CN1092337A - Solid-liquid suspended substance treatment facility and catalytic multi-phase reactor - Google Patents

Solid-liquid suspended substance treatment facility and catalytic multi-phase reactor Download PDF

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Publication number
CN1092337A
CN1092337A CN94101116A CN94101116A CN1092337A CN 1092337 A CN1092337 A CN 1092337A CN 94101116 A CN94101116 A CN 94101116A CN 94101116 A CN94101116 A CN 94101116A CN 1092337 A CN1092337 A CN 1092337A
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China
Prior art keywords
described equipment
filter core
district
leaches
gas
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CN94101116A
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CN1050533C (en
Inventor
厄林·莱特
珀·罗特鲁德
彼得·利安
特朗德·迈尔斯塔德
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Equinor ASA
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Statoil ASA
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/005Separating solid material from the gas/liquid stream
    • B01J8/006Separating solid material from the gas/liquid stream by filtration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/1836Heating and cooling the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/18Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
    • B01J8/20Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium
    • B01J8/22Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles with liquid as a fluidising medium gas being introduced into the liquid
    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2/00Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon
    • C10G2/30Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen
    • C10G2/32Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts
    • C10G2/34Apparatus, reactors
    • C10G2/342Apparatus, reactors with moving solid catalysts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00106Controlling the temperature by indirect heat exchange
    • B01J2208/00115Controlling the temperature by indirect heat exchange with heat exchange elements inside the bed of solid particles
    • B01J2208/00132Tubes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00049Controlling or regulating processes
    • B01J2219/00245Avoiding undesirable reactions or side-effects
    • B01J2219/0025Foam formation

Abstract

The solid-liquid suspended substance consersion unit (11) that is used for Fischer-Tropsch synthesis.It comprises that one limits in order to hold and receives the reaction vessel (12) of reaction zone of the suspended phase and the top gas compartment (16) thereof, and one makes gas reactant introduce the sintered plate of suspended substance and leaches section (13) in order to what isolate product liquid from suspended substance.Leach section (13) and comprise a housing (25), the outlet (32) of a filter core (26) and product filtrate.A pipe (38) makes the connection of setting up fluid between the gas compartment (16) above the gas compartment (29) of filtrate top and the suspended substance.

Description

Solid-liquid suspended substance treatment facility and catalytic multi-phase reactor
The present invention relates to a kind of reactor that carries out the continual multi-phase reaction, particularly, though be not ad hoc, be applicable to Fischer-Tropsch (Fischer-Tropsch) synthetic method, the forming gas catalysis that produces from methanol recapitalization changes hydro carbons (hydrocarbon) fuel into, this equipment also is applicable to other reaction systems, comprises various suspended substances (or claiming slurry) reactions for producing petrochemicals, from the suspended substance reaction of synthesis gas production oxide and dehydrogenation reaction etc.In addition, this equipment can be applicable to solid-liquid suspension processing equally.
The three phase catalytic reaction system is used in a lot of chemical processes, and the application in petro chemical industry grows with each passing day especially.The suspended substance reactor that mechanical agitation is arranged in the used three-phase system, the tower suspended substance reactor of loop bubble agitation, these reactors are used the catalyst granules that is dispersed in the liquid, so in most of application scenarios, liquid must be separated with separation of liquid products from suspended substance, or for the regeneration purpose of catalyst.In the occasion of liquid as the inertia medium, because cracking or impurity form, liquid also must be changed occasionally.
Mechanical agitation formula suspended substance reactor, because lower material Transfer amount and thermal resistance effect, it is convenient especially to be used for producing in batches, these characteristics also make to be determined to be well suited in reaction power class hour in the laboratory.Yet such reactor has a series of shortcomings and limitation, and it all is very difficult will separating catalyst granules in any continuous operation.
From the industrialization viewpoint, have only mechanical agitation formula reactor to be applied to the double-stranded hydrogenation of oils that obtains from cottonseed, soya bean, grain, sunflower seed etc. in large quantities, use a kind of Raney nickel, the product of gained comprises margarine, shortening, soap and grease etc.The work of the tower suspended substance reactor of bubble agitation is simple, because do not need to use mechanical moving element, combines the advantage of low diffusing resistance and high heat conduction efficiency, and it is very attractive that these reactors are used in a lot of industrial process.Yet, the separation of solid-liquid is normally carried out in the fine filtering of reactor outside and treatment system, catalyst suspension will be sent into reactor recirculation, sometimes be to use a kind of suspended substance pump to implement, thereby, a series of problems appear in the tower suspended substance reactor of bubble agitation running hours probably.
