CN115228387B - Continuous preparation system and method for 2-methyltetrahydrofuran - Google Patents
Continuous preparation system and method for 2-methyltetrahydrofuran Download PDFInfo
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- CN115228387B CN115228387B CN202210665600.4A CN202210665600A CN115228387B CN 115228387 B CN115228387 B CN 115228387B CN 202210665600 A CN202210665600 A CN 202210665600A CN 115228387 B CN115228387 B CN 115228387B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- JWUJQDFVADABEY-UHFFFAOYSA-N 2-methyltetrahydrofuran Chemical compound CC1CCCO1 JWUJQDFVADABEY-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 239000001257 hydrogen Substances 0.000 claims abstract description 27
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 27
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 239000007789 gas Substances 0.000 claims abstract description 19
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 238000003860 storage Methods 0.000 claims abstract description 14
- 238000001914 filtration Methods 0.000 claims abstract description 4
- VQKFNUFAXTZWDK-UHFFFAOYSA-N 2-Methylfuran Chemical compound CC1=CC=CO1 VQKFNUFAXTZWDK-UHFFFAOYSA-N 0.000 claims description 34
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- 239000003638 chemical reducing agent Substances 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 150000002431 hydrogen Chemical class 0.000 claims description 5
- 210000001503 joint Anatomy 0.000 claims description 5
- 229910000564 Raney nickel Inorganic materials 0.000 claims description 3
- NPXOKRUENSOPAO-UHFFFAOYSA-N Raney nickel Chemical compound [Al].[Ni] NPXOKRUENSOPAO-UHFFFAOYSA-N 0.000 claims description 3
- 230000005540 biological transmission Effects 0.000 claims description 3
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000013589 supplement Substances 0.000 claims description 3
- 238000010924 continuous production Methods 0.000 claims 2
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 5
- 235000017491 Bambusa tulda Nutrition 0.000 description 5
- 241001330002 Bambuseae Species 0.000 description 5
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 5
- 239000011425 bamboo Substances 0.000 description 5
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 238000004891 communication Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000005485 electric heating Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002816 fuel additive Substances 0.000 description 1
- 208000014617 hemorrhoid Diseases 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010653 organometallic reaction Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0292—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds with stationary packing material in the bed, e.g. bricks, wire rings, baffles
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/008—Details of the reactor or of the particulate material; Processes to increase or to retard the rate of reaction
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0278—Feeding reactive fluids
-
- 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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0285—Heating or cooling the reactor
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
Abstract
The invention discloses a continuous preparation system and a continuous preparation method of 2-methyltetrahydrofuran, wherein the continuous preparation system comprises a bracket, a metering tank is fixedly arranged at the upper end of the bracket near the edge of a side edge, a reaction kettle is fixedly arranged at the upper end of the bracket near the edge of the other side, a pocket bottom plate is arranged in the reaction kettle, a circulating pump is fixedly arranged on the side surface of the reaction kettle, a gas-liquid separator is arranged at the bottom end of the inner side of the bracket near the middle part, and a gas storage bottle is fixedly connected to the surface of the gas-liquid separator. According to the continuous preparation system and the method of the 2-methyltetrahydrofuran, through the structure of the system device, the catalyst can be isolated and placed, the subsequent filtering process is reduced, air contact can be prevented by debugging in the disassembly and assembly process, the solvent can be pumped from bottom to top by the aid of the circulating pump assembly, the solvent is fully mixed, the solvent can be heated and filtered in the process, and redundant hydrogen can be recycled by the aid of the gas-liquid separator.
Description
Technical Field
The invention relates to the technical field of chemical synthesis device structures, in particular to a continuous preparation system and a continuous preparation method of 2-methyltetrahydrofuran.
