CN111187637A - System and method for separating waste catalyst in Fischer-Tropsch synthesis slag wax - Google Patents

System and method for separating waste catalyst in Fischer-Tropsch synthesis slag wax Download PDF

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Publication number
CN111187637A
CN111187637A CN201811362313.6A CN201811362313A CN111187637A CN 111187637 A CN111187637 A CN 111187637A CN 201811362313 A CN201811362313 A CN 201811362313A CN 111187637 A CN111187637 A CN 111187637A
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China
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wax
catalyst
magnetic separation
synthetic wax
fischer
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Inventor
陈强
孟祥堃
胡云剑
门卓武
李永龙
卜亿峰
杨如意
张雪冰
王涛
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China Energy Investment Corp Ltd
National Institute of Clean and Low Carbon Energy
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China Energy Investment Corp Ltd
National Institute of Clean and Low Carbon Energy
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Priority to CN201811362313.6A priority Critical patent/CN111187637A/en
Publication of CN111187637A publication Critical patent/CN111187637A/en
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    • CCHEMISTRY; METALLURGY
    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10GCRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
    • C10G2/00Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon
    • C10G2/30Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen
    • C10G2/32Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts
    • C10G2/33Production of liquid hydrocarbon mixtures of undefined composition from oxides of carbon from carbon monoxide with hydrogen with the use of catalysts characterised by the catalyst used
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03CMAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03C1/00Magnetic separation
    • B03C1/02Magnetic separation acting directly on the substance being separated
    • B03C1/10Magnetic separation acting directly on the substance being separated with cylindrical material carriers
    • B03C1/14Magnetic separation acting directly on the substance being separated with cylindrical material carriers with non-movable magnets

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention relates to the field of Fischer-Tropsch synthesis slag wax treatment, and discloses a system and a method for separating a waste catalyst in Fischer-Tropsch synthesis slag wax. The system comprises: the device comprises a primary magnetic separation device, a synthetic wax intermediate tank, a waste catalyst receiving tank, a secondary magnetic separation device, a synthetic wax storage tank, a fine catalyst receiving tank and an incinerator; wherein, one-level magnetic separation device and second grade magnetic separation device all include: the device comprises a closed box body, a rotary sealing rotary drum, a magnet and a scraper blade, wherein the closed box body is provided with a slag wax inlet, a synthetic wax outlet, a waste catalyst outlet and a heating and heat-insulating structure; wherein the position of the magnet corresponds to the space between the wax residue inlet and the synthetic wax outlet in the box body; the scraper is used to remove the spent or fine catalyst on the outer surface of the drum. The recovery of the synthetic wax in the Fischer-Tropsch synthetic wax residue can be better realized.

Description

System and method for separating waste catalyst in Fischer-Tropsch synthesis slag wax
Technical Field
The invention relates to the field of Fischer-Tropsch synthesis slag wax treatment, in particular to a system for separating a waste catalyst in Fischer-Tropsch synthesis slag wax and a method for separating the waste catalyst in the Fischer-Tropsch synthesis wax in the system.
Background
In the slurry bed Fischer-Tropsch synthesis process adopting the iron-based or cobalt-based catalyst, the catalyst is gradually deactivated, so that the catalyst in the slurry bed Fischer-Tropsch synthesis reactor needs to be periodically added and discharged so as to keep the overall activity of the catalyst in the reactor to meet the requirement.
The residual wax discharged from the slurry bed reactor is slurry containing 10-20 wt% of catalyst and wax, and needs to be separated and treated to recover wax. The prior art generally adopts a filtration method to realize the separation of the waste catalyst and the wax, but has the problems of incapability of continuous production, low efficiency and high operation cost.
CN104307235A discloses sediment wax filtration equipment to be located vertical cylinder casing (6) inside central authorities central collecting pipe (5) and be the axis, parallel mount has a plurality of horizontal blade (1), and every horizontal blade (1) includes blade body (11) and surface filtration channel layer, its characterized in that at least: and a sealing device (4) is arranged at the joint of the bottom of the central collecting pipe (5) and the discharge pipe (3), and the sealing device (4) is comprehensively sealed by adopting a sealing ring (41) and a friction plate (43).
CN105542855A discloses a wax residue treatment method, which comprises the following steps: 1) heating the slag wax to keep the wax in the slag wax in a molten state; 2) carrying out high-temperature separation on the slag wax subjected to the heating treatment to obtain molten wax and solid residue; 3) and carrying out incineration treatment on the solid residues.
CN101970605A discloses a process for selectively removing fischer-tropsch catalyst, a process for selectively removing fischer-tropsch catalyst from a fischer-tropsch synthesis reactor, comprising: a step of extracting a slurry containing a Fischer-Tropsch synthesis crude oil obtained by a Fischer-Tropsch synthesis reaction and a magnetic Fischer-Tropsch catalyst from a Fischer-Tropsch synthesis reactor, a step of separating a catalyst having a predetermined particle size or more from the slurry by using a first solid-liquid separation device, and a step of separating a catalyst which has not been separated by the first solid-liquid separation device from the slurry after the catalyst having the predetermined particle size or more has been separated by using a second solid-liquid separation device; wherein the catalyst separated from the slurry by the first solid-liquid separation device is returned to the Fischer-Tropsch synthesis reactor and reused, the catalyst separated from the slurry by the second solid-liquid separation device is discharged outside the system, and the average particle diameter of the catalyst discharged outside the system is smaller than the average particle diameter of the catalyst in the slurry at the outlet of the Fischer-Tropsch synthesis reactor.
CN102186593A discloses a system for separating liquids from solids comprising: an immobilization apparatus comprising an immobilization vessel comprising a bed of magnetizable material and a magnet configured to generate a magnetic field within the immobilization vessel, wherein the immobilization vessel further comprises an immobilization vessel outlet and an immobilization vessel inlet for a fluid comprising a liquid and metal-containing particles.
