CN112169712A - Reactor for synthesizing methyl acetate by dimethyl ether carbonylation - Google Patents
Reactor for synthesizing methyl acetate by dimethyl ether carbonylation Download PDFInfo
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- CN112169712A CN112169712A CN202011181300.6A CN202011181300A CN112169712A CN 112169712 A CN112169712 A CN 112169712A CN 202011181300 A CN202011181300 A CN 202011181300A CN 112169712 A CN112169712 A CN 112169712A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—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 in tube reactors; the solid particles being arranged in tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0278—Feeding reactive fluids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/06—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 in tube reactors; the solid particles being arranged in tubes
- B01J8/067—Heating or cooling the reactor
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- 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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- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00008—Controlling the process
- B01J2208/00017—Controlling the temperature
- B01J2208/00106—Controlling the temperature by indirect heat exchange
- B01J2208/00115—Controlling the temperature by indirect heat exchange with heat exchange elements inside the bed of solid particles
- B01J2208/00132—Tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00884—Means for supporting the bed of particles, e.g. grids, bars, perforated plates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00893—Feeding means for the reactants
- B01J2208/00911—Sparger-type feeding elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/06—Details of tube reactors containing solid particles
- B01J2208/065—Heating or cooling the reactor
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention provides a reactor for synthesizing methyl acetate by dimethyl ether carbonylation, which comprises: the reactor body is provided with a reactor inlet at the upper end and a reactor outlet at the lower end; the isothermal reaction bed layer is arranged in the reactor body and can react with reaction raw materials entering from the inlet of the reactor; and the catalyst protection bed layer is arranged in the reactor body and is positioned in a space between the isothermal reaction bed layer and the inlet of the reactor, and the catalyst protection bed layer is provided with an absorption catalyst capable of absorbing carbonyl iron. The method has the advantages that the carbon monoxide is easy to generate carbonyl iron after being heated, the carbonyl iron has a poisoning effect on the catalyst, when the reactor is fed with carbonyl iron having a poisoning effect on the catalyst, the carbonyl iron can be removed through the catalyst protection bed layer, the activity of the catalyst is ensured, the catalyst resource can be saved, and an independent catalyst protection bed reactor is not required to be arranged.
Description
Technical Field
The invention relates to the field of coal chemical industry, in particular to a reactor for synthesizing methyl acetate by dimethyl ether carbonylation.
Background
Ethanol gasoline is being greatly popularized in the prior art, and the synthesis of ethanol by taking synthesis gas as a raw material becomes a hot point of research in recent years. The carbonylation of dimethyl ether and carbon monoxide under the action of molecular sieve catalyst to synthesize methyl acetate, and the hydrogenation to produce absolute ethyl alcohol is a new developed technical route. However, the carbon monoxide is easy to generate carbonyl iron after being heated, and has toxic action on the catalyst, and the prior art is provided with an independent catalyst protection bed reactor, stainless steel and high manufacturing cost.
Disclosure of Invention
The invention provides a reactor for synthesizing methyl acetate by dimethyl ether carbonylation, which aims to remove carbonyl iron in raw materials and synthesize a target product methyl acetate.
The technical scheme adopted by the invention for solving the technical problems is as follows: a reactor for the carbonylation of dimethyl ether to methyl acetate comprising: the reactor body is provided with a reactor inlet at the upper end and a reactor outlet at the lower end; the isothermal reaction bed layer is arranged in the reactor body and can react with reaction raw materials entering from the inlet of the reactor; and the catalyst protection bed layer is arranged in the reactor body and is positioned in a space between the isothermal reaction bed layer and the inlet of the reactor, and the catalyst protection bed layer is provided with an absorption catalyst capable of absorbing carbonyl iron.
Furthermore, the reactor for synthesizing methyl acetate by dimethyl ether carbonylation also comprises an adiabatic fixed bed layer which is arranged in the reactor body and is positioned between the catalyst protection bed layer and the isothermal reaction bed layer, and the adiabatic fixed bed layer is provided with a reaction catalyst capable of reacting with the reaction raw materials.
