CN112430498B - Multi-basket step-by-step supercritical fluid extraction kettle - Google Patents
Multi-basket step-by-step supercritical fluid extraction kettle Download PDFInfo
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- CN112430498B CN112430498B CN202011306898.7A CN202011306898A CN112430498B CN 112430498 B CN112430498 B CN 112430498B CN 202011306898 A CN202011306898 A CN 202011306898A CN 112430498 B CN112430498 B CN 112430498B
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- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 24
- 238000000605 extraction Methods 0.000 claims abstract description 183
- 238000007789 sealing Methods 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims description 205
- 239000012530 fluid Substances 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 4
- 239000011148 porous material Substances 0.000 claims description 4
- 230000008676 import Effects 0.000 claims description 3
- 239000002994 raw material Substances 0.000 abstract description 55
- 230000000694 effects Effects 0.000 abstract description 13
- 230000005465 channeling Effects 0.000 abstract description 11
- 238000003825 pressing Methods 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000004519 grease Substances 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 238000010276 construction Methods 0.000 description 4
- 239000000284 extract Substances 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 230000002411 adverse Effects 0.000 description 3
- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000004744 fabric Substances 0.000 description 2
- 210000001503 joint Anatomy 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 244000105624 Arachis hypogaea Species 0.000 description 1
- 240000002791 Brassica napus Species 0.000 description 1
- 235000004977 Brassica sinapistrum Nutrition 0.000 description 1
- 240000001548 Camellia japonica Species 0.000 description 1
- 240000007049 Juglans regia Species 0.000 description 1
- 235000009496 Juglans regia Nutrition 0.000 description 1
- 235000004347 Perilla Nutrition 0.000 description 1
- 244000124853 Perilla frutescens Species 0.000 description 1
- 244000000231 Sesamum indicum Species 0.000 description 1
- 235000003434 Sesamum indicum Nutrition 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 235000018597 common camellia Nutrition 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 235000020232 peanut Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000020234 walnut Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/104—Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
Landscapes
- 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)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a multi-basket stepped step supercritical fluid extraction kettle which comprises a kettle body and a kettle cover, wherein the kettle body is provided with an extraction cavity, at least 2 sections of baskets are arranged in the extraction cavity, an extraction medium inlet is arranged at the bottom of the kettle body, a basket sealing device is arranged between the inner side wall of the kettle body and the outer wall of each section of basket, two adjacent sections of baskets are not connected with each other, a flow collecting region and a top flow collecting region between the two adjacent sections of baskets and the upper part of the uppermost basket are respectively arranged, a top extraction medium outlet and a top extraction medium outlet which are aligned with the top flow collecting region and the flow collecting region between the baskets are arranged on the kettle body, and the top extraction medium outlet and the outlet end of the extraction medium outlet between the baskets are connected with a closing device. The invention can realize the step-by-step extraction of the raw materials in the multi-basket from bottom to top, avoids channeling and caking phenomena of the raw materials with high oil content in the extraction process, ensures stable, rapid and thorough extraction, and improves the extraction efficiency and effect.
Description
Technical Field
The invention relates to the technical field of supercritical fluid extraction, in particular to a multi-basket step-step supercritical fluid extraction kettle.
Background
Supercritical fluid extraction is a high-efficiency and clean chemical extraction and separation technology, and has the advantages of no toxicity, no pollution, no residue, high solubility, easy separation and the like of an extraction medium. Supercritical fluid extraction is based on the principle of using an extraction medium (e.g., supercritical carbon dioxide fluid) as a solvent, contacting the supercritical fluid with a solid substance in a supercritical state, and selectively extracting the target component at a suitable pressure and temperature.
