CN1294243C - Super critical CO2 precision separating process device - Google Patents
Super critical CO2 precision separating process device Download PDFInfo
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- CN1294243C CN1294243C CNB2004100757249A CN200410075724A CN1294243C CN 1294243 C CN1294243 C CN 1294243C CN B2004100757249 A CNB2004100757249 A CN B2004100757249A CN 200410075724 A CN200410075724 A CN 200410075724A CN 1294243 C CN1294243 C CN 1294243C
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Abstract
The present invention relates to a supercritical CO2 precise separation process device. The device is composed of a conjugate reaction process and a supercritical CO2 extraction process, which are formed in such a manner that an extraction kettle, a separator, a refrigeration compressor, settling tanks, solvent pumps, a water pump, a reaction kettle, an acid washing kettle, a raw material mixing tank, a heater, a heat exchanger, a mass flow meter, a raw material pump and connecting pipelines are connected. The present invention is characterized in that the raw material mixing tank, the raw material pump, the reaction kettle, the heat exchanger, the acid washing kettle, the small separator and a U-shaped tube are successively and sequentially connected in series in the conjugate reaction process. An extracting raw material inlet arranged at the upper part of the extraction kettle, the raw material pump and a raw material tank are successively connected with the U-shaped tube in the conjugate reaction process in series, an outlet of the extraction kettle and the separator are connected in series, a CO2 outlet of the separator and the inlets of two parallel settling tanks are connected in parallel, and the outlets of the two parallel settling tanks, and an inlet and an outlet of heat exchanged solvent of the solvent heat exchanger and an outlet of a CO2 storage tank are connected in series. An inlet of the refrigeration compressor and an outlet of the CO2 storage tank are connected in parallel, and an outlet of the refrigeration compressor and the inlets of two parallel solvent pumps are connected in parallel. The outlets of the two parallel solvent pumps and an inlet of the solvent heat exchanger are connected in parallel, and an outlet of the solvent heat exchanger and a solvent inlet at the bottom of the extraction kettle are connected in series.
Description
One, technical field
The present invention relates to a kind of device, specifically a kind of supercritical CO with Suaeda salsa vegetable seed production conjugated linolic acid
2The accurate separating technology device of producing.
Two, background technology
At present, the conjugated linolic acid kind of using in the society is a lot, and the production technique device is because of selecting the raw material difference for use, and also each is variant, but it is in short supply to exist desired raw material, and the problem of complex manufacturing can not satisfy social needs.The applicant has selected that be thick on the ground, resourceful, inexhaustible Suaeda salsa vegetable seed on natural, the alkali flat for use through long-term investigation, it is pressed the main raw material of oil as the production conjugated linolic acid, but be that the production technique of the production conjugated linolic acid of main raw material does not also have with the Suaeda salsa rapeseed oil.Research and development become the problem of urgent solution with the production technique of Suaeda salsa rapeseed oil production conjugated linolic acid.
Three, summary of the invention
The purpose of this invention is to provide a kind of supercritical CO
2The accurate separating technology device of producing solves with the Suaeda salsa rapeseed oil and produces the conjugated linolic acid problem.
Technical scheme of the present invention realizes in the following manner:
Conjugation reaction flow process and supercritical CO that the present invention is formed by connecting by extraction kettle, separator, refrigeration compressor, slurry tank, solvent pump, water pump, reactor, pickling still, raw material mixing tank, well heater, interchanger, mass flowmeter, feedstock pump and connecting pipeline
2Extraction procedure is formed, and it is characterized in that raw material mixing tank set in the conjugation reaction flow process, feedstock pump, reactor, interchanger, pickling still, little separator, U-shaped pipe successively are cascaded by preface; Supercritical CO
2The extraction feed import on the extraction kettle top that extraction procedure is set, feedstock pump, raw material mixing tank are serially connected by the U-shaped pipe in preface and the conjugation reaction flow process, and the outlet and the separator of extraction kettle are serially connected, separator CO
2Outlet and two slurry tanks in parallel inlet parallel together, the outlet of slurry tank and solvent interchanger by the import and export CO of heat exchange solvent
2The outlet of storage tank is serially connected, the import of refrigeration compressor and CO
2The outlet of storage tank is connected in parallel, the inlet parallel of the outlet of compressor and two solvent pumps in parallel together, the solvent pump outlet of two parallel connections is parallel to the import of solvent interchanger, the solvent heat exchanger exit is with the solvent inlet serial connection of extraction kettle bottom.