Background
2-methyl tetrahydrofuran (2-MeTHF) is an important organic intermediate and an excellent solvent, the solubility in water is small due to the moderate boiling point (80.2 ℃), the water separation is easy, the 2-methyl tetrahydrofuran has Lewis basicity similar to Tetrahydrofuran (THF), and can be applied to a plurality of organometallic reactions, and is widely applied to industrial production at present as a novel solvent, and the 2-MeTHF can be mutually dissolved with gasoline in any proportion, has excellent oxidation and vapor pressure and other properties, and can be used as an automobile fuel additive to replace part of gasoline, and research shows that the 2-MeTHF can not cause any influence on the performance of an engine when the proportion of the 2-MeTHF in the gasoline exceeds 60%, the oil consumption of an automobile is not increased, in addition, the 2-methyl tetrahydrofuran is also a raw material of the pharmaceutical industry, can be used for synthesizing anti-hemorrhoid medicine primary ammonia phosphate, and the like, and the 2-methyl tetrahydrofuran can be prepared by a plurality of methods, and different raw materials and different catalysts can be used; the existing continuous preparation system and method for 2-methyltetrahydrofuran have certain defects when in use, the existing structure is mainly subjected to dispersion treatment when the catalyst is stored, the existing structure is easy to contact with air, the existing structure is very troublesome when being cleaned, meanwhile, the traditional stirring mode of a stirring paddle cannot meet the use requirement, the solvents on the upper layer and the lower layer cannot be quickly mixed, in addition, in the preparation process, the waste of hydrogen is easily caused, and meanwhile, the discharged hydrogen is also easy to pollute.
Disclosure of Invention
The invention mainly aims to provide a continuous preparation system and a continuous preparation method for 2-methyltetrahydrofuran, which can effectively solve the problems in the background technology.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the continuous preparation system of 2-methyltetrahydrofuran and the method thereof comprise a bracket, wherein a metering tank is fixedly arranged at the position, close to the edge of a side edge, of the upper end of the bracket, a reaction kettle is fixedly arranged at the position, close to the edge of the other side, of the upper end of the bracket, a pocket bottom plate is arranged in the reaction kettle, a circulating pump is fixedly arranged on the side surface of the reaction kettle, a gas-liquid separator is arranged at the position, close to the middle, of the bottom end of the inner side of the bracket, and a gas storage bottle is fixedly connected to the surface of the gas-liquid separator;
the upper end surface of the pocket bottom plate is positioned at the edge and fixedly provided with a baffle plate, the inner side of the baffle plate is fixedly provided with a baffle net, the upper end of the baffle net is provided with a connecting cover, the bottom end surface of the connecting cover is positioned at the edge and fixedly provided with a shielding cover, the upper end surface of the connecting cover is positioned at the middle and is provided with a caulking groove, the surface of the caulking groove is embedded and connected with a panel, and the upper end surface of the panel is positioned at the middle and fixedly provided with a fixing seat;
the upper end surface of baffle has seted up the movable groove, the surface of movable groove is close to bottom edge department and has seted up the draw-in groove, the outside surface of shielding lid is close to bottom edge department fixed mounting has the draw-in bar, the bottom surface of caulking groove is located middle part department and has seted up put in the groove, the surface of panel is close to four corners edge and has seted up the screw, draw-in bar and draw-in groove embedding are connected.
Preferably, the bottom surface of the support is fixedly provided with supporting legs, and the surface of the support is fixedly provided with a connecting frame.
Preferably, the side surface of the metering tank is close to the first fixed frame of symmetry fixed mounting in middle part department, the upper end surface fixedly connected with first closing cap of metering tank, the upper end surface of first closing cap is located middle part department fixed mounting has the speed reducer, the upper end surface fixed mounting of speed reducer has driving motor, the upper end surface of first closing cap is close to edge fixed mounting and has the material lid of throwing, the bottom surface of metering tank is located middle part department fixed mounting has the measuring pump, the fixed surface of measuring pump installs the conveyer pipe.
Preferably, the bottom surface of speed reducer rotates and is connected with the gangbar, the fixed mounting of surface equidistance of gangbar has the stirring rake.
