CN1032753C - Process for preparing tea natural alkaloid-caffeine - Google Patents
Process for preparing tea natural alkaloid-caffeine Download PDFInfo
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- CN1032753C CN1032753C CN 93108755 CN93108755A CN1032753C CN 1032753 C CN1032753 C CN 1032753C CN 93108755 CN93108755 CN 93108755 CN 93108755 A CN93108755 A CN 93108755A CN 1032753 C CN1032753 C CN 1032753C
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- Coloring Foods And Improving Nutritive Qualities (AREA)
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Abstract
The present invention relates to a preparing method for extracting natural alkaloid, namely caffeine, from tea leaves. The preparing method is characterized in that the method comprises the following steps: firstly, removing large quantities of different tea contents in leaching liquid; using auxiliary materials with low price and easy acquirement as a masking agent of the rest impurities; finally carrying out one-step sublimation to prepare pure products of natural dehydrated caffeine. No harmful substances, such as toxic organic solvents, heavy metallic salts, etc. is used during an extraction process. The present invention has the advantages of simple and available technology and safe and convenient operation, and is suitable for the realization of industrial production. The products have the advantages of high purity, low cost and high safety.
Description
The present invention is a kind of natural alkaloid that extracts from tealeaves---the preparation technology of caffeine, belongs to field of fine chemical.
Caffeine has another name called trimethyl-xanthine, is one of main inclusion of tealeaves.The source of caffeine mainly contains two kinds of approach in the world at present: the one, from the natural coffee beans, extract; Another is to produce by the synthetic method.Though the former also is natural product, extracting method mostly is with objectionable impuritiess such as organic solvent chloroforms and makes extraction agent, has certain toxic side effect and raw and auxiliary material to cost an arm and a leg; Latter's quality and security are all not as good as natural product, and used main raw material is rare or harmful.In addition, the existing both at home and abroad preparation technology who extracts caffeine from tealeaves follows traditional method.These methods exist following shortcoming respectively: 1, utilize caffeine to be soluble in the characteristic of chloroform, with poisonous organic solvent chloroform give extraction agent; 2, adopt the compound that lead chloride etc. contains toxic heavy metal element to remove impurity; 3, complex process is loaded down with trivial details and extraction yield is lower, as distillation or repeatedly extraction and recrystallization repeatedly; 4, the potato spirit and other coloring matter that contain a great deal of in the product, purifying products, decolouring difficulty; 5, product purity is lower, and mostly is the hydrate that contains crystal water.The method that is provided as Chinese patent CN1047017A, extract with methylene dichloride or chloroform fraction exactly and will through boiling, 11 procedures such as filtration; And for example heavy metallic salt silver chloride, mercury chloride, plumbic acetate etc. have been adopted in the given method of CN1051481A.
In view of the problem of above-mentioned existence, the present invention aims to provide a kind of simple for process, easy-to-operate, product is nontoxic, all high tea natural dehydrated coffee of with low cost and extraction yield and purity because of preparation technology.
Technical characterstic of the present invention is earlier with alcohol lixiviate tealeaves, removes part lipid-soluble substance in the vat liquor again, and with the sequestering agent of giving birth to, white lime is made tannin etc., a step distils and makes the pure product of caffeine then.
The tealeaves of indication of the present invention comprises the tankage in the Tea Processing processes such as tea dust, tea ash, tea stalk, thick Lao Ye.
Technical process of the present invention mainly comprises the backflow lixiviate shown in Figure of description, filter, and distillation concentrates, and cooling is left standstill, and impurity is sheltered, and vapour is bathed evaporate to dryness, operations such as distillation.
Processing condition of the present invention and working method:
1, with tea dust or tea ash tea bits after removing foreign material etc. drop in the lixiviate jar, add the alcohol of 4～6 times of tea dust weight, aqueous alcoholic preferably, ethanol is 4-6 with the ratio of water: 1, the reflux lixiviate is 30-45 minute.If necessary, can be again with the alcohol of 2～4 times of amounts or aqueous alcoholic (4-6: 1) lixiviate 30 minutes of repeating to reflux.
2, with centrifugal, press filtration or method of pumping filtration vat liquor is separated with tea grounds.
3, with putting into concentrating unit after the vat liquor merging, can distill under normal pressure or reduced pressure, the volume of distillation concentrated solution is the 1/5-1/7 (solution density is the 1.26-1.28 grams per milliliter) of former vat liquor volume.
4, concentrated solution is put to cool place place and made it at room temperature to leave standstill cooling, treat vegetable jelly, chlorophyll, polysaccharide, vegetable-protein and other oil-soluble impurities precipitation fully, isolate supernatant liquor with decantation.
5, the life, the white lime mixture (ratio of mixture is 2: 3) that add tealeaves weight 25%～30% are made the buried body of tannin etc.; Preferably add 2 parts of unslaked limes earlier, stir into uniform pasty state, add 3 parts of white limes again, the after drying that stirs is dehydrated into powdery, and dehydration method can be oven dry or air stream drying.
