CN104888668B - A kind of F- T synthesis and the device and method separated - Google Patents
A kind of F- T synthesis and the device and method separated Download PDFInfo
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- CN104888668B CN104888668B CN201510247572.4A CN201510247572A CN104888668B CN 104888668 B CN104888668 B CN 104888668B CN 201510247572 A CN201510247572 A CN 201510247572A CN 104888668 B CN104888668 B CN 104888668B
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Abstract
The invention discloses a kind of F- T synthesis and separator, including paste state bed reactor, First Heat Exchanger, the second heat exchanger, the first filter and the second filter, the First Heat Exchanger is built in reactor top, second heat exchanger is arranged on outside the paste state bed reactor, first filter is built in the middle part of reactor, and the second filter is arranged on outside the paste state bed reactor；The invention also discloses carry out method of the F- T synthesis with separating using said apparatus；The present invention is cooled by sending into reactor lower part slurries to exchange heat in the second external heat exchanger, and flow the size circulations of reactor lower part, heat exchange efficiency can be improved, and on reactor top, because portion and top reaction are more gentle in the reactor, the heat of accumulation is contacted by First Heat Exchanger to be removed, improve space reactor utilization rate, slurries after cooling through First Heat Exchanger further can be backflowed downwards, so as to be conducive to further improving reaction efficiency due to density increase.
Description
Technical field
The present invention relates to F- T synthesis field, more particularly to a kind of F- T synthesis and the device and method separated.
Background technology
With the increasingly reduction of petroleum resources, and the mankind, to the increasingly strict of requirement of preserving the ecological environment, the world is to clean
The demand of net liquid fuel is sharply increased, and in order to meet this demand, various countries' researcher is directed to researching and developing clean combustion
The oily production technology of material, wherein being attracted most attention with Fischer-Tropsch (Fischer-Tropsch) synthetic technology.Typical fischer-tropsch synthesis process stream
Cheng Wei：First, coal/natural gas through gasification or partial oxidation, it is reforming be synthesis gas, then by synthetic gas desulfurization, deoxidizing purification
Afterwards, according to the fischer-tropsch synthesis process condition and catalyst of use, H/CO ratios is adjusted, are produced subsequently into Fischer-Tropsch synthesis device mixed
Close hydrocarbon.Finally, synthetic product can obtain different target product after separation processing modification.
Fischer-Tropsch synthesis device is the core of F- T synthesis technology, because F- T synthesis is strong exothermal reaction, is being reacted
Reaction heat must be removed in time in journey, otherwise, catalyst is easy for hot localised points occur, cause its rapid deactivation and reduction to be grown
The selectivity of paraffin products；In addition, the bed of paste state bed reactor is in three-phase turbulence state, catalyst in reactor with
Reactor wall, reactor inner member and catalyst particles intergranular can collide and rub, and be inevitably broken and efflorescence, lead
Cause to occur the powder that such as particle diameter is less than 5 μm, these powder can flow out paste state bed reactor with Fischer Tropsch waxes, cause expense
Hold in the palm iron content in synthetic wax, it is impossible to meet requirement (be no more than 5mg/kg) of the downstream hydrogenation device to charging iron content.
The content of the invention
Inside reactor temperature can be effectively controlled it is an object of the invention to provide one kind and improves space reactor profit
With the F- T synthesis and separator and method of rate.
For achieving the above object in a first aspect, the present invention uses following technical scheme：
A kind of F- T synthesis and separator, including paste state bed reactor, First Heat Exchanger, the second heat exchanger, the first mistake
Device and the second filter are filtered, the First Heat Exchanger is arranged in the paste state bed reactor and anti-positioned at the slurry bed system
The top of device is answered, second heat exchanger is arranged on outside the paste state bed reactor, and flowed into by slurry effuser and slurry
Pipe forms heat-exchanging loop with the paste state bed reactor bottom；
First filter is arranged in the paste state bed reactor and in the middle part of the paste state bed reactor
Position, is separated by filtration for treating the catalyst in the reaction product for drawing the paste state bed reactor；
Second filter is arranged on outside the paste state bed reactor, for being drawn to first filter
Filtrate be separated by filtration.
According to the F- T synthesis and separator of the present invention, it is preferable that the paste state bed reactor bottom is provided with gas point
Cloth device；One end of the slurry effuser is connected to the paste state bed reactor and is distributed positioned at first filter with gas
Position between device, the other end of the slurry effuser is connected to the charging aperture on the second heat exchanger top, and described
Slurry effuser is higher than the charging aperture of second heat exchanger with the link position of the paste state bed reactor；The slurry is flowed into
One end of pipe is connected to the position that the paste state bed reactor is located between the slurry effuser and gas distributor, the slurry
The other end that stream enters pipe is connected to the discharging opening of the second heat exchanger bottom, and the slurry flows into pipe and the slurry
The link position of bed reactor is less than the discharging opening of second heat exchanger, so as to be conducive to material in the paste state bed reactor
Circulation is formed between the second heat exchanger.It is further preferred that the slurry, which is flowed on pipe, is additionally provided with circulating pump, for making material
The forced circulation between the paste state bed reactor and the second heat exchanger, so as to control material in the paste state bed reactor
With the cycle rate between the second heat exchanger, and then the temperature in the paste state bed reactor is preferably adjusted, and set and follow
Ring pump forced circulation, which is also helped, prevents second heat exchanger by clogged up with material.
