CN1100852C - Process for regenerating hydrocarbon-transforming catalyst - Google Patents
Process for regenerating hydrocarbon-transforming catalyst Download PDFInfo
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- CN1100852C CN1100852C CN00101537A CN00101537A CN1100852C CN 1100852 C CN1100852 C CN 1100852C CN 00101537 A CN00101537 A CN 00101537A CN 00101537 A CN00101537 A CN 00101537A CN 1100852 C CN1100852 C CN 1100852C
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Abstract
The present invention relates to a method for the regeneration of a hydrocarbon conversion catalyst and special equipment thereof. The catalyst to be regenerated orderly passes through a coke combusting region, a chlorine oxidation region, a pre-drying region and a roasting region of a regenerator from top to bottom, wherein oxygen containing gas is introduced into the roasting region; after chlorine is filled, all of the oxygen containing gas is led out, enters the chlorine oxidation region and enters a circulating loop for regenerating gas to supply oxygen for coke combustion. By using the method and the special equipment thereof, no excess oxygen containing gas is discharged to the roasting region of the regenerator; thereby, measures for purifying the discharged gas in the roasting region can be canceled, and the process is simplified.
Description
The present invention relates to a kind of renovation process and equipment thereof of hydrocarbon conversion catalyst, especially face the renovation process and the equipment thereof of H-H reaction catalyzer.
This class hydrocarbon conversion catalyst contains a kind of carrier, the halogen of at least a catalytically-active metals and certain content, and the particle diameter of catalyzer is between 0.5～5.0mm.Catalyst surface is because of the carbon deposit inactivation in reaction process, and its renovation process generally needs following three steps:
(1) uses carbon deposit than the gas burning-off catalyst surface of low oxygen content.
(2) with the gas adding halide-containing of high oxygen content catalyzer is handled, with the halogen on the make-up catalyst.
(3) with the gas of high oxygen content catalyzer is calcined.
Generally realize above step with two kinds of methods on the engineering: a kind of method is to place fixed bed successively to cross bed with three kinds of required different air communication of above-mentioned three steps respectively catalyzer; Second method is that catalyzer is placed moving-bed, makes it to pass through successively three different zones, and these three zones are from top to bottom respectively by three kinds of required different air-flows of above-mentioned three steps.Second kind of catalyst regeneration process wherein, because the catalyzer Intake Quantity is few, the regeneration efficiency height, but advantages such as implement device long-term operation, and be widely used industrial, as the application number of U.S. Pat 4578370 and our company exploitation be 99106878.5, the applying date is the Chinese patent application on May 19th, 1999, belongs to second kind of catalyst regeneration process.
The movable bed catalyst renovation process is adopted in patent application 99106878.5, and reclaimable catalyst is regenerated by scorch region, chlorine oxidation zone and calcining zone in turn.In regenerative process, regeneration gas divides two-way to enter the revivifier scorch region, one tunnel temperature is lower, flow is bigger, be mainly used in and burn, another road temperature is higher, and flow is less, introduces the scorch region bottom, be mainly used in and regulate scorch region outlet catalyst temperature, to call the scorch region bottom in the following text is the overheated zone, and two-way gas and catalyzer form cross-flow, and radial flow is crossed catalyzer scorch region bed, discharge from the beds central outlet then, mix with the chlorine-containing gas of extracting out by chlorine oxidation zone, through dechlorination, dry, be divided into above-mentioned two road gases after boosting, introduce scorch region and begin next circulation.This circulation loop is called the resurgent gases circulation loop.Catalyzer after burning enters axial catalyst moving-bed chlorine oxidation zone again under action of gravity, contact with chloride oxygen-containing gas and to carry out oxychlorination, catalyzer behind the oxychlorination is under action of gravity, enter axial catalyst moving-bed calcining zone, calcine under the oxygen-containing gas effect, the catalyzer after the calcining leaves revivifier by regenerator bottoms.With chlorine-containing gas after catalyzer contacts, discharge by the chlorine-containing gas outlet of chlorine oxidation zone, in the above-mentioned chlorine oxidation zone with the mixed resurgent gases circulation loop that enters of regeneration recycle gas.The oxygen-containing gas of above-mentioned calcining zone divides two-way to discharge, and one the tunnel injects organochlorine, enters chlorine oxidation zone as chlorine-containing gas after heating, and its flow decides by burning oxygen consumption; Another road is unnecessary oxygen-containing gas emptying, and is chloride in this road emptying gas, must can enter atmosphere, the subsequent disposal complexity after alkali cleaning or the dechlorination of other means.
