CN102527084A - Method for extracting useful components from high-water-content plant raw materials - Google Patents
Method for extracting useful components from high-water-content plant raw materials Download PDFInfo
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- CN102527084A CN102527084A CN201210014448XA CN201210014448A CN102527084A CN 102527084 A CN102527084 A CN 102527084A CN 201210014448X A CN201210014448X A CN 201210014448XA CN 201210014448 A CN201210014448 A CN 201210014448A CN 102527084 A CN102527084 A CN 102527084A
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Abstract
The invention discloses a process for sub-critically extracting useful components from high-water-content plant raw materials. In the process, liquefied methyl ether is taken as a solvent, useful components in high-water-content plant raw materials can be extracted at the normal temperature, a process for drying, airing or manual drying plant raw materials is eliminated, partial loss of useful components of the plants in a raw material drying process is avoided, and heat-sensitive and photosensitive components in plants are particularly prevented from being damaged by decomposing. The process plays a certain role in dehydrating during extraction of useful components from plants, and has contribution to the post-treatment of plant residues. A method disclosed by the invention can be used for extracting various effective components such as plant pigments, alkaloids, plant general glycosides and the like, and is particularly suitable for extracting processing of capsochrome, marigold phytoxanthin, nicotiana alkaloids, ginseng general glycosides and the like.
Description
Technical field
The present invention relates to utilize and possess certain absorptive organic solvent; Useful component to high aqueous plant raw material carries out method of extraction; Partly remove the moisture in the raw material, make the material after the extraction present drying regime, help discharging in the technology depositing and utilizing again of plant slag.
Background technology
Contain the various compositions useful in the root of plant, stem, the leaf,, generally all will it dried, dry or artificial drying, remove wherein and extract again after the most of moisture in order to extract these compositions to the mankind.This traditional method not only long, time-consuming, the part material of operation is lost because of going rotten; And the useful component in the plant has a certain proportion of loss in the process of drying; Especially many plant components are thermal sensitivity or light sensitivity, and destruction very easily is decomposed.The inventive method is intended to the plant material with wet of aquatic foods is carried out solvent extraction, obtains useful component wherein.It is a lot of to have certain absorptive solvent, like high concentration ethanol, low aqueous glycerol, liquid methyl ether, liquefied ammonia etc.
Summary of the invention
The object of the present invention is to provide the extracting process of useful component in a kind of high aqueous plant raw material.
The extracting process of useful component in the high aqueous plant raw material, the extract that height is contained moisture is inserted in the airtight extraction container, and container is vacuumized; Inject extractant and flood extract, carry out counter-current extraction, extracting pressure is the saturated vapour pressure of extractant under the corresponding extraction temperature; After extraction finished, with solid phase that is extracted and the liquid phase separation that extracts, the extract in the liquid phase separated with extractant; And remove solvent composition remaining in the extract, obtain thick extract; Remove solvent composition remaining in the solid phase, obtain plant residue; All separation and the solvent recovery cycle that removes are used; Wherein extraction container being vacuumized, the control container inner pressure be-0.02Mpa～-0.09Mpa, preferably-0.08Mpa, extractant is liquid methyl ether, liquefied ammonia etc., and extraction times is 4～8 times, and extraction temperature is-20 ℃～50 ℃, preferred 20～35 ℃; Total extraction time is 60～240 minutes, preferred 90～200 minutes; Extracting pressure is 0.2 Mpa～1.2Mpa, preferred 0.6Mpa～0.9Mpa.
Use method of the present invention to can be used to extract bright height and contain various material compositions such as phytochrome in the moisture plant material, alkaloid, plant general glycoside with wet; Extraction and precipitation overall process can be carried out at normal temperatures or under the low temperature; Be extracted material and need do not pass through pyroprocess, the separation that the thermal sensitivity composition is able to guarantee the quality.
The specific embodiment
Specify below and realize method step of the present invention and implementation:
The plant material that height is moisture carries out preliminary treatment: clean, remove nonuseable part, shred or grind.Its objective is that the micro-structural that makes plant destroys, help solvent-extracted carrying out, that pretreated raw material demonstrates is thread, powder or pulpous state; For use.
