CN106955648A - Tubular reaction system for gas-solid-liquid three-phase highly exothermic reaction - Google Patents
Tubular reaction system for gas-solid-liquid three-phase highly exothermic reaction Download PDFInfo
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- CN106955648A CN106955648A CN201710369180.4A CN201710369180A CN106955648A CN 106955648 A CN106955648 A CN 106955648A CN 201710369180 A CN201710369180 A CN 201710369180A CN 106955648 A CN106955648 A CN 106955648A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 96
- 239000007788 liquid Substances 0.000 title claims abstract description 82
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 49
- 239000012530 fluid Substances 0.000 claims abstract description 31
- 238000001816 cooling Methods 0.000 claims abstract description 11
- 230000005540 biological transmission Effects 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 13
- 238000012856 packing Methods 0.000 claims description 13
- 230000003197 catalytic effect Effects 0.000 claims description 3
- 239000007789 gas Substances 0.000 abstract description 49
- 239000003054 catalyst Substances 0.000 abstract description 36
- 206010020843 Hyperthermia Diseases 0.000 abstract description 2
- 230000036031 hyperthermia Effects 0.000 abstract description 2
- 239000010410 layer Substances 0.000 description 19
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 14
- 239000012071 phase Substances 0.000 description 14
- 238000002474 experimental method Methods 0.000 description 10
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 9
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 9
- 229940043265 methyl isobutyl ketone Drugs 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 238000012546 transfer Methods 0.000 description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 5
- 238000004939 coking Methods 0.000 description 5
- 229910052739 hydrogen Inorganic materials 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 208000002925 dental caries Diseases 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- QIXDHVDGPXBRRD-UHFFFAOYSA-N 2,3,5-trimethylcyclohexa-2,5-diene-1,4-dione Chemical compound CC1=CC(=O)C(C)=C(C)C1=O QIXDHVDGPXBRRD-UHFFFAOYSA-N 0.000 description 2
- SHOJXDKTYKFBRD-UHFFFAOYSA-N 4-Methyl-3-penten-2-one, 9CI Chemical compound CC(C)=CC(C)=O SHOJXDKTYKFBRD-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 230000009849 deactivation Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000005984 hydrogenation reaction Methods 0.000 description 2
- 125000000654 isopropylidene group Chemical group C(C)(C)=* 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- AUFZRCJENRSRLY-UHFFFAOYSA-N 2,3,5-trimethylhydroquinone Chemical class CC1=CC(O)=C(C)C(C)=C1O AUFZRCJENRSRLY-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000004054 benzoquinones Chemical class 0.000 description 1
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 1
- 208000012839 conversion disease Diseases 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
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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
- B01J8/02—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
- B01J8/06—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 in tube reactors; the solid particles being arranged in tubes
-
- 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
- B01J8/02—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
-
- 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
- B01J8/02—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
- B01J8/0292—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 with stationary packing material in the bed, e.g. bricks, wire rings, baffles
-
- 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
- B01J8/02—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
- B01J8/06—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 in tube reactors; the solid particles being arranged in tubes
- B01J8/067—Heating or cooling the reactor
-
- 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
- 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
- B01J2208/00831—Stationary elements
-
- 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
- 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
- B01J2208/00831—Stationary elements
- B01J2208/0084—Stationary elements inside the bed, e.g. baffles
-
- 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
- B01J2208/00—Processes carried out in the presence of solid particles; Reactors therefor
- B01J2208/00796—Details of the reactor or of the particulate material
- B01J2208/00893—Feeding means for the reactants
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
Abstract
The invention discloses a kind of tubular reaction system for gas-solid-liquid three-phase highly exothermic reaction, including：Reactor, is divided into first, second and third cavity from top to bottom；Multiple fluid distributors, are arranged in the second cavity, are connected with the first cavity, including straight tube and distribution pipe, and distribution pipe includes necking section, aditus laryngis end and flared section；Multiple catalysis tubulations, positioned at the lower section of fluid distributor, are connected with the 3rd cavity；Liquid conducting pipes, gas transmission pipeline, convey liquids and gases into the first cavity respectively；The preheater preheated to liquid；The heat-conducting medium of cooling catalysis tubulation；The deflection plate of water conservancy diversion heat-conducting medium；The circulation heat exchanger of cooling heat transferring medium；The cooler cooled down to the product of reactor；The knockout drum connected with cooler.The tubular reaction system of the present invention can make gas-liquid mixed uniform, it is to avoid localized hyperthermia inside beds, improve the conversion ratio and selectivity of reaction, it is to avoid catalyst is burned.
