CN103962064B - A kind of method adopting up-flow reactor F-T synthesis - Google Patents
A kind of method adopting up-flow reactor F-T synthesis Download PDFInfo
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Abstract
A kind of method adopting up-flow reactor F-T synthesis, raw material of synthetic gas enters from calandria type fixed bed reactor bottom, contacts with fischer-tropsch synthetic catalyst, reacts under Fischer-Tropsch synthesis condition, the inner surface of its reaction tube is smooth, and outer surface has groove.The heavy constituent that reaction produces derives from reactor bottom, and light component and the water of unreacted synthesis gas and generation in reactor are derived from reactor head, enter piece-rate system; The separating obtained gaseous stream part of piece-rate system enters recycle compressor supercharging Posterior circle and mixes to reactor inlet and unstripped gas, and a part is as tail gas discharger.Adopt method provided by the invention, solve the problem that existing fixed bed reactors are axial, radial symmetry gradient is large, in addition, reactor bed pressure drop of the present invention is little, and separation equipment is few, reduction energy consumption of can reducing investment outlay.
Description
Technical field
The present invention relates to a kind of method of being produced hydro carbons by hydrogen and carbon monoxide by F-T synthesis, more particularly, is a kind of method adopting up flow type calandria type fixed bed reactor synthesizing liquid hydrocarbon.
Background technology
Coal, natural gas or biomass conversion are synthesis gas, then synthesizing (F-T synthesis) by Fischer-Tropsch is hydrocarbon products, high-quality liquid fuel can be obtained if gasoline, diesel oil and aviation kerosine and other industrial chemicals are as lube base oil, food grade wax etc. through deep processing, this Technology Ways receives the very big concern of world energy sources chemical industry, and it is the artificial oil technique of core that many international energy companies develop respectively with F-T synthesis.
The technique adopting calandria type fixed bed reactor to carry out F-T synthesis has simple to operate, and the feature that flexible form is various, by many research institutions as the technology first researched and developed.But many problems that fixed bed reactors exist limit it and apply on a large scale, such as: fixed bed reactors exist focus due to the reactor that affects conducted heat; Conversion per pass is low, needs to carry out compression cycle to a large amount of circulating air, and energy consumption is high and reactor pressure decrease is large; The use of large granular catalyst makes catalyst performance be affected etc.
By part heat transfer problem can be solved to the improvement of reactor, such as CN1736574A discloses a kind of non-hot spot calandria type fixed bed reactors, this reactor increases in a set of cooling to manage in reaction tube, cooling medium can in reaction tube in pipe and reactor enclosure intrastratal flow heat-obtaining, this scheme can increase heat exchange area, the radial temperature difference of beds can be reduced, effectively solve heat transfer problem, but it is very complicated that this improvement makes reactor become, and the cooled interior pipe of the reactor useful space occupies very most of.
In order to improve the bad shortcoming of fixed-bed heat transfer performance, in prior art, liquid medium is imported the method for reactor, because liquid has larger thermal capacitance, liquid medium adds the focus that can reduce beds.Such as, in US5786393, add part inert fluid in F-T synthesis fixed bed reactors, apparent velocity, higher than 1cm/s, obviously can improve reactivity worth and increase C
5 +saturated hydrocarbons yield.CN1662476A discloses a kind of method, and the fluid media (medium) of inertia is imported reactor, and continuous print liquid medium flow can promote the transfer of heat, significantly improves reactivity worth.But also there is limitation in this method, the restriction of the device pressure drop because respond, can only reach certain numerical value by fluid (comprising gas phase and the liquid phase) total amount of reactor, namely show that liquid phase adds the rear throughput needing to reduce gas phase, therefore overall catalytic activity or conversion ratio can be affected.
For Fischer-Tropsch synthesis, normally catalyst grain size is less, the activity that can reach is higher, selective better, but when fluid flux is fixing, the less reactor pressure decrease of catalyst granules is also larger, and the catalyst grain size therefore loaded in reaction tube is generally at 2 ~ 5mm, and fluid flux is also limited in certain limit.Syrup state bed Fischer Tropsch synthesis can utilize the catalyst of less than 200 μm, is one of high, selective good reason of its activity.Adopt the up-flow reactor of lower charging, can reactor pressure decrease be reduced.US4413063 proposes the Fischer-Tropsch synthesis method that a kind of synthesis gas and cooling fluid enter from reactor lower end, compared with obtaining larger fluid flux under low pressure drop, thus can improve reactivity worth like this.But adopt and need in this way to ensure that in beds, cooling fluid is necessary for continuous phase, and need separation and the recycle unit of cooling fluid, reaction system is comparatively complicated.
