CN107827900A - A kind of method that Tara seeds pod prepares ellagic acid - Google Patents
A kind of method that Tara seeds pod prepares ellagic acid Download PDFInfo
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- CN107827900A CN107827900A CN201711113651.1A CN201711113651A CN107827900A CN 107827900 A CN107827900 A CN 107827900A CN 201711113651 A CN201711113651 A CN 201711113651A CN 107827900 A CN107827900 A CN 107827900A
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- ellagic acid
- tara seeds
- seeds pod
- tara
- organic solvent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D493/00—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system
- C07D493/02—Heterocyclic compounds containing oxygen atoms as the only ring hetero atoms in the condensed system in which the condensed system contains two hetero rings
- C07D493/06—Peri-condensed systems
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- Organic Chemistry (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention discloses a kind of method that Tara seeds pod prepares ellagic acid, specific steps include：1st, dry Tara seeds pod is crushed with granular mill；2nd, draw particle to obtain extract solution with extract by solvents tower, then reclaim organic solvent, then obtained talas of tannic acid is scattered in deionized water；3rd, toward adding alkali in the talas of tannic acid aqueous solution, while blast air oxidation and obtain ellagic acid crude product, re-refine to obtain the ellagic acid of high-purity.This method can obtain the ellagic acid of high-purity, and the conversion ratio of talas of tannic acid reaches more than 99%, improves its utilization ratio while increasing Tara seeds pod added value, it is possible to achieve industrialized production, effectively reduce to gallic degree of dependence.
Description
Technical field
The present invention relates to a kind of preparation method of ellagic acid, specially a kind of tower draws the method that Fruit pod prepares ellagic acid.
Background technology
Tower is drawn containing about 50% talas of tannic acid in Fruit pod, and it falls within hydrolysable tannins as Chinese tannin, I
Fruit pod is mainly drawn from Peru's import tower by state.Domestic Natural Resources of Gallnuts shortage now, causes cost of material constantly to rise, tower draws Fruit pod
There is necessarily alternative to Chinese gall, while its price is more much lower than Chinese gall, so increasingly by domestic manufacturer
Favor.Ellagic acid is to be widely present in various mushy fruits, nut etc.Plant tissueIn a kind of natural polyphenol component, it shows pair
Chemical substance induces canceration and other a variety of cancerations to have obvious inhibitory action, particularly pairColon cancer, the cancer of the esophagus, liver cancer, lung
Cancer, tongue andSkin neoplasinEtc. there is good inhibiting effect.Its price is 3-4 times of talas of tannic acid price, thus draws Fruit pod with tower
Directly preparing ellagic acid considerably increases its added value, and more preferable economic benefit can be brought to enterprise.European patent
（EP0390107A2）One kind is disclosed using Chinese gall as raw material, is extracted and hydrolyzed with methanol, the tan that content is 50-60% is obtained and spends
Acid, but Chinese gall price is drawn high than tower, and obtained ellagic acid quality is low, poor appearance, it is impossible to be used in food additives.Patent
It is that raw material prepares ellagic acid that CN101434608A, which discloses one kind and draws powder with tower, is first extracted with ethanol, is then carried out with hydrogen peroxide
Hydrolysis and oxidation, but excitant larger diethylamine or triethylamine are used in purifying, considerable influence can be produced to the quality of product,
And hydrogen peroxide is used in hydrolysis and oxidation, there is larger corrosivity.Patent CN101768165 also discloses that a kind of tower draws powder system
The method of standby ellagic acid, extracts talas of tannic acid with water first, then arrives ellagic acid by reaction again.Water consumption be present in this method
It is larger, and be filtration difficulty in extraction tannin, cause extraction efficiency low, waste time and energy.Secondly used in refined ellagic acid
Pyridine with strong toxicity, it is dangerous to add production.Patent CN105175427 discloses prepares tan flower with flower again for raw material
Acid, but due to spending middle tannin acid content low again, therefore this method complex operation, and obtained ellagic acid content is relatively low（58%）.This
Tara seeds pod is prepared into larger particles by method, and this reduces residual of the solvent in waste residue, reduces loss, while also favourable
It is time saving and energy saving in the suction filtration of product.The introducing of ultrasonic extraction also increases while extraction time is shortened simultaneously effectively carries
Take rate.It is beaten simultaneously in product purification using the organic solvent of basic nonhazardous, avoids the actual bodily harm to operator.
