CN111686648A - Fixed bed hydrogenation micro-interface reaction system - Google Patents
Fixed bed hydrogenation micro-interface reaction system Download PDFInfo
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- CN111686648A CN111686648A CN201910196653.4A CN201910196653A CN111686648A CN 111686648 A CN111686648 A CN 111686648A CN 201910196653 A CN201910196653 A CN 201910196653A CN 111686648 A CN111686648 A CN 111686648A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 123
- 238000005984 hydrogenation reaction Methods 0.000 title claims abstract description 53
- 239000007788 liquid Substances 0.000 claims abstract description 180
- 239000007789 gas Substances 0.000 claims abstract description 71
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 59
- 239000001257 hydrogen Substances 0.000 claims abstract description 56
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 56
- 239000000839 emulsion Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims description 54
- 239000003054 catalyst Substances 0.000 claims description 42
- 238000000926 separation method Methods 0.000 claims description 39
- 230000007246 mechanism Effects 0.000 claims description 18
- 239000012295 chemical reaction liquid Substances 0.000 claims description 17
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- 230000008901 benefit Effects 0.000 abstract description 11
- 230000005501 phase interface Effects 0.000 abstract description 6
- 238000005265 energy consumption Methods 0.000 abstract description 4
- 230000036632 reaction speed Effects 0.000 abstract description 2
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- 239000012071 phase Substances 0.000 description 32
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0242—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly vertical
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
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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
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/001—Controlling catalytic processes
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
- B01J8/0278—Feeding reactive fluids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00823—Mixing elements
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Abstract
The invention provides a fixed bed hydrogenation micro-interface reaction system. The system comprises: a fixed bed reactor and a micro-interface generator; the micro-interface generator is connected with the fixed bed reactor, the pressure energy of hydrogen and/or the kinetic energy of liquid in the reaction process are converted into the surface energy of hydrogen bubbles in the hydrogenation reaction process, the hydrogen bubbles are crushed into micro-bubbles, the micro-bubbles and the liquid are mixed to form a gas-liquid emulsion, and the gas-liquid emulsion enters the fixed bed reactor to perform subsequent reaction; the fixed bed hydrogenation micro-interface reaction system has the advantages of low energy consumption, low operating pressure, large gas-liquid mass transfer phase interface area, high apparent reaction speed, high gas utilization rate and the like.
Description
Technical Field
The invention relates to the technical field of fixed bed reaction systems, in particular to a fixed bed hydrogenation micro-interface reaction system.
Background
At present, gas-liquid-solid and other gas-liquid reaction processes widely exist in the fields of energy, petrifaction, fine chemical engineering and the like. Such as oxidation, hydrogenation, chlorination, and other gas-liquid heterogeneous reactions, the macroscopic reaction rate is generally limited by the mass transfer process. The volume mass transfer coefficient of the gas-liquid reaction is mainly influenced by the mass transfer coefficient and the gas-liquid phase interface area. The research shows that the influence degree of the phase interface area on the volume mass transfer coefficient is large, and the regulation and the control are easy. Therefore, increasing the interfacial area is considered an effective way to increase the rate of gas-liquid macroscopic reactions.
The fixed bed reactor is a common chemical reactor form, and means that a granular solid catalyst or a solid reactant is filled in the reactor to form a stacked bed layer with a certain height, and a gas or liquid material flows through a static fixed bed layer through a granular gap and simultaneously realizes a heterogeneous reaction process. The reactor is characterized in that solid particles filled in the reactor are fixed, and the reactor is different from a moving bed and a fluidized bed in which solid materials move in the reactor, and is also called a packed bed reactor. Fixed bed reactors are widely used in gas-solid phase reactions and liquid-solid phase reactions.
However, the hydrogenation in a fixed bed reaction system to react hydrogen with a reaction liquid has problems: has the problems of large operation pressure, small gas-liquid mass transfer phase interface area, slow apparent reaction speed, low gas utilization rate, large investment, low high consumption, difficult operation and the like.
Disclosure of Invention
In view of the above, the invention provides a fixed bed hydrogenation micro-interface reaction system, which aims to solve the problem of large energy consumption due to insufficient reaction caused by small contact area of hydrogen and liquid in the prior art.
