CN104888668A - Fischer-Tropsch synthesis and separation device and method - Google Patents
Fischer-Tropsch synthesis and separation device and method Download PDFInfo
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- CN104888668A CN104888668A CN201510247572.4A CN201510247572A CN104888668A CN 104888668 A CN104888668 A CN 104888668A CN 201510247572 A CN201510247572 A CN 201510247572A CN 104888668 A CN104888668 A CN 104888668A
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Abstract
The invention discloses a Fischer-Tropsch synthesis and separation device, which consists of a slurry bed reactor, a first heat exchanger, a second heat exchanger, a first filter apparatus and a second filter apparatus. The first heat exchanger is disposed on the upper part of the reactor internally, the second heat exchanger is arranged outside the slurry bed reactor, the first filter apparatus is arranged at the middle part of the reactor internally, and the second filter apparatus is disposed outside the slurry bed reactor. The invention also discloses a method of Fischer-Tropsch synthesis and separation with the device. According to the invention, the slurry at the lower part of the reactor is sent into the external second heat exchanger to conduct heat exchange cooling, and the slurry at the lower part of the reactor flows circularly, so that the heat exchange efficiency is improved. Also, at the upper part of the reactor, as the reactions at the middle part and the upper part are mild, the accumulated heat is removed by first heat exchanger contact, and the reactor space utilization is enhanced. Because of density increase, the slurry cooled by the first heat exchanger can flow back further downward, thereby being conducive to further improvement of the reaction efficiency.
Description
Technical field
The present invention relates to F-T synthesis field, particularly a kind of F-T synthesis and the device and method be separated.
Background technology
Along with the minimizing day by day of petroleum resources; and the mankind are to the increasingly stringent required of preserving the ecological environment; the demand of the world to cleaning liquid fluid fuel sharply increases; in order to meet this demand; various countries' researcher is devoted to research and development clean fuel oil production technology, wherein attracts most attention with Fischer-Tropsch (Fischer-Tropsch) synthetic technology.Typical fischer-tropsch synthesis process flow process is: first, the gasification of coal/natural gas via or partial oxidation, reforming be synthesis gas, again by after synthetic gas desulfurization, deoxidizing purification, according to the fischer-tropsch synthesis process condition adopted and catalyst, adjustment H/CO ratio, then enters Fischer-Tropsch synthesis device and produces hydrocarbon mixture.Finally, synthetic product can obtain different target product after being separated processing upgrading.
Fischer-Tropsch synthesis device is the core of F-T synthesis technology, because F-T synthesis is strong exothermal reaction, must in time reaction heat be removed in course of reaction, otherwise, just easily there is hot localised points in catalyst, causes its rapid deactivation and reduce the selective of long chain alkane product; In addition, the bed of paste state bed reactor is in three-phase turbulence state, catalyst can collide and rub with reactor wall, reactor inner member and catalyst particles intergranular in reactor, inevitably be broken and efflorescence, cause occurring that such as particle diameter is lower than the powder of 5 μm, these powder can flow out paste state bed reactor with Fischer Tropsch waxes, cause iron content in Fischer Tropsch waxes, cannot meet the requirement (be no more than 5mg/kg) of downstream hydrogenation device to charging iron content.
Summary of the invention
The object of the present invention is to provide and a kind ofly can effectively control inside reactor temperature and improve the F-T synthesis of space reactor utilization rate and separator and method.
First aspect for achieving the above object, the present invention by the following technical solutions:
A kind of F-T synthesis and separator, comprise paste state bed reactor, First Heat Exchanger, the second heat exchanger, the first filter and the second filter, described First Heat Exchanger to be arranged in described paste state bed reactor and to be positioned at the top of described paste state bed reactor, described second heat exchanger is arranged on outside described paste state bed reactor, and forms heat-exchanging loop by slurry effuser and slurry inflow pipe and described paste state bed reactor bottom;
Described first filter is arranged in described paste state bed reactor and the position be positioned in the middle part of described paste state bed reactor, carries out isolated by filtration for the catalyst treated in the product of drawing described paste state bed reactor;
It is outside that described second filter is arranged on described paste state bed reactor, carries out isolated by filtration for the filtrate of drawing described first filter.
