CN114100192A - Method for preparing wormwood protoplasm by supercritical carbon dioxide extraction process - Google Patents
Method for preparing wormwood protoplasm by supercritical carbon dioxide extraction process Download PDFInfo
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- CN114100192A CN114100192A CN202111523940.5A CN202111523940A CN114100192A CN 114100192 A CN114100192 A CN 114100192A CN 202111523940 A CN202111523940 A CN 202111523940A CN 114100192 A CN114100192 A CN 114100192A
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- extraction
- wormwood
- carbon dioxide
- preparing
- supercritical carbon
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- 235000009051 Ambrosia paniculata var. peruviana Nutrition 0.000 title claims abstract description 38
- 235000003097 Artemisia absinthium Nutrition 0.000 title claims abstract description 38
- 240000001851 Artemisia dracunculus Species 0.000 title claims abstract description 38
- 235000017731 Artemisia dracunculus ssp. dracunculus Nutrition 0.000 title claims abstract description 38
- 235000003261 Artemisia vulgaris Nutrition 0.000 title claims abstract description 38
- 239000001138 artemisia absinthium Substances 0.000 title claims abstract description 38
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 title claims abstract description 20
- 210000000805 cytoplasm Anatomy 0.000 title claims description 3
- 238000000605 extraction Methods 0.000 claims abstract description 53
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 239000000287 crude extract Substances 0.000 claims abstract description 8
- 238000001704 evaporation Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 230000008020 evaporation Effects 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000000746 purification Methods 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 3
- 238000000194 supercritical-fluid extraction Methods 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 24
- 239000001569 carbon dioxide Substances 0.000 description 12
- 229910002092 carbon dioxide Inorganic materials 0.000 description 12
- 241001435059 Artemisia argyi Species 0.000 description 5
- 235000010894 Artemisia argyi Nutrition 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000003443 antiviral agent Substances 0.000 description 1
- 244000052616 bacterial pathogen Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 208000023504 respiratory system disease Diseases 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0203—Solvent extraction of solids with a supercritical fluid
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/1456—Removing acid components
- B01D53/1475—Removing carbon dioxide
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
- B01D53/18—Absorbing units; Liquid distributors therefor
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The application discloses a method for preparing wormwood raw pulp by a supercritical carbon dioxide extraction process, which belongs to the technical field of supercritical extraction and comprises the following steps of: cleaning wormwood, drying at low temperature, and crushing the dried wormwood to obtain a primary processed material; step two, extraction: putting the primary processed material into an extraction device for extraction to obtain a crude extract; step three, heating: filtering the crude extract, heating in an evaporation kettle, heating to 40-50 ℃, stirring and evaporating to obtain the wormwood raw stock. The application for preparing the wormwood raw pulp has the advantages of high extraction efficiency, simple steps and high content of effective components.
Description
Technical Field
The invention relates to the technical field of supercritical extraction processes, in particular to a method for preparing wormwood raw pulp by a supercritical carbon dioxide extraction process.
Background
The principle of the supercritical carbon dioxide extraction separation process is that under the supercritical state, supercritical carbon dioxide is contacted with a substance to be separated, so that the substances with different polarity, boiling point and molecular weight are selectively and sequentially extracted. The extraction material obtained corresponding to each pressure range cannot be single, but the condition can be controlled to obtain the mixed components with the optimal proportion, then the supercritical fluid is changed into the common gas by the methods of decompression and temperature rise, and the extracted material is completely or basically precipitated, thereby achieving the purpose of separation and purification, so the supercritical fluid carbon dioxide extraction process is formed by the combination of extraction and separation.
The artemisia argyi grass, also called artemisia argyi and artemisia argyi, is a plant commonly owned in southern China, the history of the artemisia argyi for preventing pestilence is thousands of years, and the modern medical pharmacology proves that the artemisia argyi is an antibacterial and antiviral drug, has the effects of inhibiting and killing germs and preventing and treating respiratory diseases.
