CN103131448B - Method and device for fluid-bed destructive distillation of oil shale - Google Patents
Method and device for fluid-bed destructive distillation of oil shale Download PDFInfo
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- CN103131448B CN103131448B CN201110413827.1A CN201110413827A CN103131448B CN 103131448 B CN103131448 B CN 103131448B CN 201110413827 A CN201110413827 A CN 201110413827A CN 103131448 B CN103131448 B CN 103131448B
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Abstract
The invention discloses a method and a device for fluid-bed destructive distillation of oil shale. The method and the device for the fluid-bed destructive distillation of the oil shale solve the problems caused by high coal burning load borne by a coal burning device in an existing destructive distillation technique and also solve the problem of low extraction rate of shale oil. The method for the fluid-bed destructive distillation of the oil shale comprises the steps that a section of destructive distillation reaction is carried out on oil shale raw materials (27) and high-temperature heat carriers after the oil shale raw materials (27) and the high-temperature heat carriers are mixed in a lifting pipe destructive distillation reactor (24); the oil shale raw materials enter a bed type destructive distillation reactor (21) for a second section of destructive distillation reaction after the first section destructive distillation reaction is carried out on the oil shale raw materials, and then mixed carbocoal is formed and enters a pipe type coal burning device (14) after oil gas contained in the mixed carbocoal is extracted in a steaming mode; and a section of coal burning is carried out on the mixed carbocoal which enters the pipe type coal burning device; and the mixed carbocoal enters a bed type coal burning device (5) for a second section of coal burning after the first section coal burning is carried out on the mixed carbocoal. The invention discloses the device for the fluid-bed destructive distillation of the oil shale, wherein the device for the fluid-bed destructive distillation of the oil shale is used for realizing the method for the fluid-bed destructive distillation of the oil shale. The method and the device for the fluid-bed destructive distillation of the oil shale are mainly used for destructive distillation processing of various kinds of powder oil shale raw materials.
Description
Technical field
The invention belongs to oil shale distillation technical field, relate to a kind of fluidized bed dry distillation method and apparatus of resinous shale.
Background technology
Along with the scarcity day by day of petroleum resources and the arrival of Waste Era of Oil, countries in the world utilize oil shale distillation technology to produce shale oil, have become important aspect alternative, that supplement petroleum resources.Resinous shale is called again oil shale, is that one contains organic sedimentogeneous rock.Organism in resinous shale consists of two kinds of materials conventionally: a kind of is bituminous matter, and another kind of is high molecular polymer (being referred to as oil female).Inorganics in resinous shale mainly contains quartz, kaolin, clay, mica, carbonatite and sulfurous iron ore etc.Resinous shale, after heating destructive distillation, generates shale oil, carbonization gas and shale semicockes.Shale oil can, directly as oil fuel, also can further produce the vehicle fuels such as gasoline, diesel oil.The fluidized bed dry distillation technology of resinous shale, there is the features such as destructive distillation hot strength is high, dry distillation rate fast, the shale oil quality better of generation, oil-collecting ratio height, referring to the introduction of the documents such as Chinese patent CN101440293A, < < Coal Chemical Industry > > magazine the 3rd phase of June in 2009 " resinous shale solid thermal carriers fluidized retoring oil refining process pilot scale research " (document 1).
Technique described in CN101440293A and document 1, make charcoal in device, make charcoal generated high-temperature heat carrier (cycling hot ash or high temperature shale ashes) some after heat-obtaining, discharge destructive distillation device, separately some mixes, is heated with resinous shale raw material; After dry distillation reactor, generate the mixing semicoke that shale semicockes and thermal barrier mix, mix semicoke and generate high-temperature heat carrier at the burning-off coke in device of making charcoal.Use high-temperature heat carrier as oil shale distillation thermal source, energy consumption is lower.The composition of high-temperature heat carrier of the present invention, the high temperature shale ashes that the device of making charcoal described in the cycling hot ash that the device (being circulating fluidized bed combustor) that is equivalent to make charcoal described in CN101440293A generates or document 1 generates.
Mainly there are following two problems in above-mentioned two kinds of retorting techniques.1. be all a large amount of high heating value mixing semicokes that generate after dry distillation reactor all to be sent into the device of making charcoal make charcoal (being burning-off coke), the load of making charcoal that the device that makes to make charcoal is born is higher, causes that charcoal temperature is difficult to control, the easy overtemperature of the device of making charcoal damages.2. only with a fluidized bed dry distillation reactor, carry out dry distillation reactor, because part resinous shale raw material reaction is incomplete, make the yield of shale oil lower, generally can only account for 75%～85% of resinous shale raw material oleaginousness.
Summary of the invention
The object of this invention is to provide a kind of fluidized bed dry distillation method and apparatus of resinous shale, with solve existing oil shale fluidized bed dry distillation technology existing because of use the device of making charcoal to make charcoal to make make charcoal the load of making charcoal that device bears higher, cause charcoal temperature to be difficult to the problem of controlling and the easy overtemperature of the device of making charcoal damages, because using a fluidized bed dry distillation reactor to carry out dry distillation reactor, make the problem that shale oil yield is lower in addition.
