Hydrogenation reaction tube, continuous hydrogenation production device and hydrogenation method
By installing an overflow pipe and a spiral pipe inside the hydrogenation reaction tube, combined with a gas distributor and a separator, the gas, liquid, and solid phases are fully mixed, solving the problems of high cost, high safety risk, and low yield of existing hydrogenation equipment, and realizing efficient and safe continuous hydrogenation production.
Patent Information
- Application Number
- CN202310820112.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-07-06
- Publication Date
- 2026-02-24
- Estimated Expiration
- 2043-07-06
AI Technical Summary
Existing intermittent hydrogenation equipment is costly, poses significant safety risks, produces poor product quality, and has low yields. Furthermore, continuous hydrogenation reactors suffer from severe side reactions under high temperature and pressure, leading to system safety issues.
Design a hydrogenation reaction tube comprising a reaction tube body, an overflow pipe, and a spiral tube, combined with a gas distributor and a separator to achieve thorough mixing of the gas, liquid, and solid phases. Improve reaction efficiency through the overflow pipe and spiral tube structure, and realize the recycling of catalyst and hydrogen.
It improves the efficiency of hydrogenation reaction, reduces equipment costs and safety risks, increases product yield, simplifies operation procedures, and is suitable for large-scale production.
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Figure CN116786039B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of chemical technology, and in particular to hydrogenation reaction tubes, continuous hydrogenation production equipment, and hydrogenation methods. Background Technology
[0002] Hydrogenation is one of the most important reaction processes in the chemical and petroleum refining industries. Common hydrogenation processes can be batch or continuous. Batch hydrogenation often uses pressure vessels or bubbling reactors with stirring devices, while continuous liquid-phase hydrogenation can use trickle bed reactors or tubular reactors with continuous gas-liquid-solid flow in the same direction. Because hydrogenation reactions require high pressure and efficient stirring, batch hydrogenation units need high-pressure designs, high stirring speeds, and good system sealing, resulting in high equipment design and manufacturing costs, large initial investments, and high daily maintenance costs. Intermittent hydrogenation has relatively long reaction times and is prone to side reactions under high temperature and pressure, resulting in low product content, poor quality, and low yield. Furthermore, hydrogenation reduction under high temperature and pressure involves vigorous reactions, large quantities of materials in the system, and potentially hazardous materials such as catalysts and hydrogen, posing significant safety risks to the reaction system. In addition, the output of a single pressure vessel is low, and large-scale production requires a large investment in equipment. Therefore, this applicant proposes a hydrogenation reaction tube, a continuous hydrogenation production device, and a hydrogenation method to solve the above problems. Summary of the Invention
[0003] To address the technical problems mentioned in the background section, the objective of this invention is achieved through the following technical solution:
[0004] This application provides a hydrogenation reaction tube, including a reaction tube body, which is vertically arranged. End caps are fixed at both the upper and lower ends of the reaction tube body. A raw material inlet, a catalyst inlet, and a gas inlet are respectively opened at the bottom of the side of the reaction tube body. An overflow pipe is fixed inside the reaction tube body. The outer wall of the overflow pipe is connected to the inner wall of the reaction tube body via a spiral tube. The bottom of the overflow pipe is sealed, and gaps are left between the upper and lower ends of the overflow pipe and the end caps of the reaction tube body. A discharge pipe is fixed inside the overflow pipe. The lower end of the discharge pipe extends into the overflow pipe, and a gap is left between the lower end of the discharge pipe and the bottom of the overflow pipe. The upper end of the discharge pipe extends beyond the end cap at the top of the reaction tube body. A gas distributor is installed at the bottom of the reaction tube body, located below the overflow pipe, and is connected to the gas inlet.
[0005] This application also provides a continuous hydrogen production apparatus having the above-mentioned hydrogenation reaction tube, which further includes a preheating kettle, a separator, a precipitation tube, and a fractionation tower. The preheating kettle is connected to the hydrogenation reaction tube, the hydrogenation reaction tube is connected to the separator, the separator is connected to the precipitation tube, and the precipitation tube is connected to the fractionation tower.
[0006] Furthermore, the preheating vessel is provided with a first inlet and a first outlet. The first outlet is connected to the raw material inlet of the hydrogenation reaction tube through a first delivery pump. A stirring mechanism is installed inside the preheating vessel.
