CN106732574A - A kind of alkane dehydrogenating catalyst containing mixing Pt crystal and preparation method thereof - Google Patents
A kind of alkane dehydrogenating catalyst containing mixing Pt crystal and preparation method thereof Download PDFInfo
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- CN106732574A CN106732574A CN201611029686.2A CN201611029686A CN106732574A CN 106732574 A CN106732574 A CN 106732574A CN 201611029686 A CN201611029686 A CN 201611029686A CN 106732574 A CN106732574 A CN 106732574A
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/62—Platinum group metals with gallium, indium, thallium, germanium, tin or lead
- B01J23/622—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead
- B01J23/626—Platinum group metals with gallium, indium, thallium, germanium, tin or lead with germanium, tin or lead with tin
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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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- 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
- C07C5/3335—Catalytic processes with metals
- C07C5/3337—Catalytic processes with metals of the platinum group
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
- C07C2523/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals
- C07C2523/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36
- C07C2523/56—Platinum group metals
- C07C2523/62—Platinum group metals with gallium, indium, thallium, 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
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The invention discloses a kind of alkane dehydrogenating catalyst containing mixing Pt crystal, the catalyst is made up of active component, auxiliary agent and the part of carrier three, active component is Pt, auxiliary agent is alkali metal and IV B races metal, wherein Pt IVB Complex Crystals concentrate on carrier inside, and Pt alkali metal octahedral crystals concentrate on carrier surface.The invention also discloses the preparation method of above-mentioned catalyst, the method first prepares Pt IVB metal impregnation liquid of the acid concentration in 1 3M, on incipient impregnation to carrier, is placed through room temperature, dries, is calcined the carrier that the crystal of Sn containing Pt is obtained；Then acid concentration is the Pt alkali metal maceration extracts of 0.2 0.8M again, on incipient impregnation to the carrier containing Pt Sn, is obtained after room temperature placement, drying, roasting.Compared to the catalyst containing only single crystal, more preferably, inactivation is slower, and the life-span is longer for catalyst dehydrogenation activity of the present invention containing mixing Pt crystal.
Description
Technical field
The present invention relates to the catalyst and preparation method of a kind of corresponding alkene of dehydrogenating low-carbon alkane system, low-carbon (LC) is particularly improved
Dehydrating alkanes alkene catalyst activity and the catalyst in life-span and preparation method thereof, belong to field of catalyst preparation.
Background technology
Propylene is important Organic Chemicals, and the byproduct of the conventional refinery process such as steam cracking and catalytic cracking is it
Main source, therefore propylene yield is limited by the production of major product ethene and product oil.The propylene yield of current traditional handicraft can not
Meet demand of the market to propylene, the replacement production new technique of propylene, including dehydrogenating propane (PDH), methyl alcohol are gradually paid close attention in market
Five kinds of techniques such as alkene (MTO, MTP) processed, DCC (DCC), olefin cracking and olefin(e) disproportionation.Comparatively speaking, third
Alkane De-hydrogen Technology advantage becomes apparent, it possess technology maturation, good product quality, high conversion rate, accessory substance it is few the advantages of.At present
Industrialized preparing propylene by dehydrogenating propane production technology is mainly the Oleflex techniques of Uop Inc., the Oleflex techniques of Uop Inc.
Used precious metals pt catalyst.Propane catalytic dehydrogenating reaction is limited by thermodynamical equilibrium, must high temperature, low pressure it is severe
Carried out under the conditions of quarter.
