CN2589914Y - Supercritical carbon dioxide drying equipment - Google Patents

Supercritical carbon dioxide drying equipment Download PDF

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Publication number
CN2589914Y
CN2589914Y CN 02295010 CN02295010U CN2589914Y CN 2589914 Y CN2589914 Y CN 2589914Y CN 02295010 CN02295010 CN 02295010 CN 02295010 U CN02295010 U CN 02295010U CN 2589914 Y CN2589914 Y CN 2589914Y
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CN
China
Prior art keywords
drier
carbon dioxide
supercritical carbon
drying device
stop valve
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN 02295010
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Chinese (zh)
Inventor
周亚松
张绍金
姜国伟
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China University of Petroleum Beijing
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China University of Petroleum Beijing
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Priority to CN 02295010 priority Critical patent/CN2589914Y/en
Application granted granted Critical
Publication of CN2589914Y publication Critical patent/CN2589914Y/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Abstract

The utility model relates to a supercritical CO2 drying device which is provided with a CO2 feeder connected with a cooler connected with a booster pump, wherein, the outlet end of the booster pump is connected with at least one drier contained in a thermostatic control device; the front part of the inlet side of the drier is provided with a connector which can be disconnected with the booster pump, and the outlet end of the drier is connected with a detector. The utility model overcomes the defects of a well-known structure, and can safely, reliably and continuously dry articles with identical or different components via supercritical CO2 without interrupting the drying process. In addition, the utility model can help the dried articles be conveniently loaded and unloaded, help to observe the drying degree of the dried articles with high efficiency, regulate temperature and pressure, have reliable and safe drying process and cause the CO2 to be reused by combining with a CO2 recycling pressurizing system.

