CN101328415A - Piston type fluidized bed low temperature dry distillation technological process - Google Patents
Piston type fluidized bed low temperature dry distillation technological process Download PDFInfo
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Abstract
The invention relates to a process method for low temperature carbonization on a fluidized bed. The process method uses the principle of a lift pipe fluid catalytic cracker, uses a lift pipe reactor of the lift pipe fluid catalytic cracker as a carbonization reactor, uses a catalyst regenerator of the lift pipe fluid catalytic cracker as a high-temperature water gas generator, and uses high-temperature water gas as a fluidizing medium and a heat carrier of a carbonization raw material. The carbonization method comprises the following steps that: a carbonizing raw material is conveyed to the lift pipe fluidized bed reactor for a carbonization reaction of the raw material; the reacted oil and gas are separated to produce a carbonized product; carbonized carbocoal enters the water gas regenerator; carbon in the carbonized carbocoal, oxygen and water vapour in air are subjected to oxidation reaction and water gas reaction; the water gas obtained in the reaction is used as the fluidizing medium and the heat carrier during the carbonization process; and solid clinkers produced after the carbonized carbocoal is subjected to the water gas reaction are discharged. Compared with the prior art, the method has the advantages of simple process, high production capacity, less equipment and so on, and can be used in oil shale, oil sand, coal and other substances to produce liquid petroleum products.
Description
Technical field
The present invention relates to a kind of derived energy chemical technology, particularly low-temperature pyrolysis Technology specifically relates to solid mineral piston type fluidized bed low temperature dry distillation technological process such as a kind of resinous shale, oil-sand, peat, coal.
Background technology
Along with worldwide Economic development, the oil consumption in the global range constantly increases, and causes oil supply day to be becoming tight, and oil price is constantly soaring, and energy security becomes global problem.Particularly in China, because rapid economy development, the consumption of oil increases rapidly, but domestic crude production rate far can not be caught up with growth of requirement speed, cause the crude oil import amount to increase progressively fast year by year, Chinese crude oil in 2007 and processed oil import volume surpass 1.8 hundred million tons, and externally interdependency reaches 47%, barrier line near 50%, the seriously energy security of prestige association China.
In order to reduce the dependence to Imported oil, country is implementing corresponding national Oil Safety strategy, as carries out national strategic oil reserve, optimizes energy structure, develops substitute energy etc. in good time.Wherein, solid energy pyrolysis oil preparation technology such as resinous shale, oil-sand, coal, peat are competitive substitute energy developing direction because of method is simple relatively, investment is less.Along with the intensification of oil production degree, the ratio of mink cell focus increases, and effective utilization of super viscous crude more and more causes people's attention as lighting.The gas of resinous shale, oil-sand, coal/solid heat carrier rapid pyrolysis technical market has a extensive future, and good economic benefit and good environment social benefit are arranged.Resources such as the coal of China, resinous shale and oil-sand are abundanter, also are the favourable condition of carrying out the substitute energy technology.
The retorting technique development of the solid energy such as resinous shale, oil-sand, coal, peat has early formed some representative industrial technologies, reclaims Technology, maoming oil shale fluidized retoring Technology etc. as Fushun type retort and product.
The history in existing 80 years of Fushun type retort is still occupied an leading position in the oil shale distillation field, is representing the traditional retorting technique level of China.Fushun type retort is upright cylinder internally heated retort oven, and top is retort section, and the bottom is a gasification section.Saturated air is in furnace bottom enters stove, and the gas that generates with the burning of fixed carbon in the semicoke mixes with thermal cycling coal gas, finishes dry distillation reactor by the bed of material.Oil gas is derived by furnace roof, enters direct washing recovery system, obtains shale oil through separation.
The characteristics of Fushun type retort: 1) furnace binding is simple; 2) can handle the low lean ore resinous shale of oil length; 3) make full use of fixed carbon in the semicoke, heat is self-sufficient and achieve a surplus; 4) go into operation comparatively convenient.
The shortcoming of Fushun type retort: 1) go into furnace oil shale piece footpath 12～75mm, the resinous shale utilization ratio only is 80%, and＜12mm resinous shale is rejected; 2) resinous shale of giving up takies a large amount of soils, has polluted environment; 3) tar productivity hangs down 60～65%; 4) single stove processing power is little, and throughput is low; 5) caloric power of gas is low; 6) directly washing, water loss are big, sewage disposal expense height.