Preferably, the side surface of reation kettle is close to middle part department symmetry fixed mounting and has the second fixed bolster, the side surface of reation kettle is located one side fixed mounting of second fixed bolster and has the flange, the upper end surface fixed mounting of reation kettle has the second closing cap, the upper end surface of second closing cap is close to middle part department fixed mounting has the butt joint board, the surface fixed mounting of butt joint board has the expansion arm, the surface of expansion arm is close to the other end and rotates and be connected with the fixed arm, the surface fixed mounting of fixed arm has the cylinder, the opposite side surface fixed mounting of fixed arm has the anticreep seat, the quantity of reation kettle is provided with two, connect through the transmission pipe between the reation kettle.
Preferably, the upper end surface fixed mounting of circulating pump has first treatment jar, the surface of first treatment jar is close to middle part department fixed mounting has first communication pipe, the upper end surface fixed mounting of first treatment jar has the mounting bracket, the bottom surface fixed mounting of mounting bracket has the automatically controlled ware, the bottom surface fixed mounting of automatically controlled ware has the electric rod, the bottom surface fixed mounting of circulating pump has the second treatment jar, the side surface of second treatment jar is close to middle part department fixed mounting has the second communication pipe, the butt joint groove has been seted up to the bottom surface of second treatment jar inboard, the inboard surface embedding of second treatment jar is connected with the lining section of thick bamboo, the upper end surface fixed mounting of lining section of thick bamboo has the filter screen, the side surface of lining section of thick bamboo is close to middle part department and has been seted up the toper through-hole, the side surface of lining section of thick bamboo is close to bottom edge symmetry fixed mounting has the dead head, the surface of dead head is close to edge and has been seted up the screw groove, the bottom surface spiral connection of lining section of thick bamboo inboard has the screw thread head, the bottom surface fixed mounting of screw thread head has the screw head.
Preferably, the upper end surface fixed mounting of gas-liquid separator has the inlet tube, the side surface of gas-liquid separator is close to bottom department fixed mounting has the exit tube, the side surface of gas-liquid separator is close to upper end edge fixed mounting has the outlet duct, the surface of outlet duct is close to one end department fixed mounting has the automatically regulated valve, the surface of outlet duct is located the opposite side fixed mounting of automatically regulated valve and has the condenser, the surface of outlet duct is close to other end department fixed mounting has the hydrogen compressor.
Preferably, the flowmeter is fixedly arranged on the upper end surface of the gas storage bottle, the shunt pipe is fixedly arranged on the upper end surface of the flowmeter, the electric control valve is fixedly arranged on the surface of the shunt pipe, and the gas storage bottle is provided with two tanks.
The invention also discloses a continuous preparation method of the 2-methyltetrahydrofuran, which comprises the following steps:
s1, putting the reserved amount of 2-methylfuran into a metering tank, putting the 2-methylfuran to be processed and a Raney nickel catalyst into a first reaction kettle, and then putting the 2-methylfuran to be processed and a palladium carbon catalyst into a second reaction kettle;
s2, respectively opening a gas storage bottle for storing nitrogen and hydrogen, so that the nitrogen and hydrogen mixture activates and dries the catalyst, and gradually eliminates air in a system device, and the output quantity of the hydrogen can be gradually increased in the process, so that the hydrogen content in the reaction kettle is continuously improved;
s3, starting a circulating pump, filtering the pumped solvent by using a second treatment tank, heating the pumped solvent by matching with a first treatment tank, gradually heating the interiors of the two groups of reaction kettles to a certain temperature, keeping the interiors of the two groups of reaction kettles in a certain pressure environment, and simultaneously opening a metering pump at the bottom of a metering tank, so that the stored 2-methylfuran can be pumped out at a certain rate to meet the preparation consumption supplement of the 2-methylfuran, thereby ensuring continuous preparation;
and S4, after the liquid entering the gas-liquid separator reaches a certain liquid level, opening a valve body connected with the gas-liquid separator and externally connected with the gas-liquid separator to obtain liquid for further rectification.
Preferably, the circulating pump is electrically connected with an external power supply.
