CN115041104B - Device and method for preparing n-propionaldehyde from carbon dioxide - Google Patents
Device and method for preparing n-propionaldehyde from carbon dioxide Download PDFInfo
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- CN115041104B CN115041104B CN202210638295.XA CN202210638295A CN115041104B CN 115041104 B CN115041104 B CN 115041104B CN 202210638295 A CN202210638295 A CN 202210638295A CN 115041104 B CN115041104 B CN 115041104B
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- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 title claims abstract description 146
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 27
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 132
- 239000007788 liquid Substances 0.000 claims abstract description 93
- 239000012074 organic phase Substances 0.000 claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000012071 phase Substances 0.000 claims abstract description 32
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 12
- 239000007789 gas Substances 0.000 claims description 41
- 238000009833 condensation Methods 0.000 claims description 37
- 230000005494 condensation Effects 0.000 claims description 37
- 238000007789 sealing Methods 0.000 claims description 23
- 238000004891 communication Methods 0.000 claims description 19
- 230000007246 mechanism Effects 0.000 claims description 12
- 238000005192 partition Methods 0.000 claims description 10
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 8
- 239000005977 Ethylene Substances 0.000 claims description 8
- 230000006835 compression Effects 0.000 claims description 7
- 238000007906 compression Methods 0.000 claims description 7
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 4
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 230000002093 peripheral effect Effects 0.000 claims description 4
- 238000001308 synthesis method Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 238000000605 extraction Methods 0.000 abstract description 28
- 239000000376 reactant Substances 0.000 abstract description 12
- 238000006243 chemical reaction Methods 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 2
- 238000009835 boiling Methods 0.000 abstract 1
- 239000008346 aqueous phase Substances 0.000 description 11
- 239000000463 material Substances 0.000 description 6
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 5
- 238000005086 pumping Methods 0.000 description 5
- 238000005119 centrifugation Methods 0.000 description 4
- 230000005484 gravity Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000007798 antifreeze agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CREMABGTGYGIQB-UHFFFAOYSA-N carbon carbon Chemical compound C.C CREMABGTGYGIQB-UHFFFAOYSA-N 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012024 dehydrating agents Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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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
- B01J8/08—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
- B01J8/10—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/49—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reaction with carbon monoxide
- C07C45/50—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reaction with carbon monoxide by oxo-reactions
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
- C07C45/78—Separation; Purification; Stabilisation; Use of additives
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
- C07C5/42—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with a hydrogen acceptor
Abstract
The invention discloses a device and a method for preparing n-propionaldehyde by carbon dioxide, belonging to the field of carbon dioxide emission reduction. According to the invention, the reactant obtained by the reaction is extracted twice during the extraction of the n-propionaldehyde, so that the extraction amount is ensured, and incomplete extraction is avoided. The method comprises primary extraction and secondary extraction; primary extraction: firstly, carrying out gas-liquid separation on reactants under low pressure, gasifying the n-propionaldehyde under low pressure, wherein the separated gas contains the n-propionaldehyde and unreacted raw material gas, and condensing the collected gas into n-propionaldehyde liquid due to the low boiling point of the n-propionaldehyde; and (3) re-extraction: and carrying out centrifugal separation on the liquid obtained after gas-liquid separation to obtain an organic phase solution and a water phase solution, extracting n-propionaldehyde from the organic phase solution, and recovering the catalyst from the water phase solution for reuse.
Description
Technical Field
The invention belongs to the field of carbon dioxide emission reduction, and particularly relates to a device and a method for preparing n-propionaldehyde by using carbon dioxide.
Background
Propionaldehyde is an organic compound, is a colorless transparent liquid, is mainly used for preparing synthetic fibers, rubber accelerators, anti-aging agents and the like, and can also be used as an antifreeze agent, a lubricant, a dehydrating agent and the like. Carbon dioxide is not only the most important greenhouse gas, but also the carbon-carbon resource which is widely distributed and most abundant on the earth. The prior method for preparing the n-propionaldehyde by utilizing the carbon dioxide comprises the steps of firstly preparing ethylene by taking ethane and the carbon dioxide as raw materials; the ethylene reacts with carbon monoxide and hydrogen by the oxo synthesis method to prepare the n-propionaldehyde under the participation of the catalyst. The reactant obtained after the completion of the reaction contains not only the desired n-propionaldehyde but also an unreacted raw material gas and a catalyst solution to be recycled, and therefore, the n-propionaldehyde needs to be separated and extracted. Therefore, there is a need for a device and a method for preparing n-propionaldehyde from carbon dioxide, which solve the above problems.
The invention provides a device for preparing n-propionaldehyde by carbon dioxide and a preparation method thereof. The method comprises primary extraction and secondary extraction; primary extraction: firstly, carrying out gas-liquid separation on reactants under low pressure, gasifying the n-propionaldehyde under low pressure, wherein the separated gas contains the n-propionaldehyde and unreacted raw material gas, and then condensing the collected gas to collect n-propionaldehyde liquid; and (3) re-extraction: and carrying out centrifugal separation on the liquid obtained after gas-liquid separation to obtain an organic phase solution and a water phase solution, extracting n-propionaldehyde from the organic phase solution, and recovering the catalyst from the water phase solution for reuse.