In one aspect, the present invention provides a fixed bed hydrogenation micro-interface reaction system, comprising: the system comprises a fixed bed reactor, a micro-interface generator and a gas-liquid separation tank; wherein,
the micro-interface generator is connected with the fixed bed reactor, the pressure energy of hydrogen and/or the kinetic energy of liquid in the reaction process are converted into the surface energy of hydrogen bubbles in the hydrogenation reaction process, the hydrogen bubbles are crushed into micro bubbles, the micro bubbles are mixed with the liquid in the reaction process to form gas-liquid emulsion, and then the gas-liquid emulsion enters the fixed bed reactor for subsequent reaction;
the fixed bed reactor is used as a reaction site of hydrogenation reaction to form a stable gas-liquid reinforced fixed bed reaction system when the gas-liquid emulsion enters the fixed bed reactor;
the fixed bed reactor is used as a reaction site of hydrogenation reaction to form a stable gas-liquid reinforced fixed bed reaction system when the gas-liquid emulsion enters the fixed bed reactor;
the gas-liquid separation tank is connected with the fixed bed reactor and is used for carrying out gas-liquid separation on the mixture after the reaction in the fixed bed reactor.
Further, in the fixed bed hydrogenation micro-interface reaction system, the micro-interface generator is selected from one or more of a pneumatic micro-interface generator, a hydraulic micro-interface generator and a gas-liquid linkage micro-interface generator.
Further, in the fixed bed hydrogenation micro-interface reaction system, the micro-interface generator is arranged at the upper part of the fixed bed reactor.
Further, in the fixed bed hydrogenation micro-interface reaction system, the micro-interface generator is arranged at the lower part of the fixed bed reactor.
Further, in the above fixed bed hydrogenation micro-interface reaction system, the fixed bed reactor comprises: a reaction tank and a catalyst bed layer; wherein,
the reaction tank is a tank body and is used for providing a reaction space for the gas-liquid emulsion, and a mixture outlet used for outputting the reacted mixture is arranged on the reaction tank;
the catalyst bed is fixed inside the reaction tank, and a catalyst for improving the reaction efficiency of the gas-liquid emulsion is arranged in the catalyst bed.
Further, in the fixed bed hydrogenation micro-interface reaction system, the method further comprises: the device comprises a raw material tank, a power mechanism and a feeding preheater; wherein,
the raw material tank is connected with the power mechanism and used for storing hydrogen and reaction liquid;
the other end of the power mechanism is connected with the feeding preheater and used for providing power for conveying hydrogen and reaction liquid;
the other end of the feed preheater is connected with the micro-interface reactor and is used for preheating the hydrogen and the reaction liquid so as to enable the hydrogen and the reaction liquid to reach the specified temperature.
Furthermore, in the fixed bed hydrogenation micro-interface reaction system, the raw material tank comprises a liquid raw material tank and a gas raw material buffer tank; wherein,
the liquid raw material tank is connected with the feeding pump and used for storing liquid raw materials;
the gas raw material buffer tank is connected with the compressor and used for storing hydrogen.
Further, in the fixed bed hydrogenation micro-interface reaction system, the power mechanism comprises: a feed pump and compressor; wherein,
the feeding pump is connected with the liquid feeding preheater and is used for providing power for conveying liquid raw materials;
the compressor is connected with the gas feed preheater and is used for providing power for conveying hydrogen.
Further, in the above fixed bed hydrogenation micro-interface reaction system, the feed preheater comprises: a liquid feed preheater and a gas feed preheater; wherein,
the liquid feed preheater is connected with the micro-interface generator and is used for preheating the liquid raw material to a specified temperature and sending the liquid raw material into the micro-interface generator;
the gas feed preheater is connected to the micro-interface generator for preheating the hydrogen gas to a specified temperature and feeding it into the micro-interface generator.
Further, in the fixed bed hydrogenation micro-interface reaction system, when the number of the fixed bed reactors is more than one, the highest positions of the connecting pieces connected with each other are sequentially higher than the highest position of the fixed bed reactor arranged in front from back to front.
Compared with the prior art, the fixed bed hydrogenation micro-interface reaction system has the beneficial effects that the micro-interface generator is added in the fixed bed reaction system, hydrogen is crushed into gas with the diameter of 1 mu m or less and d <1mm, a micro-bubble system is formed, micro-bubbles have the advantages of rigidity, good independence, difficult coalescence and the like, so that the gas-liquid reaction is enhanced in the gas-liquid reaction process, the mass transfer efficiency is improved, and emulsion containing a large number of micro-bubbles is obtained, so that a higher phase interface area is formed in the reactor.
