Propylene carbonylation reaction device
By employing an external circulation heat transfer system and a static mixer in the propylene carbonylation reactor, the problems of reactor temperature fluctuation and high maintenance difficulty were solved, achieving stable temperature control and improved reaction efficiency, simplifying the equipment structure and reducing costs.
Patent Information
- Application Number
- CN202423093739.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-16
- Publication Date
- 2025-12-02
- Estimated Expiration
- 2034-12-16
AI Technical Summary
In existing propylene carbonylation reaction processes, the reactor temperature fluctuates greatly, temperature control is difficult, the equipment structure is complex, maintenance is difficult, and there are problems with stirring and sealing leakage.
An independent external circulation heat transfer system and a static mixer are used to regulate the temperature of the first and second reactors respectively. The internal coil is removed, and a mixer is used instead of a stirrer to achieve stable control of the reaction temperature and thorough mixing of materials.
It reduces the reactor's heat load and maintenance difficulty, improves the reaction conversion rate, simplifies the equipment structure, reduces equipment investment and maintenance costs, and avoids stirring seal leakage.
Smart Images
Figure CN223615882U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of chemical synthesis technology, specifically to a propylene carbonylation reaction apparatus. Background Technology
[0002] Butanol and octanol are important raw materials for basic organic synthesis, mainly used in the production of plasticizers, solvents, dehydrating agents, defoamers, dispersants, flotation agents, petroleum additives, and synthetic fragrances. The wide range of applications of butanol and octanol has led to a year-on-year increase in their usage and production.
[0003] The low-pressure carbonyl synthesis of propylene to produce butyraldehyde is the most widely used process in the production of butanol and octanol. In this process, n-butyraldehyde is used as a solvent. Propylene reacts with syngas and hydrogen under the action of a catalyst to produce n-butyraldehyde and isobutyraldehyde. n- / isobutyraldehyde can be hydrogenated to produce n-butanol and isobutanol, which are then separated by distillation to obtain n-butanol and isobutanol products. Alternatively, n- / isobutyraldehyde can be separated into n-butyraldehyde and isobutyraldehyde by an isomerization column, with isobutyraldehyde as a byproduct. n-Butyraldehyde is condensed and dehydrated under the catalysis of sodium hydroxide to produce octenal. Octenal is hydrogenated to produce crude octanol, which is then distilled to obtain the product octanol.
[0004] The existing process flow for propylene carbonylation reaction is as follows: Figure 1 As shown. The core of the process is two carbonyl synthesis reactors, and the specific reaction process includes:
[0005] Syngas enters the first carbonyl synthesis reactor R-101 from below the impeller at the bottom of the stirrer. Propylene feed, reaction circulating liquid, and catalyst solution returned by circulating pumps P-101A / B are added to the first reactor R-101 between the two sets of impellers in the stirrer. The upper impeller generates axial flow, ensuring complete mixing of the solutions in the reactor and minimizing the temperature gradient. Since the carbonyl synthesis reaction is exothermic, the reaction solution is drawn from the bottom of the reactor using the first reactor circulating pumps P-101A / B and cooled by the first reactor's cooler E-101. A portion is returned to the first reactor, while the other portion passes through the internal coils of the second carbonyl synthesis reactor R-102 and returns to the first carbonyl synthesis reactor. The reaction liquid containing dissolved catalyst, byproducts and unreacted propylene from R-101 enters the second carbonyl synthesis reactor; the synthesis gas is mixed with the reaction tail gas from R-101 and enters the bottom of R-102 from the bottom of the impeller of the stirrer A-102 through the gas distributor; the purge gas discharged to the reactor vent condenser E-102 is condensed and discharged to the fuel gas main through the demister; butyraldehyde and other substances condensed in the reactor vent condenser return to R-102 under gravity.
[0006] In the actual process, due to the coordinated temperature control of the two reactors and the relatively complex equipment structure, the first carbonyl synthesis reactor has a large circulating heat load. Therefore, the propylene carbonylation reaction process is prone to problems such as large temperature fluctuations in the reactors, difficulty in adjusting the temperature of the two reactors, and high maintenance difficulty of the equipment. Utility Model Content
[0007] To address the shortcomings of existing technologies, this utility model discloses a propylene carbonylation reaction apparatus. This apparatus can independently control the temperature of each reactor, reducing temperature fluctuations and stabilizing production. The apparatus of this utility model has a simplified structure, effectively reducing equipment investment costs and equipment maintenance difficulties.