Description
Technical field
It is espespecially a kind of to be used for gas-solid-liquid three-phase the present invention relates to the structure-design technique field of three-phase highly exothermic reaction equipment
The tubular reaction system of highly exothermic reaction.
Background technology
Gas-solid-liquid three-phase catalytic hydrogenation reaction, especially exothermic heat of reaction amount are big, and catalyst non-refractory or high temperature are volatile
The fixed-bed type phase reaction of (noble metal catalyst) living, the realization of industrialization of this kind of reaction is always the technological difficulties of industry.
Hot speed is slow due to moving for traditional fixed bed reactors, and bed temperature rise exceedes the tolerance range of catalyst and can not used；Tubulation
Formula reaction system can not solve the uniform problem between each tubulation after the uniform mixed aerosol of gas-liquid again.It can not only influence between gas-liquid
Mass transfer and heat transfer, can also cause reactant in the uneven distribution of catalyst bed interlayer, cause different gases between different beds
With the distribution of liquid air speed, partial material overreaction, partial material incomplete reaction, reaction yield is reduced, and is frequently present of bed
Layer catalyst hot-spot coking and deactivation burns.
Patent CN2430213Y describes a kind of liquid distribution trough of tubular reaction system, for each row to reactor
Pipe evenly distributing liquid, but the distributor can not realize that the atomization of gas-liquid is uniformly mixed, and the uneven mixing of gas-liquid still can not
Avoid catalyst coking and deactivation.
Therefore, the applicant is directed to providing a kind of new tubular reaction for gas-solid-liquid three-phase highly exothermic reaction
System.
The content of the invention
It is an object of the invention to provide a kind of tubular reaction system for gas-solid-liquid three-phase highly exothermic reaction, it can be with
Make gas and liquid well mixed, improve reaction rate, it is to avoid localized hyperthermia inside catalyst layer, cause catalyst to be burned.
In order to solve the above technical problems, the invention provides a kind of shell and tube for gas-solid-liquid three-phase highly exothermic reaction is anti-
System is answered, including：Reactor, the reactor is divided into the first cavity, the second cavity and the 3rd cavity from top to bottom；It is multiple
Fluid distributor, is arranged in second cavity, and its entrance is connected with first cavity, and the fluid distributor includes connecting
Logical straight tube and distribution pipe, the distribution pipe include necking section, aditus laryngis end and the flared section being sequentially communicated, the necking section and institute
State straight tube connection；Multiple catalysis tubulations, are arranged in second cavity, and are located at the lower section of the fluid distributor, and institute
State catalysis tubulation to correspond with the fluid distributor, the outlet of the catalysis tubulation is connected with the 3rd cavity；Liquid
Conveyance conduit, is connected with the first cavity of the reactor, for conveying liquid into first cavity；Air shooter
Road, is connected with the first cavity of the reactor, for conveying gas into first cavity；Preheater, is arranged on described
On liquid conducting pipes, for being preheated to liquid；Heat-conducting medium, is arranged in the second cavity of the reactor, and position
In the outside of the catalysis tubulation；Deflection plate, is arranged in the second cavity of the reactor, and outside the catalysis tubulation
Portion, for heat-conducting medium described in water conservancy diversion；Circulation heat exchanger, is arranged on outside the reactor, and it is imported and exported respectively at described the
Two cavitys are connected, for being cooled down to the heat transferring medium in second cavity；Cooler, with the reactor
The outlet connection of three cavitys, the material for the exit to the reactor carries out cooling treatment；Knockout drum, it is and described
Cooler is connected, for separating gas and liquid in the material after cooling.
