CN104496990A - Method for extracting caffeine by low temperature crystallization - Google Patents
Method for extracting caffeine by low temperature crystallization Download PDFInfo
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- CN104496990A CN104496990A CN201410583402.9A CN201410583402A CN104496990A CN 104496990 A CN104496990 A CN 104496990A CN 201410583402 A CN201410583402 A CN 201410583402A CN 104496990 A CN104496990 A CN 104496990A
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- caffeine
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- chloroform
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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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- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
- Tea And Coffee (AREA)
Abstract
The invention discloses a method for extracting caffeine in tea by low temperature crystallization. Through immersion, extraction, chloroform recovery, dissolution, filtration, decoloring filtration and natural crystallization, high purity caffeine is prepared. The whole method for extraction is carried out at a low temperature, has low energy consumption and high efficiency, is realized conveniently, has easily operatable and simple processes, a high extraction rate and can produce high purity caffeine.
Description
Technical field
The invention belongs to retrofit field, particularly a kind of method from Extraction of Caffeine From Tea.
Background technology
Caffeine is a kind of alkaloid extract from tealeaves, coffee cherry etc., and moderately using has the effect of dispelling fatigue, excitor nerve, can be used for treatment neurasthenia and stupor recovery clinically.Tea is the important sources of caffeine, and the research of therefore extracting natural caffeine technology from tea is extremely paid attention to always.
Containing caffeine 2%-5% in tealeaves, current general subliming method is from Extraction of Caffeine From Tea, and because the sublimation temperature of trimethyl-xanthine is at about 178 DEG C, therefore this method needs at high temperature to carry out, and technique is comparatively complicated.In order to make extraction process more simple, need a kind of Carbonado Diamond method in tealeaves that can realize at low temperatures at present badly.
Summary of the invention
In order to realize above object, the invention provides a kind of method of low temperature crystallization extracting caffeine, its technique is simple, can realize easily at low temperatures.
Technical scheme provided by the present invention is:
A method for low temperature crystallization extracting caffeine, comprises the following steps:
(1) tealeaves is put into pure water to soak, the weight ratio of tea is 1:7-1:10, and the temperature of pure water is 85-95 DEG C, and the time of immersion is 40-50 minute, obtains leach liquor;
(2) repeating step (1) 3 time or more;
(3) extracted by leach liquor chloroform, the weight ratio of chloroform and leach liquor is 1:5, obtains extract;
(4) carry out obtaining caffeine crude product after chloroform reclaims to extract;
(5) caffeine crude product and water are dissolved at 80-100 DEG C by weight 1:8, lysate carries out filtration and obtains filtered liquid;
(6) put into gac in filtered liquid to decolour, temperature remains on 60-80 DEG C, and time 40-50 minute, obtains destainer;
(7) destainer carries out filtration and obtains filtrate;
(8) filtrate carries out spontaneous nucleation in temperature 10-20 DEG C of situation, obtains high purity caffeine.
Wherein, filtered liquid is visual in step (5) when being judged as that clarity is not enough, filtered liquid chloroform is extracted, the weight ratio of chloroform and leach liquor is 1:5, obtain extract, chloroform is carried out to extract and reclaims acquisition caffeine crude product again, and then caffeine crude product and water are dissolved by weight 1:8 at 80-100 DEG C, lysate carries out filtration and obtains filtered liquid, repeats this step until filtered liquid is visual be judged as clarification.
Beneficial effect of the present invention is: the whole leaching process of the present invention all carries out under low-temperature condition, and energy consumption is low, efficiency is high, realization is convenient; Each step easy handling, technique is simple; Extraction yield is high, and gained caffeine purity is high.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Details are as follows for the step that the present invention comprises from the method for Extraction of Caffeine From Tea.
Step (1), puts into pure water by tealeaves and soaks, and the weight ratio of tea is 1:7 ~ 1:10, and the temperature of pure water is 85-95 DEG C, and the time of immersion is 40-50 minute, obtains leach liquor.After this step completes, the effective constituent in tealeaves can decompose in leach liquor.
Step (2), repeating step (1) 3 time or more, makes the effective constituent of the overwhelming majority in tealeaves to soak out.
Step (3), extracts leach liquor chloroform.Chloroform and water body complementation mix, and the solubleness of caffeine in chloroform is greater than the solubleness in water body, and therefore in extraction process, caffeine can be transferred in chloroform.The weight ratio of the chloroform that this step is used and leach liquor is 1:5.After having extracted, the chloroform being dissolved with caffeine is separated, remember extract.
Step (4), carries out obtaining caffeine crude product after chloroform reclaims to extract.The mode reclaimed chloroform can be distillation etc.Chloroform is recovered rear remaining material and is caffeine crude product.
