CN215337336U - Supercritical carbon dioxide drying device - Google Patents
Supercritical carbon dioxide drying device Download PDFInfo
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- CN215337336U CN215337336U CN202121029516.0U CN202121029516U CN215337336U CN 215337336 U CN215337336 U CN 215337336U CN 202121029516 U CN202121029516 U CN 202121029516U CN 215337336 U CN215337336 U CN 215337336U
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Abstract
The utility model discloses a supercritical carbon dioxide drying device, which relates to the technical field of supercritical drying equipment and comprises a carbon dioxide liquid storage bottle, a drying kettle and a separation component for separating moisture from carbon dioxide, wherein an air outlet of the drying kettle is connected with the separation component, and the separation component is connected with the carbon dioxide liquid storage bottle; the separation component is also provided with a compressor used for extracting carbon dioxide in the drying kettle in parallel; according to the utility model, the compressor is arranged in parallel with the separation component, so that the pressure in the drying kettle can be reduced to the pressure of the carbon dioxide liquid storage bottle, and when the carbon dioxide in the kettle can not be automatically discharged, the carbon dioxide in the kettle can be timely discharged by using the compressor, so that the carbon dioxide in the kettle can be recycled, the phenomenon that the kettle cover is directly opened to cause large waste of the carbon dioxide can be avoided, residual moisture extracted from the carbon dioxide can be discharged, and the better and thorough drying effect on the materials can be ensured.
Description
Technical Field
The utility model relates to the technical field of supercritical drying equipment, in particular to a supercritical carbon dioxide drying device.
Background
The supercritical drying technology is a new chemical technology developed in recent years. The commonly used drying technologies such as normal temperature drying, baking drying and the like often inevitably cause material agglomeration in the drying process, thereby generating the results of coarsening of material base particles, sharp reduction of specific surface, great reduction of pores and the like, which is extremely disadvantageous for the acquisition of nano materials and the preparation of high specific surface materials; the supercritical drying technology is drying under the conditions of critical pressure and critical medium, and can avoid the shrinkage and fragmentation of the material in the drying process, thereby keeping the original structure and state of the material and preventing the agglomeration and coagulation of primary nanoparticles, which is very significant for the preparation of various nano materials.
The supercritical carbon dioxide fluid is a good drying medium because the critical temperature of the carbon dioxide is close to room temperature, and the supercritical carbon dioxide fluid is non-toxic, non-flammable and non-explosive, has gas and liquid properties, and has strong diffusivity and good dissolving capacity. The liquid carbon dioxide replacement supercritical drying method is to perform supercritical drying by using carbon dioxide to replace an organic solvent as a drying medium. The method comprises the steps of replacing a liquid solvent in a material with liquid carbon dioxide, heating and pressurizing to enable the carbon dioxide to reach a supercritical state, and finally drying the material by utilizing the supercritical property of the carbon dioxide. The supercritical carbon dioxide extraction drying method is the combination of the supercritical extraction technology and the supercritical fluid drying technology, compared with the liquid carbon dioxide replacement supercritical drying method, the method can omit the step of replacing the solvent by the liquid carbon dioxide, directly extract the solvent in the micropores of the material by the supercritical carbon dioxide, dry the material under the condition of basically keeping the original structure and simplify the operation steps.
The application number is '201010565950.0', the name is 'a device and a method for drying food by supercritical carbon dioxide', carbon dioxide is introduced into a drying chamber, then the temperature is raised and the pressure is increased to the supercritical state, moisture in the food is absorbed, finally the carbon dioxide is discharged by using the high-pressure atmosphere in the drying chamber, the carbon dioxide enters a gas-water separator for moisture separation, the moisture is discharged from the gas-water separator, and the carbon dioxide is recycled; however, in the actual operation process, it is found that when the drying chamber is opened after the drying process is finished, a large amount of carbon dioxide still exists in the drying chamber, and it can be determined that carbon dioxide in the drying chamber cannot be completely discharged and remains, and the direct opening of the drying chamber to exhaust air causes a large amount of waste of carbon dioxide, and the remaining carbon dioxide gas has a weak ability to dissolve moisture, and the moisture is easily absorbed by the food again due to the long-time retention in the drying chamber, so that the food is not completely dried.
Therefore, how to improve the drying efficiency of the material to be dried is a technical problem which needs to be solved urgently in the field.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a supercritical carbon dioxide drying device, which is used for solving the problems in the prior art, reducing the waste of carbon dioxide and improving the drying effect of an article to be dried.
