CN210700036U - Temperature-pressure-controllable supercritical reaction equipment - Google Patents
Temperature-pressure-controllable supercritical reaction equipment Download PDFInfo
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- CN210700036U CN210700036U CN201921248590.4U CN201921248590U CN210700036U CN 210700036 U CN210700036 U CN 210700036U CN 201921248590 U CN201921248590 U CN 201921248590U CN 210700036 U CN210700036 U CN 210700036U
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 57
- 238000000926 separation method Methods 0.000 claims abstract description 23
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 19
- 239000010959 steel Substances 0.000 claims abstract description 19
- 238000010992 reflux Methods 0.000 claims abstract description 4
- 238000009530 blood pressure measurement Methods 0.000 claims description 4
- 238000006073 displacement reaction Methods 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 19
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 238000004321 preservation Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000004338 Dichlorodifluoromethane Substances 0.000 description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 239000001569 carbon dioxide Substances 0.000 description 4
- PXBRQCKWGAHEHS-UHFFFAOYSA-N dichlorodifluoromethane Chemical compound FC(F)(Cl)Cl PXBRQCKWGAHEHS-UHFFFAOYSA-N 0.000 description 4
- 235000019404 dichlorodifluoromethane Nutrition 0.000 description 4
- 239000012530 fluid Substances 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005273 aeration Methods 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000012782 phase change material Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
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Abstract
The utility model discloses a temperature-controllable pressure-controllable supercritical reaction device, which adopts the technical scheme that the device comprises a gas steel cylinder, a booster pump, a reactor and a separating tank which are connected in sequence, wherein the reactor and the booster pump are respectively provided with a pressure display control mechanism, and the reactor is also provided with a temperature display control mechanism and a safety valve; the reflux port of the separation tank is connected to the outlet end of the gas steel cylinder, and the outlet end of the separation tank is connected with a vacuum pump. An object of the utility model is to provide a convenient operation, security performance height, with low costs supercritical reaction system not only will aerify and the reaction part operation has the function of accuse temperature accuse pressure moreover to gaseous recoverable cyclic utilization.
Description
Technical Field
The utility model relates to a controllable temperature accuse pressure supercritical reaction equipment, more specifically says, it relates to the technical field of supercritical reaction equipment.
Background
The supercritical fluid is completely different from the fluid at normal temperature and normal pressure, and has a plurality of unique properties, such as disappearance of a gas-liquid interface, near zero surface tension, large heat conductivity coefficient, low viscosity and the like. These properties are embodied as: 1. the organic phase-change material has good intersolubility with most organic matters, and is particularly applied to supercritical separation; 2. the viscosity is low, the mobility is good, and the method is particularly applied to supercritical reaction; 3. the diffusivity is good, and the supercritical fluid is particularly applied to being used as a reaction medium, such as a porous material void introduction substance, surface coating and the like; 4. easy to control, and the density near the critical point has large variation with temperature and pressure, and is particularly applied to extraction and back extraction in supercritical separation.
Based on the advantages, the supercritical fluid is widely applied to chemical separation, medicine purification and separation of effective components of traditional Chinese medicines such as supercritical extraction; material processing such as supercritical surface coating; chemical reactions such as in supercritical reactions, etc. The current relatively mature equipment is supercritical carbon dioxide extraction equipment, but most equipment does not have gas recovery equipment. The equipment for supercritical reaction and material treatment is basically designed based on a laboratory, is operated manually, is separated from aeration and reaction, lacks temperature and pressure display and control, is complicated to operate, and has higher experience requirements on operators. Preventing the industrial application thereof.
SUMMERY OF THE UTILITY MODEL
Not enough to prior art exists, the utility model aims to provide a convenient operation, security performance height, with low costs supercritical reaction system not only will aerify and the reaction divides the operation, has the function of accuse temperature accuse pressure moreover to gaseous recoverable cyclic utilization.
In order to achieve the above purpose, the utility model provides a following technical scheme: a supercritical reaction device capable of controlling temperature and pressure comprises a gas steel cylinder, a booster pump, a reactor and a separating tank which are connected in sequence, wherein the reactor and the booster pump are respectively provided with a pressure display control mechanism, and the reactor is also provided with a temperature display control mechanism and a safety valve; the reflux port of the separation tank is connected to the outlet end of the gas steel cylinder, and the outlet end of the separation tank is connected with a vacuum pump.
In order to reduce the cost, the pressure display control mechanism and the temperature display control mechanism preferably comprise a simple control system and a feedback system, wherein the simple control system and the feedback system are respectively arranged on the reactor and the booster pump.
