CN103611331B - A kind of supercritical extraction/reaction integrated apparatus - Google Patents
A kind of supercritical extraction/reaction integrated apparatus Download PDFInfo
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- CN103611331B CN103611331B CN201310666641.6A CN201310666641A CN103611331B CN 103611331 B CN103611331 B CN 103611331B CN 201310666641 A CN201310666641 A CN 201310666641A CN 103611331 B CN103611331 B CN 103611331B
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 41
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 23
- 238000000605 extraction Methods 0.000 claims abstract description 68
- 239000012530 fluid Substances 0.000 claims abstract description 38
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 239000000284 extract Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 12
- 238000001514 detection method Methods 0.000 claims description 6
- 230000004044 response Effects 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 3
- 230000010354 integration Effects 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 239000002351 wastewater Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 229920005610 lignin Polymers 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000010525 oxidative degradation reaction Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- -1 react Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000009284 supercritical water oxidation Methods 0.000 description 2
- LVGUZGTVOIAKKC-UHFFFAOYSA-N 1,1,1,2-tetrafluoroethane Chemical compound FCC(F)(F)F LVGUZGTVOIAKKC-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 241000736199 Paeonia Species 0.000 description 1
- 235000006484 Paeonia officinalis Nutrition 0.000 description 1
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- 239000002537 cosmetic Substances 0.000 description 1
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- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910017053 inorganic salt Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
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- 238000012827 research and development Methods 0.000 description 1
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- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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Abstract
The present invention relates to a kind of supercritical device, particularly relate to a kind of supercritical extraction/reaction integrated apparatus, described extraction fluid reservoir I passes sequentially through condenser, pump I is connected with mixer entrance I, mixer outlet is connected with extraction cells entrance, and extraction cells outlet I is connected with separative element by valve V；Anti-applicating fluid and entrainer storage tank II are connected with pump II entrance, and pump II is exported I and is connected with mixer entrance II by valve I, pump II export II pass sequentially through valve II, give hot device II, valve III is connected with reactor entrance I；Reactor outlet passes sequentially through valve VI, quencher is connected with gas-liquid separator；Extraction cells outlet II is connected with reactor entrance II by valve IV, and the present invention has the beneficial effect that and can realize individually extracting, reacting, and can realize again extraction/reaction integration operation.
Description
Technical field
The present invention relates to a kind of supercritical device, particularly relate to a kind of supercritical extraction/reaction integrated apparatus.
Background technology
The characteristic of the existing gas of supercritical fluid, have again some characteristics of liquid concurrently, some character is between gas and the character of liquid, the density of supercritical fluid is close to the density of liquid, viscosity and diffusion coefficient etc. are close with gas, this makes they existing strong solvabilities, has again strong diffusivity.And these character such as density, viscosity, diffusion coefficient, dielectric constant, solvability etc., can be adjusted by pressure and temperature within the specific limits, especially pronounced in this regulation effect of its Near The Critical Point.
Various advantages energy based on supercritical fluid, to it further with receiving much concern.Wherein supercritical extraction technique can not be ignored with the superiority of supercritical fluid reaction technology, and its application relates to numerous industries such as chemical industry, biology, medicine, environmental protection, cosmetics, health, food, printing and dyeing, new material especially.Supercritical extraction technique especially supercritical CO2Extraction, because its supercritical temperature (31.1 DEG C) and supercritical pressure (7.387MPa) are relatively low, operating condition is relatively mild, the highest to equipment requirements, and density is close to liquid, there is the biggest solvability, viscosity close to gas, diffusivity big more than 100 times than liquid, solvability and selectivity can be adjusted by changing pressure and temperature, extraction rate is fast, and the characteristics such as the operating time is short receive much concern.Shooting flow precursor reactant especially supercritical water oxidation, utilize what water was had in the supercritical state special nature (weak hydrogen bond action, dielectric constant is similar to organic solvent, high diffusion coefficient, low viscosity etc.), can be used for all conglomeraties and decompose if any machine waste water exhaustive oxidation, Toxic, hardly degraded organic substance are