CN113717173B - Method for recovering caffeine from caffeine refining mother liquor - Google Patents
Method for recovering caffeine from caffeine refining mother liquor Download PDFInfo
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- CN113717173B CN113717173B CN202111012217.0A CN202111012217A CN113717173B CN 113717173 B CN113717173 B CN 113717173B CN 202111012217 A CN202111012217 A CN 202111012217A CN 113717173 B CN113717173 B CN 113717173B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D473/00—Heterocyclic compounds containing purine ring systems
- C07D473/02—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6
- C07D473/04—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms
- C07D473/06—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3
- C07D473/12—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms with radicals containing only hydrogen and carbon atoms, attached in position 1 or 3 with methyl radicals in positions 1, 3, and 7, e.g. caffeine
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Abstract
The invention relates to the technical field of chemical process technology, in particular to a method for recovering caffeine from caffeine refining mother liquor, which has high caffeine recovery rate and low process cost; the whole process is a physical process and does not involve solvent extraction, resin adsorption and other processes, and the process is green and environment-friendly; the method comprises the following steps: 1) Pretreatment of caffeine refining mother liquor: clarifying and removing impurities from the refined caffeine mother liquor by an ultrafiltration tubular ceramic membrane UF-I ultrafiltration system with the molecular weight of 10000-300000Dal, controlling the temperature to be 18-50 ℃ to obtain clarified and bright refined caffeine mother liquor; 2) Decolorizing and desalting the clarified liquid of the caffeine refined mother liquor obtained in the step 1) by an NF-II nanofiltration system, controlling the temperature at 18-50 ℃, adding top washing water with the volume 5 times that of the concentrated solution, and obtaining a decolorized liquid with the caffeine yield being more than or equal to 99%; 3) Concentrating the decolored liquid obtained in the step 2) at high temperature by an NF-III nanofiltration system.
Description
Technical Field
The invention relates to the technical field of chemical process technology, in particular to a method for recovering caffeine from caffeine refining mother liquor.
Background
In the chemical synthesis production process of caffeine, the finished caffeine product is required to meet the quality standards specified in pharmacopoeias of China and various countries, and the technological process needs a refining working section, wherein the refining working section is a process of adding an oxidant and active carbon to decolor after redissolving a crude caffeine product at a high temperature, and cooling, crystallizing, filtering and drying a decolored liquid to form the finished caffeine product. During the refining process, the residual content of caffeine in the refined mother liquor after crystallization filtration is about 15-20% of the crude caffeine.
The caffeine in the conventional refined mother liquor is extracted by a single solvent extraction method (chloroform extraction), a mixed solvent extraction method, resin adsorption and the like. The solvent extraction method has the advantages that the solvent is used for completely extracting caffeine, pigments and other impurities, the content of the obtained caffeine pigments is high when the solvent is distilled and recovered, the energy consumption is high when the solvent is recovered, a certain amount of solvent is remained in discharged wastewater, the environmental pollution is easily caused, the using amount of the solvent is large, and the effective utilization rate is low; in the resin adsorption process, an analytic agent is introduced, and in the resin regeneration process, a large amount of waste acid and waste alkali liquor are generated, so that the yield of caffeine is low.
Disclosure of Invention
In order to solve the technical problems, the invention provides the method for recovering the caffeine from the caffeine refining mother liquor, which has high caffeine recovery rate and low process cost; the whole process is a physical process and does not involve solvent extraction, resin adsorption and other processes, and the process is green and environment-friendly.
The invention relates to a method for recovering caffeine from caffeine refining mother liquor, which comprises the following steps:
1) Pretreatment of caffeine refining mother liquor: clarifying and removing impurities from the refined caffeine mother liquor by an ultrafiltration tubular ceramic membrane UF-I ultrafiltration system with the molecular weight of 10000-300000Dal, controlling the temperature to be 18-50 ℃ to obtain clarified and bright refined caffeine mother liquor;
2) Decolorizing and desalting clear liquor of the caffeine refined mother liquor obtained in the step 1) by an NF-II nanofiltration system, controlling the temperature at 18-50 ℃, adding top washing water with the volume 5 times that of concentrated liquor, and obtaining decolorized liquor with the caffeine yield more than or equal to 99%;
3) Concentrating the decolorized solution obtained in the step 2) at high temperature by an NF-III nanofiltration system, controlling the temperature to be 40-50 ℃ to obtain a concentrated solution with the caffeine mass concentration of 8-10% and a dialyzed clear solution;
4) The nanofiltration dialysis cleaning in the step 3) is used as the top washing water in the step 2), so that the use efficiency of water is improved, and the discharge amount of wastewater is reduced;
5) Cooling, crystallizing and filtering the concentrated solution obtained in the step 3) to obtain caffeine and a crystallization mother solution I;
6) And (3) returning the crystallization mother liquor in the step 4) to the step 2) for reuse, so that the overall yield is improved.