According to the F- T synthesis and separator of the present invention, it is preferable that the slurry effuser and the First Heat Exchanger
The distance between be the paste state bed reactor height 1/4-1/2, more preferably described paste state bed reactor height
1/4-1/3, research find, when be set between the slurry effuser and the First Heat Exchanger it is above-mentioned apart from when, can protect
The Temperature Distribution in reactor is preferably kept in card reactor while reaction compartment, local run aways are prevented.
In the present invention, because reactor lower part reacts more violent, it is preferable that second heat exchanger is provided with multigroup,
Such as 2-5 groups or 3-4 groups, are evenly arranged around the paste state bed reactor, to strengthen the effect for removing heat.
According to the F- T synthesis and separator of the present invention, first filter, which can be reduced, leaves the slurry bed system
The catalyst of the reaction product entrained with of reactor, it will be appreciated by those skilled in the art that the filtering of above-mentioned filter effect can be realized
Device has a variety of.Preferably, first filter includes one or more filtering pipe fittings, and the filtering pipe fitting includes outer mistake
Chimney filter, interior screen pipe, outer discharge nozzle and interior discharge nozzle, the interior screen pipe are arranged on inside the outer screen pipe, and institute
The filter opening diameter for stating interior screen pipe is less than the filter opening diameter of the outer screen pipe；The top of the outer screen pipe is provided with outer backwash
Mouthful, for introducing counter-flushing liquid into the outer screen pipe, the top of the interior screen pipe is provided with interior backwash mouth, for institute
State and counter-flushing liquid is introduced in interior screen pipe；The outer discharge nozzle is connected to the bottom of the outer screen pipe, described outer for drawing
Filtration product between screen pipe and interior screen pipe simultaneously sends the paste state bed reactor back to；The interior discharge nozzle is connected in described
The bottom of screen pipe, for drawing the filtration product in the interior screen pipe.It is further preferred that the filter is provided with more
Group, such as 3-12 groups or 5-8 groups, around the paste state bed reactor side, wall is evenly arranged, and every group of filter includes 3-30
Root, preferably 5-25 roots, more preferably 10-20 roots filter pipe fitting, to improve filtering rate.
According to the F- T synthesis and separator of the present invention, it is preferable that the bottom of the outer screen pipe is non-filtered section, example
As described non-filtered section it is of length no more than it is described it is outer filtering length of tube 1/2, the interior screen pipe be located at the non-filtered section
It is interior, it is this to can be designed so that institute be directly acted in the presence of inertia by filtering the reaction product entered through outer screen pipe
The surface of interior screen pipe is stated, but is flowed downward, is contacted in the bottom of the outer screen pipe with the interior screen pipe, due to reaction
Product is parallel with the filtering surface of the interior screen pipe, so that the catalyst granules for being attached to the interior filtering pipe surface is taken away,
Help to maintain filter opening unimpeded, improve filter efficiency.
According to the F- T synthesis and separator of the present invention, it is preferable that a diameter of 15-60 of filter opening of the outer screen pipe is micro-
Rice, percent opening is not less than 30%, and the filter opening of the interior screen pipe is a diameter of 1-10 microns, and percent opening is described outer not less than 60%
1.5 times of the diameter of screen pipe not less than the interior filtering pipe diameter；It is further preferred that the filter opening diameter of the outer screen pipe
For 20-50 microns, percent opening is not less than 35%；The filter opening of the interior screen pipe is a diameter of 2-8 microns, and percent opening is not less than
65%, 1.5-3 times of a diameter of interior filtering pipe diameter of the outer screen pipe；It is further preferred that the outer filtering
The filter opening of pipe is a diameter of 30-40 microns, and percent opening is 40-50%；The filter opening of the interior screen pipe is a diameter of 4-6 microns, perforate
Rate is 70-80%, 1.8-2.5 times of a diameter of interior filtering pipe diameter of the outer screen pipe.
According to the F- T synthesis and separator of the present invention, second filter includes at least one filter element,
The filter element includes head tank, mixing tank and filter；The discharging opening of the head tank and the discharging opening difference of mixing tank
The charging aperture of the filter is connected to by pipeline；The discharge outlet of the filter is respectively equipped with head tank circulation pipe, mixed
Batch can circulation pipe and discharge nozzle, the discharging opening of the filter are connected to the charging of the head tank by head tank circulation pipe
Mouthful, the discharging opening of the filter is connected to the charging aperture of the mixing tank by mixing tank circulation pipe；The discharge nozzle and institute
The discharging opening connection of filter is stated, for the qualified filtrate of the filter to be sent out.
According to the F- T synthesis and separator of the present invention, it is preferable that at least one described filter element is two mistakes
Filter unit, respectively by-pass filtration unit and secondary filtration unit；Wherein, the by-pass filtration unit is used for first mistake
The filtrate that filter device is drawn is separated by filtration, and the secondary filtration unit is used for the filtrate obtained to the by-pass filtration unit
It is separated by filtration.