6, meal is put into the distillation jar, under normal pressure or reduced pressure, distilled, make natural dehydrated coffee because of pure product.Decompression sublimation condition vacuum tightness is 0.1-0.3 normal atmosphere, and sublimation temperature is 105 ℃-120 ℃.
The present invention can extract 75～85% of content of caffeine in the tealeaves.
The sample that adopts the present invention's preparation is through sending Anhui Import and Export Commodities Inspection Bureau, The People's Republic of's check, and content of caffeine is up to 99.96%, and all other indexs also all are better than the standard of Chinese new edition pharmacopeia and 21 editions (U.S.P.XXI) defineds of American Pharmacopeia.
The present invention compares with domestic and international prior art, has following advantage:
1, simple for process, easy-to-operate, with low cost, be easy to realize suitability for industrialized production.
2, equal height of extraction yield and purity and material therefor greatly reduce.
3, do not adopt any deleterious organic solvent and other objectionable impuritiess in the leaching process, product is no any other toxic side effect in the intake scope that allows.
Provide embodiment below.
Embodiment:
Take by weighing 1 kilogram of low and middle-grade green tea end, add 6 kilograms of moisture edible ethanols (5: 1), water-bath refluxing extraction 30 minutes is filtered.Filter residue adds moisture edible ethanol (5: 1) again and repeats refluxing extraction 30 minutes for 4 kilograms, filter and merging filtrate, be evaporated to 1/6 of original volume, concentrated solution is positioned over shady and cool place and leaves standstill cooling 10 hours, incline and supernatant liquor, substrate is used and is higher than 80 ℃ equal-volume hot wash, washings is incorporated supernatant liquor into, in supernatant liquor, add 85 gram unslaked limes, stir into a paste, slowly add 170 gram white limes again while stirring, evaporate to dryness powdering in vapor bath then, under 200 ℃ of anoxic conditions distillation make about 185～216 gram pure white needle-like dehydrated coffees because of.
Claims (5)
1, a kind of natural alkaloid that from tealeaves, extracts---the preparation method of caffeine, it is characterized in that earlier with reflow of alcohol lixiviate tealeaves, vat liquor distillation is concentrated, at room temperature cooling precipitates then, the decant separation of supernatant, remove part lipid-soluble substance in the vat liquor, with the sequestering agent of giving birth to, the white lime mixture is made tannin etc., step distillation makes the pure product of caffeine then again.
2, method according to claim 1, the alcohol that the lixiviate that it is characterized in that refluxing is adopted is aqueous alcoholic, ethanol is 4-6 with the ratio of water: 1, extraction time is 30-45 minute; Vat liquor is concentrated into the 1/5-1/7 (solution density is the 1.26-1.28 grams per milliliter) of original volume through distillation.
3, method according to claim 1 is characterized in that concentrated solution is put to limit Liang Chu to make it at room temperature to leave standstill cooling, treats that oil-soluble impurities precipitation fully, isolates supernatant liquor with decantation.
4, according to claim 1 or 3 described methods, it is characterized in that in supernatant liquor adding and give birth to the white lime mixture, make the buried body of tannin etc., add-on is the 25%-30% of tealeaves weight, ratio of mixture is 2: 3; Preferably add 2 parts of unslaked limes earlier, and then constantly add 3 parts of white limes, be dehydrated into powdery after stirring.
5, according to claim 1 or 4 described methods, it is characterized in that the meal after the dehydration is put into the distillation jar, under normal pressure or reduced pressure, distil, the decompression sublimation condition is a vacuum tightness 0.1-0.3 normal atmosphere, sublimation temperature is 105 ℃-120 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93108755 CN1032753C (en) | 1993-07-23 | 1993-07-23 | Process for preparing tea natural alkaloid-caffeine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93108755 CN1032753C (en) | 1993-07-23 | 1993-07-23 | Process for preparing tea natural alkaloid-caffeine |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1097757A CN1097757A (en) | 1995-01-25 |
| CN1032753C true CN1032753C (en) | 1996-09-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93108755 Expired - Fee Related CN1032753C (en) | 1993-07-23 | 1993-07-23 | Process for preparing tea natural alkaloid-caffeine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1032753C (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045603C (en) * | 1997-08-19 | 1999-10-13 | 玉溪师范高等专科学校 | Process for extracting caffeine from waste tea dust |
| CN103012402A (en) * | 2012-12-18 | 2013-04-03 | 唐翔 | Method for extracting caffeine from tea |
| CN103891964A (en) * | 2014-04-20 | 2014-07-02 | 张文艳 | Method for massively extracting caffeine from tea |
| CN104250249A (en) * | 2014-09-18 | 2014-12-31 | 卢仁华 | Method for extracting caffeine from tea leaves by concentration and sublimation method |
| CN106046003B (en) * | 2016-05-31 | 2018-07-24 | 合肥师范学院 | A method of from Extraction of Caffeine From Tea |
| CN108752343B (en) * | 2018-08-23 | 2020-11-10 | 江苏天晟药业股份有限公司 | Preparation method of citric acid caffeine |
-
1993
- 1993-07-23 CN CN 93108755 patent/CN1032753C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN1097757A (en) | 1995-01-25 |
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