In order to make the operation procedure simpler and more accurate, the feedback system preferably receives a signal that the pressure measurement value sent by the simple control system reaches the set value of the booster pump and sends a closing signal to the booster pump and the first valve to control the booster pump and the first valve to close.
In order to achieve an automatic effect and thus reduce human resources, preferably, the feedback system receives a signal that a pressure measurement value sent by the simple control system is lower than a reactor set value and sends an opening signal to the booster pump and the first valve to control the booster pump and the first valve to open.
For better control of the gas admission, it is preferred that the first valve is located between the inlet end of the booster pump and the outlet end of the gas cylinder.
In order to improve the safety, the feedback system preferably receives a signal that the value of the pressure measured value sent by the simple control system exceeds the set value of the reactor and sends an opening signal to the safety valve to control the safety valve to open.
In order to filter dust with different particle sizes in the gas and achieve better circulation effect, preferably, a gas filter screen is arranged between the outlet end of the reactor and the inlet end of the separation tank.
For ease of installation and efficiency, the booster pump is preferably a positive displacement plunger pump or a speed type centrifugal pump.
In order to improve the reaction efficiency, the reactor is preferably a reaction vessel provided with a stirrer, a drum reactor, a tube furnace or a rotary reactor.
In order to ensure reliability and low energy consumption, the simple control system preferably adopts a PLC controller.
The utility model has the advantages that: the system of the utility model can be used for the supercritical reaction of various gases or extraction; the simple control system is adopted to display and control the temperature and the pressure, so that the cost is low; the pressure equipment is provided with a safety valve, and the pressure can be automatically released when reaching a set value so as to prevent safety accidents; the tail end is connected with a separation tank for gas circulation application; the accessories in the equipment are standard spare parts, can be combined at will to be suitable for different operations, and can be widely used for supercritical operation.
Drawings
FIG. 1: is a schematic diagram with control points of the utility model;
FIG. 2: in the simple control system schematic diagram of the utility model, x is a given value, e is a deviation, p is a controller output, q is a manipulated variable, f is an interference, y is a controlled variable, and z is a measured value;
in the figure: 1. a first valve body; 2. a second valve body; 3. a third valve body; 4 a fourth valve body; 5. a fifth valve body; 6. a sixth valve body; 7. a seventh valve body.
Detailed Description
The technical solution of the present invention is further illustrated by the following embodiments and accompanying drawings.
As shown in fig. 1 to 2, a supercritical reaction apparatus with controllable temperature and pressure comprises a gas steel cylinder, a booster pump, a reactor and a separation tank which are connected in sequence, wherein the reactor and the booster pump are respectively provided with a pressure display control mechanism, and the reactor is also provided with a temperature display control mechanism and a safety valve; the reflux port of the separation tank is connected to the outlet end of the gas steel cylinder, and the outlet end of the separation tank is connected with a vacuum pump.
The pressure display control mechanism and the temperature display control mechanism comprise simple control systems respectively arranged on the reactor and the booster pump and a feedback system connected with the simple systems. The simple control system in the reactor is used for display control of the temperature and the pressure in the reactor, and the simple control system in the pressurization is used for display control of the pressure of the booster pump.
The feedback system receives a signal that a pressure measurement numerical value sent by the simple control system reaches a set value of the booster pump, sends a closing signal to the booster pump and the first valve 1 and controls the booster pump and the first valve 1 to be closed. When the system pressure reaches the set pressure of the booster pump, the first valve 1 and the plunger pump are automatically closed.
The feedback system receives a signal that a pressure measured value sent by the simple control system is lower than a reactor set value and sends an opening signal to the booster pump and the first valve 1 to control the booster pump and the first valve 1 to be opened. When the reaction pressure is lower than the set lower pressure limit of the reactor, the automatic control system automatically charges gas.
The first valve 1 is arranged between the inlet end of the booster pump and the outlet end of the gas steel cylinder.
The feedback system receives a signal that a pressure measured value sent by the simple control system exceeds a reactor set value and sends an opening signal to the safety valve to control the safety valve to be opened. When the system pressure exceeds the set upper pressure limit of the reactor, the pressure is automatically released through a safety valve.
And a gas filter screen is arranged between the outlet end of the reactor and the inlet end of the separation tank.
The booster pump is a positive displacement plunger pump or a speed type centrifugal pump.
The reactor is a reaction kettle, a drum-type reactor, a tube furnace or a rotary reactor provided with a stirrer.
The simple control system adopts a PLC controller.
The simple control system adopts a PLC controller. The PLC controller adopts a PID control rule and a DDZ-III type electric explosion-proof actuator.
The reaction equipment comprises any one of the devices combined into supercritical equipment.
