CN106046003B - A method of from Extraction of Caffeine From Tea - Google Patents

A method of from Extraction of Caffeine From Tea Download PDF

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Publication number
CN106046003B
CN106046003B CN201610394609.0A CN201610394609A CN106046003B CN 106046003 B CN106046003 B CN 106046003B CN 201610394609 A CN201610394609 A CN 201610394609A CN 106046003 B CN106046003 B CN 106046003B
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caffeine
solution
extraction
tea
boiling condition
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CN106046003A (en
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王方阔
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SINOPHARM BIOTECHNOLOGY (HUANGSHAN) Co.,Ltd.
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Hefei Normal University
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D473/00Heterocyclic compounds containing purine ring systems
    • C07D473/02Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6
    • C07D473/04Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms
    • C07D473/06Heterocyclic 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
    • C07D473/12Heterocyclic 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

Abstract

The invention discloses a kind of methods from Extraction of Caffeine From Tea, include the following steps:Mixing in solution A is added in tealeaves, is heated to slight boiling condition, 15 30min of slight boiling condition is kept, filtrate is obtained by filtration;By concentrating filter liquor, roast, distilling obtains caffeine, wherein solution A is one kind in alkaline aqueous solution or inorganic salt solution.The present invention is at low cost, be avoided that roast and sublimation process in generate due to there are problems that for organic solvent carbonization or burn, extraction time can be greatly shortened, improve extraction efficiency, and easy to operate, high income, caffeine it is high-quality.

