CN101890254B - Separation system and method for high-temperature and high-pressure complex fluid - Google Patents
Separation system and method for high-temperature and high-pressure complex fluid Download PDFInfo
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- CN101890254B CN101890254B CN 200910143361 CN200910143361A CN101890254B CN 101890254 B CN101890254 B CN 101890254B CN 200910143361 CN200910143361 CN 200910143361 CN 200910143361 A CN200910143361 A CN 200910143361A CN 101890254 B CN101890254 B CN 101890254B
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Abstract
The invention discloses a separation system for high-temperature and high-pressure complex fluid, which comprises a first reactor, a first heat exchanger and a first separator, which are connected in turn by pipes, wherein the first separator is provided with gas-phase, liquid-phase and solid-phase product outlet pipes and a liquid level control device which comprises a hollow buoy, a connecting rod fixedly connected below the buoy and a core plug fixedly connected with the lower end of the connecting rod; and the core plug is matched with a solid-phase product outlet at the bottom of the first separator. The invention also discloses a method for separating the three phases of the high-temperature and high-pressure complex fluid by using the separation system. The high-temperature and high-pressure complex fluid can be generated by supercritical gasification of carbon compounds.
Description
Technical field
The present invention relates to be used for the piece-rate system of HTHP complex fluid, and the separation method that is used for the HTHP complex fluid.The invention still further relates to the fluid level control device and the method for first separator in piece-rate system.Said HTHP complex fluid for example can produce through carbon compound is carried out supercritical gasification.
Background technology
Living beings (comprise agricultural crop straw powder such as microalgae powder, cotton stalk powder, potato powder of straw; Or the like) or the supercritical gasification technology of the carbon compound of coal etc. be a new technique; The supercritical gasification technology of carbon compound is exactly to utilize fluid under the super critical condition as gasifying agent, carbon compound is changed into the technology of imflammable gas, tar and solid residue.The research in this field both at home and abroad launches, but mainly concentrates on aspect the output and concrete gas composition of gasifying process, consersion unit and available gas in the research emphasis in this field at present.And it is still rare for the reaction afterproduct technology of separating.Especially connecting the technology and the method for carrying out through ultra (Asia) critical reaction of the separator carbon compound that two-stage is similar does not occur as yet.In order to make reacted gas, tar and solid residue realize effectively separating, and make and separate the back residue and get into next step system's continuation participation gasification reaction.
The equipment that becomes known for separating mixture uses cyclone separator mostly, and its principle is to utilize the difference of each part proportion of mixture to reach the purpose of separation.Cyclone separator generally includes a pipeline that wherein is provided with the central streams kinetoplast, and distributing fin is arranged on the liquid, utilizes distributing fin to make in the rotation of the mixture of excessive rolling flow ipe.Result as the centrifugal force that produces because of rotation; The heavier component of mixture is outwards thrown; And in the zone of liquid, the moving than light component of mixture; So the separation of mixture can realize through outlet device is set in position, and light, the heavy ends that separate can be discharged separatedly.
Cyclone separator uses in a lot of occasions, and for example, inlet cyclones is applied to gravity separation vessel.Inlet cyclones guarantees that the mixture of coming in is further separating the preliminary treatment of confirming before the generation; For this purpose; Inlet cyclones is connected with the import of gravity separation vessel, and is provided with a heavy component outlet and a light component outlet, wherein; Two outlets are flowed out with further separating mixture in the inside of gravity separation vessel, and a case description of inlet cyclones is in European patent application EP 1187667A2.
But there is certain limitation in cyclone separator for the complex fluid that separates above-mentioned multi phase state.A shortcoming of known cyclone separator is, cyclone separator is mainly used in the occasion of gas solid separation, is used for device that the heavy component that separates and the light component that separates are discharged discretely owing to must be provided with in the separator, and these dischargers are all comparatively huge.
The method of general purpose control liquid level is mechanical switch such as liquid level gauge and by-pass valve control at present.For the container of some holding liquid, when liquid level is low, need open valve feed liquor body,, liquid level then needs valve-off when reaching a certain height.Especially in the long-time use of HTHP complex fluid, because valve switch belongs to mechanical action, there is poor sensitivity in this method in long-time use, shortcomings such as fragile, fault rate height.Inventor of the present invention utilizes the character of fluid under high-temperature and high-pressure conditions, according to Archimedes' principle, has developed a kind of method that can control HTHP complex fluid liquid level automatically.Through in container, keeping a constant liquid level to reach the purpose that high temperature, high pressure complex fluid are separated.
Chinese patent CN101296738A discloses a kind of separator.Relate to the cyclone separator that a kind of mixture separation with air inclusion, liquid and solid becomes heavy component and light component.This separator mainly comprises: the housing of the flowing space that the qualification mixture is flowed through; Be arranged on the liquid of the elongation in the flowing space; Treat that separating mixture can carry along it; At least one is arranged on the eddy flow initiation element between liquid and the inner housing, and this eddy flow initiation element is crooked so that the mixture that makes into rotates motion so that this mixture separation is become heavy ends and light component.Be used to get rid of the heavy component of separation and the remover of light component, this discharger comprises that at least one is defined in the inner flow channel of said at least one swirl element.This patent is improved a kind of novel cyclone separator on original cyclone separator basis.
