CN108654596A - A kind of propane dehydrogenation catalyst and preparation method thereof - Google Patents
A kind of propane dehydrogenation catalyst and preparation method thereof Download PDFInfo
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- CN108654596A CN108654596A CN201810402705.4A CN201810402705A CN108654596A CN 108654596 A CN108654596 A CN 108654596A CN 201810402705 A CN201810402705 A CN 201810402705A CN 108654596 A CN108654596 A CN 108654596A
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- 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
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/26—Chromium
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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- 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
- C07C5/3332—Catalytic processes with metal oxides or metal sulfides
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- C07C2523/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- C07C2523/26—Chromium
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention discloses a kind of propane dehydrogenation catalyst and preparation method thereof, which mixes using chromium composite oxides as active component with high-performance heat carrier, and binder and modifying element is added, is prepared through kneading, extrusion, drying, roasting.Each composition quality percentage composition is followed successively by：Chromium composite oxides 55 80%, high-performance heat carrier 10 30%, modifying element 0.1 10.0%, binder surplus.The present invention improves dispersion degree of the chromium on carrier, effectively increases the conversion ratio of the effective rate of utilization and raw material propane of active component by synthesizing chromium composite oxides；The activity and selectivity of catalyst is improved by metal-modified processing, and then improves propene yield；It is handled by high-temperature vapor, greatly reduces the acid amount and acid strength of carrier surface, effectively reduce coking and the olefin cracking reaction of catalyst；High-performance heat carrier is added, effectively increases catalyst use efficiency, improves device produce load.
Description
Technical field
The present invention relates to a kind of catalyst for dehydrogenation of low-carbon paraffin and preparation method thereof, specifically, are related to a kind of propane and urge
The catalyst and preparation method thereof of fluidized dehydrogenation propylene.
Background technology
Propylene is a kind of important industrial chemicals, is widely used in production polypropylene, acrylic acid, propylene oxide and acrylonitrile etc.
Chemical products.China's propylene is mainly derived from the coproduction of the techniques such as naphtha pyrolysis and catalytic cracking or by-product, but as propylene disappears
The increase year by year of the amount of expense, traditional production of propylene have been unable to meet demand, and therefore, preparing propylene by dehydrogenating propane technology is fast-developing,
As the third-largest propylene source after methanol-to-olefins.
For chromium system propane dehydrogenation catalyst, since the prior art mostly uses infusion process supported active on the alumina support
Component, this method influence the loading and dispersion degree of active component on the alumina support, reduce the effective of active component
Utilization rate influences the reactivity and selectivity of catalyst；The presence in a large amount of acid sites, causes catalyst quickly to be tied on aluminium oxide
Burnt and olefin cracking.For this purpose, catalyst is frequently with alkalinous metal or its oxide modifying, to reduce carrier acid amount, but this change
Property processing, cause the strong interaction of basic anhydride and chromium oxide, to inhibit dehydrogenation activity, cause high valence chrome complete
It restores entirely and reduces olefine selective.Dehydrogenating propane is strong endothermic reaction, and as reaction carries out, reaction bed temperature is rapid
It reduces and causes to react and regenerate frequent switching so that catalyst treatment amount reduces, and is reduced so as to cause device produce load.
Invention content
The object of the present invention is to provide a kind of propane dehydrogenation catalysts and preparation method thereof, and the catalyst is with chromium combined oxidation
Object is active component, with one or more of sodium, potassium, iron, titanium, vanadium, zirconium, zinc, copper, nickel for modifying element, improves catalysis
Agent dehydrogenation activity and selectivity, meanwhile, high-performance heat carrier is added in the catalyst, improves the thermal capacity of catalyst, makes to urge
Agent bed rate of temperature fall slows down, and extends the reaction time, improves device produce load.
The object of the invention to solve the technical problems is realized using following technical scheme.
A kind of propane dehydrogenation catalyst proposed according to the present invention, using chromium composite oxides as active component, with high-performance
Heat carrier mixes, and binder is added, with one or more of sodium, potassium, iron, titanium, vanadium, zirconium, zinc, copper, nickel for modifying element, warp
Kneading, extrusion, drying, roasting are prepared.