[0007] Furthermore, the separator is a cyclone separator, which is equipped with a second feed inlet, a top exhaust port, a side discharge port and a bottom discharge port. The second feed inlet is connected to the discharge pipe of the hydrogenation reaction tube, the top exhaust port is connected to the gas inlet of the hydrogenation reaction tube through a gas pump, and the bottom discharge port is connected to the catalyst inlet of the hydrogenation reaction tube through a second feed pump.
[0008] Furthermore, a regulating valve is installed at the bottom discharge port.
[0009] Furthermore, a third feed inlet and a third discharge outlet are respectively opened on the side wall of the sedimentation tube. The third feed inlet is connected to the side discharge outlet of the separator. A baffle is vertically installed inside the sedimentation tube, and the third feed inlet and the third discharge outlet are located on both sides of the baffle.
[0010] Furthermore, the fractionation tower is equipped with a fourth feed inlet, which is connected to the third discharge outlet.
[0011] This application also provides a hydrogenation method using the above-described continuous hydrogenation reactor, comprising the following steps:
[0012] Step S1: Add the raw materials and catalyst to the preheating kettle at a ratio of 99:1, and heat to 50-70℃ under the stirring of the stirring mechanism for later use;
[0013] Step S2: Connect the nitrogen gas source to the gas inlet and introduce nitrogen to replace the air in the hydrogenation reaction tube and separator;
[0014] Step S3: Connect the hydrogen gas source to the gas inlet, and introduce hydrogen to replace the nitrogen in the hydrogenation reaction tube and separator. After the replacement is completed, continue to introduce hydrogen until the pressure in the hydrogenation reaction tube reaches 1.3-1.5 MPa.
[0015] Step S4: Inject cooling water into the spiral tube of the hydrogenation reaction tube to maintain the reaction temperature of the hydrogenation reaction tube at 95-105℃. Pump the mixed raw materials in the preheating kettle into the hydrogenation reaction tube and continuously introduce hydrogen gas to maintain the hydrogen pressure in the hydrogenation reaction tube at 1.3-1.5Mpa.
[0016] Step S5: The mixture obtained in step S4 is fed into a separator to obtain crude hydrogenation product, catalyst and hydrogen. The crude hydrogenation product is fed into a precipitation tube to further separate the catalyst. The catalyst and hydrogen are refluxed to the hydrogenation reaction tube.
[0017] Step S6: After precipitation in the precipitation tube, the crude hydrogenated product obtained in step S5 is sent to the fractionation tower for fractionation to obtain the finished hydrogenated product.
[0018] The technical solutions provided in this application have at least the following technical effects or advantages:
[0019] 1. By installing an overflow pipe inside the hydrogenation reaction tube, and leaving space between the overflow pipe and the top of the hydrogenation reaction tube, a certain amount of gas phase space is always left in the upper part of the reactor, so that the reactant can fully contact and react with the hydrogen gas in the upper part when it overflows, thereby improving the efficiency of the hydrogenation reaction.
[0020] 2. By installing a spiral tube between the hydrogenation reaction tube and the overflow tube, the reaction temperature can be controlled to ensure the safety of the reaction. On the other hand, it can also play a role in fully stirring the gas, liquid and solid during the rising process, thereby improving the efficiency of the reaction.
[0021] 3. By opening a catalyst inlet at the bottom of the hydrogenation reaction tube, the catalyst can be recycled, reducing the cost of use. Attached Figure Description
[0022] The accompanying drawings, which form part of this application, are used to provide a further understanding of the invention. The illustrative embodiments of the invention and their descriptions are used to explain the invention and do not constitute an improper limitation of the invention.
[0023] Figure 1 This is a schematic diagram of the hydrogenation reaction tube structure according to an embodiment of this application;
[0024] Figure 2 This is a schematic diagram of the continuous hydrogenation production apparatus according to an embodiment of this application.
[0025] The following are labeled in the attached diagram: 1. Preheating kettle; 2. Hydrogenation reaction tube; 21. Reaction tube body; 211. Raw material inlet; 212. Catalyst inlet; 213. Gas inlet; 22. Spiral tube; 23. Overflow pipe; 24. Discharge pipe; 25. Gas distributor; 3. Separator; 4. Sedimentation tube; 5. Distillation tower; 6. First transfer pump; 7. Second transfer pump; 8. Gas pump. Detailed Implementation
[0026] To better understand the above technical solutions, the following detailed description, in conjunction with the accompanying drawings and specific embodiments, will illustrate the technical solutions in detail. Obviously, the described embodiments are merely some embodiments of the present invention, and not all embodiments. The following description of at least one exemplary embodiment is merely illustrative and is in no way intended to limit the present invention or its application or use. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without inventive effort are within the scope of protection of the present invention.
