CN1814576A - Fischer-tropsch synthesis method utilizing fluidized bed reactor - Google Patents
Fischer-tropsch synthesis method utilizing fluidized bed reactor Download PDFInfo
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Abstract
The invention relates to a method for compounding FT by using fluidized-bed reactor. The invention includes the following technology process: mixing the compounding gas and circling gas, pressurizing and heating, taking FT compounding reaction in fluidized-bed reactor, the reaction temperature is 300-500 degree centigrade, pressure is 2.0-5.0MPa, operation linear speed is 0.3-0.7m/s. The gas distributing device in reactor ensures the equality of the fluid, removing the heat by inner cooling pipe, keeping the catalyst by the gas-solid separation device, ensuring the catalyst renewing online. The outlet gas would take dust removal and cooling process, and taking separation, the oil phase is the product. Recycling the organic in the water phase, releasing the gas phase, most part could be circled.
Description
Technical field
The present invention relates to a kind of method of utilizing fluidized-bed reactor synthetic gas to be converted into hydrocarbon products.
Background technology
The Fischer-Tropsch building-up process is the process of utilizing based on synthetic gas synthetic hydrocarbon under the effect of catalyzer of hydrogen and carbon monoxide.
According to the difference of employing catalyzer, the Fischer-Tropsch synthesis device can have multiple choices, and wherein paste state bed reactor and fluidized-bed reactor are two kinds of main reactor patterns that adopt.
In in recent years the report and patent, the synthetic paste state bed reactors that adopt of Fischer-Tropsch carry out more.Adopting the characteristics of paste state bed reactor is that temperature of reactor is relatively low, be easy to control, but transformation efficiency is lower, and the liquid-solid separation of reactor slurry is comparatively difficult.
Adopting the characteristics of the Fischer-Tropsch building-up process of fluidized-bed reactor is that temperature is higher, and transformation efficiency is also higher, does not have the comparatively liquid-solid separation problem of the reactor slurry of difficulty, but interior gas of reactor and solid need uniform distribution, and reaction back gas solid separation requires height.
On the whole, adopting paste state bed reactor still is that fluidized-bed reactor cuts both ways, and mainly still depends on target product.Which kind of technological process no matter, long-term continous-stable operation is crucial.
Summary of the invention
Purpose of the present invention is exactly to carry out Fischer-Tropsch synthetic method for the fluidized-bed reactor that utilizes that a kind of operation of steady and continuous for a long time is provided.
Purpose of the present invention can be achieved through the following technical solutions: a kind of fluidized-bed reactor that utilizes carries out Fischer-Tropsch synthetic method, it is characterized in that this method comprises following processing step:
(1) with H
2With CO be the fresh synthesis gas of main component with after circulation gas mixes, through the recycle compressor pressurization and be heated to temperature through one or more levels interchanger and be not less than 100 ℃, enter fluidized-bed reactor, Fischer-Tropsch synthesis takes place under the effect of fischer-tropsch synthetic catalyst; Temperature of reaction is 300~500 ℃, and pressure is that 2.0~5.0MPa, operating linear velocity are 0.3~0.7m/s, and the catalyst body volume concentrations in the fluidized-bed reactor dense-phase bed is 5~30%;
(2) in reactor, guarantee that by distribution device in gas-fluid the fluid distribution of gas fluidized bed is good; Remove heat and byproduct steam by the cold pipe of interior heat exchange; Gas-solid separation equipment by the top remains on catalyzer in the catalytic bed; Need at set intervals that catalyzer is carried out online partial discharge and add to guarantee catalyst concn, activity and average selectivity with part, the long-term continous-stable operation of this technology has been guaranteed in all these measures;
(3) high-temperature gas that comes out from reactor is earlier through a dedusting cooling unit, and granules of catalyst and the recovery part high temperature condensable product removing in the high-temperature gas to be carried secretly are delivered to the product groove after the product of generation reduces pressure after filtration;
(4) gas that comes out from the dedusting cooling unit is after one or more levels interchanger cooling, delivering to a triphase separator separates water, oil phase and gas phase, oil phase is sent to the product groove as the cryogenic condensation product after reducing pressure, send reaction water rectification cell recovery oxygen-bearing organic matter wherein after the water decompression, a gas phase part reclaims wherein behind the available gas composition emptying or the gas that acts as a fuel is used, and the overwhelming majority is circulated by recycle compressor;
(5) the reactor inlet unstripped gas has multiple preheating method, can by with the dust removing units exit gas or/and reactor outlet gas or/and the heat exchange of dust removal installation exit gas, the recovery part heat; Can further provide the part heat in addition with conventional interchanger.
