CN212549473U - Catalyst recycling device for producing valeronitrile through solvent-free hydrogenation - Google Patents
Catalyst recycling device for producing valeronitrile through solvent-free hydrogenation Download PDFInfo
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- CN212549473U CN212549473U CN202020976138.6U CN202020976138U CN212549473U CN 212549473 U CN212549473 U CN 212549473U CN 202020976138 U CN202020976138 U CN 202020976138U CN 212549473 U CN212549473 U CN 212549473U
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Abstract
The utility model relates to a hydrogenation catalyst recycles device, especially relates to a device that intermittent type cauldron formula hydrogenation reactor catalyst recycles. The utility model relates to a catalyst recycling device of solvent-free hydrogenation production valeronitrile, including the hydrogenation cauldron that sets gradually, filter and liquid storage pot, through first pipe connection between hydrogenation cauldron and the filter, through second pipe connection between filter and the liquid storage pot, be equipped with clean valve under hydrogenation cauldron feed valve and the hydrogenation cauldron on the hydrogenation cauldron, feed valve and clean valve under the last bleeder valve of hydrogenation cauldron and the filter of being equipped with on the first pipeline, bleeder valve and filter lotion valve on being equipped with the filter on the filter, be equipped with the business turn over valve under business turn over valve and the liquid storage pot on the second pipeline, the liquid storage pot includes air discharge valve and liquid storage pot nitrogen valve on the liquid storage pot.
Description
Technical Field
The utility model relates to a hydrogenation catalyst recycles device, especially relates to a device that intermittent type cauldron formula hydrogenation reactor catalyst recycles.
Background
The batch reactor is the most common hydrogenation reactor and is used for realizing liquid-liquid, gas-liquid, liquid-solid, gas-liquid-solid and other multiphase reaction processes. It uses the noble metals of skeleton nickel, palladium carbon, platinum carbon, etc. as catalyst to make various hydrogenation reactions. The catalyst often plays a decisive role in the overall hydrogenation reaction during the reaction. In addition, the value of the noble metal catalyst is very high, so that the hydrogenation reaction is carried out by using the kettle type reactor in the industrial production at present, and the recycling of the catalyst is particularly important (the catalyst recycling device of the utility model is only suitable for the intermittent kettle type reactor).
The role of the catalyst in the reaction process is very important in order to ensure the purity and quality of the hydrogenation product. Most of the tank reactors are pressurized closed pressure vessels, so that a certain temperature and pressure are always applied in the production process, solid catalysts must be added and separated in each batch of product reaction, the catalysts are required to be repeatedly separated and added in the continuous production of the reactors, and at present, in actual operation, the catalysts are filtered by a filter, manually taken out of the filter, and then put into the reactor to serve as the catalysts for the next batch. The operation not only wastes a large amount of manpower and material resources, but also prolongs the production time, so that the productivity and the quality of the product are restricted. It also brings unsafe operation and causes accidents.
In view of the above, the present inventors have studied on this, and developed a recycling apparatus for hydrogenation catalyst, which has been developed.
Disclosure of Invention
The utility model aims at providing a hydrogenation catalyst recycles device, the erection joint is in the same place, can pass through the internal circulation to the catalyst in the reation kettle, and the contactless is external, realizes in the system that the circulation is used mechanically, and a batch connects a batch of continuous used repeatedly, has both solved artifical problem of taking out the catalyst from the filter, has guaranteed again that the safety of catalyst throws the material and has had no loss circulation to use. Meanwhile, the quality of the product and the safety and reliability of operation are greatly improved.
In order to achieve the above object, the solution of the present invention is:
the utility model provides a catalyst recycling device of solvent-free hydrogenation production valeronitrile, is including the hydrogenation cauldron that sets gradually, filter and liquid storage pot, through first pipe connection between hydrogenation cauldron and the filter, pass through the second pipe connection between filter and the liquid storage pot, be equipped with the purge valve under hydrogenation cauldron feed valve and the hydrogenation cauldron on the hydrogenation cauldron, be equipped with bleeder valve on the hydrogenation cauldron on the first pipeline, feed valve and filter purge valve under the filter, the filter is equipped with bleeder valve on the filter, be equipped with the filter on the second pipeline and go into the bleeder valve under business turn over valve and the liquid storage pot, the liquid storage pot includes air discharge valve and liquid storage pot nitrogen valve on the liquid storage pot.
The filter is provided with a filter washing liquid valve.