Preferably, the liquid conducting pipes are connected with the top of the first cavity of the reactor, for making liquid certainly
Entered under above in first cavity；The gas transmission pipeline is connected with the bottom of the first cavity of the reactor,
For making gas enter from bottom to top in first cavity.
Preferably, the caliber of the straight tube is the 1/5~1/3 of the caliber of the catalysis tubulation；The trunnion of the distribution pipe
Caliber for the straight tube caliber 1/5~1/3；The expansion angle of the flared section of the distribution pipe is 6~15 °；Described point
The maximum caliber of the flared section of pipe arrangement is the 1/3~3/5 of the caliber of the catalysis tubulation.
Preferably, the length of the catalysis tubulation is 6~15m, and caliber is 20~30mm；Urged described in three of arbitrary neighborhood
It is in equilateral triangle arrangement to change tubulation, and the distance between the outer tube wall of the adjacent catalysis tubulation is 8~16mm；The catalysis row
The first packing layer, Catalytic Layer and the second packing layer are sequentially provided with from top to bottom in pipe, the height of first packing layer is 20~
100mm, the distance of outlet of the upper end away from the catalysis tubulation of first packing layer is 200~400mm, first filler
The distance of outlet of the upper end away from the fluid distributor of layer is 100~200mm.
Preferably, the deflection plate includes many sub- deflection plates, and many sub- deflection plates are in turn connected to form helicoidal structure,
The angle of the sub- deflection plate and horizontal plane is 25 °~45 °, the maximum spacing between the adjacent sub- deflection plate be 300~
600mm。
Preferably, the knockout drum is provided with first gas outlet and second gas outlet, and the first gas goes out
Mouth is connected with the gas transmission pipeline, and the second gas outlet is connected with external environment condition.
Preferably, in the catalysis tubulation, the volume space velocity scope of liquid is 1~5h-1, the volume space velocity scope of gas
For 200~800h-1。
Preferably, the flow velocity of the heat transferring medium is 0.7~1.5m/s.
The tubular reaction system for gas-solid-liquid three-phase highly exothermic reaction of the present invention can realize following at least one
Beneficial effect.
1st, liquid is entered in the first cavity of reactor by conveyance conduit respectively after gas and preheating, and the two is through excessively stream
Body distributor entered after full and uniform mixing to be reacted in catalyst tubulation, and reacted product enters through subcooler
Row cooling is handled, and the product after cooling carries out gas-liquid separation by knockout drum again, so that reaction is completed, in addition, in reaction
During, heat-conducting medium carries out cooling processing to the catalyst and reaction mass in catalysis tubulation, it is to avoid catalyst temperature mistake
High and burn out, the setting of fluid distributor can be such that gas and liquid is sufficiently mixed uniformly, so that in catalyst tubulation quickly
Haptoreaction, and product can be from the quick stripping on catalyst, it is to avoid overreaction, reduces catalyst coking.
2nd, the first cavity is entered from top to bottom by making gas, liquid enters the second cavity from top to bottom, so that
Gas and liquid are tentatively mixed in the first cavity, and mixed gas and liquid are carried out again by fluid distributor again
Mixing, further mixes gas and liquid and is more uniformly distributed.
3rd, by the way that deflection plate is set into helical baffles, helical baffles can produce certain to the flowing of heat-conducting medium
Disturbance, so as to effectively improve the thermal conductivity factor of heat-conducting medium, it is to avoid catalysis tubulation local temperature is too high, burns out catalyst.
Brief description of the drawings
The present invention is described in further detail with reference to the accompanying drawings and detailed description：
Fig. 1 is a kind of specific embodiment of the tubular reaction system for gas-solid-liquid three-phase highly exothermic reaction of the present invention
Structural representation；
Fig. 2 is the structural representation of the fluid distributor and catalysis tubulation shown in Fig. 1；
Fig. 3 is the arrangement schematic diagram of multiple catalysis tubulations shown in Fig. 1.
Drawing reference numeral explanation：
Reactor 1, fluid distributor 2, straight tube 21, distribution pipe 22 is catalyzed tubulation 3, liquid conducting pipes 4, gas conveying
Pipeline 5, preheater 6, deflection plate 7, circulation heat exchanger 8, cooler 9, knockout drum 10, first gas outlet 11, the second gas
Body outlet 12, liquid outlet 13.