Disclosure of Invention
The invention aims to provide a device for preparing n-propionaldehyde from carbon dioxide and a preparation method thereof, which aim to solve the problems of the prior art in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: the device for preparing the n-propionaldehyde by the carbon dioxide comprises a low-pressure separation tank, wherein the low-pressure separation tank is divided into an upper gas-liquid separation zone and a lower liquid-liquid separation zone, and the upper gas-liquid separation zone and the lower liquid-liquid separation zone are separated by a partition plate.
Preferably, the gas-liquid separation zone comprises a feeding port and a gas collection bin arranged at the top end of the low-pressure separation tank, and the gas collection bin is communicated with the low-pressure separation tank through a condensation pipe;
preferably, the liquid-liquid separation zone comprises a centrifugal separation mechanism rotatably mounted in the center of the low-pressure separation tank, and a water phase collection bin and an organic phase collection bin which are arranged at the bottom end of the low-pressure separation tank; the centrifugal separation mechanism comprises a centrifugal bin arranged in the low-pressure separation tank, a centrifugal shaft is rotatably arranged at the middle shaft of the centrifugal bin, and centrifugal plates are arranged at intervals in the circumferential direction of the centrifugal shaft; the bottom end of the centrifugal shaft is externally connected with a driving mechanism; the water phase collecting bin is used for collecting the solution in the middle of the centrifugal bin, and the organic phase collecting bin is used for collecting the solution centrifugally thrown out by the centrifugal bin.
Preferably, the baffle is funnel-shaped, and the bottom of baffle is opened has the intercommunication mouth that communicates gas-liquid separation district and liquid-liquid separation district.
Preferably, the bottom end of the centrifugal bin is communicated with the water phase collecting bin through a discharge pipe; the peripheral edge of centrifugation storehouse upper end is provided with the guide plate, the guide plate slope sets up, the least significant end of guide plate is linked together through honeycomb duct and organic collection storehouse mutually.
Preferably, the centrifugal bin is vertically and slidably mounted in the low-pressure separation tank, and the bottom end of the centrifugal shaft is in key connection with the driving mechanism; along the sliding direction of the centrifugal bin, a compression spring is arranged between the centrifugal bin and the bottom plate of the low-pressure separation tank; the discharging pipe and the flow guide pipe are internally provided with a closed unit; the sealing unit is used for opening the discharge pipe and the guide pipe when the centrifugal bin is located at the lowest position.
Preferably, the sealing unit comprises countersunk holes arranged in the discharge pipe and the diversion pipe, a sealing plate is vertically and slidably mounted in a large hole of the countersunk hole, a support pillar is fixedly mounted below the sealing plate, and the diameter of the support pillar is smaller than that of a small hole of the countersunk hole; the support column is used for contacting the bottom surface of the low-pressure separation tank when the centrifugal bin is positioned at the lowest position, jacking the sealing plate and opening the discharge pipe and the flow guide pipe; the bottom surface of the centrifugal bin is also provided with a locking unit which is used for locking the centrifugal bin and the low-pressure separation tank when the closing plate is opened and releasing the locking after the collection of the water-phase collection bin and the organic-phase collection bin is finished.
Preferably, the material inlet, the gas collection bin, the water phase collection bin and the organic phase collection bin are all internally provided with a weighing unit.
Preferably, a pressure pumping fan is arranged at the joint of the condensation pipe and the low-pressure separation tank, the pressure pumping fan is rotatably installed in the condensation pipe, a first rotating shaft is fixedly installed in the middle of the pressure pumping fan, and the bottom end of the first rotating shaft is connected with the top key of the centrifugal shaft.
Preferably, a condensing plate is rotatably mounted in the gas-liquid separation zone and is arranged at two ends of the condensing pipe; the condensation plate is rotatably arranged on the inner wall of the low-pressure separation tank through a second rotating shaft; and a worm wheel is fixedly mounted on the second rotating shaft and is in transmission connection with a worm fixedly mounted on the first rotating shaft.
Preferably, a sealing block for sealing the communication opening is fixedly arranged at the upper part of the centrifugal shaft, and the sealing block seals the communication opening when the centrifugal bin is located at the lowest position.
Preferably, the top end of the low-pressure separation tank is also provided with a closing assembly for closing the condensation pipe, the closing assembly comprises a closing plate which is slidably mounted at the top end of the low-pressure separation tank, and the closing plate is used for isolating the communication between the condensation pipe and the low-pressure separation tank; a driving spring is arranged on the closing plate and the low-pressure separation tank along the sliding direction of the closing plate, and the driving spring drives the closing plate to seal the condensation pipe; the first rotating shaft is fixedly provided with a rotating ring, rotating rods are arranged at intervals in the circumferential direction of the rotating ring, one end of each rotating rod is hinged to the corresponding rotating ring, and the other end of each rotating rod is vertically slidably mounted on the sealing plate.
