CN106823451A - Improve CO2The charging process of supercritical extract yield - Google Patents
Improve CO2The charging process of supercritical extract yield Download PDFInfo
- Publication number
- CN106823451A CN106823451A CN201710107741.3A CN201710107741A CN106823451A CN 106823451 A CN106823451 A CN 106823451A CN 201710107741 A CN201710107741 A CN 201710107741A CN 106823451 A CN106823451 A CN 106823451A
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- China
- Prior art keywords
- raw material
- cloth bag
- steel wire
- yield
- cloth
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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
Abstract
One kind improves CO2The charging process of supercritical extract yield, belongs to supercritical extraction technique field, it is possible to resolve the filling of extraction process loading method is tight in the prior art, and permeability is poor so that extraction yield is unstable and yield is relatively low, the big problem of waste of raw materials, comprises the following steps：If taking dry raw material to be loaded in some cloth bags, and some steel wire lumps are uniformly placed in cloth bag, sealed, taken 8 cloth bags tilings and be positioned over extractive reaction kettle bottom；If separately taking dry raw material, dissipate in 8 cloth bag upper stratas of the first step；The raw material upper strata that 8 cloth bags equipped with raw material and steel wire lump are laid in second step bulk storage is taken again；If dissipating dry raw material again on cloth bag of the 3rd step equipped with raw material and steel wire lump；In this order, alternately placing cloth bag and raw material equipped with raw material and steel wire lump, the output needed for successively.Present invention discharging stabilization, yield is high, can substantially reduce processing cost.
Description
Technical field
The invention belongs to supercritical extraction technique field, and in particular to one kind improves CO2The charging of supercritical extract yield
Technique.
Background technology
Existing traditional extraction process loading method, simply all fills feed chamber by raw material, and material is filled closely, led to
Permeability is very poor so that extraction yield is unstable and yield is relatively low, and waste of raw materials is larger.Therefore, existing traditional extraction process
Loading method, it is unactual also impracticable, it is impossible to meet the requirement of efficiently extraction active principle.
The content of the invention
The present invention is tight in order to solve extraction process loading method filling in the prior art, and permeability is poor so that extract
Rate is unstable and yield is relatively low, the big problem of waste of raw materials, there is provided one kind improves CO2The charger of supercritical extract yield
Skill.
The present invention is adopted the following technical scheme that：
One kind improves CO2The charging process of supercritical extract yield, it is characterised in that：Comprise the following steps：
If a. taking dry raw material to be loaded in some cloth bags, and some steel wire lumps are uniformly placed in cloth bag, sealed, take 8 cloth bags
Tiling is positioned over extractive reaction kettle bottom；
If b. separately taking dry raw material, dissipate in 8 cloth bag upper stratas of the first step；
C. the raw material upper strata that 8 cloth bags equipped with raw material and steel wire lump are laid in second step bulk storage is taken again；
If d. dissipating dry raw material again on cloth bag of the 3rd step equipped with raw material and steel wire lump；
E. in this order, alternately placing cloth bag and raw material equipped with raw material and steel wire lump, the output needed for successively.
The arrangement of raw material and steel wire lump is in the cloth bag：Cloth bag bottom places one layer of raw material, is placed on raw material
Layer of steel wire ball, then one layer of raw material is placed on steel wire lump, sequentially it is sequentially placed with this, the output needed for.
The mass ratio of the raw material summation in the quality of the raw material of every layer of bulk storage and 8 cloth bags is 1:1.
The cloth bag is canvas bag.
Beneficial effects of the present invention are as follows：
Existing traditional CO2Supercritical extraction process charging technology, the effective extract matter for extracting is less, causes and operates into
This height, uneconomical, extract yield height is unstable, and fluctuation is larger, and the active ingredient concentration extracted is also relatively low, often up to
Less than the standard required by enterprise, therefore, existing extraction charging technology is very undesirable.
Use the present invention extraction charging process technology, it is adaptable to raw material be fine particle shape and powder raw material, it is especially wet
It is 20%-70% wet feeds to spend（Permeability is very poor）Supercritical extract active principle operation.Solve CO well2It is overcritical
The problem of material permeability difference in extraction, discharging stabilization, yield is high, can substantially reduce processing cost.