Embodiment
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
The accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this
Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.
A kind of tubular reaction system for gas-solid-liquid three-phase highly exothermic reaction of the present embodiment, including：Reactor 1, instead
Device 1 is answered to be divided into the first cavity, the second cavity and the 3rd cavity from top to bottom；Multiple fluid distributors 2, are arranged on the second chamber
In body, its entrance is connected with the first cavity, and fluid distributor 2 includes the straight tube 21 and distribution pipe 22 of connection, and distribution pipe 22 includes
Necking section, aditus laryngis end and the flared section being sequentially communicated, necking section are connected with the straight tube 21；Multiple catalysis tubulations 3, are arranged on the
In two cavitys, and it is located at the lower section of fluid distributor 2, and catalysis tubulation 3 is corresponded with fluid distributor 2, catalysis tubulation 3
Outlet is connected with the 3rd cavity；Liquid conducting pipes 4, are connected with the first cavity of reactor 1, for being conveyed into the first cavity
Liquid；Gas transmission pipeline 5, is connected with the first cavity of reactor 1, for conveying gas into the first cavity.Specifically, gas
Body conveyance conduit 5 is passed into the first cavity again after first being connected outside reactor 1 with liquid conducting pipes 4.
Tubular reaction system in the present embodiment also includes：Preheater 6, is arranged on liquid conducting pipes 4, for pair
Liquid is preheated；Heat-conducting medium, is arranged in the second cavity of reactor 1, and positioned at the outside of catalysis tubulation 3；Deflection plate
7, it is arranged in the second cavity of reactor 1, and outside catalysis tubulation 3, for water conservancy diversion heat-conducting medium；Circulation heat exchanger 8,
It is arranged on outside reactor 1, it is imported and exported respectively at the connection of the second cavity, it is cold for being carried out to the heat transferring medium in the second cavity
But cool；Cooler 9, the outlet with the 3rd cavity of reactor 1 is connected, and the material for the exit to reactor 1 is carried out
Cooling treatment；Knockout drum 10, is connected with cooler 9, for separating gas and liquid in the material after cooling.
As shown in Fig. 2 the caliber D2 of straight tube 21 be catalyzed tubulation 3 caliber D1 1/5~1/3, for example, 1/5,4/15,
1/3；The caliber D3 of the trunnion of distribution pipe 22 is the 1/5~1/3 of the caliber D2 of straight tube 21, for example, 1/5,4/15,1/3；Distribution pipe
The expansion angle α of 22 flared section is 6~15 °, for example, 7 °, 8 °, 11 °, 12 °, 14 °；The largest tube of the flared section of distribution pipe 22
Footpath is the 1/3~3/5 of the caliber D1 of catalysis tubulation 3, for example, 1/3,2/5,7/15,8/15.
Specifically, catalysis tubulation 3 length L be 6~15m, for example, 7m, 8m, 10m, 12m, 13m, 14m, by repeatedly examination
Test and show, if the length of catalysis tubulation 3 is too small, residence time of the material in tubulation is short, and reaction conversion ratio is low, if length is too
Long, then not only pressure difference is big, and residence time of material is oversize, easily causes catalyst coking.
Specifically, catalysis tubulation 3 caliber D1 be 20~30mm, for example, 22mm, 23mm, 25mm, 26mm, 28mm,
29mm, the caliber of catalysis tubulation 3 needs the catalyst particle size more than 15 times, shows by test of many times, if the catalysis diameter of tubulation 3
Too small, the boundary effect of catalyst is big, is unfavorable for material being uniformly distributed in catalyst surface, if the catalysis diameter of tubulation 3 is too big,
It is unfavorable for the timely removal of reaction heat.