[0027] Example 1
[0028] like Figure 1The hydrogenation reaction tube 2 shown includes a reaction tube body 21, a spiral tube 22, an overflow pipe 23, and a discharge pipe 24. The reaction tube body 21 is a cylindrical tube, vertically arranged, with end caps fixed at both ends to form a closed reaction space inside. A raw material inlet 211, a catalyst inlet 212, and a gas inlet 213 are respectively opened on the bottom side of the reaction tube body 21. A gas distributor 25 is installed at the bottom of the reaction tube body 21, communicating with the gas inlet 213 to evenly distribute the gas within the hydrogenation reaction tube 2. The raw material inlet 211 and the catalyst inlet 212 are both located above the gas distributor 25.
[0029] like Figure 1 As shown, the overflow pipe 23 is coaxially installed inside the reaction tube body 21. The bottom of the overflow pipe 23 is sealed, and gaps are left between the upper and lower ends of the overflow pipe 23 and the upper and lower end caps of the reaction tube body 21. The outer wall of the overflow pipe 23 is connected to the inner wall of the reaction tube body 21 through a spiral tube 22, thereby forming a spiral upward material channel between the inner wall of the reaction tube 21, the outer wall of the spiral tube 22, and the outer wall of the overflow pipe 23. When the raw materials and hydrogen enter the reaction tube body, they spiral upward along the material channel, achieving thorough mixing of liquid raw materials, fixed catalyst, and hydrogen to improve the sufficiency of the reaction and increase the product yield. The spiral tube is connected to a circulating water pump to regulate the temperature inside the hydrogenation reaction tube.
[0030] like Figure 1 As shown, an outlet pipe 24 is fixed inside the overflow pipe 23. The outlet pipe 24 is fixedly connected to the upper end cap of the reaction tube body 21. The lower end of the outlet pipe 24 passes through the end cap and extends into the overflow pipe 23. A gap is left between the lower end of the outlet pipe 24 and the bottom of the overflow pipe 23, so that the material can be easily extracted from the bottom of the reaction tube body 21.
[0031] The technical solutions described in the embodiments of this application have at least the following technical effects or advantages:
[0032] 1. By installing an overflow pipe inside the hydrogenation reaction tube, and leaving space between the overflow pipe and the top of the hydrogenation reaction tube, a certain amount of gas phase space is always left in the upper part of the reactor, so that the reactant can fully contact and react with the hydrogen gas in the upper part when it overflows, thereby improving the efficiency of the hydrogenation reaction.
[0033] 2. By installing a spiral tube between the hydrogenation reaction tube and the overflow tube, the reaction temperature can be controlled to ensure the safety of the reaction. On the other hand, it can also play a role in fully stirring the gas, liquid and solid during the rising process, thereby improving the efficiency of the reaction.
[0034] 3. The structure is simple, which enables the gas, liquid and solid phases to be fully mixed and contacted, ensuring effective mass and heat transfer and reducing energy consumption.
[0035] Example 2
[0036] like Figure 2 The continuous hydrogen production apparatus shown includes a preheating kettle 1, a hydrogenation reaction tube 2, a separator 3, a precipitation tube 4, and a fractionation tower 5.
[0037] like Figure 1 , Figure 2 As shown, the preheating vessel 1 is a sealed tank. A first inlet is located on the upper side of the preheating vessel 1, and a first outlet is located at the bottom. The first outlet is connected to the raw material inlet 211 of the hydrogenation reaction tube 2 via a first delivery pump 6. A stirring mechanism is installed inside the preheating vessel 1. During use, the raw materials and catalyst are added to the preheating vessel 1 through the first inlet. After stirring and heating, the materials are pumped into the hydrogenation reaction tube 2 from the raw material inlet 211 at the bottom of the tube via the first delivery pump 6. A three-way connector is installed at the gas inlet 213 of the hydrogenation reaction tube 2. The other two ports of the three-way connector are connected to a hydrogen gas source and a nitrogen gas source via valves, respectively.
