CN114832731B - Spiral reactor for coupling efficient compact strong endothermic/exothermic reaction - Google Patents
Spiral reactor for coupling efficient compact strong endothermic/exothermic reaction Download PDFInfo
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Abstract
The application relates to a spiral reactor for coupling efficient compact strong endothermic/exothermic reactions, which comprises the following steps: a. preparing a spiral stainless steel tube; b. welding and connecting the spiral stainless steel tube and the flange; c. a fluid distribution device is designed at the front end of the porous spiral tube; d. filling a first reaction catalyst in the stainless steel tube, introducing a first raw material gas into the stainless steel tube through an inlet, and discharging the first raw material gas through a lower outlet; e. the outer wall of the spiral stainless steel pipe and the reactor shell form a second reaction cavity, and a second catalyst is filled in the second reaction cavity; f. the second raw material gas is introduced into the second reaction cavity through the side inlet, the heat released by catalytic combustion is quickly transferred to the catalyst through the spiral stainless steel tube, and the tail gas is discharged through the side outlet. The catalyst is uniformly heated, the response time is fast, the mass transfer time of the catalyst is long, the volume is small, the structure is compact and the like through the staggered distribution of the reaction cavities, and the catalyst has great application value in industry.
Description
Technical Field
The application relates to the technical field of gas-solid heterogeneous catalysis, in particular to a spiral reactor for coupling efficient, compact and strong endothermic/exothermic reactions.
Background
The chemical industry is a support of national economy and is closely related to our lives. The catalyst is used as the core for strengthening chemical processes and is a key technology in various industries such as energy, chemical industry, environmental protection and the like, so how to design and develop a high-efficiency catalyst and a reactor is important.
In chemical production, most of catalytic processes are strong heat absorption and strong heat radiation gas-solid multiphase reactions, and catalytic reactions are usually carried out in a form of filling a particle catalyst in a fixed bed reactor, and in order to ensure that the catalyst reaction temperature is reached and the temperature of the reactor is maintained to be uniform, an external electric heater or a fuel combustion form is usually adopted for continuously supplying heat. In industrial practical application, the conventional reactor has low heat efficiency and poor heat transfer performance of catalyst materials, 30-50% of heat loss is usually caused, a large number of heat preservation devices are usually added outside the reactor to reduce the heat loss, the reaction devices are large in scale, and the problems of internal cold and hot spots, slow temperature starting, uneven bed heating and the like cannot be avoided.
The micro-reactor is valued by universities, companies and institutions from the middle 90 th century, and the micro-channel reactor relieves the problems of uneven heat transfer, mass transfer limitation and the like of the catalyst bed to a certain extent, so that chemical reaction under the uniform temperature or even isothermal conditions is possible. However, the catalyst coating amount is low, the catalyst falling rate is high, the processing cost of the matrix is high, and the processing precision is extremely high, so that the catalyst is limited to experimental research and pilot plant test stages, and the catalyst cannot be applied to large-scale industry.
The application fully combines the advantages of long residence time, high catalyst loading capacity, simple operation, micro-reactor pressure reduction, small volume, uniform heat transfer and the like of the particle catalyst, further reduces the cold start time and temperature response characteristic of the catalyst, provides a spiral reactor preparation method for coupling efficient compact and strong endothermic/exothermic reactions, provides a specific feasible scheme for developing the efficient catalyst reactor preparation with uniform and controllable temperature, low energy consumption, small volume and high efficiency, and has very high industrial application value.
Disclosure of Invention
The application aims to solve the problems of low internal cold and hot spots, slow temperature start, uneven bed heating, low catalyst coating amount, high catalyst falling rate, high matrix processing cost and the like of a conventional fixed bed reactor in the prior art, fills the blank of application of a spiral tube reactor in the field of catalysis, and provides a spiral reactor for coupling efficient, compact and strong endothermic/exothermic reactions.