(1) method step:
1, charging: material that will be to be extracted is sent in the extraction container of construction of pressure vessel; Charge is not more than 60% of extractor volume, and container is vacuumized, and extracts air wherein out; Usually container inner pressure should reduce to-0.02Mpa～-0.09Mpa, optimum pressure is-0.08Mpa.
2, extraction: in extraction container, inject liquefaction methyl ether extractant and flood extract, carry out counter-current extraction.Solvent load is advisable with the submergence material; In immersion process, can also make material and solvent generation relative displacement with the method for machinery, the method or the ultrasonic method of device pucking gas; To improve extraction efficiency, extraction process is a known adverse current method in the industry, and extraction times is 4～8 times.Different with its existence in material according to needing the content of extraction component in the material, the time of extraction always is 60～240 minutes, preferred 90～200 minutes.The extraction temperature scope is-20 ℃～50 ℃, preferred 20～35 ℃.Extracting pressure is the saturated vapour pressure of liquefaction methyl ether under the corresponding extraction temperature; When non-methyl ether gas such as residual air is arranged in the extractor; Extracting pressure can consider from safety a little more than the saturated vapour pressure of solvent under the extraction temperature, and extracting pressure is advisable not to be higher than 1.1 times of liquefaction methyl ether saturated vapour pressure; Actual extraction container pressure is generally at 0.5Mpa～1.2Mpa, preferred 0.6Mpa～0.9Mpa.
3, material precipitation: when reaching the extraction yield technological requirement of setting; After extracting the liquid flux in the extractor out, open the air bleeding valve of extractor, make the residual solvent gasification and the feed separation of adsorbing in the material; Discharge extractor; In this precipitation process, in order to improve the efficient of precipitation, be in container additional heat to keep the rapid evaporation of solvent.After precipitation was accomplished, the material after being extracted can be discharged extractor, and extractor can get into next production cycle.Temperature of charge can change between methyl ether boiling point-24.9 is ℃ to 50 ℃ during precipitation, in order to raise the efficiency, will be in container in the precipitation process additional heat, the solvent removal effect is better when keeping temperature of charge and being not less than 0 ℃; Along with deviating from and decrease of temperature of solvent, extractor pressure 1.2Mpa～-constantly reduce between the 0.08Mpa, for the solvent in the recovered material as much as possible, when precipitation finishes the pressure of extractor with-be advisable below the 0.08Mpa.
4, extract evaporation: material is carried out the extract of counter-current extraction gained, get into vapo(u)rization system,, solvent is separated with extract, promptly obtain the extract product through continuous or pot type evaporation intermittently; The extract evaporating temperature is controlled in 0 ℃～50 ℃ scopes; Evaporating pressure is controlled at 0.5 Mpa～1.2Mpa; After most of solvent is evaporated; Carry out vacuum evaporation again to reclaim the solvent in the extract as far as possible, the vacuum evaporation temperature is controlled in 0 ℃～50 ℃ scopes, and pressure is controlled at-below the 0.08Mpa.
5, solvent recovery: from material and in the extract, evaporate the solvent gas that, through compressor compresses liquefaction, liquid solvent flows back to the solvent circulating tank, recycles.From material and in the extract, evaporate the solvent gas that, use compressor compresses liquefaction, compression pressure is between 0.5Mpa～1.2Mpa, and condensing temperature is between 10 ℃～40 ℃.
(2), implementation
Further specify method of the present invention with some specific embodiments below:
Embodiment 1: the extraction of bright capsochrome: bright capsicum is got 3000 ㎏ after removing seed and grinding, send in the extractor of construction of pressure vessel; After closing feeding-passage; The device internal pressure is reduced to-0.08Mpa, squeeze into liquefaction methyl ether extractant and carry out counter-current extraction 8 times, the extraction time is 150～200 minutes; Extraction temperature is 20 ℃～35 ℃, extracting pressure 0.6 Mpa～0.9Mpa; Constantly carry out mechanical agitation in the extraction process to improve extraction efficiency.The extract of extraction gained gets into vapo(u)rization system, and the solvent gasification is separated with extract, and promptly obtaining with capsicum red pigment and capsaicine is the thick product of plant extraction of many water of useful component.Extraction pumps extract in the extractor after accomplishing, and opens the air outlet valve of extractor, makes the solvent gasification and the feed separation of adsorbing in the material in the extractor, discharges extractor.In material precipitation process will to the material in additional heat to keep the rapid evaporation of solvent.After precipitation was accomplished, the capsicum residue after being extracted can be discharged extractor, and extractor can get into next production cycle.From material and in the extract, evaporate the solvent gas that, through compressor compresses liquefaction, liquid solvent flows back to the solvent circulating tank, recycles.