Oil company, Maoming in 1967 build up (1 ton of raw material)/time resinous shale fluidized retoring Technology (imitative IV type catalytic cracking unit), be two device fluidized retoring devices, resinous shale fluidized retoring Technology mainly adopts the fluidization of solid principle.Resinous shale is made particle below 500 microns, fluidized retoring de-oiling after drying, oil gas condensation are reclaimed, and the powder after the de-oiling enters the fluidisation device of making charcoal and makes charcoal, high temperature shale ashes after burning are as thermal barrier and fresh feed HYBRID RETORTING, and unnecessary shale ashes efflux.The industrial experiment device debugged in 1974, finish industrial experiment, for the design large-scale plant provides data and practical experience.Main operational condition is as follows:
(1) flow velocity 0.4～0.6m/S in the reactor
(2) residence time of material 3～6min
(3) reactor temperature is 470～480 ℃
110～120 ℃ of (4) the two device temperature difference
(5) bed density 160～220kg/m
3
(6) heat requirement 200,000 Kcal/t of reactor institute
In March, 2004～2004 year October, rich Shen, Shanghai build up in Harbin Gas Works (2 tons of raw materials)/time resinous shale fluidized retoring oil refining industrial experiment device-imitative IV type catalytic cracking unit; In November, 2004～2005 year June, the fs industrial experiment is debugged and finished to the industrial experiment device, fully verified the feasibility and the advance of resinous shale fluidized retoring technology.The main operational condition of fluidized reaction is similar to maoming oil shale fluidized retoring technology with technological process.
Maoming oil shale fluidized retoring Technology adopts solid high temperature shale ashes as thermal barrier and fresh feed HYBRID RETORTING, influenced the throughput of distillation apparatus, and owing to be the boiling type fluidized-bed, there is more serious air-teturning mixed phenomenon, cause secondary reactions such as olefinic polymerization, influenced product yield.
CN1621493A title " oil shale material fluidized bed dry distillation and decarbonization process " report: utilize the fluidized-bed reaction principle, the powdery resinous shale is under fluidized state, with high temperature dry gas and/or high-temperature steam is thermal barrier and fluidizing medium, with the shale oil gasification that contains in the resinous shale, dry gas also has certain solvency action to the organism in the resinous shale, i.e. fluidized retoring de-oiling simultaneously.Resinous shale (semicoke) after the separation de-oiling is under the condition of oxygen enrichment, with the carbon in the high temperature air fluidisation and the shale that burns, i.e. fluidized decarbonization.The high-temperature flue gas that the decarburizing reaction device produces is provided with energy-recuperation system, and flue gas discharges after deviating from compound such as sulphur nitrogen after the energy recovery.The main deficiency of this method is system complex, not only comprise two fluidized-bed reactors and supporting relevant device, the heating system of high-temperature flue gas energy-recuperation system and hot carrier gas etc. also need be set, and these systems all are the work systems under the hot environment, and investment and process cost are all higher.
Summary of the invention
At the deficiencies in the prior art, the invention provides a kind of piston type fluidized bed low temperature dry distillation technological process, it is reasonable that the inventive method has Btu utilization, and flow process and equipment are simple, and plant capacity is big, the oil yield rate advantages of higher.
Piston type fluidized bed low temperature dry distillation technological process of the present invention comprises following content, utilize the lifting tube flowing catalytic cracking device principle, riser reactor with lifting tube flowing catalytic cracking device is the dry distillation reactor device, catalyst regenerator with lifting tube flowing catalytic cracking device is the high-temperature water gas producer, with the high-temperature water gas is the fluidizing medium and the thermal barrier of destructive distillation raw material, the destructive distillation raw material is transported in the riser tube fluidized-bed reactor, in riser reactor, carry out the dry distillation reactor of raw material, material is through settling vessel behind the dry distillation reactor, reaction back oil gas enters separation system from settling vessel and obtains the destructive distillation product, the solid matter of settling vessel is the destructive distillation semicoke, the destructive distillation semicoke enters water-gas machine, the water-gas machine bottom feeds water vapor and air, in the high-temperature water gas producer, carbon in the destructive distillation semicoke, airborne oxygen and water vapor carry out oxidation and water-gas reaction, the water-gas that reaction obtains is used as the fluidizing medium and the thermal barrier of retort process, and the solid lime-ash that the destructive distillation semicoke carries out after the water-gas reaction is discharged.
