CN118253262B - Reaction device for preparing methyl acetate by dimethyl ether carbonylation - Google Patents
Reaction device for preparing methyl acetate by dimethyl ether carbonylation Download PDFInfo
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- CN118253262B CN118253262B CN202410672706.6A CN202410672706A CN118253262B CN 118253262 B CN118253262 B CN 118253262B CN 202410672706 A CN202410672706 A CN 202410672706A CN 118253262 B CN118253262 B CN 118253262B
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- dimethyl ether
- methyl acetate
- carbonylation
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 93
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 238000005810 carbonylation reaction Methods 0.000 title claims abstract description 31
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 title claims abstract description 25
- KXKVLQRXCPHEJC-UHFFFAOYSA-N acetic acid trimethyl ester Natural products COC(C)=O KXKVLQRXCPHEJC-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 230000006315 carbonylation Effects 0.000 title claims abstract description 24
- 230000003197 catalytic effect Effects 0.000 claims abstract description 112
- 238000002156 mixing Methods 0.000 claims abstract description 68
- 238000012544 monitoring process Methods 0.000 claims abstract description 41
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 30
- 239000002131 composite material Substances 0.000 claims abstract description 12
- 239000000945 filler Substances 0.000 claims description 31
- 238000009834 vaporization Methods 0.000 claims description 16
- 230000008016 vaporization Effects 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000007789 sealing Methods 0.000 claims description 13
- 230000001681 protective effect Effects 0.000 claims description 10
- 238000001228 spectrum Methods 0.000 claims description 10
- 238000007599 discharging Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 238000005728 strengthening Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 12
- 238000012856 packing Methods 0.000 abstract description 9
- 239000007789 gas Substances 0.000 description 93
- 229920006395 saturated elastomer Polymers 0.000 description 13
- 238000010521 absorption reaction Methods 0.000 description 11
- 239000012495 reaction gas Substances 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 229910002091 carbon monoxide Inorganic materials 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000011157 data evaluation Methods 0.000 description 3
- 230000005389 magnetism Effects 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 238000003331 infrared imaging Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 210000001503 joint Anatomy 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000003351 stiffener Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000009849 deactivation Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052680 mordenite Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000011218 segmentation Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 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
- B01J8/001—Controlling catalytic processes
-
- 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
- B01J8/0015—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor
- B01J8/002—Feeding of the particles in the reactor; Evacuation of the particles out of the reactor with a moving instrument
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0278—Feeding reactive fluids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/36—Preparation of carboxylic acid esters by reaction with carbon monoxide or formates
- C07C67/37—Preparation of carboxylic acid esters by reaction with carbon monoxide or formates by reaction of ethers with carbon monoxide
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a reaction device for preparing methyl acetate by dimethyl ether carbonylation, which belongs to the technical field of dimethyl ether carbonylation treatment, and is characterized in that a rotary disk with four catalytic beds is rotatably arranged between a pair of reaction towers, wherein two catalytic beds are positioned outside the pair of reaction towers and serve as standby reaction beds, in the reaction process, a sectional feeding mode is adopted to ensure that the mixing degree and the temperature of mixed gas entering a catalytic reaction part reach the standard, the inner and outer distribution positions of the two groups of catalytic beds are exchanged according to a preset monitoring period, the saturation degree of catalytic packing after the reaction is monitored by utilizing a composite monitoring mechanism and is used as a judging factor for whether the catalytic packing needs to be replaced or not, and compared with the traditional mode of switching standby reactors, the continuous reaction is ensured, the original catalytic reaction environment is not changed, in addition, the internal and external catalytic bed exchange process is not required to be opened, and the replacement is simpler.
Description
Technical Field
The invention relates to the technical field of dimethyl ether carbonylation treatment, in particular to a reaction device for preparing methyl acetate by dimethyl ether carbonylation.
Background
Dimethyl ether is an environment-friendly fuel, has wide application prospect in the field of clean energy, can be converted into chemicals with high added value through carbonylation reaction, comprises methyl acetate, and is widely applied to the fields of chemical industry, medicine, pesticide and the like.
In the carbonylation of dimethyl ether, the performance of the catalyst is one of the key factors, and directly influences the reaction rate, the product selectivity and the quality of the product. The dimethyl ether is gasified and then mixed with CO to enter a carbonylation reactor, methyl acetate is generated through carbonylation reaction, separated methyl acetate reacts with hydrogen in a hydrogenation reactor to obtain ethanol and methanol, the separated ethanol is used as a product for sale, and the methanol is returned to a dimethyl ether synthesis unit to be used as a raw material.
