CN111282512A - Carbonyl metal complex high-pressure reaction kettle and operation method thereof - Google Patents
Carbonyl metal complex high-pressure reaction kettle and operation method thereof Download PDFInfo
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- CN111282512A CN111282512A CN202010145859.7A CN202010145859A CN111282512A CN 111282512 A CN111282512 A CN 111282512A CN 202010145859 A CN202010145859 A CN 202010145859A CN 111282512 A CN111282512 A CN 111282512A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/18—Stationary reactors having moving elements inside
- B01J19/20—Stationary reactors having moving elements inside in the form of helices, e.g. screw reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0073—Sealings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J4/00—Feed or outlet devices; Feed or outlet control devices
- B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
Abstract
The application discloses carbonyl metal complex high-pressure reaction kettle and an operation method thereof: comprises a reaction kettle body and a driving mechanism; the solid material inlet and the slag material outlet are formed in the shell of the reaction kettle body, so that continuous production is realized, and the production efficiency is improved; by arranging the material propelling and stirring mechanism in the reaction kettle, solid materials are mechanically stirred, so that the synthesis reaction is stably carried out, and the speed of the synthesis reaction is increased; the outer wall of the reaction kettle is provided with a cooling water jacket to prevent the thermal decomposition of the carbonyl metal complex of the reaction product; the double cold-state shaft sealing mechanism is arranged at the end cover of the reaction kettle body, so that the leakage of carbon monoxide is avoided, and the corrosion of metal powder of a carbonyl metal complex decomposition product of a reaction product to a sealing structure is avoided. In conclusion, the method can realize continuous production, prolong the service life of high-pressure reaction kettle equipment, avoid carbon monoxide gas leakage, keep the synthesis reaction in a stable reaction state and reduce the production cost.
Description
Technical Field
The disclosure generally relates to the technical field of reaction kettle devices, and particularly relates to a carbonyl metal complex high-pressure reaction kettle and an operation method thereof.
Background
The carbonyl method for refining metal belongs to a metallurgical method for extracting metal powder in the field of gas phase metallurgy, and the method utilizes carbon monoxide gas and raw materials containing active metal as reactants to generate carbonyl metal complex under certain temperature and pressure. Metal carbonyl complexes are very unstable and can rapidly decompose into metal and carbon monoxide gases at certain temperatures (. gtoreq.100 ℃) and metal powders can be obtained by separation techniques, such as: nickel, iron, tungsten, molybdenum, cobalt, niobium, tantalum, vanadium, rhenium, manganese, thorium, hafnium, ruthenium, and the like. The method adopted by the carbonyl metal synthesis reaction is generally divided into a normal pressure method (P is less than 1.0MPa), a medium pressure method (P is more than or equal to 1.0MPa and less than 7.0MPa) and a high pressure method (P is more than or equal to 7.0MPa) in the industry, the 20 th century and the 30 th era, and the German BASF company adopts the high pressure carbonyl method to refine nickel and iron at first; in the 50 s of the 20 th century, russian northern nickel company refined iron by using a high-pressure carbon monoxide recycling carbonyl process; in the 70 s of the 20 th century, the carbonyl laboratory of the Beijing Steel research institute utilized Cu-Ni alloy raw materials, and the carbon monoxide circulation technology was adopted, so that the synthesis rate of nickel carbonyl was 95%.
At present, the typical structure of the traditional vertical high-pressure reaction kettle is a low-carbon alloy steel integrally forged cylinder body, a stainless steel plate is lined in the cylinder body, and the upper part and the lower part of the cylinder body are provided with flanges and cover plates. The charging opening and the discharging opening are provided with opening and closing mechanisms. Sealing and transmission parts are arranged in the structural design of the charging opening and the discharging opening. The outside of the reaction kettle is provided with a heat-insulating layer. The reaction kettle is provided with 3 thermocouple temperature measuring points for measuring the temperature in the reaction kettle. Before each synthesis reaction, manual feeding is carried out in a high-pressure synthesis kettle. And sealing the flanges and the cover plate of the feed inlet and the discharge outlet, and cutting off the gas inlet and outlet valves. Before the synthesis reaction starts, flushing the high-pressure synthesis kettle with nitrogen to discharge air in the reaction kettle; after the air in the kettle is completely discharged, adding 30MPa of nitrogen into the high-pressure kettle for leakage detection so as to ensure that the sealing performance of the high-pressure reaction kettle reaches the design safety standard; then, the nitrogen gas is discharged, and the remaining nitrogen gas is purged with carbon monoxide gas. After the reaction gas carbon monoxide is cleaned, the pressure in the reaction kettle is gradually increased to more than 10MPa, the temperature of the reaction gas carbon monoxide entering the reaction kettle is gradually increased to about 200 ℃, and the reaction is started. After the synthesis reaction is finished, cutting off a gas inlet and outlet valve, and gradually reducing the temperature of the reaction kettle to the normal temperature by adopting normal-temperature carbon monoxide; introducing nitrogen into the high-pressure synthesis kettle step by step for disinfection, expelling residual carbon monoxide and carbonyl complex gas out of the reaction kettle, and adjusting the pressure to normal pressure. Opening flanges and cover plates of the feed inlet and the discharge outlet, checking the appearances of fasteners such as bolts, nuts, washers and the like, and checking or replacing sealing elements; and finally, manually discharging the reaction residues out of the reaction kettle. The vertical intermittent high-pressure reaction kettle has the problems of long reaction period, high production cost, easy fatigue damage, serious leakage, high operating strength of workers, low synthesis speed, synthesis rate and product yield and the like.