The invention also provides a method for preparing n-propionaldehyde by carbon dioxide, which is suitable for the device for preparing n-propionaldehyde, and mainly comprises the following steps:
s1: preparing ethylene by using ethane and carbon dioxide as raw materials, reacting the ethylene with carbon monoxide and hydrogen by using a oxo synthesis method under the participation of a catalyst, and introducing an obtained liquid flow from a feed inlet of a low-pressure separation tank;
s2: the liquid flow enters a low-pressure separation tank and then undergoes gas-liquid separation, the n-propionaldehyde in the liquid flow is gasified and enters a gas collection bin through a condensation pipe for condensation and collection, and the liquid flow enters a liquid-liquid separation zone through a communication port;
s3: the liquid flow is centrifugally separated by a centrifugal bin, the organic phase enters an organic phase collecting bin to extract n-propionaldehyde, and the water phase enters a water phase collecting bin to extract a catalyst;
s4: the n-propionaldehyde extracted from the organic phase collection bin and the n-propionaldehyde collected by condensation of the gas collection bin are the prepared n-propionaldehyde.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, the reactant obtained by the reaction is extracted twice during the extraction of the n-propionaldehyde, so that the extraction amount is ensured, and incomplete extraction is avoided. The method comprises primary extraction and secondary extraction; primary extraction: firstly, carrying out gas-liquid separation on reactants under low pressure, gasifying n-propionaldehyde under low pressure, wherein the separated gas contains the n-propionaldehyde and unreacted raw material gas, and then condensing the collected gas to obtain collected n-propionaldehyde liquid; and (3) re-extraction: and carrying out centrifugal separation on the liquid obtained after gas-liquid separation to obtain an organic phase solution and a water phase solution, extracting n-propionaldehyde from the organic phase solution, and recovering the catalyst from the water phase solution for reuse.
2. The invention utilizes the driving force of the centrifugal shaft to drive the pressure extraction fan to rotate. The rotation of the pressure extraction fan can not only lead the airflow into the gas collection bin for collection, but also further reduce the air pressure in the low-pressure separation tank and promote the gasification rate of the n-propionaldehyde. In addition, the low pressure is also helpful for the separation of organic phase and water phase in the liquid-liquid separation zone.
3. According to the invention, the centrifugal shaft is automatically separated from the first rotating shaft by the key connection arrangement when the centrifugal bin is positioned at the lowest position, and the closing plate automatically seals the condenser pipe; and in other time, the centrifugal shaft and the first rotating shaft are in key connection transmission, so that the closing plate is driven to open the condensing pipe, and the pressure extraction fan and the condensing plate are driven to rotate.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an apparatus for producing n-propanal from carbon dioxide according to the present invention;
FIG. 2 is a schematic view of a partial cross-section of an apparatus for preparing n-propylaldehyde according to the present invention;
FIG. 3 is an enlarged view of a portion A of FIG. 2 according to the present invention;
FIG. 4 is a schematic structural view of a half section of a device for preparing n-propylaldehyde according to the present invention;
FIG. 5 is an enlarged partial view of portion B of FIG. 4 in accordance with the present invention;
FIG. 6 is an enlarged, fragmentary view of portion C of FIG. 4 in accordance with the present invention;
FIG. 7 is an enlarged partial view of portion D of FIG. 4 in accordance with the present invention;
FIG. 8 is a process flow diagram of a method for preparing n-propanal from carbon dioxide according to the present invention.
In the drawings, the components represented by the respective reference numerals are listed below:
11-a low-pressure separation tank, 12-a gas-liquid separation zone, 13-a liquid-liquid separation zone, 14-a partition plate, 15-a feeding port, 16-a gas collection bin, 17-a condensation pipe, 18-a water phase collection bin, 19-an organic phase collection bin, 21-a centrifugal bin, 22-a centrifugal shaft, 23-a centrifugal plate, 24-a communication port, 25-a discharging pipe, 26-a guide plate, 27-a guide pipe, 31-a compression spring, 32-a counter sink hole, 33-a sealing plate, 34-a support column, 35-a locking unit, 41-a pressure-pumping fan, 42-a first rotating shaft, 43-a condensation plate, 44-a second rotating shaft, 45-a worm wheel, 46-a worm, 51-a sealing block, 52-a closing plate, 53-a driving spring, 54-a rotating ring and 55-a rotating rod.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-8, an apparatus for preparing n-propanal from carbon dioxide comprises a low-pressure separation tank 11, wherein the low-pressure separation tank 11 is divided into an upper gas-liquid separation zone 12 and a lower liquid-liquid separation zone 13, which are separated by a partition 14.
