CN116059923B - Coke burning reactor and method for propane dehydrogenation spent agent, regenerator and regeneration method for propane dehydrogenation spent agent - Google Patents

Coke burning reactor and method for propane dehydrogenation spent agent, regenerator and regeneration method for propane dehydrogenation spent agent Download PDF

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Publication number
CN116059923B
CN116059923B CN202111269491.6A CN202111269491A CN116059923B CN 116059923 B CN116059923 B CN 116059923B CN 202111269491 A CN202111269491 A CN 202111269491A CN 116059923 B CN116059923 B CN 116059923B
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gas
char
catalyst bed
regenerant
burning
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CN116059923A (en
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方大伟
刘昌呈
王春明
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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Sinopec Research Institute of Petroleum Processing
China Petroleum and Chemical Corp
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/0242—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds the fluid flow within the bed being predominantly vertical
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/02—Heat treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J38/00—Regeneration or reactivation of catalysts, in general
    • B01J38/04—Gas or vapour treating; Treating by using liquids vaporisable upon contacting spent catalyst
    • B01J38/12—Treating with free oxygen-containing gas
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C5/00—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms
    • C07C5/32—Preparation of hydrocarbons from hydrocarbons containing the same number of carbon atoms by dehydrogenation with formation of free hydrogen
    • C07C5/321—Catalytic processes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/584—Recycling of catalysts

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Fluid Mechanics (AREA)
  • Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)

Abstract

The invention relates to the technical field of regeneration of a propane dehydrogenation spent agent, in particular to a scorching reactor and a scorching method for the propane dehydrogenation spent agent, and a regenerator and a regenerating method for the propane dehydrogenation spent agent. The coke burning reactor provided by the invention comprises an upper burning zone and a lower burning zone which are communicated up and down, and the lower burning zone comprises at least two lower burning gas inlets and a radial thickness change rule of a catalyst bed, so that the lower burning gas radially flows through the catalyst bed, the carbon deposit content in the primary coke burning spent agent can be rapidly removed, the temperature of the catalyst bed is prevented from flying, and the catalyst and the internal components of the coke burning reactor are prevented from being destroyed due to flying temperature. Meanwhile, the method for burning the propane dehydrogenation spent catalyst is carried out in the burning reactor, so that the carbon deposit amount of the primary burnt spent catalyst can be further removed, and the catalyst sintering phase change caused by the over-temperature of the catalyst bed is effectively avoided.

Description

Coke burning reactor and method for propane dehydrogenation spent agent, regenerator and regeneration method for propane dehydrogenation spent agent
Technical Field
The invention relates to the technical field of regeneration of a propane dehydrogenation spent agent, in particular to a scorching reactor and a scorching method for the propane dehydrogenation spent agent, and a regenerator and a regenerating method for the propane dehydrogenation spent agent.
Background
If abnormal production operation, fluctuation of raw materials or exceeding of impurity content occurs in the propane dehydrogenation device, carbon deposit of the catalyst can be rapidly increased to form core coke (carbon deposit amount in the catalyst is more than 5 wt%). In the cyclic regeneration process of the catalyst, the high-carbon catalyst is gradually brought to a regenerator, the existence of high carbon content on the catalyst can cause the overtemperature of a regenerated coke-burning bed, the catalyst carrier is sintered into inactive alpha-Al 2O3 balls, and the regeneration equipment can be damaged by the high temperature of the local coke-burning bed. The carbon deposition on the catalyst metal center is generally divided into reversible carbon and irreversible carbon, the reversible carbon can further react on the metal center to form irreversible carbon or graphitic carbon, and graphitic carbon, although it can also be hydro-gasified, reacts very slowly. The core coke on the catalyst is generally considered to be graphitic carbon and is not readily combustible.
When the industrial propane dehydrogenation regeneration device is burnt, graphite carbon of catalyst core coke is difficult to ignite, so that amorphous carbon easy to burn is continuously generated on the surface of the catalyst by a continuous catalyst circulation method, the temperature is increased by the combustion of amorphous carbon to ignite graphite carbon deposit, but the temperature of a burning bed layer is controlled very carefully, the temperature of the bed layer is avoided from flying due to the mass combustion of graphite carbon, high-content carbon residue on dead zone catalysts can be completely burnt through multiple circulation, the activity of normal catalysts cannot be effectively recovered due to the long-time burning in a black burning state, and the economic benefit of the device is correspondingly reduced.
Thus, there is a need for a char reactor for propane dehydrogenation spent.
Disclosure of Invention
The invention aims to solve the problems that carbon deposit in a propane dehydrogenation spent agent is difficult to remove rapidly when a conventional propane dehydrogenation regeneration device is burnt, a catalyst bed is damaged due to temperature runaway, and the like, and provides a novel burnt reactor and a burnt method for the propane dehydrogenation spent agent, a regenerator for the propane dehydrogenation spent agent and a regeneration method.
In order to achieve the above object, a first aspect of the present invention provides a char reactor for dehydrogenation of propane to-be-produced agent, the char reactor comprising an upper combustion zone and a lower combustion zone which are communicated up and down; wherein the lower combustion zone comprises a housing provided with a lower gas outlet tube; the inside of the shell is provided with a catalyst bed which is annularly arranged around the central axis of the shell, the catalyst bed is filled with a primary burning regenerant, and the inside of the shell is divided into a gas feeding area and a gas discharging area;
wherein the side wall of the housing is provided with at least two lower char gas inlets for introducing lower char gas into the gas feed zone;
Wherein, from top to bottom, the radial thickness of the catalyst bed is sequentially reduced;
The gas feeding zone is used for enabling the lower burnt gas to flow radially through the catalyst bed, contact with the primary burnt regenerant and re-burn, and the obtained gas product is discharged through the lower gas outlet pipe after being collected in the gas discharging zone.
