CA2010972C - Process and device for separating a mixture of ingredient substances from the extracting agent - Google Patents
Process and device for separating a mixture of ingredient substances from the extracting agent Download PDFInfo
- Publication number
- CA2010972C CA2010972C CA002010972A CA2010972A CA2010972C CA 2010972 C CA2010972 C CA 2010972C CA 002010972 A CA002010972 A CA 002010972A CA 2010972 A CA2010972 A CA 2010972A CA 2010972 C CA2010972 C CA 2010972C
- Authority
- CA
- Canada
- Prior art keywords
- mixture
- pressure
- vessel
- pressure vessel
- relief valve
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/06—Flash distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/16—Evaporating by spraying
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/30—Accessories for evaporators ; Constructional details thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/02—Feed or outlet devices therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
- B01J2219/00083—Coils
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/18—Details relating to the spatial orientation of the reactor
- B01J2219/185—Details relating to the spatial orientation of the reactor vertical
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Extraction Or Liquid Replacement (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Steroid Compounds (AREA)
- Fats And Perfumes (AREA)
Abstract
The invention relates to a process and a device for separating a mixture obtained in an extractor and consisting of solvents and ingredient substances, the extraction pressure of the mixture being reduced. The aim of the invention is to design an unsophisticated and rapid separation process particularly suitable for substances of high viscosity. The invention provides for a process wherein the mixture is directly injected into a large chamber via a relief valve.
Description
Process And Device For Separating A Mixture Of Ingredient Substances From The Extracting Agent The invention relates to a process for separating a mixture obtained in an extractor and consisting of solvents and ingredient substances from said solvents, while reducing the pressure of the mixture.
Processes are known in which the ingredient substances are extracted with the aid of solvents. Patent DE-OS 21 27 611, for instance, describes the production of spice extracts using supercritical COz for extracting ethereal oils. Gases such as N20, SF6, CI?3C1, CAFzCl, ethane, ethylene, etc. are known as extracting agents. DE-OS 28 27 002 describes the extraction of hop by means of COZ and patent DE-OS 33 39 181, the owner of which is the applicant, deals with a process for the decaffeination of tea leaves. Finally patent DE-OS 32 13 595 relates to the regeneration of caffeine-laden activated carbon with the aid of hot water.
The extraction only represents one step of the overall process for the production of ingredients, the mixture of extracting agent and ingredients has to be subjected to a separation process in order to obtain the ingredient substances. A known method is to expand the high-pressure solvent and ingredients via a relief valve and to evaporate the solvent in a further step, the extract collecting in a precipitation vesse 1. All process units are interconnected with pipes.
Such processes cause major difficulties if, for instance, the ingredients are of a high viscosity. If said substances already precipitate when the mixture is depressurized in t:he valves or pipes, said components will become clogged and sticky.
The major objective of the invention is, inter alia, to provide an unsophisticated and rapid method of separation for ingredients of high viscosity.
The invention provides for a method of separating a mixture coming from an extractor and comprising solvents and ingredient substances: in which method the mixture is relieved from an extraction pressure to a lower pressure and passed into a large-volume container. For the separation of high-viscosity substances contained in the mixture from the solvent, the mixture is sprayed by way of a pressure-relief valve directly into the large-volume container.
This process combines expansion, evaporation and precipitation in a single vessel, thus avoiding pipe or valve clogging because t;he ingredients immediately precipitate in a large chamber.
An embodiment of the invention provides for the expansion of the mixture into a large heated chamber. This method is particularly useful if the viscosity of the ingredients can be reduced by heating, thus facilitating the precipitation of said substances.
A variant of the embodiment described above is characterized in that the mixture is directly saturated with an evaporable solvent in the vicinity of the relief valve and/or in that the mixture is expanded in a large chamber filled or saturated with a vaporized solvent.
The invention also provides for a device required for the implementation of the process described above, the device comprising a pressure vessel with feed means for the mixture and discharge conduits for the separated solvent.
The device for implementing the process is characterized in that the pressure vessel wall and, preferably, the pressure vessel cover have a relief valve for injecting the mixture directly into the pressure vessel.
If the pressure vessel cover can be equipped with only one inlet device to meet design requirements, the invention provides for a valve seat mounted directly on the inlet opening.
In order to facilitate the emptying of the vessel, the invention provides for a collecting vessel for the ingredients within the pressure vessel.
It is useful t:o install a heating device in the pressure vessel in order to permit direct heating of the collecting vessel. To this en.d, a heating system such as a heating coil is installed between the outside of the collecting vessel wall and the insides of the pressure vessel shell.
In order to withdraw the extract from the pressure vessel, the invention provides for a vessel design permitting removal of the collecting vessel from the pressure vessel via its bottom equipped with quick-release clamping devices.