As shown in figure 3, three catalysis tubulations 3 of arbitrary neighborhood are in equilateral triangle arrangement, and the outer tube of adjacent catalyst tubulation 3
The distance between wall is 8~16mm, for example, 9mm, 11mm, 12mm, 14mm, 15mm, show by test of many times, if this spacing
Too small, then the resistance between heat-conducting medium and catalysis tubulation 3 is too big, if spacing is too big, the viscous layer fluid of tubulation outer wall can not
Quick flowing, pipe external thermal resistance becomes big, heat transfer coefficient reduction, and the reaction heat in catalysis tubulation 3 can not be distributed in time.
The first packing layer, Catalytic Layer and the second packing layer, first filler are sequentially provided with from top to bottom in catalysis tubulation 3
The height d2 of layer is 20~100mm, for example, 30mm, 40mm, 50mm, 60mm, 65mm, 70mm, 80mm, 85mm, 90mm, first
The upper end of packing layer away from catalysis tubulation 3 outlet apart from d1 be 200~400mm, for example, 230mm, 250mm, 270mm,
300mm, 350mm, 380mm, outlet of the upper end away from the fluid distributor 2 of the first packing layer apart from d3 be 100~
200mm, for example, 110mm, 130mm, 140mm, 150mm, 170mm, 180mm, 190mm.
Specifically, deflection plate 7 includes many sub- deflection plates 7, many sub- deflection plates 7 are in turn connected to form helicoidal structure,
The angle of sub- deflection plate 7 and horizontal plane is 25 °~45 °, for example, 27 °, 28 °, 30 °, 32 °, 33 °, 34 °, adjacent sub- deflection plate 7
Between maximum spacing be 300~600mm, for example, 400mm, 450mm, 480mm, 500mm, 530mm, 570mm, test of many times
Show, if the maximum spacing between sub- deflection plate 7 is too small, shell resistance is big, and maximum spacing is too big, then can reduce fluid to row
The shearing of tube outer surface viscous layer, reduces mass tranfer coefficient.
Specifically, knockout drum 10 is provided with first gas outlet 11 and second gas outlet 12, first gas outlet
11 are connected with gas transmission pipeline 5, and second gas outlet 12 is connected with external environment condition.
Specifically, in catalysis tubulation 3, the volume space velocity scope of liquid is 1~5h-1, for example, 1.6h-1、2.0h-1、
2.5h-1、3.0h-1、3.5h-1、4.0h-1、4.5h-1, the volume space velocity scope of gas is 200~800h-1, for example, 300h-1、
400h-1、500h-1、600h-1、700h-1, under this two-phase air speed, gas-liquid two-phase raw material can reach uniform quick with catalyst
Haptoreaction is adsorbed, and reactant can be from the quick stripping on catalyst, it is to avoid overreaction, reaction selectivity is improved,
Catalyst coking is reduced, heat transfer coefficient can also be improved, it is to avoid local overheating, burn out catalyst.Test of many times shows, if air speed
It is too low, it is unfavorable for heat and mass transfer, if air speed is too high, not only heat and mass transport is improved not substantially, and easily increase catalyst
Percentage of damage.
Specifically, the flow velocity of heat transferring medium be 0.7~1.5m/s, for example, 0.8m/s, 1.0m/s, 1.2m/s, 1.3m/s,
1.4m/s, test of many times shows that if the flow velocity is too low, heat transfer effect is poor, Ruo Taigao, then resistance is too big.
In addition, in other specific embodiments, liquid conducting pipes can also be with connecting at the top of the first cavity of reactor
Logical, for making liquid enter from top to bottom in the first cavity, the bottom of the first cavity of gas transmission pipeline and reactor connects
It is logical, for making gas enter from bottom to top in the first cavity.
The following is the tubular reaction system in existing tubular reaction system and the present embodiment in two kinds of highly exothermic reactions
The contrast test and its result of system.
The first reaction：Synthesizing methyl isobutyl ketone reacts
Following 3 steps reaction should occur altogether using acetone and hydrogen as Material synthesis methyl iso-butyl ketone (MIBK)：
The first step：Two molecule acetone are condensed under base catalyst effect, generate the diacetone alcohol of a molecule.
2CH3COCH3→(CH3)2COHCH2COCH3 (1)
Second step：Diacetone alcohol is dehydrated under acidic catalyst effect, generates isopropylidene acetone.