For addressing the above problem, the technical solution used in the present invention is: a kind of fluidized bed dry distillation method of resinous shale, is characterized in that: the method in turn includes the following steps:
A. the resinous shale raw material after pulverizing enters the bottom of riser tube dry distillation reactor device through resinous shale material feeding tube, the high-temperature heat carrier that bed formula is made charcoal in device enters the bottom of riser tube dry distillation reactor device through high-temperature heat carrier transfer lime, after resinous shale raw material mixes with high-temperature heat carrier, up along riser tube dry distillation reactor device under the castering action of the lift gas being passed into by the bottom of riser tube dry distillation reactor device, carry out one section of dry distillation reactor;
B. the resinous shale raw material after one section of dry distillation reactor and the thermal barrier mixing with it, the shale oil and the carbonization gas that also have one section of dry distillation reactor to generate, by the outlet of riser tube dry distillation reactor device, enter bed formula dry distillation reactor device, resinous shale raw material after one section of dry distillation reactor carries out two sections of dry distillation reactors in bed formula dry distillation reactor device dense bed, obtain the shale oil that two sections of dry distillation reactors generate, carbonization gas and shale semicockes, shale semicockes and thermal barrier in bed formula dry distillation reactor device dense bed are mixed to form mixing semicoke mutually, the cyclonic separator of the oil gas that one section and two sections of dry distillation reactors generate in being located at bed formula dry distillation reactor device isolated and mixed half and defocusedly by bed formula dry distillation reactor device, flowed out, mixing semicoke in bed formula dry distillation reactor device dense bed flows downward, enter the stripping stage of being located at bed formula dry distillation reactor device below, in stripping stage, pass into water stripping steam, stripping goes out to mix semicoke entrained oil gas, mixing semicoke in stripping stage after stripping flows to the bottom of stripping stage, through semicoke transfer lime, enter the make charcoal bottom of device of tubular type,
C. enter the mixing semicoke that tubular type makes charcoal in device and contact with one section of air of making charcoal, along tubular type, making charcoal, device is up to carry out one section and makes charcoal;
D. one section of mixing semicoke after making charcoal enters the bed formula device of making charcoal by the make charcoal outlet of device of tubular type, in bed formula is made charcoal device dense bed, contact with two sections of air of making charcoal and carry out two sections and make charcoal, remaining coke on burning-off mixing semicoke, generate high-temperature heat carrier, make charcoal and two sections of flue gases of generating of making charcoal are discharged by the bed formula device of making charcoal after the cyclonic separator of being located at bed formula and making charcoal in device is isolated high-temperature heat carrier for one section, the high-temperature heat carrier that bed formula is made charcoal in device dense bed by bed formula make charcoal device flow out, a part is discharged destructive distillation device after heat-obtaining cooling, another part enters the bottom of riser tube dry distillation reactor device through high-temperature heat carrier transfer lime, mix with resinous shale raw material.
Be used for the fluidized bed dry distillation device of the resinous shale of realizing aforesaid method, comprise a bed formula dry distillation reactor device, the bed formula device of making charcoal, and with bed formula the make charcoal heat-obtaining discharger of high-temperature heat carrier in device dense bed of bed formula that device is connected of making charcoal, bed formula dry distillation reactor device and the bed formula device of making charcoal is set up in parallel, it is characterized in that: the fluidized bed dry distillation device of resinous shale is also provided with a riser tube dry distillation reactor device and the tubular type device of making charcoal, riser tube dry distillation reactor device and bed formula dry distillation reactor device are set up in parallel, tubular type device and the bed formula device of making charcoal of making charcoal coaxially arranges, the bottom of riser tube dry distillation reactor device is provided with resinous shale material feeding tube, bottom is provided with lift gas sparger, the outlet of riser tube dry distillation reactor device passes in bed formula dry distillation reactor device, in bed formula dry distillation reactor device, be provided with cyclonic separator, the top of bed formula dry distillation reactor device is provided with oil gas collection chamber and oil gas vent pipe, below is provided with stripping stage, in stripping stage, be provided with stripping baffles, stripped vapor sparger, the bottom of stripping stage is provided with semicoke transfer lime, the make charcoal bottom of device of the outlet of semicoke transfer lime and tubular type is connected, the make charcoal bottom of device of tubular type is provided with one section of air-distributor of making charcoal, the make charcoal outlet of device of tubular type passes into bed formula and makes charcoal in device, bed formula is made charcoal in device and is provided with cyclonic separator, the make charcoal top of device of bed formula is provided with flue gas collection chamber and smoke outlet tube, bottom is provided with two sections of air-distributors of making charcoal, bed formula is made charcoal and is provided with high-temperature heat carrier transfer lime between device and riser tube dry distillation reactor device, the entrance of high-temperature heat carrier transfer lime passes into bed formula and makes charcoal in device, outlet is connected in the bottom of riser tube dry distillation reactor device, the described bed formula heat-obtaining discharger of high-temperature heat carrier in device dense bed of making charcoal comprises high-temperature heat carrier drainage conduit, the entrance of high-temperature heat carrier drainage conduit and the bed formula device of making charcoal is connected, outlet is connected with heat collector, heat collector is connected with thermal barrier blow-down drum by pipeline, semicoke transfer lime, in high-temperature heat carrier transfer lime and high-temperature heat carrier drainage conduit, be equipped with flowrate control valve.
The present invention adopts fluidization to produce shale oil; Adopt the present invention, there is following beneficial effect: (1) the present invention adopts tubular type device and the bed formula two sections of compound technology of making charcoal of device of making charcoal of making charcoal, and each device of making charcoal is only born a part for the load of always making charcoal, all lower.Like this, just make the charcoal temperature of two devices of making charcoal all easily control, the device overtemperature that prevented from making charcoal damages, and can guarantee the device long-term operation of making charcoal.And, tubular type make charcoal device and bed formula make charcoal the scantlings of the structure of device can be less.(2) two sections of compound technology of making charcoal of the present invention, the ability of making charcoal is strong, mix semicoke and make charcoal completely that (mixing semicoke is made charcoal in device after two sections are made charcoal in make charcoal device and bed formula of tubular type, conventionally can more than 95% coke of burning-off), thereby can recycle more coke heat output.(3) the present invention has used the tubular type device of making charcoal; Make charcoal compared with device with conventional bed formula, the tubular type utensil of making charcoal has the stronger ability of making charcoal and better turndown ratio.In tubular type, make charcoal in device, mix semicoke and contact with fresh air all the time, make to make charcoal speed and the efficiency of making charcoal are higher; Thus, also can reduce the make charcoal reserve of high-temperature heat carrier in device of bed formula, dwindle the make charcoal scantlings of the structure of device of bed formula, reduce investment outlay.(4) the present invention adopts riser tube dry distillation reactor device and two sections of compound destructive distillation reaction technologies of bed formula dry distillation reactor device; Resinous shale raw material carries out after one section of dry distillation reactor in riser tube dry distillation reactor device, and unreacted completely resinous shale raw material can carry out two sections of dry distillation reactors in bed formula dry distillation reactor device, thereby can make the yield of shale oil higher.Under the operational condition proposing in the present invention, shale oil yield can account for 80%～90% of resinous shale raw material oleaginousness.(5) the present invention has used a riser tube dry distillation reactor device, its advantage be simple in structure, turndown ratio good.
