CN107282078A - Dehydrogenation of isobutane catalyst and preparation method thereof and dehydrogenating technology - Google Patents
Dehydrogenation of isobutane catalyst and preparation method thereof and dehydrogenating technology Download PDFInfo
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- CN107282078A CN107282078A CN201610192871.7A CN201610192871A CN107282078A CN 107282078 A CN107282078 A CN 107282078A CN 201610192871 A CN201610192871 A CN 201610192871A CN 107282078 A CN107282078 A CN 107282078A
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/28—Regeneration or reactivation
- B01J27/32—Regeneration or reactivation of catalysts comprising compounds of halogens
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0205—Impregnation in several steps
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
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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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/16—Reducing
- B01J37/18—Reducing with gases containing free hydrogen
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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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- 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
- C07C5/327—Formation of non-aromatic carbon-to-carbon double bonds only
- C07C5/333—Catalytic processes
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2527/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- C07C2527/06—Halogens; Compounds thereof
- C07C2527/135—Compounds comprising a halogen and titanum, zirconium, hafnium, germanium, tin or lead
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- 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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Abstract
The present invention relates to catalytic dehydrogenation technical field, and in particular to a kind of dehydrogenation of isobutane catalyst and preparation method thereof and dehydrogenating technology.The preparation method comprises the following steps：Step 1: preparing appropriate platinum group metal dipping solution, add among carrier, impregnate under negative pressure, by the carrier impregnated drying, roasting；Step 2: preparing the first appropriate auxiliary agent dipping solution, add among the carrier handled by step one, impregnate under negative pressure, by carrier drying, the roasting after dipping；Step 3: preparing the second appropriate auxiliary agent dipping solution, add among the carrier handled by step 2, impregnate under negative pressure, by carrier drying, the roasting after dipping；Step 4: step one, which is repeated several times, arrives step 3, dehydrogenation of isobutane catalyst is obtained.Using infusion process by the load of the multiple substep of active component on a catalyst, the distribution of active component evenly can be made on a catalyst, make catalyst activity it is higher, more stable.
Description
Technical field
The present invention relates to catalytic dehydrogenation technical field, and in particular to a kind of dehydrogenation of isobutane catalyst and its preparation
Method, and the dehydrogenating technology of isobutene is prepared using the catalyst by dehydrogenation of isobutane.
Background technology
Liquefied petroleum gas (LPG) is the byproduct of catalytic cracking unit and steam cracking device.At present, portion big absolutely
Divide liquefied petroleum gas to both function as cheap civil liquefied gas, make a low multiple use, value is not also closed
Reason exploitation.With " implementation of West-east Gas and civil natural gas pipeline engineering, clean and effective and heat profit
It must replace the fuel market of liquefied gas with the high natural gas of rate, originally superfluous refinery's liquefied gas occur
Further overstock and cause surplus.Therefore, C4 alkene and iso-butane in making use of liquefied petroleum gas pass through alkyl
It is a kind of effective way for developing liquefied petroleum gas to change reaction generation high-knock rating gasoline, there is splendid industry
Prospect and economic benefit.
In liquefied petroleum gas, normal butane accounts for 10%, but normal butane hardly participates in alkylated reaction；If
Alkene normal butane dehydrogenation can be made, then high-knock rating gasoline is generated by alkylated reaction, then liquefaction stone
Oil gas utilization ratio will be greatly improved.