At present, methyl acetate is prepared by a dimethyl ether carbonylation method mainly by using mordenite molecular sieve as a catalyst, but the catalyst is fast in deactivation and poor in stability. The catalyst needs to be replaced frequently in the process of preparing the methyl acetate, so that the operation is complicated, the carbonylation reaction is interrupted in the process of replacing the catalyst, and the methyl acetate cannot be continuously produced for a long time, so that certain defects exist. In order to realize that the carbonylation reaction is not interrupted in the process of replacing the catalyst, the existing standby reactor is switched to ensure that the carbonylation reaction is continuously carried out, but the original carbonylation reaction environment is directly exchanged in the mode, the standby reactor needs to be timely adjusted to a proper reaction parameter, and the continuous implementation of the carbonylation reaction is not facilitated due to the difference of the current and the later reaction environments; in addition, the reactants are generally directly introduced when raw materials are supplied, the temperature and the mixing degree of the reactants when the reactants enter the carbonylation reactor are not well controlled, and the high-efficiency conversion of the products is not facilitated.
To this end, we have proposed a reaction apparatus for preparing methyl acetate by carbonylation of dimethyl ether, aiming at the above problems.
Disclosure of Invention
Compared with the prior art, the invention provides a reaction device for preparing methyl acetate by dimethyl ether carbonylation, which is characterized in that a rotating disk with four catalytic beds is rotatably arranged between a pair of reaction towers, wherein two catalytic beds are positioned outside the pair of reaction towers and serve as standby reaction beds, in the reaction process, the mixed degree and the temperature of mixed gas entering a catalytic reaction part are ensured to reach the standard in a sectional feeding mode, the inner and outer distribution positions of the two groups of catalytic beds are exchanged in a preset monitoring period, the saturation degree of the reacted catalytic packing is monitored by utilizing a composite monitoring mechanism and used as a judging factor for whether the reaction is needed to be replaced or not, and the mode of quickly rotating and exchanging the catalytic beds is adopted.
The aim of the invention can be achieved by the following technical scheme:
The reaction device for preparing methyl acetate by dimethyl ether carbonylation comprises a bearing structure and reaction towers embedded and arranged on the left side and the right side of the bearing structure, wherein a gas mixing box with an exhaust valve at one side of the bottom end is arranged at the top end of the reaction tower, a heating vaporization tank with a dimethyl ether feeding pipe at the top end is arranged above a pair of reaction towers, a conveying pipe connected with the top ends of the pair of gas mixing boxes is fixed at the bottom end of the heating vaporization tank, and an air inlet pipe is externally connected to the gas mixing box;
The catalytic reaction device is characterized in that the reaction tower is arranged below the gas mixing box, a catalytic reaction part is arranged inside the reaction tower and is provided with a pair of rotary grooves on opposite end walls of the catalytic reaction part, a catalytic carrier which rotates based on the center of a bearing structure is embedded between the pair of rotary grooves, the catalytic carrier comprises a rotary disk which is rotatably arranged between the pair of rotary grooves, four embedded grooves are uniformly formed in the rotary disk along the circumferential direction of the rotary disk, a catalytic bed filled with catalytic filler is embedded inside each embedded groove, and a discharge pipe is externally connected to the bottom end of the reaction tower;
the composite monitoring mechanism used for acquiring the saturation of the catalytic filler is arranged in the front-back direction of the supporting structure, and consists of a spectrum monitoring system and a weight monitoring system which are arranged up and down.
Further, the bearing structure comprises a lower bearing bracket and an upper bearing table, and the bottoms of the upper bearing table and the lower bearing bracket are of circular structures taking the middle points of a pair of reaction towers as circle centers.
Further, a second driving motor is fixedly installed in the middle of the top end of the upper bearing table, and the second driving end of the driving motor penetrates through the bottom end of the circle center of the rotating disc and is fixedly installed.
Further, the conveyer pipe is the three-way pipe, the tip of conveyer pipe connection gas mixing case one side is equipped with one section reservation portion, the conveyer pipe is located the both ends of reservation portion and is equipped with the solenoid valve respectively, add one section reservation portion, can be with the dimethyl ether gas of heating vaporization in advance quantitative storage in reservation portion of heating vaporization jar department, adopt the mode of segmentation feeding, the mode of importing the gas mixing incasement with moderate dimethyl ether gas, rethread intake pipe is to the reaction gas of gas mixing incasement introduction moderate carbon monoxide, hydrogen, carry out the mixture in the gas mixing incasement for a period of time and obtain the mixed gas, compare and directly continuously let in, on the one hand improves the mixture ratio accuracy, on the other hand improves the mixed degree of mixed gas, mixed gas is by gas mixing case gas vent discharge catalytic reaction portion, improve catalytic reaction effect.
