CN102009003A - Cyclone separator, slurry-bed reaction and separation system and method as well as application thereof in Fischer-Tropsch synthesis technology - Google Patents
Cyclone separator, slurry-bed reaction and separation system and method as well as application thereof in Fischer-Tropsch synthesis technology Download PDFInfo
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- CN102009003A CN102009003A CN 200910092042 CN200910092042A CN102009003A CN 102009003 A CN102009003 A CN 102009003A CN 200910092042 CN200910092042 CN 200910092042 CN 200910092042 A CN200910092042 A CN 200910092042A CN 102009003 A CN102009003 A CN 102009003A
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Abstract
The invention relates to a cyclone separator comprising a main body of the cyclone separator, a liquid discharging pipe, a solid discharging pipe and at least one sucking pipe, wherein one end of the liquid discharging pipe is positioned into the main body of the cyclone separator, the other end of the liquid discharging pipe passes through the top of the main body of the cyclone separator and is positioned outside the main body of the cyclone separator; the solid discharging pipe is connected to the bottom of the main body of the cyclone separator and is communicated with the internal space of the main body of the cyclone separator; one end of the sucking pipe is communicated with a cyclone feeding hole in the main body of the cyclone separator, and the other end of the sucking pipe faces to the bottom direction of the main body of the cyclone separator; and the bottom of the solid discharging pipe is higher than the bottom of the sucking pipe. The invention also relates to a slurry-bed reaction and separation system, a material separating method for slurry-bed reaction and the application of the slurry-bed reaction and separation system in the Fischer-Tropsch synthesis technology. The technical scheme utilizing the cyclone separator, the separation system and the separation method in the invention can be used for realizing the solid-liquid separation of slurry materials inside a slurry-bed reactor.
Description
Technical field
The present invention relates to chemical field.Specifically, relate to cyclone separator and slurry attitude bed Reaction Separation system and separation method and the application in fischer-tropsch synthesis process thereof that a kind of product liquid that is used for paste state bed reactor separates with solid catalyst.
Background technology
As everyone knows, the oil reserves in the world as industrial blood are limited.Yet, also increasing along with the continuous development of human society to the needs of crude oil, make limited petroleum resources reduce day by day and cause its price to rise steadily, thereby between the oil demand that increases day by day and limited petroleum resources the bigger contradiction of generation.
In order to reduce the depending on unduly of limited petroleum resources, people have developed the technology of utilizing solid fuel (as coal) or fuel gas (as natural gas) prepare liquid fuel.For example, can utilize coal or natural gas to obtain the synthesis gas of carbon monoxide and hydrogen, by Fischer-Tropsch is synthetic this synthesis gas (comprising carbon monoxide and hydrogen) is converted into liquid fuel then, as liquid fuels such as various hydro carbons, alcohols or ethers etc.
Realize that the synthetic reactor of Fischer-Tropsch has polytype, comprise fixed bed reactors, paste state bed reactor etc., wherein, because paste state bed reactor has advantages such as simple in structure, easy to operate, that conversion ratio is high, dispersion effect is even, thereby comparatively is widely used in the chemical reaction of the multiple chemical field that comprises Fischer-Tropsch synthesis.
Utilizing paste state bed reactor to carry out in the fischer-tropsch reaction process, mainly contain the synthesis gas (comprising carbon monoxide and hydrogen) of gaseous state, solid-state catalyst granules and liquid synthetic product (as liquid fuel) in the paste state bed reactor, and solid-state catalyst granules is entrained in usually with liquid fuel and become serum materials.Therefore, in order to obtain the liquid fuel of higher quality, it is very important how the solid catalyst particle being separated effectively with liquid fuel.
At present, Chang Yong method is in the paste state bed reactor outside above-mentioned serum materials to be separated.For example, the serum materials in the paste state bed reactor is transported to the outside from this paste state bed reactor, can adopts gravitational settling, filtration, extraction or magnetic separation technique etc. that liquid fuel and catalyst granules are separated then, to obtain liquid fuel.
Yet, this operation that separates in the paste state bed reactor outside must again be transported in paste state bed reactor by pump the catalyst after separating inevitably, not only prolonged the operating time of paste state bed reactor largely, influence operating efficiency, and utilizing catalyst granules after pump will separate to be transported to again in the process in the paste state bed reactor, be easy to cause the wearing and tearing of catalyst granules, the particle diameter that makes on the one hand catalyst granules diminishes and has increased the difficulty of later separation, activity of such catalysts is reduced, shortened the service life of catalyst.
Thereby, need a kind of technical scheme that can separate serum materials in paste state bed reactor inside.
Summary of the invention
The objective of the invention is to overcome the defective of in the paste state bed reactor outside serum materials being separated traditionally, and provide a kind of cyclone separator that serum materials is separated in paste state bed reactor inside that is applicable to, and can be implemented in slurry attitude bed Reaction Separation system and the separation method thereof that separate serum materials slurry attitude bed inside.
According to an aspect of the present invention, a kind of cyclone separator is provided, this cyclone separator comprises that top is that cylindrical, the bottom of top closure is obconic cyclone separator main body, and wherein, this cyclone separator also comprises liquid discharge nozzle, solid discharge nozzle and at least one suction tube; One end of described liquid discharge nozzle is positioned at described cyclone separator main body, the other end and passes the top of described cyclone separator main body and be positioned at outside the described cyclone separator main body; Described solid discharge nozzle is connected in the bottom of described cyclone separator main body and is communicated with the inner space of described cyclone separator main body; One end of described suction tube is communicated with eddy flow charging aperture in the described cyclone separator main body, the other end is towards the bottom direction of described cyclone separator main body; The bottom of described solid discharge nozzle is higher than the bottom of described suction tube.
According to a further aspect in the invention, a kind of slurry attitude bed Reaction Separation system also is provided, comprise paste state bed reactor and equipment for separating liquid from solid, wherein, described equipment for separating liquid from solid comprises the inner eddy flow separator that is arranged in the described paste state bed reactor, this inner eddy flow separator comprises at least one suction tube, and this suction tube can be drawn into the serum materials in the described paste state bed reactor in the described inner eddy flow separator and carry out the solid-liquid rotational flow separation.