In Chinese patent 102794167A, " dehydrogenation of isobutane prepares different isobutene used catalyst and its preparation side
A kind of catalyst reacted suitable for dehydrogenation of isobutane and preparation method thereof is disclosed in method "；In Chinese patent
It is public in 102211972A " hydrotalcite loaded catalyst is in the purposes during dehydrogenation of isobutane prepares different isobutene "
Opened it is a kind of prepare the catalyst of isobutene for dehydrogenation of isobutane, can obtain higher iso-butane conversion ratio and
Selective isobutene；Chinese patent 10186266913B " dehydrogenation of isobutane prepare isobutene catalyst and its
One kind is disclosed in preparation method " has higher iso-butane conversion ratio, higher isobutyl under the conditions of high-temperature low-pressure
Catalyst of alkene selectivity and reaction stability and preparation method thereof；European patent EP 2712674 (A1) " alkane
Disclosed in the composition of hydrocarbon dehydrogenation " in a kind of catalyst for low-carbon alkanes, patent and describe load
The preparation method of body and catalyst, and the catalyst is tested applied to dehydrogenation of isobutane, obtain higher different
Butanes conversion and selective isobutene." dehydrogenation of isobutane produces isobutene use to Chinese patent 102000593B
One kind is disclosed in catalyst, its preparation method and dehydrogenating technology " and uses infusion process by whole active components one
It is secondary to be supported on supported catalyst.Above-mentioned catalyst and preparation method effectively increase catalyst activity and different
Butanes conversion, but usage cycles are shorter, catalyst stability is relatively low, influence production efficiency.
The content of the invention
An object of the present invention is to provide a kind of preparation method of dehydrogenation of isobutane catalyst, using dipping
The load of the multiple substep of active component on a catalyst, can urge active component being distributed in evenly by method
In agent, make active higher, the more stable, service life of catalyst longer.
To realize above-mentioned technical purpose, the present invention uses following technical scheme：
The preparation method of dehydrogenation of isobutane catalyst, comprises the following steps：
Step 1: preparing appropriate platinum group metal dipping solution, the platinum group metal dipping solution prepared is added
Enter among the carrier after shaping, impregnate under negative pressure, the carrier impregnated is dried at a proper temperature,
Roasting；
Step 2: preparing the first appropriate auxiliary agent dipping solution, the first auxiliary agent dipping solution prepared is added
Enter among the carrier handled by step one, impregnate under negative pressure, by the carrier after dipping at a proper temperature
Drying, roasting；
Step 3: preparing the second appropriate auxiliary agent dipping solution, the second auxiliary agent dipping solution prepared is added
Enter among the carrier handled by step 2, impregnate under negative pressure, by the carrier after dipping at a proper temperature
Drying, roasting；
Step 4: step one, which is repeated several times, arrives step 3, using infusion process bearing the multiple substep of active component
It is loaded on carrier, obtains dehydrogenation of isobutane catalyst.
In above-mentioned steps, heat-resistant oxide is used for carrier, using platinum group as major catalyst, with
IVth A races element is that the first auxiliary agent, alkali metal or alkaline-earth metal are the second auxiliary agent, using halogen as modifying agent；
Above-mentioned active component (at least twice) is impregnated on carrier several times using incipient impregnation；Impregnate every time
When, carrier impregnates 1~10 hour under negative pressure -0.01~-0.08MPa；Every time the carrier after dipping 80~
Dry 5~20 hours, be preferred with 110~120 DEG C, 10~15 hours under the conditions of 180 DEG C；Load after drying
Body is calcined 2~15 hours under the conditions of 400~600 DEG C.
Wherein, the heat-resistant oxide used in the present invention is aluminum oxide (γ-Al2O3), silica (Si02)
With the mixture of one or both of Si-Al molecular sieve any of the above ratio, with aluminum oxide (γ-Al2O3)
It is preferred.
Major catalyst used in the present invention is platinum group metal, including ruthenium (Ru), rhodium (Rh), palladium (Pd), osmium
(Os), iridium (Ir), platinum (Pt) one or more of metals therein, wherein with metal platinum (Pt) and palladium
(Pd) it is preferred；
The first auxiliary agent used in the present invention is the IVth A races metal element, including germanium (Ge), tin (Sn), lead (Pb)
One or more of metals therein, wherein being preferred with metallic tin (Sn)；
The second auxiliary agent used in the present invention is alkali and alkaline earth metal ions, including lithium (Li), sodium (Na), potassium
(K), rubidium (Rb), caesium (Cs), francium (Fr) one or more of metals therein, wherein with metallic potassium (K)
It is preferred with sodium (Na).
The predecessor of each metalloid element of the present invention be the chloride containing metal component, nitrate,
Carbonate or hydroxide, the available corresponding acid of halogen, wherein being preferred with hydrochloric acid.