Further, the isothermal reaction bed comprises: the two reactor tube plates are arranged along the horizontal direction, are arranged in the reactor body in parallel at intervals, and form a sealed space between the two reactor tube plates and the inner wall of the reactor body; the upper end of the heat exchange tube is connected with the tube plate of the reactor positioned above and is communicated with the heat-insulating fixed bed layer, the lower end of the heat exchange tube is connected with the tube plate of the reactor positioned below and is communicated with the outlet of the reactor, and an isothermal reaction catalyst is arranged in the heat exchange tube.
Further, the heat exchange tubes are multiple and arranged in the sealed space at intervals in parallel.
Further, the reactor body further comprises a reactor shell side water supply inlet and a reactor shell side steam outlet, the reactor shell side water supply inlet and the reactor shell side steam outlet are both communicated with the sealing space, and the reactor shell side steam outlet is located above the reactor shell side water supply inlet.
Furthermore, an accommodating space is formed between the tube plate of the reactor positioned below and the bottom of the reactor body, and the reactor for synthesizing the methyl acetate by carbonylation of the dimethyl ether further comprises a discharge opening which is arranged on the side wall of the lower end of the reactor body and is communicated with the accommodating space.
Further, the reactor for synthesizing the methyl acetate by carbonylating the dimethyl ether also comprises a gas distributor which is arranged in the reactor body and is connected with the lower end of the inlet of the reactor.
Further, the height of the catalyst protection bed layer along the vertical direction is 500-1000 mm.
Further, the height of the heat insulation fixed bed layer along the vertical direction is 300-1000 mm.
The method has the advantages that the carbon monoxide is easy to generate carbonyl iron after being heated, the carbonyl iron has a toxic effect on the catalyst, and when the reactor is fed with carbonyl iron having a toxic effect on the catalyst, the carbonyl iron can be removed through the catalyst protection bed layer, so that the activity of the catalyst is ensured, and the catalyst resource can be saved.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 is a schematic structural diagram of an embodiment of the present invention.
Reference numbers in the figures: 1. an inlet of the reactor; 2. a catalyst loading port; 3. a gas distributor; 4. a reactor tube sheet; 5. a heat exchange pipe; 6. a discharge opening; 7. an outlet of the reactor; 8. a reactor shell side feed water inlet; 9. a reactor shell side steam outlet; 10. fixing the bed layer in an insulating way; 11. a catalyst protection bed layer; 12. inert ceramic balls.
Detailed Description
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
As shown in figure 1, the embodiment of the invention provides a reactor for synthesizing methyl acetate by carbonylation of dimethyl ether, which comprises a reactor body, an isothermal reaction bed layer and a catalyst protection bed layer 11. The upper end of the reactor body is provided with a reactor inlet 1, and the lower end is provided with a reactor outlet 7. The isothermal reaction bed is arranged in the reactor body and can react with the reaction raw materials entering from the inlet 1 of the reactor. The catalyst protection bed layer 11 is arranged in the reactor body and is positioned in a space between the isothermal reaction bed layer and the inlet 1 of the reactor, and the catalyst protection bed layer 11 is provided with an absorption catalyst capable of absorbing carbonyl iron. Among these, the catalyst loaded with the absorption catalyst is a commercially available catalyst, such as: k306 in southern chemistry, QXJ-01 in Azurite, RA-201 in the southwest institute of chemical industry, and W108 in Wuhan Kelin.
The carbon monoxide is easy to generate carbonyl iron after being heated, which has a toxic effect on the catalyst, and when the reactor is fed with carbonyl iron having a toxic effect on the catalyst, the carbonyl iron can be removed through the catalyst protection bed layer 11, so that the activity of the catalyst is ensured, and the catalyst resource can be saved.