The present invention is mainly used in the destructive distillation processing of various granular resinous shale raw materials.
Below in conjunction with accompanying drawing, embodiment and embodiment, the present invention is further detailed explanation.Accompanying drawing, embodiment and embodiment do not limit the scope of protection of present invention.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of the fluidized bed dry distillation device of resinous shale of the present invention.
Embodiment
Referring to Fig. 1, the fluidized bed dry distillation device (referred to as destructive distillation device) of resinous shale of the present invention, comprise a bed formula dry distillation reactor device 21, the bed formula device 5 of making charcoal, and with bed formula the make charcoal heat-obtaining discharger of device dense bed 6 interior high-temperature heat carriers of bed formula that device 5 is connected of making charcoal; Bed formula dry distillation reactor device 21 and the bed formula device 5 of making charcoal is set up in parallel.Destructive distillation device is also provided with a riser tube dry distillation reactor device 24 and the tubular type device 14 of making charcoal; Riser tube dry distillation reactor device 24 is set up in parallel with bed formula dry distillation reactor device 21, and tubular type device 14 and the bed formula device 5 of making charcoal of making charcoal coaxially arranges.As shown in Figure 1, the tubular type device 14 of making charcoal is stretched to bed formula and is made charcoal in device 5 by the make charcoal bottom of device 5 of bed formula.
The bottom of riser tube dry distillation reactor device 24 is provided with resinous shale material feeding tube 26, and bottom is provided with lift gas sparger 31.The outlet of riser tube dry distillation reactor device 24 passes in bed formula dry distillation reactor device 21, is generally the top that is positioned at bed formula dry distillation reactor device dense bed 22 interfaces.The overall structure of the dry distillation reactor of riser tube shown in Fig. 1 device 24, similar to fluid catalytic cracking (FCC) riser reactor in petroleum refining process.Riser tube dry distillation reactor device 24 uses cross section for circular metal tube manufacture, liner insulating and wearing-resistant lining (figure slightly); Vertical height (from top to bottom) is generally 10～40m, and interior diameter is generally 200～5000mm.
The housing of bed formula dry distillation reactor device 21 is mainly comprised of superposed cylindrical metal cylindrical shell and the inverted round table face shape metal cylinder that is positioned at bottom, liner insulating and wearing-resistant lining (figure slightly).In bed formula dry distillation reactor device 21, be provided with cyclonic separator; Cyclonic separator shown in Fig. 1, for the dipleg of the first cyclonic separator 19 of being installed in series and 20, two cyclonic separators of the second cyclonic separator stretches in bed formula dry distillation reactor device dense bed 22 (stretching to the top of bed formula dry distillation reactor device dense bed 22).The top of bed formula dry distillation reactor device 21 is provided with oil gas collection chamber 18 and oil gas vent pipe 33, and below is provided with stripping stage 28; The top of stripping stage 28 is connected with the bottom of bed formula dry distillation reactor device 21.The housing of stripping stage 28 is mainly comprised of a cylindrical metal cylindrical shell, liner insulating and wearing-resistant lining (figure slightly).In stripping stage 28, be provided with stripping baffles (shown in Fig. 1 is herring-bone stripping baffles), stripped vapor sparger 29.The overall structure of the formula of bed shown in Fig. 1 dry distillation reactor device 21-stripping stage 28, similar to FCC settling vessel.
The bottom of stripping stage 28 is provided with semicoke transfer lime 25, which is provided with flowrate control valve 11, to mix the flow of semicoke in control tube.The make charcoal bottom of device 14 of the outlet of semicoke transfer lime 25 and tubular type is connected, and the make charcoal bottom of device 14 of tubular type is provided with one section of air-distributor 15 of making charcoal.
The make charcoal outlet of device 14 of tubular type passes into bed formula and makes charcoal in device 5, is to be generally positioned at the make charcoal top at device dense bed 6 interfaces of bed formula.The make charcoal overall structure of device 14 of tubular type shown in Fig. 1, similar to FCC riser reactor.The tubular type device 14 of making charcoal uses cross section for circular metal tube manufacture, liner insulating and wearing-resistant lining (figure slightly); Vertical height (from top to bottom) is generally 10～40m, and interior diameter is generally 200～5000mm.
The make charcoal housing of device 5 of bed formula is mainly comprised of superposed cylindrical metal cylindrical shell and the inverted round table face shape metal cylinder that is positioned at bottom, liner insulating and wearing-resistant lining (figure slightly).Bed formula is made charcoal in device 5 and is provided with cyclonic separator; Cyclonic separator shown in Fig. 1, for the dipleg of the 3rd cyclonic separator 3 that is installed in series and 4, two cyclonic separators of the 4th cyclonic separator stretches to bed formula, make charcoal in device dense bed 6 (stretch to bed formula make charcoal the top of device dense bed 6).The make charcoal top of device 5 of bed formula is provided with flue gas collection chamber 2 and smoke outlet tube 34, and bottom is provided with two sections of air-distributors 12 of making charcoal.The make charcoal overall structure of device 5 of the formula of bed shown in Fig. 1, similar to FCC revivifier.
Bed formula is made charcoal and is provided with high-temperature heat carrier transfer lime 23 between device 5 and riser tube dry distillation reactor device 24.The entrance of high-temperature heat carrier transfer lime 23 passes into bed formula and makes charcoal in device 5, and being positioned at the bed formula device dense bed 6 of making charcoal (is to be generally positioned at bed formula make charcoal middle part or the bottom of device dense bed 6 height; The outlet of high-temperature heat carrier transfer lime 23 is connected in the bottom of riser tube dry distillation reactor device 24.High-temperature heat carrier transfer lime 23 is provided with flowrate control valve 11, with the flow of high-temperature heat carrier in control tube.