Disclosure of Invention
In view of the above-mentioned defects or shortcomings in the prior art, it is desirable to provide a carbonyl metal complex high-pressure reactor and an operation method thereof, which can realize continuous production, prolong the service life of high-pressure reactor equipment, reduce leakage, maintain stable reaction conditions of synthesis reaction, reduce production cost, have a simple structure and are easy to realize, compared with the prior art.
In a first aspect, the present application provides a metal carbonyl complex autoclave comprising: a driving mechanism and a reaction kettle body;
the drive mechanism includes: a motor and a speed reducer; the rotating shaft of the motor is connected with the input rotating shaft of the speed reducer through a coupling; an output rotating shaft of the speed reducer is connected with a universal shaft;
the reaction kettle body is of a horizontal structure; one end of the reaction kettle body is provided with a kettle body cover plate, and the other end of the reaction kettle body is provided with an end socket; a cover plate is arranged on the outer side of the kettle body cover plate; a kettle body flange is arranged at the opening of the end socket, and a carbon monoxide gas inlet is also arranged on the side wall of the end socket; the top of the shell of the reaction kettle body is sequentially provided with a solid material inlet, a nitrogen outlet and a mixed gas outlet; the solid material inlet and the nitrogen inlet are arranged adjacently and are positioned on one side, close to the end socket, of the top of the shell of the reaction kettle body; the mixed gas outlet is adjacent to the nitrogen outlet and is positioned on one side, close to the cover plate, of the top of the reaction kettle body shell; a slag outlet is formed in the bottom of the shell of the reaction kettle body and is positioned on one side, close to the cover plate, of the bottom of the shell of the reaction kettle body; a sealing mechanism is arranged at the position of the opening on the outer side of the cover plate; the top of the sealing mechanism is provided with a cooling carbon monoxide gas inlet, and the bottom of the sealing mechanism is provided with a carbon monoxide gas outlet; a material propelling and stirring mechanism arranged in parallel with the reaction kettle body is arranged in the reaction kettle body; the outer shaft of the middle shaft of the material propelling and stirring mechanism is connected with the universal shaft through the sealing mechanism; a middle shaft is arranged at the center of the material propelling and stirring mechanism; two ends of the middle shaft are respectively provided with a double-roller supporting component; the double roller support assembly comprises: the support roller and the two support columns; the bottoms of the two support columns are fixed on the inner wall of the reaction kettle body, and the included angle is 30-60 degrees; the supporting rollers are arranged at the tops of the two supporting columns; the middle part of the middle shaft is provided with at least one suspension bearing, and the end part of the suspension bearing is fixed on the inner wall of the reaction kettle body; the reaction kettle body is provided with kettle body supports, and the number of the kettle body supports is at least four.
According to the technical scheme provided by the embodiment of the application, the sealing mechanism comprises: the cooling chamber, the coupling, the first high-pressure seal and the second high-pressure seal; the cooling chamber is positioned in the sealing mechanism; the coupling is arranged in the cooling chamber, and two ends of the coupling are respectively connected with an outer shaft of the material propelling and stirring mechanism and the universal shaft; the first high-pressure seal is arranged at the central opening of the cover plate; and the second high-pressure sealing ring is arranged at an opening of an end cover of the cooling small chamber.
According to the technical scheme provided by the embodiment of the application, the outer wall of the reaction kettle body is also provided with a cooling water mechanism; the cooling water mechanism includes: a cooling water jacket, a cooling water outlet and a cooling water inlet; the cooling water jacket is arranged on the outer wall of the shell of the reaction kettle body; the cooling water outlet is arranged at the top of the cooling water jacket; the cooling water inlet is arranged at the bottom of the cooling water jacket.
According to the technical scheme that this application embodiment provided, the mist exit is provided with the filter, just the filter is located the reation kettle is internal.
According to the technical scheme provided by the embodiment of the application, at least four thermometer openings are formed in the upper side wall of the reaction kettle body.
According to the technical scheme that this application embodiment provided, cauldron body flange detachably with the open connection of head.
According to the technical scheme provided by the embodiment of the application, the driving mechanism is provided with a first base and used for installing the motor and the speed reducer of the driving mechanism.
According to the technical scheme that this application embodiment provided, the reation kettle body be provided with the corresponding base two that sets up of cauldron body support is used for the installation the reation kettle body.