In a second aspect, the present invention provides a method for burning propane dehydrogenation spent agent, which is carried out in a burning reactor provided in the first aspect, wherein the method comprises the following steps:
(1) Contacting a propane dehydrogenation spent catalyst with upper burnt gas in an upper combustion zone and performing primary burning to obtain a primary burnt regenerant which flows downwards into a catalyst bed in a lower combustion zone;
(2) The lower burnt gas enters the gas feeding area through at least two lower burnt gas inlets, flows radially through the catalyst bed, contacts with the primary burnt regenerant and is subjected to re-burning to obtain a gas product and the burnt regenerant; wherein the gas products are collected in a gas discharging area and discharged through a gas outlet pipe.
In a third aspect, the present invention provides a regenerator for a propane dehydrogenation spent agent, the regenerator being divided from top to bottom into a coke burning zone, a cooling zone, an oxychlorination zone and a drying zone;
wherein the scorch zone is a scorch reactor provided in the first aspect.
In a fourth aspect, the present invention provides a process for regenerating a propane dehydrogenation spent agent, the process being carried out in a regenerator provided in the third aspect, the process comprising: and (3) sequentially carrying out scorching treatment, cooling treatment, oxychlorination treatment and drying treatment on the propane dehydrogenation spent catalyst to obtain the propane dehydrogenation regenerant.
Compared with the prior art, the invention has the following advantages:
(1) The coke burning reactor provided by the invention comprises an upper burning zone and a lower burning zone which are communicated up and down, and the lower burning zone comprises at least two lower burning gas inlets and a radial thickness change rule of a catalyst bed, so that the lower burning gas radially flows through the catalyst bed, the carbon deposit content in the primary coke burning spent agent can be rapidly removed, the temperature of the catalyst bed is prevented from flying, and the catalyst and the internal components of the coke burning reactor are prevented from being destroyed due to flying temperature;
(2) The method for burning the propane dehydrogenation spent catalyst is carried out in the burning reactor, particularly, the carbon deposit amount of the propane dehydrogenation spent catalyst is regulated and controlled according to the carbon deposit amount of the propane dehydrogenation spent catalyst or the temperature rise of a bed layer caused by the primary burning regenerant entering a catalyst bed, the oxygen content in the lower burning gas passing through the lower burning gas inlet can be further removed, and the catalyst sintering phase change caused by the overtemperature of the catalyst bed is effectively avoided.
Drawings
FIG. 1 is a schematic diagram of the lower combustion zone of a char reactor for the dehydrogenation of propane to-be-produced agent provided by the present invention;
fig. 2 is a schematic diagram of the lower combustion zone of a prior art propane dehydrogenation unit regenerator.
Description of the reference numerals
1. A lower gas outlet pipe 2, a catalyst bed 3, and a gas feed zone
4. Gas discharging area 5, lower part burnt gas inlet 6 and discharging port
7. Outer side surface 8, inner side surface 9 and upper plate surface
10. Lower plate 11, oxygen analyzer 12 and air injection line
13. Gas distribution plate
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In the present invention, unless specified otherwise, the "top" of the container refers to the 0-10% position of the container from top to bottom; the "upper portion" of the container refers to the 10-40% position from top to bottom of the container; the "middle" of the container refers to the 40-60% position from top to bottom of the container; the "lower portion" of the container refers to the 60-90% position from top to bottom of the container; the "bottom" of the container refers to the 90-100% position of the container from top to bottom.
The first aspect of the invention provides a scorch reactor for dehydrogenating a spent propane, which comprises an upper combustion zone and a lower combustion zone which are communicated up and down; wherein the lower combustion zone comprises a housing provided with a lower gas outlet tube; the inside of the shell is provided with a catalyst bed which is annularly arranged around the central axis of the shell, the catalyst bed is filled with a primary burning regenerant, and the inside of the shell is divided into a gas feeding area and a gas discharging area;
wherein the side wall of the housing is provided with at least two lower char gas inlets for introducing lower char gas into the gas feed zone;
Wherein, from top to bottom, the radial thickness of the catalyst bed is sequentially reduced;
The gas feeding zone is used for enabling the lower burnt gas to flow radially through the catalyst bed, contact with the primary burnt regenerant and re-burn, and the obtained gas product is discharged through the lower gas outlet pipe after being collected in the gas discharging zone.
In the present invention, unless otherwise specified, the spent catalyst means a carbonaceous catalyst waiting for burning, and the regenerated catalyst means a non-carbonaceous catalyst after burning regeneration.
In the present invention, the radial thickness of the catalyst bed refers to the difference between the major radius and the minor radius of the catalyst bed on the same horizontal plane, i.e., the difference between the outer radius of the catalyst bed and the inner radius of the catalyst bed on the same horizontal plane, unless otherwise specified.
In the present invention, the kind of the propane dehydrogenation spent catalyst is not limited, and includes, but is not limited to, propane dehydrogenation spent catalyst conventional in the art.
In the present invention, unless otherwise specified, the fact that the char reactor comprises an upper combustion zone and a lower combustion zone which are communicated up and down means that the char reactor comprises an upper combustion zone and a lower combustion zone, the upper combustion zone is disposed above the lower combustion zone, and the upper combustion zone and the lower combustion zone are communicated.
According to the present invention, preferably, the upper combustion zone is used for contacting propane dehydrogenation spent agent with upper coking gas and performing primary coking to obtain the primary coking regenerant. In the present invention, the primary burn is intended to remove easily removed char from the propane dehydrogenation spent catalyst.