The purpose of this invention is to provide a continuous reproducible, the simple regeneration of hyolrocarbon conversion catalyst method of flow process and specific equipment thereof, in this method, calcining zone does not have unnecessary oxygen-containing gas emptying.
For achieving the above object, the invention provides a kind of like this renovation process, contain a kind of carrier, the halogen of at least a catalytically-active metals and certain content, and the reclaimable catalyst of particle diameter between 0.5～5.0mm, its regeneration step comprises: a) reclaimable catalyst enters the radially moving-bed of catalyst scorch region of revivifier, and contains the carbon deposit that the oxygen regeneration gas contacts the burning-off catalyst surface; B) catalyzer after burning enters axial catalyst moving-bed chlorine oxidation zone under action of gravity, contacts with chlorine-containing gas and carries out oxychlorination; C) catalyzer behind the oxychlorination enters the predrying district of axial catalyst moving-bed under action of gravity, carries out predrying under high temperature, the effect of exsiccant predry pathogenic dryness; D) catalyzer after predrying enters axial catalyst moving-bed calcining zone under action of gravity, calcine under the oxygen-containing gas effect; E) catalyzer after the calcining leaves revivifier by regenerator bottoms, after the degassing, reduction are handled, enters reactive system and begins next circulation.In the above step a)～d), the mode of gas circulation and processing is: introduce oxygen-containing gas in the calcining zone, oxygen-containing gas is derived through behind the beds of calcining zone, enter chlorine oxidation zone after annotating chlorine, with draw after the beds of chlorine oxidation zone contacts, be mixed into the dechlorination system with the reprocessing cycle oxygen deprivation gas of deriving by scorch region, the dehumidification system dechlorination, dry, perhaps carry out separately being mixed into dehumidification system with reprocessing cycle oxygen deprivation gas again after dechlorination is handled, gas mixture after the processing is divided into two-way, one the tunnel for burning gas, enters scorch region after the heating, and one the tunnel is predry pathogenic dryness, enter predrying district after the heating, with the overheated zone that returns the scorch region bottom after catalyzer contacts, and then enter the resurgent gases circulation loop, described dechlorination system itself, on the dechlorinator, perhaps after described dechlorination system, be provided with the gas drain.
The present invention also provides a kind of special-purpose reclaim equiment that is used to realize renovation process of the present invention, this equipment comprises scorch region, chlorine oxidation zone, predrying district and calcining zone from top to bottom successively, wherein, the bottom of scorch region is the overheated zone, there was hot gas conduit to link to each other between predrying district and the overheated zone, between scorch region and the chlorine oxidation zone, between chlorine oxidation zone and the predrying district, between predrying district and the calcining zone, have only the catalyzer conduit to be connected.
The unusual effect of the inventive method is, because of between chlorine oxidation zone and calcining zone, having set up predrying district, with through dechlorination, dried high temperature regeneration circulation gas is predrying the catalyzer that burns with oxychlorination, catalyzer after predrying enters calcining zone again, so just reduced the dry gas consumption of calcining zone effectively, the oxygen-containing gas inlet of calcining zone is decided by burning required oxygen-consumption, the gas that enters calcining zone can all enter chlorine oxidation zone, and then enter the resurgent gases circulation loop, for burning oxygen supply, thereby make calcining zone not have unnecessary oxygen-containing gas emptying, can cancel the control techniques of calcining zone emptying gas.In whole gas circulation, only after dechlorination system or dechlorination system, the gas drain is set, be used for regulating the pressure of scorch region, simplified flow process like this, reduced facility investment and process cost.