In a second aspect, a method for operating a metal carbonyl complex autoclave, the metal carbonyl complex autoclave according to any one of the above, comprising:
step S1, checking the linkage condition of the motor, the speed reducer, the shaft and the material propelling and stirring mechanism, and checking the rotating speed output condition of the speed reducer;
step S2, keeping the set rotating speed of the reaction kettle, introducing nitrogen from the nitrogen inlet to replace residual air in the kettle, and discharging mixed gas of nitrogen and air from the nitrogen outlet, wherein correspondingly, the air is replaced and discharged by a related system connected with the reaction kettle, and the mixed gas is sent to a tail gas collecting and processing system;
step S5, solid raw materials enter a reaction kettle through the solid material inlet, in step S3, a valve on a pipeline connecting the nitrogen inlet and the nitrogen outlet is closed, carbon monoxide gas is introduced from the carbon monoxide gas inlet, gas is discharged from the mixed gas outlet, the pressure in the reaction kettle is increased to a set reaction pressure, the pressure is maintained, and the discharged mixed gas of the carbon monoxide and the nitrogen is sent to a tail gas collecting and treating system; switching the vent gas to a carbon monoxide and metal carbonyl complex gas system; correspondingly, the associated system connected with the reaction kettle also needs to replace and discharge the nitrogen, and the mixed gas is sent to a tail gas collecting and processing system; introducing carbon monoxide gas with the same pressure from the carbon monoxide gas inlet, discharging the carbon monoxide gas from the mixed gas outlet, and enabling the discharged carbon monoxide gas to enter a carbon monoxide circulating system; introducing normal-temperature carbon monoxide gas with the same pressure into the cooling chamber of the sealing mechanism from the cooling carbon monoxide gas inlet, and introducing the carbon monoxide gas discharged from the carbon monoxide gas outlet into a carbon monoxide circulating system; checking the leakage condition of the carbon monoxide gas at the sealing mechanism, checking the leakage condition of a related system connected with the reaction kettle, and taking the condition that no continuous bubbles occur as a qualification;
step S4, circulating cooling water is introduced from the cooling water inlet, the circulating cooling water is discharged from the cooling water outlet, the circulation of the circulating cooling water is kept during the operation of the reaction kettle, and the flow of the circulating water is adjusted according to the temperature in the reaction kettle;
under the action of the material propelling and stirring mechanism, the reaction kettle runs from one end to the other end of the reaction kettle, the material transfer and heat exchange among gas and solid phases are enhanced by stirring solid materials, and the retention time of the solid materials in the reaction kettle is adjusted at any time according to set time so as to obtain the optimal reaction yield;
step S6, keeping the carbon monoxide gas introduced from the carbon monoxide gas inlet under the set reaction pressure, and adjusting the carbon monoxide pressure through a carbon monoxide compressor and an adjusting valve group; the temperature in the reaction kettle is adjusted through the temperature and the flow of the entering carbon monoxide gas and the flow of the cooling water in the cooling water jacket;
step S7, discharging the reaction solid residue out of the reaction kettle from the slag outlet;
step S8, mixing the carbonyl metal complex gas of the synthetic reaction product into high-pressure carbon monoxide gas, and discharging the gas mixture out of the reaction kettle from the mixed gas outlet through the filter in the kettle;
step S9, when the vehicle is about to stop or needs to stop in case of an accident, the rotation of mechanical equipment needs to be maintained, the circulation of circulating cooling water needs to be maintained, and the carbon monoxide gas entering the kettle is switched to normal temperature; stopping the feeding of the solid raw materials; taking out the residual heat in the reaction kettle through carbon monoxide gas until the temperature in the reaction kettle is reduced to normal temperature; the discharged mixed gas of the carbonyl metal complex and the carbon monoxide is sent into a tail gas collecting and treating system; replacing residual carbon monoxide gas in the reaction kettle by using nitrogen;
step S10, carrying out remote control on the output rotating speed of the motor and the speed reducer; the temperature in the reaction kettle is displayed on site and in a central control room through a plurality of thermometer ports, and the temperature and the flow of the carbon monoxide entering the reaction kettle and the flow of cooling water are controlled according to the temperature and the flow of the carbon monoxide;
steps S1-S10 are executed in a loop.
To sum up, the beneficial effect of this application:
the solid material inlet and the slag material outlet are arranged on the shell of the reaction kettle body, so that continuous production is realized, the effective reaction time of high-pressure synthesis of the carbonyl metal complex is greatly prolonged, the production auxiliary time is eliminated or reduced, and the production efficiency is improved; the solid material is mechanically stirred by arranging the material propelling and stirring mechanism in the reaction kettle body, so that the full contact between the surface of the solid material and carbon monoxide gas is facilitated, the diffusion of carbonyl metal complex molecules generated on the surface of the solid material is facilitated, the mass transfer and the heat transfer of the material and the whole reaction system are facilitated, the speed of the synthesis reaction is accelerated, and the whole synthesis reaction is stably carried out; the outer wall of the reaction kettle body is provided with a cooling water jacket to prevent the thermal decomposition of the carbonyl metal complex of the reaction product; by arranging the sealing mechanism on the outer side of the cover plate, the leakage of carbon monoxide is avoided by adopting double cold state sealing, and particularly, the corrosion of the metal powder of the carbonyl metal complex decomposition material of the reaction product to the sealing is avoided; therefore, the continuous production can be realized, the service life of the high-pressure reaction kettle equipment is prolonged, the leakage amount is reduced, the stable reaction condition of the synthetic reaction is kept, and the production cost is reduced.
Drawings
Other features, objects and advantages of the present application will become more apparent upon reading of the following detailed description of non-limiting embodiments thereof, made with reference to the accompanying drawings in which:
FIG. 1 is a schematic structural diagram of a carbonyl metal complex autoclave.
Fig. 2 is a schematic structural view of the sealing mechanism.
Fig. 3 is a schematic structural view of the support roller.
