A furfural hydrogenation reaction system and reaction method

Abstract

The invention relates to a furfural hydrogenation reaction system and a reaction method. The system comprises a gas phase raw material storage tank and a hydrogen storage tank. The gas phase raw material storage tank and the hydrogen storage tank are connected to the tube side of a suspended bed tubular reactor through a feeding unit. The shell side of the suspended bed tubular reactor is connected to a heat removal unit. The tube side outlet of the suspended bed tubular reactor is connected to a product separation tank through a heat exchange device. The liquid phase outlet of the product separation tank is connected to a product tank. The system has the characteristics of simple structure, reasonable design, and can not only improve heat exchange efficiency, but also can timely remove reaction heat, which is beneficial to the stable operation of the hydrogenation reaction.

Description

Technical Field

[0001] The invention belongs to a furfural hydrogenation reaction system and a reaction method. Background Art

[0002] Furfural hydrogenation to produce furfuryl alcohol or 2-methylfuran and other products generally adopts liquid phase hydrogenation or gas phase hydrogenation process. The liquid phase hydrogenation process has high pressure, high temperature, high conversion rate, many by-products, but large equipment scale and processing capacity. The gas phase hydrogenation process has low pressure, low temperature, few by-products, but small equipment scale and large land occupation. The process of furfural catalytic hydrogenation to produce hydrogenated products is exothermic. Whether it is liquid phase hydrogenation or gas phase hydrogenation process, there are difficulties in heat removal from the reactor, high reaction hot spot temperature, easy to overheat / fly high temperature, etc., which may accelerate the progress of side reactions, is not conducive to the stable operation of the device, and there are process risks such as runaway temperature and explosion. Summary of the invention

[0003] The purpose of the present invention is to overcome the defects in the prior art and provide a furfural hydrogenation reaction system and reaction method which have a simple structure, a reasonable design, can not only improve the heat exchange efficiency, but also can remove the heat of the reaction in time to facilitate the stable operation of the hydrogenation reaction.

[0004] The object of the present invention is achieved as follows: a furfural hydrogenation reaction system comprises a gas phase raw material storage tank and a hydrogen storage tank, wherein the gas phase raw material storage tank and the hydrogen storage tank are connected to the tube side of a suspended bed tubular reactor through a feeding unit, the shell side of the suspended bed tubular reactor is connected to a heat removal unit, the tube side outlet end of the suspended bed tubular reactor is connected to a product separation tank through a heat exchange device, and the liquid phase outlet of the product separation tank is connected to a product tank.

[0005] Preferably, a plurality of single tubes are provided inside the suspended bed tubular reactor, a cushion particle layer is provided inside the single tube, and a catalyst particle layer is provided on the top of the cushion particle layer.

[0006] Preferably, the diameter of a single tube of the suspended bed tubular reactor is 15 to 50 mm.

[0007] Preferably, the diameter of the cushion particles in the cushion particle layer is 5 to 10 mm.

[0008] Preferably, the catalyst in the catalyst particle layer is spherical, and the diameter of the spherical catalyst is 0.3 mm to 5 mm.

[0009] Preferably, the feeding unit includes a vaporizer connected to a gas phase raw material storage tank and a hydrogen storage tank respectively, a circulating heating part is provided at the lower part of the vaporizer, a gas phase outlet at the top of the vaporizer is connected to a separation tank, the top of the separation tank is connected to the tube side inlet end of the suspended bed tubular reactor, and the lower liquid outlet of the separation tank is connected to the liquid phase reflux port of the vaporizer.

[0010] Preferably, the circulating heating part includes a circulating pipe arranged between the bottom and the upper part of the vaporizer and connected to the vaporizer, a circulating pump is provided on the circulating pipe at the bottom of the vaporizer, a heater is provided on the circulating pipe between the circulating pump and the upper part of the vaporizer, and the shell side of the heater is connected to the steam pipe and the condensate pipe.

[0011] Preferably, the heat removal unit comprises a heat transfer tank connected to the lower part of the shell side of the suspended bed tubular reactor, and the heat transfer tank is connected to the upper part of the shell side of the suspended bed tubular reactor via a heat transfer pump.

[0012] Preferably, the gas phase outlet of the product separation tank is connected to the vaporizer through a hydrogen compressor and the hot side end of a heat exchange device, and the tube side outlet end of the suspended bed tubular reactor is connected to the product separation tank through the cold side end of a heat exchange device.

[0013] The present invention also provides a reaction method using the furfural hydrogenation reaction system, the reaction method comprising the following steps:

[0014] Step 1: The gaseous raw material in the gaseous raw material storage tank enters the vaporizer, is pressurized by a circulating pump arranged at the lower part of the vaporizer, and exchanges heat with the steam in the shell side of the heater in the tube side of the heater. The heated gaseous raw material is flushed into the upper part of the vaporizer;

[0015] The circulation pump 3 has a head of 20 to 150 m; the steam pressure in the steam pipeline is 0.5 to 4.0 MPa, and the gas phase raw material temperature at the outlet of the heater tube is 65 to 165°C;

[0016] The raw material in the gas phase raw material storage tank is furfural at room temperature;

[0017] Step 2: The hydrogen from the hydrogen storage tank and the hydrogen from the hydrogen compressor enters the middle of the vaporizer and vaporizes the raw materials from the heater tube side, and then enters the separation tank after vaporization;

[0018] The ratio of the hydrogen flow rate from the hydrogen compressor to the hydrogen flow rate from the hydrogen storage tank entering the vaporizer is 5 to 30:1;

[0019] The gas temperature at the outlet of the vaporizer is 90-180°C;

[0020] Step 3: The vaporized gas phase enters the separation tank and is flash separated. The liquid phase after flash separation flows back into the vaporizer through the liquid phase reflux port of the vaporizer. The flash temperature in the separation tank is 90-180°C.