Chinese patent CN201176413Y discloses a kind of three phase separator, relates to a kind of three phase separator that is applied in the systems such as up-flow anaerobic reactor UASB and anaerobic grain sludge expanded bed EGSB.Be mainly used in gas collection, sludge settling and the mud scum silica frost processing procedure; Its major technique is characterized as: comprise some sealing glands, some baffle plates, some deflection plates and some collection chambers; The some deflection plates that become certain angle of inclination with horizontal plane at first are installed on the base of these some collection chambers; In the bottom of these some deflection plates some baffle plates are installed, these some baffle plates should and some deflection plates between keep a relative spacing distance.Bottom between per two collection chambers near two baffle plates between a sealing gland is installed, keep a relative spacing distance between this sealing gland and this two baffle plate.This patent provides a kind of can separate the organic wastewater of high concentration, and is not prone to the efflux of solids mistake, thereby can not reduce the novel three phase separator of the load of reactor.
At present use the separator in living beings or coal gasifying process to be cyclone separator mostly, and cyclone separator is a kind of the most frequently used traditional separator.Cyclone separator mainly separates according to the gravity size of each component in the mixture, and heavy component after will separating then and light component are discharged through discharger.There is narrow application range in above-mentioned two kinds of separators, and service condition is simple, and the shortcoming that internal structure is complicated is especially used the gas, liquid, solid separating effect that is difficult to realize continuous effective under high temperature in this technology, the high pressure supercriticality in the complex fluid.Also have a reason be exactly the said separator of this technology be the small-sized non-standard equipment in laboratory, size is smaller, not seeing at present has the cyclone separator that is fit to its size.As the feeder apparatus of the main gasification reaction of next stage, if the comparatively complicated separator of utilization structure will cause continuous feeding to be difficult to guarantee.Complex fluid in this technology is the fluid-mixing that contains solid particle, all can have blockage problem in any one place, so inventor of the present invention has selected for use the comparatively simple separator of homemade structure to come to reduce as far as possible the system pipeline possibility of jamming.
Chinese patent CN201168461Y discloses the two-way oil water separator of a kind of float-type.Be specifically related to the two-way separator of a kind of profit.It is characterized in that comprising the ball float that is provided with coupling in the housing, housing of tubular, housing is respectively equipped with upper end cover and bottom end cover in two ends up and down, is equipped with through hole on upper end cover and the bottom end cover.This patent utilization gravity makes the oily waste water layering, realizes the profit two-way stratification through ball float, has simple in structurely, and cost is low, and the advantage of Rapid Realization water-oil separating, this patent are equally applicable to the different weight of density, light oil separates.But the device that this patent is just separated to the profit two under the normality condition mutually.
Summary of the invention
For overcoming the deficiency that exists in the above-mentioned prior art, the present invention provides a kind of piece-rate system of HTHP complex fluid, and this system comprises: first reactor, and said first reactor is carbon compound supercritical solvent extraction or gasification reactor; Be connected first separator of said first reactor downstream through pipeline, said first separator has: the gas-phase product export pipeline that is positioned at the said first separator top; Be positioned at the liquid product export pipeline on the sidewall of said first separator; And the solid product export pipeline that is positioned at said first separator bottom.
Said first separator also has fluid level control device, and said fluid level control device is arranged on the inside of said first separator, is used to control the liquid level of the inner liquid product of said first separator.
In a kind of preferred implementation of piece-rate system of the present invention, said fluid level control device comprises: the floating drum of hollow; Be fixedly connected on the connecting rod of said floating drum below; And the plug that is fixedly connected on the lower end of said connecting rod, said plug matches with the solid product outlet of said first separator bottom.
In a kind of preferred implementation of piece-rate system of the present invention, be connected with first heat exchanger through pipeline between said first reactor and said first separator; The downstream of said gas-phase product export pipeline are connected to second heat exchanger, and the downstream of said second heat exchanger are connected to second separator.
In a kind of preferred implementation of piece-rate system of the present invention, the downstream of said liquid product export pipeline are connected to fluid reservoir.
In a kind of preferred implementation of piece-rate system of the present invention, the downstream of said solid product export pipeline are connected to second reactor, and said second reactor is the overcritical or subcritical solvent gasification reactor of carbon compound.
In a kind of preferred implementation of piece-rate system of the present invention; The height of said first separator is 180mm to 1000mm, and internal diameter is that
is to
In a kind of preferred implementation of piece-rate system of the present invention, the material of said first separator is 304 stainless steels, 316 stainless steels or inconel 625 stainless steels, and heatproof to 150 ℃ is to 400 ℃, and withstand voltage is 10.0MPa to 40MPa.
In a kind of preferred implementation of the present invention, the height of said floating drum is 60mm to 600mm; Internal diameter is a heatproof to 150 to 400 ℃ 304 stainless steels, 316 stainless steels or inconel 625 stainless steels for the material of
said floating drum, and material thickness is 0.1mm to 3mm.
In a kind of preferred implementation of piece-rate system of the present invention, be provided with an aperture in the roof of said floating drum, make the inside of said floating drum keep gas communication with outside, be zero thereby make inside and outside differential pressure.
In a kind of preferred implementation of the present invention, the internal diameter of said aperture is that
is to
In a kind of preferred implementation of piece-rate system of the present invention, said floating drum is cylindrical or spherical, and each angle and face are slick and sly shape; And the bottom of said first separator is taper, and the drift angle of said plug and said taper is complementary.