Reference numbers in the figures: 1. a first base; 2. a second base; 3. a motor; 4. a speed reducer; 5. a cardan shaft; 6. a sealing mechanism; 7. a cover plate; 8. a cover plate of the kettle body; 9. a reaction kettle body; 10. a cooling water jacket; 11. a material propelling and stirring mechanism; 12. sealing the end; 13. a kettle body flange; 14. a filter; 15. a kettle body support; 16. a carbon monoxide gas inlet; 17. a solid material inlet; 18. a nitrogen inlet; 19. a thermometer port; 20. a cooling water outlet; 21. a nitrogen outlet; 22. a mixed gas outlet; 23. cooling a carbon monoxide gas inlet; 24. a cooling water inlet; 25. a slag outlet; 26. a carbon monoxide gas outlet; 27. supporting the rollers; 28. a suspension bearing; 29. a middle shaft; 30. cooling the chamber; 31. a coupling; 32. first high-pressure sealing; 33. and the second high-pressure seal.
Detailed Description
The present application will be described in further detail with reference to the following drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention. It should be noted that, for convenience of description, only the portions related to the present invention are shown in the drawings.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
Example one
2000 ton/year carbonyl iron powder high-pressure reaction kettle
Please refer to fig. 1, which is a schematic structural diagram of a first embodiment of a metal carbonyl complex autoclave provided by the present application, comprising: a driving mechanism and a reaction kettle body 9;
the drive mechanism includes: a motor 3 and a speed reducer 4; the rotating shaft of the motor 3 is connected with the input rotating shaft of the speed reducer 4 through a coupling 31; an output rotating shaft of the speed reducer 4 is connected with a universal shaft 5;
the reaction kettle body 9 is of a horizontal structure; one end of the reaction kettle body 9 is provided with a kettle body cover plate 8, and the other end of the reaction kettle body is provided with an end enclosure 12; a cover plate 7 is arranged on the outer side of the kettle cover plate 8; a kettle flange 13 is arranged at an opening of the end enclosure 12, and a carbon monoxide gas inlet 16 is also arranged on the side wall of the end enclosure 12; the top of the shell of the reaction kettle body 9 is sequentially provided with a solid material inlet 17, a nitrogen inlet 18, a nitrogen outlet 21 and a mixed gas outlet 22; the solid material inlet 17 and the nitrogen inlet 18 are arranged adjacently and are positioned on one side, close to the end socket 12, of the top of the shell of the reaction kettle body 9; the mixed gas outlet 22 is arranged adjacent to the nitrogen outlet 21 and is positioned on one side, close to the cover plate 7, of the top of the shell of the reaction kettle body 9; a slag outlet 25 is formed in the bottom of the shell of the reaction kettle body 9 and is positioned on one side, close to the cover plate 7, of the bottom of the shell of the reaction kettle body 9; a sealing mechanism 6 is arranged at an opening on the outer side of the cover plate 7; the top of the sealing mechanism 6 is provided with a cooling carbon monoxide gas inlet 23, and the bottom of the sealing mechanism is provided with a carbon monoxide gas outlet 26; a material propelling and stirring mechanism 11 which is arranged in parallel with the reaction kettle body 9 is arranged in the reaction kettle body 9; the outer shaft of the middle shaft 29 of the material propelling and stirring mechanism 11 is connected with the universal shaft 5 through the sealing mechanism 6; a middle shaft 29 is arranged at the center of the material propelling and stirring mechanism 11; two ends of the middle shaft 29 are respectively provided with a double-roller supporting component; the double roller support assembly comprises: a support roller 27 and two support columns; one end of each of the two support columns is fixed on the inner wall of the kettle body, and the included angle is 30-60 degrees; the supporting rollers 27 are arranged at the tops of the two supporting columns; a suspension bearing 28 is arranged in the middle of the middle shaft 29, and the root of the suspension bearing 28 is fixed on the inner wall of the reaction kettle body 9; the reaction kettle body 9 is provided with kettle body supports 15, and the number of the kettle body supports is at least four.