The supercritical fluid extraction kettle is the most important core equipment in supercritical fluid extraction, and at present, the commonly used supercritical fluid extraction kettle mainly comprises a kettle body, a material basket, a kettle cover and a jacket, wherein the material basket in the kettle body is of a single-section or multi-section structure, and an upper section of material basket and a lower section of material basket are tightly connected through screws. When the extraction kettle is used for extraction, materials are firstly respectively filled into each section of material basket, then each section of material basket is hung in the kettle body by a material basket group connected by screws, after the kettle cover is covered, an extraction medium is introduced into the kettle body, and moves from bottom to top and contacts with the materials in the material basket, so that soluble components in the materials are dissolved and extracted. However, when the extraction kettle with the structure is used for carrying out supercritical extraction of materials, the following problems mainly exist:
1) The loaded basket or basket group is heavy, a larger power device is needed for lifting and taking out the basket, the height of the tightly connected basket group is higher, and enough operation height and space which are convenient for lifting and taking out the basket group are reserved above the cover body of the extraction kettle in order to adapt to the lifting and taking out of the basket group, so that a higher workshop is needed, the manufacturing cost and equipment cost of the workshop are increased, and the problems are particularly outstanding for a large-scale extraction kettle;
2) When extracting powder raw materials with larger bulk density and high oil content (for example, the oil content is more than 30%), the powder raw materials are usually easy to generate serious caking phenomenon due to the action of self-bulk gravity or precipitation of grease after the raw materials are crushed, and then obvious channeling is generated when an extraction medium enters the raw materials, so that the flow distribution of the extraction medium is unbalanced, the raw materials in a material basket are subjected to extraction dead angle, the extraction speed is low, the extraction is uneven and incomplete, the residual quantity of products in the raffinate is large, the extraction cost and the loss of products are increased, and the large-scale effective extraction production of the raw materials which are easy to agglomerate or have high oil content cannot be realized in practice.
3) When the supercritical fluid extraction is carried out on the raw materials by adopting the material basket groups with the tightly connected multi-section material baskets, the raw materials in the lowest section material basket are generally easy to be extracted or completely extracted because the extraction medium moves from bottom to top in the extraction kettle. As the extraction medium is saturated from bottom to top, the material in the basket above is no longer effectively extracted, which in turn increases the resistance to the fluid. On the other hand, for kernel raw materials with rich oil content, the phenomenon that the screen mesh at the top of the material basket is blocked by the oil-powder mixture interweaved together often occurs, so that the pressure difference between the fluid inlet and the fluid outlet of the extraction kettle is large, and the formation of the pressure difference further causes the agglomeration of the raw materials and the vicious circle of the screen mesh blocking, so that the extraction production cannot be normally performed.
Disclosure of Invention
The invention aims to solve the technical problems that: the utility model provides a overcome prior art's not enough, provide a simple structure, convenient to use's multi-basket step substep supercritical fluid extraction cauldron, this extraction cauldron can realize the step substep extraction from bottom to top of raw materials in the multi-basket to can avoid the raw materials to produce channeling and caking phenomenon and appear the risk that the screen cloth blockked up in the extraction process, ensure extraction stability, quick, thoroughly, improved extraction efficiency and effect greatly, with the high-efficient quick and large-scale extraction production of successfully realizing high grease content raw materials.
The technical scheme adopted for solving the technical problems is as follows: the utility model provides a multi-basket step supercritical fluid extraction cauldron, including the cauldron body that has the extraction chamber and locate the cauldron lid on the cauldron body, be equipped with 2 at least sections material baskets in the extraction chamber, the bottom of the cauldron body is equipped with the extraction medium import that is linked together with the extraction chamber, be equipped with material basket sealing device between the internal lateral wall of cauldron and the every section material basket outer wall, be not connected each other between two upper and lower adjacent sections material baskets, be equipped with material basket interval collector and top collector respectively between two adjacent sections material baskets and the upper portion that is located the material basket of top, be equipped with on the cauldron body with the top extraction medium export that aligns with top collector and a plurality of material basket interval extraction medium export that aligns with material basket interval collector, the exit end of top extraction medium export and material basket interval extraction medium export all is connected with closing device.
