GB2091292A - Separating Wax From Simmondsia Using Gas Under Supercritical Conditions - Google Patents

Separating Wax From Simmondsia Using Gas Under Supercritical Conditions Download PDF

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Publication number
GB2091292A
GB2091292A GB8137117A GB8137117A GB2091292A GB 2091292 A GB2091292 A GB 2091292A GB 8137117 A GB8137117 A GB 8137117A GB 8137117 A GB8137117 A GB 8137117A GB 2091292 A GB2091292 A GB 2091292A
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United Kingdom
Prior art keywords
extraction
separation
pressure
critical
temperature
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Granted
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GB8137117A
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GB2091292B (en
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Abbott Products GmbH
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Kali Chemie Pharma GmbH
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Publication of GB2091292A publication Critical patent/GB2091292A/en
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Expired legal-status Critical Current

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Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0203Solvent extraction of solids with a supercritical fluid
    • 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
    • C11B11/00Recovery or refining of other fatty substances, e.g. lanolin or waxes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/74Recovery of fats, fatty oils, fatty acids or other fatty substances, e.g. lanolin or waxes

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Extraction Or Liquid Replacement (AREA)
  • Fats And Perfumes (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)
  • Jellies, Jams, And Syrups (AREA)
  • Fertilizers (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

Wax is extracted from seed kernels of species of Simmondsia by means of gas under supercritical conditions, separation of the wax being achieved by providing sub-critical conditions, the gas being returned into the extraction stage and the wax being removed. CO2 is the preferred gas.