In this embodiment, the reaction kettle body 9 is a horizontal structure, the kettle internals are 304 stainless steel, and the shell is a 16MnR inner lining 304 stainless steel thin plate; the motor 3 provides power for the reaction kettle, is an NHM3-350 type hydraulic motor, and has the power range of 10-60 kw; the first stage of the speed reducer 4 is an XWD type two-stage cycloidal pin speed reducer, the speed ratio is 143, and the frame number is x 85; the second stage of the speed reducer 4 is a ZL-85-10- | type flat shaft gear speed reducer, wherein a is 850, i is 20, and the flat shaft gear speed reducer is arranged; the universal shaft 5 is used for conducting the speed of the speed reducer 4 and the reaction kettle body 9;
the kettle cover plate 8, the cover plate 7, the seal head 12, the flange 13 and the shell form a pressure-bearing shell of the reaction kettle body 9; the cover plate 8 and the cover plate 7 of the kettle body are connected through bolts, and the cover plate 7 or the flange 13 can be opened when the interior of the kettle body is overhauled; a carbon monoxide gas inlet 16 arranged on the side wall of the end enclosure 12 and used for introducing carbon monoxide gas; the solid material inlet 17 is arranged at one side of the top of the shell of the reaction kettle body 9, which is close to the end socket 12, is adjacent to the nitrogen inlet 18, and is used for feeding solid materials into the reaction kettle body 9; a nitrogen inlet 18 and a nitrogen outlet 21 are arranged at the top of the shell of the reaction kettle body 9, nitrogen is introduced into the reaction kettle before starting to replace air in the reaction kettle, and nitrogen is introduced into the reaction kettle before stopping to replace carbon monoxide in the reaction kettle; a mixed gas outlet 22, which is arranged at one side of the top of the shell of the reaction kettle body 9 close to the cover plate 7, is adjacent to the nitrogen gas outlet 21, and is used for discharging the mixed gas of the reaction product metal carbonyl complex gas and the circulating carbon monoxide gas; the slag outlet 25 is arranged at one side of the bottom of the shell of the reaction kettle body 9, which is close to the cover plate 7, and is used for discharging slag after reaction in the reaction kettle body 9; the sealing mechanism 6 is arranged at an opening on the outer side of the cover plate 7, the universal shaft 5 is connected with the outer shaft of the middle shaft 29 of the material propelling and stirring mechanism 11 in a cooling chamber of the sealing mechanism 6, and the sealing mechanism 6 provides sealing for a rotating shaft of the reaction kettle; normal-temperature high-pressure carbon monoxide enters the cooling chamber from the cooling carbon monoxide gas inlet 23 and is discharged from the cooling chamber from the carbon monoxide gas outlet 26, so that the carbonyl metal complex gas in the reaction kettle can be prevented from leaking to the cooling chamber along the sealing surface, and meanwhile, the sealing effect can be improved by cooling the sealing surface; the material propelling and stirring mechanism 11 is arranged inside the reaction kettle body 9 and used for propelling and mechanically stirring solid materials, so that the solid materials are in full contact with carbon monoxide gas, carbonyl metal complex molecules generated on the surface of the solid materials are diffused, the heat transfer between the materials and the whole reaction system is facilitated, the solid materials are mechanically stirred, the speed of the synthesis reaction can be increased, and the whole synthesis reaction can be stably carried out; a central shaft 29, which is a central shaft of a rotating blade of the material propelling and stirring mechanism 11, and drives the material propelling and stirring mechanism 11 to rotate; the supporting rollers 27 are arranged at two ends of the middle shaft 29 and are used for supporting the rotation of the material propelling and stirring mechanism 11; the suspension bearings 28 are arranged in the middle of the middle shaft 29, and the number of the suspension bearings is one, so that the suspension bearings can overcome the deflection of the middle shaft 29; and at least four kettle body supports 15 for supporting the weight of the kettle body and guiding the thermal displacement of the kettle body in a working state to the free end of the kettle body.
In any preferred embodiment, the sealing mechanism 6 comprises: cooling chamber 30, coupling 31, first high pressure seal 32 and second high pressure seal 33; the cooling chamber 30 is located within the sealing mechanism 6; the coupling 31 is arranged in the cooling chamber 30, and both ends of the coupling are respectively connected with the outer shaft of the material propelling and stirring mechanism 11 and the universal shaft 5; the first high-pressure seal 32 is arranged at the central opening of the cover plate 7; the second high-pressure seal 33 is disposed around the opening of the end cap of the cooling chamber 30.
In this embodiment, the cooling chamber 30 is located inside the sealing mechanism 6, where the cold carbon monoxide gas cools the sealing mechanism; a coupling 31 disposed in the cooling chamber 30 and having both ends connected to the outer shaft of the material propelling and stirring mechanism 11 and the universal shaft 5, respectively; the first high-pressure seal 32 is arranged at the central opening of the cover plate 7 and adopts high-pressure static seal; and a second high-pressure seal 33 is arranged at the opening of the end cover of the cooling small chamber 30, and adopts a combined high-pressure dynamic seal.
In any preferred embodiment, a cooling water mechanism is further arranged on the outer wall of the reaction kettle body 9; the cooling water mechanism includes: a cooling water jacket 10, a cooling water outlet 20 and a cooling water inlet 24; the cooling water jacket 10 is arranged on the outer wall of the shell of the reaction kettle body 9; the cooling water outlet 20 is arranged at the top of the cooling water jacket 10; the cooling water inlet 24 is arranged at the bottom of the cooling water jacket 10.
In this embodiment, the cooling water jacket 10 is disposed on the outer wall of the reaction kettle body 9 to provide a cooling effect for the reaction kettle, and the circulation of the circulating cooling water is maintained during the operation of the reaction kettle to avoid the over-high temperature in the reaction kettle; a cooling water inlet 24 arranged at the bottom of the cooling water jacket 10 and used for introducing circulating cooling water; and a cooling water outlet 20 disposed at the top of the cooling water jacket 10 for discharging the circulating cooling water.
In any preferred embodiment, a filter 14 is disposed at the mixed gas outlet 22, and the filter 14 is located in the reaction kettle body 9.
In the present embodiment, the filter 14, which is provided at the mixed gas outlet 22 and is located in the reaction vessel body 9, is used for filtering dust in the mixture of carbon monoxide gas and metal carbonyl complex gas in the reaction vessel, and the particle size of the filtered dust is 150 μm or less, and the filter 19 is of a type such as SRT | -type reverse-baffled T-type filter, and the filtering accuracy is 100 mesh.
In any preferred embodiment, the upper side wall of the reaction kettle body 9 is provided with at least four temperature measuring ports 19.
In this embodiment, the thermometer port 19 is disposed on the sidewall of the reaction vessel body 9 for displaying the temperature of the reaction vessel in situ and in the central control room, and the temperature of the reaction vessel can be used as a basis for controlling the temperature and flow rate of carbon monoxide entering the reaction vessel and the flow rate of cooling water in the water jacket.