Summary of the invention
The object of this invention is to provide a kind of method of synthesizing liquid hydrocarbon, both can solve the problem that calandria type fixed bed reactor exists heat transfer difficult and focus, also can solve the Utilizing question of superior performance small grain size catalyst in fixed bed F-T synthesis.
Method provided by the present invention comprises the following steps:
(1) raw material of synthetic gas enters from calandria type fixed bed reactor bottom, contacts with fischer-tropsch synthetic catalyst, reacts under Fischer-Tropsch synthesis condition; The reaction tube of described calandria type fixed bed reactor respectively by reactor upper perforated plate and reactor lower perforated plate stationary arrangement in reactor shell, the inner surface of described reaction tube is smooth, and outer surface has groove;
(2) heavy constituent that reaction produces derives from reactor bottom, and light component and the water of unreacted synthesis gas and generation in reactor are derived from reactor head, enter piece-rate system;
(3) the separating obtained gaseous stream part of piece-rate system enters recycle compressor supercharging Posterior circle and mixes to reactor inlet and unstripped gas, and a part is as tail gas discharger.
Described reaction tube is carbon structural steels or austenitic stainless steel, and inner surface is smooth, and outer surface is formed with the spiral type groove of certain rule through hot and cold machining.Catalyst packing is in reaction tube, and cooling medium flows through reactor shell side, and namely with the exterior surface of reaction tube, take the heat that reaction produces out of reactor, deflection plate is distributed in the middle of reactor according to a determining deviation.
The characteristic parameter of described reaction tube outer surface groove is: every meter has 200 ~ 2000 grooves, groove depth 0.5 ~ 1.5mm, groove width 0.2 ~ 1.0mm, and lead angle is 3 ~ 5 °.Preferably, every meter has 300 ~ 800 grooves, groove depth 1.0 ~ 1.2mm, groove width 0.5 ~ 0.8mm.Channel section can be T-shaped, rectangle, trapezoidal, triangle, zigzag, and when channel section is non-rectangular shape, described groove width refers to the mean breadth of groove.
The two ends up and down of described reaction tube have the light pipe portion of 200 ~ 500mm.On reactor, lower perforated plate is connected with the light pipe portion at the two ends up and down of reaction tube.
Described shell and tube reactor housing is made up of reactor upper cover, reactor shell, reactor low head, reactor low head is arranged reactor feed mouth and feed distributor, reactor upper cover is arranged reactor discharging opening, cooling medium outlet is set on the top of reactor shell, cooling medium entrance is set in the bottom of reactor shell.
Described calandria type fixed bed reactor, the cooling medium of employing can be pure water, oil, melt salt, water vapour, conventional gas etc.
Described fischer-tropsch synthetic catalyst is Co based Fischer-Tropsch synthesis catalyst, and with oxide basis, cobalt metal component mass content is 1% ~ 60%, and granularity is 0.2 ~ 2mm.Preferably, cobalt metal component mass content is 5% ~ 50%, and granularity is 0.5 ~ 1.5mm.One or more auxiliary agents of metal and nonmetalloid can be contained in described Co based Fischer-Tropsch synthesis catalyst.Co based Fischer-Tropsch synthesis catalyst can, with precipitation, impregnating preparation method preparation, need to process certain hour under suitable drying and roasting condition.The shape of catalyst can be column, spherical, hollow ball, ring-type, saddle, trilobal cross bar, four blade profile bars etc.
Described Fischer-Tropsch synthesis condition is: pressure 1 ~ 5MPa, temperature 150 ~ 300 DEG C, unstripped gas gas hourly space velocity 500 ~ 6000h
-1, H
2with CO ratio 1 ~ 3, be preferably: reaction pressure 2 ~ 4MPa, temperature is 180 ~ 230 DEG C, gas hourly space velocity 1000 ~ 3000h
-1, H
2with CO ratio 1.8 ~ 2.5.