The application relates to a spiral reactor for coupling efficient compact strong endothermic/exothermic reactions, which is realized by the following technical scheme:
a spiral reactor for efficient compact strong endothermic/exothermic reaction coupling, characterized in that:
a. preparing a spiral stainless steel pipe, specifically designing pipe diameter, length and number according to reaction types, and preparing the spiral stainless steel pipe;
b. adopting a welding method to weld the spiral stainless steel pipe and the flange;
c. a fluid distribution device is designed at the front end of the spiral stainless steel pipe, so that reactants in each reaction pipe are uniformly distributed;
d. filling a catalyst required by a first reaction in a spiral stainless steel tube, introducing a first raw material gas into a reactor through a front inlet, completely reacting the first raw material gas with the catalyst, and discharging the first raw material gas through a lower outlet;
e. all the outer walls of the spiral stainless steel pipes and the reactor shell form a second reaction cavity;
f. filling a second catalyst in the second reaction cavity, introducing a second raw material gas into the reactor through a side inlet, completely reacting the second raw material gas by the second catalyst, and discharging the second raw material gas through a side outlet;
g. the second catalyst catalyzes and burns the second raw material gas, and the generated heat is quickly transferred to the catalyst through the spiral stainless steel tube, so that the catalyst quickly reaches the required reaction temperature; the reaction temperature is 500 to 1000℃and preferably 600 to 850 ℃.
Furthermore, the catalyst required by the first reaction can be porous particles, a coating can be prepared on the surface of stainless steel, and the whole reaction tube can be integrally formed by adopting a 3D printing porous material. It can also be prepared by compounding particles and a coating.
Further, the catalyst required by the second reaction can be porous particles, a coating can be prepared on the surface, or the particles and the coating can be prepared in a composite way.
Further, the first reaction cavity and the second reaction cavity may be porous spiral pipes, or may be fiber mats, foam materials, corrugated pipes, corrugated nets, porous pipes, porous nets, or the like, and the molding mode is not limited to welding, but may be anchoring, sleeving, nesting, or the like.
Further, the materials of the first reaction cavity and the second reaction cavity can be stainless steel, and also can be Fe-Cr-Al alloy, carbon, siC, ceramic, cordierite or aluminum and the like.
Furthermore, the front end of the porous spiral tube is provided with a fluid distribution device, and the fluid distribution device can be dispensed through a silk screen and foam metal without a fluid distributor.
Further, the spiral microreactor can be square, rectangular, round and the like, and the size of the spiral microreactor can be 0.01-100 m, wherein the size range of the spiral pipe hole is preferably 0.3-20 mm, and the size range of the wall is preferably 0.2-20 mm.
Furthermore, the front end is flanged to connect the front end and the rear end, and a quick connector is adopted or welded integrally.
Furthermore, the first reaction cavity and the second reaction cavity adopt a vertical staggered structure, and can also be in the form of disjoint coaxial tubes in the same direction.
Compared with the prior art, the application has the following positive effects:
the reactor realizes the construction of the catalytic reactor on macroscopic and microscopic levels, skillfully adopts the spiral pipe to fill the catalyst, and the catalyst particles with the micron size are uniformly distributed in a reaction tube with a few millimeters and heated uniformly, so that the amplification effect of the catalyst can be obviously reduced while the heat transfer and mass transfer efficiency is enhanced. Furthermore, the coupling of catalytic reaction is realized by carrying out heat absorption and heat release of different reactions on the inner wall and the outer wall of the same reaction tube, the heat transfer efficiency is greatly enhanced, the limitation of mass and heat transfer is reduced, the response time of the catalytic reactor is greatly reduced, the purpose of high-efficiency operation is realized, and the energy consumption and carbon emission are remarkably reduced.
Based on the existing simple processing technology, the application fully combines the advantages of the particle catalyst and the advantages of the microreactor, realizes the purposes of miniaturization, integration and scale of the catalytic reactor, provides a specific and feasible scheme for developing the preparation of the high-efficiency catalyst reactor with uniform and controllable temperature, low energy consumption, small volume and high efficiency, and has important significance in the field of process reinforcement.
Description of the drawings:
fig. 1: the application relates to a catalytic reactor;
fig. 1-1: a partial view of a catalytic reactor designed according to the application;
fig. 2: example 1 effect time of the application versus conventional reactor map;
fig. 3: inventive example 1 space velocity vs. conventional reactor map.