Because petroleum resources are in the world reducing, to use natural gas to become and have more attraction as the energy, its importance of method that makes its quality rise to high-grade hydrocarbon fuel is simultaneously increasing.
Therefore, one object of the present invention is to provide a kind of reactor that can carry out heterogeneous catalytic reaction continuously, and it can not produce the shortcoming in the prior art.
The more specific purpose of the present invention is to provide a kind of reactor that natural gas is changed into diesel fuel through synthesis gas that is applicable to.
The problem that catalyst in Fischer-Tropsch (Fischer-Tropsch) suspended substance reactor assembly/paraffin separates is addressed in one piece of report that USDOE delivers recently, and the report conclusion is said:
" at the internal ramp of the immersion reactor suspended substance that is used for some small-scale or experimental scale, because the operation difficulty can not be worked effectively.An a kind of part with its wall may be suitable for when experimental scale is used as the reactor of filter, but is unpractical as the coml reactor.Inner filter has the danger of obstruction, will cause too early outage, and the factory that produces in enormous quantities is not allowed this risk ".
Many places are addressed the internal ramp that is immersed in the reaction suspension and are employed in a research project in the report, yet, rely on pressure differential filtered fluid stream when beginning, can flow smoothly, but very fast filter can stop up, therefore report that conclusion says, continued operation is unpractiaca, thereby in commercial-scale production occasion, is necessary to make the outside that is separated in reactor of solid-liquid to carry out.
The present patent application people finds, opposite with above-mentioned conclusion, can be Fischer-Tropsch synthesis a kind of continuous reaction system is provided, solid/liquid separation wherein is unnecessary carries out in an external filter devices, in addition, the production to commercial scale can reach enough big filtering traffic.
According to one aspect of the invention, a kind of solid-liquid suspended substance consersion unit is provided, be used for generating in the suspended phase of the liquid medium that contains the fine particle catalyst reaction of liquid product, equipment includes: one limits and holds suspended phase and the reaction vessel of the reaction zone of the gas compartment above suspended phase; The device in the suspended phase of gas reactant and/or other components introducing container lower area; The section that leaches that is used for from suspended phase, isolating product liquid, it comprises that a housing and one limit the filter core (filter element) that leaches the district with housing, leach the outlet that the district has a filtrate; Leach district and reaction zone inner suspension mutually above, form the device of fluid connection between that part of volume that occupies by gas during use; One sets up the device of average pressure reduction by filter core; In one embodiment, the device of setting up average pressure reduction by filter core among embodiment, comprises a valve and a control module of being connected with the outlet that leaches the district therein.Another kind of version is, filter core contacts with suspended substance in the suspension tagma, and housing centers on reaction vessel at least in part.
This equipment also can be used for slightly different purpose, and such as various forms of processing occasions, for example, ion-exchange is purified, and removes unwanted component (trace impurity, spot).
Thereby, from wide significance, the invention provides a kind of solid-liquid suspended substance treatment facility, wherein product liquid contains from liquid medium in the suspended phase of finely disintegrated catalyst and separates, and this device includes: one limits the container of the treatment region that holds suspended phase and suspended phase upper gas; The device in gas reactant and/or other components introducing container lower area suspended phase; The section that leaches that is used for from suspended phase, isolating product liquid, it comprises that a housing and one therewith limit the filter core that leaches the district, leach the outlet that the district has a filtrate; Leach district's top treatment region inner suspension mutually above, forms the device of fluid connection between that part of volume that occupies by gas during use; One sets up the device of average pressure reduction by filter core, filter core contact with suspended substance in the suspension tagma and housing at least in part around container.
The present patent application people finds, is communicated with leaching between district and the reaction zone (or treatment region), can prevent that solid matter from generating (term " reaction zone " can refer to reaction zone in suitable occasion, also can refer to treatment region) on filter core.It is believed that this is reached by following reason, because the disturbance of suspended substance, for example bubble is upward through suspended substance, and the shake that can cause filter core place pressure is shaken or fluctuate, sets up fluid between the district and is communicated with and can promotes or strengthen this filter and move or shake and shake with leaching at reaction zone.
Thereby this system comparatively speaking not only simply but also effective is considered to the maximum separating step of problem usually and implements too difficulty, and under suitable condition of work, filtration members can self-cleaning.
Preferably the part of shell holds reaction vessel at least, and filter core can be to be made of reaction vessel part wall body, and this is made of filtering material.In an example that changes to some extent, filter core is positioned at the outside of container, and container is discontinuous in the filter core region.In another variation instance, filter core is the inside that is positioned at container, and housing is made of the part of chamber wall.Setting up fluid between the gas that is preferably in suspended phase top and the gas that leaches the top, district is communicated with.