Embodiment 2: the extraction of aztec marigold leaf flavine: through the marigold flower of broken wall treatment, pulverize after draining surface moisture, get 3000 ㎏, send in the extractor of construction of pressure vessel, close feeding-passage after, the device internal pressure is reduced to-0.08Mpa.Squeeze into liquefaction methyl ether extractant and carry out counter-current extraction 6 times, the extraction time is 120～160 minutes, 20 ℃～35 ℃ of extraction temperature, extracting pressure 0.6Mpa～0.9Mpa.The extract of extraction gained gets into vapo(u)rization system, and the solvent gasification is separated with extract, and promptly obtaining with the aztec marigold leaf flavine is the plant extract product of many water of useful component.Extraction removes the solvent in the material by the condition among the embodiment 1 after accomplishing, and from extractor, discharges the marigold residue, reclaims solvent and recycles.
Embodiment 3: the extraction of plant alkaloid: the new fresh tobacco leaf after the harvesting is got 3000 ㎏ after crushed, sends in the extractor of construction of pressure vessel, close feeding-passage after, the device internal pressure is reduced to-0.08Mpa.Squeeze into liquefaction methyl ether extractant and carry out counter-current extraction 4 times, the extraction time is 100～150 minutes, 20 ℃～35 ℃ of extraction temperature, extracting pressure 0.6Mpa～0.9Mpa.The extract of extraction gained gets into vapo(u)rization system, and the solvent gasification is separated with extract, and promptly obtaining with the nicotine is the thick product of plant alkaloid of many water of main component.Extraction removes the solvent in the material by the condition among the embodiment 1 after accomplishing, and from extractor, takes out tobacco leaf, reclaims solvent and recycles.
Embodiment 4: the extraction of plant general glycoside: get fresh ginseng 1000 ㎏, pulverize behind the flush away earth, send in the extractor of construction of pressure vessel, close feeding-passage after, the device internal pressure is reduced to-0.08Mpa.Squeeze into liquefaction methyl ether extractant and carry out counter-current extraction 5 times, the extraction time is 150 minutes, 20 ℃～35 ℃ of extraction temperature, extracting pressure 0.8 Mpa～1.2Mpa.The extract of extraction gained gets into vapo(u)rization system, and the solvent gasification is separated with extract, promptly obtains being rich in the thick product of plant general glycoside of many water of panaquilon.Extraction removes the solvent in the material by the condition among the embodiment 1 after accomplishing, and from extractor, takes out genseng, reclaims solvent and recycles.
What more than enumerate only is to realize several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (5)
1. the extracting process of useful composition in the high aqueous plant raw material, the extract of treating that height is contained moisture is inserted in the airtight extraction container, and container is vacuumized; Inject extractant and flood extract, carry out counter-current extraction, extracting pressure is the saturated vapour pressure of extractant under the corresponding extraction temperature; After extraction finished, with the solid phase of extraction and the liquid phase separation that extracts, the extract in the liquid phase separated with extractant; And remove solvent composition remaining in the extract, obtain thick extract; Remove solvent composition remaining in the solid phase, obtain plant residue; All separation and the solvent recovery cycle that removes are used; It is characterized in that: extraction container is vacuumized, the control container inner pressure be-0.02Mpa～-0.09Mpa, preferred-0.08Mpa, extractant is the methyl ether that liquefies, and extraction times is 4～8 times, and extraction temperature is-20 ℃～50 ℃, preferred 20～35 ℃; Total extraction time is 60～240 minutes, preferred 90～200 minutes; Extracting pressure is 0.2 Mpa～1.2Mpa, preferred 0.6Mpa～0.9Mpa.
2. the extracting process of useful composition in the high aqueous plant raw material according to claim 1; It is characterized in that: bright capsicum is inserted in the airtight extractor after removing seed and grinding; Container inner pressure is reduced to-0.08Mpa, inject liquefaction methyl ether extractant and carry out counter-current extraction 8 times, the extraction time is 150～200 minutes; Extraction temperature is 20 ℃～35 ℃, extracting pressure 0.6 Mpa～0.9Mpa; From extractor, extract extract out, remove the solvent in the extract, obtain with capsicum red pigment and capsaicine be useful component thick product.
