CN110013887A - The in situ regeneration method of catalyst inactivation - Google Patents
The in situ regeneration method of catalyst inactivation Download PDFInfo
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- CN110013887A CN110013887A CN201810019659.XA CN201810019659A CN110013887A CN 110013887 A CN110013887 A CN 110013887A CN 201810019659 A CN201810019659 A CN 201810019659A CN 110013887 A CN110013887 A CN 110013887A
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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
- B01J38/00—Regeneration or reactivation of catalysts, in general
- B01J38/02—Heat treatment
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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
- 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
- B01J38/14—Treating with free oxygen-containing gas with control of oxygen content in oxidation gas
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Abstract
The present invention relates to a kind of in situ regeneration method of catalyst inactivation, mainly solve the problems, such as to need the outer coke burning regeneration of device in the prior art.The present invention by using a kind of catalyst inactivation in situ regeneration method, in-situ regeneration is carried out to the catalyst of inactivation on catalyst situ regeneration device, described device includes air distribution system, in-situ regeneration device, heating furnace, cooler, gas-liquid separator, analysis system, control system, air distribution system entrance is connected to gas access pipeline, outlet is connected with in-situ regeneration device, in-situ regeneration device is externally provided with heating furnace, inside is inserted with thermocouple, in-situ regeneration device outlet with successively with cooler, gas-liquid separator is connected, the gaseous phase outlet of gas-liquid separator is connected with analysis system, the control system preferably solves the above problem using the technical solution of PLC, it can be used in the in-situ regeneration of catalyst inactivation.
Description
Technical field
The present invention relates to a kind of in situ regeneration method of catalyst inactivation.
Background technique
Tail gas contains a variety of gas such as propylene, propane, oxygen, hydrogen, carbon dioxide during HPPO method production propylene oxide
Body can make whole device have explosion danger, therefore must because of the great recovery value of propylene, and when oxygen content is higher in tail gas
Deoxidation treatment must be carried out to the oxygen in gas.
In existing deoxy technology, catalysis is burnt due to low burning and initiation temperature, without the pollutant emissions such as NOx and combustion gas
Concentration requires low excellent combustibility, is the current most effective way for solving organic pollutant discharge and the recycling of certain organic matters
Diameter.Propylene tail gas is while carrying out catalysis reaction, due in addition to generating carbon dioxide and water, also generating there are condensation reaction
A part of coke deposits on a catalyst, to make catalyst surface area reduce, activity reduction, i.e. catalyst inactivation.For product
The regeneration of high-temperature oxydation burn off carbon deposit can be used in decaying catalyst caused by charcoal, and activity can partially or completely be restored, in work
Industry production in may continue to using.
Catalyst regeneration is divided into in-situ regeneration and ex-situ regeneration, for the above this deoxidation catalysis reaction, catalyst
After inactivation, it is necessary to stop, discharging, decaying catalyst is transported to regenerating furnace and carries out coke burning regeneration outside device, dress will be greatly increased in this way
It unloads the workload of catalyst, increases cost, the problems such as the abrasion being also easy to happen during Catalyst packing.
Currently, catalyst inactivation regenerates shorter mention in-situ regeneration problem.The present invention loses for the carbon distribution of dehydrogenation catalyst
It is living, a kind of coke burning regeneration method in situ is devised, a series of problems of the outer coke burning regeneration of device is avoided.
Summary of the invention
The technical problem to be solved by the present invention is to need coke burning regeneration outside device in the prior art, provide a kind of new
Catalyst inactivation in situ regeneration method, having the advantages that can in-situ regeneration.