Filter the hydrostatic pressure that (going out) liquid forms at the hydrostatic pressure that reaction vessel inner suspension body forms in the district greater than leaching, its result forms pressure differential between the two, therefore the space with reaction zone inner suspension body top is interconnected with the space that leaches filtrate top in the district, can prevent from excessively to be raise by the pressure reduction that hydrostatic pressure forms.Connection between two chambeies can preferably be communicated with the layout of the pipe of two parts gas at the reaction zone top with leach the pipe that extends between the top, district and connect and realize easily by one, helps to leach all gas that gathers on top, district and escapes away by it.
The vibration by the formed pressure differential of filter core or the size or the amplitude of pulsation are best, the amplitude that is substantially equal to or is a bit larger tham hydrostatic pressure difference.And preferably can keep a lower value by the average pressure reduction of filter core, typical situation is to be lower than 6 millibars (or 600 handkerchiefs).If average pressure reduction can be lower than a critical value (this value is 6 millibars in instance system), filter just can be realized automatically cleaning.Be worth when pressure surpasses this slightly, the caking of particle will appear in filter surfaces, and this situation is very common to filter, so filter capacity has just progressively reduced.If liquid stream reverse flow (countercurrent washing) caking by system will disappear, also just can recover original filter capacity.If force value is higher, catalyst granules may penetrate filter, and when this situation took place, the decline of filter capacity just may exist all the time, adopts countercurrent washing can not increase filter capacity.Fluid communicating pipe is except that constituting between the gas phase that makes suspended substance top and the inside of filtering section fluid is communicated with, and also provides one may pass filter core and be trapped within the passage that the escape of gas that leaches the district is gone out.
The product of gaseous state or component can be by any devices easily, and for example anti-container independent outlet is escaped away or overflowed by fluid communication easily.Find that in test if clogged tube or serious the obstruction, filter core can be filled up very soon so.Certainly, limit a scope can for fluid communicating pipe pressure by filter core, thus as described prevent to set up undesirable damage pressure like that, otherwise, when having significant pressure to fall between the inside of reaction vessel and the outside, this meeting causes that the pressure of damage forms probably.
Preferably filter core has fine screen mesh, the filamentary webs of spirality winding, thin vertical silk screen or metallic particles sinter, and even more ideal is that the surface that filter core contacts with suspended substance will be done very smoothly.
The material of filter core and catalyst are preferably selected like this, and promptly the size of the eyelet of filter core maximum or aperture should should be the same order of magnitude with the size of catalyst granules, and the size of particle preferably is not less than half of size in hole.
The device of introducing gas reactant or component can be various suitable devices, chews such as bubble cap tray, one group of jet pipe, and sintered plate etc. preferably are arranged at the bottom of reaction vessel.Reactant can be CO and H 2, product then is methyl alcohol and higher hydrocarbon (for example reactant of gas renormalizing).
The pressure oscillation value may be the magnitude of pressure reduction, for example is the 10-200% of pressure reduction, and actual pressure difference can be the 1-100 millibar, is preferably the 2-50 millibar.
Container preferably is provided with the import and/or the outlet of a liquid reactants, and a superposed gas vent is preferably arranged, and is provided with to comprise that also flushing leaches the device of section and filter core.
The layout that preferably leaches district's outlet can make the filtrate that leaches in the district keep a constant liquid level.In one embodiment, the outlet that leaches the district includes a pipe of being inverted U-shaped, and its top section defines the liquid level that leaches in the district.In the example of a variation, the outlet that leaches the district includes and is arranged at the weir plate that leaches in the section, limits the liquid level that leaches in the district with it.In another variation instance, the outlet that leaches the district includes to be positioned at and leaches the upwardly extending pipe in district, and the height of its opening defines the liquid level that leaches in the district.
Preferably reaction vessel is provided with heat conducting device, and it can comprise one group of vertically arranged pipe heat supply transmitting medium circulation cycle.
In a most preferred embodiment, above the suspended substance and to leach above the district that the fluid between the gas is communicated be with a communicating pipe.In the example of a variation, the wall of reaction vessel, the housing top that leaches section forms a dome, and the gas of suspended substance top forms directly with the gas of filtering area top and is communicated with whereby.
In order to adapt to higher productivity ratio, can be equipped with the higher filtering surface of efficient, this can realize by adopting more complicated or compound filter core (profile).