[0038] like Figure 1 , Figure 2 As shown, separator 3 is a cyclone separator. A second inlet and a side outlet are provided on the side of separator 3. The second inlet is connected to the outlet pipe 24 of the hydrogenation reaction tube 2. The second inlet is tangentially positioned to the shell of separator 3, allowing material to enter separator 3 tangentially, thus achieving solid-liquid separation. A vertical dike is installed at the inner end of the side outlet, with the top of the dike higher than the height of the second inlet. A top exhaust port is provided at the top of separator 3, connected to the gas inlet 213 of hydrogenation reaction tube 2 via a gas pump 8. A bottom outlet is provided at the bottom of separator 3, connected to the catalyst inlet 212 of hydrogenation reaction tube 2 via a second feed pump 7. During operation, the reacted material in hydrogenation reaction tube 2 enters separator 3 through outlet pipe 24, while unreacted hydrogen flows back to hydrogenation reaction tube 2 from the top exhaust port for re-reaction, thus avoiding hydrogen waste and conserving hydrogen resources. The reaction products are separated from the catalyst by separator 3. After overflowing through the weir, the reaction products flow out of separator 3 from the side outlet. The catalyst settles to the bottom of separator 3 and can be recycled back to the hydrogenation reaction tube 2 via the second feed pump 7, reducing the amount of catalyst used and lowering production costs. A regulating valve (not shown) is installed at the bottom outlet. If the hydrogenation reaction does not meet the target, the regulating valve can be opened to allow for cyclic hydrogenation. The length of the hydrogenation reaction tube 2 can be selected according to the hydrogenation time of different materials, and multiple hydrogenation reaction tubes 2 can be connected in series for hydrogenation.
[0039] like Figure 2As shown, the sedimentation tube 4 is a sealed tank. A baffle is vertically installed on the inner side of the sedimentation tube 4, with the top of the baffle abutting against the top of the sedimentation tube 4 and a gap between the bottom of the baffle and the bottom of the sedimentation tube 4. A third feed inlet and a third discharge outlet are respectively opened on both sides of the sedimentation tube 4, located on opposite sides of the baffle. The third feed inlet is connected to the side discharge outlet of the separator 3. The fractionation tower 5 is equipped with a fourth feed inlet, which is connected to the third discharge outlet. The reaction product enters from the left side of the sedimentation tube 4. Residual catalyst in the reaction product falls to the bottom of the sedimentation tube 4 after being blocked by the baffle. The precipitated reaction product flows out of the sedimentation tube 4 from the upper end of the other side of the baffle and enters the fractionation tower 5 for fractionation to obtain the hydrogenated product.
[0040] The technical solutions described in the embodiments of this application have at least the following technical effects or advantages:
[0041] 1. By opening a catalyst inlet at the bottom of the hydrogenation reaction tube and connecting the bottom outlet of the separator to the catalyst inlet, the catalyst can be recycled, reducing the cost of use;
[0042] 2. By connecting the top exhaust port of the separator to the gas inlet, hydrogen can be recycled, avoiding waste and reducing production costs.
[0043] 3. By using one or more sets of hydrogenation reaction tubes in series, it can adapt to different hydrogenation times for different materials, thus improving the applicability of the device. At the same time, the device has a simple structure, low equipment investment, and is convenient for daily operation, maintenance and repair.
[0044] 4. The hydrogenation time is relatively short, there are fewer side reactions, and the product yield is high; the continuous process can reduce labor intensity and enable large-scale production.
[0045] Example 3
[0046] This application provides a hydrogenation method using the hydrogenation of crotonaldehyde to prepare butyraldehyde as an example, comprising the following steps:
[0047] Step S1: Add crotonaldehyde and Raney nickel to the preheating kettle at a ratio of 99:1, and heat to 50°C under stirring of the stirring mechanism for later use;
[0048] Step S2: Open the valve of the nitrogen gas source to connect the nitrogen gas source with the gas inlet, and introduce nitrogen into the hydrogenation reaction tube and separator to replace the air in them, so as to avoid an explosion accident during hydrogenation.
[0049] Step S3: Close the valve of the nitrogen gas source and open the valve of the hydrogen gas source to connect the hydrogen gas source with the gas inlet. Introduce hydrogen into the hydrogenation reaction tube and separator to replace the nitrogen gas therein. After the replacement is completed, continue to introduce hydrogen gas to maintain the pressure in the hydrogenation reaction tube at 1.3 MPa.