Step (5), dissolves caffeine crude product and water by weight 1:8 at 80-100 DEG C, and lysate carries out filtration and obtains filtered liquid.Filtration procedure can utilize duplex strainer to carry out.This step makes caffeine composition return in solution.In this step, if filtered liquid is visual when being judged as that clarity is not enough, so filtered liquid needs to re-start extraction-dissolution process, namely filtered liquid chloroform is extracted, the weight ratio of chloroform and leach liquor is 1:5, obtains extract, carries out chloroform reclaim acquisition caffeine crude product again to extract, and then caffeine crude product and water are dissolved at 80-100 DEG C by weight the ratio of 1:8, lysate carries out filtration and obtains filtered liquid.The object repeating extraction-dissolution process is to guarantee that filtered liquid is enough clarified.During general enforcement, the extraction repeated-dissolution process number of times is at 1-2 time.
Step (6), put into gac in filtered liquid and decolour, temperature remains on 60-80 DEG C, and time 40-50 minute, obtains destainer.During decolouring, the part by weight of gac is about 8%, and this step can guarantee that the caffeine purity of gained promotes further.
Step (7), destainer carries out filtration and obtains filtrate.Filtration procedure can utilize duplex strainer to realize equally.
Step (8), filtrate carries out spontaneous nucleation in temperature 10-20 DEG C of situation, obtains high purity caffeine.
For embodiment, the present invention will be described below.
Embodiment one
(1) tealeaves is put into pure water to soak, the weight ratio of tea is 1:7, and the temperature of pure water is 85 DEG C, and the time of immersion is 40 minutes, obtains leach liquor;
(2) repeating step (1) 3 time;
(3) extracted by leach liquor chloroform, the weight ratio of chloroform and leach liquor is 1:5, obtains extract;
(4) carry out obtaining caffeine crude product after chloroform reclaims to extract;
(5) caffeine crude product and water are dissolved at 80-100 DEG C by weight the ratio of 1:8, lysate carries out filtration and obtains filtered liquid;
(6) put into gac in filtered liquid to decolour, temperature remains on 60-80 DEG C, 40 minutes time, obtains destainer;
(7) destainer carries out filtration and obtains filtrate;
(8) filtrate carries out spontaneous nucleation within the scope of temperature 10-20 DEG C, obtains high purity caffeine.
In the present embodiment, the caffeine purity extracted is 97.8%, and extraction yield is 1.542%.
Embodiment two
(1) tealeaves is put into pure water to soak, the weight ratio of tea is 1:10, and the temperature of pure water is 90 DEG C, and the time of immersion is 50 minutes, obtains leach liquor;
(2) repeating step (1) 3 time;
(3) extracted by leach liquor chloroform, the weight ratio of chloroform and leach liquor is 1:5, obtains extract;
(4) carry out obtaining caffeine crude product after chloroform reclaims to extract;
(5) caffeine crude product and water are dissolved at 80-100 DEG C by weight 1:8, lysate carries out filtration and obtains filtered liquid;
(6) put into gac in filtered liquid to decolour, temperature remains on 60-80 DEG C, 45 minutes time, obtains destainer;
(7) destainer carries out filtration and obtains filtrate;
(8) filtrate carries out spontaneous nucleation in temperature 10-20 DEG C of situation, obtains high purity caffeine.
In the present embodiment, the caffeine purity extracted is 98.3%, and extraction yield is 1.732%.
Embodiment three
(1) tealeaves is put into pure water to soak, the weight ratio of tea is 1:9, and the temperature of pure water is 95 DEG C, and the time of immersion is 50 minutes, obtains leach liquor;
(2) repeating step (1) 4 time;
(3) extracted by leach liquor chloroform, the weight ratio of chloroform and leach liquor is 1:5, obtains extract;
(4) carry out obtaining caffeine crude product after chloroform reclaims to extract;
(5) caffeine crude product and water are dissolved at 80-100 DEG C by weight 1:8, lysate carries out filtration and obtains filtered liquid; Filtered liquid chloroform is extracted, the weight ratio of chloroform and leach liquor is 1:5, obtain extract, chloroform is carried out to extract and reclaims acquisition caffeine crude product again, and then caffeine crude product and water are dissolved at 80-100 DEG C by weight the ratio of 1:8, lysate carries out filtering again obtaining filtered liquid;
(6) put into gac in filtered liquid to decolour, temperature remains on 60-80 DEG C, 50 minutes time, obtains destainer;
(7) destainer carries out filtration and obtains filtrate;
(8) filtrate carries out spontaneous nucleation in temperature 10-20 DEG C of situation, obtains high purity caffeine.
In the present embodiment, the caffeine purity extracted is 98.7%, and extraction yield is 1.943%.