The mass percentage of above-mentioned catalyst, each ingredient is respectively：
Further, the chromium composite oxides by chromium solution with containing one or more elements in aluminium, silicon, phosphorus solution or
Colloidal sol mixes, and is obtained by crystallization, calcination process；The mass percentage of chromium oxide is 15- in gained chromium composite oxides
35%.
Further, the high-performance heat carrier is one in Alpha-alumina, silicon nitride, silicon carbide, zirconium dioxide, boron nitride
Kind or several mixing.
Further, the binder is the mixing of one or more of Aluminum sol, Ludox, SB powder.
Following technical scheme also can be used to realize in the object of the invention to solve the technical problems.
A kind of preparation method of propane dehydrogenation catalyst, includes the following steps：
(1) chromium composite oxides are prepared
(1.1) by chromium solution with containing one or more elements in aluminium, silicon, phosphorus solution or colloidal sol at 50-80 DEG C mix
Conjunction stirs evenly, and obtains mixed solution；Wherein, chromium source is the oxide of soluble chromic salts or chromium, and silicon source is sodium metasilicate or silicon
Colloidal sol, silicon source are the mixing of one or more of Aluminum sol, aluminum nitrate, Alusil, phosphorus aluminium glue；
(1.2) step (1.1) is prepared into gained mixed solution and alkaline matter is added under stirring conditions, it is molten to adjust mixing
Liquid pH value is 8-10, and solution is made to become sticky slurries；The alkaline matter is sodium hydroxide, potassium hydroxide, ammonium hydroxide, second two
It is one or more in amine, hexa；
(1.3) the slurries dislocation for preparing step (1.2) is sealed at 150-200 DEG C and is stirred in the autoclave with stirring
Crystal is taken out after mixing crystallization 5-70 hours, chromium composite oxides are obtained through drying, roasting；
(2) catalyst is prepared
(2.1) the chromium composite oxides that step (1.3) prepares are uniformly mixed with ultra-fine high-performance heat carrier, are added viscous
Mixture, kneading extruding are in strip；
(2.2) wet bar prepared by step (2.1) is dried, calcination process；
(2.3) product sodium, potassium, iron after roasting step (2.2), titanium, vanadium, zirconium, zinc, copper, one kind in nickel or several
The solution dipping of kind element mixing is modified；
(2.4) the modified product of step (2.3) is dried, roasts and obtains modified catalyst；
(2.5) modified catalyst for obtaining step 2.4 carries out high-temperature vapor burin-in process 8-16 hours, obtains propane
Dehydrogenation；
In above-mentioned preparation method, chromium composite oxides, high-performance heat carrier, modifying element mass percentage successively
For：55-80%, 10-30%, 0.1-10.0%, surplus are binder.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
The preparation method of a kind of propane dehydrogenation catalyst above-mentioned, wherein step (1.3) crystal is done at 120 DEG C
2-6 hours dry, 500-600 DEG C roasts 4-8 hours, obtains chromium composite oxides.
The preparation method of a kind of propane dehydrogenation catalyst above-mentioned, wherein step (2.2) is dry, calcination process condition
For：It is 2-6 hours dry in 120 DEG C, it is roasted 4-8 hours in 450-550 DEG C.
A kind of preparation method of propane dehydrogenation catalyst above-mentioned, wherein step (2.4) is 2-6 hours dry in 120 DEG C,
550-650 DEG C of roasting obtains modified catalyst in 4-8 hours.
The preparation method of a kind of propane dehydrogenation catalyst above-mentioned, wherein step (2.5) is in 650-850 DEG C of temperature, often
It presses, high-temperature vapor burin-in process is carried out under 100% water vapor conditions.
Compared with prior art, beneficial effects of the present invention are as follows：
(1) by synthesizing chromium composite oxides, dispersion degree of the chromium on carrier is improved, the effective of active component is improved
Utilization rate effectively increases the conversion ratio of raw material propane；
(2) activity and selectivity that catalyst is effectively increased by metal-modified processing, improves purpose product propylene
Yield；
(3) high-temperature vapor is handled, and is greatly reduced the acid amount and acid strength of carrier surface, is effectively reduced catalyst
Coking and olefin cracking reaction；
(4) high-performance heat carrier is added in catalyst, effectively raises the thermal capacity of catalyst, it is anti-to extend dehydrogenating propane
Between seasonable, the utilization ratio of catalyst is improved, device working ability is effectively increased.