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention adopts the full membrane method process to recover the caffeine in the caffeine crystallization mother liquor, and adopts the ceramic membrane + nanofiltration full membrane method process, and the processes are all physical processes, so that the process is simple, the operation is convenient and fast, and the energy consumption is low;
(2) The invention is a solvent-free process method, which not only saves the energy consumption of solvent regeneration, but also can improve the industrial production environment and avoid the risk of environmental pollution caused by solvent leakage and solvent residue in sewage;
(3) The membrane core (ceramic membrane and NF membrane) adopted by the invention can be completely regenerated, and the waste water generated in the regeneration process is less, so that the discharge amount of sewage of enterprises can be reduced;
(4) In the NF-III concentration process, the invention can realize the recycling of 90 percent of water and realize the energy conservation and emission reduction of enterprises.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
The invention provides a method for recovering caffeine from caffeine refining mother liquor, which comprises the following steps: 1) The pretreatment step of the caffeine refining mother liquor comprises the following steps: the pretreatment of the caffeine refined mother liquor comprises the steps of filtering the caffeine refined mother liquor by an ultrafiltration tubular ceramic membrane system to remove impurities and clarify, wherein in the pretreatment process of the caffeine refined mother liquor, the aperture of the ultrafiltration tubular ceramic membrane is 10000-300000Dal, and the temperature is controlled at 18-50 ℃ to obtain a pretreatment solution of the caffeine refined mother liquor; 2) Removing impurities (decoloring and desalting) from the pretreatment solution obtained in the step 1) at 30-50 ℃ by an NF-II nanofiltration system to obtain a decolored solution, wherein the molecular weight of a nanofiltration membrane used by the NF-II nanofiltration system is 800-3000Dal, the pretreatment solution is concentrated by 10-20 times, and deionized water with the volume of 3-5 times of that of the concentrated solution is added; 3) Concentrating the decolorized solution in the step 2) at 30-60 ℃ by an NF-III nanofiltration system to obtain nanofiltration concentrated solution, wherein the molecular weight of a nanofiltration membrane used by the NF-III system is 150-500Dal, one part of the dialysate subjected to nanofiltration concentration can be used as top washing water in the step 2), and the other part of the dialysate can be used as water for producing other working sections;
4) And (3) cooling, crystallizing and filtering the concentrated solution obtained in the step 3) to obtain caffeine and a small amount of crystallization mother liquor I, wherein the crystallization temperature is 18-30 ℃, and the crystallization mother liquor I is returned to the step 3), so that the recovery rate of the caffeine can be improved to be more than 95%.
The process for recovering caffeine by using a full-membrane method comprises the steps of clarifying and removing impurities by using an UF-I ultrafiltration tube type ceramic membrane, decoloring and desalting by using an NF-II nanofiltration system, and concentrating and recovering caffeine by using an NF-III nanofiltration system, wherein the recovery rate of caffeine is up to 95 percent, and the recovery rate of water is up to 90 percent
The invention is further illustrated below with reference to specific examples:
example 1
Taking 200kg of caffeine refined mother liquor, wherein the content of caffeine is 1.52%, the conductance is 7500 mu S/cm, clarifying and impurity removing are carried out by an ultrafiltration tubular ceramic membrane of 300000Dal, decoloring and desalting are carried out on the obtained clarified liquor by an NF-II nanofiltration membrane of 3000 Dalton, 50kg of deionized water is added, concentrated liquor is discharged, the decolored liquor with the yield of 240kg and the conductance of 98% and 6350 mu S/cm is obtained, the decolored liquor enters an NF-III nanofiltration system of 500Dal for nanofiltration and concentration, the obtained concentrated liquor is subjected to temperature reduction, crystallization and filtration to obtain a caffeine product, and the yield of the product can reach 65.8%;
example 2
Taking 200kg of caffeine refined mother liquor, wherein the content of caffeine is 1.58%, the conductance is 7700 mu S/cm, clarifying and impurity-removing through 100000Dal ultrafiltration tubular ceramic membranes, decoloring and desalting the obtained clear liquor through 2000Dal NF-II nanofiltration membranes, adding 50kg of deionized water, discharging the concentrated liquor to obtain 240kg of decolored liquor with the yield of 98% and the conductance of 5100 mu S/cm, allowing the decolored liquor to enter a 300Dal NF-III nanofiltration system for nanofiltration concentration, cooling, crystallizing and filtering the obtained concentrated liquor to obtain a caffeine product, and the yield of the product can reach more than 75%;