In the present invention, it will be understood by those skilled in the art that the paste state bed reactor also includes material import and export, than
Such as it is located at the unstripped gas air inlet below gas distributor, the catalyst feeds above gas distributor, positioned at reaction
Top vent at the top of device and the slurry outlet positioned at reactor bottom etc., above-mentioned material import and export are set to this area
Know, repeat no more here.Preferably, reactor head exit is provided with anti-Vapor Entrainment separator, to separate exhaust
In solid, liquid phase.
Second aspect for achieving the above object, the present invention uses following technical scheme：
A kind of method for carrying out F- T synthesis using above-mentioned F- T synthesis and separator, methods described is using described
Paste state bed reactor carries out Fischer-Tropsch synthesis, and the heat on reactor top is removed using the First Heat Exchanger, second is utilized
Heat exchanger removes the heat of reactor lower part；The reaction for drawing the paste state bed reactor is treated using first filter
Catalyst in product is separated by filtration, and the filtrate drawn using second filter to first filter is entered
Row is separated by filtration.
Method in accordance with the invention it is preferred that first filter is drawn using second filter
The process that filtrate is separated by filtration comprises the following steps：
Step a, circulation solvent be well mixed with filter aid in the mixing tank, feeding filter, filtrate cycle time
To the mixing tank；The process is repeated, until forming a metafiltration cake outside the filter element of the filter, the batch mixing is cut out
Tank；
Step b, the slurries to be separated in the head tank are sent into the filter, filtrate cycle returns to the raw material
Tank；After the process is repeated until solid concentration is qualified in filtrate, sent out by the discharging opening of the filter.
It will be understood by those skilled in the art that in stepb, with the continuous progress of filter process, meeting on the filter cake
New filter residue is constantly enriched with, it is therefore preferred that in the running of the filter element, in addition it is also necessary to the mistake of the filter
Filter cake outside filtering element is cleared up, such as periodic cleaning, is either cleared up or according to filter cake thickness according to filter pressure
Clear up etc., then repeat step a and step b.It is further preferred that the circulation solvent is refined Fischer Tropsch waxes,
The filter aid is carclazyte and diatomite.Wherein, carclazyte be used for catalyst in step b filtration cycle in adsorption slurry and
Other solid impurities, and diatomite can then form certain flow channel and porosity in filter cake, and using refined
Fischer Tropsch waxes circulate the filter cake to be formed and are more beneficial for keeping stable in stepb.
One of the method according to the invention is preferably carried out mode, and second filter is provided with double-filtration list
Member, to realize double-filtration, wherein, the filtrate drawn using the by-pass filtration unit to first filter was carried out
Filter separation；With secondary filtration unit；It is used to enter the filtrate that the by-pass filtration unit is obtained using the secondary filtration unit
Row is separated by filtration.During with only with by-pass filtration, double-filtration is more beneficial for iron ion content during judging filtration cycle and reached
To the desired time, it is to avoid the product wax iron content caused by when the iron content of waxy stone raw material is fluctuated is exceeded.In addition, adopting
When using double-filtration, although grade one filter load is larger, the filtering load of secondary filter is relatively reduced, the use of filter cake
Life-span can extend, simultaneously because secondary filtration can select product wax during interval and two kinds of forms of continuous feed, filtration cycle
Index be easier control, and can with flexible modulation filtration cycle amount and adsorption time control two-stage load problem, realize
The long period steady running of device.
The method according to the invention, in step a and step d, filter operation temperature is preferably 150~200 DEG C, more excellent
Elect 170-180 DEG C as；In step a, forming the process of filter cake includes mass ratio being 1:4-1:10, more preferably 1:6-1:8
Diatomite and carclazyte mixture with circulation solvent mix to form filter cake to filter；In addition, in the by-pass filtration unit, institute
The solid content for stating diatomite and carclazyte mixture and the mixed serum of circulation solvent configuration is 6-10wt%, more preferably 7-
8wt%；In the secondary filtration unit, diatomite and the carclazyte mixture is consolidated with the mixed serum of circulation solvent configuration
Content is 0.1-4wt%, more preferably 0.2-2wt%, to improve filter effect.
Compared with prior art, the device that provides of the present invention is provided with the First Heat Exchanger that is built in reactor top and external
In the second heat exchanger of reactor lower part, in reactor lower part, fresh feed gas is contacted with catalyst, and it is reacted compared with reactor
Portion and top are more violent, are cooled by sending into reactor lower part slurries to exchange heat in the second external heat exchanger, and make reaction
The size circulations flowing of device bottom, can improve heat exchange efficiency, and be conducive to gas to be contacted with the uniform of catalyst, improve anti-
Answer efficiency；Portion and top reaction are more gentle in the reactor, and the heat of accumulation can be by slurries with being arranged on reactor
The First Heat Exchanger contact in portion is removed, and improves space reactor utilization rate, meanwhile, slurries after cooling through First Heat Exchanger by
It in density increase, further can downwards backflow, so as to be conducive to gas to be contacted with the uniform of catalyst, improve reaction efficiency.