The make charcoal heat-obtaining discharger of device dense bed 6 interior high-temperature heat carriers of described bed formula comprises high-temperature heat carrier drainage conduit 7; High-temperature heat carrier drainage conduit 7 is provided with flowrate control valve 11, with the flow of high-temperature heat carrier in control tube.The entrance of high-temperature heat carrier drainage conduit 7 and the bed formula device 5 of making charcoal is connected, and is to be generally connected in bed formula the make charcoal middle part of device dense bed 6 height or the position of bottom.The outlet of high-temperature heat carrier drainage conduit 7 is connected with the bottom of heat collector 8, and the top of heat collector 8 is connected with the top of thermal barrier blow-down drum 10 by pipeline 9.Heat collector 8 can be used various FCC external warmers, the water (figure slightly) at the general environment for use temperature of heat-obtaining medium.Thermal barrier blow-down drum 10 is a metal vessel.
Each pipeline in destructive distillation device, is all used cross section for circular metal tube, liner insulating and wearing-resistant lining (figure slightly).The interior diameter of each pipeline is mainly determined according to the flow of material and/or medium in each pipeline, density calculation.
Set flowrate control valve 11 in semicoke transfer lime 25, high-temperature heat carrier transfer lime 23 and high-temperature heat carrier drainage conduit 7, can use various conventional for controlling the flowrate control valve of solid powder/particle flow, as used guiding valve.Lift gas sparger 31, stripped vapor sparger 29, one section of make charcoal air-distributor 15 and two sections of air-distributors 12 of making charcoal can be used conventional annular sparger or dendroid sparger.
Adopt the destructive distillation device shown in Fig. 1 to carry out the method (referred to as method for destructive distillation) of oil shale fluidized bed dry distillation of the present invention, in turn include the following steps:
A. the resinous shale raw material 27 after pulverizing enters the bottom of riser tube dry distillation reactor device 24 through resinous shale material feeding tube 26, the high-temperature heat carrier that bed formula is made charcoal in device 5 enters the bottom of riser tube dry distillation reactor device 24 through high-temperature heat carrier transfer lime 23.Resinous shale raw material 27 with high-temperature heat carrier after mix the bottom of riser tube dry distillation reactor device 24, up along riser tube dry distillation reactor device 24 under the castering action of the lift gas 32 being passed into by the lift gas sparger 31 of being located at riser tube dry distillation reactor device 24 bottoms, carry out one section of dry distillation reactor.
B. shale oil and the carbonization gas of the resinous shale raw material after one section of dry distillation reactor and the thermal barrier mixing with it, one section of dry distillation reactor generation in addition, by the outlet of riser tube dry distillation reactor device 24, enter bed formula dry distillation reactor device 21, wherein the resinous shale raw material after one section of dry distillation reactor and the thermal barrier that mixes with it are to falling in bed formula dry distillation reactor device dense bed 22.Resinous shale raw material after one section of dry distillation reactor carries out two sections of dry distillation reactors in bed formula dry distillation reactor device dense bed 22, obtains shale oil, carbonization gas and shale semicockes that two sections of dry distillation reactors generate.
Shale semicockes and thermal barrier in bed formula dry distillation reactor device dense bed 22 are mixed to form mixing semicoke mutually.One section and two sections of oil gas 17 that dry distillation reactor generates, also have at the interior stripping of stripping stage 28 and mix the oil gas that mixing semicoke that half defocused water vapor and stripping go out is carried secretly, it is defocused that the first cyclonic separator 19 in being located at bed formula dry distillation reactor device 21 and the second cyclonic separator 20 are isolated mixing half together, by oil gas collection chamber 18 and oil gas vent pipe 33, by the top of bed formula dry distillation reactor device 21, flowed out, enter fractionating system and carry out fractionation (embodiment 1～embodiment 6 herewith; Figure slightly).Described oil gas, refers to one section and two sections of shale oil and carbonization gas that dry distillation reactor generates.The first cyclonic separator 19 and the isolated mixing semicoke of the second cyclonic separator 20, in dipleg falls into bed formula dry distillation reactor device dense bed 22.
Mixing semicoke in bed formula dry distillation reactor device dense bed 22 flows downward, and enters the stripping stage 28 of being located at bed formula dry distillation reactor device 21 belows.Through stripped vapor sparger 29, in stripping stage 28, pass into water stripping steam 30, stripping goes out to mix semicoke entrained oil gas.Mixing semicoke after the interior stripping of stripping stage 28 flows to the bottom of stripping stage 28, through semicoke transfer lime 25, enters the make charcoal bottom of device 14 of tubular type.
C. enter the mixing semicoke that tubular type makes charcoal in device 14 and contact with the one section of air 16 (pressurized air) of making charcoal being passed into by one section of air-distributor 15 of making charcoal, along tubular type, making charcoal, device 14 is up to carry out one section and makes charcoal.
D. one section of mixing semicoke after making charcoal enters the bed formula device 5 of making charcoal together with one section of flue gas of generating of making charcoal by the make charcoal outlet of device 14 of tubular type.Wherein one section of mixing semicoke after making charcoal is made charcoal in device dense bed 6 to falling into bed formula, in bed formula is made charcoal device dense bed 6, contact with two sections of air 13 (pressurized air) of making charcoal that passed into by two sections of air-distributors 12 of making charcoal and carry out two sections and make charcoal, remaining coke on burning-off mixing semicoke, generates high-temperature heat carrier.
Make charcoal and two sections of flue gases 1 that generate of making charcoal are isolated after high-temperature heat carrier through the 3rd cyclonic separator 3 and the 4th cyclonic separator 4 being located at bed formula and making charcoal in device 5 for one section, by flue gas collection chamber 2 and smoke outlet tube 34, by the make charcoal top of device 5 of bed formula, discharged.The 3rd cyclonic separator 3 and the isolated high-temperature heat carrier of the 4th cyclonic separator 4, fall into bed formula through dipleg and make charcoal in device dense bed 6.