In accordance with a further aspect of the present invention, a kind of feed separation method that is used to starch the reaction of attitude bed also is provided, this method comprises inner solid-liquid rotational flow separation step, this inside solid-liquid rotational flow separation step comprises being drawn in the inner eddy flow separator by at least one suction tube by reacting the serum materials that produces in the described paste state bed reactor, in this inner eddy flow separator the serum materials that transports is carried out inner solid-liquid rotational flow separation, described inner eddy flow separator is arranged on the inside of paste state bed reactor.
In addition, according to another aspect of the invention, also provide the application of above-mentioned slurry attitude bed Reaction Separation system of the present invention in fischer-tropsch synthesis process.
According to cyclone separator provided by the present invention, this cyclone separator is provided with suction tube, and an end of suction tube is communicated with the eddy flow charging aperture of cyclone separator, and the other end extends downwards and be lower than the solid discharge nozzle of cyclone separator.Thereby, this cyclone separator is suitable for being arranged on the inside of paste state bed reactor, suck in this cyclone separator to carry out rotational flow separation by the serum materials of its suction tube paste state bed reactor, output to the paste state bed reactor outside through the relative lighter liquid after the rotational flow separation by the liquid discharge nozzle then, heavier solid (as catalyst granules) is discharged in the paste state bed reactor again by the solid discharge nozzle relatively.
This shows, utilize cyclone separator provided by the present invention can be implemented in the inner Separation of Solid and Liquid that realizes serum materials of paste state bed reactor.
According to slurry attitude bed Reaction Separation system provided by the present invention and the feed separation method that is used to starch the reaction of attitude bed, utilization is by being arranged on the inner eddy flow separator of paste state bed reactor inside, the serum materials that can produce reaction in this paste state bed reactor inside carries out Separation of Solid and Liquid, thereby has overcome the defective that must separate serum materials in the paste state bed reactor outside traditionally.
Description of drawings
Fig. 1 is the structural representation according to cyclone separator of the present invention;
Fig. 2 is the schematic diagram according to a kind of embodiment of slurry attitude bed Reaction Separation of the present invention system;
Fig. 3 and Fig. 4 are respectively the schematic diagram according to the another kind of preferred implementation of slurry attitude bed Reaction Separation of the present invention system.
The description of reference numerals of critical piece
Cyclone separator main body 1
Eddy flow charging aperture 5
Paste state bed reactor 10
Inner eddy flow separator 11,11 '
Backwash tube 14
Outside cyclone separator 18
Air intake control valve 22
Gas exhausting valve 23
Holder 27
The 3rd pipeline 28
The specific embodiment
Below with reference to accompanying drawing the specific embodiment of the present invention is described in detail.
As shown in Figure 1, cyclone separator provided by the invention comprises: top is that cylindrical, the bottom of top closure is obconic cyclone separator main body 1, wherein, this cyclone separator also comprises liquid discharge nozzle 2, solid discharge nozzle 3 and at least one suction tube 4; One end of liquid discharge nozzle 2 is positioned at cyclone separator main body 1, the other end and passes the top of cyclone separator main body 1 and be positioned at outside the cyclone separator main body; Solid discharge nozzle 3 is connected in the bottom of cyclone separator main body 1 and is communicated with the inner space of cyclone separator main body 1; One end of suction tube 4 is communicated with eddy flow charging aperture 5 in the cyclone separator main body 1, the other end extends towards the bottom direction of cyclone separator main body 1; The bottom of solid discharge nozzle 3 is higher than the bottom of suction tube 4.
This cyclone separator is provided with at least one suction tube 4, and this suction tube 4 is positioned at the outside of cyclone separator main body 1.And, one end of suction tube 4 is communicated with eddy flow charging aperture 5, the other end extends towards the bottom direction of cyclone separator main body 1, and the end of this suction tube 4 surpasses the end (bottom level of solid discharge nozzle 3 is than the high 50-500mm of bottom level of suction tube 4) of solid discharge nozzle 3.Thereby, cyclone separator with suction tube 4 is fit to be arranged on the inside of paste state bed reactor very much, by the serum materials in the suction tube 4 absorption paste state bed reactors, and the serum materials drawn can be transported in this cyclone separator along the tangential direction with respect to the inwall of cyclone separator main body 1, thereby carry out rotational flow separation.The main improvements of cyclone separator provided by the present invention and traditional cyclone separator are the setting of suction tube 4, thereby can adopt each structure member of traditional cyclone separator, satisfy the material that sucks in the cyclone separators by suction tube 4 being connected of suction tube 4 and cyclone separator and can in this cyclone separator, carry out rotational flow separation as long as make.
In the rotational flow separation process, heavier feeds (is the heavier material of density, as catalyst granules) accumulate in the bottom of this cyclone separator, and can emit continuously or off and on by solid discharge nozzle 3, and light material (is the lighter material of density, as liquid fuel as product) then can be positioned at the top of the heavier feeds of deposition, and can emit by liquid discharge nozzle 2, realize separating of heavier feeds and light material thus.
Preferably, the highly high 50-500mm in bottom (port) of the bottom of solid discharge nozzle 3 (port) aspect ratio suction tube 4, as depicted in figs. 1 and 2, the spacing between the bottom (port) of the bottom of solid discharge nozzle 3 (port) and suction tube 4 is H.Because the bottom (port) of bottom (port) the aspect ratio suction tube 4 of solid discharge nozzle 3 is highly high, thereby can produce pressure differential, when generation negative pressure in the cyclone separator main body is drawn serum materials to pass through suction tube 4, be convenient to port absorption serum materials by this suction tube 4 that is positioned at lower position.
Preferably, the port of solid discharge nozzle 3 is higher than the serum materials 12 of paste state bed reactor, as shown in Figure 2, so that the solid material after the discharging separation.
Be discharged into cyclone separator main body outside for the ease of the light material (as liquid fuel) that obtains after the rotational flow separation by liquid discharge nozzle 2, preferably, the length of liquid discharge nozzle 2 in cyclone separator should satisfy: in carrying out the rotational flow separation process, the port of this liquid discharge nozzle 2 is used for the light material (as liquid fuel) that isolated at suction obtains.And preferably, the port of liquid discharge nozzle 2 is not used in the heavier feeds (as catalyst granules) after the isolated at suction.Thereby preferably, the length of liquid discharge nozzle 2 in cyclone separator is the 1/4-1/2 of diameter of the cylindrical part of cyclone separator main body 1.