Furthermore, the fixed bed hydrogenation micro-interface reaction system has the advantages of high gas utilization rate, high desulfurization rate, less investment, low energy consumption, flexible process and the like in engineering by providing the micro-interface generator.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
FIG. 1 is a schematic structural diagram of an ascending fixed bed hydrogenation micro-interface reaction system provided by an embodiment of the invention;
FIG. 2 is a schematic structural diagram of an ascending multistage fixed bed hydrogenation micro-interface reaction system according to an embodiment of the present invention;
FIG. 3 is a schematic structural diagram of a descending fixed bed hydrogenation micro-interface reaction system provided by an embodiment of the invention;
FIG. 4 is a schematic structural diagram of a descending multistage fixed bed hydrogenation micro-interface reaction system according to an embodiment of the present invention.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described below with reference to examples; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
Referring to fig. 1, in the ascending fixed bed hydrogenation Micro-interface reaction system provided in the embodiment of the present invention, a Micro Interface Generator (MIG) is disposed at a lower portion of a fixed bed reactor, hydrogen gas is broken into Micro bubbles by the MIG during use, a gas-liquid emulsion formed by mixing the formed Micro bubbles and liquid enters the fixed bed reactor through a lower inlet of the fixed bed reactor to perform a subsequent reaction, and a mixture after the reaction is discharged through an upper outlet of the fixed bed reactor to form the ascending fixed bed hydrogenation Micro-interface reaction system, where the system includes: the device comprises a fixed bed reactor 4, a micro-interface generator, a gas-liquid separation tank 5, a raw material tank, a power mechanism and a feeding preheater; the device comprises a raw material tank, a feeding preheater, a micro-interface reactor, a gas-liquid separation tank and a gas-liquid separation tank, wherein the raw material tank is connected with a power mechanism and used for storing hydrogen and reaction liquid, the other end of the power mechanism is connected with the feeding preheater and used for providing power for conveying the hydrogen and the reaction liquid, the other end of the feeding preheater is connected with the micro-interface reactor and used for preheating the hydrogen and the reaction liquid so as to enable the hydrogen and the reaction liquid to reach a specified temperature, the micro-interface generator is arranged at the lower part of a fixed bed reactor 4 and used for crushing the hydrogen into micro bubbles; before the reaction starts, the hydrogen and the liquid are conveyed out through the raw material tank, are provided with power by the power mechanism and are conveyed into the feeding preheater, and enter the micro-interface generator after being preheated by the feeding preheater; the micro-interface generator sets up 4 lower parts of fixed bed reactor, the pressure energy with hydrogen and/or the kinetic energy of the liquid in the reaction process convert into the surface energy of hydrogen bubble in hydrogenation reaction process, make hydrogen breakage be the microbubble, and make microbubble and the liquid mixture of reaction in-process form the gas-liquid emulsion, make the gas-liquid emulsion again enter fixed bed reactor 4 through the import of fixed bed reactor lower part and carry out subsequent reaction again, the product after the reaction is accomplished passes through the export on 4 upper portions of fixed bed reactor and spreads into in gas-liquid separation jar 5, separate through gas-liquid separation jar 5 again, at last discharged.
It is understood that the specific location of the micro-interface generator is not limited in this embodiment, and it is only necessary to dispose it at the lower portion of the fixed bed reactor 4.