Above description is only the general introduction of technical solution of the present invention, in order to better understand the technical means of the present invention,
And can be implemented in accordance with the contents of the specification, and in order to allow the above and other objects, features and advantages of the present invention can
It is clearer and more comprehensible, special below to lift preferred embodiment, detailed description are as follows.
Specific implementation mode
It is of the invention to reach the technological means and effect that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Preferred embodiment further illustrates the present invention.
Embodiment 1
Weigh 1579 grams of Cr (NO3)3·9H2O is dissolved in deionized water, and 2000 grams of Ludox are added and stir evenly, continue to stir
It is slowly added to 250 gram of 10% sodium hydroxide solution, 300 gram of 10% hexa solution liquid continues to stir after becoming sticky shape
It mixes 2 hours, slurries is poured into sealing stirring in autoclaves of the 5000ml with polytetrafluoroethyllining lining and react 50 under the conditions of 180 DEG C
Hour, it takes out 120 DEG C and dries 4 hours, 600 DEG C of roastings obtain small particle chromium composite oxides A in 6 hours.
Embodiment 2
Weigh 1579 grams of Cr (NO3)3·9H2O, 5147 grams of Al (NO3)3·9H2O is dissolved in deionized water, and it is slow to continue stirring
250 gram of 10% sodium hydroxide solution is added, 300 gram of 10% hexa solution liquid continues stirring 2 after becoming sticky shape
Hour, it is small that slurries are poured into sealing stirring reaction 50 under the conditions of 180 DEG C in autoclaves of the 5000ml with polytetrafluoroethyllining lining
When, it takes out 120 DEG C and dries 4 hours, 600 DEG C of roastings obtain small particle chromium composite oxides B in 6 hours.
Embodiment 3
700 grams of A are weighed, 100 grams of ultra-fine Alpha-aluminas are uniformly mixed the boehmite kneading that 300 grams of nitric acid acidifications are added
It squeezes and is in strip after uniformly, 2 hours dry at 120 DEG C, 600 DEG C roast 6 hours, obtain unmodified catalyst C1, weigh 57 grams
ZrCl4, deionized water is added and is prepared into solution, weighs 1000 grams of C1Homogeneous impregnation is in ZrCl4In solution, stand 2 hours after
It is dried at 120 DEG C 4 hours, 600 DEG C roast 6 hours, obtain modified catalyst C2, by modified catalyst C2At 750 DEG C, normal pressure,
Under 100% water vapor conditions, high-temperature vapor burin-in process is carried out 12 hours, obtain propane dehydrogenation catalyst D.
Wherein, chromium oxide mass content 20% on catalyst, zirconium oxide mass content 3%.
Embodiment 4
700 grams of B are weighed, 100 grams of ultra-fine Alpha-aluminas are uniformly mixed the boehmite kneading that 300 grams of nitric acid acidifications are added
It squeezes and is in strip after uniformly, 2 hours dry at 120 DEG C, 600 DEG C roast 6 hours, obtain unmodified catalyst C3, weigh 57 grams
ZrCl4, deionized water is added and is prepared into solution, weighs 1000 grams of C3Homogeneous impregnation is in ZrCl4In solution, stand 2 hours after
It is dried at 120 DEG C 4 hours, 600 DEG C roast 6 hours, obtain modified catalyst C4, by modified catalyst C4At 680 DEG C, normal pressure,
Under 100% water vapor conditions, high-temperature vapor burin-in process is carried out 14 hours, obtain propane dehydrogenation catalyst E.
Wherein, chromium oxide mass content 20% on catalyst, zirconium oxide mass content 3%.
