CN102416307B - A kind of internal-circulation type paste state bed reactor and application thereof - Google Patents
A kind of internal-circulation type paste state bed reactor and application thereof Download PDFInfo
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- CN102416307B CN102416307B CN201110074590.9A CN201110074590A CN102416307B CN 102416307 B CN102416307 B CN 102416307B CN 201110074590 A CN201110074590 A CN 201110074590A CN 102416307 B CN102416307 B CN 102416307B
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Abstract
A kind of internal-circulation type paste state bed reactor and application thereof.In reactor shell, arrange 1 ~ 160 built-in cylindrical shell, the height of built-in cylindrical shell and the aspect ratio of reactor shell are 0.1 ~ 1.0, and the built-in cylindrical shell bottom of every root is provided with gas distributor.Slurries constantly circulate in reactor, without the need to slurry outside circulation, do not need outer circulation pump.In addition, built-in cylindrical shell adopts suitable quantity and diameter ratio, so there is not slurries short circuit problem and bed instability problem.Described paste state bed reactor is used for coal Direct Hydrogenation liquefaction process, oily coal faces hydrogen and is total in sweetening process or fischer-tropsch synthesis process.
Description
Technical field
The present invention relates to a kind of paste state bed reactor, more particularly, is a kind of internal-circulation type paste state bed reactor, and it faces the application of hydrogen altogether in sweetening process or fischer-tropsch synthesis process at coal Direct Hydrogenation liquefaction process, oily coal.
Background technology
Paste state bed reactor is mainly used in the fields such as biochemical industry, sewage disposal, medication chemistry, agricultural byproducts processing, fine chemistry industry, petrochemical industry, Coal Chemical Industry, chemical industry metallurgical.Due to the solid of various gas, liquid and particle size can be there is in reactor, so this type of reactor designs and operating parameter is a lot.According to the difference of reaction mechanism, the designing requirement of slurry bed system is widely different.Some slurry bed system operate at normal temperatures and pressures, and what have operates under normal temperature high voltage, and what have to heat lower operation at normal pressure, and what have operates under temperature-pressure.
Be total in sweetening process in DCL/Direct coal liquefaction or oily coal, adopt superfine catalyst to reduce catalyst amount, thus propose slurry bed system designing requirement.Reaction characteristics requires that in reactor, slurries are with larger inspiratory flow rate, thus strengthens heat, matter transmission effect.Adopt during outer circulation mode and need circulating pump.Under this circulating pump operates in high pressure, the condition of high temperature, and containing a certain amount of solia particle in slurries, wear phenomenon cannot be avoided, so very harsh to the requirement of circulating pump.Inner eycle can improve liquid flow rate in bed equally, but needs to solve the problems such as Dead Core Problems, gas assignment problem, built-in air-lift tube design.
Application number be 200610083439.0 and the patent of 200610089023.x individually disclose a kind of slurry bed circulatory flow reactor and a kind of slurry reactor equipment, both all adopt outer circulation form to realize serum recycle flowing.
Application number be 200710037008.5 patent discloses a kind of slurry reactor device with Inner eycle and external heat-exchanging and application thereof.Its Inner eycle refers to that the gas Inner eycle that reactor bottom exists, this reactor are mainly used in synthesis gas and produce liquid fuel.
Application number be 200720155903 Chinese patent a kind of Novel internal circulation paste state bed reactor is disclosed, produce the organic matters such as hydro carbons, alcohols, ethers, lipid for the synthesis of gas.This reactor center arranges a up big and down small riser, and gas and slurries therefrom upwards flow.Riser tube wall is wound around coil pipe, for pipetting reaction release heat.But can there is a lot of problem when facing hydrogen for DCL/Direct coal liquefaction or coal and transforming in this reactor: first can run into slurries short circuit problem, and namely inlet slurry directly flows out from outlet at bottom, and does not enter riser; Secondly when suitability for industrialized production, adopt a riser, because diameter is large, be difficult to ensure that distribution of gas is even; 3rd, bubble in a riser on flowing, if bed is higher, due to the poly-loose effect of bubble, too many air pocket can be formed, when air pocket breaks, cause bed unstable; 4th, solid particles sediment problem is not considered in reactor bottom design, if for Coal liquefaction operation, easily form dead angle, causes coking.