To solve the above problems, The technical solution adopted by the invention is as follows: a kind of in situ regeneration method of catalyst inactivation,
In-situ regeneration carried out to the catalyst of inactivation on catalyst situ regeneration device, described device include air distribution system, it is in situ again
Raw device, heating furnace, cooler, gas-liquid separator, analysis system, control system, air distribution system entrance are connected to gas access pipeline,
Outlet is connected with in-situ regeneration device, and in-situ regeneration device is externally provided with heating furnace, and inside is inserted with thermocouple, in-situ regeneration device export and according to
Secondary to be connected with cooler, gas-liquid separator, the gaseous phase outlet of gas-liquid separator is connected with analysis system, and the control system uses
PLC (programmable logic controller (PLC)) control；The oxygen-nitrogen mixture that medium prepares certain oxygen content by air distribution system is burnt, by original
Position regenerator top is passed through, and carries out in-situ regeneration to catalyst, control heating furnace is to reactor temperature programming, in real time record catalysis
Agent bed temperature and reaction end gas composition.
In above-mentioned technical proposal, it is preferable that in-situ regeneration device is fixed bed reactors.
In above-mentioned technical proposal, it is preferable that the pipeline that air distribution system is connected with in-situ regeneration device is equipped with counterbalance valve, pressure
Table and pressure sensor.
In above-mentioned technical proposal, it is preferable that gas-liquid separator lower part is equipped with tapping line, gaseous phase outlet and analysis system phase
Pipeline even is equipped with counterbalance valve.
In above-mentioned technical proposal, it is preferable that gas access pipeline is equipped with pressure reducing valve.
In above-mentioned technical proposal, it is preferable that control system by signal wire respectively with air distribution system, temperature control system,
Liquidometer, counterbalance valve, analysis system on pressure sensor, gas-liquid separator are connected.
In above-mentioned technical proposal, it is preferable that in-situ regeneration device tube core sets 5 thermocouples, and regenerator is placed on a cylinder
The center of formula heating furnace, heating furnace use open electric heating furnace, and heating furnace has 5 bringing-up sections, and wherein first segment is
Preheating section, intermediate three sections are isothermal section, and the 5th section is soaking zone, and catalyst bed upper and lower part is equipped with packing layer.
In above-mentioned technical proposal, it is preferable that described device is equipped with overtemperature, overpressure alarm function.
The present invention relates to a kind of in-situ regeneration is illegal, catalyst mill brought by the outer coke burning regeneration of decaying catalyst device is solved
Damage increases the problem of production cost；Real-time control burns the proportion of medium (mainly containing oxygen gas mixture), burns easily in resolver
The problem of catalyst bed hot-spot occurs；Real-time monitoring is carried out to tail gas composition is burnt, convenient for grasping regeneration progress.This dress
It sets and does not need shut-down, discharging, catalyst abrasion caused by avoiding because of ex-situ regeneration improves work efficiency, and reduction is produced into
This.Meanwhile device is equipped with air distribution system, can deploy the oxygen content for burning medium in real time, prevent catalyst bed temperature runaway.This
Outside, it is additionally provided with on-line chromatograph at device exhaust discharge, can be formed with real-time detection regeneration tail gas, control regeneration event, at any time
Grasp the regeneration level of catalyst.This regeneration method can carry out coke burning regeneration in situ to decaying catalyst, improve work efficiency,
Reduce production cost.Meanwhile the oxygen content for burning medium can be deployed in real time, prevent catalyst bed temperature runaway；It can also supervise in real time
Reaction end gas composition is surveyed, convenient for monitoring regeneration progress, grasps the regeneration level of catalyst at any time, achieves preferable technology effect
Fruit.
Detailed description of the invention
Fig. 1 is decaying catalyst situ regeneration device flow chart of the present invention.
In Fig. 1,1. oxygen pipeline, 2. nitrogen pipeline, 3. spare air pipe, 4. air distribution system, 5. fixed bed reactors, 6.
Heating furnace, 7. counterbalance valve, 8. pressure gauge and pressure sensor, 9. thermocouple, 10. cooler,Gas-liquid separator,Liquid level
Meter,Tapping valve,Counterbalance valve,On-line chromatograph,Pressure reducing valve.
Fig. 2 is fixed bed reactors sectional view.
Fig. 3 is that catalyst regeneration experimental reactor die temperature and oxygen consumption rate change over time figure.
The present invention will be further described below by way of examples, but is not limited only to the present embodiment.