According to F-T synthesis of the present invention and separator, preferably, described paste state bed reactor bottom is provided with gas distributor; One end of described slurry effuser is connected to the position of described paste state bed reactor between described first filter and gas distributor, the other end of described slurry effuser is connected to the charging aperture on described second heat exchanger top, and the link position of described slurry effuser and described paste state bed reactor is higher than the charging aperture of described second heat exchanger; One end of described slurry inflow pipe is connected to the position of described paste state bed reactor between described slurry effuser and gas distributor, the other end of described slurry inflow pipe is connected to the discharging opening of described second heat exchanger bottom, and the link position of described slurry inflow pipe and described paste state bed reactor is lower than the discharging opening of described second heat exchanger, thus is conducive to material and is formed between described paste state bed reactor and the second heat exchanger and circulate.Further preferably, described slurry inflow pipe is also provided with circulating pump, for making material forced circulation between described paste state bed reactor and the second heat exchanger, thus the cycle rate of material between described paste state bed reactor and the second heat exchanger can be controlled, and then regulate temperature in described paste state bed reactor better, and circulating pump forced circulation is set also helps and prevent described second heat exchanger by clogged up with material.
According to F-T synthesis of the present invention and separator, preferably, distance between described slurry effuser and described First Heat Exchanger is the 1/4-1/2 of described paste state bed reactor height, the more preferably 1/4-1/3 of described paste state bed reactor height, research finds, when being set to above-mentioned distance between described slurry effuser and described First Heat Exchanger, in the Temperature Distribution ensureing to keep better while reaction compartment in reactor in reactor, local run aways can be prevented.
In the present invention, because reactor lower part reaction is comparatively violent, preferably, described second heat exchanger is provided with many groups, and such as 2-5 group or 3-4 group, be evenly arranged around described paste state bed reactor, to strengthen the effect removing heat.
According to F-T synthesis of the present invention and separator, described first filter can reduce the catalyst of the product entrained with leaving described paste state bed reactor, it will be appreciated by those skilled in the art that the filter that can realize above-mentioned filter effect has multiple.Preferably, described first filter comprises one or more filtration pipe fitting, described filtration pipe fitting comprises outer screen pipe, inner filtration pipe, outer discharge nozzle and interior discharge nozzle, described inner filtration pipe is arranged on described outer screen pipe inside, and the filter opening diameter of described inner filtration pipe is less than the filter opening diameter of described outer screen pipe; The top of described outer screen pipe is provided with outer backwash mouth, and for introducing counter-flushing liquid in described outer screen pipe, the top of described inner filtration pipe is provided with interior backwash mouth, for introducing counter-flushing liquid in described inner filtration pipe; Described outer discharge nozzle is connected to the bottom of described outer screen pipe, sends described paste state bed reactor back to for the filtration product of drawing between described outer screen pipe and inner filtration pipe; Described interior discharge nozzle is connected to the bottom of described inner filtration pipe, for drawing the filtration product in described inner filtration pipe.Further preferably, described filter is provided with many groups, such as 3-12 group or 5-8 group, is evenly arranged around described paste state bed reactor sidewall, and often organize filter and comprise 3-30 root, preferred 5-25 root, more preferably 10-20 root filters pipe fitting, to improve filtering rate.
According to F-T synthesis of the present invention and separator, preferably, the bottom of described outer screen pipe is non-filtered section, the such as length of described non-filtered section is no more than 1/2 of described outer screen pipe length, described inner filtration pipe is positioned at described non-filtered section, this design can make to filter through outer screen pipe the surface that the product that enters can not directly act on described inner filtration pipe under the effect at inertia, but flow downward, contact with described inner filtration pipe in the bottom of described outer screen pipe, because product is parallel with the filtering surface of described inner filtration pipe, thus take away the catalyst granules being attached to described inner filtration tube-surface, contribute to keeping filter opening unimpeded, improve filter efficiency.
According to F-T synthesis of the present invention and separator, preferably, the filter opening diameter of described outer screen pipe is 15-60 micron, percent opening is not less than 30%, the filter opening diameter of described inner filtration pipe is 1-10 micron, percent opening is not less than 60%, and the diameter of described outer screen pipe is not less than 1.5 times of described inner filtration pipe diameter; Further preferably, the filter opening diameter of described outer screen pipe is 20-50 micron, and percent opening is not less than 35%; The filter opening diameter of described inner filtration pipe is 2-8 micron, and percent opening is not less than 65%, and the diameter of described outer screen pipe is 1.5-3 times of described inner filtration pipe diameter; Still more preferably, the filter opening diameter of described outer screen pipe is 30-40 micron, and percent opening is 40-50%; The filter opening diameter of described inner filtration pipe is 4-6 micron, and percent opening is 70-80%, and the diameter of described outer screen pipe is 1.8-2.5 times of described inner filtration pipe diameter.