Summary of the invention
The object of this invention is to provide a kind of paste state bed reactor and the application thereof with Inner eycle effect.
Internal-circulation type paste state bed reactor provided by the present invention, comprise reactor shell, top end socket, bottom bulkhead, charging aperture and discharging opening, 1 ~ 160 built-in cylindrical shell is set in reactor shell, the diameter of built-in cylindrical shell and the diameter proportion of reactor shell are 0.05 ~ 0.95, the height of built-in cylindrical shell and the aspect ratio of reactor shell are 0.1 ~ 1.0, and the built-in cylindrical shell bottom of every root is provided with gas distributor.
Arrange the built-in cylindrical shell that 7 ~ 120 axis are parallel in described reactor shell, the diameter of built-in cylindrical shell and the diameter proportion of reactor shell are 0.1 ~ 0.7, and the height of built-in cylindrical shell and the aspect ratio of reactor shell are 0.2 ~ 0.6.
Described built-in cylindrical shell and reactor shell are fixed together with fixed component, this fixed component reduces the impact on slurry flow area as far as possible while the mechanical requirements of satisfied necessity.Built-in cylindrical shell can be uniform in the layout of reactor shell cross section, also can according to certain regular arrangement.In same reactor, the upper end of all built-in cylindrical shells can in same level, also can not in same level.The lower end of all built-in cylindrical shells can in same level, also can not in same level, preferably not in same level.In same reactor, built-in cylindrical shell can be same height, also can select differing heights.
At the top end socket of reactor and/or upper side, 1 ~ 2 discharging opening is set.Gas and slurries can be discharged from a discharging opening, also can discharge from gas vent and serum outlet respectively.
In a preferred scheme, described bottom bulkhead is ellipse head or dome head or cone end socket, arranges 1 slurries material inlet, arrange 1 ~ 3 gas feed mouth at other positions of bottom bulkhead in bottom bulkhead center.
When bottom bulkhead is cone end socket, the cone angle of cone is less than 120 °, preferably 15 ° ~ 75 °.
In another preferred scheme, 1 ~ 3 gas feed mouth is only set at bottom bulkhead, slurries material inlet is not set.This paste state bed reactor is more suitable for Fischer-Tropsch synthesis.
Gas distributor is placed in built-in cylindrical shell bottom, higher than built-in cylindrical shell lower end 10 ~ 500mm, preferably 100 ~ 400mm.The built-in cylindrical shell of every root configures a gas distributor.The gas tank of the gas distributor of each built-in cylindrical shell is communicated with total gas tank, and total gas tank is fixed on reactor bottom, and is communicated with the gas feed mouth of reactor.
Described gas distributor is made up of the pipe of dendritic shape, the pipe of toroidal or the combination of the two, and the pipe of dendritic shape and the internal diameter of annular pipe are 5 ~ 200mm, preferably 5 ~ 100mm, further preferred 10 ~ 60mm.Some that the pipe of dendritic shape and/or the pipe of toroidal distribute is given vent to anger aperture, and hole diameter is 0.5 ~ 90mm, preferably 0.5 ~ 60mm, further preferred 1.0 ~ 30mm.Described aperture can upwards be opened, and also can open downwards, can also upper and lower mixing open.
An application for any one paste state bed reactor above-mentioned, described paste state bed reactor is used for coal Direct Hydrogenation liquefaction process, oily coal faces hydrogen and is total in sweetening process or fischer-tropsch synthesis process.
Slurry feed enters paste state bed reactor by slurries material inlet, gas from gas charging aperture is introduced, each gas distributor is entered after total gas tank, at reactor bottom, enter from built-in cylindrical shell lower end after slurries raw material mixes with loop slurry, upwards flow together with gas distributor gas out, continue to move upward from built-in cylindrical shell gas out, and discharge reactor by top discharge mouth, major part slurries carry the lateral current downflow of a small amount of bubble at built-in cylindrical shell secretly, form Inner eycle, remainder slurries upwards flow, through discharging opening outflow reactor after slurry tank is assembled.Define Inner eycle in described paste state bed reactor, slurries flowing velocity is increased, the motive force of its Inner eycle is the inside and outside differential static pressure of built-in cylindrical shell.