In another aspect of this invention, also provide the piece-rate system that adopts above-mentioned HTHP complex fluid to come the separation method that the HTHP complex fluid is separated, said separation method comprises the steps:
Carbon compound, catalyst and supercritical fluid are provided in said first reactor; In said first reactor, to carry out supercritical fluid extraction or gasification reaction, said supercritical fluid can be water, carbon dioxide, benzene and the various organic solvent that uses in the conventional shooting flow body technology.Overcritical is notion to a special phase of solvent or fluid, and promptly when the temperature and pressure of certain fluid reached some values simultaneously, this fluid just reached supercriticality.
Will be in said first reactor product of supercritical fluid extraction or gasification reaction transfer in said first heat exchanger, in said first heat exchanger, carrying out heat exchange, thereby make the product cooling;
Cooled product is transferred in said first separator, and each phase constituent in the product is separated into gas-phase product, liquid product and solid product in said first separator.
In a kind of preferred implementation of separation method of the present invention; Further comprising the steps of: as to make said gas-phase product leave said first separator and get into second heat exchanger and carry out heat exchange and be cooled, then get into second separator further to separate through said gas-phase product export pipeline.
In a kind of preferred implementation of separation method of the present invention, further comprising the steps of: as to make said liquid product leave said first separator and get into fluid reservoir and be stored subsequent use through said liquid product export pipeline.
In a kind of preferred implementation of separation method of the present invention; Further comprising the steps of: as to make said solid product leave said first separator and get into second reactor through said solid product export pipeline; And in said second reactor, catalyst and supercritical fluid are provided, to carry out further supercritical fluid gasification reaction therein.
In a kind of preferred implementation of separation method of the present invention, the operating pressure of said first reactor is 10.0MPa to 40.0MPa, and operating temperature is 150 ℃ to 650 ℃.
In a kind of preferred implementation of separation method of the present invention, the operating pressure of said second reactor is 10.0MPa to 40.0MPa, and operating temperature is 150 ℃ to 850 ℃.
In a kind of preferred implementation of separation method of the present invention, the operating pressure of said first separator is 10.0MPa to 40.0MPa, and operating temperature is 150 ℃ to 400 ℃.
In a kind of preferred implementation of separation method of the present invention, said second separator is operated under normal temperature and normal pressure.
Built-in buoy formula separator among the present invention can separate to the complex fluid of the liquid-solid three-phase of gassiness under the high-temperature high-pressure state.Existing relatively separation, the separator among the present invention has simple in structure, and function is special, is easy to realize that the scope of application is extensive, and separating effect is advantage relatively reliably.
In conjunction with the drawings some exemplary embodiments of the present invention are described below, specified formation of the present invention, action principle and various advantage thereof.
Description of drawings
Fig. 1 is the generalized schematic of system of the present invention;
Fig. 2 is the generalized schematic of fluid level control device of the present invention;
Fig. 3 is the generalized schematic of the fluid level control device of Fig. 2 of the present invention when being arranged in the separator.
The specific embodiment
With reference to the accompanying drawings, some exemplary embodiments of the present invention are described.
The present invention provides a kind of piece-rate system of HTHP complex fluid, and this system comprises: first reactor 1, and said first reactor 1 is carbon compound supercritical solvent extraction or gasification reactor; Be connected first separator 3 in said first reactor 1 downstream through pipeline; Said first separator 3 has: the gas-phase product export pipeline that is positioned at said first separator 3 tops; In a kind of preferred implementation of piece-rate system of the present invention, between said first reactor 1 and said first separator 3, be connected with first heat exchanger 2 through pipeline; The downstream of said gas-phase product export pipeline are connected to second heat exchanger 4, and the downstream of said second heat exchanger 4 are connected to second separator 5; Be positioned at the liquid product export pipeline on the sidewall of said first separator 3, in a kind of preferred implementation of piece-rate system of the present invention, the downstream of said liquid product export pipeline are connected to fluid reservoir 6; And the solid product export pipeline that is positioned at said first separator 3 bottoms; In a kind of preferred implementation of piece-rate system of the present invention; The downstream of said solid product export pipeline are connected to second reactor 7, and said second reactor 7 is the overcritical or subcritical solvent gasification reactor of carbon compound.
Said first separator 3 also has fluid level control device, and said fluid level control device is arranged on the inside of said first separator 3, is used to control the liquid level of the inner liquid product of said first separator 3.
In a kind of preferred implementation of piece-rate system of the present invention, said fluid level control device comprises: the floating drum 9 of hollow; Be fixedly connected on the connecting rod 11 of said floating drum 9 belows; And the plug 12 that is fixedly connected on the lower end of said connecting rod 11, said plug 12 matches with the solid product outlet of said first separator 3 bottoms.
In a kind of preferred implementation of piece-rate system of the present invention; The height of said first separator 3 is 180mm to 1000mm; Internal diameter is 304 stainless steels, 316 stainless steels or inconel 625 stainless steels for
to
material; And heatproof to 150 ℃ is to 400 ℃, and withstand voltage is 10.0MPa to 40MPa.
In a kind of preferred implementation of the present invention, the height of said floating drum 9 is 60mm to 600mm; Internal diameter is a heatproof to 150 ℃ to 400 ℃ 304 stainless steels, 316 stainless steels or inconel 625 stainless steels for the material of
said floating drum 9, and material thickness is 0.1mm to 3mm.
In a kind of preferred implementation of piece-rate system of the present invention, be provided with an aperture 10 in the roof of said floating drum 9, make the inside of said floating drum 9 keep gas communication with outside, be zero thereby make inside and outside differential pressure.