According to F-T synthesis of the present invention and separator, described second filter comprises at least one filter element, and described filter element comprises head tank, mixing tank and filter; The discharging opening of described head tank and the discharging opening of mixing tank are connected to the charging aperture of described filter respectively by pipeline; The discharge outlet of described filter is respectively equipped with head tank circulation pipe, mixing tank circulation pipe and discharge nozzle, the discharging opening of described filter is connected to the charging aperture of described head tank by head tank circulation pipe, the discharging opening of described filter is connected to the charging aperture of described mixing tank by mixing tank circulation pipe; Described discharge nozzle is connected with the discharging opening of described filter, for the qualified filtrate of described filter being sent.
According to F-T synthesis of the present invention and separator, preferably, at least one described filter element is two filter elements, is respectively single filter unit and cascade filtration unit; Wherein, the filtrate that described single filter unit is used for described first filter is drawn carries out isolated by filtration, and described cascade filtration unit is used for carrying out isolated by filtration to the filtrate that described single filter unit obtains.
In the present invention, it will be appreciated by those skilled in the art that, described paste state bed reactor also comprises material import and export, such as be positioned at the unstripped gas air inlet below gas distributor, be positioned at catalyst feeds above gas distributor, be positioned at the top vent of reactor head and be positioned at the slurry outlet etc. of reactor bottom, being set to of above-mentioned material import and export is well known, repeats no more here.Preferably, reactor head exit is provided with anti-Vapor Entrainment separator, to isolate the solid, liquid phase in exhaust.
Second aspect for achieving the above object, the present invention by the following technical solutions:
A kind of method utilizing above-mentioned F-T synthesis and separator to carry out F-T synthesis, described method comprises and utilizes described paste state bed reactor to carry out Fischer-Tropsch synthesis, utilize described First Heat Exchanger to remove the heat on reactor top, utilize the second heat exchanger to remove the heat of reactor lower part; The catalyst utilizing described first filter to treat in the product of drawing described paste state bed reactor carries out isolated by filtration, utilizes described second filter to carry out isolated by filtration to the filtrate that described first filter is drawn.
According to method of the present invention, preferably, described second filter is utilized to comprise the steps: the process that the filtrate that described first filter is drawn carries out isolated by filtration
Step a, mixed in described mixing tank with filter aid by circulating solvent, send into filter, filtrate cycle gets back to described mixing tank; Repeat this process, until form one deck filter cake outside the filter element of described filter, cut out described mixing tank;
Step b, the slurries to be separated in described head tank are sent into described filter, filtrate cycle gets back to described head tank; Repeat this process until in filtrate solid concentration qualified after, sent by the discharging opening of described filter.
It will be appreciated by those skilled in the art that, in stepb, along with constantly carrying out of filter process, the filter residue that on described filter cake, the continuous enrichment of meeting is new, therefore, preferably, in the running of described filter element, also need to clear up the filter cake outside the filter element of described filter, such as periodic cleaning, or clear up according to filter pressure, or clear up etc. according to filter cake thickness, then repeat step a and step b.Further preferably, described circulating solvent is refining Fischer Tropsch waxes, and described filter aid is carclazyte and diatomite.Wherein, carclazyte is for the catalyst in the filtration cycle of step b in adsorption slurry and other solid impurity, diatomite then can form certain flow channel and porosity in filter cake, and the filter cake utilizing refining Fischer Tropsch waxes circulation to be formed more is conducive to keeping stable in stepb.
According to one of method of the present invention preferably embodiment, described second filter is provided with double-filtration unit, to realize double-filtration, wherein, utilizes described single filter unit to carry out isolated by filtration to the filtrate that described first filter is drawn; With cascade filtration unit; Described cascade filtration unit is utilized to carry out isolated by filtration for the filtrate obtained described single filter unit.With when only adopting single filter, double-filtration is more conducive to judging that in filtration cycle process, iron ion content meets the requirements of the time, and the product wax iron content caused when fluctuation appears in the iron content avoided because of waxy stone raw material exceeds standard.In addition, when adopting double-filtration, although grade one filter load is larger, but the filtration load of secondary filter reduces relatively, the service life of filter cake can extend, and simultaneously because cascade filtration can select interval and continuous feed two kinds of forms, in filtration cycle process, the index of product wax more easily controls, and flexible modulation filtration cycle amount and adsorption time can control two-stage load problem, achieve the long period steady running of device.