According to the invention, at least 2 sections of material baskets which are not connected with each other are arranged in the extraction kettle, and the single material basket can be independently and sequentially hoisted when the material basket is hoisted into the kettle, so that the single material basket entering and exiting the kettle body is lighter in weight, the hoisting and the taking out of the material basket are easier and more convenient, the automatic operation is facilitated, and the working efficiency is greatly improved; because the height of the single basket is far smaller than that of a basket group formed by tightly connecting a plurality of sections of baskets, the operation height and the space requirement for the baskets to enter and exit the extraction kettle are greatly reduced, and the construction and maintenance cost of equipment and the construction cost of a factory building can be obviously reduced.
The material basket material collecting area and the top end collecting area are respectively arranged between two adjacent material baskets and at the upper part of the uppermost material basket, the kettle body is provided with a top end extraction medium outlet aligned with the top end collecting area and a plurality of material basket extraction medium outlets aligned with the material basket collecting area, and the materials in the material basket can be extracted by selectively switching the closing device of the top end extraction medium outlet and the material basket extraction medium outlet after the materials in the lowest material basket are extracted by the extraction medium, and then enter the upper material basket for secondary extraction after being redistributed in the material basket collecting area, and the materials in the material basket are extracted step by step from bottom to top.
When the raw materials in the upper material saving basket are extracted, the raw materials in the lower material saving basket are extracted for a certain time in advance, the raw materials become more and more loose, the resistance to the extraction medium is less and less, the unsaturation degree (purity) of the extraction medium entering the upper material saving basket is higher and higher, the phenomenon that the extraction medium is saturated when entering the upper material saving basket is avoided, and the raw materials in the upper material saving basket can be completely extracted. Namely, the step extraction not only avoids the adverse effect of the high grease content of the raw materials in the lower material-saving basket on the upper material-saving basket, but also greatly reduces the flow resistance of the extraction medium in the raw materials, reduces the caking and channeling of the raw materials, ensures the uniformity and effectiveness of the extraction, avoids the risk of screen blockage, ensures the extraction production, particularly the extraction in a large extraction kettle, can be continuously and stably carried out, and greatly improves the extraction efficiency and effect.
Further, the closing device comprises a fluid outlet pipe connected with the top extraction medium outlet and the outlet end of the extraction medium outlet between the material baskets, and a fluid outlet valve is arranged on the fluid outlet pipe.
Further, a top filter device and a support device between the material baskets are arranged at the top of the material basket, and a bottom filter device is arranged at the bottom of the material basket.
Further, the support device between the material baskets comprises a flange connected with the top of the material basket, the middle of the flange is of a hollow structure, and the side wall of the flange is provided with a through hole.
Further, the middle part of the flange forms a collecting area between the material baskets.
Further, the top filter device and the bottom filter device each comprise a pair of pore plates and a screen mesh clamped between the two pore plates.
Further, an instrument interface tube is arranged on the side wall of the kettle body.
Further, a pressing device is further arranged between the uppermost material basket and the kettle cover in the extraction cavity, the top end of the pressing device is in contact with the kettle cover, the bottom end of the pressing device is in butt joint with the flange, and a top end collecting area is formed between the pressing device and the uppermost material basket.
Further, a kettle cover sealing device is arranged at the joint of the kettle cover and the inner side wall of the kettle body.
Further, the outer wall of the kettle body is wrapped with a jacket, and the jacket is provided with a jacket water inlet, a jacket water outlet, a jacket water self-circulation inlet and a jacket water self-circulation outlet.
The multi-basket stepped step supercritical fluid extraction kettle has the beneficial effects that:
(1) According to the invention, 2 sections, 3 sections or more sections of material baskets are arranged in the extraction kettle, and two adjacent sections of material baskets are independent and are not connected with each other, and are only stacked in the kettle body sequentially, when the material baskets are hoisted and taken out, single section of material basket can be hoisted and taken out separately in sequence, and because the single section of material basket is lighter in weight, the hoisting and taking out of the material basket are more convenient, simple and easy, a high-power device is not required, automatic operation is facilitated, and the working efficiency is greatly improved; and the height of the single-section basket is far smaller than that of a basket group formed by tightly connecting the plurality of sections of baskets, so that the operation height and space required by the baskets to enter and exit the extraction kettle are greatly reduced, and the construction and maintenance cost of equipment and the construction cost of a factory building can be obviously reduced.