In a kind of preferred implementation of the present invention, the internal diameter of said aperture 10 is that
is to
In a kind of preferred implementation of piece-rate system of the present invention, said floating drum 9 is cylindrical or spherical, and each angle and face are slick and sly shape; And the bottom of said first separator is taper, and said plug 12 is complementary with the drift angle of said taper.
In another aspect of this invention, also provide the piece-rate system that adopts above-mentioned HTHP complex fluid to come the separation method that the HTHP complex fluid is separated, said separation method comprises the steps:
Carbon compound, catalyst and supercritical fluid are provided in said first reactor 1; In said first reactor 1, to carry out supercritical fluid extraction or gasification reaction, said supercritical fluid can be water, carbon dioxide, benzene and the various organic solvent that uses in the conventional shooting flow body technology;
Will be in said first reactor 1 product of supercritical fluid extraction or gasification reaction transfer in said first heat exchanger 2, in said first heat exchanger 2, carrying out heat exchange, thereby make the product cooling;
Cooled product is transferred in said first separator 3, and each phase constituent in the product is separated into gas-phase product, liquid product and solid product in said first separator 3.
In a kind of preferred implementation of separation method of the present invention; Further comprising the steps of: as to make said gas-phase product leave said first separator 3 and get into said second heat exchanger 4 and carry out heat exchange and be cooled, then get into said second separator 5 further to separate through said gas-phase product export pipeline.
In a kind of preferred implementation of separation method of the present invention, further comprising the steps of: as to make said liquid product leave said first separator 3 and get into said fluid reservoir 6 through said liquid product export pipeline.
In a kind of preferred implementation of separation method of the present invention; Further comprising the steps of: as to make said solid product leave said first separator 3 and get into said second reactor 7 through said solid product export pipeline; And in said second reactor 7, catalyst and supercritical fluid are provided, to carry out further supercritical fluid gasification reaction therein.
In a kind of preferred implementation of separation method of the present invention, the operating pressure of said first reactor 1 is 10.0MPa to 40.0MPa, and operating temperature is 150 ℃ to 650 ℃; In a kind of preferred implementation of separation method of the present invention, the operating pressure of said second reactor 7 is 10.0MPa to 40.0MPa, and operating temperature is 150 ℃ to 850 ℃; In a kind of preferred implementation of separation method of the present invention, the operating pressure of said first separator is 10.0MPa to 40.0MPa, and operating temperature is 150 ℃ to 400 ℃; And in a kind of preferred implementation of separation method of the present invention, said second separator 5 is operated under normal temperature and normal pressure.
In other words, the present invention provides a kind of being used for that the HTHP complex fluid is separated the system and method for controlling with liquid level, and said system comprises the first separator 3 float-type fluid level controller inner with placing separator that places between the two-stage reactor.First reactor 1 in the two-stage reactor is carbon compound supercritical solvent extraction or gasification reactor, and second reactor 7 is the overcritical or subcritical solvent gasification reactor of carbon compound.In the present invention; Carbon compound such as living beings or coal is after 1 reaction of first reactor; Product gets into first separator 3 after first heat exchanger 2 is cooled to uniform temperature; The continuous effective of utilizing the effect of floating drum 9 to make to keep in first separator 3 certain liquid level to realize fluid mixture is separated, and separates the back gas-phase product and gets into second heat exchanger 4, gets into second separator 5 under the normal temperature and pressure through a heat exchange again; Oil-phase product after the separation is pressed under the inside and outside differential pressure effect in the fluid reservoir 6 automatically, and separation back solid product gets into second reactor 7 to be continued to react with supercritical fluid.Because technologic particularity; Complex fluid in the separator is to contain the subcritical of gas, liquid, solid three-phase or (overcritical) fluid under high temperature, the high pressure; Adopt conventional cyclone separator to be difficult to reach separating effect; And traditional control liquid level method is difficult to continue to use under this HTHP and the operating mode that has solid particle to exist, and for fear of above-mentioned contingent situation, inventor of the present invention selects for use among Fig. 2 built-in floating drum 9 to reach that liquid level is controlled and the purpose of three phase separation.Wherein the size of floating drum 9 and weight according in the separator to keep liquid level height confirm that the material of floating drum 9 can be selected the less heat-resistance type metal material of density for use.
Preferably the high temperature high voltage resistant three phase separator is adopted in the separation of first reactor, 1 effluent, promptly first reactor, 1 effluent advances separator and carries out gas, liquid, solid and separate, and the gas phase thing is CH in first separator 3 of HTHP
4, H
2, imflammable gas and a spot of CO such as CO
2, these gases carry out next step gas, liquid separation through second separator 5 that second heat exchanger 4 cools off back entering normal temperature and pressure, to remove the micro-moisture that brings out with gas phase; The liquid product of first separator 3 of HTHP is thick oils such as asphalitine or tar, because the pressure reduction of first separator 3 and fluid reservoir 6 reaches 10-40MPa, gets into fluid reservoir 6 automatically so be arranged in the tar on liquid level upper strata in first separator 3; HTHP first separator 3 solid formations are living beings or the solid residue of coal behind gasification reaction, and these residues carry out next step supercritical reaction with flow-like direct entering second reactor 7.
Preferably the fluid in first separator 3 is in ultra (Asia) critical condition; Certain variation can take place in physical property, phase and solubility with temperature and the variation of pressure under above-mentioned high-temperature and high-pressure conditions of living beings or coal, catalyst, tar light oil and water or other fluid, and above-mentioned reaction afterproduct is in the state of dissolving each other under a certain temperature and pressure.Phase can take place and separates in said mixture when heat exchanger is cooled to uniform temperature, makes through in first separator 3, keeping certain liquid level all the time that gas phase is constantly evaporated, oil phase is positioned at the liquid level upper strata all the time, the solid phase continuous feed.