(CH3)2COHCH2COCH3→(CH3)2C=CHCOCH3+H2O (2)
3rd step：Isopropylidene acetone is hydrogenated with hydrogenation catalyst effect, generates MIBK.
(CH3)2C=CHCOCH3+H2→(CH3)2CHCH2COCH3 (3)
In the presence of resin type supported precious metal catalyst, above-mentioned three-step reaction can be successively in same catalyst bed
Completed in layer, the reaction heat about 1450KJ/Kg of logistics weight is converted into the reaction, thermal discharge is big, current tubulation reaction skill
Art is slow due to gas-liquid skewness and rate of heat transfer, causes bed gas-liquid air speed uneven, there is the bed temperature difference greatly, temperature control
System is difficult, causes product selectivity relatively low, the easy temperature runaway inactivation of beds.
1st, using conventional traditional tubular reaction system
Liquid is assigned in each tubulation internal catalyst bed layer with distributor pipe (including cavity plus straight length), gas raw material
Tube side cavity is then directly entered, it is 25% normal that conventional breach is installed in NATURAL DISTRIBUTION, housing in tubulation using bed pressure difference
Advise segmental baffle, baffle(s) spacing 400mm.
Reaction condition is：Reactor inlet temperature：90 DEG C, pressure：2.9MPa, liquid air speed：1.5h-1, gas space velocity：
300h-1。
Reaction result is：Reactor maximum temperature：150 DEG C, MIBK (methyl isobutyl ketone, water white transparency
Liquid) selectivity：94%, acetone conversion per pass：30%.
2nd, using the tubular reaction system of the present invention
Using the fluid distributor shown in the patent flow and Fig. 2 shown in Fig. 1, gas (hydrogen) is mixed with liquid (acetone)
Enter the fluid distribution cavity of reactor afterwards, by the atomizing effect of fluid distributor itself, fluid is fully atomized, uniform point
It is distributed in each tubulation bed.
The following is the condition and result of three experiments：
2.1. reaction condition is：Reactor inlet temperature：100 DEG C, pressure：2.9MPa, liquid air speed：1.5h-1, gas space
Speed：300h-1；
Reaction result is：Maximum temperature in reactor：130 DEG C, MIBK selectivity：95%, acetone conversion per pass：
35%.
2.2. reaction condition is：Reactor inlet temperature：95 DEG C, pressure：3.0MPa, liquid air speed：2.0h-1, gas space
Speed：400h-1。
Reaction result is：Maximum temperature in reactor：135 DEG C, MIBK selectivity：95%, acetone conversion per pass：
34%.
2.3. reaction condition is：Reactor inlet temperature：100 DEG C, pressure：3.0MPa, liquid air speed：2.4h-1, gas space
Speed：500h-1。
Reaction result is：Maximum temperature in reactor：130 DEG C, MIBK selectivity：95.1%, acetone conversion per pass：
33%.
Contrast the once experiment of traditional reactor and three experiments of reactor of the present invention are understood, on reactor inlet temperature
Degree, the once experiment of traditional reactor is less than three experiments of invention reactor, still, for maximum temperature in reactor,
Three times but more than reactor of the present invention once tested of traditional reactor are tested, it follows that traditional reactor is compared, this
The reactor of invention has good radiating effect, it is possible to prevente effectively from reactor temperature is too high, causes catalyst to burn mistake
It is living.
In addition, compared to traditional reactor, reactor of the invention by adjust pressure, gas space velocity, liquid air speed from
And effectively increase the selectivity of product and the conversion ratio of liquid phase substance.
Second of reaction：2,3,5- trimethylbenzoquinone hydrogenation synthesis 2,3,5- Trimethyl Hydroquinones
The reaction descriptions：In the presence of activated carbon supported noble metal catalyst, 2,3,5-trimethylbenzoquinoe reacts with hydrogen
TMHQ is synthesized, the reaction is strong exothermal reaction, the reaction heat for being converted into weight of material is 1100KJ/
Kg, at reaction conditions, benzoquinones are liquid phase, and hydrogen is gas phase, are reacted for gas-liquid-solid phase reaction, and due to the intensity of activated carbon
Problem, can only use bed technology.