Description

The supercritical carbon dioxide drying device
Technical field
The utility model relates to a kind of drying device, especially a kind of supercritical carbon dioxide drying device.
Background technology
Drying device is a kind of common equipment of chemical industry, and present known drying device can be divided into following three classes by drying principles: 1, heated drying device; 2, Minton dryer; 3, freeze drying plant.
The shortcoming that above-mentioned three class drying devices all exist is: this body structures of article is all had significantly destroy, the good physics of product self, chemical property have loss significantly after drying; And existing drying device all is step, and efficient is low.
Summary of the invention
The technical problems to be solved in the utility model is: providing a kind of can carry out dry device, especially a kind of supercritical carbon dioxide drying device to article.
Another technical problem to be solved in the utility model is: provide a kind of safe, reliable, do not need to interrupt the supercritical carbon dioxide drying device that dry run just can be carried out continuous drying to the article of identical or different composition.
Technical solution of the present utility model is: a kind of supercritical carbon dioxide drying device, this device has a carbon dioxide feeder, this feeder connects a cooling device, described cooling device is connected with a booster, the port of export of this booster connects at least one drier, this drier is placed in the thermostatically-controlled equipment, and the arrival end front portion of drier is provided with a connector that can break away from booster, and the port of export of described drier connects a detector.
Aforesaid supercritical carbon dioxide drying device is provided with first Pressure gauge and first stop valve between the pipeline of described feeder and cooling device, and this first stop valve is near the feeder setting.
Aforesaid supercritical carbon dioxide drying device, the pipeline between the anterior connector that is provided with of described booster and drier is provided with second Pressure gauge, safety valve and second stop valve, and second Pressure gauge is near the booster setting.
Aforesaid supercritical carbon dioxide drying device, described booster is for annotating the plug pump.
Aforesaid supercritical carbon dioxide drying device, described cooling device are cold-trap.
Aforesaid supercritical carbon dioxide drying device, described drier are a plurality of being arranged in parallel, and its arrival end is connected with the port of export of first demultplexer respectively, and the arrival end of this demultplexer connects booster; The port of export of these a plurality of driers is connected with the arrival end of second demultplexer respectively, and the port of export of this second demultplexer is connected to detector.All be connected with connector and stop valve between the arrival end of described each drier and first demultplexer, and stop valve is near this first demultplexer setting.Be provided with stop valve between the port of export of described each drier and second demultplexer.
Advantage of the present utility model and characteristics are:
1, utilizes supercritical CO 2Can carry out drying to the article that contain organic solvent.
2, the loading and unloading article that are dried are convenient, and drying can be carried out continuously, the degree of drying of the article that can Real Time Observation be dried, efficient height.
3, temperature and pressure can be regulated, and dry run is reliable, safety, can be in conjunction with CO 2Reclaim pressure charging system, make CO 2Recycle.
4, use CO 2Be drier, nontoxic, solubility is big, and is cheap, can reach the efficient pollution-free drying.
5, drying device can be provided with the drier of a plurality of different volumes, and independent mutually, is applicable to the different dryings at the same time or separately that require different volumes or different article.
Description of drawings
Fig. 1 is the structural representation of supercritical carbon dioxide drying device;
Fig. 2 is the another example structure schematic diagram of supercritical carbon dioxide drying device.
The specific embodiment
In order to specify the utility model, be described further below in conjunction with accompanying drawing.
Embodiment 1
As shown in Figure 1, a kind of supercritical carbon dioxide drying device that the utility model proposes, comprise carbon dioxide feeder 1, this feeder 1 connects a cooling device 4, described cooling device 4 is connected with a booster 5, and the port of export of this booster 5 connects at least one drier 15, and this drier 15 is placed in the thermostatically-controlled equipment 13, and the arrival end front portion of drier 15 is provided with a connector 11 that can break away from booster, and the port of export of described drier connects a detector 23.
In the present embodiment, carbon dioxide feeder 1 can be a dioxide bottle or air accumulator, in order to judge whether carbon dioxide is applicable to this dry device 15, on dioxide bottle, be connected with first Pressure gauge 3, and be provided with first stop valve 2 at the front end of first Pressure gauge 3, when first Pressure gauge 3 shows CO 2When gas pressure is lower than setting value, then close first stop valve 2, change feeder 1, or gas cylinder.In order to make carbon dioxide enter booster 5, CO with liquid state 2Gas cylinder is inverted and is provided with.
Described booster 5 and drier 15 anterior 11 of connectors that are provided with are provided with second Pressure gauge 6, overvoltage protection safety valve 7 and second stop valve 8, and second Pressure gauge 6 is provided with near booster 5.
Booster 5 is for annotating the plug pump in the present embodiment, and cooling device 4 can be a cold-trap.The described connector 11 the highest pressure that can bear 16Mpa, described drier 15 adopt the highest sealing ring sealing that can bear 16Mpa, break away from the article that loading and unloading are dried thereby can be convenient to drier 15 with connector 11.In addition, can also be at the port of export of drier in conjunction with CO 2Reclaim pressure charging system, make CO 2Recycle.Above-mentioned first and second Pressure gauge and stop valve, and safety valve also can be arranged in the pipeline of drying device as required in known manner.
Operation principle of the present utility model is: utilize the character of supercritical liq, reach the purpose to the article drying.Supercritical fluid is that a kind of temperature and pressure is in the no vapour on the critical point, the material phase that liquid property and gas property were distinguished and had concurrently in the liquid interface, its character has mutability and controllability, promptly near critical point, the solvent properties of the minor variations meeting remarkable influence fluid of pressure and temperature, as density, solubility parameter etc., thereby can come equilibrium response (balancing each other and solubility), the mass transfer characteristic (heat transfer coefficient, mass tranfer coefficient) of the hierarchy of control, thereby reach dry purpose by the temperature and pressure of the hierarchy of control.