Further, the inside rotation of gas mixing case has the axis of rotation, the lower extreme of axis of rotation runs through to the gas mixing case below, the axis of rotation is located the inside end wall of gas mixing case and is located the end wall of gas mixing case below and has cup jointed respectively and has gone up gas distribution fan and lower gas distribution fan, the interior end wall of catalytic reaction portion top carries out rotary drive's driving motor one to the axis of rotation through a plurality of stiffener fixed mounting, after dimethyl ether gas and reaction gas ration are assembled into the gas mixing case in, start driving motor one, utilize and go up gas distribution fan to stir the mixed gas, improve the mixing effect, after the mixed operation is accomplished, open the discharge valve of gas mixing case department, the mixed gas evenly distributes into catalytic bed department under the effect of the lower gas distribution fan of lasting rotation, in order to realize mixed gas and the abundant and even contact of catalytic packing.
Further, the catalytic bed bottom flushes the setting mutually with the gomphosis groove bottom, catalytic bed bottom outer wall inlays and is equipped with the magnetism layer of inhaling, gomphosis groove bottom inner wall inlays to establish and installs and inhale layer assorted electromagnetic ring with magnetism, utilizes magnetism to inhale the mode of installation and realizes the location between catalytic bed and the gomphosis groove, when needs are with catalytic bed separation gomphosis groove, only need break electromagnetic ring, can follow the downward dismantlement of gomphosis groove bottom with catalytic bed, easy operation.
Furthermore, the guide table movably attached to the outer end wall of the rotary disk is fixedly embedded on the inner wall of the reaction tower, which is positioned at the catalytic reaction part, so that the rotary tightness between the rotary disk and the two reaction towers is improved, and the mixed gas is subjected to catalytic reaction from top to bottom through the catalytic bed.
Further, the spectrum monitoring system comprises a protective cover which is fixed at the top end of the supporting structure and corresponds to the position of the embedded groove, an infrared camera device with a camera end extending to the inner side of the protective cover is arranged on the protective cover, the weight monitoring system is arranged on the bottom end wall of the supporting structure and corresponds to the position of the embedded groove, and a sensing table attached to the lower side of the catalytic bed is fixedly arranged at the telescopic end of the electric telescopic rod.
Further, the outer diameter of the sensing table is larger than that of the bottom end of the catalytic bed, and a pressure sensor is embedded in the upper end face of the sensing table.
Further, a pair of sealing plates positioned below the rotating disk are fixedly installed between the reaction towers, through grooves matched with the sensing table in a fitting mode are formed in the sealing plates, the sealing plates are in sealing butt joint with the sensing table, and the rotating disk is used for realizing that catalytic packing at the catalytic bed is always in a sealing environment in the rotating process, so that the original catalytic environment parameters of the catalytic reaction part are disturbed due to the fact that the catalytic beds are in contact with the external environment in the exchanging process of the two groups of catalytic beds.
Compared with the prior art, the invention has the advantages that:
(1) According to the scheme, the rotating disc with four catalytic beds is rotatably arranged between the pair of reaction towers, wherein the two catalytic beds are positioned outside the pair of reaction towers and serve as standby reaction beds, the inside and outside distribution positions of the two groups of catalytic beds are changed after the preset reaction time, the composite monitoring mechanism is used for monitoring the saturation of catalytic filler after the reaction in the catalytic beds, the composite monitoring mechanism is used as a judging factor for judging whether the catalytic filler needs to be replaced or not, when the saturation threshold is not reached, the position is replaced again, when the saturation threshold is reached, the saturated catalytic filler is replaced, and the mode of quickly rotating and replacing the reaction beds is adopted.
(2) According to the scheme, the conveying pipe with the reserved portion is additionally arranged between the heating vaporization tank and the pair of gas mixing boxes, dimethyl ether gas heated and vaporized at the heating vaporization tank is stored in the reserved portion quantitatively in advance, a sectional feeding mode is adopted, a proper amount of dimethyl ether gas is converged into the gas mixing boxes, a proper amount of reaction gas of carbon monoxide and hydrogen is led into the gas mixing boxes through the air inlet pipe, a certain period of mixing is carried out in the gas mixing boxes to obtain mixed gas, the mixed gas is mixed in the gas mixing boxes to reach the standard range temperature more easily, compared with direct continuous feeding, on one hand, the mixing proportion accuracy is improved, on the other hand, the mixing degree of the mixed gas is improved, the mixed gas is discharged into the catalytic reaction portion through the gas mixing box exhaust port, and the catalytic reaction effect is improved.