A plurality of sintered titanium filter rods are arranged in the filter (a screw hole pattern plate is arranged in the filter, and external thread connecting screw threads are welded at the upper ends of the sintered titanium filter rods, namely the sintered titanium filter rods are connected to the screw hole pattern plate in a threaded mode). The sintered titanium filter stick is cylindrical and is formed by sintering tiny titanium metal balls at high temperature. When the material enters the sintered titanium filter stick in the filter, the hydrogenated liquid is separated out through the holes formed by the metal balls, and the catalyst is left on the surface of the sintered titanium filter stick. When the catalyst is recovered, the hydrogenated liquid reversely punches the inner wall of the sintered titanium filter stick, and the catalyst is punched back into the hydrogenation reaction kettle by using gravity. Because the fixed filter is adopted, the catalyst can be recycled under the closed condition without opening or contacting.
The hydrogenation reaction kettle comprises a self-suction stirring device. Under the high-speed operation of the hollow shaft, hydrogen in the hydrogenation reaction kettle enters the hollow shaft through the air suction disc at the upper end of the hollow shaft and is thrown out of the distribution disc at the middle lower end of the hollow shaft to become a large amount of tiny hydrogen bubbles which are uniformly distributed in liquid, so that the catalyst, the liquid raw material and the hydrogen (solid, liquid and gas) are fully mixed and fully reacted.
From inhaling formula agitating unit and including agitator motor and hollow shaft, be equipped with air suction disc and distribution disc on the hollow shaft, the distribution disc is located the latter half of hollow shaft, air suction disc is located the first half of hollow shaft.
A hollow shaft fixing device is arranged in the hydrogenation reaction kettle and is rotatably connected with one end of the hollow shaft. The hollow shaft can be fixed, so that the hollow shaft only rotates without generating other displacements.
The utility model discloses a theory of operation does: the hydrogenation liquid is pressed out by the pressure of the hydrogenation reaction kettle, and after being filtered by the filter, a small amount of hydrogenation liquid is temporarily stored in the liquid storage tank, and then the hydrogenation liquid is sent to the next procedure. After the material pressing is finished, the hydrogenation liquid in the liquid storage tank is pressurized by nitrogen and flows back into the filter, and the catalyst in the filter is blown back into the hydrogenation reaction kettle.
The utility model discloses a first pipeline, the second pipeline, hydrogenation cauldron, filter and liquid storage pot all can set up the sight glass in order to conveniently observe the condition.
The utility model discloses an operating procedure does:
operation one, catalyst feeding:
1. and opening a feeding valve of the hydrogenation kettle, putting a certain amount of hydrogenation catalyst into the hydrogenation reaction kettle, and closing the feeding valve of the hydrogenation kettle. When hydrogenation is carried out, hydrogen is introduced through a hydrogen pipe on the hydrogenation kettle and reacts under stirring. And after the hydrogenation is finished, sampling and discharging qualified materials.
Operation II, discharging and recycling the catalyst:
2-1, opening an upper discharging valve of the hydrogenation kettle, opening a lower feeding valve of the filter, opening an upper inlet and outlet valve of the filter, opening a lower inlet and outlet valve of the liquid storage tank, and finally opening an upper exhaust valve of the liquid storage tank, wherein the hydrogenation liquid enters the liquid storage tank for temporary storage through the filter under the pressure of the kettle, and the catalyst is blocked in the filter by the sintered titanium filter stick.
2-2, after the liquid storage tank is filled with the hydrogenation liquid, closing an upper air outlet valve of the liquid storage tank, closing a lower inlet and outlet valve of the liquid storage tank, closing an upper inlet and outlet valve of the filter, opening an upper outlet valve of the filter, and allowing the hydrogenation liquid to enter the next procedure.
And 2-3, closing a discharge valve on the filter when the material pressing of the hydrogenation liquid in the kettle is finished, and preparing for recycling the catalyst.
And 2-4, opening an upper inlet and outlet valve of the filter, opening a lower inlet and outlet valve of the liquid storage tank, opening a nitrogen valve of the liquid storage tank, slowly reversely flowing the stored hydrogenation liquid into the filter, and returning the catalyst in the filter to the hydrogenation reaction kettle again under the action of the reversely flowing hydrogenation liquid.
And 2-5, when the pressure of the hydrogenation liquid in the liquid storage tank is over, closing a nitrogen valve of the liquid storage tank, closing a lower inlet and outlet valve of the liquid storage tank, closing an upper inlet and outlet valve of the filter, closing a lower feeding valve of the filter, and closing an upper discharging valve of the hydrogenation kettle, so that the catalyst recycling is finished. And (5) continuing feeding the next batch of the hydrogenation reaction kettle.
