CN105233765A - High-air speed selectively-catalytic unit and method used in hypergravity field - Google Patents
High-air speed selectively-catalytic unit and method used in hypergravity field Download PDFInfo
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Abstract
The invention belongs to the technical field of catalytic reactions and provides a high-air speed selectively-catalytic unit and method used in a hypergravity field to overcome the technical problem of difficulty in industrial realization of high-air speed gas-catalytic reactions in a hypergravity field in the prior art. The unit comprises a shell equipped with gas circulation ports, a liquid inlet and a liquid outlet; a catalyst filling device is arranged in the shell; the upper end of the catalyst filling device is connected with a rotating shaft of a motor; the center of the bottom of the shell is provided with the liquid inlet; one side of the bottom is provided with the liquid outlet; the gas circulation ports are respectively arranged on the upper and lower ends of the shell and located at two sides of the liquid inlet; and the catalyst filling device is a concentric cylinder, four surfaces of the catalyst filling device are porous planar mediums, a plurality of small holes are arranged, and porous planes are loaded with a catalyst. The invention has the following beneficial effects: in the catalytic process, gas flux is great, pressure drop is small, and energy consumption is low; a gas phase and a liquid phase stay for a short period of time, only few by-products are produced, and the number of target products per unit time is large; and the apparatus has a small size, the usage amount of the catalyst is decreased, and cost is reduced.
Description
Technical field
The invention belongs to catalytic reaction technical field, be specifically related to a kind of super gravity field high and medium speed selective catalysis apparatus and method, the catalytic process in the fields such as petrochemical industry, Coal Chemical Industry, pharmacy, environmental protection can be widely used in.
Background technology
Catalysis in petrochemical industry, Coal Chemical Industry, pharmacy, the fields such as environmental protection there is critical role.All there is the problem of interior diffusion in nearly all catalytic process, as the diffusion between reaction mass, the diffusion between reaction mass and catalyst, the diffusion between product and catalyst.Because mass transfer effect is poor, the following shortcoming of catalytic reaction ubiquity in gravitational field: 1, catalyst amount is large, and catalyst use efficiency is low; 2, mass transfer is slow; 3, the time of staying of material is long, and accessory substance is many; 4, energy consumption is large; 5, catalyst reaction equipment volume is large.In order to address these problems, patent (CN:1507940A, CN:1895766A) is applied to catalytic reaction process high-gravity technology, achieves good effect.
As everyone knows, industrially the solution-air biphasic catalysis reaction of high-speed accounts for significant proportion, if do not reach catalyst requirement air speed in course of reaction, byproduct of reaction increases, and the accumulated heat often produced causes catalysqt deactivation.This is because there is catalytic reaction in catalyst active center after this type of reaction solution-air contact, release certain heat, if remove heat not in time, side reaction increases simultaneously, selective reduction, and gas also must speed leave, no person's reaction depth is deepened, and accessory substance also can increase.In addition, for the ease of Facility Layout, increase gas speed often through reduction reactor body sum and reach air speed requirement, the time of staying shortens in the reactor to cause gas, have impact on the mass transport process between solution-air, the target product of unit interval also can reduce, and the more important thing is and liquid flooding may occur, and reaction cannot be carried out.But, disclosed process patent (CN:1507940A at present, CN:1895766A) solution-air with adverse current or and the form of stream contact catalytic reaction, be applicable to the solution-air biphasic catalysis reaction under low-speed, be not suitable for solution-air biphasic catalysis under high-speed and react.
This is mainly: when solution-air contacts with countercurrent flow, then operating process generation liquid flooding when gas space velocity is higher, and reaction heat can not remove in time, and reaction depth is deepened, and side reaction increases, selective variation.In engineering practice, in order to avoid liquid flooding, often need augmenting response body to amass to reduce gas speed, but this cause again and is difficult to reach catalysis instructions for use air speed, causes accessory substance to increase equally.In addition, the contact drop of countercurrent flow is excessive, in order to ensure to react requirement to gas space velocity, generally needs to add high-power air compressor machine, causes the uneconomical and factory's operating cost of operating cost to increase.And and streamed pressure drop and cross-current configuration pressure drop difference are little, but and the mass transfer force of stream is lower slightly.When air speed is larger, gas effciency is low causes the target product conversion ratio in the unit interval to reduce.
