CN116747811A - Diffusion welding micro-channel reactor with catalyst - Google Patents
Diffusion welding micro-channel reactor with catalyst Download PDFInfo
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- CN116747811A CN116747811A CN202310741240.6A CN202310741240A CN116747811A CN 116747811 A CN116747811 A CN 116747811A CN 202310741240 A CN202310741240 A CN 202310741240A CN 116747811 A CN116747811 A CN 116747811A
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- 238000009792 diffusion process Methods 0.000 title abstract description 33
- 238000003466 welding Methods 0.000 title abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 185
- 239000011949 solid catalyst Substances 0.000 claims abstract description 123
- 238000000034 method Methods 0.000 claims abstract description 23
- 230000008569 process Effects 0.000 claims abstract description 19
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- 238000001354 calcination Methods 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 229910045601 alloy Inorganic materials 0.000 claims description 2
- 239000000956 alloy Substances 0.000 claims description 2
- 229910000856 hastalloy Inorganic materials 0.000 claims description 2
- 238000003754 machining Methods 0.000 claims description 2
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- 239000010935 stainless steel Substances 0.000 claims description 2
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0053—Details of the reactor
- B01J19/0073—Sealings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/02—Apparatus characterised by being constructed of material selected for its chemically-resistant properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00783—Laminate assemblies, i.e. the reactor comprising a stack of plates
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00801—Means to assemble
- B01J2219/00804—Plurality of plates
- B01J2219/00808—Sealing means
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00819—Materials of construction
- B01J2219/00835—Comprising catalytically active material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00873—Heat exchange
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00993—Design aspects
- B01J2219/00995—Mathematical modeling
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Abstract
The invention belongs to the technical field of chemical reaction reinforcement, and particularly relates to a diffusion welding micro-channel reactor with a catalyst. According to the invention, the necking-shaped concave cavities for fixing the solid catalyst are arranged on the reaction flow channel along the fluid advancing direction in the reaction flow channel of the reaction plate, so that the problems that the diffusion welding micro-channel reactor accurately fixes the catalyst position in the channel and the heat exchange capacity of the reaction side under laminar flow is weak can be solved. In addition, the catalyst replacement method of the invention can solve the problem that the solid catalyst is difficult to replace in the micro-channel by utilizing the cooperation of the catalyst and the detachable pipe box. Meanwhile, the specific stacking form of the reaction plate and the heat exchange plate can solve the problems of catalyst filling of the diffusion welding micro-channel reactor and uneven temperature distribution of the reaction flow channel of the diffusion welding micro-channel reactor in the amplifying process.
Description
Technical Field
The invention belongs to the technical field of chemical reaction reinforcement, and particularly relates to a diffusion welding micro-channel reactor with a catalyst.
Background
Compared with an intermittent reaction kettle, the micro-channel reactor can realize the refinement and the serialization of the reaction process, can precisely control the reaction time, can improve the reaction conversion rate and the selectivity, and has extremely important experience, safety and environmental protection values in the technical field of chemical reaction reinforcement. However, due to the small size of the channels of the microchannel reactor, the microchannel reactor needs to be enlarged to increase the yield.
For this reason, in chinese patent publication No. CN112403413B, an integrated countercurrent enhanced diffusion welding micro-channel reactor is disclosed, and the diffusion welding micro-channel reactor is characterized in that a plurality of parallel semicircular channels are etched on each plate by chemical etching technology, the radius of the channels is generally 0.5-2.5 mm, then a plurality of plates with parallel semicircular channels are welded to form a core body by using a vacuum diffusion welding process, and finally the diffusion welding micro-channel reactor with a quantity amplifying characteristic is formed by other processes. The diffusion welding microchannel reactor not only remarkably improves the flux of reactants, but also maintains the high-efficiency and compact characteristics of the microchannel reactor. However, since most chemical reactions require a solid catalyst, there is a high demand for a technology of filling a microchannel with the solid catalyst in addition to the realization of an internal amplification process of the microchannel reactor; the mere internal amplification, while neglecting the basic catalyst filling process, is clearly unsuitable.