In the inventive method, the destructive distillation raw material can be various solid energy substances, as resinous shale, oil-sand, coal, peat etc., can be a kind of, also can be wherein several mixtures.The destructive distillation raw material generally need be crushed to certain particle size, so that carry out fluidized-bed reaction, general granularity preferably below 6mm, is preferably in below the 3mm below 10mm.Breaking method and equipment can adopt the method and apparatus of this area routine, as high pressure pulverizing mill etc.
In the inventive method, the fluidized bed dry distillation condition is generally 450～520 ℃ of temperature, is preferably 470～500 ℃, and the reaction times was generally 1～10 second, was preferably 2～5 seconds.Other operational condition requires and the temperature of reaction requirement according to goods fluid as gas-solid ratio, inlet air temperature degree etc., can determine by the existing knowledge design in this area.The also available dry gas of riser reactor inlet water coal gas, stack gas, superheated vapour etc. carry out flow and temperature adjustment.
In the inventive method, the service temperature of high-temperature water gas producer is 620～900 ℃, is preferably 700～790 ℃, and reaction pressure 0.15～0.20MPa is preferably 0.18MPa.Water vapour that feeds and air (4～8: 4v/v), gas-solid ratio 4.5: 1v/v; Water generation reaction coal gas and lime-ash.Other condition can be determined by the design of this area general knowledge according to the requirement of goods fluid and temperature of reaction.
In the inventive method, other operational condition can be by the fluidization principle, correlated condition with reference to fluid catalytic cracking, the dry distillation of coal, oil shale distillation and water-gas production process is determined, can suitably adjust according to raw material properties simultaneously, can be-0.2～0.5MPa as working pressure, water-gas machine and riser reactor gas phase pressure reduction are 15～25kPa etc.
In the inventive method, separation system can be isolated products such as water-gas, dry gas, thick gas and oil, gas oil, heavy oil that obtains in the separation system and slurry oil can loop back riser reactor, also can discharge further processing, and perhaps part loops back riser reactor and partly discharges processing.
Can transform a little having riser fluid catalytic cracking now in the inventive method, also can build new device by riser tube catalytic unit principle design.If transform existing riser fluid catalytic cracking, only need increase the destructive distillation raw material feeder can operate, and during operation, the solid lime-ash in the high-temperature water gas producer is discharged, and also can small amount of recycled return riser tube dry distillation reactor device.The solid lime-ash of discharging still has higher temperature, can carry out heat recuperation.The inventive method is that the throughput of the destructive distillation raw material fluidizing medium and the thermal barrier mode of production is 4～5 times of solid thermal carriers mode throughput with the high-temperature water gas.
Fluidized bed low temperature dry distillation technological process of the present invention utilizes riser tube fluidisation catalytic unit principle, in conjunction with the distillation process characteristics, with riser reactor design is the dry distillation reactor device, revivifier is designed to the high-temperature water gas producer, the high-temperature water gas producer is at high temperature operated, delivery medium and thermophore that the high-temperature water gas that obtains directly reacts as riser tube fluidized retoring, simplified technical process on the one hand, reduced device quantity, high temperature service quantity particularly, also improve the throughput of device greatly, improved production efficiency.In addition,, reduced calorific loss, improved heat utilization ratio owing to reduced system and device.By semicoke being carried out the high-temperature water gas reaction, in byproducts such as the valuable service water coal gas of acquisition, effectively controlled the reaction liberated heat, this heat enough is used for retort process.Adopt riser reactor, reaction mass is the plug flow state in reactor, and no air-teturning mixed phenomenon has been avoided the reactions such as after polymerization of alkene, has improved tar productivity.
Description of drawings
Fig. 1 is a kind of idiographic flow synoptic diagram of fluidized bed low temperature dry distillation technological process of the present invention (will have riser fluid catalytic cracking now simply transforms).
Wherein: 1-riser reactor, 2-settling vessel, 3-high-temperature water gas producer, 4-separation column, 5-destructive distillation raw material feeder, 6-main air blower, 7-circulation oil tank, the 8-reaction oil gas, 9-rich gas, 10-raw gasline, the 11-solar oil, 12-heavy gas oil, 13-slurry oil, 14-water-gas, 15-lime-ash, 16-high-temperature water gas generator inlet water vapor, the 17-riser reactor replenishes gas, 18-lime-ash cooling Low Temperature Steam, 19-heavy oil.
Embodiment
Further specify the inventive method and technique effect below in conjunction with accompanying drawing.