[0021] Step 4: the gas phase separated by flash evaporation in a separation tank enters the tube side of a suspended bed tubular reactor; there are gaps between the cushion particles in the cushion particle layer and the catalyst particles in the catalyst particle layer when they are piled up, and the gas phase enters the catalyst particle layer through the bottom of the tube side of the suspended bed tubular reactor. Due to the existence of gaps, the flow rate of the gas phase increases, and some catalyst particles are blown away by the airflow and move upward with the direction of the airflow; after the catalyst is dispersed to a certain extent, the gap between the bed expands, the gas flow rate decreases, and the catalyst particles fall under the action of gravity. In the above process, the flow rate of the gas phase can be slowed down to enhance mass transfer and heat transfer, and at the same time, the catalyst particles flip during the movement, thereby increasing the contact between the gas phase and the surface of the catalyst particles and improving the catalytic efficiency;

[0022] Step 5: The shell side of the suspended bed tubular reactor is filled with a heat-conducting medium, and the heat in a plurality of single tubes is exchanged with the heat-conducting medium. The heat-conducting medium after the heat exchange enters a heat transfer tank for cooling. The heat transfer tank is provided with a cooling water coil for exchanging heat with the heat-conducting medium. The heat-conducting medium after the heat exchange is replenished into the shell side of the suspended bed tubular reactor through a heat transfer pump;

[0023] The heat transfer medium is heat transfer oil or hot water;

[0024] Step 6: The process gas after the reaction in the tube side of the suspended bed tubular reactor enters the heat exchange device to exchange heat with the circulating gas in the gas phase outlet of the product separation tank. The process gas after heat exchange enters the product separation tank for flash separation, and the separated liquid phase enters the product tank for storage;

[0025] The process gas temperature entering the heat exchange device is 100-185°C, and the process gas temperature exiting the heat exchange device is 14-40°C;

[0026] The flash temperature in the product separation tank is 14-40°C;

[0027] Step 7: The circulating gas in the product separation tank enters the hydrogen compressor through the gas phase outlet of the product separation tank to be pressurized, then preheated in the heat exchange device, and merges with the hydrogen coming out of the hydrogen storage tank and enters the vaporizer.

[0028] A furfural hydrogenation reaction system and reaction method prepared according to the above scheme are applicable to hydrogenation reaction systems in which the raw materials are all gas phase. By setting up a suspended bed tubular reactor, it not only overcomes the defect that a main reaction pipeline is set inside the reactor for catalytic hydrogenation reaction in the traditional technology, which causes the heat to be unable to be quickly removed, but also solves the defect that the diameter of several reaction pipelines is too small, resulting in low catalytic efficiency and poor mass transfer and heat transfer effects. The present invention adopts a suspended bed tubular reactor, and a plurality of single tubes are arranged inside the suspended bed tubular reactor. A cushion particle layer and a catalyst particle layer are arranged inside the single tube. There are gaps between the cushion particles in the cushion particle layer and the catalyst particles in the catalyst particle layer when they are stacked. The gas phase enters the catalyst particle layer through the bottom of the suspended bed tubular reactor tube. Due to the existence of the gap, the flow rate of the gas phase increases, and some catalyst particles are blown away by the airflow and move upward with the direction of the airflow; after the catalyst is dispersed to a certain extent, the bed gap expands, the gas flow rate decreases, and the catalyst particles fall under the action of gravity. The above process can slow down the flow rate of the gas phase. Mass transfer and heat transfer, while the catalyst particles flip during the movement, improve the contact between the gas phase and the surface of the catalyst particles, and improve the catalytic efficiency; it is particularly important to note that: the enhanced mass transfer and heat transfer in the present invention is not only reflected in reducing the flow rate of the reaction gas, but also includes the ability to disperse the catalyst particles to achieve the purpose of lowering the temperature of the entire catalyst bed; further, the present invention preheats the circulating gas to increase the temperature of the hydrogen and cooperates with the circulating heating part to achieve effective vaporization of the gas-phase raw material. The above process not only improves the utilization efficiency of the waste heat of the reaction gas, but also can improve the gasification efficiency of the gas-phase raw material, ensuring the stable and rapid operation of the hydrogenation reaction; further, the shell side medium in the present invention is heat transfer oil or hot water, which is filled in the shell side of the suspended bed tubular reactor (that is, arranged on the outside of the tube side). The present invention includes a number of single tubes. The above arrangement can realize the timely removal of the heat generated by the reaction to avoid overheating / flying temperature and the like. It has a simple structure, a reasonable design, and can not only improve the heat exchange efficiency, but also can remove the heat of the reaction in time, which is conducive to the stable operation of the hydrogenation reaction. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 It is a structural schematic diagram of the present invention.

[0030] Figure 2 It is a schematic diagram of the structure inside a single tube of the present invention. DETAILED DESCRIPTION

[0031] In order to have a clearer understanding of the technical features, purposes and effects of the present invention, the specific implementation of the present invention is now described with reference to the accompanying drawings, in which the same reference numerals represent the same components. In order to make the drawings concise, each figure only schematically shows the parts related to the invention, and they do not represent the actual structure of the product.

[0032] like Figure 1 , 2 As shown, the present invention is a furfural hydrogenation reaction system and reaction method, wherein the reaction system comprises a gas phase raw material storage tank 1 and a hydrogen storage tank 15, wherein the gas phase raw material storage tank 1 and the hydrogen storage tank 15 are connected to the tube side of the suspended bed tubular reactor 10 through a feeding unit, the shell side of the suspended bed tubular reactor 10 is connected to a heat removal unit, the tube side outlet end of the suspended bed tubular reactor 10 is connected to a product separation tank 9 through a heat exchange device 8, and the liquid phase outlet of the product separation tank 9 is connected to a product tank 14. The present invention can not only solve the problem of heat release in the catalytic hydrogenation process of furfural well by setting a suspended bed tubular reactor 10, but also effectively improve the catalytic efficiency.