Summary of the invention
In order to solve the industrial high-speed solution-air catalytic reaction being difficult to realize in super gravity field at present, there is technical barrier in the present invention, proposes a kind of super gravity field high and medium speed selective catalysis apparatus and method.Solve the technical barrier that existing hypergravity catalysis technique is not suitable for high-speed solution-air catalytic reaction.
The present invention is realized by following technical scheme: a kind of super gravity field high and medium speed selective catalysis device, structure comprises the housing being provided with gas flow port and liquid entrance, Catalyst packing device is established in housing, Catalyst packing device upper end is connected with the rotating shaft of motor, liquid-inlet is established at housing bottom center, liquid outlet is established in side, bottom, housing upper and lower side and be positioned at liquid-inlet both sides and offer gas flow port respectively; Catalyst packing device is the concentric circles ring body be made up of porous flat plate, and the porous media that load has catalyst is filled in filling device inside.
Described concentric circles ring body is made up of four porous flat plates, and hole size is 10-800 order, described porous media granular size 20-150 order, and porous media filling porosity is 0.60-0.95, the outside diameter d of concentric circles ring body lower planes
2than internal diameter d
1ratio range 2-6, height h and outside diameter d
2ratio range 3-10.
The material of described porous flat plate is stainless steel or engineering plastics; Multi hole surface medium is active carbon, alundum (Al2O3) or kaolin.Be preferably active carbon.
Utilize the catalysis process of above-mentioned super gravity field high and medium speed selective catalysis device, comprise the steps: that reacting gas enters from gas flow port, catalyst layer is entered again from the upper multi hole surface of Catalyst packing device or lower multi hole surface, then from lower multi hole surface or the outflow of upper multi hole surface of Catalyst packing device, reacted gas flows out from gas vent; Liquid enters from liquid-inlet, spurts into the inner ring multi hole surface of Catalyst packing device, inflow catalyst layer, then flows out from the outer shroud multi hole surface of Catalyst packing device; The mixing that solution-air two-phase is strong in the catalyst layer of High Rotation Speed, mass transfer and reaction are carried out in turbulence; Reacted liquid flows out from liquid outlet.
The gas space velocity scope of described catalytic reaction is 10000-20000h
-1, liquid space velocity range is 200-300h
-1, catalytic reaction temperature 0-1000 DEG C, pressure is 0-10MPa, and Catalyst packing device rotary speed is 100-2000r/min.
The present invention has following features: solution-air two-phase of the present invention has contacted catalytic process with cross-current configuration in filler device.The top and bottom of the filling device of catalyst all have gas flow port, and gas is entered from the upper multi hole surface of filling device, and lower multi hole surface flows out, or enters from the lower multi hole surface of filling device, and upper multi hole surface flows out.Liquid enters from the inner ring multi hole surface of packed catalyst device, in super gravity field, be torn into rapidly drop, brin and liquid film, increases solution-air contact area.Gas enters in liquid by quality transmission, then completes catalytic reaction in the activated centre of catalyst after entering from upper porous area or lower porous area, and final gas flows out from lower multi hole surface or upper multi hole surface.Solution-air contacts with cross-current configuration, not easily liquid flooding is there is under high-speed, reaction depth can be controlled by the change of rotating speed, the raising of rotating speed, the time of staying of liquid phase reduces, and drop, brin and liquid film that liquid is torn in super gravity field are less, reduce heat and transmit resistance, reaction heat can shift out in time; This process gas channel cross-section does not change, and not reversely with liquid contacts, and pressure drop is less, and operating cost is low; Catalytic reaction process, mass-transfer efficiency is high, and total conversion is better than conventional catalyst equipment and existing overweight catalytic unit.
