CN103228357B - The method of regenerate zeolites catalyst - Google Patents
The method of regenerate zeolites catalyst Download PDFInfo
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- CN103228357B CN103228357B CN201180057262.6A CN201180057262A CN103228357B CN 103228357 B CN103228357 B CN 103228357B CN 201180057262 A CN201180057262 A CN 201180057262A CN 103228357 B CN103228357 B CN 103228357B
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/7007—Zeolite Beta
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/40—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11, as exemplified by patent documents US3702886, GB1334243 and US3709979, respectively
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/7034—MTW-type, e.g. ZSM-12, NU-13, TPZ-12 or Theta-3
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/7046—MTT-type, e.g. ZSM-23, KZ-1, ISI-4 or EU-13
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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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/70—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65
- B01J29/72—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of types characterised by their specific structure not provided for in groups B01J29/08 - B01J29/65 containing iron group metals, noble metals or copper
- B01J29/74—Noble metals
- B01J29/7469—MTW-type, e.g. ZSM-12, NU-13, TPZ-12 or Theta-3
-
- 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
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/90—Regeneration or reactivation
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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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- Crystallography & Structural Chemistry (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
According to the present invention, provide the renovation process of the catalyst for hydroconversion process.In some embodiments, described method comprises the reproducer comprising " original position " oxygen calcination controlled in described process reactor.
Description
The cross reference of related application
This application claims the priority of the U.S. Provisional Patent Application numbers 61/418,212 submitted on November 30th, 2010, its disclosure is all incorporated herein by reference.
Invention field
The present invention relates to the regeneration of zeolite catalyst.
Background of invention
Many hydroconversion process, such as light olefin is to the conversion of more higher alkene, and oxygenate is to the conversion of gasoline, and methylated aromatic compounds is to the disproportionation of dimethylbenzene and transalkylation, with propylene to the hydration of isopropyl alcohol and Di Iso Propyl Ether, zeolite catalyst is advantageously used to carry out.Such catalyst comprises ZSM-5, β, ZSM-12, ZSM-23, modenite, and one or more in other zeolite, and described zeolite can have one or more metals with its combination, and such as so-called noble metal is as platinum.In technical process, these catalyst accumulation coke, such as, to about 30wt% or even higher level, cause significant inactivation.Depend on described technique and catalyst, the zeolite catalyst of such inactivation can be reproduced, at least to a certain extent.Typically, described inactivation and regeneration cycle occur, and one-period is in the level of many years to several moon or even a couple of days.
United States Patent (USP) 6,380, has set forth a kind of such regeneration techniques in 119.
One of problem run in described inactivation and regeneration cycle is, if use oxygen/noble gas mixtures to burn coke, significant permanent deactivation may occur because of steam treatment at elevated temperatures.The present inventor has been found that a kind of method of regenerate zeolites, and the method alleviates hydro-thermal steam inactivation.
Summary of the invention
The present invention relates to the regeneration of zeolite catalyst.
In one embodiment, described renovation process alleviates hydro-thermal steam inactivation.
In one embodiment, described zeolite catalyst comprises one or more metals.
In one embodiment, described hydroconversion process comprises the first hydrocarbon feed stream is being enough to transform described first feed stream to the second and contacting under the condition of different feed streams from the fixed bde catalyst comprising at least one zeolite.
In one embodiment, described feed stream comprises non-aromatic hydrocarbons, aromatic hydrocarbon, and containing be selected from the one or more heteroatomic hydrocarbon of oxygen, sulphur, nitrogen and their mixture one or more.
In one embodiment, described catalyst comprises and is selected from ZSM-5, β, ZSM-12, ZSM-23, one or more the zeolite in modenite.
In one embodiment, described catalyst comprises one or more metals, preferably includes at least one noble metal, at least one more preferably in platinum, palladium, rhodium, ruthenium.In a further preferred embodiment, one or more metals described are selected from copper, silver, tin and their mixture, optionally also containing at least one noble metal.
