CN1201842C - Method and equipment for separating synthetic oil and catalyst in slurry reactor - Google Patents
Method and equipment for separating synthetic oil and catalyst in slurry reactor Download PDFInfo
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- CN1201842C CN1201842C CN 03118581 CN03118581A CN1201842C CN 1201842 C CN1201842 C CN 1201842C CN 03118581 CN03118581 CN 03118581 CN 03118581 A CN03118581 A CN 03118581A CN 1201842 C CN1201842 C CN 1201842C
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Abstract
The present invention discloses a separation method of liquid synthetic oil and a solid catalyst in a slurry state bed reactor and a device. The method of the present invention is characterized in that oil slurry containing a catalyst is distributed with a group of separating units; after the settlement separation is carried out, the solid catalyst can form concentrated oil slurry by downward settlement, and is sent back to the reaction zone of a slurry state bed reactor; a part of synthetic oil can upward flow and form purifying oil in a separated mode with the concentrated oil slurry, and the purifying oil is main products of the reactor. The separating unit comprises a casing, an oil slurry inlet, an oil slurry distribution pipe, a lower partition plate, a concentrated oil slurry outlet, an upper partition plate and a purifying oil outlet. The present invention has the characteristics of simple and available structure and stable device running.
Description
Technical field
The invention belongs to Separation of Solid and Liquid, especially the separation method of liquid artificial oil and solid catalyst and equipment in the paste state bed reactor.
Background technology
Paste state bed reactor is the gas-solid liquid reactor that is used for the F-T method, and wherein the isolation technics of liquid artificial oil and solid catalyst is the key of this reaction process always.
US4605678 has proposed to allow slurries to be separated by a kind of magnetization filter element with high-gradient magnetic field, make catalyst and synthetic oil from.Purify the product further upgrading processing of artificial oil as paste state bed reactor, isolated catalyst is by backwash filter element Returning reactor.Though high-gradient magnetic field helps to have the separation of ferromagnetism catalyst, but still needs filter element to filter catalyst, stop up filter part micropore problem with regard to unavoidable generation catalyst like this.
US5811469 has proposed to carry out separating of artificial oil and catalyst with a kind of downcomer charging product filter in slurry attitude bed synthesis reactor.In reactor, adopt an enterprising conduit that goes out down, a tubular type filter is arranged in the conduit, to be separated contains catalyst slurry from the conduit conduit that enters suitable for reading, because the sedimentation of catalyst concentrates, the serum density of conduit bottom is increased, and flow downward rapidly from the conduit end opening comes out to enter slurries the reactor.When the slurries that contain catalyst were flowed through conduit from top to bottom, the part artificial oil entered in the filter tube by filter filter part, and extracts reactor out thus, reached separating of artificial oil and catalyst.The artificial oil that this patent is described is difficult to realize that this is because also there is settlement issues in the catalyst in the reactor slurry, therefore also has the catalyst concentration gradient with separating of catalyst.Slurry oil in the outer reactor of the density of conduit bottom slurries and end opening does not exist density contrast or density to differ very little, the flowing velocity of slurries is very little in the conduit, be difficult to form the crossing current state on filter filter part surface, can't stop trickle catalyst granules to enter filter part micropore and stop up filtration channel, the filter filter efficiency be descended gradually or ineffective fully.
US6217830 propose to use varsol to carry out the method for supercritical extract under super critical condition, carries out separating of artificial oil and catalyst.Make and be in overcritical or contact with the synthetic slurry oil that contains catalyst near the varsol of supercriticality, under certain temperature and pressure condition, the part artificial oil is dissolved in and forms rich synthetic oil phase in the varsol, another part artificial oil and catalyst then form rich catalyst slurry, by separating this two-phase, reach separating of artificial oil and catalyst.The method and apparatus complexity that this patent is described, equipment investment and operating cost are all bigger.