The chemical components of the wormwood are complex, the extraction and separation process of the wormwood is a bottleneck for restricting the development of the wormwood, and compared with other extraction processes, the supercritical technology can fully extract the effective components, remove the ineffective components to the maximum extent and easily recover carbon dioxide as an extraction solvent, so that the applicant applies the supercritical carbon dioxide extraction technology to the extraction of the effective components of the wormwood and provides a preparation method of the wormwood raw stock.
Disclosure of Invention
The invention aims to provide a method for preparing wormwood raw stock by a supercritical carbon dioxide extraction process, and provides a method for extracting effective components of wormwood by applying a supercritical carbon dioxide extraction technology to obtain wormwood raw stock.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for preparing folium Artemisiae Argyi primary pulp by supercritical carbon dioxide extraction process comprises the following steps,
step one, preparing raw materials: cleaning wormwood, drying at low temperature, and crushing the dried wormwood to obtain a primary processed material;
step two, extraction: putting the primary processed material into an extraction device for extraction to obtain a crude extract, wherein the extraction device comprises a base and a purification cylinder filled with a purification liquid, the base is fixedly connected with an extraction box and a fan box, an air inlet pipe is communicated between the extraction boxes, the extraction box and the fan box are communicated with an exhaust pipe, and a fan is arranged in the fan box; the bottom of the fan box is coaxially and rotatably connected with a limiting ring, the inner wall of the limiting ring is symmetrically and fixedly connected with limiting sheets along the axis of the limiting ring, the top of the purification cylinder is fixedly sleeved with a connecting ring, the top of the connecting ring is symmetrically provided with through grooves for containing the corresponding limiting sheets, the connecting ring is also coaxially provided with an annular limiting groove, the through grooves are communicated with the annular limiting groove, the top of the purification cylinder is provided with a connecting hole, and the fan is also communicated with a connecting pipe which penetrates through the limiting ring and the connecting hole;
step three, heating: filtering the crude extract, heating in an evaporation kettle, heating to 40-50 ℃, stirring and evaporating to obtain the wormwood raw stock.
The working principle and the beneficial effects of the invention are as follows: according to the scheme, the wormwood is crushed in advance and then subjected to low-temperature drying and supercritical carbon dioxide extraction, so that the solubility of the chemical components of the wormwood in supercritical carbon dioxide is improved, the wormwood raw pulp can be obtained by heating, the extraction efficiency is high, the steps are simple, and the content of effective components is high.
When the purification cylinder is installed, the through grooves on the two sides of the connecting ring are respectively aligned to the limiting sheets on the two sides, the purification cylinder is inserted into the limiting ring, the limiting sheets on the two sides respectively extend into the corresponding through grooves, and the connecting pipe penetrates through the connecting hole and extends into the purification cylinder; and because logical groove and spacing groove are the intercommunication, the spacing ring is rotated with the bottom of fan case and is connected, consequently fixes purifying barrel this moment, rotates the spacing ring again, and the spacing piece that the spacing ring drove both sides shifts over to the spacing inslot through leading to the groove, through the cooperation of spacing piece and spacing groove for purifying barrel can not drop downwards, accomplishes purifying barrel's installation promptly.
The fan pumps redundant carbon dioxide gas in the drying box into the fan box through the exhaust pipe, and the redundant carbon dioxide gas is discharged into the purifying cylinder through the connecting pipe and is fully absorbed by the purifying liquid in the purifying cylinder. When a purifying cylinder is required to be detached, the limiting ring is rotated reversely to enable the limiting piece to move to the through groove, so that the purifying cylinder can be taken out downwards, and better purifying liquid is facilitated.
Further, the extraction pressure of the extraction box in the second step is 20-50 Mpa, the extraction time is 2-3 h, and the extraction temperature is 30-50 ℃.
Further, the heating temperature in the third step is 45 ℃.
Further, an annular rubber pad is sleeved on the top of the connecting ring. After the connecting ring is contacted with the bottom of the fan box, the rubber pad can be extruded to deform, on one hand, the bottom of the fan box can be prevented from being extruded, on the other hand, the annular rubber pad surrounds the connecting pipe, and the rubber pad can enable the purifying cylinder to keep good sealing performance.
