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A dmf recycling process

A process and drug technology, applied in the field of DMF recovery process, can solve the problems of large equipment investment, complex process, large energy consumption, etc., and achieve the effects of reduced waste liquid discharge, simple process operation, and high resource utilization rate

Active Publication Date: 2015-11-18
TIANJIN PHARMA GROUP GENCOM PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional process usually uses rectification or extraction to remove the water and recover the solvent. However, the rectification process takes a long time to remove water and requires a rectification tower. The equipment investment is relatively large and the energy consumption is large. However, the extraction method needs to find a suitable Extractant, the process of recovering solvent is more complicated, another organic solvent is introduced, the cost of separating solvent and extractant is high, and the recovery rate of solvent is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add one part of toluene to four parts of dimethylformamide mother liquor, the drug intermediate, the volume of the added toluene is greater than or equal to the volume of the water separator, stir, heat up, the liquid temperature is 93°C, and there is a distillate, the liquid temperature is 99°C, and the air temperature is 80°C Generate total backflow and separate water at any time. The reflux timer is over for 4 hours, the liquid temperature is 130°C, the air temperature is 115°C, the temperature is lowered to 50°C, and the water and toluene in the water separator are separated to prepare for vacuum distillation. The vacuum degree of the mother liquor is -0.097MPa, heating, the condenser is fed with ethanol at -10°C, under the condition of stirring, vacuum distillation is carried out, the liquid temperature is 39°C, the air temperature is 32°C, there is a fraction produced, which is a toluene fraction, and the toluene fraction can be recycled use. The liquid temperatu...

Embodiment 2

[0015] Add one part of toluene to four parts of dimethylformamide mother liquor, the drug intermediate, the volume of the added toluene is greater than or equal to the volume of the water separator, stir, heat up, the liquid temperature is 93°C, and there is a distillate, the liquid temperature is 99°C, and the air temperature is 80°C Generate total backflow and separate water at any time. The reflux timer is over for 5.5 hours, the liquid temperature is 130°C, the air temperature is 115°C, the temperature is lowered to 50°C, and the water and toluene in the water separator are separated to prepare for vacuum distillation. The vacuum degree of the mother liquor is -0.097MPa, heating, the condenser is fed with ethanol at -10°C, under the condition of stirring, vacuum distillation is carried out, the liquid temperature is 39°C, the air temperature is 32°C, there is a fraction produced, which is a toluene fraction, and the toluene fraction can be recycled use. The liquid tempera...

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Abstract

The invention provides a DMF recovery technology. The technology comprises the following steps: adding toluene to a medicine intermediate dimethyl formamide (DMF) mother liquor from a pharmaceutical production workshop, carrying out stirring heating to 80-130DEG C, carrying out infinite reflux timing water separation for 4-5.5h, maintaining the water layer level in a water separator at a position accounting for 1 / 2 of the volume of the water separator, separating out water when water exceeds the liquid level, cooling after finishing the water separation, and respectively completely taking out the upper-layer toluene and the lower-layer water in the water separator; and cooling the reaction liquid to below 30DEG C, carrying out reduced pressure distillation under the degree of vacuum below -0.095Mpa to obtain a toluene fraction, heating to 60-65DEG C to obtain a DMF fraction, and stopping heating for distillation ending when the liquid temperature rises to 105DEG C. No new organic solvents are introduced in the solvent recovery process of the technology, so the cost consumed by the introduction of the new components in the recovery process is avoided; and the technology adopts the reduced pressure distillation, so the energy and the cost are saved, and the DMF content and the water content of the recovered DMF accord with reuse requirements.

Description

technical field [0001] The invention belongs to the technical field of solvent recovery of pharmaceutical intermediates, and in particular relates to a DMF recovery process. Background technique [0002] Dimethylformamide (DMF) is widely used as a solvent in raw materials and pharmaceutical intermediates. During production, a solution of DMF, water, a small amount of toluene and a small amount of pharmaceutical ingredients is obtained. The solution is dimethylformamide waste liquid. If it is not recovered, it will cause environmental pollution and increase the pressure on environmental protection, and on the other hand, the production cost will increase. In order to recycle DMF, water, toluene and trace drug impurities must be removed. The traditional process usually uses rectification or extraction to remove the water and recover the solvent. However, the rectification process takes a long time to remove water and requires a rectification tower. The equipment investment is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C233/03C07C231/24
Inventor 姜起栋芮庆云张齐王笑玉
Owner TIANJIN PHARMA GROUP GENCOM PHARMA