In the embodiment, the height of the catalyst protection bed layer 11 in the vertical direction is 500-1000 mm, and a catalyst filling port 2 is further arranged beside the inlet 1 of the reactor and used for filling a catalyst.
The reactor for synthesizing methyl acetate by dimethyl ether carbonylation also comprises an adiabatic fixed bed layer 10 which is arranged in the reactor body and is positioned between the catalyst protective bed layer 11 and the isothermal reaction bed layer, and the adiabatic fixed bed layer 10 is provided with a reaction catalyst capable of reacting with reaction raw materials. Please refer to chinese patent application with application No. CN201510964686.0, publication No. CN201510964686.0, and publication date 20170627, which is entitled catalyst for producing methyl acetate by carbonylation of dimethyl ether and its application.
The adiabatic fixed bed 10 contributes to increasing the temperature of the isothermal reaction bed, thereby increasing the reaction activity of the catalyst and the selectivity of the product, and on the other hand, by-producing steam with higher pressure. Wherein, the height of adiabatic fixed bed layer 10 along vertical direction is 300 ~ 1000 mm.
Specifically, the isothermal reaction bed comprises two reactor tube sheets 4 and heat exchange tubes 5. The two reactor tube plates 4 are arranged along the horizontal direction, the two reactor tube plates 4 are arranged in the reactor body along the vertical direction at intervals in parallel, and a sealing space is formed between the two reactor tube plates 4 and the inner wall of the reactor body. The upper end of the heat exchange tube 5 is connected with the reactor tube plate 4 positioned above and is communicated with the heat-insulating fixed bed layer 10, the lower end of the heat exchange tube 5 is connected with the reactor tube plate 4 positioned below and is communicated with the reactor outlet 7, and an isothermal reaction catalyst is arranged in the heat exchange tube 5.
The temperature difference between the inside and the outside of the heat exchange tube 5 is small, so that reactants can continue to react at a higher temperature, and gas after the reaction is discharged from the outlet of the reactor, wherein the heat released by the isothermal reaction bed layer can be used for producing a byproduct of 1.5-2.0 MPa (G) of steam.
As shown in fig. 1, the heat exchange tubes 5 are plural and arranged at the sealed space in parallel at intervals in the horizontal direction. The increased number of heat exchange tubes 5 can increase the treatment capacity of the reactants and the catalyst in the embodiment and improve the treatment efficiency.
The reactor body further comprises a reactor shell side water supply inlet 8 and a reactor shell side steam outlet 9, the reactor shell side water supply inlet 8 and the reactor shell side steam outlet 9 are both communicated with the sealing space, and the reactor shell side steam outlet 9 is positioned above the reactor shell side water supply inlet 8.
The reactor shell side water supply inlet 8 can introduce deoxygenated water into the sealed space, and the deoxygenated water is discharged from the reactor shell side steam outlet 9 by absorbing the temperature of the heat exchange tube 5 and generating the byproduct steam. Wherein isothermal reaction is carried out in the heat exchange tube 5, the temperature difference between the inside and the outside of the tube is controlled to be 10-20 ℃, and high-pressure (1.5-2.0 MPa) (G) steam is byproduct.
Preferably, a containing space is formed between the lower reactor tube plate 4 and the bottom of the reactor body, inert ceramic balls 12 are arranged in the containing space, and the lower end of the heat exchange tube 5 and the reactor outlet 7 are both communicated with the containing space.
The inert ceramic balls 12 are used as a support and cover material for the catalyst in the reactor, and can buffer the impact of gas entering the reactor on the catalyst, protect the catalyst and improve the distribution of the gas in the reactor.
It should be noted that inert ceramic balls 12 are disposed above and below the catalyst protection bed 11 to buffer the impact of gas entering the reactor on the catalyst and protect the catalyst protection bed 11.
The reactor for synthesizing methyl acetate by dimethyl ether carbonylation also comprises a discharge opening 6 which is arranged on the side wall of the lower end of the reactor body and is communicated with the containing space. The discharge opening 6 can be used to discharge the catalyst and inert ceramic balls 12 of the above-mentioned respective sections.