Comparative example 1
Weigh 1315.75 grams of Cr (NO3)3·9H2O is added deionized water and is prepared into solution, weighs 1000 grams of bar shaped γ-oxygen
Change alumina supporter to be impregnated in the chromium nitrate solution prepared, be dried at 120 DEG C after standing 2 hours 4 hours, 600 DEG C of roastings 6 are small
When, obtain unmodified catalyst S1, weigh 57 grams of ZrCl4Deionized water is added and is prepared into solution, weighs 1000 grams of S1Homogeneous impregnation
In ZrCl4In solution, dried at 120 DEG C after standing 2 hours 4 hours, 600 DEG C roast 6 hours, obtain modified catalyst S2, will
Modified catalyst S2At 750 DEG C, normal pressure under 100% water vapor conditions, carries out high-temperature vapor burin-in process 12 hours, obtains
Propane dehydrogenation catalyst F.
Embodiment 5
Above-mentioned propane dehydrogenation catalyst D, E, F are fitted into the insulation fix bed bed reactors of laboratory 1000ml, 620 DEG C logical
It is passed through propane reaction after entering hydrogen reducing 2min, reaction product is analyzed by on-line chromatograph.Experiment condition：Reaction temperature is 620
DEG C, propane mass space velocity 2.0h-1, reaction pressure is normal pressure.The experimental evaluation of preparing propylene by dehydrogenating propane the results are shown in Table 1.
1 preparing propylene by dehydrogenating propane reaction result of table
Experimental evaluation the result shows that：The catalyst prepared using the method for the present invention, the high conversion rate of propane, Propylene Selectivity
Good, the catalyst on-line operation time is long, and catalyst bed temperature drop is few, illustrates catalyst dehydrogenating propane prepared by the method for the present invention
It has excellent performance, is conducive to the returns and efficiency for improving dehydrogenating propane.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, according to the technical essence of the invention
To any simple modification, equivalent change and modification made by above example, in the range of still falling within technical solution of the present invention.
Claims (10)
1. a kind of propane dehydrogenation catalyst, it is characterised in that mixed with high-performance heat carrier using chromium composite oxides as active component
It closes, binder is added, with one or more of sodium, potassium, iron, titanium, vanadium, zirconium, zinc, copper, nickel for modifying element, through kneading, squeeze
Item, drying, roasting are prepared.
2. catalyst as described in claim 1, it is characterised in that the mass percentage of each ingredient is respectively：
3. catalyst as described in claim 1, it is characterised in that the chromium composite oxides are by chromium solution and containing aluminium, silicon, phosphorus
In one or more elements solution or colloidal sol mixing, obtained by crystallization, calcination process；Oxygen in gained chromium composite oxides
The mass percentage for changing chromium is 15-35%.
4. catalyst as described in claim 1, it is characterised in that the high-performance heat carrier is Alpha-alumina, silicon nitride, carbon
One or more of SiClx, zirconium dioxide, boron nitride mix.
5. catalyst as described in claim 1, it is characterised in that the binder is one in Aluminum sol, Ludox, SB powder
Kind or several mixing.
6. a kind of preparation method of propane dehydrogenation catalyst, it is characterised in that include the following steps：
(1) chromium composite oxides are prepared
(1.1) by chromium solution with containing one or more elements in aluminium, silicon, phosphorus solution or colloidal sol mix and stir at 50-80 DEG C
It mixes uniformly, obtains mixed solution；Wherein, chromium source is the oxide of soluble chromic salts or chromium, and silicon source is sodium metasilicate or Ludox,
Silicon source is the mixing of one or more of Aluminum sol, aluminum nitrate, Alusil, phosphorus aluminium glue；
(1.2) step (1.1) is prepared into gained mixed solution and alkaline matter is added under stirring conditions, adjust mixed solution PH
Value is 8-10, and solution is made to become sticky slurries；The alkaline matter is sodium hydroxide, potassium hydroxide, ammonium hydroxide, ethylenediamine, six
It is one or more in methenamine；
(1.3) the slurries dislocation for preparing step (1.2) is in the autoclave with stirring, and sealing stirring is brilliant at 150-200 DEG C
Crystal is taken out after changing 5-70 hours, chromium composite oxides are obtained through drying, roasting；
(2) catalyst is prepared
(2.1) the chromium composite oxides that step (1.3) prepares are uniformly mixed with ultra-fine high-performance heat carrier, bonding is added
Agent, kneading extruding are in strip；
(2.2) wet bar prepared by step (2.1) is dried, calcination process；
(2.3) one or more of product sodium, potassium, iron, titanium, vanadium, zirconium, zinc, copper, nickel after roasting step (2.2) member
The solution dipping of element mixing is modified；
(2.4) the modified product of step (2.3) is dried, roasts and obtains modified catalyst；
(2.5) modified catalyst for obtaining step 2.4 carries out high-temperature vapor burin-in process 8-16 hours, obtains dehydrogenating propane
Catalyst；
In above-mentioned preparation method, chromium composite oxides, high-performance heat carrier, modifying element mass percentage be followed successively by：55-
80%, 10-30%, 0.1-10.0%, surplus are binder.
