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
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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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