In addition, the filtering pipe fitting of the first filter of the present invention is longitudinally arranged at the middle part of reactor, it can reduce
Obstruction to pulp flow in reactor, while the slurry of longitudinal flow can also effectively remove consolidating for filtering pipe fitting surface attachment
Body obturator, improves filter efficiency.
In addition, in the second filter of the present invention, what powder or irony catalyst in waxy stone were formed in step a
Filter cake surface and inside are trapped under the double action of absorption and the interception of filter cake, and further effect is filtered in raising by circulation
Clarified after fruit, and if using traditional direct filter type, such as the slurries added with filter aid directly are passed through into mistake
Filter, in order to realize the trickle powder removed in slurries, it has to using the minimum filter in filter opening aperture, easily block, separately
Outer filter aid equally exists the filtering of an adsorption equilibrium, therefore directly filters the filtering effect for the application claims being difficult to
Really.
Brief description of the drawings
Fig. 1 is the F- T synthesis of the present invention and the structural representation of separator；
Fig. 2 is the structural representation of filtering pipe fitting in Fig. 1；
Fig. 3 is the schematic diagram of the second filter of the present invention.
Embodiment
Below in conjunction with accompanying drawing, the present invention is described in detail, but the present invention is not limited only to this.
As shown in figure 1, the F- T synthesis that the present invention is provided includes paste state bed reactor 1, First Heat Exchanger with separator
2nd, the second heat exchanger 3, the first filter 9 and the second filter 11, wherein, the First Heat Exchanger 2 is arranged at the slurry
In state bed reactor 1 and positioned at the top of the paste state bed reactor 1, for removing the top of paste state bed reactor 1
Heat.
Second heat exchanger 3 is arranged on outside the paste state bed reactor 1, and is flowed into by slurry effuser 31 and slurry
Pipe 32 forms heat-exchanging loop with the bottom of paste state bed reactor 1.Preferably, the bottom of paste state bed reactor 1 is provided with gas
Distributor 4, for making unstrpped gas be uniformly distributed in the paste state bed reactor 1, the gas distributor 4 can be ability
Any one in the conventional gas distributor in domain or its improved form, such as be introduced directly into type or the distribution of dividing plate profile gas
Device；One end of the slurry effuser 31 is connected to the paste state bed reactor 1 positioned at first filter 9 and gas point
Position between cloth device 4, the other end of the slurry effuser 31 is connected to the charging aperture on the top of the second heat exchanger 3, and
And the slurry effuser 31 is higher than the charging aperture of second heat exchanger 3 with the link position of the paste state bed reactor 1, with
The material in the paste state bed reactor 1 is set to enter in second heat exchanger 3；One end that the slurry flows into pipe 32 connects
The position that the paste state bed reactor 1 is located between the slurry effuser 31 and gas distributor 4 is connected to, the slurry is flowed into
The other end of pipe 32 is connected to the discharging opening of the bottom of the second heat exchanger 3, and the slurry flows into pipe 32 and the slurry
The link position of bed reactor 1 is less than the discharging opening of second heat exchanger 3, so that the material after cooling returns to institute
State paste state bed reactor 1.Because the temperature of the material in reactor 1 is higher than the temperature of second heat exchanger 3, material is because of temperature
Difference forms density contrast, so as to be conducive to material to form circulation between the heat exchanger 3 of paste state bed reactor 1 and second.
In the present invention, it will be understood by those skilled in the art that the heat exchanger 3 of the First Heat Exchanger 2 and second has no spy
It is different to require, it can be any one in the conventional heat exchanger in this area or its improved form, repeat no more here.
In a preferred embodiment, the slurry effuser 31 or slurry flow on pipe 32 and are additionally provided with circulating pump (in figure
It is not shown), for making material forced circulation between the heat exchanger 3 of paste state bed reactor 1 and second, by being followed described in control
Ring pump, so as to cycle rate of the control material between the heat exchanger 3 of paste state bed reactor 1 and second, and then more preferably
Ground adjusts the temperature in the paste state bed reactor 1, and setting circulating pump forced circulation to also help prevents described second to change
Hot device 3 is blocked by slurry.
In the present invention, it will be understood by those skilled in the art that the paste state bed reactor 1 is additionally provided with material import and export,
Such as it is located at the unstripped gas air inlet 7 of the lower section of gas distributor 4, the catalyst feeds 8 above gas distributor 4, position
In the top vent 5 at the top of reactor 1 and slurry outlet 6 positioned at the bottom of reactor 1 etc., above-mentioned material import and export is set
It is set to it is known in the art that repeating no more here.