According to method of the present invention, in step a and steps d, filter operation temperature is preferably 150 ~ 200 DEG C, is more preferably 170-180 DEG C; In step a, forming the process of filter cake, to comprise mass ratio be 1:4-1:10, is more preferably the diatomite of 1:6-1:8 and carclazyte mixture and mixes with circulating solvent and form filter cake to filter; In addition, in described single filter unit, the solid content of the mixed serum that described diatomite and carclazyte mixture and circulating solvent configure is 6-10wt%, is more preferably 7-8wt%; In described cascade filtration unit, the solid content of the mixed serum that described diatomite and carclazyte mixture and circulating solvent configure is 0.1-4wt%, is more preferably 0.2-2wt%, to improve filter effect.
Compared with prior art, device provided by the invention is provided with the First Heat Exchanger being built in reactor top and the second heat exchanger being placed on reactor lower part, at reactor lower part, fresh feed gas and catalyst exposure, it is more violent that it reacts comparatively in the middle part of reactor and top, by reactor lower part slurries being sent into heat exchange cooling in the second external heat exchanger, and the size circulations of reactor lower part is flowed, heat exchange efficiency can be improved, and be conducive to the uniform contact of gas and catalyst, improve reaction efficiency; Portion and top reaction comparatively gentleness in the reactor, the heat of accumulation can be contacted with the First Heat Exchanger being arranged on reactor top by slurries and remove, improve space reactor utilization rate, simultaneously, slurries after First Heat Exchanger cooling increase due to density, can backflow downwards further, thus be conducive to the uniform contact of gas and catalyst, improve reaction efficiency.
In addition, the filtration pipe fitting of the first filter of the present invention is longitudinally arranged on the middle part of reactor, can reduce the obstruction to pulp flow in reactor, the slurry of longitudinal flow effectively can also remove the solid obstruction thing filtering pipe fitting surface attachment simultaneously, improves filter efficiency.
In addition, in the second filter of the present invention, filter cake surface and inner is trapped under the absorption of filter cake that powder in waxy stone or irony catalyst are formed in step a and the double action of interception, and clarified after circulating and improving filter effect further, if and adopt traditional direct filter type, such as the slurries being added with filter aid are directly passed through filter, in order to realize removing the trickle powder in slurries, have to adopt the minimum filter in filter opening aperture, easy blocking, there is the filtration of an adsorption equilibrium equally in filter aid in addition, therefore the filter effect being difficult to the application claims realized directly is filtered.
Accompanying drawing explanation
Fig. 1 is the structural representation of F-T synthesis of the present invention and separator;
Fig. 2 is the structural representation filtering pipe fitting in Fig. 1;
Fig. 3 is the schematic diagram of the second filter of the present invention.
Detailed description of the invention
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, F-T synthesis provided by the invention and separator comprise paste state bed reactor 1, First Heat Exchanger 2, second heat exchanger 3, first filter 9 and the second filter 11, wherein, described First Heat Exchanger 2 to be arranged in described paste state bed reactor 1 and to be positioned at the top of described paste state bed reactor 1, for removing the heat on described paste state bed reactor 1 top.
Described second heat exchanger 3 is arranged on outside described paste state bed reactor 1, and forms heat-exchanging loop by slurry effuser 31 and slurry inflow pipe 32 with described paste state bed reactor 1 bottom.Preferably, described paste state bed reactor 1 bottom is provided with gas distributor 4, be uniformly distributed in described paste state bed reactor 1 for making unstrpped gas, described gas distributor 4 can be any one or its improved form in the gas distributor commonly used of this area, such as directly importing type or dividing plate profile gas distributor; One end of described slurry effuser 31 is connected to the position of described paste state bed reactor 1 between described first filter 9 and gas distributor 4, the other end of described slurry effuser 31 is connected to the charging aperture on described second heat exchanger 3 top, and the link position of described slurry effuser 31 and described paste state bed reactor 1, higher than the charging aperture of described second heat exchanger 3, can enter in described second heat exchanger 3 to make the material in described paste state bed reactor 1; One end of described slurry inflow pipe 32 is connected to the position of described paste state bed reactor 1 between described slurry effuser 31 and gas distributor 4, the other end of described slurry inflow pipe 32 is connected to the discharging opening of described second heat exchanger 3 bottom, and the link position of described slurry inflow pipe 32 and described paste state bed reactor 1, lower than the discharging opening of described second heat exchanger 3, returns described paste state bed reactor 1 to make the material after cooling.Because the temperature of the material in reactor 1 is higher than the temperature of described second heat exchanger 3, material forms density contrast because of temperature difference, thus is conducive to material and is formed between described paste state bed reactor 1 and the second heat exchanger 3 and circulate.