Preferably adopt the size dimension of built-in float level controller to fix; When temperature, pressure is in a certain scope in first separator 3; The gravity of floating drum 9 equals the buoyancy of liquid level in first separator 3; And there is certain variation in first separator, 3 inner fluids along with temperature, pressure changes, and floating drum 9 is realized self-regulation liquid level function according to self the big I of gravity, have avoided liquid levels in first separator 3 to overflow like this or the generation of liquid level emptying situation.Wherein the gravity of fluid level controller designs according to the mean value of first separator, 3 inner fluid density.When first separator, 3 inner fluid density are big, higher liquid level can be kept, when first separator, 3 inner fluid density are less than normal, relatively low liquid level can be kept.
Preferably an aperture 10 is opened in cylindrical floating drum 9 tops in first separator 3; Making floating drum 9 external and internal pressure differences is zero; Thereby reduced the load performance of float-type fluid level controller material; The material density that pressure-bearing property is high is bigger, selects for use the less material of density can reach the purpose that enlarges controllable liquid level scope, reduces difficulty of processing and cut down finished cost.And adopt the float-type fluid level controller to have advantages such as the realization of being simple and easy to, reliable and stable, cost are lower, simplicity of design; Adopting traditional liquid level controlling method is that the chain liquid level that realizes of liquid level gauge and motor-driven valve is controlled; Traditional liquid level gauge can't bear so high temperature and pressure simultaneously; In case liquid level gauge or motor-driven valve are malfunctioning, will cause a lot of adverse consequences, therefore use conventional method to be difficult to realize effluent after the above-mentioned reaction is carried out the purpose of three phase separation.
Existing isolation technics adopts cyclone separator mostly, and cyclone separator becomes light component and heavy ends with mixture separation under centrifugal action.Be mainly used in and separate the fine dust particles of sneaking in the gas phase, seldom use it to realize that gas-liquid-solid three-phase separates continuously.Be used for device that heavy component that separates and the light component that separates are discharged discretely owing to must be provided with in the cyclone separator, these dischargers are general huger, especially the midget plant in the technology involved in the present invention more are difficult to realization.Liquid level gauge and motor-driven valve that tradition is used all use mechanical switch, have poor sensitivity, shortcomings such as fragile, fault rate height.Inventor of the present invention utilizes the character of fluid under high-temperature and high-pressure conditions, according to Archimedes' principle, has developed the float-type fluid level controller that can control HTHP complex fluid liquid level automatically.
In order to overcome the shortcoming that above-mentioned separator and fluid level controller in use exist; First separator 3 all adopts high temperature high-pressure resistant material to make with built-in buoy 9 among the present invention, has effectively avoided some drawbacks of above-mentioned cyclone separator and tank level control system.Have simple for structurely, separating effect is reliable, and liquid level in can the control separator of continous-stable.Through first separator 3 first reactor 1 and second reactor 7 are coupled together, for the continous-stable operation that realizes carbon compound supercritical extract and gasification reaction is supplied raw materials.
As shown in Figure 1; Carbon compound (for example coal), catalyst and supercritical fluid get into first reactor 1 and carry out supercritical reaction; Reaction back effluent directly gets into first separator 3 and separates after heat exchanger 2 carries out heat exchange, and the gas-phase product after the separation gets into second separator 5 through second heat exchanger, 4 backs; Oil tank 6, the first separators 3 bottom solid residues after separating under the liquid product entering normality get into second reactor, 7 continued and carry out next step supercritical gasification reaction.Wherein first reactor 1 is operated under pressure 10.0-40.0MPa, temperature 150-650 ℃ condition usually; Filling carbon compound (for example coal), catalyst and supercritical fluid extracts or gasification reaction in first reactor 1; Reacted effluent directly gets in first separator 3 through heat exchanger 2 backs; First separator 3 is operated under pressure 10.0-40.0MPa, temperature 150-400 ℃ condition usually, and the gases in first separator 3 after separating are upwards evaporation constantly, gets in second heat exchanger 4 through the gas phase pipeline and cools off; Cooling back gas gets into standing separation in second separator 5, and second separator 5 is operation at normal temperatures and pressures usually.Separating back liquid constantly flows in the fluid reservoir 6 under differential pressure action; Perhaps intermittently opening valve enters the oil phase on liquid level upper stratas in first separator 3 in the fluid reservoir 6; Fluid reservoir 6 operation under normal temperature and pressure conditions usually; Solid product after the separation directly gets into second reactor 7, carries out the next stage supercritical reaction with the catalyst and the supercritical fluid that get into second reactor 7, and wherein second reactor 7 is common operates under pressure 10.0-40.0MPa, temperature 150-850 ℃ condition.
The material that can adopt separation method of the present invention to separate can be the mixture that contains solid particle, tar and imflammable gas; Wherein solid particle be particle diameter at 20-300 purpose living beings or coal particle, can be agricultural crop straw powder such as coal dust, microalgae powder, cotton stalk powder, potato powder of straw etc.Wherein oil phase substance is the tar material behind the gasification reaction, can be gas oil, vacuum distillate, deasphalted oil, catalytic cracking recycle oil, shale oil, coal tar wet goods.Wherein gaseous substance is CH
4, H
2, CO, C
2H
4Deng imflammable gas and a spot of CO
2The catalyst that relates in this technology is the used catalyst of gasifying process such as alkali metal or alkaline-earth metal catalyst, noble metal catalyst, iron, nickel, cobalt, molybdenum, rhodium.