1st, using conventional traditional tubular reaction system
Liquid is assigned in each tubulation internal catalyst bed layer with distributor pipe (including cavity plus straight length), gas raw material
Tube side cavity is then directly entered, it is 25% normal that conventional breach is installed in NATURAL DISTRIBUTION, housing in tubulation using bed pressure difference
Advise segmental baffle, baffle(s) spacing 400mm.
Reaction condition is：Reactor inlet temperature：80℃；Pressure：3.9MPa；Liquid air speed：2.0h-1, gas space velocity：
400h-1。
Reaction result is：Reactor maximum temperature：140℃；Product selectivity, 99.2%；Feed stock conversion：99.1%.
2nd, using the tubular reaction system of the present invention
Using the fluid distributor shown in the patent flow and Fig. 2 shown in Fig. 1, gas (hydrogen) and liquid (2,3,5- tri-
Methylbenzoquinone) mixing after enter reactor fluid distribution cavity, by the atomizing of fluid distributor, by the abundant mist of fluid
Change, be uniformly distributed in each tubulation bed.
The following is the condition and result of three experiments
2.1 reaction conditions are：Reactor inlet temperature：90 DEG C, pressure：3.9MPa, liquid air speed：2.0h-1, gas space
Speed：500h-1.
Reaction result is：Reactor maximum temperature：130 DEG C, product selectivity：99.5%, feed stock conversion：99.8%.
2.2 reaction conditions are：Reactor inlet temperature：90 DEG C, pressure：3.9MPa, liquid air speed：3.5h-1, gas space
Speed：800h-1。
Reaction result is：Reactor maximum temperature：130 DEG C, product selectivity：99.7%, feed stock conversion：99.6%.
Contrast the once experiment of traditional reactor and three experiments of reactor of the present invention are understood, on reactor inlet temperature
Degree, the once experiment of traditional reactor is less than three experiments of invention reactor, still, for maximum temperature in reactor,
Three times but more than reactor of the present invention once tested of traditional reactor are tested, it follows that traditional reactor is compared, this
The reactor of invention has good radiating effect, it is possible to prevente effectively from reactor temperature is too high, causes catalyst to burn mistake
It is living.
In addition, compared to traditional reactor, reactor of the invention by adjust pressure, gas space velocity, liquid air speed from
And effectively increase the selectivity of product and the conversion ratio of liquid phase substance.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (8)
1. a kind of tubular reaction system for gas-solid-liquid three-phase highly exothermic reaction, it is characterised in that including：Reactor, institute
State reactor and be divided into the first cavity, the second cavity and the 3rd cavity from top to bottom；Multiple fluid distributors, are arranged on described
In second cavity, its entrance is connected with first cavity, and the fluid distributor includes the straight tube and distribution pipe of connection, described
Distribution pipe includes necking section, aditus laryngis end and the flared section being sequentially communicated, and the necking section is connected with the straight tube；
Multiple catalysis tubulations, are arranged in second cavity, and are located at the lower section of the fluid distributor, and the catalysis row
Pipe is corresponded with the fluid distributor, and the outlet of the catalysis tubulation is connected with the 3rd cavity；
Liquid conducting pipes, are connected with the first cavity of the reactor, for conveying liquid into first cavity；
Gas transmission pipeline, is connected with the first cavity of the reactor, for conveying gas into first cavity；
Preheater, is arranged on the liquid conducting pipes, for being preheated to liquid；
Heat-conducting medium, is arranged in the second cavity of the reactor, and positioned at the outside of the catalysis tubulation；
Deflection plate, is arranged in the second cavity of the reactor, and outside the catalysis tubulation, for being led described in water conservancy diversion
Thermal medium；
Circulation heat exchanger, is arranged on outside the reactor, and it is imported and exported respectively at second cavity connection, for described
Heat transferring medium in second cavity is cooled down；
Cooler, the outlet with the 3rd cavity of the reactor is connected, and the material for the exit to the reactor enters
Row cooling treatment；
Knockout drum, is connected with the cooler, for separating gas and liquid in the material after cooling.