In order to achieve the purpose, the utility model provides the following scheme: the utility model provides a supercritical carbon dioxide drying device which comprises a carbon dioxide liquid storage bottle, a drying kettle and a separation component for separating moisture from carbon dioxide, wherein the carbon dioxide liquid storage bottle is connected with an air inlet of the drying kettle through a pressure pump, an air outlet of the drying kettle is connected with the separation component, and the separation component is connected with the carbon dioxide liquid storage bottle; the separation component is also provided with a compressor in parallel for pumping out the carbon dioxide in the drying kettle, and a first valve and a second valve thereof are respectively arranged between the separation component and the drying kettle and between the compressor and the drying kettle.
Preferably, the second valve is a self-control valve, a pressure transmitter for detecting the pressure in the pipeline is further arranged on the pipeline between the separation component and the drying kettle, and the pressure transmitter is electrically connected with the self-control valve.
Preferably, the separation component comprises a cooler, a gas-water separator and a moisture adsorber thereof which are sequentially connected, the cooler is connected with the drying kettle, and the moisture adsorber is connected with the carbon dioxide liquid storage bottle.
Preferably, a condenser for condensing carbon dioxide gas is arranged on a pipeline between the carbon dioxide liquid storage bottle and the separation assembly and between the carbon dioxide liquid storage bottle and the compressor.
Preferably, the pipeline between the self-control valve and the drying kettle and the pipeline between the compressor and the drying kettle are also provided with a filter for filtering the material to be dried.
Preferably, a preheater for preheating carbon dioxide is further arranged between the pressurizing pump and the drying kettle.
Preferably, a plurality of drying kettles are connected in parallel in the drying device, and valves are independently arranged between the plurality of drying kettles, the filter and the preheater.
Preferably, a flow meter for monitoring the flow of the carbon dioxide is further arranged on a pipeline between the carbon dioxide liquid storage bottle and the drying kettle.
The utility model also provides a supercritical carbon dioxide drying method, which comprises the following steps:
1) adding a material to be dried into a drying kettle, and heating the drying kettle and a preheater to a set temperature;
2) opening a carbon dioxide pump, and filling carbon dioxide into the drying kettle until the pressure in the drying kettle reaches a set pressure, so that the carbon dioxide reaches a supercritical state;
3) after drying is finished, opening an automatic control valve to enable the mixed gas of the carbon dioxide and the water in the drying kettle to enter a cooler and a gas-water separator for separation;
4) when the pressure in the drying kettle is reduced to the pressure in the carbon dioxide liquid storage bottle, closing the automatic control valve, opening a valve between the compressor and the filter, and recovering the carbon dioxide in the drying kettle through the compressor;
5) and finally, opening the drying kettle, and taking out the materials to finish the drying process.
Preferably, after step 1), the drying kettle is evacuated and then step 2) is performed.
Compared with the prior art, the utility model has the following technical effects:
1. according to the utility model, the compressor is arranged in parallel with the separation component, so that the pressure in the drying kettle can be reduced to the pressure of the carbon dioxide liquid storage bottle, and when the carbon dioxide in the kettle can not be automatically discharged, the compressor can be used for discharging the carbon dioxide, so that the carbon dioxide in the kettle can be recycled, the phenomenon that the kettle cover is directly opened to cause large waste of the carbon dioxide is avoided, the drying cost is improved, meanwhile, the moisture extracted from the carbon dioxide can be discharged in time, the capacity of the carbon dioxide carrying the moisture after the carbon dioxide is changed into a gaseous state from a supercritical state is prevented from being reduced, the moisture separated from the carbon dioxide is retained in the drying kettle for a long time and is absorbed by the material again, and the better and thorough drying effect on the material is ensured;
2. the compressor and the separating assembly are arranged in parallel, so that the initial automatic exhaust process of the drying kettle is independent from the later passive air extraction process, the two-stage exhaust process is ensured to be normally carried out, the compressor and the separating assembly are prevented from being connected in series, and the normal exhaust of the drying kettle is influenced by the fact that the compressor does not work in the initial exhaust process;
3. according to the utility model, the branch pipe is arranged on the exhaust pipeline of the compressor, and air remained in the drying kettle is removed through the compressor before an experiment, so that the purity of the supercritical carbon dioxide fluid is ensured, the water carrying efficiency of the supercritical carbon dioxide is improved, and the drying efficiency is further improved.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without inventive exercise.