In addition, can be provided with and leach section more than one and realize, in one embodiment, these leach section and include filter core and the housing that is spaced apart from each other on the vertical direction, housing has that overlap may be not overlapping yet, yet, in the embodiment of a variation, the section that leaches of one group of vertical direction each interval can be arranged.Best, each housing that leaches section is flanged (FLGD) each pipeline section, forms a rigid structure by connector in conjunction with (for example using bolt) between each section together.
The present invention's effect in the method that natural gas (methyl alcohol) is changed into higher hydrocarbons fuel is good especially, this relates at first by steam reformation, partial oxidation or both is comprehensive, or the reformation by methyl alcohol produces carbon monoxide and hydrogen, makes CO and H with Fischer-Tropsch synthesis 2Catalysis changes and forms higher hydrocarbons fuel, such as liquid paraffin, these products is separated or/and the hydro carbons (hydrocarbon) of cracking to form required rate range.
Diesel fuel with this method is produced comes from its quality and characteristic, and it is much better more than common diesel fuel.Secondly at first, it does not comprise sulphur, and from the viewpoint to ambient influnence, this point is very important, and, it has very high Cetane number, thereby the product that it and more low-grade diesel fuel composition are mixed formation can satisfy the standard of high-quality scope.The 3rd, in fact it does not comprise burning the time can not produce the harmful components of coal smoke, and need add additive hardly and just can successfully use at low temperatures.
The present invention can make it to realize by the whole bag of tricks, now consults each accompanying drawing as an example and narrates with some embodiment, wherein:
Fig. 1 is the cross-sectional that is used to realize by the three-phase suspended substance consersion unit of the inventive method;
Fig. 2 and Fig. 3 are the cross section sketch maps of simplifying, and by a part that leaches section two kinds of multi-form filtrate liquid levels that make are shown and keep constant system;
Fig. 4 is and Fig. 2 and the similar view of Fig. 3 that the location arrangements of a kind of variation of filter core is shown;
Fig. 5 is the schematic perspective view that leaches a section part, and the another kind of possible location arrangements of filter core is shown;
Fig. 6 is a level cross-sectionn figure, and the another kind of form that filter core is arranged is shown;
Fig. 7 is the sketch similar with Fig. 1, and a kind of example of variation is shown;
Fig. 8 is the vertical cross-section diagram that the filtration system of another kind of embodiment is amplified;
Fig. 9 is the part vertical cross-section diagram of another embodiment; And
Figure 10 illustrates the result curve figure in a kind of experimental example.
As shown in Figure 1, consersion unit 11 includes a reaction vessel 12 and and leaches section 13.Reaction vessel 12 include one substantially in a tubular form pipeline section 14 and be positioned at the reverse taper portion 15 of its top.Pipeline section 14 limits suspension tagma 20, wherein contain the suspended substance that forms by the liquid medium that contains the fine particle catalyst (for example hydrocarbon products), tapering part 15 is overflow and limit a gas compartment 16 in order to the top at reaction zone to prevent that suspended substance from bubbling as expansion chamber, and tapering part 15 can include and is used for fragmentation or reduces the attachment device (not shown) that foam forms.
In the bottom of container 12, a gas access 17 and a gas distributor 18 are arranged, gas is introduced in the suspension tagma by 17 and 18.There are 19, one groups of heat-transfer tubes 21 that between a public inlet 22 and a public outlet 23, extend of a gas vent that communicates with the gas compartment 16 to be positioned at reaction vessel at the top of container 12, heat exchange medium is arranged in the pipe.Equipment 11 is implemented control by a large amount of sensor control valves, pump etc., and 24 is one of them (pressure sensor or temperature sensors) in the drawings, enumerates as an example.
Leach section 13 and comprise a circular shell 24, it near the lower peripheral of tapering part 15 around container 12, the part of chamber wall is to constitute and constituted filter core 26 by the metal sintering thing, the pore-free part 27 of chamber wall extends in the housing 25 at top and bottom respectively, and housing 25 limits one effectively with chamber wall and leaches the district 28 and the gas compartment 29 that is positioned at its top.
An outlet that leaches district 28 keeps constant device as the liquid level that makes filtrate, and a pipe 31 extends upward from the outlet opening 32 near housing 25 bottoms.One horizontal connection tube section 33 defines the liquid level 34 that leaches filtrate in the district and extends downward delivery valve 35 places, and valve 35 is product liquids in order to emptying pin inner accumulated down of opening.Certainly, pin down can be received the groove jar of product liquid and replaces with holding.Efferent duct 31 is the filled with liquid product between perforate 32 and horizontal pipeline section 33.