In any preferred embodiment, the kettle flange 13 is detachably connected with the opening of the end enclosure 12.
In this embodiment, the connection manner of the tank flange 13 and the opening of the end enclosure 12 is not limited herein, and optionally, the high-pressure bolt connection is specifically: the kettle body flange 13 is connected to the opening of the end enclosure 12 through a high-pressure bolt.
In any preferred embodiment, the driving mechanism is provided with a first base 1, a motor 3 and a speed reducer 4 for mounting the driving mechanism.
In the embodiment, a first base 1 is arranged below the driving mechanism and used for installing a motor 3 and a speed reducer 4.
In any preferred embodiment, the reaction kettle body 9 is provided with a second base 2 arranged corresponding to the kettle body support 15 and used for mounting the reaction kettle body 9.
In this embodiment, the second base 2 is disposed on the reaction kettle body 9, and is disposed corresponding to the kettle body support 15, and is used for installing the reaction kettle body 9.
Example two
A method for operating a metal carbonyl complex autoclave, the metal carbonyl complex autoclave based on any one of the above, comprising:
step S1, checking the linkage condition of the motor 3, the speed reducer 4, the shaft 5 and the material propelling and stirring mechanism 1, and checking the rotation speed output condition of the speed reducer 4;
step S2, keeping the set rotation speed of the reaction kettle, introducing nitrogen from the nitrogen inlet 18 to replace residual air in the kettle, and discharging mixed gas of nitrogen and air from the nitrogen outlet 21, wherein correspondingly, the air is replaced and discharged by a related system connected with the reaction kettle, and the mixed gas is sent to a tail gas collecting and processing system;
step S3, closing a valve on a pipeline connecting the nitrogen inlet 18 and the nitrogen outlet 21, introducing carbon monoxide gas from the carbon monoxide gas inlet 16, discharging gas from the mixed gas outlet 22, raising the pressure in the reaction kettle to a set reaction pressure, maintaining the pressure, and sending the discharged carbon monoxide and nitrogen mixed gas into a tail gas collecting and treating system; switching the vent gas to a carbon monoxide and metal carbonyl complex gas system; correspondingly, the associated system connected with the reaction kettle also needs to replace and discharge the nitrogen, and the mixed gas is sent to a tail gas collecting and processing system; introducing carbon monoxide gas with the same pressure from the carbon monoxide gas inlet 16, discharging the carbon monoxide gas from the mixed gas outlet 22, and introducing the discharged carbon monoxide gas into a carbon monoxide circulating system; introducing normal-temperature carbon monoxide gas with the same pressure into the cooling chamber 30 of the sealing mechanism 6 from the cooling carbon monoxide gas inlet 23, and introducing the carbon monoxide gas discharged from the carbon monoxide gas outlet 26 into a carbon monoxide circulation system; checking the leakage condition of the carbon monoxide gas at the sealing mechanism 6, checking the leakage condition of a related system connected with the reaction kettle, and taking the condition that no continuous bubbles are generated as qualified;
step S4, circulating cooling water is introduced from the cooling water inlet 24, the circulating cooling water is discharged from the cooling water outlet 20, the circulation of the circulating cooling water is kept during the operation of the reaction kettle, and the flow rate of the circulating water is adjusted according to the temperature in the reaction kettle;
step S5, solid raw materials enter the reaction kettle through the solid material inlet 17, the solid raw materials run from one end to the other end of the reaction kettle under the action of the material propelling and stirring mechanism 11, the material transfer and heat exchange among gas-solid phases are enhanced by stirring the solid materials, and the retention time of the solid materials in the reaction kettle is adjusted at any time according to the set time so as to obtain the optimal reaction yield;
step S6, keeping the carbon monoxide gas introduced from the carbon monoxide gas inlet 16 under the set reaction pressure, and adjusting the carbon monoxide pressure through a carbon monoxide compressor and an adjusting valve group; the temperature in the reaction kettle is adjusted through the temperature and the flow of the entering carbon monoxide gas and the flow of the cooling water in the cooling water jacket;
step S7, discharging the reaction solid residue out of the reaction kettle from the slag outlet 25;
step S8, mixing the carbonyl metal complex gas of the synthetic reaction product into high-pressure carbon monoxide gas, and discharging the gas mixture out of the reaction kettle from the mixed gas outlet 22 through the filter 14 in the kettle;
step S9, when the vehicle is about to stop or needs to stop in case of an accident, the rotation of mechanical equipment needs to be maintained, the circulation of circulating cooling water needs to be maintained, and the carbon monoxide gas entering the kettle is switched to normal temperature; stopping the feeding of the solid raw materials; taking out the residual heat in the reaction kettle through carbon monoxide gas until the temperature in the reaction kettle is reduced to normal temperature; the discharged mixed gas of the carbonyl metal complex and the carbon monoxide is sent into a tail gas collecting and treating system; replacing residual carbon monoxide gas in the reaction kettle by using nitrogen;
step S10, performing remote control on the output rotation speeds of the motor 3 and the speed reducer 4; the temperature in the reaction kettle is displayed on site and in a central control room through a plurality of thermometer ports 19, and the temperature and the flow of the carbon monoxide entering the reaction kettle and the flow of cooling water are controlled according to the temperature and the flow of the carbon monoxide;
steps S1-S10 are executed in a loop.
