A microchannel catalytic module, a microchannel reactor and a method for producing succinic anhydride

CN122141675APending Publication Date: 2026-06-05CHINA PETROLEUM & CHEMICAL CORP +2
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
CHINA PETROLEUM & CHEMICAL CORP
Filing Date
2024-12-05
Publication Date
2026-06-05

AI Technical Summary

Technical Problem

In the existing technology, maleic anhydride hydrogenation reactors have problems such as low heat exchange efficiency, complex reactor design, high manufacturing difficulty, and are not suitable for gas-liquid-solid three-phase reactions.

Method used

By employing a microchannel catalytic module and reaction device, and utilizing the efficient heat and mass transfer capabilities of the microchannel reactor, a gas-liquid-solid three-phase maleic anhydride hydrogenation reaction is achieved, thus solving the problem of difficulty in heat extraction during the maleic anhydride hydrogenation reaction.

Benefits of technology

This enabled more precise reaction control, improved maleic anhydride conversion and succinic anhydride selectivity, and reduced production energy consumption and equipment investment.

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Abstract

Provided are a micro-channel catalytic module and a micro-channel reaction device comprising the same, which are obtained by mixing a binder, a pore-forming agent, a precursor and water, introducing CO2 to obtain a catalytic slurry, freeze-drying, and calcining to obtain a shaped catalytic module carrier; impregnating an active component, drying, and calcining to obtain an oxidation state catalytic module. The micro-channel reaction device comprises the micro-channel catalytic module as a reaction micro-channel, and liquid and / or gaseous materials pass through and undergo catalytic reaction. The micro-channel reaction device of the present application can realize production of succinic anhydride from maleic anhydride, realize gas-solid-liquid three-phase reaction, solve the problem of difficult heat removal in the reaction of maleic anhydride hydrogenation, can more accurately control the reaction conditions, reduce side reactions, and improve conversion rate and selectivity.
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Description

Technical Field

[0001] This invention relates to microchannel reaction apparatus, particularly a microchannel reaction apparatus packed with a catalytic module, and a method for producing succinic anhydride using the same. Background Technology

[0002] Succinic anhydride is an important chemical raw material. It is widely used in pharmaceuticals, pesticides, coatings, food, agriculture, petrochemicals, corrosion protection, gas purification, textiles, plastics, and scientific research.

[0003] The main production methods for succinic acid include succinic acid dehydration, direct oxidation of cyclohexane, homogeneous catalytic reaction of maleic anhydride, and heterogeneous catalytic reaction of maleic anhydride, among which the heterogeneous catalytic reaction of maleic anhydride has attracted the most attention. However, the maleic anhydride hydrogenation reaction releases a large amount of heat, leading to a rise in reactor temperature and affecting the selectivity of succinic anhydride in the maleic anhydride hydrogenation reaction. Therefore, solving the heat removal problem in the maleic anhydride hydrogenation reaction is key to the industrial application of the technology. US2245404(A) discloses a method for removing the heat of the maleic anhydride hydrogenation reaction using an internal heat exchanger tube, thereby controlling the temperature rise of the catalyst bed. However, this method cannot uniformly remove the heat of reaction and also affects the distribution of the reaction liquid within the reactor, thus affecting the catalyst's reaction performance. Therefore, this method is not suitable for heat removal in large-scale reaction plants.

[0004] CN101891718A discloses a continuous production process for maleic anhydride to succinic anhydride via hydrogenation. Maleic anhydride and a solvent are dissolved and reacted in a trickle-bed reactor. After gas-liquid separation, the finished succinic anhydride is obtained, and the separated solvent is recovered. This method has significant advantages over batch stirred tank processes, effectively improving production efficiency. However, the reaction pressure is relatively high (2.0-8.0 MPa), resulting in high energy consumption, and it cannot effectively address the strong exothermic effect of the maleic anhydride hydrogenation reaction to succinic anhydride.