One communicating pipe 38, pipe 38 had a valve 39 being communicated with to get up between two gas compartments 16 and 29.Thereby communicating pipe 38 also is communicated with the connection of having set up liquid between the gas compartment 16,29 and efferent duct 31 with pipe 31, and housing 25 is also having an inlet 36 that has a valve 37 near its top.
When work, gas reactant is introduced in catalyst suspension and the fluid product by distributor 18, and catalyst granules is suspended state in liquid.By various sensors (for example 24 and hot conducting system 21,22,23 to keep correct temperature.Enter after fluid product filters by filter core 26 and leach district 28.This is to impel realization by the pressure differential by filter core, and pressure differential is to cause that by the hydrostatic pressure of the difference in height existence of suspended substance liquid level and filtrate liquid level the position on the vertical direction of the horizontal pipeline section 33 of efferent duct 31 makes the liquid level 34 of filtrate keep constant.
The disturbance motion of suspended substance helps to prevent the formation of any filtration caking, and pressure oscillation by filter core 26 or vibration also can avoid filter core 26 to be stopped up by catalyst granules, and this moment, valve 39 was in opening.
Gaseous product and all unreacted gas reactants are emitted by exporting 19, because the space 29 inner accumulated gases of having avoided communicating pipe 38 above filtrate are arranged.
Leaching section 13 can such as forming gas, or with the liquid that is suitable for, wash such as pure product with the gas that is suitable for, and open valve 37 this moment, and shut off valve 35 and 39 forces flushing liquor stream oppositely by filter core 26 like this.
When normal running, the part catalyst is removed and replaces with catalyst new or that regenerated.For seem clear for the purpose of, the equipment that is used for this purpose is not shown among Fig. 1, but is appreciated that any modular system that is used for this purpose all can adopt.
A kind of filtrate liquid level that makes of variation keeps constant system to be shown in Fig. 2, in this system, the weir plate 41 of one ring-type is arranged in the housing 25, the filtrate product is collected between filter core 26 and the weir plate 41 and from the outside overflow of weir plate, thereby filtrate liquid level 34 has been determined at the top of weir plate, the outlet 42 of filtrate product is positioned on the housing 25 of weir plate 41 outsides, the volume that such layout leaches the district has reduced, thereby to a given filtrate volume flow, its linear velocity has increased, see that on the whole the refining effect that leaches section can improve.
The another kind of filtrate liquid level 34 that makes keeps constant device shown in Fig. 3, on this occasion in, liquid level is to set by a vertical output tube that extends down in leaching the district 51.
Among the embodiment shown in Figure 4, filter core 103 is positioned at reactor wall 14, thereby a part 104 that leaches the section housing and be by reactor wall 14 constitutes, filtrate that may be by filter core 103 and any gas can emit pipe 106 and are connected with delivery outlet 107 with communicating pipe 38 and by a valve 108 by control module 109 controls from leaching section 105 by a pipe 106, anyly leaching the deposit that section bottom is gathered, open valve 111 washes away deposit by a pipe 110 when needing.Sedimental processing and flushing (in this or other embodiment) can be on purpose by the size of selected control module suitably and suitably the design outlet make it realization.
Among the embodiment shown in Figure 5, filter core 136 is positioned at the outside of reactor wall 14, but is received in as shown in Figure 1 in the external shell 25.Reactor wall 14 interrupts in the zone of filter core 136 and is replaced by some bars 131, contacts with filter core 136 so that allow suspended substance.
If the ability that productivity ratio can be born greater than filter core 26 can increase its filter capacity with the increase effective filtration area so.A kind of method that realizes is to replace (as shown in Figure 6) to the filter that a string plane of the filter core 26 usefulness filter core 61 of ring-type constitutes.
Other form is to adopt two (or more a plurality of) to be positioned at the section that leaches of another top.Fig. 7 shows this layout, wherein has three to leach section 71,81 what vertical direction separated each other, and 91 and each have a filter core 72,82 and 92; One circular shell 73,83 and 93; One leaches district 74,84 and 94; One filtrate product outlet 75,85 and 95.Each outlet 75,85 and 95 includes one and is inverted U-shaped part and in each occasion, and the top of U-shaped defines the CL of filtrates in each respective area 74,84 and 94.Leach district 74 by being provided with each, 84,94 communicating pipes 76,86 that communicate and that be connected with a common manifold 131,96, make and leach district's gas compartment on 74,84,94 tops and the gas compartment 16 on 20 tops, suspension tagma is communicated with each other, manifold 131 is communicated with the gas compartment 16 by valve 132, manifold 131 also with the outlet 75,85 of those products, 95 are connected.Countercurrent washing is by each valve on shut off valve 132 and the pipeline 75,85,95,76,86,96, and unlatching nitrogen transfer valve 77,87 and 97 is implemented.