(2) According to the invention, the multi-section material basket which is not connected with each other is adopted, the multi-section material basket can be used for dispersing and charging, and during extraction, the weight of raw materials in the single-section material basket is lighter, so that the self-accumulation gravity of the raw materials is reduced, the generation of raw material caking and channeling is reduced, and the extraction effect is improved;
(3) According to the invention, the flow collecting area between the material baskets and the top flow collecting area are respectively arranged between the two adjacent material baskets and at the upper part of the material basket positioned at the uppermost part, and the extraction medium is redistributed in the flow collecting area between the material baskets and then upwards enters the upper material basket after passing through the lower material basket, so that the extraction medium is changed into laminar flow from linear flow after being redistributed before entering the upper material basket, the phenomenon that the extraction medium directly flows into the upper material basket in various different flow paths and flow velocities before entering the upper material basket is avoided, and the channeling phenomenon is caused, and the uniformity and the extraction effect of extraction are effectively improved;
(4) According to the invention, through a top extraction medium outlet aligned with a top current collecting area on a kettle body and a plurality of material basket extraction medium outlets which are different in height and aligned with material basket current collecting areas, and the outlet ends of the top extraction medium outlet and the material basket extraction medium outlet are connected with a closing device, in the extraction process, the extraction medium is sequentially extracted from materials in a material basket step by step from bottom to top by selectively switching the closing device; when the raw materials in the upper material saving basket are extracted, all the raw materials in the material basket below the upper material saving basket are extracted for a certain time in advance, the raw materials become more and more loose, the resistance of the extraction medium is less and less, the unsaturation degree (purity) of the extraction medium entering the upper material saving basket is higher and higher, and the raw materials in the upper material saving basket can be completely extracted. Namely, the step extraction not only avoids the adverse effect of high grease content of the raw materials in the lower material saving basket on the upper material saving basket, but also greatly reduces the flow resistance of the extraction medium in the raw materials, reduces caking and channeling of the raw materials, ensures uniform and efficient extraction of the extraction medium, avoids the risk of screen blockage, ensures continuous and stable extraction production, greatly improves the extraction efficiency and effect, particularly extraction in a large extraction kettle, and realizes large-scale and efficient extraction production of kernel raw materials with very high oil content such as camellia seed kernels, peanuts, walnut kernels, rapeseed kernels, sesame seeds, perilla seeds, star oil Teng Guo and the like.
Drawings
FIG. 1 is a schematic diagram of a multi-basket step supercritical fluid extraction vessel according to the present invention;
FIG. 2-is a schematic view of the structure of the basket.
The above reference numerals: 1-tank, 2-extraction chamber, 3-tank cap, 4-jacket, 5-jacket water inlet, 6-jacket water outlet, 7-jacket water self-circulation inlet, 8-jacket water self-circulation outlet, 9-first basket, 10-second basket, 11-third basket, 12-extraction medium inlet, 13-basket sealing device, 14-first collecting region, 15-second collecting region, 16-top collecting region, 17-extraction medium primary outlet, 18-extraction medium secondary outlet, 19-top extraction medium outlet, 20-first fluid outlet pipe, 21-second fluid outlet pipe, 22-top fluid outlet pipe, 23-first fluid outlet valve, 24-second fluid outlet valve, 25-top fluid outlet valve, 26-quick opening mechanism, 27-meter interface pipe, 28-pressing device, 29-tank cap sealing device, 30-top filtering device, 31-inter-basket supporting device, 32-bottom filtering device, 33-flange, 34-through hole.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings, but these embodiments do not limit the scope of the invention in any way.
Example 1
The utility model provides a multi-material basket step substep supercritical fluid extraction cauldron, includes the cauldron body 1 that has extraction chamber 2, locates the cauldron lid 3 on the cauldron body 1 and wraps up in the cover 4 of cauldron body 1 outer wall, the cauldron body 1 is connected through quick-opening mechanism 26 with the cauldron lid 3, and quick-opening mechanism 26 is the clamp, be equipped with on the cover 4 with extraction chamber 2 be linked together jacket water inlet 5, jacket water outlet 6, jacket water self-loopa import 7 and jacket water self-loopa export 8, still be equipped with closing device 28 between the material basket and the cauldron lid 3 that are located the top in the extraction chamber 2, still be equipped with instrument interface pipe 27 on the cauldron body 1 lateral wall.