The volume ratio of total gas feed flow and slurry feed flow is 5 ~ 2000Nm
3/ m
3, preferably 200 ~ 1200Nm
3/ m
3.
Carry under one's arms in described slurry feed gas, its gas liquid ratio is 0.5 ~ 600Nm
3/ m
3.
Paste state bed reactor be used for coal Direct Hydrogenation liquefaction process or oily coal face hydrogen altogether sweetening process time, reaction pressure is 3.0 ~ 30MPa, and reaction temperature is 300 ~ 510 DEG C of scopes, and the slurries time of staying is 5 ~ 100 minutes, preferably 10 ~ 70 minutes.
Described reactor may be used alone, can also be used in combination.In the course of reaction participated in there being coal dust, preferred multiple reactor series connection uses.
Paste state bed reactor provided by the invention, feature is that slurries constantly circulate in reactor, without the need to slurry outside circulation, does not need outer circulation pump.In addition, built-in cylindrical shell adopts suitable quantity and diameter ratio, so there is not slurries short circuit problem and bed instability problem.This reactor enhances the performance easy to operate of device, thus can prolong operation cycle, reduces operating cost.Described Inner eycle paste state bed reactor is applied to the slurries time of staying longer course of reaction, as coal Direct Hydrogenation liquefaction process or oily coal face hydrogen coprocessing technical process.
Accompanying drawing explanation
Fig. 1 is Inner eycle paste state bed reactor structural representation provided by the invention.
Fig. 2 is Inner eycle paste state bed reactor ruuning situation schematic diagram provided by the invention.
Fig. 3 is that built-in cylindrical shell arranges schematic diagram.
Fig. 4 is gas distributor structural representation.
Detailed description of the invention
Below in conjunction with accompanying drawing, method of the present invention is illustrated further, but not thereby limiting the invention.
As shown in Figure 1, Inner eycle paste state bed reactor provided by the invention comprises reactor shell 1, top end socket 2 and bottom bulkhead 3, arrange gas discharge mouth 4 in the center of top end socket 2, reactor top arranges slurry tank 5, and is communicated with the slurry discharge mouth 6 of reactor upper side.Slurries material inlet 7 is set in bottom bulkhead 3 center, gas feed mouth 8 is set at other positions of bottom bulkhead.Arrange 1 ~ 160 built-in cylindrical shell 9 in reactor shell 1, every root built-in cylindrical shell 1 bottom is provided with gas distributor 10.The gas tank of the gas distributor 10 of each built-in cylindrical shell is communicated with total gas tank 12 through pipeline 11, and total gas tank 12 is fixed on reactor bottom, and is communicated with the gas feed mouth 8 of reactor through pipeline 13.
As shown in Figure 2, Inner eycle paste state bed reactor operation operation conditions provided by the invention is such: under certain pressure and uniform temperature, gas enters reactor from gas feed mouth 8, and slurries a small amount of gas of carrying under one's arms enters from the slurries material inlet 7 of reactor bottom.At reactor bottom, enter from built-in cylindrical shell 9 lower end after fed slurry mixes with loop slurry, upwards flow together with gas distributor gas out.Because gas is fast and liquid speed is all higher, mass transfer, heat transfer effect strengthen.Continue to move upward, until discharge reactor from reactor head gas discharge mouth 4 from built-in cylindrical shell gas out.Major part slurries are carried a small amount of bubble secretly and are flowed downward, and form Inner eycle.Remainder slurries upwards flow, and slurry tank in upper end is assembled and by slurry discharge mouth 6 outflow reactor.
Fig. 3 is the layout schematic diagram being provided with 12 built-in cylindrical shells 9 in reactor shell 1, is evenly arranged in reactor cross section.
Fig. 4 is gas distributor structural representation, is made up of the pipe of dendritic shape and the tube combinations of toroidal.
Below by embodiment, internal-circulation type paste state bed reactor of the present invention and application thereof are illustrated further, but not thereby limiting the invention.
Embodiment 1
Internal-circulation type paste state bed reactor of the present invention is adopted to carry out the reaction of coal Direct Hydrogenation liquefaction.Wherein, reactor shell internal diameter 1.5 meters, height 25 meters.Built-in cylinder internal diameter 0.35 meter, high 9.3 meters, built-in cylindrical shell quantity 10, is evenly arranged in reactor cross section.Built-in cylindrical shell lower end arranges gas distributor, and the internal diameter of gas distributor pipe is 20mm, and the spilehole diameter on pipe is 5mm, quantity 150.