The high-temperature heat carrier that bed formula is made charcoal in device dense bed 6 is flowed out by the bed formula device 5 of making charcoal, and a part is discharged destructive distillation device after heat-obtaining cooling.Referring to Fig. 1, a part of high-temperature heat carrier enters heat collector 8 through high-temperature heat carrier drainage conduit 7, by heat-obtaining medium heat-obtaining cooling (be normally cooled to below 100 ℃, become Low Temperature Thermal carrier).After the cooling of high-temperature heat carrier heat-obtaining, by pipeline 9, enter thermal barrier blow-down drum 10, finally by thermal barrier blow-down drum 10, discharge destructive distillation device (can be used as material of construction uses).The present invention discharges a part of high-temperature heat carrier the amount of destructive distillation device, according to the material balance calculative determination of destructive distillation device.
By the bed formula high-temperature heat carrier that another part bed formula that device 5 flows out makes charcoal in device dense bed 6 of making charcoal, through high-temperature heat carrier transfer lime 23, enter the bottom of riser tube dry distillation reactor device 24, mix with resinous shale raw material 27.
Above-mentioned steps A～D continuously, loop.
The operational condition of above-mentioned method for destructive distillation is generally as follows:
In steps A, the particle diameter of resinous shale raw material 27 is not more than 3mm, and oleaginousness is 5%～35%, and water content is not higher than 15%.The high-temperature heat carrier entering in riser tube dry distillation reactor device 24 is 2～7 with the ratio of the weight rate of resinous shale raw material 27; The make charcoal temperature identical (embodiment 1～embodiment 6 herewith) of device dense bed 6 of the temperature of described high-temperature heat carrier and bed formula is 650～750 ℃.The temperature that enters the resinous shale raw material 27 of resinous shale material feeding tube 26 is envrionment temperature (embodiment 1～embodiment 6 herewith).Lift gas 32 can be dry gas (main ingredient is carbon 1, carbon 2), is to compress by the dry gas under envrionment temperature the compression dry gas (embodiment 1～embodiment 6 herewith) forming, and absolute pressure is 0.15～0.6MPa.Lift gas 32 can also be water vapor, and temperature is 450～550 ℃.The residence time (carry out the time of one section dry distillation reactor) of resinous shale raw material 27 in riser tube dry distillation reactor device 24 is 3～8min; The temperature in riser tube dry distillation reactor device 24 exits is 450～550 ℃, and absolute pressure is the absolute pressure at 0.1～0.4MPa[and bed formula dry distillation reactor device 21 tops basic identical (embodiment 1～embodiment 6 herewith)]; The average linear speed of riser tube dry distillation reactor device 24 interior lift gas 32 is that this average air linear speed of 7～15m/s[refers to that lift gas 32 enters backward mobile average linear speed within riser tube dry distillation reactor device 24 (calculating under the temperature in riser tube dry distillation reactor device 24 exits and absolute pressure condition)].Enter resinous shale raw material 27 in riser tube dry distillation reactor device 24 after one section of dry distillation reactor, transformation efficiency is 20%～30%.This transformation efficiency is one section of dry distillation reactor transformation efficiency, and the shale oil that is defined as one section of dry distillation reactor generation accounts for the weight percentage of resinous shale raw material 27 oleaginousness.
The vertical height of riser tube dry distillation reactor device 24 is mainly according to the total height calculative determination of its operational condition and bed formula dry distillation reactor device 21 and stripping stage 28, and interior diameter is mainly according to the mobility scale calculative determination of lift gas 32 average linear speeds.
In step B, the time that resinous shale raw material after one section of dry distillation reactor carries out two sections of dry distillation reactors in bed formula dry distillation reactor device dense bed 22 is 2～10min, the temperature (i.e. two sections of dry distillation reactor temperature) of bed formula dry distillation reactor device dense bed 22 is 450～550 ℃, the linear gas velocity of bed formula dry distillation reactor device 21 dilute phase sections is 0.2～1.2m/s, and the absolute pressure at bed formula dry distillation reactor device 21 tops is 0.1～0.4MPa.The dilute phase section of bed formula dry distillation reactor device 21, refers to the section that is positioned at bed formula dry distillation reactor device dense bed 22 tops, interface.Described gas, is mainly included in the interior stripping of stripping stage 28 and mixes oil gas, a section and the two sections of oil gas that dry distillation reactor generates that half defocused water vapor, mixing semicoke that stripping goes out are carried secretly.In operating process, bed formula dry distillation reactor device dense bed 22 is in inflation fluidized state.
Resinous shale raw material after one section of dry distillation reactor carries out the preferably 3～6min of time of two sections of dry distillation reactors, preferably 470～530 ℃ of the temperature of bed formula dry distillation reactor device dense bed 22 in bed formula dry distillation reactor device dense bed 22.
The time that resinous shale raw material after one section of dry distillation reactor carries out two sections of dry distillation reactors in bed formula dry distillation reactor device dense bed 22 is preferably 3.5～4.5min, and the temperature of bed formula dry distillation reactor device dense bed 22 is preferably 480～520 ℃.
The interior diameter of bed formula dry distillation reactor device 21 top cylinder shape cylindrical shells is mainly according to the mobility scale calculative determination of bed formula dry distillation reactor device 21 dilute phase section linear gas velocities, the height of bed formula dry distillation reactor device dense bed 22 mainly carries out the time of two sections of dry distillation reactors and the reserve calculative determination of bed formula dry distillation reactor device 21 interior mixing semicokes in bed formula dry distillation reactor device dense bed 22 according to the resinous shale raw material after one section of dry distillation reactor, the height of bed formula dry distillation reactor device 21 dilute phase sections is mainly according to the settling height calculative determination that mixes semicoke.