degraded, lignin depolymerization etc., completely, thoroughly, end product is water, N to oxidative degradation2、CO2Etc. the inorganic matter of little molecule, and the dissolubility that inorganic salt is in supercritical water is the lowest, can be easily separated, processed waste water recoverable, additionally by controlling the temperature and pressure of reaction, can selective adjustment degree of oxidation, obtain small organic molecule, for chemical industry after separation.In recent years, mixing such as water and other Organic substances such as ethanol, phenol, acetone etc. is jointly processed by biomass as supercritical fluid and produces basic chemical and become the trend that becomes popular.And, the specific components that supercritical extraction technique combines with supercritical reaction technology in process organic wastewater, treated substance becomes new development direction, the most gradually such as supercritical CO2From organic wastewater, extract organic component, by supercritical water reaction, organic component oxidative degradation become gas preparing gas fuel；From waste agronomic crop or black liquid, extract lignin, carry out depolymerization with supercritical water/ethanol, produce small-molecule chemical product or liquid fuel etc..And there is no report both at home and abroad for extraction/reaction integrated equipment for wastewater treatment, but supercritical extraction and reaction separate device have some to report, as CN1994507A discloses a kind of low-pressure supercritical extraction process and device, this equipment mainly meets 1,1,1,2-tetrafluoroethane is as the working condition of supercritical fluid, and operating pressure is 0.8～8.0MPa, and pressure limit is less, the extraction fluid that equipment can use is single, it is impossible to be widely used in as supercritical CO2Equitemperature and the slightly higher fluid of pressure, it is impossible to be widely used.Same CN102391912A also discloses the supercritical extracting equipment of a kind of peony essential oil, and equipment is mainly for the purpose of abstracting tree peony quintessence oil, and equipment has the specificity of height, is not suitable for extracting other raw materials, restricted bigger.Two kinds of extraction equipments all have the highest specificity, it is difficult to extensively extract object from solid (such as agricultural wastes), liquid (organic wastewater).CN202786160U discloses a kind of tubular type supercritical biomass by hydrolyzation liquefying plant, CN201632252U discloses a kind of tower supercritical reaction apparatus, CN101164912A discloses a kind of corrosion-resisting clogging-proof overcritical water oxidation reaction apparatus, three all describes supercritical reaction apparatus, all can realize the purpose of supercritical water oxidation degraded raw material, but use type of fluid single, it is impossible to adapt to the research purpose to Supercritical Ethanol, phenol, acetone etc..The most do not occur that supercritical extraction and supercritical reaction integration apparatus, especially equipment can use fluid to have general applicability such as water, ethanol, phenol, acetone, CO both at home and abroad2All can use and an integration apparatus vacancy especially of temperature and pressure intelligentized control method, the present invention is precisely in order to adapt to current research and development needs, meet from extraction, be reacted to the operation of material isolation integral, multiple supercritical fluid is used in mixed way and is equipped with entrainer and jointly acts on, and the highly scientific research of intelligent precise numerical monitor requires and designs creation.
Summary of the invention
The present invention is directed to supercritical extraction and consersion unit in prior art cannot meet equipment general applicability, the integration operation of supercritical extraction/reaction, multiple fluid mixing and jointly act on entrainer, the modern scientific research requirement such as digital display, the supercritical extraction of design/reaction integrated apparatus.
The invention provides a kind of supercritical extraction/reaction integrated apparatus, described storage tank I passes sequentially through condenser, pump I is connected with mixer entrance I, and mixer outlet is connected with extraction cells entrance, and extraction cells outlet I is connected with separative element by valve V；Storage tank II is connected with pump II entrance, and pump II is exported I and is connected with mixer entrance II by valve I, and pump II exports and II passes sequentially through valve II, preheater II, valve III are connected with reactor entrance I；Reactor outlet passes sequentially through valve VI, quencher is connected with gas-liquid separator；Extraction cells outlet II is connected with reactor entrance II by valve IV.
Supercritical device of the prior art is only used for reaction or the extraction of a kind of material, and extraction equipment and reaction unit are separate, there is no the device of integration, supercritical extraction and supercritical reaction are combined together by the present invention, realize supercritical extraction the most close-coupled processing to supercritical reaction, convection cell has general applicability simultaneously, both single fluid extraction/reaction had been met, meeting again multiple fluid mixing complicated extraction/course of reaction coefficient with entrainer, three separate lines meet and extracts, react, extract/react difference requirement.