Description

A method of from Extraction of Caffeine From Tea
Technical field
The present invention relates to Carbonado Diamond technical field more particularly to a kind of methods from Extraction of Caffeine From Tea.
Background technology
Caffeine is also known as caffeine, and its chemical name is 1,3,7- trimethyl -3,7- dihydro -1H- purine -2,6- diketone water Close object, chemical formula C8H10N4O2, relative molecular weight 194.2, soluble easily in water, ether, chloroform, dichloromethane, for white knot Crystalline flour end, odorless, bitter.Caffeine is a kind of xanthine alkaloid compound, is a kind of central nervous excitation agent, can be temporary Drive away sleepiness and regain one's vigor.There are coffee, tea, soft drink and the energy drink of caffeine ingredient in very great demand, therefore, coffee Because being also the psychotropic substances being most commonly used in the world.Contain alkaloid in tealeaves, alkaloid includes mainly caffeine, can Theobromine and theophylline, wherein caffeine account for major part, and content 3-5% is the important sources of medical caffeine.Usually from tealeaves Extraction obtains caffeine.
Currently, the method for extracting caffeine has:Solvent extraction method, supercritical CO2Extraction method, adsorbent and eluant, eluent extract Method, wherein solvent extraction method is most common method.Solvent extraction method is mainly extracted by using organic solvent such as ethyl alcohol, And combine Soxhlet extraction device to carry out the repeatedly extracting of continuous cycle, by concentrate, roast, distilling obtains caffeine.But solvent Extraction method selects the organic solvents such as ethyl alcohol to do Extraction solvent, and the rate of recovery is relatively low, and cost is higher;Roast and sublimation process in by Product is set to be easy carbonization or burn in the presence of the organic solvents such as ethyl alcohol;Continuous cycle extracting is carried out using Soxhlet extraction device When, elapsed time is longer.
Invention content
Basic background technology, the present invention propose a kind of method from Extraction of Caffeine From Tea, The present invention is at low cost, be avoided that roast and sublimation process in generate due to the presence of organic solvent carbonization or what is burnt ask Topic, can greatly shorten extraction time, improve extraction efficiency, and easy to operate, high income, caffeine it is high-quality.
A kind of method from Extraction of Caffeine From Tea proposed by the present invention, includes the following steps:Solution A is added in tealeaves Middle mixing is heated to slight boiling condition, keeps slight boiling condition 15-30min, filtrate is obtained by filtration;By concentrating filter liquor, roasts, rises China obtains caffeine, wherein solution A is one kind in alkaline aqueous solution or inorganic salt solution.
Preferably, the bulking value (g/ml) of tealeaves and solution A is than being 1:6-10.
Preferably, the weight fraction of solute is 3-4wt% in solution A.
Preferably, solution A be calcium hydroxide aqueous solution, aqueous sodium carbonate, sodium-chloride water solution, magnesium chloride brine or One kind in calcium chloride water.
Preferably, tealeaves is crushed, mixing in solution A is added after grinding, be heated to slight boiling condition, keep slight boiling condition Filtrate is obtained by filtration in 15-30min;Filtrate is concentrated to give concentrate;Calcium oxide mixing is added into concentrate, roasts to obtain Dried powder;Dried powder is taken to handle to obtain caffeine through distillation, wherein solution A is alkaline aqueous solution or inorganic salt solution In one kind.
Preferably, the bulking value (g/ml) of calcium oxide and concentrate is than being 1:3-5.
Preferably, it takes dried powder to be warming up to 120 DEG C or more, handles to obtain caffeine through distillation.
Above-mentioned water is purified water.
The present invention selects water cheap and easy to get to replace organic solvent, can reduce cost, and be avoided that and roasting and rising Carbonization is generated during China due to there are problems that for organic solvent or is burnt;Using directly heating cooperation inorganic salt solution Or the extracting method of alkaline aqueous solution can greatly shorten extraction time compared to conventional solvent Soxhlet extraction, improve extraction effect Rate, and it is easy to operate, equipment is convenient, is suitble to industrialized production;Select inorganic salt solution or alkaline aqueous solution to tealeaves into Row extraction, can be obviously shortened extraction time, improve yield, and can improve the quality of product caffeine.
Specific implementation mode
In the following, technical scheme of the present invention is described in detail by specific embodiment.
Embodiment 1
A method of from Extraction of Caffeine From Tea, include the following steps:Mixing in alkaline aqueous solution is added in tealeaves, It is heated to slight boiling condition, slight boiling condition 20min is kept, filtrate is obtained by filtration;By concentrating filter liquor, roast, distilling obtains coffee Cause.
Embodiment 2
A method of from Extraction of Caffeine From Tea, include the following steps:Tealeaves is added in inorganic salt solution and is mixed It is even, it is heated to slight boiling condition, slight boiling condition 15min is kept, filtrate is obtained by filtration;By concentrating filter liquor, roast, distilling obtains coffee Coffee because.
Embodiment 3
A method of from Extraction of Caffeine From Tea, include the following steps:It is 3wt% chlorine that weight fraction, which is added, in tealeaves Change mixing in calcium aqueous solution, be heated to slight boiling condition, keeps slight boiling condition 30min, filtrate is obtained by filtration;By concentrating filter liquor, It roasts, distilling obtains caffeine, wherein the bulking value (g/ml) of tealeaves and calcium chloride water is than being 1:6.Caffeine it is pure Degree is 99.1%, yield 2.16%.
Embodiment 4
A method of from Extraction of Caffeine From Tea, include the following steps:It is 4wt% chlorine that weight fraction, which is added, in tealeaves Change mixing in magnesium aqueous solution, be heated to slight boiling condition, keeps slight boiling condition 20min, filtrate is obtained by filtration;By concentrating filter liquor, It roasts, distilling obtains caffeine, wherein the bulking value (g/ml) of tealeaves and magnesium chloride brine is than being 1:10.Caffeine Purity is 99.0%, yield 2.05%.
Embodiment 5
A method of from Extraction of Caffeine From Tea, include the following steps:Tealeaves is crushed, weight point is added after grinding Number is mixing in 3.5wt% sodium-chloride water solutions, is heated to slight boiling condition, keeps slight boiling condition 25min, filtrate is obtained by filtration; Filtrate is concentrated to give concentrate;Calcium oxide mixing is added into concentrate, roasts to obtain dried powder;Dried powder is taken to heat up It to 120 DEG C or more, handles to obtain caffeine through distillation, wherein bulking value (g/ml) ratio of tealeaves and sodium-chloride water solution is 1:7, the bulking value (g/ml) of calcium oxide and concentrate is than being 1:5.The purity of caffeine is 99.3%, yield 1.93%.
Embodiment 6
A method of from Extraction of Caffeine From Tea, include the following steps:Tealeaves is crushed, weight point is added after grinding Number is mixing in 3.8wt% aqueous sodium carbonates, is heated to slight boiling condition, keeps slight boiling condition 20min, filtrate is obtained by filtration; Filtrate is concentrated to give concentrate;Calcium oxide mixing is added into concentrate, roasts to obtain dried powder;Dried powder is taken to heat up It to 120 DEG C or more, handles to obtain caffeine through distillation, wherein bulking value (g/ml) ratio of tealeaves and aqueous sodium carbonate is 1:9, the bulking value (g/ml) of calcium oxide and concentrate is than being 1:3.The purity of caffeine is 99.1%, yield 2.57%.
Embodiment 7
A method of from Extraction of Caffeine From Tea, include the following steps:Tealeaves is crushed, weight point is added after grinding Number is mixing in 3.2wt% calcium hydroxide aqueous solutions, is heated to slight boiling condition, keeps slight boiling condition 15min, filter is obtained by filtration Liquid;Filtrate is concentrated to give concentrate;Calcium oxide mixing is added into concentrate, roasts to obtain dried powder;Take dried powder 120 DEG C or more are warming up to, handles to obtain caffeine through distillation, wherein the bulking value (g/ of tealeaves and calcium hydroxide aqueous solution Ml) than being 1:6, the bulking value (g/ml) of calcium oxide and concentrate is than being 1:4.The purity of caffeine is 99.4%, and yield is 3.60%.
Test example 1
Compare 1 group:Make calcium hydroxide aqueous solution into purified water, other modes of operation are the same as embodiment 7.
Compare 2 groups:Make calcium hydroxide aqueous solution into tap water, other modes of operation are the same as embodiment 7.
Compare 3 groups:Take tealeaves according to solvent extraction method extracting caffeine.
Detect embodiment 7,1 group of control, 2 groups of control, 3 groups of caffeine purity extracted of control and calculated yield, knot Fruit such as following table:
Group Yield % Caffeine purity %
Embodiment 7 3.60 99.4
Compare 1 group 0 ---
Compare 2 groups 0.5 98.3
Compare 3 groups 1.48 97.9
As can be seen from the above table, individual purified water extraction is less than caffeine;Simple tap water can only extract on a small quantity Caffeine, yield are too low;The caffeine purity that solvent extraction method obtains is relatively low, and yield is also far below the present invention;The present invention extracts Obtained caffeine is high-quality, high income.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, Any one skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (4)