Embodiment four
(1) tealeaves is put into pure water to soak, the weight ratio of tea is 1:10, and the temperature of pure water is 90 DEG C, and the time of immersion is 50 minutes, obtains leach liquor;
(2) repeating step (1) 4 time;
(3) extracted by leach liquor chloroform, the weight ratio of chloroform and leach liquor is 1:5, obtains extract;
(4) carry out obtaining caffeine crude product after chloroform reclaims to extract;
(5) caffeine crude product and water are dissolved at 80-100 DEG C by weight 1:8, lysate carries out filtration and obtains filtered liquid; Filtered liquid chloroform is extracted, the weight ratio of chloroform and leach liquor is 1:5, obtain extract, chloroform is carried out to extract and reclaims acquisition caffeine crude product again, and then caffeine crude product and water are dissolved at 80-100 DEG C by weight the ratio of 1:8, lysate carries out filtering again obtaining filtered liquid; Repeat this step 2 time;
(6) put into gac in filtered liquid to decolour, temperature remains on 60-80 DEG C, 50 minutes time, obtains destainer;
(7) destainer carries out filtration and obtains filtrate;
(8) filtrate carries out spontaneous nucleation in temperature 10-20 DEG C of situation, obtains high purity caffeine.
In the present embodiment, the caffeine purity extracted is 99.3%, and extraction yield is 2.190%.
As can be seen from the above embodiments, the DNA purity of present method caffeine is subject to the re-extract-dissolving times influence of filtered liquid in step (5), and number of times is larger, and the purity of gained is higher, is also subject to the time effects of activated carbon decolorizing simultaneously.Extraction yield is then subject to the factor impacts such as infusion of tea number of times.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. a method for low temperature crystallization extracting caffeine, is characterized in that, comprises the following steps:
(1) tealeaves is put into pure water to soak, the weight ratio of tea is 1:7-1:10, and the temperature of pure water is 85-95 DEG C, and the time of immersion is 40-50 minute, obtains leach liquor;
(2) repeating step (1) 3 time or more;
(3) extracted by leach liquor chloroform, the weight ratio of chloroform and leach liquor is 1:5, obtains extract;
(4) carry out obtaining caffeine crude product after chloroform reclaims to extract;
(5) caffeine crude product and water are dissolved at 80-100 DEG C by weight 1:8, lysate carries out filtration and obtains filtered liquid;
(6) put into gac in filtered liquid to decolour, temperature remains on 60-80 DEG C, and time 40-50 minute, obtains destainer;
(7) destainer carries out filtration and obtains filtrate;
(8) filtrate carries out spontaneous nucleation in temperature 10-20 DEG C of situation, obtains high purity caffeine.
2. the method for a kind of low temperature crystallization extracting caffeine according to claim 1, it is characterized in that: filtered liquid is visual in step (5) when being judged as that clarity is not enough, filtered liquid chloroform is extracted, the weight ratio of chloroform and leach liquor is 1:5, obtain extract, chloroform is carried out to extract and reclaims acquisition caffeine crude product again, and then caffeine crude product and water are dissolved at 80-100 DEG C by weight 1:8, lysate carries out filtration and obtains filtered liquid, repeats this step until filtered liquid is visual be judged as clarification.
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| CN201410583402.9A CN104496990A (en) | 2014-10-27 | 2014-10-27 | Method for extracting caffeine by low temperature crystallization |
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| CN201410583402.9A CN104496990A (en) | 2014-10-27 | 2014-10-27 | Method for extracting caffeine by low temperature crystallization |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1047017A (en) * | 1989-05-12 | 1990-11-21 | 江苏省卫生防疫站 | From tealeaves, extract the method for natural caffeine |
| CN1056692A (en) * | 1991-06-06 | 1991-12-04 | 冯世型 | From tealeaves, produce the method for natural caffeine |
| CN1172112A (en) * | 1997-08-19 | 1998-02-04 | 玉溪师范高等专科学校 | Process for extracting caffeine from waste tea dust |
| CN104130260A (en) * | 2014-07-07 | 2014-11-05 | 李华 | Caffeine extraction method |
-
2014
- 2014-10-27 CN CN201410583402.9A patent/CN104496990A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1047017A (en) * | 1989-05-12 | 1990-11-21 | 江苏省卫生防疫站 | From tealeaves, extract the method for natural caffeine |
| CN1056692A (en) * | 1991-06-06 | 1991-12-04 | 冯世型 | From tealeaves, produce the method for natural caffeine |
| CN1172112A (en) * | 1997-08-19 | 1998-02-04 | 玉溪师范高等专科学校 | Process for extracting caffeine from waste tea dust |
| CN104130260A (en) * | 2014-07-07 | 2014-11-05 | 李华 | Caffeine extraction method |
Non-Patent Citations (1)
| Title |
|---|
| 胡秋辉等: "《茶叶中咖啡因和茶多酚提取技术研究》", 《天然产物研究与开发》, vol. 9, no. 2, 30 June 1997 (1997-06-30), pages 63 - 66 * |
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Application publication date: 20150408 |