CN119701800A - Internal circulation fluidized bed and method for calcium cycle catalytic methane dry reforming - Google Patents
Internal circulation fluidized bed and method for calcium cycle catalytic methane dry reforming Download PDFInfo
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Abstract
The invention discloses an internal circulating fluidized bed and a method for calcium circulating catalytic methane dry reforming, wherein the internal circulating fluidized bed comprises an external reactor and an internal reactor, the external reactor is sleeved outside the internal reactor, the inside of the internal reactor is used as a carbon capturing zone for carrying out carbon dioxide adsorption reaction, the area between the internal reactor and the external reactor is used as a carbon conversion zone for carrying out methane dry reforming and catalyst regeneration reaction, the bottoms of the carbon capturing zone and the carbon conversion zone are communicated through a circulating feed inlet, a discharge port at the top of the carbon capturing zone is connected with a gas-solid separator, a solid outlet of the gas-solid separator is connected with the carbon conversion zone, an exhaust gas inlet and an air distribution plate are arranged at the bottom of the internal reactor, a raw material gas inlet is arranged at the bottom of the side wall of the external reactor, and a synthetic gas outlet and a feed inlet are arranged at the top of the external reactor.
Description
Technical Field
The invention relates to the technical field of methane dry reforming reactor design, in particular to an internal circulating fluidized bed device and method for calcium circulating catalytic methane dry reforming.
Background
The dry reforming reaction of methane can convert two greenhouse gases CH 4 and CO 2 into synthesis gas for downstream synthesis of chemical products such as methanol. However, the reaction process temperatures are as high as 1000 ℃ or higher, requiring a large energy input to drive the reaction. The calcium-cycle methane dry reforming technology combines the CO 2 capturing and converting processes, and CaO is used as a bifunctional catalyst, so that on one hand, the adsorption and enrichment of CO 2 on the surface of the catalyst can be promoted, and on the other hand, the calcium-cycle methane dry reforming technology is used as a carrier of a methane dry reforming catalyst, and the surface of the catalyst can be loaded with Ni, ce and other metal elements. The technology can reduce the temperature of methane dry reforming reaction to 600-800 ℃, and greatly reduces the industrial energy consumption of the reaction. In addition, the requirement on the concentration of CO 2 is reduced by adopting the calcium-based catalyst, and industrial waste gas containing a large amount of CO 2 can be directly adopted as a raw material, so that the step of separating CO 2 before the dry reforming reaction is omitted, and the pretreatment time and the economic cost are effectively reduced.
In the prior researches, the dry reforming reaction of the calcium-cycle methane mainly adopts a fixed bed form, and generally comprises two steps of CO 2 pre-adsorption and dry reforming reaction. Because the two-step reaction is a high-temperature reaction, in the industrial process, the frequent gas switching not only reduces the production efficiency, but also causes the safety problem of valves and equipment, thereby preventing the practical application of the technology.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides an internal circulating fluidized bed and a method for calcium circulating catalytic methane dry reforming, which realize the circulation of two-step reactions in the same device and solve the problem that the existing calcium circulating methane dry reforming device cannot continuously and stably produce.
The technical scheme of the invention is as follows:
In a first aspect of the invention, an internal circulating fluidized bed for calcium-cycle catalytic methane dry reforming is provided, comprising an external reactor and an internal reactor, wherein the external reactor is sleeved outside the internal reactor, the inside of the internal reactor is used as a carbon capture zone for carbon dioxide adsorption reaction, and the area between the internal reactor and the external reactor is used as a carbon conversion zone for methane dry reforming and catalyst regeneration reaction;
The bottom of the carbon capture zone is communicated with the bottom of the carbon conversion zone through a circulating feed inlet, a discharge port at the top of the carbon capture zone is connected with a gas-solid separator, and a solid outlet of the gas-solid separator is connected with the carbon conversion zone;
the bottom of the inner reactor is provided with an exhaust gas inlet and an air distribution plate, the bottom of the side wall of the outer reactor is provided with a raw material gas inlet, and the top of the outer reactor is provided with a synthetic gas outlet and a feeding port.
In some embodiments of the invention, the air distribution plate is positioned above an exhaust gas inlet that is fed with industrial exhaust gas containing CO 2 gas.