FIG. 1 is a schematic view of the structure of a drying apparatus according to the present invention;
wherein, 1, a carbon dioxide liquid storage bottle; 2. a pressure pump; 3. drying the kettle; 4. a compressor; 5. a cooler; 6. a first gas-water separator; 7. a second gas-water separator; 8. a moisture adsorber; 9. a condenser; 10. a first valve; 11. a pressure transmitter; 12. a self-control valve; 13. a filter; 14. a preheater; 15. a first temperature sensor; 16. a second temperature sensor; 17. a pressure gauge; 18. a safety valve; 19. a flow meter; 20. and (4) branch pipes.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The utility model aims to provide a supercritical carbon dioxide drying device, which is used for solving the problems in the prior art, reducing the waste of carbon dioxide and improving the drying effect of an article to be dried.
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in further detail below.
Example 1:
as shown in fig. 1, the embodiment provides a supercritical carbon dioxide drying device, which includes a carbon dioxide liquid storage bottle 1, a drying kettle 3 and a separation assembly for separating moisture from carbon dioxide, wherein the carbon dioxide liquid storage bottle 1 is connected with an air inlet of the drying kettle 3 through a pressure pump 2, an air outlet of the drying kettle 3 is connected with the separation assembly, and the separation assembly is connected with the carbon dioxide liquid storage bottle 1; the separating component is also provided with a compressor 4 used for extracting carbon dioxide from the drying kettle 3 in parallel, and a first valve 10 and a second valve thereof are respectively arranged between the separating component, the compressor 4 and the drying kettle 3.
When the drying device works, all valves in an initial state are closed, no carbon dioxide exists in a pipeline in the system, the carbon dioxide liquid storage bottle 1 is filled with the carbon dioxide, firstly, a material to be dried is placed into the drying kettle 3, then the carbon dioxide is introduced into the drying kettle 3 through the pressure pump 2 until the pressure in the drying kettle 3 reaches a preset pressure, then the drying kettle 3 is heated, the carbon dioxide in the drying kettle 3 is in a supercritical state, the moisture in the material in the drying kettle 3 is absorbed, after a period of reaction, an exhaust valve and a first valve 10 of the drying kettle 3 are opened, the carbon dioxide in the drying kettle 3 is gradually discharged into the separation assembly, and the carbon dioxide and the moisture are separated; when the pressure in the drying kettle 3 is reduced to the pressure in the carbon dioxide liquid storage bottle 1, the first valve 10 is closed, the second valve is opened, the compressor 4 is started to pump out the carbon dioxide in the drying kettle 3, finally, the pressure is adjusted to be normal pressure in the drying kettle 3, the kettle body is opened, the material to be dried is taken out, and drying is completed.
From this, this embodiment is through parallelly connected compressor 4 that sets up with the separator assembly, can reduce to 1 pressure of carbon dioxide stock solution bottle in drying kettle 3, when carbon dioxide can not the automatic discharge in the cauldron, utilize compressor 4 to discharge it, not only can carry out recycle to carbon dioxide in the cauldron, avoid carbon dioxide to waste in a large number, improve drying cost, can also in time discharge carbon dioxide extraction's moisture, prevent that carbon dioxide from being reduced by the ability that carries moisture behind the supercritical state becoming gaseous state, the moisture that appears in the carbon dioxide is detained for a long time in drying kettle 3 and is appeared by the absorptive condition of material again, guarantee to the better thorough of drying effect of material.
It should be noted that the initial stage of the exhaust of the drying kettle 3 is an exhaust process which is spontaneously performed due to a strong internal pressure of the kettle, and unnecessary equipment except for gas-water separation should be avoided as much as possible on the exhaust pipeline; if the compressor 4 is connected in series with the separation component, the compressor can seriously obstruct the normal exhaust process because the compressor does not need to work in the exhaust initial stage of the drying kettle 3; therefore, the compressor 4 and the separating component are arranged in parallel in the embodiment, so that the automatic exhaust process at the initial stage of the drying kettle 3 is independent from the passive air exhaust process at the later stage, the automatic exhaust process and the passive air exhaust process are not interfered with each other, and the normal operation of the two-stage exhaust process is ensured.
In order to ensure that the carbon dioxide recovered by the compressor 4 has a low moisture content, a moisture adsorption device may be connected in series after the compressor 4.
The second valve is automatic control valve 12 in this embodiment, still be provided with the pressure transmission 11 that is arranged in detecting the pipeline pressure on the pipeline between separator and drying kettle 3, pressure transmitter 11 sets up between automatic valve 12 and drying kettle 3, be connected with the automatic control valve electricity, and the two is connected with the PLC controller electricity simultaneously, utilize pressure transmitter 11 to monitor the pressure in drying kettle 3 constantly, and feed back the data control automatic control valve 12 volume of discharging to the PLC controller according to it, thereby stabilize accuse pressure to drying kettle 3.