The heavier feeds that obtains after the rotational flow separation (as catalyst granules) emits by solid discharge nozzle 3.For the ease of to solid discharging control, preferably, on solid discharge nozzle 3, be connected with baiting valve 6, as diaphragm valve.
When carrying out rotational flow separation, can utilize this baiting valve 6 to realize intermittently blowing.Specifically, when just carrying out rotational flow separation, baiting valve 6 is closed.Along with the carrying out of rotational flow separation, what separate to obtain can accumulate in the bottom of cyclone separator main body than heavy material (as catalyst granules).When degree that the needs that gather than heavy material discharge, baiting valve 6 can be opened, thereby allow to emit by this baiting valve 6 than heavy material.After the discharging of finishing than heavy material, again baiting valve 6 is closed, make accumulating after the separation than heavy material.Constantly repeat said process, thus in the process of rotational flow separation, off and on discharging separate obtain than heavy material (as catalyst granules).
Description by above parts, structure and running thereof to cyclone separator, can know that this cyclone separator is applicable to is arranged in the paste state bed reactor, and the serum materials in the paste state bed reactor is carried out rotational flow separation, thereby overcome the technological deficiency that to separate serum materials in the outside of paste state bed reactor traditionally and bring in the inside of this paste state bed reactor.
As shown in Figure 2, slurry attitude bed Reaction Separation provided by the invention system comprises: paste state bed reactor 10 and equipment for separating liquid from solid, this equipment for separating liquid from solid comprises the inner eddy flow separator 11 that is arranged in the described paste state bed reactor 10, this inner eddy flow separator 11 comprises at least one suction tube 4, and this suction tube 4 can be drawn into the serum materials in the described paste state bed reactor 10 in the described inner eddy flow separator 11 and carry out the solid-liquid rotational flow separation.
Compare with traditional slurry attitude bed Reaction Separation system, the main improvements of slurry attitude bed Reaction Separation system of the present invention are: be provided with in the inside of paste state bed reactor 10 (dotted line schematically shows in Fig. 2) and be applicable to the inner eddy flow separator 11 that carries out centrifugation in this paste state bed reactor 10 inside, thereby can carry out centrifugation to the serum materials in the paste state bed reactor 10 in the inside of this paste state bed reactor 10.
The inner eddy flow separator 11 that is arranged in paste state bed reactor 10 sucks the inside of this inner eddy flow separator 11 by at least one suction tube 4 with serum materials, to carry out rotational flow separation.Inner eddy flow separator 11 can utilize suction tube 4 to draw serum materials in the paste state bed reactors 10 by the mode of any appropriate.For example, can utilize the inside and outside pressure differential of inner eddy flow separator 11, can also form negative pressure in the inside of inner eddy flow separator 11 by pump.
This inner eddy flow separator 11 can be can be by suction tube 4 with the absorb cyclone separator arbitrarily of cyclone separator 11 inside of the serum materials in the paste state bed reactor 10.Preferably, the inner eddy flow separator 11 that is arranged in the paste state bed reactor 10 is above-mentioned cyclone separator provided by the present invention.Can both be in any suitable manner combine individually and/or in combination about the above-mentioned feature of cyclone separator provided by the present invention with the inner eddy flow separator 11 here.
For example, preferably, inner eddy flow separator 11 comprises that top is the cylindrical of top closure, the bottom is obconic cyclone separator main body 1, the upper end of suction tube 4 is communicated with eddy flow charging aperture 5 in the cyclone separator main body 1, the lower end of suction tube 4 can extend in the serum materials 12 in the paste state bed reactor 10, the bottom of inner eddy flow separator main body 1 is provided with solid discharge nozzle 3, be connected with baiting valve 6 on this solid discharge nozzle 3, equipment for separating liquid from solid also comprises liquid discharge nozzle 2, one end of liquid discharge nozzle 2 is positioned at cyclone separator main body 1, the other end of liquid discharge nozzle 2 passes the top of cyclone separator main body 1 and is positioned at the outside of paste state bed reactor 10, is delivered to the reactor outside thereby inner eddy flow can be separated the liquid that obtains.
For another example, preferably, the bottom level of solid discharge nozzle 3 is than the high 50-500mm of bottom level of suction tube 4, so that when solid discharge nozzle 3 and suction tube 4 all insert serum materials, forms pressure differential between the bottom of the bottom of solid discharge nozzle 3 and suction tube 4.
Be arranged on the embodiment of described paste state bed reactor 10 according to inner eddy flow separator 11, when carrying out rotational flow separation, need carry out inner solid-liquid rotational flow separation step, this inside solid-liquid rotational flow separation step comprises being drawn in the inner eddy flow separator 11 by at least one suction tube 4 by reacting the serum materials that produces in the paste state bed reactor 10, in this inner eddy flow separator 11 serum materials that transports is carried out inner solid-liquid rotational flow separation.
Serum materials in the paste state bed reactor 10 generally includes solid catalyst particle and liquid fuel.This serum materials is absorbed behind the cyclone separator 11 by at least one suction tube 4, in this inner eddy flow separator, carry out rotational flow separation, thereby make solid catalyst particle (certainly, in this solid catalyst particle, also may still can be doped with a spot of liquid remnants) be deposited on the bottom of inner eddy flow separator 11, and then can discharge in the paste state bed reactor 10 by solid discharge nozzle 3, to continue its catalytic action of performance; Separate the liquid fuel that obtains and then can be discharged to the outside by liquid discharge nozzle 2 on the top of inner eddy flow device 11 (being positioned on the solid catalyst particle).
This shows, in slurry attitude bed Reaction Separation provided by the present invention system, and being used to of utilizing that this piece-rate system carries out the feed separation method of starching the reaction of the attitude bed inside that can be implemented in paste state bed reactor realize separation to serum materials, thereby overcome the defective that must carry out centrifugation in the outside of paste state bed reactor traditionally and bring.