In some embodiments of the invention, two feed gas inlets are symmetrically arranged left and right, air distribution pipes are arranged at the feed gas inlets, the air distribution pipes are buried in the calcium-based catalyst, and exhaust holes are uniformly distributed on the air distribution pipes.
In some embodiments of the invention, the wall surfaces of the inner reactor and the outer reactor are connected with temperature adjusting devices, and the temperature adjusting devices comprise thermocouples, heating wires and a temperature control system.
In some embodiments of the invention, the catalyst is a calcium-based bifunctional catalyst for dry reforming of methane, and the supported metals include nickel, iron, and platinum.
In some embodiments of the invention, the bottom of the outer reactor is provided with a discharge opening.
In some embodiments of the invention, the exhaust gas discharge port of the gas-solid separator is connected to a pollutant treatment system by a conduit.
In a second aspect of the invention, there is provided a method of operating an internal circulating fluidized bed for calcium-cycle catalytic methane dry reforming comprising:
Waste heat is carried out on the catalyst in the inner reactor and the outer reactor;
introducing industrial waste gas containing CO 2 into the inner reactor through a waste gas inlet to uniformly fluidize catalyst particles;
In the inner reactor, the catalyst adsorbs nitrogen dioxide in the industrial waste gas, and the adsorbed catalyst and the industrial waste gas enter a gas-solid separator;
separating industrial waste gas and catalyst by a gas-solid separator, and allowing the separated catalyst to enter an external reactor;
in the external reactor, the raw material gas is introduced into CH 4 raw material gas, the catalyst reacts with methane, the catalyst is regenerated, and the methane is subjected to dry reforming to generate a synthetic gas product;
The regenerated catalyst enters the inner reactor again through the circulating feed inlet, so that the reaction is circularly carried out.
In some embodiments of the invention, during the carbon capture reaction, an amount of industrial waste gas doped with H 2 O is introduced at the waste gas port, so that the gasification reaction of coke occurs simultaneously in the inner reactor.
In some embodiments of the invention, the catalyst is a Ni/CaO dual function catalyst.
One or more of the technical schemes of the invention has the following beneficial effects:
(1) The invention adopts the internal circulating fluidized bed technology, solves the problem of discontinuous reaction of the fixed bed reactor, realizes continuous and stable calcium circulating methane dry reforming reaction in the same reactor, and remarkably improves the production efficiency.
(2) According to the invention, through continuous cyclic reaction of the catalyst, efficient utilization of CO 2 adsorption heat is realized, so that the requirement on an external heat source is reduced, the energy utilization efficiency of the reactor is improved, and the industrial energy consumption of methane dry reforming is greatly reduced.
(3) Aiming at the problem of carbon deposition of the catalyst, the method directly mixes a small amount of H 2 O into industrial waste gas, has potential to realize synchronous decarburization in the catalyst regeneration process, does not influence continuous execution of dry reforming reaction in an external reactor, effectively saves the catalyst regeneration time, and further promotes industrial application of calcium-cycle methane dry reforming.
(4) Compared with the interconnected double-bed fluidized bed, the internal circulation reactor has the advantages of more compact structure, lower energy consumption and smaller energy loss between the internal reactor and the external reactor, so that the calcium-based catalyst particles are heated more uniformly, the migration and agglomeration of the active phase of the catalyst caused by uneven heating are effectively reduced, and the risk of catalyst deactivation is reduced.
(5) Compared with a double-zone fluidized bed, the internal circulation reactor provided by the invention obviously improves the separation efficiency of CaO and CaCO 3 particles, and realizes effective circulation fluidization of the CaO and CaCO 3 particles, thereby being beneficial to enhancing the selectivity of products and improving the production efficiency of methane dry reforming.
Drawings
FIG. 1 is a schematic diagram of the structure of an internal circulating fluidized bed for calcium-cycle catalytic methane dry reforming of the present invention;
FIG. 2 is a top view of an internal circulating fluidized bed for calcium-cycle catalyzed methane dry reforming according to the present invention;
FIG. 3 is a schematic diagram of the catalyst and product flow in the circulating fluidized bed in the calcium-cycled dry methane reforming of the present invention.