With continued reference to fig. 1, the feedstock tank includes: a liquid raw material tank 9 and a gas raw material buffer tank 12, wherein the liquid raw material tank 9 and the gas raw material buffer tank 12 are used for respectively storing a liquid raw material and a gas raw material; the power mechanism comprises: a feed pump 10 and a compressor 13, wherein the feed pump 10 and the compressor 13 are configured to power delivery of the liquid feedstock and the gaseous feedstock, respectively; the feed preheater comprises: a liquid feedstock preheater 11 and a gas feedstock preheater 14, wherein the liquid feedstock preheater 11 and the gas feedstock preheater 14 are used to preheat the liquid feedstock and the gas feedstock, respectively; the inside catalyst bed that is used for promoting the reaction of gas-liquid emulsion that is equipped with of micro-interface generator includes: the gas-liquid linkage type micro-interface generator comprises a gas-liquid linkage type micro-interface generator 3 and a pneumatic micro-interface generator 15, wherein a gas-liquid linkage type micro-interface generator liquid phase inlet 1 and a gas-liquid linkage type micro-interface generator gas phase inlet 2 are arranged on the gas-liquid linkage type micro-interface generator 3, and a pneumatic micro-interface generator liquid phase inlet 16 and a pneumatic micro-interface generator gas phase inlet 17 are arranged on the pneumatic micro-interface generator 15; the gas-liquid separation tank 5 is provided with a liquid phase outlet 7 and a gas phase outlet 6; before the reaction starts, the liquid in the liquid raw material tank 9 is supplied with power by the feed pump 10 and is transmitted into the liquid raw material preheater 11 for preheating, one path of the preheated liquid enters into the gas-liquid linkage type micro-interface generator 3 through the gas-liquid linkage type micro-interface generator liquid phase inlet 1 of the gas-liquid linkage type micro-interface generator 3, the other path of the preheated liquid enters into the pneumatic type micro-interface generator 15 through the pneumatic type micro-interface generator liquid phase inlet 16 of the pneumatic type micro-interface generator 15, the hydrogen in the gas raw material buffer tank 12 enters into the gas raw material preheater 14 for preheating through the power provided by the compressor 13, one path of the preheated hydrogen enters into the gas-liquid linkage type micro-interface generator 3 through the gas phase inlet 2 of the gas-liquid linkage type micro-interface generator, the other path enters into the pneumatic type micro-interface generator 15 through the gas phase inlet 17 of the pneumatic type micro-interface generator, the hydrogen entering the micro interface generator is broken into micro bubbles and mixed with liquid to form gas-liquid emulsion, the formed gas-liquid emulsion enters the fixed bed reactor 4 through an inlet at the lower part of the fixed bed reactor 4 and fully and completely reacts under the catalytic action of the catalyst, the product after the reaction is finished is conveyed into the gas-liquid separation tank 5 through an outlet at the upper part of the fixed bed reactor 4, the unreacted gas raw material and other gas generated by the reaction are extracted from a gas phase outlet 6 of the gas-liquid separation tank 5 through the separation of the gas-liquid separation tank 5, and the liquid phase reaction product is extracted from a liquid phase outlet 7 of the gas-liquid separation tank 5, respectively collected and subjected to subsequent treatment.
It is understood that the number of the fixed bed reactors 4 is not limited in this example, and only needs to be configured according to the needs of the reaction system; meanwhile, the specific positions of the gas phase outlet 6 and the liquid phase outlet 7 of the gas-liquid separation tank 5 are not limited, and only the two are required to discharge the gas and the liquid. Of course, the invention is applicable to the catalyst systems already mentioned, but also to other hydrogenation catalyst systems not mentioned. The operation temperature is properly adjusted according to the activation temperature of the catalyst when different catalysts are used, without affecting the outstanding advantages of the reactor of the invention that the operation pressure can be greatly (or doubly) reduced and the space velocity (handling capacity) can be increased under different catalyst systems.
Referring to fig. 2, the difference between the system and the ascending fixed bed hydrogenation micro-interface reaction system shown in fig. 1 is that the system has a plurality of catalyst beds, each catalyst bed is provided with a corresponding micro-interface generator 3, each micro-interface generator 3 is connected with a gas raw material preheater 14, and the system can make the reaction more complete and thorough due to more catalyst beds.
Referring to fig. 3, in the descending fixed bed hydrogenation Micro-interface reaction system provided in the embodiment of the present invention, a Micro Interface Generator (MIG) is disposed at the upper portion of the fixed bed reactor, hydrogen is broken into Micro bubbles by the Micro interface Generator during use, a gas-liquid emulsion formed by mixing the formed Micro bubbles and liquid enters the fixed bed reactor through an inlet at the upper portion of the fixed bed reactor to perform a subsequent reaction, and a mixture after the reaction is discharged through an outlet at the lower portion of the fixed bed reactor to form the descending fixed bed hydrogenation Micro-interface reaction system. In particular, in the present system, in order to ensure that the reactants can fill the fixed bed reactor 4 during the reaction, the highest point of the outlet connecting pipe should be higher than the fixed bed reactor 4. The system comprises: the device comprises a fixed bed reactor 4, a micro-interface generator, a gas-liquid separation tank 5, a raw material tank, a power mechanism and a feeding preheater; the device comprises a raw material tank, a feeding preheater, a micro-interface reactor, a gas-liquid separation tank and a gas-liquid separation tank, wherein the raw material tank is connected with a power mechanism and used for storing hydrogen and reaction liquid, the other end of the power mechanism is connected with the feeding preheater and used for providing power for conveying the hydrogen and the reaction liquid, the other end of the feeding preheater is connected with the micro-interface reactor and used for preheating the hydrogen and the reaction liquid so as to enable the hydrogen and the reaction liquid to reach a specified temperature, the micro-interface generator is arranged at the upper part of a fixed bed reactor 4 and used for crushing the hydrogen into micro bubbles; before the reaction starts, the hydrogen and the liquid are conveyed out through the raw material tank, are provided with power by the power mechanism and are conveyed into the feeding preheater, and enter the micro-interface generator after being preheated by the feeding preheater; the micro-interface generator sets up fixed bed reactor 4's upper portion, the pressure energy with hydrogen and/or the kinetic energy of the liquid of reaction in-process turn into the surface energy of hydrogen bubble at hydrogenation reaction in-process, make hydrogen breakage be the microbubble, and make the microbubble and the liquid mixture of reaction in-process form the gas-liquid emulsion, make the gas-liquid emulsion again carry out subsequent reaction in getting into fixed bed reactor 4 through the import on fixed bed reactor 4 upper portion again, the product after the reaction is accomplished passes through in the export of fixed bed reactor 4 lower part spreads into gas-liquid separation jar 5, separate through gas-liquid separation jar 5 again, at last by the discharge.