Preferably, the gas-liquid separation zone 12 comprises a feed inlet 15 and a gas collection bin 16 arranged at the top end of the low-pressure separation tank 11, and the gas collection bin 16 is communicated with the low-pressure separation tank 11 through a condensation pipe 17;
preferably, the liquid-liquid separation zone 13 comprises a centrifugal separation mechanism rotatably mounted in the center of the low-pressure separation tank 11, and a water phase collection bin 18 and an organic phase collection bin 19 which are arranged at the bottom end of the low-pressure separation tank 11; the centrifugal separation mechanism comprises a centrifugal bin 21 arranged in the low-pressure separation tank 11, a centrifugal shaft 22 is rotatably arranged at the middle shaft of the centrifugal bin 21, and centrifugal plates 23 are arranged at intervals in the circumferential direction of the centrifugal shaft 22; the bottom end of the centrifugal shaft 22 is externally connected with a driving mechanism; the water phase collecting bin 18 is used for collecting the solution in the middle of the centrifugal bin 21, and the organic phase collecting bin 19 is used for collecting the solution centrifugally thrown out by the centrifugal bin 21.
Preferably, the partition 14 is funnel-shaped, and a communication port 24 for communicating the gas-liquid separation region 12 and the liquid-liquid separation region 13 is formed at the bottom end of the partition 14.
The method comprises primary extraction and secondary extraction; primary extraction: firstly, carrying out gas-liquid separation on reactants under low pressure, gasifying n-propionaldehyde under low pressure, wherein the separated gas contains the n-propionaldehyde and unreacted raw material gas, and then condensing the collected gas to obtain collected n-propionaldehyde liquid; and (3) re-extraction: and carrying out centrifugal separation on the liquid obtained after gas-liquid separation to obtain an organic phase solution and a water phase solution, extracting n-propionaldehyde from the organic phase solution, and recovering the catalyst from the water phase solution for reuse. As shown in fig. 1, the specific workflow is as follows: the liquid reactant stream obtained after the reaction in the preceding step is introduced from the inlet 15 into the low-pressure separation tank 11 for separation. As shown in FIG. 2, the reactant is introduced into a gas-liquid separation zone 12 in the upper middle portion of a low-pressure separation tank 11. Because the pre-process is a high pressure environment, n-propanal is a liquid. And then the normal propionaldehyde is gasified by the low pressure in the low-pressure separation tank 11, the normal propionaldehyde gas and the unreacted raw material gas are collected by the gas collection bin 16 above the low-pressure separation tank 11, and the normal propionaldehyde is condensed and collected into liquid in the gas collection bin 16 to finish the primary extraction of the normal propionaldehyde. As shown in fig. 2, the liquid in the gas-liquid separation zone 12 flows back through the funnel-shaped partition 14 and enters the liquid-liquid separation zone 13 below through the communication port 24. The funnel-shaped partition plate 14 of the invention enables the size of the communication port 24 to be smaller, thereby prolonging the time for reactants to flow on the isolation plate and enabling the gas to be completely separated; and simultaneously, the water vapor in the liquid-liquid separation zone 13 can be prevented from escaping into the gas separation zone. As shown in FIG. 4, the liquid enters the liquid-liquid separation zone 13 for centrifugal separation, and the centrifugal shaft 22 in the centrifugal bin 21 rotates to drive the liquid to rotate and centrifuge through the centrifugal plate 23. Because the mass of the organic matter is large, under the centrifugal action, the n-propionaldehyde solution is positioned at the outer side of the centrifugal bin 21, the inorganic solution containing the catalyst is positioned at the inner side of the centrifugal bin 21, then the classification and collection are carried out, and the n-propionaldehyde solution positioned at the outer side is further extracted, for example, by a rectifying tower; and (4) reintroducing the catalyst solution positioned at the inner side into the pre-process for recycling. Compared with the method of directly guiding the reactant into the rectifying tower for extraction, the method has the advantages that the reactant is firstly extracted once and then guided into the rectifying tower, so that the workload of the rectifying tower can be effectively reduced, and the working efficiency of the rectifying tower is improved.
Preferably, the bottom end of the centrifugal bin 21 is communicated with the water phase collecting bin 18 through a discharge pipe 25; the peripheral edge of the upper end of the centrifugal bin 21 is provided with a guide plate 26, the guide plate 26 is obliquely arranged, and the lowest end of the guide plate 26 is communicated with the organic phase collecting bin 19 through a guide pipe 27.
As shown in fig. 2, the liquid of the present invention is separated into an organic phase and a liquid phase when it is centrifuged in the centrifugal chamber 21, and n-propanal is present in the organic phase. When the liquid above is continuously introduced into the centrifugal chamber 21, the liquid in the centrifugal chamber 21 is continuously raised. Under the centrifugal effect, the organic phase solution overflows the centrifugal bin 21, enters the guide plate 26 positioned on the peripheral edge of the upper end of the centrifugal bin 21, and is guided to the organic phase collecting bin 19 by the guide plate 26 which is obliquely arranged to be collected.