Industrial dehydrogenating propane production propylene is carried out at a high temperature of 620 DEG C or so, except dehydrogenation main reaction, also just like
The side reactions such as cracking, aromatisation and polymerization, these side reactions can accelerate catalyst surface carbon deposit, make rapid catalyst deactivation, urge
Agent needs repeated regeneration.Therefore, activity, anti-carbon and the regeneration rear stability for improving catalyst are that dehydrogenating low-carbon alkane is urged
The emphasis and focus of agent research.A kind of catalyst disclosed in Chinese patent CN 1069226C, bears respectively on the alumina support
Carry Sn, Pt and K, although improve the activity and selectivity of catalyst, but catalyst preparation process is complicated, increased catalyst
Preparation cost, and without provide catalyst repeatedly regeneration after performance.One disclosed in the B of Chinese patent CN 103055857
Catalyst for dehydrogenation of low-carbon paraffin is planted, various auxiliary agents are added in carrier shaping, and active component Pt is incorporated into carrier using infusion process,
Various helping is introduced during stability after the activity of catalyst and regeneration is improved, but the patent there is not offer carrier shaping preparation process
Influence of the agent to its mechanical strength.A kind of catalyst for dehydrogenation of low-carbon paraffin disclosed in Chinese patent CN 103055953B, using small
The method of inorganic oxygen-containing and the thing doping of particle diameter aluminium obtains mixed oxidization alumina supporter, enhances catalytic mechanical intensity, but
The less stable of catalyst, iso-butane conversion ratio from the 44.3% of initial reaction stage, by dropping to 27.9% after 72h.
The introducing of active component Pt is complexed using the independent dip loadings of Pt or Pt-Sn in above-mentioned catalyst preparation process
To on carrier, catalyst can be only formed single Pt crystal to co-impregnation, so cause mechanical strength, activity, the stabilization of catalyst
Property and anti-carbon poor-performing.Prepared with the dipping method that co-impregnation is combined using substep, first step dipping makes Pt and transition
The crystal that the complex compound that metal Sn is formed is formed concentrates on carrier inside, and second step dipping makes the octahedron that Pt is formed with alkali metal
The document that crystal concentrates on carrier surface is not yet reported.
The content of the invention
The technical problems to be solved by the invention are that the active component Pt of catalyst in existing technology of preparing is single crystal form,
Cause catalyst easy coking and deactivation in use at high temperature, there is provided a kind of system of the alkane dehydrogenating catalyst containing mixing Pt crystal
Preparation Method, inactivation is slow when catalyst prepared by the method is used at high temperature, and activation recovering is normal after regeneration.
A kind of alkane dehydrogenating catalyst containing mixing Pt crystal, is made up of active component, auxiliary agent and the part of carrier three, activity
Component is Pt, and auxiliary agent is one or more in alkali metal and IV B races metal, and remaining is carrier, and carrier is Al2O3；Wherein Pt-
IVB crystal concentrates on carrier inside, and Pt- crystalline alkali metals concentrate on carrier surface.
Catalyst of the present invention, on the basis of the weight of prepared catalyst, the content of Pt for 0.1%~
0.5%, auxiliary element content is 0.1~2.0wt%, and remaining is carrier.
Catalyst of the present invention, wherein alkali metal are preferably at least one in K and Rb, and IV B races metal is preferably
Sn.Alkali metal is 0.5~2 with the atomic ratio that the atomic ratio of Pt is 5~20, Sn and Pt.
Present invention also offers a kind of preparation method of abovementioned alkyl dehydrogenation, including：
1) platiniferous presoma and IVB metal salt solutions are well mixed and obtain Pt-IVB metal impregnation liquid, then add salt
Acid solution to the acid concentration of maceration extract is 1-3M, then incipient impregnation on carrier, room temperature is placed, drying, roasting, be obtained and contain
The carrier of Pt-IVB crystal；
2) platiniferous presoma and alkali metal salt soln are well mixed, adding hydrochloric acid solution to the acid concentration of maceration extract is
0.2-0.8M, on incipient impregnation to the carrier containing Pt-IVB, is obtained after room temperature placement, drying, roasting.
Catalyst of the present invention is used for dehydrogenating low-carbon alkane, especially propane or dehydrogenation of isobutane, for low-carbon alkanes
The reaction condition of dehydrogenation is as follows：500 DEG C -650 DEG C of reaction temperature, pressure is normal pressure, H2/ hydrocarbon (mol ratios)=0.2-2, gas is total
Air speed 500-5000h-1.Catalyst needs to carry out reduction treatment before the reaction, and treatment conditions are 500 DEG C -600 DEG C, reduce 1-5h.