Brief description of the drawings
Fig. 1 is raw material type of feed schematic diagram in cloth bag of the present invention；
Fig. 2 is raw material type of feed schematic diagram in extractive reaction kettle of the present invention；
Fig. 3 is extraction process flow figure of the present invention；
Wherein：1- raw materials；2- steel wire lumps；3- cloth bags.
Specific embodiment
With reference to the drawings and specific embodiments, the present invention will be further described.
One kind improves CO2The charging process of supercritical extract yield, comprises the following steps：
If a. taking dry raw material 1 to be loaded in some cloth bags, and some steel wire lumps 2 are uniformly placed in cloth bag, sealed, take 8 cloth
Bag tiling is positioned over extractive reaction kettle bottom；
If b. separately taking dry raw material 1, dissipate in 8 cloth bag upper stratas of the first step；
C. the upper strata of raw material 4 that 8 cloth bags 3 equipped with raw material 1 and steel wire lump 2 are laid in second step bulk storage is taken again；
If d. dissipating dry raw material 1 again on cloth bag 3 of the 3rd step equipped with raw material 1 and steel wire lump 2；
E. in this order, cloth bag 3 and raw material 1 equipped with raw material 1 and steel wire lump 2 are alternately placed successively, and the output needed for is
Only.
The arrangement of raw material 1 and steel wire lump 2 is in the cloth bag 3：The bottom of cloth bag 3 places one layer of raw material 1, in raw material 1
Upper placement layer of steel wire ball 2, then one layer of raw material 1 is placed on steel wire lump 2, sequentially it is sequentially placed with this, the output needed for.
The mass ratio of the summation of raw material 1 in the quality of the raw material 1 of every layer of bulk storage and 8 cloth bags 3 is 1:1.
The cloth bag 3 is canvas bag.
Embodiment 1, CO2Local flavor constituent test Contrast on effect in supercritical extract vinasse：
1. material requested and testing equipment are tested
Spirit distiller grain：There is provided by Fenjiu Group company of Shanxi Province（It is 60% or so to lose groove moisture content, loses groove moisture content more low better）；
High-pureness carbon dioxide：Purity >=99.99%, food-grade；
Testing equipment：The supercritical extracting equipment of the wound Science and Technology Ltd. of Sichuan Deyang four production.
After installing raw material（Fed with Traditional Method and the inventive method respectively）, by by CO2Injection extraction kettle, pressure-regulating temp-regulating
It is carried extract in the supercritical state, into separating still, then vinasse extract is parsed by decompression（Flavor substance）.
3. implementation process is extracted
After ready work, by boiler water filling heating, cistern water level is checked, boiler heating-up temperature is set to 50-
60 DEG C, as extraction and separator CO2When the temperature for exporting testing temperature point reaches the scope of technique permission, start to be added to kettle
Heat preheating.
Start refrigeration plant, open compressor, start outdoor cooling tower exhausting motor and circulating pump motor, cooling-water machine is entered
Coolant-temperature gage sets the temperature range of unit starting, opens handpiece Water Chilling Units, while cooling water circulating pump is opened, observation condenser,
Flow container point for measuring temperature temperature, distributes cooling water supply amount as one sees fit.
On main frame extraction temperature and separation temperature are set according to contrast experiment's requirement.
During charging, vinasse are entered into kettle with Traditional Method and the present invention respectively, quick-actuating closure is then hung in into extractor, insert wedge
Block and active fastening block complete charging.
In extraction separation process, start oil pump, carbon dioxide pump, carbon dioxide stream is regulated by contrast experiment's requirement
Amount, observation pressure adjusts pressure valve in good time, and extracting pressure, I Stress control of separation are required into numerical value in contrast experiment.
180 min are normally run in system, separator I, the vent valves of II bottom are opened respectively, release all extractions
Flavor substance.
Table 1 is conventional method and the inventive method CO2In supercritical extract vinasse local flavor Comparative experiment parameter and
Yield Data Comparison.
Table 1
Embodiment 2, CO2Supercritical extract Seabuckthorm Seed Oil test effect is contrasted：
1. material requested and testing equipment are tested
Seabuckthorn seeds：High-quality seabuckthorn seeds compressing tablet, moisture 10% ~ 13%；
High-pureness carbon dioxide：Purity >=99.99%, food-grade；
Testing equipment：The supercritical extracting equipment of the wound Science and Technology Ltd. of Sichuan Deyang four production.