In the suspended substance system of diethylbenzene/17% vanadine of testing, for the poor value that keep-ups pressure is below the 6m millibar, found that each filter core 72,82,92 vertical direction sizes should be above about 70-75 centimetre, yet, fluid dynamic characteristic according to every kind of specific suspended substance system, this numerical value may change with different suspended substance systems, thereby, may obtain desirable pressure differential under these conditions.So be necessary to choose different filtrate liquid levels and different filter core positions according to filtrate and the density difference between the suspended substance.
A kind of other similar arrangement has been shown, the filter core 72,82,92 that has three vertical direction to separate each other in this embodiment among Fig. 8.But, this sentences a single external shell 98 and two inner shape walls 88,78 replace three independent housings, and annular wall 88,78 is respectively at filter core 92,82 and 82, upwards stretch out between 72, annular wall 88,78 stops on differing heights, thereby determined CL 89,79 separately.The filtrate CL 99 that interrelates with filter core 92 is to be determined by the position of outlet 101.During use, the filtrates at different levels above wall 78 and 88 enter in the space that is limited by housing 98, and by public outlet 101 outputs.
In this embodiment, the one public gas compartment 29 is arranged above filtrates at different levels, it directly is communicated with the gas compartment 16, because reactor vessel wall 14 stops on certain altitude and the gas compartment 16 is limit by the dome 102 that external shell 98 continues to extend to form.Dome 102 have one the outlet 19(not shown).If only use a filter core, so this layout adopts proper in the embodiment shown in fig. 1.
Fig. 9 illustrates another embodiment, has wherein adopted a stringly to leach section 113, because all to leach section 113 size and dimensions identical, so only one of them is described.Leach trivial section and comprise an outer cylindrical wall 114 that connects by flange 115 and reactor vessel wall, also have, filter core 116 is that the porous part by chamber wall constitutes, and limits like this and leaches district 117.Each leaches the flushing liquor inlet 122 that section 113 respectively has a band valve 123, and these inlets are connected with a public flushing liquor supply pipe 124.
Leaching the outlet that district 117 is provided with liquid, this is that pipe 118 by the valve of being controlled with controlled unit 120 119 constitutes, be loaded on one communicating pipe 121 and leach 117 top, district and by communicate a public communicating pipe 125 (consulting Fig. 1) with the gas compartment 16 above the suspended substance, the openend of public communicating pipe 125 extends into the space 16 of suspended substance top, and the valve 126 that an operate as normal is opened often is housed on the pipe.Also can change to some extent is every communicating pipe 121 all can install the valve (not shown).
Can make communicating pipe 121 and may be trapped within all gas that leaches 117 tops, district escapes into the suspended substance top by public communicating pipe 125 and valve 126 the gas compartment 16.
Control module 120 controls that link with valve 119 are from the flow of the product liquid that leaches district 117, to set up the average differential pressure by filter core 116.In fact, control module is to remain on one by the liquid-column height that makes communicating pipe 121 to determine in the scope, the hydrostatic head of filtrate side of keeping filter core 116 is with respect to the hydrostatic pressure of suspended phase, be a little purposes, control module 120 can be provided with the liquid level that can detect in communicating pipe 121 or the device (not shown) of pressure, like this, when detecting liquid level, the sensing device of control module 120 reached in limited time, control valve 119 goes out product liquid Vent from leach district 117, Vent goes out process and continues up to liquid level and reduce to the lower position, this moment control module 120 shut off valves 119, liquid level begins again to end when rising reaches upper limit position in communicating pipe immediately, so constantly circulation also can infer repeatedly certainly from leaching district 117 output product liquid stream continuously.
In the suspension tagma, equal the depth H s and the suspended substance density p of suspended substance with specific plane height 127 corresponding hydrostatic pressures sProduct, the hydrostatic pressure of calculating on same plane 127 that leaches district's filtrate equals the height H f of the output plane 128 of plane above 127 to its and the density p of filtrate fProduct, so the expression plane 128 height H f should satisfy following equation:
H fρ f=H sρ s-△P
△ P is that △ P can use △ Hs ρ by the required very little pressure differential of filter core 116 herein sExpression, wherein △ Hs is corresponding to the additional suspended substance hydrostatic head of small pressure difference.