Specific embodiment
[embodiment 1]
The present invention provide one kind do not need disassembly decaying catalyst, the method for being able to carry out coke burning regeneration in situ, mainly according to
Following device is ask to carry out.
As shown in Figure 1, the device is mainly made of gas-phase feed metering units, reaction member and product separative unit.
Control system uses PLC control system, and the parameters such as temperature, pressure, flow can automatic collection, control, record and printing.System
Parameter curve, autoreport are automatically generated, and is equipped with a variety of safety protection functions.
(1) gas feed metering units
The present apparatus uses three road gases: the first via is oxygen, and the second tunnel is nitrogen, and oxygen and nitrogen pass through air distribution system,
As medium is burnt, third road gives over to spare for mixing according to a certain percentage；In addition, nitrogen can be used for device purging and displacement and
Device is airtight.
Air distribution system composition mainly has: computer system, controller, air chest.
Computer system includes computer, automatic distributing software and control card；
Control cabinet includes control box main body, control panel, power supply；
Air chest includes distribution cabinet, mass flow controller, shut-off valve and matches circuits, to guarantee accurate distribution,
And control pressure.
(2) reaction member
Reaction member main body is a fixed bed reactors, and reactor inlet is equipped with pressure gauge, pressure sensor, spring
Formula safety valve, reaction pressure can upload computer, live can also read, and the setting of safety valve ensure that the operation peace of reactor
Entirely.
Reactor tube core sets 5 thermocouples, and reactor is placed on the center of a column type heating furnace, and heating furnace is adopted
With open electric heating furnace, heating furnace has 5 bringing-up sections, and wherein first segment is preheating section, and intermediate three sections are isothermal section, and the 5th
Section is soaking zone.
In order to mitigate the labor intensity of operator, heating furnace is additionally provided with temperature programming, in the shutting down stage of device, instead
Device heating and cooling process is answered, this mode can be used.
Each bringing-up section of heating furnace is provided with temperature safety switch, when detecting that this section of furnace temp reach the height of setting
When ceiling value, the power supply of the heating furnace can be automatically cut off, plays the function of protection reactor.
Reactor pressure protection mechanism is mainly spring pressure safety valve, when system pressure superelevation to the limiting value of setting
When, the pressure of reaction system is laid down in spring loaded safety valve take-off, has the function that protect tankage safety.
(3) product separative unit
Reaction effluent initially enters cooler and is cooled down, and product temperatur can be dropped to 50 DEG C or so by cooler.
Gas-liquid separator, which is entered back into, by reaction product after cooling carries out gas-liquid separation.The gas that gas-liquid separator separates go out, through carrying on the back
After the control of pressure valve back pressure, it is vented after carrying out gas phase composition analysis into on-line chromatograph.
Gas-liquid separator is equipped with pressure difference transmitter and detects liquid level, will after the liquid level in separator reaches the height of setting
Liquid level warning is provided, operator directly can release liquid by gas-liquid separator bottom tapping bivalve group.
To prevent organic gas from liquefying in gas-liquid separator, gas-liquid separator bottom carries out heat preservation heat tracing, by gas-liquid point
From the control of device temperature more than organic gas condensing temperature.It prevents organic gas from liquefying, influences the accuracy and gas-liquid of test
Separating effect.
The application method of device are as follows:
The bolt of reactor head is opened, thermocouple sheath is placed in designated position and the fixation of inside reactor
It is good, filler, decaying catalyst, filler are successively then filled to designated position；Bolt is tightened, then thermocouple is inserted into casing
In fix.
The oxygen-nitrogen mixture that medium prepares certain oxygen content by air distribution system is burnt, is passed through by reactor top；Control
Heating furnace records reaction bed temperature and reaction end gas composition to reactor temperature programming in real time.
HPPO method production propylene oxide propylene tail gas dehydrogenation catalyst coke burning regeneration is carried out using the present apparatus to test.