[0033] Furthermore, a plurality of single tubes 12 are provided inside the suspended bed tubular reactor 10, a cushion particle layer 13 is provided inside the single tube 12, and a catalyst particle layer 11 is provided on top of the cushion particle layer 13. The tube side of the suspended bed tubular reactor 10 in the present invention is composed of a plurality of single tubes 12, and hydrogen and gaseous raw materials enter the catalyst bed in the single tube 12 for catalytic reaction after vaporization, and the cushion particle layer 13 and the catalyst particle layer 11 are laid in the single tube 12, which can increase the flow rate of hydrogen and gaseous raw materials in the early stage and reduce their flow rate in the later stage, so as to achieve the purpose of fully contacting the gas phase with the top catalyst particle layer 11 to improve the catalytic efficiency, and at the same time, the catalyst particles are dispersed to achieve the characteristic of being able to reduce the temperature of the entire catalyst bed.

[0034] Furthermore, the diameter of the single tube 12 of the suspended bed tubular reactor 10 is 15 to 50 mm. By limiting the diameter of the single tube 12, it can be seen that the present invention abandons the technical solution of using a thicker main reaction tube in the traditional technology, so as to solve the defects of the traditional technology that the reactor is difficult to remove heat, the reaction hot spot temperature is high, and it is easy to overheat / fly away from the temperature; but in the traditional concept, the use of several thinner pipes has the problems of low catalytic efficiency and pipe heat exchange efficiency. On the one hand, the present invention reduces the temperature of the entire catalyst bed by dispersing the catalyst particles, and on the other hand, it achieves the purpose of removing its heat by reducing the gas phase flow rate (i.e., increasing the residence time of the gas phase in the single tube 12); at the same time, the catalyst particles can roll, rotate, float, and fall with the airflow, so that their surface can be fully in contact with the gas phase to achieve the purpose of improving the catalytic efficiency.

[0035] Furthermore, the diameter of the cushion particles in the cushion particle layer 13 is 5 to 10 mm. The purpose of providing cushion particles is to increase the flow rate of the gas phase to create conditions for the rise and fall of the catalyst particles, to support the catalyst particles and lay a foundation for laying relatively fine catalyst particles, and to stabilize the flow rate of the gas.

[0036] Furthermore, the catalyst in the catalyst particle layer 11 is spherical, and the diameter of the spherical catalyst is 0.3 mm to 5 mm. The catalyst described in the present invention can be in the shape of a cuboid, a cube, a rugby ball or a sphere, preferably a spherical structure to facilitate rotation. The rotation of the sphere can achieve maximum contact between the gas phase and the surface of the catalyst particles, so as to achieve the purpose of improving the catalytic efficiency. It should be noted that, preferably, the diameter of the spherical catalyst described in the present invention is smaller than the diameter of the cushion layer particles.

[0037] Further, the feeding unit includes a vaporizer 2 connected to the gas phase raw material storage tank 1 and the hydrogen storage tank 15 respectively, a circulating heating part is provided at the lower part of the vaporizer 2, a gas phase outlet at the top of the vaporizer 2 is connected to the separation tank 5, the top of the separation tank 5 is connected to the tube side inlet end of the suspended bed tubular reactor 10, and the lower liquid outlet of the separation tank 5 is connected to the liquid phase reflux port of the vaporizer 2. The present invention can realize the vaporization of the gas phase raw material by setting the vaporizer 2, laying a foundation for its entry into the suspended bed tubular reactor 10.

[0038] Furthermore, the circulation heating part includes a circulation pipe 19 disposed between the bottom and the upper part of the vaporizer 2 and connected to the vaporizer 2, a circulation pump 3 is disposed on the circulation pipe 19 at the bottom of the vaporizer 2, a heater 4 is disposed on the circulation pipe 19 between the circulation pump 3 and the upper part of the vaporizer 2, and the shell side of the heater 4 is connected to the steam pipe 18 and the condensate pipe 17. The provision of the circulation heating part enables the addition of gaseous raw materials, laying a foundation for accelerating the vaporization of the gaseous raw materials.

[0039] Furthermore, the heat removal unit includes a heat transfer tank 6 connected to the lower part of the shell side of the suspended bed tubular reactor 10, and the heat transfer tank 6 is connected to the upper part of the shell side of the suspended bed tubular reactor 10 through a heat transfer pump 7. The above arrangement can realize timely removal of heat in the tube side of the suspended bed tubular reactor 10, and timely cooling of the heat transfer medium for removing heat in the heat transfer tank 6, so as to achieve the purpose of ensuring the normal operation of the suspended bed tubular reactor 10.

[0040] Furthermore, the gas phase outlet of the product separation tank 9 is connected to the vaporizer 2 through the hydrogen compressor 16 and the hot side end of the heat exchange device 8, and the tube side outlet end of the suspended bed tubular reactor 10 is connected to the product separation tank 9 through the cold side end of the heat exchange device 8. The present invention can realize the recycling of the circulating gas in the product separation tank 9, the recycling of the waste heat of the reaction gas, and the preheating of the hydrogen coming out of the hydrogen storage tank 15 through the above-mentioned arrangement, so as to achieve the purpose of improving the vaporization efficiency of the gas phase raw material.

[0041] The present invention also provides a reaction method using the furfural hydrogenation reaction system, the reaction method comprising the following steps:

[0042] Step 1: The gaseous raw material in the gaseous raw material storage tank 1 enters the vaporizer 2, is pressurized by the circulating pump 3 arranged at the lower part of the vaporizer 2, and exchanges heat with the steam in the shell side of the heater 4 in the tube side of the heater 4, and the heated gaseous raw material is flushed into the upper part of the vaporizer 2;

[0043] The circulation pump 3 has a head of 20 to 150 m; the steam pressure in the steam pipe 18 is 0.5 to 4.0 MPa, and the gas phase raw material temperature at the outlet of the heater 4 is 65 to 165°C;

[0044] The raw material in the gas phase raw material storage tank 1 is room temperature furfural;

[0045] Step 2: The hydrogen storage tank 15 and the hydrogen from the hydrogen compressor 16 enter the middle of the vaporizer 2, and vaporize the raw materials from the tube side of the heater 4, and then enter the separation tank 5 after vaporization;

[0046] The ratio of the hydrogen flow rate from the hydrogen compressor 16 to the hydrogen flow rate from the hydrogen storage tank 15 entering the vaporizer 2 is 5 to 30:1;

[0047] The gas temperature at the outlet of the vaporizer 2 is 90-180°C;

[0048] Step 3: The vaporized gas phase enters the separation tank 5 and is flash separated. The liquid phase after flash separation flows back into the vaporizer 2 through the liquid phase reflux port of the vaporizer 2. The flash temperature in the separation tank 5 is 90-180°C.