The marks in the drawings are:
1 a front inlet, a front inlet and a rear inlet,
2 a fluid dispensing device for dispensing a fluid,
3 a catalyst, wherein the catalyst is a catalyst,
4 a spiral stainless steel pipe, wherein the stainless steel pipe is provided with a plurality of grooves,
5 a second reaction cavity body is arranged on the bottom of the first reaction cavity body,
a lower outlet of the water tank is provided with a lower outlet,
a side outlet at the 7-side,
an 8-side inlet port,
9 a reactor shell body, wherein the reactor shell body,
a 10-flange, which is provided with a flange,
11 a second catalyst.
Detailed Description
The following provides a specific embodiment of a spiral reactor for coupling efficient, compact and strong endothermic/exothermic reactions according to the present application.
Example 1:
a spiral reactor for coupling efficient compact strong endothermic/exothermic reactions is characterized in that,
a. designing pipe diameter, length and quantity according to the reaction type, and preparing a spiral stainless steel pipe 4;
b. welding the spiral stainless steel pipe 4 and the flange 10 by adopting a welding method;
c. the front end of the porous spiral tube is provided with a fluid distribution device 2 for realizing the uniform distribution of reactants in each reaction tube;
d. filling a stainless steel tube 4 with a catalyst for preparing hydrogen by reacting phi 3*5 methanol, introducing a methanol aqueous solution with a water-alcohol ratio of 3 into the reactor through a front inlet 1, controlling the reaction temperature to 210 ℃ and the airspeed to 2000 for reaction, and generating H by the reaction 2 And CO is discharged through the lower outlet 6;
e. the outer walls of all the spiral stainless steel pipes 4 and the reactor shell 9 form a second reaction cavity 5;
f. the second reaction cavity is filled with a catalytic combustion catalyst, CH4 gas with the flow rate of 100ml/min is introduced into the reactor through the side inlet 8, and is discharged through the side outlet 7 after the catalytic combustion catalyst is completely reacted;
g. the heat generated by catalytic combustion quickly passes through the methanol hydrogen production catalyst in the spiral stainless steel pipe, so that the catalyst can quickly reach the required reaction temperature, the equilibrium time in the reaction process is only 20min, and no additional heat supply is needed in the reaction engineering.
The first reaction cavity is a porous spiral tube, the material is 316 stainless steel, the diameter is 12mm, the length is 100mm, the particle catalyst is filled, and the catalyst is 0.75-2 mmNi-based catalyst.
The second reaction chamber is a fiber mat with a material of 316. After the high-temperature treatment of the fiber felt, preparing an alumina coating by adopting a slurry method, wherein the thickness of the coating is 0.2-0.3mm, the main material of the coating is gamma-Al 2O3, soaking the fiber felt in Pt solution, and then roasting the fiber felt for 2 hours at 600 ℃ in a protective gas atmosphere. The second reaction cavity is formed by vertically placing a fiber felt and the first reaction cavity.
The front end of the porous spiral tube is provided with a fluid distribution device, and a porous alumina layer is adopted for gas distribution. The front end is flanged for front-rear end connection.
Control group: a tubular reactor is produced by a certain equipment factory in Jiangsu Suzhou, the material is 316, the pipe diameter is 127mm, the height is 100mm, the front end is flanged, and the heating mode adopts an external electric heating catalyst which is 0.75-2 mmNi-based catalyst. And introducing methanol water reaction gas into the reactor, wherein the water-alcohol ratio is 3, the reaction temperature is 210 ℃, and the space velocity is 2000. The front end of the porous spiral tube is provided with a fluid distribution device, and a porous alumina layer is adopted for gas distribution. The front end is flanged for front-rear end connection. The specific effect diagrams are shown in fig. 2 and 3.