An object of the present invention is by providing the renovation process of improvement to improve and/or extending catalyst inactivation and regeneration cycle, wherein one or more metals to be incorporated in described catalyst or on described catalyst when, reduce the agglomeration of one or more metals described, this improves described catalyst at hydrocarbon, one or more instructions of the activity particularly in aromatic hydrocarbon method for transformation.
Another object of the present invention allows the life-span of described catalyst (process cycles number) to be lengthened to exceed by using with regard to temperature and water partial pressure more harsh other program (ex situ and other program) obtainable life-span.
With reference to following detailed description, preferred embodiment, embodiment and appended claims, these and other objects, feature and advantage will become apparent.
Describe in detail
According to the present invention, provide the method for regeneration for the catalyst of hydroconversion process.
In some embodiments, described method comprises the reproducer comprising " original position " oxygen calcination controlled in described process reactor.The strict control of described " original position " aspect allowable temperature, water partial pressure and oxygen content.The detail of described program is appreciated that by reference to following detailed explanation and specific embodiment.Grasp and of the present disclosurely it will be understood by those skilled in the art that described method can be put into practice to be different from the following concrete mode set forth herein.
(1) when described system not hydrocarbonaceous and water time, original position causes the oxygen calcination of described catalyst.The temperature of reactor should be low, about 650-700 °F/340-370 ° C, adopts oxygen content in the gas of 0.5 volume % (all the other are nitrogen) in the porch of reactor beds.In some embodiments, effluent separator should run at alap temperature, consistent with the temperature of described entire system, and the water of accumulation is regularly got rid of.In preferred embodiments, recyclegas also can pass through mole sieve drier, but this is optional.Described regeneration is carried out under 50-200psig.Temperature rise not should more than 100 °F/55 ° of C (less temperature rise is better), and by by regulate described reactor inlet oxygen content control.Dry air is incorporated in reactor feed gas, to regulate entrance oxygen content.Described regeneration is carried out, and does not have oxygen or in exit gas, has the entrance oxygen content of certain mark simultaneously at reactor exit.Described entrance regeneration gas charging rate is about 0.5 to 2.0NM
3/ hr/kg catalyst.
(2) when exit gas reaches the inlet gas oxygen concentration of 70-80%, the inlet temperature of described bed is brought up to about 750 °F/400 ° C.Entrance oxygen content is remained on 0.5% volume.The main body of coke calcination should occur in step (1) and (2).
(3) when exit gas reaches the inlet gas oxygen concentration of 70-80% again, entrance oxygen concentration is increased to 1.0 volume %, and inlet temperature is remained on 750 °F/400 ° C (but, if lower temperature support is burnt substantially, the i.e. oxygen consumption of about 50% or more, described inlet temperature can be lowered).Do not allow any bed tempertaure more than 850 °F/450 ° of C, if need to reduce reactor inlet oxygen content to reduce any hot(test)-spot temperature.
(4) when exit gas reaches the inlet gas oxygen concentration of 70-80% again, described bed inlet temperature is increased to 800 °F/425 ° C, keeps oxygen content in the inlet gas of 1 volume % simultaneously.Now, described regeneration should be almost complete, wherein burnt significantly beyond the coke of 90%, and temperature rise should be low.Do not allow any bed tempertaure more than 850 °F/450 ° of C, if need to reduce reactor inlet oxygen content to reduce any hot(test)-spot temperature.
(5) when described exit gas reaches the inlet gas oxygen concentration of 90-100%; temperature is increased to 850 °F/450 ° C; if purification of combustion wishes that (this may be unnecessary completely; especially for large pore zeolite as ZSM-12; β, modenites etc., because burned significantly beyond the coke of 90%; and remaining coke can provide some to prevent the protection of steam inactivation and metal function sintering in a small amount), otherwise directly proceed to next step.Now heat release should be no longer included.Entrance oxygen content can be increased to 7 volume % further, complete to guarantee described calcination.In some embodiments, should not allow described bed tempertaure more than 850 °F/450 ° of C, and in order to this object, if need to reduce reactor inlet oxygen content, to reduce any hot(test)-spot temperature.