example 3
Taking 200kg of caffeine refined mother liquor, wherein the content of caffeine is 1.66%, conducting 7130 mu S/cm, clarifying and removing impurities by an ultrafiltration tubular ceramic membrane of 10000Dal, decoloring and desalting the obtained clarified liquor by an NF-II nanofiltration membrane of 2000Dal, adding 50kg of deionized water, discharging the concentrated liquor to obtain a decolored liquor with yield of 240kg and conductivity of 5010 mu S/cm, nano-filtering and concentrating the decolored liquor in an NF-III nanofiltration system of 200Dal, cooling and crystallizing the concentrated liquor obtained at the temperature of 40-50 ℃ to obtain a caffeine product, wherein the yield of the product is 88.3%;
example 4
Taking 200kg of caffeine refined mother liquor, wherein the content of caffeine is 1.61%, the conductance is 7300 mu S/cm, clarifying and impurity removing are carried out by an 20000Dal ultrafiltration tube type ceramic membrane, the obtained clear liquor is subjected to decoloration and desalination by an 800Dal NF-I nanofiltration membrane, 50kg of top washing water is added, the concentrated liquor is discharged, the decolored liquor with the yield of 240kg and the conductance of 3700 mu S/cm is obtained, the decolored liquor enters a 150 Dalton NF-III nanofiltration system for nanofiltration and concentration, the obtained concentrated liquor is subjected to temperature reduction, crystallization and filtration to obtain a caffeine product, and the yield of the product is 43%;
example 5
Taking 200kg of caffeine refined mother liquor, wherein the content of caffeine is 1.6%, conducting 7130 mu S/cm, clarifying and removing impurities by an ultrafiltration tubular ceramic membrane of 10000Dal, decoloring and desalting the obtained clarified liquor by an NF-II nanofiltration membrane of 2000Dal, adding 50.0kg of top washing water, discharging concentrated liquor to obtain a decolored liquor with the yield of 240kg and the conductivity of 5010 mu S/cm, carrying out nanofiltration and concentration on the decolored liquor in an NF-III nanofiltration system of 200Dal, and carrying out cooling crystallization and filtration on the concentrated liquor obtained at the temperature of 30-40 ℃ to obtain a caffeine product, wherein the yield of the product is 65.3%;
example 6
The mother liquor obtained after the last step of crystallization and filtration in the embodiment 3 is returned to a NF-II nanofiltration concentration system, one part of NF-II nanofiltration concentration and dialysis water can be used as NF-I top washing water, and the other part of NF-II nanofiltration concentration and dialysis water can be used as water for other working sections, so that the total yield of caffeine can be improved, the discharge amount of sewage can be reduced by recycling reclaimed water, the total yield of caffeine is higher than 95%, and the recycling rate of water is higher than 90%.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, it is possible to make various improvements and modifications without departing from the technical principle of the present invention, and those improvements and modifications should be also considered as the protection scope of the present invention.
Claims (3)
1. A method for recovering caffeine from caffeine refining mother liquor is characterized by comprising the following steps:
the method comprises the following steps: adding caffeine refined mother liquor into circulation tank, filtering, clarifying and removing impurities by ultrafiltration tubular ceramic membrane UF-I ultrafiltration system with molecular weight of 10000-300000Dal, and controlling temperature to 18-50 deg.C;
step two; carrying out decoloration and desalination on the clarified ultrafiltration clear liquid through an NF-II nanofiltration system at a certain temperature, controlling the temperature to be 18-50 ℃, and adding top washing water with the volume 5 times that of the concentrated solution to obtain low-salt and low-pigment decoloration clear liquid I;
step three: concentrating the decolorized clear liquid I by an NF-III nanofiltration system to obtain a nanofiltration concentrated solution II of high-temperature and high-concentration caffeine, and controlling the temperature to be 40-50 ℃;
step four: and cooling, crystallizing and filtering the nanofiltration concentrated solution II at the temperature of 20 ℃ to obtain the caffeine.
2. The method for recycling caffeine from caffeine refining mother liquor according to claim 1, wherein NF-II used in the second step has a molecular weight of 800 to 3000Dal.
3. The method for recovering caffeine from caffeine refining mother liquor according to claim 2, wherein the molecular weight of NF-III used in step three is 150 to 500Dal.
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