Method for extracting oxytetracycline from oxytetracycline mother liquor

A technology of oxytetracycline mother and oxytetracycline, which is applied in the field of oxytetracycline production, can solve the problems of large amount of waste water, large amount of waste water, environmental pollution, etc., reduce difficulty and cost, improve adsorption effect, and have good adsorption selectivity Effect

Inactive Publication Date: 2015-11-18
河北健民淀粉糖业有限公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0002] At present, the technology of extracting oxytetracycline from the mother liquor of oxytetracycline production is immature. In the mother liquor of oxytetracycline, the salt content is high (ammonium oxalate 1.0-1.6%) and the ammonia nitrogen content is high, and the mother liquor of oxytetracycline also contains high Oxytetracycline with a concentration of about 1000-1200u / ml has a strong killing effect on microorganisms and cannot be biochemically treated, and the amount of wastewater produced by oxytetracycline manufacturers is large (usually the volume of wastewater is 2.5-4 times the volume of fermentation broth) , consumes a lot of water resources, produces a lot of waste water, and seriously pollutes the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Oxytetracycline mother liquor is added acid to adjust pH to 2.0, filters to obtain oxytetracycline clarification mother liquor, gets oxytetracycline clarification mother liquor 2000ml, and oxytetracycline concentration is 1016u / ml, takes strong polar macroporous adsorption resin (in the form of Lanxiao LXT-081 resin is an example, LXT-081 resin is a macroporous styrene-based adsorption resin) 60ml column packing, followed by 4% sodium hydroxide, purified water, 4% hydrochloric acid solution and washed to neutrality, and oxytetracycline The clarified mother liquor passes through the macroporous adsorption resin, the adsorption temperature is normal temperature, the flow rate is 10bv / h, and the concentration of the adsorbed oxytetracycline is 278u / ml. The recovery rate is 72.6%. h desorption, and then post-treatment to obtain oxytetracycline and recovery of ethanol, the desorption rate is 99.21%. The total recovery rate of oxytetracycline was 72%.

Embodiment 2

[0021] Get oxytetracycline mother liquor and adjust pH to 4.8, filter, obtain oxytetracycline clarification mother liquor, get oxytetracycline clarification mother liquor 2000ml, oxytetracycline concentration is 1200u / ml, get strong polar macroporous adsorption resin (take Lan Xiao LXT- 081 resin as an example, LXT-081 resin is a macroporous styrene-based adsorption resin,) 60ml column, followed by 4% sodium hydroxide, purified water, 4% hydrochloric acid solution and washed to neutral, clarified oxytetracycline The mother liquor passes through the macroporous adsorption resin, the adsorption temperature is normal temperature, the flow rate is 6bv / h, the concentration of oxytetracycline in the adsorbed water is 322u / ml, and the recovery rate is 68.3%. attached, and then post-treatment to obtain oxytetracycline and recovery of ethanol. The desorption rate was 98.8%. The total recovery rate of oxytetracycline was 67.5%.

Embodiment 3

[0023] Get oxytetracycline to refine mother liquor and adjust pH to 8.0, filter to obtain oxytetracycline clarification mother liquor, get oxytetracycline clarification mother liquor 2000ml, oxytetracycline concentration is 1200u / ml, get strong polar macroporous adsorption resin (using Lanxiao LXT -081 resin as an example, LXT-081 resin is a macroporous styrene-based adsorption resin,) 60ml column, followed by 4% sodium hydroxide, purified water, 4% hydrochloric acid solution and washed to neutral, oxytetracycline The clarified mother liquor passes through the macroporous adsorption resin, the adsorption temperature is normal temperature, the flow rate is 3bv / h, the concentration of oxytetracycline is 374u / ml, and the recovery rate is 63.17%. After the adsorption is saturated, use 95% ethanol at a temperature of 10°C and the flow rate is 5BV / h desorption, and then post-treatment to obtain oxytetracycline and reclaim ethanol. The desorption rate was 96.3%. Total yield of oxyt...

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Abstract

The invention discloses a method for extracting oxytetracycline from oxytetracycline mother liquor. The method comprises the following steps: step (a) preparing an oxytetracycline mother liquor, adjusting the pH value of the oxytetracycline mother liquor to 2-8, and filtering the oxytetracycline mother liquor to obtain a clear oxytetracycline mother liquor; (b) resin absorption: making the clear mother liquor obtained in the step (a) go through resin so as to absorb oxytetracycline in the clear mother liquor by the resin; (c) elution and separation: taking ethanol or methanol as the eluent, and eluting oxytetracycline, which is absorbed by the resin in the step (b), by the eluent to obtain a desorption solution; (d) oxytetracycline production: subjecting the desorption solution obtained in the step (c) to vacuum distillation so as to separate and recycle the organic solvent and obtain oxytetracycline. The provided method can reduce the resource wastes and generate high economic benefits. In the other aspect, the wastewater treatment becomes easier and the treatment cost is reduced.

Description

technical field [0001] The invention relates to the technical field of oxytetracycline production. Background technique [0002] At present, the technology of extracting oxytetracycline from the mother liquor of oxytetracycline production is immature. In the mother liquor of oxytetracycline, the salt content is high (ammonium oxalate 1.0-1.6%) and the ammonia nitrogen content is high, and the mother liquor of oxytetracycline also contains high Oxytetracycline with a concentration of about 1000-1200u / ml has a strong killing effect on microorganisms and cannot be biochemically treated, and the amount of wastewater produced by oxytetracycline manufacturers is large (usually the volume of wastewater is 2.5-4 times the volume of fermentation broth) , consumes a lot of water resources, produces a lot of waste water, and seriously pollutes the environment. Contents of the invention [0003] The technical problem to be solved in the present invention is to provide a method for ex...

Claims

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Application Information

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IPC IPC(8): C07C237/26C07C231/24
Inventor 纪俊荣田彩霞王冀民梁伟明
Owner 河北健民淀粉糖业有限公司
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