CN108786798A - A kind of preparation method of catalyst for dehydrogenation of low-carbon paraffin - Google Patents
A kind of preparation method of catalyst for dehydrogenation of low-carbon paraffin Download PDFInfo
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- CN108786798A CN108786798A CN201710299800.1A CN201710299800A CN108786798A CN 108786798 A CN108786798 A CN 108786798A CN 201710299800 A CN201710299800 A CN 201710299800A CN 108786798 A CN108786798 A CN 108786798A
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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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- 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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- 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 preparation methods of catalyst for dehydrogenation of low-carbon paraffin, including following content：（1）Prepare Pt-Sn maceration extracts：The soluble-salt for taking appropriate platinum, is dissolved in deionized water, then the soluble salt of tin is added into the solution, stirs evenly, appropriate ethylenediamine tetra-acetic acid is added into solution, stirs evenly, and Pt-Sn maceration extracts are made；（2）Use step（1）Obtained maceration extract impregnated carrier, dry, then the second promoter metal is loaded on carrier, obtains final catalyst by roasting.Pt and Sn are carried on carrier surface by the present invention by the way that total immersion method is complexed, and make catalyst that can still keep greater activity under higher carbon deposition quantity, are extended one way operation cycle of catalyst, are reduced device operating cost.
Description
Technical field
The present invention relates to a kind of preparation methods of catalyst for dehydrogenation of low-carbon paraffin.
Background technology
The exploitation of North America shale gas already leads to Gas Prices declining to a great extent relative to crude oil price, and in shale gas
A large amount of condensed liquid（NGLs）Yield also increases rapidly.The low-carbon alkanes such as ethane, propane, butane are rich in shale gas condensed liquid,
Ethane can be used as cracking stock to produce ethylene, therefore the demand of propylene rapid growth has only been unable to by FCC technologies.It will be natural
Gas（Conventional gas, shale gas, coal bed gas, combustible ice etc.）In dehydrogenating low-carbon alkane preparing low-carbon olefins be solve this ask
The effective way of topic.And it is increasingly deficient with petroleum resources, the production of propylene is raw material to original from the simple oil that relies on
Expect the diversified technology path transformation in source, is increasingly becoming a kind of trend.In recent years, the technology of dehydrogenating propane production propylene
The technology development for achieving large development, especially dehydrogenating propane (PDH) propylene processed is very fast, has become the third-largest production of propylene
Method.
Currently, dehydrogenating low-carbon alkane technology includes mainly：Anaerobic dehydrogenation and aerobic dehydrogenation two major classes.In anaerobic dehydrogenation technology
Again based on Pt systems noble metal dehydrogenation technology and Cr systems De-hydrogen Technology.Main anaerobic dehydrogenation technology includes in the world：Uop Inc.
Oleflex techniques, the Catofin techniques of ABB Lu Musi companies, the Star techniques of Kang Fei (Uhde) company,
The FBD-4 techniques of Snamprogetti/Yarsintz companies, PDH techniques of Lin De/BASF AG etc..Wherein with Catofin
The leading technology technology employed in new device is had become with Oleflex techniques.Catalyst is used in Oleflex techniques
Pt systems noble metal catalyst, catalyst used in Catafin techniques are Cr systems dehydrogenation.Aerobic De-hydrogen Technology there is no work
Industry example.
In the research process of noble metal dehydrogenation catalyst, people find that a small amount of Pt, Ir, Ru, Re are distributed to very early
Al with high-specific surface area2O3、SiO2On just have higher dehydrogenation activity.These catalyst initial activities are very high, but can be rapid
Carbon distribution inactivates, and reaction selectivity is poor, and the side reactions such as hydrogenolysis are more.The main reason for Pt catalyst inactivations is carbon distribution and sintering.Carbon distribution
It can be inhibited by reducing carrier acid amount, the sintering of Pt particles is then avoided by introducing Sn components.By studying for many years, people
Sum up Pt-Sn/ Al2O3The effect of Sn components in catalyst：（1）Catalyst surface Pt granularities are made to reduce by geometric effect
To promote the dispersion of Pt；（2）Make the enrichment of catalyst surface Pt charges by electronic effect to promote the de- of carbon distribution predecessor
It is attached；（3）Be conducive to catalyst surface carbon distribution to be migrated to carrier position by metal position；（4）Change the phase interaction between metal and carrier
With；（5）The generation for promoting Hydrogen spillover is disappeared carbon ability with maintaining catalyst activity and improving catalyst；（6）Regulating catalyst surface
It is acid；（7）Contribute to Pt to be anchored on SnOX and forms Pt-SnOX-Al2O3" sandwich " structure.