Compared with the prior art, the invention has the following beneficial effects:
in the invention, 1) for storing the catalyst, the catalyst can be put into the tray from above the caulking groove, then the panel is closed, the catalyst can be conveniently and uniformly collected and cleaned later by utilizing the holes on the surface of the baffle net when the influence of the catalyst on the preparation process is not influenced, and the opportunity of contact between air and the catalyst can be reduced when the pocket bottom plate component is disassembled by utilizing staggered superposition of the shielding cover and the baffle plate;
2) After the preparation raw materials are put into the reaction kettle for reaction preparation, a circulating pump can be started, so that the solvent at the bottom is pumped into a second treatment tank from a second communicating pipe, doped impurities are not easy to flow out through a conical through hole and are finally blocked and deposited in a twisting head by a filter screen, and after the solution enters the first treatment tank, the solution can be heated to meet the reaction preparation requirement;
3) The hydrogen separated by the gas-liquid separator passes through the automatic regulating valve and the condenser in sequence, and finally is charged into a gas storage bottle for storing the hydrogen under the drive of a hydrogen compressor, so that the hydrogen carried in the prepared product can be recycled on one hand, and the pollution caused by hydrogen emission can be reduced on the other hand.
Drawings
FIG. 1 is a schematic diagram of the overall structure of the present invention;
FIG. 2 is a schematic diagram of the structure of the metering tank of the present invention;
FIG. 3 is a schematic diagram of a connecting structure of a reaction kettle of the invention;
FIG. 4 is an enlarged view of FIG. 3 at A;
FIG. 5 is a schematic view of a second cover and pocket floor assembly connection structure according to the present invention;
FIG. 6 is a schematic view of the bottom plate assembly of the pocket of the present invention in a disassembled configuration;
FIG. 7 is an enlarged view at B in FIG. 6;
FIG. 8 is a schematic view of the split construction of the circulation pump assembly of the present invention;
FIG. 9 is a schematic view of a gas-liquid separator assembly according to the present invention;
fig. 10 is a schematic view of the structure of the gas cylinder of the present invention.
In the figure: 1. a bracket; 101. a support leg; 102. a connecting frame; 2. a metering tank; 201. a first fixed frame; 202. a first cover; 203. a speed reducer; 204. a driving motor; 205. a feeding cover; 206. a metering pump; 207. a delivery tube; 3. a reaction kettle; 301. a second fixed frame; 302. a flange; 303. a second cover; 304. an abutting plate; 305. a movable arm; 306. a fixed arm; 307. a cylinder; 308. an anti-drop seat; 4. a pocket bottom plate; 401. a baffle; 402. a blocking net; 403. a connection cover; 404. a shielding cover; 405. a caulking groove; 406. a panel; 407. a fixing seat; 408. a movable tank 5 and a circulation pump; 501. a first treatment tank; 502. a first communication pipe; 503. a mounting frame; 504. an electric controller; 505. an electric heating rod; 506. a second treatment tank; 507. a second communicating pipe; 508. a liner; 509. a filter screen; 5010. a conical through hole; 5011. a fixed head; 5012. a thread head; 5013. the head is turned. 6. A gas-liquid separator; 601. feeding a pipe; 602. a pipe outlet; 603. an air outlet pipe; 604. an automatic regulating valve; 605. a condenser; 606. a hydrogen compressor; 7. a gas cylinder; 701. a flow meter; 702. a shunt; 703. an electrically controlled valve.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
1-10, a continuous preparation system of 2-methyltetrahydrofuran and a method thereof, comprising a bracket 1, wherein a metering tank 2 is fixedly arranged at the position, close to the edge of a side edge, of the upper end of the bracket 1, a reaction kettle 3 is fixedly arranged at the position, close to the edge of the other side, of the upper end of the bracket 1, a pocket bottom plate 4 is arranged in the reaction kettle 3, a circulating pump 5 is fixedly arranged on the side surface of the reaction kettle 3, a gas-liquid separator 6 is arranged at the position, close to the middle, of the bottom end of the inner side of the bracket 1, and a gas storage bottle 7 is fixedly connected to the surface of the gas-liquid separator 6;
the upper end surface of the pocket bottom plate 4 is fixedly provided with a baffle plate 401 at the edge, the upper end surface of the pocket bottom plate 4 is fixedly provided with a baffle net 402 at the inner side of the baffle plate 401, the upper end of the baffle net 402 is provided with a connecting cover 403, the bottom end surface of the connecting cover 403 is fixedly provided with a shielding cover 404 at the edge, the upper end surface of the connecting cover 403 is provided with a caulking groove 405 at the middle part, the surface of the caulking groove 405 is embedded and connected with a panel 406, and the upper end surface of the panel 406 is fixedly provided with a fixed seat 407 at the middle part;