Further, the separation assembly in the embodiment comprises a cooler 5, a gas-water separator and a moisture adsorber 8 thereof, which are connected in sequence, wherein the cooler 5 is connected with the drying kettle 3, and the moisture adsorber 8 is connected with the carbon dioxide liquid storage bottle 1; the cooler 5 is used for cooling the carbon dioxide to change the carbon dioxide from a supercritical state to a gaseous state, so that the capacity of carrying moisture is reduced, and the carbon dioxide gas and the moisture are easier to separate; the gas-water separator is used for thoroughly separating carbon dioxide gas from moisture, two gas-water separators can be arranged in series, namely a first gas-water separator 6 and a second gas-water separator 7, so as to ensure the separation effect of the moisture and the carbon dioxide, and drainage valves are arranged at the bottoms of the first gas-water separator 6 and the second gas-water separator 7; the moisture adsorber 8 is used for adsorbing residual moisture in the carbon dioxide gas to ensure the purity of the carbon dioxide.
In order to convert the carbon dioxide discharged from the drying kettle 3 into liquid, a condenser 9 for condensing the carbon dioxide gas is disposed on the pipeline between the carbon dioxide liquid storage bottle 1 and the separation assembly and between the carbon dioxide liquid storage bottle and the compressor 4 in the embodiment.
Because the drying kettle 3 can dry the nano-scale powder, and the supercritical carbon dioxide and the carbon dioxide gas thereof may carry the powder in the discharging process, in order to prevent the large particles to be dried from blocking the automatic control valve 12 and the compressor 4 thereof, the main pipeline between the automatic control valve 12, the compressor 4 and the drying kettle 3 in the embodiment is further provided with a filter 13 for filtering the material to be dried.
In this embodiment, a heating jacket for heating the drying kettle 3 is arranged outside the drying kettle 3, in order to reduce the heat required by the heating kettle body, a preheater 14 for preheating carbon dioxide is further arranged between the heating pump 2 and the drying kettle 3 in this embodiment, and is used for preheating carbon dioxide gas, and a first temperature sensor 15 for detecting temperature is arranged at the preheater 14; the drying kettle 3 is also provided with a second temperature sensor 16, a pressure gauge 17 and a safety valve 18 thereof, the pressure gauge 17 and the safety valve 18 thereof are common devices on the drying kettle 3, and the description of the embodiment is omitted.
The drying device disclosed in this embodiment is not limited to only having one drying kettle 3, and may be arranged in parallel, and a plurality of drying kettles 3, the filter 13 and the preheater 14 thereof are all provided with valves individually, and the drying process is relatively independent. Preferably, a smaller volume of the experimental drying kettle 3 can be provided for studying the drying process.
In order to guarantee the accuracy of experiment, this embodiment sets up a branch pipe 20 on compressor 4's exhaust pipe, this branch pipe 20 is parallelly connected with the pipeline of retrieving carbon dioxide, set up the valve on branch pipe 20, can switch between evacuation process and the carbon dioxide recovery process thereof, be arranged in getting rid of the air that is detained in drying kettle 3 through compressor 4 before the experiment, guarantee supercritical carbon dioxide fluid purity, improve supercritical carbon dioxide and carry water efficiency, and then improve drying efficiency, get rid of the influence of air to material drying process in drying kettle 3, ensure experimental research's accuracy. Of course, the air may be discharged through the compressor 4 in the actual drying process to ensure the drying efficiency.
Further, a flow meter 19 for monitoring the flow rate of carbon dioxide is further arranged on a pipeline between the carbon dioxide liquid storage bottle 1 and the drying kettle 3 in the embodiment.
It should be noted that, in the present embodiment, the flow meter 19, the first temperature sensor 15, the second temperature sensor 16, and the pressure gauge 17 are all electrically connected to the PLC controller, and the whole drying device is automatically controlled by the PLC controller, and the PLC control program and the control method thereof are numerical values of those skilled in the art, which are not described in detail in this embodiment.