The content of the invention
The purpose of the present invention is to be directed to problem above, there is provided a kind of high yield, the Tara seeds pod of low cost prepare ellagic acid
Method.This method can obtain the ellagic acid of high-purity, and the conversion ratio of talas of tannic acid reaches more than 99%, increases Tara seeds pod
Its utilization ratio is improved while added value, it is possible to achieve industrialized production, effectively reduce to gallic dependence journey
Degree.
To realize object above, the technical solution adopted by the present invention is：A kind of method that Tara seeds pod prepares ellagic acid, bag
Include following steps：
1）Crush：Tara seeds pod of the water content in 10-15% is crushed with granular mill, controlled in 20-40 mesh；
2）Extraction：The Tara seeds pod particle of crushing is added in extractor, adds the organic solvent of 1-1.5 times of mass ratio,
40-50oUltrasonic extraction twice, merges extract solution, then extract solution is transferred in oxidation tank, recycling design under C, obtains extracting dense
Contracting thing；
3）Oxidation：The sodium carbonate deionized water solution that mass concentration ratio is 2-4% is added into extraction concentrat, adding quality is
Tower draws 3-5 times of particle, air is then blasted, in 30-40o10-15 hours are reacted under C, then add concentrated sulfuric acid regulation system
PH value 1-3, stirring and crystallizing, centrifugation, obtain ellagic acid crude product；
4）It is refined：Obtained ellagic acid crude product is disperseed to be beaten in organic solvent, centrifuges, obtains high-purity ellagic acid.
Preferably, step（2）In, the organic solvent of addition is methanol.
Preferably, step（3）In, the oxidant of oxidation step is air, and need not separately add other pro-oxidants.
Preferably, step（4）In, the mashing organic solvent of addition is methanol, ethanol or acetone.
Beneficial effects of the present invention：
Tara seeds pod is prepared into larger particles by this method, and this reduces residual of the solvent in waste residue, reduces loss, simultaneously
The suction filtration of product is also beneficial to, it is time saving and energy saving.The introducing of ultrasonic extraction also increases while extraction time is shortened simultaneously
Effective recovery rate.It is beaten simultaneously in product purification using the organic solvent of basic nonhazardous, avoids the body to operator
Body injures.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, below to the specific reality of the present invention
The mode of applying elaborates.Many details are elaborated in the following description in order to fully understand the present invention.But this
Invention can be implemented with being much different from other modes described here, and those skilled in the art can be without prejudice to the present invention
Similar improvement is done in the case of intension, therefore the present invention is not limited to the specific embodiments disclosed below.
A kind of method that Tara seeds pod prepares ellagic acid, comprises the following steps：
1）Crush：Tara seeds pod of the water content in 10-15% is crushed with granular mill, controlled in 20-40 mesh；
2）Extraction：The Tara seeds pod particle of crushing is added in extractor, adds the organic solvent of 1-1.5 times of mass ratio,
40-50oUltrasonic extraction twice, merges extract solution, then extract solution is transferred in oxidation tank, recycling design under C, obtains extracting dense
Contracting thing；
3）Oxidation：The sodium carbonate deionized water solution that mass concentration ratio is 2-4% is added into extraction concentrat, adding quality is
Tower draws 3-5 times of particle, air is then blasted, in 30-40o10-15 hours are reacted under C, then add concentrated sulfuric acid regulation system
PH value 1-3, stirring and crystallizing, centrifugation, obtain ellagic acid crude product；
4）It is refined：Obtained ellagic acid crude product is disperseed to be beaten in organic solvent, centrifuges, obtains high-purity ellagic acid.
Preferably, step（2）In, the organic solvent of addition is methanol.
Preferably, step（3）In, the oxidant of oxidation step is air, and need not separately add other pro-oxidants.
Preferably, step（4）In, the mashing organic solvent of addition is methanol, ethanol or acetone.
Example 1:
Crush：Tara seeds pod of the 200kg water content 12% is taken, particle diameter 20-40 mesh is crushed to granular mill, it is standby
Extraction：The 200kg Tara seeds pods crushed are added in ultrasonic extraction tank, add 260kg industrial methanols, opening is stirred
Mix, reaction system is heated to 40-50oC, ultrasonic extraction 30 minutes, is cooled to room temperature, centrifuge, collect filtrate, filter residue is added and carried
Take in tank, add 200kg industrial methanols, repeat extraction once.Merge filtrate twice, be transferred in oxidation tank, returned in oxidation tank
Receive methanol 420kg.