3. the extracting process of useful composition in the high aqueous plant raw material according to claim 1; It is characterized in that: the wet marigold flower that will handle after pulverizing is inserted in the airtight extraction container; Container inner pressure is reduced to-0.08Mpa, inject liquefaction methyl ether extractant and carry out counter-current extraction 6 times, the extraction time is 120～160 minutes; Extraction temperature is 20 ℃～35 ℃, extracting pressure 0.6 Mpa～0.9Mpa; From extractor, extract extract out, remove the solvent in the extract, obtaining with the aztec marigold leaf flavine is the thick product of useful component.
4. the extracting process of useful composition in the high aqueous plant raw material according to claim 1; It is characterized in that: the fresh tobacco leaf after will pulverizing is inserted in the airtight extraction container; Container inner pressure is reduced to-0.08Mpa, inject liquefaction methyl ether extractant and carry out counter-current extraction 4 times, the extraction time is 100～150 minutes; Extraction temperature is 20 ℃～35 ℃, extracting pressure 0.6 Mpa～0.9Mpa; From extractor, extract extract out, remove the solvent in the extract, obtaining with the nicotine is the thick product of main component.
5. the extracting process of useful composition in the high aqueous plant raw material according to claim 1; It is characterized in that: the genseng that the aquatic foods after will pulverizing are wet is inserted in the airtight extraction container; Container inner pressure is reduced to-0.08Mpa, inject liquefaction methyl ether extractant and carry out counter-current extraction 5 times, the extraction time is 150 minutes; Extraction temperature is 20 ℃～35 ℃, extracting pressure 0.6 Mpa～0.9Mpa; From extractor, extract extract out, remove the solvent in the extract, obtain being rich in panaquilon's thick product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104585519A (en) * | 2014-10-20 | 2015-05-06 | 吕梁广汇生物科技股份有限公司 | Laying hen feed rich in xanthophyll |
| CN106962972A (en) * | 2017-03-20 | 2017-07-21 | 河南中烟工业有限责任公司 | A kind of counterextraction method for lifting discarded tobacco leaf quality |
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| CN1422685A (en) * | 2002-12-17 | 2003-06-11 | 广西大学 | Microwave-pretreating extraction method for effective component of plant |
| EP1397186B1 (en) * | 2001-06-06 | 2007-01-03 | Naturel Corporation, LLC | A low temperature process for extracting principal components from plants |
| CN101912696A (en) * | 2010-09-26 | 2010-12-15 | 祁鲲 | Subcritical extraction method using liquid ammonia as solvent |
| CN102258883A (en) * | 2011-06-24 | 2011-11-30 | 苏州大学 | Dynamic cycle extraction method for plant extracts and application thereof |
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2012
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| EP1397186B1 (en) * | 2001-06-06 | 2007-01-03 | Naturel Corporation, LLC | A low temperature process for extracting principal components from plants |
| CN1422685A (en) * | 2002-12-17 | 2003-06-11 | 广西大学 | Microwave-pretreating extraction method for effective component of plant |
| CN101912696A (en) * | 2010-09-26 | 2010-12-15 | 祁鲲 | Subcritical extraction method using liquid ammonia as solvent |
| CN102258883A (en) * | 2011-06-24 | 2011-11-30 | 苏州大学 | Dynamic cycle extraction method for plant extracts and application thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104585519A (en) * | 2014-10-20 | 2015-05-06 | 吕梁广汇生物科技股份有限公司 | Laying hen feed rich in xanthophyll |
| CN104585519B (en) * | 2014-10-20 | 2017-12-15 | 吕梁广汇生物科技股份有限公司 | A kind of egg feedstuff rich in lutein |
| CN106962972A (en) * | 2017-03-20 | 2017-07-21 | 河南中烟工业有限责任公司 | A kind of counterextraction method for lifting discarded tobacco leaf quality |
| CN106962972B (en) * | 2017-03-20 | 2018-03-27 | 河南中烟工业有限责任公司 | A kind of counterextraction method for lifting discarded tobacco leaf quality |
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Application publication date: 20120704 |