The relational expression of being discussed is corresponding to embodiment shown in Figure 9, certainly, also generally is applicable to all occasions.
The vertical concussion campaign of filtrate in pipe 121 has strengthened the formation of removing the ability that is attached to the catalyst granules on the filter core 116 and helping to prevent to lump and filtering caking.
Diameter by rationally determining each pipe etc., in addition can utilize since not the disturbance motion between the homophase cause any resonance phenomena in the system, above-mentioned effect is further increased.
Thereby leach district 113 and can implement flushing by flushing liquor input pipe 122 and valve 123, when delivery valve 119 and public connection pipe valve 126(also can change to some extent, valve-not shown is being installed separately communicating pipe) close, flushing oppositely enters and passes filter 116 with fluid, yet, leach district 117 removing any sediment that may accumulate if want to wash, but so open valve 119 flushing liquor stream passes through to allow faster.
To equipment shown in Figure 9, constitute the parts that leach section 113 by design carefully, the few similar parts of entire reaction equipment quantity available assemble, and further, these parts can be the standardized products that is easy to obtain, such as standard pipe, flange.Valve member or the like.Specifically, make the flange size that leaches section identical, the flange that links with filter core 116 and adopt identical cylindrical wall section 114 for example, can make so overall structure firmly, good rigidity, and dismounting and assembling are also very easy.The major function of cylindrical wall section is to hold to receive fluid and make overall structure that good rigidity be arranged in reactor.
When gross pressure surpasses certain value, the size of reactor external component shown in Figure 9 (such as outer cylindrical wall 114 and particularly flange and their fixture) will become greater to not only inconvenience but also unpractical degree, in this case, entire reaction container assembly can be packaged in the interior (not shown) of pressure-bearing shell of an outside.
The present invention will be in conjunction with doing further narration in the following experimental example.
Have the laboratory installation that is similar to cylinder shown in Fig. 1 with one, done some experiments.The length of this device and diameter are respectively 1250 millimeters and 55 millimeters, and its average pore size of used filter core is 30 microns, and the length of filter core is 200 millimeters.
Oily by the heat conduction that Meng Shandou (Monsanto) supplies with, form by diethylbenzene (95%) and a spot of cumene and sec-butylbenzene, vanadine (20% weight) is used to suspended phase, and the particle of alumina is cut into 53 microns at first, and the experiment condition in the experiment is as follows:
Pressure 1 crust
Temperature 20-25 ℃
Gas velocity 6 cels on surface
At initial start-up period, it is constant that the ability of separation roughly becomes, and remains on 750-800 kilogram/rice 2Hour.Its result draws in Figure 10.
Figure 10 illustrates the separating power (kilogram/rice of measuring in the above-mentioned example as the production time function 2Hour), the pressure differential that calculates, promptly the driving force of Fen Liing is also shown in Figure 10, and the mean value shown in the figure is approximately 5 millibars.
Through 40 days production, can observe separating power only had a spot of decline, and can lead up to a conclusion thus, and the time prolongs and can also reach 700 kilograms/meter at least 2Hour separating power.

Claims (25)

1, solid-liquid suspended substance treatment facility (11), wherein product liquid is separated from the suspended phase (20) that the liquid medium that comprises the fine particle catalyst forms, and this equipment includes: one limits in order to hold and receives the container (12) of treatment region of the gas above suspended phase (20) and the suspended phase (20); Be arranged in container (12) lower area in order to introduce gas reactant and/or other components device (17,18) to suspended phase (20); Leach section (13) with one in order to what from suspended phase (20), isolate product liquid, this leaches section (13) and includes a shell (25) and filter core (26), both define one together and leach district (28), leach the outlet (32) that district (28) has product filtrate (abbreviation of filter liquor); It is characterized in that,, set up the device (38) of fluid connection when during leaching district (28) and treatment region, working between occupied that part (16) of the gas above the suspended phase (20) by means of device (38); Respectively set up device (31,32,33) by the average pressure reduction of filter core (26); Filter core (26) is arranged to contact with suspended substance in the treatment region, and shell (25) is at least in part round container (12).
2, by the described equipment of claim 1, it is characterized in that: shell (25) is around at least a portion that surrounds container (12).
3, by claim 1 or 2 described equipment, it is characterized in that: filter core (26) is that the part wall by the container made from filtering material (12) constitutes.
4, by claim 1 or 2 described equipment, it is characterized in that: filter core (136) letter is positioned at the outside of container (12), and container (12) is discontinuous in the zone of filter core (136).