Now described regeneration is done, and temperature of reactor should be reduced to 600-700 °F, purges out oxygen with drying nitrogen, and for carrying out ready for operation according to the starting order that catalyst that is fresh or regeneration is used for correlation technique.
Importantly, the described regeneration temperature low as far as possible (that is, only when oxygen just increases temperature when (70 volume %) breaks through in fact, not increasing temperature before this) when coke is burned.Object removes most of coke under possible minimum temperature.Typically, in regeneration, once oxygen starts to break through, operator starts raised temperature immediately to realize the highest burn rate, and we have found that this makes described catalyst be exposed to more water at relatively high temperatures.Although the inventive method needs the calcination time slightly grown, it carries out under lower mean temperature, decreases inactivation, because the impact of temperature on inactivation is index, and time effects is linear.Described new method also reduces described catalyst vapor partial pressure run at relatively high temperatures, because the coke of rich hydrogen be allowed to described catalyst at lower temperature comparatively early time burn (particularly when described separator is by frequent draining, be maintained at low temperature, and if use recirculating gas gas dryer time).
Summarize below be aromatic compounds transalkylation catalyst (Pt-ZSM-12,0.1wt%Pt top bed and HZSM-5 bottom bed) pilot-plant regeneration result.As by as shown in processing performance and catalyst characterization performance, the regeneration latter two catalyst of about 32 % by weight coke regains the almost duplicate activity with fresh catalyst on a catalyst.
Catalyst sorption capacity before and after the regeneration of TransPlus reactor and active (alpha test) are shown in table 1 below.Described alpha test is described in United States Patent (USP) 3, and 354,078 and JournalofCatalysis, 4,527 (1965); 6,278 (1966); With 61, in 395 (1980).The experiment condition of described test used herein comprises steady temperature and the changeable flow of 538 ° of C, as at JournalofCatalysis, describes in detail in 61,395 (1980).Described test can be repeated to ± 10% by those skilled in the art.
Table 1
Hexane absorbs according to United States Patent (USP) 6,048,816 and 6, and 046, the program determination described in 372.
Give in table 2 before being regenerated below and the other characteristic of described catalyst afterwards.
Table 2
As seen in the table, specificity of catalyst and processing performance all confirm that described renovation process successfully almost recovers fresh activity completely.Almost identical with the rate of ageing (about 3.6 ° of C/ months) of fresh catalyst at described regenerated catalyst rate of ageing (about 3.4 ° of C/ months), hydrogen consumption also indicates the recovery completely of metal function.Described catalyst aging rate maintains the increase instruction of the temperature required by constant conversion.
The order of step is important.Described O was raised before the coke burning appropriate amount at a lower temperature
2concentration can cause too high bed tempertaure change, and this promotes inactivation.
After explaining the present invention so in detail in conjunction with specific embodiments, grasp of the present disclosure those skilled in the art will recognize that, those skilled in the art can make various other and change when not deviating from the spirit and scope of the present invention, and the present invention can be implemented by the mode set forth to be different from upper mask body.
The trade name used in this article by
tMsymbol or
symbol indicates, and represent that described title may be protected by some trade mark right, such as they may be the registration marks in various judicial power.The all patents quoted herein and patent application, test program and other file are fully incorporated herein by reference to so open not inconsistent with the present invention degree, and the whole authorities be allowed in order to this introducing.When listing numerical lower limits and numerical upper limits in this article, the scope from any lower limit to any upper limit is conceived.