Description

SPECIFICATION Process for the Separation of Valuable Matter from Plant Material This invention relates to a method for the separation of valuable substances from plant matter.
Forty-five to fifty percent by weight of the total weight of fully ripened seed kernels of plants of the species Simmondsia (simmondsia chinensis and simmonsia california) consist of a fluid wax.
This wax is a mixture of long-chain fatty acid esters, the acid component of which is formed from higher, straight chain acids and the alcohol component of which is formed from higher, monovalent alcohols. Thus it differs substantially from normal plant oils, which, as is known, are triglycerides of glycerol. Owing to its good stability it has a variety of uses, for example as a carrier or excipient for cosmetic or pharmaceutical formulations.
Methods used hitherto for the separation and isolation of the wax include cold or hot extrusion of the seed kernels, or the extraction of the wax with various solvents from the previously ground or compressed seed kernels.
Apart from the fact that with mechanical extrusion only approximately 60 to 70% of the wax content can be extracted, usual commercial qualities, which have been obtained by extrusion, still contain portions of cell matter. These portions of cell matter which are intrusive for many purposes, must be separated in further process steps. However, particular filtering methods, which use conventional filter media such as, for example, kieselguhr, silica gel, fuller's earth or alumina, in fact yield a product, which is free of solid components, but these filtering methods have an adverse influence on the stability of the wax. Thus, waxes purified by filtration through active media quickly become rancid and unusable when stored under normal conditions.
Methods of extraction of the wax components by means of solvents have not been used technically to date. Furthermore, products obtained in such a way still contain residues of solvent and without further purification operations they are consequently unusable for cosmetic or pharmaceutical purposes.
According to the present invention there is provided a method for the separation of valuable substances from plant matter, wherein seed kernels of species of Simmondsia are subjected to extraction in an extraction stage by means of a gas under supercritical conditions, thereby to obtain a phase containing valuable substances, and wherein this phase is transferred into a separation stage, where separation of the valuable substances occurs by providing or establishing subcritical conditions, whereby a substantially pure stable vegetable wax is obtained as the valuable substance, the gas being returned from the separation stage to the extraction stage.
In general, any gas which is physiologically harmless, and which is chemically inert to the plant wax, can be used as the extraction medium; such gases include for example: carbon dioxide, various halogenated hydrocarbons including, CHF3, CF3-CF3,CHCl-CF2,CF CF2=CH2, 2,CF3-CH3, CHF2-CH3,CHF2Cl, CF 3Cl, CF2=CF2, CF2Cl2, CCl3-CHCl2 and C3Fs, sulphur hexafluoride, nitrous oxide, sulphur dioxide, and various hydrocarbons including ethane, ethene, propaner propene, etc. Mixtures of two or more of such gases may be used but carbon dioxide is particularly preferred.
In the extraction stage the seed kernels are exposed to the extraction medium under conditions such that the gas is supercritical both as regards temperature and also as regards pressure. The critical parameters of the gases mentioned above are well-known.
The temperature at which the extraction takes place is preferably in the range of from the critical temperature up to 500C, preferably up to 200C.
above the critical temperature, and the pressure is preferably in the range from the critical pressure up to 500 bar, preferably up to 350 bar above the critical pressure.
In the case where the extraction medium is carbon dioxide, the extraction is conveniently carried out at a temperature in the range of from 31.3 to 800C., preferably 31.3 to 500C., and at a pressure in the range of from 72 to 600 bar, preferably 72 to 300 bar.
From the extraction stage, the phase containing the valuable matter is passed over into the separation stage in which separation of the valuable substances takes place by providing or establishing subcritical conditions. The temperature at which the separation takes place is preferably in the range of from the critical temperature to 1 50C. below the critical temperature, and the pressure is preferably in the range of from the critical pressure to 25 bar below the critical pressure.
In the case where the extraction medium is carbon dioxide, the separation is conveniently carried out at a temperature in the range of 31.3cm. to 1 50C. and at a pressure in the range from 72 to 45 bar.
By providing or establishing subcritical conditions in the separation stage, the solvent power of the extraction medium for the extracted valuable substances is reduced such that the latter separate in the separation stage from the extraction medium and can be carried off during the extraction process, for example through a sluice, or after the extraction process has been completed. Any aqueous components which have also been separated during the extraction process form a separate phase in the separation stage and can be separated from the wax without difficulty.
The extraction medium can be re-used directly without any further purification requiring intensive work and energy, so that no additional emission problems arise. In order to be re-introduced into the extraction stage, the extraction medium merely has to be converted into the supercritical state as regards temperature and pressure, i.e. the alteration in temperature and pressure which was made for separation is cancelled again.
The separated vegetable wax can be removed from the separation stage after the extraction is completed if the present process is conducted as a batch process. However, it is possible to remove the vegetable wax-e.g. via a sluice-if the present process is conducted as a continuous process. With both methods of operation extraction periods of 1 to 12 hours, preferably 3 to 7 hours, are sufficient, to obtain the end product in the purity desired.
With the present method therefore it is possible to obtain the desired product in a short time, thereby minimizing the overheads for apparatus, manpower and energy, and also to avoid any undue burden on the environment. The circulation of the extraction medium offers in particular the possibility of automating the process cycle and, consequently, of conducting the extraction in a particularly economical way.
The vegetable wax obtained can be supplied directly for utilization in foodstuffs, pharmaceutical or cosmetic products etc; however, it can also be hydrated and used as a hydrated product.
The invention will now be illustrated by the following Examples in which specific process conditions are identified as follows:~ Extraction container: Pressure' P Temperature t Separation container: Pressure P2 Temperature t2 Example 1 100 g. of previously ground seed kernels of Simmondsia are loaded into an extraction container and extracted with carbon dioxide gas under supercritical conditions; separation is effected in a separate container and the process conditions are:~ P1 200 bar ti 400C.
P2 50 bar t2 200C.
Extraction time 4h 41 g. of a clear, light yellow wax are obtained and removed from the separation container; in addition, 3.5 g. water are isolated. 55 g. of a pulverulent de-oiled product remain in the extraction container.
The analysis of the wax was as follows C384luid ester approx. 10% C40-fluid ester approx. 30% C42-fluid ester approx. 50% C,-fluid ester approx. 10% Example 2 100 g. of simmondsia seed kernels, stripped of the brown pellicle and ground, are loaded into the extraction container and extracted with carbon dioxide gas under supercritical conditions, and separation is effected under subcritical conditions, the process conditions being P1 300 bar ti 400C.
P2 50 bar t2 200 C.
Extraction time 4h 40 g. of a clear, light yellow fatty acid estermixture are removed from the separation container. In addition 7.5 g. water are separated and 53 g. of a pulverulent residue remains in the extraction vessel.
Example 3 100 g. of ground seed kernels of the Simmondsia chinensis plant are treated with carbon dioxide gas under supercritical conditions and separation is effected under subcritical conditions, the process conditions being P1 150 bar ti 500C.
P2 50 bar t2 200 C.
Extraction time 4h 36 g. of a clear light yellow wax are recovered in.
the separation container, and in addition 3.5 g.
water are separated while 60 g. de-waxed base material remain as a residue in the extraction - container.