Containing CO and H that unreacted is complete in gaseous stream described in step (3)
2and the CO that reaction generates
2and C
1~ C
5hydro carbons mist.Portion gas returns Fischer-Tropsch synthesis device entrance.The volume ratio of the described gas stream and fresh feed gas that return Fischer-Tropsch synthesis device entrance is 0.1 ~ 8, preferably 0.5 ~ 3.
The present invention can adopt multistage reactor, or reactor is in parallel and the combining form of series winding.
The present invention compared with prior art, has the following advantages:
(1), owing to adopting the calandria type fixed bed reactor of the reeded reaction tube of outer surface tool, tube side-shell-side heat transfer obtains strengthening, solves the problem that existing fixed bed reactors are axial, radial symmetry gradient is large.
(2), adopt the mode of lower charging, reactor bed pressure drop is little, without recycle compressor or can adopt little head compressor, and reduces separation equipment, reduction energy consumption of reducing investment outlay; The reduction of internal circulating load is simultaneously conducive to reducing material linear velocity in reactor, can increase residence time of material, improve conversion per pass, add heavy distillate proportion in product.
(3), adopt method of the present invention, smaller particle size and more low intensive catalyst can be applied on fixed bed reactors, thus obtain higher activity and selectivity.
Accompanying drawing explanation
Fig. 1 is calandria type fixed bed reactor structural representation of the present invention.
Fig. 2 is the reaction tube generalized section of calandria type fixed bed reactor of the present invention.
Fig. 3 is the method flow schematic diagram of up-flow reactor F-T synthesis provided by the invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, method provided by the present invention is further described, but therefore the present invention is not subject to any restriction.
In Fig. 1: 1-reactor feed mouth; 2-charging aperture filter plate; 3-reactor low head; 4-lower perforated plate; 5-deflection plate; 6-reactor shell; 7-reaction tube; 8-upper perforated plate; 9-reactor upper cover; 10-reactor upper sieve plate; 11-reactor discharging opening; 12-cooling medium entrance; 13-cooling medium exports.
Fig. 1 is calandria type fixed bed reactor structural representation of the present invention.As shown in Figure 1, described calandria type fixed bed reactor comprises lower perforated plate on reactor shell, reactor (8,4), reaction tube 7, deflection plate 5, described reaction tube 7 respectively by reactor upper perforated plate 8 and reactor lower perforated plate 4 stationary arrangement in reactor shell 6, the inner surface of described reaction tube 7 is smooth, and outer surface has groove.Described reactor shell is made up of reactor upper cover 9, reactor shell 6, reactor low head 3, reactor low head 3 is arranged reactor feed mouth 1 and feed distributor 2, reactor upper cover 9 is arranged reactor discharging opening 11, reactor upper sieve plate 10, cooling medium outlet 13 are set on the top of reactor shell, cooling medium entrance 12 is set in the bottom of reactor shell.
Reaction mass is introduced from reactor feed mouth 1, after feed distributor 2, enter and be equipped with in the reaction tube 7 of catalyst, react after reaction raw materials and catalyst exposure, the reaction raw materials do not run out of and product flow out from reaction tube 7 lower end, are derived after reactor upper sieve plate 10 by reactor discharging opening 11.Cooling medium enters reactor shell side from cooling medium entrance 12, horizontal and vertical flowing is formed under the restriction of deflection plate 5, the heat that reaction produces passes to cooling medium through reaction tube 7 tube wall, and the cooling medium after heat absorption derives reactor from cooling medium outlet 13.
Fig. 2 is the generalized section of reaction tube, and D is reaction tube external diameter, and d is tube inner diameter, outer surface helical groove.