The present invention uses bed formula dry distillation reactor device 21, and the complexity that its operation is controlled is lower.And, at the interior stripping of stripping stage 28, mix the oil gas that interior two sections of dry distillation reactors of oil gas, bed formula dry distillation reactor device dense bed 22 that half defocused water vapor, mixing semicoke that stripping goes out carry secretly generate, can make bed formula dry distillation reactor device dense bed 22 in inflation fluidized state as fluidizing medium, do not need to use dry gas, so the energy consumption of bed formula dry distillation reactor device 21 is lower.In addition, the temperature of bed formula dry distillation reactor device dense bed 22 can keep comparatively stablely.
In step B, the temperature of the interior mixing semicoke of stripping stage 28 bed is 480～520 ℃.Enter mixing semicoke in stripping stage 28 after stripping, conventionally can stripping go out and more than 95% carry oil gas (embodiment 1～embodiment 6 herewith) secretly.The coke content of the mixing semicoke after the interior stripping of stripping stage 28, is generally 3%～15%.
In step C, entering mixing semicoke that tubular type makes charcoal in device 14, in tubular type is made charcoal device 14, to carry out one period of making charcoal be 5～40s; The make charcoal temperature in device 14 exits of tubular type is 600～750 ℃, and absolute pressure is 0.1～0.4MPa; The average air linear speed that tubular type is made charcoal in device 14 is that this average air linear speed of 1～10m/s[refers to that one section of air 16 of making charcoal enters the tubular type backward mobile average linear speed within device 14 (calculating under tubular type is made charcoal the temperature in device 14 exits and absolute pressure condition) of making charcoal].Tubular type the make charcoal absolute pressure basic identical (embodiment 1～embodiment 6 herewith) at device 5 tops of the absolute pressure in device 14 exits and bed formula of making charcoal.Enter mixing semicoke that tubular type makes charcoal in device 14 after one section is made charcoal, conventionally can be by the coke of burning-off 30%～70%; By the weight percentage of burning-off coke, equal to mix one section of semicoke make charcoal before and after the difference of contained weight of coke percentage ratio divided by the weight percentage of (after being stripping) contained coke before mixing one section of semicoke and making charcoal, then be multiplied by 100%.In tubular type, make charcoal in device 14, also burn the remaining oil gas of carrying secretly of mixing semicoke after stripping.
Tubular type is made charcoal the vertical height of device 14 mainly according to the make charcoal total height calculative determination of device 5 and stripping stage 28 of its operational condition and bed formula, and interior diameter is mainly according to the mobility scale calculative determination of average air linear speed.
In step D, it is 3～8min that one section of mixing semicoke after making charcoal carries out two periods of making charcoal in bed formula is made charcoal device dense bed 6, the make charcoal temperature (i.e. two sections of charcoal temperatures) of device dense bed 6 of bed formula is 650～750 ℃, the make charcoal linear gas velocity of device 5 dilute phase sections of bed formula is 0.1～1.2m/s, and the make charcoal absolute pressure at device 5 tops of bed formula is 0.1～0.4MPa.The make charcoal dilute phase section of device 5 of bed formula, refers to and is positioned at the make charcoal section of device dense bed 6 tops, interfaces of bed formula.Described gas, is mainly one section and makes charcoal and two sections of flue gases that generate of making charcoal.In operating process, bed formula is made charcoal device dense bed 6 in inflation fluidized state.
Bed formula is made charcoal the interior diameter of device 5 top cylinder shape cylindrical shells mainly according to the make charcoal mobility scale calculative determination of device 5 dilute phase section linear gas velocities of bed formula, the bed formula height of the device dense bed 6 mixing semicoke after mainly making charcoal according to a section of making charcoal carries out the make charcoal reserve calculative determination of device 5 interior high-temperature heat carriers of two periods of making charcoal and bed formula in bed formula is made charcoal device dense bed 6, and bed formula is made charcoal the height of device 5 dilute phase sections mainly according to the settling height calculative determination of high-temperature heat carrier.Mixing semicoke after the interior stripping of stripping stage 28 is interior after two sections are made charcoal at tubular type device 14, the bed formula device 5 of making charcoal of making charcoal, conventionally can more than 95% coke of burning-off.
Technique described in CN101440293A, resinous shale raw material particle size is large (being less than 30mm); Although can reduce the Crashing Costs of resinous shale raw material, there are the following problems: 1. make the yield of shale oil reduce; 2. cause fluidisation and the difficulty of transportation of resinous shale raw material in destructive distillation device, be unfavorable for the maximization construction of destructive distillation device; 3. in fluidized bed dry distillation chamber, make the hot fluidizing medium of destructive distillation produce channel, bias current, cause resinous shale raw material to conduct heat inhomogeneous, and affect the destructive distillation effect of resinous shale raw material and the quality of the shale oil generating.For this technique, the technique described in the document 1 that this specification sheets is quoted is used particle diameter to be not more than the resinous shale raw material of 3mm, comparatively suitable.The present invention also uses the resinous shale raw material 27 of this particle diameter, can make like this resinous shale raw material 27 normally fluidisation and destructive distillation in riser tube dry distillation reactor device 24 and bed formula dry distillation reactor device 21, improves the yield of shale oil; The coke that can also make to mix on semicoke when making charcoal for one section, two sections burns better simultaneously, thereby reclaims more heat.Use particle diameter to be not more than the resinous shale raw material 27 of 3mm, under operational condition of the present invention, shale oil yield can account for 80%～90% (shale oil yield of the present invention is the yield of actual acquisition) of resinous shale raw material 27 oleaginousness.
According to explanation of the present invention or requirement, the destructive distillation operational condition that the technician in oil shale distillation field can select the present invention to propose depending on concrete operations situation, selects various device member, carries out design, operation and the control of destructive distillation device.
The present invention, one section of make charcoal air 16 and two sections of all pressurized air (embodiment 1～embodiment 6 is herewith) for being formed by the air compressing under envrionment temperature of air 13 of making charcoal.Envrionment temperature of the present invention is 25～35 ℃, and pressure is absolute pressure, and percentage ratio is weight percentage, and interior diameter all refers to the interior diameter of the insulating and wearing-resistant lining of metal cylinder or pipe lining.In Fig. 1, the arrow of unreceipted Reference numeral represents the flow direction of various materials and/or medium.