The extraction cavity 2 is internally provided with at least 2 material baskets which can be 2 sections, 3 sections, 4 sections or more, in this embodiment, 3 sections are arranged, the first material basket 9, the second material basket 10 and the third material basket 11 are arranged from bottom to top, the bottom of the kettle body 1 is provided with an extraction medium inlet 12 communicated with the extraction cavity 2, a material basket sealing device 13 is arranged between the inner side wall of the kettle body 1 and the outer wall of each material basket, the material basket sealing device 13 is a sealing ring, the upper adjacent material basket and the lower adjacent material basket are not connected with each other, a material basket collecting region and a top collecting region are respectively arranged between the two adjacent material baskets and the upper part of the uppermost material basket, in this embodiment, the material basket collecting region comprises a first collecting region 14 (positioned between the first material basket 9 and the second material basket 10) and a second collecting region 15 (positioned between the second material basket 10 and the third material basket 11) from bottom to top, and the compressing device 28 and the third material basket 11 form the top collecting region 16.
In order to reduce the lifting difficulty of the material basket, at least 2 sections of material baskets which are not connected with each other are adopted, so that the material basket positioned above is directly overlapped on the material basket positioned below the material basket, and therefore, only a single section of material basket is required to be independently and sequentially lifted and taken out in the lifting and taking-out process, and as the single section of material basket (containing raw materials) has lighter weight, the power of equipment in lifting is reduced, and the loading and unloading portability of the raw materials is effectively improved;
Meanwhile, the height of the single-section material basket is far smaller than that of a material basket group formed by tightly connecting the plurality of sections of material baskets, so that more height and space on the upper part of the kettle body 1 are not required to be occupied when the single-section material basket is hoisted and taken out, the building height of a factory building is reduced, the building cost of the factory building is greatly reduced, the space of the factory building can be effectively and fully utilized, and the space utilization rate of the factory building is improved;
In addition, the raw materials in the multi-section basket can be respectively charged, and during extraction, the weight of the raw materials in the single basket is lighter, so that the gravity of the raw materials stacked on the single basket is reduced, the generation of raw material agglomeration and channeling in extraction is reduced, and the extraction efficiency and effect are improved.
The prior extraction kettles are directly and tightly connected by screws, and extraction media directly flow into the upper material-saving basket from the lower material-saving basket, and as the extraction media form a plurality of different flow paths and flow rates in the lower material-saving basket, channeling phenomenon is generated when the extraction media enter the upper material-saving basket. According to the invention, the flow collecting area between the material baskets and the top flow collecting area 16 are respectively arranged between the two adjacent material baskets and at the upper part of the material basket positioned at the uppermost part, so that extraction medium flows through the lower material basket, is redistributed in the flow collecting area between the material baskets and then upwards enters the upper material basket, the extraction medium is converted into laminar flow from linear flow through redistribution before entering the upper material basket, the extraction medium is prevented from directly flowing into the upper material basket in various different flow paths and flow velocities before entering the upper material basket, and a large amount of channeling is further generated, and the extraction efficiency and the extraction effect are effectively improved.
The kettle body 1 is provided with a top extraction medium outlet 19 aligned with the top collecting region 16 and a plurality of inter-basket extraction medium outlets (2 in this embodiment, specifically, a first extraction medium outlet 17 and a second extraction medium outlet 18 from bottom to top) aligned with the basket collecting region along different heights, the first extraction medium outlet 17, the second extraction medium outlet 18 and the top extraction medium outlet 19 are all communicated with the extraction cavity 2 and aligned with the first collecting region 14, the second collecting region 15 and the top collecting region 16 respectively, and the outlet ends thereof are connected with a closing device for controlling fluid outflow, the closing device comprises a first fluid outlet pipe 20, a second fluid outlet pipe 21 and a top fluid outlet pipe 22 respectively connected with the outlet ends of the first extraction medium outlet 17, the second extraction medium outlet 18 and the top extraction medium outlet 19, and a first fluid outlet valve 23, a second fluid outlet valve 24 and a top fluid outlet valve 25 are respectively arranged on the first fluid outlet pipe 20, the second fluid outlet pipe 21 and the top fluid outlet pipe 22.