The current combination of microchannels and solid catalysts can be divided into two types, filling and coating. The catalyst is made into foam metal and filled into channels in Chinese patent publication No. CN105968123B, the catalyst and the micro channels are combined by utilizing micro channels of the foam metal, the average pore diameter of the foam metal is 0.1-10 mm, the length of the foam metal is 10-1000 mm, the foam metal can be filled into the channels after the plate sheet is machined into larger grooves, the filling mode is not suitable for a diffusion welding micro channel reactor, and the filling foam metal has larger flow resistance. In the chinese patent with publication number CN115245790a, the catalyst is coated on the inner surface of the channel by immersing the channel in the precursor liquid, then drying in the air, and baking, so that the catalyst and the reactor become an integral body, but the obvious problem is that the amount of the catalyst used in the channel is small, and the catalyst is difficult to replace after deactivation, most importantly, the temperature required in the vacuum diffusion welding process of the diffusion welding microchannel reactor is 1800-2000 ℃, and even if the catalyst is coated on the inner wall of the channel first, it is difficult to ensure that the active components of the catalyst are not deactivated in the ultra-high temperature environment in the diffusion welding process. Based on the above, whether a novel diffusion welding microchannel reactor can be developed or not, so that the high processing capacity and the high compactness of the reactant materials of the novel diffusion welding microchannel reactor are ensured, and meanwhile, the novel diffusion welding microchannel reactor also has the advantages of convenience in filling of a solid catalyst, simplicity in positioning and convenience in assembly and disassembly of the whole structure, and is a technical problem to be solved in recent years.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a catalyst-carrying diffusion welding microchannel reactor, which can easily realize accurate fixing of single-point positions, even multiple-point positions, of a solid catalyst, is beneficial to improving flexible use of the solid catalyst, can effectively save the reaction space of a reaction runner, and can effectively ensure the filling convenience of the solid catalyst.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a catalyst-carrying diffusion-welded microchannel reactor, characterized in that: a necking-shaped concave cavity for fixing a solid catalyst is arranged on the reaction flow channel along the fluid travelling direction in the reaction flow channel of the reaction plate; the pockets satisfy the following relationship:
wherein:
P n when the material inlet of the reaction runner is taken as the origin of coordinates, the position point of the recess of the nth stage is in mm;
n is the number of stages of the recess;
l is the length of the reaction plate, and the unit is mm;
D n the recess amplitude in mm for the n-th stage of the pocket;
i is the neck section length of the pocket in mm.
Preferably, the solid catalyst is a cylindrical controllable structure catalyst with a hollow straight cylindrical shape, a through groove with a groove length direction parallel to the axis of the solid catalyst is arranged at the outer wall of the solid catalyst, and the groove bottoms of the through grooves are connected with the hollow channels of the solid catalyst by virtue of radially extending communication holes; the minimum depth of the through groove is greater than or equal to 0.5mm; the straight-through grooves form a turbulent flow area, and the solid areas of the solid catalyst form a porous medium area; the hydraulic radius of the solid catalyst is 0.5-2.5 mm, the hydraulic radius is smaller than the hydraulic radius of the reaction flow channel and larger than the hydraulic radius of the concave cavity with the largest concave amplitude, the length of the solid catalyst is 1-10 mm, and the difference between the diameter of the solid catalyst and the diameter of the reaction flow channel is smaller than 0.1mm.
Preferably, the solid catalyst is a cylindrical controllable structure catalyst with a hollow straight cylindrical shape, the outer wall and the inner wall of the solid catalyst are respectively provided with a W-shaped groove penetrating through two ends of the solid catalyst, and the bottoms of the W-shaped grooves are connected with the hollow channels of the solid catalyst by virtue of radially extending communication holes; the minimum depth of the W-shaped groove is more than or equal to 0.5mm; the W-shaped grooves form a turbulent flow area, and the solid areas of the solid catalyst form porous medium areas; the hydraulic radius of the solid catalyst is 0.5-2.5 mm, the hydraulic radius is smaller than the hydraulic radius of the reaction flow channel and larger than the hydraulic radius with the largest concave amplitude, the length of the solid catalyst is 1-10 mm, and the difference between the diameter of the solid catalyst and the diameter of the reaction flow channel is smaller than 0.1mm.
Preferably, the solid catalyst is a spherical controllable structure catalyst with a hollow spherical shape, through holes are radially arranged between the outer wall and the inner wall of the solid catalyst in a penetrating way, and the minimum aperture of the through holes is more than or equal to 0.5mm; the through holes form a turbulent flow area, and the solid area of the solid catalyst forms a porous medium area; the hydraulic radius of the solid catalyst is 0.5-2.5 mm, and the hydraulic radius is smaller than the hydraulic radius of the reaction flow channel and larger than the hydraulic radius of the concave cavity with the largest concave amplitude, and the difference between the diameter of the solid catalyst and the diameter of the reaction flow channel is smaller than 0.1mm.
Preferably, the porous medium area is formed by a calcination process, the diameter of the holes in the porous medium area is 1-100 mu m, and the porosity is 20% -45%;
preferably, the catalyst replacement method comprises the steps of:
s1, disassembling a reaction inlet pipe box;
s2, introducing high-pressure drying fluid into the reaction outlet pipe box, so that the high-pressure drying fluid enters the reaction flow channel through the material outlet of the reaction plate, and the original solid catalyst in the reaction flow channel is flushed out;
s3, filling a new solid catalyst into the reaction flow channel;
s4, the reaction inlet pipe is packaged back, and the catalyst replacement process is completed.
Preferably, the heat exchanger further comprises a core body, and the heat exchanger comprises a first heat exchange plate, a first reaction plate, a second reaction plate and a second heat exchange plate which are sequentially and repeatedly arranged from top to bottom, wherein grooves are concavely formed on adjacent surfaces of the first reaction plate and the second reaction plate, so that when the two reaction plates are mutually adhered, the grooves on the two reaction plates are mutually matched to form a reaction runner, the first heat exchange plate is provided with an upper heat exchange runner or a prefabricated groove at the position of the first heat exchange plate is matched with an upper plate surface of the first reaction plate to form an upper heat exchange runner, and the second heat exchange plate is provided with a lower heat exchange runner or a prefabricated groove at the position of the second heat exchange plate is matched with a lower plate surface of the second reaction plate to form a lower heat exchange runner; the projection plane is taken along the assembly direction of the parallel core body, the pipe orifices between the upper heat exchange flow channel and the reaction flow channel and between the lower heat exchange flow channel and the reaction flow channel are mutually crossed, and the rest flow channel areas of the reaction flow channel and the two heat exchange flow channels are mutually overlapped.