Preferably, inner solid-liquid rotational flow separation step comprises that also the solid material that the solid-liquid rotational flow separation is obtained is discharged into (this can realize by the baiting valve 6 that connects on the solid discharge nozzle 3) in the described paste state bed reactor 10 off and on, the liquid material that the solid-liquid rotational flow separation is obtained is transported to the outside of paste state bed reactor 10, thereby realizes separating of catalyst granules and liquid fuel product.
For the further degree of purity that improves the liquid material that obtains through the inner eddy flow separating step, and catalyst as much as possible is directly recycled in the Returning reactor, preferably, as shown in Figure 2, liquid discharge nozzle 2 is provided with piping filter 13.Thereby, utilize piping filter 13 to carry out filtration step, with further realization Separation of Solid and Liquid to the liquid material that obtains through described inner solid-liquid rotational flow separation.
When the liquid material that separates the back acquisition passes through this piping filter 13 by the pipeline conveying, the tiny solid particle that is entrained in this liquid material is just remained by this piping filter 13, but liquid still allows to pass through, thus make by after the degree of purity of liquid higher.Certainly,, just need not to be provided with in addition piping filter 13, also need after separation, not carry out filtration step by this piping filter 13 if the degree of purity of the liquid material that obtains after the inner solid-liquid rotational flow separation of process has reached required requirement.
Piping filter 13 can adopt the filter of realization Separation of Solid and Liquid commonly used, for example, and basket filter, l type filter or y-type filter.Usually, the filtering accuracy of filter (allowing the maximum particle diameter by the particle of this filter) is about the 5-10 micron.
When filtration was carried out a period of time of after, because gathering of tiny solid particle can cause the decline of strainability.Thereby as shown in Figure 2, piping filter 13 is connected with backwash tube 14, and promptly backwash tube 14 links to each other with piping filter 13, thereby can utilize the recoil medium by backwash tube 14 that piping filter 13 is recoiled.Separation method provided by the present invention comprises that also utilization recoil medium carries out the recoil step of backflush process to piping filter 13.
The recoil medium can be not influence gas or the liquid that paste state bed reactor 10 internal reactions carry out, and for example, the recoil medium can be any one in nitrogen or the inert gas; The recoil medium can also be a part of separating the comparatively pure liquid material of back acquisition.
For fear of the interference between inner solid-liquid rotational flow separation step and the recoil step, for same inner eddy flow separator 11, inner solid-liquid rotational flow separation step is not carried out simultaneously with the recoil step, and the step that promptly recoils and inner solid-liquid rotational flow separation step hocket.
Specifically, as shown in Figure 2, be provided with backwash valve 15, in the pipeline of carrying liquid material, be provided with liquid bleeder valve 16 at backwash tube 14.
When carrying out inner solid-liquid rotational flow separation step, need be transported to the outside with separating the liquid material that obtains, this moment, backwash valve 15 cut out, and liquid bleeder valve 16 is opened.
And when needs recoiled step, backwash valve 15 was opened, and fed the recoil medium of relatively high pressure, simultaneously liquid bleeder valve 16 cut out, and medium directly flows away by liquid bleeder valve 16 to prevent to recoil.At this moment, the recoil medium can only wash by piping filter 13 and to this filter.
As shown in Figure 4, for the recoil medium of gaseous state is provided to backwash tube 14, be provided with the source of the gas (not shown) and be communicated with the also gas buffer jar 20 of stored-gas, also be provided with heater 21 and air intake control valve 22 in the pipeline between source of the gas and gas buffer jar 20 with this source of the gas.Because environment temperature is higher relatively in the paste state bed reactor, be about 200 ℃ to 300 ℃, gas be heated to by heater 21 with paste state bed reactor in after the close temperature of environment temperature, utilize this gas to recoil again, thereby can not influence normally carrying out of paste state bed reactor internal reaction.Gas buffer jar 20 communicates with backwash tube 14 by pipeline, with the recoil medium to backwash tube 14 supply gaseous states.
Because for same inner eddy flow separator, inner solid-liquid rotational flow separation step can not be carried out simultaneously with the recoil step, therefore in order to ensure the liquid material after can obtaining constantly to separate, preferably, described equipment for separating liquid from solid comprises two described inner eddy flow separators 11 and 11 ' that can be used alternatingly, each described inner eddy flow separator is provided with piping filter and backwash tube, as shown in Figure 3.
That is to say that the inner eddy flow separators 11 and 11 ' that are arranged in the paste state bed reactor 10 are two, thereby make that another carried out described inner solid-liquid rotational flow separation step when one of them carried out described recoil step.That is, there is not the stage that is in the step that recoils simultaneously in these two inner eddy flow separators 11 and 11 '.
When carrying out inner solid-liquid rotational flow separation step with reference to 3, one inner eddy flow separators of figure 11, liquid bleeder valve 16 is opened, and backwash valve 15 cuts out.After work a period of time (as 10-15 minute), liquid bleeder valve 16 cuts out, backwash valve 15 is opened simultaneously, another backwash valve 15 ' cuts out, another liquid bleeder valve 16 ' is opened, at this moment, inner eddy flow separator 11 step that recoils, and another inner eddy flow separator 11 ' carries out inner solid-liquid rotational flow separation step.After the recoil step of inner eddy flow separator 11 is carried out a period of time (as 5 second-3 minute, the time of the step that recoils is shorter with respect to the time of carrying out inner solid-liquid rotational flow separation step), backwash valve 15 cuts out.At this moment, inner eddy flow separator 11 step that neither recoils is not carried out inner solid-liquid rotational flow separation step yet.When another inner eddy flow separator 11 ' carries out inner solid-liquid rotational flow separation step after a period of time (as 10-15 minute), again to this another inner eddy flow separator 11 ' step that recoils.So constantly repeat this process, be used alternatingly two inner eddy flow separators 11 and 11 '.
Certainly, also can adjust the time of recoil step, so that there is not out-of-work situation in two inner eddy flow separators 11 and 11 '.
