CN1219734C - Method for preparing compound phenolhydrocarbon sodium - Google Patents
Method for preparing compound phenolhydrocarbon sodium Download PDFInfo
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- CN1219734C CN1219734C CNB031245706A CN03124570A CN1219734C CN 1219734 C CN1219734 C CN 1219734C CN B031245706 A CNB031245706 A CN B031245706A CN 03124570 A CN03124570 A CN 03124570A CN 1219734 C CN1219734 C CN 1219734C
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a deep-processing method for Chinese herbal medicine, particularly to a method for producing and preparing compound phenolhydrocarbon sodium. Compound phenolhydrocarbon sodium is a compound extracted from whole herb of origanum and haichow elsholtzia herb of labiate of herbaceous plants. Compound phenolhydrocarbon sodium mainly contains active components, such as thymol, oxyzymol, p-polycymene, etc. and is named. The present invention separates active components from raw materials by a supercritical carbon dioxide extraction method, active components extracted in supercutical fluid are separated from a separator by a pressure reduction method or a temperature rise method, and appointed active components are obtained. The present invention carries out vapour separation, concentration and extraction by a hot reflux extraction device, the active components of supercritical carbon dioxide extraction are added in water soluble substances and are stirred evenly with insoluble lipoid substances after the water soluble substances extracted by the present invention are sprayed and dried, and compound products of compound phenolhydrocarbon sodium with different contents are obtained. The yield is improved to 0.55% from 0.13% of an original distillation method.
Description
Technical field
The present invention relates to the deep processing of herbal medicine, refer in particular to a kind of preparation method of compound Fentingna
Background technology
Compound Fentingna is by a kind of compound that extracts in herbaceous plant labiate Origanum and the Elsholtzia herb.Mainly contain effective constituents such as thymol, isothymol and p-cymene hydrocarbon and name.Compound Fentingna has antisepsis and anti-inflammation, anti-oxidant, aid digestion, clear heat, diuresis, dries, quenches one's thirst, antipruritic, antiviral, the health care effect of waiting for a long time.Range of application: industries such as medicine, food, tea-drinking, healthcare products, air freshener, makeup, washing composition, fodder additives.Originally distillating method extracts effective ingredients such as volatility, and it is extremely low that this method is not only extracted, and only is 0.13%, and extraction cost high price costliness, the more important thing is influences quality product, through repeatedly experiment showed, distillation method following unfavorable factor and shortcoming is arranged:
1. the topmost factor of composition output and quality that influences is a degree of heat.See that theoretically it is big more to add heat, the quantity of steam of generation is many more, and extraction rate is fast more.But the condensation ability of necessary consideration equipment in the production, if the vapour amount is big more, the condensation scarce capacity then causes extract to scatter and disappear and emulsification.With regard to working equipment, jacket steam pressure the condensation scarce capacity then occurs greater than more than the 0.1mpa, and it is overheated to distill, and the volatilization of volatilization composition is scattered and disappeared and emulsification, is difficult in process of production grasp.
2. another principal element of influence extraction volatile oil is the fineness degree of medicinal material.Medicinal material is thin more, and the speed of then extracting volatile component is fast more.This is because medicinal material is cut carefully more, and cell tissue and phenol glandular cell destroy many more, and contained effective ingredient can directly contact with steam and vaporize, thereby has accelerated the speed of extracting, and scatters and disappears also soon and many simultaneously.And medicine is too thin, and the soup after the extraction need flow into next procedure, makes soup be difficult to filter.
3. how much amount of water also is one of factor of influence extraction.Amount of water very little because chuck heating, extraction time is longer, distillate is more, extract certain hour after, a water yield seldom easily causes and distills out saturated aqua aromatica or the emulsive phenomenon appears in volatile component in jar; Amount of water is too many, and the volatilization composition that steams needs through more water, has partly water-soluble phenomenon to occur, and extract also reduces relatively, thereby the extraction of compound Fentingna compound is difficult to reach requirement.
4. be heated to when extracting boil before, adopt the open steam heating.Can accelerate the speed of boiling like this, when nearly being heated to boiling (80 ℃-90 ℃), the chuck of promptly migrating heating if continue to adopt the open steam heating, then can steam saturated aqua aromatica and can not get phenolic compound.If over-heating then easily makes jar soup of the interior dregs of a decoction rush to pipeline, pollute distillate, giving to extract has increased by a big difficulty again.
These unfavorable factors have caused the difficulty of the extraction of the effective ingredient that Labiatae Origanum and elscholtiza belong to.