(3) The combined type monitoring mechanism in this scheme comprises spectrum monitoring system and weight monitoring system, and the inside and outside distribution position of two sets of catalytic beds is changed with preset reaction time in the reaction process, utilizes spectrum monitoring system and weight monitoring system to carry out infrared image contrast and proportion contrast to the catalytic packing in the catalytic bed respectively, and the detection method that both combine together is more accurate to the detection of catalytic packing saturation.
Drawings
Fig. 1 is a schematic view of the external structure of the present invention.
Fig. 2 is a partial cross-sectional view of the present invention.
FIG. 3 is a schematic view showing the structure of the pair of reaction towers of the present invention separated from the supporting structure.
FIG. 4 is a schematic view showing the structure of the junction of a pair of reaction towers and a rotating disk according to the present invention.
FIG. 5 is a schematic view showing the structure of a pair of reaction towers of the present invention separated from a rotary disk.
Fig. 6 is a schematic structural diagram of the rotary disk of the present invention separated from the catalytic bed.
Fig. 7 is a schematic cross-sectional view of the present invention.
Fig. 8 is a schematic view of the structure of the present invention when the catalyst bed is detached downward.
The reference numerals in the figures illustrate:
1. a reaction tower; 101. a rotary groove; 102. a guide table; 2. heating the vaporization tank; 201. a dimethyl ether feed pipe; 3. a delivery tube; 301. a reservation section; 4. a gas mixing box; 401. an air inlet pipe; 5. feeding an air distribution fan; 6. a lower air distribution fan; 7. driving a first motor; 8. a rotating disc; 801. a fitting groove; 802. an electromagnetic ring; 9. a catalytic bed; 901. a magnetic attraction layer; 10. a support structure; 1001. an upper support table; 1002. a lower support bracket; 11. a second driving motor; 12. a sensing table; 121. a pressure sensor; 13. an electric telescopic rod; 14. a discharge pipe; 15. an infrared imaging device; 16. a sealing plate; 17. and a protective cover.
Detailed Description
The drawings in the embodiments of the present invention will be combined; the technical scheme in the embodiment of the invention is clearly and completely described; obviously; the described embodiments are only a few embodiments of the present invention; but not all embodiments, are based on embodiments in the present invention; all other embodiments obtained by those skilled in the art without undue burden; all falling within the scope of the present invention.
Example 1:
The invention discloses a reaction device for preparing methyl acetate by dimethyl ether carbonylation, referring to fig. 1-3, which comprises a bearing structure 10 and reaction towers 1 embedded and installed on the left side and the right side of the bearing structure 10, wherein the bearing structure 10 comprises a lower bearing bracket 1002 and an upper bearing bracket 1001, the bottoms of the upper bearing bracket 1001 and the lower bearing bracket 1002 are of circular structures taking the middle points of a pair of reaction towers 1 as circle centers, and nesting grooves for nesting the reaction towers 1 are formed on the two sides of the upper bearing bracket 1001 and the lower bearing bracket 1002.
The top of a pair of reaction towers 1 inlays and establishes the gas mixing box 4 that installs bottom one side and have discharge valve, the heating vaporization jar 2 that has dimethyl ether inlet pipe 201 in the top is installed to the top of a pair of reaction towers 1, heating vaporization jar 2 internally mounted has the heater for carry out the heating vaporization to imported dimethyl ether raw materials, heating vaporization jar 2 bottom mounting has the conveyer pipe 3 that is connected with a pair of gas mixing box 4 top, the external intake pipe 401 that has on the gas mixing box 4, the intake pipe 401 is used for letting in the reaction gas of carbon monoxide and hydrogen to gas mixing box 4, the reaction gas mixes with the dimethyl ether after the vaporization in gas mixing box 4 and obtains the mist.