Alkane dehydrogenating catalyst of the present invention containing mixing Pt crystal has good effect to low-carbon alkanes catalytic dehydrogenation, should
The dehydrogenation reaction activity of catalyst propane is very high, significantly improves the conversion per pass of propane, and in 600 DEG C of reaction temperature, pressure is
Normal pressure, the volume space velocity of propane is 1000h-1, H2The conversion ratio of/hydrocarbon (mol ratios)=0.6 time propane is more than 33%, and selectivity is big
In 90%, and with good regenerating stability, extend catalyst service life.The preparation method of catalyst of the present invention possesses good
Good operability,
Specific embodiment
Following embodiment is used to be specifically described know-why of the invention, implementation and effect, but this hair
Bright method and core concept is not limited except as.
Comparative example 1
Catalyst A：Pt, Sn and K are prepared using co-impregnation in catalyst A, and the preparation method is containing only a kind of Pt crystal, Pt：
0.3w%, Sn：0.6w% and K：0.9w%.
(1) prepared by carrier.A certain amount of alumina powder is mixed with the sesbania powder that mixed powder mass fraction is 5% is accounted for
Uniformly, citric acid that mass concentration is 5% and mass concentration are added for 15% dust technology carries out kneading, the kneading time is 1h,
The last extrusion on banded extruder again, after room temperature dries in the air 8h, then at 120 DEG C of drying 4h, the carrier of drying is last for the carrier after extrusion
900 DEG C of roasting 6h, obtain final carrier in Muffle furnace, and its water absorption rate is 83%, and intensity is 80N/.
(2) it is that 0.18M stannous chloride water acid solution mixes by 2ml concentration 0.2M chloroplatinic acid aqueous solutions and 7.4ml concentration
It is even, according to the saturated water adsorptive value of used carrier, the dipping being finally configured to is made to hydrochloric acid and water is added in above-mentioned Pt-Sn maceration extracts
The concentration of the hydrochloric acid of liquid is 1.5M.The potassium nitrate of 0.58g is dissolved in above-mentioned maceration extract, adding deionized water makes maceration extract volume
It is 22ml, shakes up and be impregnated on the carrier of 26.66g, room temperature is placed 12 hours, dried 5 hours at 120 DEG C, is calcined at 550 DEG C
4 hours, obtain finished catalyst A.
Comparative example 2
Catalyst B：Pt, Sn and Rb are prepared using co-impregnation in catalyst B, and the preparation method is containing only a kind of Pt crystal, Pt：
0.3w%, Sn：0.6w% and Rb：0.9w%.
(1) carrier is prepared with support preparation method in (1) of comparative example 1.
(2) it is that 0.18M stannous chloride water acid solution mixes by 2ml concentration 0.2M chloroplatinic acid aqueous solutions and 7.4ml concentration
It is even, according to the saturated water adsorptive value of used carrier, the dipping being finally configured to is made to hydrochloric acid and water is added in above-mentioned Pt-Sn maceration extracts
The concentration of the hydrochloric acid of liquid is 1.5M.The rubidium nitrate of 0.35g is dissolved in above-mentioned maceration extract, adding deionized water makes maceration extract volume
It is 22ml, shakes up and be impregnated on the carrier of 26.66g, room temperature is placed 12 hours, dried 5 hours at 120 DEG C, is calcined at 550 DEG C
4 hours, obtain finished catalyst B.
Embodiment 1
Catalyst C：Catalyst C is Pt and Sn elder generation's co-impregnations to carrier inside, and co-impregnation is prepared Pt and K to carrier surface again
, the preparation method makes two kinds of crystal containing Pt-Sn and Pt-K in catalyst, Pt：0.3w%, Sn：0.6w% and K：0.9w%.
(1) carrier is prepared with support preparation method in (1) of comparative example 1.