Summary of the invention
The present invention is the separator that adopts solid-liquid counter-current separation principle and a plurality of separative element in parallel to form, a kind of simple continuous solid-liquid separating method is provided for the catalyst slurry that contains in the paste state bed reactor, make in the device that artificial oil describes by the present invention or the outer separator of device is constantly separated, for the operation of paste state bed reactor continous-stable provides condition.The present invention also provides this method used separation equipment in addition.
The invention provides the separation method of a kind of paste state bed reactor liquid artificial oil and solid catalyst, it is characterized in that: the slurry oil distribution that contains catalyst enters a component from the unit, in separative element, carry out sedimentation separation, the downward sedimentation of solid catalyst forms concentrated slurry oil, discharge separative element then, the concentrated slurry oil that each separative element is discharged is sent the reaction zone of paste state bed reactor back to; The part artificial oil upwards flows, and separates the formation clean oil with concentrated slurry oil, upwards discharges separative element then, and the clean oil that each separative element comes out becomes the major product of reactor.
The separation equipment that the inventive method is used, it is characterized in that: this separation equipment is made up of from the unit a component, wherein separative element is a kind of body structure, comprises housing, slurry oil inlet, slurry oil distributor pipe, division board, concentrated slurry oil outlet down, goes up division board and clean oil outlet.
It is the porous coil pipe that the present invention recommends the slurry oil distributor pipe, and last division board and following division board are porous plate or porous coil pipe.
The number of described separative element is by the decision of the character of the character of the diameter of the output of paste state bed reactor artificial oil, separative element, slurries and catalyst.
Equipment for separating liquid from solid of the present invention both can use in the outside of paste state bed reactor, also can use in the inside of paste state bed reactor.When inside reactor uses, both can be positioned at reaction zone top, also can be positioned at the reaction zone bottom.
Big for liquid viscosity height, density, solid particle is little, the Separation of Solid and Liquid situation of difficult, can when entering separator, solidliquid mixture add certain amount of solvent or diluent, liquid viscosity, density are diminished, thereby accelerate the sedimentation separation of solid particle, also can take high-intensity magnetic field in the separative element bottom, make ferromagnetism solid catalyst particle in the slurry oil under magnetic field effect, accelerate the speed of sedimentation separation.
Solid-liquid separating method of the present invention and equipment, the low problem of separative efficiency that has caused at filter part surface deposition because of a large amount of solid particles when having solved isolated by filtration.Compared with prior art, the present invention has simple and characteristics stable equipment operation.At first, slurry attitude bed F-T synthetic catalysts such as precipitation swage for present employing, because the smallest particles diameter is greater than 20 microns, separative element can not use filter element, therefore in equipment running process, there is not the blockage problem of filtering part, and the stability of the separative efficiency of artificial oil and device operation all will significantly improve, and under the situation of particularly separating in device, can keep the long-term stability operation of reactor.
Accompanying drawing and description of drawings
Fig. 1 is a kind of separation equipment of being made up of 8 separative elements of the present invention.
Fig. 2 is a kind of structure of separative element of the present invention.
Fig. 3 is the another kind of structure of separative element of the present invention.
Fig. 4 is the third structure of separative element of the present invention.
Fig. 5 is the 4th a kind of structure of separative element of the present invention.
Fig. 6 is a kind of structure of porous coil pipe.
Fig. 7 is a kind of structure of porous plate.
Fig. 8 is a kind of structure that separation equipment of the present invention is positioned at paste state bed reactor top.
Fig. 9 is the another kind of structure that separation equipment of the present invention is positioned at paste state bed reactor top.
Figure 10 is the third structure that separation equipment of the present invention is positioned at paste state bed reactor top.
Figure 11 is a kind of structure that separation equipment of the present invention is positioned at the paste state bed reactor bottom.
Figure 12 is the another kind of structure that separation equipment of the present invention is positioned at the paste state bed reactor bottom.
Figure 13 is the third structure that separation equipment of the present invention is positioned at the paste state bed reactor bottom.