Another object of the present invention is to provide using dehydrogenation of isobutane catalyst made from the above method, into
In product catalyst, on the basis of carrier quality, the weight/mass percentage composition of platinum group metal is 0.15~0.5wt%,
The weight/mass percentage composition of IVth A races metal element is 0.5~2wt%, the quality percentage of alkali and alkaline earth metal ions
Content is 0.15~5wt%, and halogen content is 0.01-5wt%.
Wherein, the mol ratio of the IVth A races element and platinum group is 1:1~6, preferably 1:1~3.
Present invention also offers the dehydrogenating technology of the preparing isobutene through dehydrogenation of iso-butane using above-mentioned catalyst, catalysis
Dehydrogenation reaction can use fluid bed, moving bed, fixed bed reactors, be preferred with fixed bed, using hydrogen to be dilute
Release agent；The reaction temperature of catalytic dehydrogenation is 400~700 DEG C, and reaction pressure is normal pressure~1Mpa, gaseous mass
Air speed is 0.1~10h-1。
Wherein, charging proportioning：Gas mole ratio is iso-butane：Hydrogen=1:0.1~10, preferably 1:0.1~5.
In addition, the catalyst has pretreatment and regeneration step, the pretreatment is in 300~500 DEG C of hydrogen
Reduced 1~10 hour in stream, wherein being preferred with 2~4 hours；It is regenerated as existing the catalyst tied carbon and inactivated
Burnt under air atmosphere, temperature is burnt for 250~500 DEG C, wherein being preferred with 300~450 DEG C.After burning
Oxychlorination updates catalyst again, active component is disperseed again.
Compared with prior art, the present invention has following features：
(1) each active component is supported on carrier using multiple step impregnation method, is conducive to improving each activity
Decentralization and the uniformity of the component on carrier, so that the activity and selectivity of catalyst is improved, and conversion
Rate is high, service life can also increase.
(2) using hydrogen as diluent, beneficial to raising iso-butane conversion ratio, while coking amount is reduced,
Extend the service cycle of catalyst.
(3) catalyst inactivated because tying carbon is regenerated using air burn mode, and method is simple, effective.
Embodiment
With reference to specific embodiment, the present invention is expanded on further.In the following detailed description, only pass through
The mode of explanation describes some one exemplary embodiments of the present invention.Associated description is inherently illustrative,
It is not intended to limit the scope of the claims.
Embodiment 1
(1) alumina support for weighing a certain amount of shaping is put into impregnating equipment；
(2) a certain amount of chloroplatinic acid H is weighed2PtCl6(in terms of 0.15%Pt), with appropriate diluted hydrochloric acid dissolution
Afterwards, it is added in carrier, is impregnated under negative pressure -0.07MPa 1 hour, 10 are then dried at 110 DEG C small
When, 500 DEG C are calcined 4 hours under air atmosphere；
(3) appropriate butter of tin SnCl is weighed4(in terms of 0.35%Sn), it is water-soluble with appropriate deionization
Xie Hou, adds the carrier that step (2) is obtained, is impregnated 1 hour under negative pressure -0.07MPa, then at 110 DEG C
Lower drying 10 hours, 500 DEG C are calcined 4 hours under air atmosphere；
(4) appropriate potassium chloride (in terms of 0.5%K) is weighed, after appropriate deionized water dissolving, step is added
Suddenly the carrier that (3) are obtained, impregnates 1 hour under negative pressure -0.07MPa, 10 is then dried at 110 DEG C
Hour, 500 DEG C are calcined 4 hours under air atmosphere；
(5) carrier that processing is obtained by step (4) is repeated once according to step (2) to step (4),
Obtain catalyst A.The catalyst components content Pt 0.3wt%, Sn 0.7wt%, K 1.0wt%, Cl
1.73wt%.
10ml catalyst A is fitted into fixed bed reactors, reduced 1 hour in 500 DEG C of hydrogen streams,
Dehydrogenation reaction is carried out under conditions of 560 DEG C of reaction temperature, reaction pressure 0.1MPa.Feed composition mol ratio is different
Butane：Hydrogen=1：1, mass space velocity 2h-1.Catalyst A reactivity worth is as shown in table 1.