[0005] CN202111249887.4 discloses a method and reactor for the hydrogenation reaction of maleic anhydride. Its characteristic is that maleic anhydride feedstock and hydrogen gas enter the first hydrogenation reaction section of the hydrogenation reactor. The reactants exiting the first hydrogenation reaction section are led out of the reactor, cooled, and then returned to the next hydrogenation reaction section, until the hydrogenation reaction is completed in each section. This method requires the installation of a cooler in the middle of the reactor, the loading process is complex, and the reactor design and fabrication are difficult.

[0006] CN202111249891.0 discloses a tubular reactor for preparing succinic anhydride and a method for preparing succinic anhydride. The method is characterized by a tubular reactor where the tubes are used for the hydrogenation reaction of maleic anhydride feedstock to prepare succinic anhydride, and a shell is used for the flow of a cooling medium. A feedstock heat exchanger is connected to the liquid inlet at the bottom of the tubes; a gas-liquid separator inlet is connected to the outlet at the top of the tubes; the gas phase outlet at the top of the gas-liquid separator is connected to the gas phase inlet at the bottom of the tubes; and a cooling medium storage tank is used to provide cooling medium to the shell. The tubular reactor used in this method suffers from uneven gas-liquid distribution, which is detrimental to the complete conversion of maleic anhydride. To ensure the conversion rate of maleic anhydride, a large amount of hydrogen is required for circulation (the molar ratio of hydrogen to maleic anhydride is 15).

[0007] Microchannel reactors possess excellent heat and mass transfer properties, making them particularly suitable for highly exothermic reactions. They are generally used for gas-phase or liquid-phase reactions. For example, patent CN202111520982.3, "A Process System and Preparation Method for Synthesizing Acetic Acid or Acetic Anhydride Using a Microchannel Reactor," mentions a microchannel gas-liquid mixing hydrogenation method using a liquid catalyst. Patent 201910148773.7, "An Integrated Oxygen- and Hydrogen-Permeable Catalytic Membrane Microreactor for the One-Step Oxidation of Benzene to Phenol," assembles a hydrogen-permeable membrane, an oxygen-permeable membrane, and a titanium-silicon molecular sieve into a catalytic membrane microreactor for the one-step oxidation of benzene to phenol. This method involves a complex reactor structure, making the fabrication of microchannel membrane reactors difficult, and is, in principle, also a gas-liquid reaction. It is not suitable for gas-liquid-solid three-phase reactions.

[0008] Most existing technologies suffer from low heat exchange efficiency, leading to low efficiency in the maleic anhydride hydrogenation reaction. To improve heat extraction efficiency during the reaction, improved technologies employ complex reactor designs, which also introduce problems such as uneven gas-liquid distribution, complex reactor design, and high manufacturing difficulty. While microchannel reaction technology has excellent mass and heat transfer efficiency, it is mainly applicable to gas-phase reactions, liquid-phase reactions, and gas-liquid mixed reactions, and has not been seen in the three-phase gas-liquid-solid maleic anhydride hydrogenation reaction. Summary of the Invention

[0009] To address the shortcomings of existing technologies, this invention provides a microchannel catalytic module, a microchannel reaction device, and a method for producing succinic anhydride. Utilizing the efficient heat and mass transfer capabilities of the microchannel reactor, and through the design of the catalytic module and microchannel device, a gas-liquid-solid three-phase maleic anhydride hydrogenation reaction is achieved, solving the problems of difficulty in heat extraction, large investment in production equipment, and high energy consumption in existing technologies for maleic anhydride hydrogenation reactions.

[0010] To achieve the above technical objectives, the technical solution of the present invention is as follows:

[0011] The first aspect of the technical objective of this invention is to provide a method for preparing a microchannel catalytic module, comprising:

[0012] (1) A binder, a pore-forming agent, a precursor, and water are mixed to obtain a gel slurry; wherein the precursor is selected from at least one of alumina, zirconium oxide, kaolin, hydroxyapatite, and silica; the pore-forming agent is selected from at least one of citrate, dimethyl maleate, succinate, dimethyl terephthalate, and phthalate; CO2 is introduced into the gel slurry under stirring to obtain a catalytic slurry;

[0013] (2) The catalytic slurry obtained in step (1) is placed in a mold, freeze-dried to form a preform, and calcined to obtain a shaped catalytic module carrier;

[0014] (3) The active metal is loaded onto the catalyst module support of step (2) by impregnation, dried and calcined to obtain the oxidized catalyst module.