Disclosed prior art patent (CN:1507940A, CN:1895766A) reverse-flow and parallel type hypergravity catalysis rule is different from this process, the lower planes of its filling device is non-porous plane, and solution-air two-phase flows into from multi hole surface inside and outside filling device or flows out.Reverse-flow hypergravity catalysis method, its gas enters from the outer shroud multi hole surface of filling device, inner ring multi hole surface flows out, solution-air two-phase reverse movement, although mass transfer force is slightly larger than this method, easily liquid flooding occurs, operation is difficult to control, and because reverse movement causes pressure drop excessive, the solution-air catalytic process of large air speed cannot be applied to.In addition, parallel type hypergravity catalysis method, gas flows into from the inner ring multi hole surface of filling device together with liquid, and outer shroud multi hole surface flows out.The method experiment shows that pressure drop is little, but solution-air is that gas mass transfer force in a liquid weakens, and reduces the mass-transfer efficiency between solution-air with the form also flowed contact.When air speed is larger, cause gas effciency low, do not give play to the advantage of hypergravity catalysis technique completely.
Compared with prior art, the invention has the beneficial effects as follows: in catalytic process, gas flux is large, and pressure drop is little, and energy consumption is low; Gas phase, the liquid phase time of staying are short, and accessory substance is few, and unit interval target product is many; Equipment volume is little, and catalyst amount reduces, and cost reduces.
Accompanying drawing explanation
fig. 1for super gravity field high and medium speed selective catalysis apparatus structure of the present invention signal
figure;
fig. 2for the signal of Catalyst packing apparatus structure
figure;
fig. 3for Catalyst packing apparatus structure is faced
figure;
fig. 4for Catalyst packing apparatus structure is overlooked
figure.
in figure: 1-housing; 2-motor; 3-gas feed; 4-liquid-inlet; 5-liquid outlet; 6-gas vent; 7-Catalyst packing device; Multi hole surface under 7.1-; 7.2-outer shroud multi hole surface; The upper multi hole surface of 7.3-; 7.4-inner ring multi hole surface; H-donut height; The internal diameter of d1-concentric circles ring body lower planes; The external diameter of d2-concentric circles ring body lower planes.
Detailed description of the invention
Below in conjunction with
accompanying drawingdescribe the present invention in detail, enter with gas from lower multi hole surface, upper multi hole surface flows out for example describes in detail.
as Fig. 1,2shown in, a kind of super gravity field high and medium speed selective catalysis device, structure comprises the housing 1 being provided with gas flow port and liquid entrance, Catalyst packing device 7 is established in housing, Catalyst packing device 7 upper end is connected with the rotating shaft of motor 2, liquid-inlet 4 is established at housing bottom center, and liquid outlet 5 is established in side, bottom, housing upper and lower side and be positioned at liquid-inlet 4 both sides and offer gas flow port respectively; Catalyst packing device 7 is the concentric circles ring body be made up of porous flat plate, and the porous media that load has catalyst is filled in filling device inside.
Described concentric circles ring body is made up of four porous flat plates, and hole size is 10-800 order, described porous media granular size 20-150 order, and porous media filling porosity is 0.60-0.95, the outside diameter d of concentric circles ring body lower planes
2than internal diameter d
1ratio range 2-6, height h and outside diameter d
2ratio range 3-10.The material of porous flat plate is stainless steel or engineering plastics; Multi hole surface medium is active carbon, alundum (Al2O3) or kaolin.
Detailed process is: reacting gas enters from gas feed 3, then enters catalyst layer from the lower multi hole surface 7.1 of Catalyst packing device 7, and then flow out from the upper multi hole surface 7.3 of Catalyst packing device 7, reacted gas flows out from gas vent 6; Liquid enters from liquid-inlet 4, spurts into the inner ring multi hole surface 7.4 of Catalyst packing device 7, inflow catalyst layer, then flows out from the outer shroud multi hole surface 7.2 of Catalyst packing device 7; The mixing that solution-air two-phase is strong in the catalyst layer of High Rotation Speed, mass transfer and reaction are carried out in turbulence; Reacted liquid flows out from liquid outlet 5.