In the present invention, it will be understood by those skilled in the art that described First Heat Exchanger 2 and the second heat exchanger 3 there is no particular/special requirement, can be any one or its improved form in the heat exchanger of this area routine, repeat no more here.
In a preferred embodiment, described slurry effuser 31 or slurry inflow pipe 32 are also provided with circulating pump (not shown), for making material forced circulation between described paste state bed reactor 1 and the second heat exchanger 3, by controlling described circulating pump, thus the cycle rate of material between described paste state bed reactor 1 and the second heat exchanger 3 can be controlled, and then regulate temperature in described paste state bed reactor 1 better, and circulating pump forced circulation is set also helps and prevent described second heat exchanger 3 from being blocked by slurry.
In the present invention, it will be appreciated by those skilled in the art that, described paste state bed reactor 1 is also provided with material import and export, such as be positioned at the unstripped gas air inlet 7 below gas distributor 4, be positioned at the catalyst feeds 8 above gas distributor 4, the top vent 5 being positioned at reactor 1 top and the slurry outlet 6 etc. be positioned at bottom reactor 1, being set to of above-mentioned material import and export is well known, repeats no more here.
In the present invention, forming gas enters reactor 1 from raw material air inlet 7, by being uniformly dispersed in the slurry of gas distributor 4 in reactor 1, and contact with the catalyst granules introduced through catalyst feeds 8 in uphill process, thus generate the product containing liquid hydrocarbon.Removed by First Heat Exchanger 2 and the second heat exchanger 3 by Fischer-Tropsch synthesis liberated heat, in reactor 1 bottom, fresh feed gas and catalyst exposure, it is more violent that it reacts comparatively in the middle part of reactor 1 and top, therefore, reactor 1 lower slurry sent into heat exchange in the second external heat exchanger 3 and lower the temperature, and the size circulations of reactor 1 bottom is flowed, improve heat exchange efficiency, and be conducive to the uniform contact of gas and catalyst, improve reaction efficiency; Preferably, described second heat exchanger 3 is provided with many groups, and such as 2-5 group or 3-4 group are evenly arranged around described paste state bed reactor 1, to strengthen cooling-down effect.Because portion and top react comparatively gentle in reactor 1, the heat therefore accumulated can be removed by First Heat Exchanger 2 contact, improves reactor 1 space availability ratio.Preferably, the distance between described slurry effuser 31 and described First Heat Exchanger 2 is the 1/4-1/2 of described paste state bed reactor 1 height, more preferably the 1/4-1/3 of described paste state bed reactor 1 height.In addition, the slurries after First Heat Exchanger 1 is lowered the temperature increase due to density, can backflow downwards further, thus be conducive to the uniform contact of gas and catalyst, improve reaction efficiency.Meanwhile, the slurry of reactor 1 bottom deposit can be discharged by the slurry outlet 6 bottom reactor 1; After reaction, remaining gas is drawn through reactor head exhaust outlet 5, and preferably, described paste state bed reactor top vent 5 place is provided with anti-Vapor Entrainment separator 10, to isolate the solid, liquid phase in exhaust.
Described first filter arranges 9 in described paste state bed reactor 1 and the position be positioned in the middle part of described paste state bed reactor, carries out isolated by filtration for the catalyst treated in the product of drawing described paste state bed reactor 1.As shown in Figure 2, in a preferred embodiment, described first filter 9 comprises one or more filtration pipe fitting, described filtration pipe fitting comprises outer screen pipe 91, inner filtration pipe 92, outer discharge nozzle 93 and interior discharge nozzle 94, described inner filtration pipe 92 is arranged on described outer screen pipe 91 inside, and the filter opening diameter of described inner filtration pipe 92 is less than the filter opening diameter of described outer screen pipe 91; The top of described outer screen pipe 91 is provided with outer backwash mouth 911, and for introducing counter-flushing liquid in described outer screen pipe 91, the top of described inner filtration pipe 92 is provided with interior backwash mouth 921, for introducing counter-flushing liquid in described inner filtration pipe 92; Described outer discharge nozzle 93 is connected to the bottom of described outer screen pipe 91, for drawing the filtration product between described outer screen pipe 91 and inner filtration pipe 92; Described interior discharge nozzle 94 is connected to the bottom of described inner filtration pipe 92, for drawing the filtration product in described inner filtration pipe 92.Preferably, the filter opening diameter of described outer screen pipe 91 is 15-60 micron, and percent opening is not less than 30%, and the filter opening diameter of described inner filtration pipe 92 is 1-10 micron, percent opening is not less than 60%, and the diameter of described outer screen pipe 91 is not less than 1.5 times of described inner filtration pipe 92 diameter; Further preferably, the filter opening diameter of described outer screen pipe 91 is 20-50 micron, and percent opening is not less than 35%; The filter opening diameter of described inner filtration pipe 92 is 2-8 micron, and percent opening is not less than 65%, and the diameter of described outer screen pipe 91 is 1.5-3 times of described inner filtration pipe 92 diameter; Still more preferably, the filter opening diameter of described outer screen pipe 91 is 30-40 micron, and percent opening is 40-50%; The filter opening diameter of described inner filtration pipe 92 is 4-6 micron, and percent opening is 70-80%, and the diameter of described outer screen pipe 91 is 1.8-2.5 times of described inner filtration pipe 92 diameter.