Operation three, waste catalyst recovery:
when the catalyst is recycled for a certain period of time, it is necessary to take out the catalyst for activation or to recover it as a spent catalyst.
And 3-1, discharging the hydrogenation reaction kettle, opening an upper discharging valve of the hydrogenation kettle, opening a lower feeding valve of the filter, opening an upper discharging valve of the filter, and directly pressing the hydrogenation liquid into the next procedure.
And 3-2, closing the upper discharge valve of the filter, closing the lower feed valve of the filter and then closing the upper discharge valve of the hydrogenation kettle after the material pressing of the hydrogenation liquid in the hydrogenation reaction kettle is finished.
And 3-3, opening a filter drain valve, and putting the catalyst into a prepared iron bucket. And opening a filter washing liquid valve, adding washing liquid into the filter and discharging the catalyst at the same time until the catalyst is completely discharged.
And 3-4, closing the filter drain valve and closing the filter washing liquid valve.
3-5, repeating the operations according to the first operation and the second operation, and continuously recycling the catalyst.
Drawings
FIG. 1 is a schematic structural diagram of a kettle type hydrogenation catalyst recycling device in the embodiment;
wherein the reference numbers: 1. a hydrogenation reaction kettle; 2. a filter; 3. a liquid storage tank; 4. a self-priming stirring device; 5. sintering the titanium filter stick; 6. a hydrogenation kettle feed valve; 7. a discharge valve is arranged on the hydrogenation kettle; 8. a purge valve is arranged at the bottom of the hydrogenation kettle; 9. a filter wash valve; 10. a discharge valve is arranged on the filter; 11. an inlet and outlet valve on the filter; 12. a filter purge valve; 13. a filter lower feed valve; 14. an upper exhaust valve of the liquid storage tank; 15. a nitrogen valve of the liquid storage tank; 16. a lower inlet and outlet valve of the liquid storage tank; 171. a stirring motor; 172. a hollow shaft; 173. a suction plate; 174. a distribution tray; a hollow shaft fixture; 181. a first conduit; 182. a second conduit.
Detailed Description
Example 1
This is further illustrated below in connection with FIG. 1:
the utility model provides a catalyst recycling device of solvent-free hydrogenation production valeronitrile, is including the hydrogenation cauldron 1 that sets gradually, filter 2 and liquid storage pot 3, is connected through first pipeline 181 between hydrogenation cauldron 1 and the filter 2, is connected through second pipeline 182 between filter 2 and the liquid storage pot 3. A hydrogenation kettle feed valve 6 and a hydrogenation kettle lower drain valve 8 are arranged on the hydrogenation reaction kettle 1; the first pipeline 181 is provided with an upper discharging valve 7 of the hydrogenation kettle, a lower feeding valve 13 of the filter and a clean valve 12 of the filter; the filter 2 is provided with a filter washing liquid valve 9 and a filter upper discharge valve 10; the second pipeline 182 is provided with an upper filter inlet and outlet valve 11 and a lower liquid storage tank inlet and outlet valve 16; the liquid storage tank 3 comprises a liquid storage tank upper exhaust valve 14 and a liquid storage tank nitrogen valve 15.
A plurality of sintered titanium filter rods 5 are arranged in the filter 2 (a screw hole pattern plate is arranged in the filter 2, and external thread connecting screw threads are welded at the upper ends of the sintered titanium filter rods 5, namely the sintered titanium filter rods 5 are connected on the screw hole pattern plate in a threaded manner). The sintered titanium filter stick 5 is cylindrical and is formed by sintering tiny titanium metal balls at high temperature. When the material enters the sintered titanium filter stick 5 in the filter 2, the hydrogenated liquid is separated out through the holes formed by the metal balls, and the catalyst is left on the surface of the sintered titanium filter stick 5. When the catalyst is recovered, the inner wall of the sintered titanium filter stick 5 is reversely punched by the hydrogenation liquid, and the catalyst is flushed back into the hydrogenation reaction kettle 1 by utilizing gravity. Because the fixed filter 3 is adopted, the catalyst can be recycled under the closed condition without opening or contacting.