Example 2:
the embodiment provides a supercritical carbon dioxide drying method, which comprises the following steps:
1) adding a material to be dried into the drying kettle 3, and heating the drying kettle 3 and the preheater 14 to a set temperature;
2) opening a carbon dioxide pump, filling carbon dioxide into the drying kettle 3 until the pressure in the drying kettle 3 reaches a set pressure, so that the carbon dioxide in the kettle is in a supercritical state, and extracting moisture in the material to be dried;
3) after drying, opening the self-control valve 12 to enable the mixed gas of the carbon dioxide and the moisture in the drying kettle 3 to enter the cooler 5 and the gas-water separator for separation, condensing the separated carbon dioxide gas through the condenser 9 and then entering the carbon dioxide liquid storage bottle 1 for storage;
4) when the pressure in the drying kettle 3 is reduced to the pressure in the carbon dioxide liquid storage bottle 1, closing the automatic control valve 12, opening the first valve 10 between the compressor 4 and the filter 13, and recovering the carbon dioxide in the drying kettle 3 through the compressor 4;
5) and finally, opening the drying kettle 3, and taking out the materials to finish the drying process.
Wherein, after step 1), close the valve between compressor 4 and condenser 9, open the valve on the branch pipe 20, to 3 evacuation of drying kettle, get rid of the influence of air in the cauldron to the drying process, guarantee supercritical carbon dioxide fluid purity, improve supercritical carbon dioxide and carry water efficiency, and then improve drying efficiency, then carry out step 2).
It should be noted that the drying method disclosed in this embodiment may be divided into intermittent drying and continuous drying, wherein in the intermittent drying method, carbon dioxide is introduced into the drying kettle 3 until the internal pressure of the kettle is stable, the pressure pump 2 is closed, the self-control valve 12 is opened after the reaction is performed for a certain time, and carbon dioxide is discharged; in the continuous drying method, after carbon dioxide is introduced into the drying kettle 3 until the pressure inside the kettle body is stable, the pressure pump 2 continues to work, the automatic control valve 12 is opened, the pressure in the drying kettle 3 is kept stable, and the carbon dioxide is continuously discharged and circulated in the whole device.
The adaptation according to the actual needs is within the scope of the utility model.
It will be evident to those skilled in the art that the utility model is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the utility model being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (8)
1. A supercritical carbon dioxide drying device is characterized by comprising a carbon dioxide liquid storage bottle, a drying kettle and a separation component for separating moisture from carbon dioxide, wherein the carbon dioxide liquid storage bottle is connected with an air inlet of the drying kettle through a pressure pump, an air outlet of the drying kettle is connected with the separation component, and the separation component is connected with the carbon dioxide liquid storage bottle; the separation component is also provided with a compressor in parallel for pumping out the carbon dioxide in the drying kettle, and a first valve and a second valve thereof are respectively arranged between the separation component and the drying kettle and between the compressor and the drying kettle.
2. The supercritical carbon dioxide drying apparatus according to claim 1, wherein the second valve is a self-control valve, a pressure transmitter for detecting the pressure in the pipeline is further disposed on the pipeline between the separation assembly and the drying kettle, and the pressure transmitter is electrically connected to the self-control valve.
3. The supercritical carbon dioxide drying device as claimed in claim 2, wherein the separation assembly comprises a cooler, a gas-water separator and a moisture adsorber thereof, the cooler is connected with the drying kettle, and the moisture adsorber is connected with the carbon dioxide liquid storage bottle.
4. The supercritical carbon dioxide drying apparatus according to claim 3 is characterized in that a condenser for condensing carbon dioxide gas is arranged on a pipeline between the carbon dioxide storage bottle and the separation component and between the carbon dioxide storage bottle and the compressor.
5. The supercritical carbon dioxide drying apparatus according to claim 4, wherein a filter for filtering the material to be dried is further provided on the pipeline between the self-control valve, the compressor and the drying kettle.
6. The supercritical carbon dioxide drying apparatus according to claim 5, wherein a preheater for preheating carbon dioxide is further provided between the pressure pump and the drying kettle.
7. The supercritical carbon dioxide drying apparatus according to claim 6, wherein a plurality of drying kettles are connected in parallel in the drying apparatus, and valves are separately provided between the plurality of drying kettles and the filter and the preheater thereof.
8. The supercritical carbon dioxide drying apparatus according to claim 1, wherein a flow meter for monitoring the flow rate of carbon dioxide is further provided on the pipeline between the carbon dioxide storage bottle and the drying kettle.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113108558A (en) * | 2021-05-14 | 2021-07-13 | 中昊光明化工研究设计院有限公司 | Supercritical carbon dioxide drying device and drying method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113108558A (en) * | 2021-05-14 | 2021-07-13 | 中昊光明化工研究设计院有限公司 | Supercritical carbon dioxide drying device and drying method thereof |
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