Special-purpose reclaim equiment provided by the present invention, be characteristics according to renovation process, set up predrying district, predrying district is linked to each other with the hot gas conduit of crossing of overheated zone, and between scorch region and the chlorine oxidation zone, between chlorine oxidation zone and the predrying district, between predrying district and the calcining zone, have only the catalyzer conduit to be connected, in operating process, be full of catalyzer in the catalyzer conduit, form dense bed, make the gas of chlorine oxidation zone isolate with chlorine oxidation zone and calcining zone respectively by dense catalyst bed with scorch region and predrying separating respectively from, the gas in predrying district by dense catalyst bed.This device structure mode can realize the gas circulating of the inventive method well, finishes the regeneration of hydrocarbon conversion catalyst of the present invention.
Describe the present invention in detail below in conjunction with accompanying drawing, but accompanying drawing does not limit the present invention.
Accompanying drawing and drawing explanation:
Accompanying drawing 1 is a general flow chart around reclaim equiment of the present invention reaches.
As shown in Figure 1, reclaimable catalyst enters buffer zone 40 from revivifier 1 top continuously or in batches through catalyst inlet 9, and buffer zone 40 is revivifier 1 internal pressure vertexs, has nitrogen-sealed pipeline 117 to link to each other, and is nitrogen control to keep this district.Under action of gravity, catalyzer enters the cylindrical space that moving-bed of catalyst scorch region 41 is radially surrounded by Intranet 4 and outer net 3 through many catalyst transport pipelines 2 continuously from buffer zone 40, contact the carbon deposit of burning-off catalyst surface with the oxygen-containing gas cross-flow, the pressure of scorch region is between 0.35～1.5MPa, be generally 0.6～1.2MPa, the residence time of catalyzer is between 0.5～3.0 hour, catalyst coke content is in 0.01～10% (weight) scope, burning gas introduces from managing 106, the temperature in of burning gas is between 400～500 ℃, generally between 440～480 ℃, oxygen level is between 0.4～1.0% (mole), generally between 0.5～0.7% (mole).The bottom of scorch region 41 is overheated zones 42, it is crossed hot gas conduit 115 by one and links to each other with predrying district 44, the reaction bed temperature of scorch region 41 is generally 400～550 ℃, its top temperature be controlled at make local area and chlorine oxidation zone 43, calcining zone 45 bed temperature all under support of the catalyst top temperature allowed to bear, after burning, coke content on the catalyzer drops to below 0.2% (weight), and the reprocessing cycle oxygen deprivation gas after burning is through managing 101 by scorch region 41 derivation.Catalyzer after burning enters axial catalyst moving-bed chlorine oxidation zone 43 by catalyzer conduit 5 under action of gravity, contact with chlorine-containing gas, carries out oxychlorination.
Catalyzer is piled naturally in catalyzer conduit 5 bottoms and is ended, form dense catalyst bed, the bed temperature of chlorine oxidation zone 43 and overheated zone 42 temperature outs are roughly the same, between 510～540 ℃, be generally 525～535 ℃, pressure equates or lower slightly 5～10kPa with scorch region 41, catalyzer is 1～3 hour in this residence time, be generally 2 hours, local area has a chlorine-containing gas outlet pipe 108 and a chlorine-containing gas inlet tube 109 at least, enter the chlorine-containing gas temperature in of chlorine oxidation zone 43 between 510～550 ℃ through managing 109, be generally 530 ℃, cl content is between 0.1～1.0% (weight), and oxygen level is between 3～21% (moles), isolate with scorch region 41 and predrying district 44 respectively by dense catalyst bed through the chlorine-containing gas behind the beds, catalyzer is behind oxychlorination, and its cl content reaches 0.5～1.5% (weight), generally in 1% (weight), catalyzer behind the oxychlorination enters the predrying district 44 of axial catalyst moving-bed under action of gravity.
