CN115138303B - Device for preparing n-propyl acetate from carbon dioxide and preparation method thereof - Google Patents
Device for preparing n-propyl acetate from carbon dioxide and preparation method thereof Download PDFInfo
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- CN115138303B CN115138303B CN202210802883.2A CN202210802883A CN115138303B CN 115138303 B CN115138303 B CN 115138303B CN 202210802883 A CN202210802883 A CN 202210802883A CN 115138303 B CN115138303 B CN 115138303B
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- temperature reaction
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- reaction furnace
- carbon dioxide
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 76
- YKYONYBAUNKHLG-UHFFFAOYSA-N propyl acetate Chemical compound CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 39
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000006243 chemical reaction Methods 0.000 claims abstract description 77
- 239000003054 catalyst Substances 0.000 claims abstract description 70
- 230000008929 regeneration Effects 0.000 claims abstract description 42
- 238000011069 regeneration method Methods 0.000 claims abstract description 42
- 230000007246 mechanism Effects 0.000 claims abstract description 40
- 230000000694 effects Effects 0.000 claims abstract description 12
- 239000003610 charcoal Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000007789 gas Substances 0.000 claims description 64
- 239000002994 raw material Substances 0.000 claims description 35
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 14
- 238000009423 ventilation Methods 0.000 claims description 14
- 238000007789 sealing Methods 0.000 claims description 13
- 239000012495 reaction gas Substances 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000002073 nanorod Substances 0.000 claims description 6
- 230000008021 deposition Effects 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 230000001360 synchronised effect Effects 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 229910001868 water Inorganic materials 0.000 abstract description 5
- 230000009467 reduction Effects 0.000 abstract description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 6
- 239000005977 Ethylene Substances 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 4
- 210000001503 joint Anatomy 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 230000033001 locomotion Effects 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 240000009088 Fragaria x ananassa Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 235000007688 Lycopersicon esculentum Nutrition 0.000 description 1
- 240000008790 Musa x paradisiaca Species 0.000 description 1
- 240000003768 Solanum lycopersicum Species 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 235000021015 bananas Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 229940117927 ethylene oxide Drugs 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005839 oxidative dehydrogenation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 235000021012 strawberries Nutrition 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/02—Heat treatment
-
- 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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
-
- 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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
- B01J38/12—Treating with free oxygen-containing gas
- B01J38/16—Oxidation gas comprising essentially steam and oxygen
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/132—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group
- C07C29/136—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH
- C07C29/14—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring by reduction of an oxygen containing functional group of >C=O containing groups, e.g. —COOH of a —CHO group
-
- 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
- C07C45/505—Asymmetric hydroformylation
-
- 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
- C07C5/32—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with formation of free hydrogen
- C07C5/327—Formation of non-aromatic carbon-to-carbon double bonds only
- C07C5/333—Catalytic processes
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/08—Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
-
- 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
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/584—Recycling of catalysts
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a device for preparing n-propyl acetate from carbon dioxide in the field of carbon dioxide emission reduction and a preparation method thereof, and the device comprises a high-temperature reaction furnace, wherein the upper end of the high-temperature reaction furnace is provided with an air inlet mechanism, and the lower end of the high-temperature reaction furnace is provided with an air outlet; the high-temperature reaction furnace is rotationally provided with a hollow rotating clamping plate for bearing a catalyst, and the upper end and the lower end of the hollow rotating clamping plate are respectively connected with the upper end and the lower end of the regeneration mechanism; the regeneration mechanism is used for recovering the activity of the catalyst by adopting a charcoal burning regeneration mode. The invention can make the catalyst circulate in the high temperature reaction furnace and the regeneration mechanism, and the prepared high Wen Yixi gas is utilized to heat the catalyst in the regeneration mechanism, so that the catalyst reacts with the outside water-containing air to perform charcoal burning regeneration, the catalyst activity is recovered, the replacement of the catalyst is completed under the condition of no shutdown, and the production efficiency is improved.
Description
Technical Field
The invention belongs to the field of carbon dioxide emission reduction, and particularly relates to a device for preparing n-propyl acetate from carbon dioxide and a preparation method thereof.