Referring to fig. 2,4 and 5, a catalytic reaction part is arranged in the reaction tower 1 below the gas mixing tank 4, rotating grooves 101 are formed in opposite end walls of the catalytic reaction part, a catalytic carrier rotating based on the center of the supporting structure 10 is embedded between the rotating grooves 101, the catalytic carrier comprises a rotating disk 8 rotatably arranged between the rotating grooves 101, a driving motor II 11 is fixedly arranged in the middle of the top end of the upper supporting table 1001, and the driving end of the driving motor II 11 penetrates through the bottom end of the center of the circle of the rotating disk 8 and is fixedly arranged;
Referring to fig. 2, 5-7, four engaging grooves 801 are uniformly formed on the rotating disk 8 along the circumferential direction thereof, the outer diameter of each engaging groove 801 is smaller than the inner diameter of the reaction tower 1, a catalytic bed 9 filled with catalytic filler is embedded in each engaging groove 801, a guide table 102 movably attached to the outer end wall of the rotating disk 8 is fixedly embedded on the inner wall of the reaction tower 1 at the catalytic reaction part, so as to improve the tightness of rotation between the rotating disk 8 and the two reaction towers 1, the catalytic bed 9 rotates to the catalytic reaction part, so that the mixed gas performs catalytic reaction from top to bottom through the catalytic bed 9, and performs catalytic reaction with the mixed gas led downwards by the gas mixing box 4, a discharge pipe 14 is externally connected to the bottom end of the reaction tower 1, and methyl acetate product obtained after the reaction is discharged from the discharge pipe 14.
The bottom end of the catalytic bed 9 is flush with the bottom end of the embedded groove 801, the magnetic attraction layer 901 is embedded on the outer wall of the bottom end of the catalytic bed 9, the electromagnetic ring 802 matched with the magnetic attraction layer 901 is embedded on the inner wall of the bottom end of the embedded groove 801, the positioning between the catalytic bed 9 and the embedded groove 801 is realized by utilizing a magnetic attraction installation mode, and when the catalytic bed 9 needs to be detached from the embedded groove 801, the catalytic bed 9 can be detached downwards from the bottom of the embedded groove 801 only by disconnecting the electromagnetic ring 802, so that the operation is simple.
Example 2:
in this embodiment, based on embodiment 1, a mixing optimization process is performed on the mixed gas before the mixed gas enters the catalytic reaction part, specifically:
Referring to fig. 2 and 7, the conveying pipe 3 is a three-way pipe, a section of reserved portion 301 is arranged at an end portion of one side of the conveying pipe 3 connected with the gas mixing tank 4, electromagnetic valves are respectively arranged at two ends of the reserved portion 301, a section of reserved portion 301 is additionally arranged, dimethyl ether gas heated and vaporized at the heating vaporization tank 2 can be stored in the reserved portion 301 in a quantitative mode in advance, a proper amount of dimethyl ether gas is introduced into the gas mixing tank 4 in a sectional feeding mode, then a proper amount of reaction gas of carbon monoxide and hydrogen is introduced into the gas mixing tank 4 through the air inlet pipe 401, and a certain period of mixing is carried out in the gas mixing tank 4 to obtain mixed gas.
The inside rotation of gas mixing tank 4 has the axis of rotation, the lower extreme of axis of rotation runs through to gas mixing tank 4 below, the axis of rotation is located the inside end wall of gas mixing tank 4 and is located on the end wall of gas mixing tank 4 below and has cup jointed respectively and has spread gas fan 5 and lower gas fan 6, the interior end wall of catalytic reaction portion top carries out rotary drive's driving motor one 7 through a plurality of stiffener fixed mounting to the axis of rotation, after dimethyl ether gas and reaction gas ration are assembled into gas mixing tank 4 in, start driving motor one 7, utilize last gas fan 5 to stir the mixed gas, improve the mixing effect, after the mixed operation is accomplished, open the discharge valve of gas mixing tank 4 department, the mixed gas evenly distributes into catalytic bed 9 department under the effect of continuous pivoted lower gas fan 6, in order to realize mixed gas and the abundant and even contact of catalytic packing.