According to the present invention, preferably, the lower combustion zone is configured to contact and re-burn the primary-burning regenerant and lower burning gas to obtain the burnt regenerant. In the present invention, the re-scorch is intended to remove hard-to-remove carbon deposits, such as core coke, etc., in the as-burned regenerant.
According to the present invention, preferably, the char reactor further comprises a feed inlet and a discharge outlet; further preferably, the feed inlet is disposed at the top of the upper combustion zone, and the discharge outlet is disposed at the bottom of the lower combustion zone. In the present invention, the feed inlet is used for introducing the propane dehydrogenation spent agent into the char reactor; the discharge port is used for leading the burning regenerant out of the burning reactor.
According to the present invention, preferably, the gas feed zone is a region formed by an outer side surface of the catalyst bed and an inner wall of the housing, and the gas discharge zone is a region surrounded by an inner side surface of the catalyst bed.
In the invention, the catalyst bed is designed into an inverted trapezoid structure, and the radial thickness of the catalyst bed is reduced from top to bottom in sequence, so that lower burnt gas radially flows through the catalyst bed, contacts with the primary burnt regenerant filled in the catalyst bed and is burnt again, and the generated heat can be quickly brought out of the catalyst bed, thereby avoiding the catalyst bed from being damaged by the flying temperature of the catalyst bed and the internal components of the reactor.
According to the invention, preferably, the radial thickness of the catalyst bed decreases in a range of 30-80%, preferably in a range of 50-70%, from top to bottom. That is, the ratio of the difference in the radial thickness of the catalyst bed disposed above to the radial thickness of the catalyst bed disposed below to the radial thickness of the catalyst bed disposed above is 30 to 80%, preferably 50 to 70%. In the invention, when the decreasing amplitude is less than 30%, the radial thickness of the lower catalyst bed is too large, which is not beneficial to heat transfer and diffusion, and the bed layer can generate temperature runaway; when the decreasing amplitude is 80%, the radial thickness of the lower catalyst bed is too thin, but the downward flow channels of the catalyst are also narrowed, which is unfavorable for the flow of the catalyst.
According to the invention, preferably, the ratio of the radial thickness of the catalyst bed to the radius of the shell is between 0.5 and 0.8:1, preferably 0.6 to 0.7:1. when the ratio is less than 0.5:1, the radial thickness of the catalyst bed is small, which is not beneficial to the flow of the catalyst; when the ratio is > 0.8:1, the radial bed thickness of the catalyst is large, which is unfavorable for the radial penetration of the burnt gas flow.
According to the present invention, preferably, the catalyst bed is provided with an upper plate surface and a lower plate surface, which are both plate surfaces through which gas cannot pass; the catalyst bed is provided with an inner side surface and an outer side surface which are net surfaces through which gas can pass. This arrangement ensures that the lower burnt gas flows radially through the catalyst bed.
According to the present invention, preferably, the upper plate surface and the lower plate surface of the catalyst bed each independently extend in the radial direction of the housing to be connected to the inner wall of the housing.
According to the invention, preferably, the lower gas outlet pipe is connected to the upper plate surface of the catalyst bed; further preferably, the outer diameter of the lower gas outlet pipe is equal to or greater than the width of the gas discharge region in the radial direction of the housing, and the outer diameter of the lower gas outlet pipe is preferably equal to the width of the gas discharge region in the radial direction of the housing.
According to the invention, preferably, the lower gas outlet pipe extends in the longitudinal direction of the housing to and through the upper combustion zone.
In the present invention, the number of the lower burnt gas inlets depends on the maximum carbon deposition amount of the catalyst at the time of full-load operation of the apparatus, and the higher the carbon deposition amount, the larger the number of burnt gas inlets used. Preferably, the number of lower char gas inlets is 2-10, preferably 3-6.
In some embodiments of the present invention, preferably, two adjacent lower char gas inlets are disposed at equal intervals on a side wall of the housing.
In some embodiments of the invention, preferably, the ratio of the height of the catalyst bed to the spacing of adjacent two of the lower char gas inlets is from 3 to 9:1, preferably 4-5:1. the height of the catalyst bed refers to the distance between the upper plate surface and the lower plate surface of the catalyst bed.
According to the present invention, preferably, each of the lower char gas inlets is provided with an oxygen analyzer and an air injection line for regulating the oxygen content in the lower char gas passing through the lower char gas inlet.
According to the invention, the carbon deposit content in the primary coking agent can be removed rapidly by regulating and controlling the oxygen content change rule in the lower coking gas passing through the lower coking gas inlet, and the generated heat can be brought out of the catalyst bed rapidly, so that the catalyst and the reactor structure are prevented from being damaged due to the temperature runaway of the catalyst bed. Preferably, the oxygen content in the lower char gas passing through the lower char gas inlet increases in sequence from top to bottom.
In some embodiments of the invention, preferably, the oxygen content of the lower char gas is increased in a range of 2-10% by volume from top to bottom.
According to the invention, preferably, the catalyst bed is used to contact the primary char regenerant with a lower char gas and re-char to obtain a char regenerant and a gas product.
According to the present invention, preferably, there is a gap between the outer side surface of the catalyst bed and the inner wall of the housing; further preferably, the width of the gap in the radial direction of the housing is 5-15%, preferably 5-10% of the radius of the housing. When the gap is less than 5% or greater than 15%, it is disadvantageous that the inlet gas is uniformly distributed along the annular side.
According to the present invention, preferably, a gas distribution plate is further provided inside the housing, the gas distribution plate being provided at an outlet of the lower char gas inlets for distributing the lower char gas passing through each of the lower char gas inlets.