Preferably, the first heat exchange plate, the first reaction plate, the second reaction plate and the second heat exchange plate which are sequentially stacked from top to bottom are a group of sub-modules, and the sub-modules are more than two groups and are sequentially assembled along the assembly direction of the core body.
Preferably, the upper heat exchange flow channel and the lower heat exchange flow channel at the core body are overlapped with each other on the projection of the assembly direction of the parallel core body; the pipe inlet and the pipe outlet of each heat exchange runner of the core are respectively provided with a heat exchange inlet pipe box and a heat exchange outlet pipe box, and the pipe inlet end and the pipe outlet end of the reaction runner of the core are respectively fixedly connected with a reaction outlet pipe box and a reaction inlet pipe box, wherein:
the core body and the reaction inlet pipe box form detachable thread sealing fit through bolts and sealing gaskets, and the other end of the core body is welded with the reaction outlet pipe box; the heat exchange inlet pipe box and the heat exchange outlet pipe box are respectively welded at two sides of the core body.
Preferably, the flow direction of the fluid in the reaction flow channel and each heat exchange flow channel is concurrent flow or countercurrent flow or cross flow or staggered countercurrent flow; the cross sections of the grooves and the prefabricated grooves at the two heat exchange plates are semicircular grooves or semi-elliptic grooves or rectangular grooves or arched grooves with the hydraulic radius of 0.5-2 mm, and the flow passage forms of the grooves and the prefabricated grooves at the two heat exchange plates are straight flow passages or wavy flow passages or zigzag flow passages; the material of each reaction plate and each heat exchange plate is stainless steel or titanium material or nickel base alloy or hastelloy, and the processing mode of each reaction plate and each heat exchange plate is chemical etching or machining.
The invention has the beneficial effects that:
1) Through the scheme, the recess is arranged in the reaction flow channel of the microchannel reactor, so that the precise fixation of single-point positions, even multi-point positions, of the solid catalyst can be easily realized, the flexible use of the solid catalyst is improved, and the reaction space of the reaction flow channel can be effectively saved. In actual use, due to the existence of the concave cavities, the solid catalyst can slide to the concave cavities by gravity or under the pushing of fluid after being filled from the inlet, and the solid catalyst has the characteristics of convenient filling and accurate positioning. In addition, multistage recess also is favorable to strengthening the heat exchange ability of reaction side, especially in order to realize long enough dwell time and make the condition that reaction side flow state is laminar, the existence of multistage recess can arouse the velocity of flow change many times, and accurate control vortex takes place the position, and the multiple spot breaks the fluid boundary layer, improves the problem that the heat exchange ability of core reaction zone is difficult to improve under the laminar flow state.
2) Furthermore, the invention also carries out controllable control on the structure of the solid catalyst, solves the problem of matching the commercial catalyst with the traditional micro-channel reactor, and can adapt to the appearance structures of different channel types by customizing the structure of the solid catalyst. For example: for the zigzag micro-channel, the shape structure of the solid catalyst can be made into a sphere, so that the solid catalyst can be filled conveniently; for the straight flow passage micro-channel, the solid catalyst can be made into a cylinder shape, so that the solid catalyst can be filled into the micro-channel, and the heat transfer capacity of the solid catalyst can be enhanced. Compared with the traditional commercial catalyst, the solid catalyst, namely the catalyst with the controllable structure, has controllable structure and higher manufacturing precision. By controlling the structure of the solid catalyst, the solid part of the solid catalyst is porous medium, so that materials can still contact active components in the solid part in a diffusion mode, and holes or grooves are formed in the surface of the solid part, so that occupied space of the solid catalyst in a microchannel is reduced, pressure drop of the microchannel is reduced, pumping power is saved, and the solid catalyst is conveniently filled into or purged out of the microchannel. In addition, the existence of grooves or holes on the outer wall and even the inner wall of the solid catalyst can also help to form a special channel between the solid catalyst and the flow channel, thereby promoting the heat transfer-mass transfer process, enhancing the heat conduction and heat convection process, reducing the heat conduction resistance, increasing the convection heat transfer coefficient and reducing the heat loss. The existence of the special channel can also control the material flow direction, realize the customization of the catalyst reaction process path and improve the reaction selectivity and conversion rate.
3) The spherical solid catalyst is more suitable for wavy reaction channels, and can solve the problem that the catalyst in the tortuous channels is difficult to fill. The spherical solid catalyst can flexibly flow in the micro-channel or the reaction flow channel by utilizing the characteristic of small spherical movement resistance, and the spherical solid catalyst can ensure that any spherical surface crossing in the flow direction has the same structure, so that great difference in the effect of chemical reaction can not occur when fluid passes through any spherical surface of the axisymmetric spherical solid catalyst.