2. extraction process and extraction implementation process embodiment 1.
After the normal extraction process of system is completed, separator I, the vent valves of II bottom are opened respectively, release all
The Seabuckthorm Seed Oil of extraction.
Table 2 is conventional method and the inventive method CO2The parameter and yield number of supercritical extract Seabuckthorm Seed Oil contrast test
According to contrast
Table 2
By the CO of both the above different material2Supercritical extract Experimental comparison, other each extraction parameters it is close in addition improve
In the case of Parameter Conditions, change loading method, after being fed using present invention process, display yield is higher, illustrates that the present invention can
Energy consumption is greatlyd save, is conducive to improving productivity effect.
Claims (4)
1. it is a kind of to improve CO2The charging process of supercritical extract yield, it is characterised in that：Comprise the following steps：
If a. taking dry raw material（1）In loaded on some cloth bags, and some steel wire lumps are uniformly placed in cloth bag（2）, seal, take 8
Cloth bag tiling is positioned over extractive reaction kettle bottom；
If b. separately taking dry raw material（1）, dissipate in 8 cloth bag upper stratas of the first step；
C. 8 are taken again equipped with raw material（1）And steel wire lump（2）Cloth bag（3）It is laid in the raw material of second step bulk storage（4）Upper strata；
D. raw material is housed in the 3rd step（1）And steel wire lump（2）Cloth bag（3）If on dissipate dry raw material again（1）；
E. in this order, alternately place successively and raw material is housed（1）And steel wire lump（2）Cloth bag（3）And raw material（1）, it is raw needed for
Untill yield.
2. one kind according to claim 1 improves CO2The charging process of supercritical extract yield, it is characterised in that：The cloth
Bag（3）Middle raw material（1）And steel wire lump（2）Arrangement be：Cloth bag bottom places one layer of raw material（1）, in raw material（1）Upper placement
Layer of steel wire ball（2）, then in steel wire lump（2）One layer of raw material of upper placement（1）, sequentially it is sequentially placed with this, the output needed for.
3. one kind according to claim 1 improves CO2The charging process of supercritical extract yield, it is characterised in that：Every layer
The raw material of bulk storage（1）Quality and 8 cloth bags（3）In raw material（1）The mass ratio of summation is 1:1.
4. the one kind according to Claims 2 or 3 improves CO2The charging process of supercritical extract yield, it is characterised in that：Institute
State cloth bag（3）It is canvas 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 |
Applications Claiming Priority (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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| CN106823451A true CN106823451A (en) | 2017-06-13 |
| CN106823451B CN106823451B (en) | 2020-12-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111937914A (en) * | 2020-09-21 | 2020-11-17 | 祁克兰 | 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 |
| US20090026136A1 (en) * | 2007-06-08 | 2009-01-29 | Beltz Robert J | Method of removing oil from a mixture of tool steel swarf granular material and 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 |
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2017
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| CN1557924A (en) * | 2004-01-12 | 2004-12-29 | 浙江大学 | Supercritical CO2 extraction process for preparing ant oil |
| US20090026136A1 (en) * | 2007-06-08 | 2009-01-29 | Beltz Robert J | Method of removing oil from a mixture of tool steel swarf granular material and oil |
| CN103038195A (en) * | 2010-06-22 | 2013-04-10 | 乌尔里希·迪茨 | Device and method for solubilizing, separating, removing and reacting carboxylic acids in oils, fats, aqueous or organic solutions by means of micro- or nanoemulsification |
| 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 |
| CN205461116U (en) * | 2016-01-18 | 2016-08-17 | 宁波大学 | Flavonoid's extraction element |
| CN106047470A (en) * | 2016-08-01 | 2016-10-26 | 岳西县光圣茶油有限公司 | Supercritical extraction process of tea oil with stomach-nourishing glutinous millet |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111937914A (en) * | 2020-09-21 | 2020-11-17 | 祁克兰 | Insecticide and preparation method thereof |
| 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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| CN106823451B (en) | 2020-12-18 |
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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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