Background
N-propyl acetate, naturally occurring in strawberries, bananas and tomatoes. The product, which can be obtained by esterification of acetic acid with 1-propanol, has typical properties of esters. Is colorless transparent liquid at normal temperature, is mutually soluble with ethanol and diethyl ether, has special fruit fragrance, is widely used as excellent solvent for paint, printing ink, nitrolacquer, varnish and various resins, and is also applied to the essence and spice industry. Carbon dioxide is the most dominant greenhouse gas and is also the most widely distributed and most abundant carbon-resource on earth. The prior method for preparing n-propyl acetate by using carbon dioxide comprises the steps of preparing ethylene by using ethylene and carbon dioxide as raw materials; reacting ethylene with carbon monoxide and hydrogen by using an oxo process to prepare n-propanal; reducing the obtained n-propanal into n-propanol; and reacting n-propanol with acetic acid to obtain n-propyl acetate through esterification. Wherein, when preparing ethylene by utilizing carbon dioxide and ethane, a process for preparing ethylene by oxidative dehydrogenation of ethane by carbon dioxide is used. The process requires the use of a catalyst to participate in the reaction at high temperatures. The catalyst loses activity under the action of long-time high temperature, so that the reaction rate is influenced, and the production efficiency is reduced. Therefore, there is a need for a device for preparing n-propyl acetate from carbon dioxide and a preparation method thereof, which solve the above problems.
The invention provides a device for preparing n-propyl acetate from carbon dioxide and a preparation method thereof, which enable a catalyst to circularly flow in a high-temperature reaction furnace and a regeneration mechanism, heat the catalyst in the regeneration mechanism by using the prepared high Wen Yixi gas, enable the catalyst to react with outside water-containing air to perform charcoal burning regeneration, recover the activity of the catalyst, complete the replacement of the catalyst under the condition of no shutdown, and improve the production efficiency.
Disclosure of Invention
The invention aims to provide a device for preparing n-propyl acetate from carbon dioxide and a preparation method thereof, which are used for solving the problems of the prior art in the background art.
In order to achieve the above purpose, the present invention provides the following technical solutions: the device for preparing n-propyl acetate from carbon dioxide comprises a high-temperature reaction furnace, wherein the upper end of the high-temperature reaction furnace is provided with an air inlet mechanism, and the lower end of the high-temperature reaction furnace is provided with an air outlet; the high-temperature reaction furnace is rotationally provided with a hollow rotating clamping plate for bearing a catalyst, and the upper end and the lower end of the hollow rotating clamping plate are respectively connected with the upper end and the lower end of the regeneration mechanism; the regeneration mechanism is used for recovering the activity of the catalyst by adopting a charcoal burning regeneration mode.
Preferably, the regeneration mechanism comprises a spiral conveying rod rotatably arranged in a ventilation bin, the ventilation bin is fixedly arranged beside the high-temperature reaction furnace, and the bin wall of the ventilation bin is communicated with the inside and outside air; the upper end and the lower end of the ventilation bin are respectively communicated with the upper end and the lower end of the hollow rotating clamping plate; the spiral conveying rod is a hollow rod, a hollow conveying pipeline is arranged in the spiral conveying rod, and the hollow conveying pipeline is communicated with an air outlet of the high-temperature reaction furnace.
Preferably, the upper end and the lower end of the regeneration mechanism are connected with the upper end and the lower end of the hollow rotating clamping plate through obliquely arranged material conveying pipelines; the upper end of the regeneration mechanism is higher than the upper end of the hollow rotating clamping plate, and the lower end of the regeneration mechanism is lower than the lower end of the hollow rotating clamping plate.
Preferably, the gas inlet mechanism comprises a gas inlet arranged at the upper end of the high-temperature reaction furnace, a four-way pipe is arranged at the gas inlet, one end interface of the four-way pipe is connected with the gas inlet, two adjacent horizontal end interfaces are respectively connected with a carbon dioxide input device and an ethane input device, and a stamping component is arranged at a corresponding vertical end interface; the stamping assembly comprises a vertical piston which is slidably mounted along the extending direction of the vertical interface, and a hinge shaft is arranged at one end of the vertical piston, which is far away from the air inlet; the upper end of the high-temperature reaction furnace is provided with a crankshaft externally connected with a driving source, and the crankshaft is hinged with the vertical piston through a hinge shaft.
Preferably, horizontal pistons are horizontally arranged in the interfaces at the two horizontal ends, and one end of each horizontal piston, which is far away from the air inlet, is hinged with a swing rod; the middle part of the swing rod is hinged on the high-temperature reaction furnace, the lower end of the swing rod is hinged with the horizontal piston, and the upper end of the swing rod is connected with the crankshaft through a connecting rod; when the horizontal piston is positioned at the limit position far away from the air inlet, the vertical piston is positioned at the limit position close to the air inlet; when the horizontal piston is positioned at the limit position close to the air inlet, the vertical piston is positioned at the limit position far away from the air inlet.