Example 3:
In this embodiment, on the basis of embodiments 1 and 2, a composite monitoring mechanism for acquiring the saturation of the catalytic filler is installed in the front-rear direction of the supporting structure 10, the composite monitoring mechanism is structurally refined, and the following detailed description is made on the specific process of using the composite monitoring mechanism to monitor the saturation of the catalytic filler:
The combined type monitoring mechanism consists of a spectrum monitoring system and a weight monitoring system which are arranged up and down, the spectrum monitoring system comprises a protective cover 17 which is fixed at the top end of a supporting structure 10 and corresponds to the position of a jogging groove 801, an infrared camera device 15 with a camera end extending to the inner side of the protective cover 17 is arranged on the protective cover 17, the weight monitoring system is arranged on the bottom end wall of the supporting structure 10 and corresponds to the position of the jogging groove 801, a sensing table 12 which is attached to the lower part of a catalytic bed 9 is fixedly arranged at the telescopic end of the electric telescopic rod 13, the outer diameter of the sensing table 12 is larger than the outer diameter of the bottom end of the catalytic bed 9, and a pressure sensor 121 is arranged on the upper end face of the sensing table 12 in an embedded manner;
The method is characterized in that a rotating disc 8 with four catalytic beds 9 is rotatably arranged between a pair of reaction towers 1, wherein two catalytic beds 9 are positioned outside the pair of reaction towers 1 to serve as standby reaction beds, the upper end and the lower end of the standby pair of catalytic beds 9 are respectively propped against an upper bearing table 1001 and a sensing table 12 in an initial state, so that sealed storage is realized, the inner and outer distribution positions of the two groups of catalytic beds 9 are exchanged for a preset reaction time in the reaction process, and saturation monitoring is carried out on catalytic filling materials after the reaction in the catalytic beds 9 by utilizing a composite monitoring mechanism;
In the saturation monitoring process, the internal and external distribution positions of the two groups of catalytic beds 9 are exchanged with a preset reaction time in the reaction process, when catalytic fillers participating in the reaction are exchanged to the composite monitoring mechanism, the infrared imaging equipment 15 is used for carrying out thermal infrared shooting on the catalytic fillers to obtain a thermal infrared image, after the thermal infrared image is obtained, the electromagnetic ring 802 is disconnected, the catalytic beds 9 are separated from the embedded groove 801, the catalytic beds 9 are arranged on the sensing table 12, and the pressure sensor 121 is used for carrying out quality detection on the catalytic beds 9 and the catalytic fillers.
A sealing plate 16 positioned below the rotary disk 8 is fixedly arranged between the pair of reaction towers 1, a through groove matched with the sensing table 12 in a fit way is formed in the sealing plate 16, the sealing plate 16 is in sealing butt joint with the sensing table 12, and the rotary disk 8 is used for realizing that catalytic packing at the catalytic beds 9 is always in a sealing environment in the rotating process, so that the catalytic environmental parameters of the catalytic reaction part are disturbed due to the contact of the catalytic beds 9 with the external environment in the exchanging process of the two groups of catalytic beds 9;
The composite monitoring mechanism is connected with a control system, and the control system comprises a data acquisition unit, a data evaluation unit and a regulation and control unit, wherein the data acquisition unit is used for acquiring a thermal infrared image of the catalytic filler shot by the infrared camera equipment 15 and weight data after the catalytic filler is reacted, acquired by the pressure sensor 121, and sending the thermal infrared image and the weight data to the data evaluation unit;
The data evaluation unit is used for carrying out comprehensive analysis after receiving the thermal infrared image and the weight data, and specifically comprises the following steps: obtaining absorption peak intensity on an infrared spectrum according to a thermal infrared image, performing difference calculation on preset saturated absorption peak intensity and absorption peak intensity to obtain an absorption peak intensity difference Q 1, and performing difference calculation on preset saturated weight data and weight data to obtain a quality difference Z 1;
When the absorption peak intensity difference Q 1 is larger than the preset absorption peak intensity difference Q or the quality difference Z 1 is larger than the preset quality difference Z, an unsaturated signal is generated, when the absorption peak intensity difference Q 1 is smaller than or equal to the preset absorption peak intensity difference Q and the quality difference Z 1 is smaller than or equal to the preset quality difference Z and the quality difference Z 1 is smaller than or equal to the preset quality difference Z, the smaller the absorption peak intensity difference Q 1 is, the intensity of the absorption peak is not increased along with the increase of the absorption time any more, but tends to be stable or reach a platform state, and at the moment, the catalytic filler reaches a saturation approaching state, the saturated signal is generated, and the unsaturated signal and the saturated signal are sent to a regulating and controlling unit;
When the regulation and control unit receives an unsaturated signal, the internal and external distribution positions of the two groups of catalytic beds 9 are replaced by a second driving motor 11, so that unsaturated catalytic fillers continue to participate in the reaction, and saturation is monitored intermittently in a preset time;
When the regulating unit receives the saturation signal, it indicates that the catalytic filler participating in the reaction has reached a saturated state, and at this time, the new catalytic filler exchanged into the reaction tower 1 continues to participate in the reaction, and for the saturated catalytic filler, referring to fig. 8, only the electric telescopic rod 13 is needed to descend the catalytic bed 9 away from the bottom end of the rotating disc 8, and at this time, the saturated catalytic filler can be further exchanged.