Described catalyzer can be common iron-based, Co based Fischer-Tropsch synthesis catalyst, it also can be the fischer-tropsch synthetic catalyst of other any compositions, employed catalyzer should be able to satisfy in the cycle of long-term operation continuously active and selectivity and stablize not breakable requirement.
Described material synthesis gas is with H
2With CO be main, H
2/ CO is than between 0.5~6.
Described reactor is provided with a non-return valve and accident scavenging line at unstripped gas inlet, is used to alleviate and handles the obstruction of operation fluctuation of operating conditions distribution device in gas-fluid greatly the time.
The online interpolation of the catalyzer of described reactor and the realization of discharging, need one or more catalyzer medial launders, be used for catalyst charge and discharging, the outlet of medial launder is provided with the particle that one or more strainers are carried secretly when capturing catalyst transport, and the bottom has weighing instrument accurately to weigh to guarantee that the catalyst in reactor load is constant substantially.
Described catalyst charge and discharging are carried by the high pressure gas dilute phase, material gas weight ratio, i.e. and the ratio of catalyzer and high pressure gas conveying weight rate is 5~30, is not prone to obstruction with the degree of wear that reduces catalyzer and pipeline; The adding speed of catalyzer or the speed that draws off are mainly regulated by the differential pressure between catalyzer medial launder and the reactor; Described high pressure gas can be high-pressure inert gas such as nitrogen, also can be high-pressure process gas such as synthetic gas.
The preheating method of described inlet unstripped gas is determined according to heat exchange network optimization design, and is the highest to guarantee the energy comprehensive utilization ratio.
Described dedusting cooling unit can adopt one of following dual mode:
(1) the quenching column washing type of cooling;
(2) gas solid separation postcooling mode.
The dedusting cooling unit of the described employing quenching column washing type of cooling is made up of quenching column, quenching column recycle pump and quenching column recirculation cooler at least, and the dedusting refrigerating function is finished in quenching column.
The dedusting cooling unit of described employing gas solid separation postcooling mode is made up of gas-solid separation equipment, water cooler, gas-liquid separator at least; Gas-solid separation equipment can be equipment such as electric precipitator or strainer, and the heat-eliminating medium of water cooler can be general heat-eliminating medium, also can be the process gas of reactor into.
Description of drawings
Fig. 1 is the Fischer-Tropsch synthesis process schema of a commerical test;
Fig. 2 is the Fischer-Tropsch synthesis process schema of an industrial installation.
Embodiment
Below in conjunction with specific embodiment the present invention is illustrated.
As shown in Figure 1, from the H outside the battery limit (BL)
2/ CO mixes with most of tail gas from triphase separator 18 than being 2.0 fresh synthesis gas, enter recycle compressor 1 compression, incoming stock then gas one-level preheater 2, carry out heat exchange with exit gas from quenching column 11, unstripped gas is heated to 100 ℃, simultaneously the quenching column exit gas is cooled to 120 ℃ from 170 ℃. the incoming stock again gas secondary of the gas after one-level preheating preheater 3, be preheating to 145 ℃, enter synthesis reactor.The unstripped gas of reactor 5 inlet is provided with the obstruction that a non-return valve 28 and accident scavenging line 29 are used to alleviate and handle operation fluctuation of operating conditions distribution device in gas-fluid 6 greatly the time.