In the present invention, forming gas enters in reactor 1 from raw material air inlet 7, by gas distributor 4 in reactor
It is uniformly dispersed, and is contacted in uphill process with the catalyst granules introduced through catalyst feeds 8 in slurry in 1, so that
Generate the reaction product containing liquid hydrocarbon.The heat exchanger 3 of First Heat Exchanger 2 and second is passed through by Fischer-Tropsch synthesis liberated heat
Remove, in the bottom of reactor 1, fresh feed gas is contacted with catalyst, it reacts more violent compared with the middle part of reactor 1 and top,
Therefore, the lower slurry of reactor 1 is sent into heat exchange in the second external heat exchanger 3 to cool, and follows the slurry of the bottom of reactor 1
Circulation is moved, and improves heat exchange efficiency, and is conducive to gas to be contacted with the uniform of catalyst, improves reaction efficiency；Preferably, it is described
Second heat exchanger 3 is provided with multigroup, such as 2-5 groups or 3-4 groups, is evenly arranged around the paste state bed reactor 1, to strengthen drop
Temp effect.Because portion and top reaction are more gentle in reactor 1, therefore the heat of accumulation can pass through First Heat Exchanger 2
Contact is removed, and improves the space availability ratio of reactor 1.Preferably, between the slurry effuser 31 and the First Heat Exchanger 2
Distance be the height of paste state bed reactor 1 1/4-1/2, the 1/ of the more preferably described height of paste state bed reactor 1
4-1/3.In addition, the slurries after cooling through First Heat Exchanger 1 further can be backflowed downwards, so as to be conducive to due to density increase
Gas is contacted with the uniform of catalyst, improves reaction efficiency.Meanwhile, the slurry of the bottom deposit of reactor 1 can pass through reactor 1
The slurry outlet 6 of bottom is discharged；The remaining reacted device top vent 5 of gas is drawn after reaction, it is preferable that the slurry
Anti- Vapor Entrainment separator 10 is provided with bed reactor head exhaust outlet 5, to separate the solid, liquid phase in exhaust.
First filter sets 9 in the paste state bed reactor 1 and in the middle part of the paste state bed reactor
Position, be separated by filtration for treating the catalyst in the reaction product for drawing the paste state bed reactor 1.Such as Fig. 2 institutes
Show, in a preferred embodiment, first filter 9 includes one or more filtering pipe fittings, the filtering pipe fitting bag
Outer screen pipe 91, interior screen pipe 92, outer discharge nozzle 93 and interior discharge nozzle 94 are included, the interior screen pipe 92 is arranged on the outer filtering
Inside pipe 91, and filter opening diameter of the filter opening diameter less than the outer screen pipe 91 of the interior screen pipe 92；The outer mistake
The top of chimney filter 91 is provided with outer backwash mouth 911, for introducing counter-flushing liquid, the interior screen pipe into the outer screen pipe 91
92 top is provided with interior backwash mouth 921, for introducing counter-flushing liquid into the interior screen pipe 92；The outer discharge nozzle 93 connects
The bottom of the outer screen pipe 91 is connected to, for drawing the filtration product between the outer screen pipe 91 and interior screen pipe 92；Institute
The bottom that interior discharge nozzle 94 is connected to the interior screen pipe 92 is stated, for drawing the filtration product in the interior screen pipe 92.It is excellent
Selection of land, the filter opening of the outer screen pipe 91 is a diameter of 15-60 microns, and percent opening is not less than 30%, the filter of the interior screen pipe 92
Bore dia is 1-10 microns, and percent opening is not less than 60%, and the diameter of the outer screen pipe 91 is straight not less than the interior screen pipe 92
1.5 times of footpath；It is further preferred that the filter opening of the outer screen pipe 91 is a diameter of 20-50 microns, percent opening is not less than 35%；
The filter opening of the interior screen pipe 92 is a diameter of 2-8 microns, and percent opening is not less than 65%, the outer screen pipe 91 it is a diameter of described
1.5-3 times of the interior diameter of screen pipe 92；It is further preferred that the filter opening of the outer screen pipe 91 is a diameter of 30-40 microns, open
Porosity is 40-50%；The filter opening of the interior screen pipe 92 is a diameter of 4-6 microns, and percent opening is 70-80%, the outer screen pipe
1.8-2.5 times of 91 a diameter of interior diameter of screen pipe 92.
In the reactor 1 of the present invention, reaction product to be drawn largely is urged through the outer filtering and removing of screen pipe 91
Enter after agent in outer screen pipe 91, it is further tiny through the interior filtering and removing of screen pipe 92 in the outer screen pipe 91
Drawn after catalyst granules through the interior discharge nozzle 94, remaining material is through institute between the outer screen pipe 91 and interior screen pipe 92
State outer discharge nozzle 93 to draw, storage tank can be further fed into or returned in the paste state bed reactor 1.By treating the anti-of extraction
Answer product to carry out double-filtration, can effectively prevent that filter opening from blocking, improve filter efficiency, be particularly suitable for the slurry bed system of the present invention
Reactor.In addition, the filtering pipe fitting of the present invention can also periodically be drawn using the outer backwash mouth 911 and interior backwash mouth 921
Enter flushing liquor to backwash the outer screen pipe 91 and interior screen pipe 92, to reduce filtration resistance.