About the incorporation way of Sn components, there are many approach.Conventional method is made of by the soluble precursor of Sn components
Solution, dip loading individually load or grade mutual load with Pt groups on carrier, as Chinese patent CN96117222.3,
CN98114083.1 etc..《It is catalyzed journal》（1987, volume 8, the 4th phase）"Pt-Sn/Al2O3The existence of Sn in catalyst
It is referred to a kind of solvay-type dehydrogenation in influence to dehydrogenating propane reaction ", is shown in dehydrogenating propane reaction excellent
Performance.It is referred in CN87101513A and CN200910011770.5, CN200910011771.X, CN200910011772.4
Dehydrogenation Sn components are introduced during alumina catalyst support plastic.CN201410841699.4 discloses one kind
The presoma of Sn is added in the Nano sol of Pt and is sufficiently mixed by the preparation method of dehydrogenation, then also through sodium borohydride
Original obtains the Pt Nano sols containing Sn, then other auxiliary agents and impregnated carrier are added into colloidal sol.In the prior art, Pt, Sn and load
Interaction and position between body do not illustrate mostly.How to make to form better position relationship between Pt, Sn and carrier, from
And improve the anti-carbon deposition ability of catalyst and reduce the influence that carbon deposit brings catalytic activity, it is that the technology to be solved always is asked
Topic.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of preparation method of catalyst for dehydrogenation of low-carbon paraffin, passes through network
It amounts to leaching method and Pt and Sn is carried on carrier surface, make catalyst that can still keep greater activity under higher carbon deposition quantity, extend
One way operation cycle of catalyst, reduce device operating cost.
The preparation method of the catalyst for dehydrogenation of low-carbon paraffin of the present invention, including following content：
（1）Prepare Pt-Sn maceration extracts：The soluble salt for taking appropriate platinum, is dissolved in deionized water, then into the solution be added tin can
Dissolved salt stirs evenly, and appropriate ethylenediamine tetra-acetic acid is added into solution（EDTA）, stir evenly, Pt-Sn maceration extracts be made.
（2）Use step（1）Obtained maceration extract impregnated carrier, dry, then the second promoter metal is loaded to load by roasting
On body, final catalyst is obtained.
In the method for the present invention, the mass concentration of Pt is 0.001% ~ 0.8%, preferably 0.025% ~ 0.5% in Pt-Sn maceration extracts；
The mass concentration of Sn is 0.001% ~ 4%, preferably 0.05% ~ 2%；EDTA mass concentrations are 0.003% ~ 5%, preferably 0.01% ~ 4.5%.
In the method for the present invention, the compound containing platinum can be one kind or several in chloroplatinic acid, chloramine platinum or platinum nitrate
Kind, preferably chloroplatinic acid；The soluble salt of tin can be one or more of butter of tin, tin oxalate or stannous sulfate, preferably four
Stannic chloride.
In the method for the present invention, the mass ratio of maceration extract and carrier is 2:1~4:1；The dip time is 1 ~ 20 hour,
It is preferred that 3 ~ 10 hours；
In the method for the present invention, the carrier is activity Al2O3, crystal form can be γ, δ or θ types.Carrier can be it is spherical,
The suitable shapes such as bar shaped, microballoon or abnormity, particle equivalent diameter are generally 0.2 ~ 4mm, and preferred particle size is 0.5 ~ 2mm.
In the method for the present invention, drying temperature is 100 ~ 130 DEG C, 10 ~ 24 hours drying times；Calcination temperature is 450 ~ 550
DEG C, preferably 480 ~ 520 DEG C；Roasting time is 3 ~ 12 hours, preferably 4 ~ 6 hours.
In the method for the present invention, is known to those skilled in the art, routine may be used in the loading process of second auxiliary agent
Infusion process, dipping after be dried and roast, complete load；The second auxiliary agent presoma can be its soluble nitre
Hydrochlorate, chloride or sulfate.
The catalyst for dehydrogenation of low-carbon paraffin of the present invention has following property：Using activated alumina as carrier, Pt is activearm
Point, Sn is the first auxiliary agent, and a kind of metal selected from Li, Na, K, Fe, Ni, Cu, Zn, Ga, Mn, Ce, Mg, V is the second auxiliary agent；With
On the basis of catalyst weight, Pt is that 0.1% ~ 1%, Sn is 0.1% ~ 5% based on the element based on the element, and the second auxiliary agent is based on the element
0.5% ~ 4%, surplus is carrier.
