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Method of recovering terramycin from terramycin production mother liquid

A technology of oxytetracycline and mother liquor, which is applied in the directions of organic chemistry, separation/purification of carboxylic acid amides, etc., to achieve the effects of easy treatment, low cost, and simple and easy method.

Inactive Publication Date: 2007-09-12
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no report on recovering oxytetracycline from the mother liquor of oxytetracycline production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Oxytetracycline refining mother liquor is added alkali to adjust pH to 5.4, filters, and obtains oxytetracycline clarification mother liquor, gets oxytetracycline clarification mother liquor 500ml, and oxytetracycline concentration is 526mg / l; The NKA-2 type produced by the University Chemical Plant is an example. NKA-2 is a styrene-diethylbenzene structure) 10ml column is packed, and is treated with 4% hydrochloric acid, acetone, 4% sodium hydroxide solution successively and washed to neutrality, The clarified mother liquor of oxytetracycline was passed through a macroporous adsorption resin column, the adsorption temperature was 10° C., the flow rate was 2 BV / h, the concentration of oxytetracycline was 211 mg / l, and the recovery rate was 59.9%. After the adsorption is saturated, use 95% ethanol to desorb at a temperature of 25°C and a flow rate of 4BV / h, then obtain oxytetracycline through rectification and recover ethanol, and the desorption rate is 97.5%. Through ex...

Embodiment 2

[0016] Get oxytetracycline refining mother liquor and add alkali to adjust pH to 9.0, filter to obtain oxytetracycline clarification mother liquor, get oxytetracycline clarification mother liquor 500ml, oxytetracycline concentration is 526mg / l; The NKA-2 type produced by the University Chemical Plant is an example. NKA-2 is a styrene-diethylbenzene structure) 10ml column is packed, and is treated with 4% hydrochloric acid, acetone, 4% sodium hydroxide solution successively and washed to neutrality, The clarified mother liquor of oxytetracycline was passed through a macroporous adsorption resin column, the adsorption temperature was 25° C., the flow rate was 8 BV / h, the concentration of oxytetracycline was 125 mg / l, and the recovery rate was 76.2%. After the adsorption is saturated, use 95% ethanol to desorb at a temperature of 60°C and a flow rate of 1 BV / h, then post-process to obtain oxytetracycline and recover ethanol, with a desorption rate of 98.8%. Through experiments, t...

Embodiment 3

[0018] Get oxytetracycline refining mother liquor and add alkali to adjust pH to 2.0, filter to obtain oxytetracycline clarification mother liquor, get oxytetracycline clarification mother liquor 500ml, oxytetracycline concentration is 526mg / l; The NKA-2 type produced by the University Chemical Plant is an example. NKA-2 is a styrene-diethylbenzene structure) 10ml column is packed, and is treated with 4% hydrochloric acid, acetone, 4% sodium hydroxide solution successively and washed to neutrality, The clarified mother liquor of oxytetracycline was passed through a macroporous adsorption resin column, the adsorption temperature was 10° C., the flow rate was 5 BV / h, the concentration of oxytetracycline was 125 mg / l, and the recovery rate was 68.0%. After the adsorption is saturated, use 95% ethanol to desorb at a temperature of 60°C and a flow rate of 1 BV / h, then post-process to obtain oxytetracycline and recover ethanol, with a desorption rate of 98.8%. Through experiments, t...

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PUM

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Abstract

This invention relates to a method for recovering terramycin from terramycin mother liquid, which adds acid or alkali to a terramycin mother liquid to adjust pH to 2-9 to be filtered and get the clarified mother liquid, and puts strong polarity large hole adsorption resin into an adsorption post to adsorb terramycin from the clarified mother liquid controlling the temperature at 10-15deg.C and flow rate at 2-16BV / h, takes ethanol, methanol or acetone organic solvent as the eluent and controls the temperature at 25-60deg.C and flow rate at 1-4BV / h to carry out desorption, then the desorption solution is distilled to separate out terramycin and recovers organic solvent.

Description

technical field [0001] The present invention relates to the production of oxytetracycline, specifically, it is the method for recovering oxytetracycline from the mother liquor of producing oxytetracycline with adsorption resin. Background technique [0002] The oxytetracycline production mother liquor contains about 0.05-0.08% oxytetracycline, and also contains relatively high concentrations of protein, polysaccharide compounds, oxalic acid, inorganic substances, etc., and the oxytetracycline in the mother liquor is recovered and treated, and then the wastewater On the one hand, it can reduce the waste of resources and obtain economic benefits, and on the other hand, it can also reduce the difficulty and cost of wastewater treatment. There is no report on the recovery of oxytetracycline from the mother liquor of oxytetracycline production. Contents of the invention [0003] The object of the present invention is to provide a kind of method that reclaims oxytetracycline fr...

Claims

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Application Information

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IPC IPC(8): C07C237/26C07C231/22
Inventor 赵玉明龚点图薛祯祯
Owner NANJING UNIV
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