Further, the purification cylinder is provided with a pressure release valve. The carbon dioxide gas is blown into towards the interior of the purification cylinder continuously by the fan, and when the internal pressure of the purification cylinder is large, the pressure release valve opens to discharge redundant carbon dioxide gas outwards.
Further, the drying box is hinged with a sealing door. The sealing door can be opened to place the articles to be dried into the drying box, and the sealing door has a better sealing effect.
Furthermore, the bottom fixedly connected with motor of fan case, the active segment of motor is fixed to be cup jointed with the driving gear, the fixed driven gear who cup joints with driving gear meshing of spacing ring. The motor drive driving gear rotates, and the driving gear passes through driven gear drive spacing ring and rotates to replace the manual work to rotate the spacing ring.
Further, base fixedly connected with support, shown support fixedly connected with cylinder, the expansion end fixedly connected with of cylinder is used for supporting the backup pad of purifying cylinder. The supporting plate is driven by the cylinder to move up and down, so that the purifying cylinder can be taken down or installed conveniently. Drawings
FIG. 1 is a front view of an extraction apparatus according to the present invention;
FIG. 2 is a transverse cross-sectional view of the stop collar of FIG. 1;
fig. 3 is a schematic structural view of fig. 2 when the limiting plate and the through groove are aligned.
Detailed Description
The following is further detailed by way of specific embodiments:
reference numerals in the drawings of the specification include: the device comprises a purification cylinder 1, a limiting ring 2, a fan box 3, a base 4, an exhaust pipe 5, an extraction box 6, an air inlet pipe 7, a micro-jet device 8, a connecting pipe 9, a connecting ring 10, a through groove 11, a limiting groove 12 and a limiting sheet 13.
In the following statements, all the directional terms such as "left", "right", "upper", "lower", etc. are based on the directions shown in the drawings, and in practice, the corresponding structures do not affect the implementation of the schemes under the condition that the relative positions are kept unchanged by the same directional changes based on the directions.
Example (b): a method for preparing folium Artemisiae Argyi primary pulp by supercritical carbon dioxide extraction process comprises the following steps,
step one, preparing raw materials: cleaning wormwood, drying at low temperature, and crushing the dried wormwood to obtain a primary processed material;
step two, extraction: putting the primary processed material into an extraction device for extraction to obtain a crude extract, wherein the extraction pressure of an extraction box is 20-50 Mpa, the extraction time is 2-3 h, and the extraction temperature is 30-50 ℃;
step three, heating: filtering the crude extract, heating in an evaporation kettle, heating to 45 deg.C, stirring, and evaporating to obtain folium Artemisiae Argyi juice.
According to the scheme, the wormwood is crushed in advance and then subjected to low-temperature drying and supercritical carbon dioxide extraction, so that the solubility of the chemical components of the wormwood in supercritical carbon dioxide is improved, the wormwood raw pulp can be obtained by heating, the extraction efficiency is high, the steps are simple, and the content of effective components is high.
As shown in fig. 1, the extraction device comprises a base 4 and a purification cylinder 1 filled with a purification liquid, wherein the purification liquid is a sodium hydroxide solution, the base 4 is fixedly connected with an extraction box 6 and a fan box 3, an air inlet pipe 7 is communicated between the extraction box 6, the extraction box 6 and the fan box 3 are communicated with an exhaust pipe 5, and a fan is arranged in the fan box 3; the bottom coaxial rotation of fan case 3 is connected with spacing ring 2, spacing ring 2's inner wall is along its axis symmetry fixedly connected with spacing piece 13, the fixed hookup at the top of purification cartridge 1 has go-between 10, the top symmetry of go-between 10 is equipped with and is used for holding logical groove 11 that corresponds spacing piece 13, go-between 10 is still coaxial to be equipped with annular spacing groove 12, lead to groove 11 and annular spacing groove 12 intercommunication, the top of purification cartridge 1 is equipped with the connecting hole, the fan still communicates has connecting pipe 9 that passes spacing ring 2 and connecting hole.