4) In actual design, the problem of the adaptation of the solid catalyst and the shape of the micro-channel can be further solved by means of the specific solid catalyst; the heat and mass transfer process of the solid catalyst can be further enhanced by customizing the structure and the size of the solid catalyst with high precision, the efficient matching with the multistage concave cavities is realized, and finally the purposes of filling, fixing and replacing the catalyst are realized more easily.
5) As a preferable scheme of the scheme, the invention further ensures each reaction flow channel 1 by respectively arranging a mode of overlapping the corresponding reaction plate and the heat exchange plate: 1, the temperature uniformity and the temperature control capability of the reaction flow channel are improved along with the heat exchange process, and the conversion rate and the selectivity of the reaction flow channel are improved. In addition, through setting up two reaction plates as each other mirror image, when buckling each other and keeping microchannel characteristic, increased the usage space of reaction side runner, increased material circulation, reduced the passageway pressure drop, obviously also do benefit to further optimizing the filling, fixing and the change effect of catalyst.
6) The reaction material throughput of the diffusion welding micro-channel reactor is increased by arranging a plurality of parallel flow channels on the heat exchange plate and the reaction plate and by arranging the core body in a multi-plate stacking mode. In addition, the heat exchange side flow channel and the reaction side flow channel are crossed at the inlet and the outlet and overlapped at the rest in the stacking direction, so that reasonable arrangement of the corresponding pipe boxes is facilitated; on the other hand, the temperature control of the heat exchange flow channel on the reaction flow channel and the uniformity of the thermal efficiency of a plurality of reaction flow channels are ensured.
7) The sealing mode of the reaction inlet pipe box is realized by matching the bolt fastening and the sealing gasket such as a multiple chemical corrosion resistant gasket, so that the contradiction that the traditional full-diffusion micro-channel reactor needs to be filled with the catalyst before vacuum diffusion welding sealing is solved, and the overheat deactivation of the solid catalyst in the ultra-high temperature diffusion welding environment is avoided. Meanwhile, the filling of the solid catalyst can be completed before the sealing of the detachable diffusion welding micro-channel reactor through the detachable reaction inlet pipe box, and the solid catalyst can be replaced on line directly by disassembling the reaction inlet pipe box and by means of blowing after the deactivation of the solid catalyst, so that the device is very flexible and convenient to use. The adoption of the multiple chemical corrosion resistant gasket can prevent the material leakage caused by the corrosion of the reaction material to the gasket, and can also solve the multiple elastic compensation problem possibly existing in a mechanical sealing mode under the condition of large temperature change caused by reaction, thereby preventing the material leakage caused by the loss and pre-tightening of bolts under the temperature change condition.
8) From the above, it can be seen that the microchannel reactor of the invention has the characteristics of convenient catalyst fixing and simple catalyst replacement process; in addition, the reactor utilizes the micro-channel to strengthen the reaction and heat exchange process, and the device occupies small area and has low installation difficulty. The invention also provides a catalyst structure with a controllable structure, which is used for solving the problems of rapid filling and online replacement of the catalyst; the catalyst structure can be used for controlling the catalytic reaction path, and the effect is remarkable.
Drawings
FIG. 1 is a layout position diagram of pockets;
FIG. 2 is a view showing a disassembled state of the solid catalyst and the reaction plate;
FIGS. 3, 4 and 5 are schematic perspective views of three embodiments of solid catalysts;
fig. 6 is a schematic perspective view of a heat exchange plate;
FIG. 7 is a schematic view of a disassembled state of the core;
FIG. 8 is a schematic perspective view of a microchannel reactor.
The actual correspondence between each label and the component name of the invention is as follows:
10-core; 10 a-a first reaction plate; 10 b-a second reaction plate; 10 c-a first heat exchange plate; 10 d-a second heat exchange plate; 11-pockets; 12-grooves; 13-prefabricating grooves;
20-a solid catalyst; a 21-porous media region; 22-spoiler region;
31-reaction inlet manifold box; 32-reaction outlet pipe box;
41-a heat exchange inlet pipe box; 42-a heat exchange outlet pipe box;
50-bolts.
Detailed Description
For ease of understanding, the specific structure and operation of the present invention will be further described herein with reference to FIGS. 1-8:
in the structure embodying the present invention, referring to fig. 8, the core 10 formed by each reaction plate and heat exchange plate is assembled with the corresponding tube box to form the microchannel reactor shown in fig. 8.
More specifically, the structure shown in fig. 8 includes first a reaction-heat exchange functional unit, i.e., the core 10, and also includes four tube boxes in different orientations, i.e., a reaction inlet tube box 31, a reaction outlet tube box 32, a heat exchange inlet tube box 41, and a heat exchange outlet tube box 42. The reaction-heat exchange functional unit includes a plurality of groups of sub-modules, each group of sub-modules includes a first heat exchange plate 10c, a first reaction plate 10a, a second reaction plate 10b and a second heat exchange plate 10d, which are sequentially stacked from top to bottom as shown in fig. 7. At this time, the first and second reaction plates 10a and 10b constitute the aforementioned reaction plates, and the first and second heat exchange plates 10c and 10d constitute the aforementioned heat exchange plates.