In the method for the present invention, Pt is with Sn species by using EDTA as the active component of ligand formation macromolecular in maceration extract
Growth precursor, can be to avoid in dip loading active component, and Pt species go deep into the relatively narrow duct in gap, and are largely present in
At the larger duct in aperture.The larger duct in aperture can play higher appearance carbon effect, even if catalyst is in pyroreaction
Quickly, a large amount of carbon distribution will not be also completely clogged with soot towards the catalyst duct of dehydrogenation active component, and reactants and products are still
It can free in and out, to make catalyst that can still keep greater activity under higher carbon deposition quantity, extend the one way fortune of catalyst
The turn-week phase reduces device operating cost.Meanwhile the active component growth precursor of macromolecular formed in carrier surface it is close to each other
Pt and Sn cluster, generate concerted catalysis effect, have superior alkane conversion and olefine selective.
Specific implementation mode
With reference to the embodiment technical solution that the present invention will be described in detail, but the present invention is not limited to following embodiments.
Embodiment 1
Prepare Pt-Sn maceration extracts：0.68g chloroplatinic acids are dissolved in 100ml deionized waters, then crystallization is added into the solution
Butter of tin 0.74g, stirs to dissolve.3g EDTA are added into the solution again, are sufficiently stirred, Pt-Sn maceration extracts are made.
Weigh 50g ball-type γ-Al2O3Carrier is placed in Rotary Evaporators, vacuumizes 60min.Maceration extract is sucked rotation to steam
It sends out in instrument, closes vacuum pump, normal temperature and pressure impregnates 6 hours.
Then bath temperature is risen to 80 DEG C, moves into beaker, is placed in 110 DEG C of baking oven after catalyst vacuum is drained
It is 15 hours dry.Then catalyst is moved in Muffle furnace, 500 DEG C roast 5 hours.Use the aqueous solution dipping of potassium nitrate above-mentioned again
Catalyst, then final catalyst is obtained after drying, roasting.
The weight percent that each metal simple-substance accounts for carrier in the catalyst is：Pt 0.5wt%, Sn 0.5wt%, K
0.8wt%, the catalyst are denoted as A.
Comparative example 1
Dehydrogenation is prepared according to the patent CN87101513A methods disclosed.Each metal simple-substance accounts for carrier in the catalyst
Weight percent is：Pt 0.5wt%, Sn 0.5wt%, K 0.8wt%, the catalyst are denoted as B1.
Comparative example 2
0.68g chloroplatinic acids are dissolved in 100ml deionized waters, then stannic chloride pentahydrate 0.74g is added into the solution, are stirred
It mixes and makes it dissolve, Pt-Sn mixed impregnant liquors are made.
Weigh 50g ball-type γ-Al2O3Carrier is placed in Rotary Evaporators, vacuumizes 60min.Maceration extract is sucked rotation to steam
It sends out in instrument, closes vacuum pump, normal temperature and pressure impregnates 6 hours.
Then bath temperature is risen to 80 DEG C, moves into beaker, is placed in 110 DEG C of baking oven after catalyst vacuum is drained
It is 15 hours dry.Then catalyst is moved in Muffle furnace, 500 DEG C roast 5 hours.Use the aqueous solution dipping of potassium nitrate above-mentioned again
Catalyst, then final catalyst is obtained after drying, roasting.
The weight percent that each metal simple-substance accounts for carrier in the catalyst is：Pt 0.5wt%, Sn 0.5wt%, K
0.8wt%, the catalyst are denoted as B2.
Comparative example 3
Prepare the γ-Al containing Sn2O3Carrier：The aluminum trichloride solution of a certain amount of 0.98M and 0.01M butter of tin solution are mixed
After conjunction, a certain amount of 8% ammonium hydroxide is added, is uniformly mixed in neutralizing tank at 60 ~ 80 DEG C, control ph 7.0 ~ 9.0, filtering, water
After washing, being acidified, balling-up of pressurizeing in oil ammonia column, by drying, aging, it to get grain size is 1.5mm that 4 hours are roasted at 650 ~ 750 DEG C
The 0.5wt% containing Sn ball-type aluminium oxide.
0.68g chloroplatinic acids are dissolved in 100ml deionized waters, 50g ball-type γ-Al are weighed2O3Carrier is placed in rotation and steams
It sends out in instrument, vacuumizes 60min.Platinum acid chloride solution is sucked in Rotary Evaporators, vacuum pump is closed, normal temperature and pressure impregnates 6 hours.