In order to store the liquid material that is transported to the paste state bed reactor outside, preferably, described slurry attitude bed Reaction Separation system also comprises the storage tank 17 that is positioned at paste state bed reactor 10 outsides, and this storage tank is communicated with the described other end of liquid discharge nozzle 2.Thereby the liquid material after separation after the output, can be stored into this liquid material the storage tank 17 that is arranged in described paste state bed reactor 10 outsides in the paste state bed reactor 10.
Generally, in carrying out course of reaction, the operating pressure in the paste state bed reactor 10 is 2.0-5.0Mpa.Enter in the storage tank for the ease of separating the liquid material that obtains, preferably, pressure in this storage tank 17 is lower than the operating pressure in the paste state bed reactor 10 slightly, and further preferably, the operating pressure in the pressure ratio paste state bed reactor 10 in the storage tank 17 hangs down 0.2-0.5Mpa.And, in order to make the paste state bed reactor gas inside, can also speed to exit (as shown in Figure 4) by pipeline, with control paste state bed reactor 10 pressure inside finishing the discharge in time of reaction back.
In addition, in order to ensure the quality that is stored in liquid material in the storage tank 17, preferably, the temperature in the temperature of storage tank 17 and the paste state bed reactor 10 is consistent substantially.This can realize by in storage tank 17 heater being set.
For the serum materials in the paste state bed reactor 10 is entered in the inner eddy flow separator 11 by suction tube 4, to carry out rotational flow separation, preferably, liquid discharge nozzle 2 is provided with pump, and the operation of described pump makes the serum materials 12 in the paste state bed reactor 10 to enter to carry out the solid-liquid rotational flow separation in the inner eddy flow separator 11 and make isolated liquid material can derive paste state bed reactor 10.Thereby, when inner eddy flow separator 11 carries out inner solid-liquid rotational flow separation step, can start this pump, can be in the inner eddy flow separator 11 inner negative pressure that form, thereby the serum materials 12 in the paste state bed reactor 10 can be entered in the inner eddy flow separator 11, also the liquid material that separate to obtain can be pumped to internally the outside of paste state bed reactor 10 in the cyclone separator 11, perhaps this liquid material be transported in the storage tank 17 of storaging liquid material (if described piece-rate system is provided with storage tank 17).
Liquid material is being transported in the embodiment of storage tank 17, the negative pressure that can also not utilize pump to produce realizes that serum materials is drawn in the inner eddy flow separator 11.Specifically, the position of storage tank 17 can be arranged so that the liquid level of liquid material in this storage tank 17 is lower than the liquid level of serum materials 12 in the paste state bed reactor 10, carry out the solid-liquid rotational flow separation thereby make paste state bed reactor 10 interior serum materials 12 can under the effect of paste state bed reactor 10 inside and outside differential pressures, enter inner eddy flow separator 11, and make isolated liquid material can derive paste state bed reactor 10.
In this case, because the setting of having omitted pump, thereby can save the energy, also can reduce the maintenance cost of piece-rate system.
Certainly, can also adopt various technological means commonly used to realize that pressure in the storage tank 17 is a little less than the pressure in the inner eddy flow separator 17.
In order further to improve the degree of purity of the liquid material that is transported to paste state bed reactor 10 outsides, preferably, described equipment for separating liquid from solid also comprises the outside cyclone separator 18 that is positioned at outside the paste state bed reactor 10, carries out outside solid-liquid rotational flow separation step by this outside cyclone separator 18.
For example, the charging aperture of this outside cyclone separator 18 can be communicated with the described other end of liquid discharge nozzle 2, carrying out further solid-liquid rotational flow separation through the liquid material that inner eddy flow separator 11 separates.In this situation, described outside solid-liquid rotational flow separation step comprises utilizes the 18 pairs of isolated liquid materials of outside cyclone separator that are positioned at outside the paste state bed reactor 10 to carry out further solid-liquid rotational flow separation.Thereby, separating the liquid material that obtains through the inner eddy flow separating step is imported into again in the outside cyclone separator 18, and carry out outside rotational flow separation step by this outside cyclone separator 18, thereby further remove the impurity that is entrained in the liquid material that separation obtains through the inner eddy flow separating step, can further improve its degree of purity.
If be provided with piping filter 13 in liquid discharge nozzle 2, then said external solid-liquid rotational flow separation step comprises that the liquid material that utilizes after being positioned at paste state bed reactor 10 18 pairs outer of outside cyclone separators step being separated after filtration carries out further solid-liquid rotational flow separation.In this embodiment, because the liquid material that separates acquisition through the inner eddy flow separating step has passed through filtration treatment through piping filter 13 time, thereby the fluent material after outside cyclone separator 18 separates can obtain better degree of purity.
For another example, be provided with in the situation of storage tank 17 in piece-rate system, the charging aperture of outside cyclone separator 18 can be communicated with storage tank 17, the material in the storage tank 17 is carried out further solid-liquid rotational flow separation.Under this situation, described outside solid-liquid rotational flow separation step comprises utilizes the liquid material that is arranged in the 18 pairs of storage tanks 17 of outside cyclone separator outside the paste state bed reactor 10 to carry out further solid-liquid rotational flow separation.
Said external cyclone separator 18 can have one or more, can be according to the requirement of the requirement of concrete workplace and separation accuracy and selected.Have higher relatively degree of purity at the liquid material that separates acquisition through outside cyclone separator 18, this liquid material also as the recoil medium, is used for piping filter 13 is carried out above-mentioned recoil step.Then can be transported to again in the paste state bed reactor 10 and separate the solid particle (less catalyst granules, also may be doped with liquid usually becomes paste-like) that obtains, continue its catalytic action of performance through outside cyclone separator 18.As shown in Figure 4, by pump 26 this paste-like material is transported in the paste state bed reactor 10 by first pipeline 24.
In order further to obtain the higher liquid feul of degree of purity again, preferably, described equipment for separating liquid from solid also comprises the membrane separator 19 that is positioned at outside the described paste state bed reactor 10, and described separation method also comprises the film separating step.