Example 2:
a spiral reactor for efficient compact strong endothermic/exothermic reaction coupling comprising the steps of:
a. designing pipe diameter, length and quantity according to the reaction type, and preparing a spiral stainless steel pipe 4;
b. welding the spiral stainless steel pipe 4 and the flange 10 by adopting a welding method;
c. the front end of the porous spiral tube is provided with a fluid distribution device 2 for realizing the uniform distribution of reactants in each reaction tube;
d. the stainless steel tube 4 is filled with a catalyst 3 required by the first reaction, the first raw material gas is introduced into the reactor through the front inlet 1, and is discharged through the lower outlet 6 after the catalyst 3 is completely reacted;
e. the outer walls of all the spiral stainless steel pipes 4 and the reactor shell 9 form a second reaction cavity 5;
f. filling a second catalyst 11 in the second reaction cavity, introducing a second raw material gas into the reactor through a side inlet 8, and discharging the second raw material gas through a side outlet 7 after the second catalyst 11 is completely reacted;
g. the second catalyst 11 catalytically combusts the second feed gas to produce heat which is rapidly transferred to the catalyst 3 through the helical stainless steel tube 4 to rapidly reach its desired reaction temperature.
The first reaction cavity is a porous spiral tube, and is made of 316 stainless steel, and has a diameter of 12mm and a length of 120mm. The internal coating adopts a slurry method to prepare an alumina coating, the thickness of the coating is 0.2-0.3mm, and the main material of the coating is gamma-Al 2 O 3 The active component of the Ni-based catalyst is prepared by an impregnation method, and the loading of the active component is 30%.
The second reaction chamber is a fiber mat with a material of 316. After the high-temperature treatment of the fiber felt, preparing an alumina coating by adopting a slurry method, wherein the thickness of the coating is 0.2-0.3mm, the main material of the coating is gamma-Al 2O3, soaking the fiber felt in Pt solution, and then roasting the fiber felt for 2 hours at 600 ℃ in a protective gas atmosphere. The second reaction cavity is formed by vertically placing a fiber felt and the first reaction cavity.
The front end of the porous spiral tube is provided with a fluid distribution device, and a porous alumina layer is adopted for gas distribution. The front end is flanged for front-rear end connection.
Introducing methanol-water reaction gas into the first reaction cavity, wherein the water-alcohol ratio is 3, the reaction temperature is 210 ℃, and the space velocity is 2000; CO and H2 are introduced into the second cavity, the flow is 200ml/min, and no additional heat supply is needed in the reaction engineering.
Example 3
A spiral reactor for efficient compact strong endothermic/exothermic reaction coupling comprising the steps of:
a. designing pipe diameter, length and quantity according to the reaction type, and preparing a spiral stainless steel pipe 4;
b. welding the spiral stainless steel pipe 4 and the flange 10 by adopting a welding method;
c. the front end of the porous spiral tube is provided with a fluid distribution device 2 for realizing the uniform distribution of reactants in each reaction tube;
d. the stainless steel tube 4 is filled with a catalyst 3 required by the first reaction, the first raw material gas is introduced into the reactor through the front inlet 1, and is discharged through the lower outlet 6 after the catalyst 3 is completely reacted;
e. the outer walls of all the spiral stainless steel pipes 4 and the reactor shell 9 form a second reaction cavity 5;
f. filling a second catalyst 11 in the second reaction cavity, introducing a second raw material gas into the reactor through a side inlet 8, and discharging the second raw material gas through a side outlet 7 after the second catalyst 11 is completely reacted;
g. the second catalyst 11 catalytically combusts the second feed gas to produce heat which is rapidly transferred to the catalyst 3 through the helical stainless steel tube 4 to rapidly reach its desired reaction temperature.
The first reaction cavity is a porous spiral tube, and is made of 316 stainless steel, and has a diameter of 12mm and a length of 120mm. The internal catalyst adopts foam metal, the material is foam Ni, the coating adopts a slurry method to prepare an alumina coating, the thickness of the coating is 0.2-0.3mm, the main material of the coating is gamma-Al 2O3, and the coating weight is 45%. The active component of the Ni-based catalyst is prepared by an impregnation method, and the loading of the active component is 35%.
The second reaction chamber is a fiber mat with a material of 316. After the high-temperature treatment of the fiber felt, preparing an alumina coating by adopting a slurry method, wherein the thickness of the coating is 0.2-0.3mm, the main material of the coating is gamma-Al 2O3, soaking the fiber felt in Pt solution, and then roasting the fiber felt for 2 hours at 600 ℃ in a protective gas atmosphere. The second reaction cavity is formed by vertically placing a fiber felt and the first reaction cavity.
The front end of the porous spiral tube is provided with a fluid distribution device, and a porous alumina layer is adopted for gas distribution. The front end is flanged for front-rear end connection.