By adopting the technical scheme, the method has the advantages that,
example 1:
the utility model provides a supercritical reaction equipment of controllable control by temperature change pressure. According to the schematic diagram shown in figure 1, the method is used for carbon dioxide supercritical reaction. The equipment consists of a carbon dioxide steel cylinder, a plunger pump, a high-pressure reaction kettle with a stirring device and a separation tank.
And (2) operation steps of 1, loading the reaction materials into a high-pressure reaction kettle, and screwing a feed inlet of the high-pressure reaction kettle.
2. And closing the carbon dioxide steel cylinder, opening the first valve 1, the second valve 2, the third valve 3, the sixth valve 6 and the seventh valve 7, opening the vacuum pump, and closing the vacuum pump when the vacuum degree of the system is zero.
3. The third valve 3, the sixth valve 6 and the seventh valve 7 are closed. Setting the inflation pressure of a plunger pump, setting the temperature program, the heating speed, the heat preservation temperature and the heat preservation time of the reaction kettle, setting the upper limit and the lower limit of the reaction pressure of the reaction kettle and setting the stirring speed of the reaction kettle.
4. And opening a carbon dioxide steel cylinder, starting a plunger pump, and inflating the reaction kettle.
5. After the reaction is finished, the second valve 2 and the third valve 3 are closed after the gas is put into the separation tank, and the fourth valve 4 is opened to balance the pressure. The product was then removed from the reaction kettle.
When the system pressure reaches the set pressure of the plunger pump, the valve 1 and the plunger pump are automatically closed, when the system pressure exceeds the set upper pressure limit, the pressure is automatically released through the safety valve, and if the reaction pressure is lower than the lower limit, the system is automatically controlled to automatically charge air.
The system adopts a negative feedback system, a PID control rule and a DDZ-III type electric actuator;
the gas can be recycled according to the condition after being separated by the separating tank.
Example 2:
the utility model provides a supercritical reaction equipment of controllable control by temperature change pressure. According to the schematic diagram shown in figure 1, is used for ethylene supercritical reaction. The equipment consists of an ethylene steel cylinder, a reciprocating compressor, a high-pressure tubular reactor and a separation tank.
And 1, loading the reaction materials into a high-pressure tubular reactor, and screwing a feed inlet of the high-pressure tubular reactor.
2. Closing the ethylene steel cylinder, opening the first valve 1, the second valve 2, the third valve 3, the sixth valve 6 and the seventh valve 7, opening the vacuum pump, and closing the vacuum pump when the vacuum degree of the system is zero.
3. And closing the third valve 3, the sixth valve 6 and the seventh valve 7, setting the inflation pressure of the reciprocating compressor, setting the temperature program, the heating speed, the heat preservation temperature and the heat preservation time of the high-pressure tubular reactor, and setting the upper limit and the lower limit of the pressure of the high-pressure tubular reactor.
4. The ethylene steel cylinder is opened, the reciprocating compressor is started, and the high-pressure tubular reactor is aerated.
5. After the reaction is finished, the gas is put into the separation tank, the second valve 2 and the third valve 3 are closed, and the fourth valve 4 is opened to balance the pressure. The product is then removed from the high pressure tubular reactor.
When the system pressure reaches the set pressure of the reciprocating compressor, the valve 1 and the reciprocating compressor are automatically closed, when the system pressure exceeds the set upper pressure limit, the pressure is automatically released through a safety valve, and if the reaction pressure is lower than the lower limit, the system is automatically controlled to automatically charge air.
The system adopts a negative feedback system and a PID control rule and a DDZ-III type electric actuator.
The gas can be recycled according to the condition after being separated by the separating tank.
Example 3:
the utility model provides a supercritical reaction equipment of controllable control by temperature change pressure. According to the schematic diagram shown in figure 1, the method is used for the dichlorodifluoromethane supercritical reaction. The equipment consists of a dichlorodifluoromethane steel cylinder, a plunger pump, a high-pressure drum reactor and a separation tank.
And (2) an operation step 1 of loading the reaction materials into the high-pressure drum-type reactor and screwing a feed inlet of the high-pressure drum-type reactor.
2. And (3) closing the dichlorodifluoromethane steel cylinder, opening the first valve 1, the second valve 2, the third valve 3, the sixth valve 6 and the seventh valve 7, opening the vacuum pump, and closing the vacuum pump when the vacuum degree of the system is zero.
3. The third valve 3, the sixth valve 6 and the seventh valve 7 are closed. Setting the inflation pressure of a plunger pump, setting the temperature program, the heating speed, the heat preservation temperature and the heat preservation time of the high-pressure drum-type reactor, and setting the upper limit and the lower limit of the pressure of the high-pressure drum-type reactor.