Preferably, the centrifugal bin 21 is vertically and slidably mounted in the low-pressure separation tank 11, and the bottom end of the centrifugal shaft 22 is in key connection with a driving mechanism; along the sliding direction of the centrifugal bin 21, a compression spring 31 is arranged between the centrifugal bin 21 and the bottom plate of the low-pressure separation tank 11; the discharge pipe 25 and the guide pipe 27 are internally provided with closed units; the closing unit is used for opening the discharge pipe 25 and the guide pipe 27 when the centrifugal bin 21 is located at the lowest position.
Preferably, the closing unit comprises a counter bore 32 arranged in the discharge pipe 25 and the guide pipe 27, a closing plate 33 is vertically and slidably mounted in a large hole of the counter bore 32, a support column 34 is fixedly mounted below the closing plate 33, and the diameter of the support column 34 is smaller than that of a small hole of the counter bore 32; the supporting column 34 is used for contacting the bottom surface of the low-pressure separation tank 11 when the centrifugal bin 21 is positioned at the lowest position, jacking the closing plate 33, and opening the discharge pipe 25 and the guide pipe 27; still install locking unit 35 on the bottom surface of centrifugation storehouse 21, locking unit 35 is used for locking centrifugation storehouse 21 and low pressure knockout drum 11 when closing plate 33 is opened, removes locking after aqueous phase collection storehouse 18, organic phase collection storehouse 19 collect and finish.
As the liquid continuously enters the centrifugal bin 21, the liquid in the centrifugal bin 21 is more and more, and needs to be collected in time. The invention judges the solution amount in the centrifugal bin 21 by gravity, automatically classifies and collects the solution, and avoids manual operation. As shown in FIG. 4, the gravity applied to the bottom surface of the centrifugal chamber 21 increases as the liquid entering the centrifugal chamber 21 increases, and the centrifugal chamber 21 moves downward in the low pressure separation tank 11 to compress the compression spring 31. When the weight of the liquid in the centrifugal bin 21 reaches a preset value, the centrifugal bin 21 is located at the lowest position, the sealing unit opens the discharge pipe 25 and the flow guide pipe 27, so that the aqueous phase solution located in the discharge pipe 25 can enter the aqueous phase collecting bin 18 for collection, the organic phase solution located in the flow guide pipe 27 can enter the organic phase collecting bin 19 for collection, and the classification collection is completed. The specific working principle of the sealing unit is shown in fig. 6, taking the sealing unit in the draft tube 27 as an example, when the liquid in the centrifugal bin 21 continuously increases, the centrifugal bin 21 continuously moves downwards, and at this time, the draft tube 27 continuously moves downwards along with the centrifugal bin 21, and the support column 34 in the counter bore 32 is firstly contacted with the bottom surface of the low pressure separation tank 11. The support columns 34 support the closing plate 33 by the bosses at the bottom ends thereof first to move upward in the counter bored holes 32. When the centrifugal bin 21 is located at the lowest position, the supporting column 34 just supports the closing plate 33 to be separated from the perforation of the counter sink 32, so that the counter sink 32 is opened, the flow guide pipe 27 is communicated with the organic phase collecting bin 19 located below the flow guide pipe, and the organic phase solution is collected. The same applies to the closed unit in the tapping pipe 25. As shown in fig. 7, the present invention also provides an embodiment of the locking unit 35, when the centrifuge basket 21 is located at the lowest position, the locking unit 35 moved down to the lowest position as the centrifuge basket 21 moves down. As shown in fig. 7, the locking unit 35 of the present invention is an elastic locking block, and when the centrifugal chamber 21 is located at the lowest position, the elastic locking block will be locked with the low pressure separation tank 11 to lock the centrifugal chamber 21 and the low pressure separation tank 11; when the aqueous phase collection chamber 18 and the organic phase collection chamber 19 collect the organic phase, the gravity of the centrifugal chamber 21 is reduced, but the position of the centrifugal chamber 21 is not changed, and the closed unit is still in the open state. When the preset value is collected, the air cylinder drives the annular unlocking piece to unlock the elastic clamping block, and the centrifugal bin 21 is reset under the restoring force of the compression spring 31.
Preferably, the material inlet 15, the gas collection bin 16, the aqueous phase collection bin 18 and the organic phase collection bin 19 are all provided with a weighing unit.
The centrifugal shaft 22 rotates continuously when the centrifugal bin 21 collects the waste water. In order to avoid that excessive liquid directly overflows the centrifugal bin 21 during centrifugation, the invention needs to classify and collect the liquid in time and reduce the liquid amount in the separation bin. Since the separation interface of the organic phase and the aqueous phase is not fixed with the change of the liquid amount in the centrifugal chamber 21, the organic phase solution may be collected by the aqueous phase collecting chamber 18 through the discharging pipe 25. Therefore, the weighing units are arranged in the material inlet 15, the gas collecting bin 16, the water phase collecting bin 18 and the organic phase collecting bin 19, according to the principle of conservation of mass, when the weight of the materials collected by the gas collecting bin 16, the water phase collecting bin 18 and the organic phase collecting bin 19 reaches a preset value, the preset value is an input value of the material inlet 15 in the time period, the locking unit 35 is driven to unlock, and the centrifugal bin 21 rebounds under the restoring force of the compression spring 31 and reciprocates in a circulating mode.