The operating condition of the inventive method is more simple than conventional separation method; The size of when technological design, designing floating drum 9 according to the operating mode and the character of material in first separator 3; And the condition according to equipment is optimized; And can on the basis of experiment or simulation, adjust according to feedstock property, product requirement etc.Each equipment that the present invention relates to uses material to be the high temperature high voltage resistant metal alloy compositions, can be nichrome materials such as inconel material, Hastelloy, incoloy material.Wherein built-in buoy 9 is because the gravitate influence is more obvious, and the material of selecting for use only need satisfy heat resistance, and to make floating drum 9 inside and outside differential pressures be zero through above floating drum 9, opening an aperture 10, so just reduced the requirement to material, and the while can cut down finished cost.
As shown in Figure 1, the fluid that gets in first separator 3 is the complex fluid of the reacted HTHP of supercritical gasification of living beings or coal, and the separation of this fluid is wanted much complicated than general normality (normal temperature and pressure) fluid.Owing to generated the mixing shape fluid that comprises imflammable gas, tar and solid residue behind raw material process supercritical extract or the gasification reaction; Compare more simple and reliable with liquid level in floating drum 9 controls first separator 3 with liquid level gauge with existing valve; Reduced possibility of jamming; When system stable operation, floating drum 9 can be in a certain fixing position in first separator 3, has saved mechanical adjustment switches such as flimsy valve or liquid level gauge.In design process, to reach inside and outside differential pressure be zero through above floating drum 9, opening an aperture 10, reduced the performance requirement to material.
As above shown in Figure 1; Gas in first separator 3 is discharged through the top exhaust line continuously; Liquid are in the profit stratification state in first separator 3, are directly extruded through the pressure differential between first separator 3 and the fluid reservoir 6 in the liquid level upper oil phase, and the solid particle that is sunken to bottom simultaneously becomes fluid state to pass through underground pipelines to discharge continuously; In same separator, realized the purpose of water, oil, gas three phase separation, the advantage of compared with prior art have simplification device, raising the efficiency.Because the fluid in first separator 3 is in subcritical (overcritical) state; Certain variation can take place with the fluctuation of temperature, pressure in the density of fluid; Floating drum 9 can move up and down along with the buoyancy of fluid; Floating drum 9 can design according to the minimum density values of fluid in design process, and when the fluid density in first separator 3 increased, floating drum 9 can be kept the liquid level of certain altitude all the time like this.Avoided following plug 12 to block the generation of fluid passage.
Description with reference to Fig. 2 and Fig. 3
Liquid level controlling method described in Fig. 2 and Fig. 3 is provided with the float-type fluid level controller of coupling in first separator 3 of taper.Fluid level controller comprises cylindrical floating drum 9, intermediate connecting rod 11 and following 12 3 parts of plug.Three parts are as a whole through being welded into.The shape of wherein top floating drum 9 can be cylindric, spherical, the first half is cylindric and the spherical geometry such as be formed by connecting of the latter half.Whole fluid level controller places first separator, 3 the insides, thereby can swim in the purpose that reaches the control liquid level in the separator in the liquid through self gravitation, and concrete implementation process is following:
Fluid evenly gets in first separator 3 with certain speed continuously, and the size of float-type fluid level controller is that design draws according to the physical property of fluid of required control.When first separator, 3 inner fluid density change with temperature and pressure; Floating drum 9 can be regulated liquid level according to the gravity of self; Following plug 12 causes the variation of fluid flowing passage size with floating drum 9 floating height change, thereby guarantees charging rate and inlet amount in the following gasification reactor.Because system temperature and pressure are in stable state in running, floating drum 9 is in a certain fixing height in first separator 3.
This method is not only applicable to go for equally in the simple fluid under the low-temp low-pressure operating mode in the above-mentioned complex fluid.
Above-mentioned float-type fluid level controller has the following advantages: simple in structure, be easy to realize, and especially use the generation that can reduce some potential safety hazards in the multi-phase complex fluid under HTHP.
In a kind of preferred implementation of the present invention, adopt following design:
One, the concrete structure size of first separator 3
Specifically being of a size of of first separator 3: high 180mm-1000mm; Internal diameter is
First separator, 3 materials are: 304, high temperature high voltage resistant, corrosion resistant material such as 316 stainless steels, inconel 625 stainless steels;
Wherein first separator 3 needs heatproof to arrive 150-400 ℃, and withstand voltage is 10-40MPa;
First separator, 3 the inside media are: the reacted CO of carbon compound supercritical gasification, H
2, CH
4, C
2H
6Deng imflammable gas and CO
2Gas, coal tar, comprise the three-phase mixtures such as residue (belonging to high-temperature, high pressure fluid) of catalyst
Two, the concrete structure size of built-in buoy 9
Specifically being of a size of of built-in buoy 9: high 60mm-600mm; Internal diameter does
Floating drum 9 materials are that heatproof arrives high temperature resistant, corrosion resistant materials such as 150-400 ℃ 304,316 stainless steels and inconel 625 stainless steels, and the material density of only making floating drum is generally at 6.5-8.0g/cm
3, wherein floating drum 9 roofs have an internal diameter and do
Aperture 10; Can keep floating drum 9 external and internal pressures to equate that thereby the floating drum material does not need requirement of withstand voltage,, require the floating drum material very thin like this because floating drum mainly leans on self buoyancy to regulate fluid level; Gravity is less relatively, thereby reaches the effect of control liquid level through self gravitation.