The supercritical carbon dioxide drying is to utilize carbon dioxide distinctive performance under supercriticality; solvent in the dissolved product and impurity; avoid the capillary force that in solvent evaporation process, produces and the pore structure that causes caves in; thereby reach the purpose of in drying, protecting the product self structure to greatest extent, be in particular in the ultra-fine grain that can obtain bigger serface, large pore volume.
In order to make the character of the stable performance supercriticality of carbon dioxide, the utility model through high pressure injection plug measuring pump 5 pressurizations, adopted thermostat 13 that carbon dioxide is worked under its supercriticality before carbon dioxide enters drier 15 simultaneously.
The course of work of the present utility model is: referring to shown in Figure 1, disconnect connector 11, take off drier 15, the article of the needs drying of packing into, with drier 15 and 11 airtight connections of connector, and with the correctly connection as requested of each joint in the pipeline, close stop valve 18, open first stop valve, 2 leak tests, start thermostat 13, and make it reach uniform temperature (40~100 ℃), start cold-trap 4 simultaneously and reach uniform temperature (0~10 ℃), start and annotate plug pump 5, observe second Pressure gauge 6, reach behind the certain pressure (8~14Mpa), open second stop valve 8, and regulate stop valve 18, gas is flowed out with certain flow, by observing the degree of drying that detector 23 detects the article that are dried in real time, after reaching desired degree of drying, close stop valve 8, gas in the emptying drier 15, the arrival end and the connector 11 of drier 15 are thrown off, take out the article that are dried.
In the course of the work, observe first Pressure gauge 3 at any time, work as CO 2When gas pressure is lower than setting value, then close first stop valve 2, change CO 2Air supply source is to guarantee normally carrying out of dry run.
The supercritical carbon dioxide drying device that the utility model proposes, be with nontoxic, free of contamination carbon dioxide as drier, and under supercriticality, article are carried out drying, so said apparatus drying efficiency height, pollution-free.This drying device can be regulated temperature and pressure by control thermostat 13, notes plug pump 5, and dry run is reliable, safety; Connector 11 by drier 15 arrival ends are provided with can load and unload the article that are dried easily; Be arranged on the detector 23 of drier 15 ports of export by observation, the degree of drying of the article that can Real Time Observation be dried improves drying efficiency.
The supercritical carbon dioxide drying device that utilization the utility model proposes, overcome the defective that known technology exists, do not destroy the self structure of the article that are dried in dry run, still can keep the good physics of article, chemical property after drying, and the ultra-fine grain that can obtain having bigger serface, the large pore volume article that are dried.
Embodiment 2
As shown in Figure 2, in the supercritical carbon dioxide drying device that the utility model proposes a plurality of driers can be set, in the accompanying drawing of present embodiment, illustrated three driers 14,15,16 have been set, these a plurality of drying devices are arranged in parallel, its arrival end is connected with the port of export of first demultplexer 9 respectively, and the arrival end of this demultplexer 9 connects booster 5 (annotating the plug pump); The port of export of these a plurality of driers is connected with the arrival end of second demultplexer 24 respectively, and the port of export of this second demultplexer 24 is connected to detector 23.Wherein, correspondingly on the pipeline of the arrival end of described each drier 14,15,16 and 9 of first demultplexers be connected with connector 10,11,12 and stop valve 20,21,22, and stop valve is provided with near this first demultplexer 9.The corresponding stop valve 17,18,19 that is provided with on the pipeline of the port of export of described each drier 14,15,16 and 24 of second demultplexers.For reaching the purpose of the different article of continuous drying, the volume of these a plurality of driers can be identical, or different, and it all can bear the pressure of 8~14Mpa.Connector, the stop valve that is provided with between each drier and pipeline is the highest simultaneously all can bear 16Mpa pressure.And the highest sealing ring that can bear 16MPa pressure is housed in each drier, so that the loading and unloading of the article that are dried.
Its course of work is: disconnect connector 10, take off one of them drier, as drier 16 (this drier can be arranged to the capacity of 200ml), the dry article of needs of packing into connect each joint, close stop valve 17,18,19, and stop valve 21,22, open first, two stop valves 2,8, leak test, start thermostat 13 then, make it reach design temperature (40~100 ℃), start cold-trap 4 simultaneously and reach design temperature (0~10 ℃), start and annotate plug pump 5, observe Pressure gauge 6, (8~14Mpa), adjusting stop valve 19 makes gas flow out with certain flow and enters detector 23 after reaching setting pressure, observe detector 23, after test sample reaches certain degree of drying, close stop valve 20, gas in the emptying drier 16, unload drier 16, take out the article that are dried.
In drier 16 work, can take off drier 18 (can be arranged to the 100ml capacity) and drier 17 (can be arranged to the 50ml capacity) respectively, the different article that are dried of packing into, open stop valve 21,22 then, regulate stop valve 18,17, observe detector 23, its down-stream is same as above.
The drier of a plurality of different volumes can be set in the above-mentioned drying device, and independent mutually, different volumes or different types of thing that is dried can be put in the different driers, carry out drying at the same time or separately and handle.Owing to be provided with a plurality of driers, therefore not needing to interrupt dry run just can carry out continuous drying to the thing that is dried of similar and different kind, has further improved drying efficiency.
Other structure, operating process and the operation principle of present embodiment and obtained beneficial effect are identical with embodiment 1, do not repeat them here.
The above person only; only be specific embodiment of the utility model, when can not with the scope implemented of qualification the utility model, so the displacement of its equivalent assemblies; or, all should still belong to the category that this patent is contained according to equivalent variations and modification that the utility model scope of patent protection is done.

