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Method of recycling butanol through tetracycline hydrochloride crystallization mother liquor

A technology of tetracycline hydrochloride and crystallization mother liquor, applied in the separation/purification of hydroxyl compounds, organic chemistry and other directions, can solve the problems of high consumption of steam and condensed water, low recovery rate of butanol, serious air pollution, etc. The effect of reducing production cost and high yield

Active Publication Date: 2013-08-14
JIANGSU SAIDELI PHARMA MACHINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above-mentioned method for recovering butanol from the tetracycline hydrochloride crystallization mother liquor has the following 5 defects: (1) ammonia gas is discharged, which seriously pollutes the air. In the production process of tetracycline hydrochloride, ammonia water is used to adjust the pH value, excessive urea is used to react with tetracycline alkali, etc. process, resulting in the existence of ammonia substances in the mother liquor of tetracycline hydrochloride crystallization. When the mother liquor of tetracycline hydrochloride is distilled, ammonia gas will be generated, which will be discharged into the air and cause serious pollution; (2) the recovery rate of butanol is low in the distillation of the final discharge The raffinate contains butanol, whose content is about 1% (w / w); (3) High energy consumption As mentioned above, the azeotropic mixture of butanol and water has a process of repeated vaporization and condensation, resulting in steam and condensed water (4) The process is complicated as mentioned above, and the azeotropic mixture of butanol and water needs to be repeatedly static and stratified during the process; (5) The recovery cost is high, the recovery rate of butanol is low and the energy consumption high lead to high recycling costs

Method used

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Examples

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Effect test

Embodiment 1

[0021] A method for recovering butanol from tetracycline hydrochloride crystallization mother liquor, the steps are as follows:

[0022] (1) Mixing: Mix 45kg of tetracycline hydrochloride crystallization mother liquor with 500g of sulfuric acid with a mass concentration of 40% at room temperature;

[0023] (2) One-time distillation: take the mixed solution obtained in step (1) and add it to the distillation kettle for distillation. The temperature is raised to 118°C to stop. The fractions are collected and condensed during the temperature rise, and the remaining residual liquid in the distillation kettle is collected;

[0024] (3) Dehydration: take the fractions obtained in step (2) and use pervaporation organic membrane device or pervaporation inorganic membrane device for dehydration treatment at 80~95℃ to obtain butanol and butanol with water content less than or equal to 0.8% by mass. Permeate liquid containing butanol;

[0025] (4) Secondary distillation: Take the butanol-contain...

Embodiment 2

[0029] A method for recovering butanol from tetracycline hydrochloride crystallization mother liquor, the steps are as follows:

[0030] (1) Mixing: Mix 45kg of tetracycline hydrochloride crystallization mother liquor with 500g of sulfuric acid with a mass concentration of 60% at room temperature;

[0031] (2) One-time distillation: take the mixed solution obtained in step (1) and add it to the distillation kettle for distillation. The temperature is raised to 115°C to stop. During the heating period, fractions are collected and condensed, and the remaining residual liquid in the distillation kettle is collected;

[0032] (3) Dehydration: take the fractions obtained in step (2) and use pervaporation organic membrane device or pervaporation inorganic membrane device for dehydration treatment at 80~95℃ to obtain butanol and butanol with water content less than or equal to 0.8% by mass. Permeate liquid containing butanol;

[0033] (4) Secondary distillation: Take the butanol-containing p...

Embodiment 3

[0037] A method for recovering butanol from tetracycline hydrochloride crystallization mother liquor, the steps are as follows:

[0038] (1) Mixing: At room temperature, mix 55kg of tetracycline hydrochloride crystallization mother liquor with 500g of sulfuric acid with a mass concentration of 40%;

[0039] (2) One-time distillation: take the mixed solution obtained in step (1) and add it to the distillation kettle for distillation. The temperature is raised to 120°C to stop. The distillate is collected and condensed during the temperature rise, and the remaining residue in the distillation kettle is collected;

[0040] (3) Dehydration: take the fractions obtained in step (2) and use pervaporation organic membrane device or pervaporation inorganic membrane device for dehydration treatment at 80~95℃, respectively, the water content is less than or equal to 0.8% by body mass. Alcohol and penetrant containing butanol;

[0041] (4) Secondary distillation: Take the butanol-containing perme...

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Abstract

The invention relates to a method of recycling butanol through tetracycline hydrochloride crystallization mother liquor, and belongs to the technical field of pharmacy. The method comprises the following steps of: adding sulfuric acid in the tetracycline hydrochloride crystallization mother liquor at room temperature, and then, distilling the mother liquor to obtain a mixture of butanol and water, dewatering the mixture through an organic pervaporation membrane device or inorganic pervaporation membrane device to respectively obtain butanol and dialysate, utilizing the obtained butanol in the extraction process of tetracycline hydrochloride, mixing the obtained dialysate with the residual distillate of the distilling process, distilling to obtain an azeotropic mixture of butanol and water, mixing the obtained zeotropic mixture of butanol and water with the next batch of tetracycline hydrochloride crystallization mother liquor with sulfuric acid, continuing the treatment process, and treating the obtained secondary residual distillate in an environmental protection device. The method provided by the invention has the advantages of simple technique, convenience for operation, energy conservation, emission reduction, high yield and low cost.

Description

Technical field [0001] The invention relates to a method for recovering butanol from tetracycline hydrochloride crystallization mother liquor, and belongs to the technical field of pharmacy. Background technique [0002] Tetracycline hydrochloride, alias tetracycline hydrochloride, chemical name: 6-methyl-4-(dimethylamino)-3,6,10,12,12a-pentahydroxy-1,11-dioxo-1,4, 4a,5,5a,6,11,12a-octahydro-2-tetrabenzamide hydrochloride, molecular formula C 22 H 24 N 2 O 8 ·HCl. [0003] Tetracycline hydrochloride is a broad-spectrum antibiotic that has antibacterial effects on Gram-positive and Gram-negative bacteria, and against pneumococcus, hemolytic streptococcus, diphtheria, tetanus, anthracis, perfringens, influenza, etc. It has a strong effect on mycoplasma, chlamydia, rickettsia, spirochetes and amoeba, etc. Its antibacterial mechanism is mainly to prevent aminoacyl T-RNA from binding to the A site of the 30S subunit of the riboprotein. Preventing the growth of peptide chains hinders p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/12C07C29/76
Inventor 顾根生张庆武
Owner JIANGSU SAIDELI PHARMA MACHINE
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