The compound mode different according to piece-rate system, this membrane separator 19 also can have multiple different set-up mode.For example, the charging aperture of described membrane separator 19 can be communicated with the described other end of liquid discharge nozzle 2, will carrying out further Separation of Solid and Liquid through the liquid material that described inner eddy flow separator separates, thereby described film separating step comprises utilizing and is positioned at paste state bed reactor 10 outer 19 pairs of isolated liquid materials of membrane separator and carries out further Separation of Solid and Liquid.In this case, above-mentioned storage tank 17 and outside cyclone separator 18 are not set, but membrane separator 19 directly is connected with the port of the liquid discharge nozzle 2 of inner eddy flow separator 11.Thereby this embodiment can be saved the cost of piece-rate system, but the degree of purity of the liquid material that liquid discharge nozzle 2 is flowed out requires higher relatively.
If be provided with piping filter 13 in liquid discharge nozzle 2, then above-mentioned film separating step comprises that the liquid material that utilizes after being positioned at paste state bed reactor 10 19 pairs outer of membrane separators step being separated after filtration carries out further Separation of Solid and Liquid.In this embodiment, because the liquid material that separates acquisition through the inner eddy flow separating step has passed through filtration treatment through piping filter 13 time, thereby the fluent material after membrane separator 19 separates can obtain better degree of purity.
For another example, the charging aperture of membrane separator 19 is communicated with storage tank 17, so that the material in the storage tank 17 is carried out further Separation of Solid and Liquid, then described film separating step comprises and utilizes the liquid material that is arranged in the outer 19 pairs of storage tanks 17 of membrane separator of paste state bed reactor 10 to carry out further Separation of Solid and Liquid.
And for example, be provided with in piece-rate system under the situation of outside cyclone separator 18, described membrane separator 19 can be positioned at the downstream of outside cyclone separator 18, is used for the liquid material that separates through described outside cyclone separator 18 is carried out further Separation of Solid and Liquid.Then described film separating step comprises that utilization is positioned at paste state bed reactor 10 outer 19 pairs of liquid materials after outside cyclone separator 18 separates of membrane separator and carries out further Separation of Solid and Liquid.
Under the situation that is provided with storage tank 17 and outside cyclone separator 18, storage tank 17 also can be communicated with membrane separator 19.For example, by the 3rd pipeline 28 shown in Figure 4.Membrane separator 19 separates all right conduct recoil of the part medium that the back obtains comparatively pure liquid material, and is used for piping filter 13 is carried out backflush process.For example, by second pipeline 25 shown in Figure 4.As shown in Figure 4, all communicate from the gas of gas buffer jar 20 with from the liquid material of membrane separator 19 with backwash tube 14.But preferably, the valve (not shown) of control gas and the valve of control liquid material can be set respectively in pipeline, thereby avoid entering backwash tube 14 simultaneously, just use the recoil medium of liquid or the gas step that recoils respectively separately from the gas of gas buffer jar 20 with from the liquid material of membrane separator 19.
Certainly, after the processing of finishing liquid material, the liquid material that meets the demands can be transported in the holder 27.The solid particle (as catalyst granules) that membrane separator 19 separates the back acquisition can turn back to continuation use in the reactor, but as a rule, because the solid grain size that obtain this moment is less, if be transported in the paste state bed reactor 10 more again, can make separation subsequently more difficult, therefore it can be drained, and should not be transported to again in the paste state bed reactor 10 again.
Various combination mode according to piece-rate system, this holder 27 also can be used for receiving liquid material from the liquid discharge nozzle 2 of inner eddy flow separator 11, from the liquid material of storage tank 17, from the liquid material of outside cyclone separator 18, as long as this liquid material satisfies the condition that is stored in holder 27.
More than described the specific embodiment of slurry attitude bed Reaction Separation provided by the present invention system, and the feed separation method that is used to starch the reaction of attitude bed provided by the invention has been described in detail in the lump in conjunction with this slurry attitude bed Reaction Separation system.But, it will be understood by those skilled in the art that above detailed description to theme of the present invention is descriptive, rather than be used to limit scope of the present invention.Protection scope of the present invention should be limited by claim.And, under the prerequisite that does not break away from protection domain of the present invention, can make various improvement, interpolation, deletion and replacement etc. to foregoing description of the present invention.Therefore, the parts (as piping filter 13, storage tank 17, outside cyclone separator 18, membrane separator 19 etc.) that relate in the above-mentioned slurry attitude bed Reaction Separation system, and in the above-mentioned separation method related step (as recoil step, filtration step, outside solid-liquid rotational flow separation step, film separating step etc.) can both be in any way individually and/or in combination in conjunction with in the present invention.
In addition, though foregoing description mainly is described in conjunction with the use of paste state bed reactor, the present invention is not limited to this.Under the enlightenment of the description of above specification, technical scheme provided by the present invention also can be applicable to the workplace of any suitable use technical scheme of the present invention.But preferably, the reaction of carrying out in paste state bed reactor 10 is a Fischer-Tropsch synthesis, and the described serum materials that is produced by reaction contains product liquid and the employed solid catalyst of reaction that responds and produce.
The present invention also provides the application of above-mentioned slurry attitude bed Reaction Separation system in fischer-tropsch synthesis process.
Claims (38)
1. cyclone separator, this cyclone separator comprises that top is that cylindrical, the bottom of top closure is obconic cyclone separator main body (1), it is characterized in that this cyclone separator also comprises liquid discharge nozzle (2), solid discharge nozzle (3) and at least one suction tube (4); One end of described liquid discharge nozzle (2) is positioned at described cyclone separator main body (1), the other end and passes the top of described cyclone separator main body (1) and be positioned at outside the described cyclone separator main body; Described solid discharge nozzle (3) is connected in the bottom of described cyclone separator main body (1) and is communicated with the inner space of described cyclone separator main body (1); One end of described suction tube (4) is communicated with eddy flow charging aperture (5) in the described cyclone separator main body (1), the other end extends towards the bottom direction of described cyclone separator main body (1); The bottom of described solid discharge nozzle (3) is higher than the bottom of described suction tube (4).
2. cyclone separator according to claim 1, wherein, the bottom level of described solid discharge nozzle (3) is than the high 50-500mm of bottom level of described suction tube (4).
3. cyclone separator according to claim 1, wherein, the length of described liquid discharge nozzle (2) in cyclone separator is the 1/4-1/2 of diameter of the cylindrical part of described cyclone separator main body (1).