[0049] Step 4: the gas phase separated by flash evaporation in the separation tank 5 enters the tube side of the suspended bed tubular reactor 10; there are gaps between the cushion particles in the cushion particle layer 13 and the catalyst particles in the catalyst particle layer 11 when they are piled up, and the gas phase enters the catalyst particle layer 11 through the bottom of the tube side of the suspended bed tubular reactor 10. Due to the existence of gaps, the flow rate of the gas phase increases, and some catalyst particles are blown away by the airflow and move upward with the direction of the airflow; after the catalyst is dispersed to a certain extent, the bed gap expands, the gas flow rate decreases, and the catalyst particles fall under the action of gravity. In the above process, the flow rate of the gas phase can be slowed down to improve the intensified mass transfer and heat transfer. At the same time, the catalyst particles flip during the movement process, which increases the contact between the gas phase and the surface of the catalyst particles and improves the catalytic efficiency;

[0050] Step 5: The shell side of the suspended bed tubular reactor 10 is filled with a heat-conducting medium, and the heat in the plurality of single tubes 12 is heat-exchanged with the heat-conducting medium. The heat-conducting medium after the heat exchange enters the heat transfer tank 6 for cooling. The heat transfer tank 6 is provided with a cooling water coil for heat exchange with the heat-conducting medium. The heat-conducting medium after the heat exchange is replenished into the shell side of the suspended bed tubular reactor 10 through the heat transfer pump 7;

[0051] The heat transfer medium is heat transfer oil or hot water;

[0052] Step 6: The process gas after the reaction in the tube side of the suspended bed tubular reactor 10 enters the heat exchange device 8 to exchange heat with the circulating gas in the gas phase outlet of the product separation tank 9. The process gas after heat exchange enters the product separation tank 9 for flash separation, and the separated liquid phase enters the product tank 14 for storage;

[0053] The process gas temperature entering the heat exchange device 8 is 100-185°C, and the process gas temperature exiting the heat exchange device 8 is 14-40°C;

[0054] The flash temperature in the product separation tank 9 is 14-40°C;

[0055] Step 7: The circulating gas in the product separation tank 9 enters the hydrogen compressor 16 through the gas phase outlet of the product separation tank 9 to be pressurized, then preheated in the heat exchange device 8, and merges with the hydrogen coming out of the hydrogen storage tank 15 to enter the vaporizer 2.

[0056] The present invention is a complete furfural hydrogenation reaction system, which not only overcomes the problem that the heat of the hydrogenation reaction caused by the reaction gas used in the traditional technology is too high and cannot be removed in time, but also can solve the problem of low catalytic efficiency and poor mass transfer and heat transfer effect of using several small diameter pipes in the traditional concept. At the same time, the present invention also uses the waste heat of the reaction gas to heat the circulating gas to achieve the purpose of improving the vaporization efficiency of the gas phase raw material. Further, the present invention can reduce the temperature in the single tube, improve the mass transfer and heat transfer efficiency, and on this basis, cooperate with the heat removal unit to achieve the purpose of improving the stable operation of the equipment.

[0057] In order to explain the present invention in more detail, the present invention is further described in conjunction with embodiments. Specific embodiments are as follows:

[0058] Example 1

[0059] A furfural hydrogenation reaction system includes a gas phase raw material storage tank 1 and a hydrogen storage tank 15, wherein the gas phase raw material storage tank 1 and the hydrogen storage tank 15 are connected to the tube side of a suspended bed tubular reactor 10 through a feeding unit, the shell side of the suspended bed tubular reactor 10 is connected to a heat removal unit, the tube side outlet of the suspended bed tubular reactor 10 is connected to a product separation tank 9 through a heat exchange device 8, and the liquid phase outlet of the product separation tank 9 is connected to a product tank 14. A plurality of single tubes 12 are arranged inside the suspended bed tubular reactor 10, a cushion particle layer 13 is arranged inside the single tube 12, and a catalyst particle layer 11 is arranged on the top of the cushion particle layer 13. The diameter of the single tube 12 of the suspended bed tubular reactor 10 is 15 mm. The diameter of the cushion particles in the cushion particle layer 13 is 5 mm. The catalyst in the catalyst particle layer 11 is spherical, and the diameter of the spherical catalyst is 0.3 mm. The feeding unit includes a vaporizer 2 connected to a gas phase raw material storage tank 1 and a hydrogen storage tank 15 respectively, a circulating heating part is provided at the lower part of the vaporizer 2, a gas phase outlet at the top of the vaporizer 2 is connected to a separation tank 5, a top of the separation tank 5 is connected to the tube side inlet end of the suspended bed tubular reactor 10, and a lower liquid outlet of the separation tank 5 is connected to a liquid phase reflux port of the vaporizer 2. The circulating heating part includes a circulating pipeline 19 provided between the bottom and the upper part of the vaporizer 2 and connected to the vaporizer 2, a circulating pump 3 is provided on the circulating pipeline 19 at the bottom of the vaporizer 2, a heater 4 is provided on the circulating pipeline 19 between the circulating pump 3 and the upper part of the vaporizer 2, and the shell side of the heater 4 is connected to a steam pipeline 18 and a condensate pipeline 17. The heat removal unit includes a heat transfer tank 6 connected to the lower part of the shell side of the suspended bed tubular reactor 10, and the heat transfer tank 6 is connected to the upper part of the shell side of the suspended bed tubular reactor 10 through a heat transfer pump 7. The gas phase outlet of the product separation tank 9 is connected to the vaporizer 2 through the hydrogen compressor 16 and the hot side end of the heat exchange device 8, and the tube side outlet end of the suspended bed tubular reactor 10 is connected to the product separation tank 9 through the cold side end of the heat exchange device 8.