Oxidation：3% sodium carbonate deionized water solution 1000kg is added into oxidation tank, stirring is opened, blasts air, body
System is warming up to 30-40oC, reacts 12 hours, cooling, with concentrated sulfuric acid regulation system pH value to 2.0, stirring and crystallizing 2 hours, centrifuges,
Obtain ellagic acid crude product.
It is refined：Gained ellagic acid crude product is transferred in treatment tank, adds 200kg95% ethanol, is beaten under 40-50oC
Slurry 3 hours, is cooled to room temperature, centrifuges, recycling design, dries product in 90-100oC obtains vacuum drying chamber, obtain ellagic acid
Fine work 89.5kg, total recovery 86%, product content 99.16%.
Example 2:
Tara seeds pod of the 200kg water content 10% is taken, particle diameter 20-40 mesh is crushed to granular mill, it is standby
Extraction：The 200kg Tara seeds pods crushed are added in ultrasonic extraction tank, add 250kg industrial methanols, opening is stirred
Mix, reaction system is heated to 40-50oC, ultrasonic extraction 30 minutes, is cooled to room temperature, centrifuge, collect filtrate, filter residue is added and carried
Take in tank, add 220kg industrial methanols, repeat extraction once.Merge filtrate twice, be transferred in oxidation tank, returned in oxidation tank
Receive methanol 425kg.
Oxidation：3% sodium carbonate deionized water solution 1200kg is added into oxidation tank, stirring is opened, blasts air, body
System is warming up to 30-40oC, reacts 12 hours, cooling, with concentrated sulfuric acid regulation system pH value to 2.5, stirring and crystallizing 2 hours, centrifuges,
Obtain ellagic acid crude product.
It is refined：Gained ellagic acid crude product is transferred in treatment tank, adds 210kg95% methanol, is beaten under 40-50oC
Slurry 3 hours, is cooled to room temperature, centrifuges, recycling design, dries product in 90-100oC obtains vacuum drying chamber, obtain ellagic acid
Fine work 91.3kg, total recovery 87.8%, product content 99.03%.
Example 3:Crush：Tara seeds pod of the 200kg water content 15% is taken, particle diameter 20-40 is crushed to granular mill
Mesh, it is standby
Extraction：The 200kg Tara seeds pods crushed are added in ultrasonic extraction tank, add 220kg industrial methanols, opening is stirred
Mix, reaction system is heated to 40-50oC, ultrasonic extraction 30 minutes, is cooled to room temperature, centrifuge, collect filtrate, filter residue is added and carried
Take in tank, add 200kg industrial methanols, repeat extraction once.Merge filtrate twice, be transferred in oxidation tank, returned in oxidation tank
Receive methanol 400kg.
Oxidation：3% sodium carbonate deionized water solution 1100kg is added into oxidation tank, stirring is opened, blasts air, body
System is warming up to 30-40oC, reacts 12 hours, cooling, with concentrated sulfuric acid regulation system pH value to 3.0, stirring and crystallizing 2 hours, centrifuges,
Obtain ellagic acid crude product.
It is refined：Gained ellagic acid crude product is transferred in treatment tank, adds 200kg95% acetone, is beaten under 40-50oC
Slurry 3 hours, is cooled to room temperature, centrifuges, recycling design, dries product in 90-100oC obtains vacuum drying chamber, obtain ellagic acid
Fine work 87.6kg, total recovery 85.3%, product content 99.89%.
It should be noted that herein, term " comprising ", "comprising" or its any other variant are intended to non-row
His property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and
And also include the other element being not expressly set out, or also include for this process, method, article or equipment institute inherently
Key element.
Specific case used herein is set forth to the principle and embodiment of the present invention, the explanation of above example
It is only intended to help the method and its core concept for understanding the present invention.Described above is only the preferred embodiment of the present invention, should
When pointing out due to the finiteness of literal expression, and unlimited concrete structure objectively be present, for the common skill of the art
For art personnel, under the premise without departing from the principles of the invention, some improvement, retouching or change can also be made, can also incited somebody to action
Above-mentioned technical characteristic is combined by rights；These improve retouching, change or combination, or the not improved structure by invention
Think and technical scheme directly applies to other occasions, be regarded as protection scope of the present invention.