1. a kind of method from Extraction of Caffeine From Tea, which is characterized in that include the following steps:Tealeaves is added in solution A Mixing is heated to slight boiling condition, keeps slight boiling condition 15-25min, filtrate is obtained by filtration;Filtrate is concentrated to give concentrate;To Calcium oxide mixing is added in concentrate, roasts, distilling obtains caffeine, wherein solution A is calcium hydroxide aqueous solution, sodium carbonate One kind in aqueous solution, sodium-chloride water solution, magnesium chloride brine or calcium chloride water;
The weight fraction of solute is 3-4wt% in solution A;
Tealeaves and the w/v of solution A are 1g:6-10ml.
2. according to claim 1 from the method for Extraction of Caffeine From Tea, which is characterized in that crush tealeaves, after grinding Mixing in solution A is added, is heated to slight boiling condition, keeps slight boiling condition 15-25min, filtrate is obtained by filtration;Filtrate is concentrated to give To concentrate;Calcium oxide mixing is added into concentrate, roasts to obtain dried powder;Dried powder is taken to handle to obtain coffee through distillation Coffee because.
3. according to claim 2 from the method for Extraction of Caffeine From Tea, which is characterized in that the weight of calcium oxide and concentrate Amount volume ratio is 1g:3-5ml.
4. according to claim 2 from the method for Extraction of Caffeine From Tea, which is characterized in that dried powder is taken to be warming up to It 120 DEG C or more, handles to obtain caffeine through distillation.
CN201610394609.0A 2016-05-31 2016-05-31 A method of from Extraction of Caffeine From Tea Active CN106046003B (en)

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CN109699662A (en) * 2019-02-26 2019-05-03 廊坊市维金农业科技有限公司 A kind of preparation method of the disease-resistant preparation of the plant anthelmintic containing caffeine
CN110859234A (en) * 2019-11-29 2020-03-06 湖北工业大学 High GABA low caffeine black tea dissolved bean and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1051481A (en) * 1989-11-09 1991-05-22 石天齐 From tealeaves, extract production method of natural caffeine
CN1097757A (en) * 1993-07-23 1995-01-25 煤炭科学研究总院合肥研究所 Process for preparing tea natural alkaloid-caffeine
CN102453031A (en) * 2010-10-20 2012-05-16 曾科 Method for extracting caffeine from tea leaf

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1051481A (en) * 1989-11-09 1991-05-22 石天齐 From tealeaves, extract production method of natural caffeine
CN1097757A (en) * 1993-07-23 1995-01-25 煤炭科学研究总院合肥研究所 Process for preparing tea natural alkaloid-caffeine
CN102453031A (en) * 2010-10-20 2012-05-16 曾科 Method for extracting caffeine from tea leaf

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Address after: 242700 No.59, Meilin Avenue, Huangshan Economic Development Zone, Huangshan City, Anhui Province

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Patentee before: HEFEI NORMAL University