the upper end surface of the baffle 401 is provided with a movable groove 408, the position, close to the bottom end edge, of the surface of the movable groove 408 is provided with a clamping groove, the position, close to the bottom end edge, of the outer side surface of the shielding cover 404 is fixedly provided with a clamping strip, the position, close to the bottom end edge, of the embedding groove 405 is provided with a throwing groove, the position, close to the four corner edges, of the surface of the panel 406 is provided with screw holes, and the clamping strip is connected with the clamping groove in an embedded mode;
the bottom end surface of the bracket 1 is fixedly provided with a supporting leg 101, and the surface of the bracket 1 is fixedly provided with a connecting frame 102;
a first fixing frame 201 is symmetrically and fixedly arranged on the side surface of the metering tank 2 close to the middle, a first sealing cover 202 is fixedly connected to the upper end surface of the metering tank 2, a speed reducer 203 is fixedly arranged on the upper end surface of the first sealing cover 202 at the middle, a driving motor 204 is fixedly arranged on the upper end surface of the speed reducer 203, a feeding cover 205 is fixedly arranged on the upper end surface of the first sealing cover 202 close to the edge, a metering pump 206 is fixedly arranged on the bottom end surface of the metering tank 2 at the middle, and a conveying pipe 207 is fixedly arranged on the surface of the metering pump 206;
a linkage rod is rotatably connected to the bottom end surface of the speed reducer 203, and stirring paddles are fixedly arranged on the surface of the linkage rod at equal intervals;
the side surface of the reaction kettle 3 is symmetrically and fixedly provided with a second fixed frame 301 near the middle part, one side surface of the reaction kettle 3 positioned on the second fixed frame 301 is fixedly provided with a flange 302, the upper end surface of the reaction kettle 3 is fixedly provided with a second sealing cover 303, the upper end surface of the second sealing cover 303 is fixedly provided with an abutting plate 304 near the middle part, the surface of the abutting plate 304 is fixedly provided with a movable arm 305, the surface of the movable arm 305 is fixedly connected with a fixed arm 306 near the other end in a rotating way, the surface of the fixed arm 306 is fixedly provided with a cylinder 307, the other side surface of the fixed arm 306 is fixedly provided with an anti-drop seat 308, the number of the reaction kettles 3 is two, and the reaction kettles 3 are connected through a transmission pipe;
the upper end surface of the circulating pump 5 is fixedly provided with a first treatment tank 501, the surface of the first treatment tank 501 is fixedly provided with a mounting frame 503 near the middle part, the bottom end surface of the mounting frame 503 is fixedly provided with an electric controller 504, the bottom end surface of the electric controller 504 is fixedly provided with an electric heating rod 505, the bottom end surface of the circulating pump 5 is fixedly provided with a second treatment tank 506, the side surface of the second treatment tank 506 is fixedly provided with a second communication pipe 507 near the middle part, the bottom end surface of the inner side of the second treatment tank 506 is provided with a butt joint groove, the inner side surface of the second treatment tank 506 is embedded and connected with a lining barrel 508, the upper end surface of the lining barrel 508 is fixedly provided with a filter screen 509, the side surface of the lining barrel 508 is provided with a conical through hole 5010 near the middle part, the side surface of the lining barrel 508 is symmetrically and fixedly provided with a fixing head 5011 near the bottom end edge, the surface of the fixing head 5011 is provided with a spiral groove near the edge, the bottom end surface of the inner side of the lining barrel 508 is spirally connected with a threaded head 5012, and the bottom end surface of the threaded head 5012 is fixedly provided with a screwing head 5013;
an inlet pipe 601 is fixedly arranged on the upper end surface of the gas-liquid separator 6, an outlet pipe 602 is fixedly arranged on the side surface of the gas-liquid separator 6 near the bottom end, an outlet pipe 603 is fixedly arranged on the side surface of the gas-liquid separator 6 near the upper end edge, an automatic regulating valve 604 is fixedly arranged on the surface of the outlet pipe 603 near one end, a condenser 605 is fixedly arranged on the surface of the outlet pipe 603 on the other side of the automatic regulating valve 604, and a hydrogen compressor 606 is fixedly arranged on the surface of the outlet pipe 603 near the other end;
the upper end surface fixed mounting of gas bomb 7 has flowmeter 701, and the upper end surface fixed mounting of flowmeter 701 has shunt tubes 702, and the surface fixed mounting of shunt tubes 702 has automatically controlled valve 703, and gas bomb 7 is provided with two jars.