As shown in Figure 1, the inventive method can simply be transformed having lifting tube flowing catalytic cracking device now.The destructive distillation raw material is transported to the opening for feed of riser reactor 1 through destructive distillation raw material feeder 5, transmission through high-temperature water gas 15 and the additional gas 17 of riser reactor, enter riser reactor 1 and carry out dry distillation reactor, reacting rear material enters settling vessel 3, in settling vessel 3, high-temperature water gas producer 3 is separated and entered to consubstantiality material (destructive distillation semicoke), gaseous substance (reaction oil gas 8) enters separation column 4 to be separated, after separating, can obtain rich gas 9 (comprising dry gas and water-gas), raw gasline 10, solar oil 11, heavy gas oil 12, slurry oil 13 and heavy oil 19 etc., various products can further be handled use.Separation column 4 isolated heavy oil and slurry oil can all or part ofly loop back the further reaction of riser reactor and obtain light-end products.
In high-temperature water gas producer 3, main air blower 6 delivers air in the high-temperature water gas producer, high-temperature water gas generator inlet water vapor 16 enters from high-temperature water gas producer 3 bottoms, destructive distillation semicoke and airborne oxygen and water vapor carry out oxidation and water-gas reaction, and the high-temperature water gas 14 of generation partly or entirely is used for the fluidization delivery medium and the thermal barrier of riser reactor 2.The lime-ash that carries out after oxidation and the water-gas reaction is discharged after Low Temperature Steam 18 heat exchange.
Design the production equipment of following structural parameter and operating parameters.
Riser reactor: diameter 1124mm, height 27200mm, wall thickness 12mm
Riser reactor temperature: 470～500 ℃
The dry distillation reactor time: 2.7s
High-temperature water gas generator temperature: 700～790 ℃
Settling vessel pressure: 1.5～1.7kg/cm
2
Two tower pressure reduction: 0.15～0.25kg/cm
2
Riser reactor replenishes gas: ≮ 2000m
3/ h
Main air blower flow: 100320Nm
3/ hmax
High-temperature water gas steam of generator amount: 1800～3000kg/h
Heavy oil goes out device, not cyclical operation, and slurry oil all loops back riser reactor.
Carry out following embodiment and comparative example experiment by said apparatus and condition.
Raw material: maoming oil shale (character is mass content) water ratio 2%, oil length 7.15%, tar productivity＞95% is produced 1 ton of about 14 tons of resinous shale of oil require.
Produce by 6,000,000 t/a (destructive distillation raw material treatment capacity) treatment capacity, adopt the as above riser tube fluidized retoring-water-gas production equipment of parameter and condition.Deliver to raw material tank below its granularity of powdery maoming oil shale 3mm, through spiral propeller, deliver to the riser reactor lower end, adjust high-temperature water gas temperature to 650～680 ℃ with superheated vapour, enter in the riser reactor with 750t/h powdery maoming oil shale, reaction mass passes through riser reactor, semicoke and gas-oil separation in settling vessel with the plug flow fluidized-bed reaction; The destructive distillation semicoke is delivered to the high-temperature water gas producer, generates process water coal gas with superheated vapour and warm air reaction.Oil gas is delivered to oil and gas separating system to be separated, and obtains all gases and liquid product.
Powdery maoming oil shale working ability: 7,50t,/h=,600 ten thousand t/a
650～680 ℃ gaseous heat-carrier: keep system's thermal equilibrium aequum
Product: liquid oil 42.75 ten thousand t/a
Dry gas 31,800 ten thousand m
3/ a
Lime-ash 4,420,000 t/a
(amount of burnt 360,000 t/a)
Water-gas 56,265 ten thousand m
3/ a
Water-gas (CO+H
2)＞89% (volume), (H
2)/(CO)=2 (volume).
Comparative example 1
Pressing device and the condition of embodiment 1, is the dry distillation reactor that thermal barrier carries out raw material with the solid lime-ash just.Be mixed in the riser reactor by 600t/h solid shale lime-ash thermal barrier and powdery 150t/h maoming oil shale.
Powdery maoming oil shale working ability: 1,50t,/h=,120 ten thousand t/a
Can get: liquid oil 8.6 ten thousand t/a
Dry gas 6,360 ten thousand m
3/ a
Lime-ash 88.5 ten thousand t/a
Amount of burnt 7.26 ten thousand t/a
Water-gas 11,253 ten thousand m
3/ a
With the solid lime-ash is thermal barrier, and for identical production equipment, its processing power reduces greatly.
