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
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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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