The reaction bed temperature in predrying district 44 is generally about 530 ℃ between 510～550 ℃, and the residence time of catalyzer is 0.5～3 hour, is generally 1 hour.Linked to each other by catalyzer conduit 6 between predrying district and the chlorine oxidation zone, the bottom catalyzer of catalyzer conduit 6 is piled naturally and is ended, and can stop the chlorine-containing gas of chlorine oxidation zone 43 to enter predrying district 44.Catalyzer after predrying enters axial catalyst moving-bed calcining zone 45 through catalyzer conduit 7, the bottom catalyzer of catalyzer conduit 7 is piled naturally and is ended, can stop the high oxygen-containing gas of calcining zone 45 to enter predrying district 44, catalyzer is calcined through oxygen-containing gas in calcining zone 45, promotes that metal disperses at catalyst surface.
At calcining zone 45, reaction bed temperature is higher 10～60 ℃ than the bed temperature in predrying district 44, general high 30～40 ℃, local area pressure is to keep calcining zone 45 through managing the self-balancing pressure of 111 dechlorination oxidation zones, 43 oxygen-containing gas flows, than the slightly high 0.1～10kPa of chlorine oxidation zone 43, in local area, the residence time of catalyzer is 0.5～3 hour, is generally 1 hour.The oxygen level of the oxygen-containing gas through managing 114 introducing local areas is between 5～21% (moles), first drying heats with calcining well heater 13 before entering local area, and its temperature is as the criterion to keep reaction bed temperature, is generally 540～580 ℃, its water-content is not higher than 50ppm, generally below 20ppm.Oxygen-containing gas is drawn out of and all enters chlorine oxidation zone 43 through behind the beds.
The mode of above step gas circulation and processing is: introduce oxygen-containing gas from managing 114 in the calcining zone 45, oxygen-containing gas is through deriving from managing 111 behind the beds of calcining zone 45, annotate chlorine after chlorine-containing gas inlet tube 109 enters chlorine oxidation zone 43 by pipe 110, contacting the back with the beds of chlorine oxidation zone 43 is drawn by chlorine-containing gas outlet pipe 108, be mixed into dechlorination system 15 with the reprocessing cycle oxygen deprivation gas of deriving and after 10 heat exchange of reprocessing cycle interchanger, enter pipe 102 by scorch region 41, dehumidification system 17 dechlorinations, dry, after perhaps carrying out the dechlorination processing separately, be mixed into dehumidification system 17 with reprocessing cycle oxygen deprivation gas again, dechlorination system 15 is own, goes up or be provided with gas drain 16 as the dechlorinator after dechlorination system 15.The dry and cold regeneration recycle gas that comes out from dechlorination system 15, dehumidification system 17, its vapour content is lower than 100ppm, generally be lower than 50ppm, enter reprocessing cycle compressor 14 and boost through managing 116, be warming up to 350～470 ℃ with the reprocessing cycle oxygen deprivation gas heat exchange of coming out from revivifier then in reprocessing cycle interchanger 10, heat exchange is divided into two-way after heating up, and one the tunnel for burning gas, enter recirculation heater 11 through managing 105, heating enters scorch region 41 after manage 106; One the tunnel is predry pathogenic dryness, enter well heater 12 through managing 107, be heated between 510～550 ℃, be generally about 530 ℃, enter predrying district 44 through managing 112 afterwards, carry out predryingly to the catalyzer with oxychlorination of burning, turn back to the overheated zone 42 of scorch region 41 bottoms from crossing hot gas conduit 115 then, and then enter the resurgent gases circulation loop from chlorine oxidation zone 43.
Catalyzer after the calcining leaves revivifier by revivifier 1 bottom through catalyst outlet 8, enters reactive system after the degassing, reduction, the next circulation of beginning.