Preferably, the connectors at the two horizontal ends are hinged with an opening plate near the air inlet, and the opening plate is opened and closed towards the direction near one side of the air inlet.
Preferably, the cross-sectional area ratio of the interfaces at the two horizontal ends is 16:9.
Preferably, a sealing opening used for communicating the four-way pipe with the inside of the high-temperature reaction furnace is arranged at the joint of the four-way pipe connected with the air inlet, a sealing block is fixedly arranged on the vertical piston, the vertical piston is positioned at the limit position close to the air inlet, and the sealing opening is opened.
Preferably, the lower end of the vertical piston is fixedly provided with a telescopic shaft, and the sealing block is fixedly arranged on the telescopic shaft; a rotating plate is rotatably arranged on the sealing opening and is in threaded connection with the telescopic shaft; the rotating plate is provided with a grating-shaped through hole.
Preferably, the telescopic shaft extends to the bottom end of the high-temperature reaction furnace, and the hollow rotating clamping plate is in threaded connection with the telescopic shaft.
Preferably, the bottom end of the telescopic shaft is provided with a pawl, a ratchet wheel is arranged beside the pawl, and the ratchet wheel is rotatably arranged on the bottom surface of the high-temperature reaction furnace; the ratchet wheel is in transmission connection with the spiral conveying rod through a bevel gear set and a synchronous belt.
The invention also provides a method for preparing n-propyl acetate by using carbon dioxide, which is suitable for the device for preparing n-propyl acetate, and comprises the following main steps:
s1: putting the catalyst nanorod catalyst into a hollow rotating clamping plate, starting an external driving power supply to drive a crankshaft to rotate, rotating the hollow rotating clamping plate and a spiral conveying rod, and enabling the catalyst to start flowing in a high-temperature reaction furnace and a regeneration mechanism;
s2: carbon dioxide and ethane are respectively introduced from the interfaces at the two horizontal ends of the four-way pipe, and the horizontal piston extrudes raw material gas into the gas inlet according to a preset proportion;
s3: the vertical piston stirs, compresses and mixes the raw material gas at the gas inlet and then squeezes the raw material gas into the high-temperature reaction furnace;
s4: discharging the reaction gas after the high-temperature reaction from the gas outlet, conveying the reaction gas to be cooled through a hollow conveying pipe, and conveying the reaction gas to the next working procedure;
s5: when the temperature of the reaction gas is reduced through the hollow conveying pipe, the catalyst conveyed by the spiral conveying rod is heated, and the catalyst reacts with the outside air containing water vapor at a high temperature state, so that the catalyst is regenerated by removing carbon deposition.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention can make the catalyst circulate in the high temperature reaction furnace and the regeneration mechanism, and the prepared high Wen Yixi gas is utilized to heat the catalyst in the regeneration mechanism, so that the catalyst reacts with the outside water-containing air to perform charcoal burning regeneration, the catalyst activity is recovered, the replacement of the catalyst is completed under the condition of no shutdown, and the production efficiency is improved.
2. When the carbon dioxide and the ethane are extruded into the four-way pipe according to the proportion, the carbon dioxide and the ethane are compressed, mixed and stirred, and extruded into the high-temperature reaction furnace for reaction, so that the raw material gas can be fully mixed and contacted, and the reaction rate is improved. According to the invention, the crankshaft rotates to drive the vertical piston to press raw material gas into the high-temperature reaction furnace, and the vertical piston drives the rotating plate and the hollow rotating clamping plate to repeatedly rotate simultaneously through the vertical reciprocating motion of the vertical piston with the telescopic shaft, so that the power source is saved, and the reaction rate is improved. The repeated rotation of the hollow rotating clamping plate agitates the raw material gas in the high temperature reaction furnace on one hand, so that the raw material gas is fully contacted with the catalyst, and the reaction rate is improved; on the other hand, the flow of the catalyst can be promoted, and the catalyst is prevented from blocking in the hollow rotating clamping plate.