Preferably, a pressure suction fan 41 is arranged at the connection position of the condensation pipe 17 and the low pressure separation tank 11, the pressure suction fan 41 is rotatably installed in the condensation pipe 17, a first rotating shaft 42 is fixedly installed in the middle of the pressure suction fan 41, and the bottom end of the first rotating shaft 42 is in key connection with the top end of the centrifugal shaft 22.
As shown in FIG. 4, the rotation of the eccentric shaft 22 via the keyed connection drives the rotation of the first rotating shaft 42, and the first rotating shaft 42 drives the rotation of the pumping fan 41. The invention utilizes the driving force of the centrifugal shaft 22 to drive the pressure extraction fan 41 to rotate. The rotation of the pressure-extracting fan 41 not only can guide the gas flow into the gas collecting bin 16 for storage, but also can further reduce the gas pressure in the low-pressure separation tank 11 and promote the vaporization rate of the n-propanal. In addition, the low pressure also facilitates the separation of the organic phase and the aqueous phase in the liquid-liquid separation zone 13.
Preferably, a condensing plate 43 is further rotatably mounted in the gas-liquid separation zone 12, and the condensing plate 43 is disposed at two ends of the condensing pipe 17; the condensing plate 43 is rotatably mounted on the inner wall of the low pressure separation tank 11 through a second rotating shaft 44; a worm wheel 45 is fixedly mounted on the second rotating shaft 44, and the worm wheel 45 is in transmission connection with a worm 46 fixedly mounted on the first rotating shaft 42.
To prevent excess water vapor from entering the gas collection bin 16, the purity of the collected n-propanal is affected. As shown in fig. 5, the first rotating shaft 42 rotates to rotate the worm 46, the screw rotates the second rotating shaft 44 via the worm wheel 45, and the second rotating shaft 44 rotates the condensing plate 43. The condensation plates 43 are arranged at the two ends of the condensation pipe 17, and the water vapor is condensed on the condensation plates 43 and then thrown away from the condensation plates 43 due to the rotation of the condensation plates 43 to enter the liquid-liquid separation zone 13 at the lower part.
Preferably, a closing block 51 for closing the communication port 24 is fixedly arranged at the upper part of the centrifugal shaft 22, and the closing block 51 closes the communication port 24 when the centrifugal bin 21 is located at the lowest position. When the organic phase collection bin 19 and the aqueous phase collection bin 18 are used for collecting, the invention needs to warn to close the communication port 24 to prevent the liquid above from entering the centrifugal bin 21, so as to prevent the liquid which is not centrifuged from directly leaving from the discharge pipe 25 to influence the collection of the n-propionaldehyde. As shown in FIG. 4, when the centrifugal bin 21 moves downward, the centrifugal shaft 22 moves downward, a sealing block 51 is fixedly disposed on the upper portion of the centrifugal shaft 22, and when the centrifugal bin 21 is located at the lowest position, the sealing block 51 just seals the communication opening 24.
Preferably, the top end of the low-pressure separation tank 11 is further provided with a closing assembly for closing the condensation pipe 17, the closing assembly comprises a closing plate 52 slidably mounted on the top end of the low-pressure separation tank 11, and the closing plate 52 is used for isolating the communication between the condensation pipe 17 and the low-pressure separation tank 11; a driving spring 53 is provided at the closing plate 52 and the low pressure separation tank 11 along the sliding direction of the closing plate 52, and the driving spring 53 drives the closing plate 52 to close the condensation duct 17; a rotating ring 54 is fixedly mounted on the first rotating shaft 42, rotating rods 55 are arranged at intervals in the circumferential direction of the rotating ring 54, one end of each rotating rod 55 is hinged to the corresponding rotating ring 54, and the other end of each rotating rod 55 is vertically and slidably mounted on the closing plate 33.
Because the present invention needs to determine whether the locking unit 35 is unlocked and whether the organic phase and the liquid phase are completely collected according to the mass of the collected substances, the gas collection chamber 16 needs to stop collecting when the organic phase collection chamber 19 and the water phase collection chamber 18 collect the substances, thereby avoiding changing the mass. The present invention is further provided with a closing assembly at the junction of the condensation duct 17 and the low pressure separator tank 11, as shown in fig. 5. When the organic phase collecting bin 19 and the aqueous phase collecting bin 18 are not collecting, the rotation of the centrifugal shaft 22 drives the first rotating shaft 42 to rotate, the first rotating shaft 42 drives the rotating ring 54 to rotate, the rotating ring 54 drives the rotating rod 55 to rotate, and due to the centrifugal force, the rotating rod 55 can prop open the closing plate 52 when rotating, so that the closing plate 52 is opened. When the organic phase collection bin 19 and the aqueous phase collection bin 18 start to collect, the centrifugal bin 21 is located at the lowest position, the centrifugal shaft 22 moves downwards to enable the key to be just separated from the first rotating shaft 42, the first rotating shaft 42 stops rotating, the rotating ring 54 stops rotating, the rotating rod 55 stops rotating, the centrifugal force disappears, the closing plate 52 closes the condensation pipe 17, and the gas collection bin 16 stops collecting. The invention utilizes the key connection arrangement to ensure that when the centrifugal bin 21 is positioned at the lowest position, the centrifugal shaft 22 is automatically separated from the first rotating shaft 42, and the closing plate 52 automatically seals the condensation pipe 17; during the rest of the time, the centrifugal shaft 22 is in keyed connection with the first rotating shaft 42, and drives not only the closing plate 52 to open the condensation duct 17, but also the pressure fan 41 and the condensation plate 43 to rotate.