The structure schematic diagram of a lower combustion zone of a coking reactor for dehydrogenating a spent agent of propane is shown as figure 1, and the lower combustion zone comprises a shell, and a lower gas outlet pipe 1 is arranged on the shell; the inside of the shell is provided with a catalyst bed 2 which is annularly arranged around the central axis of the shell, the catalyst bed 2 is filled with a primary burning regenerant, and the inside of the shell is divided into a gas feeding area 3 and a gas discharging area 4;
wherein the side wall of the housing is provided with at least two lower char gas inlets 5, the lower char gas inlets 5 being for introducing lower char gas into the gas feed zone 3; the radial thickness of the catalyst bed 2 decreases from top to bottom in sequence; the gas feeding zone 3 is used for enabling lower burnt gas to flow radially through the catalyst bed 2, contact with the primary burnt regenerant and re-burn, and the obtained gas product is discharged through the lower gas outlet pipe 1 after being collected in the gas discharging zone 4;
Wherein, the bottom of the lower combustion zone is provided with a discharge hole 6, the catalyst bed 2 is provided with an upper plate surface 9 and a lower plate surface 10, which are plate surfaces through which gas cannot pass; the upper plate surface 9 and the lower plate surface 10 of the catalyst bed respectively and independently extend along the radial direction of the shell to be connected with the inner wall of the shell; the catalyst bed 2 is provided with an inner side surface 8 and an outer side surface 7 which are net surfaces through which gas can pass; the lower gas outlet pipe 1 is connected with the upper plate surface 9 of the catalyst bed; the outer diameter of the lower gas outlet pipe 1 is equal to the width of the gas discharging area 4 along the radial direction of the shell;
Wherein the number of the lower burnt gas inlets 5 is 5, and each lower burnt gas inlet 5 is provided with an oxygen analyzer 11 and an air injection line 12; the interior of the housing is also provided with a gas distribution plate 13, the gas distribution plate 13 being arranged at the outlet of the lower char gas inlet 5.
According to a particularly preferred embodiment of the present invention, the char reactor comprises an upper combustion zone and a lower combustion zone in up-down communication; wherein the lower combustion zone comprises a housing provided with a lower gas outlet tube; the inside of the shell is provided with a catalyst bed which is annularly arranged around the central axis of the shell, the catalyst bed is filled with a primary burning regenerant, and the inside of the shell is divided into a gas feeding area and a gas discharging area;
wherein the side wall of the housing is provided with at least two lower char gas inlets for introducing lower char gas into the gas feed zone;
Wherein, from top to bottom, the radial thickness of the catalyst bed is sequentially reduced;
Wherein the gas feeding zone is used for enabling the lower burnt gas to radially flow through the catalyst bed, contact with the primary burnt regenerant and re-burn, and the obtained gas product is discharged through the lower gas outlet pipe after being collected in the gas discharging zone;
The gas feeding zone is a zone formed by the outer side surface of the catalyst bed and the inner wall of the shell, and the gas discharging zone is a zone of the inner side surface of the catalyst bed surrounding the city;
Wherein, the catalyst bed is provided with an upper plate surface and a lower plate surface which are both plate surfaces through which gas cannot pass; the catalyst bed is provided with an inner side surface and an outer side surface which are mesh surfaces through which gas can pass; the upper plate surface and the lower plate surface of the catalyst bed respectively and independently extend along the radial direction of the shell to be connected with the inner wall of the shell.
In a second aspect, the present invention provides a method for burning propane dehydrogenation spent agent, which is carried out in a burning reactor provided in the first aspect, wherein the method comprises the following steps:
(1) Contacting a propane dehydrogenation spent catalyst with upper burnt gas in an upper combustion zone and performing primary burning to obtain a primary burnt regenerant which flows downwards into a catalyst bed in a lower combustion zone;
(2) The lower burnt gas enters the gas feeding area through at least two lower burnt gas inlets, flows radially through the catalyst bed, contacts with the primary burnt regenerant and is subjected to re-burning to obtain a gas product and the burnt regenerant; wherein the gas products are collected in a gas discharging area and discharged through a gas outlet pipe.
In the present invention, the kind of the propane dehydrogenation spent agent has a wide selection range. Preferably, the carbon deposition amount of the propane dehydrogenation spent agent is from 0.2 to 10wt%, for example, from 0.2wt%, 0.5wt%, 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, 6wt%, 8wt%, 10wt%, and any value in the range of any two values, preferably from 0.5 to 8wt%.
In some embodiments of the invention, preferably, the oxygen content of the upper char gas is in the range of 0.4 to 1.5 volume%, preferably 0.5 to 1.3 volume%; the inlet temperature is 480-550 ℃, preferably 490-540 ℃.
In the present invention, a wide selection range is provided for the kind of the upper burnt gas as long as the oxygen content in the upper burnt gas satisfies the above-described limitation. Preferably, the upper char gas includes, but is not limited to, a mixed gas containing oxygen and air.
In some embodiments of the invention, preferably, the conditions of primary scorch include: the temperature is 480-550 ℃, preferably 490-540 ℃; the time is 1-6h, preferably 3-5h; the gas-agent ratio is 2000-4000:1, preferably 2500-3500:1. wherein the gas-agent ratio is the dosage ratio of the upper burnt gas in mL and the propane dehydrogenation spent agent in mL.
In some embodiments of the invention, the char formation amount of the primary char regenerant is preferably 0.2 to 5wt%, for example, preferably 0.2wt%, 0.5wt%, 1wt%, 2wt%, 3wt%, 5wt%, and any value in the range of any two values, preferably 0.5 to 3wt%.
In some embodiments of the invention, preferably, the oxygen content of the lower char gas is from 1 to 15% by volume, preferably from 2 to 10% by volume; the inlet temperature is 510-580 ℃, preferably 530-560 ℃.