[0015] Furthermore, the binder is used to assist in the molding of catalyst powder, as is well known to those skilled in the art; specifically, it is selected from at least one of nitric acid, guar gum, chitin, cellulose, hydroxypropyl cellulose, polyvinylpyrrolidone, and polyvinyl alcohol.

[0016] Furthermore, the mixing ratio of the precursor / binder, pore-forming agent and water by weight is 100:1-10:3-15:100-300.

[0017] Furthermore, in step (2), during the freezing process of the catalytic slurry, CO2 and water are released slowly and sequentially under these conditions, forming microchannels in the substrate without disrupting the overall regularity of the catalytic functional modules or causing the catalyst channels to collapse. The amount of CO2 introduced is 5%-15% of the gel weight, and the introduction time is 60-120 minutes.

[0018] Furthermore, the freeze-drying temperature in step (2) is -10℃ to -40℃.

[0019] Furthermore, the roasting in step (2) is carried out at 400℃-900℃ for 12 hours.

[0020] Furthermore, the impregnation in step (3) adopts the equal volume impregnation method, in which the soluble salt containing the active metal is impregnated onto the catalyst module carrier in step (2) in equal volume.

[0021] Furthermore, the drying in step (3) is carried out at 70-180℃ for 6-24 hours. The calcination is carried out at 400-600℃ for 3-12 hours.

[0022] Furthermore, step (3) also includes a reduction process to obtain a reduced catalytic module, wherein the reduction process involves placing the catalytic module in a hydrogen atmosphere at 450-650°C for 3-24 hours. The reduced catalytic module needs to be stored under inert conditions.

[0023] Furthermore, the inert condition preservation involves immersing the reduced-state catalytic module in an inert solvent and then sealing it with nitrogen gas for preservation.

[0024] The second technical objective of this invention is to provide a microchannel catalytic module prepared using the above-described preparation method.

[0025] The microchannel catalytic module prepared in this invention has through-holes that allow liquids or gases to pass through and react on the catalyst surface. This microchannel catalytic module can realize liquid-solid reactions, gas-solid reactions, or gas-liquid-solid reactions.

[0026] The technical objective of the third aspect of this invention is to provide a microchannel reaction device, in which the microchannel catalytic module is used as a microchannel for the reaction, allowing liquid and / or gaseous materials to pass through and undergo a catalytic reaction.

[0027] Furthermore, the microchannel reaction device includes a sealed reactor shell, a gas-liquid mixer disposed at one end of the reactor shell, a reaction liquid distributor connected to the gas-liquid mixer, a reaction liquid distributor connected to a plurality of reaction liquid inlet components, the reaction liquid inlet components being connected to a product outlet component at the other end via a catalytic module tank, the product outlet component being connected to a reaction product collection tank, and also includes a cooling medium tank disposed around the microchannel catalytic modules, and necessary device connection components, wherein the catalytic module tank is filled with the microchannel catalytic modules.

[0028] Furthermore, the catalytic module tank has a length of 100.2mm-1000.2mm, a width of 3.2mm-20.2mm, and a thickness of 0.3mm-5.2mm.

[0029] The fourth aspect of this invention aims to provide a method for producing succinic anhydride. Hydrogen gas is introduced into the microchannel reaction device to adjust the pressure. A cooling medium is introduced into the cooling medium tank to adjust the reaction temperature. Maleic anhydride solution is mixed with hydrogen gas in a gas-liquid mixer, then enters the reaction liquid distributor. The reaction liquid enters the catalytic module tank through the reaction liquid inlet assembly to begin the reaction. The reaction product enters the reaction product collection tank through the product outlet assembly. A back pressure valve is connected to the exhaust gas outlet of the collection tank to stabilize the reactor pressure.

[0030] Furthermore, hydrogen gas is introduced to raise the pressure in the reactor to the reaction pressure, which is 1 MPa-6 MPa, and the hydrogen gas hourly space velocity is 30 h⁻¹. -1 -300h -1 The hydrogen consumption accounts for 1%-5% of the total hydrogen flow.