[0008] To achieve the above technical objectives, this utility model proposes a propylene carbonylation reaction apparatus, comprising:
[0009] The first reactor is provided with a lower feed port for inputting hydrogen and synthesis gas, an upper feed port for inputting propylene and catalyst solution, and the liquid outlet of the first reactor is connected to the upper feed port of the first reactor via a first condenser.
[0010] The second reactor includes a shell and a second mixer disposed within the shell; the second reactor is provided with a lower feed inlet for inputting hydrogen and syngas, and the liquid outlet of the second reactor is connected to the upper feed inlet of the second reactor via a second condenser;
[0011] The pipeline connecting the liquid outlet of the first reactor and the first condenser is provided with a first branch connecting to the upper feed inlet of the second reactor; the gas outlet of the first reactor is connected to the lower feed inlet of the second reactor; and the pipeline connecting the liquid outlet of the second reactor and the second condenser is provided with a second branch for outputting the reacted material.
[0012] In this invention, both the first and second reactors are equipped with independent external circulation heat transfer systems: the reactants in the first reactor are discharged from the liquid outlet, cooled by the first condenser, and then returned to the upper feed inlet, thereby achieving the purpose of regulating the reaction temperature in the first reactor; the reactants in the second reactor are discharged from their liquid outlet, cooled by the second condenser, and then returned to the upper feed inlet, achieving the purpose of efficiently regulating the reaction temperature in the second reactor. Compared with the prior art's technique of inputting part of the reactants from the first reactor into the coil inside the second reactor for coordinated temperature control, this invention reduces the heat load on the first reactor and achieves higher efficiency in temperature control of the second reactor, resulting in more stable overall process temperature control. Furthermore, this invention eliminates the difficult-to-maintain internal coil inside the second reactor, thus reducing the difficulty of process maintenance. In this invention, static mixing replaces the agitator in the second reactor, promoting material mixing, improving reaction efficiency, and avoiding the problem of leakage from the agitator seal.
[0013] The process for the propylene carbonylation reaction using this invention includes:
[0014] The reaction feedstocks, syngas and hydrogen, are fed into the first reactor from the bottom inlet and mixed with the circulating material fed into the top inlet after being heated by the first condenser. At the same time, the raw material propylene and catalyst solution are also fed into the first reactor from the top inlet. Most of the carbonylation reaction takes place in the first reactor to produce n-butyraldehyde and isobutyraldehyde.
[0015] The post-reaction materials from the first reaction (including catalyst solution, products, byproducts, and unreacted propylene) are fed into the second reactor through the upper inlet. Syngas, hydrogen, and unreacted gaseous materials from the first reactor are fed into the second reactor through the lower inlet. The materials fed into the second reactor are fully mixed by the second mixer and continue to undergo carbonylation reaction within the second reactor. During the reaction, some materials are discharged from the liquid outlet of the second reactor, condensed by the second condenser, and returned to the second reactor, thereby regulating the temperature within the reaction and improving the conversion rate.
[0016] Compared with the prior art, the beneficial effects of this utility model are as follows: The second reactor in the propylene carbonylation reaction device of this utility model is equipped with a separate external circulation heat transfer system, thereby realizing independent temperature control of the second reactor, reducing the circulating heat load of the first reactor, and which is conducive to the temperature control stability of the overall process; a mixer is set in the second reaction to replace the traditional agitator, which promotes the full mixing of the reactants, improves the reaction conversion rate, simplifies the process equipment, avoids the problem of stirring and sealing leakage, and reduces equipment investment and maintenance costs. Attached Figure Description
[0017] The accompanying drawings, which form part of this application, are used to provide a further understanding of the present invention. The illustrative embodiments of the present invention and their descriptions are used to explain the present invention and do not constitute an undue limitation of the present invention. In the drawings:
[0018] Figure 1 This diagram illustrates the structure of propylene carbonylation in the prior art.
[0019] The attached figure includes the following reference numerals: R-101 First carbonyl synthesis reactor, E-101 Cooler for the first reactor, P-101 A / B Circulation pump, R-102 Second carbonyl synthesis reactor, and E-102 Reactor vent condenser.
[0020] Figure 2 A structural diagram of the propylene carbonylation reaction apparatus of this invention is shown.