The invention is explained below on the basis of the following drawings:
Fig. 1: Cross-sectional view of the pressure vessel, simplified configuration Fig. 2: Detail drawing of a valve seat in the pressure vessel cover Device 1 in Figure 1 consists of an essentially cylindrical pressure vessel 2 with cover 3 and bottom 4, the latter being remov<~d by means of hydraulic system 5, once the quick-release clamping device 6 has been actuated.
Pressure vessel 2 accommodates collecting vessel 7 for the extracted ingredients 8, vessel 7 being equipped with heating coil 9.
Processes are known in which the ingredient substances are extracted with the aid of solvents. Patent DE-OS 21 27 611, for instance, describes the production of spice extracts using supercritical COz for extracting ethereal oils. Gases such as N20, SF6, CI?3C1, CAFzCl, ethane, ethylene, etc. are known as extracting agents. DE-OS 28 27 002 describes the extraction of hop by means of COZ and patent DE-OS 33 39 181, the owner of which is the applicant, deals with a process for the decaffeination of tea leaves. Finally patent DE-OS 32 13 595 relates to the regeneration of caffeine-laden activated carbon with the aid of hot water.
The extraction only represents one step of the overall process for the production of ingredients, the mixture of extracting agent and ingredients has to be subjected to a separation process in order to obtain the ingredient substances. A known method is to expand the high-pressure solvent and ingredients via a relief valve and to evaporate the solvent in a further step, the extract collecting in a precipitation vesse 1. All process units are interconnected with pipes.
Such processes cause major difficulties if, for instance, the ingredients are of a high viscosity. If said substances already precipitate when the mixture is depressurized in t:he valves or pipes, said components will become clogged and sticky.
The major objective of the invention is, inter alia, to provide an unsophisticated and rapid method of separation for ingredients of high viscosity.
The invention provides for a method of separating a mixture coming from an extractor and comprising solvents and ingredient substances: in which method the mixture is relieved from an extraction pressure to a lower pressure and passed into a large-volume container. For the separation of high-viscosity substances contained in the mixture from the solvent, the mixture is sprayed by way of a pressure-relief valve directly into the large-volume container.
This process combines expansion, evaporation and precipitation in a single vessel, thus avoiding pipe or valve clogging because t;he ingredients immediately precipitate in a large chamber.
An embodiment of the invention provides for the expansion of the mixture into a large heated chamber. This method is particularly useful if the viscosity of the ingredients can be reduced by heating, thus facilitating the precipitation of said substances.
A variant of the embodiment described above is characterized in that the mixture is directly saturated with an evaporable solvent in the vicinity of the relief valve and/or in that the mixture is expanded in a large chamber filled or saturated with a vaporized solvent.
The invention also provides for a device required for the implementation of the process described above, the device comprising a pressure vessel with feed means for the mixture and discharge conduits for the separated solvent.
The device for implementing the process is characterized in that the pressure vessel wall and, preferably, the pressure vessel cover have a relief valve for injecting the mixture directly into the pressure vessel.
If the pressure vessel cover can be equipped with only one inlet device to meet design requirements, the invention provides for a valve seat mounted directly on the inlet opening.
In order to facilitate the emptying of the vessel, the invention provides for a collecting vessel for the ingredients within the pressure vessel.
It is useful t:o install a heating device in the pressure vessel in order to permit direct heating of the collecting vessel. To this en.d, a heating system such as a heating coil is installed between the outside of the collecting vessel wall and the insides of the pressure vessel shell.
In order to withdraw the extract from the pressure vessel, the invention provides for a vessel design permitting removal of the collecting vessel from the pressure vessel via its bottom equipped with quick-release clamping devices.
The invention is explained below on the basis of the following drawings:
Fig. 1: Cross-sectional view of the pressure vessel, simplified configuration Fig. 2: Detail drawing of a valve seat in the pressure vessel cover Device 1 in Figure 1 consists of an essentially cylindrical pressure vessel 2 with cover 3 and bottom 4, the latter being remov<~d by means of hydraulic system 5, once the quick-release clamping device 6 has been actuated.
Pressure vessel 2 accommodates collecting vessel 7 for the extracted ingredients 8, vessel 7 being equipped with heating coil 9.
Cover 3 has a conical seat 10 located in the centre and required for valve rod 11. Said rod slides up and down in valve body 12 (see arrows 13) in order to open and close spray orifice 14.
The mixture from the extractor is fed to vessel 2 via line 15, which communicates with valve body 12, and it enters said vessel through the valve seat 10 in cover 3. The extracting agent, e.g. CO2, leaves device 1 via line 16, arrow 17 showing the flow direction.