CN103846160A discloses a separation method of slurry bed fischer-tropsch synthesis heavy product and catalyst, comprising: degassing slurry of Fischer-Tropsch synthesis heavy products from a slurry bed reactor and magnetic Fischer-Tropsch synthesis catalyst particles, and then feeding the slurry into a separator; in the settling zone of the lower middle part of the separator, the large particles of the catalyst are settled by gravity and are primarily separated from the heavy Fischer-Tropsch synthesis product; wherein the dilute slurry enters a magnetic separation area at the middle upper part of the separator, and the thick slurry rich in catalyst particles at the lower part of the separator automatically circulates back to the slurry bed reactor; the middle upper part of the separator is provided with a magnetic separation area close to the wall of the separator, the magnetic separation area consists of a magnet arranged outside the separator, a fluid flow channel in the separator and a catalyst guide pipe, and is provided with n layers of magnetic separation devices; the slurry after the preliminary separation enters a magnetic separation area along the fluid flow channel, a first layer of magnetic separation device from bottom to top of the magnetic separation area firstly adsorbs catalyst particles, when the adsorbed catalyst particles reach a set amount, the magnetic field of the device is removed, the catalyst particles without magnetic adsorption sink to the catalyst guide pipe by gravity, flow to the bottom of the separator along the catalyst guide pipe and circulate back to the slurry bed reactor, meanwhile, a second layer of magnetic separation device from bottom to top of the magnetic separation area is started to adsorb the catalyst particles flowing upwards along with the liquid, then the magnetic field is removed, and the catalyst particles without magnetic adsorption sink to the catalyst guide pipe by gravity; until the nth magnetic separation device starts the magnetic field and removes the magnetic field operation, make more catalyst particles separate and circulate back to the slurry bed reactor in the magnetic separation zone, after the nth magnetic separation device is processed, only contain the heavy product of Fischer-Tropsch synthesis of a small amount of catalyst particles and enter the filtering zone on the upper portion of the separator along the said fluid flow path; one or more groups of filter elements are arranged in the filter area, and the Fischer-Tropsch synthesis heavy product containing a small amount of catalyst particles after magnetic separation is discharged out of the separator after the catalyst particles are further separated by the filter elements; periodically back washing the filter element to make the filtered catalyst particles flow to the bottom of the separator along the guide pipe by means of gravity and circulate back to the slurry bed reactor.
But the practical application of the prior art still has the problems of poor continuous operability, complex process and low recovery rate of the synthetic wax.
Disclosure of Invention
The invention aims to solve the problems of poor operation continuity, complex process and low recovery rate of synthetic wax in the separation of waste catalysts from Fischer-Tropsch synthetic wax residues in the prior art, and provides a system and a method for separating the waste catalysts from the Fischer-Tropsch synthetic wax residues.
In order to achieve the above object, a first aspect of the present invention provides a system for separating a spent catalyst from fischer-tropsch wax residue, comprising:
the device comprises a primary magnetic separation device, a synthetic wax intermediate tank, a waste catalyst receiving tank, a secondary magnetic separation device, a synthetic wax storage tank, a fine catalyst receiving tank and an incinerator; wherein the content of the first and second substances,
the primary magnetic separation device is used for performing primary magnetic separation on Fischer-Tropsch synthesis slag wax generated by the Fischer-Tropsch synthesis device, storing the obtained waste catalyst into the waste catalyst receiving tank, and storing the obtained synthetic wax liquid into the synthetic wax intermediate tank;
the secondary magnetic separation device is used for carrying out secondary magnetic separation on the synthetic wax liquid from the synthetic wax intermediate tank, storing the obtained fine catalyst into the fine catalyst receiving tank, storing the obtained synthetic wax into the synthetic wax storage tank,
the incinerator is used for incinerating the waste catalyst from the waste catalyst receiving tank and the fine catalyst from the fine catalyst receiving tank;
wherein, the first-stage magnetic separation device and the second-stage magnetic separation device both comprise the following parts:
the device comprises a closed box body, a rotary sealing rotary drum, a magnet and a scraper blade, wherein the closed box body is provided with a wax residue inlet, a synthetic wax outlet, a waste catalyst outlet and a heating and heat-insulating structure;
the position of the magnet corresponds to the space between the wax residue inlet and the synthetic wax outlet in the box body, and the magnet is used for attracting the waste catalyst in the Fischer-Tropsch synthetic wax residue or the fine catalyst in the synthetic wax liquid to be attached to the outer surface of the rotary drum; the scraper is used to remove spent or fine catalyst on the outer surface of the drum.
The second aspect of the invention provides a method for separating a waste catalyst in Fischer-Tropsch synthesis slag wax, which comprises the following steps:
(a) carrying out flash evaporation and cooling on the Fischer-Tropsch synthesis product to obtain Fischer-Tropsch synthesis residue wax from which synthesis gas and light hydrocarbon are removed;
(b) introducing the wax residue into the system provided by the invention, and carrying out primary magnetic separation in a primary magnetic separation device of the system under the first heating and inert atmosphere to obtain a waste catalyst and a synthetic wax liquid;
(c) and introducing the synthetic wax liquid into a secondary magnetic separation device of the system, and performing secondary magnetic separation under a second heating and inert atmosphere to obtain the synthetic wax and the fine catalyst.
Preferably, in step (a), the flash pressure is 0.3-1MPa, and the temperature reached by the temperature reduction is 120-230 ℃.
Preferably, in step (b), the slag wax flows downwards by inertia and gravity, and the rotating direction of the rotating cylinder in the primary magnetic separation device is opposite to the flowing direction of the slag wax.
Preferably, the surface linear velocity of the drum rotation is 0.01 to 1.5 m/s.
Preferably, in step (b), the first heating temperature is 120-230 ℃; the working pressure of the primary magnetic separation device is 0.1-0.8 MPa.
Preferably, in the primary magnetic separation device, the magnetic induction intensity of the primary magnetic separation is 100-15000 gauss.
Preferably, in step (c), the second heating temperature is 120-230 ℃; the working pressure of the secondary magnetic separation device is 0.1-0.8 MPa.
In the secondary magnetic separation device, the magnetic induction intensity of the secondary magnetic separation is 800-25000 gauss.
Through the technical scheme, the system provided by the invention utilizes the two-stage magnetic separation device, wherein the fixed magnet and the rotary drum are particularly arranged, so that the magnet can attract the waste catalyst in the slag wax to be attached to the surface of the rotary drum and remove the slag wax under the protection of heating and inert atmosphere, thereby realizing the separation of the waste catalyst in the Fischer-Tropsch synthesis slag wax. The device is simple and convenient to operate and can continuously run. By utilizing the device, the method for separating the waste catalyst in the Fischer-Tropsch synthesis slag wax can better realize the recovery of the synthesis wax in the Fischer-Tropsch synthesis slag wax.
Drawings
FIG. 1 is a schematic flow diagram of a process for separating spent catalyst from Fischer-Tropsch wax residue provided by the present invention;
FIG. 2 is a schematic cross-sectional view of an apparatus for magnetically separating a spent catalyst from Fischer-Tropsch wax residue provided by the present invention.