Embodiment 1
Adopt method of the present invention to carry out sorbierite catalytic hydrogenation and prepare biogasoline (C
5above alkane).The hole size at Catalyst packing device four sides is 800 orders, and the catalyst loaded in device is supported Pt catalysts, and load capacity is 0.7%, and its carrier is active carbon, filling porosity 0.6, porous media granular size 20 order.The outside diameter d of concentric circles ring body lower planes
2than internal diameter d
1ratio range 2, height h and outside diameter d
2ratio range 10, sorbitol solution enters from liquid-inlet 4, and air speed is 200h
-1, hydrogen enters from gas feed 3, and air speed is 10000h
-1; Operating pressure is 10MPa, and temperature is 1000 DEG C, and rotating speed is 2000r/min.Run after 3h hour, the distribution of record product and conversion ratio record.Adopt the disclosed catalysis process of patent (CN:1507940A, CN:1895766A), complete this catalytic process under identical operating conditions, product distribution and conversion ratio record
as table 1, pressure drop contrast is shown in
table 2, found that total conversion of the present invention is better than openly method, main because reverse-flow hypergravity catalysis process, gas-liquid contact time is long, catalysis depth down, C
5above alkane conversion reduces; And mass-transfer efficiency is lower between parallel type gravity Method solution-air, hydrogen mass-transfer efficiency, lower than the inventive method, causes total conversion to reduce.In addition, the inventive method gas-phase pressure drop is all less than openly method, by measuring, obtains the C of same output
5alkane, kinetic energy consumption than counter-current catalytic method reduce about 45%, than and flow catalysis method reduce 34%.
table 1:
table 2:
| Equipment | The inventive method | Reverse-flow hypergravity catalysis | Parallel type gravity Method |
| Pressure drop | 200 Pa | 1500 Pa | 800 Pa |
Embodiment 2
Adopt the present invention to carry out benzene selective catalytic hydrogenation and prepare cyclohexane, the hole size at Catalyst packing device four sides is 10 orders, and the catalyst loaded in device is the commercial ruthenium series hydrocatalyst of support type, and its carrier is active carbon, filling porosity 0.95, porous media granular size 150 order.The outside diameter d of concentric circles ring body lower planes
2than internal diameter d
1ratio range 6, height h and outside diameter d
2ratio range 3.Benzole soln enters from liquid-inlet 4, and air speed is 300h
-1, hydrogen enters from gas feed 3, and air speed is 20000h
-1, operating pressure is 0MPa, and temperature is 0 DEG C, and rotating speed is 100r/min.Run after 3h hour, the distribution of record product and conversion ratio record.Adopt the disclosed catalysis process of patent (CN:1507940A, CN:1895766A), complete this catalytic process under identical operating conditions, product distribution and conversion ratio record
as table 3, pressure drop contrast is shown in
table 4.
table 3
table 4
| Equipment | The inventive method | Reverse-flow hypergravity catalysis | Parallel type gravity Method |
| Pressure drop | 1500 Pa | 6500 Pa | 3500 Pa |
Result shows: total conversion of the present invention is better than openly method, and main because reverse-flow hypergravity catalysis process, liquid flooding occurs with this understanding, reaction heat cannot shift out, and side reaction increases, and conversion ratio reduces; And mass-transfer efficiency is lower between parallel type gravity Method solution-air, hydrogen mass-transfer efficiency, lower than the inventive method, causes total rate to reduce.In addition, the inventive method gas-phase pressure drop is all less than openly method, by measuring, obtains the cyclohexane of same output, and kinetic energy consumption reduces about 65% than counter-current catalytic method, than and flow catalysis method and reduce 45%.
Embodiment 3
Adopt the present invention to carry out benzene selective catalytic hydrogenation and prepare cyclohexane, the hole size at Catalyst packing device four sides is 500 orders; The catalyst loaded in device is the commercial ruthenium series hydrocatalyst of support type, and its carrier is active carbon, filling porosity 0.8, porous media granular size 80 order, porous media granular size 120 order.The outside diameter d of concentric circles ring body lower planes
2than internal diameter d
1ratio range 4, height h and outside diameter d
2ratio range 8.Benzole soln enters from liquid-inlet 4, and air speed is 250h
-1, hydrogen enters from gas feed 3, and air speed is 15000h
-1, operating pressure is 5MPa, and temperature is 300 DEG C, and rotating speed is 800r/min.Run after 3h hour, the distribution of record product and conversion ratio record.