4. And opening a dichlorodifluoromethane steel cylinder, starting a plunger pump, and inflating the high-pressure drum-type reactor.
5. After the reaction is finished, the gas is put into the separation tank, the second valve 2 and the third valve 3 are closed, and the fourth valve 4 is opened to balance the pressure. The product is then removed from the high pressure drum reactor.
When the system pressure reaches the set pressure of the plunger pump, the valve 1 and the plunger pump are automatically closed, when the system pressure exceeds the set upper pressure limit, the pressure is automatically released through the safety valve, and if the reaction pressure is lower than the lower limit, the system is automatically controlled to automatically charge air.
The system adopts a negative feedback system and a PID control rule and a DDZ-III type electric actuator.
It is above only the utility model discloses a preferred embodiment, the utility model discloses a scope of protection does not only confine above-mentioned embodiment, the all belongs to the utility model discloses a technical scheme under the thinking all belongs to the utility model discloses a scope of protection. It should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A controllable temperature and pressure supercritical reaction device is characterized in that: the device comprises a gas steel cylinder, a booster pump, a reactor and a separating tank which are connected in sequence, wherein the reactor and the booster pump are respectively provided with a pressure display control mechanism, and the reactor is also provided with a temperature display control mechanism and a safety valve; the reflux port of the separation tank is connected to the outlet end of the gas steel cylinder, and the outlet end of the separation tank is connected with a vacuum pump.
2. The controllable temperature and pressure supercritical reaction equipment according to claim 1 is characterized in that: the pressure display control mechanism and the temperature display control mechanism comprise simple control systems respectively arranged on the reactor and the booster pump and a feedback system connected with the simple systems.
3. The controllable temperature and pressure supercritical reaction equipment according to claim 2 is characterized in that: the feedback system receives a signal that a pressure measurement numerical value sent by the simple control system reaches a set value of the booster pump, sends a closing signal to the booster pump and the first valve and controls the booster pump and the first valve to be closed.
4. The controllable temperature and pressure supercritical reaction equipment according to claim 2 is characterized in that: the feedback system receives a signal that a pressure measured value sent by the simple control system is lower than a reactor set value and sends an opening signal to the booster pump and the first valve to control the booster pump and the first valve to be opened.
5. The controllable temperature and pressure supercritical reaction apparatus according to any one of claims 3 or 4, characterized in that: the first valve is arranged between the inlet end of the booster pump and the outlet end of the gas steel cylinder.
6. The controllable temperature and pressure supercritical reaction equipment according to claim 2 is characterized in that: the feedback system receives a signal that a pressure measured value sent by the simple control system exceeds a reactor set value and sends an opening signal to the safety valve to control the safety valve to be opened.
7. The controllable temperature and pressure supercritical reaction equipment according to claim 1 is characterized in that: and a gas filter screen is arranged between the outlet end of the reactor and the inlet end of the separation tank.
8. The controllable temperature and pressure supercritical reaction equipment according to claim 1 is characterized in that: the booster pump is a positive displacement plunger pump or a speed type centrifugal pump.
9. The controllable temperature and pressure supercritical reaction equipment according to claim 1 is characterized in that: the reactor is a reaction kettle, a drum-type reactor, a tube furnace or a rotary reactor provided with a stirrer.
10. The controllable temperature and pressure supercritical reaction equipment according to claim 2 is characterized in that: the simple control system is a PLC controller.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921248590.4U CN210700036U (en) | 2019-08-02 | 2019-08-02 | Temperature-pressure-controllable supercritical reaction equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921248590.4U CN210700036U (en) | 2019-08-02 | 2019-08-02 | Temperature-pressure-controllable supercritical reaction equipment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN210700036U true CN210700036U (en) | 2020-06-09 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201921248590.4U Active CN210700036U (en) | 2019-08-02 | 2019-08-02 | Temperature-pressure-controllable supercritical reaction equipment |
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| Country | Link |
|---|---|
| CN (1) | CN210700036U (en) |
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2019
- 2019-08-02 CN CN201921248590.4U patent/CN210700036U/en active Active
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| GR01 | Patent grant | ||
| CP03 | Change of name, title or address |
Address after: 312300 No. 5 Weiqi East Road, Hangzhou Bay Economic and Technological Development Zone, Shangyu District, Shaoxing City, Zhejiang Province Patentee after: Zhejiang Haichuang lithium battery technology Co.,Ltd. Address before: 312369 No. 5, Weiqi East Road, Hangzhou Bay Economic and Technological Development Zone, Shangyu District, Shaoxing City, Zhejiang Province Patentee before: ZHEJIANG MEIDU HAICHUANG LITHIUM ELECTRICITY TECHNOLOGY Co.,Ltd. |
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