CN109554218A - The technique of fat-soluble compound in a kind of supercritical fluid extraction idesia - Google Patents
The technique of fat-soluble compound in a kind of supercritical fluid extraction idesia Download PDFInfo
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- CN109554218A CN109554218A CN201910056571.XA CN201910056571A CN109554218A CN 109554218 A CN109554218 A CN 109554218A CN 201910056571 A CN201910056571 A CN 201910056571A CN 109554218 A CN109554218 A CN 109554218A
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- 241001299699 Idesia Species 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 12
- 150000001875 compounds Chemical class 0.000 title claims abstract description 8
- 238000000605 extraction Methods 0.000 claims abstract description 32
- 238000000926 separation method Methods 0.000 claims abstract description 30
- 238000005516 engineering process Methods 0.000 claims abstract description 8
- 230000003068 static effect Effects 0.000 claims abstract description 6
- 239000000463 material Substances 0.000 claims abstract description 4
- 238000012545 processing Methods 0.000 abstract description 2
- 239000000284 extract Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- 238000000227 grinding Methods 0.000 description 5
- 239000003921 oil Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229930014626 natural product Natural products 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000012530 fluid Substances 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 3
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 3
- 102000004190 Enzymes Human genes 0.000 description 2
- 108090000790 Enzymes Proteins 0.000 description 2
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 2
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 2
- 229960004488 linolenic acid Drugs 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 210000000697 sensory organ Anatomy 0.000 description 2
- 239000000344 soap Substances 0.000 description 2
- 238000000638 solvent extraction Methods 0.000 description 2
- 238000002137 ultrasound extraction Methods 0.000 description 2
- OYHQOLUKZRVURQ-NTGFUMLPSA-N (9Z,12Z)-9,10,12,13-tetratritiooctadeca-9,12-dienoic acid Chemical compound C(CCCCCCC\C(=C(/C\C(=C(/CCCCC)\[3H])\[3H])\[3H])\[3H])(=O)O OYHQOLUKZRVURQ-NTGFUMLPSA-N 0.000 description 1
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- KYARBIJYVGJZLB-UHFFFAOYSA-N 7-amino-4-hydroxy-2-naphthalenesulfonic acid Chemical compound OC1=CC(S(O)(=O)=O)=CC2=CC(N)=CC=C21 KYARBIJYVGJZLB-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 244000147058 Derris elliptica Species 0.000 description 1
- 206010061958 Food Intolerance Diseases 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- 241000218998 Salicaceae Species 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- AXFBAIOSECPASO-UHFFFAOYSA-N pentacyclo[6.6.2.02,7.04,16.011,15]hexadeca-1(14),2(7),3,5,8(16),9,11(15),12-octaene Chemical compound C1=C(C=C23)C4=C5C3=CC=CC5=CC=C4C2=C1 AXFBAIOSECPASO-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007127 saponification reaction Methods 0.000 description 1
- 239000010729 system oil Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention discloses the technique of fat-soluble compound in supercritical fluid extraction idesia, extraction process parameter: extraction temperature is 15~40 DEG C, and extracting pressure is 20~50MPa, 120~300min of static extracting time.Separating technology parameter: separation reactor I is 6~15MPa, 20~45 DEG C of separation temperature with separation reactor I I pressure.Crushing material granularity is 20~40 mesh.Technique extraction yield of the invention is high, and extraction conditions readily satisfies, and processing step is safe and reliable, is worthy to be popularized.
Description
Technical field
The invention belongs to extracting substances technical fields, and in particular to fat-solubleization in a kind of supercritical fluid extraction idesia
The technique for closing object.
Technical background
The common extracting method of natural products has solvent extraction method, ultrasonic extraction, microwave loss mechanisms and enzyme to mention at present
It follows the example of.Although extracting modes such as extraction methods, recovery rate is higher, it has inevitable defect, that is, has solvent residual
It stays, for thermal sensitivity food, heating can cause certain unsaturated fatty acids that the chemicals such as the variation, such as DHA, ARA of matter occur
The change of matter generation matter.And natural extract is mainly used for the fields such as food, cosmetics.With the improvement of living standards, people
It is higher and higher to the nutritional quality of the products such as food, cosmetics, sensible quality, freshness requirement, it is obtained by extraction
Natural products be extremely difficult to require, so the abstraction technique of low temperature, organic solvent-free is gradually valued by people.Currently,
Low temperature, no solvent residue high-new extraction and separation technology mainly have supercritical extract fluid technique, aqueous enzymatic method technology, pulverize
Technology, molecularly distilled etc..