In the present invention, a wide selection range is provided for the kind of the lower-part coke-oven gas as long as the oxygen content in the lower-part coke-oven gas satisfies the above-mentioned limitation. Preferably, the lower char gas includes, but is not limited to, a mixed gas containing oxygen and air.
In some embodiments of the invention, preferably, the re-scorching conditions comprise: the temperature is 520-580 ℃, preferably 540-560 ℃; the time is 1-5h, preferably 2-3h; the gas-agent ratio is 2000-4000:1, preferably 2500-3500:1. wherein the gas-agent ratio is the ratio of the total lower burnt gas in mL to the amount of the primary burnt regenerant in mL.
In some embodiments of the invention, preferably, the char formation amount of the char regenerant is less than or equal to 0.2wt%.
In the present invention, when the carbon deposit amount of the charred regeneration agent does not satisfy the above-described limit, that is, when the carbon deposit amount of the charred regeneration agent is > 0.2wt%, the step (2) is repeated until the carbon deposit amount of the charred regeneration agent satisfies the above-described limit.
In some embodiments of the present invention, preferably, when the carbon deposition amount of the propane dehydrogenation spent agent is > 2.5wt%, the oxygen content in the lower char gas through each of the lower char gas inlets increases in sequence from top to bottom; or when the carbon deposit amount of the propane dehydrogenation spent agent is 0.2-2.5wt%, the oxygen content in the lower burnt gas through each of the lower burnt gas inlets is the same.
In some embodiments of the invention, preferably, when the primary char regenerant enters the catalyst bed, the temperature rise of the catalyst bed is > 3 ℃, the oxygen content in the lower char gas passing through each of the lower char gas inlets increases in sequence from top to bottom; or when the primary coking regenerant enters the catalyst bed, and the temperature rise of the catalyst bed is less than or equal to 3 ℃, the oxygen content of the lower coking gas passing through each lower coking gas inlet is the same.
In a third aspect, the present invention provides a regenerator for a propane dehydrogenation spent agent, the regenerator being divided from top to bottom into a coke burning zone, a cooling zone, an oxychlorination zone and a drying zone; wherein the scorch zone is a scorch reactor provided in the first aspect.
In the invention, the discharge port of the coking reactor is connected with the inlet of the cooling zone for cooling the coking regenerant without special explanation.
In the invention, under the condition of no special condition, the scorching zone aims at contacting and reacting the propane dehydrogenation spent catalyst with the scorching gas to remove the carbon deposit amount of the propane dehydrogenation spent catalyst, thereby obtaining the scorching regenerant; the drying area is used for cooling the burnt spent agent to obtain a cooling regenerant; the oxychlorination zone aims at contacting and reacting a cooling spent agent with oxychlorination gas to obtain an oxychlorination regenerant; the drying zone aims to remove water and surface residual chlorine from the oxychlorination regenerant through high-temperature drying to obtain the propane dehydrogenation regenerant.
In a fourth aspect, the present invention provides a process for regenerating a propane dehydrogenation spent agent, the process being carried out in a regenerator provided in the third aspect, the process comprising: and (3) sequentially carrying out scorching treatment, cooling treatment, oxychlorination treatment and drying treatment on the propane dehydrogenation spent catalyst to obtain the propane dehydrogenation regenerant.
In the present invention, the types of the propane dehydrogenation spent catalyst are all defined according to the above description, and the present invention is not described herein.
In some embodiments of the present invention, preferably, the process of the scorch treatment includes: the propane dehydrogenation spent agent is contacted with upper burnt gas and is subjected to primary burning, so that a primary burnt regenerant is obtained; and (3) contacting the primary burning regenerant with lower burning gas and performing re-burning to obtain the burning regenerant. Wherein, the conditions of upper burning gas, primary burning, lower burning gas and re-burning are all defined according to the above description, and the invention is not repeated here.
In some embodiments of the present invention, preferably, the cooling process includes: and (3) contacting the charred regenerant with a cooling medium and performing heat exchange to obtain the cooling regenerant at 80-150 ℃. Wherein the cooling medium includes, but is not limited to, air, water, and the like.
In some embodiments of the present invention, preferably, the oxychlorination process comprises: and (3) contacting the burnt regenerated catalyst with oxychlorination gas and reacting to obtain the oxychlorination regenerated catalyst. Wherein the oxygen content in the oxychlorination gas is preferably 10-20% by volume, and the chlorine content is preferably 5-10% by volume; the reaction conditions include: the temperature is 500-530 ℃, preferably 510-520 ℃; the gas-agent ratio is 800-1500:1, preferably 1000-1200:1, a step of; the time is 2-6 hours, preferably 4-5 hours. The gas-agent ratio is the ratio of the amount of oxychlorinated gas in mL to the amount of the coke-burning regenerating agent in g.
In some embodiments of the present invention, preferably, the drying process includes: drying the oxychlorination regenerant at 550-600 ℃ for 1-4h to obtain the propane dehydrogenation regenerant.
The present invention will be described in detail by examples.
