CN109536273A - The technique of fatty acid substance in a kind of supercritical fluid extraction sesame - Google Patents

The technique of fatty acid substance in a kind of supercritical fluid extraction sesame Download PDF

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Publication number
CN109536273A
CN109536273A CN201910056557.XA CN201910056557A CN109536273A CN 109536273 A CN109536273 A CN 109536273A CN 201910056557 A CN201910056557 A CN 201910056557A CN 109536273 A CN109536273 A CN 109536273A
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CN
China
Prior art keywords
extraction
technique
fatty acid
sesame
supercritical fluid
Prior art date
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Pending
Application number
CN201910056557.XA
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Chinese (zh)
Inventor
杨再文
宋大为
孙太林
刘敏
龙艺
李井强
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Guizhou Aerospace Wujiang Electro Mechanical Equipment Co Ltd
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Guizhou Aerospace Wujiang Electro Mechanical Equipment Co Ltd
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Application filed by Guizhou Aerospace Wujiang Electro Mechanical Equipment Co Ltd filed Critical Guizhou Aerospace Wujiang Electro Mechanical Equipment Co Ltd
Publication of CN109536273A publication Critical patent/CN109536273A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/104Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material

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  • 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)
  • Fats And Perfumes (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses the technique of fatty acid substance in supercritical fluid extraction sesame, extraction process parameter: extraction temperature is 15~40 DEG C, and extracting pressure is 20~45MPa, 120~300min of static extracting time, and pressurize pump frequency 35Hz.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.Baking process parameter: 70~120 DEG C, belt speed: 30~60cm/min.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

The technique of fatty acid substance in a kind of supercritical fluid extraction sesame
Technical field
The invention belongs to extracting substances technical fields, and in particular to fatty acid object in a kind of supercritical fluid extraction sesame The technique of matter.
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..
Sesame is one of China's major oil crops, is the annual herb plant of Pedaliaceae, sesame category.Contain in sesame Protein, grease, carbohydrate, minerals, vitamin and lignin.The oil that main component in sesame is 45%~63% Rouge, 19~31% protein, 20~25% carbohydrate.Sesamin also known as sesamin, sesamin, sesamin, it is a kind of Fat-soluble phenol organic matter.With going deep into for research work, Japanese, which has found that sesamin has, reduces cholesterol, liver protection shield Liver eliminates interior free yl, promotes a variety of physiological active functions such as alcohol metabolism.
The extracting process of common sesame oil: solvent extraction method, ultrasonic extraction, microwave loss mechanisms and enzyme extraction method, Supercritical fluid extraction etc..In common extracting process, only solvent extraction method often uses the extraction of natural products to produce, 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 fatty acid substance in sesame.
Summary of the invention
The object of the present invention is to provide the techniques of fatty acid substance in supercritical fluid extraction sesame, to overcome existing skill Art extracts deficiency existing for the technique of fatty acid substance in sesame.
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~ 45MPa, 120~300min of static extracting time, pressurize pump frequency 35Hz.Separating technology parameter: separation reactor I and separation reactor I I are pressed Power is 6~15MPa, 20~45 DEG C of separation temperature.Crushing material granularity is 20~40 mesh.Baking process parameter: 70~120 DEG C, Belt speed: 30~60cm/min.Under process above parameter, it can obtain and be difficult to expect effect of extracting, compare the prior art Achieve significant progress.
Specifically, supercritical CO of the invention2The technique of fatty acid substance in fluid extraction sesame, including following step It is rapid:
Step 1: the sesame after screening baking being crushed, grinding particle size is 20~40 mesh;The sesame crushed is taken, is put Enter in supercritical extraction reactor, technological parameter is arranged: extraction temperature is 15~40 DEG C, extracting pressure is 20~45MPa, 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 carbon dioxide inlet valve allows it slowly to be let out Pressure allows the pressure gauge reading in extraction kettle to be 0.
Wherein: the grinding particle size of sesame is 20~40 mesh in step 1;In step 4, in pressure leak process, slowly to carry out, instead It, sesame powder can be with supercritical CO2Plug net is penetrated, is gone in separating still, so that pipeline pollutes.In pressure leak process, extraction Taking pressure release speed in kettle is 0.001~0.10MPa/s.
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 fatty acid substance in fluid extraction sesame, comprising the following steps:
Step 1: the sesame after screening baking being crushed, grinding particle size is 20~40 mesh;The sesame crushed is taken, is put Enter in supercritical extraction reactor, technological parameter is arranged: extraction temperature is 15~40 DEG C, extracting pressure is 20~45MPa, 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.
Points for attention: the grinding particle size of sesame is 20 mesh in step 1;In step 4, in pressure leak process, slowly to carry out, instead It, sesame powder can be with supercritical CO2Plug net is penetrated, is gone in separating still, so that pipeline pollutes.In pressure leak process, extraction Taking pressure release speed in kettle is 0.001~0.10MPa/s.
Embodiment 2:
Step 1: sesame after screening parch being crushed, grinding particle size is 40 mesh;The sesame crushed is taken, super face is put into In boundary's extraction kettle, technological parameter is arranged: extraction temperature is 15~40 DEG C, extracting pressure is 20~45MPa, the static extracting time 120~300min;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: the indexs such as sense organ, the nutritional ingredient that oil product is obtained by extraction in embodiment 1, embodiment 2 are carried out respectively Test experiments.
1, experimental material: the sesame oil that embodiment 1, embodiment 2 are obtained by extraction.
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
Sense organ Meet the standard of national sesame oil Meet the standard of national sesame oil
Acid value (mg/g) Less than 0.6 Less than 0.6
Peroxide value (mmol/kg) Less than 2.7 Less than 2.6
Unsaturated fatty acid (%) Greater than 80 Greater than 85
Linolenic acid (%) Greater than 0.2 Greater than 0.3
Sesamin (%) Greater than 0.8 Greater than 0.4
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 (4)