In reactor 1 of the present invention, enter in outer screen pipe 91 wait the product of drawing after described outer screen pipe 91 filtering and removing major part catalyst, drawing through described interior discharge nozzle 94 after the catalyst granules that described inner filtration pipe 92 filtering and removing is tiny further in described outer screen pipe 91, between described outer screen pipe 91 and inner filtration pipe 92, remaining material is drawn through described outer discharge nozzle 93, can send into storage tank further or return in described paste state bed reactor 1.Carry out double-filtration by the product treating extraction, can effectively prevent filter opening from blocking, improve filter efficiency, be particularly suitable for paste state bed reactor of the present invention.In addition, filtration pipe fitting of the present invention can also utilize described outer backwash mouth 911 and the regular flushing liquor of introducing of interior backwash mouth 921 to carry out backwash, to reduce filtration resistance to described outer screen pipe 91 and inner filtration pipe 92.
In a preferred embodiment of filtration pipe fitting of the present invention, the bottom of described outer screen pipe 91 is non-filtered section 912 (namely not arranging the part of filter opening), preferably, the length of described non-filtered section 912 is the 1/3-1/2 of the length of described outer screen pipe 91, and described inner filtration pipe 92 is positioned at described non-filtered section 912.This design can make to filter through outer screen pipe 91 surface that the product that enters can not directly act on described inner filtration pipe 92 under the effect at inertia, but flow downward, contact with described inner filtration pipe 92 in the bottom of described outer screen pipe 91, because the flow direction of product is parallel with the filtering surface of described inner filtration pipe 92, thus the catalyst granules being attached to described inner filtration pipe 92 surface can be taken away, contribute to keeping filter opening unimpeded, improve filter efficiency.Still more preferably, described first filter 9 is provided with many groups, such as 3-12 group or 5-8 group, be evenly arranged around described paste state bed reactor 1 inwall, often organize the first filter 9 and comprise 3-30 root, preferred 5-25 root, more preferably 10-20 root filters pipe fitting, to improve filtering rate.
It is outside that described second filter 11 is arranged on described paste state bed reactor 1, carries out isolated by filtration for the filtrate of drawing described first filter 9.In one embodiment of the invention, described second filter 11 comprises at least one filter element, preferably, as shown in Figure 3, at least one described filter element is two filter elements, be respectively single filter unit 12 and cascade filtration unit 13, described single filter unit 12 comprises one-level head tank 121, one-level mixing tank 122 and grade one filter 123; The discharging opening of described one-level head tank 121 and the discharging opening of one-level mixing tank 122 are connected to the charging aperture of described grade one filter 123 respectively by pipeline; The discharge outlet of described grade one filter 123 is respectively equipped with one-level head tank circulation pipe 124, one-level mixing tank circulation pipe 125 and one-level discharge nozzle 126, the discharging opening of described grade one filter 123 is connected to the charging aperture of described one-level head tank 121 by one-level head tank circulation pipe 124, the discharging opening of described grade one filter 123 is connected to the charging aperture of described one-level mixing tank 122 by one-level mixing tank circulation pipe 125; Described one-level discharge nozzle 126 is connected with the discharging opening of described grade one filter 123, for the qualified filtrate of described grade one filter 123 being sent.
Described cascade filtration unit 13 comprises secondary raw materials tank 131, secondary mixing tank 132 and secondary filter 133; The charging aperture of described secondary raw materials tank 131 is connected to the discharging opening of described grade one filter 123 by described one-level discharge nozzle 126, the discharging opening of described secondary raw materials tank 131 and the discharging opening of secondary mixing tank 132 are connected to the charging aperture of described secondary filter 133 respectively by pipeline; The discharge outlet of described secondary filter 133 is respectively equipped with secondary raw materials tank circulation pipe 134, secondary mixing tank circulation pipe 135 and secondary discharge nozzle 136, the discharging opening of described secondary filter 133 is connected to the charging aperture of described secondary raw materials tank 131 by secondary raw materials tank circulation pipe 134, the discharging opening of described secondary filter 133 is connected to the charging aperture of described secondary mixing tank 132 by secondary mixing tank circulation pipe 135; Described secondary discharge nozzle 136 is connected with the discharging opening of described secondary filter 133, for the qualified filtrate of described secondary filter 133 being sent.