The invention also provides a method for preparing n-propionaldehyde by carbon dioxide, which is suitable for the device for preparing n-propionaldehyde and mainly comprises the following steps:
s1: ethane and carbon dioxide are used as raw materials to prepare ethylene, then the ethylene is used as the raw material to react with carbon monoxide and hydrogen by using a oxo synthesis method under the participation of a catalyst, and the obtained liquid flow is introduced from a material inlet 15 of a low-pressure separation tank 11;
s2: the liquid flow enters a low-pressure separation tank 11 to carry out gas-liquid separation, the n-propionaldehyde in the liquid flow is gasified and enters a gas collection bin 16 through a condensation pipe 17 to be condensed and collected, and the liquid flow enters a liquid-liquid separation zone 13 through a communication port 24;
s3: the liquid flow is centrifugally separated by a centrifugal bin 21, the organic phase enters an organic phase collecting bin 19 to extract n-propionaldehyde, and the water phase enters a water phase collecting bin 18 to extract a catalyst;
s4: the n-propionaldehyde extracted from the organic phase collection bin 19 and the n-propionaldehyde collected by condensation in the gas collection bin 16 are the prepared n-propionaldehyde.
Claims (6)
1. The device for preparing n-propionaldehyde by using carbon dioxide is characterized in that: the device comprises a low-pressure separation tank (11), wherein the low-pressure separation tank (11) is divided into an upper gas-liquid separation zone (12) and a lower liquid-liquid separation zone (13), and the upper gas-liquid separation zone and the lower liquid-liquid separation zone are separated by a partition plate (14);
the gas-liquid separation zone (12) comprises a feeding port (15) and a gas collection bin (16) arranged at the top end of the low-pressure separation tank (11), and the gas collection bin (16) is communicated with the low-pressure separation tank (11) through a condensation pipe (17);
the liquid-liquid separation zone (13) comprises a centrifugal separation mechanism rotatably arranged in the center of the low-pressure separation tank (11), and a water phase collection bin (18) and an organic phase collection bin (19) which are arranged at the bottom end of the low-pressure separation tank (11); the centrifugal separation mechanism comprises a centrifugal bin (21) arranged in the low-pressure separation tank (11), a centrifugal shaft (22) is rotatably arranged at the middle shaft of the centrifugal bin (21), and centrifugal plates (23) are arranged at intervals in the circumferential direction of the centrifugal shaft (22); the bottom end of the centrifugal shaft (22) is externally connected with a driving mechanism; the water phase collecting bin (18) is used for collecting the solution in the middle of the centrifugal bin (21), and the organic phase collecting bin (19) is used for collecting the solution centrifugally thrown out by the centrifugal bin (21);
the partition plate (14) is funnel-shaped, and the bottom end of the partition plate (14) is provided with a communication port (24) for communicating the gas-liquid separation region (12) and the liquid-liquid separation region (13);
the bottom end of the centrifugal bin (21) is communicated with the water phase collecting bin (18) through a discharge pipe (25); a guide plate (26) is arranged on the peripheral edge of the upper end of the centrifugal bin (21), the guide plate (26) is obliquely arranged, and the lowest end of the guide plate (26) is communicated with the organic phase collection bin (19) through a guide pipe (27);
the centrifugal bin (21) is vertically and slidably mounted in the low-pressure separation tank (11), and the bottom end of the centrifugal shaft (22) is in key connection with the driving mechanism; along the sliding direction of the centrifugal bin (21), a compression spring (31) is arranged between the centrifugal bin (21) and the bottom plate of the low-pressure separation tank (11); the discharging pipe (25) and the guide pipe (27) are internally provided with closed units; the sealing unit is used for opening the discharge pipe (25) and the guide pipe (27) when the centrifugal bin (21) is located at the lowest position;
the sealing unit comprises a counter sink (32) arranged in the discharge pipe (25) and the guide pipe (27), a sealing plate (33) is vertically and slidably mounted in a large hole of the counter sink (32), a supporting column (34) is fixedly mounted below the sealing plate (33), and the diameter of the supporting column (34) is smaller than that of a small hole of the counter sink (32); the supporting column (34) is used for contacting the bottom surface of the low-pressure separation tank (11) when the centrifugal bin (21) is located at the lowest position, jacking the closing plate (33), and opening the discharge pipe (25) and the guide pipe (27); the bottom surface of the centrifugal bin (21) is also provided with a locking unit (35), the locking unit (35) is used for locking the centrifugal bin (21) and the low-pressure separation tank (11) when the closing plate (33) is opened, and the locking is released after the water phase collection bin (18) and the organic phase collection bin (19) are collected;
the upper part of the centrifugal shaft (22) is fixedly provided with a sealing block (51) for sealing the communication opening (24), and when the centrifugal bin (21) is located at the lowest position, the sealing block (51) seals the communication opening (24).