In a preferred embodiment of the filtering pipe fitting of the present invention, the bottom of the outer screen pipe 91 is non-filtered section
912 (parts for being not provided with filter opening), it is preferable that the length of the non-filtered section 912 is the length of the outer screen pipe 91
1/3-1/2, the interior screen pipe 92 is located in non-filtered section 912.This can be designed so that is filtered through outer screen pipe 91
The reaction product of entrance will not directly act on the surface of the interior screen pipe 92 in the presence of inertia, but flow downward,
Contacted in the bottom of the outer screen pipe 91 with the interior screen pipe 92, due to flow direction and the interior filtering of reaction product
The filtering surface of pipe 92 is parallel, so as to take away the catalyst granules for being attached to the surface of interior screen pipe 92, helps to protect
Hold filter opening unimpeded, improve filter efficiency.It is further preferred that first filter 9 is provided with multigroup, such as 3-12 groups,
Or 5-8 groups, it is evenly arranged around the inwall of paste state bed reactor 1, every group of first filter 9 includes 3-30 roots, preferably 5-
25, more preferably 10-20 roots filter pipe fitting, to improve filtering rate.
Second filter 11 is arranged on outside the paste state bed reactor 1, for first filter 9
The filtrate of extraction is separated by filtration.In one embodiment of the invention, second filter 11 includes at least one
Individual filter element, it is preferable that as shown in figure 3, at least one described filter element is two filter elements, respectively one-level mistake
Unit 12 and secondary filtration unit 13 are filtered, the by-pass filtration unit 12 includes one-level head tank 121, the and of one-level mixing tank 122
Grade one filter 123；The discharging opening of the one-level head tank 121 and the discharging opening of one-level mixing tank 122 are connected by pipeline respectively
It is connected to the charging aperture of the grade one filter 123；The discharge outlet of the grade one filter 123 is respectively equipped with one-level head tank and followed
Endless tube 124, one-level mixing tank circulation pipe 125 and one-level discharge nozzle 126, the discharging opening of the grade one filter 123 pass through one-level
Head tank circulation pipe 124 is connected to the charging aperture of the one-level head tank 121, and the discharging opening of the grade one filter 123 passes through
One-level mixing tank circulation pipe 125 is connected to the charging aperture of the one-level mixing tank 122；The one-level discharge nozzle 126 and described one
The discharging opening connection of level filter 123, for the qualified filtrate of the grade one filter 123 to be sent out.
The secondary filtration unit 13 includes secondary raw materials tank 131, two grades of mixing tanks 132 and secondary filter 133；It is described
The charging aperture of secondary raw materials tank 131 is connected to the discharging opening of the grade one filter 123, institute by the one-level discharge nozzle 126
The discharging opening of the discharging opening and two grades of mixing tanks 132 of stating secondary raw materials tank 131 is connected to the secondary filtration by pipeline respectively
The charging aperture of device 133；The discharge outlet of the secondary filter 133 is respectively equipped with secondary raw materials tank circulation pipe 134, two grades of batch mixings
Tank circulation pipe 135 and two grades of discharge nozzles 136, the discharging opening of the secondary filter 133 are connected by secondary raw materials tank circulation pipe 134
The charging aperture of the secondary raw materials tank 131 is connected to, the discharging opening of the secondary filter 133 passes through two grades of mixing tank circulation pipes
135 are connected to the charging aperture of two grades of mixing tanks 132；The discharging of two grades of discharge nozzles 136 and the secondary filter 133
Mouth connection, for the qualified filtrate of the secondary filter 133 to be sent out.
During operation, the method for operation of the by-pass filtration unit 12 is as follows：The first step, will circulation solvent and filter aid in institute
State in one-level mixing tank 122 and be well mixed, send into grade one filter, filtrate cycle returns to the one-level mixing tank 122；Repeating should
Process, until forming a metafiltration cake outside the filter element of the grade one filter 123, cuts out the one-level mixing tank 122, that is, follows
Ring solvent is returned to after one-level mixing tank 122, stops the Matter Transfer between the one-level mixing tank 122 and grade one filter 123.
Second step and then the slurries to be separated in the one-level head tank 121 are sent into the grade one filter 123, filtrate cycle is returned
To the one-level head tank 121；After the process is repeated until solid concentration is qualified in filtrate, pass through the grade one filter 123
Discharging opening send out.The filtrate that the secondary filtration unit 13 is used to obtain the by-pass filtration unit 12 carries out filtering point
From its method of operation is with the by-pass filtration unit 12.
It will be understood by those skilled in the art that in second step, with the continuous progress of filter process, meeting on the filter cake
New filter residue is constantly enriched with, it is therefore preferred that in the running of the by-pass filtration unit 12, in addition it is also necessary to the one-level
Filter cake outside the filter element of filter 123 is cleared up, such as periodic cleaning, or is cleared up according to filter pressure, or
Person clears up etc. according to filter cake thickness, then repeatedly the first step and second step.
Preferably, the circulation solvent is refined Fischer Tropsch waxes, and the filter aid is carclazyte and diatomite；Filter
150~200 DEG C, preferably 170-180 DEG C of operation temperature；In the first step and second step, forming the process of filter cake is included matter
Amount is than being 1:4-1:10, preferably 1:6-1:8 diatomite and carclazyte mixture mixes to form filter cake to filter with circulation solvent.