The hydrogenation reaction kettle 1 comprises a self-suction type stirring device 4. Under the high-speed operation of the hollow shaft 172, hydrogen in the hydrogenation reactor 1 enters the hollow shaft 172 through the air suction disc 173 at the upper end of the hollow shaft 172, is thrown out of the distribution disc 174 at the middle lower end of the hollow shaft 172, becomes a large amount of tiny hydrogen bubbles, and is uniformly distributed in liquid, so that the catalyst, the liquid raw material and the hydrogen (solid, liquid and gas) are fully mixed and fully reacted.
The self-priming stirring device 4 comprises a stirring motor 171 and a hollow shaft 172, wherein the hollow shaft 172 is provided with a suction disc 173 and a distribution disc 174, the distribution disc 174 is positioned at the lower half part of the hollow shaft 172, and the suction disc 173 is positioned at the upper half part of the hollow shaft 172.
A hollow shaft fixing device 175 is arranged in the hydrogenation reaction kettle 1, and the hollow shaft fixing device 175 is rotatably connected with one end of the hollow shaft 172. It is possible to fix the hollow shaft 172 so that it only rotates without any other displacement.
The utility model discloses a theory of operation does: the hydrogenation liquid is pressed out by the pressure of the hydrogenation reaction kettle 1, and after being filtered by the filter 2, a small amount of hydrogenation liquid is temporarily stored in the liquid storage tank 3, and then the hydrogenation liquid is sent to the next procedure. After the material pressing is finished, the hydrogenated liquid in the liquid storage tank 3 is pressurized by nitrogen and flows back into the filter 2, and the catalyst in the filter 2 is blown back into the hydrogenation reaction kettle 1.
The utility model discloses a first pipeline 181, second pipeline 182, hydrogenation cauldron 1, filter 2 and liquid storage pot 3 all can set up the sight glass in order to make things convenient for the observation condition.
The utility model discloses an operating procedure does:
operation one, catalyst feeding:
1. and opening a feeding valve 6 of the hydrogenation kettle, putting a certain amount of hydrogenation catalyst into the hydrogenation reaction kettle 1, and closing the feeding valve 6 of the hydrogenation kettle. When hydrogenation is carried out (hydrogen can be added into the hydrogenation reaction kettle through an additional hydrogen pipeline or the existing valve of the hydrogenation reaction kettle is opened for addition), hydrogen is introduced and the reaction is carried out under stirring. And after the hydrogenation is finished, sampling and discharging qualified materials.
Operation II, discharging and recycling the catalyst:
2-1, opening an upper discharging valve 7 of the hydrogenation kettle, opening a lower feeding valve 13 of the filter, opening an upper inlet and outlet valve 11 of the filter, opening a lower inlet and outlet valve 16 of the liquid storage tank, and finally opening an upper exhaust valve 14 of the liquid storage tank, wherein the hydrogenation liquid enters the liquid storage tank 3 for temporary storage through the filter 2 under the pressure of the kettle, and the catalyst is blocked in the filter 2 by the sintered titanium filter stick 5.
2-2, after the liquid storage tank 3 is filled with the hydrogenation liquid, closing an upper air outlet valve 14 of the liquid storage tank, closing a lower inlet and outlet valve 16 of the liquid storage tank, closing an upper inlet and outlet valve 11 of the filter, opening an upper outlet valve 10 of the filter, and allowing the hydrogenation liquid to enter the next process.
And 2-3, closing a discharge valve 10 on the filter 2 when the material pressing of the hydrogenation liquid in the kettle is finished, and preparing for recycling the catalyst.
2-4, opening an upper inlet and outlet valve 11 of the filter, opening a lower inlet and outlet valve 16 of the liquid storage tank, and opening a nitrogen valve 15 of the liquid storage tank, slowly reversely flowing the stored hydrogenation liquid into the filter 2, and returning the catalyst in the filter 2 to the hydrogenation reaction kettle 1 under the action of the reversely flowing hydrogenation liquid.
And 2-5, closing the nitrogen valve 15 of the liquid storage tank when the pressure of the hydrogenated liquid in the liquid storage tank 3 is over, closing the lower inlet/outlet valve 16 of the liquid storage tank, closing the upper inlet/outlet valve 11 of the filter, closing the lower feeding valve 13 of the filter, and closing the upper discharging valve 7 of the hydrogenation kettle, thus finishing the recycling of the catalyst. And the hydrogenation reaction kettle 1 continues to feed the next batch.
Operation three, waste catalyst recovery:
when the catalyst is recycled for a certain period of time, it is necessary to take out the catalyst for activation or to recover it as a spent catalyst.
