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Method for reclaiming oxalic acid from terramycin purification liquid

A technology for oxytetracycline and purification liquid, which is applied in chemical instruments and methods, separation/purification of carboxylic acid compounds, organic chemistry, etc., can solve problems such as intractability, and achieve low cost, reduced treatment difficulty, and simple and easy methods. Effect

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

AI Technical Summary

Problems solved by technology

[0003] The average concentration of oxalic acid in the oxytetracycline mother liquor is about 9300mg / L, accounting for about 30% of the total COD of the mother liquor, and the mother liquor contains a high concentration of NH 3 -N, intractable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Get oxalic acid concentration and be 9000mg / L, oxytetracycline concentration be 14000mg / L, 500ml of oxytetracycline purification solution of pH=1.8, precision filter; , D301 type is a styrene skeleton) 10ml column, after being treated with dilute hydrochloric acid and dilute sodium hydroxide solution to form OH type, the above-mentioned oxytetracycline purification solution is adsorbed on the column, the adsorption temperature is 5 °C, and the flow rate is 6BV / h. The concentration of oxalic acid in the adsorbed water was 576mg / L, and the recovery rate was 93.6%. After adsorption saturation, 0.85% ammonia water was used for desorption at a temperature of 25° C. and a flow rate of 2 BV / h to obtain an ammonium oxalate solution with a desorption rate of 95.3%.

[0015] Adsorb the effluent to enter the subsequent process, add ammonia water to adjust the pH to 4.7-4.9 isoelectric point of oxytetracycline, precipitate oxytetracycline crystals, filter to obtain oxytetracycline ...

Embodiment 2

[0017] Get oxalic acid concentration and be 9000mg / L, oxytetracycline concentration be 14000mg / L, 500ml of oxytetracycline purification solution of pH=1.8, precision filter; For example, the D315 type is an acrylic acid skeleton) 10ml column, treated with dilute hydrochloric acid and dilute sodium hydroxide solution to form OH type, then put the above-mentioned oxytetracycline purification solution on the column for adsorption, the adsorption temperature is 25°C, and the flow rate is 10BV / h , the concentration of oxalic acid in the adsorbed water was 972 mg / L, and the recovery rate was 89.2%. After adsorption saturation, 1.5% ammonia water was used for desorption at a temperature of 35° C. and a flow rate of 3 BV / h to obtain an ammonium oxalate solution with a desorption rate of 96.7%.

[0018] Adsorb the effluent to enter the subsequent process, add ammonia water to adjust the pH to 4.7-4.9 isoelectric point of oxytetracycline, precipitate oxytetracycline crystals, filter to ...

Embodiment 3

[0020] Get oxalic acid concentration and be 9000mg / L, oxytetracycline concentration be 14000mg / L, 500ml of oxytetracycline purification solution of pH=1.8, precision filter; , D382 type is a styrene skeleton) 10ml column, after being treated with dilute hydrochloric acid and dilute sodium hydroxide solution to form OH type, the above-mentioned oxytetracycline purification solution is adsorbed on the column, the adsorption temperature is 35°C, and the flow rate is 15BV / h. The concentration of oxalic acid in the adsorbed water was 990mg / L, and the recovery rate was 89.0%. After saturated adsorption, desorb with 3.5% ammonia water at a temperature of 50°C and a flow rate of 4BV / h to obtain an ammonium oxalate solution, and directly obtain ammonium oxalate crystals after cooling, with a desorption rate of 98.2%.

[0021] Adsorb the effluent to enter the subsequent process, add ammonia water to adjust the pH to 4.7-4.9 isoelectric point of oxytetracycline, precipitate oxytetracycli...

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PUM

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Abstract

The invention relates to a method of recovering oxalic acid from supercidin cleaning liquor. It comprises following steps: filtering supercidin cleaning liquor and getting clarified solution, feeding clarified solution to absorption column filled with weak basic ion exchange resin which is treated with normal method, the oxalic acid is adsorbed, the liquor is discharged to subsequent process: adding ammonial solution to adjust supercidin isoelectric point for separation by crystallization, ading ammonial solution to said ion exchange resin column to remove oxalic acid and getting ammonium oxalate, recovering oxalic acid. The invention is characterized by high oxalic acid recovery rate of 89- 93.6%, reduced ammonia solution consumption by 80%, increased supercidin recovery rate of 95%, simple process, reusable resin and low cost.

Description

technical field [0001] The present invention relates to the production method of oxytetracycline, specifically, relate to the method for reclaiming oxalic acid from the purification solution of oxytetracycline. Background technique [0002] In the existing oxytetracycline production process, in order to increase the yield of oxytetracycline, remove impurities and improve filtration conditions, a certain amount of oxalic acid needs to be added to the fermentation broth, and its pH is adjusted to 1.75-1.85, and then decolorized by resin Obtain oxytetracycline purification solution, then adjust it to the isoelectric point of oxytetracycline with pH 4.7-4.9 with ammonia water, so that oxytetracycline crystallizes out, and obtain crude oxytetracycline and mother liquor after solid-liquid separation in centrifuge, and remove waste water from mother liquor deal with. [0003] The average concentration of oxalic acid in the oxytetracycline mother liquor is about 9300mg / L, accountin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C55/06C07C51/42C07C51/47C02F1/58C02F101/34
Inventor 赵玉明陈飞李琼林
Owner NANJING UNIV
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