The gas that enters reactor 5 at first carries out the uniform of gas through a distribution device in gas-fluid 6, the catalyzer in the reactor 5 is blown afloat the uniform distribution of back realization response device internal activator.Reactor 5 is removed reaction heat by the cold pipe 7 of built-in multipass heat exchange and is guaranteed that temperature of reaction is about 390 ℃.The heat-eliminating medium of walking in the cold pipe of heat exchange is the oiler feed with boiler water circulating pump 9 pump circulation, and the gas-vapor mix after the heat exchange will enter the high pressure steam of drum 8 by-product 40bar.The adding mode of feedwater not only can add from the top of drum, also can directly add from the inlet of boiler water circulating pump 9, can realize in emergency circumstances the demand of cooling rapidly.The gas inlet operate at line speeds of determining according to service temperature, working pressure and the inlet flow rate of reactor 5 is about 0.6m/s.
The volumetric concentration of fluidized-bed bed emulsion zone catalyzer is 10%.For activity, selectivity and the loading capacity kept stable that guarantees catalyst in reactor, need regularly carry out the online interpolation and the discharging of catalyzer.Live catalyst in the catalyst charge groove 23 is transported in the reactor 5 by the high pressure nitrogen of trench bottom, and by regulating catalyst charge groove 23 pressure, the differential pressure between assurance catalyst charge groove 23 and the reactor 5 guarantees the adding speed of catalyzer.Catalyst charge groove 23 tops are provided with a charge chute strainer 24 and speed to put on the pipeline to prevent that catalyzer from taking to.And the regular discharging of catalyzer is transported to catalyzer blowpit 27 by high pressure nitrogen, by regulating catalyzer blowpit 27 pressure, guarantees the discharge rate that the differential pressure between reactor 5 and the catalyzer blowpit 27 is regulated catalyzer.Because catalyst entrainment is more serious, is provided with two- stage filter 25 and 26 and comes particle in the captured gas.Catalyst charge groove and catalyzer blowpit all have weighing instrument accurately to weigh, and guarantee that catalyst loading is constant substantially.The material gas weight ratio of carrying is 10.
After in fluidized-bed reactor 5 Fischer-Tropsch synthesis taking place, gas-solid mixture captures most granules of catalyst get off through a built-in cyclonic separator 10, and gas enters the dedusting cooling unit again and removes granules of catalyst and the condensation recovery part high temperature condensable product of carrying secretly in the gas.
The dedusting cooling unit comprises following unit equipment: quenching column 11, quenching column recycle pump 13 and quenching column recirculation cooler 14, the dedusting refrigerating function is finished in quenching column 11.
The gases that enter in the quenching column 11 have passed through twice washing and cooling: at first, the tower bottoms body portion is extracted out, through 13 circulations of quenching column recycle pump, is cooled to 120 ℃ by quenching column recirculation cooler 14, delivers on the top tray ascending gas to be washed and cool off; Ascending gas contacts at cat head with liquid from cryogenic condensation thing medial launder 19 more then, washs and cools off, and sends quenching column at last.After above washing and cooling, the essentially no granules of catalyst of exit gas is carried secretly, and temperature out is cooled to 170 ℃.
The incoming stock gas one-level of the gas preheater 2 that goes out quenching column 11 carries out heat exchange with unstripped gas and is cooled to 120 ℃, enters quenching column water cooler 17 again with gas cooling to 40 ℃, enters triphase separator 18.In triphase separator, with the unstripped gas of fresh synthesis gas as reactor inlet, the small part gas that acts as a fuel enters pipe network to gas phase as tail gas overwhelming majority circulation; Water enters reaction water medial launder 21, removes the oxygen-bearing organic matter in the rectifying recovery unit recycle-water after the decompression; Oil phase enters 19 decompressions of cryogenic condensation thing medial launder, and portioned product is sent to quenching column 11 as the cooling washing liq with cryogenic condensation thing recycle pump 20, and portioned product is sent to the pan tank unit.
The high temperature condensation product process filter 15 that comes out in the quenching column bottom removes by filter the granules of catalyst in the liquid, enters 16 decompressions of high temperature condensation product medial launder then, and the high temperature condensation product after the flash distillation is sent to the pan tank unit as product.
Used catalyzer is the high-temp and high-strength iron-base fischer-tropsch synthesis catalyst.