[0060] A reaction method using a furfural hydrogenation reaction system, the reaction method comprising the following steps:

[0061] Step 1: The gaseous raw material in the gaseous raw material storage tank 1 enters the vaporizer 2, is pressurized by the circulating pump 3 arranged at the lower part of the vaporizer 2, and exchanges heat with the steam in the shell side of the heater 4 in the tube side of the heater 4, and the heated gaseous raw material is flushed into the upper part of the vaporizer 2;

[0062] The head of the circulating pump 3 is 20-150m; the steam pressure in the steam pipe 18 is 0.5-4.0MPa, and the gas phase raw material temperature at the outlet of the heater 4 pipe side is 65°C;

[0063] The raw material in the gas phase raw material storage tank 1 is room temperature furfural;

[0064] Step 2: The hydrogen storage tank 15 and the hydrogen from the hydrogen compressor 16 enter the middle of the vaporizer 2, and vaporize the raw materials from the tube side of the heater 4, and then enter the separation tank 5 after vaporization;

[0065] The ratio of the hydrogen flow rate from the hydrogen compressor 16 to the hydrogen flow rate from the hydrogen storage tank 15 entering the vaporizer 2 is 5:1;

[0066] The gas temperature at the outlet of the vaporizer 2 is 90°C;

[0067] Step 3: The vaporized gas phase enters the separation tank 5 and is flash separated. The liquid phase after flash separation flows back into the vaporizer 2 through the liquid phase reflux port of the vaporizer 2. The flash temperature in the separation tank 5 is 90°C.

[0068] Step 4: the gas phase separated by flash evaporation in the separation tank 5 enters the tube side of the suspended bed tubular reactor 10; there are gaps between the cushion particles in the cushion particle layer 13 and the catalyst particles in the catalyst particle layer 11 when they are piled up, and the gas phase enters the catalyst particle layer 11 through the bottom of the tube side of the suspended bed tubular reactor 10. Due to the existence of gaps, the flow rate of the gas phase increases, and some catalyst particles are blown away by the airflow and move upward with the direction of the airflow; after the catalyst is dispersed to a certain extent, the bed gap expands, the gas flow rate decreases, and the catalyst particles fall under the action of gravity. In the above process, the flow rate of the gas phase can be slowed down to improve the intensified mass transfer and heat transfer. At the same time, the catalyst particles flip during the movement process, which increases the contact between the gas phase and the surface of the catalyst particles and improves the catalytic efficiency;

[0069] Step 5: The shell side of the suspended bed tubular reactor 10 is filled with a heat-conducting medium, and the heat in the plurality of single tubes 12 is heat-exchanged with the heat-conducting medium. The heat-conducting medium after the heat exchange enters the heat transfer tank 6 for cooling. The heat transfer tank 6 is provided with a cooling water coil for heat exchange with the heat-conducting medium. The heat-conducting medium after the heat exchange is replenished into the shell side of the suspended bed tubular reactor 10 through the heat transfer pump 7;

[0070] The heat transfer medium is heat transfer oil or hot water;

[0071] Step 6: The process gas after the reaction in the tube side of the suspended bed tubular reactor 10 enters the heat exchange device 8 to exchange heat with the circulating gas in the gas phase outlet of the product separation tank 9. The process gas after heat exchange enters the product separation tank 9 for flash separation, and the separated liquid phase enters the product tank 14 for storage;

[0072] The process gas temperature entering the heat exchange device 8 is 100°C, and the process gas temperature exiting the heat exchange device 8 is 14°C;

[0073] The flash temperature in the product separation tank 9 is 14°C;

[0074] Step 7: The circulating gas in the product separation tank 9 enters the hydrogen compressor 16 through the gas phase outlet of the product separation tank 9 to be pressurized, then preheated in the heat exchange device 8, and merges with the hydrogen coming out of the hydrogen storage tank 15 to enter the vaporizer 2.

[0075] Example 2

[0076] A furfural hydrogenation reaction system includes a gas phase raw material storage tank 1 and a hydrogen storage tank 15, wherein the gas phase raw material storage tank 1 and the hydrogen storage tank 15 are connected to the tube side of a suspended bed tubular reactor 10 through a feeding unit, the shell side of the suspended bed tubular reactor 10 is connected to a heat removal unit, the tube side outlet of the suspended bed tubular reactor 10 is connected to a product separation tank 9 through a heat exchange device 8, and the liquid phase outlet of the product separation tank 9 is connected to a product tank 14. A plurality of single tubes 12 are arranged inside the suspended bed tubular reactor 10, a cushion particle layer 13 is arranged inside the single tube 12, and a catalyst particle layer 11 is arranged on the top of the cushion particle layer 13. The diameter of the single tube 12 of the suspended bed tubular reactor 10 is 50 mm. The diameter of the cushion particles in the cushion particle layer 13 is 10 mm. The catalyst in the catalyst particle layer 11 is spherical, and the diameter of the spherical catalyst is 5 mm. The feeding unit comprises a vaporizer 2 connected to a gas phase raw material storage tank 1 and a hydrogen storage tank 15 respectively, a circulating heating part is provided at the lower part of the vaporizer 2, a gas phase outlet at the top of the vaporizer 2 is connected to a separation tank 5, a top of the separation tank 5 is connected to the tube side inlet end of the suspended bed tubular reactor 10, and a lower liquid outlet of the separation tank 5 is connected to a liquid phase reflux port of the vaporizer 2. The circulating heating part comprises a circulating pipeline 19 provided between the bottom and the upper part of the vaporizer 2 and connected to the vaporizer 2, a circulating pump 3 is provided on the circulating pipeline at the bottom of the vaporizer 2, a heater 4 is provided on the circulating pipeline between the circulating pump 3 and the upper part of the vaporizer 2, and the shell side of the heater 4 is connected to a steam pipeline 18 and a condensate pipeline 17. The heat removal unit comprises a heat transfer tank 6 connected to the lower part of the shell side of the suspended bed tubular reactor 10, and the heat transfer tank 6 is connected to the upper part of the shell side of the suspended bed tubular reactor 10 through a heat transfer pump 7. The gas phase outlet of the product separation tank 9 is connected to the vaporizer 2 through the hydrogen compressor 16 and the hot side end of the heat exchange device 8, and the tube side outlet end of the suspended bed tubular reactor 10 is connected to the product separation tank 9 through the cold side end of the heat exchange device 8.