[0050] Step S4: Inject cooling water into the spiral tube of the hydrogenation reaction tube to maintain the reaction temperature of the hydrogenation reaction tube at 95°C. Pump the mixed raw materials in the preheating kettle into the hydrogenation reaction tube and continuously introduce hydrogen gas to maintain the hydrogen pressure in the hydrogenation reaction tube at 1.3 MPa. Control the hydrogenation time by adjusting the feed and discharge rates to ensure that the hydrogenation conversion rate (which can be sampled and analyzed) meets the target. If the target is not met, the second feed pump at the bottom of the separator can be turned on to continue the circulation reaction.
[0051] Step S5: Once the target is reached, the mixture obtained in step S4 is fed into a separator to obtain crude hydrogenation product, catalyst, and hydrogen. The crude hydrogenation product is fed into a precipitation tube for further separation of the catalyst. The catalyst and hydrogen are then returned to the hydrogenation reaction tube. By adjusting the regulating valve at the bottom of the separator, the catalyst precipitated at the bottom of the separator can carry some of the reactants back into the hydrogenation reaction tube; the catalyst at the bottom of the precipitation tube can be periodically discharged.
[0052] Step S6: The crude hydrogenated product obtained in step S5 is further decomposed through a precipitation tube to remove the catalyst and then sent to a fractionation tower for fractionation to obtain the finished hydrogenated product.
[0053] Example 4
[0054] This application provides a hydrogenation method using the hydrogenation of crotonaldehyde to prepare butyraldehyde as an example, comprising the following steps:
[0055] Step S1: Add crotonaldehyde and Raney nickel to the preheating kettle at a ratio of 99:1, and heat to 70°C under the stirring of the stirring mechanism for later use;
[0056] Step S2: Open the valve of the nitrogen gas source to connect the nitrogen gas source with the gas inlet, and introduce nitrogen into the hydrogenation reaction tube and separator to replace the air in them, so as to avoid an explosion accident during hydrogenation.
[0057] Step S3: Close the valve of the nitrogen gas source and open the valve of the hydrogen gas source to connect the hydrogen gas source with the gas inlet. Introduce hydrogen into the hydrogenation reaction tube and separator to replace the nitrogen gas therein. After the replacement is completed, continue to introduce hydrogen gas to maintain the pressure in the hydrogenation reaction tube at 1.5 MPa.
[0058] Step S4: Inject cooling water into the spiral tube of the hydrogenation reaction tube to maintain the reaction temperature of the hydrogenation reaction tube at 100℃. Pump the mixed raw materials in the preheating kettle into the hydrogenation reaction tube and continuously introduce hydrogen gas to maintain the hydrogen pressure in the hydrogenation reaction tube at 1.5 MPa. Control the hydrogenation time by adjusting the feed and discharge rates to ensure that the hydrogenation conversion rate (which can be sampled and analyzed) meets the target. If the target is not met, the second feed pump at the bottom of the separator can be turned on to continue the circulation reaction.
[0059] Step S5: Once the target is reached, the mixture obtained in step S4 is fed into a separator to obtain crude hydrogenation product, catalyst, and hydrogen. The crude hydrogenation product is fed into a precipitation tube for further separation of the catalyst. The catalyst and hydrogen are then returned to the hydrogenation reaction tube. By adjusting the regulating valve at the bottom of the separator, the catalyst precipitated at the bottom of the separator can carry some of the reactants back into the hydrogenation reaction tube; the catalyst at the bottom of the precipitation tube can be periodically discharged.
[0060] Step S6: The crude hydrogenated product obtained in step S5 is further decomposed through a precipitation tube to remove the catalyst and then sent to a fractionation tower for fractionation to obtain the finished hydrogenated product.
[0061] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the exemplary embodiments according to this application. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.
[0062] In the description of this invention, it should be understood that the orientation or positional relationship indicated by directional terms such as "front, back, up, down, left, right", "horizontal, vertical, horizontal" and "top, bottom" is generally based on the orientation or positional relationship shown in the accompanying drawings, and is only for the convenience of describing this invention and simplifying the description. Unless otherwise stated, these directional terms do not indicate or imply that the device or element referred to must have a specific orientation or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on the scope of protection of this invention. The directional terms "inner" and "outer" refer to the inner and outer contours relative to the outline of each component itself.
[0063] Furthermore, it should be noted that the use of terms such as "first" and "second" to define components is merely for the purpose of distinguishing the corresponding components. Unless otherwise stated, the above terms have no special meaning and therefore should not be construed as limiting the scope of protection of this invention.
[0064] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.