The implementation result of the described device of present embodiment is as follows:
(1) unstripped gas two-stage heat exchange has made full use of the heat of quenching column outlet hot gas, reasonable energy utilization.
(2) by regularly carrying out the online discharging and the interpolation of catalyzer, in constant cycle of operation, activity of such catalysts, selectivity and charge capacity change little, and be basicly stable in operational condition; Catalyzer and pipe wear under the nitrogen dilute phase is carried are few.
(3) drum system byproduct steam is stable, and service temperature is easy to adjust when fluctuation occurring
(4) the gas solid content behind built-in cyclonic separator separate solid is low and stable, and the catalyst loss amount is few
(5) by washing and cooling, the solid content in the gas of quenching column outlet all is reduced to below the 1ppm basically, has guaranteed the stable operation of follow-up cooling heat exchanger; Quenching column tower top temperature control stabilization is stabilized in about 170 ℃.
(6) at device continuously in 30 days of operation, the fault of parking does not appear causing because of technology or equipment reason.
(7) the CO+CO2 total conversion rate remains on more than 80%, and the above component selectivity of C5 is not less than 50%.
As shown in Figure 2, be a schema of producing the full scale plant of 1,000,000 tons of oil products per year.Basic identical with Fig. 1, difference mainly is to be that the dedusting cooling unit is made up of an electric precipitator 42, a water cooler 43 and a separator 44, and in addition, flow process is not always from 49 backflow cryogenic condensation product of cryogenic product medial launder.
Because other parts are basic consistent with embodiment, narrate following dedusting cooling unit here emphatically.The gas that comes out from reactor 36 at first enters an electric precipitator 42, remove most catalyst solid particles of carrying secretly in the gas, enter water cooler 42 coolings then, in separator 44 the high temperature condensable product is reclaimed, gas goes follow-up gas-gas heat exchanger 31 further to cool off.
This method has been simplified flow process, saved the investment of a rectifying tower and two pumps, but increased the investment of electric precipitator, it is economically feasible that such configuration object is produced 1000000 tons of such full scale plants of the above rank of oil product per year, the result shows: though the equipment gross investment increases to some extent, the maintenance cost of equipment reduces.
The efficiency of dust collection of the described device of present embodiment is with approaching with embodiment 1, and other implementation results are also suitable substantially, but the continous-stable cycle of operation is considerably beyond the pilot plant of embodiment one.Wherein, CO+CO
2Total conversion rate remains on more than 81%, and the above component selectivity of C5 is between 50%~60%.
Claims (10)
1. one kind is utilized fluidized-bed reactor to carry out Fischer-Tropsch synthetic method, it is characterized in that this method comprises following processing step:
(1) with H
2With CO be the fresh synthesis gas of main component with after circulation gas mixes, through the recycle compressor pressurization and be heated to temperature through one or more levels interchanger and be not less than 100 ℃, enter fluidized-bed reactor, Fischer-Tropsch synthesis takes place under the effect of fischer-tropsch synthetic catalyst; Temperature of reaction is 300~500 ℃, and pressure is that 2.0~5.0MPa, operating linear velocity are 0.3~0.7m/s, and the catalyst body volume concentrations in the fluidized-bed reactor dense-phase bed is 5~30%;
(2) in reactor, guarantee that by distribution device in gas-fluid the fluid distribution of gas fluidized bed is good; Remove heat and byproduct steam by the cold pipe of interior heat exchange; Gas-solid separation equipment by the top remains on catalyzer in the catalytic bed; Need at set intervals that catalyzer is carried out online partial discharge and add to guarantee catalyst concn, activity and average selectivity with part, the long-term continous-stable operation of this technology has been guaranteed in all these measures;
(3) high-temperature gas that comes out from reactor is earlier through a dedusting cooling unit, and granules of catalyst and the recovery part high temperature condensable product removing in the high-temperature gas to be carried secretly are delivered to the product groove after the product of generation reduces pressure after filtration;
(4) gas that comes out from the dedusting cooling unit is after one or more levels interchanger cooling, delivering to a triphase separator separates water, oil phase and gas phase, oil phase is sent to the product groove as the cryogenic condensation product after reducing pressure, send reaction water rectification cell recovery oxygen-bearing organic matter wherein after the water decompression, a gas phase part reclaims wherein behind the available gas composition emptying or the gas that acts as a fuel is used, and the overwhelming majority is circulated by recycle compressor;
(5) the reactor inlet unstripped gas has multiple preheating method, can by with the dust removing units exit gas or/and reactor outlet gas or/and the heat exchange of dust removal installation exit gas, the recovery part heat; Can further provide the part heat in addition with conventional interchanger.