Embodiment
On the small test device of the device of fluidized bed dry distillation shown in Fig. 1, by the step of the dry distillation method of oil shale described in this specification sheets embodiment part, carry out 6 groups of tests (embodiment 1～embodiment 6).Resinous shale raw material 27 all adopts cananga oil shale powder raw material, and character is in Table 1; Inlet amount (entering the weight rate of the resinous shale raw material 27 of resinous shale material feeding tube 26) is 150kg/ days.
In embodiment 1～embodiment 6, the linear gas velocity of bed formula dry distillation reactor device 21 dilute phase sections is 0.65m/s.The temperature of the interior mixing semicoke of stripping stage 28 bed is 500 ℃, and stripping medium is the water stripping steam 30 of 500 ℃.Through high-temperature heat carrier drainage conduit 7, enter the high-temperature heat carrier of heat collector 8, all by heat-obtaining medium (water under envrionment temperature) heat-obtaining, be cooled to 100 ℃.Lift gas 32 is the compression dry gas of 0.3MPa (absolute pressure), and one section of make charcoal air 16 and two sections of air 13 of making charcoal are the pressurized air of 0.4MPa (absolute pressure), and test ambient temperature is 25～26 ℃.
The character of embodiment 1～embodiment 6 remaining operational condition, product distribution and portioned product, respectively in Table 2～table 8.Wherein, the product in table 2～table 7 distributes, and all refers to that the total product of destructive distillation device distributes.In each embodiment, by the make charcoal coke content of the high-temperature heat carrier that device 5 flows out of bed formula, all identical in tubular type device 14 and the bed formula interior coke content through two sections of high-temperature heat carriers that generate after making charcoal of device 5 of making charcoal of making charcoal with the mixing semicoke after the interior stripping of stripping stage 28 described in table 2～table 7.Bed formula described in table 2～table 7 is made charcoal and is discharged the ratio of destructive distillation device after the interior a part of high-temperature heat carrier heat-obtaining cooling of device dense bed 6, all refers to that this part high-temperature heat carrier accounts for the percentage ratio of resinous shale raw material 27 weight rates that enter resinous shale material feeding tube 26 by make charcoal weight rate that device dense bed 6 flows out through high-temperature heat carrier drainage conduit 7 of bed formula.
The character (embodiment 1～embodiment 6) of table 1 resinous shale raw material
| Project | Data |
| Bulk specific gravity (sedimentation state), g/ml | 1.04 |
| Specific heat, cal/kg ℃ | 0.259 |
| Oleaginousness (aluminium rice steamer method mensuration), % | 8.5 |
| Water content, % | 6.9 |
| Ash oontent (combustion method mensuration), % | 70.4 |
| Size distribution, % | |
| Below 20 μ m | 16.5 |
| 20～ |
6 |
| 40～80μm | 5.1 |
| 80～110μm | 2.3 |
| 110～149μm | 3.1 |
| 149～500μm | 18.2 |
| 500～ |
20 |
| 1000～1500μm | 18.5 |
| 1500～3000μm | 10.3 |
The operational condition of table 2 embodiment 1 and product distribute
[note]: embodiment 2～embodiment 6 herewith.
The operational condition of table 3 embodiment 2 and product distribute
The operational condition of table 4 embodiment 3 and product distribute
The operational condition of table 5 embodiment 4 and product distribute
The operational condition of table 6 embodiment 5 and product distribute
The operational condition of table 7 embodiment 6 and product distribute
The character of table 8 embodiment 1～embodiment 6 portioned products
Claims (2)
1. a fluidized bed dry distillation method for resinous shale, is characterized in that: the method in turn includes the following steps:
A. the resinous shale raw material (27) after pulverizing enters the bottom of riser tube dry distillation reactor device (24) through resinous shale material feeding tube (26), the high-temperature heat carrier that bed formula is made charcoal in device (5) enters the bottom of riser tube dry distillation reactor device (24) through high-temperature heat carrier transfer lime (23), after resinous shale raw material (27) mixes with high-temperature heat carrier, up along riser tube dry distillation reactor device (24) under the castering action of the lift gas (32) being passed into by the bottom of riser tube dry distillation reactor device (24), carry out one section of dry distillation reactor;
B. the resinous shale raw material after one section of dry distillation reactor and the thermal barrier mixing with it, the shale oil and the carbonization gas that also have one section of dry distillation reactor to generate, by the outlet of riser tube dry distillation reactor device (24), enter bed formula dry distillation reactor device (21), resinous shale raw material after one section of dry distillation reactor carries out two sections of dry distillation reactors in bed formula dry distillation reactor device dense bed (22), obtain the shale oil that two sections of dry distillation reactors generate, carbonization gas and shale semicockes, shale semicockes and thermal barrier in bed formula dry distillation reactor device dense bed (22) are mixed to form mixing semicoke mutually, the cyclonic separator of the oil gas (17) that one section and two sections of dry distillation reactors generate through being located at bed formula dry distillation reactor device (21) in isolates that mixing half is defocused is flowed out by bed formula dry distillation reactor device (21), mixing semicoke in bed formula dry distillation reactor device dense bed (22) flows downward, enter the stripping stage (28) of being located at bed formula dry distillation reactor device (21) below, in stripping stage (28), pass into water stripping steam (30), stripping goes out to mix semicoke entrained oil gas, mixing semicoke in stripping stage (28) after stripping flows to the bottom of stripping stage (28), through semicoke transfer lime (25), enter the make charcoal bottom of device (14) of tubular type,
C. enter the mixing semicoke that tubular type makes charcoal in device (14) and contact with one section of air of making charcoal (16), along tubular type, making charcoal, device (14) is up to carry out one section and makes charcoal;
