CN106823451B - Increase of CO2Charging process for supercritical extraction yield - Google Patents
Increase of CO2Charging process for supercritical extraction yield Download PDFInfo
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- CN106823451B CN106823451B CN201710107741.3A CN201710107741A CN106823451B CN 106823451 B CN106823451 B CN 106823451B CN 201710107741 A CN201710107741 A CN 201710107741A CN 106823451 B CN106823451 B CN 106823451B
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- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000000194 supercritical-fluid extraction Methods 0.000 title claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 69
- 239000004744 fabric Substances 0.000 claims abstract description 44
- 238000000605 extraction Methods 0.000 claims abstract description 27
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 26
- 239000010959 steel Substances 0.000 claims abstract description 26
- 238000011068 loading method Methods 0.000 claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- 238000007789 sealing Methods 0.000 claims abstract description 4
- 230000035699 permeability Effects 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 3
- 238000007599 discharging Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 238000003892 spreading Methods 0.000 abstract description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- 238000012360 testing method Methods 0.000 description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 241000229143 Hippophae Species 0.000 description 5
- 235000003145 Hippophae rhamnoides Nutrition 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 4
- 239000000796 flavoring agent Substances 0.000 description 4
- 235000019634 flavors Nutrition 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 3
- 235000015112 vegetable and seed oil Nutrition 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000001816 cooling Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 235000019198 oils Nutrition 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005057 refrigeration Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
Images
Classifications
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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
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0215—Solid material in other stationary receptacles
- B01D11/0219—Fixed bed of solid material
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
Improve CO2A loading process of supercritical extraction yield belongs to the technical field of supercritical extraction, can solve the problems of the prior art that the loading method of the extraction process is tightly filled and has poor permeability, so that the extraction yield is unstable and lower, and the raw material waste is large, and comprises the following steps: taking a plurality of raw materials, putting the raw materials into a plurality of cloth bags, uniformly putting a plurality of steel wire balls in the cloth bags, sealing the cloth bags, and flatly laying 8 cloth bags at the bottom of an extraction reaction kettle; taking a plurality of raw materials, and scattering the raw materials on the upper layer of 8 cloth bags in the first step; spreading 8 cloth bags filled with raw materials and steel wire balls on the upper layer of the raw materials scattered in the second step; a plurality of raw materials are further scattered on the cloth bag filled with the raw materials and the steel wire balls in the third step; according to the sequence, the cloth bags filled with the raw materials and the steel wire balls and the raw materials are alternately placed in turn until the required production capacity is reached. The invention has stable discharging and high yield, and can greatly reduce the processing cost.
Description
Technical Field
The invention belongs to the technical field of supercritical extraction, and particularly relates to a method for improving CO2The loading process of supercritical extraction yield.
Background
The existing traditional extraction process charging method only charges all raw materials into a charging kettle, so that the materials are very tightly filled, the permeability is very poor, the extraction yield is unstable and low, and the raw material waste is large. Therefore, the existing traditional extraction process charging method is impractical and cannot meet the requirement of high-efficiency extraction of effective substances.
Disclosure of Invention
The invention aims to solve the problem of extraction process in the prior artThe charging method has the problems of tight filling, poor permeability, unstable extraction yield, low yield and large waste of raw materials, and provides a method for improving CO2The loading process of supercritical extraction yield.
The invention adopts the following technical scheme:
improve CO2The loading process of the supercritical extraction yield is characterized in that: the method comprises the following steps:
a. taking a plurality of raw materials, putting the raw materials into a plurality of cloth bags, uniformly putting a plurality of steel wire balls in the cloth bags, sealing the cloth bags, and flatly laying 8 cloth bags at the bottom of an extraction reaction kettle;
b. taking a plurality of raw materials, and scattering the raw materials on the upper layer of 8 cloth bags in the first step;
c. spreading 8 cloth bags filled with raw materials and steel wire balls on the upper layer of the raw materials scattered in the second step;
d. a plurality of raw materials are further scattered on the cloth bag filled with the raw materials and the steel wire balls in the third step;
e. according to the sequence, the cloth bags filled with the raw materials and the steel wire balls and the raw materials are alternately placed in turn until the required production capacity is reached.
The arrangement mode of the raw materials and the steel wire balls in the cloth bag is as follows: placing a layer of raw materials on the bottom layer of the cloth bag, placing a layer of steel wire balls on the raw materials, placing a layer of raw materials on the steel wire balls, and sequentially placing the raw materials in the order of the raw materials to obtain the required production.
The mass ratio of the dispersed raw materials of each layer to the total mass of the raw materials in 8 cloth bags is 1: 1.
The cloth bag is a sailcloth bag.
The invention has the following beneficial effects:
existing conventional CO2The loading technology of the supercritical extraction process has the advantages of less extracted effective extraction substances, high operation cost, high and non-economical efficiency, unstable extract yield, high volatility and low concentration of extracted effective components, and often fails to meet the standards required by enterprises, so the existing loading technology of the extraction process is not ideal.