Example 1
The coke burning reactor comprises an upper combustion zone and a lower combustion zone which are communicated up and down; the schematic structure of the lower combustion zone is shown in fig. 1, and the lower combustion zone comprises a shell, wherein a lower gas outlet pipe 1 is arranged on the shell, and the outer diameter of the lower gas outlet pipe 1 = the width of a gas discharging zone 4 along the radial direction of the shell; the inside of the shell is provided with a catalyst bed 2 which is annularly arranged around the central axis of the shell, the catalyst bed 2 is filled with a primary burning regenerant, and the inside of the shell is divided into a gas feeding area 3 and a gas discharging area 4; the side wall of the shell is provided with 5 lower-part coking gas inlets, two adjacent lower-part coking gas inlets are arranged on the side wall of the shell at equal intervals, the gas feeding area 3 is an area formed by the outer side surface of the catalyst bed and the inner wall of the shell, and the gas discharging area 4 is an area of the inner side surface of the catalyst bed surrounding the city; the catalyst bed is provided with an upper plate surface 9 and a lower plate surface 10, which are plates through which gas cannot pass; the catalyst bed is provided with an inner side surface 8 and an outer side surface 7 which are net surfaces through which gas can pass; the upper plate 9 and the lower plate 10 of the catalyst bed each independently extend in the radial direction of the housing to connect with the inner wall of the housing.
Wherein, the height ratio of the distance between two adjacent burnt gas inlets to the catalyst bed is 5:1, a step of; the radial thickness of the catalyst bed is gradually decreased from top to bottom in a range of 50%; the ratio of the radial thickness of the catalyst bed to the radius of the shell is 0.6-0.7:1, a step of; the height ratio of the catalyst bed to the shell was 1:1.
A method of scorching, the method being carried out in the above-described scorching reactor, the method comprising:
(1) Contacting propane dehydrogenation spent catalyst (carbon deposit amount is 7.61 wt%) with upper burning gas (inlet temperature is 535 ℃ C., oxygen content is 1.3 vol%) in upper combustion zone and making primary burning to obtain primary burning regenerant (carbon deposit amount is 1.3 wt%) flowing downwards into catalyst bed in lower combustion zone; the conditions of the primary scorch include: the temperature is 535 ℃ and the time is 4 hours; the gas-to-agent ratio is 3350:1, a step of;
(2) When the carbon deposit amount of the propane dehydrogenation spent agent is more than 2.5 weight percent, the oxygen content in lower burnt gas (with the temperature of 535 ℃) passing through 5 lower burnt gas inlets is sequentially increased to 10 percent from top to bottom, the lower burnt gas enters a gas feeding area, radially flows through a catalyst bed, contacts with the primary burnt regenerant and is subjected to re-burning, and a gas product and the burnt regenerant are obtained (the carbon deposit amount is 0.019 weight percent); wherein, the gas products are collected in a gas discharging area and discharged through a gas outlet pipe; the re-scorch conditions included: the temperature is 535 ℃ and the time is 2 hours; the gas-to-agent ratio is 3350:1, a step of; in the process of re-burning, the temperature rise of the catalyst bed is at most 2 ℃; the carbon deposit amount of the burnt regenerant is lower than a critical value (< 0.2 wt%) and namely, the burning of the propane dehydrogenation spent regenerant is successfully completed.
Comparative example 1
In comparison with example 1, the scorch reactor comprises an upper combustion zone and a lower combustion zone which are communicated with each other up and down; the schematic structure of the lower combustion zone is shown in fig. 2, and the side wall of the shell is provided with 1 lower burnt gas inlet; the radial thickness of the catalyst bed was the same from top to bottom, and the radial thickness of the catalyst bed to the radius ratio of the shell was 0.7:1.
In comparison with example 1, except that in step (2), the lower burnt gas (temperature: 535 ℃ C., oxygen content: 5% by volume) was directly contacted with the as-burnt spent agent and subjected to re-burning to obtain a burnt regenerator (carbon deposit amount: 0.68% by weight), wherein the temperature was 535 ℃ C., time was 4 hours; the gas-to-agent ratio is 3350:1, a step of; in the process of re-scorching, the temperature rise of the catalyst bed is 8 ℃ at most.
Because the carbon deposit amount of the burnt regenerant is higher than the critical value (0.2 wt%) and the process step (2) is repeated, the burning is continued for 4 hours at 535 ℃, the temperature rise of the catalyst bed in the burning process is 0 ℃, the carbon deposit amount of the regenerant after the re-burning is 0.67wt% and the index requirement less than 0.2wt% cannot be met.
Comparative example 2
In comparison with example 1, the scorch reactor comprises an upper combustion zone and a lower combustion zone which are communicated with each other up and down; the schematic structure of the lower combustion zone is shown in fig. 2, and the side wall of the shell is provided with 1 lower burnt gas inlet; the radial thickness values of the catalyst beds are the same from top to bottom, and the ratio of the difference between the primary radius and the secondary radius of the catalyst beds to the radius of the shell is 0.7:1.
In comparison with example 1, except that in step (2), the lower burnt gas (temperature: 560 ℃ C., oxygen content: 5% by volume) was directly contacted with the as-burnt spent agent and subjected to re-burning to obtain a burnt regenerator (carbon deposit amount: 0% by weight), wherein the temperature: 560 ℃ C., time was 4 hours; the gas-to-agent ratio is 3350:1, a step of; in the process of re-scorching, the temperature rise of the catalyst bed is 15 ℃ at most.
The catalyst undergoes a phase change after the scorch, from theta alumina to inactive alpha alumina, so that the scorch cannot be performed using this condition.
Example 2
The char reactor shown in example 1 was followed, except that the number of lower char gas inlets was replaced with 3.