3. The telescopic shaft can drive the rotating plate and the hollow rotating clamping plate to repeatedly rotate, and can also provide power for the spiral rotating rod, so that a power source is saved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed for the description of the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic structural diagram of an apparatus for preparing n-propyl acetate from carbon dioxide according to the present invention;
FIG. 2 is a schematic diagram of the apparatus for preparing n-propyl acetate according to the present invention in a cross-sectional view;
FIG. 3 is an enlarged partial schematic view of portion A of FIG. 2 in accordance with the present invention;
FIG. 4 is a partially enlarged schematic illustration of portion B of FIG. 2 in accordance with the present invention;
FIG. 5 is an enlarged partial schematic view of portion C of FIG. 2 in accordance with the present invention;
FIG. 6 is a schematic view of the top punch assembly of the high temperature reactor of the present invention;
FIG. 7 is a schematic view of the structure of the bottom of the high temperature reactor of the present invention;
FIG. 8 is a process flow diagram of a method for preparing n-propyl acetate from carbon dioxide according to the present invention.
In the drawings, the list of components represented by the various numbers is as follows:
11-high temperature reaction furnace, 12-gas outlet, 13-hollow rotating clamping plate, 14-ventilation bin, 15-spiral conveying rod, 16-hollow conveying pipe, 17-conveying pipeline, 21-gas inlet, 22-four-way pipe, 23-carbon dioxide conveying device, 24-ethane conveying device, 25-vertical piston, 26-hinging shaft, 27-crankshaft, 28-horizontal piston, 29-swinging rod, 30-connecting rod, 31-opening and closing plate, 41-closing opening, 42-closing block, 51-telescopic shaft, 52-rotating plate, 53-through hole, 61-pawl, 62-ratchet wheel, 63-bevel gear set and 64-synchronous belt.
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.
Referring to fig. 1-8, a device for preparing n-propyl acetate from carbon dioxide comprises a high-temperature reaction furnace 11, wherein an air inlet mechanism is arranged at the upper end of the high-temperature reaction furnace 11, and an air outlet 12 is arranged at the lower end of the high-temperature reaction furnace 11; a hollow rotating clamping plate 13 for bearing a catalyst is rotatably arranged in the high-temperature reaction furnace 11, and the upper end and the lower end of the hollow rotating clamping plate 13 are respectively connected with the upper end and the lower end of a regeneration mechanism; the regeneration mechanism is used for recovering the activity of the catalyst by adopting a charcoal burning regeneration mode.
Preferably, the regeneration mechanism comprises a spiral conveying rod 15 rotatably arranged in a ventilation bin 14, the ventilation bin 14 is fixedly arranged beside the high-temperature reaction furnace 11, and the bin wall of the ventilation bin is communicated with the inside and outside air; the upper end and the lower end of the ventilation bin 14 are respectively communicated with the upper end and the lower end of the hollow rotating clamping plate 13; the screw conveying rod 15 is a hollow rod, a hollow conveying pipe 16 is arranged in the hollow conveying rod, and the hollow conveying pipe 16 is communicated with the air outlet 12 of the high-temperature reaction furnace 11.
Preferably, the upper end and the lower end of the regeneration mechanism are connected with the upper end and the lower end of the hollow rotating clamping plate 13 through a material conveying pipeline 17 which is obliquely arranged; the upper end of the regeneration mechanism is higher than the upper end of the hollow rotating clamping plate 13, and the lower end of the regeneration mechanism is lower than the lower end of the hollow rotating clamping plate 13.
The catalyst of the invention adopts a nano rod catalyst, and the nano material has high catalytic activity due to the characteristics of high specific surface energy, high surface defect and the like. It has been found by analysis that when a nanorod catalyst is adopted, the main reason for catalyst deactivation is surface carbon deposition, and the activity of the catalyst can be recovered by adopting a charcoal burning regeneration mode. As shown in fig. 1 and 2, raw material gases of carbon dioxide and ethane are extruded into a high-temperature reaction furnace 11 through a gas inlet mechanism, and react under high-temperature conditions in the presence of a catalyst to generate ethylene. As shown in fig. 2 and 3, the generated high Wen Yixi enters the hollow conveying pipe 16 through the air outlet 12 at the bottom end of the high-temperature reaction furnace 11, and the high Wen Yixi radiates heat during the conveying process, so that the catalyst on the spiral blades of the spiral conveying rod 15 is heated. Because the ventilation bin 14 has the bin wall ventilated, the outside is air containing water vapor, at the moment, the catalyst is heated and reacts with water and oxygen, carbon deposit on the catalyst is discharged by carbon burning, the catalyst recovers activity, and the catalyst flows into the hollow rotating clamping plate 13 again to be catalyzed. The invention puts the catalyst nano rod catalyst into the hollow rotating clamping plate 13, starts the external driving power supply to drive the crankshaft 27 to rotate, the hollow rotating clamping plate 13 and the spiral conveying rod 15 rotate, and the catalyst starts to flow in the high-temperature reaction furnace 11 and the regeneration mechanism. The catalyst flows in the hollow rotating clamping plate 13, so that the contact area with the raw material gas is increased, and the catalytic speed is improved. The catalyst flows from the upper end to the lower end of the hollow rotating clamping plate 13 due to self gravity, enters the bottom end of the spiral conveying rod 15 through the obliquely arranged conveying pipeline 17, is conveyed to the top end in a spiral mode and burns carbon to restore activity, and then enters the hollow clamping plate again. The invention can make the catalyst circulate in the high temperature reaction furnace 11 and the regeneration mechanism, and the prepared high Wen Yixi gas is utilized to heat the catalyst in the regeneration mechanism, so that the catalyst reacts with the outside water-containing air to perform charcoal burning regeneration, the catalyst activity is recovered, the replacement of the catalyst is completed under the condition of no shutdown, and the production efficiency is improved.