In the figure, 1, an exhaust gas inlet, 2, an air distribution plate, 3, an air distribution pipe, 4, a circulating feed inlet, 5, an outer reactor, 6, an inner reactor, 7, a synthesis gas outlet, 8, a discharge port, 9, a temperature adjusting device, 10, an exhaust gas discharge port, 11, a gas-solid separator, 12, a feed supplement port, 13, a solid outlet, 14, an exhaust hole, 15-an air distribution pipe, 16 and a discharge port.
Detailed Description
The invention will be further described with reference to the drawings and examples.
Example 1
In a typical embodiment of the invention, an internal circulating fluidized bed for calcium circulating catalytic methane dry reforming is provided, as shown in fig. 1, and comprises an external reactor 5 and an internal reactor 6, wherein the external reactor 5 is sleeved outside the internal reactor 6, the inside of the internal reactor 6 is used as a carbon capture zone for carbon dioxide adsorption reaction, and the area between the internal reactor 6 and the external reactor 5 is used as a carbon conversion zone for methane dry reforming and catalyst regeneration reaction;
The bottom of the carbon capture zone is communicated with the bottom of the carbon conversion zone through a circulating feed inlet, a discharge port 8 at the top of the carbon capture zone is connected with a gas-solid separator 11, and a solid outlet 13 of the gas-solid separator 11 is connected with the carbon conversion zone;
the bottom of the inner reactor 6 is provided with an exhaust gas inlet 1 and an air distribution plate 2, the bottom of the side wall of the outer reactor 5 is provided with a raw material gas inlet, and the top of the outer reactor 5 is provided with a synthetic gas outlet 7 and a feed supplement port 12.
In this embodiment, the air distribution plate 2 is located above the exhaust gas inlet 1, the exhaust gas inlet 1 is used for introducing industrial exhaust gas containing CO 2 gas, the air distribution plate 2 is located at the bottom of the inner reactor 6 and is used for uniformly distributing the introduced air flow on the flow section of the inlet of the inner reactor 6, and in the inner reactor 6, the surface of the calcium-based catalyst uniformly adsorbs CO 2 in the industrial exhaust gas and then converts the CO 2 into CaCO 3.
In this embodiment, two feed gas inlets are symmetrically arranged left and right, air distribution pipes 15 are installed at the feed gas inlets, the air distribution pipes 15 are buried in the calcium-based catalyst, air exhaust holes 14 are uniformly distributed on the air distribution pipes 15 to ensure that reactant methane (CH 4) gas can be uniformly introduced into the outer reactor 5, regeneration of calcium oxide and dry reforming reaction of methane are completed in the outer reactor 5 to generate carbon monoxide and hydrogen, a synthesis gas outlet 7 is positioned at the top of the outer reactor 5 and is responsible for discharging product synthesis gas, a feed inlet 12 is positioned at the top of the outer reactor 5 and is used for periodically replenishing the catalyst, and a feed outlet 16 is positioned at the bottom of the outer reactor 5 and is used for periodically replacing the catalyst.
In the embodiment, the gas-solid separator 11 is positioned at the upper part of the inner reactor 6, the material inlet 8 is connected with the inner reactor 6, the solid outlet 13 of the gas-solid separator is connected with the outer reactor 5, the solid outlet 13 of the gas-solid separator extends into the catalyst particle layer of the outer reactor 5 to maintain pressure balance, and the upper part of the gas-solid separator 11 is provided with an exhaust gas discharge port 10. At the discharge port 8, the industrial waste gas carrying the calcium carbonate catalyst particles enters a gas-solid separator 11, at a solid outlet 13, the solid catalyst obtained by centrifugal separation enters the outer reactor 5, and at the waste gas discharge port 10, the decarbonized gas which does not participate in the reaction is discharged after the gas-solid separation and then is conveyed to downstream facilities to complete further pollutant treatment. The circulating feed port 4 is arranged at the bottom of the inner reactor 6, so that the calcium oxide catalyst which has fully reacted can smoothly return to the inner reactor 6 and continue to participate in the carbon capturing process. And the circulating feed port 4 is used for realizing the circulation of the catalyst by utilizing the pressure difference of the internal and external reactors at the same horizontal section.