2. a kind of fluidized-bed reactor that utilizes according to claim 1 carries out Fischer-Tropsch synthetic method, it is characterized in that, described catalyzer can be common iron-based, Co based Fischer-Tropsch synthesis catalyst, it also can be the fischer-tropsch synthetic catalyst of other any compositions, employed catalyzer should be able to satisfy in the cycle of long-term operation continuously active and selectivity and stablize not breakable requirement.
3. a kind of fluidized-bed reactor that utilizes according to claim 1 carries out Fischer-Tropsch synthetic method, it is characterized in that described material synthesis gas is with H
2With CO be main, H
2/ CO is than between 0.5~6.
4. a kind of fluidized-bed reactor that utilizes according to claim 1 carries out Fischer-Tropsch synthetic method, it is characterized in that, described reactor is provided with a non-return valve and accident scavenging line at unstripped gas inlet, is used to alleviate and handles the obstruction of operation fluctuation of operating conditions distribution device in gas-fluid greatly the time.
5. a kind of fluidized-bed reactor that utilizes according to claim 1 carries out Fischer-Tropsch synthetic method, it is characterized in that, the online interpolation of the catalyzer of described reactor and the realization of discharging, need one or more catalyzer medial launders, be used for catalyst charge and discharging, the outlet of medial launder is provided with the particle that one or more strainers are carried secretly when capturing catalyst transport, and the bottom has weighing instrument accurately to weigh to guarantee that the catalyst in reactor load is constant substantially.
6. a kind of fluidized-bed reactor that utilizes according to claim 5 carries out Fischer-Tropsch synthetic method, it is characterized in that, described catalyst charge and discharging are carried by the high pressure gas dilute phase, material gas weight ratio, the ratio that is catalyzer and high pressure gas conveying weight rate is 5~30, is not prone to obstruction with the degree of wear that reduces catalyzer and pipeline; The adding speed of catalyzer or the speed that draws off are mainly regulated by the differential pressure between catalyzer medial launder and the reactor; Described high pressure gas can be high-pressure inert gas such as nitrogen, also can be high-pressure process gas such as synthetic gas.
7. a kind of fluidized-bed reactor that utilizes according to claim 1 carries out Fischer-Tropsch synthetic method, it is characterized in that, the preheating method of described inlet unstripped gas is determined according to heat exchange network optimization design, and is the highest to guarantee the energy comprehensive utilization ratio.
8. a kind of fluidized-bed reactor that utilizes according to claim 1 carries out Fischer-Tropsch synthetic method, it is characterized in that described dedusting cooling unit can adopt one of following dual mode:
(1) the quenching column washing type of cooling;
(2) gas solid separation postcooling mode.
9. a kind of fluidized-bed reactor that utilizes according to claim 8 carries out Fischer-Tropsch synthetic method, it is characterized in that, the dedusting cooling unit of the described employing quenching column washing type of cooling is made up of quenching column, quenching column recycle pump and quenching column recirculation cooler at least, and the dedusting refrigerating function is finished in quenching column.
10. a kind of fluidized-bed reactor that utilizes according to claim 8 carries out Fischer-Tropsch synthetic method, it is characterized in that the dedusting cooling unit of described employing gas solid separation postcooling mode is made up of gas-solid separation equipment, water cooler, gas-liquid separator at least; Gas-solid separation equipment can be equipment such as electric precipitator or strainer, and the heat-eliminating medium of water cooler can be general heat-eliminating medium, also can be the process gas of reactor into.
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