Preferably, the gas inlet mechanism comprises a gas inlet 21 arranged at the upper end of the high-temperature reaction furnace 11, a four-way pipe 22 is arranged at the gas inlet 21, one end interface of the four-way pipe 22 is connected with the gas inlet 21, two adjacent horizontal end interfaces are respectively connected with a carbon dioxide input device 23 and an ethane input device 24, and a stamping assembly is arranged at a corresponding vertical end interface; the punching assembly comprises a vertical piston 25 which is slidably mounted along the extension direction of the vertical interface, and a hinge shaft 26 is arranged at one end of the vertical piston 25 away from the air inlet 21; the upper end of the high temperature reaction furnace 11 is provided with a crankshaft 27 externally connected with a driving source, and the crankshaft 27 is hinged with the vertical piston 25 through a hinge shaft 26.
Preferably, horizontal pistons 28 are horizontally arranged in the interfaces at the two horizontal ends, and one end, far away from the air inlet 21, of each horizontal piston 28 is hinged with a swing rod 29; the middle part of the swing rod 29 is hinged on the high-temperature reaction furnace 11, the lower end of the swing rod is hinged with the horizontal piston 28, and the upper end of the swing rod is connected with the crankshaft 27 through the connecting rod 30; when the horizontal piston 28 is positioned at the limit position far away from the air inlet 21, the vertical piston 25 is positioned at the limit position close to the air inlet 21; when the horizontal piston 28 is positioned at the limit position close to the air inlet 21, the vertical piston 25 is positioned at the limit position far away from the air inlet 21.
Preferably, the two horizontal end interfaces are hinged with an opening and closing plate 31 near the air inlet 21, and the opening and closing plate 31 is opened and closed towards the direction near the air inlet 21.
The raw material gases of the invention are carbon dioxide and ethane, which need to be fully mixed and fully contacted to improve the reaction rate. The present invention mixes the carbon dioxide and ethane when they are proportionally extruded into the four-way pipe 22, and then extrudes them into the high temperature reaction furnace 11 for reaction. As shown in fig. 2 and 5, the raw material gases of carbon dioxide and ethane are respectively extruded into the horizontal two-end ports of the four-way pipe 22, and at this time, the horizontal piston 28 is positioned at the limit position far from the air inlet 21, and the vertical piston 25 is positioned at the limit position near to the air inlet 21. The crankshaft 27 rotates under the action of an external driving source, and drives the horizontal piston 28 to horizontally reciprocate through the connecting rod 30 and the swinging rod 29. The horizontal pistons 28 at the two ends move towards each other to squeeze the raw material gas entering the joints of the two horizontal ends towards the middle, and squeeze the raw material gas into the joints of the middle of the four-way pipe 22. As shown in fig. 4, in the process of moving the horizontal piston 28 in opposite directions, because of the air pressure extrusion, the opening and closing plate 31 positioned at the joint of the two horizontal ends and close to the air inlet 21 is opened to allow the raw material gas to enter the middle joint of the four-way pipe 22 for mixing, and at the moment, the vertical piston 25 also moves upwards under the action of the crankshaft 27 to provide space for the raw material gas, so that the raw material gas is ensured to completely enter the middle joint of the four-way pipe 22 and not to remain in the joint of the two horizontal ends due to the air pressure. Then the vertical piston 25 moves downwards under the action of the crankshaft 27 to extrude the gas into the high-temperature reaction furnace 11, the horizontal pistons 28 at the two ends start to move in opposite directions, and the opening and closing plate 31 is closed under the action of air pressure to prevent the raw gas from reentering the interfaces at the two horizontal ends.