A method of scorching, the method being carried out in the above-described scorching reactor, the method comprising:
(1) Contacting propane dehydrogenation spent catalyst (carbon deposit amount is 7.61 wt%) with upper burning gas (temperature is 535 ℃ C., oxygen content is 1.3 vol%) in upper combustion zone and performing primary burning to obtain primary burning regenerant (carbon deposit amount is 1.3 wt%) flowing downwards into catalyst bed in lower combustion zone; the conditions of the primary scorch include: the temperature is 535 ℃ and the time is 4 hours; the gas-to-agent ratio is 3350:1, a step of;
(2) When the carbon deposit amount of the propane dehydrogenation spent agent is more than 2.5 weight percent, the oxygen content in lower burnt gas (with the temperature of 535 ℃) passing through 3 lower burnt gas inlets is sequentially increased to 10 percent from top to bottom, the lower burnt gas enters a gas feeding area, radially flows through a catalyst bed, contacts with the primary burnt regenerant and is subjected to re-burning, and a gas product and the burnt regenerant (with the carbon deposit amount of 0.021 weight percent) are obtained; wherein, the gas products are collected in a gas discharging area and discharged through a gas outlet pipe; the re-scorch conditions included: the temperature is 535 ℃ and the time is 2 hours; the gas-to-agent ratio is 3350:1, a step of; in the process of re-scorching, the temperature rise of the catalyst bed is at most 3 ℃. The carbon deposit content of the regenerant after re-burning is 0.021wt% and reaches the index requirement of less than 0.2wt%, namely, the burning of the propane dehydrogenation spent agent is successfully completed.
Example 3
A scorch reactor as shown in example 1.
A method of scorching, the method being carried out in the above-described scorching reactor, the method comprising:
(1) Contacting propane dehydrogenation spent catalyst (carbon deposit amount is 7.61 wt%) with upper burning gas (temperature is 535 ℃ C., oxygen content is 1.3 vol%) in upper combustion zone and performing primary burning to obtain primary burning regenerant (carbon deposit amount is 1.3 wt%) flowing downwards into catalyst bed in lower combustion zone; the conditions of the primary scorch include: the temperature is 535 ℃ and the time is 4 hours; the gas-to-agent ratio is 3350:1, a step of;
(2) When the carbon deposit amount of the propane dehydrogenation spent agent is more than 2.5 weight percent, the oxygen content in lower coke burning gas (with the temperature of 560 ℃) passing through 5 lower coke burning gas inlets sequentially increases to 10 percent from top to bottom, and the lower coke burning gas enters a gas feeding area, radially flows through a catalyst bed, contacts with the primary coke burning regenerant and is subjected to re-burning, so that a gas product and the coke burning regenerant (with the carbon deposit amount of 0.025 weight percent) are obtained; wherein, the gas products are collected in a gas discharging area and discharged through a gas outlet pipe; the re-scorch conditions included: the temperature is 560 ℃ and the time is 2 hours; the gas-agent ratio is 2500:1, a step of; in the process of re-burning, the temperature rise of the catalyst bed is at most 5 ℃; the carbon deposition amount of the coke burning regenerant is lower than a critical value (< 0.2%) and the coke burning is successfully completed.
Compared with comparative examples 1-2, the method for burning propane dehydrogenation spent agent is carried out in the burning reactor, and combines the carbon deposition amount of the propane dehydrogenation spent agent or the bed temperature rise caused by the primary burning regeneration agent entering into the catalyst bed is regulated and controlled to control the oxygen content in the lower burning gas passing through the lower burning gas inlet, so that the carbon deposition amount of the primary burning spent agent can be further removed, and the catalyst sintering phase change caused by the overtemperature of the catalyst bed is effectively avoided.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.

Claims (28)

1. A scorch reactor for propane dehydrogenation spent agent, which is characterized in that the scorch reactor comprises an upper combustion zone and a lower combustion zone which are communicated up and down; wherein the lower combustion zone comprises a housing provided with a lower gas outlet tube; the inside of the shell is provided with a catalyst bed which is annularly arranged around the central axis of the shell, the catalyst bed is filled with a primary burning regenerant, and the inside of the shell is divided into a gas feeding area and a gas discharging area;
wherein the side wall of the housing is provided with at least two lower char gas inlets for introducing lower char gas into the gas feed zone;
the radial thickness of the catalyst bed is sequentially reduced from top to bottom, and the radial thickness of the catalyst bed is reduced by 30-80%;
The gas feeding zone is used for enabling the lower burnt gas to flow radially through the catalyst bed, contact with the primary burnt regenerant and re-burn, and the obtained gas product is discharged through the lower gas outlet pipe after being collected in the gas discharging zone.
2. The char reactor of claim 1, wherein the upper combustion zone is configured to contact propane dehydrogenation spent and upper char gas and perform a primary char to obtain the primary char regenerant;
The lower combustion zone is used for contacting the primary coking regenerant with lower coking gas and re-coking to obtain the coking regenerant.
3. The char reactor of claim 2, wherein the char reactor further comprises a feed inlet and a discharge outlet;
the feed inlet is arranged at the top of the upper combustion zone, and the discharge outlet is arranged at the bottom of the lower combustion zone.
4. The char reactor according to claim 2, wherein the gas feed zone is a region formed by an outer side surface of the catalyst bed and an inner wall of the housing, and the gas discharge zone is a region surrounded by an inner side surface of the catalyst bed.
5. The char reactor according to claim 1, wherein the radial thickness of the catalyst bed decreases in a range of 50-70% from top to bottom.
6. The char reactor of claim 5, wherein the ratio of the radial thickness of the catalyst bed to the radius of the shell is 0.5-0.8:1.
7. The char reactor of claim 5, wherein the ratio of the radial thickness of the catalyst bed to the radius of the shell is 0.6-0.7:1.
8. The char reactor according to claim 1, wherein the catalyst bed is provided with an upper plate surface and a lower plate surface, both of which are plate surfaces through which gas cannot pass; the catalyst bed is provided with an inner side surface and an outer side surface which are mesh surfaces through which gas can pass;
the upper plate surface and the lower plate surface of the catalyst bed respectively and independently extend along the radial direction of the shell to be connected with the inner wall of the shell.