Embodiment 2
(1) alumina support for weighing a certain amount of shaping is put into impregnating equipment；
(2) weigh and a certain amount of use chloroplatinic acid H2PtCl6(in terms of 0.08%Pt), it is molten with appropriate watery hydrochloric acid
Xie Hou, is added in carrier, is impregnated under negative pressure -0.04MPa 1 hour, 10 are then dried at 110 DEG C
Hour, 500 DEG C are calcined 2 hours under air atmosphere；
(3) appropriate butter of tin SnCl is weighed4(in terms of 0.3%Sn), with appropriate deionized water dissolving
Afterwards, the carrier that step (2) is obtained is added, is impregnated 1 hour under negative pressure -0.04MPa, then at 110 DEG C
Lower drying 10 hours, 500 DEG C are calcined 2 hours under air atmosphere；
(4) appropriate potassium chloride (in terms of 0.3%K) is weighed, after appropriate deionized water dissolving, step is added
Suddenly the carrier that (3) are obtained, impregnates 1 hour under negative pressure -0.04MPa, 10 is then dried at 110 DEG C
Hour, 500 DEG C are calcined 2 hours under air atmosphere；
(5) time processing is repeated twice according to the order of step (2) to step (4) to be obtained by step (4)
Carrier, obtain catalyst B.Catalyst components content Pt 0.24wt%, Sn 0.9wt%, K 0.9wt%,
Cl 2.11wt%.Catalyst B reactivity worth evaluates be the same as Example 1, refers to table 1.
Comparative example 1
(1) alumina support for weighing a certain amount of shaping is put into impregnating equipment；
(2) weigh and a certain amount of use chloroplatinic acid H2PtCl6(in terms of 0.5%Pt) and appropriate butter of tin SnCl4
(in terms of 0.8%Sn), after appropriate diluted hydrochloric acid dissolution, is added in carrier, under negative pressure -0.08MPa
Dipping 1 hour, is then dried 10 hours at 110 DEG C, and 500 DEG C are calcined 4 hours under air atmosphere；
(3) appropriate potassium chloride (in terms of 0.8%K) is weighed, after appropriate deionized water dissolving, step is added
Suddenly the carrier that (2) are obtained, impregnates 1 hour under negative pressure -0.04MPa, 10 is then dried at 110 DEG C
Hour, 500 DEG C are calcined 4 hours under air atmosphere, obtain catalyst C.The catalyst components content
Pt 0.5wt%, Sn 0.8wt%, K 0.8wt%, Cl 1.56wt%.Catalyst C reactivity worth is evaluated with implementation
Example 1, refers to table 1.
The dehydrogenation of isobutane reactivity worth of table 1
By catalyst A, B, C at 400~500 DEG C of temperature, burnt in the atmosphere of air,
Oxychlorination updates at 480~510 DEG C, and the dehydrogenation reaction performance after catalyst regeneration is as shown in table 2.
Dehydrogenation of isobutane reactivity worth after table 2 regenerates
The conversion ratio of the catalyst prepared from Tables 1 and 2, the inventive method is higher, isobutene selection
More preferably, reactivity is more preferable, more stable for performance.
Schematical embodiment of the invention is the foregoing is only, the scope of the present invention is not limited to.
Any those skilled in the art, it is made on the premise of the design of the present invention and principle is not departed to be equal
Change and modification, all should belong to the scope of protection of the invention.