The invention is through setting up the top extraction medium outlet 19 aligned with top collecting zone and multiple material basket extraction medium outlets of different heights and aligned with material basket collecting zone on the kettle body 1, and connect the fluid outlet valve in the outlet end of extraction medium outlet 19 and material basket extraction medium outlet, in the course of extracting, open the first fluid outlet valve 23 first, close the second fluid outlet valve 24 and top fluid outlet valve 25, the extraction medium extracts the first material basket 9 first and then carries the extracted product to enter the first collecting zone 14, and flow out from the first grade outlet 17 of extraction medium; closing the first fluid outlet valve 23, opening the second fluid outlet valve 24 to enable the extraction medium to flow into the first material saving basket 9 from the bottom of the kettle body 1, then flow into the second material saving basket 10 after being redistributed in the first collecting area 14, and flow out of the extraction medium secondary outlet 18 with the extracted product; closing the second fluid outlet valve 24, opening the top fluid outlet valve 25, enabling the extraction medium to flow into the first material saving basket 9 and the second material saving basket 10 from the bottom of the kettle body 1, then flow into the third material saving basket 11 after being redistributed in the second collecting region 15, and flow out from the top extraction medium outlet 19 after entering the top collecting region 16 with the extracted product; when the number of the sections of the basket is more than 3 sections, the step extraction is still carried out according to the process.
In the extraction process, when the raw materials in the second section basket 10 are extracted, the raw materials in the first section basket 9 are extracted for a certain time in advance, so that the unsaturation degree (purity) of the extraction medium entering the second section basket 10 is improved; when the raw materials in the third material saving basket 11 are extracted, the raw materials in the first material saving basket 9 and the second material saving basket 10 are extracted for a period of time in advance, so that the unsaturation degree (purity) of the extraction medium entering the third material saving basket 11 is improved, the phenomenon of saturation of the extraction medium in the whole extraction process is avoided, the raw materials in each level of material basket are fully extracted completely, and the adverse effect of high grease of the raw materials in the lower material saving basket on the upper material saving basket is avoided; meanwhile, the flow resistance of the extraction medium in the raw materials can be greatly reduced by step extraction, the phenomena of caking and channeling of the raw materials are reduced, the uniform, thorough and rapid extraction of the extraction medium is ensured, and the extraction efficiency and the extraction effect of the raw materials are greatly improved.
When the raw materials in the upper material basket are extracted, all the grease in the raw materials in the lower material basket are completely extracted or nearly completely extracted and flow out through the extraction medium outlet, so that the phenomenon of screen blockage caused by the adhesion and agglomeration of a large amount of grease and fine powder in a short time is avoided, continuous and stable extraction production is ensured, and the extraction efficiency and effect are greatly improved.
The top of material basket is equipped with top filter equipment 30 and material inter-basket strutting arrangement 31, and its bottom is equipped with bottom filter equipment 32, top filter equipment 30 and bottom filter equipment 32 all include a pair of orifice plate and press from both sides the screen cloth of locating between two orifice plates, material inter-basket strutting arrangement 31 include with the flange 33 that the material basket top is connected, the middle part of flange 33 is hollow structure, the lateral wall of flange 33 is equipped with the through-hole 34 that runs through, the middle part of flange 33 constitutes the mass flow district between the material basket. The inter-basket supporting device 31 is used for supporting the upper basket in the two adjacent baskets, so that the upper basket is directly stacked on the top of the flange 33, and the extraction medium flows into the inter-basket extraction medium outlet through the through holes 34 after passing through the inter-basket collecting region.