7. the preparation method of propane dehydrogenation catalyst as claimed in claim 6, it is characterised in that step (1.3) described crystal
2-6 hours dry at 120 DEG C, 500-600 DEG C roasts 4-8 hours, obtains chromium composite oxides.
8. the preparation method of propane dehydrogenation catalyst as claimed in claim 6, it is characterised in that step (2.2) is dry, roasts
The condition of processing is：It is 2-6 hours dry in 120 DEG C, it is roasted 4-8 hours in 450-550 DEG C.
9. the preparation method of propane dehydrogenation catalyst as claimed in claim 6, it is characterised in that step (2.4) is dry in 120 DEG C
2-6 hours dry, 550-650 DEG C of roasting obtains modified catalyst in 4-8 hours.
10. the preparation method of propane dehydrogenation catalyst as claimed in claim 6, it is characterised in that step (2.5) is in temperature
650-850 DEG C, normal pressure carries out high-temperature vapor burin-in process under 100% water vapor conditions.
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| CN110743593A (en) * | 2019-10-31 | 2020-02-04 | 中国石油大学(华东) | Application of boron-carbon-nitrogen material in catalyzing oxidative dehydrogenation of low-carbon alkane to prepare olefin |
| WO2020224584A1 (en) * | 2019-05-06 | 2020-11-12 | 中国石油化工股份有限公司 | Catalyst for dehydrogenating organic hydrogen storage raw material, carrier for catalyst, hydrogen storage alloy, and method for providing high purity hydrogen |
| CN114763316A (en) * | 2021-01-15 | 2022-07-19 | 中国科学院大学 | Method for preparing propylene by directly dehydrogenating propane through efficient catalysis of mesoporous spinel |
| CN115041208A (en) * | 2022-05-17 | 2022-09-13 | 大连理工大学 | Forming method of honeycomb-shaped boron nitride and application of honeycomb-shaped boron nitride in oxidative dehydrogenation of low-carbon alkane |
| CN115487801B (en) * | 2021-06-18 | 2024-03-26 | 中国石油化工股份有限公司 | Dehydrogenation catalyst, preparation method and application thereof |
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| WO2020224584A1 (en) * | 2019-05-06 | 2020-11-12 | 中国石油化工股份有限公司 | Catalyst for dehydrogenating organic hydrogen storage raw material, carrier for catalyst, hydrogen storage alloy, and method for providing high purity hydrogen |
| CN110743593A (en) * | 2019-10-31 | 2020-02-04 | 中国石油大学(华东) | Application of boron-carbon-nitrogen material in catalyzing oxidative dehydrogenation of low-carbon alkane to prepare olefin |
| CN114763316A (en) * | 2021-01-15 | 2022-07-19 | 中国科学院大学 | Method for preparing propylene by directly dehydrogenating propane through efficient catalysis of mesoporous spinel |
| CN114763316B (en) * | 2021-01-15 | 2023-10-20 | 中国科学院大学 | Method for preparing propylene by directly dehydrogenating propane through high-efficiency catalysis of Kong Jian spar |
| CN115487801B (en) * | 2021-06-18 | 2024-03-26 | 中国石油化工股份有限公司 | Dehydrogenation catalyst, preparation method and application thereof |
| CN115041208A (en) * | 2022-05-17 | 2022-09-13 | 大连理工大学 | Forming method of honeycomb-shaped boron nitride and application of honeycomb-shaped boron nitride in oxidative dehydrogenation of low-carbon alkane |
| CN115041208B (en) * | 2022-05-17 | 2024-02-23 | 大连理工大学 | Forming method of honeycomb boron nitride and application of honeycomb boron nitride in oxidative dehydrogenation of low-carbon alkane |
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