The spectrum monitoring system and the weight monitoring system are used for respectively carrying out infrared image comparison and specific gravity comparison on the catalytic filler in the catalytic bed 9, the detection method combining the spectrum monitoring system and the weight monitoring system is more accurate in detecting the saturation degree of the catalytic filler, when the detection result is that the saturation threshold value is not reached, the position of the catalytic filler which is not reached is replaced, and the catalytic filler which is not reached is continuously involved in the reaction until the saturated catalytic filler is not replaced again when the saturated catalytic filler reaches the saturation threshold value in continuous monitoring, so that the saturated catalytic filler is replaced, and a mode of rapidly rotating and replacing a reaction bed is adopted.
To sum up: in the reaction process, dimethyl ether gas heated and vaporized at the heating vaporization tank 2 is quantitatively stored in the reserved part 301 in advance, a proper amount of dimethyl ether gas is converged into the gas mixing tank 4 in a sectional feeding mode, then a proper amount of reaction gas of carbon monoxide and hydrogen is introduced into the gas mixing tank 4 through the gas inlet pipe 401, and mixed gas is obtained by mixing in the gas mixing tank 4 for a certain period of time, the mixed gas is mixed in the gas mixing tank 4 to reach the temperature and the mixing degree in a standard range more easily, after the mixed gas of the gas mixing tank 4 is exhausted, the dimethyl ether gas stored in the reserved part 301 is introduced into the gas mixing tank 4, and is matched with a proper amount of reaction gas to be introduced for cyclic repetition, so that compared with the direct continuous feeding, on one hand, the mixing ratio accuracy is improved, on the other hand, the mixing degree of the mixed gas is improved, and the mixed gas is discharged into the catalytic reaction part through the gas outlet of the gas mixing tank 4, and the catalytic reaction effect is improved;
The inside and outside distribution position of two groups of catalytic beds 9 are exchanged after the preset reaction time, the saturation degree of catalytic filler after the reaction in the catalytic beds 9 is monitored by utilizing the compound monitoring mechanism, the position is exchanged again when the saturation threshold is not reached as a judging factor for whether the replacement is needed, the saturated catalytic filler is replaced when the saturation threshold is reached, compared with the mode of the existing mode of switching the standby reactor by adopting the quick rotating exchange reaction bed, the continuous reaction is ensured, the original catalytic environment is not changed, in addition, the saturated catalytic filler is moved out of the reaction tower 1 along with the rotation of the rotating disk, the reaction tower 1 is not required to be opened, and the replacement is simpler.
The above; is only a preferred embodiment of the present invention; the scope of the invention is not limited in this respect; any person skilled in the art is within the technical scope of the present disclosure; equivalent substitutions or changes are made according to the technical proposal of the invention and the improved conception thereof; are intended to be encompassed within the scope of the present invention.
Claims (10)
1. The utility model provides a reaction unit of dimethyl ether carbonylation preparation methyl acetate, includes bearing structure (10) and inlays to establish and install in reaction tower (1) of bearing structure (10) left and right sides, its characterized in that: the reaction device is characterized in that a gas mixing box (4) with an exhaust valve at one side of the bottom end is arranged at the top end of the reaction tower (1), a pair of heating vaporization tanks (2) with dimethyl ether feeding pipes (201) at the top ends are arranged above the reaction tower (1), conveying pipes (3) connected with the top ends of the pair of gas mixing boxes (4) are fixed at the bottom ends of the heating vaporization tanks (2), and an air inlet pipe (401) is externally connected to the gas mixing boxes (4);
The catalytic reaction device is characterized in that the reaction tower (1) is positioned below the gas mixing box (4) and internally provided with a catalytic reaction part, a pair of rotary grooves (101) are formed in opposite end walls of the catalytic reaction part, a catalytic carrier which rotates based on the center of a bearing structure (10) is embedded between the rotary grooves (101), the catalytic carrier comprises a rotary disk (8) which is rotatably arranged between the rotary grooves (101), four embedded grooves (801) are uniformly formed in the rotary disk (8) along the circumferential direction of the rotary disk, a catalytic bed (9) filled with catalytic filler is embedded in each embedded groove (801), and a discharging pipe (14) is externally connected to the bottom end of the reaction tower (1);
the composite monitoring mechanism for acquiring the saturation of the catalytic filler is arranged in the front-back direction of the supporting structure (10), and consists of a spectrum monitoring system and a weight monitoring system which are arranged up and down.
2. The reaction device for preparing methyl acetate by carbonylation of dimethyl ether according to claim 1, wherein: the bearing structure (10) comprises a lower bearing bracket (1002) and an upper bearing table (1001), wherein the bottoms of the upper bearing table (1001) and the lower bearing bracket (1002) are of a circular structure taking the middle points of a pair of reaction towers (1) as circle centers.