Claims
1. A hydrogenation reaction tube, characterized in that, The device includes a reaction tube body, which is vertically arranged. End caps are fixed at both the top and bottom of the reaction tube body. A raw material inlet, a catalyst inlet, and a gas inlet are respectively opened at the bottom of the side of the reaction tube body. An overflow pipe is fixed inside the reaction tube body. The outer wall of the overflow pipe is connected to the inner wall of the reaction tube body via a spiral tube. The inner wall of the reaction tube, the outer wall of the spiral tube, and the outer wall of the overflow pipe form a spirally upward material channel. The bottom of the overflow pipe is sealed, and gaps are left between the upper and lower ends of the overflow pipe and the end caps of the reaction tube body. A discharge pipe is fixed inside the overflow pipe. The lower end of the discharge pipe extends into the overflow pipe, and a gap is left between the lower end of the discharge pipe and the bottom of the overflow pipe. The upper end of the discharge pipe extends beyond the end cap at the top of the reaction tube body. A gas distributor is installed at the bottom of the reaction tube body, located below the overflow pipe, and is connected to the gas inlet.
2. A continuous hydrogen production apparatus having the hydrogenation reaction tube of claim 1, characterized in that, It also includes a preheating kettle, a separator, a precipitation tube, and a fractionation tower. The preheating kettle is connected to the hydrogenation reaction tube, the hydrogenation reaction tube is connected to the separator, the separator is connected to the precipitation tube, and the precipitation tube is connected to the fractionation tower.
3. The continuous hydrogenation production apparatus according to claim 2, characterized in that, The preheating vessel is provided with a first inlet and a first outlet. The first outlet is connected to the raw material inlet of the hydrogenation reaction tube through a first delivery pump. A stirring mechanism is installed inside the preheating vessel.
4. The continuous hydrogenation production apparatus according to claim 2, characterized in that, The separator is a cyclone separator, which is provided with a second feed inlet, a top exhaust port, a side discharge port and a bottom discharge port. The second feed inlet is connected to the discharge pipe of the hydrogenation reaction tube. The top exhaust port is connected to the gas inlet of the hydrogenation reaction tube through a gas pump. The bottom discharge port is connected to the catalyst inlet of the hydrogenation reaction tube through a second feed pump.
5. The continuous hydrogenation production apparatus according to claim 4, characterized in that, A regulating valve is installed at the bottom discharge port.
6. The continuous hydrogenation production apparatus according to claim 4, characterized in that, The sedimentation tube has a third inlet and a third outlet on its side wall. The third inlet is connected to the side outlet of the separator. A baffle is vertically installed inside the sedimentation tube. The third inlet and the third outlet are located on both sides of the baffle.
7. The continuous hydrogenation production apparatus according to claim 6, characterized in that, The fractionation tower is provided with a fourth feed inlet, which is connected to the third discharge outlet.
8. A hydrogenation method using the continuous hydrogenation production apparatus according to any one of claims 2-7, characterized in that, Includes the following steps: Step S1: Add the raw materials and catalyst to the preheating kettle at a ratio of 99:1, and heat to 50-70℃ under the stirring of the stirring mechanism for later use; Step S2: Connect the nitrogen gas source to the gas inlet and introduce nitrogen to replace the air in the hydrogenation reaction tube and separator; Step S3: Connect the hydrogen gas source to the gas inlet, and introduce hydrogen to replace the nitrogen in the hydrogenation reaction tube and separator. After the replacement is completed, continue to introduce hydrogen until the pressure in the hydrogenation reaction tube reaches 1.3-1.5 MPa. Step S4: Inject cooling water into the spiral tube of the hydrogenation reaction tube to maintain the reaction temperature of the hydrogenation reaction tube at 95-105℃. Pump the mixed raw materials in the preheating kettle into the hydrogenation reaction tube and continuously introduce hydrogen gas to maintain the hydrogen pressure in the hydrogenation reaction tube at 1.3-1.5Mpa. Step S5: The mixture obtained in step S4 is fed into a separator to obtain crude hydrogenation product, catalyst and hydrogen. The crude hydrogenation product is fed into a precipitation tube to further separate the catalyst. The catalyst and hydrogen are refluxed to the hydrogenation reaction tube. Step S6: After precipitation in the precipitation tube, the crude hydrogenated product obtained in step S5 is sent to the fractionation tower for fractionation to obtain the finished hydrogenated product.
Citation Information
Patent Citations
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CN102719271A
Continuous hydrogenation production system device
CN202226826U
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CN2609929Y
Petroleum distillate processing reactor
SU1098559A1