Method for recovering terramycin from terramycin production wastewater.

A technology of oxytetracycline and oxytetracycline alkali, which is applied in the field of wastewater treatment of oxytetracycline production, can solve the problems of extraction agent loss, easily polluted flux, and high recovery cost, and achieve low cost, simple process, and low cost of use cheap effect

Inactive Publication Date: 2010-07-21
TONGJI UNIV
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, during extraction and recovery, the loss of extractant is serious, resulting in high recovery costs, while the membrane separation method is prone to fouling due to the high concentration of organic matter in the waste liquid, and the flux decays rapidly
Chinese invention patents 200710021381 and 200710021382 disclose two methods of using ion exchange resins to recover oxytetracycline from the mother liquor of oxytetracycline production. Although the ion exchange resin method has the advantages of simple process and good selective adsorption, the oxytetracycline wastewater It also contains a large amount of protein and polysaccharide organic matter. After long-term use, the efficiency will be reduced due to the saturation of the resin's functional groups, and the organic matter characteristics of the ion exchange resin itself will cause it to be oxidized and decomposed during repeated use. problems
In addition, the regeneration process of ion exchange resin is not complete, and the cost of using acid and alkali agents is high, which restricts the industrial application of ion exchange resin method in the recovery of oxytetracycline wastewater

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The oxytetracycline waste liquid is added with alkali to adjust the pH to 7, and the suspended particles in the water are removed after precision filtration with a precision filter to obtain the clarified waste liquid of oxytetracycline. Take 200 mL of the clarified waste liquid of oxytetracycline, and the concentration of oxytetracycline is 468mg / L; Get 13X type zeolite molecular sieve (with the 13X type molecular sieve produced by Shanghai Zeolite Molecular Sieve Co., Ltd.

[0016] Sieve as an example) 10ml column, the above-mentioned oxytetracycline clarified waste liquid flows through the adsorption column for adsorption, the adsorption temperature is 25°C, the flow rate is 2BV / h, the concentration of oxytetracycline in the adsorption water is 59.3mg / L, and the recovery rate is 87.3% . After adsorption saturation, use 0.5M ammonia solution to desorb at a temperature of 25°C and a flow rate of 1BV / h to obtain an oxytetracycline ammonium solution. The concentration of...

Embodiment 2

[0018] Add or subtract the oxytetracycline waste liquid to adjust the pH to 5, filter to obtain the oxytetracycline clarified waste liquid, take 200 mL of the oxytetracycline clarified waste liquid, and the concentration of oxytetracycline is 468 mg / L. Take 5A type zeolite molecular sieve (taking the 5A type molecular sieve produced by Shanghai Zeolite Molecular Sieve Co., Ltd. as an example) 10ml to pack into a column, and flow the above-mentioned oxytetracycline clarified waste liquid through the adsorption column for adsorption. The adsorption temperature is 10°C and the flow rate is 8BV / h. The concentration of oxytetracycline was 282 mg / L, and the recovery rate was 39.7%. After adsorption saturation, use 1M sodium hydroxide solution at a temperature of 25°C and a flow rate of 2BV / h for desorption to obtain an oxytetracycline alkali solution. The concentration of oxytetracycline is 1836mg / L, and the desorption rate is 98.7%. The impurity content in the desorption liquid is ...

Embodiment 3

[0020] Add or subtract the oxytetracycline waste liquid to adjust the pH to 9, filter to obtain the clarified waste liquid of oxytetracycline, take 200 mL of the clarified waste liquid of oxytetracycline, and the concentration of oxytetracycline is 56 mg / L; The 10X type molecular sieve produced by Molecular Sieve Co., Ltd. as an example) 10ml column, the above-mentioned oxytetracycline clarified waste liquid flows through the adsorption column for adsorption, the adsorption temperature is 20°C, the flow rate is 1BV / h, and the concentration of oxytetracycline in the adsorbed water is 14mg / L , the recovery rate was 75.0%. After adsorption saturation, use 1M ammonia solution to desorb at a temperature of 25°C and a flow rate of 1BV / h to obtain an oxytetracycline ammonium solution. The concentration of oxytetracycline is 800mg / L, and the desorption rate is 95.2%. The impurity content in the desorption liquid is lower than 5%. After the conventional wastewater treatment process, i...

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Abstract

The invention relates to a method for recovering terramycin from terramycin c wastewater, in particular to a method for treating terramycin wastewater. The method comprises the following steps: first adjusting the PH value of the terramycin production wastewater and clarifying the wastewater by filtration; loading the absorption column with a hydrophilic zeolite molecular sieve (one of the 3A, 4A, 5A, 10 X, 13 X or Y types of molecular sieves); running the clarified terramycin wastewater through the absorption column, with the velocity of the flow between 1 to 12 BV/h under the temperature of 5-100 DEG C, the terramycin is absorbed by the absorption column; then desorbing the solution by alkali solution (Ammonia, sodium hydroxide solution or sodium carbonate solution) of 0.1 to 2.0 M under the temperature of 10 to 100 DEG C with the velocity of the flow between 1 to 4 BV/h to get high-concentration terramycin alkali solution; after the crystallization treatment, the crystal oxytetracycline dihyclorate obtained can directly be used as drug product. The recycle rate of the terramycin is 40-90 percent. The method of the invention is easy to operate and the zeolite molecular sieve can be repeatedly used. The treatment cost of the invention is lower than the treatment cost of methods of the same type. The method of the invention can be widely applied to recover terramycin from terramycin production wastewater.

Description

technical field [0001] The invention relates to a treatment method for oxytetracycline production wastewater, in particular to a method for recovering low-concentration oxytetracycline from oxytetracycline production wastewater. Background technique [0002] At present, the concentration of oxytetracycline in the oxytetracycline production waste liquid is about 20-600mg / L. Because oxytetracycline is difficult to oxidize and biodegrade, and it has inhibitory properties on microorganisms in the wastewater biological treatment process, it is not conducive to pharmaceutical wastewater biochemical treatment. As a result, oxytetracycline wastewater needs to be diluted in large quantities before treatment. However, oxytetracycline has considerable recovery value. For the recovery of oxytetracycline in the waste liquid of oxytetracycline production, attempts have been made through extraction, membrane separation, ion exchange resin and other methods, but there are application probl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C02F9/04B01J20/34C07C237/36C07C237/42C02F1/66C02F1/28C02F101/34C02F101/38C02F103/36
Inventor 邓慧萍赵纯黎园胥红潘若平陈鑫
Owner TONGJI UNIV
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