Introducing methanol-water reaction gas into the first reaction cavity, wherein the water-alcohol ratio is 3, the reaction temperature is 210 ℃, and the space velocity is 2000; and CO and H2 are introduced into the second cavity, and the flow is 300ml/min. No extra heat supply is needed in the reaction engineering.
Example 4
A spiral reactor for efficient compact strong endothermic/exothermic reaction coupling comprising the steps of:
a. designing pipe diameter, length and quantity according to the reaction type, and preparing a spiral stainless steel pipe 4;
b. welding the spiral stainless steel pipe 4 and the flange 10 by adopting a welding method;
c. the front end of the porous spiral tube is provided with a fluid distribution device 2 for realizing the uniform distribution of reactants in each reaction tube;
d. the stainless steel tube 4 is filled with a catalyst 3 required by the first reaction, the first raw material gas is introduced into the reactor through the front inlet 1, and is discharged through the lower outlet 6 after the catalyst 3 is completely reacted;
e. the outer walls of all the spiral stainless steel pipes 4 and the reactor shell 9 form a second reaction cavity 5;
f. filling a second catalyst 11 in the second reaction cavity, introducing a second raw material gas into the reactor through a side inlet 8, and discharging the second raw material gas through a side outlet 7 after the second catalyst 11 is completely reacted;
g. the second catalyst 11 catalytically combusts the second feed gas to produce heat which is rapidly transferred to the catalyst 3 through the helical stainless steel tube 4 to rapidly reach its desired reaction temperature.
The first reaction cavity is a porous spiral net, and is made of Fe-Cr-Al alloy, and has a diameter of 6mm and a length of 60mm. The internal catalyst adopts a coating method to prepare a coating, the coating adopts a slurry method to prepare an alumina coating, the thickness of the coating is 0.2-0.3mm, the main material of the coating is gamma-Al 2O3, and the coating weight is 45%. The active component of the Ni-based catalyst is prepared by an impregnation method, and the loading of the active component is 35%.
The second reaction chamber is a fiber mat with a material of 316. After the high-temperature treatment of the fiber felt, preparing an alumina coating by adopting a slurry method, wherein the thickness of the coating is 0.2-0.3mm, the main material of the coating is gamma-Al 2O3, soaking the fiber felt in Pt solution, and then roasting the fiber felt for 2 hours at 600 ℃ in a protective gas atmosphere. The second reaction cavity is formed by vertically placing a fiber felt and the first reaction cavity.
The front end of the porous spiral tube is provided with a fluid distribution device, and a porous alumina layer is adopted for gas distribution. The front end is flanged for front-rear end connection.
Introducing methanol-water reaction gas into the first reaction cavity, wherein the water-alcohol ratio is 3, the reaction temperature is 210 ℃, and the space velocity is 2000; and CO and H2 are introduced into the second cavity, and the flow is 300ml/min. No extra heat supply is needed in the reaction engineering.
The foregoing is merely a preferred embodiment of the present application, and it should be noted that modifications and adaptations to those skilled in the art may be made without departing from the concept of the present application, and are intended to be within the scope of the present application.