Adopt the disclosed catalysis process of patent (CN:1507940A, CN:1895766A), complete this catalytic process under identical operating conditions, product distribution and conversion ratio record
as table 5, pressure drop contrast is shown in
table 6, found that total conversion of the present invention is better than openly method, main because reverse-flow hypergravity catalysis process, liquid flooding occurs with this understanding, reaction heat cannot shift out, and side reaction increases, and conversion ratio reduces; And mass-transfer efficiency is lower between parallel type gravity Method solution-air, hydrogen mass-transfer efficiency, lower than the inventive method, causes total rate to reduce.In addition, the inventive method gas-phase pressure drop is all less than openly method, by measuring, obtains the cyclohexane of same output, and kinetic energy consumption reduces about 52% than counter-current catalytic method, than and flow catalysis method and reduce 35%.
table 5
table 6:
| Equipment | The inventive method | Reverse-flow hypergravity catalysis | Parallel type gravity Method |
| Pressure drop | 1200 Pa | 7100 Pa | 3200 Pa |
Embodiment 4
Adopt the present invention to carry out benzene selective catalytic hydrogenation and prepare cyclohexane, the hole size at Catalyst packing device four sides is 600 orders; The catalyst loaded in device is the commercial ruthenium series hydrocatalyst of support type, and its carrier is active carbon, filling porosity 0.85, porous media granular size 50 order.The outside diameter d of concentric circles ring body lower planes
2than internal diameter d
1ratio range 3, height h and outside diameter d
2ratio range 10.Benzole soln enters from liquid-inlet 4, and air speed is 280h
-1, hydrogen enters from gas feed 3, and air speed is 11000h
-1; Operating pressure is 4MPa, and temperature is 200 DEG C, and rotating speed is 1500r/min.Run after 3h hour, the distribution of record product and conversion ratio record.
Adopt the disclosed catalysis process of patent (CN:1507940A, CN:1895766A), complete this catalytic process under identical operating conditions, product distribution and conversion ratio record
as table 7, pressure drop contrast is shown in
table 8, found that total conversion of the present invention is better than openly method, main because reverse-flow hypergravity catalysis process, liquid flooding occurs with this understanding, reaction heat cannot shift out, and side reaction increases, and conversion ratio reduces; And mass-transfer efficiency is lower between parallel type gravity Method solution-air, hydrogen mass-transfer efficiency, lower than the inventive method, causes total rate to reduce.In addition, the inventive method gas-phase pressure drop is all less than openly method, by measuring, obtains the cyclohexane of same output, and kinetic energy consumption reduces about 55% than counter-current catalytic method, than and flow catalysis method and reduce 35%.。
table 7
table 8
| Equipment | The inventive method | Reverse-flow hypergravity catalysis | Parallel type gravity Method |
| Pressure drop | 1050 Pa | 6800 Pa | 3100 Pa |
Embodiment 5:
Adopt the present invention to carry out benzene selective catalytic hydrogenation and prepare cyclohexane, the hole size at Catalyst packing device four sides is 500 orders, and the catalyst loaded in device is the commercial ruthenium series hydrocatalyst of support type, and its carrier is alundum (Al2O3), filling porosity 0.8, porous media granular size 30 order.The outside diameter d of concentric circles ring body lower planes
2than internal diameter d
1ratio range 6, height h and outside diameter d
2ratio range 10; Benzole soln enters from liquid-inlet 4, and air speed is 250h
-1, hydrogen enters from gas feed 3, and air speed is 15000h
-1; Operating pressure is 5MPa, and temperature is 300 DEG C, and rotating speed is 800r/min.Run after 3h hour, the distribution of record product and conversion ratio record.Acquired results is identical with embodiment 3 measured result.
Embodiment 6: adopt the present invention to carry out benzene selective catalytic hydrogenation and prepare cyclohexane, the hole size at Catalyst packing device four sides is 600 orders; The catalyst loaded in device is the commercial ruthenium series hydrocatalyst of support type, and its carrier is kaolin, filling porosity 0.85, porous media granular size 65 order.The outside diameter d of concentric circles ring body lower planes
2than internal diameter d
1ratio range 2, height h and outside diameter d
2ratio range 5; Benzole soln enters from liquid-inlet 4, and air speed is 280h
-1, hydrogen enters from gas feed 3, and air speed is 11000h
-1; Operating pressure is 4MPa, and temperature is 200 DEG C, and rotating speed is 1500r/min.Run after 3h hour, the distribution of record product and conversion ratio record.Acquired results is with embodiment 4 acquired results.