In this embodiment, the wall surfaces of the inner reactor 6 and the outer reactor 5 are connected with a temperature adjusting device 9, the temperature adjusting device 9 includes a thermocouple, an electric heating wire and a temperature control system, the thermocouple is used for detecting the temperatures in the inner reactor 6 and the outer reactor 5, the electric heating wire is installed on the inner wall surface of the inner reactor 6 and the outer reactor 5 and used for heating the inner reactor 6 and the outer reactor 5, the electric heating wire is used as a supplementary heat source, the temperature control system is used for adjusting the temperatures of the inner reactor and the outer reactor, and the electric heating wire can realize accurate control of the temperatures of the inner reactor and the outer reactor through cooperation with the thermocouple and the temperature control system.
Further, the gas-solid separator 11 and its external piping are equipped with a good insulation system. The wall surface of the inner reactor 6 can realize the heat transfer process from inside to outside, and can transfer the reaction heat of the inner reactor 6 to the outer reactor 5.
In this example, the catalyst is a calcium-based bifunctional catalyst for dry reforming of methane, and the supported metals include nickel, iron, and platinum.
As shown in fig. 2, the inner reactor 6 and the outer reactor 5 are cylindrical, and the height, the cross-sectional area, the included angle and other dimensions of the inner reactor 6 and the outer reactor 5 can be adjusted according to the reaction kinetic parameters. The cross-sectional area of the inner reactor 6 and the outer reactor 5 should be proportional to the residence time of the reaction. The structure shown in the figure is only schematic and needs to be properly adjusted according to the kinetic parameters under different conditions of reaction temperature, reactant concentration, catalyst and the like.
As shown in fig. 3, the working principle of the internal circulating fluidized bed for calcium circulating catalytic methane dry reforming provided in this embodiment is as follows:
Firstly, the catalysts Ni/CaO in the inner reactor 6 and the outer reactor 5 are preheated to 650-750 ℃ by electric heating. Then, the industrial waste gas containing 2-20vol% of CO 2 is introduced into the waste gas inlet 1, the gas passes through the air distribution plate 2 to uniformly fluidize catalyst particles, and the catalyst particles and Ni/CaO undergo CO 2 adsorption reaction in the inner reactor 6 to form Ni/CaCO 3. After the reaction is completed, the industrial waste gas carries Ni/CaCO 3 particles into the gas-solid separator 11. The decarbonized industrial waste gas is discharged from the waste gas discharge port 10 and enters downstream for waste heat recovery, pollutant treatment and the like. Simultaneously, CH 4 raw gas is introduced into the air distribution pipes 15 at the left side and the right side, ni/CaCO 3 particles captured by the gas-solid separator 11 carry heat released by carbon fixation reaction to enter the outer reactor 5, the heat is fully reacted with CH 4 to realize the regeneration of a Ni/CaO catalyst, and the generated synthesis gas (CO and H 2) is discharged from the product discharge port 7 at the upper part. Finally, the Ni/CaO catalyst enters the inner reactor 6 again through the circulating feed port 4, so that the reaction is circulated.
Example 2
In an exemplary embodiment of the present invention, there is provided a method of operating an internal circulating fluidized bed for calcium-cycle catalytic methane dry reforming, comprising:
Waste heat is carried out on the catalyst in the inner reactor and the outer reactor;
introducing industrial waste gas containing CO 2 into the inner reactor through a waste gas inlet to uniformly fluidize catalyst particles;
In the inner reactor, the catalyst adsorbs nitrogen dioxide in the industrial waste gas, and the adsorbed catalyst and the industrial waste gas enter a gas-solid separator;
separating industrial waste gas and catalyst by a gas-solid separator, and allowing the separated catalyst to enter an external reactor;
in the external reactor, the raw material gas is introduced into CH 4 raw material gas, the catalyst reacts with methane, the catalyst is regenerated, and the methane is subjected to dry reforming to generate a synthetic gas product;
The regenerated catalyst enters the inner reactor again through the circulating feed inlet, so that the reaction is circularly carried out.
Aiming at the problem of carbon deposition of the catalyst in the dry reforming process, in the carbon trapping reaction process, industrial waste gas doped with a certain amount of H 2 O is introduced into a waste gas port, so that the gasification reaction of coke synchronously occurs in the inner reactor. At this time, CO 2 generated by coke gasification is captured by CaO at the same time, and the generated CaCO 3 enters the outer reactor 5 and further participates in the dry reforming reaction of methane as a reactant. Therefore, the device can synchronously carry out catalyst regeneration and decarbonization, does not influence the continuity of the dry reforming reaction in the external reactor, and obviously saves the time required by catalyst regeneration.