Summary of the invention
The objective of the invention is to be improved at shortcoming that exists in the background technology and problem, provide a kind of employing supercritical carbon dioxide extraction equipment to extract Labiatae Origanum or elscholtiza genus phenolic compound and effective ingredient, and it is safe and reliable, nontoxic, be extracted material and can not change its activity, be called as the preparation method of a kind of compound Fentingna of green bio extractive technique.
Technical scheme of the present invention is:
A a, the cauline leaf of getting wild marjoram or elscholtiza are crushed to 40 orders after drying, and raw material is packed into to reinstall to extract in the still behind the cloth bag add a cover sealing;
B, carbonic acid gas is connected in the raw material still, opens carbonic acid gas, raw material still temperature transfers to 37-40 ℃, pressure 13mpa-14mpa, the extraction time is 3.5-4.5 hour, insoluble lipid effective ingredient extract;
B a, the raw material slag after will extracting are put into the thermal backflow still, heat to 70-90 ℃ after being incorporated in the solvent of 2 times of raw materials again, pressure 1-1.5mpa, with separated in 5.5-6.5 hour, centrifuging, after concentrating water-soluble paste;
B, water-soluble paste put into drying plant carry out spraying drying, coffee-like powder;
C stirs the water-soluble powder of separating in the raw material slag in the insoluble lipid effective ingredient extract of supercritical carbon dioxide extraction in the A step and the B step at last, promptly gets the compound Fentingna compound products of different content.
The present invention has following technical characterstic and advantage:
1, any gas all has one " stagnation point ", and gas is pairing temperature and pressure in stagnation point, is called " critical temperature " and " emergent pressure ".When the temperature and pressure of gas is higher than its critical temperature and emergent pressure, claim that then this gas is supercutical fluid.This moment, this fluidic density approached density of liquid, and its viscosity and spread coefficient are then close with common gases, and the break bounds fluid that faces of special property generally all has extremely strong dissolving power.Utilize this principle, select for use and be not easy to react with other material, the carbon dioxide nontoxic to human body contacts with natural matter under specific criticality, relevant natural component will be dissolved among the supercritical carbon dioxide fluid, reached separating of effective ingredient and raw material, during Labiatae Origanum and elscholtiza belong to except aromatic series effective constituent, the lipoid substance that also contains a great deal of, acetic acid ox ester, this Ester viscosity height, be difficult to water-soluble, have only the supercritical carbon dioxide method for extracting of employing just can reach effective ingredient and separate, by the method for decompression or intensification, the effective ingredient that extracts in the supercutical fluid is separated in separator then with raw material, promptly obtain specified effective ingredient, Here it is adopts the simple procedure of supercritical carbon dioxide extraction.But in adopting supercritical carbon dioxide extraction, because solubility with temperature and the pressure change of various materials in supercritical co, so before extraction, will determine the target composition, and it is relative maximum to calculate and design its solubleness according to the physicals of target composition, but not the supercritical pressure and the temperature of effective ingredient and relative solubility minimum, the highest to guarantee the effective ingredient in the extract, invalid element is minimum.
2, supercritical carbon dioxide extraction apparatus can only be used for volatile aromatic series extraction, to with the raw material behind the supercritical carbon dioxide extraction, carry out the vapor removal concentration extraction with heat reflux extraction equipment, after its extraction water-soluble substances carries out spraying drying, stir with insoluble lipoid substance in the effective ingredient adding water-soluble substances with supercritical carbon dioxide extraction again, promptly get the compound Fentingna compound products of different content, output brings up to 0.55% from 0.13% of original distillation method.
Embodiment
Embodiment one
1, extracts ground wild marjoram or elscholtiza cauline leaf and partly be put in the basket, be bundled into the horizontal sky of wisp again and sling and dry or air-dry, raw material such as the color and luster in vegetative period and quality after air-dry; Again raw material is processed into powder to 40 order, selects the wild marjoram or the Chinese Mosla Herb 50kg that process for use, raw material is packed into to reinstall behind the cloth bag to extract in the still add a cover sealing.
2, carbonic acid gas is filled in the still, and open carbonic acid gas still temperature and transfer to 37 ℃, pressure 13mpa, the extraction time is 3.5 hours, promptly drives still and gets thing, the insoluble lipid effective ingredient that will extract behind the drainage of the rising again bottle of packing into is interior stand-by.
3, the raw material slag after the extraction is put into the thermal backflow still, be incorporated in the water of 2 times of raw materials again after, heat to 70 ℃, pressure 1mpa separated with 5.5 hours, centrifuging must water-soluble paste after concentrating.
4, water-soluble paste is put into drying plant and carry out spraying drying, get coffee-like powder.
5, at last the water-soluble powder of separating in the insoluble lipid effective ingredient extract of supercritical carbon dioxide extraction and the raw material slag is stirred, promptly get the compound Fentingna compound products of different content.