As shown in Figure 1, the oil-catalyst slurry that contains that is produced by slurry attitude bed F-T synthesis reactor enters a component from the unit by 1 distribution of slurry oil inlet, in separative element, carry out sedimentation separation, the downward sedimentation of solid catalyst forms concentrated slurry oil, discharge separative element by concentrated slurry oil outlet 3 then, send the reaction zone of paste state bed reactor after the concentrated slurry oil that each separative element is discharged merges back to; The part artificial oil upwards flows, and separates the formation clean oil with concentrated slurry oil, upwards discharges separative element by clean oil outlet 2 then, becomes the major product of reactor after the clean oil that each separative element comes out merges.
The number of separative element shown in Figure 1 is 8, in the practical application: as being 10 meters for a diameter, the slurry attitude bed F-T synthesis reactor of year producing 500,000 tons of artificial oils, when adopting in the device separation method, the number of separative element is 1-8; For catalyst can sedimentation in 60 minutes 20 centimetres contain the catalyst slurry liquid system, with the separation equipment of the separative element composition of 7 10 rice diameters, can reach separating fully of artificial oil and concentrated slurry oil.The number of separative element can be determined with following formula of reduction:
In the formula: the number of n---separative element
The annual production of w---artificial oil, kg
The kinematic viscosity of slurry oil in the v---separative element, m
2/ s
π---pi
D---separative element diameter, m
T---on-stream time, s
D---separating catalyst minimum diameter, m
ρ
C---density of catalyst, kg/m
3
ρ
0--slurry oil density in the-separative element, kg/m
3
G---acceleration of gravity, m/s
2
Among Fig. 2, Fig. 3, Fig. 4 and Fig. 5, separative element comprises housing 23, be positioned at the slurry oil distributor pipe 5 at housing 23 middle parts, be positioned at the last division board 9 on housing 23 tops and be positioned at the following division board 6 of housing 23 bottoms.
Among Fig. 2, slurry oil distributor pipe 5 is porous coil pipes, and the porous coil pipe is provided with slurry oil inlet 1, and following division board 6 and last division board 9 are porous plates, and following division board 6 belows form down gathering room 7, and following gathering room 7 is provided with and concentrates slurry oil outlet 3; Last division board 9 tops form gathering room 10, and last gathering room 10 is provided with clean oil outlet 2.During use, slurry oil to be separated enters separative element inside by slurry oil inlet 1, radially be uniformly distributed in the separative element through slurry oil distributor pipe 5, because the sedimentation of catalyst, form concentrated slurry oil in the separative element bottom, concentrated slurry oil warp division board 6 down enters down gathering room 7, exports 3 extraction separative elements through concentrating slurry oil again.Clean oil upwards enters gathering room 10 through last division board 9, under the effect of external and internal pressure difference, discharges separative element through clean oil outlet 2.
The difference of Fig. 3 and Fig. 2 is: following division board 6 is porous coil pipes, which is provided with to concentrate slurry oil outlet 3, and the concentrated slurry oil that forms in the separative element bottom during use enters down in the porous coil pipe of division board 6 and by concentrated slurry oil and exports 3 extraction separative elements.
The difference of Fig. 4 and Fig. 2 is: going up division board 9 is porous coil pipes, which is provided with clean oil outlet 2, during use, discharges separative element in the porous coil pipe of division board 9 and by clean oil outlet 2 on the clean oil in separative element upwards enters.
The difference of Fig. 5 and Fig. 2 is: following division board 6 and last division board 9 all are porous coil pipes, and the porous coil pipe of following division board 6 is provided with and concentrates slurry oil outlet 3, and the porous coil pipe of last division board 9 is provided with clean oil outlet 2.During use: in separative element, because the sedimentation of catalyst forms concentrated slurry oil in the separative element bottom, concentrated slurry oil enters down in the porous coil pipe of division board 6 and by concentrated slurry oil and exports 3 extraction separative elements; Clean oil upwards enters in the porous coil pipe of division board 9, under the effect of external and internal pressure difference, discharges separative element through clean oil outlet 2.