In this example, the catalyst is a Ni/CaO dual function catalyst, including a calcium-based dual function catalyst useful for dry reforming of methane, supported metals including, but not limited to, nickel, iron, platinum, etc., with the Ni/CaO catalyst representing only one example.
While the foregoing description of the embodiments of the present invention has been presented in conjunction with the drawings, it should be understood that it is not intended to limit the scope of the invention, but rather, it is intended to cover all modifications or variations within the scope of the invention as defined by the claims of the present invention.
Claims (10)
1. The internal circulating fluidized bed for calcium circulating catalytic methane dry reforming is characterized by comprising an external reactor and an internal reactor, wherein the external reactor is sleeved outside the internal reactor, the inside of the internal reactor is used as a carbon capture zone for carrying out carbon dioxide adsorption reaction, and a region between the internal reactor and the external reactor is used as a carbon conversion zone for carrying out methane dry reforming and catalyst regeneration reaction;
The bottom of the carbon capture zone is communicated with the bottom of the carbon conversion zone through a circulating feed inlet, a discharge port at the top of the carbon capture zone is connected with a gas-solid separator, and a solid outlet of the gas-solid separator is connected with the carbon conversion zone;
the bottom of the inner reactor is provided with an exhaust gas inlet and an air distribution plate, the bottom of the side wall of the outer reactor is provided with a raw material gas inlet, and the top of the outer reactor is provided with a synthetic gas outlet and a feeding port.
2. The internal circulating fluidized bed for calcium-cycling catalyzed dry methane reforming of claim 1, wherein the air distribution plate is positioned above an exhaust gas inlet that is fed with an industrial exhaust gas comprising CO 2 gas.
3. The internal circulating fluidized bed for calcium-circulating catalytic methane dry reforming as claimed in claim 1, wherein two feed gas inlets are symmetrically arranged on the left and right sides, air distribution pipes are arranged at the feed gas inlets, the air distribution pipes are buried in a calcium-based catalyst, and exhaust holes are uniformly distributed on the air distribution pipes.
4. The internal circulating fluidized bed for calcium-cycling catalytic dry methane reforming according to claim 1, wherein the wall surfaces of the internal reactor and the external reactor are connected with temperature regulating devices, and the temperature regulating devices comprise thermocouples, heating wires and a temperature control system.
5. The internal circulating fluidized bed for calcium-cycled catalytic dry methane reforming of claim 1, wherein the catalyst is a calcium-based dual function catalyst for dry methane reforming, and the supported metal comprises nickel, iron, and platinum.
6. The internal circulating fluidized bed for calcium-cycling catalyzed dry methane reforming of claim 1, wherein the bottom of the external reactor is provided with a discharge port.
7. The internal circulating fluidized bed for calcium-cycling catalyzed dry methane reforming of claim 1, wherein the exhaust gas discharge port of the gas-solid separator is connected to the pollutant treating system by a conduit.
8. A method of operating an internal circulating fluidized bed for calcium-cycle catalytic methane dry reforming according to any one of claims 1-7, comprising:
Waste heat is carried out on the catalyst in the inner reactor and the outer reactor;
introducing industrial waste gas containing CO 2 into the inner reactor through a waste gas inlet to uniformly fluidize catalyst particles;
In the inner reactor, the catalyst adsorbs nitrogen dioxide in the industrial waste gas, and the adsorbed catalyst and the industrial waste gas enter a gas-solid separator;
separating industrial waste gas and catalyst by a gas-solid separator, and allowing the separated catalyst to enter an external reactor;
in the external reactor, the raw material gas is introduced into CH 4 raw material gas, the catalyst reacts with methane, the catalyst is regenerated, and the methane is subjected to dry reforming to generate a synthetic gas product;
The regenerated catalyst enters the inner reactor again through the circulating feed inlet, so that the reaction is circularly carried out.
9. The method of claim 8, wherein during the carbon capture reaction, an industrial waste gas containing a certain amount of H 2 O is introduced into the waste gas port, so that the gasification reaction of coke occurs synchronously in the inner reactor.
10. The method of operating an internal circulating fluidized bed for calcium-cycled catalytic dry methane reforming of claim 8, wherein the catalyst is a Ni/CaO dual function catalyst.
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