The extraction charging process is suitable for fine granular and powdery raw materialsThe operation of supercritical extraction of effective substances from material, especially wet material with 20-70% humidity (poor permeability). Well solve the problem of CO2The difficult problem of poor material permeability in supercritical extraction, stable discharge, high yield and greatly reduced processing cost.
Drawings
FIG. 1 is a schematic view showing the manner of filling the raw material in the cloth bag according to the present invention;
FIG. 2 is a schematic view of the filling manner of raw materials in the extraction reaction kettle according to the present invention;
FIG. 3 is a flow diagram of the extraction process of the present invention;
wherein: 1-raw material; 2-steel wire balls; 3-cloth bag.
Detailed Description
The invention is further described with reference to the accompanying drawings and specific embodiments.
Improve CO2The charging process of supercritical extraction yield comprises the following steps:
a. taking a plurality of raw materials 1, putting a plurality of steel wire balls 2 in a plurality of cloth bags, sealing, and laying 8 cloth bags at the bottom of an extraction reaction kettle;
b. taking a plurality of raw materials 1, and scattering the raw materials on the upper layer of 8 cloth bags in the first step;
c. then 8 cloth bags 3 filled with the raw materials 1 and the steel wire balls 2 are flatly paved on the upper layer of the raw materials 4 scattered in the second step;
d. a plurality of raw materials 1 are further dispersed on the cloth bag 3 filled with the raw materials 1 and the steel wire balls 2 in the third step;
e. according to the sequence, the cloth bags 3 filled with the raw materials 1 and the steel wire balls 2 and the raw materials 1 are alternately placed in turn until the required production capacity is reached.
The arrangement mode of the raw material 1 and the steel wire balls 2 in the cloth bag 3 is as follows: placing a layer of raw material 1 on the bottom layer of the cloth bag 3, placing a layer of steel wire balls 2 on the raw material 1, placing a layer of raw material 1 on the steel wire balls 2, and sequentially placing the raw materials in the order until the required production is achieved.
The mass ratio of the dispersed raw material 1 of each layer to the total mass of the raw materials 1 in the 8 cloth bags 3 is 1: 1.
The cloth bag 3 is a sailcloth bag.
Example 1, CO2Comparing the test effects of the flavor components in the supercritical extraction vinasse:
1. materials and test equipment for testing
White spirit vinasse: supplied by Fenjiu group company of Shanxi province (the water content of the throwing groove is about 60%, the lower the water content of the throwing groove is, the better);
high purity carbon dioxide: the purity is more than or equal to 99.99 percent, and the food grade is realized;
test equipment: supercritical extraction equipment manufactured by Sichuan Deyang Sichuang science and technology Limited.
After charging the raw materials (by charging respectively using the conventional method and the method of the invention), CO is introduced2Injecting into extraction kettle, regulating pressure and temperature to make it carry extract under supercritical state, introducing into separation kettle, and separating out distiller's grains extract (flavor substances) under reduced pressure.
3. Extraction process
After the preparation work is done, the hot water tank is filled with water for heating, the water level of the hot water tank is checked, the heating temperature of the hot water tank is set to 50-60 ℃, and when CO is generated in the extraction and separation device2And when the temperature of the temperature measuring point at the outlet reaches the range allowed by the process, heating and preheating the kettle body.
Starting the refrigeration equipment, starting the compressor, starting the outdoor cooling tower air draft motor and the circulating pump motor, setting the water inlet temperature of the water cooler to be within the temperature range for starting the unit, starting the water cooler, simultaneously starting the cooling water circulating pump, observing the temperature of temperature measuring points of the condenser and the liquid tank, and distributing the supply amount of cooling water as required.
And setting the extraction temperature and the separation temperature on the computer host according to the comparison experiment requirements.
During charging, the conventional method and the method are respectively used for putting the vinasse into a kettle, then a quick-opening cover is hung into an extractor, and a wedge block and a movable clamping block are inserted to complete charging.
In the extraction separation process, an oil pump and a carbon dioxide pump are started, the flow of carbon dioxide is adjusted according to the comparison experiment requirements, a pressure valve is adjusted in time by observing pressure, and the extraction pressure and the separation I pressure are controlled to be numerical values required by the comparison experiment.
And (4) when the system normally operates for 180 min, respectively opening discharge valves at the bottoms of the separators I and II, and discharging all extracted flavor substances.
Table 1 shows the CO of the conventional Process and of the Process of the invention2And comparing the parameters and yield data of the flavor component comparison test in the supercritical extraction vinasse.
TABLE 1
Example 2, CO2Comparing the test effects of the supercritical extraction of the sea buckthorn seed oil:
1. materials and test equipment for testing
Sea-buckthorn seed: high-quality seabuckthorn seed tablets with the water content of 10-13%;
high purity carbon dioxide: the purity is more than or equal to 99.99 percent, and the food grade is realized;
test equipment: supercritical extraction equipment manufactured by Sichuan Deyang Sichuang science and technology Limited.