Cylindrical structure above the floating drum is designed to cylindrical or spherical, can make each angle and face be in slick and sly shape, and floating drum 9 just can not be because of with first separator, 3 inwalls collisions and can't homing like this.If make very clearly demarcated rectangle of corner angle or wedge angle type floating drum, will be easy to stick together with inwall and can't well carry out self function.
Needing the liquid level of control in first separator 3 is 1/10 to 2/3 place of first separator, 3 total heights, and the variable density scope of complex dielectrics is at 0.6-0.8g/cm in first separator 3
3, wherein, the size of floating drum 9 is to design through liquid level and fluid density calculating value that needs are controlled.Floating drum was placed on first separator, 3 inside before system's operation; Then through control system feeding discharging balance make the fluid flow that gets into first separator 3 be controlled at before within the designed range, so just can make the liquid level of keeping certain altitude in first separator 3 all the time.
Main beneficial effect
First separator 3 is between two key reaction devices (1 and 7); Can stable operation play very crucial effect to whole system; It is the key component that can the assurance system stable operation; So the liquid level that must keep certain height in first separator 3 can make first reactor, 1 reacted medium get in second reactor 7 continuously.If when liquid level is full in first separator 3, system jams will occur, cause system shutdown probably; If when liquid level was zero (separator is empty) in first separator 3, top fluid just can't get into second reactor 7 to be reflected, so also can cause system to move continuously.For not fixedly requirements of liquid level in first separator 3, only otherwise occur liquid level completely or dummy status just.So the floating drum among the present invention does not have sensing system; Because the function of floating drum be guarantee to have in first separator 3 certain altitude liquid level just; And need not measure the concrete height of inner liquid level, do not come the induction level height so mention through sensor in the invention.Equally; Also can connect sensor and learn how many first separator, 3 inner concrete liquid levels are; But because the complexity of first separator, 3 interior media and the operating mode of HTHP; General sensor can't bear so high temperature and pressure simultaneously, must select for use special material and strict accurate welding manner could guarantee the result of use of sensor.
And the medium among the present invention is the complex dielectrics that contains solid particle; Such medium is easy to equipment and instrument are caused certain washing away; So use traditional valve and liquid level gauge all to be easy to the phenomenon that results in blockage; Select for use the floating drum among the present invention to avoid the pipeline blockage phenomenon, system is moved continuously has very big advantage.
Begin start-up just, system will have the regular hour just can reach stable state, wherein, mainly leans on the monolithic stability of charging and discharge system regulating system, and first separator 3 is a middle access phase of whole system just.When system begins to fluctuate; Floating drum will play the effect of regulating liquid level; When system reaches in the stable operation process, floating drum will be in some relatively-stationary height, and the fluid that such first separator 3 flows into second reactor is exactly a metastable flow.What but entire system stable mainly leaned on is charging and discharge system, and the present invention does not stress the system stability problem, but the steady and continuous of Special attention will be given to first separator 3 parts has continuous fluid to get in second reactor in promptly separating and reacts.
Other beneficial effect
Existing liquid level controlling method is all through using traditional type liquid level gauge and by-pass valve control to realize; Valve in use occurs malfunctioning easily; Problems such as leakage are especially used in containing the medium of solid particle, and its service life can be shorter; Though traditional liquid level gauge kind is a lot; But the small-sized liquid level gauge at this high-temperature and high-pressure conditions does not also have producer to make at present, and comprehensive above-mentioned many disadvantages contains at HTHP to the mechanical control method of liquid level at present that can there be a lot of drawbacks in use in the complication system of solid particle.
The float level controller is through careful design on the technology among the present invention; Can solve the problem that above-mentioned liquid level gauge and valve in use run into; If using the traditional liquid level meter then to cause easily stops up communicating pipe, material requires problems such as high, that manufacture difficulty is big; And liquid level gauge can only indicate liquid level and can not control liquid level, must be used with valve and could control liquid level, and valve uses under above-mentioned operating mode and is easy to go wrong.The separator built-in buoy can be kept the liquid level of certain altitude according to the gravity of self in separator.The interior gas phase of separator is constantly volatilized, and oil phase pours, and solid material gets into continuously participates in reaction in next step reactor, thereby realizes good separating effect.
Claims (15)
1. the piece-rate system of a HTHP complex fluid, this system comprises:
First reactor, said first reactor is carbon compound supercritical solvent extraction or gasification reactor;
Be connected first separator of said first reactor downstream through pipeline, said first separator has:
Be positioned at the gas-phase product export pipeline at the said first separator top;
Be positioned at the liquid product export pipeline on the sidewall of said first separator; And
Be positioned at the solid product export pipeline of said first separator bottom,
Said first separator also has fluid level control device, and said fluid level control device is arranged on the inside of said first separator, is used to control the liquid level of the inner liquid product of said first separator, and said fluid level control device comprises:
The floating drum of hollow;
Be fixedly connected on the connecting rod of said floating drum below; And
Be fixedly connected on the plug of the lower end of said connecting rod, said plug matches with the solid product outlet of said first separator bottom.
2. the piece-rate system of HTHP complex fluid as claimed in claim 1 is characterized in that: be connected with first heat exchanger through pipeline between said first reactor and said first separator; The downstream of said gas-phase product export pipeline are connected to second heat exchanger, and the downstream of said second heat exchanger are connected to second separator.