(2) it is the mixing of 0.18M stannous chloride water acid solution by 1.5ml concentration 0.2M chloroplatinic acid aqueous solutions and 7.4ml concentration
Uniformly, according to the saturated water adsorptive value of used carrier, the leaching being finally configured to is made to hydrochloric acid and water is added in above-mentioned Pt-Sn maceration extracts
The concentration of the hydrochloric acid of stain liquid is 1.5M, and maceration extract volume is 22ml, shakes up and is impregnated on the carrier of 26.66g, and room temperature places 12
Hour, dried 5 hours at 120 DEG C, it is calcined 4 hours at 550 DEG C, the carrier containing Pt-Sn is obtained.
The potassium nitrate of 0.5ml concentration 0.2M chloroplatinic acid aqueous solutions and 0.58g is well mixed, according to the saturation of used carrier
Water absorption, makes the concentration of the hydrochloric acid of the maceration extract being finally configured to be 0.5M to hydrochloric acid and water is added in above-mentioned Pt-K maceration extracts,
Maceration extract volume is 22ml, shakes up and impregnates on the carrier containing Pt-Sn, and room temperature is placed 12 hours, is dried 5 hours at 120 DEG C,
It is calcined 4 hours at 550 DEG C, obtains finished catalyst C.
Embodiment 2
Catalyst D：Catalyst D be Pt and Sn elder generations co-impregnation to carrier inside, Pt and Rb again co-impregnation to carrier surface system
Standby, the preparation method makes two kinds of crystal containing Pt-Sn and Pt-Rb in catalyst, Pt：0.3w%, Sn：0.6w% and Rb：
0.9w%.
(1) carrier is prepared with support preparation method in (1) of comparative example 1.
(2) it is the mixing of 0.18M stannous chloride water acid solution by 1.5ml concentration 0.2M chloroplatinic acid aqueous solutions and 7.4ml concentration
Uniformly, according to the saturated water adsorptive value of used carrier, the leaching being finally configured to is made to hydrochloric acid and water is added in above-mentioned Pt-Sn maceration extracts
The concentration of the hydrochloric acid of stain liquid is 1.5M, and maceration extract volume is 22ml, shakes up and is impregnated on the carrier of 26.66g, and room temperature places 12
Hour, dried 5 hours at 120 DEG C, it is calcined 4 hours at 550 DEG C, the carrier containing Pt-Sn is obtained.
The rubidium nitrate of 0.5ml concentration 0.2M chloroplatinic acid aqueous solutions and 0.35g is well mixed, according to the saturation of used carrier
Water absorption, makes the concentration of the hydrochloric acid of the maceration extract being finally configured to be 0.5M to hydrochloric acid and water is added in above-mentioned Pt-Rb maceration extracts,
Maceration extract volume is 22ml, shakes up and impregnates on the carrier containing Pt-Rb, and room temperature is placed 12 hours, is dried 5 hours at 120 DEG C,
It is calcined 4 hours at 550 DEG C, obtains finished catalyst D.
Reaction evaluating, appreciation condition are carried out to catalyst A, B, C and D：600 DEG C of reaction temperature, pressure is normal pressure, propane
Volume space velocity is 1000h-1, H2/ hydrocarbon (mol ratios)=0.6.Catalyst needs to carry out hydrogen reducing treatment, treatment conditions before the reaction
It is 500 DEG C, reduces 4h.Evaluation result such as table 1.
The dehydrogenation reaction performance of the catalyst of table 1
Find out from the reaction evaluating data of table 1, the reactivity worth for possessing the catalyst C and D of mixed-crystal structure is better than
Only possess the catalyst A and B of single crystal structure.
Circular response-regeneration condition：Catalyst A, B, C and D are circulated the survey of reaction-regeneration catalyzing dehydrogenation activity
It is fixed.Reaction evaluating condition is constant.Catalyst regeneration conditions：It is 5% with oxygen content at 500 DEG C after catalyst H reacts 5 hours
Nitrogen and oxygen mixture burn carbon distribution on catalyst, the burn soot time is 3h, then small in 480 DEG C of reductase 12s with hydrogen
When, having reduced rear catalyst then carries out reaction evaluating experiment.Circular response-regenerated outcome is listed in table 2, and each data are reaction 5h
Interior average value.