Raw material: Angola's oil-sand (character is mass content) water ratio＜3.5%, oil length 10%～15%, tar productivity＞95% is produced 1 ton of about 10.5 tons of oil-sand of oil require, gas production rate 30m
3/ t.
According to 6,000,000 t/a oil shale processes device and the conditions of embodiment 1, replace maoming oil shale with Angola's oil-sand.
Powdery Angola oil-sand working ability 7,50t,/h=,600 ten thousand t/a
650～680 ℃ gaseous heat-carrier: keep system's thermal equilibrium aequum
Can get: liquid oil 570,000 t/a
Dry gas 18,000 ten thousand m
3/ a
Lime-ash 5,290,000 t/a
(amount of burnt 30,000 t/a)
Water-gas 11,625 ten thousand m
3/ a
Raw material: brown coal (mass content) water ratio＜3.5%, tar productivity are 150%～180% of aluminium rice steamer yields, produce 1 ton of about 5 tons of brown coal of oil require, gas production rate 200m
3/ t.
Powdery brown coal working ability: 7,50t,/h=,600 ten thousand t/a
650～680 ℃ gaseous heat-carrier: keep system's thermal equilibrium aequum
Can get: liquid oil 1,200,000 t/a
Dry gas 12,000 ten thousand m
3/ a
Lime-ash 930,000 t/a
(amount of burnt 4,290,000 t/a)
Water-gas 6,641,750,000 m
3/ a
With Fischer-Tropsch process water-gas synthetic petroleum: with water-gas 6,641,750,000 m
3/ a
Can get: light synthetic 2,190,000 t/a are C wherein
5 +1,280,000 t/a
By-product CO
22,190,000 t/a
Use water-gas hydrogen manufacturing, can get high-purity H
2: 300,000 t/a.
Claims (10)
1, a kind of fluidized bed low temperature dry distillation technological process, utilize the lifting tube flowing catalytic cracking device principle, it is characterized in that: the riser reactor with lifting tube flowing catalytic cracking device is the dry distillation reactor device, catalyst regenerator with lifting tube flowing catalytic cracking device is the high-temperature water gas producer, with the high-temperature water gas is the fluidizing medium and the thermal barrier of destructive distillation raw material, the destructive distillation raw material is transported in the riser tube fluidized-bed reactor, in riser reactor, carry out the dry distillation reactor of raw material, material is through settling vessel behind the dry distillation reactor, reaction back oil gas enters separation system from settling vessel and obtains the destructive distillation product, the solid matter of settling vessel is the destructive distillation semicoke, the destructive distillation semicoke enters water-gas machine, the water-gas machine bottom feeds water vapor and air, in the high-temperature water gas producer, carbon in the destructive distillation semicoke, airborne oxygen and water vapor carry out oxidation and water-gas reaction, the water-gas that reaction obtains is used as the fluidizing medium and the thermal barrier of retort process, and the solid lime-ash that the destructive distillation semicoke carries out after the water-gas reaction is discharged.
2, in accordance with the method for claim 1, it is characterized in that: described destructive distillation raw material is the solid energy substance, comprises in resinous shale, oil-sand, coal and the peat one or more.
3, in accordance with the method for claim 1, it is characterized in that: riser tube fluidized bed dry distillation condition is 450～520 ℃ of temperature, and the reaction times is 1～10 second.
4, in accordance with the method for claim 1, it is characterized in that: riser tube fluidized bed dry distillation condition is 470～500 ℃ of temperature, and the reaction times is 2～5 seconds.
5, in accordance with the method for claim 1, it is characterized in that: the service temperature of high-temperature water gas producer is 620～900 ℃.
6, in accordance with the method for claim 1, it is characterized in that: the service temperature of high-temperature water gas producer is 700～790 ℃.
7, in accordance with the method for claim 1, it is characterized in that: isolated heavy oil of separation system and slurry oil loop back riser reactor, perhaps discharge further and handle, and perhaps part loops back riser reactor and partly discharges processing.
8, in accordance with the method for claim 1, it is characterized in that: destructive distillation raw material pulverizing to granularity is below the 6mm.
9, in accordance with the method for claim 1, it is characterized in that: the throughput that with the high-temperature water gas is the destructive distillation raw material fluidizing medium and the thermal barrier mode of production is 4～5 times of solid thermal carriers mode throughput.
10, in accordance with the method for claim 1, it is characterized in that: the water-gas of riser reactor inlet carries out flow and temperature adjustment with dry gas, stack gas or superheated vapour.
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