Then bath temperature is risen to 80 DEG C, moves into beaker, is placed in 110 DEG C of baking oven after catalyst vacuum is drained
It is 15 hours dry.Then catalyst is moved in Muffle furnace, 500 DEG C roast 5 hours.Use the aqueous solution dipping of potassium nitrate above-mentioned again
Catalyst, then final catalyst is obtained after drying, roasting.
The weight percent that each metal simple-substance accounts for carrier in the catalyst is：Pt 0.5wt%, Sn 0.5wt%, K
0.8wt%, the catalyst are denoted as B3.
Comparative example 4
0.74g stannic chloride pentahydrates are dissolved in 100mL deionized waters, 50g ball-type γ-Al are weighed2O3Carrier is placed in rotation and steams
It sends out in instrument, vacuumizes 60min.Platinum acid chloride solution is sucked in Rotary Evaporators, vacuum pump is closed, normal temperature and pressure impregnates 6 hours.
Then bath temperature is risen to 80 DEG C, moves into beaker, is placed in 110 DEG C of baking oven after catalyst vacuum is drained
It is 15 hours dry.Then catalyst is moved in Muffle furnace, 500 DEG C roast 5 hours.
0.68g chloroplatinic acids are dissolved in 100ml deionized waters, above-mentioned carrier is impregnated.Dipping, dry and method of roasting
Ibid.It uses the aqueous solution of potassium nitrate to impregnate above-mentioned catalyst again, then obtains final catalyst after drying, roasting.
The weight percent that each metal simple-substance accounts for carrier in the catalyst is：Pt 0.5wt%, Sn 0.5wt%, K
0.8wt%, the catalyst are denoted as B4.
Embodiment 2
Prepare Pt-Sn maceration extracts：0.41g chloroplatinic acids are dissolved in 100ml deionized waters, then crystallization is added into the solution
Butter of tin 1.5g, stirs to dissolve.4g EDTA are added into the solution again, are sufficiently stirred, Pt-Sn maceration extracts are made.
Weigh 50g ball-type θ-Al2O3Carrier is placed in Rotary Evaporators, vacuumizes 50min.Maceration extract is sucked rotation to steam
It sends out in instrument, closes vacuum pump, normal temperature and pressure impregnates 5 hours.
Then bath temperature is risen to 70 DEG C, moves into beaker, is placed in 120 DEG C of baking oven after catalyst vacuum is drained
It is 11 hours dry.Then catalyst is moved in Muffle furnace, 510 DEG C roast 4 hours.Use the aqueous solution dipping of zinc nitrate above-mentioned again
Catalyst, then final catalyst is obtained after drying, roasting.
The weight percent that each metal simple-substance accounts for carrier in the catalyst is：Pt 0.3wt%, Sn 1wt%, Zn
0.75wt%, the catalyst are denoted as C.
Embodiment 3
Prepare Pt-Sn maceration extracts：0.82g chloroplatinic acids are dissolved in 100ml deionized waters, then crystallization is added into the solution
Butter of tin 0.44g, stirs to dissolve.3g EDTA are added into the solution again, are sufficiently stirred, Pt-Sn maceration extracts are made.
Weigh 50g ball-type γ-Al2O3Carrier is placed in Rotary Evaporators, vacuumizes 60min.Maceration extract is sucked rotation to steam
It sends out in instrument, closes vacuum pump, normal temperature and pressure impregnates 7 hours.
Then bath temperature is risen to 85 DEG C, moves into beaker, is placed in 110 DEG C of baking oven after catalyst vacuum is drained
It is 10 hours dry.Then catalyst is moved in Muffle furnace, 520 DEG C roast 3 hours.Use the aqueous solution dipping of gallium nitrate above-mentioned again
Catalyst, then final catalyst is obtained after drying, roasting.
The weight percent that each metal simple-substance accounts for carrier in the catalyst is：Pt 0.7wt%, Sn 0.3wt%, Ga
0.4wt%, the catalyst are denoted as D.
Embodiment 4
It takes catalyst prepared by above example and comparative example to carry out conventional hydrothermal dechlorination, and carries out propane in micro-reactor and take off
Hydrogen evaluation experimental.