Description of the reference numerals
1 bracket 2 case 3 magnet
4 slag wax inlet 5 shell 6 rotary drum
7 shaft 8 waste catalyst outlet 9 scraper
10 outlet for synthetic wax
E2 synthetic wax intermediate tank E3 waste catalyst receiving tank of E1 first-level magnetic separation device
E5 synthetic wax storage tank E6 fine catalyst receiving tank of E4 two-stage magnetic separation device
E7 incinerator
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
In a first aspect, the present invention provides a system for separating a spent catalyst from fischer-tropsch wax residue, as shown in fig. 1 and 2, comprising:
a primary magnetic separation device E1, a synthetic wax intermediate tank E2, a waste catalyst receiving tank E3, a secondary magnetic separation device E4, a synthetic wax storage tank E5, a fine catalyst receiving tank E6 and an incinerator E7; wherein the content of the first and second substances,
the primary magnetic separation device E1 is used for carrying out primary magnetic separation on Fischer-Tropsch synthesis slag wax generated by a Fischer-Tropsch synthesis device, storing the obtained waste catalyst into the waste catalyst receiving tank E3, and storing the obtained synthetic wax liquid into the synthetic wax intermediate tank E2;
the secondary magnetic separation device E4 is used for carrying out secondary magnetic separation on the synthetic wax liquid from the synthetic wax intermediate tank E2, storing the obtained fine catalyst into the fine catalyst receiving tank E6, storing the obtained synthetic wax into the synthetic wax storage tank E5,
the incinerator E7 is used for incineration treatment of the spent catalyst from the spent catalyst receiving tank E3 and the fine catalyst from the fine catalyst receiving tank E6;
wherein, the primary magnetic separation device E1 and the secondary magnetic separation device E4 both comprise the following parts:
a closed box body 2 provided with a wax residue inlet 4, a synthetic wax outlet 10, a waste catalyst outlet 8 and a heating and heat-preserving structure, a rotatable sealed rotary drum 6 arranged in the box body 2, a magnet 3 fixed in the rotary drum 6, and a scraper 9 arranged at the waste catalyst outlet 8 and contacted with the outer surface of the rotary drum 6;
the position of the magnet 3 corresponds to the space between the wax residue inlet 4 and the synthetic wax outlet 10 in the box body 2, and is used for attracting the waste catalyst in the Fischer-Tropsch synthetic wax residue or the fine catalyst in the synthetic wax liquid to be attached to the outer surface of the rotary drum 6; the scraper 9 is used to remove the spent catalyst or fine catalyst on the outer surface of the drum 6.
In the invention, the structures of the primary magnetic separation device E1 and the secondary magnetic separation device E4 can be as shown in FIG. 2, the devices can be horizontally placed, and the whole box body 2 is horizontally placed on the bracket 1. The box 2 may be a horizontally placed long cylinder with the central axis of the cylinder parallel to the ground. The drum 6 is disposed coaxially with the casing 2. The diameter of the drum 6 is smaller than that of the box 2, and preferably, the box 2 is arranged at a distance from the drum 6; in the first-stage magnetic separation device E1, a space for Fischer-Tropsch synthesis wax residue flowing or waste catalyst moving is formed, and the space formed between the rotary drum 6 and the box body 2 can contain the Fischer-Tropsch synthesis wax residue or the waste catalyst; in the secondary magnetic separation device E4, a space for the synthetic wax liquid to flow or for the fine catalyst to move is formed, and a space formed between the drum 6 and the casing 2 can accommodate the synthetic wax liquid to flow or the fine catalyst. In the primary magnetic separation device E1 and the secondary magnetic separation device E4, the magnet 3 is fixedly arranged inside the rotary drum 6 and does not rotate along with the rotary drum 6. There is no contact between the magnet 3 and the drum 6 so that the drum 6 can rotate freely. In the present invention, it is preferable that the drum 6 is disposed at a distance from the magnets 3, and the magnets 3 occupy 1/4-5/6 of the inner circumference of the drum 6. The magnet 3 is arranged to form a magnetic area and a non-magnetic area inside the box body 2. The magnetic area can correspond to the space between the wax residue inlet 4 and the synthetic wax outlet 10, and the Fischer-Tropsch synthetic wax residue passes through the magnetic area in the primary magnetic separation device; in the secondary magnetic separation device, synthetic wax liquid passes through the magnetic area. Attraction of the magnet 3 to the catalyst with magnetic properties can be achieved in the magnetic zone. The rest space in the box body 2 is the nonmagnetic zone and comprises a waste catalyst outlet 8, and the Fischer-Tropsch synthesis slag wax or the synthesis wax liquid does not pass through the nonmagnetic zone. While the Fischer-Tropsch wax is in the magnetized zone, the contained spent catalyst may be attracted to the surface of the rotating drum 6. While the synthetic wax liquid is in the magnetic zone, fine catalyst that may be contained is attracted to the surface of the rotating drum 6. When the drum 6 rotates to a non-magnetic region, the attracted spent catalyst or fine catalyst may fall off. The magnet 3 can be a cylindrical body with the bottom surface and the top surface in the same fan shape, the cylindrical body and the rotary drum 6 are coaxially arranged, the central angle of the fan shape can be 90-300 degrees, and the requirement of providing a magnetic field for attracting the catalyst in the slag wax can be met. The magnet 3 may be a permanent magnet or an electromagnet consisting of a magnetic coil, and may be composed of a plurality of small magnets.
According to the invention, the primary magnetic separation device also comprises a drive device for driving the rotation direction of the rotary drum 6 to be opposite to the flow direction of the Fischer-Tropsch wax residue in the box body 2; the secondary magnetic separation apparatus further comprises drive means for driving the drum 6 to rotate in a direction opposite to the direction of flow of the synthetic wax liquid in the tank 2. Thus, when the rotary drum 6 rotates and passes through the magnetic area, the waste catalyst in the Fischer-Tropsch synthesis slag wax passing through the magnetic area or the fine catalyst in the synthesis wax liquid is attracted in a contact or non-contact mode; the drum 6 then rotates with the spent or fine catalyst into the nonmagnetic zone and does not contact the Fischer-Tropsch wax or synthetic wax liquid, and the spent or fine catalyst can leave the drum 6 in the nonmagnetic zone. The drum 6 from which the spent catalyst or the fine catalyst has been removed can continue to rotate to reenter the magnetic zone, repeating the operation of attracting the spent catalyst or the fine catalyst.
