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Method for recovering caffeine from caffeine refined mother liquor

A mother liquor recovery and caffeine technology, applied in the direction of organic chemistry, can solve the problems of high caffeine pigment content, low effective utilization rate, low caffeine yield, etc., to avoid solvent leakage, save energy consumption, and simple process Effect

Active Publication Date: 2021-11-30
上海赛奥分离技术工程有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the solvent extraction method, there is no selective extraction of caffeine, pigment and other impurities by the solvent. When the solvent is distilled and recovered, the content of caffeine and pigment obtained is high, the energy consumption is high when recovering the solvent, and a certain amount remains in the discharged wastewater Solvents are easy to cause environmental pollution, the amount of solvents is large, and the effective utilization rate is low; while the resin adsorption process will firstly introduce a desorbent, and the second resin regeneration process will produce a large amount of waste acid and waste lye, and the third is the recovery of caffeine. low rate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] Take 200kg of caffeine refined mother liquor, in which the content of caffeine is 1.52%, and the conductivity is 7500μS / cm. It is clarified and removed by a 300000Dal ultrafiltration tubular ceramic membrane, and the obtained clarified solution is filtered by a 3000Dalton NF-II nanofiltration The membrane is decolorized and desalinated, 50kg of deionized water is added, and the concentrated solution is discharged to obtain 240kg of decolorized solution with a yield of 98% and a conductivity of 6350μS / cm. The caffeine product is obtained after the liquid is cooled and crystallized and filtered, and the yield of the product can reach 65.8%;

example 2

[0025] Take 200kg of caffeine refined mother liquor, in which the content of caffeine is 1.58%, and the conductivity is 7700μS / cm. It is clarified and removed by 100000Dal ultrafiltration tubular ceramic membrane, and the obtained clarified solution is decolorized by 2000Dal NF-II nanofiltration membrane. Desalting, adding 50kg of deionized water, draining the concentrated solution, and obtaining 240kg of decolorized solution with a yield of 98% and a conductance of 5100 μS / cm. The decolorized solution enters a 300Dal NF-III nanofiltration system for nanofiltration concentration, and the obtained concentrated solution is cooled. After crystallization and filtration, the caffeine product can be obtained, and the yield of the product can reach more than 75%;

example 3

[0027] Take 200kg of caffeine refined mother liquor, wherein the content of caffeine is 1.66%, the conductivity is 7130μS / cm, and the ultrafiltration tubular ceramic membrane of 10000Dal is used to clarify and remove impurities, and the obtained clarified liquid is decolorized by NF-II nanofiltration membrane of 2000Dal Desalination, add 50kg deionized water, discharge the concentrated liquid, and obtain 240kg of decolorized liquid with a yield of 90% and a conductivity of 5010μS / cm. The decolorized liquid enters the 200Dal NF-III nanofiltration system for nanofiltration concentration, and the temperature is controlled at 40-50 The concentrated solution obtained at ℃ is cooled to crystallize and filtered to obtain the caffeine product, and the yield of the product is 88.3%;

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Abstract

The invention relates to the technical field of chemical process technologies, in particular to a method for recovering caffeine from caffeine refined mother liquor, and the method is high in caffeine recovery rate and low in process cost. The whole technological process is a physical process, does not involve the processes of solvent extraction, resin adsorption and the like, and is green and environment-friendly. The method comprises the following steps: 1) pretreatment of caffeine refined mother liquor: clarifying and removing impurities from the caffeine refined mother liquor through an ultrafiltration tube type ceramic membrane UF-I ultrafiltration system with the molecular weight of 10000-300000 Dal, and controlling the temperature to be 18-50 DEG C to obtain clarified and transparent caffeine refined mother liquor; (2) decolorizing and desalting the clarified liquid of the caffeine refining mother liquid obtained in the step (1) through an NF-II nanofiltration system, controlling the temperature to be 18-50 DEG C, and adding top washing water which is 5 times of the volume of the concentrated liquid to obtain a decolorized solution with the caffeine yield being greater than or equal to 99%; and (3) carrying out high-temperature concentration on the decolored solution obtained in the step (2) through an NF-III nanofiltration system.

Description

technical field [0001] The invention relates to the technical field of chemical technology, in particular to a method for recovering caffeine from caffeine refining mother liquor. Background technique [0002] In the production process of chemical synthesis of caffeine, the caffeine finished product must meet the quality standards stipulated in the Pharmacopoeia of my country and other countries. The process requires a refining section. The refining section is to add oxidants and activated carbon to decolorize the crude caffeine after reconstitution at high temperature, and the decolorization solution After cooling, crystallization, filtration, and drying, the process of forming the finished caffeine. During the refining process, the residual amount of caffeine in the refined mother liquor after crystallization and filtration is about 15-20% of the crude caffeine. [0003] Conventional extraction of caffeine in refined mother liquor includes single solvent extraction (chloro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D473/12
CPCC07D473/12
Inventor 孙威广张荻陈可刘旭红
Owner 上海赛奥分离技术工程有限公司
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