Special equipment for maleic anhydride hydrogenation

By designing a reactor for the three-stage blade structure, reaction jacket and catalyst filter, the problems of decreased selectivity and strong exothermic in the maleic anhydride hydrogenation process are solved, and high selectivity and stable hydrogenation reactions are achieved, avoiding equipment wear and overtemperature accidents.

CN223042673UActive Publication Date: 2025-07-01YUNNAN DAWEI HENGYUAN CHEM CO LTD
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Patent Information

Application Number
CN202422147500.X
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-09-03
Publication Date
2025-07-01
Estimated Expiration
2034-09-03

AI Technical Summary

Technical Problem

Most of the existing maleic anhydride hydrogenation processes are solvent methods, which lead to a decrease in selectivity and high catalyst stability requirements. The hydrogenation reaction is a strong exothermic reaction, and special equipment is required to balance and release energy.

Method used

A reactor including a three-stage blade structure was designed. The air inlet holes of the blades were balanced according to the feed amount, equipped with a reaction jacket and a catalyst filter, and magnetic drive and static sealing, combined with electromagnetic control to achieve stable and safe reaction.

Benefits of technology

The high selectivity and conversion rate of the solvent-free hydrogenation process of the manic anhydride is achieved, which avoids equipment wear and overtemperature accidents, and ensures the stability and safety of the reaction.

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Abstract

The utility model discloses special equipment for maleic anhydride hydrogenation, which comprises a power assembly, a reaction assembly and a protection assembly, and is characterized in that the reaction assembly adopts the structure that a closed reaction kettle consists of a kettle cover and a kettle body, an air vent is formed in the kettle cover, a stirrer is arranged in the kettle body, and the protection assembly is arranged in the kettle body; a lower stirring shaft of the stirrer is connected with a stirring shaft of the power assembly through a coupler; a paddle of the stirrer is divided into three sections and is mounted on the lower stirring shaft, and the paddle is of a porous structure; a reaction jacket is arranged outside the kettle body, the reaction jacket is filled with heating medium steam or heat-conducting oil in a reaction temperature rising and controlling stage, and when the reaction temperature exceeds a dangerous temperature critical value, a refrigerant is introduced through an electromagnetic valve for cooling, so that the effect of safe temperature control is achieved. The device is applied to a new maleic anhydride solvent-free method direct catalytic hydrogenation process, and can realize faster reaction rate, control reaction heat preservation, balance and release energy released in the reaction process, and avoid overtemperature accidents.
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Description

Technical Field

[0001] The utility model belongs to the organic synthesis hydrogenation process equipment in the chemical industry field, and particularly relates to a special equipment for directly catalytic hydrogenation of maleic anhydride without solvent method. Background Art

[0002] At present, the mature maleic anhydride hydrogenation processes on the market are all solvent method liquid-phase hydrogenation, which requires a large amount of solvent. Removing the solvent requires a large amount of heat and multiple-stage reactions, resulting in a decrease in selectivity and higher requirements for the stability of the catalyst. In view of this, the applicant has developed a bulk method hydrogenation process (i.e., direct catalytic hydrogenation of maleic anhydride without solvent method) and a catalyst. The bulk method hydrogenation process has higher selectivity and conversion rate, but has higher requirements for the reaction equipment and requires special design to meet its requirements. Since the applicant's developed bulk method hydrogenation process has a large amount of maleic anhydride added during the hydrogenation process, and the catalyst has high activity, the hydrogenation reaction is a strong exothermic reaction, so it is necessary to balance and release the energy released during the reaction process. The utility model is a special equipment for maleic anhydride hydrogenation designed to meet the bulk method hydrogenation process and catalyst. Summary of the Utility Model

[0003] The purpose of the utility model is to provide a special equipment for maleic anhydride hydrogenation.