Select a kind of ub-bituminous coal as raw material, its character is in table 1.Coal sample being milled down to average grain diameter is 60 μm, drying 30 minutes under the protection of 105 DEG C of temperature, high pure nitrogen.Selecting with condensed-nuclei aromatics is the solvent naphtha of key component, is made into coal, solid content 45% in slurries after hydrotreatment with coal dust.Iron catalyst is added, active component content 1.5% in pulping process.
With purity be the hydrogen of 99% as unstrpped gas, gas, liquid volume ratio are 810Nm
3/ m
3.Coal slurry pumps into reactor after preheating, and flow is 45m
3/ h.React under reactor pressure 18MPa, temperature 450 DEG C of operating conditions.
While gathering logistics data, to gas, slurries sampling analysis.Result shows, the conversion ratio of dry ash free basis coal reaches 75%, and vapour, diesel oil distillate total recovery are 43%.
Embodiment 2
Adopt the paste state bed reactor identical with embodiment 1 to carry out oily coal to face hydrogen and refine altogether, other conditions are identical with embodiment 1 with coal raw material, and just being changed by the solvent naphtha taking condensed-nuclei aromatics as key component is heavy crude (the density 1.011g/cm of initial boiling point 310 DEG C
3), make coal with coal dust.Result shows, the conversion ratio of dry ash free basis coal reaches 63%, and vapour, diesel oil distillate total recovery are 52%.
Table 1
M in table 1
adwater content, A
dash content, V
dafit is volatile matter.Ad represents air-dried basis; D represents dry base; Daf represents dry ash free basis.
Embodiment 3
The mode of two paste state bed reactor serial operations identical with embodiment 1 is adopted to carry out the reaction of coal Direct Hydrogenation liquefaction.Raw material is identical with embodiment 1 with operating condition, and result shows, the conversion ratio of dry ash free basis coal reaches 93%, and vapour, diesel oil distillate yield are 53%.
Embodiment 4
Adopt internal-circulation type paste state bed reactor of the present invention to carry out Fischer-Tropsch synthesis, other parameters of reactor are identical with embodiment 1, and just liquid outlet opening moves down 5 meters, simultaneously built-in heat exchanger in every built-in cylindrical shell of root.With a certain amount of paraffin for original liquid mobile phase, reactor bottom is without slurry feed mouth.Unstripped gas composition is based on carbon monoxide and hydrogen, and its mol ratio is CO/H
2=1.5.Raw gas flow 9750Nm
3/ h.Catalyst is the Fe-series catalyst of average grain diameter 60 μm, and catalyst weight content is 7%.Reactor operating pressure 3.0MPa, under temperature 260 DEG C of operating conditions, CO conversion ratio is 92.7%, hydrogen conversion 67.2%.
Claims (11)
1. an internal-circulation type paste state bed reactor, comprise reactor shell, top end socket, bottom bulkhead, charging aperture and discharging opening, it is characterized in that, the built-in cylindrical shell that 7 ~ 120 axis are parallel is set in described reactor shell, the diameter of built-in cylindrical shell and the diameter proportion of reactor shell are 0.05 ~ 0.23, the height of built-in cylindrical shell and the aspect ratio of reactor shell are 0.1 ~ 1.0, the built-in cylindrical shell bottom of every root is provided with gas distributor, described gas distributor is by the pipe of dendritic shape, the pipe of toroidal or the combination of the two are formed, the pipe of dendritic shape and the internal diameter of annular pipe are 5 ~ 200mm, on the pipe of described dendritic shape and/or the pipe of toroidal, distribution is given vent to anger aperture, hole diameter is 0.5 ~ 90mm.
2. according to paste state bed reactor according to claim 1, it is characterized in that, 1 ~ 2 discharging opening is set at the top end socket of reactor and/or upper side.
3. according to paste state bed reactor according to claim 1, it is characterized in that, described bottom bulkhead is ellipse head or dome head or cone end socket, arranges 1 slurries material inlet, arrange 1 ~ 3 gas feed mouth at other positions of bottom bulkhead in bottom bulkhead center.