Circular response-the regenerability of the catalyst of table 2
Be can be seen that by possessing single crystalline substance after repetitious reaction-regeneration from the circular response-regeneration data of table 2
Catalyst A and the B dehydrogenation activity of body structure decline substantially, catalyst C and D the dehydrogenation stabilization for possessing mixed-crystal structure.
Claims (5)
1. a kind of alkane dehydrogenating catalyst containing mixing Pt crystal, is made up of, its feature active component, auxiliary agent and the part of carrier three
It is that active component is Pt, auxiliary agent is one or more in alkali metal and IV B races metal, and remaining is carrier, and carrier is
Al2O3；Wherein Pt-IVB Complex Crystals concentrate on carrier inside, and Pt- alkali metal octahedral crystals concentrate on carrier surface.
2. catalyst according to claim 1, it is characterised in that on the basis of the weight of institute's catalyst, the content of Pt is
0.1%~0.5%, auxiliary element content is 0.1~2.0wt%, and remaining is carrier.
3. catalyst according to claim 1 and 2, it is characterised in that described alkali metal is at least in K and Rb
Kind, the IV B races metal is Sn.
4. catalyst according to claim 3, it is characterised in that alkali metal is 5~20, Sn and Pt's with the atomic ratio of Pt
Atomic ratio is 0.5~2.
5. according to the preparation method of any described catalyst of claim 1-4, it is characterised in that
1) platiniferous presoma and IVB metal salt solutions are well mixed and obtain Pt-IVB metal impregnation liquid, then add hydrochloric acid molten
Liquid to the acid concentration of maceration extract is 1-3M, then incipient impregnation on carrier, room temperature is placed, drying, roasting, be obtained and contain Pt-
The carrier of IVB crystal；
2) platiniferous presoma and alkali metal salt soln are well mixed, it is 0.2- to add hydrochloric acid solution to the acid concentration of maceration extract
0.8M, on incipient impregnation to the carrier containing Pt-IVB, is obtained after room temperature placement, drying, roasting.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325523A (en) * | 2018-02-02 | 2018-07-27 | 华东理工大学 | A kind of propane dehydrogenation catalyst and preparation method thereof |
| US10981149B2 (en) | 2019-03-18 | 2021-04-20 | Uop Llc | Dehydrogenation catalyst with optimum modifier profile index |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6872300B1 (en) * | 2002-03-29 | 2005-03-29 | Uop Llc | Reforming catalyst with chelated promotor |
| CN104588011A (en) * | 2013-11-01 | 2015-05-06 | 中国石油化工股份有限公司 | Alkane dehydrogenation catalyst and preparation method thereof |
| CN105582979A (en) * | 2014-10-22 | 2016-05-18 | 中国石油化工股份有限公司 | Dehydrogenation catalyst for light alkanes and preparation method thereof |
-
2016
- 2016-11-14 CN CN201611029686.2A patent/CN106732574B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6872300B1 (en) * | 2002-03-29 | 2005-03-29 | Uop Llc | Reforming catalyst with chelated promotor |
| CN104588011A (en) * | 2013-11-01 | 2015-05-06 | 中国石油化工股份有限公司 | Alkane dehydrogenation catalyst and preparation method thereof |
| CN105582979A (en) * | 2014-10-22 | 2016-05-18 | 中国石油化工股份有限公司 | Dehydrogenation catalyst for light alkanes and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108325523A (en) * | 2018-02-02 | 2018-07-27 | 华东理工大学 | A kind of propane dehydrogenation catalyst and preparation method thereof |
| CN108325523B (en) * | 2018-02-02 | 2021-01-08 | 华东理工大学 | Propane dehydrogenation catalyst and preparation method thereof |
| US10981149B2 (en) | 2019-03-18 | 2021-04-20 | Uop Llc | Dehydrogenation catalyst with optimum modifier profile index |
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