In the invention, preferably, as shown in fig. 2, in the primary magnetic separation device, the fischer-tropsch synthesis wax residue can enter the device from the wax residue inlet 4, and is directly introduced to the surface of the rotary drum 6, and flows into the space between the box body 2 and the rotary drum 6 in a counterclockwise direction under the action of inertia and gravity, and the space through which the magnet 3 flows corresponding to the wax residue is a magnetic area, so as to provide a magnetic field to attract the waste catalyst in the wax residue; the waste catalyst is attached to the surface of the rotary drum 6, and the wax residue after catalyst removal continuously flows into the bottom of the device anticlockwise and is discharged from a synthetic wax outlet 10; the rotary drum 6 with the waste catalyst continuously rotates along the clockwise direction, does not meet with the Fischer-Tropsch synthesis slag wax, and rotates to a non-magnetic area, so that the waste catalyst is not attracted by a magnetic field any more, can be separated from the rotary drum 6 through the scraper 9, and is discharged from the waste catalyst outlet 8. Similarly, in the secondary magnetic separation device, the synthetic wax liquid can enter the device from the wax residue inlet 4 and is directly introduced to the surface of the rotary drum 6, and flows into the space between the box body 2 and the rotary drum 6 in a counterclockwise direction under the action of inertia and gravity, and the space through which the magnet 3 flows corresponding to the synthetic wax liquid is a magnetic area which provides a magnetic field to attract the fine catalyst in the synthetic wax liquid; the fine catalyst is attached to the surface of the rotary drum 6, and the synthetic wax liquid without the catalyst continuously flows into the bottom of the device anticlockwise and is discharged from a synthetic wax outlet 10; the rotary drum 6 with the fine catalyst continuously rotates clockwise without meeting the synthetic wax liquid and then rotates to a non-magnetic area, the fine catalyst is not attracted by a magnetic field any more and can be separated from the rotary drum 6 through the scraper 9 and is discharged out of the device from a waste catalyst outlet 8.
According to the present invention, preferably, the synthetic wax outlet is provided at the bottom of the tank and is opened downward, the wax residue inlet is provided above one side of the tank, and the spent catalyst outlet is provided below a different side of the tank from the wax residue inlet. As shown in fig. 2, the wax residue inlet 4 and the synthetic wax outlet 10 are in the magnetic region, and the spent catalyst outlet 8 is in the non-magnetic region. Preferably, the wax inlet 4 is provided to be upwardly open; the spent catalyst outlet 8 is provided so as to be open downward.
In the invention, the size of the device can be determined according to the treatment requirement of the wax residue, and the treatment capacity of the wax residue can be met. The diameters of the magnet 3, the drum 6 and the case 2 may be increased in this order.
According to the present invention, preferably, sealing structures are respectively provided at the wax residue inlet, the synthetic wax outlet, and the spent catalyst outlet to seal the case. So as to ensure that the waste catalyst is not contacted with air and is dangerous. Meanwhile, the rotary drum 6 is also arranged to seal the magnet 3 inside and is not in direct contact with the Fischer-Tropsch synthesis slag wax, the waste catalyst and the synthetic wax.
With reference to fig. 2, the primary magnetic separation device E1 and the secondary magnetic separation device E4 each include: the device comprises a rotating shaft 7, a magnet 3 (fixed), a rotary drum 6 (rotatable), a box body 2 (a shell 5 is provided with a steam coil pipe or an electric tracing wire with a heat insulation structure), a wax residue feeding hole 4, a scraping plate 9, a synthetic wax outlet 10, a waste catalyst outlet 8 and a support 1. In the first-stage magnetic separation device E1, the Fischer-Tropsch synthesis slag wax flows into the device from the slag wax feed inlet 4, flows to the bottom of the box body 2 anticlockwise under the action of inertia and gravity, passes through a magnetic area with a magnetic field generated by the magnet 3, and is attracted to and attached to the outer surface of the rotary drum 6 by the waste catalyst in the Fischer-Tropsch synthesis slag wax; the rotary drum 6 rotates clockwise under the drive of the motor, the waste catalyst rotates to a non-magnetic area along with the rotary drum 6, and the waste catalyst falls off from the rotary drum 6 under the action of the scraper 9, and then leaves the device from a waste catalyst outlet 8. The Fischer-Tropsch synthesis residue wax flowing to the bottom of the box body 2 is separated to obtain waste catalyst, and synthetic wax liquid containing micro catalyst fine powder flows out of the device from a synthetic wax outlet 10 below the device. In the secondary magnetic separation device E2, synthetic wax liquid flows into the device from the wax residue inlet 4, flows anticlockwise to the bottom of the box body 2 under the action of inertia and gravity, passes through a magnetic area with a magnetic field generated by the magnet 3, and fine catalyst in the synthetic wax liquid is attracted and attached to the outer surface of the rotary drum 6; the rotating drum 6 is driven by the motor to rotate clockwise, the fine catalyst rotates to a non-magnetic area along with the rotating drum 6, and the fine catalyst falls off from the rotating drum 6 under the action of the scraper 9, and then leaves the device from the waste catalyst outlet 8. The fine catalyst is separated from the synthetic wax liquid flowing to the bottom of the box body 2 to obtain qualified synthetic wax, and the qualified synthetic wax flows out of the device from a synthetic wax outlet 10 below the device.
In the present invention, the scraper 9 is preferably disposed perpendicular to the surface of the drum 6. To more effectively remove the spent or fine catalyst from the surface of the drum 6.
In a second aspect, the present invention provides a method for separating a waste catalyst from fischer-tropsch synthesis residue wax, as shown in fig. 1, including:
(a) carrying out flash evaporation and cooling on the Fischer-Tropsch synthesis product to obtain Fischer-Tropsch synthesis residue wax from which synthesis gas and light hydrocarbon are removed;
(b) introducing the wax residue into the system provided by the invention, and carrying out primary magnetic separation in a primary magnetic separation device of the system under the first heating and inert atmosphere to obtain a waste catalyst and a synthetic wax liquid;
(c) and introducing the synthetic wax liquid into a secondary magnetic separation device of the system, and performing secondary magnetic separation under a second heating and inert atmosphere to obtain the synthetic wax and the fine catalyst.
The system provided by the invention is used for separating the catalyst in the Fischer-Tropsch synthesis wax residues. In the method provided by the invention, the Fischer-Tropsch synthesis reaction in the step (a), such as the Fischer-Tropsch synthesis product obtained by a slurry bed reactor, can be purified and then introduced into the system provided by the invention.
In the invention, the Fischer-Tropsch synthesis product can be slurry which is synthesized by synthesis gas in a slurry bed reactor in the presence of a Fischer-Tropsch synthesis catalyst and contains a waste catalyst and synthetic wax. Wherein the solid content of the spent catalyst may be in the range of 10-20% by weight. The step (a) can be carried out in a slag wax flash tank, and the synthesis gas and the low-carbon hydrocarbon dissolved in the slag wax are volatilized and removed through pressure reduction. Preferably, the flash pressure is from 0.3 to 1 MPa. Meanwhile, the temperature of the wax slag can be reduced, and the temperature reached by the temperature reduction can be 120-230 ℃, and is preferably 150-200 ℃.