The pipeline that is located at the outlet of extraction kettle king-post top extraction mixed solution and is located between the import on separator top is provided with motor-driven control valve, is provided with manual modulation valve in motor-driven control valve one side, and the front of motor-driven control valve is provided with heated water bath.
At solvent pump outlet and extraction kettle bottom CO
2The pipeline of the import of solvent is provided with heated water bath.
Periphery and extraction kettle king-post periphery at extraction kettle are provided with heating jacket, the import of the heating jacket bottom of extraction kettle periphery and the outlet on top are with well heater, water pump serial connection, form closed circulation line, heating jacket on the king-post is divided into three sections from bottom to up, the import of every section heating jacket bottom and the outlet on top and well heater, water pump are serially connected, and form closed circulation line.
Periphery at reactor is provided with heating jacket, and the top of heating jacket is provided with a circulation import, is provided with a loop exit in the heating jacket bottom, and it is imported and exported with the recycle pump that is located at the reactor next door, the jar of heating and is serially connected, and forms closed circulation line.
Be provided with a pond on the top of interchanger, the import and export in pond and the cooling fluid of horizontal interchanger are imported and exported and are serially connected.
Compared with the prior art the present invention has the following advantages:
1, simple, reasonable in design, the control stabilization, easy to operate of technical process.
2, conjugation reaction technology combines with supercritical extraction process, makes main raw material with the Suaeda salsa rapeseed oil, the conjugated linolic acid super quality and competitive price of production.
Four, description of drawings
Fig. 1-process flow diagram of the present invention;
1-extraction kettle, 2-separator, 3-slurry tank, 4-CO among the figure
2Storage tank 5-refrigeration compressor 6-solvent pump 7-feedstock pump 8-water pump 9-raw material mixing tank 10-well heater 11-heated water bath 12-manual modulation valve 13-motor-driven control valve 14-solvent interchanger 15-raw material 16-heating tank 17-reactor 18-recycle pump 19-pond, 20-water pump, 21-interchanger, 22-pickling still 23-tank 24-little separator 25-U-shaped pipe
This flow process is except that the timing blowdown, and whole process of production all is to finish under airtight state.
Five, embodiment
For further disclosing technical scheme of the present invention, be described in detail by embodiment below in conjunction with Figure of description:
The present invention is by extraction kettle 1, separator 2, slurry tank 3, CO
2The supercritical CO of storage tank 4, refrigeration compressor 5, solvent pump 6, feedstock pump 7, water pump 8, well heater 10, heated water bath 11, manual modulation valve 12, motor-driven control valve 13, solvent interchanger 14, feedstock pump 15, composition
2Extraction procedure and form by the conjugation reaction flow process that raw material mixing tank 9, heating tank 16, reactor 17, recycle pump 18, pond 19, water pump 20, interchanger 21, pickling still 22, tank 23, little separator 24 and U-shaped pipe 25 are formed.Raw material mixing tank 9 in the conjugation reaction flow process, feedstock pump 15, reactor 17, interchanger 21, pickling still 22, little separator 24, U-shaped pipe 25 successively are serially connected by preface; Supercritical CO
2U-shaped pipe 25 in the extraction feed import on extraction kettle 1 top of extraction procedure, feedstock pump 7, raw material mixing tank 9 and the conjugation reaction flow process is serially connected, and the outlet at extraction kettle king-post top and two separators 2 are serially connected the CO at separator 2 tops by preface
2Outlet is connected in parallel with the lower inlet of two slurry tanks in parallel 3, and the outlet at slurry tank 3 tops and the import and export by the heat exchange solvent of solvent interchanger 14 are serially connected, and solvent interchanger 14 is by heat exchange solvent outlet and refrigeration compressor 5 imports, CO
2The outlet of storage tank 4 is connected in parallel, the inlet parallel of the outlet of compressor 5 and two solvent pumps in parallel 6 together, the outlet of the solvent pump 6 of two parallel connections and the inlet parallel of solvent interchanger 14 together, the import of the outlet of solvent interchanger 14 and extraction kettle 1 bottom is serially connected.