As shown in Figure 6, the porous coil pipe constitutes three layers of donut by pipe, is made of channel connection between annulus, has aperture 22 on the porous coil pipe.When porous coil pipe during as slurry oil distributor pipe 5, hole 22 openings are all downward, and when as last division board 9 or down during division board 6, the opening direction in hole 22 can make progress, also can be downward.The porous coil pipe is provided with the medium gateway, and when as slurry oil distributor pipe 5, the medium gateway is a slurry oil inlet 1; When as last oil collecting pipe 9, the medium gateway is clean oil outlet 2; When as next part oil pipe 6, the medium gateway is for concentrating slurry oil outlet 3.This porous coil pipe also can be other shape, as spirality etc.
As shown in Figure 7, porous plate is for offering the pore structure of many circles on a flat board.Can certainly offer the hole of other shape, this not added restriction, porous plate also can adopt grid or grid configuration.
Fig. 8 is positioned at the middle structure of reactor for gas channel 19; Fig. 9 is positioned at reactor structure all around for gas channel 19; Figure 10 is positioned at the outer structure of reactor device for gas channel 19.
As Fig. 8, Fig. 9 and shown in Figure 10, synthesis gas 16 enters the reaction zone 18 of paste state bed reactor through feed distributor 17, product and unreacting material upwards enter gas-liquid separation zone 20 through gas channel 19, overflow in the gas from liquid, discharge from reactor head outlet 30.The oil-catalyst slurry baffling that contains after the degassing enters equipment for separating liquid from solid through the slurry oil inlet 1 of each separative element, after Separation of Solid and Liquid, concentrate slurry oil by concentrating the reaction zone of sending back to after slurry oil outlet 3 is discharged in the reactor, clean oil is discharged the back as the reactor major product by clean oil outlet 2, discharges reactor under the effect of external and internal pressure difference.Vertical wear or the gas channel 19 of the outer separator of device can be one also can be a plurality of.
Figure 11 is positioned at the middle structure of reactor for gas channel 19, and Figure 12 is positioned at reactor structure all around for gas channel 19, and Figure 13 is positioned at the outer structure of reactor device for gas channel 19.
As Figure 11, Figure 12 and shown in Figure 13, synthesis gas 16 enters the reaction zone 18 of paste state bed reactor through feed distributor 17,, product and unreacting material upwards enter gas-liquid separation zone 20, overflow in the gas from liquid, discharge from reactor head outlet 30.The slurry oil that contains catalyst enters sedimentation separation district 32 through gas channel 19, and most of catalyst concentrates in the sedimentation of sedimentation separation district, concentrates slurry oil and is extracted out the reaction zone that sends back to the reactor by concentrating slurry oil outlet 33 by pump from reactor bottom.Clarification slurry oil baffling enters equipment for separating liquid from solid through the slurry oil inlet 1 of each separative element, after Separation of Solid and Liquid, concentrated slurry oil in the separator is extracted the reaction zone that sends back in the reactor by concentrating slurry oil outlet 3 out by pump, and clean oil is discharged reactor by clean oil outlet 2 under the effect of external and internal pressure difference.Vertical wear or the gas channel 19 of the outer separator of device can be one also can be a plurality of.
Equipment for separating liquid from solid of the present invention is used for starching the separation that attitude bed F-T synthesis reactor contains oil-catalyst slurry, and the separation especially for containing oil-catalyst slurry in the indirect coal liquefaction slurry attitude bed synthesis reactor also can be used for other similar Separation of Solid and Liquid place.
The isolated concentrated slurry oil of self-separation device of the present invention, the mode that exports reaction zone 18 in 3 Returning reactors by concentrated slurry oil can be to return after establishing the pump pressurization on the return pipeline, also can be to utilize synthesis gas 16 incoming flows to form pressure reduction through swab will concentrate slurry oil suction reaction zone.
Claims (4)
1. the separation method of artificial oil and catalyst in the paste state bed reactor, it is characterized in that: the slurry oil distribution that contains catalyst enters a component from the unit, in separative element, carry out sedimentation separation, the downward sedimentation of solid catalyst forms concentrated slurry oil, discharge separative element then, the concentrated slurry oil that each separative element is discharged is sent the reaction zone of paste state bed reactor back to; The part artificial oil upwards flows, and separates the formation clean oil with concentrated slurry oil, discharges separative element then, and the clean oil that each separative element comes out becomes the major product of reactor.