[0021] The above figures include the following reference numerals:
[0022] 1-First reactor, 11-First mixer, 2-Second reactor, 21-Second mixer, 31-First condenser, 32-Second condenser, 33-Third condenser, 41-First branch, 42-Second branch, 43-Third branch, 44-Fourth branch, 45-Fifth branch, 5-Gas distributor, 6-Condensate tank, 71-Level gauge, 72-First switch valve, 73-Second switch valve, 74-Thermometer. Detailed Implementation
[0023] To facilitate understanding of this utility model, a more comprehensive description of it will be provided below, along with preferred embodiments. However, it should be understood that these embodiments are merely for more detailed explanation and should not be construed as limiting the utility model in any way, i.e., not limiting the scope of protection of this utility model.
[0024] Unless otherwise defined, the technical terms used in the following embodiments have the same meanings as commonly understood by those skilled in the art to which this invention pertains. Unless otherwise specified, the experimental reagents used in the following embodiments are conventional biochemical reagents; and the experimental methods described are conventional methods.
[0025] Example 1
[0026] An apparatus for propylene carbonylation reaction, such as Figure 1 As shown, the device includes:
[0027] The first reactor 1 is provided with a lower feed port for inputting hydrogen and synthesis gas, an upper feed port for inputting propylene and catalyst solution, and the liquid outlet of the first reactor 1 is connected to the upper feed port of the first reactor 1 via a first condenser 31.
[0028] The second reactor 2 includes a shell and a second mixer 21 disposed inside the shell; the second reactor 2 is provided with a lower feed port for inputting hydrogen and synthesis gas, and the liquid outlet of the second reactor 2 is connected to the upper feed port of the second reactor 2 via a second condenser 32.
[0029] The pipeline connecting the liquid outlet of the first reactor 1 and the first condenser 31 is provided with a first branch 41 that connects to the upper feed inlet of the second reactor 2; the gas outlet of the first reactor 1 is connected to the lower feed inlet of the second reactor 2; and the pipeline connecting the liquid outlet of the second reactor 2 and the second condenser 32 is provided with a second branch 42 for outputting the reacted material.
[0030] Compared with the prior art, (1) the above technical solution removes the inner coil in the second reactor 2 and adds an external circulation reaction heat transfer system including the second condenser 32, thereby enhancing the cooling and temperature reduction of the reactants in the second reactor 2 and reducing the temperature fluctuation of the first reactor 1, thus stabilizing production; in addition, the traditional inner coil heat transfer is very difficult to maintain, and removing it can increase the effective operating time. (2) The above technical solution uses a mixer to replace the agitator in the prior art, avoiding the problem of agitation seal leakage. At the same time, adding a mixer in the shell can make the reactants more fully mixed and improve the reaction conversion rate.
[0031] It should be noted that the present invention does not limit the source of the catalyst solution input into the first reactor 1. The catalyst solution may be selected from the downstream product-catalyst separation process, the catalyst washing process, or the catalyst preparation process, or a mixed catalyst solution from multiple sources.
[0032] It should be noted that this invention does not restrict the source of materials fed into the lower inlet of the second reactor 2, and the purpose of the lower inlet does not limit the scope of protection of this invention. If only propylene and syngas are used as raw materials in a specific carbonylation reaction, then the lower inlets of the first reactor and the second reactor 2 are used to feed syngas. If syngas and hydrogen are used as raw materials in a specific carbonylation reaction, then the lower inlets of the first reactor and the second reactor 2 are used to feed syngas and hydrogen. Alternatively, under specific operating conditions, the materials may be selected from newly input syngas and hydrogen, unreacted materials from the first reactor 1, separated gas from the subsequent product-catalyst separation process, etc., or a mixture of the above-mentioned sources. This does not limit the scope of protection of this invention.
[0033] Optionally, the lower feed inlet of the second reactor 2 includes two secondary feed inlets arranged at the top and bottom, which facilitates stratified control based on the different compositions of the gaseous materials input into the lower feed inlet of the second reactor 2 during the actual process, thereby improving the reaction efficiency within the second reactor 2.
[0034] It should be noted that the present invention does not limit the specific structure of the second mixer. Those skilled in the art can select components or devices that can promote material mixing based on the present invention. The second mixer may include several layers of porous distribution plates arranged vertically. The gaseous material for the reaction is input through a pipe connected to the bottom of the porous distribution plate, and the circulating liquid is input through a pipe connected to the top. Through reverse contact reaction, the reacted material flows out of the mixer laterally, thereby realizing the static mixing of the material input into the reactor.