It is further preferred that in the by-pass filtration unit 12, diatomite and the carclazyte mixture is mixed with circulation solvent configuration
The solid content for closing slurries is 6-10wt%, preferably 7-8wt%；In the secondary filtration unit 13, the diatomite and white
The solid content of earth mixtures and the mixed serum of circulation solvent configuration is 0.1-4wt%, preferably 0.2-2wt%.
Claims (14)
1. a kind of F- T synthesis and separator, including paste state bed reactor, First Heat Exchanger, the second heat exchanger, the first filtering
Device and the second filter, the First Heat Exchanger are arranged in the paste state bed reactor and positioned at the slurry reactor
The top of device, second heat exchanger is arranged on outside the paste state bed reactor, and flows into pipe by slurry effuser and slurry
Heat-exchanging loop is formed with the paste state bed reactor bottom；
First filter is arranged on the position in the paste state bed reactor and in the middle part of the paste state bed reactor,
It is separated by filtration for treating the catalyst in the reaction product for drawing the paste state bed reactor；
Second filter is arranged on outside the paste state bed reactor, for the filter drawn to first filter
Liquid is separated by filtration；
First filter include one or more filtering pipe fittings, the filtering pipe fitting include outer screen pipe, interior screen pipe,
Outer discharge nozzle and interior discharge nozzle, the interior screen pipe are arranged on inside the outer screen pipe, and the filter opening of the interior screen pipe
Diameter is less than the filter opening diameter of the outer screen pipe；The top of the outer screen pipe is provided with outer backwash mouth, for described outer
Counter-flushing liquid is introduced in screen pipe, the top of the interior screen pipe is provided with interior backwash mouth, for drawing into the interior screen pipe
Enter counter-flushing liquid；The outer discharge nozzle is connected to the bottom of the outer screen pipe, for drawing the outer screen pipe and interior filtering
Filtration product between pipe simultaneously sends the paste state bed reactor back to；The interior discharge nozzle is connected to the bottom of the interior screen pipe,
For drawing the filtration product in the interior screen pipe；
The paste state bed reactor also includes the top vent and the slurry outlet positioned at bottom positioned at top.
2. F- T synthesis according to claim 1 and separator, it is characterised in that the paste state bed reactor bottom is set
There is gas distributor；One end of the slurry effuser be connected to the paste state bed reactor positioned at first filter with
Position between gas distributor, the other end of the slurry effuser is connected to the charging aperture on the second heat exchanger top,
And the slurry effuser is higher than the charging aperture of second heat exchanger with the link position of the paste state bed reactor；It is described
One end that slurry flows into pipe is connected to the position that the paste state bed reactor is located between the slurry effuser and gas distributor
Put, the other end of the slurry inflow pipe is connected to the discharging opening of the second heat exchanger bottom, and the slurry flows into pipe
It is less than the discharging opening of second heat exchanger with the link position of the paste state bed reactor.
3. F- T synthesis according to claim 2 and separator, it is characterised in that the slurry effuser and described the
The distance between one heat exchanger is the 1/4-1/2 of the paste state bed reactor height.
4. F- T synthesis according to claim 1 and separator, it is characterised in that the bottom of the outer screen pipe is non-
Fillter section, the interior screen pipe is located in non-filtered section.
5. F- T synthesis according to claim 4 and separator, it is characterised in that the filter opening diameter of the outer screen pipe
For 15-60 microns, percent opening is not less than 30%, and the filter opening of the interior screen pipe is a diameter of 1-10 microns, and percent opening is not less than
60%, 1.5-3 times of a diameter of interior filtering pipe diameter of the outer screen pipe.
6. F- T synthesis according to claim 1 and separator, it is characterised in that second filter is included extremely
A few filter element, the filter element includes head tank, mixing tank and filter；The discharging opening and batch mixing of the head tank
The discharging opening of tank is connected to the charging aperture of the filter by pipeline respectively；The discharge outlet of the filter is respectively equipped with original
Batch can circulation pipe, mixing tank circulation pipe and discharge nozzle, the discharging opening of the filter are connected to described by head tank circulation pipe
The charging aperture of head tank, the discharging opening of the filter is connected to the charging aperture of the mixing tank by mixing tank circulation pipe；Institute
The discharging opening that discharge nozzle is stated with the filter is connected, for the qualified filtrate of the filter to be sent out.
7. F- T synthesis according to claim 6 and separator, it is characterised in that at least one described filter element
For two filter elements, respectively by-pass filtration unit and secondary filtration unit；Wherein, the secondary filtration unit is used for institute
The filtrate that by-pass filtration unit obtains is stated to be separated by filtration.
8. F- T synthesis and separator according to any one of claim 1-5, it is characterised in that second heat exchange
Device is provided with 2-5 groups, is evenly arranged around the paste state bed reactor；
First filter is provided with 3-12 groups, and around the paste state bed reactor side, wall is evenly arranged, every group of filter bag
Include 3-30 roots filtering pipe fitting.