Idesia polycarpa is Flacourtiaceae, one kind of idesia subordinate.Its dry fruit oil content 35%~40%, idesia
In contain the unsaturated fatty acids such as linoleic acid, oleic acid, linolenic acid.Idesia is also woody oil tree species, is known as " the oil on tree
The good reputation in library ", pulp account for total 62.3% of fruit, and seed accounts for 37.6%.Its extract can soap system or lubricating oil, be excellent
The excellent raw material of matter edible oil and advanced skin-protection soap, health care product.The extracting process of common idesia oil mainly includes solvent leaching
Formulation, ultrasonic extraction, microwave loss mechanisms and enzyme extraction method, supercritical fluid extraction etc..In common extracting process, only
The extraction for having solvent extraction method often to use natural products produces, and this extracting process not only has dissolvent residual, and production cost is higher.
Supercritical CO2The principle of extraction separation process is to utilize supercritical CO2Have to certain special natural products special molten
Solution effect, utilizes supercritical CO2Solvability and its density relationship, i.e., using pressure and temperature to supercritical CO2Dissolve energy
The influence of power and carry out.In supercritical CO2It is in contact with the substance to be separated, makes it selectively polarity size, boiling point
The height ingredient different with molecular size range is extracted in turn.
At present it is believed that supercritical CO2It is mainly following several to extract advantage: 1) critical-temperature and critical pressure (Tc
=31.1 DEG C, Pc=7.38MPa), operating condition is mild, destroys to effective component few；2)CO2It can regard as and nothing as water phase
Malicious, cheap organic solvent；3)CO2It is stable in use, nontoxic, do not burn, be safe, is free from environmental pollution, and can avoid
The oxidation of product；4)CO2Nitrate and harmful heavy metal, and the residual without hazardous solvent are free of in extract；5) exist
Supercritical CO2When extraction, the substance being extracted can be precipitated by reduction pressure, or raising temperature, it is not necessary to by extracting repeatedly
Operation.
However in the prior art, there are no use supercritical CO2The technique for extracting fat-soluble compound in idesia.
Summary of the invention
It is existing to overcome the object of the present invention is to provide the technique of fat-soluble compound in supercritical fluid extraction idesia
Technology extracts deficiency existing for the technique of liposoluble substance in idesia.
Technical scheme is as follows:
Key point of the invention is: extraction process parameter: extraction temperature be 15~40 DEG C, extracting pressure be 20~
50MPa, 120~300min of static extracting time.Separating technology parameter: separation reactor I and separation reactor I I pressure are 6~15MPa, divide
From 20~45 DEG C of temperature.Crushing material granularity is 20~40 mesh.Under process above parameter, it can obtain and be difficult to expect extraction
Effect achieves significant progress than the prior art.
Specifically, supercritical CO of the invention2The technique of liposoluble substance in fluid extraction idesia, including following step
It is rapid:
Step 1: the idesia after screening being crushed, grinding particle size is 20~40 mesh；The idesia handled well is taken, is put
Enter in supercritical extraction reactor, technological parameter is arranged: extraction temperature is 15~40 DEG C, extracting pressure is 20~50MPa, static extracting
120~300min of time；Separation reactor I and separation reactor I I pressure are 6~15MPa, 20~45 DEG C of separation temperature.
Step 2: starting force (forcing) pump, starting pressurization pump frequency is 10~15Hz, slowly promotes pressurization pump frequency, makes its extraction
Pressure reaches set numerical value.
Step 3: the extract in 30min, separate collection separation reactor I and separation reactor I I.
Step 4: after the dwell time, closing force (forcing) pump, supercritical CO2Inlet valve allows it slowly to carry out pressure release, allows
Pressure gauge reading in extraction kettle is 0.
Wherein: the grinding particle size of idesia is 20~40 mesh in step 1；In step 4, in pressure leak process, slowly to carry out,
Conversely, idesia powder can be with supercritical CO2Plug net is penetrated, is gone in separating still, so that pipeline pollutes.Pressure leak process
In, pressure release speed is 0.001~0.10MPa/s in extraction kettle.
Technique extraction yield of the invention is high, and extraction conditions readily satisfies, and processing step is safe and reliable, is worthy to be popularized.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.
Embodiment 1:
A kind of supercritical CO2The technique of liposoluble substance in fluid extraction idesia, comprising the following steps:
Step 1: the idesia (non-pulp separation) after screening being crushed, grinding particle size is 20 mesh；It takes and crushes
Idesia is put into supercritical extraction reactor, and technological parameter is arranged: extraction temperature is 15~40 DEG C, extracting pressure be 20~
50MPa, 120~300min of static extracting time；Separation reactor I and separation reactor I I pressure are 6~15MPa, separation temperature 20~45
℃。
Step 2: starting force (forcing) pump, starting pressurization pump frequency is 10~15Hz, slowly promotes pressurization pump frequency, makes its extraction
Pressure reaches set numerical value.
Step 3: the extract in 30min, separate collection separation reactor I and separation reactor I I.
Step 4: after the dwell time, closing force (forcing) pump, supercritical CO2Inlet valve allows it slowly to carry out pressure release, allows
Pressure gauge reading in extraction kettle is 0.