Claims (8)

1, a kind of supercritical carbon dioxide drying device, it is characterized in that: this device has a carbon dioxide feeder, this feeder connects a cooling device, described cooling device is connected with a booster, the port of export of this booster connects at least one drier, this drier is placed in the thermostatically-controlled equipment, and the arrival end front portion of drier is provided with a connector that can break away from booster, and the port of export of described drier connects a detector.
2, supercritical carbon dioxide drying device as claimed in claim 1 is characterized in that: be provided with first Pressure gauge and first stop valve between the pipeline of described feeder and cooling device, and this first stop valve is near the feeder setting.
3, supercritical carbon dioxide drying device as claimed in claim 1, it is characterized in that: the pipeline between the anterior connector that is provided with of described booster and drier is provided with second Pressure gauge, safety valve and second stop valve, and second Pressure gauge is near the booster setting.
4, supercritical carbon dioxide drying device as claimed in claim 1 is characterized in that: described booster is for annotating the plug pump.
5, supercritical carbon dioxide drying device as claimed in claim 1 is characterized in that: described cooling device is a cold-trap.
6, as each described supercritical carbon dioxide drying device of claim 1-5, it is characterized in that: described drier is a plurality of being arranged in parallel, its arrival end is connected with the port of export of first demultplexer respectively, and the arrival end of this demultplexer connects booster; The port of export of these a plurality of driers is connected with the arrival end of second demultplexer respectively, and the port of export of this second demultplexer is connected to detector.
7, supercritical carbon dioxide drying device as claimed in claim 6 is characterized in that: all be connected with connector and stop valve between the arrival end of described each drier and first demultplexer, and stop valve is near this first demultplexer setting.
8, supercritical carbon dioxide drying device as claimed in claim 6 is characterized in that: be provided with stop valve between the port of export of described each drier and second demultplexer.
CN 02295010 2002-12-30 2002-12-30 Supercritical carbon dioxide drying equipment Expired - Fee Related CN2589914Y (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101433562B (en) * 2008-12-17 2011-09-07 中国林业科学研究院林产化学工业研究所 Method for preparing ginkgo leaf extract powder using supercritical liquid desiccation and device thereof
CN102113699B (en) * 2010-11-19 2012-11-21 广东海洋大学 Device and method for drying food by supercritical carbon dioxide
CN102906519A (en) * 2010-05-17 2013-01-30 日产自动车株式会社 Drying method, and drying device
CN104482728A (en) * 2014-10-28 2015-04-01 浙江工业大学 Supercritical CO2 drying method and device for valsartan
CN112013632A (en) * 2020-09-10 2020-12-01 河南科技大学 Drying method
CN114136060A (en) * 2021-11-30 2022-03-04 唐川 Control system of supercritical carbon dioxide drying equipment

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101433562B (en) * 2008-12-17 2011-09-07 中国林业科学研究院林产化学工业研究所 Method for preparing ginkgo leaf extract powder using supercritical liquid desiccation and device thereof
CN102906519A (en) * 2010-05-17 2013-01-30 日产自动车株式会社 Drying method, and drying device
CN102906519B (en) * 2010-05-17 2015-09-16 日产自动车株式会社 Drying means and drying device
US10177416B2 (en) 2010-05-17 2019-01-08 Nissan Motor Co., Ltd. Drying method and drying apparatus
CN102113699B (en) * 2010-11-19 2012-11-21 广东海洋大学 Device and method for drying food by supercritical carbon dioxide
CN104482728A (en) * 2014-10-28 2015-04-01 浙江工业大学 Supercritical CO2 drying method and device for valsartan
CN112013632A (en) * 2020-09-10 2020-12-01 河南科技大学 Drying method
CN114136060A (en) * 2021-11-30 2022-03-04 唐川 Control system of supercritical carbon dioxide drying equipment

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GR01 Patent grant
C17 Cessation of patent right
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20031203

Termination date: 20100201