH value, and recycling oxytetracycline, wherein the recycling rate of oxytetracycline reaches 93%-96%; and (4) adding recycled oxytetracycline into absolute methanol which is 5 times of volume dose of oxytetracycline, adding a small amount of calcium chloride to aid dissolving, filtering, adding hydrochloric acid methanol, and crystallizing, so as to obtain oxytetracycline hydrochloride. According to the method, inorganic salt, namely calcium salt, is filtered and separated by virtue of a membrane, the concentrated solution is subjected to alkalization crystallization to generate oxytetracycline, oxytetracycline is refined by virtue of hydrochloric acid ethanol so as to generate oxytetracycline hydrochloride, and the content of obtained oxytetracycline hydrochloride reaches 96%.

Description

technical field [0001] The invention belongs to the production technical field of oxytetracycline hydrochloride, and in particular relates to a method for recovering oxytetracycline hydrochloride from oxytetracycline hydrochloride crystallization mother liquor by a membrane separation method. Background technique [0002] Oxytetracycline hydrochloride crystallization mother liquor is a kind of highly acidic industrial waste liquid, the main components are solvent methanol and a small amount of water, in which the content of organic matter such as oxytetracycline is 1-3%, and the content of inorganic ions such as calcium ion and chloride ion Around 4%. The waste liquid produced in the production of oxytetracycline hydrochloride generally has a large amount of solvent (generally, the amount of waste liquid is more than 5 times that of oxytetracycline hydrochloride production), and the high acidity and antibiotic components make it difficult to carry out biodegradation methods....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/24C07C237/26
Inventor 苏令陆波王天池
Owner 扬州联博药业有限公司
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