The embodiment of the invention also discloses a continuous preparation method of the 2-methyltetrahydrofuran, which comprises the following steps:
s1, putting 2-methylfuran with a reserved amount into a metering tank 2, putting 2-methylfuran to be processed and Raney nickel catalyst into a first reaction kettle 3, and then putting 2-methylfuran to be processed and palladium carbon catalyst into a second reaction kettle 3;
s2, respectively opening a gas storage bottle 7 for storing nitrogen and hydrogen, so that the nitrogen and hydrogen mixture activates and dries the catalyst, and gradually eliminates air in a system device, and the output quantity of the hydrogen can be gradually increased in the process, so that the hydrogen content in the reaction kettle 3 is continuously improved;
s3, starting a circulating pump 5, filtering the pumped solvent by using a second treatment tank 506, heating the pumped solvent by matching with a first treatment tank 501, gradually heating the interiors of the two groups of reaction kettles 3 to a certain temperature, keeping the interiors at a certain pressure environment, and simultaneously opening a metering pump 206 at the bottom of a metering tank 2, so that the stored 2-methylfuran can be pumped out at a certain rate to meet the preparation consumption supplement of the 2-methylfuran, thereby ensuring continuous preparation;
s4, after the liquid entering the gas-liquid separator 6 reaches a certain liquid level, opening a valve body connected with the gas-liquid separator and externally connected with the gas-liquid separator to form a receiving tank for further rectifying the obtained liquid;
the circulating pump 5 is electrically connected with an external power supply.
Working principle: after the device preparation process starts, the speed reducer 203 can be started, the driving motor 204 drives the internal stirring structure to mix according to the set speed, the metering pump 206 is opened, pre-stored 2-methylfuran is led out according to the set speed, so as to meet the replenishing requirement of the 2-methylfuran, before that, when the inside of the device is dried and emptied by using nitrogen and hydrogen, the opening degree of the electric control valve 703 can be controlled, so that after a certain amount of gas is discharged through the flowmeter 701, the content ratio of the hydrogen in the device is gradually controlled by the gas storage bottle 7 for storing the nitrogen and the hydrogen respectively, after the preparation raw materials are put into the reaction kettle 3 to perform reaction preparation, the circulating pump 5 can be started, so that the solvent at the bottom is pumped into the second processing tank 506 from the second communicating pipe 507, the doped impurities are not easy to flow out through the conical through hole 5010, and are finally blocked and deposited in the interior of the rotary head 5013 by the filter screen 509, after the first processing tank 501 is further fed into the first processing tank 501, so as to meet the reaction preparation requirement, the catalyst is always stored in the interior of the baffle network 402, the catalyst is completed through the hole 406, the catalyst is completely, the catalyst is filled in the interior of the baffle plate 406, the catalyst is easily stored in the baffle tank through the baffle network, the baffle plate 406 is removed from the inner part, the inner part is easy to be connected with the movable cover 408 through the movable cover 408, and the movable cover 408 can be moved to the movable cover 408, and the movable cover is connected with the movable cover 408, and the movable cover can be moved to the bottom through the movable cover 408, and the movable cover 408.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. The continuous preparation system of 2-methyltetrahydrofuran comprises a bracket (1), and is characterized in that: the device is characterized in that metering tanks (2) are fixedly arranged at the upper end of the support (1) close to the edge of the side, two reaction kettles (3) are arranged, the reaction kettles (3) are connected through transmission pipes, a first reaction kettles (3) is fixedly arranged at the edge of the upper end of the support (1) close to the other side, a second reaction kettles (3) are fixedly arranged below the first reaction kettles (3), a pocket bottom plate (4) is arranged in the reaction kettles (3), a circulating pump (5) is fixedly arranged on the side surface of the reaction kettles (3), a gas-liquid separator (6) is arranged at the position, close to the middle, of the bottom end of the inner side of the support (1), and a gas storage bottle (7) is fixedly connected to the surface of the gas-liquid separator (6);