[0077] A reaction method using a furfural hydrogenation reaction system, the reaction method comprising the following steps:

[0078] Step 1: The gaseous raw material in the gaseous raw material storage tank 1 enters the vaporizer 2, is pressurized by the circulating pump 3 arranged at the lower part of the vaporizer 2, and exchanges heat with the steam in the shell side of the heater 4 in the tube side of the heater 4, and the heated gaseous raw material is flushed into the upper part of the vaporizer 2;

[0079] The circulation pump 3 has a head of 20 to 150 m; the steam pressure in the steam pipe 18 is 0.5 to 4.0 MPa, and the gas phase raw material temperature at the outlet of the heater 4 is 165°C;

[0080] The raw material in the gas phase raw material storage tank 1 is room temperature furfural;

[0081] Step 2: The hydrogen storage tank 15 and the hydrogen from the hydrogen compressor 16 enter the middle of the vaporizer 2, and vaporize the raw materials from the tube side of the heater 4, and then enter the separation tank 5 after vaporization;

[0082] The ratio of the hydrogen flow rate from the hydrogen compressor 16 to the hydrogen flow rate from the hydrogen storage tank 15 entering the vaporizer 2 is 30:1;

[0083] The gas temperature at the outlet of the vaporizer 2 is 180°C;

[0084] Step 3: The vaporized gas phase enters the separation tank 5 and is flash separated. The liquid phase after flash separation flows back into the vaporizer 2 through the liquid phase reflux port of the vaporizer 2. The flash temperature in the separation tank 5 is 180°C.

[0085] Step 4: the gas phase separated by flash evaporation in the separation tank 5 enters the tube side of the suspended bed tubular reactor 10; there are gaps between the cushion particles in the cushion particle layer 13 and the catalyst particles in the catalyst particle layer 11 when they are piled up, and the gas phase enters the catalyst particle layer 11 through the bottom of the tube side of the suspended bed tubular reactor 10. Due to the existence of gaps, the flow rate of the gas phase increases, and some catalyst particles are blown away by the airflow and move upward with the direction of the airflow; after the catalyst is dispersed to a certain extent, the bed gap expands, the gas flow rate decreases, and the catalyst particles fall under the action of gravity. In the above process, the flow rate of the gas phase can be slowed down to improve the intensified mass transfer and heat transfer. At the same time, the catalyst particles flip during the movement process, which increases the contact between the gas phase and the surface of the catalyst particles and improves the catalytic efficiency;

[0086] Step 5: The shell side of the suspended bed tubular reactor 10 is filled with a heat-conducting medium, and the heat in the plurality of single tubes 12 is heat-exchanged with the heat-conducting medium. The heat-conducting medium after the heat exchange enters the heat transfer tank 6 for cooling. The heat transfer tank 6 is provided with a cooling water coil for heat exchange with the heat-conducting medium. The heat-conducting medium after the heat exchange is replenished into the shell side of the suspended bed tubular reactor 10 through the heat transfer pump 7;

[0087] The heat transfer medium is heat transfer oil or hot water;

[0088] Step 6: The process gas after the reaction in the tube side of the suspended bed tubular reactor 10 enters the heat exchange device 8 to exchange heat with the circulating gas in the gas phase outlet of the product separation tank 9. The process gas after heat exchange enters the product separation tank 9 for flash separation, and the separated liquid phase enters the product tank 14 for storage;

[0089] The process gas temperature entering the heat exchange device 8 is 185°C, and the process gas temperature exiting the heat exchange device 8 is 40°C;

[0090] The flash temperature in the product separation tank 9 is 40°C;

[0091] Step 7: The circulating gas in the product separation tank 9 enters the hydrogen compressor 16 through the gas phase outlet of the product separation tank 9 to be pressurized, then preheated in the heat exchange device 8, and merges with the hydrogen coming out of the hydrogen storage tank 15 to enter the vaporizer 2.

[0092] Example 3

[0093] A furfural hydrogenation reaction system includes a gas phase raw material storage tank 1 and a hydrogen storage tank 15, wherein the gas phase raw material storage tank 1 and the hydrogen storage tank 15 are connected to the tube side of a suspended bed tubular reactor 10 through a feeding unit, the shell side of the suspended bed tubular reactor 10 is connected to a heat removal unit, the tube side outlet of the suspended bed tubular reactor 10 is connected to a product separation tank 9 through a heat exchange device 8, and the liquid phase outlet of the product separation tank 9 is connected to a product tank 14. A plurality of single tubes 12 are arranged inside the suspended bed tubular reactor 10, a cushion particle layer 13 is arranged inside the single tube 12, and a catalyst particle layer 11 is arranged on the top of the cushion particle layer 13. The diameter of the single tube 12 of the suspended bed tubular reactor 10 is 32 mm. The diameter of the cushion particles in the cushion particle layer 13 is 7.5 mm. The catalyst in the catalyst particle layer 11 is spherical, and the diameter of the spherical catalyst is 2.6 mm. The feeding unit includes a vaporizer 2 connected to a gas phase raw material storage tank 1 and a hydrogen storage tank 15 respectively, a circulating heating part is provided at the lower part of the vaporizer 2, a gas phase outlet at the top of the vaporizer 2 is connected to a separation tank 5, a top of the separation tank 5 is connected to the tube side inlet end of the suspended bed tubular reactor 10, and a lower liquid outlet of the separation tank 5 is connected to a liquid phase reflux port of the vaporizer 2. The circulating heating part includes a circulating pipeline provided between the bottom and the upper part of the vaporizer 2 and connected to the vaporizer 2, a circulating pump 3 is provided on the circulating pipeline at the bottom of the vaporizer 2, a heater 4 is provided on the circulating pipeline between the circulating pump 3 and the upper part of the vaporizer 2, and the shell side of the heater 4 is connected to a steam pipeline 18 and a condensate pipeline 17. The heat removal unit includes a heat transfer tank 6 connected to the lower part of the shell side of the suspended bed tubular reactor 10, and the heat transfer tank 6 is connected to the upper part of the shell side of the suspended bed tubular reactor 10 through a heat transfer pump 7. The gas phase outlet of the product separation tank 9 is connected to the vaporizer 2 through the hydrogen compressor 16 and the hot side end of the heat exchange device 8, and the tube side outlet end of the suspended bed tubular reactor 10 is connected to the product separation tank 9 through the cold side end of the heat exchange device 8.