When the mixture has been injected into the heated chamber of vessel 1 (indicated by arrow 18), the extracting agent is separated from the ingredient substances at a pressure lower than. that of the solvent, said substances collecting in vessel 7. The viscosity is controlled by means of heating coil 9.
In order to withdraw the extract from the vessel, the quick-release clamping devices 6 of bottom 4 are actuated and the bottom is lowered so that vessel 7 can be replaced by an empty vessel which is inserted and secured by means of clamping device 6.
If a valve seat cannot be arranged in vessel cover 3, the assembly shown in Figure 2 is installed. In this case, the valve and seat l0a are mounted on cover 3a, the injection orifice being funnel-shaped.
It is of course possible to vary the embodiments described in this application but yet to maintain the design principle. Severa7_ valve seats can be installea in zne cover for injecting large quantities. Furthermore, feed lines for hot air, superheated steam, hot solvent, etc. may be provided but are not shown in the diagrams. Apart from the heating coil, other types of heating are suitable, e.g. inductive heaters.
The mixture from the extractor is fed to vessel 2 via line 15, which communicates with valve body 12, and it enters said vessel through the valve seat 10 in cover 3. The extracting agent, e.g. CO2, leaves device 1 via line 16, arrow 17 showing the flow direction.
When the mixture has been injected into the heated chamber of vessel 1 (indicated by arrow 18), the extracting agent is separated from the ingredient substances at a pressure lower than. that of the solvent, said substances collecting in vessel 7. The viscosity is controlled by means of heating coil 9.
In order to withdraw the extract from the vessel, the quick-release clamping devices 6 of bottom 4 are actuated and the bottom is lowered so that vessel 7 can be replaced by an empty vessel which is inserted and secured by means of clamping device 6.
If a valve seat cannot be arranged in vessel cover 3, the assembly shown in Figure 2 is installed. In this case, the valve and seat l0a are mounted on cover 3a, the injection orifice being funnel-shaped.
It is of course possible to vary the embodiments described in this application but yet to maintain the design principle. Severa7_ valve seats can be installea in zne cover for injecting large quantities. Furthermore, feed lines for hot air, superheated steam, hot solvent, etc. may be provided but are not shown in the diagrams. Apart from the heating coil, other types of heating are suitable, e.g. inductive heaters.
Claims (10)
1. A method of separating a mixture coming from an extractor and comprising solvents and ingredient substances, in which method the mixture is relieved from an extraction pressure to a lower pressure and passed into a large-volume container, and wherein for the separation of high-viscosity substances contained in the mixture from the solvent, the mixture is sprayed by way of a pressure-relief valve directly into the large-volume container.
2. The method according to claim 1, wherein the large-volume container in which the mixture is relieved of pressure is heated.
3. The method according to claim 1 or 2, wherein the mixture is mixed directly with evaporating solvent in the region of the pressure-relief valve.
4. The method according to claim 1, 2 or 3, wherein the large-volume container in which the mixture is relieved of pressure is filled with solvent vapour.
5. An apparatus for carrying out the method according to any one of claims 1 to 4 comprising:
a pressure vessel;
feed means for the mixture; and discharge conduits for the solvent which is separated from the mixture;
wherein a pressure-relief valve for directly feeding the mixture into the pressure vessel is provided in a wall of the pressure vessel.
a pressure vessel;
feed means for the mixture; and discharge conduits for the solvent which is separated from the mixture;
wherein a pressure-relief valve for directly feeding the mixture into the pressure vessel is provided in a wall of the pressure vessel.
6. The apparatus according to claim 5, wherein the pressure-relief valve is provided in a cover of the pressure vessel.
7. The apparatus according to claim 5 or 6, wherein a valve seat is mounted directly on the pressure vessel with a feed opening for the mixture under pressure.
8. The apparatus according to claim 5, 6 or 7, wherein a collecting vessel for the substances contained in the mixture is provided in the pressure vessel.
9. The apparatus according to claim 8, wherein heating means is provided between an outside wall of the collecting vessel and an inside wall of the pressure vessel.
