Continuous crystallization method of tetracycline

A tetracycline base and tetracycline technology, applied in organic chemistry, carboxylic acid amide separation/purification, etc., can solve the problems of material handling, storage, drying workload, operator physical damage, and labor intensity, etc., to achieve The effect of shortening the solution supersaturation time, high degree of filtration automation and improving the production environment

Inactive Publication Date: 2020-01-31
NINGXIA QIYUAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are following technical defects in this method: 1. the plate-and-frame filtration operation technique of tetracycline fermentation liquid is backward, the degree of automation is low, and the labor intensity of personnel is high; Large physical damage; ③Single-tank crystallization is used for crystallization, which takes a long time to operate, low equipment utilization rate, and low degree of automation; ④The process water consumption is large, the waste water discharge is large, and the treatment cost is high; ⑤The water content of tetracycline alkali is too high, and the material Handling, storage, and drying workload is heavy

Method used

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  • Continuous crystallization method of tetracycline
  • Continuous crystallization method of tetracycline

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Dilute tetracycline fermentation broth (potency 27825μ / ml) with water to titer 8000μ / ml, cool down to 10°C, acidify with oxalic acid, adjust pH value to 1.7, add purifiers (yellow blood salt, zinc sulfate, borax) after purification Ceramic ultra-membrane filtration, in the later stage of filtration, use pH 1.7 oxalic acid water for top washing, and tetracycline filtrate and oxalic acid top washing water are mixed evenly and then sampled for testing.

[0027] Take 4L of the above-mentioned tetracycline filtrate and oxalic acid top wash water mixture, with a potency of 6575μ / ml, mix the tetracycline filtrate and ammonia water in the delivery pipeline through a peristaltic pump (control the flow rate ratio of filtrate and ammonia water at 50:1), and then continue to flow to In the 2L reaction flask, the crystallization temperature was controlled at 5°C, and the pH value was at 4.5. After feeding for 20 minutes and the volume of the mixed solution reaches 70-80% of the volu...

Embodiment 2

[0029] Dilute tetracycline fermentation broth (potency 28017μ / ml) with water to titer 8000μ / ml, cool to 10°C, acidify with oxalic acid, adjust pH value to 1.6, add purifiers (yellow blood salt, zinc sulfate, borax) after purification Ceramic ultra-membrane filtration, in the later stage of filtration, oxalic acid water with pH 1.8 is used to circulate the top wash, and the tetracycline filtrate and oxalic acid top wash water are evenly mixed and then sampled for testing.

[0030] Take 4L of the above-mentioned tetracycline filtrate and oxalic acid top washing water mixture, with a potency of 6240μ / ml, mix the tetracycline filtrate and ammonia water in the delivery pipeline through a peristaltic pump (control the flow rate ratio of filtrate and ammonia water to 30:1), and then continue to flow to In a 2L reaction flask, control the crystallization temperature at 5°C and the pH value at 5.0. When the feeding time is 40min, when the volume of the mixed solution reaches 70-80% of ...

Embodiment 3

[0032] Dilute tetracycline fermentation broth (potency 31076μ / ml) with water to titer 9000μ / ml, cool down to 10°C, acidify with oxalic acid, adjust pH value to 1.8, add purifiers (yellow blood salt, zinc sulfate, borax) after purification Ceramic ultra-membrane filtration, in the later stage of filtration, oxalic acid water with pH 1.9 is used for top washing, and the tetracycline filtrate and oxalic acid top washing water are mixed evenly and then sampled for testing.

[0033] Take 4L of the above-mentioned tetracycline filtrate and oxalic acid top washing water mixture, the potency is 8285μ / ml, mix the tetracycline filtrate and ammonia water in the delivery pipeline through a peristaltic pump (control the flow rate ratio of filtrate and ammonia water to 40:1), and then continue to flow to In the 2L reaction flask, the crystallization temperature was controlled at 7°C, and the pH value was 4.6. When the feeding time is 30 minutes and the volume of the mixed solution reaches 7...

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Abstract

The invention relates to a continuous crystallization method of tetracycline. The method comprises the following steps of: preparing raw materials; the invention discloses a continuous crystallizationmethod of tetracycline. The method is characterized by comprising the following process steps: diluting tetracycline fermentation liquor, cooling, acidifying with oxalic acid, purifying, and filtering by using a ceramic ultrafiltration film; then directly mixing the tetracycline filtrate and ammonia water in a conveying pipeline, and continuously feeding the mixture into a reaction container forcrystallization; and when feeding is carried out for 20-40 minutes and the volume of the mixed material liquid reaches 70-80% of the volume of the reaction device, transferring the material liquid into a buffer device for continuous crystallization under the condition of continuous feeding, and after continuous crystallization of the tetracycline is completed, carrying out suction filtration and drying to obtain the tetracycline. The continuous crystallization of the tetracycline is realized, the crystallization efficiency and the product yield are greatly improved, the quality of the producedproduct is stable, the production environment is greatly improved, the production cost is reduced, and the method is an energy-saving and emission-reducing tetracycline crystallization method.

Description

technical field [0001] The invention belongs to the technical field of biology and new medicine, in particular to a continuous crystallization method of tetracycline base. Background technique [0002] Tetracycline (erythromycin, Er) is a class of tetracyclic antibiotics, which have a good inhibitory effect on Gram-positive bacteria, negative bacteria, rickettsia, viral viruses, spirochetes and even protozoa, and have a good inhibitory effect on Mycobacterium tuberculosis , Proteus, etc. are invalid. Its mechanism of action is that after binding to the 30S subunit of the ribosome, it can prevent aminoacyl tRNA from binding to the ribosome. [0003] In the prior art, the crystallization process of the tetracycline fermented liquid is as follows: after the tetracycline fermented liquid fermented and produced with Streptomyces aureus is cooled, acidified, plate and frame press filter, acid water top washing, the tetracycline filtrate (tetracycline filtrate Potency control 800...

Claims

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Application Information

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IPC IPC(8): C07C231/24C07C237/26
CPCC07C231/24C07C2603/46
Inventor 孙瑞君王东东王良张志
Owner NINGXIA QIYUAN PHARMA
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