3. The reaction device for preparing methyl acetate by carbonylation of dimethyl ether according to claim 2, wherein: the middle part of the top end of the upper bearing table (1001) is fixedly provided with a second driving motor (11), and the driving end of the second driving motor (11) penetrates through to the bottom end of the circle center of the rotating disc (8) and is fixedly arranged.
4. The reaction device for preparing methyl acetate by carbonylation of dimethyl ether according to claim 1, wherein: the conveying pipe (3) is a three-way pipe, a section of reserved portion (301) is arranged at one end portion of the conveying pipe (3) connected with one side of the gas mixing box (4), and electromagnetic valves are respectively arranged at two ends of the reserved portion (301) of the conveying pipe (3).
5. The reaction device for preparing methyl acetate by carbonylation of dimethyl ether according to claim 1, wherein: the inside rotation of gas mixing tank (4) has the axis of rotation, the lower extreme of axis of rotation runs through to gas mixing tank (4) below, the axis of rotation is located the inside end wall of gas mixing tank (4) and is located on the end wall of gas mixing tank (4) below and has cup jointed respectively and has spread gas fan (5) and lower gas fan (6), the inner wall of catalytic reaction portion top carries out rotary drive's driving motor one (7) through a plurality of strengthening rods fixed mounting.
6. The reaction device for preparing methyl acetate by carbonylation of dimethyl ether according to claim 1, wherein: the bottom of the catalytic bed (9) is flush with the bottom of the embedded groove (801), the outer wall of the bottom of the catalytic bed (9) is embedded with the magnetic attraction layer (901), and the inner wall of the bottom of the embedded groove (801) is embedded with the electromagnetic ring (802) matched with the magnetic attraction layer (901).
7. The reaction device for preparing methyl acetate by carbonylation of dimethyl ether according to claim 1, wherein: the inner wall of the reaction tower (1) at the catalytic reaction part is fixedly embedded with a guide table (102) movably attached to the outer end wall of the rotary disk (8).
8. The reaction device for preparing methyl acetate by carbonylation of dimethyl ether according to claim 1, wherein: the spectrum monitoring system comprises a protective cover (17) fixed at the top end of the supporting structure (10) and corresponding to the position of the embedded groove (801), an infrared camera device (15) with a camera end extending to the inner side of the protective cover (17) is arranged on the protective cover (17), the weight monitoring system is arranged on the bottom end wall of the supporting structure (10) and corresponding to the position of the embedded groove (801), and a sensing table (12) attached to the lower side of the catalytic bed (9) is fixedly arranged at the telescopic end of the electric telescopic rod (13).
9. The reaction device for preparing methyl acetate by carbonylation of dimethyl ether according to claim 8, wherein: the outer diameter of the sensing table (12) is larger than that of the bottom end of the catalytic bed (9), and a pressure sensor (121) is embedded and arranged on the upper end face of the sensing table (12).
10. The reaction device for preparing methyl acetate by carbonylation of dimethyl ether according to claim 9, wherein: a sealing plate (16) positioned below the rotary disk (8) is fixedly arranged between the pair of reaction towers (1), and a through groove matched with the sensing table (12) in a fitting way is formed in the sealing plate (16).
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| CN102974301A (en) * | 2011-09-07 | 2013-03-20 | 厦门福美科技有限公司 | Novel continuous fluid contact reaction apparatus |
| CN106731563A (en) * | 2015-11-19 | 2017-05-31 | 中国石油化工股份有限公司 | A kind of processing method and processing device of chloride organic exhaust gas |
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| CN104995167B (en) * | 2012-12-21 | 2017-05-17 | 英国石油化学品有限公司 | Integrated process for the production of methyl acetate and methanol from synthesis gas and dimethylether |
| CN117942757B (en) * | 2024-02-22 | 2024-07-16 | 安徽优环环保设备制造有限公司 | High adsorptivity industrial waste gas treatment device |
| CN117884046B (en) * | 2024-03-14 | 2024-06-04 | 安徽碳鑫科技有限公司 | Dimethyl ether carbonylation continuous treatment device and method convenient for replacing catalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102974301A (en) * | 2011-09-07 | 2013-03-20 | 厦门福美科技有限公司 | Novel continuous fluid contact reaction apparatus |
| CN106731563A (en) * | 2015-11-19 | 2017-05-31 | 中国石油化工股份有限公司 | A kind of processing method and processing device of chloride organic exhaust gas |
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