4. according to any described cyclone separator among the claim 1-3, wherein, on described solid discharge nozzle (3), be connected with baiting valve (6).
5. starch attitude bed Reaction Separation system for one kind, comprise paste state bed reactor (10) and equipment for separating liquid from solid, it is characterized in that, described equipment for separating liquid from solid comprises the inner eddy flow separator (11) that is arranged in the described paste state bed reactor (10), this inner eddy flow separator (11) comprises at least one suction tube (4), and this suction tube (4) can be drawn into the serum materials in the described paste state bed reactor (10) in the described inner eddy flow separator (11) and carry out the solid-liquid rotational flow separation.
6. slurry attitude bed Reaction Separation according to claim 5 system, wherein, described inner eddy flow separator (11) comprises that top is that cylindrical, the bottom of top closure is obconic cyclone separator main body (1); The upper end of described suction tube (4) is communicated with eddy flow charging aperture (5) in the described cyclone separator main body (1), and the lower end of described suction tube (4) can extend in the serum materials (12) in the described paste state bed reactor (10); The bottom of described inner eddy flow separator main body (1) is provided with solid discharge nozzle (3), is connected with baiting valve (6) on this solid discharge nozzle (3); Described equipment for separating liquid from solid also comprises liquid discharge nozzle (2), one end of described liquid discharge nozzle (2) is positioned at described cyclone separator main body (1), and the other end of described liquid discharge nozzle (2) passes the top of described cyclone separator main body (1) and is positioned at the outside of described paste state bed reactor (10).
7. slurry attitude bed Reaction Separation according to claim 6 system, wherein, the bottom level of described solid discharge nozzle (3) is than the high 50-500mm of bottom level of described suction tube (4).
8. slurry attitude bed Reaction Separation according to claim 6 system, wherein, described liquid discharge nozzle (2) is provided with piping filter (13).
9. slurry attitude bed Reaction Separation according to claim 8 system, wherein, described piping filter (13) is connected with backwash tube (14).
10. slurry attitude bed Reaction Separation according to claim 9 system, wherein, described equipment for separating liquid from solid comprises two described inner eddy flow separators (11,11 ') that can be used alternatingly, and each described inner eddy flow separator is provided with piping filter and backwash tube.
11. according to any described slurry attitude bed Reaction Separation system among the claim 6-10, wherein, this slurry attitude bed Reaction Separation system also comprises the storage tank (17) that is positioned at described paste state bed reactor (10) outside, and this storage tank is communicated with the described other end of described liquid discharge nozzle.
12. according to any described slurry attitude bed Reaction Separation system among the claim 6-10, wherein, described liquid discharge nozzle (2) is provided with pump, and the operation of described pump makes the serum materials (12) in the described paste state bed reactor (10) to enter to carry out the solid-liquid rotational flow separation in the described inner eddy flow separator (11) and make isolated liquid material can derive described paste state bed reactor (10).
13. slurry attitude bed Reaction Separation according to claim 11 system, wherein, the position of described storage tank (17) is arranged so that the liquid level of the interior liquid material of this storage tank (17) is lower than the liquid level of serum materials (12) in the described paste state bed reactor (10), carry out the solid-liquid rotational flow separation thereby make the interior serum materials (12) of described paste state bed reactor (10) under the effect of described paste state bed reactor (10) inside and outside differential pressure, enter described inner eddy flow separator (11), and make isolated liquid material can derive described paste state bed reactor (10).
14. according to any described slurry attitude bed Reaction Separation system among the claim 6-10, wherein, described equipment for separating liquid from solid also comprises the outside cyclone separator (18) that is positioned at outside the described paste state bed reactor (10), the charging aperture of this outside cyclone separator (18) is communicated with the described other end of described liquid discharge nozzle (2), carrying out further solid-liquid rotational flow separation through the liquid material that described inner eddy flow separator (11) separates.
15. slurry attitude bed Reaction Separation according to claim 11 system, wherein, described equipment for separating liquid from solid also comprises the outside cyclone separator (18) that is positioned at outside the described paste state bed reactor (10), the charging aperture of described outside cyclone separator (18) is communicated with described storage tank (17), so that the material in the described storage tank (17) is carried out further solid-liquid rotational flow separation.
16. according to any described slurry attitude bed Reaction Separation system among the claim 6-10, wherein, described equipment for separating liquid from solid also comprises the membrane separator (19) that is positioned at outside the described paste state bed reactor (10), the charging aperture of this membrane separator (19) is communicated with the described other end of described liquid discharge nozzle (2), carrying out further Separation of Solid and Liquid through the liquid material that described inner eddy flow separator (10) separates.
17. slurry attitude bed Reaction Separation according to claim 11 system, wherein, described equipment for separating liquid from solid also comprises the membrane separator (19) that is positioned at outside the described paste state bed reactor (10), the charging aperture of described membrane separator (19) is communicated with described storage tank (17), so that the material in the described storage tank (17) is carried out further Separation of Solid and Liquid.
18. slurry attitude bed Reaction Separation according to claim 14 system, wherein, described equipment for separating liquid from solid also comprises the membrane separator (19) that is positioned at described outside cyclone separator (18) downstream, carrying out further Separation of Solid and Liquid through the liquid material that described outside cyclone separator (18) separates.
19. slurry attitude bed Reaction Separation according to claim 15 system, wherein, described equipment for separating liquid from solid also comprises the membrane separator (19) that is positioned at described outside cyclone separator (18) downstream, carrying out further Separation of Solid and Liquid through the liquid material that described outside cyclone separator (18) separates.
20. the application of any described slurry attitude bed Reaction Separation system in fischer-tropsch synthesis process among the claim 5-19.
21. feed separation method that is used to starch the reaction of attitude bed, this method comprises inner solid-liquid rotational flow separation step, this inside solid-liquid rotational flow separation step comprises being drawn in the inner eddy flow separator (11) by at least one suction tube (4) by reacting the serum materials that produces in the paste state bed reactor (10), in this inner eddy flow separator (11) serum materials that transports is carried out inner solid-liquid rotational flow separation, described inner eddy flow separator (11) is arranged on the inside of described paste state bed reactor (10).