The present invention shown in Figure 1, be provided with buffer zone 40 above scorch region 41, this is in order to realize catalyzer moving continuously in revivifier better, to realize strict cyclic regeneration, certainly there is not this buffer zone to be fine, this existing in the prior art successful application yet.
Claims (4)
1. the renovation process of a hydrocarbon conversion catalyst, described catalyzer contains a kind of carrier, the halogen of at least a catalytically-active metals and certain content, the particle diameter of catalyzer is between 0.5～5.0mm, in reaction process, catalyst surface is because of the carbon deposit inactivation, and its regeneration step comprises:
A) reclaimable catalyst enters the radially moving-bed of catalyst scorch region (41) of revivifier (1), and contains the carbon deposit that the oxygen regeneration gas contacts the burning-off catalyst surface;
B) catalyzer after burning enters axial catalyst moving-bed chlorine oxidation zone (43) under action of gravity, contacts with chlorine-containing gas and carries out oxychlorination;
C) catalyzer behind the oxychlorination enters the predrying district of axial catalyst moving-bed (44) under action of gravity, carries out predrying under high temperature, the effect of exsiccant predry pathogenic dryness;
D) catalyzer after predrying enters axial catalyst moving-bed calcining zone (45) under action of gravity, calcine under the oxygen-containing gas effect;
E) catalyzer after the calcining leaves revivifier by revivifier (1) bottom, after the degassing, reduction are handled, enters reactive system and begins next circulation;
In the above step a)～d), the mode of gas circulation and processing is: introduce oxygen-containing gas in the calcining zone (45), derive behind the beds of oxygen-containing gas through calcining zone (45), enter chlorine oxidation zone (43) after annotating chlorine, with draw after the beds of chlorine oxidation zone (43) contacts, be mixed into dechlorination system (15) with the reprocessing cycle oxygen deprivation gas of deriving by scorch region (41), dehumidification system (17) dechlorination, dry, perhaps carry out separately being mixed into dehumidification system (17) with reprocessing cycle oxygen deprivation gas again after dechlorination is handled, gas mixture after the processing is divided into two-way, one the tunnel for burning gas, enter scorch region (41) after the heating, one the tunnel is predry pathogenic dryness, enter predrying district (44) after the heating, with the overheated zone (42) that returns scorch region (41) bottom after catalyzer contacts, and then enter the resurgent gases circulation loop, described dechlorination system (15) itself, on the dechlorinator, perhaps be provided with gas drain (16) afterwards in described dechlorination system (15).
2. according to the renovation process of the described hydrocarbon conversion catalyst of claim 1, it is characterized in that,
A) in scorch region (41), the treatment condition of catalyzer are: pressure is between 0.35～1.5MPa, the residence time of catalyzer is between 0.5～3.0 hour, catalyst coke content is in 0.01～10 weight % scope, the temperature in of burning gas is between 400～500 ℃, oxygen level between 0.4～1.0 mole of %, the beds top temperature be controlled at make local area and chlorine oxidation zone (43), calcining zone (45) bed temperature all under support of the catalyst top temperature allowed to bear;
B) in chlorine oxidation zone (43), the treatment condition of catalyzer are: the bed temperature of chlorine oxidation zone (43) is between 510～540 ℃, pressure equates or lower slightly 5～10kPa with scorch region (41), catalyzer is 1～3 hour in this residence time, introduce the chlorine-containing gas temperature in of chlorine oxidation zone (43) between 510～550 ℃ through pipe (109), cl content is between 0.1～1.0 weight %, and oxygen level is between 3～21 moles of %;
C) in predrying district (44), the treatment condition of catalyzer are: the bed temperature of predrying district (44) is between 510～550 ℃, and the residence time of catalyzer is between 0.5～3 hour;
D) in calcining zone (45), the treatment condition of catalyzer are: bed temperature is higher 10～60 ℃ than the bed temperature of predrying district (44), local area pressure is to keep the self-balancing pressure of calcining zone (45) through pipe (111) dechlorination oxidation zone (43) oxygen-containing gas flow, the residence time of catalyzer is 0.5～3 hour, the oxygen level of the oxygen-containing gas through managing (114) introducing local area is between 5～21 moles of %, oxygen-containing gas is drawn out of and all enters chlorine oxidation zone (43) through behind the beds.