It is understood that the specific location of the micro-interface generator is not limited in this embodiment, and it is only necessary to dispose it at the lower portion of the fixed bed reactor 4.
With continued reference to fig. 3, the feedstock tank includes: a liquid raw material tank 9 and a gas raw material buffer tank 12, wherein the liquid raw material tank 9 and the gas raw material buffer tank 12 are used for respectively storing a liquid raw material and a gas raw material; the power mechanism comprises: a feed pump 10 and a compressor 13, wherein the feed pump 10 and the compressor 13 are configured to power delivery of a liquid feedstock and a gaseous feedstock, respectively; the feed preheater comprises: a liquid feedstock preheater 11 and a gas feedstock preheater 14, wherein the liquid feedstock preheater 11 and the gas feedstock preheater 14 are used to preheat the liquid feedstock and the gas feedstock, respectively; the inside catalyst bed that is used for promoting the reaction of gas-liquid emulsion that is equipped with of micro-interface generator, it includes: the gas-liquid linkage type micro-interface generator comprises a gas-liquid linkage type micro-interface generator 3 and a pneumatic micro-interface generator 15, wherein a gas-liquid linkage type micro-interface generator liquid phase inlet 1 and a gas-liquid linkage type micro-interface generator gas phase inlet 2 are arranged on the gas-liquid linkage type micro-interface generator 3, and a pneumatic micro-interface generator liquid phase inlet 16 and a pneumatic micro-interface generator gas phase inlet 17 are arranged on the pneumatic micro-interface generator 15; the gas-liquid separation tank 5 is provided with a liquid phase outlet 7 and a gas phase outlet 6; before the reaction starts, the liquid in the liquid raw material tank 9 is supplied with power by the feed pump 10 and is transmitted into the liquid raw material preheater 11 for preheating, one path of the preheated liquid enters into the gas-liquid linkage type micro-interface generator 3 through the gas-liquid linkage type micro-interface generator liquid phase inlet 1 of the gas-liquid linkage type micro-interface generator 3, the other path of the preheated liquid enters into the pneumatic type micro-interface generator 15 through the pneumatic type micro-interface generator liquid phase inlet 16 of the pneumatic type micro-interface generator 15, the hydrogen in the gas raw material buffer tank 12 enters into the gas raw material preheater 14 for preheating through the power provided by the compressor 13, one path of the preheated hydrogen enters into the gas-liquid linkage type micro-interface generator 3 through the gas phase inlet 2 of the gas-liquid linkage type micro-interface generator, the other path enters into the pneumatic type micro-interface generator 15 through the gas phase inlet 17 of the pneumatic type micro-interface generator, the hydrogen entering the micro interface generator is broken into micro bubbles and mixed with liquid to form gas-liquid emulsion, the formed gas-liquid emulsion enters the fixed bed reactor 4 through an inlet at the upper part of the fixed bed reactor 4 and fully and completely reacts under the catalytic action of the catalyst, the product after the reaction is finished is conveyed into the gas-liquid separation tank 5 through an outlet at the lower part of the fixed bed reactor 4, the gas raw material which is not completely reacted and other gas generated by the reaction are extracted from a gas phase outlet 6 of the gas-liquid separation tank 5 through the separation of the gas-liquid separation tank 5, and the liquid phase reaction product is extracted from a liquid phase outlet 7 of the gas-liquid separation tank 5, respectively collected and subjected to subsequent treatment.