[0004] The purpose of the utility model is realized as follows: A special equipment for maleic anhydride hydrogenation includes a power component, a reaction component and a protection component. The reaction component is characterized in that it consists of a kettle cover and a kettle body to form a closed reaction kettle. There is a vent on the kettle cover, and there is a stirrer in the kettle body. The lower stirring shaft of the stirrer is connected to the stirring shaft of the power component through a coupling; the blades of the stirrer are installed in three sections on the lower stirring shaft, and the blades are of porous structure; there is a reaction jacket outside the kettle body. During the reaction heating and temperature control stage, the reaction jacket is filled with hot medium steam or heat transfer oil. When the reaction temperature exceeds the critical dangerous temperature, the solenoid valve is used to introduce refrigerant to cool down to achieve the effect of safe temperature control.

[0005] The purpose of the utility model can also be realized as follows: For the three-section blades of the stirrer, the sizes of the air inlets of each section of the blade are different. The design requirement is that according to the rated feeding amount of maleic anhydride, by calculating the pressure generated by maleic anhydride on the air inlet, each layer of the blade can maintain balance and stability during operation, so as to promote the stable reaction of the system.

[0006] A catalyst filter with a pore diameter <= 5μm is provided on the blade of the stirrer to prevent small catalyst particles from entering the blade and the shaft to cause mechanical wear.

[0007] The described power assembly includes an outer rotating body, an inner rotating body, inner bearing ceramics, and a stirring shaft. Both the outer rotating body and the inner rotating body are multi-group tile-shaped rare earth permanent magnet materials. The outer rotating body transmits the power of the motor to the inner rotating body through the magnetic force passing through the sealing cover, and then the inner rotating body transmits it to the stirring shaft to achieve magnetic drive for non-contact torque transmission. The inner rotating body is sealed within the reactor sealing system by the sealing cover, and static sealing is achieved relying on the sealing cover.

[0008] The end bearing of the stirring shaft of the described power assembly adopts a labyrinth seal structure.

[0009] The described power assembly is directly connected to the motor and the reducer in a straight connection structure.

[0010] The described power assembly is controlled by electricity, with a frequency of 0 - 60 Hz.

[0011] The described protection assembly includes a pressure gauge, a safety manhole, a lifting lug, and a blind plate. The pressure gauge is connected to the parameter interface of the control panel to monitor the pressure inside the kettle in real time.

[0012] The utility model has the following beneficial effects: The utility model is specially designed according to the process characteristics of the direct catalytic hydrogenation process of maleic anhydride without solvent and the specific situation of the catalyst used. It has been proved by experiments that it can meet the production process requirements.

[0013] In the process of direct catalytic hydrogenation of maleic anhydride without solvent, the addition amount of maleic anhydride is relatively large, and the catalyst has high activity. It is necessary to quickly balance and release the energy released during the reaction. Therefore, the design features of the present utility model are as follows: 1) Blades are arranged in three sections on the stirring shaft. According to the feeding amount of rated maleic anhydride, the sizes of the air inlets of each section of blades are different. By calculating the pressure generated by maleic anhydride on the air inlet, each layer of blades can maintain balance and stability during operation, thereby promoting the stable reaction of the system. The stirring blades are of porous structure, which can allow the gas to better contact with liquid maleic anhydride along with the movement of the blades, achieving a faster reaction rate. 2) A reaction jacket is added outside the reaction kettle, and a water inlet and a water outlet are provided. During the reaction, low-pressure steam is introduced for heat preservation. When the temperature exceeds the limit, the valve is cut off and cooling water is introduced for cooling to ensure the safety of the reaction. 3) According to the current situation that the catalyst used has small particles, a catalyst filter is arranged on the blade, and its pore diameter <= 5μm, which can prevent small catalyst particles from entering the blade and the shaft to cause mechanical wear, thereby protecting the equipment. 4) In the power assembly, multiple groups of tile-shaped rare earth permanent magnetic materials are used to form an inner rotating body and an outer rotating body, and the power is transmitted through the magnetic force through the sealing cover body. The inner rotating body is sealed in the reaction kettle sealing system by the sealing cover body and rotates synchronously with the outer rotating body. The equipment relies on the sealing cover body to achieve static sealing. Due to the use of static sealing, high pressure resistance, zero leakage and no pollution are achieved. At the same time, magnetic drive belongs to non-contact torque transmission, which can effectively avoid phenomena such as overload and vibration, and effectively protect the equipment. 5) In terms of structural design, the motor and the reducer are directly connected to the power assembly. The whole machine has a compact and reasonable structure, large stirring torque, stable and reliable operation, and small vibration and noise. Description of the Drawings

[0014] Figure 1 It is a schematic structural diagram of the present utility model.