When the extraction device is used for extraction, a large amount of carbon dioxide is remained in the extraction device after extraction, so that when the purification cylinder 1 is installed, the through grooves 11 on the two sides of the connecting ring 10 are respectively aligned to the limiting pieces 13 on the two sides, the purification cylinder 1 is inserted into the limiting ring 2, the limiting pieces 13 on the two sides respectively extend into the corresponding through grooves 11, and the connecting pipe 9 penetrates through the connecting hole and extends into the purification cylinder 1; and because logical groove 11 and spacing groove 12 are the intercommunication, spacing ring 2 rotates with the bottom of fan case 3 to be connected, consequently fixes purifying barrel 1 this moment, rotates spacing ring 2 again, and spacing piece 13 that spacing ring 2 drove both sides changes over to spacing groove 12 through leading to groove 11 in, through spacing piece 13 and spacing groove 12's cooperation for purifying barrel 1 can not drop downwards, accomplishes purifying barrel 1's installation promptly.
The fan pumps redundant carbon dioxide gas in the drying box into the fan box 3 through the exhaust pipe 5, and the redundant carbon dioxide gas is discharged into the purifying cylinder 1 through the connecting pipe 9 and is fully absorbed by the purifying liquid in the purifying cylinder 1. When the purifying cylinder 1 is required to be disassembled, the limiting ring 2 rotates reversely to enable the limiting sheet 13 to move to the through groove 11, so that the purifying cylinder 1 can be taken out downwards, and better purifying liquid is convenient to use.
It should be noted that various changes and modifications can be made by those skilled in the art without departing from the structure of the invention, and these changes and modifications should be construed as being within the scope of the invention, which does not affect the effect of the invention and the applicability of the patent. The scope of the claims of the present application shall be determined by the contents of the claims, and the description of the embodiments and the like in the specification shall be used to explain the contents of the claims.
Claims (8)
1. A method for preparing wormwood protoplasm by a supercritical carbon dioxide extraction process is characterized by comprising the following steps: comprises the following steps of (a) carrying out,
step one, preparing raw materials: cleaning wormwood, drying at low temperature, and crushing the dried wormwood to obtain a primary processed material;
step two, extraction: putting the primary processed material into an extraction device for extraction to obtain a crude extract, wherein the extraction device comprises a base and a purification cylinder filled with a purification liquid, the base is fixedly connected with an extraction box and a fan box, an air inlet pipe is communicated between the extraction boxes, the extraction box and the fan box are communicated with an exhaust pipe, and a fan is arranged in the fan box; the bottom of the fan box is coaxially and rotatably connected with a limiting ring, the inner wall of the limiting ring is symmetrically and fixedly connected with limiting sheets along the axis of the limiting ring, the top of the purification cylinder is fixedly sleeved with a connecting ring, the top of the connecting ring is symmetrically provided with through grooves for containing the corresponding limiting sheets, the connecting ring is also coaxially provided with an annular limiting groove, the through grooves are communicated with the annular limiting groove, the top of the purification cylinder is provided with a connecting hole, and the fan is also communicated with a connecting pipe which penetrates through the limiting ring and the connecting hole;
step three, heating: filtering the crude extract, heating in an evaporation kettle, heating to 40-50 ℃, stirring and evaporating to obtain the wormwood raw stock.
2. The method for preparing the wormwood raw pulp by the supercritical carbon dioxide extraction process according to claim 1, which is characterized by comprising the following steps: and the extraction pressure of the extraction box in the second step is 20-50 Mpa, the extraction time is 2-3 h, and the extraction temperature is 30-50 ℃.
3. The method for preparing the wormwood raw pulp by the supercritical carbon dioxide extraction process according to claim 2, which is characterized in that: the heating temperature of the third step is 45 ℃.
4. The method for preparing the wormwood raw pulp by the supercritical carbon dioxide extraction process according to claim 3, which is characterized by comprising the following steps: and the top of the connecting ring is sleeved with an annular rubber pad.