[0031] Furthermore, the maleic anhydride solution is a solution containing 5%-50% maleic anhydride by weight, and the solvent is selected from at least one of tetrahydrofuran, γ-butyrolactone, cyclohexane, benzene, toluene, and acetone.

[0032] Furthermore, the cooling medium is selected from at least one of methanol, ethanol, tetrahydrofuran, water, diethyl ether, acetone, ethyl acetate, ethylene glycol, dimethylformamide, ethylene glycol monomethyl ether, butanol, octanol, and octyl acetate. The temperature of the cooling medium is 40℃-180℃, and the cooling medium is circulated and cooled externally to the microchannel reactor using a conventional circulating pump and heat exchanger, which is well known to those skilled in the art and will not be described in detail.

[0033] Furthermore, the gas-liquid mixer is a device in the prior art that can achieve good gas-liquid mixing effect, and its selection is well known to those skilled in the art, with a microchannel mixer being preferred.

[0034] Furthermore, in the microchannel mixer, the reaction liquid enters an internal channel with a diameter of 0.5 mm to 2 mm, while the gas is dispersed into microbubbles by the microchannel dispersion module through an external channel with a diameter of 0.5 mm to 2 mm, permeating into the reaction liquid to form a uniform gas-liquid mixture. The microchannel dispersion module is made of alumina or sintered metal and has a controllable microchannel pore size distribution range.

[0035] Furthermore, the reactor inlet assembly is a gas-liquid distribution assembly with a micro-damper structure. The damper operates with a pressure difference of 1 MPa-MPa, and the average pressure difference generated by each damper is <0.1%, ensuring that the reactants are uniformly distributed in the reactor unit.

[0036] Furthermore, the microchannel catalytic module within the catalytic module tank has a length of 100mm-1000mm, a width of 3mm-20mm, and a thickness of 0.1mm-5mm. The microchannel catalytic module has a mesoporous structure with internal microchannel through-holes. The active metal on the microchannel catalytic module is nickel, or a combination of nickel and copper. The loading of the active metal, based on the total weight of the microchannel catalytic module, is 15-50%, preferably 15-35%.

[0037] Furthermore, the reactor outlet component is a component with back pressure function. The reactants react under pressure in the microchannel reactor. After the reactants pass through the reactor outlet component, the pressure decreases and they enter the reaction product collection tank. The average pressure difference between each back pressure reactor outlet component is <0.1%.

[0038] The technical solution of the present invention has the following advantages:

[0039] (1) The microchannel catalytic module prepared by the present invention has through-holes inside, which can be used as channels for reactants, providing a basis for realizing liquid-solid reaction, gas-solid reaction and gas-liquid-solid reaction.

[0040] (2) In order to solve the problem of heat transfer efficiency in the preparation of maleic anhydride from succinic anhydride, the present invention applies a microchannel reactor to this reaction and designs and prepares a corresponding microchannel catalytic module to realize the gas-solid-liquid three-phase reaction, which solves the problem of the difficulty in heat extraction in the hydrogenation reaction of maleic anhydride. It can more accurately control the reaction conditions, reduce side reactions, and improve the conversion rate and selectivity.

[0041] Other features and advantages of the present invention will be described in detail in the following detailed description section. Attached Figure Description

[0042] Figure 1 SEM image of the microchannel catalytic module prepared in Example 1;

[0043] Figure 2 The adsorption-desorption isotherms are for C1, C2, Z1, and Z2.

[0044] Figure 3 This is a schematic diagram of the microchannel reaction device in Example 3;

[0045] Figure 4 This is a cross-sectional view of the single-layer substrate of the microchannel reaction device in Example 3. Detailed Implementation

[0046] The following non-limiting embodiments are intended to enable those skilled in the art to more fully understand the invention, but do not limit the invention in any way.

[0047] Example 1

[0048] Preparation of microchannel catalytic modules:

[0049] (1) Weigh 1000g of hydrated alumina, 30g of guar gum powder, 20g of polyvinyl alcohol 800, and 10g of methyl citrate and place them in a stainless steel stirred tank. A vent pipe is installed at the bottom of the stirred tank. Then add 1600ml of an aqueous solution containing 10g of nitric acid, adjust the stirring speed to 550 / rpm, and introduce CO2 to mix the mixture evenly. After the slurry becomes viscous and a large number of microbubbles are generated on the surface, turn off the CO2 to obtain the catalytic slurry.