Experimental procedure:
(1) by the inertia Al of diameter 6mm2O3Porcelain ball is packed into reactor tube in-core, is filled to the position away from nozzle 71cm, then
Decaying catalyst is filled to the position away from nozzle 68cm, then recharges Al2O3The porcelain ball extremely position away from nozzle 48cm；
(2) by reactor tube core sleeve five thermocouples TE-1114, TE-1115, TE-1116, TE-1117 and
TE-1118 is placed in the position away from nozzle 48cm, 68cm, 69.5cm, 71cm and 76cm respectively, investigates burn medium not respectively
Temperature variations into catalyst, into catalyst bed and when leaving catalyst；Wherein, TE-1115, TE-1116,
This three thermocouples of TE-1117 respectively correspond the position on edge, center and lower edge on catalyst bed, i.e. catalyst bed layer height
It is about 20ml for 3cm, volume, is detailed in Fig. 2.
(3) it installs reactor and starts to test after being passed through the air-tightness of nitrogen detection system；Matched by air distribution system
The oxygen-nitrogen mixture conduct for setting oxygen content 3% burns medium and is passed through reactor；Heating furnace temperature program is set, to reactor journey
Sequence heating；In temperature-rise period, the variation of close observation reaction bed temperature and device exhaust composition variation, to observe in time
Progress is burnt, time recording reactor tube walls and die temperature in timely experimentation, and mixed into and out of the oxygen nitrogen of reactor
The oxygen content of gas burns progress to investigate；
(4) when detection reaction bed temperature is without obvious temperature rise, and into and out of the oxygen content in the oxygen-nitrogen mixture of reactor
When unchanged, illustrate to burn completion；It is passed through nitrogen and carries out purging cooling；
(5) experimental data is exported, experimental result, the oxygen-nitrogen mixture of 3% oxygen content, 400 DEG C of constant temperature items of reactor are analyzed
Under part, catalyst regeneration experimental reactor die temperature and oxygen consumption rate change over time figure and see Fig. 3.
[embodiment 2]
The present invention provide one kind do not need disassembly decaying catalyst, the method for being able to carry out coke burning regeneration in situ, mainly according to
Following device is ask to carry out.
As shown in Figure 1, the device is mainly made of gas-phase feed metering units, reaction member and product separative unit.
Control system uses PLC control system, and the parameters such as temperature, pressure, flow can automatic collection, control, record and printing.System
Parameter curve, autoreport are automatically generated, and is equipped with a variety of safety protection functions.
(1) gas feed metering units
The present apparatus uses three road gases: the first via is oxygen, and the second tunnel is nitrogen, and oxygen and nitrogen pass through air distribution system,
As medium is burnt, third road gives over to spare for mixing according to a certain percentage；In addition, nitrogen can be used for device purging and displacement and
Device is airtight.
Air distribution system composition mainly has: computer system, controller, air chest.
Computer system includes computer, automatic distributing software and control card；
Control cabinet includes control box main body, control panel, power supply；
Air chest includes distribution cabinet, mass flow controller, shut-off valve and matches circuits, to guarantee accurate distribution,
And control pressure.
(2) reaction member
Reaction member main body is a fixed bed reactors, and reactor inlet is equipped with pressure gauge, pressure sensor, spring
Formula safety valve, reaction pressure can upload computer, live can also read, and the setting of safety valve ensure that the operation peace of reactor
Entirely.
Reactor tube core sets 4 thermocouples, and reactor is placed on the center of a column type heating furnace, and heating furnace is adopted
With open electric heating furnace, heating furnace has 4 bringing-up sections, and wherein first segment is preheating section, and intermediate 2 sections are isothermal section, and the 4th
Section is soaking zone.
In order to mitigate the labor intensity of operator, heating furnace is additionally provided with temperature programming, in the shutting down stage of device, instead
Device heating and cooling process is answered, this mode can be used.
Each bringing-up section of heating furnace is provided with temperature safety switch, when detecting that this section of furnace temp reach the height of setting
When ceiling value, the power supply of the heating furnace can be automatically cut off, plays the function of protection reactor.
Reactor pressure protection mechanism is mainly spring pressure safety valve, when system pressure superelevation to the limiting value of setting
When, the pressure of reaction system is laid down in spring loaded safety valve take-off, has the function that protect tankage safety.