Claims (10)

Claims
1. A method for the separation of valuable substances from plant matter, wherein seed kernels of species of Simmondsia are subjected to extraction in an extraction stage by means of a gas under supercritical conditions, thereby to obtain a phase containing valuable substances, and wherein this phase is transferred into a separation stage, where separation of the valuable substances occurs by providing or establishing subcritical conditions, whereby a substantially pure stable vegetable wax is obtained as the valuable substance, the gas being returned from the separation stage to the extraction stage.
2. A method as claimed in Claim 1 wherein the gas is carbon dioxide.
3. A method as claimed in Claim 1 or 2, wherein the temperature at which the extraction takes place is from the critical temperature up to 500 C. above the critical temperature.
4. A method as claimed in any one of Claims 1 to 3, wherein the temperature at which the extraction takes place is from the critical temperature up to 200C. above the critical temperature.
5. A method as claimed in any one of Claims 1 to 4, wherein the temperature at which the separation takes place is from the critical temperature to 1 50C. below the critical temperature.
6. A method as claimed in any one of Claims 1 to 5, wherein the pressure at which the extraction takes place is from the critical pressure up to 500 bar above the critical pressure.
7. A method as claimed in any one of Claims 1 to 6, wherein the pressure at which the extraction takes place is from the critical pressure up to 350 bar above the critical pressure.
8. A method as claimed in any one of Claims 1 to 7, wherein the pressure at which the separation takes place is from the critical pressure to 25 bar below the critical pressure.
9. A method for the separation of valuable substances from plant matter, substantially as hereinbefore described in any one of the foregoing Examples.
10. Vegetable wax obtained from seed kernels of species of Simmondsia by the method claimed in any preceding claim.
GB8137117A 1981-01-15 1981-12-09 Separating wax from simmondsia using gas under supercriticcal conditions Expired GB2091292B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE19813101025 DE3101025A1 (en) 1981-01-15 1981-01-15 METHOD FOR ISOLATING VALUABLES FROM PLANT MATERIAL

Publications (2)

Publication Number Publication Date
GB2091292A true GB2091292A (en) 1982-07-28
GB2091292B GB2091292B (en) 1984-03-21

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ID=6122639

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GB8137117A Expired GB2091292B (en) 1981-01-15 1981-12-09 Separating wax from simmondsia using gas under supercriticcal conditions

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JP (1) JPS57145195A (en)
AT (1) AT372608B (en)
AU (1) AU7951282A (en)
BE (1) BE891781A (en)
DD (1) DD201915A5 (en)
DE (1) DE3101025A1 (en)
DK (1) DK12982A (en)
ES (1) ES8306788A1 (en)
FI (1) FI820074L (en)
FR (1) FR2497823A1 (en)
GB (1) GB2091292B (en)
GR (1) GR75832B (en)
IL (1) IL64587A0 (en)
IT (1) IT1195293B (en)
NL (1) NL8105301A (en)
NO (1) NO820104L (en)
NZ (1) NZ199390A (en)
PT (1) PT74018B (en)
SE (1) SE8200069L (en)
ZA (1) ZA817997B (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4466923A (en) * 1982-04-01 1984-08-21 The United States Of America As Represented By The Secretary Of Agriculture Supercritical CO2 extraction of lipids from lipid-containing materials
US4675133A (en) * 1983-06-25 1987-06-23 Fried. Krupp Gesellschaft Mit Beschrankter Haftung Process for apparatus for the recovery of fats and oils
US5138075A (en) * 1983-07-05 1992-08-11 Kuraray Co., Ltd. Extractive separation method
FR2799660A1 (en) * 1999-10-19 2001-04-20 Hitex Production of active extract for use in cosmetic, pharmaceutical or food compositions, by extracting starting material with supercritical carbon dioxide containing cosolvent also serving as excipient in final composition
FR2865644A1 (en) * 2004-01-29 2005-08-05 Oreal Producing a cosmetic composition for treating keratinic materials, especially hair, comprises percolating a fluid under pressure through an ester composition in solid or paste form
WO2006082437A1 (en) * 2005-02-04 2006-08-10 The University Of York Isolation and fractionation of waxes from plants
US7091366B2 (en) 2003-09-25 2006-08-15 Thar Technologies, Inc. Recovery of residual specialty oil
WO2007017205A3 (en) * 2005-08-06 2007-03-29 Degussa Method for obtaining fruit wax