Points for attention: the grinding particle size of idesia is 20 mesh in step 1；In step 4, in pressure leak process, slowly to carry out,
Conversely, idesia powder can be with supercritical CO2Plug net is penetrated, is gone in separating still, so that pipeline pollutes.Pressure leak process
In, pressure release speed is 0.001~0.10MPa/s in extraction kettle.
Embodiment 2:
Step 1: the de- seed idesia after screening being crushed, grinding particle size is 40 mesh；The idesia crushed is taken, is put
Enter in supercritical extraction reactor, technological parameter is arranged: extraction temperature is 15~40 DEG C, extracting pressure is 20~50MPa, static extracting
120~300min of time；Separation reactor I and separation reactor I I pressure are 6~15MPa, 20~45 DEG C of separation temperature.
Step 2: starting force (forcing) pump, starting pressurization pump frequency is 10~15Hz, slowly promotes pressurization pump frequency, makes its extraction
Pressure reaches set numerical value.
Step 3: the extract in 30min, separate collection separation reactor I and separation reactor I I.
Step 4: after the dwell time, closing force (forcing) pump, supercritical CO2Inlet valve allows it slowly to carry out pressure release, allows
Pressure gauge reading in extraction kettle is 0.
Detection method: sense organ, nutritional ingredient and microorganism that oil product is obtained by extraction in embodiment 1, embodiment 2 are referred to respectively
Mark performance test experiment.
1, experimental material: the idesia oil that embodiment 1, embodiment 2 obtain.
2, it experimental method: is detected referring to the corresponding national standard of the People's Republic of China (PRC).
3, experimental result:
Experimental result is as shown in table 1.
1 separation reactor I of table forms testing result with the sense organ of extract, fatty acid in separation reactor I I
| Detection project | Separation reactor I | Separation reactor I I |
| Acid value (mg/g) | Less than 10 | Less than 10 |
| Saponification number (mmol/kg) | Less than 200 | Less than 200 |
| Unsaturated fatty acid (%) | Greater than 80 | Greater than 85 |
| Linolenic acid (%) | Greater than 0.2 | Greater than 0.3 |
| Linoleic acid (%) | Greater than 65 | Greater than 70 |
| Lead (mg/kg) | It is not detected | It is not detected |
| Arsenic (mg/kg) | It is not detected | It is not detected |
| Benzo (α) pyrene (μ g/kg) | It is not detected | It is not detected |
The above is only preferable examples of the present invention, not to making any data and formal limitation, it is all according to
According to technical spirit of the invention to any data modification, equivalent variations made by example is applied above, the technology of the present invention reality is still fallen within
Within the scope of matter.
Claims (3)
1. the technique of fat-soluble compound in a kind of supercritical fluid extraction idesia, it is characterised in that: extraction process parameter: extraction
Taking temperature is 15~40 DEG C, and extracting pressure is 20~50MPa, 120~300min of static extracting time.
2. the technique of fat-soluble compound in supercritical fluid extraction idesia according to claim 1, it is characterised in that:
Separating technology parameter: separation reactor I is 6~15MPa, 20~45 DEG C of separation temperature with separation reactor I I pressure.
3. the technique of fat-soluble compound in supercritical fluid extraction idesia according to claim 1, it is characterised in that:
Crushing material granularity is 20~40 mesh.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811191235 | 2018-10-12 | ||
| CN2018111912358 | 2018-10-12 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109554218A true CN109554218A (en) | 2019-04-02 |
Family
ID=65873491
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910056571.XA Pending CN109554218A (en) | 2018-10-12 | 2019-01-22 | The technique of fat-soluble compound in a kind of supercritical fluid extraction idesia |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110643420A (en) * | 2019-11-13 | 2020-01-03 | 贵州航天乌江机电设备有限责任公司 | Process for extracting and refining oil from idesia polycarpa |
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|---|---|---|---|---|
| CN101230541A (en) * | 2007-12-13 | 2008-07-30 | 中国人民解放军总后勤部军需装备研究所 | Hemp softening oil, preparation method and use thereof |
| CN102212415A (en) * | 2011-04-26 | 2011-10-12 | 刘长根 | Biodiesel prepared from Idesia polycarpa var.vestita Diels oil and preparation method thereof |
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2019
- 2019-01-22 CN CN201910056571.XA patent/CN109554218A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101230541A (en) * | 2007-12-13 | 2008-07-30 | 中国人民解放军总后勤部军需装备研究所 | Hemp softening oil, preparation method and use thereof |
| JP2014510164A (en) * | 2011-02-14 | 2014-04-24 | カウンスィル オブ サイエンティフィック アンド インダストリアル リサーチ | Improved process for producing fatty acid alkyl esters (biodiesel) from triglyceride oils by using environmentally friendly solid base catalysts |
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Non-Patent Citations (1)
| Title |
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