[0015] Figure 2 It is a schematic structural diagram of the power assembly.

[0016] The meanings of the symbols in the figure are as follows:

[0017] Power assembly 1: including outer rotating body 11, inner rotating body 12, cooling water joint 13, inner bearing ceramic 14, stirring shaft 15.

[0018] Reaction assembly 2: including kettle cover 21, coupling 22, lower stirring shaft 23, cooling pipe 24, blade 25, kettle body 26, reaction jacket 27, ventilation port 28.

[0019] Protection assembly 3: including pressure gauge 31, safety manhole 32, lifting lug 33, blind plate 34. Detailed Implementation Modes

[0020] The technical problem solved by the present utility model is as follows: In the process of hydrogenation in the maleic anhydride solvent-free direct catalytic hydrogenation process invented by the applicant, since the addition amount of maleic anhydride is relatively large during the hydrogenation process, and the catalyst has high activity, and the hydrogenation reaction is a strong exothermic reaction, it is necessary to balance and release the energy released during the reaction process. Based on this, the present utility model adopts a three-stage (or three-section type) blade structure. According to the feeding amount of rated maleic anhydride, the sizes of the air inlet holes of each stage of blades are different. By calculating the pressure generated by maleic anhydride on the air inlet, each layer of blades can maintain balance and stability during operation, thereby promoting the stable reaction of the system and ensuring the hydrogenation stability at various depths in the kettle. A jacket is added to the outer layer of the reaction kettle, and a water inlet and a water outlet are provided. During the reaction, low-pressure steam is introduced for heat preservation, and when the temperature exceeds the limit, the cut-off valve is used to introduce cooling water for cooling to ensure the safety of the reaction. According to the conditions of the existing catalyst, a catalyst filter with a pore diameter <= 5μm is provided on the blade of the present utility model, which can prevent small catalyst particles from entering the blade and the shaft to cause mechanical wear, thereby protecting the equipment.

[0021] In order to make the purpose, technical solution and advantages of the present utility model clearer, the following will further describe the specific embodiments of the present utility model in detail with reference to the accompanying drawings.

[0022] Figure 1 、 Figure 2 FIG. is a schematic structural diagram of a special equipment for maleic anhydride hydrogenation of the present utility model, which includes a power assembly 1 (also called a magnetic seal stirring assembly), a reaction assembly 2, and a protection assembly 3. The magnetic seal stirring assembly includes an outer rotating body 11, an inner rotating body 12, a cooling water joint 13, an inner bearing ceramic 14, and a stirring shaft 15. The reaction assembly includes a kettle cover 21, a coupling 22, a lower stirring shaft 23, a cooling pipe 24, a blade 25, a kettle body 26, a reaction jacket 27, and a ventilation port 28. The protection assembly 3 includes a pressure gauge 31, a safety manhole 32, a lifting lug 33, and a blind plate 34. The magnetic seal stirring assembly is controlled by electricity, with a frequency of 0 - 60 Hz. There are 3 air holes for the ventilation port 28 on the kettle cover 21, which are mainly used for introducing nitrogen, hydrogen, and connecting the vent pipe. The lifting lug 33 is used to fix the equipment on the steel platform to protect the stability of the equipment. The blade 25 of the stirrer is a porous structure, which is more conducive to the dispersion of gas in the liquid. There are four external flange ports on the reaction jacket 27, which can realize the control of reaction heat preservation and connect the solenoid valve to control the coolant. When the reaction temperature exceeds the set dangerous value, the cut-off valve controls the addition of the coolant for forced circulation to reduce the temperature in the reaction kettle and avoid over-temperature accidents.