2. separation method according to claim 1 is characterized in that: contain the slurry oil elder generation and solvent or mixing diluents of catalyst, enter separative element again.
3. separation method according to claim 2 is characterized in that: be applied with high-intensity magnetic field in the separative element bottom.
4. realize the separation equipment of separation method according to claim 1 for one kind, it is characterized in that: this separation equipment is made up of from the unit a component, wherein separative element is a kind of body structure, comprise housing, the slurry oil distributor pipe, following division board and last division board, described slurry oil distributor pipe is positioned at the middle part of housing, last division board is positioned at the top of housing, following division board is positioned at lower part of frame, the slurry oil distributor pipe is the porous coil pipe, the porous coil pipe is provided with the slurry oil inlet, last division board and following division board are porous plate or porous coil pipe, when last division board was porous plate, its top forms went up gathering room, and last gathering room is provided with the clean oil outlet, when last division board was the porous coil pipe, the porous coil pipe was provided with the clean oil outlet; When division board was porous plate instantly, its below formed gathering room down, and following gathering room is provided with and concentrates the slurry oil outlet, and when division board was the porous coil pipe instantly, the porous coil pipe was provided with and concentrates the slurry oil outlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03118581 CN1201842C (en) | 2003-01-28 | 2003-01-28 | Method and equipment for separating synthetic oil and catalyst in slurry reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03118581 CN1201842C (en) | 2003-01-28 | 2003-01-28 | Method and equipment for separating synthetic oil and catalyst in slurry reactor |
Publications (2)
| Publication Number | Publication Date |
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| CN1433838A CN1433838A (en) | 2003-08-06 |
| CN1201842C true CN1201842C (en) | 2005-05-18 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 03118581 Expired - Fee Related CN1201842C (en) | 2003-01-28 | 2003-01-28 | Method and equipment for separating synthetic oil and catalyst in slurry reactor |
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1319635C (en) * | 2005-09-12 | 2007-06-06 | 南京工业大学 | Separation process for preparing synthetic oil catalyst by slurry bed reactor |
| CN100443155C (en) | 2006-05-31 | 2008-12-17 | 中国石油化工股份有限公司 | Slurry bed circulatory flow reactor and uses thereof |
| CN101970604A (en) * | 2008-03-14 | 2011-02-09 | 日本石油天然气·金属矿物资源机构 | Method for removing magnetic particles from Fischer-Tropsch crude oil, and method for producing Fischer-Tropsch crude oil |
| CN105344467A (en) * | 2014-08-21 | 2016-02-24 | 扬州市大洋水务设备有限公司 | Novel magnetic separation settler |
| CN104888667B (en) * | 2015-05-15 | 2018-01-02 | 神华集团有限责任公司 | The Fischer-Tropsch synthetic piece-rate system and method for a kind of paste state bed reactor |
| CN106512867B (en) * | 2015-09-11 | 2019-07-02 | 国家能源投资集团有限责任公司 | The method for arranging of gas-liquid-solid multiphase flow reactor and its filter |
| CN105771817B (en) * | 2016-04-20 | 2017-12-26 | 武汉凯迪工程技术研究总院有限公司 | The separator and method of catalyst and heavy hydrocarbon in paste state bed reactor |
| CN111303937A (en) * | 2019-08-20 | 2020-06-19 | 武汉兰兆科技有限公司 | Electric separation device and electric separation process for on-line recycling of Fischer-Tropsch synthesis catalyst |
| CN113969181B (en) * | 2020-07-24 | 2023-01-10 | 中国石油化工股份有限公司 | Device and method for separating solid particles in catalytic cracking slurry oil |
| CN113969182B (en) * | 2020-07-24 | 2023-01-10 | 中国石油化工股份有限公司 | Device and method for separating solid particles in catalytic cracking slurry oil |
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Granted publication date: 20050518 Termination date: 20110128 |