5, by the described equipment of claim 1, it is characterized in that: filter core (103) is positioned at container, and the housing of filter core is to be made of the part of chamber wall (104).
6, by the described equipment of above any one claim, it is characterized in that: described fluid connection device (38) is to be positioned between the gas (16) and the gas (29) above the filtrate of suspended phase top during work.
7, by the described equipment of claim 6, it is characterized in that: described fluid connecting device is a pipe (38) that is communicated with two parts gases (16) and (19).
8, by the described equipment of claim 7, it is characterized in that: being provided with of pipe (38) that connects two parts gas helps make any escape of gas that leaches top, district that accumulates in to go out.
9, by the described equipment of claim 6, it is characterized in that: chamber wall is cut off on certain position, leaches district's housing (98) and forms a dome (102) above container top, thereby directly be communicated with between the gas above the gas of suspended substance top and the filtrate.
10, by above-mentioned any described equipment of claim, it is characterized in that: the device of setting up the average pressure reduction by filter core (103) comprises with leaching to distinguish and exports a valve (108) and a control module (109) that is connected.
11, by above any described equipment of claim, it is characterized in that: leach district's outlet (31,32,33; 41; 42; 51) layout can provide a CL for the filtrate that leaches in the district.
12, by the described equipment of claim 11; It is characterized in that: the average pressure reduction by filter core (26) is to rely on suspended substance surface and the difference between the filtrate liquid level in the suspension tagma (20) to realize.
13, by claim 11 or 12 described equipment; It is characterized in that: the outlet that leaches district (28) comprises a pipe section, and its part (31,33) limits one and is inverted U-shaped, and inverted U-shaped top (33) define the liquid level (34) that leaches in the district (28).
14, by claim 11 or 12 described equipment, it is characterized in that: the outlet that leaches district (28) comprises that is arranged on a weir plate (41) that leaches in the section, and it defines the liquid level (34) that leaches in the district (28).
15, by claim 11 or 12 described equipment, it is characterized in that: the outlet that leaches district (28) comprises that one is positioned to leach and distinguishes upwardly extending pipe (51), and it is at the certain altitude opening, and opening part defines the liquid level (34) that leaches district (28).
16, by above any described equipment of claim, it is characterized in that: filter core (26) comprises a fine screen mesh, the filamentary webs that spirality is twined, metallic particles sinter or ceramic material.
17,, it is characterized in that by above any described equipment of claim: with the contacted cartridge surface of suspended substance to process very smooth.
18, by above any described equipment of claim, it is characterized in that: in container (12), also comprise heat conducting device (21,22,23).
19, by the described equipment of claim 18, it is characterized in that: heat conducting device comprises that is positioned at the vertically arranged pipe of container (12) (21), is used for making the heat-conduction medium circulation.
20, by above any described equipment of claim, it is characterized in that: a gas vent (19) is arranged at treatment region top.
21, by above any described equipment of claim, it is characterized in that: comprise a device (37), it is used for flushing and leaches section and filter core (26).
22, by above any described equipment of claim, it is characterized in that: comprise that several leach section (71,81,91).
23, by the described equipment of claim 22, it is characterized in that: leach section (71,81,91) and respectively comprise separated filter core on the vertical direction (72,82,92) and partly overlapping at least housing (73,89,93).
24, by claim 22 or 23 described equipment, it is characterized in that: the housing that respectively leaches section is flanged (FLGD) pipeline section form, and they interconnect and are fixed into a rigid structure.
25, by above any described equipment of claim, it is characterized in that: consersion unit is provided with outside pressure-bearing shell.
CN94101116A 1993-01-28 1994-01-28 Solid/liquid slurry treatment apparatus and catalytic multi-phase reactor Expired - Lifetime CN1050533C (en)

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GB939301723A GB9301723D0 (en) 1993-01-28 1993-01-28 Solid/liquid treatment apparatus and catalytic multi-phase reactor

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GB9515370D0 (en) 1995-10-04
CA2154184A1 (en) 1994-08-04
GB2289856B (en) 1997-06-04
DK84995A (en) 1995-09-27
AU6011994A (en) 1994-08-15
CN1050533C (en) 2000-03-22
GB2289856A (en) 1995-12-06
ZA94346B (en) 1995-07-18
MY134552A (en) 2007-12-31
CA2154184C (en) 2004-03-23
DZ1750A1 (en) 2002-02-17
DK172646B1 (en) 1999-04-06
GB9301723D0 (en) 1993-03-17
WO1994016807A1 (en) 1994-08-04

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