1. the technique of fatty acid substance in a kind of supercritical fluid extraction sesame, it is characterised in that: extraction process parameter: extraction Temperature is 15~40 DEG C, and extracting pressure is 20~45MPa, 120~300min of static extracting time, and pressurize pump frequency 35Hz.
2. the technique of fatty acid substance in supercritical fluid extraction sesame according to claim 1, it is characterised in that: point Separating process parameter: separation reactor I is 6~15MPa, 20~45 DEG C of separation temperature with separation reactor I I pressure.
3. the technique of fatty acid substance in supercritical fluid extraction sesame according to claim 1, it is characterised in that: object Material grinding particle size is 20~40 mesh.
4. the technique of fatty acid substance in supercritical fluid extraction sesame according to claim 1, it is characterised in that: dry Curing process parameter: 70~120 DEG C, belt speed: 30~60cm/min.
CN201910056557.XA 2018-10-12 2019-01-22 The technique of fatty acid substance in a kind of supercritical fluid extraction sesame Pending CN109536273A (en)

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CN2018111920655 2018-10-12

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110776991A (en) * 2019-11-20 2020-02-11 湖北中烟工业有限责任公司 Method for extracting fatty acid from Chinese yam
CN113881494A (en) * 2021-11-09 2022-01-04 贵州汇腾科技有限公司 Method for producing strong-flavor rapeseed oil by supercritical fluid extraction technology

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1827756A (en) * 2006-04-04 2006-09-06 青岛大学 Extraction method for sesame essential oil
CN102994215A (en) * 2012-11-15 2013-03-27 山西五台山沙棘制品有限公司 Method for extracting rice bran by using supercritical CO2
CN104031734A (en) * 2014-06-26 2014-09-10 叶新 Method for preparing sesame oil by enzymolysis and supercritical fluid extraction
CN105087152A (en) * 2015-08-10 2015-11-25 查光圣 Supercritical extraction technology for seasame oil

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1827756A (en) * 2006-04-04 2006-09-06 青岛大学 Extraction method for sesame essential oil
CN102994215A (en) * 2012-11-15 2013-03-27 山西五台山沙棘制品有限公司 Method for extracting rice bran by using supercritical CO2
CN104031734A (en) * 2014-06-26 2014-09-10 叶新 Method for preparing sesame oil by enzymolysis and supercritical fluid extraction
CN105087152A (en) * 2015-08-10 2015-11-25 查光圣 Supercritical extraction technology for seasame oil

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110776991A (en) * 2019-11-20 2020-02-11 湖北中烟工业有限责任公司 Method for extracting fatty acid from Chinese yam
CN113881494A (en) * 2021-11-09 2022-01-04 贵州汇腾科技有限公司 Method for producing strong-flavor rapeseed oil by supercritical fluid extraction technology

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Application publication date: 20190329