Claims (9)
1., for regenerating the method for the zeolite catalyst that can be used for hydroconversion process, wherein said renovation process comprises oxygen calcination to remove the coke deposited in described hydroconversion process process over the catalyst, and described renovation process comprises:
(i) in the fixed bed comprising described zeolite catalyst, measure at reactor inlet place, under the average reactor temperature that is not more than 370 DEG C, measure at the gas access place of reactor beds, 0.5 volume %O
2with under the atmosphere of balance inert gas, start oxygen calcination, prerequisite selects to comprise the condition of oxygen flow and gross pressure, make along on any point of described reactor beds not more than the temperature rise of 55 DEG C; Then
(ii) as the O of exit gas
2content reaches described inlet gas O
2during 70 volume % or larger of content, the inlet temperature of described bed is raised, but is increased to and is not more than 400 DEG C, and prerequisite is alternative condition, and making is not having temperature more than 450 DEG C along on any point of described reactor beds; Then
(iii) as the O of exit gas
2content reaches described inlet gas O
2during 70 volume % or larger of content, the O of described entrance
2content is raised to 1.0 volume %, keeps described reactor inlet temperature to be not more than 400 DEG C simultaneously, and prerequisite selects to comprise the condition of oxygen flow and gross pressure, makes do not having temperature more than 450 DEG C along on any point of described reactor beds; Then
(iv) as the O of exit gas
2content reaches described inlet gas O
2during 70 volume % or larger of content, the gas inlet temperature of described bed is raised, but is increased to and is not more than 425 DEG C, keeps the O of described entrance simultaneously
2content is at 1.0 volume %, and prerequisite selects to comprise the condition of oxygen flow and gross pressure, makes do not having temperature more than 450 DEG C along on any point of described reactor beds; Then
V () is as the O of exit gas
2content reaches described inlet gas O
2during 90 volume % or larger of content, the gas inlet temperature of described bed is raised, but is increased to and is not more than 450 DEG C, keeps the O of described entrance simultaneously
2content is at 1.0 volume %, and prerequisite selects to comprise the condition of oxygen flow and gross pressure, makes do not having temperature more than 450 DEG C along on any point of described reactor beds; Then
(vi) described entrance O is raised
2content is to 6-8 volume %, and prerequisite selects to comprise the condition of oxygen flow and gross pressure, makes do not having temperature more than 450 DEG C along on any point of described reactor beds; Then
(vii) reduce reactor inlet temperature to 370 DEG C or lower, and remove O
2charging, under making described bed be in inert atmosphere;
(viii) progress of starting sequence being used for described method according to catalyst that is fresh or regeneration carries out, and starts or continue described hydroconversion process.
2. the process of claim 1 wherein that described hydroconversion process comprises the first hydrocarbon feed stream and is being enough to transform described first hydrocarbon feed stream to the second and contacting under the condition of different feed streams from the fixed bde catalyst comprising at least one zeolite.
3. the method for claim 2, wherein said first hydrocarbon feed stream comprises non-aromatic hydrocarbons, aromatic hydrocarbon, and containing be selected from the one or more heteroatomic hydrocarbon of oxygen, sulphur, nitrogen and their mixture one or more.
4. the method any one of claim 1-3, wherein said hydroconversion process is selected from the conversion of light olefin to more higher alkene, oxygenate is to the conversion of gasoline, and methylated aromatic compounds is to the disproportionation of dimethylbenzene and/or transalkylation, and propylene is to the hydration of isopropyl alcohol and Di Iso Propyl Ether.
5. the method any one of claim 1-3, wherein said zeolite catalyst comprises and is selected from ZSM-5, β, ZSM-12, ZSM-23, one or more the zeolite in modenite.
6. the method any one of claim 1-3, wherein said zeolite catalyst also comprises one or more metals.
7. the method any one of claim 1-3, wherein said zeolite catalyst comprises at least one metal being selected from platinum, palladium, rhodium and ruthenium.
8. the method any one of claim 1-3, wherein said zeolite catalyst comprises one or more metals being selected from copper, silver, tin and their mixture.