In addition, as shown in fig. 2, after the reaction channels formed by the grooves 12 at the first reaction plate 10a and the second reaction plate 10b are used for accommodating the solid catalyst 20, the fluid traveling direction of the reaction channels and the fluid traveling direction of the heat exchange channels formed by the prefabricated grooves 13 at the two heat exchange plates have the characteristics of coincidence and intersection at the same time on the projection of the stacking direction. In other words, the projections of part of the channels of the inlet and the outlet of the heat exchange plate in the stacking direction are intersected with the reaction channels, and the projections of the rest of the channels in the stacking direction are overlapped with the reaction channels, as shown in fig. 7. At this time, the projection surfaces are formed along the assembly direction of the parallel core 10, the pipe openings between the upper heat exchange flow channel and the reaction flow channel and between the lower heat exchange flow channel and the reaction flow channel are all crossed, and the rest flow channel areas of the reaction flow channel and the two heat exchange flow channels are overlapped with each other.
Further, the grooves 12 at each reaction plate may be in various manners, such as straight grooves or wave grooves, and the like, so as to form straight flow channel type reaction-heat exchange functional subunits and wave flow channel type reaction-heat exchange functional subunits.
In order to precisely control the fixing position of the solid catalyst 20, the present invention may further provide a multistage recess 11 in the flow path of the reaction plate to flexibly fix the catalystAnd (5) a chemical agent position. The arrangement position of the pockets 11 satisfies the following relation:wherein n is the number of stages and L is the plate length; the magnitude of the recess 11 satisfies the relation: d (D) (n) =0.1n; the units are all millimeters. At this time, the material inlet of the reaction runner is taken as the origin of coordinates, the position of the concave cavity 11 of the first stage is positioned at the center of the plate, and the amplitude of the concave cavity 11 is 0.1mm; the second stage of pockets 11 are located at 0.75L of the plate, the pockets 11 being 0.2mm in amplitude, and so on; the length of the recess 11 is 1-3 mm.
Furthermore, each heat exchange plate can be subdivided into a direct-current channel heat exchange plate and a wave-shaped channel heat exchange plate according to different channel forms. The working medium flowing in the heat exchange plate is used as a second flowing working medium, and the working medium flowing in the reaction plate is used as a first flowing working medium; the flow directions of the first flowing working medium and the second flowing working medium can be concurrent or countercurrent, and reasonable flow directions can be freely selected according to the physical properties and chemical properties of the first flowing working medium and the second flowing working medium, the required chemical reaction temperature gradient distribution control and the like.
Specifically, the reaction inlet pipe box 31 in this embodiment is a detachable mechanical seal pipe box, and the opposite side is a reaction outlet pipe box 32; if the detachable diffusion welding micro-channel reactor needs the downstream flow mode of the relation between the flow directions of the first flowing working medium and the second flowing working medium in the use process, the heat exchange inlet pipe box 41 of the second flowing working medium and the heat exchange outlet pipe box 42 of the second flowing working medium are communicated with the pipe orifice of the heat exchange plate. If the flow direction relation of the first flowing working medium and the second flowing working medium is in a countercurrent flow mode in the use process of the detachable diffusion welding micro-channel reactor, the reaction inlet pipe box 31 and the reaction outlet pipe box 32 are unchanged, and the heat exchange inlet pipe box 41 and the heat exchange outlet pipe box 42 are replaced. In addition, in order to facilitate the filling and replacement of the solid catalyst 20, the present invention provides the reaction inlet pipe box 31 as a mechanical seal pipe box; the other tube boxes are diffusion welded sealed tube boxes, which are not detachable without damaging the core 10. In order to achieve good sealing performance, corresponding matching grooves and sealing gaskets are respectively arranged at the mechanical matching positions of the core body 10 and the corresponding pipe box; the mating groove and gasket may be multi-layered, primarily to prevent chemical corrosion and temperature changes that may cause the bolt 50 to lose pretension, preventing leakage of chemicals and reaction products.
In particular, a cylindrical solid catalyst 20 and a spherical solid catalyst 20 are also provided in fig. 2 to 5.
When the solid catalyst 20 is a cylindrical controllable structure catalyst with a hollow straight cylindrical shape, a through groove with a groove length direction parallel to the axis of the solid catalyst 20 is arranged at the outer wall of the solid catalyst 20, and the bottom of the through groove is connected with the hollow channel of the solid catalyst 20 by virtue of a radially extending communication hole; the minimum depth of the through groove is greater than or equal to 0.5mm; the through grooves constitute a turbulence zone 22, and the solid areas of the solid catalyst 20 constitute a porous medium area 21.
When the solid catalyst 20 is a cylindrical controllable structure catalyst with a hollow straight cylindrical shape, the outer wall and the inner wall of the solid catalyst 20 are respectively provided with a W-shaped groove penetrating through the two ends of the solid catalyst 20, and the bottoms of the W-shaped grooves are connected with the hollow channels of the solid catalyst 20 by virtue of radially extending communication holes; the minimum depth of the W-shaped groove is more than or equal to 0.5mm; the W-shaped grooves constitute a turbulence zone 22, and the solid areas of the solid catalyst 20 constitute a porous medium area 21.