The present invention in actual applications, with water, the Suaeda salsa rapeseed oil, potassium hydroxide solution successively adds in the raw material mixing tank 9 in 1: 0.25～0.6: 2～4 mass percent ratio, squeeze in the reactor 17 with feedstock pump 15, before the adding, the stirrer rotating speed of reactor 17 is 400r/min, transfer to 800r/min after adding, be warming up to 180 ℃-210 ℃, with recycle pump 18, heating tank 16 is given the raw material heating cycle with reactor 17 periphery heating jackets, pressure-controlling is below 1.5MPa, be incubated 6-9 hour, then with interchanger 21 cooling heat exchange, (with water pump 20 with the water cycle in pond 19 in interchanger 21), raw material after the heat exchange enters and fills in the pickling still 22 of concentrated hydrochloric acid in the solution of 1: 1 ratio dilute with water, be stirred to complete molten after, the standing sedimentation separates two, the upper strata is a reaction oil, lower floor is a waste liquid, the reaction oil on upper strata is through little separator 24,25 incoming stock jars 9 of U-shaped pipes, add in the extraction kettle 1 with feedstock pump 7 with mass flowmeter 26 meterings by pipeline, before reaction oil adds, earlier be heated to 35 ℃ for the acid solution of extraction kettle 1, extract the temperature to 60 ℃ of king-post, CO with well heater 10
2The CO of storage tank 4
2With refrigeration compressor 5 compression condensations, pressurize through 14 heat exchange of solvent interchanger through solvent pump 6, through heated water bath 11 heating, enter the still from the bottom of extraction kettle 1, reaction oil in the still is extracted, and the extraction mixed solution comes out from extraction kettle king-post top, through heated water bath 11 heating, enter separator 2 and separate, the CO after the separation
2Enter two CO in parallel from separator 2 tops
2Slurry tank 3 settlement separate, the CO after the separation
2Lowered the temperature by heat exchange through the solvent interchanger,, carry out reciprocation cycle through solvent pump 6 extraction kettles 1 more again through the refrigeration compressor compression condensation.Sink to the bottom of separator 2 through separating 2 isolated transparent oily matter, it promptly is conjugated linolic acid, enter the finished product conjugated linolic acid jar from separator 2 bottoms, the waste liquid of extraction kettle bottom, waste liquid in the slurry tank 3 is discharged in the waste liquid storage pond, and the processing parameter of extraction is: compressor delivery pressure is 3-6MPa, and extraction kettle king-post pressure is 10-20MPa, in the extraction kettle temperature 35-60 ℃, 60-130 ℃ of extraction kettle king-post temperature.
Claims (6)
1, a kind of supercritical CO
2Accurate separating technology device, the conjugation reaction flow process and the supercritical CO that are formed by connecting by extraction kettle, separator, refrigeration compressor, slurry tank, solvent pump, water pump, reactor, pickling still, raw material mixing tank, well heater, interchanger, mass flowmeter, feedstock pump and connecting pipeline
2Extraction procedure is formed, and it is characterized in that raw material mixing tank set in the conjugation reaction flow process, feedstock pump, reactor, interchanger, pickling still, little separator, U-shaped pipe successively are cascaded by preface; Supercritical CO
2The extraction feed import on the extraction kettle top that extraction procedure is set, feedstock pump, raw material mixing tank are serially connected by the U-shaped pipe in preface and the conjugation reaction flow process, and the outlet and the separator of extraction kettle are serially connected, separator CO
2Outlet and two slurry tanks in parallel inlet parallel together, the outlet of slurry tank and solvent interchanger by the import and export CO of heat exchange solvent
2The outlet of storage tank is serially connected, the import of refrigeration compressor and CO
2The outlet of storage tank is connected in parallel, the inlet parallel of the outlet of compressor and two solvent pumps in parallel together, the solvent pump outlet of two parallel connections is parallel to the import of solvent interchanger, the solvent heat exchanger exit is with the solvent inlet serial connection of extraction kettle bottom.