[0023] The utility model relates to a special device for maleic anhydride hydrogenation, which comprises a power assembly, a reaction assembly and a protection assembly. It is characterized in that the reaction assembly is structured as a closed reaction kettle composed of a kettle cover 21 and a kettle body 26. An air vent 28 is arranged on the kettle cover 21, and a stirrer is arranged inside the kettle body 26. The lower stirring shaft 23 of the stirrer is connected to the stirring shaft 15 of the power assembly through a coupling 22; the paddle blades 25 of the stirrer are installed on the lower stirring shaft 23 in three sections, and the paddle blades 25 are of a porous structure; a reaction jacket 27 is arranged outside the kettle body 26. During the reaction heating and temperature control stage, heat medium steam or heat-conducting oil is filled in the reaction jacket 27. When the reaction temperature exceeds the critical dangerous temperature, a refrigerant is introduced through a solenoid valve to cool down to achieve the effect of safe temperature control.

[0024] For the three-section paddle blades 25 of the stirrer, the sizes of the air inlet holes of each section of paddle blade 25 are different. The design requirement is that according to the rated feeding amount of maleic anhydride, by calculating the pressure generated by maleic anhydride on the air inlet, each layer of paddle blade can maintain balance and stability during operation, so as to promote the stable reaction of the system.

[0025] A catalyst filter is arranged on the paddle blade 25 of the stirrer, and its pore diameter <= 5μm to prevent small catalyst particles from entering the paddle blade and the shaft to cause mechanical wear.

[0026] The power assembly includes an outer rotating body 11, an inner rotating body 12, an inner bearing ceramic 14, and a stirring shaft 15. Both the outer rotating body 11 and the inner rotating body 12 are multi-group tile-shaped rare earth permanent magnet materials. The outer rotating body 11 transmits the power of the motor to the inner rotating body 12 through the magnetic force through the sealing cover body, and then the inner rotating body 12 transmits it to the stirring shaft 15 to realize the magnetic drive of non-contact torque transmission; the inner rotating body 12 is sealed in the reaction kettle sealing system by the sealing cover body, and static sealing is realized by relying on the sealing cover body.

[0027] The lower support end bearing of the stirring shaft 15 of the power assembly adopts a labyrinth seal structure.

[0028] The power assembly is directly connected to the motor and the speed reducer.

[0029] The power assembly is controlled by electricity, and the frequency is 0 - 60Hz.

[0030] The protection assembly includes a pressure gauge 31, a safety manhole 32, a lifting lug 33 and a blind plate 34. The pressure gauge 31 is connected to the parameter interface of the control panel to monitor the pressure in the kettle in real time.

[0031] The working process of the present utility model is as follows: The maleic anhydride raw material is transported into the reaction kettle through a metering pump via a pipeline. The catalyst in the required proportion is added through the safety manhole 32. Nitrogen replacement is carried out 3 times through the nitrogen inlet and the vent, and then hydrogen replacement is carried out 3 times through the hydrogen inlet and the vent. Steam is introduced into the reaction jacket 27 to heat up the reaction system. After reaching the target temperature, the magnetic seal stirring assembly 1 is started. After setting the corresponding frequency of 50 Hz, hydrogen is introduced until the set pressure is reached, and the reaction starts. After reacting for a certain period of time according to the process requirements and passing the sampling analysis, the reaction liquid is transported to the next process. During this period, the relevant parameters of the monitoring and protection assembly 3 are monitored through the control panel and necessary adjustments are made according to the situation. Since the new process of direct catalytic hydrogenation of maleic anhydride without solvent uses a catalyst in the form of small particles with d < 50 μm, a catalyst filter with a pore diameter <= 5 μm is provided on the impeller to prevent small catalyst particles from entering the impeller and the shaft, causing mechanical wear, and thus protecting the equipment.