Claims (9)
1. the preparation method of dehydrogenation of isobutane catalyst, it is characterised in that comprise the following steps：
Step 1: preparing appropriate platinum group metal dipping solution, the platinum group metal dipping solution prepared is added
Enter among the carrier after shaping, impregnate under negative pressure, the carrier impregnated is dried at a proper temperature,
Roasting；
Step 2: preparing the first appropriate auxiliary agent dipping solution, the first auxiliary agent dipping solution prepared is added
Enter among the carrier handled by step one, impregnate under negative pressure, by the carrier after dipping at a proper temperature
Drying, roasting；
Step 3: preparing the second appropriate auxiliary agent dipping solution, the second auxiliary agent dipping solution prepared is added
Enter among the carrier handled by step 2, impregnate under negative pressure, by the carrier after dipping at a proper temperature
Drying, roasting；
Step 4: step one, which is repeated several times, arrives step 3, using infusion process bearing the multiple substep of active component
It is loaded on carrier, obtains dehydrogenation of isobutane catalyst.
2. the preparation method of dehydrogenation of isobutane catalyst as claimed in claim 1, it is characterised in that：It is described
Dehydrogenation of isobutane catalyst uses heat-resistant oxide for carrier, using platinum group as major catalyst, with
IVth A races element is that the first auxiliary agent, alkali metal or alkaline-earth metal are the second auxiliary agent, using halogen as modifying agent.
3. the preparation method of dehydrogenation of isobutane catalyst as claimed in claim 2, it is characterised in that：
The heat-resistant oxide is more than one or both of aluminum oxide, silica and Si-Al molecular sieve
The mixture of arbitrary proportion；
The platinum group metal is the mixing of one or both of ruthenium, rhodium, iridium, palladium and platinum any of the above ratio
Thing；
IVth A races element is the mixture of one or both of germanium, tin and lead any of the above ratio；
The alkali metal or alkaline-earth metal are that the one or more of lithium, sodium, potassium, caesium, calcium and magnesium are any
The mixture of ratio.
4. the preparation method of dehydrogenation of isobutane catalyst as claimed in claim 1, it is characterised in that：
Every time during dipping, carrier impregnates 1~10 hour under negative pressure -0.01~-0.08MPa；
The carrier after dipping is dried 5~20 hours under the conditions of 80~180 DEG C every time；
Carrier after drying is calcined 2~15 hours under the conditions of 400~600 DEG C.
5. the preparation method of dehydrogenation of isobutane catalyst as claimed in claim 4, it is characterised in that：
Every time during dipping, carrier impregnates 6~8 hours under negative pressure -0.01~-0.08MPa；
The carrier after dipping is dried 10~15 hours under the conditions of 110~120 DEG C every time；
Carrier after drying is calcined 8~10 hours under the conditions of 400~600 DEG C.
6. the dehydrogenation of isobutane catalyst prepared using such as any one of claim 1-5 methods described.
7. dehydrogenation of isobutane catalyst as claimed in claim 6, it is characterised in that：In terms of carrier quality,
The weight/mass percentage composition of platinum group metal is 0.15~0.5wt%, the weight/mass percentage composition of the first auxiliary agent for 0.5~
2wt%, the weight/mass percentage composition of the second auxiliary agent is 0.15~5wt%, and modifier content is 0.01-5wt%.
8. the dehydrogenating technology of preparing isobutene through dehydrogenation of iso-butane, it is characterised in that：Using described in claim 6
Catalyst, using hydrogen as diluent, using fixed bed reactors；The reaction temperature of catalytic dehydrogenation be 400~
700 DEG C, reaction pressure is normal pressure~1Mpa, and gaseous mass air speed is 0.1~10h-1, gas volume ratio is different
Butane：Hydrogen=1:0.1~10.
9. dehydrogenating technology as claimed in claim 8, it is characterised in that：The catalyst have pretreatment and again
Raw step, the pretreatment is to be reduced 1~10 hour in 300~500 DEG C of hydrogen streams；It is regenerated as that carbon will be tied
And the catalyst inactivated burns in air atmosphere, temperature is burnt for 250~500 DEG C, the catalyst after burning
Oxychlorination updates again, active component is disperseed again.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110841726A (en) * | 2019-12-02 | 2020-02-28 | 西安凯立新材料股份有限公司 | Regeneration method of catalyst for isobutane dehydrogenation |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110841726A (en) * | 2019-12-02 | 2020-02-28 | 西安凯立新材料股份有限公司 | Regeneration method of catalyst for isobutane dehydrogenation |
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