3-1, discharging from the hydrogenation reactor 1, opening the upper discharging valve 7 of the hydrogenation reactor, opening the lower feeding valve 13 of the filter, opening the upper discharging valve 10 of the filter, and directly pressing the hydrogenation liquid into the next process.
And 3-2, when the material pressing of the hydrogenation liquid in the hydrogenation reaction kettle 1 is finished, closing the upper discharge valve 10 of the filter, closing the lower feed valve 13 of the filter, and then closing the upper discharge valve 7 of the hydrogenation reaction kettle.
3-3, opening a filter drain valve 12 and putting the catalyst into a prepared iron bucket. The filter washing liquid valve 9 is opened, and the catalyst is discharged while the washing liquid is added to the filter 2 until the catalyst is completely discharged.
And 3-4, closing the filter drain valve 12 and closing the filter washing liquid valve 9.
3-5, repeating the operations according to the first operation and the second operation, and continuously recycling the catalyst.
Example 2
The procedure was as in example 1 except that the first line was inclined at an angle of 45 to 60 degrees with respect to the line connecting the valve of the upper outlet of the reactor and the valve at the bottom of the filter, so that the catalyst was withdrawn and returned to the reactor by gravity.
The above-mentioned embodiment is only used for explaining the utility model concept, and not to the limit of the utility model protection, and all utilize this concept to be right the utility model discloses carry out insubstantial change, all shall fall into the scope of protection of the utility model.
Claims (6)
1. A catalyst recycling device for producing valeronitrile by solvent-free hydrogenation is characterized in that: including the hydrogenation cauldron that sets gradually, filter and liquid storage pot, through first pipe connection between hydrogenation cauldron and the filter, through second pipe connection between filter and the liquid storage pot, last hydrogenation cauldron feed valve and the lower clean valve of hydrogenation cauldron of being equipped with of hydrogenation cauldron, be equipped with the last bleeder valve of hydrogenation cauldron on the first pipeline, feed valve and filter drain valve under the filter, the filter is equipped with bleeder valve on the filter, be equipped with the filter on the second pipeline and go into the bleeder valve under business turn over valve and the liquid storage pot, the liquid storage pot includes air relief valve and liquid storage pot nitrogen valve on the liquid storage pot.
2. The apparatus for recycling catalyst in the production of valeronitrile by solvent-free hydrogenation according to claim 1, wherein: the filter is provided with a filter washing liquid valve.
3. The apparatus for recycling catalyst in the production of valeronitrile by solvent-free hydrogenation according to claim 1, wherein: a plurality of sintered titanium filter rods are arranged in the filter.
4. The apparatus for recycling catalyst in the production of valeronitrile by solvent-free hydrogenation according to claim 1, wherein: the hydrogenation reaction kettle comprises a self-suction stirring device.
5. The apparatus for recycling catalyst in the production of valeronitrile by solvent-free hydrogenation according to claim 4, wherein: from inhaling formula agitating unit and including agitator motor and hollow shaft, be equipped with air suction disc and distribution disc on the hollow shaft, the distribution disc is located the latter half of hollow shaft, air suction disc is located the first half of hollow shaft.
6. The apparatus for recycling catalyst in the production of valeronitrile by solvent-free hydrogenation according to claim 5, wherein: a hollow shaft fixing device is arranged in the hydrogenation reaction kettle and is rotatably connected with one end of the hollow shaft.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202020976138.6U CN212549473U (en) | 2020-06-02 | 2020-06-02 | Catalyst recycling device for producing valeronitrile through solvent-free hydrogenation |
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| CN202020976138.6U CN212549473U (en) | 2020-06-02 | 2020-06-02 | Catalyst recycling device for producing valeronitrile through solvent-free hydrogenation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114487000A (en) * | 2021-12-09 | 2022-05-13 | 清华大学 | Transient short hot wire method-based sub-supercritical fluid thermal conductivity testing device |
| CN114917853A (en) * | 2022-05-11 | 2022-08-19 | 顶峰油脂化工(泰兴)有限公司 | Method for intermittent hydrogenation reaction |
-
2020
- 2020-06-02 CN CN202020976138.6U patent/CN212549473U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114487000A (en) * | 2021-12-09 | 2022-05-13 | 清华大学 | Transient short hot wire method-based sub-supercritical fluid thermal conductivity testing device |
| CN114917853A (en) * | 2022-05-11 | 2022-08-19 | 顶峰油脂化工(泰兴)有限公司 | Method for intermittent hydrogenation reaction |
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