Preferably, the cross-sectional area ratio of the interfaces at the two horizontal ends is 16:9. If the feeding amount is unbalanced, the reaction of the raw material gas is incomplete, and the purity of the generated gas is affected. In order to ensure the accuracy of the feeding amount and improve the production efficiency as much as possible, the feeding amount is set according to the proportion of 16:9 of a reaction equation, and the cross-sectional area ratio of the interfaces at the two horizontal ends is 16:9.
Preferably, a sealing opening 41 for communicating the four-way pipe 22 with the inside of the high-temperature reaction furnace 11 is arranged at the interface of the four-way pipe 22 and the air inlet 21, a sealing block 42 is fixedly arranged on the vertical piston 25, the vertical piston 25 is positioned at the limit position close to the air inlet 21, and the sealing opening 41 is opened. In order to ensure that the two raw materials gases can be fully mixed at the middle junction of the four-way pipe 22, the invention firstly performs compression mixing when the raw materials gases are pressed into the high-temperature reaction furnace 11 from the middle junction of the four-way pipe 22. As shown in fig. 4, the raw material gas in the four-way pipe 22 of the present invention is required to pass through the closed port 41 to enter the high temperature reaction furnace 11. Immediately after the vertical piston 25 starts to move downward, the closing port 41 is closed by the closing block 42, and at this time, the two raw material gases are compressed, promoting mixing. When the vertical piston 25 moves down to the limit position, the closing block 42 moves down to the limit position to just open the opening and closing port 41, and the raw material gas enters the high temperature reaction wheel. When the vertical piston 25 is returned upward, the closing block 42 immediately closes the closing port 41.
Preferably, a telescopic shaft 51 is fixedly arranged at the lower end of the vertical piston 25, and the sealing block 42 is fixedly arranged on the telescopic shaft 51; a rotating plate 52 is rotatably arranged on the closed port 41, and the rotating plate 52 is in threaded connection with the telescopic shaft 51; the rotating plate 52 is provided with a fence-shaped through hole 53. To further ensure that the two feed gases are thoroughly mixed and in sufficient contact at the intermediate junction of the four-way pipe 22. The invention compresses and mixes the raw material gas and simultaneously stirs and mixes the raw material gas. As shown in fig. 4, when the vertical piston 25 moves downward to compress the raw material gas, the telescopic shaft 51 fixedly arranged at the bottom end of the vertical piston 25 moves downward, and the telescopic shaft 51 moves downward to drive the rotating plate 52 in threaded connection with the telescopic shaft to rotate on the sealing port 41, so that the raw material gas positioned at the middle junction of the four-way pipe 22 is stirred and mixed.
Preferably, the telescopic shaft 51 extends to the bottom end of the high-temperature reaction furnace 11, and the hollow rotating clamping plate 13 is in threaded connection with the telescopic shaft 51. As shown in fig. 2, the telescopic shaft 51 of the present invention vertically reciprocates along with the vertical piston 25, and the hollow rotating clamping plate 13 which is screw-coupled thereto also repeatedly rotates, so that on one hand, the raw material gas in the high temperature reaction furnace 11 is agitated to be fully contacted with the catalyst, thereby improving the reaction rate; on the other hand, the repeated rotation of the hollow rotating clamping plate 13 can also promote the flow of the catalyst and prevent the catalyst from blocking materials in the hollow rotating clamping plate 13. According to the invention, the crankshaft 27 rotates to drive the vertical piston 25 to press raw material gas into the high-temperature reaction furnace 11, and the vertical piston 25 drives the telescopic shaft 51 to vertically reciprocate and simultaneously drive the rotating plate 52 and the hollow rotating clamping plate 13 to rotate, so that the power source is saved.