During operation, the method for operation of described single filter unit 12 is as follows: the first step, mixed in described one-level mixing tank 122 with filter aid by circulating solvent, and send into grade one filter, filtrate cycle gets back to described one-level mixing tank 122; Repeat this process, until the filter element of described grade one filter 123 forms one deck filter cake outward, cut out described one-level mixing tank 122, after namely circulating solvent gets back to one-level mixing tank 122, stop the Matter Transfer between described one-level mixing tank 122 and grade one filter 123.Second step, then the slurries to be separated in described one-level head tank 121 are sent into described grade one filter 123, filtrate cycle gets back to described one-level head tank 121; Repeat this process until in filtrate solid concentration qualified after, sent by the discharging opening of described grade one filter 123.Described cascade filtration unit 13 carries out isolated by filtration for the filtrate obtained described single filter unit 12, and its method of operation is with described single filter unit 12.
It will be appreciated by those skilled in the art that, in second step, along with constantly carrying out of filter process, the filter residue that on described filter cake, the continuous enrichment of meeting is new, therefore, preferably, in the running of described single filter unit 12, also need to clear up the filter cake outside the filter element of described grade one filter 123, such as periodic cleaning, or clear up according to filter pressure, or clear up etc. according to filter cake thickness, then repeat the first step and second step.
Preferably, described circulating solvent is refining Fischer Tropsch waxes, and described filter aid is carclazyte and diatomite; Filter operation temperature 150 ~ 200 DEG C, is preferably 170-180 DEG C; In the first step and second step, forming that the process of filter cake comprises mass ratio is 1:4-1:10, is preferably the diatomite of 1:6-1:8 and carclazyte mixture and mixes with circulating solvent and form filter cake to filter.Further preferably, in described single filter unit 12, the solid content of the mixed serum that described diatomite and carclazyte mixture and circulating solvent configure is 6-10wt%, is preferably 7-8wt%; In described cascade filtration unit 13, the solid content of the mixed serum that described diatomite and carclazyte mixture and circulating solvent configure is 0.1-4wt%, is preferably 0.2-2wt%.
Claims (15)
1. a F-T synthesis and separator, comprise paste state bed reactor, First Heat Exchanger, the second heat exchanger, the first filter and the second filter, described First Heat Exchanger to be arranged in described paste state bed reactor and to be positioned at the top of described paste state bed reactor, described second heat exchanger is arranged on outside described paste state bed reactor, and forms heat-exchanging loop by slurry effuser and slurry inflow pipe and described paste state bed reactor bottom;
Described first filter is arranged in described paste state bed reactor and the position be positioned in the middle part of described paste state bed reactor, carries out isolated by filtration for the catalyst treated in the product of drawing described paste state bed reactor;
It is outside that described second filter is arranged on described paste state bed reactor, carries out isolated by filtration for the filtrate of drawing described first filter.
2. F-T synthesis according to claim 1 and separator, is characterized in that, described paste state bed reactor bottom is provided with gas distributor; One end of described slurry effuser is connected to the position of described paste state bed reactor between described first filter and gas distributor, the other end of described slurry effuser is connected to the charging aperture on described second heat exchanger top, and the link position of described slurry effuser and described paste state bed reactor is higher than the charging aperture of described second heat exchanger; One end of described slurry inflow pipe is connected to the position of described paste state bed reactor between described slurry effuser and gas distributor, the other end of described slurry inflow pipe is connected to the discharging opening of described second heat exchanger bottom, and the link position of described slurry inflow pipe and described paste state bed reactor is lower than the discharging opening of described second heat exchanger.
3. F-T synthesis according to claim 2 and separator, is characterized in that, the distance between described slurry effuser and described First Heat Exchanger is the 1/4-1/2 of described paste state bed reactor height.