4. according to paste state bed reactor according to claim 3, it is characterized in that, described bottom bulkhead is cone end socket, and the cone angle of cone is less than 120 °.
5. according to paste state bed reactor according to claim 1, it is characterized in that, 1 ~ 3 gas feed mouth is set at bottom bulkhead.
6. according to paste state bed reactor according to claim 1, it is characterized in that, the gas tank of the gas distributor of each built-in cylindrical shell is communicated with total gas tank, and total gas tank is fixed on reactor bottom, and is communicated with the gas feed mouth of reactor.
7. an application for any one paste state bed reactor of claim 1-6, is characterized in that, described paste state bed reactor is used for coal Direct Hydrogenation liquefaction process, oily coal faces hydrogen and is total in sweetening process or fischer-tropsch synthesis process.
8. in accordance with the method for claim 7, it is characterized in that, slurry feed enters paste state bed reactor by slurries material inlet, gas from gas charging aperture is introduced, each gas distributor is entered after total gas tank, at reactor bottom, enter from built-in cylindrical shell lower end after slurries raw material mixes with loop slurry, upwards flow together with gas distributor gas out, continue to move upward from built-in cylindrical shell gas out, and discharge reactor by top discharge mouth, major part slurries carry the lateral current downflow of a small amount of bubble at built-in cylindrical shell secretly, form Inner eycle, remainder slurries upwards flow, through discharging opening outflow reactor after slurry tank is assembled.
9. in accordance with the method for claim 8, it is characterized in that, the volume ratio of total gas feed flow and slurry feed flow is 500 ~ 2000Nm
3/ m
3.
10. in accordance with the method for claim 8, it is characterized in that, gas of carrying under one's arms in described slurry feed, its gas liquid ratio is 0.5 ~ 600Nm
3/ m
3.
11. in accordance with the method for claim 7, described paste state bed reactor be used for coal Direct Hydrogenation liquefaction process or oily coal face hydrogen altogether sweetening process time, reaction pressure is 3.0 ~ 30MPa, and reaction temperature is 300 ~ 510 DEG C of scopes, and the slurries time of staying is 5 ~ 100 minutes.
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| CN102962011B (en) * | 2012-11-20 | 2015-08-05 | 迈瑞尔实验设备（上海）有限公司 | A kind of High Efficiency Thermal exchange reactor |
| CN103962069B (en) * | 2013-01-31 | 2017-03-08 | 中国科学院上海高等研究院 | A kind of paste state bed reactor |
| CN106635138B (en) * | 2015-10-29 | 2018-05-18 | 中国石油化工股份有限公司 | A kind of slurry bed system method for hydrogen cracking |
| CN106635152B (en) * | 2015-10-29 | 2018-07-31 | 中国石油化工股份有限公司 | A kind of processing method of full fraction of coal tar oil |
| CN106635157B (en) * | 2015-10-29 | 2018-05-18 | 中国石油化工股份有限公司 | A kind of lightening method of inferior feedstock oil |
| CN106635158B (en) * | 2015-10-29 | 2018-08-28 | 中国石油化工股份有限公司 | A kind of lightening method of full fraction of coal tar |
| CN107983270B (en) * | 2016-10-27 | 2021-01-08 | 中国石油化工股份有限公司 | Moving bed reactor, solid acid alkylation reaction system and solid acid alkylation reaction method |
| CN108456550B (en) * | 2018-01-30 | 2020-05-12 | 煤炭科学技术研究院有限公司 | External circulation type reaction device and kerosene co-refining method |
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| CN201052457Y (en) * | 2007-07-03 | 2008-04-30 | 中国石油大学(北京) | Novel inner circulation slurry-bed reactor |
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| CN2500675Y (en) * | 2001-09-28 | 2002-07-17 | 胡建东 | Multi-pipe aerobic internal circulation three-phase biological fluidized bed |
| CN1283349C (en) * | 2004-06-25 | 2006-11-08 | 太原理工大学 | Highly effective slurry phase bed reactor |
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| CN2384947Y (en) * | 1999-07-22 | 2000-06-28 | 华东理工大学 | Honeycomb carrier fixed cell airlift internal circulating biological reactor |
| CN201052457Y (en) * | 2007-07-03 | 2008-04-30 | 中国石油大学(北京) | Novel inner circulation slurry-bed reactor |
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