Preferably, a pawl 61 is arranged at the bottom end of the telescopic shaft 51, a ratchet wheel 62 is arranged beside the pawl 61, and the ratchet wheel 62 is rotatably arranged on the bottom surface of the high-temperature reaction furnace 11; the ratchet wheel 62 is in transmission connection with the screw conveying rod 15 through a bevel gear set 63 and a synchronous belt 64. The vertical reciprocating movement of the telescopic shaft 51 not only can drive the rotating plate 52 and the hollow rotating clamping plate 13 to rotate repeatedly, but also can provide power for the spiral rotating rod. As shown in fig. 5 and 7, when the telescopic shaft 51 of the invention vertically reciprocates, the ratchet wheel 62 can only rotate unidirectionally by the arrangement of the pawl 61 and the ratchet wheel 62, and then the ratchet wheel 62 is transmitted to the screw conveying rod 15 by the bevel gear group 63 and the synchronous belt 64 to drive the screw conveying rod 15 to rotate unidirectionally, so that the catalyst is conveyed upwards, and the power source is saved.
The invention also provides a method for preparing n-propyl acetate by using carbon dioxide, which is suitable for the device for preparing n-propyl acetate, and comprises the following main steps:
s1: putting the catalyst nano rod catalyst into a hollow rotating clamping plate 13, starting an external driving power supply to drive a crankshaft 27 to rotate, rotating the hollow rotating clamping plate 13 and a spiral conveying rod 15, and starting the catalyst to flow in a high-temperature reaction furnace 11 and a regeneration mechanism;
s2: carbon dioxide and ethane are respectively introduced from the interfaces at the two horizontal ends of the four-way pipe 22, and the horizontal piston 28 extrudes raw material gas into the gas port 21 according to a preset proportion;
s3: the vertical piston 25 stirs and compresses the raw material gas at the gas inlet 21, and squeezes the raw material gas into the high-temperature reaction furnace 11;
s4: the reaction gas after the high-temperature reaction is discharged from the gas outlet 12, is conveyed and cooled through the hollow conveying pipe 16 and is conveyed to the next working procedure;
s5: when the temperature of the reaction gas is reduced through the hollow conveying pipe 16, the catalyst conveyed by the spiral conveying rod 15 is heated, and the catalyst reacts with the air containing water vapor outside in a high-temperature state, so that the catalyst is regenerated by removing carbon deposition.
Claims (6)
1. The utility model provides a device of carbon dioxide preparation acetic acid n-propyl ester which characterized in that: the device comprises a high-temperature reaction furnace (11), wherein the upper end of the high-temperature reaction furnace (11) is provided with an air inlet mechanism, and the lower end of the high-temperature reaction furnace is provided with an air outlet (12); a hollow rotating clamping plate (13) for bearing a catalyst is rotatably arranged in the high-temperature reaction furnace (11), and the upper end and the lower end of the hollow rotating clamping plate (13) are respectively connected with the upper end and the lower end of the regeneration mechanism; the regeneration mechanism is used for recovering the activity of the catalyst by adopting a charcoal burning regeneration mode;
the regeneration mechanism comprises a spiral conveying rod (15) rotatably arranged in a ventilation bin (14), the ventilation bin (14) is fixedly arranged beside the high-temperature reaction furnace (11), and the bin wall of the ventilation bin is communicated with the inside and outside air; the upper end and the lower end of the ventilation bin (14) are respectively communicated with the upper end and the lower end of the hollow rotating clamping plate (13); the spiral conveying rod (15) is a hollow rod, a hollow conveying pipe (16) is arranged in the hollow conveying rod, and the hollow conveying pipe (16) is communicated with an air outlet (12) of the high-temperature reaction furnace (11);
the gas inlet mechanism comprises a gas inlet (21) formed in the upper end of the high-temperature reaction furnace (11), a four-way pipe (22) is arranged at the gas inlet (21), one end interface of the four-way pipe (22) is connected with the gas inlet (21), two adjacent horizontal end interfaces are respectively connected with a carbon dioxide input device (23) and an ethane input device (24), and a stamping assembly is arranged at a corresponding vertical end interface; the stamping assembly comprises a vertical piston (25) which is slidably mounted along the extension direction of the vertical interface, and a hinge shaft (26) is arranged at one end of the vertical piston (25) far away from the air inlet (21); the upper end of the high-temperature reaction furnace (11) is provided with a crankshaft (27) externally connected with a driving source, and the crankshaft (27) is hinged with the vertical piston (25) through a hinge shaft (26);
a horizontal piston (28) is horizontally arranged in the interfaces at the two horizontal ends, and one end, far away from the air inlet (21), of the horizontal piston (28) is hinged with a swing rod (29); the middle part of the swing rod (29) is hinged on the high-temperature reaction furnace (11), the lower end of the swing rod is hinged with the horizontal piston (28), and the upper end of the swing rod is connected with the crankshaft (27) through the connecting rod (30); when the horizontal piston (28) is positioned at the limit position far away from the air inlet (21), the vertical piston (25) is positioned at the limit position close to the air inlet (21); when the horizontal piston (28) is positioned at the limit position close to the air inlet (21), the vertical piston (25) is positioned at the limit position far away from the air inlet (21);
the connectors at the two horizontal ends are hinged with an opening plate (31) close to the air inlet (21), and the opening plate (31) is opened and closed towards the direction close to one side of the air inlet (21);
the sealing block (42) is fixedly arranged on the vertical piston (25), the vertical piston (25) is positioned at the limit position close to the air inlet (21), and the sealing port (41) is opened;
the lower end of the vertical piston (25) is fixedly provided with a telescopic shaft (51), and the sealing block (42) is fixedly arranged on the telescopic shaft (51); a rotating plate (52) is rotatably arranged on the closed opening (41), and the rotating plate (52) is in threaded connection with the telescopic shaft (51); the rotating plate (52) is provided with a fence-shaped through hole (53).