(3) product separative unit
Reaction effluent initially enters cooler and is cooled down, and product temperatur can be dropped to 50 DEG C or so by cooler.
Gas-liquid separator, which is entered back into, by reaction product after cooling carries out gas-liquid separation.The gas that gas-liquid separator separates go out, through carrying on the back
After the control of pressure valve back pressure, it is vented after carrying out gas phase composition analysis into on-line chromatograph.
Gas-liquid separator is equipped with pressure difference transmitter and detects liquid level, will after the liquid level in separator reaches the height of setting
Liquid level warning is provided, operator directly can release liquid by gas-liquid separator bottom tapping bivalve group.
To prevent organic gas from liquefying in gas-liquid separator, gas-liquid separator bottom carries out heat preservation heat tracing, by gas-liquid point
From the control of device temperature more than organic gas condensing temperature.It prevents organic gas from liquefying, influences the accuracy and gas-liquid of test
Separating effect.
The application method of device are as follows:
The bolt of reactor head is opened, thermocouple sheath is placed in designated position and the fixation of inside reactor
It is good, filler, decaying catalyst, filler are successively then filled to designated position；Bolt is tightened, then thermocouple is inserted into casing
In fix.
The oxygen-nitrogen mixture that medium prepares certain oxygen content by air distribution system is burnt, is passed through by reactor top；Control
Heating furnace records reaction bed temperature and reaction end gas composition to reactor temperature programming in real time.
HPPO method production propylene oxide propylene tail gas dehydrogenation catalyst coke burning regeneration is carried out using the present apparatus to test.
Experimental procedure:
(1) by the inertia Al of diameter 6mm2O3Porcelain ball is packed into reactor tube in-core, is filled to the position away from nozzle 69cm, then
Decaying catalyst is filled to the position away from nozzle 65cm, then recharges Al2O3The porcelain ball extremely position away from nozzle 45cm；
(2) by 4 thermocouples in reactor tube core sleeve, be placed in respectively away from nozzle 48cm, 68cm, 71cm and
The position of 76cm is investigated respectively and burns medium and do not enter catalyst, the temperature into catalyst bed and when leaving catalyst
Situation of change.
(3) it installs reactor and starts to test after being passed through the air-tightness of nitrogen detection system；Matched by air distribution system
The oxygen-nitrogen mixture conduct for setting oxygen content 3% burns medium and is passed through reactor；Heating furnace temperature program is set, to reactor journey
Sequence heating；In temperature-rise period, the variation of close observation reaction bed temperature and device exhaust composition variation, to observe in time
Progress is burnt, time recording reactor tube walls and die temperature in timely experimentation, and mixed into and out of the oxygen nitrogen of reactor
The oxygen content of gas burns progress to investigate；
(4) when detection reaction bed temperature is without obvious temperature rise, and into and out of the oxygen content in the oxygen-nitrogen mixture of reactor
When unchanged, illustrate to burn completion；It is passed through nitrogen and carries out purging cooling；
(5) experimental data is exported, experimental result, the oxygen-nitrogen mixture of 3% oxygen content, 400 DEG C of constant temperature items of reactor are analyzed
Under part, obtains catalyst regeneration experimental reactor die temperature and oxygen consumption rate changes over time figure.
[embodiment 3]
The present invention provide one kind do not need disassembly decaying catalyst, the method for being able to carry out coke burning regeneration in situ, mainly according to
Following device is ask to carry out.
As shown in Figure 1, the device is mainly made of gas-phase feed metering units, reaction member and product separative unit.
Control system uses PLC control system, and the parameters such as temperature, pressure, flow can automatic collection, control, record and printing.System
Parameter curve, autoreport are automatically generated, and is equipped with a variety of safety protection functions.
(1) gas feed metering units
The present apparatus uses three road gases: the first via is oxygen, and the second tunnel is nitrogen, and oxygen and nitrogen pass through air distribution system,
As medium is burnt, third road gives over to spare for mixing according to a certain percentage；In addition, nitrogen can be used for device purging and displacement and
Device is airtight.
Air distribution system composition mainly has: computer system, controller, air chest.