The activation condition of catalyst：With 100% hydrogen, 500 DEG C of constant temperature 2 hours.Also the volume space velocity of Primordial Qi is 3000h-1。
The passivating conditions of catalyst：The mass velocity 1200h of the mixing gas of hydrogen sulfide and nitrogen-1, volume ratio 1:
5,500 DEG C of temperature, passivation time 1 hour.
Evaluation condition：Catalyst volume 6.0ml, volume space velocity 850h-1, reaction pressure normal pressure, reaction temperature 620
DEG C, hydrogen:The volume ratio of propane is 1:1.Catalyst is initial and 96 hours propane one way molar yields and Propylene Selectivity
It is listed in table 1.
1 embodiment of table and comparative example evaluating catalyst result.
As can be seen from the above data, there is higher conversion of propane and third using catalyst prepared by the method for the present invention
Alkene selectivity, this has benefited from the concerted catalysis effect that Pt-Sn components close to each other in catalyst generate.And the present invention is catalyzed
After reaction 96 hours, activity is less compared with initial reaction stage reduction for agent, this has benefited from the work that macromolecular is formed using EDTA as ligand
Property component growth precursor, avoids in dip loading active component, and Pt-Sn species go deep into the relatively narrow carrier duct in gap,
And be present at the larger aperture that can play higher appearance carbon effect, even if catalyst is quick in pyroreaction, a large amount of
Carbon distribution, will not be also completely clogged with soot towards the catalyst duct of dehydrogenation active component.
Claims (10)
1. a kind of preparation method of catalyst for dehydrogenation of low-carbon paraffin, it is characterised in that including following content：（1）Prepare Pt-Sn leachings
Stain liquid：The soluble salt for taking appropriate platinum, is dissolved in deionized water, then the soluble salt of tin is added into the solution, stirs evenly, Xiang Rong
Appropriate ethylenediamine tetra-acetic acid is added in liquid, stirs evenly, Pt-Sn maceration extracts are made；（2）Use step（1）Obtained maceration extract leaching
Stain alumina support, dry, then the second promoter metal is loaded on carrier, obtains final catalyst by roasting.
2. according to the method for claim 1, it is characterised in that：In Pt-Sn maceration extracts the mass concentration of Pt be 0.001% ~
0.8%, preferably 0.025% ~ 0.5%；The mass concentration of Sn is 0.001% ~ 4%, preferably 0.05% ~ 2%；The quality of ethylenediamine tetra-acetic acid
A concentration of 0.003% ~ 5%, preferably 0.01% ~ 4.5%.
3. according to the method for claim 1, it is characterised in that：In Pt-Sn maceration extracts the mass concentration of Pt be 0.025% ~
0.5%；The mass concentration of Sn is 0.05% ~ 2%；The mass concentration of ethylenediamine tetra-acetic acid is 0.01% ~ 4.5%.
4. according to the method for claim 1, it is characterised in that：The compound containing platinum is chloroplatinic acid, chloramine platinum or nitre
One or more of sour platinum.
5. according to the method for claim 1, it is characterised in that：The soluble salt of tin is that butter of tin, tin oxalate or sulfuric acid are sub-
One or more of tin.
6. according to the method for claim 1, it is characterised in that：The mass ratio of maceration extract and carrier is 2:1~4:1；Described
Dip time is 1 ~ 20 hour.
7. according to the method for claim 1, it is characterised in that：The carrier is activity Al2O3, crystal form is γ, δ or θ
Type；Particle equivalent diameter is 0.2 ~ 4mm.
8. according to the method for claim 1, it is characterised in that：Drying temperature is 100 ~ 130 DEG C, and drying time 10 ~ 24 is small
When.
9. according to the method for claim 1, it is characterised in that：Calcination temperature is 450 ~ 550 DEG C, and roasting time is 3 ~ 12 small
When.
10. according to catalyst for dehydrogenation of low-carbon paraffin prepared by the method described in claim 1 ~ 9 any claim, feature exists
In：Using activated alumina as carrier, Pt is active component, and Sn is the first auxiliary agent, one kind selected from Li, Na, K, Fe, Ni, Cu, Zn,
The metal of Ga, Mn, Ce, Mg, V are the second auxiliary agent；On the basis of catalyst weight, Pt is 0.1% ~ 1%, Sn based on the element with element
It is calculated as 0.1% ~ 5%, the second auxiliary agent is based on the element 0.5% ~ 4%, and surplus is carrier.
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| WO2024008169A1 (en) * | 2022-07-07 | 2024-01-11 | 润和科华催化剂(上海)有限公司 | Low-carbon alkane dehydrogenation catalyst, preparation method therefor and application thereof |
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