[0035] Example 2
[0036] Based on the propylene carbonylation reaction apparatus shown in Example 1, the structure of the first reactor 1 has been optimized in this example.
[0037] Optionally, the first reactor 1 includes a shell and a first mixer 11 disposed inside the shell. Replacing the agitator provided in the first reactor 1 in the prior art with the first mixer 11 can avoid the problem of leakage of the agitator seal in the first reactor 1 and further improve the safety of the device.
[0038] It should be noted that this invention does not limit the specific structure of the first mixer. Those skilled in the art can select components or devices that can promote material mixing based on this invention to promote the static mixing of materials input into the reactor.
[0039] Example 3
[0040] Based on the propylene carbonylation reaction apparatus shown in Example 1 or Example 2, in this example, the lower feed inlet of the first reactor 1 and / or the second reactor 2 is connected to a gas distributor 5, thereby promoting thorough mixing of the gaseous raw material input from the lower feed inlet with the material in the reactor and improving the reaction efficiency.
[0041] Example 4
[0042] Based on the propylene carbonylation reaction apparatus shown in Example 1, this example optimizes the structure connected to the gas outlet of the second reactor 2.
[0043] Optionally, the gas phase outlet of the second reactor 2 is connected to the condensate tank 6 via the third condenser 33, so that the product entrained from the gas outlet is separated and condensed by the third condenser 33 for gas-liquid separation. The condensate obtained is collected in the condensate tank 6 and output from the outlet of the condensate tank 6, and then enters the downstream product-catalyst separation process. This can avoid the accumulation of propane entrained in butyraldehyde condensate after it is directly returned to the reactor, thereby improving the product yield.
[0044] Optionally, the condensate tank 6 is equipped with a level gauge 71, and a first switching valve 72 connected to the level gauge 71 is provided on the pipeline connected to the outlet of the condensate tank 6. The discharge of condensate is controlled by interlocking the level gauge 71 and the first switching valve 72, thereby improving the level of process automation.
[0045] Optionally, the gas phase outlet of the third condenser 33 and / or the gas phase outlet of the condensate tank 6 are connected to the fuel gas pipeline network, and the purge gas discharged from the third condenser 33 and the condensate tank 6 can be input into the subsequent fuel gas pipeline network for processing.
[0046] Example 5
[0047] Based on the propylene carbonylation reaction apparatus shown in Example 1, this example optimizes the connection structure of the second condenser 32.
[0048] Optionally, the front end of the second condenser 32 is provided with a third branch 43 connected to its rear end. The third branch 43 is provided with a second switching valve 73, so that the proportion of the material circulating outside the second reactor 2 that has been condensed by the second condenser 32 can be adjusted according to the working conditions during actual operation. Under certain special working conditions, the material output from the outlet of the second reactor 2 can be partially returned to the second reactor 2 without being condensed by the second condenser 32, thereby reducing process energy consumption and improving the operability of temperature regulation.
[0049] Optionally, a thermometer 74 connected to the second condenser 32 is provided on the pipeline connected to the second condenser 32, which is in signal communication with the second switching valve 73. This allows the present invention to automatically adjust the proportion of circulating material condensed by the second condenser 32 according to the temperature of the external circulating material in the specific working conditions.
[0050] Example 6
[0051] Based on the propylene carbonylation reaction apparatus shown in Example 1, in this embodiment, the rear end of the first condenser 31 is provided with a fourth branch 44 connected to its front end. The fourth branch 44 is used to partially mix the material condensed by the first condenser 31 with the material reacted in the first reactor 1 under certain operating conditions, so as to facilitate the control of the temperature in the first reactor 1.
[0052] In some optional embodiments of this utility model, an interlocked thermometer and a switching valve can be installed on the fourth branch 44 to facilitate the adjustment of the flow rate of the circulating material through the fourth branch 44 according to the temperature of the circulating material after condensation in the first condenser 31 and the temperature in the first reactor 1, thereby improving the convenience of process temperature regulation.
[0053] Example 7
[0054] Based on the propylene carbonylation reaction apparatus shown in Example 1, in this embodiment, the rear end of the second condenser 32 is provided with a fifth branch 45 connected to its front end. The fifth branch 45 is used to partially mix the material condensed by the second condenser 32 with the material reacted in the second reactor 2 under certain operating conditions, thereby facilitating the control of the temperature inside the second reactor 2.