[0094] A reaction method using a furfural hydrogenation reaction system, the reaction method comprising the following steps:

[0095] Step 1: The gaseous raw material in the gaseous raw material storage tank 1 enters the vaporizer 2, is pressurized by the circulating pump 3 arranged at the lower part of the vaporizer 2, and exchanges heat with the steam in the shell side of the heater 4 in the tube side of the heater 4, and the heated gaseous raw material is flushed into the upper part of the vaporizer 2;

[0096] The circulation pump 3 has a head of 20 to 150 m; the steam pressure in the steam pipe 18 is 0.5 to 4.0 MPa, and the gas phase raw material temperature at the outlet of the heater 4 is 115°C;

[0097] The raw material in the gas phase raw material storage tank 1 is room temperature furfural;

[0098] Step 2: The hydrogen storage tank 15 and the hydrogen from the hydrogen compressor 16 enter the middle of the vaporizer 2, and vaporize the raw materials from the tube side of the heater 4, and then enter the separation tank 5 after vaporization;

[0099] The ratio of the hydrogen flow rate from the hydrogen compressor 16 to the hydrogen flow rate from the hydrogen storage tank 15 entering the vaporizer 2 is 18:1;

[0100] The gas temperature at the outlet of the vaporizer 2 is 135°C;

[0101] Step 3: The vaporized gas phase enters the separation tank 5 and is flash separated. The liquid phase after flash separation flows back into the vaporizer 2 through the liquid phase reflux port of the vaporizer 2. The flash temperature in the separation tank 5 is 135°C.

[0102] Step 4: the gas phase separated by flash evaporation in the separation tank 5 enters the tube side of the suspended bed tubular reactor 10; there are gaps between the cushion particles in the cushion particle layer 13 and the catalyst particles in the catalyst particle layer 11 when they are piled up, and the gas phase enters the catalyst particle layer 11 through the bottom of the tube side of the suspended bed tubular reactor 10. Due to the existence of gaps, the flow rate of the gas phase increases, and some catalyst particles are blown away by the airflow and move upward with the direction of the airflow; after the catalyst is dispersed to a certain extent, the bed gap expands, the gas flow rate decreases, and the catalyst particles fall under the action of gravity. In the above process, the flow rate of the gas phase can be slowed down to improve the intensified mass transfer and heat transfer. At the same time, the catalyst particles flip during the movement process, which increases the contact between the gas phase and the surface of the catalyst particles and improves the catalytic efficiency;

[0103] Step 5: The shell side of the suspended bed tubular reactor 10 is filled with a heat-conducting medium, and the heat in the plurality of single tubes 12 is heat-exchanged with the heat-conducting medium. The heat-conducting medium after the heat exchange enters the heat transfer tank 6 for cooling. The heat transfer tank 6 is provided with a cooling water coil for heat exchange with the heat-conducting medium. The heat-conducting medium after the heat exchange is replenished into the shell side of the suspended bed tubular reactor 10 through the heat transfer pump 7;

[0104] The heat transfer medium is heat transfer oil or hot water;

[0105] Step 6: The process gas after the reaction in the tube side of the suspended bed tubular reactor 10 enters the heat exchange device 8 to exchange heat with the circulating gas in the gas phase outlet of the product separation tank 9. The process gas after heat exchange enters the product separation tank 9 for flash separation, and the separated liquid phase enters the product tank 14 for storage;

[0106] The process gas temperature entering the heat exchange device 8 is 143°C, and the process gas temperature exiting the heat exchange device 8 is 27°C;

[0107] The flash temperature in the product separation tank 9 is 27°C;

[0108] Step 7: The circulating gas in the product separation tank 9 enters the hydrogen compressor 16 through the gas phase outlet of the product separation tank 9 to be pressurized, then preheated in the heat exchange device 8, and merges with the hydrogen coming out of the hydrogen storage tank 15 to enter the vaporizer 2.

[0109] In the description of the present invention, it should be noted that, unless otherwise clearly specified and limited, the terms "connection", "connected" and the like should be understood in a broad sense. For example, it can be a fixed connection, an integral connection, or a detachable connection; it can also be the internal connection of two elements; it can be a direct connection, or it can be indirectly connected through an intermediate medium. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances. The above examples are only specific descriptions of the feasible implementation methods of the present invention. They are not intended to limit the scope of protection of the present invention. All equivalent implementation methods, changes and modifications that do not deviate from the technical spirit of the present invention should be included in the scope of protection of the present invention.

Claims

1. A furfural hydrogenation reaction system, comprising a gas phase raw material storage tank (1) and a hydrogen storage tank (15), characterized in that: The gas phase raw material storage tank (1) and the hydrogen storage tank (15) are connected to the tube side of the suspended bed tubular reactor (10) via a feed unit, the shell side of the suspended bed tubular reactor (10) is connected to a heat removal unit, the tube side outlet of the suspended bed tubular reactor (10) is connected to a product separation tank (9) via a heat exchange device (8), and the liquid phase outlet of the product separation tank (9) is connected to a product tank (14); The suspended bed tubular reactor (10) has a plurality of single tubes (12) disposed inside, a cushion particle layer (13) disposed inside the single tubes (12), and a catalyst particle layer (11) disposed on top of the cushion particle layer (13); The heat removal unit comprises a heat transfer tank (6) connected to the lower part of the shell side of the suspended bed tubular reactor (10); the heat transfer tank (6) is connected to the upper part of the shell side of the suspended bed tubular reactor (10) via a heat transfer pump (7).