It is to be understood that the number of the fixed bed reactors 4 is not limited in this example, and may be configured according to the needs of the reaction system. It should be especially noted that in order to ensure that the fixed bed reactor 4 is filled with reactants, the highest point of the outlet connecting pipe should be higher than the top of the fixed bed reactor. The specific positions of the gas phase outlet 6 and the liquid phase outlet 7 of the gas-liquid separation tank 5 are not limited either, and only both of them are required to discharge the gas and the liquid. Of course, the invention is applicable to the catalyst systems already mentioned, but also to other hydrogenation catalyst systems not mentioned. The operation temperature is properly adjusted according to the activation temperature of the catalyst when different catalysts are used, without affecting the outstanding advantages of the reactor of the invention that the operation pressure can be greatly (or doubly) reduced and the space velocity (handling capacity) can be increased under different catalyst systems.
Referring to fig. 4, the system is different from the descending fixed bed hydrogenation micro-interface reaction system shown in fig. 3 in that the system has a plurality of catalyst beds, each catalyst bed is provided with a corresponding micro-interface generator 3, each micro-interface generator 3 is connected with a gas raw material preheater 14, and the system can make the reaction more complete and thorough due to more catalyst beds.
Example one
Fresh hydrogen and gasoline in one pass were mixed at 0.25: the standard volume ratio of 1 is respectively entered into a gas-liquid linkage type micro-interface generator 3 through a gas phase inlet 2 of the gas-liquid linkage type micro-interface generator and a liquid phase inlet 1 of the gas-liquid linkage type micro-interface generator, and the other path is as follows by 800: a standard volume ratio of 1 is entered into the pneumatic micro-interfacial generator 15 through the gas phase inlet 17 of the pneumatic micro-interfacial generator and the liquid phase inlet 16 of the pneumatic micro-interfacial generator, respectively. Under the action of the gas-liquid linkage micro-interface generator 3 and the pneumatic micro-interface generator 15, hydrogen is crushed into micro-bubbles with the average diameter of 1 mu m and d of less than 1mm, gas and liquid are vigorously mixed to form gas-liquid emulsion, the gas-liquid emulsion enters the bottom end of the fixed bed reactor 4, flows from bottom to top, passes through a section of catalyst bed layer 8, and is subjected to hydrodesulfurization reaction under the action of a catalyst. Reaction products enter a gas-liquid separation tank 5 from the top end of a fixed bed reactor 4, unreacted H2 of the fixed bed reactor 4, gas generated by reaction such as H2S and the like are extracted from a gas phase outlet 6 of the gas-liquid separation tank, liquid phase oil products subjected to hydrodesulfurization are extracted from a liquid phase outlet 7 of the gas-liquid separation tank, and the liquid phase oil products are respectively collected for subsequent treatment.
The reaction pressure in the fixed bed reactor 4 is 3MPa, and the reaction temperature is 220 ℃. The fixed bed reactor 4 is internally provided with a molybdenum-nickel catalyst, and the space velocity is controlled to be 0.3h-1. The sulfur content in the raw material gasoline is 120ppm, and the gasoline is subjected to hydrodesulfurizationAfter the reaction scheme treatment, the concentration was reduced to 20 ppm.
Example two
Fresh hydrogen and kerosene were mixed in one pass at 0.3: the standard volume ratio of 1 is respectively entered into a gas-liquid linkage type micro-interface generator 3 through a gas phase inlet 2 of the gas-liquid linkage type micro-interface generator and a liquid phase inlet 1 of the gas-liquid linkage type micro-interface generator, and the other path is divided into 900 parts by weight: a standard volume ratio of 1 is entered into the pneumatic micro-interfacial generator 15 through the gas phase inlet 17 of the pneumatic micro-interfacial generator and the liquid phase inlet 16 of the pneumatic micro-interfacial generator, respectively. Under the action of the gas-liquid linkage micro-interface generator 3 and the pneumatic micro-interface generator 15, the hydrogen is crushed into d with the average diameter of 1 mu m or less<1mm of microbubbles, gas and liquid are mixed vigorously to form a gas-liquid emulsion, the gas-liquid emulsion enters the top end of the fixed bed reactor 4, flows from top to bottom, passes through a section of catalyst bed layer 8, and is subjected to hydrodesulfurization reaction under the action of a catalyst. The reaction product enters a gas-liquid separation tank 5 from the bottom end of the fixed bed reactor 4, and the unreacted H in the fixed bed reactor 42And H formed by reaction2And S and other gases are extracted from a gas phase outlet 6 of the gas-liquid separation tank, and the liquid-phase oil product subjected to hydrodesulfurization is extracted from a liquid phase outlet 7 of the gas-liquid separation tank, collected respectively and subjected to subsequent treatment.