D. one section of mixing semicoke after making charcoal enters the bed formula device (5) of making charcoal by the make charcoal outlet of device (14) of tubular type, in bed formula is made charcoal device dense bed (6), contact with two sections of air of making charcoal (13) and carry out two sections and make charcoal, remaining coke on burning-off mixing semicoke, generate high-temperature heat carrier, one section make charcoal and two sections make charcoal the flue gas (1) that generates after the cyclonic separator of being located at bed formula and making charcoal device (5) in is isolated high-temperature heat carrier by device (5) discharge of making charcoal of bed formula, the high-temperature heat carrier that bed formula is made charcoal in device dense bed (6) is flowed out by the bed formula device (5) of making charcoal, a part is discharged destructive distillation device after heat-obtaining cooling, another part enters the bottom of riser tube dry distillation reactor device (24) through high-temperature heat carrier transfer lime (23), mix with resinous shale raw material (27),
In steps A, the particle diameter of resinous shale raw material (27) is not more than 3mm, oleaginousness is 5%～35%, water content is not higher than 15%, the ratio that enters the weight rate of the interior high-temperature heat carrier of riser tube dry distillation reactor device (24) and resinous shale raw material (27) is 2～7, the residence time of resinous shale raw material (27) in riser tube dry distillation reactor device (24) is 3～8min, the temperature in riser tube dry distillation reactor device (24) exit is 450～550 ℃, absolute pressure is 0.1～0.4MPa, the average linear speed of the interior lift gas of riser tube dry distillation reactor device (24) (32) is 7～15m/s, enter the interior resinous shale raw material (27) of riser tube dry distillation reactor device (24) after one section of dry distillation reactor, transformation efficiency is 20%-30%, in step B, the time that resinous shale raw material after one section of dry distillation reactor carries out two sections of dry distillation reactors in bed formula dry distillation reactor device dense bed (22) is 2～10min, the temperature of bed formula dry distillation reactor device dense bed (22) is 450～550 ℃, the linear gas velocity of bed formula dry distillation reactor device (21) dilute phase section is 0.2～1.2m/s, the absolute pressure at bed formula dry distillation reactor device (21) top is 0.1～0.4MPa, in step C, entering mixing semicoke that tubular type makes charcoal in device (14), in tubular type is made charcoal device (14), to carry out one period of making charcoal be 5～40s, the make charcoal temperature in device (14) exit of tubular type is 600～750 ℃, absolute pressure is 0.1～0.4MPa, the average air linear speed that tubular type is made charcoal in device (14) is 1～10m/s, enter mixing semicoke that tubular type makes charcoal in device (14) after one section is made charcoal, by the coke of burning-off 30%～70%, in step D, it is 3～8min that one section of mixing semicoke after making charcoal carries out two periods of making charcoal in bed formula is made charcoal device dense bed (6), the make charcoal temperature of device dense bed (6) of bed formula is 650～750 ℃, the make charcoal linear gas velocity of device (5) dilute phase section of bed formula is 0.1～1.2m/s, the make charcoal absolute pressure at device (5) top of bed formula is 0.1～0.4MPa,
In step C and step D, one section of air of making charcoal (16) and all pressurized air for being formed by the air compressing under envrionment temperature of two sections of air of making charcoal (13).
2. one kind for realizing the fluidized bed dry distillation device of the resinous shale of method described in claim 1, comprise a bed formula dry distillation reactor device (21), the bed formula device (5) of making charcoal, and with bed formula the make charcoal heat-obtaining discharger of the interior high-temperature heat carrier of device dense bed (6) of bed formula that device (5) is connected of making charcoal, bed formula dry distillation reactor device (21) and the bed formula device (5) of making charcoal is set up in parallel, it is characterized in that: the fluidized bed dry distillation device of resinous shale is also provided with a riser tube dry distillation reactor device (24) and the tubular type device (14) of making charcoal, riser tube dry distillation reactor device (24) is set up in parallel with bed formula dry distillation reactor device (21), tubular type device (14) and the bed formula device (5) of making charcoal of making charcoal coaxially arranges, the bottom of riser tube dry distillation reactor device (24) is provided with resinous shale material feeding tube (26), bottom is provided with lift gas sparger (31), the outlet of riser tube dry distillation reactor device (24) passes in bed formula dry distillation reactor device (21), in bed formula dry distillation reactor device (21), be provided with cyclonic separator, the top of bed formula dry distillation reactor device (21) is provided with oil gas collection chamber (18) and oil gas vent pipe (33), below is provided with stripping stage (28), stripping stage is provided with stripping baffles in (28), stripped vapor sparger (29), the bottom of stripping stage (28) is provided with semicoke transfer lime (25), the make charcoal bottom of device (14) of the outlet of semicoke transfer lime (25) and tubular type is connected, the make charcoal bottom of device (14) of tubular type is provided with one section of air-distributor of making charcoal (15), the make charcoal outlet of device (14) of tubular type passes into bed formula and makes charcoal in device (5), bed formula is made charcoal in device (5) and is provided with cyclonic separator, the make charcoal top of device (5) of bed formula is provided with flue gas collection chamber (2) and smoke outlet tube (34), bottom is provided with two sections of air-distributors of making charcoal (12), bed formula is made charcoal and is provided with high-temperature heat carrier transfer lime (23) between device (5) and riser tube dry distillation reactor device (24), the entrance of high-temperature heat carrier transfer lime (23) passes into bed formula and makes charcoal in device (5), outlet is connected in the bottom of riser tube dry distillation reactor device (24), the make charcoal heat-obtaining discharger of the interior high-temperature heat carrier of device dense bed (6) of described bed formula comprises high-temperature heat carrier drainage conduit (7), the entrance of high-temperature heat carrier drainage conduit (7) and the bed formula device (5) of making charcoal is connected, outlet is connected with heat collector (8), heat collector (8) is connected with thermal barrier blow-down drum (10) by pipeline (9), semicoke transfer lime (25), in high-temperature heat carrier transfer lime (23) and high-temperature heat carrier drainage conduit (7), be equipped with flowrate control valve (11).
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