3. the piece-rate system of HTHP complex fluid as claimed in claim 1 is characterized in that: the downstream of said liquid product export pipeline are connected to fluid reservoir.
4. the piece-rate system of HTHP complex fluid as claimed in claim 1 is characterized in that: the downstream of said solid product export pipeline are connected to second reactor, and said second reactor is the overcritical or subcritical solvent gasification reactor of carbon compound.
5. the piece-rate system of HTHP complex fluid as claimed in claim 1; It is characterized in that: the height of said first separator is 180mm to 1000mm, and internal diameter is that
is to
6. the piece-rate system of HTHP complex fluid as claimed in claim 1; It is characterized in that: the material of said first separator is 304 stainless steels, 316 stainless steels or inconel 625 stainless steels; And heatproof to 150 ℃ is to 400 ℃, and withstand voltage is 10MPa to 40MPa.
7. the piece-rate system of HTHP complex fluid as claimed in claim 1 is characterized in that: the height of said floating drum is 60mm to 600mm; Internal diameter is a heatproof to 150 ℃ to 400 ℃ 304 stainless steels, 316 stainless steels or inconel 625 stainless steels for the material of
said floating drum, and material thickness is 0.1mm to 3mm.
8. like the piece-rate system of claim 1 or 7 described HTHP complex fluids, it is characterized in that: being provided with an aperture in the roof of said floating drum, making the inside of said floating drum keep gas communication with outside, is zero thereby make inside and outside differential pressure.
9. the piece-rate system of HTHP complex fluid as claimed in claim 8 is characterized in that: the internal diameter of said aperture is
to
10. like the piece-rate system of claim 1 or 7 described HTHP complex fluids, it is characterized in that:
Said floating drum is cylindrical or spherical, and each angle and face are slick and sly shape; And
The bottom of said first separator is taper, and the drift angle of said plug and said taper is complementary.
11. adopt the piece-rate system of the described HTHP complex fluid of claim 1 to come the separation method that the HTHP complex fluid is separated, said separation method comprises the steps:
Carbon compound, catalyst and supercritical fluid are provided in said first reactor, in said first reactor, carrying out supercritical fluid extraction or gasification reaction,
Will be in said first reactor product of supercritical fluid extraction or gasification reaction transfer in first heat exchanger, in said first heat exchanger, carrying out heat exchange, thereby make the product cooling,
Cooled product is transferred in said first separator, and each phase constituent in the product is separated into gas-phase product, liquid product and solid product in said first separator.
12. separation method as claimed in claim 11; It is characterized in that further comprising the steps of: make said gas-phase product leave said first separator and get into second heat exchanger and carry out heat exchange and be cooled, then get into second separator further to separate through said gas-phase product export pipeline;
Making said liquid product leave said first separator and get into fluid reservoir through said liquid product export pipeline is stored subsequent use;
Make said solid product leave said first separator and get into second reactor, and in said second reactor, catalyst and supercritical fluid are provided, to carry out further supercritical fluid gasification reaction therein through said solid product export pipeline.
13. separation method as claimed in claim 11 is characterized in that:
The operating pressure of said first reactor is 10.0MPa to 40.0MPa, and operating temperature is 150 ℃ to 650 ℃.
14. separation method as claimed in claim 12 is characterized in that:
The operating pressure of said second reactor is 10.0MPa to 40.0MPa, and operating temperature is 150 ℃ to 850 ℃.
15. separation method as claimed in claim 11 is characterized in that:
The operating pressure of said first separator is 10.0MPa to 40.0MPa, and operating temperature is 150 ℃ to 400 ℃.
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| CN103193371B (en) * | 2012-01-04 | 2015-05-27 | 新奥科技发展有限公司 | Method and device for sludge oxidation by supercritical water |
| CN104152166B (en) * | 2014-06-11 | 2016-05-04 | 华南理工大学 | A kind of oil shale oil-refining integrated association hydrogen production from coal gasification utilization system and technique |
| CN104888500B (en) * | 2015-06-03 | 2017-08-25 | 北京中科诚毅科技发展有限公司 | The high-pressure separator and its design method and purposes of a kind of Multiple Optimization |
| CN106635152B (en) * | 2015-10-29 | 2018-07-31 | 中国石油化工股份有限公司 | A kind of processing method of full fraction of coal tar oil |
| CN106883893A (en) * | 2017-04-21 | 2017-06-23 | 广东工业大学 | A kind of biomass gasified tar processing system |
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| CN2623314Y (en) * | 2003-02-18 | 2004-07-07 | 张荣华 | Supercritical fluid gas-liquid phase separation device |
| CN2887402Y (en) * | 2005-12-03 | 2007-04-11 | 海尔集团公司 | Three-phase separator for printed plate board hypercritical separation |
| CN101113348A (en) * | 2007-09-06 | 2008-01-30 | 昆明理工大学 | Process for preparing bio-fuel by high-pressure fluid transformation technique |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2623314Y (en) * | 2003-02-18 | 2004-07-07 | 张荣华 | Supercritical fluid gas-liquid phase separation device |
| CN2887402Y (en) * | 2005-12-03 | 2007-04-11 | 海尔集团公司 | Three-phase separator for printed plate board hypercritical separation |
| CN101113348A (en) * | 2007-09-06 | 2008-01-30 | 昆明理工大学 | Process for preparing bio-fuel by high-pressure fluid transformation technique |
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