The reactor for synthesizing methyl acetate by dimethyl ether carbonylation also comprises a gas distributor 3 which is arranged in the reactor body and is connected with the lower end of the reactor inlet 1. The gas distributor 3 enables the gas to be distributed uniformly over the entire cross-section.
The working principle of the embodiment of the invention is as follows:
the reaction raw materials are heated to the temperature capable of initiating the reaction and then enter a reactor, carbonyl iron having toxic action on the catalyst is removed in a catalyst protective bed layer 11, then the carbonyl iron enters an adiabatic fixed bed layer 10 for reaction, the temperature of the reaction materials is raised by the released heat, then the reaction materials enter an isothermal reaction bed layer and continue to react at a higher temperature, and the reacted gas flows out from an outlet 7 of the reactor. The heat released from the isothermal reaction part produces a byproduct of 1.5-2.0 MPa (G) of steam.
Taking a device for producing 30 ten thousand tons of methyl acetate annually as an example, the specific process is as follows: mixing carbon monoxide with dimethyl ether at the pressure of 4.0-6.0 MPa (G) according to a certain proportion, exchanging heat with a reaction product in a reactor inlet/outlet heat exchanger, heating to 195 ℃, and enabling a raw material gas to be uniformly distributed through a gas distributor 3; then enters a catalyst protective bed layer 11 to remove carbonyl iron which has toxic action on the catalyst; then enters the adiabatic fixed bed layer 10 for reaction, the temperature of the material leaving the adiabatic fixed bed layer 10 is raised to 210 ℃, the material reaches the optimal temperature of the carbonylation reaction, and the material enters the isothermal reaction bed layer. The reaction raw materials continue to react, and the released heat is removed by the byproduct steam between the heat exchange tubes. The isothermal reaction is carried out at a high temperature (initial 210 ℃ and final 240 ℃) to produce 1.5 to 2.5MPa (G) of by-product steam.
Specifically, the inside diameter of the apparatus is phi 4500, wherein the catalyst guard bed 11 is 600mm high, the adiabatic fixed bed 10 is 800mm high, and the heat exchange tube 5 is 10200mm long. Compared with a tubular reactor with the same production capacity, the tubular reactor has the advantages that the tubular part is shortened by 1800mm, the bed resistance is reduced by 30kPa, and the power of a circulating carbon monoxide compressor is reduced by 2.5%.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects: the carbon monoxide is easy to generate carbonyl iron after being heated, which has a toxic effect on the catalyst, and when the reactor is fed with carbonyl iron having a toxic effect on the catalyst, the carbonyl iron can be removed through the catalyst protection bed layer 11, so that the activity of the catalyst is ensured, and the catalyst resource can be saved.
The above description is only exemplary of the invention and should not be taken as limiting the scope of the invention, so that the invention is intended to cover all modifications and equivalents of the embodiments described herein. In addition, the technical features, the technical schemes and the technical schemes can be freely combined and used.
Claims (9)
1. A reactor for synthesizing methyl acetate by dimethyl ether carbonylation is characterized by comprising:
the upper end of the reactor body is provided with a reactor inlet (1), and the lower end of the reactor body is provided with a reactor outlet (7);
the isothermal reaction bed layer is arranged in the heat exchange tube of the reactor body and can react with the reaction raw materials entering from the inlet (1) of the reactor;
and the catalyst protection bed layer (11) is arranged in the reactor body and is positioned in a space between the isothermal reaction bed layer and the inlet (1) of the reactor, and the catalyst protection bed layer (11) is provided with an absorption catalyst capable of absorbing carbonyl iron.
2. The reactor for the carbonylation of dimethyl ether to methyl acetate according to claim 1, wherein the reactor for the carbonylation of dimethyl ether to methyl acetate further comprises an adiabatic fixed bed layer (10) disposed within the reactor body and between the catalyst guard bed layer (11) and the isothermal reaction bed layer, and the adiabatic fixed bed layer (10) is provided with a reaction catalyst capable of reacting with the reaction raw material.