[0050] (2) Take a mold of 2mm×20mm×1000mm, coat the surface of the mold with dimethyl maleate, fill the mold with the catalytic slurry, freeze dry in a -30℃ freezer for 6 hours, take out the freeze-dried material, place it in a tube furnace for calcination, raise the temperature to 550℃ at a rate of 30℃ / h, and calcinate for 8 hours to obtain the catalytic module carrier Z1.

[0051] (3) The catalyst module support Z1 was impregnated with an equal volume of metal salt solution containing Ni and Cu, dried at 120℃ for 3 hours, and calcined at 420℃ for 2 hours to obtain an oxidized microchannel catalyst module, denoted as C1. The properties of the catalyst module are shown in Table 1.

[0052] Example 2

[0053] Preparation of microchannel catalytic modules:

[0054] (1) Weigh 1000g of hydrated alumina, 30g of hydroxypropyl cellulose, 20g of polyvinyl alcohol 2000, and 10g of monomethyl succinate and place them in a stainless steel stirred tank. A vent pipe is installed at the bottom of the stirred tank. Then add 1600ml of an aqueous solution containing 10g of nitric acid, adjust the stirring speed to 550 / rpm, and introduce CO2 to mix the mixture evenly. After the slurry becomes viscous and a large number of microbubbles are generated on the surface, turn off the CO2 to obtain the catalytic slurry.

[0055] (2) Take a mold of 2mm×20mm×1000mm, coat the surface of the mold with dimethyl maleate, fill the mold with the catalytic slurry, freeze dry in a -30℃ freezer for 6 hours, take out the freeze-dried material, place it in a tube furnace for calcination, raise the temperature to 550℃ at a rate of 30℃ / h, and calcinate for 8 hours to obtain the catalytic module carrier Z2.

[0056] (3) The support Z2 was impregnated with an equal volume of Ni-containing metal salt solution, dried at 120℃ for 3 hours, and calcined at 420℃ for 2 hours to obtain an oxidized microchannel catalytic module, denoted as C2. The properties of the catalytic module are shown in Table 1. Table 1.

[0057]

[0058] SEM images of the microchannel catalytic module prepared in Example 1 are shown below. Figure 1 The adsorption-desorption isotherms of C1, C2, Z1, and Z2 are shown below. Figure 2 ,from Figure 1 , Figure 2 It can be seen that the pore structure of the microchannel catalytic module is mesoporous, and the through-channels are at the micrometer level.

[0059] At 350–450 °C, catalyst modules C1 and C2 are reduced with hydrogen to reduce the active metal of the catalyst to a reduced state. After reduction, the catalyst is sealed and stored in ethanol for later use.

[0060] Example 3

[0061] Provide a microchannel reaction device, such as Figure 3 and 4As shown, the reactor includes a sealed reactor shell 4, a gas-liquid mixer 1 disposed at one end inside the reactor shell 4, a reaction liquid distributor 2 connected to the gas-liquid mixer 1, a reaction liquid distributor 2 connected to a plurality of reaction liquid inlet components 3, the reaction liquid inlet components 3 being connected to a product outlet component 6 at the other end via a catalytic module tank 12, the product outlet component 7 being connected to a reaction product collection tank 7, and a cooling medium tank 11 disposed on the back of the catalytic module tank 12, wherein the catalytic module tank 12 is filled with the microchannel catalytic module 5 prepared in Example 1 or 2.

[0062] Figure 4 This is a cross-sectional view of the single-layer substrate of the reactor. The reactor shell 8 is the sealed shell of the assembled microchannel reactor. The bottom and sides of the shell are made of metal plates, and the top is a sealed top plate. The interior of the shell is protected by pressurized inert gas to ensure the sealing effect of the microchannel reactor. The component connection slot 9 is a sealing slot on the single-layer substrate, which adopts a metal wire sealing structure to ensure that the two substrates are firmly assembled and have a good sealing effect. The component connection buckle 10 is a sealing slot on the single-layer substrate, which adopts a metal wire sealing structure to ensure that the two substrates are firmly assembled and have a good sealing effect. The cooling medium tank 11 is located on the back of the microchannel catalytic functional module tank, and its structure is the same as the back of the microchannel reaction tank. It is externally connected to the cooling medium inlet and cooling medium outlet.