2. A furfural hydrogenation reaction system according to claim 1, characterized in that: The diameter of a single tube (12) of the suspended bed tubular reactor (10) is 15 to 50 mm.

3. A furfural hydrogenation reaction system according to claim 1, characterized in that: The diameter of the cushion particles in the cushion particle layer (13) is 5 to 10 mm.

4. A furfural hydrogenation reaction system according to claim 1, characterized in that: The catalyst in the catalyst particle layer (11) is spherical, and the diameter of the spherical catalyst is 0.3 mm to 5 mm.

5. A furfural hydrogenation reaction system according to claim 1, characterized in that: The feed unit comprises a vaporizer (2) connected to a gas phase raw material storage tank (1) and a hydrogen storage tank (15) respectively, a circulating heating section is provided at the bottom of the vaporizer (2), a gas phase outlet at the top of the vaporizer (2) is connected to a separation tank (5), the top of the separation tank (5) is connected to the tube side inlet end of the suspended bed tubular reactor (10), and a liquid outlet at the bottom of the separation tank (5) is connected to a liquid phase reflux port of the vaporizer (2).

6. A furfural hydrogenation reaction system according to claim 5, characterized in that: The circulation heating section comprises a circulation pipe (19) disposed between the bottom and the top of the vaporizer (2) and connected to the vaporizer (2); a circulation pump (3) is disposed on the circulation pipe (19) at the bottom of the vaporizer (2); a heater (4) is disposed on the circulation pipe (19) between the circulation pump (3) and the top of the vaporizer (2); and a shell side of the heater (4) is connected to a steam pipe (18) and a condensate pipe (17).

7. A furfural hydrogenation reaction system according to claim 1, characterized in that: The gas phase outlet of the product separation tank (9) is connected to the vaporizer (2) via a hydrogen compressor (16) and the hot side end of the heat exchange device (8), and the tube side outlet end of the suspended bed tubular reactor (10) is connected to the product separation tank (9) via the cold side end of the heat exchange device (8).

8. A reaction method using the furfural hydrogenation reaction system according to any one of claims 1 to 7, characterized in that: The reaction method comprises the following steps: Step 1: The gaseous raw material in the gaseous raw material storage tank (1) enters the vaporizer (2), is pressurized by a circulating pump (3) arranged at the lower part of the vaporizer (2), and is heat-exchanged with the steam in the shell side of the heater (4) in the tube side of the heater (4), and the heated gaseous raw material is flushed into the upper part of the vaporizer (2); The circulation pump 3 has a head of 20 to 150 m; the steam pressure in the steam pipe (18) is 0.5 to 4.0 MPa; the temperature of the gas phase raw material at the outlet of the heater (4) pipe side is 65 to 165°C; The raw material in the gas phase raw material storage tank (1) is furfural at room temperature; Step 2: The hydrogen from the hydrogen storage tank (15) and the hydrogen from the hydrogen compressor (16) enters the middle of the vaporizer (2) and vaporizes the raw material from the tube side of the heater (4), and then enters the separation tank (5) after vaporization; The ratio of the hydrogen flow rate from the hydrogen compressor (16) to the hydrogen flow rate from the hydrogen storage tank (15) entering the vaporizer (2) is 5 to 30:1; The gas temperature at the outlet of the vaporizer (2) is 90 to 180°C; Step 3: The vaporized gas phase enters the separation tank (5) and is flash separated. The liquid phase after flash separation flows back into the vaporizer (2) through the liquid phase reflux port of the vaporizer (2). The flash temperature in the separation tank (5) is 90 to 180° C. Step 4: the gas phase after flash separation in the separation tank (5) enters the tube side of the suspended bed tubular reactor (10); the cushion particles in the cushion particle layer (13) and the catalyst particles in the catalyst particle layer (11) are stacked with gaps, and the gas phase enters the catalyst particle layer (11) through the bottom of the tube side of the suspended bed tubular reactor (10). Due to the existence of gaps, the flow rate of the gas phase increases, and some catalyst particles are blown away by the airflow and move upward along the direction of the airflow; after the catalyst is dispersed to a certain extent, the gap between the bed expands, the gas flow rate decreases, and the catalyst particles fall under the action of gravity. In the above process, the flow rate of the gas phase can be slowed down to enhance mass transfer and heat transfer. At the same time, the catalyst particles flip during the movement process, thereby increasing the contact between the gas phase and the surface of the catalyst particles and improving the catalytic efficiency; Step 5: The shell side of the suspended bed tubular reactor (10) is filled with a heat-conducting medium, and the heat in the plurality of single tubes (12) is exchanged with the heat-conducting medium. After the heat exchange, the heat-conducting medium enters a heat transfer tank (6) for cooling. The heat transfer tank (6) is provided with a cooling water coil for exchanging heat with the heat-conducting medium. After the heat exchange, the heat-conducting medium is replenished into the shell side of the suspended bed tubular reactor (10) through a heat transfer pump (7); The heat transfer medium is heat transfer oil or hot water; Step 6: the process gas after the reaction in the tube side of the suspended bed tubular reactor (10) enters the heat exchange device (8) to exchange heat with the circulating gas in the gas phase outlet of the product separation tank (9), and the process gas after the heat exchange enters the product separation tank (9) for flash separation, and the liquid phase after separation enters the product tank (14) for storage; The process gas temperature entering the heat exchange device (8) is 100 to 185° C., and the process gas temperature exiting the heat exchange device (8) is 14 to 40° C.; The flash temperature in the product separation tank (9) is 14 to 40°C; Step 7: The circulating gas in the product separation tank (9) enters the hydrogen compressor (16) through the gas phase outlet of the product separation tank (9) to be pressurized, and then preheated in the heat exchange device (8), and then merges with the hydrogen coming out of the hydrogen storage tank (15) and enters the vaporizer (2).

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