3. reclaim equiment of realizing the described renovation process of claim 1, this equipment comprises scorch region (41), chlorine oxidation zone (43), predrying district (44) and calcining zone (45) from top to bottom successively, wherein, the bottom of scorch region (41) is overheated zone (42), there was hot gas conduit (115) to link to each other between predrying district (44) and overheated zone (42), between scorch region (41) and the chlorine oxidation zone (43), between chlorine oxidation zone (43) and predrying district (44), between predrying district (44) and the calcining zone (45), have only the catalyzer conduit to be connected.
4. according to the reclaim equiment of the described renovation process of claim 3, it is characterized in that scorch region (41) top is provided with buffer zone (40).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00101537A CN1100852C (en) | 2000-01-10 | 2000-01-10 | Process for regenerating hydrocarbon-transforming catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00101537A CN1100852C (en) | 2000-01-10 | 2000-01-10 | Process for regenerating hydrocarbon-transforming catalyst |
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| Publication Number | Publication Date |
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| CN1298924A CN1298924A (en) | 2001-06-13 |
| CN1100852C true CN1100852C (en) | 2003-02-05 |
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| CN00101537A Expired - Lifetime CN1100852C (en) | 2000-01-10 | 2000-01-10 | Process for regenerating hydrocarbon-transforming catalyst |
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102007006647A1 (en) * | 2007-02-06 | 2008-08-07 | Basf Se | Process for the regeneration of a catalyst bed deactivated in the context of a heterogeneously catalyzed partial dehydrogenation of a hydrocarbon |
| CN105562124A (en) * | 2014-10-10 | 2016-05-11 | 中石化广州工程有限公司 | High-carbon spent catalyst continuous regeneration method |
| CN105498859A (en) * | 2014-10-10 | 2016-04-20 | 中石化广州工程有限公司 | Scorching method for regenerating catalyst for preparing propylene from methanol in moving bed |
| CN105983453B (en) * | 2015-02-12 | 2018-10-16 | 天津海成能源工程技术有限公司 | A kind of catalyst regeneration system using anhydrous regeneration gas |
| CN109261223B (en) * | 2018-10-24 | 2021-06-15 | 西南大学 | Catalyst regeneration chlorinator for chemical industry experiments |
| CN117323921B (en) * | 2023-12-01 | 2024-02-27 | 中控技术股份有限公司 | Method and system for controlling oxygen content of regeneration reactor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4578370A (en) * | 1985-04-25 | 1986-03-25 | Uop Inc. | Gas circulation method for moving bed catalyst regeneration zones |
| CN1034320A (en) * | 1987-12-21 | 1989-08-02 | 法国精制和总分配公司 | The method and apparatus of regenerating catalyst in fluidized bed |
| CN1082591A (en) * | 1992-04-01 | 1994-02-23 | 欧洲催化剂加工公司 | The catalyst presulfurizing method of processing hydrocarbons |
-
2000
- 2000-01-10 CN CN00101537A patent/CN1100852C/en not_active Expired - Lifetime
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4578370A (en) * | 1985-04-25 | 1986-03-25 | Uop Inc. | Gas circulation method for moving bed catalyst regeneration zones |
| CN1034320A (en) * | 1987-12-21 | 1989-08-02 | 法国精制和总分配公司 | The method and apparatus of regenerating catalyst in fluidized bed |
| CN1082591A (en) * | 1992-04-01 | 1994-02-23 | 欧洲催化剂加工公司 | The catalyst presulfurizing method of processing hydrocarbons |
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| CN1298924A (en) | 2001-06-13 |
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