Extraction cells of the present invention preferably comprises preheater I, several extraction kettles, and preheater I outlet is connected with the extraction kettle of several parallel connections.
The extraction kettle volume of several parallel connections of the present invention is different, can meet the requirement to extraction kettle volume of the different material amount.
Separative element of the present invention includes preheater III, coarse separator, preheater IV, fine seperator, and the outlet of described preheater III passes sequentially through coarse separator, preheater IV is connected with fine seperator entrance.
Storage tank of the present invention I is preferably and is connected with bus-bar entrance I, and the outlet of described bus-bar passes sequentially through filter I, depurator, filter II, condenser, pump I are connected with mixer entrance I.
Depurator of the present invention sets 3A molecular sieve in being preferably.
Separative element gas outlet of the present invention is preferably and is connected with bus-bar entrance II.
Present invention have the beneficial effect that
1. can realize single extracting operation or operation, extraction/reaction integration operation can be realized again；
2. the most applicable to solid, liquid charging stock；
The most simple to operate, safe and reliable；
4. different inventories can be extracted or alternately extraction by the extraction kettle of several parallel connections.
Accompanying drawing explanation
Accompanying drawing 1 width of the present invention,
Fig. 1 is the supercritical extraction in embodiment 1/reaction integrated apparatus structural representation；
Wherein, 1, storage tank I, 2, bus-bar, 3, filter I, 4, depurator, 5, filter II, 6, condenser, 7, pump I, 8, blender, 9, extraction cells, 10, separative element, 11, storage tank II, 12, pump II, 13, preheater II, 14, reactor, 15, quencher, 16, gas-liquid separator, 17～22, valve I～valve VI, 91, preheater I, 92, extraction kettle I, 93, extraction kettle II, 101, preheater III, 102, coarse separator, 103, preheater IV, 104, fine seperator.
Detailed description of the invention
Following non-limiting example can make those of ordinary skill in the art that the present invention is more fully understood, but limits the present invention never in any form.
Embodiment 1
A kind of supercritical extraction/reaction integrated apparatus, described storage tank I 1 is connected with bus-bar 2 entrance I, the outlet of described bus-bar 2 passes sequentially through filter I 3, depurator 4, filter II 5, condenser 6, pump I 7 are connected with blender 8 entrance I, blender 8 outlet is connected with extraction cells 9 entrance, extraction cells 9 is exported I and is connected with separative element 10 by valve V 21, and described separative element 10 gas outlet is connected with bus-bar 2 entrance II；Storage tank II 11 is connected with pump II 12 entrance, and pump II 12 outlet I is connected with blender 8 entrance II by valve I 17, and pump II 12 exports and II passes sequentially through valve II 18, preheater II 13, valve III 19 are connected with reactor 14 entrance I；Reactor 14 outlet passes sequentially through valve VI 22, quencher 15 is connected with gas-liquid separator 16；Extraction cells 9 is exported II and is connected with reactor 14 entrance II by valve IV 20；
Described extraction cells 9 includes that preheater I 91, extraction kettle I 92, extraction kettle II 93, preheater I 91 outlet are connected with extraction kettle I 92, II 93 in parallel, and extraction kettle I 92 and extraction kettle II 93 volumetric ratio are 5:1；
Described separative element 10 includes preheater III 101, coarse separator 102, preheater IV 103, fine seperator 104, the outlet of described preheater III 101 passes sequentially through coarse separator 102, preheater IV 103 is connected with fine seperator 104 entrance, and described coarse separator 102 is 2:1 with fine seperator 104 volumetric ratio；
3A molecular sieve is set in described depurator 4.
Application examples 1
It is applied to supercritical extraction:
Thing to be extracted is loaded in extraction kettle I 92, valve closing II 18, valve IV 20 is closed after device emptying leak detection, opening pump I 7, in storage tank I 1, extraction fluid passes sequentially through bus-bar 2, filter I 3, depurator 4, filter II 5, condenser 6, pump I 7 inflow blender 8；Open pump II 12, in storage tank II 11, entrainer is flowed into after blender 8 mixes with extraction fluid by pump II 12 and heats up through preheater I 91, flow in extraction kettle I 92 after arriving temperature and extract, after extraction, fluid flows into coarse separator 102 just separation by preheater III 101, flowing into fine seperator 104 by preheater IV 103 after just separating makes gas separate with extract, gas returns bus-bar 2 through check-valves, and extract is from additionally exporting collection.