22. method according to claim 21, wherein, described inner solid-liquid rotational flow separation step comprises that also the solid material that described solid-liquid rotational flow separation is obtained is discharged in the described paste state bed reactor (10) off and on, the liquid material of described solid-liquid rotational flow separation acquisition is transported to the outside of described paste state bed reactor (10).
23. method according to claim 21, wherein, this method comprises that also employing piping filter (13) will carry out the filtration step of further Separation of Solid and Liquid through the liquid material that described inner solid-liquid rotational flow separation obtains.
24. method according to claim 23, wherein, this method also comprises utilizes the recoil medium that described piping filter (13) is carried out the recoil step of backflush process, and described recoil step and described inner solid-liquid rotational flow separation step hocket.
25. method according to claim 24, wherein, the inner eddy flow separator (11,11 ') that is arranged in this paste state bed reactor (10) is two, and when one of them carried out described recoil step, another carried out described inner solid-liquid rotational flow separation step.
26. according to any described method among the claim 21-25, wherein, this method comprises that also the liquid material that will separate acquisition is stored into the storage tank (17) that is arranged in described paste state bed reactor (10) outside.
27. method according to claim 26, wherein, the position of described storage tank (17) is set to make that the liquid level of the interior liquid material of this storage tank (17) is lower than the liquid level of the serum materials in the described paste state bed reactor (10), carry out the solid-liquid rotational flow separation thereby make the interior serum materials of described paste state bed reactor (10) under the effect of described paste state bed reactor (10) inside and outside differential pressure, enter described inner eddy flow separator (11), and make the liquid material that separates acquisition derive described paste state bed reactor (10) by described suction tube (4).
28. according to any described method among the claim 21-25, wherein, by pump the serum materials in the described paste state bed reactor (10) is pumped in the described inner eddy flow separator (11) and carries out the solid-liquid rotational flow separation, and make and separate the liquid material that obtains and derive described paste state bed reactor (10).
29. according to claim 21 or 22 described methods, wherein, this method also comprises outside solid-liquid rotational flow separation step, and this outside solid-liquid rotational flow separation step comprises utilizes the outside cyclone separator (18) that is positioned at outside the described paste state bed reactor (10) that isolated liquid material is carried out further solid-liquid rotational flow separation.
30. according to any described method among the claim 23-25, wherein, this method also comprises outside solid-liquid rotational flow separation step, and this outside solid-liquid rotational flow separation step comprises utilizes the outside cyclone separator (18) that is positioned at outside the described paste state bed reactor (10) that the liquid material after separating through described filtration step is carried out further solid-liquid rotational flow separation.
31. method according to claim 26, wherein, this method also comprises outside solid-liquid rotational flow separation step, and this outside solid-liquid rotational flow separation step comprises utilizing and is arranged in the outer outside cyclone separator (18) of described paste state bed reactor (10) liquid material of described storage tank (17) is carried out further solid-liquid rotational flow separation.
32. according to claim 21 or 22 described methods, wherein, this method also comprises the film separating step, and this film separating step comprises that utilization is positioned at the outer membrane separator (19) of described paste state bed reactor (10) isolated liquid material is carried out further Separation of Solid and Liquid.
33. according to any described method among the claim 23-25, wherein, this method also comprises the film separating step, and this film separating step comprises that utilization is positioned at the outer membrane separator (19) of described paste state bed reactor (10) liquid material after separating through described filtration step is carried out further Separation of Solid and Liquid.
34. method according to claim 26, wherein, this method also comprises the film separating step, and this film separating step comprises utilizing and is arranged in the outer membrane separator (19) of described paste state bed reactor (10) liquid material of described storage tank (17) is carried out further Separation of Solid and Liquid.
35. method according to claim 29, wherein, this method also comprises the film separating step, and this film separating step comprises that utilization is positioned at the outer membrane separator (19) of described paste state bed reactor (10) liquid material after separating through described outside cyclone separator (18) is carried out further Separation of Solid and Liquid.
36. method according to claim 30, wherein, this method also comprises the film separating step, and this film separating step comprises that utilization is positioned at the outer membrane separator (19) of described paste state bed reactor (10) liquid material after separating through described outside cyclone separator (18) is carried out further Separation of Solid and Liquid.
37. method according to claim 31, wherein, this method also comprises the film separating step, and this film separating step comprises that utilization is positioned at the outer membrane separator (19) of described paste state bed reactor (10) liquid material after separating through described outside cyclone separator (18) is carried out further Separation of Solid and Liquid.
38. method according to claim 21, wherein, described reaction is a Fischer-Tropsch synthesis, and the described serum materials that is produced by reaction contains product liquid and the employed solid catalyst of reaction that responds and produce.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020143140A1 (en) * | 2019-01-10 | 2020-07-16 | 清华大学 | Separation system for slurry bed reactor |
| CN111991905A (en) * | 2020-07-30 | 2020-11-27 | 国家能源集团宁夏煤业有限责任公司 | Method and device for solid-liquid separation of slurry discharged from slurry bed |
| WO2022040844A1 (en) * | 2020-08-24 | 2022-03-03 | 中国科学院青岛生物能源与过程研究所 | Method and apparatus for extracting clean liquid from slurry reactor |
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| CN1233453C (en) * | 2003-09-03 | 2005-12-28 | 上海兖矿能源科技研发有限公司 | Automatic filtering/back purging system liquid and solid separation for in three phase paste state bed reactor |
| CN1319635C (en) * | 2005-09-12 | 2007-06-06 | 南京工业大学 | Separation process of synthetic oil catalyst prepared in slurry bed reactor |
| CN201470490U (en) * | 2009-09-07 | 2010-05-19 | 中国石油化工股份有限公司 | cyclone separator |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020143140A1 (en) * | 2019-01-10 | 2020-07-16 | 清华大学 | Separation system for slurry bed reactor |
| CN111991905A (en) * | 2020-07-30 | 2020-11-27 | 国家能源集团宁夏煤业有限责任公司 | Method and device for solid-liquid separation of slurry discharged from slurry bed |
| WO2022040844A1 (en) * | 2020-08-24 | 2022-03-03 | 中国科学院青岛生物能源与过程研究所 | Method and apparatus for extracting clean liquid from slurry reactor |
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