When the solid catalyst 20 is a spherical controllable structure catalyst with a hollow sphere shape, through holes are radially and penetratingly arranged between the outer wall and the inner wall of the solid catalyst 20, and the minimum aperture of the through holes is more than or equal to 0.5mm; the through holes constitute the turbulence areas 22, and the solid areas of the solid catalyst 20 constitute the porous medium areas 21.
Meanwhile, the hydraulic radius of the solid catalyst 20 is 0.5-2.5 mm, and the hydraulic radius is smaller than the hydraulic radius of the reaction flow channel and larger than the hydraulic radius of the concave cavity 11 with the largest concave amplitude, and the difference between the diameter of the solid catalyst 20 and the diameter of the reaction flow channel is smaller than 0.1mm.
It will be appreciated thus far that the three types of solid catalysts 20 described above, namely the porous media regions 21 of the controlled structure catalysts shown in fig. 3-5, contain a large number of pores with characteristic dimensions on the order of microns, which result mainly from the catalyst support forming process; when the first flow medium passes through the porous medium region 21, the flow path is uncontrollable, and the flow form is mainly concentration diffusion; the turbulence zone 22 of the controlled structure catalyst is then provided as a combination of holes and/or grooves, even grooves with a meandering path or axially symmetric isodiametric holes. The structure and form of the turbulent flow region can be determined according to the physical property and chemical property of the fluid working medium and the required heat and mass transfer effect. The purpose of the turbulent flow region 22 is to reduce the proportion of the first flowing medium flowing through the catalyst in a penetrating manner, improve the turbulence degree of the first flowing medium, reduce the heat conduction resistance of the catalyst, improve the convective heat transfer coefficient of the first flowing medium, and finally improve the selectivity and conversion rate of the catalytic reaction by customizing the catalytic reaction path.
Example 1:
for further understanding of the invention, the chemical reaction of hydrogen production by reforming methanol is taken as an example, and the main steps are as follows:
sa. Cu/ZnO/Al configuration 2 O 3 And (3) printing the slurry into a green body with a controllable structure by adopting a digital photo-curing 3D printing technology, calcining the green body to form a catalyst carrier, and finally adding active components into the carrier to dry and calcine the carrier to form the catalyst with the controllable structure.
Sb. the reaction flow channel and the heat exchange flow channel with the multistage recess 11 are formed by a chemical etching method, and after the corresponding reaction plates and the heat exchange plates are stacked according to a specific stacking rule, the core 10 is formed by vacuum diffusion welding. The specific stacking rule takes two reaction plates and two heat exchange plates as sub-stacking units or sub-modules as an example: two reaction plates are fastened to each other and form a stacked form of first heat exchange plates 10 c-first reaction plates 10 a-second reaction plates 10 b-second heat exchange plates 10d with the other two heat exchange plates. After the core 10 is formed, an upper clamping plate and a lower clamping plate may be additionally disposed; of course, as shown in fig. 8, the uppermost heat exchange plate and the lowermost heat exchange plate of the core 10 may be directly fixed to the corresponding tube boxes. Subsequently, the heat exchange inlet pipe box 41, the heat exchange outlet pipe box 42 and the reaction outlet pipe box 32 are welded and sealed with the core 10; after the next filling step of the solid catalyst 20 is completed, the sealing of the reaction inlet manifold 31 and the core 10 is finally completed, and the sealing mode of the reaction inlet manifold 31 and the core 10 may be mechanical sealing or welding sealing. Example 1 to facilitate catalyst replacement, a mechanical seal that is more easily removable was employed.
Sc. after the filling and sealing of the solid catalyst 20 are completed, the diffusion welding micro-channel reactor carrying the solid catalyst 20 is connected to a system platform for preparing hydrogen by reforming methanol. Firstly, continuously introducing a mixture of methanol and steam preheated in advance to a reaction side, then introducing clean high-temperature heat conduction oil to a heat exchange side, collecting hydrogen at a reaction outlet pipe box 32 after the reaction starts, and collecting heat conduction oil after heat exchange at a heat exchange outlet pipe box 42.
Sd. when it is desired to replace the solid catalyst 20 in the diffusion-welded microchannel: firstly, disassembling the diffusion welding micro-channel reactor, then disassembling the reaction inlet pipe box 31, next introducing high-pressure drying fluid such as high-pressure nitrogen or air into the reaction outlet pipe box 32, after all the used solid catalysts 20 are blown out, refilling new solid catalysts 20, then reinstalling the reaction inlet pipe box 31, and finally placing the micro-channel reactor with the replaced solid catalysts 20 on a methanol reforming hydrogen production platform for the next use.
The monolithic catalyst macrostructure provided in the step Sa can be shown in fig. 3, where the length of the solid catalyst 20 is 10mm, the outer diameter of the solid catalyst is 3.8mm, eight grooves with rectangular cross-section, length of 1mm and width of 0.5mm are formed on the outer edge of the solid catalyst, and five communicating holes with equidistant holes with aperture of 0.5mm are formed in the grooves.