Claims (4)
1. a kind of method that Tara seeds pod prepares ellagic acid, it is characterised in that comprise the following steps：
Crush：Tara seeds pod of the water content in 10-15% is crushed with granular mill, controlled in 20-40 mesh；
Extraction：The Tara seeds pod particle of crushing is added in extractor, the organic solvent of 1-1.5 times of mass ratio is added, in 40-
50oUltrasonic extraction twice, merges extract solution, then extract solution is transferred in oxidation tank, recycling design under C, obtains extraction concentration
Thing；
Oxidation：The sodium carbonate deionized water solution that mass concentration ratio is 2-4% is added into extraction concentrat, addition quality is tower
Draw particle 3-5 times, then blasts air, in 30-40o10-15 hours are reacted under C, then add concentrated sulfuric acid regulation system pH
Value 1-3, stirring and crystallizing, centrifugation, obtain ellagic acid crude product；
It is refined：Obtained ellagic acid crude product is disperseed to be beaten in organic solvent, centrifuges, obtains high-purity ellagic acid.
2. the method that a kind of Tara seeds pod according to claim 1 prepares ellagic acid, it is characterised in that step（2）In, add
The organic solvent entered is methanol.
3. the method that a kind of Tara seeds pod according to claim 1 prepares ellagic acid, it is characterised in that step（3）In, oxygen
The oxidant for changing step is air, and need not separately add other pro-oxidants.
4. the method that a kind of Tara seeds pod according to claim 1 prepares ellagic acid, it is characterised in that step（4）In, add
The mashing organic solvent entered is methanol, ethanol or acetone.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711113651.1A CN107827900A (en) | 2017-11-13 | 2017-11-13 | A kind of method that Tara seeds pod prepares ellagic acid |
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| CN201711113651.1A CN107827900A (en) | 2017-11-13 | 2017-11-13 | A kind of method that Tara seeds pod prepares ellagic acid |
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| Publication Number | Publication Date |
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| CN107827900A true CN107827900A (en) | 2018-03-23 |
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| CN201711113651.1A Pending CN107827900A (en) | 2017-11-13 | 2017-11-13 | A kind of method that Tara seeds pod prepares ellagic acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229167A (en) * | 2019-05-22 | 2019-09-13 | 珠海萱嘉君行健康产业发展有限公司 | A kind of method, ellagic acid obtained and its application preparing ellagic acid using Chinese gall |
| CN112645961A (en) * | 2020-12-23 | 2021-04-13 | 五峰赤诚生物科技股份有限公司 | Method for preparing ellagic acid by using tara tannin |
| WO2024009260A1 (en) | 2022-07-07 | 2024-01-11 | Universidade De Aveiro | Method for the recovery of ellagic acid from industrial pulp mill streams |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0390107B1 (en) * | 1989-03-29 | 1995-08-02 | Kikkoman Corporation | Process for producing ellagic acid |
| CN101768165A (en) * | 2010-01-13 | 2010-07-07 | 陕西科技大学 | Ellagic acid preparation method employing tara powder |
| CN104817567A (en) * | 2015-04-03 | 2015-08-05 | 宝鸡市虹源生物科技有限公司 | Method for preparing high-purity ellagic acid by using macroporous resin method to purify tannin |
-
2017
- 2017-11-13 CN CN201711113651.1A patent/CN107827900A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0390107B1 (en) * | 1989-03-29 | 1995-08-02 | Kikkoman Corporation | Process for producing ellagic acid |
| CN101768165A (en) * | 2010-01-13 | 2010-07-07 | 陕西科技大学 | Ellagic acid preparation method employing tara powder |
| CN104817567A (en) * | 2015-04-03 | 2015-08-05 | 宝鸡市虹源生物科技有限公司 | Method for preparing high-purity ellagic acid by using macroporous resin method to purify tannin |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110229167A (en) * | 2019-05-22 | 2019-09-13 | 珠海萱嘉君行健康产业发展有限公司 | A kind of method, ellagic acid obtained and its application preparing ellagic acid using Chinese gall |
| CN112645961A (en) * | 2020-12-23 | 2021-04-13 | 五峰赤诚生物科技股份有限公司 | Method for preparing ellagic acid by using tara tannin |
| CN112645961B (en) * | 2020-12-23 | 2023-01-17 | 五峰赤诚生物科技股份有限公司 | Method for preparing ellagic acid by using tara tannin |
| WO2024009260A1 (en) | 2022-07-07 | 2024-01-11 | Universidade De Aveiro | Method for the recovery of ellagic acid from industrial pulp mill streams |
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Application publication date: 20180323 |
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