the upper end surface of the pocket bottom plate (4) is fixedly provided with a baffle plate (401) at the edge, the inner side of the baffle plate (401) is fixedly provided with a baffle net (402) at the upper end surface of the pocket bottom plate (4), the upper end of the baffle net (402) is provided with a connecting cover (403), the bottom end surface of the connecting cover (403) is fixedly provided with a shielding cover (404) at the edge, the middle part of the upper end surface of the connecting cover (403) is provided with a caulking groove (405), the surface of the caulking groove (405) is embedded and connected with a panel (406), and the middle part of the upper end surface of the panel (406) is fixedly provided with a fixing seat (407);
the upper end surface of the baffle plate (401) is provided with a movable groove (408), the surface of the movable groove (408) close to the bottom end edge is provided with a clamping groove, the outer side surface of the shielding cover (404) close to the bottom end edge is fixedly provided with a clamping strip, the bottom end surface of the caulking groove (405) is provided with a throwing groove at the middle part, the surface of the panel (406) close to the four corner edge is provided with a screw hole, the clamping strip is connected with the clamping groove in an embedded mode, the bottom end surface of the bracket (1) is fixedly provided with supporting legs (101), and the surface of the bracket (1) is fixedly provided with a connecting frame (102);
the metering device is characterized in that a first fixing frame (201) is symmetrically and fixedly arranged at the position, close to the middle, of the side surface of the metering tank (2), a first sealing cover (202) is fixedly connected to the upper end surface of the metering tank (2), a speed reducer (203) is fixedly arranged at the position, close to the middle, of the upper end surface of the first sealing cover (202), a driving motor (204) is fixedly arranged at the upper end surface of the speed reducer (203), a feeding cover (205) is fixedly arranged at the position, close to the edge, of the upper end surface of the first sealing cover (202), a metering pump (206) is fixedly arranged at the position, close to the middle, of the bottom end surface of the metering tank (2), a conveying pipe (207) is fixedly arranged on the surface of the metering pump (206), the conveying pipe (207) is connected with a first reaction kettle (3), a linkage rod is rotationally connected to the bottom end surface of the speed reducer (203), and stirring paddles are fixedly arranged on the surface of the linkage rod at equal intervals;
the side surface of the reaction kettle (3) is close to the middle part and is symmetrically and fixedly provided with a second fixed frame (301), one side of the side surface of the reaction kettle (3) positioned on the second fixed frame (301) is fixedly provided with a flange (302), the upper end surface of the reaction kettle (3) is fixedly provided with a second sealing cover (303), the upper end surface of the second sealing cover (303) is close to the middle part and is fixedly provided with an abutting plate (304), the surface of the abutting plate (304) is fixedly provided with a movable arm (305), the surface of the movable arm (305) is close to the other end and is rotationally connected with a fixed arm (306), the surface of the fixed arm (306) is fixedly provided with a cylinder (307), and the other side surface of the fixed arm (306) is fixedly provided with an anti-drop seat (308);