The top of the pressing device 28 is connected to the kettle cover 3, the bottom of the pressing device is in butt joint with the flange 33, the pressing device 28 is a pressing ring and is used for pressing down the uppermost basket, a kettle cover sealing device 29 is arranged at the joint of the kettle cover 3 and the inner side wall of the kettle body 1, and the kettle cover sealing device 29 is a sealing ring.
The invention relates to a working principle of a multi-basket step-by-step supercritical fluid extraction kettle and a use method thereof, wherein the working principle comprises the following steps:
When the invention works, the kettle cover 3 is opened firstly, each section of material basket which is filled with raw materials is separately and sequentially hoisted in the kettle body 1, so that the third section of material basket 11 and the second section of material basket 10 are respectively stacked on the tops of the second section of material basket 10 and the first section of material basket 9, and then the kettle cover is put into a pressing device and covered with an extraction cover; closing the first fluid outlet valve 23, the second fluid outlet valve 24 and the top fluid outlet valve 25, and opening the extraction medium inlet valve at the extraction medium inlet 12 to allow the extraction medium to flow into the extraction kettle so as to equalize the pressure of all areas in the extraction kettle; starting a carbon dioxide booster pump and a heating system, opening a first fluid outlet valve 23, closing a second fluid outlet valve 24 and a top fluid outlet valve 25 after the pressure and the temperature in the extraction kettle reach the pressure and the temperature required by the process, and allowing an extraction medium to enter the kettle body 1 from the bottom of the kettle body 1 to extract raw materials in a first material saving basket 9, so that the extraction medium carries a product extracted from the first material saving basket 9 to flow upwards into a first collecting area 14 and then flow out of an extraction medium primary outlet 17;
After the first material saving basket extracts for a period of time, the first fluid outlet valve 23 is closed, the second fluid outlet valve 24 is opened, and the extracting medium upwards passes through the first material saving basket 9 and enters the first collecting area 14 to be redistributed and then enters the second material saving basket 10 to extract the raw materials in the second material saving basket 10, wherein the extracting medium carries residual products extracted in the first material saving basket 9 and products in the second material saving basket 10 to upwards flow into the second collecting area 15 and then flow out of the extracting medium secondary outlet 18;
After the second material saving basket extracts for a period of time, the second fluid outlet valve 24 is closed, the top fluid outlet valve 25 is opened, the extracting medium upwards passes through the first material saving basket 9 and the second material saving basket 10 and then enters the second collecting area 15 to be redistributed, then enters the third material saving basket 11 to extract the raw materials in the third material saving basket 11, and the extracting medium carries the residual products extracted in the second material saving basket 10 and the products in the third material saving basket 11 to upwards flow into the top collecting area 16 and then flow out of the top extracting medium outlet 19;
After the third section basket extracts for a period of time, when the products in the extraction medium flowing out of the top extraction medium outlet 19 are small, the raw materials in the third section basket 11 are fully extracted; and then the booster pump is turned off, the extraction medium inlet valve of the extraction medium inlet 12 is closed, carbon dioxide in the extraction kettle is recovered through the top fluid outlet valve 25, the last residual air in the extraction kettle is emptied, the kettle cover 3 is opened, each section of material basket is taken out in sequence, and the step-by-step extraction process of a plurality of material baskets is completed.
Example 2
This embodiment differs from embodiment 1 in that: the kettle body is internally provided with 2 material-saving baskets.
Example 3
This embodiment differs from embodiment 1 in that: the kettle body is internally provided with 6 material-saving baskets.
It should be further noted that the terms "first," "second," and the like are used herein to describe various elements, but these elements should not be limited by these terms. These terms are only used to distinguish one element from another element.
The terms "upper", "lower", "left", "right" and the like used herein to describe orientations are used for convenience in the description based on the orientation depicted in the drawings, and may vary in actual devices depending on the manner in which the devices are placed.
The present invention is not limited to the preferred embodiments, and the present invention is described above in any way, but is not limited to the preferred embodiments, and any person skilled in the art will appreciate that the present invention is not limited to the embodiments described above, while the above disclosure is directed to various equivalent embodiments, which are capable of being modified or varied in several ways, any simple modification, equivalent changes and variation of the above embodiments according to the technical principles of the present invention will still fall within the scope of the present invention.