[0063] Example 4

[0064] Preparation of succinic anhydride from maleic anhydride using a microchannel catalytic module (C1):

[0065] The reduced microchannel catalytic module C1 was filled into catalytic module tank 5, with a single catalytic module filling volume of 40 mL. A 5 wt% maleic anhydride / γ-butyrolactone solution was prepared and pumped into the microchannel reactor. A cooling medium was introduced, and the reaction temperature was controlled at 55 °C, hydrogen partial pressure at 1.0 MPa, hydrogen flow rate at 2.3 L / h, and reaction liquid flow rate at 40 mL / h. The reaction was carried out continuously for 240 h. Analysis showed that the conversion rate of maleic anhydride in the product was 99.9%, the selectivity of succinic anhydride was 98.6%, and the selectivity of GBL was 1.4%.

[0066] Example 5

[0067] Preparation of succinic anhydride from maleic anhydride using a microchannel catalytic module (C1):

[0068] The reduced microchannel catalytic module C1 was filled into catalytic module tank 5, with a single catalytic module filling volume of 40 mL. A 30 wt% maleic anhydride / γ-butyrolactone solution was prepared and pumped into the microchannel reactor. A cooling medium was introduced, and the reaction conditions were: reaction temperature 85℃, hydrogen partial pressure 3.0 MPa, hydrogen flow rate 4.5 L / h, reaction liquid flow rate 40 mL / h, and continuous reaction for 180 h. Analysis showed that the maleic anhydride conversion rate was 99.9%, the succinic anhydride selectivity was 97.5%, and the GBL selectivity was 2.5%.

[0069] Example 5

[0070] Preparation of succinic anhydride from maleic anhydride using a microchannel catalytic module (C2):

[0071] The reduced microchannel catalytic module C2 was filled into catalytic module tank 5, with a single catalytic module filling volume of 40 mL. A 50 wt% maleic anhydride / γ-butyrolactone solution was prepared and pumped into the microchannel reactor. A cooling medium was introduced, and the reaction conditions were: reaction temperature 99℃, hydrogen partial pressure 6.0 MPa, hydrogen flow rate 7.5 L / h, reaction liquid flow rate 40 mL / h, and continuous reaction for 168 h. Analysis showed that the average conversion rate of maleic anhydride was 99.9%, the selectivity of succinic anhydride was 93.7%, and the selectivity of GBL was 6.3%.

Claims

1. A method for preparing a microchannel catalytic module, comprising: (1) A binder, a pore-forming agent, a precursor and water are mixed to obtain a gel slurry; wherein the precursor is selected from at least one of alumina, zirconium oxide, kaolin, hydroxyapatite and silica; the pore-forming agent is selected from at least one of citrate, dimethyl maleate, succinate, dimethyl terephthalate and phthalate; CO2 is introduced into the gel slurry under stirring to obtain a catalytic slurry; (2) The catalytic slurry obtained in step (1) is placed in a mold, freeze-dried to form a preform, and then calcined to obtain a shaped catalytic module carrier; (3) The active metal is loaded onto the catalyst module support of step (2) by impregnation, dried and calcined to obtain the oxidized catalyst module.

2. The preparation method according to claim 1, characterized in that, The binder is selected from at least one of nitric acid, guar gum, chitin, cellulose, hydroxypropyl cellulose, polyvinylpyrrolidone, and polyvinyl alcohol.

3. The preparation method according to claim 1, characterized in that, The mixing ratio of the precursor, binder, pore-forming agent and water by weight is 100:1-10:3-15:100-300.

4. The preparation method according to claim 1, characterized in that, The amount of CO2 introduced is 5%-15% of the gel weight, and the introduction time is 60-120 minutes.