the upper end surface fixed mounting of circulating pump (5) has first treatment jar (501), the surface of first treatment jar (501) is close to middle part department fixed mounting has first communicating pipe (502), the upper end surface fixed mounting of first treatment jar (501) has mounting bracket (503), the bottom surface fixed mounting of mounting bracket (503) has electric controller (504), the bottom surface fixed mounting of electric controller (504) has electric bar (505), the bottom surface fixed mounting of circulating pump (5) has second treatment jar (506), the side surface of second treatment jar (506) is close to middle part department fixed mounting has second communicating pipe (507), the inner bottom surface of the second treatment tank (506) is provided with a butt joint groove, the inner side surface of the second treatment tank (506) is embedded and connected with a lining barrel (508), the upper end surface of the lining barrel (508) is fixedly provided with a filter screen (509), the side surface of the lining barrel (508) is provided with a conical through hole (5010) close to the middle part, the side surface of the lining barrel (508) is symmetrically and fixedly provided with a fixing head (5011) close to the bottom edge, the surface of the fixing head (5011) is provided with a screw groove close to the edge, the inner bottom surface of the lining barrel (508) is spirally connected with a thread head (5012), the bottom surface of the thread head (5012) is fixedly provided with a screwing head (5013), the first communicating pipe (502) and the second communicating pipe (507) are both connected with the same reaction kettle (3);
the upper end surface fixed mounting of gas-liquid separator (6) has intake pipe (601), intake pipe (601) connect the second reation kettle (3), the side surface of gas-liquid separator (6) is close to bottom department fixed mounting has exit tube (602), the side surface of gas-liquid separator (6) is close to upper end edge fixed mounting has outlet duct (603), the surface of outlet duct (603) is close to one end department fixed mounting and has automatic regulating valve (604), the surface of outlet duct (603) is located opposite side fixed mounting of automatic regulating valve (604) and has condenser (605), the surface of outlet duct (603) is close to other end department fixed mounting and has hydrogen compressor (606).
2. A continuous production system of 2-methyltetrahydrofuran according to claim 1, wherein: the gas storage device is characterized in that a flowmeter (701) is fixedly arranged on the upper end surface of the gas storage bottle (7), a shunt pipe (702) is fixedly arranged on the upper end surface of the flowmeter (701), an electric control valve (703) is fixedly arranged on the surface of the shunt pipe (702), and the gas storage bottle (7) is provided with two tanks.
3. A method of implementing the continuous production system of 2-methyltetrahydrofuran of claim 2, characterized by: the method comprises the following steps: s1, putting 2-methylfuran with a reserved amount into a metering tank (2), putting 2-methylfuran to be processed and Raney nickel catalyst into a first reaction kettle (3), and then putting 2-methylfuran to be processed and palladium carbon catalyst into a second reaction kettle (3); s2, respectively opening a gas storage bottle (7) for storing nitrogen and hydrogen, enabling a nitrogen and hydrogen mixture to activate and dry a catalyst, gradually removing air in a system device, gradually increasing the output quantity of hydrogen in the process, continuously lifting the hydrogen content S3 in the reaction kettle (3), starting a circulating pump (5), filtering the pumped solvent by using a second treatment tank (506), heating the pumped solvent by matching with a first treatment tank (501), gradually heating the interiors of the two groups of reaction kettles (3) to a certain temperature, keeping the temperature in a certain pressure environment, and simultaneously opening a metering pump (206) at the bottom of the metering tank (2), so that the stored 2-methyl furan can be pumped out at a certain speed to meet the preparation consumption supplement of the 2-methyl furan, thereby ensuring continuous preparation; and S4, after the liquid entering the gas-liquid separator (6) reaches a certain liquid level, opening a valve body of an external receiving tank connected with the gas-liquid separator for further rectifying the obtained liquid.
4. A method according to claim 3, characterized in that: the circulating pump (5) is electrically connected with an external power supply.
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| CN202210665600.4A CN115228387B (en) | 2022-06-13 | 2022-06-13 | Continuous preparation system and method for 2-methyltetrahydrofuran |
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