2. The apparatus for preparing n-propyl acetate from carbon dioxide as set forth in claim 1, wherein: the upper end and the lower end of the regeneration mechanism are connected with the upper end and the lower end of the hollow rotating clamping plate (13) through obliquely arranged material conveying pipelines (17); the upper end of the regeneration mechanism is higher than the upper end of the hollow rotating clamping plate (13), and the lower end of the regeneration mechanism is lower than the lower end of the hollow rotating clamping plate (13).
3. The apparatus for preparing n-propyl acetate from carbon dioxide according to claim 2, wherein: the cross-sectional area ratio of the interfaces at the two horizontal ends is 16:9.
4. A device for preparing n-propyl acetate from carbon dioxide as claimed in claim 3, wherein: the telescopic shaft (51) extends to the bottom end of the high-temperature reaction furnace (11), and the hollow rotating clamping plate (13) is in threaded connection with the telescopic shaft (51).
5. The apparatus for preparing n-propyl acetate from carbon dioxide as set forth in claim 4, wherein: a pawl (61) is arranged at the bottom end of the telescopic shaft (51), a ratchet wheel (62) is arranged beside the pawl (61), and the ratchet wheel (62) is rotatably arranged on the bottom surface of the high-temperature reaction furnace (11); the ratchet wheel (62) is in transmission connection with the spiral conveying rod (15) through a bevel gear set (63) and a synchronous belt (64).
6. A method for preparing n-propyl acetate by carbon dioxide, which is suitable for the device for preparing n-propyl acetate according to any one of claims 1-5, and is characterized in that: the method mainly comprises the following steps:
s1: putting the nano rod catalyst into a hollow rotating clamping plate (13), starting an external driving power supply to drive a crankshaft (27) to rotate, rotating the hollow rotating clamping plate (13) and a spiral conveying rod (15), and enabling the catalyst to start flowing in a high-temperature reaction furnace (11) and a regeneration mechanism;
s2: carbon dioxide and ethane are respectively introduced from the interfaces at the two horizontal ends of the four-way pipe (22), and raw material gas is extruded into the air inlet (21) by the horizontal piston (28) according to a preset proportion;
s3: the vertical piston (25) stirs and compresses the raw material gas at the gas inlet (21) and squeezes the raw material gas into the high-temperature reaction furnace (11);
s4: the reaction gas after the high-temperature reaction is discharged from the gas outlet (12), is conveyed and cooled through the hollow conveying pipe (16), and is conveyed to the next working procedure;
s5: when the temperature of the reaction gas is reduced through the hollow conveying pipe (16), the catalyst conveyed by the spiral conveying rod (15) is heated, the catalyst reacts with the air containing water vapor outside at a high temperature state, and carbon deposition is removed from the catalyst for regeneration.
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| GB528919A (en) * | 1938-10-12 | 1940-11-11 | Standard Oil Dev Co | Improvements in and relating to catalytic reaction apparatus |
| FR2780316A1 (en) * | 1998-06-24 | 1999-12-31 | Inst Francais Du Petrole | Regeneration of particulate catalysts used for reforming, paraffin isomerization and dehydrogenation |
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Denomination of invention: A device for preparing n-propyl acetate from carbon dioxide and its preparation method Effective date of registration: 20231229 Granted publication date: 20230822 Pledgee: Bank of Nanjing Co.,Ltd. Nanjing Chengnan sub branch Pledgor: Nanjing RongXin Chemical Co.,Ltd. Registration number: Y2023980074754 |
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