The reaction pressure in the fixed bed reactor 4 is 3MPa, and the reaction temperature is 250 ℃. The fixed bed reactor 4 is internally provided with a molybdenum-nickel catalyst, and the space velocity is controlled to be 1.2h-1. The sulfur content in the raw material kerosene was 150ppm, which was reduced to 50ppm after the hydrodesulfurization reaction.
EXAMPLE III
Fresh hydrogen and diesel were mixed in one pass at 0.2: the standard volume ratio of 1 is respectively entered into a gas-liquid linkage type micro-interface generator 3 through a gas phase inlet 2 of the gas-liquid linkage type micro-interface generator and a liquid phase inlet 1 of the gas-liquid linkage type micro-interface generator, and the other path is defined by 1000: a standard volume ratio of 1 is entered into the pneumatic micro-interfacial generator 15 through the gas phase inlet 17 of the pneumatic micro-interfacial generator and the liquid phase inlet 16 of the pneumatic micro-interfacial generator, respectively. Under the action of the gas-liquid linkage micro-interface generator 3 and the pneumatic micro-interface generator 15, the hydrogen is crushed into d with the average diameter of 1 mu m or less<1mm ofThe micro bubbles and gas-liquid are mixed vigorously to form gas-liquid emulsion, the gas-liquid emulsion enters the bottom end of the fixed bed reactor 4, flows from bottom to top, passes through a section of catalyst bed layer 8, and is subjected to hydrodesulfurization reaction under the action of a catalyst. The reaction product enters a gas-liquid separation tank 5 from the top end of the fixed bed reactor 4, and the unreacted H in the fixed bed reactor 42And H formed by reaction2And S and other gases are extracted from a gas phase outlet 6 of the gas-liquid separation tank, and the liquid-phase oil product subjected to hydrodesulfurization is extracted from a liquid phase outlet 7 of the gas-liquid separation tank, collected respectively and subjected to subsequent treatment.
The reaction pressure in the fixed bed reactor 4 is 6MPa, and the reaction temperature is 300 ℃. The fixed bed reactor 4 is internally provided with a FZC-302 type catalyst, and the space velocity is controlled to be 3.0h-1. The sulfur content in the raw material kerosene was 220ppm, which was reduced to 50ppm after the hydrodesulfurization reaction.
It will be appreciated that the present invention is applicable to the catalyst systems already mentioned, as well as to other hydrogenation catalyst systems not mentioned. The operation temperature is properly adjusted according to the activation temperature of the catalyst when different catalysts are used, without affecting the outstanding advantages of the reactor of the invention that the operation pressure can be greatly (or doubly) reduced and the space velocity (handling capacity) can be increased under different catalyst systems.
In addition, the micro-interface generator can be used in other multi-phase reaction technical fields to form multi-phase fluids formed by micron-scale particles such as gas-liquid-solid micro-mixed flow, gas-liquid-solid micro-nano flow, gas-liquid-solid emulsified flow, gas-liquid-solid micro-structured flow, multi-phase micro-mixed flow, multi-phase micro-nano flow, multi-phase emulsified flow, multi-phase micro-structured flow, micro-bubble, micro-gas flow, gas-liquid micro-nano emulsified flow, super micro-flow, super-micro-fluidization, micro-dispersed flow, micro-turbulence, micro-bubble flow, micro-nano bubble flow and the like, or multi-phase fluids formed by micro-nano-scale particles (micro-interface fluids for short), and can also be applied to reactions such as micro-bubble mass transfer, micro-bubble reaction, micro-bubble absorption, micro-bubble oxygenation, micro-bubble contact type, micro-mixing, micro-bubble, thereby effectively increasing the mass transfer area of the phase boundary between the gas phase and/or liquid phase and the liquid phase and/or solid phase in the reaction process.