According to the present invention, in step (b), the catalyst may be magnetically separated from the wax residue in a magnetic separation device provided by the present invention as shown in fig. 2 under a certain temperature and inert atmosphere. Preferably, in step (b), the slag wax flows downwards by inertia and gravity, and the rotating direction of the rotating cylinder in the primary magnetic separation device is opposite to the flowing direction of the slag wax. Preferably, the surface linear velocity of rotation of the drum is from 0.01 to 1.5m/s, more preferably from 0.03 to 0.8 m/s. And sufficient meeting time between the rotary drum 6 and the wax residue is ensured, and the effect of separating the waste catalyst is ensured.
According to the invention, in the magnetic separation catalyst device, the heating and heat-insulating structure can provide temperature to ensure that the wax slag is in a flowing state. Preferably, in step (b), the first heating temperature is 120-. The heating mode can be that the heat preservation structure outside the box body of the magnetic separation device provided by the invention uses steam or electric tracing, preferably uses steam for tracing. The inert atmosphere can be nitrogen to ensure the safety of the magnetic separation process and prevent the catalyst carried by the wax residue from being oxidized. The inert atmosphere is introduced to ensure that the working pressure of the device is 0.1-0.8MPa, preferably 0.1-0.3 MPa.
According to the invention, the magnets can be selected from permanent magnets and/or electromagnetic magnets, preferably permanent magnets. Preferably, in the primary magnetic separation device, the magnetic induction intensity of the primary magnetic separation is 100-15000 gauss, preferably 300-5000 gauss, and more preferably 500-2000 gauss. In the present invention, the magnetic induction of the primary magnetic separation means the magnetic induction of the magnetic field formed on the surface of the drum 2 by the magnet 3 in the primary magnetic separation device.
According to the present invention, preferably, in step (c), the second heating temperature is 120-; the working pressure of the secondary magnetic separation device is 0.1-0.8MPa, and preferably 0.1-0.3 MPa. In order to remove the fine catalyst better, preferably, in the secondary magnetic separation device, the magnetic induction intensity of the secondary magnetic separation is 800-25000 gauss, preferably 1800-15000 gauss, and more preferably 2500-10000 gauss. In the present invention, the magnetic induction of the secondary magnetic separation means the magnetic induction of the magnetic field formed on the surface of the drum 2 by the magnet 3 in the secondary magnetic separation apparatus.
With reference to FIG. 1, the synthesis gas undergoes Fischer-Tropsch synthesis in a slurry bed Fischer-Tropsch synthesis reactor. When the catalyst is replaced, discharging a product (slurry (slag wax) containing the waste catalyst and the synthetic wax) in a slurry bed Fischer-Tropsch synthesis reactor (with the pressure of 2-3MPa) into a slag wax flash tank with a stirrer, wherein the pressure of the slag wax flash tank is 0.3-1MPa, the pressure is reduced, the synthetic gas and the low-carbon hydrocarbons dissolved in the slag wax are volatilized out, and the cooled Fischer-Tropsch synthetic slag wax is obtained at the outlet of a slag wax flash tank E2; introducing the residue wax into a first-stage magnetic separation device E1 to realize the primary separation of the waste catalyst and the synthetic wax, introducing the separated synthetic wax liquid containing a small amount of fine catalyst particles into a synthetic wax intermediate tank E2, and introducing the separated waste catalyst into a waste catalyst receiving tank E3; sending the synthetic wax liquid in the synthetic wax intermediate tank E2 into a secondary magnetic separation device E4 to further separate catalyst fine powder, sending the obtained synthetic wax into a synthetic wax storage tank E5, and unloading the obtained fine catalyst into a fine catalyst receiving tank E6; the spent catalyst and fine catalyst may finally be sent to an incinerator E7 for incineration disposal.
The pressure in the invention is absolute pressure.
The present invention will be described in detail below by way of examples.
Example 1
The synthesis gas uses an iron-based catalyst to carry out Fischer-Tropsch synthesis reaction in a slurry bed Fischer-Tropsch synthesis reactor (the pressure is 3.0MPa and the temperature is 260 ℃), the obtained slurry containing the catalyst and heavy wax is discharged into a slag wax flash tank with a stirrer, and the pressure of the slag wax flash tank is 0.5 MPa. And (4) volatilizing the synthesis gas and the low-carbon hydrocarbons dissolved in the slurry due to the reduction of the pressure to obtain the Fischer-Tropsch synthesis slag wax. The temperature of the slag wax flash tank is 200 ℃, and the mass fraction of the waste catalyst in the slag wax is 15%.
The slag wax is introduced into the feed inlet of a first-stage magnetic separator E1, and the feeding amount is 300 kg/h. In the primary magnetic separator E1, the diameter of the drum 6 is 600mm, and the length is 800 mm; the magnet is a permanent magnet and a fan-shaped cylindrical body, the central angle of the fan shape is 300 degrees, and the box body 3, the rotary drum 6 and the magnet 3 are coaxially arranged. The magnetic field generated by the magnet 3 causes the magnetic induction intensity of the surface of the rotating drum 6 to be 500 gauss when the rotating drum 6 has the magnetic area.
The surface linear velocity of the drum 6 was 0.03 m/s. The Fischer-Tropsch synthesis slag wax flows anticlockwise on the inner wall of the box body 3, and the rotary drum 6 rotates clockwise; the shell of the first-stage magnetic separator E1 is heated by steam, the temperature in the magnetic separator is 180 ℃, and the pressure of the magnetic separator is 0.1 MPa. After passing through a first-stage magnetic separator E1, synthetic wax liquid with the solid content of the waste catalyst of 300 mug/g is obtained at a synthetic wax outlet 10, and the waste catalyst with the solid content of 60 weight percent is obtained at a waste catalyst outlet 8.
The synthetic wax liquid separated by the first-stage magnetic separator E1 is sent to the second-stage magnetic separator E4. In the secondary magnetic separator E4, the diameter of the drum 6 is 600mm, and the length is 800 mm; the magnets are electromagnets arranged in a sector with a central angle of 200 deg., the box 3, the drum 6 and the magnets 3 being arranged coaxially. The magnetic field generated by the magnet 3 makes the magnetic induction intensity of the surface of the rotating drum 6 10000 gauss when the rotating drum 6 has a magnetic area.