4. F-T synthesis according to claim 1 and separator, it is characterized in that, described first filter comprises one or more filtration pipe fitting, described filtration pipe fitting comprises outer screen pipe, inner filtration pipe, outer discharge nozzle and interior discharge nozzle, it is inner that described inner filtration pipe is arranged on described outer screen pipe, and the filter opening diameter of described inner filtration pipe is less than the filter opening diameter of described outer screen pipe; The top of described outer screen pipe is provided with outer backwash mouth, and for introducing counter-flushing liquid in described outer screen pipe, the top of described inner filtration pipe is provided with interior backwash mouth, for introducing counter-flushing liquid in described inner filtration pipe; Described outer discharge nozzle is connected to the bottom of described outer screen pipe, sends described paste state bed reactor back to for the filtration product of drawing between described outer screen pipe and inner filtration pipe; Described interior discharge nozzle is connected to the bottom of described inner filtration pipe, for drawing the filtration product in described inner filtration pipe.
5. F-T synthesis according to claim 4 and separator, is characterized in that, the bottom of described outer screen pipe is non-filtered section, and described inner filtration pipe is positioned at described non-filtered section.
6. F-T synthesis according to claim 5 and separator, it is characterized in that, the filter opening diameter of described outer screen pipe is 15-60 micron, percent opening is not less than 30%, the filter opening diameter of described inner filtration pipe is 1-10 micron, percent opening is not less than 60%, and the diameter of described outer screen pipe is 1.5-3 times of described inner filtration pipe diameter.
7. F-T synthesis according to claim 1 and separator, is characterized in that, described second filter comprises at least one filter element, and described filter element comprises head tank, mixing tank and filter; The discharging opening of described head tank and the discharging opening of mixing tank are connected to the charging aperture of described filter respectively by pipeline; The discharge outlet of described filter is respectively equipped with head tank circulation pipe, mixing tank circulation pipe and discharge nozzle, the discharging opening of described filter is connected to the charging aperture of described head tank by head tank circulation pipe, the discharging opening of described filter is connected to the charging aperture of described mixing tank by mixing tank circulation pipe; Described discharge nozzle is connected with the discharging opening of described filter, for the qualified filtrate of described filter being sent.
8. F-T synthesis according to claim 7 and separator, is characterized in that, at least one described filter element is two filter elements, is respectively single filter unit and cascade filtration unit; Wherein, described cascade filtration unit is used for carrying out isolated by filtration to the filtrate that described single filter unit obtains.
9. the device according to any one of claim 4-6, is characterized in that, described second heat exchanger is provided with 2-5 group, is evenly arranged around described paste state bed reactor;
Described first filter is provided with 3-12 group, is evenly arranged around described paste state bed reactor sidewall, often organizes filter and comprises 3-30 root filtration pipe fitting.
10. F-T synthesis according to claim 1 and separator, it is characterized in that, the top exit place of described paste state bed reactor is provided with anti-Vapor Entrainment separator, described slurry inflow pipe is provided with circulating pump, for making material forced circulation between described paste state bed reactor and the second heat exchanger.
11. 1 kinds of methods utilizing the F-T synthesis according to any one of claim 1-10 and separator to carry out F-T synthesis, described method comprises and utilizes described paste state bed reactor to carry out Fischer-Tropsch synthesis, utilize described First Heat Exchanger to remove the heat on reactor top, utilize the second heat exchanger to remove the heat of reactor lower part; The catalyst utilizing described first filter to treat in the product of drawing described paste state bed reactor carries out isolated by filtration, utilizes described second filter to carry out isolated by filtration to the filtrate that described first filter is drawn.
12. methods according to claim 11, is characterized in that, utilize described second filter to comprise the steps: the process that the filtrate that described first filter is drawn carries out isolated by filtration
Step a, mixed in described mixing tank with filter aid by circulating solvent, send into filter, filtrate cycle gets back to described mixing tank; Repeat this process, until form one deck filter cake outside the filter element of described filter, cut out described mixing tank;
Step b, the slurries to be separated in described head tank are sent into described filter, filtrate cycle gets back to described head tank; Repeat this process until in filtrate solid concentration qualified after, sent by the discharging opening of described filter.
13. methods according to claim 12, is characterized in that, in stepb, clear up the filter cake outside described metre filter element, then repeat step a and step b.
14. methods according to claim 13, is characterized in that, utilize described single filter unit to carry out isolated by filtration to the filtrate that described first filter is drawn; With cascade filtration unit; Described cascade filtration unit is utilized to carry out isolated by filtration for the filtrate obtained described single filter unit.
15. methods according to any one of claim 11-14, it is characterized in that, described circulating solvent is refining Fischer Tropsch waxes, and described filter aid is carclazyte and diatomite; Filter operation temperature 150 ~ 200 DEG C;
In step a, forming that the process of filter cake comprises mass ratio is that the diatomite of 1:4-1:10 and carclazyte mixture mix with circulating solvent and form filter cake to filter.
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