9. The char reactor according to claim 8, wherein the lower gas outlet pipe connects to an upper deck of the catalyst bed;
The outer diameter of the lower gas outlet pipe is larger than or equal to the radial width of the gas discharging area along the shell;
the lower gas outlet tube extends longitudinally of the housing to and through the upper combustion zone.
10. The char reactor according to claim 1, wherein the number of lower char gas inlets is 2-10.
11. The char reactor according to claim 10, wherein the number of lower char gas inlets is 3-6.
12. The char reactor according to claim 10, wherein adjacent two of the lower char gas inlets are equally spaced on the side wall of the housing;
The ratio of the height of the catalyst bed to the spacing between two adjacent lower burnt gas inlets is 3-9:1.
13. The char reactor according to claim 12, wherein the ratio of the height of the catalyst bed to the spacing of adjacent two of the lower char gas inlets is 4-5:1.
14. The char reactor according to claim 10, wherein each of the lower char gas inlets is provided with an oxygen analyzer and an air injection line for regulating the oxygen content in the lower char gas passing through the lower char gas inlet.
15. The char reactor according to claim 14, wherein the oxygen content in the lower char gas passing through the lower char gas inlet increases in sequence from top to bottom.
16. The char reactor according to claim 15, wherein the oxygen content of the lower char gas increases in the range of 2-10% by volume from top to bottom.
17. The char reactor according to any of claims 1-16, wherein the catalyst bed is used to contact the primary char regenerant with a lower char gas and re-char to obtain a char regenerant and a gas product.
18. The char reactor of claim 17, wherein there is a gap between the outer side of the catalyst bed and the inner wall of the housing;
The width of the gap along the radial direction of the shell is 5-15% of the radius of the shell.
19. The char reactor of claim 18, wherein the width of the gap in the radial direction of the housing is 5-10% of the radius of the housing.
20. The char reactor of claim 17, wherein the interior of the housing is further provided with a gas distribution plate disposed at the outlet of the lower char gas inlet.
21. A process for the scorch of a propane dehydrogenation spent agent, characterized in that it is carried out in a scorch reactor according to any one of claims 1 to 20, wherein it comprises the steps of:
(1) Contacting propane dehydrogenation spent agent with upper burnt gas in an upper combustion zone and performing primary burning to obtain a primary burnt regenerant which flows downwards into a catalyst bed of a lower combustion zone;
(2) The lower burnt gas enters the gas feeding area through at least two lower burnt gas inlets, flows radially through the catalyst bed, contacts with the primary burnt regenerant and is subjected to re-burning to obtain a gas product and the burnt regenerant; wherein the gas products are collected in a gas discharging area and discharged through a gas outlet pipe.
22. The process of claim 21, wherein the propane dehydrogenation spent catalyst has a char yield of 0.2-10wt%;
The oxygen content in the upper burnt gas is 0.4-1.5 volume percent; the inlet temperature is 480-550 ℃;
the conditions of the primary scorch include: the temperature is 480-550 ℃; the time is 1-6h; the gas-agent ratio is 2000-4000:1, a step of;
the carbon deposition amount of the primary burning regenerant is 0.2-5wt%;
The oxygen content in the lower burnt gas is 1-15% by volume; the inlet temperature is 510-580 ℃;
the re-scorching conditions include: the temperature is 510-580 ℃; the time is 1-5h; the gas-agent ratio is 2000-4000:1.
23. The process of claim 22, wherein the propane dehydrogenation spent catalyst has a char yield of 0.5-8wt%;
The oxygen content in the upper burnt gas is 0.5-1.3 volume percent; the inlet temperature is 490-540 ℃;
The conditions of the primary scorch include: the temperature is 490-540 ℃; the time is 3-5h; the gas-agent ratio is 2500-3500:1, a step of;
The carbon deposition amount of the primary burning regenerant is 0.5-3wt%;
The oxygen content in the lower burnt gas is 2-10% by volume; the inlet temperature is 530-560 ℃;
the re-scorching conditions include: the temperature is 530-560 ℃; the time is 2-3h; the gas-agent ratio is 2500-3500:1.
24. The method of claim 22, wherein the char regenerator has a char formation amount of 0.2wt% or less; or repeating the step (2) when the carbon deposit amount of the charring regenerant is more than 0.2 wt%.
25. The method of any of claims 21-24, wherein the oxygen content of the lower char gas passing through each of the lower char gas inlets increases in sequence from top to bottom when the carbon deposition amount of the propane dehydrogenation spent is > 2.5 wt%; or alternatively
When the carbon deposit amount of the propane dehydrogenation spent agent is 0.2-2.5wt%, the oxygen content in the lower coke gas through each of the lower coke gas inlets is the same.
26. The method of any of claims 21-24, wherein the oxygen content of the lower char gas passing through each of the lower char gas inlets increases in sequence from top to bottom as the primary char regenerant enters the catalyst bed, the catalyst bed temperature rise being > 3 ℃; or alternatively
When the primary coking regenerant enters the catalyst bed, and the temperature rise of the catalyst bed is less than or equal to 3 ℃, the oxygen content of the lower coking gas passing through each lower coking gas inlet is the same.
27. A regenerator for a propane dehydrogenation spent agent, which is characterized in that the regenerator is divided into a coke burning zone, a cooling zone, an oxychlorination zone and a drying zone from top to bottom;
wherein the char zone is the char reactor of any of claims 1-20.
28. A process for regenerating a propane dehydrogenation spent agent, the process being carried out in a regenerator as claimed in claim 27, the process comprising: and (3) sequentially carrying out scorching treatment, cooling treatment, oxychlorination treatment and drying treatment on the propane dehydrogenation spent catalyst to obtain the propane dehydrogenation regenerant.
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