Embodiment two
1, extracts ground wild marjoram cauline leaf and partly be put in the basket, be bundled into the horizontal sky of wisp again and sling and dry or air-dry, raw material such as the color and luster in vegetative period and quality after air-dry; Again raw material is processed into powder to 40 order, selects the wild marjoram or the Chinese Mosla Herb 50kg that process for use, raw material is packed into to reinstall behind the cloth bag to extract in the still add a cover sealing.
2, carbonic acid gas is filled in the still, and open carbonic acid gas still temperature and transfer to 38 ℃, pressure 13.5mpa, the extraction time is 4 hours, promptly drives still and gets thing, the insoluble lipid effective ingredient that will extract behind the drainage of the rising again bottle of packing into is interior stand-by.
3, the raw material slag after the extraction is put into the thermal backflow still, be incorporated in the alcohol of 2 times of raw materials again after, heat to 80 ℃, pressure 1.25mpa separated with 5 hours, centrifuging must water-soluble paste after concentrating.
4, water-soluble paste is put into drying plant and carry out spraying drying, get coffee-like powder.
5, at last the water-soluble powder of separating in the insoluble lipid effective ingredient extract of supercritical carbon dioxide extraction and the raw material slag is stirred, promptly get the compound Fentingna compound products of different content.
Embodiment three
1, extracts ground wild marjoram cauline leaf and partly be put in the basket, be bundled into the horizontal sky of wisp again and sling and dry or air-dry, raw material such as the color and luster in vegetative period and quality after air-dry; Again raw material is processed into powder to 40 order, selects the wild marjoram powder 50kg that processes for use, raw material is packed into to reinstall behind the cloth bag to extract in the still add a cover sealing.
2, carbonic acid gas is filled in the still, and open carbonic acid gas still temperature and transfer to 40 ℃, pressure 14mpa, the extraction time is 4.5 hours, promptly drives still and gets thing, the insoluble lipid effective ingredient that will extract behind the drainage of the rising again bottle of packing into is interior stand-by.
3, the raw material slag after the extraction is put into the thermal backflow still, be incorporated in the water of 2 times of raw materials again after, heat to 90 ℃, pressure 1.5mpa separated with 6.5 hours, centrifuging must water-soluble paste after concentrating.
4, water-soluble paste is put into drying plant and carry out spraying drying, get coffee-like powder.
5, at last the water-soluble powder of separating in the insoluble lipid effective ingredient extract of supercritical carbon dioxide extraction and the raw material slag is stirred, promptly get the compound Fentingna compound products of different content.
Claims (2)
1, a kind of preparation method of compound Fentingna is characterized in that:
A a, the cauline leaf of getting wild marjoram or elscholtiza are crushed to 40 orders after drying, and raw material is packed into to reinstall to extract in the still behind the cloth bag add a cover sealing;
B, carbonic acid gas is connected in the raw material still, opens carbonic acid gas, raw material still temperature transfers to 37-40 ℃, pressure 13mpa-14mpa, the extraction time is 3.5-4.5 hour, insoluble lipid effective ingredient extract;
B a, the raw material slag after will extracting are put into the thermal backflow still, heat to 70-90 ℃ after being incorporated in the solvent of 2 times of raw materials again, pressure 1-1.5mpa, with separated in 5.5-6.5 hour, centrifuging, after concentrating water-soluble paste;
B, water-soluble paste put into drying plant carry out spraying drying, coffee-like powder;
C stirs the water-soluble powder of separating in the raw material slag in the insoluble lipid effective ingredient extract of supercritical carbon dioxide extraction in the A step and the B step at last, promptly gets the compound Fentingna compound products of different content.
2, the preparation method of a kind of compound Fentingna according to claim 1 is characterized in that described solvent comprises water or alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031245706A CN1219734C (en) | 2003-06-17 | 2003-06-17 | Method for preparing compound phenolhydrocarbon sodium |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031245706A CN1219734C (en) | 2003-06-17 | 2003-06-17 | Method for preparing compound phenolhydrocarbon sodium |
Publications (2)
| Publication Number | Publication Date |
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| CN1462733A CN1462733A (en) | 2003-12-24 |
| CN1219734C true CN1219734C (en) | 2005-09-21 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB031245706A Expired - Fee Related CN1219734C (en) | 2003-06-17 | 2003-06-17 | Method for preparing compound phenolhydrocarbon sodium |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109419846B (en) * | 2017-08-31 | 2021-07-16 | 安徽天康(集团)股份有限公司 | Application of herba Moslae volatile oil in treating norovirus infectious diarrhea |
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- 2003-06-17 CN CNB031245706A patent/CN1219734C/en not_active Expired - Fee Related
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