The reaction flow channel of the reaction plate provided in the step Sb is a direct flow channel with three-stage cavities 11, the length of each cavity 11 is 2mm, the position of the cavity 11 of the first stage is positioned at the 1/2 position of the plate, and the diameter of the cavity 11 is 3.9mm; the second stage of pockets 11 are located at the 3/4 position of the plate, the pockets 11 being 3.8mm in diameter; the third stage of pockets 11 are located in the plate 7/8 position, the pockets 11 being 3.7mm in diameter, so that the catalyst fixing position will start from the second stage of pockets 11 position, depending on the physical dimensions of the catalyst of the controllable structure.
The methanol vapor in step Sc is supplied from an evaporator. Firstly, introducing the aqueous methanol solution into an evaporation device, and introducing the aqueous methanol solution into the reaction side of the microchannel reactor after the temperature of the aqueous methanol vapor is preheated to be more than 100 ℃ by an electric heating mode. The preheating temperature of the methanol vapor can be adjusted according to the reaction requirement, and a regulating valve is arranged between the evaporation device and the core 10 and used for regulating the inlet flow of the methanol vapor. In addition, the temperature of the heat transfer oil introduced into the heat exchange side of the core 10 is controlled to be 260 to 300 ℃ to increase the conversion rate of methanol, and the methanol reforming reaction is continuously and automatically operated until the reaction is completed.
The pressure of the high-pressure nitrogen or air used in the step Sd is about 4 MPa; before the reaction inlet manifold 31 is removed and reinstalled, it is considered to replace the gasket between the new reaction inlet manifold 31 and the core 10.
It has been found that the microchannel reactor or the microchannel reactor of the present invention is suitable for use in cases where the temperature is sensitive and chemical reactions such as alcohol reforming reactions and alkane reforming reactions that require the solid catalyst 20 are also suitable for use in cases where the temperature is sensitive and chemical reactions such as nitration reactions that do not require the solid catalyst 20 are also suitable for use in cases where hydrogenation reactions that are performed in a high pressure environment are required.
It will be understood by those skilled in the art that the present invention is not limited to the details of the foregoing exemplary embodiments, but includes other specific forms of the same or similar structures that may be embodied without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
The technology, shape, and construction parts of the present invention, which are not described in detail, are known in the art.
Claims (10)
1. A catalyst-carrying diffusion-welded microchannel reactor, characterized in that: a neck-shaped recess (11) for fixing the solid catalyst (20) is arranged on the reaction flow channel along the fluid travelling direction in the reaction flow channel of the reaction plate; the recess (11) satisfies the following relation:
wherein:
P n when the material inlet of the reaction runner is taken as the origin of coordinates, the position point of the recess (11) of the nth stage is in mm;
n is the number of stages of the recess (11);
l is the length of the reaction plate, and the unit is mm;
D n the recess amplitude in mm of the recess (11) of the nth stage;
i is the length of the neck section of the recess (11), in mm.
2. A catalyst-supported diffusion-welded microchannel reactor according to claim 1, wherein: the solid catalyst (20) is a cylindrical controllable structure catalyst with a hollow straight cylindrical shape, a through groove with a groove length direction parallel to the axis of the solid catalyst (20) is arranged at the outer wall of the solid catalyst (20), and the bottom of the through groove is connected with a hollow channel of the solid catalyst (20) by virtue of a radially extending communication hole; the minimum depth of the through groove is greater than or equal to 0.5mm; the through grooves form a turbulent flow area (22), and the solid areas of the solid catalyst (20) form a porous medium area (21); the hydraulic radius of the solid catalyst (20) is 0.5-2.5 mm, the hydraulic radius is smaller than the hydraulic radius of the reaction flow channel and larger than the hydraulic radius of the concave cavity (11) with the largest concave amplitude, the length of the solid catalyst (20) is 1-10 mm, and the difference between the diameter of the solid catalyst (20) and the diameter of the reaction flow channel is smaller than 0.1mm.
3. A catalyst-supported diffusion-welded microchannel reactor according to claim 1, wherein: the solid catalyst (20) is a cylindrical controllable structure catalyst with a hollow straight cylindrical shape, W-shaped grooves penetrating through two ends of the solid catalyst (20) are formed in the outer wall and the inner wall of the solid catalyst (20), and the bottoms of the W-shaped grooves are connected with the hollow channels of the solid catalyst by virtue of radially extending communication holes; the minimum depth of the W-shaped groove is more than or equal to 0.5mm; the W-shaped grooves form a turbulent flow area (22), and the solid area of the solid catalyst (20) forms a porous medium area (21); the hydraulic radius of the solid catalyst (20) is 0.5-2.5 mm, the hydraulic radius is smaller than the hydraulic radius of the reaction flow channel and larger than the hydraulic radius with the largest concave amplitude, the length of the solid catalyst (20) is 1-10 mm, and the difference between the diameter of the solid catalyst (20) and the diameter of the reaction flow channel is smaller than 0.1mm.
4. A catalyst-supported diffusion-welded microchannel reactor according to claim 1, wherein: the solid catalyst (20) is a spherical controllable structure catalyst with a hollow spherical shape, through holes are radially and penetratingly arranged between the outer wall and the inner wall of the solid catalyst (20), and the minimum aperture of the through holes is larger than or equal to 0.5mm; the through holes form a turbulent flow area (22), and the solid area of the solid catalyst (20) forms a porous medium area (21); the hydraulic radius of the solid catalyst (20) is 0.5-2.5 mm, and the hydraulic radius is smaller than the hydraulic radius of the reaction flow channel and larger than the hydraulic radius of the concave cavity (11) with the largest concave amplitude, and the difference between the diameter of the solid catalyst (20) and the diameter of the reaction flow channel is smaller than 0.1mm.