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3414977C2 (en) * 1984-04-19 1992-01-09 Hopfenextraktion HVG Barth, Raiser & Co, 8069 Wolnzach Process for the extraction of solids with compressed carbon dioxide
JPH0816233B2 (en) * 1991-08-30 1996-02-21 三井物産株式会社 Process for producing purified propolis and O / W emulsion containing purified propolis component
DE102018001205A1 (en) 2018-02-14 2019-08-14 Sven Miric Method and apparatus for extracting and / or concentrating lipophilic molecules by means of liquid or supercritical carbon dioxide

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2127596A1 (en) * 1971-06-03 1972-12-21 Hag Ag, 2800 Bremen Process for the production of vegetable fats and oils.

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4466923A (en) * 1982-04-01 1984-08-21 The United States Of America As Represented By The Secretary Of Agriculture Supercritical CO2 extraction of lipids from lipid-containing materials
US4675133A (en) * 1983-06-25 1987-06-23 Fried. Krupp Gesellschaft Mit Beschrankter Haftung Process for apparatus for the recovery of fats and oils
US5138075A (en) * 1983-07-05 1992-08-11 Kuraray Co., Ltd. Extractive separation method
FR2799660A1 (en) * 1999-10-19 2001-04-20 Hitex Production of active extract for use in cosmetic, pharmaceutical or food compositions, by extracting starting material with supercritical carbon dioxide containing cosolvent also serving as excipient in final composition
WO2001028649A1 (en) * 1999-10-19 2001-04-26 Hitex Method for supercritical fluid extraction
US7091366B2 (en) 2003-09-25 2006-08-15 Thar Technologies, Inc. Recovery of residual specialty oil
FR2865644A1 (en) * 2004-01-29 2005-08-05 Oreal Producing a cosmetic composition for treating keratinic materials, especially hair, comprises percolating a fluid under pressure through an ester composition in solid or paste form
WO2006082437A1 (en) * 2005-02-04 2006-08-10 The University Of York Isolation and fractionation of waxes from plants
WO2007017205A3 (en) * 2005-08-06 2007-03-29 Degussa Method for obtaining fruit wax

Also Published As

Publication number Publication date
BE891781A (en) 1982-04-30
FI820074L (en) 1982-07-16
IT8125240A0 (en) 1981-11-24
ES508714A0 (en) 1983-06-01
JPS57145195A (en) 1982-09-08
NZ199390A (en) 1984-05-31
ES8306788A1 (en) 1983-06-01
DD201915A5 (en) 1983-08-17
ZA817997B (en) 1982-10-27
AU7951282A (en) 1982-07-22
IL64587A0 (en) 1982-03-31
DE3101025A1 (en) 1982-08-26
AT372608B (en) 1983-10-25
GB2091292B (en) 1984-03-21
GR75832B (en) 1984-08-02
PT74018A (en) 1981-12-01
NL8105301A (en) 1982-08-02
IT1195293B (en) 1988-10-12
ATA560081A (en) 1983-03-15
SE8200069L (en) 1982-07-16
PT74018B (en) 1983-06-20
FR2497823A1 (en) 1982-07-16
NO820104L (en) 1982-07-16
DK12982A (en) 1982-07-16

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