9. F- T synthesis according to claim 1 and separator, it is characterised in that the top of the paste state bed reactor
Exit is provided with anti-Vapor Entrainment separator, and the slurry flows on pipe and is provided with circulating pump, for making material in the slurry
Forced circulation between state bed reactor and the second heat exchanger.
10. a kind of method that F- T synthesis using any one of claim 1-9 carries out F- T synthesis with separator,
Methods described carries out Fischer-Tropsch synthesis using the paste state bed reactor, and reactor is removed using the First Heat Exchanger
The heat on top, the heat of reactor lower part is removed using the second heat exchanger；Extraction institute is treated using first filter
The catalyst stated in the reaction product of paste state bed reactor is separated by filtration, using second filter to described first
The filtrate that filter is drawn is separated by filtration.
11. method according to claim 10, it is characterised in that it is single that second filter includes at least one filtering
Member, the filter element includes head tank, mixing tank and filter；The discharging opening of the head tank and the discharging opening of mixing tank point
The charging aperture of the filter is not connected to by pipeline；The discharge outlet of the filter be respectively equipped with head tank circulation pipe,
Mixing tank circulation pipe and discharge nozzle, the discharging opening of the filter are connected to the charging of the head tank by head tank circulation pipe
Mouthful, the discharging opening of the filter is connected to the charging aperture of the mixing tank by mixing tank circulation pipe；The discharge nozzle and institute
The discharging opening connection of filter is stated, for the qualified filtrate of the filter to be sent out；
The process that the filtrate drawn using second filter to first filter is separated by filtration is included such as
Lower step：
Step a, circulation solvent is well mixed with filter aid in the mixing tank, feeding filter, filtrate cycle returns to institute
State mixing tank；The process is repeated, until forming a metafiltration cake outside the filter element of the filter, the mixing tank is cut out；
Step b, the slurries to be separated in the head tank are sent into the filter, filtrate cycle returns to the head tank；Weight
After the multiple process is until solid concentration is qualified in filtrate, sent out by the discharging opening of the filter.
12. method according to claim 11, it is characterised in that in stepb, to the filter filter element outside
Filter cake is cleared up, then repeat step a and step b.
13. method according to claim 12, it is characterised in that at least one described filter element is that two filterings are single
Member, respectively by-pass filtration unit and secondary filtration unit；
The filtrate drawn using the by-pass filtration unit to first filter is separated by filtration；Utilize described two grades
Filter element is used to be separated by filtration the filtrate that the by-pass filtration unit is obtained.
14. the method according to any one of claim 11-13, it is characterised in that the circulation solvent takes for refined
Synthetic wax is held in the palm, the filter aid is carclazyte and diatomite；150~200 DEG C of filter operation temperature；
In step a, forming the process of filter cake includes mass ratio being 1:4-1:10 diatomite and carclazyte mixture and circulation
Solvent mixing to form filter cake to filter.
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| WO2017207299A1 (en) * | 2016-06-02 | 2017-12-07 | L'Air Liquide Société Anonyme pour l'Etude et l'Exploitation des Procédés Georges Claude | Slurry bubble column reactor for a fischer-tropsch process |
| CN107254327B (en) * | 2017-06-05 | 2021-12-17 | 中石化宁波工程有限公司 | Fischer-Tropsch synthetic oil process |
| CN109762600A (en) * | 2017-11-09 | 2019-05-17 | 陕西未来能源化工有限公司 | A kind of Low Temperature Fischer Tropsch synthesis paraffin classification cycle filtration system |
| CN111991905A (en) * | 2020-07-30 | 2020-11-27 | 国家能源集团宁夏煤业有限责任公司 | Method and device for solid-liquid separation of slurry discharged from slurry bed |
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| CA2154184C (en) * | 1993-01-28 | 2004-03-23 | Erling Rytter | Solid/liquid slurry treatment apparatus and catalytic multi-phase reactor |
| CN1822896A (en) * | 2003-07-15 | 2006-08-23 | 萨索尔技术(控股)有限公司 | Process for separating a catalyst from a liquid |
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| CN204724145U (en) * | 2015-05-15 | 2015-10-28 | 神华集团有限责任公司 | A kind of F-T synthesis and separator |
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| CN101396647B (en) * | 2007-09-29 | 2011-03-16 | 中科合成油技术有限公司 | Gas-liquid-solid three-phase suspended bed reactor for f-t synthesis and use thereof |
| BRPI1011148C8 (en) * | 2009-06-05 | 2018-12-18 | Solvay | process for separating liquid from a multiphase mixture contained in a vessel, use of the process, and process for the preparation of hydrogen peroxide. |
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| CA2154184C (en) * | 1993-01-28 | 2004-03-23 | Erling Rytter | Solid/liquid slurry treatment apparatus and catalytic multi-phase reactor |
| CN1822896A (en) * | 2003-07-15 | 2006-08-23 | 萨索尔技术(控股)有限公司 | Process for separating a catalyst from a liquid |
| CN101036865A (en) * | 2007-01-31 | 2007-09-19 | 华东理工大学 | Slurry bubble columun reactor having internal circulation and external heat-exchanging and the application |
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