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Caffeine methylated mother liquor cleaning process and device thereof

A clean treatment and caffeine technology, applied in the process and equipment field of caffeine methylation mother liquor cleaning treatment, can solve the problems of endangering the human immune system, large steam consumption, waste and so on, so as to improve the production operation environment and ensure life Safety and production cost reduction effects

Active Publication Date: 2014-05-28
QINGDAO UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are the following problems in the industrial use of chloroform to extract caffeine methylation mother liquor process: the recovery rate of chloroform in the extraction process is about 90%, the waste phenomenon is serious, and the unrecovered chloroform is difficult to handle; Methane is highly toxic, which can harm the human immune system and cause serious harm to the health of workers; chloroform is easy to decompose to produce phosgene when exposed to light, and phosgene is easy to explode, seriously threatening the lives of workers; trichloromethane The COD value of the mother liquor after methane extraction is as high as 35,000mg / L, which requires biochemical sewage treatment, and the sewage treatment cycle is longer; the process route for the extraction of caffeine methylation mother liquor with chloroform is long, and various equipment is complicated; the process of chloroform treatment The consumption of medium steam is large, which increases the production cost and reduces the economic benefits of the factory
The adsorption process is not complete, a part of caffeine will still remain in the mother liquor, the adsorption time is longer, and the operation cycle is longer
The mother liquor treated with macroporous adsorption resin still needs to be treated with biochemical sewage, and the follow-up work is still complicated

Method used

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  • Caffeine methylated mother liquor cleaning process and device thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: Add 1 ton of methylated mother liquor in the decompression evaporation crystallization kettle, control the temperature of the mother liquor to be 80° C., and evaporate the liquid amount to be 70% (calculated by volume), and pass the secondary mother liquor into the condenser after filtering Cool down so that the temperature of the mother liquor at the outlet is 30°C, and the crude product caffeine is obtained. After purification, the yield of caffeine is 92.0%. The mother liquor is steamed out of 40% of the liquid through a vacuum evaporator three times, and the colloidal substance is dried, pulverized, After sublimation purification treatment, the recovery rate of caffeine is 89.1%. The overall recovery of caffeine was 99.1%.

Embodiment 2

[0026] Embodiment 2: Add 1 ton of methylated mother liquor in the decompression evaporation crystallization kettle, control the temperature of the mother liquor to be 80° C., and evaporate the liquid amount to be 72% (calculated by volume), and pass the secondary mother liquor into the condenser after filtering Cool down so that the temperature of the mother liquor at the outlet is 32°C, and the crude product caffeine is obtained. After purification, the yield of caffeine is 92.4%. Three times the mother liquor is steamed out of 40% of the liquid through the decompression evaporator, and the colloidal substance is dried, pulverized, After sublimation purification treatment, the recovery rate of caffeine is 89.1%. The overall recovery of caffeine was 99.2%.

Embodiment 3

[0027] Embodiment 3: Add 1 ton of methylated mother liquor in the decompression evaporation crystallization kettle, control the temperature of the mother liquor to be 80° C., and evaporate the liquid amount to be 72% (calculated by volume), and pass the secondary mother liquor into the condenser after filtering Cool down so that the temperature of the mother liquor at the outlet is 30°C, and the crude product caffeine is obtained. After purification, the yield of caffeine is 92.4%. Three times the mother liquor is steamed out of 40% of the liquid through the decompression evaporator, and the colloidal substance is dried, pulverized, After sublimation purification treatment, the recovery rate of caffeine is 89.1%. The overall recovery of caffeine was 99.1%.

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Abstract

The invention relates to a caffeine methylated mother liquor cleaning process and a device thereof, and provides a process of separating methyl sulfate sodium by pressure reduction evaporative crystallization, extracting caffeine by cooling crystallization, separating methyl sulfate sodium by pressure reduction evaporative crystallization again, processing gelatinoid by a rotary vacuum drying technology, and recycling caffeine in the gelatinoid by sublimation, and an experiment is carried out to obtain the proper conditions for the first stage of pressure reduction evaporative crystallization that: the vacuum degree is 0.03-0.05MPa, the evaporative crystallization temperature is 80-90 DEG C, and the content of evaporated liquid is 60-75 percent by volume. The proper conditions for cooling crystallization are that the crystallization temperature is 30-45 DEG C, and the cooling crystallization time is 1-3 hours. Crystals are purified, and the recovery rate of the caffeine is 90.7%. In the second stage of pressure reduction evaporative crystallization, the content of the evaporated liquid is 35-45 percent by volume.

Description

technical field [0001] The invention belongs to the technical field of pharmacy, and in particular relates to a process and equipment for cleaning and treating caffeine methylation mother liquor. Background technique [0002] Caffeine is a central nervous system stimulant, which has the effects of eliminating fatigue, exciting nerves, and treating neurasthenia. Caffeine can be isolated and extracted from tea leaves and coffee beans, and was first synthesized by chemical methods in 1899 by Fischer. Since Tranbe, a German, published the literature on the chemical synthesis of caffeine in 1900, people have continuously created new results in the research of caffeine production methods for a century. These methods include: ethyl cyanoacetate method, cyanoacetic acid and urea synthesis method, semi-synthetic method and dimethyl urea and cyanoacetic acid synthesis method. Ethyl cyanoacetate method, that is, ethyl cyanoacetate is condensed with urea in the presence of sodium etho...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D473/12C07C305/04C07C303/44
Inventor 王英龙刘迎朱兆友禹继志吕忠泽
Owner QINGDAO UNIV OF SCI & TECH