5. The method for preparing the wormwood raw pulp by the supercritical carbon dioxide extraction process according to claim 4, which is characterized in that: the purifying cylinder is provided with a pressure release valve.
6. The method for preparing the wormwood raw pulp by the supercritical carbon dioxide extraction process according to claim 5, which is characterized in that: the extraction box is hinged with a sealing door.
7. The method for preparing the wormwood raw pulp by the supercritical carbon dioxide extraction process according to claim 6, which is characterized in that: the bottom fixedly connected with motor of fan case, the fixed driving gear that has cup jointed of activity section of motor, the fixed driven gear who has cup jointed with driving gear meshing of spacing ring.
8. The method for preparing the wormwood raw pulp by the supercritical carbon dioxide extraction process according to claim 7, which is characterized in that: the base fixedly connected with support, shown support fixedly connected with cylinder, the expansion end fixedly connected with of cylinder is used for supporting the backup pad of purifying cylinder.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111523940.5A CN114100192A (en) | 2021-12-14 | 2021-12-14 | Method for preparing wormwood protoplasm by supercritical carbon dioxide extraction process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111523940.5A CN114100192A (en) | 2021-12-14 | 2021-12-14 | Method for preparing wormwood protoplasm by supercritical carbon dioxide extraction process |
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| CN114100192A true CN114100192A (en) | 2022-03-01 |
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| CN202111523940.5A Pending CN114100192A (en) | 2021-12-14 | 2021-12-14 | Method for preparing wormwood protoplasm by supercritical carbon dioxide extraction process |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR19980013975A (en) * | 1996-08-06 | 1998-05-15 | 정명식 | Supercritical Fluid Extraction Method of Plant Metabolites Using Adsorbent |
| CN104225953A (en) * | 2013-06-21 | 2014-12-24 | 中国石油化工股份有限公司 | Absorption apparatus for absorbing aromatic hydrocarbon in geological sample through supercritical carbon dioxide extraction |
| CN209123395U (en) * | 2018-10-26 | 2019-07-19 | 江苏蜂奥生物科技有限公司 | A kind of propolis extracts the CO2 recyclable device of SCF-CO 2 |
| CN110694298A (en) * | 2019-07-15 | 2020-01-17 | 陈龙刚 | Extraction separator for bio-pharmaceuticals |
| CN212716856U (en) * | 2020-05-27 | 2021-03-16 | 无锡市正气环保科技有限公司 | Double-insulation ceramic end cover device of pulse type tail gas purifier of diesel engine |
| CN113398622A (en) * | 2021-05-14 | 2021-09-17 | 暨南大学 | Supercritical CO2Method for preparing wormwood raw pulp by extraction and molecular distillation processes |
-
2021
- 2021-12-14 CN CN202111523940.5A patent/CN114100192A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR19980013975A (en) * | 1996-08-06 | 1998-05-15 | 정명식 | Supercritical Fluid Extraction Method of Plant Metabolites Using Adsorbent |
| CN104225953A (en) * | 2013-06-21 | 2014-12-24 | 中国石油化工股份有限公司 | Absorption apparatus for absorbing aromatic hydrocarbon in geological sample through supercritical carbon dioxide extraction |
| CN209123395U (en) * | 2018-10-26 | 2019-07-19 | 江苏蜂奥生物科技有限公司 | A kind of propolis extracts the CO2 recyclable device of SCF-CO 2 |
| CN110694298A (en) * | 2019-07-15 | 2020-01-17 | 陈龙刚 | Extraction separator for bio-pharmaceuticals |
| CN212716856U (en) * | 2020-05-27 | 2021-03-16 | 无锡市正气环保科技有限公司 | Double-insulation ceramic end cover device of pulse type tail gas purifier of diesel engine |
| CN113398622A (en) * | 2021-05-14 | 2021-09-17 | 暨南大学 | Supercritical CO2Method for preparing wormwood raw pulp by extraction and molecular distillation processes |
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