[0055] In some optional embodiments of this utility model, an interlocked thermometer and a switching valve can be installed on the fifth branch 45 to facilitate the adjustment of the flow rate of the circulating material through the fifth branch 45 according to the temperature of the circulating material after condensation in the first condenser 31 and the temperature in the second reactor 2, thereby improving the convenience of process temperature regulation.
[0056] It should be noted that, in order to improve process efficiency, those skilled in the art may, based on this utility model, install devices or equipment such as circulating pumps or compressors on pipelines used for circulating liquid or gaseous materials to improve material flow efficiency, without limiting the scope of protection of this utility model.
[0057] It should be noted that, based on this utility model, those skilled in the art may choose to install a switch valve and interlocked thermometer, flow meter, pressure gauge, or level gauge, thermometer, pressure gauge, etc. on the material flow pipeline, or interlocked level gauge, thermometer, pressure gauge, etc. on the reactor, to facilitate the automated operation of this utility model, but this does not limit the scope of protection of this utility model.
[0058] It should be noted that the above description is a further detailed explanation of the present invention in conjunction with specific embodiments, and should not be construed as limiting the specific implementation of the present invention to these descriptions; the dimensional data in this embodiment do not limit the technical solution, but merely illustrate one specific working condition. For those skilled in the art to which this invention pertains, several simple improvements and modifications can be made without departing from the concept of the present invention, and all such improvements and modifications should be considered to fall within the scope of protection of the present invention.
Claims
1. A propylene carbonylation reaction apparatus, characterized in that, include: The first reactor (1) is provided with a lower feed port for inputting hydrogen and synthesis gas, and an upper feed port for inputting propylene and catalyst solution. The liquid outlet of the first reactor (1) is connected to the upper feed port of the first reactor (1) via a first condenser (31). The second reactor (2) includes a shell and a second mixer (21) disposed inside the shell; the second reactor (2) is provided with a lower feed port for inputting hydrogen and synthesis gas, and the liquid outlet of the second reactor (2) is connected to the upper feed port of the second reactor (2) via a second condenser (32); Among them, the pipeline connecting the liquid outlet of the first reactor (1) and the first condenser (31) is provided with a first branch (41) connecting the upper feed inlet of the second reactor (2); the gas outlet of the first reactor (1) is connected to the lower feed inlet of the second reactor (2); the pipeline connecting the liquid outlet of the second reactor (2) and the second condenser (32) is provided with a second branch (42) for outputting the reaction material.
2. The propylene carbonylation reaction apparatus according to claim 1, characterized in that, The first reactor (1) includes a shell and a first mixer (11) disposed within the shell.
3. The propylene carbonylation reaction apparatus according to claim 1 or 2, characterized in that, The lower feed inlet of the first reactor (1) and / or the second reactor (2) is connected to a gas distributor (5).
4. The propylene carbonylation reaction apparatus according to claim 1, characterized in that, The gas phase outlet of the second reactor (2) is connected to the condensate tank (6) via the third condenser (33).
5. The propylene carbonylation reaction apparatus according to claim 4, characterized in that, The condensate tank (6) is equipped with a level gauge (71), and a first switching valve (72) connected to the level gauge (71) is provided on the pipeline connected to the outlet of the condensate tank (6).
6. The propylene carbonylation reaction apparatus according to claim 4 or 5, characterized in that, The gas phase outlet of the third condenser (33) and / or the gas phase outlet of the condensate tank (6) are connected to the fuel gas pipeline network.
7. The propylene carbonylation reaction apparatus according to claim 1, characterized in that, The front end of the second condenser (32) is provided with a third branch (43) connected to its rear end, and a second switching valve (73) is provided on the third branch (43).
8. The propylene carbonylation reaction apparatus according to claim 7, characterized in that, A thermometer (74) connected to the second switching valve (73) is provided on the pipeline connected to the second condenser (32).
9. The propylene carbonylation reaction apparatus according to claim 1, characterized in that, The first condenser (31) has a fourth branch (44) connected to its front end at its rear end. The fourth branch (44) is used to partially mix the material condensed by the first condenser (31) with the material reacted by the first reactor (1).
10. The propylene carbonylation reaction apparatus according to claim 1, characterized in that, The second condenser (32) has a fifth branch (45) connected to its front end at the rear end. The fifth branch (45) is used to partially mix the material condensed by the second condenser (32) with the material reacted by the second reactor (2).