Claims (6)
1. The utility model provides a many material basket step substep supercritical fluid extraction cauldron, is including having the cauldron body of extraction chamber and locating the cauldron lid on the cauldron body, is equipped with 2 at least festival material baskets in the extraction chamber, and the bottom of the cauldron body is equipped with the extraction medium import that is linked together with the extraction chamber, is equipped with material basket sealing device between the internal lateral wall of cauldron and every festival material basket outer wall, its characterized in that: the upper and lower adjacent sections of material baskets are not connected with each other, a material basket-to-material flow collecting region and a top end flow collecting region are respectively arranged between the adjacent sections of material baskets and at the upper part of the uppermost material basket, a top end extraction medium outlet aligned with the top end flow collecting region and a plurality of material basket-to-material extraction medium outlets aligned with the material basket-to-material flow collecting region are arranged on the kettle body, and the outlet ends of the top end extraction medium outlet and the material basket-to-material extraction medium outlet are connected with a closing device;
the top of the material basket is provided with a top filtering device and a supporting device between the material baskets, and the bottom of the material basket is provided with a bottom filtering device;
The support device between the material baskets comprises a flange connected with the top of the material basket, the middle of the flange is of a hollow structure, and the side wall of the flange is provided with a through hole;
the middle part of the flange forms a collecting area between the material baskets;
The top filter device and the bottom filter device both comprise a pair of pore plates and a screen mesh clamped between the two pore plates.
2. The multi-basket step supercritical fluid extraction kettle as claimed in claim 1, wherein: the closing device comprises a fluid outlet pipe connected with the top extraction medium outlet and the outlet end of the extraction medium outlet between the material baskets, and a fluid outlet valve is arranged on the fluid outlet pipe.
3. The multi-basket step supercritical fluid extraction kettle as claimed in claim 1, wherein: and an instrument interface tube is further arranged on the side wall of the kettle body.
4. The multi-basket step supercritical fluid extraction kettle as claimed in claim 1, wherein: the extraction cavity is internally provided with a material basket and a kettle cover, wherein the material basket is positioned at the uppermost part of the extraction cavity, the top end of the material basket is contacted with the kettle cover, the bottom end of the material basket is abutted with the flange, and a top end collecting area is formed between the material basket and the uppermost part of the material basket.
5. The multi-basket step supercritical fluid extraction kettle according to claim 4, wherein: and a kettle cover sealing device is arranged at the joint of the kettle cover and the inner side wall of the kettle body.
6. A multi-basket, stepped, supercritical fluid extraction vessel according to any one of claims 1 to 5, wherein: the outer wall of the kettle body is wrapped with a jacket, and the jacket is provided with a jacket water inlet, a jacket water outlet, a jacket water self-circulation inlet and a jacket water self-circulation outlet.
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| EP2727637B1 (en) * | 2012-11-06 | 2019-08-28 | Uhde Inventa-Fischer GmbH | Extraction reactor and method for extraction of granular material |
| CN104548655B (en) * | 2013-10-28 | 2016-08-17 | 贵州航天乌江机电设备有限责任公司 | The manufacture method of hanging basket and hanging basket in a kind of extraction kettle |
| US11331594B2 (en) * | 2017-06-22 | 2022-05-17 | Azoth Solutions, LLC | Extraction system including a multi-port extraction vessel and extraction basket |
| CN107474947B (en) * | 2017-09-06 | 2021-01-12 | 广西壮族自治区林业科学研究院 | Distillation dual-purpose device for acid leaching of illicium verum and oil extraction of fennel and application of distillation dual-purpose device |
| CN111282309B (en) * | 2020-03-16 | 2025-07-15 | 湖北天圣药业有限公司 | A suspended point contact supercritical extraction device |
| CN111714929B (en) * | 2020-07-24 | 2025-06-13 | 湖南和广生物科技有限公司 | Self-moving material balance filtering device, extraction kettle containing the device and use method |
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