The surface linear velocity of the drum 6 was 0.05 m/s. The synthetic wax liquid flows on the inner wall of the box body 3 anticlockwise, and the rotary drum 6 rotates clockwise; the shell of the secondary magnetic separator E4 is heated by steam, the temperature in the magnetic separator is 180 ℃, and the pressure of the magnetic separator is 0.1 MPa. After passing through a secondary magnetic separator E1, synthetic wax with the solid content of the waste catalyst lower than 20 mug/g is obtained at a synthetic wax outlet 10, and fine catalyst with the solid content of 62 weight percent is obtained at a waste catalyst outlet 8.
And (3) delivering the waste catalyst and the fine catalyst separated by the first-stage magnetic separator and the second-stage magnetic separator into an incinerator, and incinerating for 4 hours at 1000 ℃, wherein organic matters are not detected in the solid waste.
Example 2
The synthesis gas uses an iron-based catalyst to carry out Fischer-Tropsch synthesis reaction in a slurry bed Fischer-Tropsch synthesis reactor (the pressure is 2.0MPa and the temperature is 270 ℃), the obtained slurry containing the catalyst and heavy wax is discharged into a slag wax flash tank with a stirrer, and the pressure of the slag wax flash tank is 0.3 MPa. And (4) volatilizing the synthesis gas and the low-carbon hydrocarbons dissolved in the slurry due to the reduction of the pressure to obtain the Fischer-Tropsch synthesis slag wax. The temperature of the slag wax flash tank is 180 ℃, and the mass fraction of the waste catalyst in the slag wax is 20%.
The slag wax is introduced into the feed inlet of a first-stage magnetic separator E1, and the feeding amount is 400 kg/h. In the primary magnetic separator E1, the diameter of the drum 6 is 600mm, and the length is 800 mm; the magnet is a permanent magnet and a fan-shaped cylindrical body, the central angle of the fan shape is 90 degrees, and the box body 3, the rotary drum 6 and the magnet 3 are coaxially arranged. The magnetic field generated by the magnet 3 causes the magnetic induction intensity of the surface of the rotating drum 6 to be 2000 gauss when the rotating drum 6 has the magnetic area.
The surface linear velocity of the drum 6 was 0.10 m/s. The Fischer-Tropsch synthesis slag wax flows anticlockwise on the inner wall of the box body 3, and the rotary drum 6 rotates clockwise; the shell of the first-stage magnetic separator E1 is heated by steam, the temperature in the magnetic separator is 150 ℃, and the pressure of the magnetic separator is 0.2 MPa. After passing through a first-stage magnetic separator E1, synthetic wax liquid with the solid content of the waste catalyst of 180 mug/g is obtained at a synthetic wax outlet 10, and the waste catalyst with the solid content of 62 weight percent is obtained at a waste catalyst outlet 8.
The synthetic wax liquid separated by the first-stage magnetic separator E1 is sent to the second-stage magnetic separator E4. In the secondary magnetic separator E4, the diameter of the rotating drum 6 is 600mm, and the length is 800 mm; the magnet is a permanent magnet and a fan-shaped cylindrical body, the central angle of the fan shape is 300 degrees, and the box body 3, the rotary drum 6 and the magnet 3 are coaxially arranged. The magnetic field generated by the magnet 3 makes the magnetic induction intensity of the surface of the rotating drum 6 be 2500 gauss when the rotating drum 6 has a magnetic area.
The surface linear velocity of the drum 6 was 0.05 m/s. The synthetic wax liquid flows on the inner wall of the box body 3 anticlockwise, and the rotary drum 6 rotates clockwise; the shell of the secondary magnetic separator E4 is heated by steam, the temperature in the magnetic separator is 150 ℃, and the pressure of the magnetic separator is 0.2 MPa. After passing through a secondary magnetic separator E1, synthetic wax with the solid content of the waste catalyst of 50 mug/g is obtained at a synthetic wax outlet 10, and fine catalyst with the solid content of 60 weight percent is obtained at a waste catalyst outlet 8.
And (3) delivering the waste catalyst and the fine catalyst separated by the first-stage magnetic separator and the second-stage magnetic separator into an incinerator, and incinerating for 4 hours at 1000 ℃, wherein organic matters are not detected in the solid waste.
Example 3
The synthesis gas uses an iron-based catalyst to carry out Fischer-Tropsch synthesis reaction in a slurry bed Fischer-Tropsch synthesis reactor (the pressure is 2.4MPa and the temperature is 300 ℃), the obtained slurry containing the catalyst and heavy wax is discharged into a slag wax flash tank with a stirrer, and the pressure of the slag wax flash tank is 1.0 MPa. And (4) volatilizing the synthesis gas and the low-carbon hydrocarbons dissolved in the slurry due to the reduction of the pressure to obtain the Fischer-Tropsch synthesis slag wax. The temperature of the slag wax flash tank is 150 ℃, and the mass fraction of the waste catalyst in the slag wax is 10%.
The slag wax is introduced into the feed inlet of a first-stage magnetic separator E1, and the feeding amount is 500 kg/h. In the primary magnetic separator E1, the diameter of the drum 6 is 600mm, and the length is 800 mm; the magnet is a permanent magnet and a fan-shaped cylindrical body, the central angle of the fan shape is 200 degrees, and the box body 3, the rotary drum 6 and the magnet 3 are coaxially arranged. The magnetic field generated by the magnet 3 makes the magnetic induction intensity of the surface of the rotary drum 6 be 1500 gauss when the rotary drum 6 has the magnetic area.
The surface linear velocity of the drum 6 was 0.20 m/s. The Fischer-Tropsch synthesis slag wax flows anticlockwise on the inner wall of the box body 3, and the rotary drum 6 rotates clockwise; the shell of the first-stage magnetic separator E1 is heated by steam, the temperature in the magnetic separator is 150 ℃, and the pressure of the magnetic separator is 0.3 MPa. After passing through a first-stage magnetic separator E1, synthetic wax liquid with the solid content of the waste catalyst of 200 mug/g is obtained at a synthetic wax outlet 10, and the waste catalyst with the solid content of 59 weight percent is obtained at a waste catalyst outlet 8.
The synthetic wax liquid separated by the first-stage magnetic separator E1 is sent to the second-stage magnetic separator E4. In the secondary magnetic separator E4, the diameter of the drum 6 is 600mm, and the length is 800 mm; the magnets are electromagnets arranged in a sector shape with a central angle of 90 DEG, and the box 3, the drum 6 and the magnets 3 are coaxially arranged. The magnetic field generated by the magnet 3 causes the magnetic induction intensity of the surface of the rotating drum 6 to be 6000 gauss when the rotating drum 6 has a magnetic area.