Application examples 2
It is applied to supercritical reaction:
Question response thing is loaded in reactor 14, after device emptying leak detection, close valve closing I 17, valve IV 20, valve VI 22.Open pump II 12, in storage tank II 11, anti-applicating fluid flows into reactor 14 by pump II 12, preheater II 13, as needed another kind of anti-applicating fluid to participate in reaction, valve I 17 can be opened, open pump I 7, in storage tank I 1, anti-applicating fluid passes sequentially through bus-bar 2, filter I 3, depurator 4, filter II 5, condenser 6, pump I 7, blender 8, preheater II 13 inflow reactor 14, reaction opens valve VI 22 after terminating, after reaction, fluid flows into gas-liquid separator 16 through quencher 15, gas is collected through manual counterbalance valve air bag, and liquid is from additionally exporting collection.
Application examples 3
It is applied to supercritical extraction/reaction:
nullThing to be extracted is loaded in extraction kettle I 92、Question response thing loads in reactor 14，Valve closing V 21 is closed after device emptying leak detection，Open pump I 7，In storage tank I 1, extraction fluid passes sequentially through bus-bar 2、Filter I 3、Depurator 4、Filter II 5、Condenser 6、Pump I 7 flows into blender 8，Close valve closing II 18、Valve III 19、Valve VI 22，In storage tank II 11, entrainer is mixed by pump II 12 inflow blender 8，Heat up through preheater I 91 after mixing，Flow in extraction kettle I 92 after arriving temperature and extract，After extraction, the fluid with extract flows into reactor 14，Close valve closing IV 20、Valve I 17，Open valve II 18、Valve III 19，Open pump II 12，In storage tank II 11, anti-applicating fluid is through pump II 12、Preheater II 13 flows into reactor 14 and reacts with extract，Reaction opens valve VI 22 after terminating，After reaction, fluid flows into gas-liquid separator 16 through quencher 15，Gas is collected through counterbalance valve air bag，Liquid is from additionally exporting collection.
Claims (4)
1. supercritical extraction/reaction integrated apparatus, it is characterized in that: storage tank I (1) is connected with bus-bar (2) entrance I, bus-bar (2) outlet passes sequentially through filter I (3), depurator (4), filter II (5), condenser (6), pump I (7) is connected with blender (8) entrance I, blender (8) outlet is connected with extraction cells (9) entrance, extraction cells (9) outlet I is connected with separative element (10) by valve V (21), separative element (10) gas outlet is connected with bus-bar (2) entrance II；Storage tank II (11) is connected with pump II (12) entrance, pump II (12) outlet I is connected with blender (8) entrance II by valve I (17), and pump II (12) exports and II passes sequentially through valve II (18), preheater II (13), valve III (19) are connected with reactor (14) entrance I；Reactor (14) outlet passes sequentially through valve VI (22), quencher (15) is connected with gas-liquid separator (16)；Extraction cells (9) outlet II is connected with reactor (14) entrance II by valve IV (20)；
Extraction cells (9) includes preheater I (91), extraction kettle I (92), extraction kettle II (93), preheater I (91) outlet is connected with extraction kettle I (92) in parallel, extraction kettle II (93), and extraction kettle I (92) and extraction kettle II (93) volumetric ratio are 5:1；
Separative element (10) includes preheater III (101), coarse separator (102), preheater IV (103), fine seperator (104), preheater III (101) outlet passes sequentially through coarse separator (102), preheater IV (103) is connected with fine seperator (104) entrance, and coarse separator (102) and fine seperator (104) volumetric ratio are 2:1；
Depurator sets 3A molecular sieve in (4).