Wherein, can realize carrying out remote control to the output rotational speed of motor 3 and speed reducer 4 through DCS.
Taking 2000t/a carbonyl iron powder as an example, sponge iron is used as raw material solid, and is shown in table 1:
TABLE 1 technical indices of sponge iron
Bulk density of sponge iron: 2.0-2.2g/cm3(ii) a Average particle size of sponge iron: 15-20 mm; the annual consumption of sponge iron: 3000 t;
technical indexes of carbon monoxide gas:
the carbon monoxide is prepared by a coke pure oxygen method, and then the carbon monoxide is subjected to washing, desulfurization, dust removal, pressure swing adsorption and compression to prepare high-purity carbon monoxide raw material gas, as shown in table 2:
TABLE 2 CO gas specifications
Annual carbon monoxide consumption of 5000 tons (4X 10 in total)6Nm3/a)；
TABLE 3 technical parameters of the synthesis kettle
TABLE 4 operating parameters of the reaction vessel
Synthesis rate of the reaction kettle: more than or equal to 95 percent.
The above description is only a preferred embodiment of the application and is illustrative of the principles of the technology employed. It will be appreciated by a person skilled in the art that the scope of the invention as referred to in the present application is not limited to the embodiments with a specific combination of the above-mentioned features, but also covers other embodiments with any combination of the above-mentioned features or their equivalents without departing from the inventive concept. For example, the above features may be replaced with (but not limited to) features having similar functions disclosed in the present application.
Claims (9)
1. A carbonyl metal complex autoclave, comprising: a driving mechanism and a reaction kettle body (9);
the drive mechanism includes: a motor (3) and a speed reducer (4); the rotating shaft of the motor (3) is connected with the input rotating shaft of the speed reducer (4) through a coupling (31); an output rotating shaft of the speed reducer (4) is connected with the universal shaft (5);
the reaction kettle body (9) is of a horizontal structure; one end of the reaction kettle body (9) is provided with a kettle body cover plate (8), and the other end of the reaction kettle body is provided with an end enclosure (12); a cover plate (7) is arranged on the outer side of the kettle cover plate (8); a kettle flange (13) is arranged at an opening of the end socket (12), and a carbon monoxide gas inlet (16) is also arranged on the side wall of the end socket (12); the top of the shell of the reaction kettle body (9) is sequentially provided with a solid material inlet (17), a nitrogen inlet (18), a nitrogen outlet (21) and a mixed gas outlet (22); the solid material inlet (17) and the nitrogen inlet (18) are arranged adjacently and are positioned on one side, close to the end socket (12), of the top of the shell of the reaction kettle body (9); the mixed gas outlet (22) is arranged adjacent to the nitrogen outlet (21) and is positioned on one side, close to the cover plate (7), of the top of the shell of the reaction kettle body (9); a slag outlet (25) is formed in the bottom of the shell of the reaction kettle body (9) and is positioned on one side, close to the cover plate (7), of the bottom of the shell of the reaction kettle body (9); a sealing mechanism (6) is arranged at an opening on the outer side of the cover plate (7); the top of the sealing mechanism (6) is provided with a cooling carbon monoxide gas inlet (23), and the bottom of the sealing mechanism is provided with a carbon monoxide gas outlet (26); a material propelling and stirring mechanism (11) which is arranged in parallel with the reaction kettle body (9) is arranged in the reaction kettle body (9); a middle shaft (29) is arranged at the center of the material propelling and stirring mechanism (11); the outer shaft of the middle shaft (29) is connected with the universal shaft (5) through the sealing mechanism (6); two ends of the middle shaft (29) are respectively provided with a double-roller supporting component; the double roller support assembly comprises: a support roller (27) and two support columns; the bottoms of the two support columns are fixed on the inner wall of the reaction kettle body (9), and the included angle is 30-60 degrees; the supporting rollers (27) are arranged at the tops of the two supporting columns; the middle part of the middle shaft (29) is provided with at least one suspension bearing (28), and the end part of the suspension bearing (28) is fixed on the inner wall of the reaction kettle body (9); the reaction kettle body (9) is provided with kettle body supports (15), and the number of the kettle body supports is at least four.
2. A metal carbonyl complex autoclave as claimed in claim 1, wherein, said sealing mechanism (6) comprises: a cooling chamber (30), a coupling (31), a first high pressure seal (32) and a second high pressure seal (33); the cooling chamber (30) is located inside the sealing mechanism (6); the coupling (31) is arranged in the cooling chamber (30), and two ends of the coupling are respectively connected with an outer shaft of the material propelling and stirring mechanism (11) and the universal shaft (5); the first high-pressure seal (32) is arranged at the central opening of the cover plate (7); the second high-pressure seal (33) is annularly arranged at an opening of an end cover of the cooling small chamber (30).
3. A carbonyl metal complex autoclave as claimed in claim 1, characterized in that, the outer wall of the autoclave body (9) is provided with a cooling water mechanism; the cooling water mechanism includes: a cooling water jacket (10), a cooling water outlet (20) and a cooling water inlet (24); the cooling water jacket (10) is arranged on the outer wall of the shell of the reaction kettle body (9); the cooling water outlet (20) is arranged at the top of the cooling water jacket (10); the cooling water inlet (24) is arranged at the bottom of the cooling water jacket (10).