2. it is used for the tubular reaction system of gas-solid-liquid three-phase highly exothermic reaction as claimed in claim 1, it is characterised in that：
The liquid conducting pipes are connected with the top of the first cavity of the reactor, for making liquid enter from top to bottom
In first cavity；
The gas transmission pipeline is connected with the bottom of the first cavity of the reactor, for making gas enter from bottom to top
In first cavity.
3. it is used for the tubular reaction system of gas-solid-liquid three-phase highly exothermic reaction as claimed in claim 1, it is characterised in that：
The caliber of the straight tube is the 1/5~1/3 of the caliber of the catalysis tubulation；
The caliber of the trunnion of the distribution pipe is the 1/5~1/3 of the caliber of the straight tube；
The expansion angle of the flared section of the distribution pipe is 6~15 °；
The maximum caliber of the flared section of the distribution pipe is the 1/3~3/5 of the caliber of the catalysis tubulation.
4. it is used for the tubular reaction system of gas-solid-liquid three-phase highly exothermic reaction as claimed in claim 1, it is characterised in that：
The length of the catalysis tubulation is 6~15m, and caliber is 20~30mm；
Three catalysis tubulations of arbitrary neighborhood are between equilateral triangle arrangement, and the outer tube wall of the adjacent catalysis tubulation
Distance is 8~16mm；
The first packing layer, Catalytic Layer and the second packing layer are sequentially provided with the catalysis tubulation from top to bottom,
The height of first packing layer is 20~100mm, outlet of the upper end away from the catalysis tubulation of first packing layer
Distance be 200~400mm, the distance of outlet of the upper end away from the fluid distributor of first packing layer for 100~
200mm。
5. it is used for the tubular reaction system of gas-solid-liquid three-phase highly exothermic reaction as claimed in claim 1, it is characterised in that：
The deflection plate includes many sub- deflection plates, and many sub- deflection plates are in turn connected to form helicoidal structure,
The angle of the sub- deflection plate and horizontal plane is 25 °~45 °, and the maximum spacing between the adjacent sub- deflection plate is 300
~600mm.
6. it is used for the tubular reaction system of gas-solid-liquid three-phase highly exothermic reaction as claimed in claim 1, it is characterised in that：
The knockout drum is exported and the gas provided with first gas outlet and second gas outlet, the first gas
Conveyance conduit is connected, and the second gas outlet is connected with external environment condition.
7. it is used for the tubular reaction system of gas-solid-liquid three-phase highly exothermic reaction as claimed in claim 1, it is characterised in that：
In the catalysis tubulation, the volume space velocity scope of liquid is 1~5h-1, the volume space velocity scope of gas for 200~
800h-1。
8. it is used for the tubular reaction system of gas-solid-liquid three-phase highly exothermic reaction as claimed in claim 1, it is characterised in that：
The flow velocity of the heat transferring medium is 0.7~1.5m/s.
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| CN109364831A (en) * | 2018-12-19 | 2019-02-22 | 上海璨谊生物科技有限公司 | Gas-liquid catalytic reaction device and system |
| CN111545134A (en) * | 2020-06-16 | 2020-08-18 | 山东鲁新设计工程有限公司 | Tube reactor and process equipment for sorbitol production |
| CN111632571A (en) * | 2020-06-22 | 2020-09-08 | 上海戊正工程技术有限公司 | A kind of reaction equipment for preparing oxamide from oxalate |
| CN113828254A (en) * | 2021-11-29 | 2021-12-24 | 北京大臻科技有限公司 | Isothermal catalytic conversion equipment and method for para-hydrogen |
| CN113856569A (en) * | 2021-09-28 | 2021-12-31 | 联化新瑞(北京)科技有限公司 | Reactor for preparing succinic anhydride through maleic anhydride hydrogenation and control method thereof |
| CN113856568A (en) * | 2021-09-28 | 2021-12-31 | 联化新瑞(北京)科技有限公司 | Reactor for preparing 1, 3-propylene glycol by hydrogenating 3-hydroxypropionaldehyde and control method thereof |
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Application publication date: 20170718 |