9. the method any one of claim 1-3, wherein said fixed bed comprises containing the first zeolite and optionally contains the first zeolite catalyst of at least one metal, and comprise the second zeolite and optionally containing the second zeolite catalyst of at least one metal, with the kind of wherein said first zeolite catalyst at described zeolite, or the presence or absence of described metal, or in the kind aspect of described metal if present, at least one aspect is different from described second zeolite catalyst.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US41821210P | 2010-11-30 | 2010-11-30 | |
| US61/418,212 | 2010-11-30 | ||
| PCT/US2011/056904 WO2012074613A1 (en) | 2010-11-30 | 2011-10-19 | Method of regenerating zeolite catalyst |
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| CN103228357A CN103228357A (en) | 2013-07-31 |
| CN103228357B true CN103228357B (en) | 2016-03-23 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014193563A1 (en) | 2013-05-31 | 2014-12-04 | Exxonmobil Chemical Patents Inc. | Transalkylation system |
| US9963403B2 (en) | 2014-10-27 | 2018-05-08 | Exxonmobil Chemical Patents Inc. | Process and apparatus for the conversion of hydrocarbons |
| WO2016099618A1 (en) | 2014-12-19 | 2016-06-23 | Exxonmobil Chemical Patents Inc. | Sulfiding process for aromatic transalkylation |
| CN112619629A (en) * | 2020-12-25 | 2021-04-09 | 青岛华世洁环保科技有限公司 | Runner regeneration method |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4300014A (en) * | 1980-08-04 | 1981-11-10 | Teijin Petrochemical Industries Ltd. | Process for isomerization of xylene |
| US4480144A (en) * | 1981-08-06 | 1984-10-30 | Mobil Oil Corporation | Regeneration of aromatics processing catalysts |
| US4876408A (en) * | 1986-12-19 | 1989-10-24 | Union Oil Company Of California | Alkylation process using a catalyst having an increased selectivity for monoalkylation |
| US6114265A (en) * | 1994-03-15 | 2000-09-05 | Exxon Research And Engineering Company | Combustion control in a fluid catalytic cracking regenerator |
| US6380119B1 (en) * | 1997-06-06 | 2002-04-30 | Basf Aktiengesellschaft | Method for regenerating a zeolitic catalyst |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3354078A (en) | 1965-02-04 | 1967-11-21 | Mobil Oil Corp | Catalytic conversion with a crystalline aluminosilicate activated with a metallic halide |
| US6048816A (en) | 1996-10-02 | 2000-04-11 | Mobil Oil Corporation | Catalyst and process for converting methanol to hydrocarbons |
| US6046372A (en) | 1996-10-02 | 2000-04-04 | Mobil Oil Corporation | Process for producing light olefins |
| US6987078B2 (en) * | 2003-10-03 | 2006-01-17 | Fina Technology, Inc. | Alkylation and catalyst regenerative process |
| US20090143218A1 (en) * | 2007-12-03 | 2009-06-04 | Bogdan Paula L | Regeneration process for a c8 alkylaromatic isomerization catalyst |
-
2011
- 2011-10-19 WO PCT/US2011/056904 patent/WO2012074613A1/en active Application Filing
- 2011-10-19 CN CN201180057262.6A patent/CN103228357B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4300014A (en) * | 1980-08-04 | 1981-11-10 | Teijin Petrochemical Industries Ltd. | Process for isomerization of xylene |
| US4480144A (en) * | 1981-08-06 | 1984-10-30 | Mobil Oil Corporation | Regeneration of aromatics processing catalysts |
| US4876408A (en) * | 1986-12-19 | 1989-10-24 | Union Oil Company Of California | Alkylation process using a catalyst having an increased selectivity for monoalkylation |
| US6114265A (en) * | 1994-03-15 | 2000-09-05 | Exxon Research And Engineering Company | Combustion control in a fluid catalytic cracking regenerator |
| US6380119B1 (en) * | 1997-06-06 | 2002-04-30 | Basf Aktiengesellschaft | Method for regenerating a zeolitic catalyst |
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| WO2012074613A1 (en) | 2012-06-07 |
| CN103228357A (en) | 2013-07-31 |
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