2. Extraction process and extraction implementation process example 1.
After the normal extraction process of the system is finished, the discharge valves at the bottoms of the separators I and II are respectively opened to discharge all the extracted seabuckthorn seed oil.
Table 2 shows the conventional process and the process according to the invention CO2Parameter and yield data comparison of supercritical extraction seabuckthorn seed oil comparison test
TABLE 2
CO passing through the above two different raw materials2Compared with supercritical extraction experiments, the method changes the charging method under the condition that other extraction parameters are similar or even the parameter conditions are improved, and the method displays higher yield after charging by applying the process of the invention, which indicates that the invention can greatly save energy consumption and is beneficial to improving production benefits.
Claims (2)
1. Improve CO2The loading process of the supercritical extraction yield is characterized in that: the method comprises the following steps:
a. taking a plurality of raw materials (1) to be filled into a plurality of cloth bags, uniformly placing a plurality of steel wire balls (2) in the cloth bags, sealing the cloth bags, and taking 8 cloth bags to be flatly laid at the bottom of an extraction reaction kettle;
b. taking a plurality of raw materials (1) and scattering the raw materials on the upper layer of 8 cloth bags in the first step;
c. then 8 cloth bags (3) filled with the raw materials (1) and the steel wire balls (2) are flatly paved on the upper layer of the raw materials (4) scattered in the second step;
d. in the third step, a plurality of raw materials (1) are further dispersed on the cloth bag (3) filled with the raw materials (1) and the steel wire balls (2);
e. according to the sequence, the cloth bags (3) filled with the raw materials (1) and the steel wire balls (2) and the raw materials (1) are alternately placed in sequence until the required production capacity is reached;
the arrangement mode of the raw materials (1) and the steel wire balls (2) in the cloth bag (3) is as follows: placing a layer of raw material (1) on the bottom layer of the cloth bag, placing a layer of steel wire balls (2) on the raw material (1), placing a layer of raw material (1) on the steel wire balls (2), and sequentially placing the raw materials in the order until the required production is achieved;
and the mass ratio of the mass of the raw material (1) dispersed in each layer to the total mass of the raw materials (1) in 8 cloth bags (3) is 1: 1.
2. A method of increasing CO according to claim 12The loading process of the supercritical extraction yield is characterized in that: the cloth bag (3) is a sailcloth bag.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710107741.3A CN106823451B (en) | 2017-02-27 | 2017-02-27 | Increase of CO2Charging process for supercritical extraction yield |
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| CN201710107741.3A CN106823451B (en) | 2017-02-27 | 2017-02-27 | Increase of CO2Charging process for supercritical extraction yield |
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| CN106823451A CN106823451A (en) | 2017-06-13 |
| CN106823451B true CN106823451B (en) | 2020-12-18 |
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| CN111937914B (en) * | 2020-09-21 | 2021-08-24 | 淮北市菲美得环保科技有限公司 | Insecticide and preparation method thereof |
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|---|---|---|---|---|
| CN1557924A (en) * | 2004-01-12 | 2004-12-29 | 浙江大学 | Supercritical CO2 extraction process for preparing ant oil |
| CN102888281A (en) * | 2012-10-19 | 2013-01-23 | 吉林人参研究院 | Method for extracting ginseng volatile oil by supercritical CO2 |
| CN103038195A (en) * | 2010-06-22 | 2013-04-10 | 乌尔里希·迪茨 | Apparatus and method for solubilization, separation, removal and reaction of carboxylic acids in oils, fats, aqueous or organic solutions by microemulsion or nanoemulsion |
| WO2014097319A1 (en) * | 2012-12-22 | 2014-06-26 | Sevak Niravkumar Prakashbhai | Extraction method for organic certifiable steviosides from organic stevia leaves |
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Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008154367A2 (en) * | 2007-06-08 | 2008-12-18 | Kalumetals, Inc. | Method of removing oil from a mixture of tool steel swarf granular material and oil |
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- 2017-02-27 CN CN201710107741.3A patent/CN106823451B/en active Active
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| CN1557924A (en) * | 2004-01-12 | 2004-12-29 | 浙江大学 | Supercritical CO2 extraction process for preparing ant oil |
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| CN102888281A (en) * | 2012-10-19 | 2013-01-23 | 吉林人参研究院 | Method for extracting ginseng volatile oil by supercritical CO2 |
| WO2014097319A1 (en) * | 2012-12-22 | 2014-06-26 | Sevak Niravkumar Prakashbhai | Extraction method for organic certifiable steviosides from organic stevia leaves |
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Effective date of registration: 20201126 Address after: 030024 Shanxi city of Taiyuan province Jinci million Berlin District Road No. 19 A Applicant after: Shanxi Food Research Institute (Ltd.) Address before: 030024 Shanxi city of Taiyuan province Jinci million Berlin District Road No. 19 A Applicant before: SHANXI FOOD INDUSTRIAL Research Institute |
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