Obviously, the fixed bed hydrogenation micro-interface reaction system provided by the invention has the beneficial effects that the micro-interface generator is added in the fixed bed reaction system, hydrogen is crushed into gas with the diameter of 1 mu m or more and d less than 1mm, a micro-bubble system is formed, micro-bubbles have the advantages of rigidity, good independence, difficult coalescence and the like, so that in the gas-liquid reaction process, the gas-liquid reaction is enhanced, the mass transfer efficiency is improved, and therefore, the emulsion containing a large number of micro-bubbles is obtained, and a higher phase interface area is formed in the reactor. Furthermore, the fixed bed hydrogenation micro-interface reaction system has the advantages of high gas utilization rate, high desulfurization rate, less investment, low energy consumption, flexible process and the like in engineering by providing the micro-interface generator.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A fixed bed hydrogenation micro-interface reaction system is characterized by comprising: the system comprises a fixed bed reactor, a micro-interface generator and a gas-liquid separation tank; the micro-interface generator is connected with the fixed bed reactor, the pressure energy of hydrogen and/or the kinetic energy of liquid in the reaction process are converted into the surface energy of hydrogen bubbles in the hydrogenation reaction process, the hydrogen bubbles are crushed into micro-bubbles, the micro-bubbles and the liquid are mixed to form a gas-liquid emulsion, and the gas-liquid emulsion enters the fixed bed reactor to perform subsequent reaction; the fixed bed reactor is used as a reaction site of hydrogenation reaction to form a stable gas-liquid reinforced fixed bed reaction system when the gas-liquid emulsion enters the fixed bed reactor; the gas-liquid separation tank is connected with the fixed bed reactor and is used for carrying out gas-liquid separation on the mixture after the reaction in the fixed bed reactor.
2. The fixed bed hydrogenation micro-interface reaction system of claim 1, wherein the micro-interface generator is selected from one or more of a pneumatic micro-interface generator, a hydraulic micro-interface generator and a gas-liquid linkage micro-interface generator.
3. The fixed bed hydrogenation micro-interfacial reaction system of claim 1, wherein the micro-interfacial generator is disposed in an upper portion of the fixed bed reactor.
4. The fixed bed hydrogenation micro-interfacial reaction system of claim 1, wherein the micro-interfacial generator is disposed in a lower portion of the fixed bed reactor.
5. The fixed bed hydrogenation micro-interfacial reaction system of claim 1, wherein the fixed bed reactor comprises: a reaction tank and a catalyst bed layer; the reaction tank is a tank body and is used for providing a reaction space for the gas-liquid emulsion, and a mixture outlet used for outputting the reacted mixture is formed in the reaction tank; the catalyst bed is fixed inside the reaction tank, and a catalyst for improving the reaction efficiency of the gas-liquid emulsion is arranged in the catalyst bed.
6. The fixed bed hydrogenation micro-interfacial reaction system of claim 1, further comprising: the device comprises a raw material tank, a power mechanism and a feeding preheater; the raw material tank is connected with the power mechanism and used for storing hydrogen and reaction liquid; the other end of the power mechanism is connected with the feeding preheater and used for providing power for conveying hydrogen and reaction liquid; the other end of the feed preheater is connected with the micro-interface reactor and is used for preheating the hydrogen and the reaction liquid so as to enable the hydrogen and the reaction liquid to reach the specified temperature.
7. The fixed bed hydrogenation micro-interface reaction system of claim 6, wherein the feed tank comprises a liquid feed tank and a gas feed surge tank; wherein the liquid raw material tank is connected with the feeding pump and used for storing the liquid raw material; the gas raw material buffer tank is connected with the compressor and used for storing hydrogen.
8. The fixed bed hydrogenation micro-interface reaction system as claimed in claim 6, wherein the power mechanism comprises: a feed pump and compressor; wherein the feed pump is connected with the liquid feed preheater and used for providing power for conveying liquid raw materials; the compressor is connected with the gas feed preheater and is used for providing power for conveying hydrogen.
9. The fixed bed hydrogenation micro-interfacial reaction system of claim 6, wherein the feed preheater comprises: a liquid feed preheater and a gas feed preheater; the liquid feed preheater is connected with the micro-interface generator and is used for preheating the liquid raw material to a specified temperature and sending the liquid raw material into the micro-interface generator; the gas feed preheater is connected to the micro-interface generator for preheating the hydrogen gas to a specified temperature and feeding it into the micro-interface generator.
10. The fixed bed hydrogenation micro-interface reaction system as claimed in claim 3, wherein the highest of the connecting pipes of the fixed bed reactor is higher than the fixed bed reactor.
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| CN201910196653.4A CN111686648A (en) | 2019-03-15 | 2019-03-15 | Fixed bed hydrogenation micro-interface reaction system |
| PCT/CN2019/090330 WO2020186643A1 (en) | 2019-03-15 | 2019-06-06 | Fixed-bed hydrogenation micro-interface reaction system |
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