Computer system includes computer, automatic distributing software and control card；
Control cabinet includes control box main body, control panel, power supply；
Air chest includes distribution cabinet, mass flow controller, shut-off valve and matches circuits, to guarantee accurate distribution,
And control pressure.
(2) reaction member
Reaction member main body is a fixed bed reactors, and reactor inlet is equipped with pressure gauge, pressure sensor, spring
Formula safety valve, reaction pressure can upload computer, live can also read, and the setting of safety valve ensure that the operation peace of reactor
Entirely.
Reactor tube core sets 5 thermocouples, and reactor is placed on the center of a column type heating furnace, and heating furnace is adopted
With open electric heating furnace, heating furnace has 5 bringing-up sections, and wherein first segment is preheating section, and intermediate three sections are isothermal section, and the 5th
Section is soaking zone.
In order to mitigate the labor intensity of operator, heating furnace is additionally provided with temperature programming, in the shutting down stage of device, instead
Device heating and cooling process is answered, this mode can be used.
Each bringing-up section of heating furnace is provided with temperature safety switch, when detecting that this section of furnace temp reach the height of setting
When ceiling value, the power supply of the heating furnace can be automatically cut off, plays the function of protection reactor.
Reactor pressure protection mechanism is mainly spring pressure safety valve, when system pressure superelevation to the limiting value of setting
When, the pressure of reaction system is laid down in spring loaded safety valve take-off, has the function that protect tankage safety.
(3) product separative unit
Reaction effluent initially enters cooler and is cooled down, and product temperatur can be dropped to 50 DEG C or so by cooler.
Gas-liquid separator, which is entered back into, by reaction product after cooling carries out gas-liquid separation.The gas that gas-liquid separator separates go out, through carrying on the back
After the control of pressure valve back pressure, it is vented after carrying out gas phase composition analysis into on-line chromatograph.
Gas-liquid separator is equipped with pressure difference transmitter and detects liquid level, will after the liquid level in separator reaches the height of setting
Liquid level warning is provided, operator directly can release liquid by gas-liquid separator bottom tapping bivalve group.
To prevent organic gas from liquefying in gas-liquid separator, gas-liquid separator bottom carries out heat preservation heat tracing, by gas-liquid point
From the control of device temperature more than organic gas condensing temperature.It prevents organic gas from liquefying, influences the accuracy and gas-liquid of test
Separating effect.
The application method of device are as follows:
The bolt of reactor head is opened, thermocouple sheath is placed in designated position and the fixation of inside reactor
It is good, filler, decaying catalyst, filler are successively then filled to designated position；Bolt is tightened, then thermocouple is inserted into casing
In fix.
The oxygen-nitrogen mixture that medium prepares certain oxygen content by air distribution system is burnt, is passed through by reactor top；Control
Heating furnace records reaction bed temperature and reaction end gas composition to reactor temperature programming in real time.
HPPO method production propylene oxide propylene tail gas dehydrogenation catalyst coke burning regeneration is carried out using the present apparatus to test.
Experimental procedure:
(1) by the inertia Al of diameter 4mm2O3Porcelain ball is packed into reactor tube in-core, is filled to the position away from nozzle 71cm, then
Decaying catalyst is filled to the position away from nozzle 68cm, then recharges Al2O3The porcelain ball extremely position away from nozzle 48cm；
(2) by reactor tube core sleeve five thermocouples TE-1114, TE-1115, TE-1116, TE-1117 and
TE-1118 is placed in the position away from nozzle 48cm, 68cm, 69cm, 71cm and 76cm respectively, respectively investigate burn medium not into
Enter catalyst, the temperature variations into catalyst bed and when leaving catalyst；Wherein, TE-1115, TE-1116,
This three thermocouples of TE-1117 respectively correspond the position on edge, center and lower edge on catalyst bed, i.e. catalyst bed layer height
It is about 26ml for 4cm, volume, is detailed in Fig. 2.