4. A metal carbonyl complex autoclave reaction kettle according to claim 1, characterized in that, the mixed gas outlet (22) is provided with a filter (14), and the filter (14) is located in the autoclave body (9).
5. A metal carbonyl complex autoclave as claimed in claim 1, characterized in that, the upper side wall of said autoclave body (9) is equipped with at least four temperature ports (19).
6. A metal carbonyl complex autoclave reactor according to claim 1, characterized in that, the vessel flange (13) is detachably connected with the opening of the end closure (12).
7. A metal carbonyl complex autoclave as claimed in claim 1, wherein, said driving mechanism is provided with a base (1), a motor (3) and a reducer (4) for mounting said driving mechanism.
8. A metal carbonyl complex autoclave as claimed in claim 1, characterized in that, said autoclave body (9) is provided with a second base (2) corresponding to said autoclave body support (15) for installing said autoclave body (9).
9. A method for operating a metal carbonyl complex autoclave, which is based on the metal carbonyl complex autoclave of any one of claims 1-8, comprising:
step S1, checking the linkage condition of the motor (3), the speed reducer (4), the shaft (5) and the material propelling and stirring mechanism (11), and checking the rotating speed output condition of the speed reducer (4);
step S2, keeping the set rotating speed of the reaction kettle, introducing nitrogen from the nitrogen inlet (18) to replace residual air in the kettle, and discharging mixed gas of nitrogen and air from the nitrogen outlet (21), wherein correspondingly, the air is replaced and discharged by a related system connected with the reaction kettle, and the mixed gas is sent to a tail gas collecting and processing system;
step S3, closing a valve on a pipeline connecting the nitrogen inlet (18) and the nitrogen outlet (21), introducing carbon monoxide gas from the carbon monoxide gas inlet (16), discharging gas from the mixed gas outlet (22), increasing the pressure in the reaction kettle to a set reaction pressure, maintaining the pressure, and feeding the discharged carbon monoxide and nitrogen mixed gas into a tail gas collecting and treating system; switching the vent gas to a carbon monoxide and metal carbonyl complex gas system; correspondingly, the associated system connected with the reaction kettle also needs to replace and discharge the nitrogen, and the mixed gas is sent to a tail gas collecting and processing system; introducing carbon monoxide gas with the same pressure from the carbon monoxide gas inlet (16), discharging the carbon monoxide gas from the mixed gas outlet (22), and introducing the discharged carbon monoxide gas into a carbon monoxide circulating system; introducing normal-temperature carbon monoxide gas with the same pressure into a cooling chamber (30) of the sealing mechanism (6) from the cooling carbon monoxide gas inlet (23), and introducing the carbon monoxide gas discharged from the carbon monoxide gas outlet (26) into a carbon monoxide circulating system; checking the leakage condition of the carbon monoxide gas at the sealing mechanism (6), checking the leakage condition of a related system connected with the reaction kettle, and taking the condition that no continuous bubbles are generated as qualified;
step S4, circulating cooling water is introduced from the cooling water inlet (24), the circulating cooling water is discharged from the cooling water outlet (20), the circulation of the circulating cooling water is kept during the operation of the reaction kettle, and the flow rate of the circulating water is adjusted according to the temperature in the reaction kettle;
step S5, solid raw materials enter a reaction kettle through the solid material inlet (17), the solid raw materials run from one end to the other end of the reaction kettle under the action of the material propelling and stirring mechanism (11), substance transfer and heat exchange among gas-solid phases are enhanced by stirring the solid materials, and the retention time of the solid materials in the reaction kettle is adjusted at any time according to set time so as to obtain the optimal reaction yield;
step S6, introducing carbon monoxide gas from the carbon monoxide gas inlet (16) under a set reaction pressure, and adjusting the pressure of the carbon monoxide gas through a carbon monoxide compressor and an adjusting valve group; the temperature in the reaction kettle is adjusted through the temperature and the flow of the entering carbon monoxide gas and the flow of the cooling water in the cooling water jacket (10);
step S7, discharging the reaction solid residue out of the reaction kettle from the slag outlet (25);
step S8, mixing the carbonyl metal complex gas of the synthetic reaction product into high-pressure carbon monoxide gas, and discharging the gas mixture out of the reaction kettle from the mixed gas outlet (22) through the filter (14) in the kettle;
step S9, when the vehicle is about to stop or needs to stop in case of an accident, the rotation of mechanical equipment needs to be maintained, the circulation of circulating cooling water needs to be maintained, and the carbon monoxide gas entering the kettle is switched to normal temperature; stopping the feeding of the solid raw materials; taking out the residual heat in the reaction kettle through carbon monoxide gas until the temperature in the reaction kettle is reduced to normal temperature; the discharged mixed gas of the carbonyl metal complex and the carbon monoxide is sent into a tail gas collecting and treating system; replacing residual carbon monoxide gas in the reaction kettle by using nitrogen;
step S10, carrying out remote control on the output rotating speeds of the motor (3) and the speed reducer (4); the temperature in the reaction kettle is displayed on site and in a central control room through a plurality of thermometer ports (19), and the temperature and the flow of the carbon monoxide entering the reaction kettle and the flow of cooling water are controlled according to the temperature and the flow of the carbon monoxide;
steps S1-S10 are executed in a loop.
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Application publication date: 20200616 |