Fig. 3 is the method flow schematic diagram of up-flow reactor F-T synthesis provided by the invention.As shown in Figure 3, calandria type fixed bed reactor 2 is entered from reaction bottom through the synthesis gas from the purification of pipeline 1, after contacting with Co based Fischer-Tropsch synthesis catalyst, carry out Fischer-Tropsch synthesis, the synthesis gas that unreacted is complete and product are derived from the top of reactor, enter high pressure hot separator 4 through pipeline 3, reaction gained heavy hydrocarbons component derives from bottom, through pipeline 11 let-off gear(stand).The gas phase 5 that high pressure hot separator 4 is separated enters cold high pressure separator 6 and carries out gas-liquid separation after cooling.Cold high pressure separator 6 gained liquid phase enters cold low separator 7, isolates light hydrocarbon component and water respectively through pipeline 13 and pipeline 12 let-off gear(stand).The separating obtained gaseous stream of cold high pressure separator 6 can be divided into two parts through pipeline 8, a part is discharged through pipeline 15 with tail gas form, another part enters recycle compressor 9 through pipeline, enters fixed bed reactors 2 after supercharging after pipeline 10 mixes with the unstripped gas from pipeline 1.Discharged through pipeline 14 by the isolated gas of separator 7.Reactor heat-obtaining system forms primarily of drum 21, water circulating pump 22 and Steam pressure control 23, by controlling the Stress control temperature of reactor of drum.
Below in conjunction with embodiment, method of the present invention is illustrated further, but not thereby limiting the invention.
Embodiment
The preparation process of fischer-tropsch synthetic catalyst used in embodiment is as follows: get alumina powder, drips distilled water to just wetting, writes down the volume consuming water, then press Co content (oxide basis) 27 % by weight and calculate, make cobalt nitrate maceration extract.Then soak to first with this solution impregnation aluminium oxide, leave standstill 8 hours, then in 120 DEG C of dryings 4 hours, 450 DEG C of roastings, 4 hours obtained catalyst in muffle furnace.Particle size range 0.5 ~ the 0.8mm of gained Co based Fischer-Tropsch synthesis catalyst.
The present embodiment adopts technological process shown in Fig. 3, and Fischer-Tropsch synthesis device adopts external diameter 38mm, wall thickness 3mm Austenitic stainless steel pipe material, and outer surface adopts cold working to form groove structure, every mitron is long comprises 500 grooves, groove depth 1.2mm, groove mean breadth 0.6mm, lead angle is 4 °.
Fischer-tropsch synthesis process condition is: material synthesis gas volume air speed 800h
-1, hydrogen and carbon monoxide mole ratios be 2.0, reaction pressure 3.0MPa, circulating air and feed gas volume are than 2.0.
Adopt method provided by the invention, under the prerequisite reaching Synthetic holography rate 95%, reactor pressure decrease is not more than 0.4MPa, and the beds temperature difference is not more than 6 DEG C.Meanwhile, the advantage of small grain size catalyst is played, and the methane production of whole device is 4.8%, C
5+productive rate is 88%, and the oil product yield of catalyst is 145g/L catalyst/h.
Comparative example
The preparation process of fischer-tropsch synthetic catalyst used in comparative example is as follows: get alumina powder, drips distilled water to just wetting, writes down the volume consuming water, then press Co content (oxide basis) 27 % by weight and calculate, make cobalt nitrate maceration extract.Then soak to first with this solution impregnation aluminium oxide, leave standstill 8 hours, then in 120 DEG C of dryings 4 hours, 450 DEG C of roastings, 4 hours obtained catalyst in muffle furnace.Particle size range 1.6 ~ the 2.0mm of gained Co based Fischer-Tropsch synthesis catalyst.
This comparative example adopts the conventional fixed bed reactors of interior diameter 32mm general surface reaction tube, and upper intake lower outlet type feeding manner, and fischer-tropsch synthesis process condition is: material synthesis gas volume air speed 800h
-1, hydrogen and carbon monoxide mole ratios be 2.0, reaction pressure 3.0MPa, circulating air and feed gas volume are than 5.0.
Under the prerequisite reaching Synthetic holography rate 95%, reactor pressure decrease is greater than 0.7MPa, and the beds temperature difference is greater than 12 DEG C.The methane production of whole device is higher than 10%, C
5+productive rate is 82%, and the oil product yield of catalyst is 122g/L catalyst/h.