(3) it installs reactor and starts to test after being passed through the air-tightness of nitrogen detection system；Matched by air distribution system
The oxygen-nitrogen mixture conduct for setting oxygen content 3% burns medium and is passed through reactor；Heating furnace temperature program is set, to reactor journey
Sequence heating；In temperature-rise period, the variation of close observation reaction bed temperature and device exhaust composition variation, to observe in time
Progress is burnt, time recording reactor tube walls and die temperature in timely experimentation, and mixed into and out of the oxygen nitrogen of reactor
The oxygen content of gas burns progress to investigate；
(4) when detection reaction bed temperature is without obvious temperature rise, and into and out of the oxygen content in the oxygen-nitrogen mixture of reactor
When unchanged, illustrate to burn completion；It is passed through nitrogen and carries out purging cooling；
(5) experimental data is exported, experimental result, the oxygen-nitrogen mixture of 3% oxygen content, 400 DEG C of constant temperature items of reactor are analyzed
Under part, catalyst regeneration experimental reactor die temperature and oxygen consumption rate change over time figure and see Fig. 3.
This regeneration method can carry out coke burning regeneration in situ to decaying catalyst, improve work efficiency, reduce production cost.
Meanwhile the oxygen content for burning medium can be deployed in real time, prevent catalyst bed temperature runaway；It can also real-time monitoring reaction end gas group
At convenient for monitoring regeneration progress, the regeneration level of grasp catalyst, achieves preferable technical effect at any time.
Claims (8)
1. a kind of in situ regeneration method of catalyst inactivation carries out the catalyst of inactivation on catalyst situ regeneration device former
Position regeneration, described device includes air distribution system, in-situ regeneration device, heating furnace, cooler, gas-liquid separator, analysis system, control
System, air distribution system entrance are connected to gas access pipeline, and outlet is connected with in-situ regeneration device, and in-situ regeneration device is externally provided with heating
Furnace, inside are inserted with thermocouple, and in-situ regeneration device exports and is successively connected with cooler, gas-liquid separator, the gas of gas-liquid separator
Mutually outlet is connected with analysis system, and the control system is controlled using PLC；It burns medium and is mixed by air distribution system with aerobic nitrogen
Gas is passed through by in-situ regeneration device top, carries out in-situ regeneration to catalyst, controls heating furnace to reactor temperature programming, in real time
Record reaction bed temperature and reaction end gas composition.
2. the in situ regeneration method of catalyst inactivation according to claim 1, it is characterised in that in-situ regeneration device is fixed bed
Reactor.
3. the in situ regeneration method of catalyst inactivation according to claim 1, it is characterised in that air distribution system and in-situ regeneration
The connected pipeline of device is equipped with counterbalance valve, pressure gauge and pressure sensor.
4. the in situ regeneration method of catalyst inactivation according to claim 1, it is characterised in that gas-liquid separator lower part is equipped with
Tapping line, the pipeline that gaseous phase outlet is connected with analysis system are equipped with counterbalance valve.
5. the in situ regeneration method of catalyst inactivation according to claim 1, it is characterised in that gas access pipeline is equipped with
Pressure reducing valve.
6. the in situ regeneration method of catalyst inactivation according to claim 1, it is characterised in that control system passes through signal wire
Respectively with the liquidometer on air distribution system, temperature control system, pressure sensor, gas-liquid separator, counterbalance valve, analysis system phase
Even.
7. the in situ regeneration method of catalyst inactivation according to claim 1, it is characterised in that in-situ regeneration device tube core sets 5
Thermocouple, regenerator are placed on the center of a column type heating furnace, and heating furnace uses open electric heating furnace, heating furnace
Have 5 bringing-up sections, wherein first segment is preheating section, and intermediate three sections are isothermal section, and the 5th section is soaking zone, on catalyst bed
Portion and lower part are equipped with packing layer.
8. the in situ regeneration method of catalyst inactivation according to claim 1, it is characterised in that described device is equipped with overtemperature, surpasses
Press warning function.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113244931A (en) * | 2020-02-11 | 2021-08-13 | 中国石油化工股份有限公司 | Catalyst and method for catalytic oxidation deoxidation of unsaturated hydrocarbon-containing gas |
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