5. The preparation method according to claim 1, characterized in that, The freeze-drying temperature in step (2) is -10℃ to -40℃; the roasting is carried out at 400℃-900℃ for 12 hours.

6. The preparation method according to claim 1, characterized in that, The drying in step (3) is performed at 70-180℃ for 6-24 hours; the calcination is performed at 400-600℃ for 3-12 hours.

7. The preparation method according to claim 1, characterized in that, Step (3) also includes a process of reducing the catalyst module to a reduced state, wherein the reduction process involves placing the catalyst module in a hydrogen atmosphere and reducing it at 450-650°C for 3-24 hours.

8. The microchannel catalytic module prepared by the preparation method according to any one of claims 1-7.

9. A microchannel reaction device, characterized in that, The microchannel catalytic module described in claim 8 is used as a microchannel for the reaction, allowing liquid and / or gaseous materials to pass through and undergo a catalytic reaction.

10. The microchannel reaction device according to claim 1, characterized in that, It includes a sealed reactor shell, a gas-liquid mixer disposed at one end inside the reactor shell, a reaction liquid distributor connected to the gas-liquid mixer, a reaction liquid distributor connected to a plurality of reaction liquid inlet components, the reaction liquid inlet components being connected to a product outlet component at the other end via a catalytic module tank, the product outlet component being connected to a reaction product collection tank, and also includes a cooling medium tank disposed around the microchannel catalytic modules, and necessary device connection components, wherein the microchannel catalytic modules are filled in the catalytic module tank.

11. A method for producing succinic anhydride, characterized in that, Implemented within the microchannel reaction apparatus of claim 10.

12. The method according to claim 11, characterized in that, The specific process is as follows: Hydrogen gas is introduced into the microchannel reaction device to adjust the pressure, cooling medium is introduced into the cooling medium tank to adjust the reaction temperature, maleic anhydride solution and hydrogen gas are introduced into the gas-liquid mixer to mix, and then enter the reaction liquid distributor. The reaction liquid enters the catalytic module tank through the reaction liquid inlet component to start the reaction. The reaction product enters the reaction product collection tank through the product outlet component. A back pressure valve is connected to the exhaust gas outlet of the collection tank to stabilize the reactor pressure.

13. The method according to claim 12, characterized in that, Hydrogen gas is introduced to raise the pressure in the reactor to the reaction pressure, which is 1 MPa-6 MPa, and the hydrogen gas hourly space velocity is 30 h⁻¹. -1 -300h -1 .

14. The method according to claim 12, characterized in that, The maleic anhydride solution is a solution with a maleic anhydride weight percentage of 5%-50%, and the solvent is selected from at least one of tetrahydrofuran, γ-butyrolactone, cyclohexane, benzene, toluene and acetone.

15. The method according to claim 12, characterized in that, The cooling medium is selected from at least one of methanol, ethanol, tetrahydrofuran, water, diethyl ether, acetone, ethyl acetate, ethylene glycol, dimethylformamide, ethylene glycol monomethyl ether, butanol, octanol, and octyl acetate; the temperature of the cooling medium is 40℃-180℃.

16. The method according to claim 12, characterized in that, The microchannel catalytic module in the catalytic module tank has a length of 100mm-1000mm, a width of 3mm-20mm, and a thickness of 0.1mm-5mm; the microchannel catalytic module has a mesoporous structure and has microchannel through holes inside.

17. The method according to claim 12, characterized in that, The active metal on the microchannel catalytic module is nickel, or nickel and copper; the loading of the active metal is 15-50% based on the total weight of the microchannel catalytic module.

Citation Information

Patent Citations

  • Continuous production process for preparing succinyl oxide by maleic anhydride hydrogenation

    CN101891718A

  • An integrated oxygen- and hydrogen-permeable catalytic membrane microreactor for the production of phenol from benzene.

    CN109745933B

  • A process system and preparation method for synthesizing acetic acid or acetic anhydride using a microchannel reactor.

    CN114031492B

  • Maleic anhydride hydrogenation reaction method and maleic anhydride hydrogenation reactor

    CN116020351A

  • Tubular reactor for preparing butanedioic anhydride and method for preparing butanedioic anhydride

    CN116020355A