10. The apparatus according to claim 8 or 9, wherein the collecting vessel can be removed from and fitted into the pressure vessel by way of a bottom provided with a quick-action closure.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEP3906169.8 | 1989-02-28 | ||
| DE3906169A DE3906169A1 (en) | 1989-02-28 | 1989-02-28 | METHOD AND DEVICE FOR SEPARATING A MIXTURE COMING FROM AN EXTRACTOR |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2010972A1 CA2010972A1 (en) | 1990-08-31 |
| CA2010972C true CA2010972C (en) | 2001-06-19 |
Family
ID=6375079
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002010972A Expired - Lifetime CA2010972C (en) | 1989-02-28 | 1990-02-27 | Process and device for separating a mixture of ingredient substances from the extracting agent |
Country Status (7)
| Country | Link |
|---|---|
| EP (1) | EP0385130B1 (en) |
| JP (1) | JP3032544B2 (en) |
| KR (1) | KR900012653A (en) |
| AT (1) | ATE98889T1 (en) |
| CA (1) | CA2010972C (en) |
| DE (2) | DE3906169A1 (en) |
| ZA (1) | ZA901469B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19702266A1 (en) * | 1997-01-23 | 1998-07-30 | Huels Chemische Werke Ag | Degassing apparatus for all non=Newtonian fluid(s), especially plastic melt |
| JP2007173253A (en) * | 2007-02-13 | 2007-07-05 | Dai Ichi High Frequency Co Ltd | Heat-treatment device |
Family Cites Families (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2166999A (en) * | 1936-12-24 | 1939-07-25 | Smith Corp A O | Quick opening pressure vessel |
| DE1035105B (en) * | 1956-04-19 | 1958-07-31 | Siemens Ag | Electrically heated kiln |
| NL6710359A (en) * | 1967-07-27 | 1969-01-29 | ||
| DE2127611C3 (en) * | 1971-06-03 | 1974-11-14 | Studiengesellschaft Kohle Mbh, 4330 Muelheim | Process for the production of spice extracts with a natural composition |
| US4115072A (en) * | 1977-04-07 | 1978-09-19 | Chevron Research Company | Retractable fluids spraying assembly |
| DE2827002B2 (en) * | 1978-06-20 | 1980-09-04 | Adam Dr. 8421 St Johann Mueller | Process for treating hops with CO2 as extraction agent |
| US4294652A (en) * | 1980-06-30 | 1981-10-13 | Monsanto Company | Falling strand devolatilizer |
| LU82835A1 (en) * | 1980-10-10 | 1981-02-02 | Labexplor Res Corp | METHOD FOR LIQUID EXTRACTION |
| AT373932B (en) * | 1981-11-12 | 1984-03-12 | Chemiefaser Lenzing Ag | METHOD FOR RECONSTRUCTING USED DIGESTIVE FLUID FLOWING GEAR, AND PLANTS FOR IMPLEMENTING THIS METHOD |
| DE3213592A1 (en) * | 1982-04-13 | 1983-10-20 | HAG GF AG, 2800 Bremen | Regeneration of caffeine-loaded active carbon with hot water |
| ZA839116B (en) * | 1982-12-16 | 1984-07-25 | Cpc International Inc | Heat-pressure-expansion process for drying pure sugars or starch hydrolysates to prepare a free-flowing powder |
| DE3339181A1 (en) * | 1983-10-28 | 1985-05-09 | Uhde Gmbh, 4600 Dortmund | METHOD AND DEVICE FOR DECAFFINATING TEA LEAVES |
| FR2603817B1 (en) * | 1986-09-15 | 1988-11-25 | Commissariat Energie Atomique | APPARATUS FOR DISTILLING BY VACUUM EVAPORATION |
-
1989
- 1989-02-28 DE DE3906169A patent/DE3906169A1/en not_active Withdrawn
-
1990
- 1990-02-03 EP EP90102169A patent/EP0385130B1/en not_active Expired - Lifetime
- 1990-02-03 DE DE90102169T patent/DE59003915D1/en not_active Expired - Lifetime
- 1990-02-03 AT AT90102169T patent/ATE98889T1/en not_active IP Right Cessation
- 1990-02-16 KR KR1019900001915A patent/KR900012653A/en not_active Application Discontinuation
- 1990-02-22 JP JP2039896A patent/JP3032544B2/en not_active Expired - Lifetime
- 1990-02-27 ZA ZA901469A patent/ZA901469B/en unknown
- 1990-02-27 CA CA002010972A patent/CA2010972C/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| DE3906169A1 (en) | 1990-08-30 |
| JPH02241502A (en) | 1990-09-26 |
| ATE98889T1 (en) | 1994-01-15 |
| EP0385130A2 (en) | 1990-09-05 |
| DE59003915D1 (en) | 1994-02-03 |
| EP0385130B1 (en) | 1993-12-22 |
| CA2010972A1 (en) | 1990-08-31 |
| JP3032544B2 (en) | 2000-04-17 |
| KR900012653A (en) | 1990-09-01 |
| EP0385130A3 (en) | 1991-01-02 |
| ZA901469B (en) | 1990-12-28 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EEER | Examination request | ||
| MKLA | Lapsed | ||
| MKEC | Expiry (correction) |
Effective date: 20121202 |