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: 2015-04-29
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

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

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

[0023] (2) One-time distillation: take the mixed solution obtained in step (1) and add it to the still for distillation, raise the temperature to 118°C to stop, collect and condense fractions during the heating period, and collect the remaining residual liquid in the still;

[0024] (3) Dehydration: The fraction obtained in step (2) is dehydrated with a pervaporation organic membrane device or a pervaporation inorganic membrane device at 80-95°C to obtain butanol and butanol with a water content less than or equal to 0.8% by mass Permeate containing butanol;

[0025] (4) Secondary distillation: Take the permeate containing butanol obtained in step (3) and the remaining raffi...

Embodiment 2

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

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

[0031] (2) One-time distillation: take the mixed solution obtained in step (1) and add it to the still for distillation, raise the temperature to 115°C to stop, collect and condense fractions during the heating period, and collect the remaining residual liquid in the still;

[0032] (3) Dehydration: The fraction obtained in step (2) is dehydrated with a pervaporation organic membrane device or a pervaporation inorganic membrane device at 80-95°C to obtain butanol and butanol with a water content less than or equal to 0.8% by mass Permeate containing butanol;

[0033] (4) Secondary distillation: take the permeate containing butanol obtained in step (3) and the remaining raffinate ob...

Embodiment 3

[0037] A method for reclaiming butanol by 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% evenly;

[0039](2) Primary distillation: Take the mixed solution obtained in step (1) and add it to the still for distillation, heat up to 120°C to stop, collect and condense fractions during the heating period, and collect the remaining residual liquid in the still;

[0040] (3) Dehydration: take the fraction obtained in step (2) and use a pervaporation organic membrane device or a pervaporation inorganic membrane device to perform dehydration treatment at 80-95°C, and obtain butyl alcohol with a water content less than or equal to 0.8% by weight respectively. Alcohol and permeate containing butanol;

[0041] (4) Secondary distillation: take the permeate containing butanol obtained ...

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PUM

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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, which 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-tetracenecarboxamide hydrochloride, molecular formula C 22 h 24 N 2 o 8 • HCl. [0003] Tetracycline hydrochloride is a broad-spectrum antibiotic, which has antibacterial effects on both Gram-positive and negative bacteria. The effect is strong, and it also has inhibitory effect on mycoplasma, chlamydia, rickettsia, spirochete and amoeba. Preventing the growth of the peptide chain hinders the synthesis of proteins, and can cause changes in the permeability of bacterial cell membranes, thereby inhibiting DNA replication. Tetracycline hydrochloride is used for infections caused ...

Claims

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Application Information

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