Claims (12)
1. adopt a method for up-flow reactor F-T synthesis, comprise the following steps:
(1) raw material of synthetic gas enters from calandria type fixed bed reactor bottom, contacts with fischer-tropsch synthetic catalyst, reacts under Fischer-Tropsch synthesis condition; The reaction tube of described calandria type fixed bed reactor respectively by reactor upper perforated plate and reactor lower perforated plate stationary arrangement in reactor shell, the inner surface of described reaction tube is smooth, and outer surface has groove;
(2) heavy constituent that reaction produces derives from reactor bottom, and light component and the water of unreacted synthesis gas and generation in reactor are derived from reactor head, enter piece-rate system;
(3) the separating obtained gaseous stream part of piece-rate system enters recycle compressor supercharging Posterior circle and mixes to reactor inlet and unstripped gas, and a part is as tail gas discharger.
2. in accordance with the method for claim 1, it is characterized in that, the characteristic parameter of described reaction tube outer surface groove is: every meter has 200 ~ 2000 grooves, groove depth 0.5 ~ 1.5mm, groove width 0.2 ~ 1.0mm, and lead angle is 3 ~ 5 °.
3. in accordance with the method for claim 2, it is characterized in that, the characteristic parameter of described reaction tube outer surface groove is: every meter has 300 ~ 800 grooves, groove depth 1.0 ~ 1.2mm, groove width 0.5 ~ 0.8mm.
4. in accordance with the method for claim 1, it is characterized in that, be arranged with 100 ~ 10000 reaction tubes in described calandria type fixed bed reactor, the interior diameter of every root reaction tube is 20 ~ 60mm, and length is 4 ~ 15m.
5. in accordance with the method for claim 4, it is characterized in that, the interior diameter of described reaction tube is 25 ~ 50mm, and length is 6 ~ 12m.
6. in accordance with the method for claim 1, it is characterized in that, the pipe thickness of described reaction tube is 1 ~ 8mm.
7. in accordance with the method for claim 1, it is characterized in that, the two ends up and down of described reaction tube have the light pipe portion of 200 ~ 500mm; On reactor, lower perforated plate is connected with the light pipe portion at the two ends up and down of reaction tube.
8. in accordance with the method for claim 1, it is characterized in that, described fischer-tropsch synthetic catalyst is Co based Fischer-Tropsch synthesis catalyst, and with oxide basis, cobalt metal component mass content is 1% ~ 60%, and granularity is 0.2 ~ 2mm.
9. in accordance with the method for claim 8, it is characterized in that, described Co based Fischer-Tropsch synthesis catalyst, with oxide basis, cobalt metal component mass content is 5% ~ 50%, and granularity is 0.5 ~ 1.5mm.
10. in accordance with the method for claim 1, it is characterized in that, described Fischer-Tropsch synthesis condition is: pressure 1 ~ 5MPa, temperature 150 ~ 300 DEG C, unstripped gas gas hourly space velocity 500 ~ 6000h
-1, H
2with CO ratio 1 ~ 3.
11. in accordance with the method for claim 1, it is characterized in that, described Fischer-Tropsch synthesis condition is: reaction pressure 2 ~ 4MPa, and temperature is 180 ~ 230 DEG C, gas hourly space velocity 1000 ~ 3000h
-1, H
2with CO ratio 1.8 ~ 2.5.
12. in accordance with the method for claim 1, it is characterized in that, containing CO and H that unreacted is complete in the gaseous stream described in step (3)
2and the CO that reaction generates
2and C
1~ C
5hydro carbons mist, the volume ratio of the described gas stream and fresh feed gas that are circulated to Fischer-Tropsch synthesis device entrance is 0.1 ~ 8.
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| CN108067167B (en) * | 2016-11-07 | 2020-11-27 | 神华集团有限责任公司 | Slurry bed reaction system and Fischer-Tropsch synthesis reaction method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1736574A (en) * | 2005-07-08 | 2006-02-22 | 清华大学 | Non-hot spot calandria type fixed bed reactors |
| CN102441352A (en) * | 2010-10-12 | 2012-05-09 | 中国石油化工股份有限公司 | Method for synthesizing Fischer Tropsch of slurry bed |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1736574A (en) * | 2005-07-08 | 2006-02-22 | 清华大学 | Non-hot spot calandria type fixed bed reactors |
| CN102441352A (en) * | 2010-10-12 | 2012-05-09 | 中国石油化工股份有限公司 | Method for synthesizing Fischer Tropsch of slurry bed |
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