3. The reactor for the carbonylation of dimethyl ether to produce methyl acetate according to claim 2 wherein the isothermal reaction bed comprises:
the two reactor tube plates (4) are arranged in the reactor body in parallel at intervals along the vertical direction, and a sealed space is formed between the two reactor tube plates (4) and the inner wall of the reactor body;
the upper end of the heat exchange tube (5) is connected with the reactor tube plate (4) positioned above and is communicated with the heat-insulating fixed bed layer (10), the lower end of the heat exchange tube (5) is connected with the reactor tube plate (4) positioned below and is communicated with the reactor outlet (7), and an isothermal reaction catalyst is arranged in the heat exchange tube (5).
4. A reactor for the carbonylation of dimethyl ether to produce methyl acetate according to claim 3 wherein the heat exchange tubes (5) are horizontally spaced apart in parallel at the sealed space.
5. The reactor for the carbonylation of dimethyl ether to methyl acetate according to claim 3 wherein the reactor body further comprises a reactor shell side feed water inlet (8) and a reactor shell side steam outlet (9), both the reactor shell side feed water inlet (8) and the reactor shell side steam outlet (9) being in communication with the sealed space, and the reactor shell side steam outlet (9) being located above the reactor shell side feed water inlet (8).
6. The reactor for the carbonylation of dimethyl ether to methyl acetate according to claim 3, wherein a containing space is formed between the lower reactor tube plate (4) and the bottom of the reactor body, and the reactor for the carbonylation of dimethyl ether to methyl acetate further comprises a discharge opening (6) which is arranged on the side wall of the lower end of the reactor body and is communicated with the containing space.
7. The reactor for the carbonylation of dimethyl ether to methyl acetate according to claim 1 further comprising a gas distributor (3) disposed within the reactor body and connected to the lower end of the reactor inlet (1).
8. The reactor for carbonylation synthesis of methyl acetate from dimethyl ether according to claim 1, wherein the height of the catalyst protection bed layer (11) along the vertical direction is 500-1000 mm.
9. The reactor for carbonylation of dimethyl ether to methyl acetate according to claim 2, wherein the height of the heat-insulating fixed bed layer (10) along the vertical direction is 300-1000 mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011181300.6A CN112169712A (en) | 2020-10-29 | 2020-10-29 | Reactor for synthesizing methyl acetate by dimethyl ether carbonylation |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011181300.6A CN112169712A (en) | 2020-10-29 | 2020-10-29 | Reactor for synthesizing methyl acetate by dimethyl ether carbonylation |
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| CN112169712A true CN112169712A (en) | 2021-01-05 |
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| CN202011181300.6A Pending CN112169712A (en) | 2020-10-29 | 2020-10-29 | Reactor for synthesizing methyl acetate by dimethyl ether carbonylation |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116786041A (en) * | 2023-06-12 | 2023-09-22 | 山东彩客东奥化学有限公司 | Catalytic hydrogenation fluidized bed cooling device and application method thereof |
| CN117884046A (en) * | 2024-03-14 | 2024-04-16 | 安徽碳鑫科技有限公司 | Dimethyl ether carbonylation continuous treatment device and method convenient for replacing catalyst |
-
2020
- 2020-10-29 CN CN202011181300.6A patent/CN112169712A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116786041A (en) * | 2023-06-12 | 2023-09-22 | 山东彩客东奥化学有限公司 | Catalytic hydrogenation fluidized bed cooling device and application method thereof |
| CN116786041B (en) * | 2023-06-12 | 2024-02-27 | 山东彩客东奥化学有限公司 | Catalytic hydrogenation fluidized bed cooling device and application method thereof |
| CN117884046A (en) * | 2024-03-14 | 2024-04-16 | 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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