Claims (2)
1. The preparation method of the spiral reactor for coupling efficient compact strong endothermic/exothermic reactions is characterized by comprising the following technical steps:
a. designing pipe diameter, length and quantity according to the reaction type, and preparing a spiral stainless steel pipe; the spiral stainless steel pipe is a first reaction cavity, the spiral stainless steel pipe is made of 316 stainless steel, has the diameter of 12mm and the length of 100mm, is filled with a granular catalyst, and the catalyst is 0.75-2 mmNi-based catalyst;
b. adopting a welding method to weld the spiral stainless steel pipe and the flange;
c. a fluid distribution device is designed at the front end of the spiral stainless steel pipe, so that reactants in each reaction pipe are uniformly distributed;
d. filling a spiral stainless steel tube with a catalyst for preparing hydrogen by reacting phi 3*5 methanol, introducing a methanol aqueous solution with a water-alcohol ratio of 3 into a reactor through a front inlet, controlling the reaction temperature to 210 ℃, and controlling the airspeed to 2000 ml/(g.h) for reaction to generate H 2 And CO is discharged through a lower outlet;
e. all the outer walls of the spiral stainless steel pipes and the reactor shell form a second reaction cavity;
f. filling a catalytic combustion catalyst in the second reaction cavity, introducing methane gas with the flow rate of 100ml/min into the reactor through a side inlet, completely reacting by the catalytic combustion catalyst, and discharging by a side outlet;
g. the heat generated by catalytic combustion quickly passes through the methanol hydrogen production catalyst in the spiral stainless steel pipe, so that the catalyst can quickly reach the required reaction temperature, the equilibrium time in the reaction process is only 20min, and no additional heat supply is needed in the reaction process;
the second reaction cavity is made of fiber felt, and the material is 316; after the high-temperature treatment of the fiber felt, preparing an alumina coating by adopting a slurry method, wherein the thickness of the coating is 0.2-0.3mm, and the main material of the coating is gamma-Al 2 O 3 Impregnating with Pt solution, and roasting at 600 ℃ for 2 hours in a protective gas atmosphere; the second reaction cavity is formed by vertically placing a fiber felt and the first reaction cavity;
the front end of the porous spiral tube is provided with a fluid distribution device, and a porous alumina layer is adopted for gas distribution; the front end is flanged for front-rear end connection.
2. The method for preparing a spiral reactor for coupling efficient, compact and strong endothermic/exothermic reactions as recited in claim 1, comprising the technical steps of:
a. designing pipe diameter, length and quantity according to the reaction type, and preparing a spiral stainless steel pipe; the spiral stainless steel pipe is made of 316 stainless steel, has the diameter of 12mm and the length of 120mm; the internal coating adopts a slurry method to prepare an alumina coating, the thickness of the coating is 0.2-0.3mm, and the main material of the coating is gamma-Al 2 O 3 Preparing an active component of the Ni-based catalyst by adopting an impregnation method, wherein the loading amount of the active component is 30%;
b. adopting a welding method to weld the spiral stainless steel pipe and the flange;
c. a fluid distribution device is designed at the front end of the spiral stainless steel pipe, so that reactants in each reaction pipe are uniformly distributed;
d. filling a catalyst required by a first reaction in a spiral stainless steel tube, introducing a first raw material gas into a reactor through a front inlet, completely reacting the first raw material gas with the catalyst, and discharging the first raw material gas through a lower outlet;
e. all the outer walls of the spiral stainless steel pipes and the reactor shell form a second reaction cavity;
f. filling a second catalyst in the second reaction cavity, introducing a second raw material gas into the reactor through a side inlet, completely reacting the second raw material gas by the second catalyst, and discharging the second raw material gas through a side outlet;
g. the second catalyst catalyzes and burns the second raw material gas, and the generated heat is quickly transferred to the catalyst through the spiral stainless steel tube, so that the catalyst quickly reaches the required reaction temperature;
the second reaction cavity is made of fiber felt, and the material is 316; after the high-temperature treatment of the fiber felt, preparing an alumina coating by adopting a slurry method, wherein the thickness of the coating is 0.2-0.3mm, and the main material of the coating is gamma-Al 2 O 3 Impregnating with Pt solution, and roasting at 600 ℃ for 2 hours in a protective gas atmosphere; the second reaction cavity is formed by vertically placing a fiber felt and the first reaction cavity;
the front end of the porous spiral tube is provided with a fluid distribution device, and a porous alumina layer is adopted for gas distribution; the front end is flanged for front-rear end connection;
introducing methanol-water reaction gas into the first reaction cavity, wherein the water-alcohol ratio is 3, the reaction temperature is 210 ℃, and the airspeed is 2000 ml/(g.h); CO and H are introduced into the second cavity 2 The flow is 200ml/min, and no additional heat supply is needed in the reaction process.
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| BRPI0711443A2 (en) * | 2006-05-08 | 2011-11-01 | Compactgtl Plc | compact catalytic reactor, methods of performing combustion, and performing a rapid reaction on it, and of controlling the thermal gradient in a catalytic reactor |
| DE102008017344A1 (en) * | 2008-04-04 | 2009-10-08 | Linde Aktiengesellschaft | Process and reactor for carrying out exothermic and endothermic reactions |
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