The surface linear velocity of the drum 6 was 0.1 m/s. The synthetic wax liquid flows on the inner wall of the box body 3 anticlockwise, and the rotary drum 6 rotates clockwise; the shell of the secondary magnetic separator E4 is heated by steam, the temperature in the magnetic separator is 200 ℃, and the pressure of the magnetic separator is 0.3 MPa. After passing through a secondary magnetic separator E1, synthetic wax with the solid content of the waste catalyst of 40 mug/g is obtained at a synthetic wax outlet 10, and fine catalyst with the solid content of 59 weight percent is obtained at a waste catalyst outlet 8.
And (3) delivering the waste catalyst and the fine catalyst separated by the first-stage magnetic separator and the second-stage magnetic separator into an incinerator, and incinerating for 4 hours at 1000 ℃, wherein organic matters are not detected in the solid waste.
Example 4
The synthesis gas uses an iron-based catalyst to carry out Fischer-Tropsch synthesis reaction in a slurry bed Fischer-Tropsch synthesis reactor (the pressure is 3.0MPa and the temperature is 260 ℃), the obtained slurry containing the catalyst and heavy wax is discharged into a slag wax flash tank with a stirrer, and the pressure of the slag wax flash tank is 0.5 MPa. And (4) volatilizing the synthesis gas and the low-carbon hydrocarbons dissolved in the slurry due to the reduction of the pressure to obtain the Fischer-Tropsch synthesis slag wax. The temperature of the slag wax flash tank is 200 ℃, and the mass fraction of the waste catalyst in the slag wax is 17%.
The slag wax is introduced into the feed inlet of a first-stage magnetic separator E1, and the feeding amount is 300 kg/h. In the primary magnetic separator E1, the diameter of the drum 6 is 600mm, and the length is 800 mm; the magnets are electromagnets arranged in a sector with a central angle of 220 deg., the box 3, the drum 6 and the magnets 3 being arranged coaxially. The magnetic field generated by the magnet 3 makes the magnetic induction intensity of the surface of the rotating drum 6 be 15000 gauss when the rotating drum 6 has a magnetic area.
The surface linear velocity of the drum 6 was 0.15 m/s. The Fischer-Tropsch synthesis slag wax flows anticlockwise on the inner wall of the box body 3, and the rotary drum 6 rotates clockwise; the shell of the first-stage magnetic separator E1 is heated by steam, the temperature in the magnetic separator is 180 ℃, and the pressure of the magnetic separator is 0.1 MPa. After passing through a first-stage magnetic separator E1, synthetic wax liquid with solid content of 120 mug/g of waste catalyst is obtained at a synthetic wax outlet 10, and waste catalyst with solid content of 63 wt% is obtained at a waste catalyst outlet 8.
The synthetic wax liquid separated by the first-stage magnetic separator E1 is sent to the second-stage magnetic separator E4. In the secondary magnetic separator E4, the diameter of the drum 6 is 600mm, and the length is 800 mm; the magnet is a permanent magnet and a fan-shaped cylindrical body, the central angle of the fan shape is 220 degrees, and the box body 3, the rotary drum 6 and the magnet 3 are coaxially arranged. The magnetic field generated by the magnet 3 makes the magnetic induction intensity of the surface of the rotating drum 6 be 1800 gauss when the rotating drum 6 has a magnetic area.
The surface linear velocity of the drum 6 was 0.05 m/s. The synthetic wax liquid flows on the inner wall of the box body 3 anticlockwise, and the rotary drum 6 rotates clockwise; the shell of the secondary magnetic separator E4 is heated by steam, the temperature in the magnetic separator is 180 ℃, and the pressure of the magnetic separator is 0.1 MPa. After passing through a secondary magnetic separator E1, synthetic wax with solid content of 60 mug/g of waste catalyst is obtained at a synthetic wax outlet 10, and fine catalyst with solid content of 57 wt% is obtained at a waste catalyst outlet 8.
And (3) delivering the waste catalyst and the fine catalyst separated by the first-stage magnetic separator and the second-stage magnetic separator into an incinerator, and incinerating for 4 hours at 1000 ℃, wherein organic matters are not detected in the solid waste.
Example 5
The synthesis gas uses an iron-based catalyst to carry out Fischer-Tropsch synthesis reaction in a slurry bed Fischer-Tropsch synthesis reactor (the pressure is 2.0MPa and the temperature is 270 ℃), the obtained slurry containing the catalyst and heavy wax is discharged into a slag wax flash tank with a stirrer, and the pressure of the slag wax flash tank is 0.3 MPa. And (4) volatilizing the synthesis gas and the low-carbon hydrocarbons dissolved in the slurry due to the reduction of the pressure to obtain the Fischer-Tropsch synthesis slag wax. The temperature of the slag wax flash tank is 180 ℃, and the mass fraction of the waste catalyst in the slag wax is 18%.
The slag wax is introduced into the feed inlet of a first-stage magnetic separator E1, and the feeding amount is 300 kg/h. In the primary magnetic separator E1, the diameter of the drum 6 is 600mm, and the length is 800 mm; the magnet is a permanent magnet and a fan-shaped cylindrical body, the central angle of the fan shape is 300 degrees, and the box body 3, the rotary drum 6 and the magnet 3 are coaxially arranged. The magnetic field generated by the magnet 3 makes the magnetic induction intensity of the surface of the rotating drum 6 be 100 gauss when the rotating drum 6 has a magnetic area.
The surface linear velocity of the drum 6 was 0.03 m/s. The Fischer-Tropsch synthesis slag wax flows anticlockwise on the inner wall of the box body 3, and the rotary drum 6 rotates clockwise; the shell of the first-stage magnetic separator E1 is heated by steam, the temperature in the magnetic separator is 180 ℃, and the pressure of the magnetic separator is 0.1 MPa. After passing through a first-stage magnetic separator E1, synthetic wax liquid with the solid content of the waste catalyst of 400 mug/g is obtained at a synthetic wax outlet 10, and the waste catalyst with the solid content of 55 weight percent is obtained at a waste catalyst outlet 8.
The synthetic wax liquid separated by the first-stage magnetic separator E1 is sent to the second-stage magnetic separator E4. In the secondary magnetic separator E4, the diameter of the drum 6 is 600mm, and the length is 800 mm; the magnets are electromagnets arranged in a sector with a central angle of 200 deg., the box 3, the drum 6 and the magnets 3 being arranged coaxially. The magnetic field generated by the magnet 3 causes the magnetic induction intensity of the surface of the rotating drum 6 to be 25000 gauss when the rotating drum 6 has the magnetic area.