2. one kind utilizes the method for device supercritical extraction described in claim 1, it is characterized in that: described method is for loading in extraction kettle I (92) by thing to be extracted, valve closing II (18), valve IV (20) is closed after device emptying leak detection, opening pump I (7), the interior extraction fluid of storage tank I (1) passes sequentially through bus-bar (2), filter I (3), depurator (4), filter II (5), condenser (6), pump I (7) inflow blender (8)；Open pump II (12), the interior entrainer of storage tank II (11) is flowed into after blender (8) mixes with extraction fluid by pump II (12) and heats up through preheater I (91), extraction in extraction kettle I (92) is flowed into after arriving temperature, after extraction, fluid is just separated by preheater III (101) inflow coarse separator (102), flowing into fine seperator (104) by preheater IV (103) after just separating makes gas separate with extract, gas returns bus-bar (2) through check-valves, and extract is from additionally exporting collection.
null3. one kind utilizes the method for device supercritical reaction described in claim 1，It is characterized in that: described method is for loading question response thing in reactor (14)，Valve closing I (17) is closed after device emptying leak detection、Valve IV (20)、Valve VI (22)，Open pump II (12)，In storage tank II (11), anti-applicating fluid passes through pump II (12)、Preheater II (13) flows into reactor (14)，As needed another kind of anti-applicating fluid to participate in reaction，Valve I (17) can be opened，Open pump I (7)，In storage tank I (1), anti-applicating fluid passes sequentially through bus-bar (2)、Filter I (3)、Depurator (4)、Filter II (5)、Condenser (6)、Pump I (7)、Blender (8)、Preheater II (13) flows into reactor (14)，Reaction opens valve VI (22) after terminating，After reaction, fluid flows into gas-liquid separator (16) through quencher (15)，Gas is collected through manual counterbalance valve air bag，Liquid is from additionally exporting collection.
null4. one kind utilizes the method for device supercritical extraction/reaction described in claim 1，It is characterized in that: described method is for loading thing to be extracted in extraction kettle I (92)、Question response thing loads in reactor (14)，Valve closing V (21) is closed after device emptying leak detection，Open pump I (7)，The interior extraction fluid of storage tank I (1) passes sequentially through bus-bar (2)、Filter I (3)、Depurator (4)、Filter II (5)、Condenser (6)、Pump I (7) flows into blender (8)，Close valve closing II (18)、Valve III (19)、Valve VI (22)，The interior entrainer of storage tank II (11) flows into blender (8) by pump II (12) and mixes，Heat up through preheater I (91) after mixing，Extraction in extraction kettle I (92) is flowed into after arriving temperature，After extraction, the fluid with extract flows into reactor (14)，Close valve closing IV (20)、Valve I (17)，Open valve II (18)、Valve III (19)，Open pump II (12)，In storage tank II (11), anti-applicating fluid is through pump II (12)、Preheater II (13) flows into reactor (14) and reacts with extract，Reaction opens valve VI (22) after terminating，After reaction, fluid flows into gas-liquid separator (16) through quencher (15)，Gas is collected through counterbalance valve air bag，Liquid is from additionally exporting collection.
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| CN109701296B (en) * | 2019-01-01 | 2022-05-06 | 中国人民解放军63653部队 | Corrosion-resistant multi-working-mode supercritical carbon dioxide extraction system |
| CN113413631A (en) * | 2021-07-09 | 2021-09-21 | 四川丁点儿食品开发股份有限公司 | Supercritical CO2Fluid dynamic countercurrent extraction separation system |
| CN113430053A (en) * | 2021-07-09 | 2021-09-24 | 四川丁点儿食品开发股份有限公司 | Fresh pepper oleoresin separation and purification process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994507A (en) * | 2006-12-05 | 2007-07-11 | 中国海洋大学 | A low-pressure supercritical extraction process and apparatus thereof |
| CN101225323A (en) * | 2008-02-03 | 2008-07-23 | 大连理工大学 | Method for preparing biodiesel from raw material by overcritical extraction-transesterification coupling process |
| CN201632252U (en) * | 2010-03-29 | 2010-11-17 | 郑州大学生化工程中心 | Tower-type supercritical reaction vessel |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1994507A (en) * | 2006-12-05 | 2007-07-11 | 中国海洋大学 | A low-pressure supercritical extraction process and apparatus thereof |
| CN101225323A (en) * | 2008-02-03 | 2008-07-23 | 大连理工大学 | Method for preparing biodiesel from raw material by overcritical extraction-transesterification coupling process |
| CN201632252U (en) * | 2010-03-29 | 2010-11-17 | 郑州大学生化工程中心 | Tower-type supercritical reaction vessel |
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