[0032] The pressure gauge 31 on the reaction kettle is connected to the parameter interface of the control panel to monitor the pressure in the reaction kettle in real time and prevent overpressure accidents. Emergency cut-off valves and bypasses are provided on the inlet pipelines of the kettle. When the temperature or pressure in the equipment exceeds the limit, the solenoid valve works to control the stop of the continuous entry of hydrogen and the progress of the external-controlled reaction, achieving safer use. At the same time, there are four external flange ports on the reaction jacket, which can realize the left and right of the reaction heat preservation and connect the solenoid valve to control the coolant. When the reaction temperature exceeds the set dangerous value, the cut-off valve controls the addition of the coolant for forced circulation to reduce the temperature in the reaction kettle and avoid over-temperature accidents.

Claims

1. A special equipment for hydrogenation of maleic anhydride, comprising a power component, a reaction component and a protection component, characterized in that the reaction component structure is a closed reactor composed of a reactor cover and a reactor body, the reactor cover is provided with a vent, a stirrer is provided in the reactor body, and the lower stirring shaft of the stirrer is connected to the stirring shaft of the power component through a coupling; the paddles of the stirrer are installed on the lower stirring shaft in three sections, and the paddles are of a porous structure; a reaction jacket is provided outside the reactor body, and the reaction jacket is filled with heat medium steam or heat transfer oil in the reaction temperature rising and temperature control stage, and when the reaction temperature exceeds the critical dangerous temperature, a solenoid valve is used to introduce a refrigerant to cool down the reaction to achieve a safe temperature control effect.

2. A special equipment for hydrogenation of maleic anhydride according to claim 1, characterized in that: The three-stage paddle of the agitator has different air inlet sizes on each paddle. The design requirement is that, based on the rated maleic anhydride feed amount, by calculating the pressure exerted by maleic anhydride on the air inlet, each layer of the paddle can maintain balance and stability during operation, thereby promoting the stable reaction of the system.

3. A special equipment for hydrogenation of maleic anhydride according to claim 1 or 2, characterized in that: The paddles of the stirrer are provided with catalyst filters, the pore size of which is less than or equal to 5 μm, so as to prevent small catalyst particles from entering the paddles and the shaft and causing mechanical wear.

4. A special equipment for hydrogenation of maleic anhydride according to claim 1, characterized in that: The power assembly includes an outer rotor, an inner rotor, an inner bearing ceramic, and a stirring shaft. The outer rotor and the inner rotor are both made of multiple groups of tile-shaped rare earth permanent magnet materials. The outer rotor uses magnetic force to transmit the power of the motor to the inner rotor through a sealing cover, and then the power is transmitted to the stirring shaft by the inner rotor, thereby realizing magnetic drive without contact torque transmission. The inner rotor is sealed in the reactor sealing system by the sealing cover, and static sealing is achieved by relying on the sealing cover.

5. A special equipment for hydrogenation of maleic anhydride according to claim 4, characterized in that: The lower support end bearing of the stirring shaft of the power assembly adopts a labyrinth seal structure.

6. A special equipment for hydrogenation of maleic anhydride according to claim 4 or 5, characterized in that: The power assembly, the motor and the reducer adopt a direct connection structure.

7. A special equipment for hydrogenation of maleic anhydride according to claim 4 or 5, characterized in that: The power assembly is electronically controlled with a frequency of 0-60 Hz.

8. The special equipment for hydrogenation of maleic anhydride according to claim 6, characterized in that: The power assembly is electronically controlled with a frequency of 0-60 Hz.

9. The special equipment for hydrogenation of maleic anhydride according to claim 1, characterized in that: The protection components include a pressure gauge, a safety manhole, a lifting lug and a blind plate. The pressure gauge is connected to a parameter interface of a control panel to monitor the pressure in the kettle in real time.

10. A dedicated equipment for hydrogenation of maleic anhydride according to claim 2, 4, 5 or 8, characterized in that: The protection components include a pressure gauge, a safety manhole, a lifting lug and a blind plate. The pressure gauge is connected to a parameter interface of a control panel to monitor the pressure in the kettle in real time.