The surface linear velocity of the drum 6 was 0.05 m/s. The synthetic wax liquid flows on the inner wall of the box body 3 anticlockwise, and the rotary drum 6 rotates clockwise; the shell of the secondary magnetic separator E4 is heated by steam, the temperature in the magnetic separator is 180 ℃, and the pressure of the magnetic separator is 0.1 MPa. After passing through a secondary magnetic separator E1, synthetic wax with a solid content of 20 mug/g of waste catalyst is obtained at a synthetic wax outlet 10, and fine catalyst with a solid content of 63 wt% is obtained at a waste catalyst outlet 8.
And (3) delivering the waste catalyst and the fine catalyst separated by the first-stage magnetic separator and the second-stage magnetic separator into an incinerator, and incinerating for 4 hours at 1000 ℃, wherein organic matters are not detected in the solid waste.
The embodiment of the device and the method provided by the invention has a better effect of separating the waste catalyst in the wax residue, can separate the waste catalyst with high solid content and the fine catalyst after the wax residue with the waste catalyst content of 10-20 wt% is subjected to secondary magnetic separation, and can obtain qualified synthetic wax products, wherein the solid content of the waste catalyst is below 60 mug/g. The device provided by the invention can realize the accumulated recovery of the synthetic wax product from the wax residue by continuous long-period operation, and the recovery rate of the synthetic wax product can reach more than 70 percent.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.

Claims (10)

1. A system for separating spent catalyst from Fischer-Tropsch synthesis wax residue, comprising:
the device comprises a primary magnetic separation device, a synthetic wax intermediate tank, a waste catalyst receiving tank, a secondary magnetic separation device, a synthetic wax storage tank, a fine catalyst receiving tank and an incinerator; wherein the content of the first and second substances,
the primary magnetic separation device is used for performing primary magnetic separation on Fischer-Tropsch synthesis slag wax generated by the Fischer-Tropsch synthesis device, storing the obtained waste catalyst into the waste catalyst receiving tank, and storing the obtained synthetic wax liquid into the synthetic wax intermediate tank;
the secondary magnetic separation device is used for carrying out secondary magnetic separation on the synthetic wax liquid from the synthetic wax intermediate tank, storing the obtained fine catalyst into the fine catalyst receiving tank, storing the obtained synthetic wax into the synthetic wax storage tank,
the incinerator is used for incinerating the waste catalyst from the waste catalyst receiving tank and the fine catalyst from the fine catalyst receiving tank;
wherein, the first-stage magnetic separation device and the second-stage magnetic separation device both comprise the following parts:
the device comprises a closed box body, a rotary sealing rotary drum, a magnet and a scraper blade, wherein the closed box body is provided with a wax residue inlet, a synthetic wax outlet, a waste catalyst outlet and a heating and heat-insulating structure;
the position of the magnet corresponds to the space between the wax residue inlet and the synthetic wax outlet in the box body, and the magnet is used for attracting the waste catalyst in the Fischer-Tropsch synthetic wax residue or the fine catalyst in the synthetic wax liquid to be attached to the outer surface of the rotary drum; the scraper is used to remove spent or fine catalyst on the outer surface of the drum.
2. The system of claim 1, wherein the first and second magnetic separation devices are arranged with the box spaced from the drum to define a space for the flow of the fischer-tropsch wax, the movement of the spent catalyst, the flow of the synthetic wax liquid, or the movement of the fine catalyst;
preferably, the drum is spaced from the magnets, which occupy 1/4-5/6 of the inner circumference of the drum.
3. The system of claim 1 or claim 2, wherein the primary magnetic separation device further comprises a drive means for driving the drum to rotate in a direction opposite to the direction of flow of the fischer-tropsch wax in the tank; the secondary magnetic separation device also comprises a driving device for driving the rotating drum to rotate in a direction opposite to the flowing direction of the synthetic wax liquid in the box body.
4. The system of claim 1, wherein in the primary and secondary magnetic separation devices, the synthetic wax outlet is disposed at a bottom of the tank and is open downward, the wax residue inlet is disposed above one side of the tank, and the spent catalyst outlet is disposed below a different side of the tank than the wax residue inlet.
5. The system according to any one of claims 1 to 4, wherein in the primary and secondary magnetic separation devices, sealing structures are provided at the wax residue inlet, the synthetic wax outlet and the spent catalyst outlet, respectively, to seal the case.
6. A method for separating a waste catalyst in Fischer-Tropsch synthesis residue wax comprises the following steps:
(a) carrying out flash evaporation and cooling on the Fischer-Tropsch synthesis product to obtain Fischer-Tropsch synthesis residue wax from which synthesis gas and light hydrocarbon are removed;
(b) introducing the wax residue into the system of any one of claims 1 to 5, and performing primary magnetic separation in a primary magnetic separation device of the system under a first heating and inert atmosphere to obtain a waste catalyst and a synthetic wax liquid;
(c) and introducing the synthetic wax liquid into a secondary magnetic separation device of the system, and performing secondary magnetic separation under a second heating and inert atmosphere to obtain the synthetic wax and the fine catalyst.
7. The process as claimed in claim 6, wherein in step (a), the flash pressure is 0.3-1MPa, and the temperature is reduced to 120-230 ℃, preferably 150-200 ℃.
8. The method according to claim 6, wherein in step (b), the slag wax flows downward by inertia and gravity, and the rotating direction of the rotating cylinder in the primary magnetic separation device is opposite to the flowing direction of the slag wax;
preferably, the surface linear velocity of rotation of the drum is from 0.01 to 1.5m/s, more preferably from 0.03 to 0.8 m/s.
9. The method as claimed in claim 6, wherein, in the step (b), the first heating temperature is 120-; the working pressure of the primary magnetic separation device is 0.1-0.8MPa, preferably 0.1-0.3 MPa;
preferably, in the primary magnetic separation device, the magnetic induction intensity of the primary magnetic separation is 100-15000 gauss, preferably 300-5000 gauss, and more preferably 500-2000 gauss.
10. The method as claimed in claim 6, wherein, in step (c), the second heating temperature is 120-230 ℃, preferably 150-200 ℃; the working pressure of the secondary magnetic separation device is 0.1-0.8MPa, preferably 0.1-0.3 MPa;
preferably, in the secondary magnetic separation device, the magnetic induction intensity of the secondary magnetic separation is 800-25000 gauss, preferably 1800-15000 gauss, and more preferably 2500-10000 gauss.
CN201811362313.6A 2018-11-15 2018-11-15 System and method for separating waste catalyst in Fischer-Tropsch synthesis slag wax Pending CN111187637A (en)

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