Claims (6)
1. a super gravity field high and medium speed selective catalysis device, structure comprises the housing (1) being provided with gas flow port and liquid entrance, Catalyst packing device (7) is established in housing, Catalyst packing device (7) upper end is connected with the rotating shaft of motor (2), it is characterized in that: liquid-inlet (4) is established at housing bottom center, liquid outlet (5) is established in side, bottom, housing upper and lower side and be positioned at liquid-inlet (4) both sides and offer gas flow port respectively; Catalyst packing device (7) is the concentric circles ring body be made up of porous flat plate, and the porous media that load has catalyst is filled in filling device inside.
2. a kind of super gravity field high and medium speed selective catalysis device according to claim 1, it is characterized in that: described concentric circles ring body is made up of four porous flat plates, hole size is 10-800 order, described porous media granular size 20-150 order, porous media filling porosity is 0.60-0.95, the outside diameter d of concentric circles ring body lower planes
2than internal diameter d
1ratio range 2-6, height h and outside diameter d
2ratio range 3-10.
3. a kind of super gravity field high and medium speed selective catalysis device according to claim 2, is characterized in that: the material of described porous flat plate is stainless steel or engineering plastics; Multi hole surface medium is active carbon, alundum (Al2O3) or kaolin.
4. a kind of super gravity field high and medium speed selective catalysis device according to claim 3, is characterized in that: described multi hole surface medium is active carbon.
5. one kind utilizes the catalysis process of the super gravity field high and medium speed selective catalysis device described in claim 1, it is characterized in that: comprise the steps: that reacting gas enters from gas flow port, catalyst layer is entered again from the upper multi hole surface (7.3) of Catalyst packing device (7) or lower multi hole surface (7.1), then from lower multi hole surface (7.1) or upper multi hole surface (7.3) outflow of Catalyst packing device (7), reacted gas flows out from gas vent (6); Liquid enters from liquid-inlet (4), spurts into the inner ring multi hole surface (7.4) of Catalyst packing device (7), inflow catalyst layer, then flows out from the outer shroud multi hole surface (7.2) of Catalyst packing device (7); The mixing that solution-air two-phase is strong in the catalyst layer of High Rotation Speed, mass transfer and reaction are carried out in turbulence; Reacted liquid flows out from liquid outlet (5).
6. a kind of catalysis process utilizing super gravity field high and medium speed selective catalysis device according to claim 5, is characterized in that: the gas space velocity scope of described catalytic reaction is 10000-20000h
-1, liquid space velocity range is 200-300h
-1, catalytic reaction temperature 0-1000 DEG C, pressure is 0-10MPa, and Catalyst packing device rotary speed is 100-2000r/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114380430A (en) * | 2021-12-28 | 2022-04-22 | 中北大学 | Integrated reaction device and method for treating nitrobenzene wastewater by strengthening iron-carbon micro-electrolysis-ozone coupling |
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| CN1327945A (en) * | 2000-05-05 | 2001-12-26 | 法国石油公司 | Low Si/Al ratio EUO structure-like zeolite and its application as catalyst |
| CN101219330A (en) * | 2007-09-14 | 2008-07-16 | 东南大学 | Method and device for fixing CO2 in stack gas by solid castoff carbonatation |
| CN101250474A (en) * | 2008-04-08 | 2008-08-27 | 山西大学 | Method and device foraging white spirit |
| CN205055982U (en) * | 2015-09-23 | 2016-03-02 | 中北大学 | Overweight field of force crowning airspeed selectivity catalytic unit |
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|---|---|---|---|---|
| CN1327945A (en) * | 2000-05-05 | 2001-12-26 | 法国石油公司 | Low Si/Al ratio EUO structure-like zeolite and its application as catalyst |
| CN101219330A (en) * | 2007-09-14 | 2008-07-16 | 东南大学 | Method and device for fixing CO2 in stack gas by solid castoff carbonatation |
| CN101250474A (en) * | 2008-04-08 | 2008-08-27 | 山西大学 | Method and device foraging white spirit |
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