2, supercritical CO according to claim 1
2Accurate separating technology device, pipeline between the import that it is characterized in that being located at the outlet of extraction kettle king-post top extraction mixed solution and being located at separator top is provided with motor-driven control valve, be provided with manual modulation valve in motor-driven control valve one side, the front of motor-driven control valve is provided with heated water bath.
3, supercritical CO according to claim 1
2Accurate separating technology device is characterized in that at solvent pump outlet and extraction kettle bottom CO
2The pipeline of the import of solvent is provided with heated water bath.
4, supercritical CO according to claim 1
2Accurate separating technology device, it is characterized in that being provided with heating jacket in the periphery and the extraction kettle king-post periphery of extraction kettle, the import of the heating jacket bottom of extraction kettle periphery and the outlet on top are with well heater, water pump serial connection, form closed circulation line, heating jacket on the king-post is divided into three sections from bottom to up, the import of every section heating jacket bottom and the outlet on top and well heater, water pump are serially connected, and form closed circulation line.
5, supercritical CO according to claim 1
2Accurate separating technology device, it is characterized in that being provided with heating jacket in the periphery of reactor, the top of heating jacket is provided with a circulation import, be provided with a loop exit in the heating jacket bottom, it is imported and exported with the recycle pump that is located at the reactor next door, the jar of heating and is serially connected, and forms closed circulation line.
6, supercritical CO according to claim 1
2Accurate separating technology device is characterized in that being provided with a pond on the top of interchanger, and the import and export in pond and the cooling fluid of horizontal interchanger are imported and exported and be serially connected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100757249A CN1294243C (en) | 2004-12-31 | 2004-12-31 | Super critical CO2 precision separating process device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100757249A CN1294243C (en) | 2004-12-31 | 2004-12-31 | Super critical CO2 precision separating process device |
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| Publication Number | Publication Date |
|---|---|
| CN1648224A CN1648224A (en) | 2005-08-03 |
| CN1294243C true CN1294243C (en) | 2007-01-10 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2004100757249A Expired - Fee Related CN1294243C (en) | 2004-12-31 | 2004-12-31 | Super critical CO2 precision separating process device |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534270A (en) * | 2011-12-27 | 2012-07-04 | 南华大学 | Multifunctional CO2 uranium leaching device |
| CN107557146B (en) * | 2017-09-27 | 2024-03-12 | 珠海澳盈生物科技有限公司 | Yolk oil extraction system with cleaning function |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5939571A (en) * | 1995-04-27 | 1999-08-17 | Sucher & Holzer Bauplanungs --und | Device and process for the production of oils or other extractable substances |
| CN1281032A (en) * | 2000-08-21 | 2001-01-24 | 孙传经 | Process for back extraction of medicinal plant oil with supercritical CO2 |
| CN1445346A (en) * | 2002-12-09 | 2003-10-01 | 陈宝义 | Method for preparing oil of ganoderma lucidum spores by supercritical Co2 extraction |
-
2004
- 2004-12-31 CN CNB2004100757249A patent/CN1294243C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5939571A (en) * | 1995-04-27 | 1999-08-17 | Sucher & Holzer Bauplanungs --und | Device and process for the production of oils or other extractable substances |
| CN1281032A (en) * | 2000-08-21 | 2001-01-24 | 孙传经 | Process for back extraction of medicinal plant oil with supercritical CO2 |
| CN1445346A (en) * | 2002-12-09 | 2003-10-01 | 陈宝义 | Method for preparing oil of ganoderma lucidum spores by supercritical Co2 extraction |
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| CN1648224A (en) | 2005-08-03 |
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