5. A catalyst-supported diffusion-welded microchannel reactor according to claim 2, 3 or 4, wherein: the porous medium region (21) is formed by a calcination process, the diameter of the holes in the porous medium region (21) is 1-100 mu m, and the porosity is 20% -45%.
6. A catalyst-supported diffusion-welded microchannel reactor according to claim 2, 3 or 4, wherein: the catalyst replacement method comprises the following steps:
s1, disassembling a reaction inlet pipe box (31);
s2, introducing high-pressure drying fluid into the reaction outlet pipe box (32) so that the high-pressure drying fluid enters the reaction flow channel through the material outlet of the reaction plate, and flushing out the original solid catalyst (20) in the reaction flow channel;
s3, filling a new solid catalyst (20) into the reaction flow channel from the inlet of the reaction plate;
s4, the reaction inlet pipe box (31) is installed back, and the catalyst replacement process is completed.
7. A catalyst-supported diffusion-welded microchannel reactor according to claim 1 or 2 or 3 or 4, wherein: the heat exchange device comprises a core body, and is characterized by further comprising a first heat exchange plate (10 c), a first reaction plate (10 a), a second reaction plate (10 b) and a second heat exchange plate (10 d) which are sequentially arranged in a stacked manner from top to bottom, wherein grooves (12) are concavely formed on adjacent surfaces of the first reaction plate (10 a) and the second reaction plate (10 b), so that when the two reaction plates are mutually adhered, the grooves (12) on the two reaction plates are mutually matched to form a reaction runner, the first heat exchange plate (10 c) is provided with an upper heat exchange runner or a prefabricated groove at the position of the first heat exchange plate (10 c) is matched with an upper plate surface of the first reaction plate (10 a) to form an upper heat exchange runner, and the second heat exchange plate (10 d) is provided with a lower heat exchange runner or a prefabricated groove at the position of the second heat exchange plate (10 d) is matched with a lower plate surface of the second reaction plate (10 b) to form a lower heat exchange runner; the projection surfaces are arranged along the assembly direction of the parallel core body (10), the pipe orifices between the upper heat exchange flow channel and the reaction flow channel and between the lower heat exchange flow channel and the reaction flow channel are mutually crossed, and the rest flow channel areas of the reaction flow channel and the two heat exchange flow channels are mutually overlapped.
8. A catalyst-supported diffusion-welded microchannel reactor according to claim 7, wherein: the first heat exchange plates (10 c), the first reaction plates (10 a), the second reaction plates (10 b) and the second heat exchange plates (10 d) which are sequentially stacked from top to bottom are a group of sub-modules, and the sub-modules are more than two groups and are sequentially assembled along the assembly direction of the core body (10).
9. A catalyst-supported diffusion-welded microchannel reactor according to claim 7, wherein: the upper heat exchange flow channel and the lower heat exchange flow channel at the core body (10) are overlapped with each other on the projection of the assembly direction of the parallel core body (10); a heat exchange inlet pipe box (41) and a heat exchange outlet pipe box (42) are respectively arranged at a pipe inlet and a pipe outlet of each heat exchange flow channel of the core body (10), and a pipe outlet end and a pipe inlet end of a reaction flow channel of the core body (10) are respectively fixedly connected with a reaction outlet pipe box (32) and a reaction inlet pipe box (31), wherein:
the core body (10) and the reaction inlet pipe box (31) form detachable thread sealing fit through a bolt (50) and a sealing gasket, and the other end of the core body (10) is welded with the reaction outlet pipe box (32); the heat exchange inlet pipe box (41) and the heat exchange outlet pipe box (42) are respectively welded at two sides of the core body (10).
10. A catalyst-supported diffusion-welded microchannel reactor according to claim 9, wherein: the flow direction of the fluid in the reaction flow channel and each heat exchange flow channel is concurrent flow or countercurrent flow or cross flow or staggered countercurrent flow; the cross sections of the grooves (12) and the prefabricated grooves (13) at the two heat exchange plates are semicircular grooves or semicircular elliptical grooves or rectangular grooves or arched grooves with the hydraulic radius of 0.5-2 mm, and the flow passage forms of the grooves (12) and the prefabricated grooves (13) at the two heat exchange plates are straight flow passages or wave-shaped flow passages or zigzag flow passages; the material of each reaction plate and each heat exchange plate is stainless steel or titanium material or nickel base alloy or hastelloy, and the processing mode of each reaction plate and each heat exchange plate is chemical etching or machining.
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| CN117268146A (en) * | 2023-11-15 | 2023-12-22 | 中国核动力研究设计院 | Diffusion welding heat exchanger and design method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117268146A (en) * | 2023-11-15 | 2023-12-22 | 中国核动力研究设计院 | Diffusion welding heat exchanger and design method thereof |
| CN117268146B (en) * | 2023-11-15 | 2024-01-26 | 中国核动力研究设计院 | Diffusion welding heat exchanger and design method thereof |
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