2. The apparatus for preparing n-propionaldehyde from carbon dioxide as claimed in claim 1, wherein: weighing units are arranged in the feeding port (15), the gas collecting bin (16), the water phase collecting bin (18) and the organic phase collecting bin (19).
3. The apparatus for preparing n-propionaldehyde from carbon dioxide as claimed in claim 2, wherein: condenser pipe (17) are provided with suction fan (41) with the junction of low pressure knockout drum (11), suction fan (41) rotate to be installed in condenser pipe (17), the middle part fixed mounting of suction fan (41) has first axis of rotation (42), the bottom of first axis of rotation (42) with the top key-type connection of centrifugal shaft (22).
4. The apparatus for producing n-propanal from carbon dioxide according to claim 3, wherein: the gas-liquid separation zone (12) is also rotatably provided with a condensing plate (43), and the condensing plate (43) is arranged at two ends of the condensing pipe (17); the condensing plate (43) is rotatably arranged on the inner wall of the low-pressure separation tank (11) through a second rotating shaft (44); and a worm wheel (45) is fixedly mounted on the second rotating shaft (44), and the worm wheel (45) is in transmission connection with a worm (46) fixedly mounted on the first rotating shaft (42).
5. The apparatus for preparing n-propionaldehyde from carbon dioxide as claimed in claim 4, wherein: the top end of the low-pressure separation tank (11) is also provided with a closing assembly for closing the condensation pipe (17), the closing assembly comprises a closing plate (52) which is slidably mounted at the top end of the low-pressure separation tank (11), and the closing plate (52) is used for isolating the communication between the condensation pipe (17) and the low-pressure separation tank (11); a driving spring (53) is arranged on the closing plate (52) and the low-pressure separation tank (11) along the sliding direction of the closing plate (52), and the driving spring (53) drives the closing plate (52) to close the condensation pipe (17); fixed mounting has swivel becket (54) on first axis of rotation (42), the circumference interval of swivel becket (54) is provided with dwang (55), the one end of dwang (55) articulates on swivel becket (54), and the vertical slidable mounting of the other end is on closing plate (33).
6. A method for preparing n-propionaldehyde by carbon dioxide, which is suitable for the device for preparing n-propionaldehyde in any one of claims 1 to 5, and is characterized in that: the method mainly comprises the following steps:
s1: ethane and carbon dioxide are used as raw materials to prepare ethylene, the ethylene is used as the raw material to react with carbon monoxide and hydrogen by using a oxo-synthesis method under the participation of a catalyst, and the obtained liquid flow is introduced from a feeding port (15) of a low-pressure separation tank (11);
s2: the liquid flow enters a low-pressure separation tank (11) and then undergoes gas-liquid separation, n-propionaldehyde in the liquid flow is gasified and enters a gas collection bin (16) through a condensation pipe (17) for condensation and collection, and the liquid flow enters a liquid-liquid separation zone (13) through a communication port (24);
s3: the liquid flow is centrifugally separated by a centrifugal bin (21), an organic phase enters an organic phase collecting bin (19) to extract n-propionaldehyde, and a water phase enters a water phase collecting bin (18) to extract a catalyst;
s4: the n-propionaldehyde extracted from the organic phase collection bin (19) and the n-propionaldehyde collected by condensation from the gas collection bin (16) are the prepared n-propionaldehyde.
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| JP2009262016A (en) * | 2008-04-23 | 2009-11-12 | Sharp Corp | Method of separating carbon dioxide and separating apparatus and washing apparatus |
| EP2263767A1 (en) * | 2009-06-17 | 2010-12-22 | M-I Epcon As | A separator tank for separating oil and gas from water |
| CN211912985U (en) * | 2020-03-13 | 2020-11-13 | 山东天力润滑油有限公司 | Gear oil processing multistage filter equipment |
| CN215505613U (en) * | 2021-05-24 | 2022-01-14 | 湖北瑞晟生物有限责任公司 | Oil-water separation device is used in aromatic plant production and processing |
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Denomination of invention: A device and method for preparing n-propanal from carbon dioxide Effective date of registration: 20231229 Granted publication date: 20230411 Pledgee: Bank of Nanjing Co.,Ltd. Nanjing Chengnan sub branch Pledgor: Nanjing RongXin Chemical Co.,Ltd. Registration number: Y2023980074754 |
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