CN106861765A - A kind of preparation method of low-carbon alkane dehydrogenation catalyst carrier - Google Patents
A kind of preparation method of low-carbon alkane dehydrogenation catalyst carrier Download PDFInfo
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- CN106861765A CN106861765A CN201510919711.3A CN201510919711A CN106861765A CN 106861765 A CN106861765 A CN 106861765A CN 201510919711 A CN201510919711 A CN 201510919711A CN 106861765 A CN106861765 A CN 106861765A
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/745—Iron
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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
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/8966—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with germanium, tin or lead
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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
- C07C5/3332—Catalytic processes with metal oxides or metal sulfides
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Abstract
The present invention relates to a kind of preparation method of low-carbon alkanes (C3-C6) catalysis dehydrogenation agent carrier, with ammoniacal liquor as precipitating reagent, iron aluminium composite oxide carrier is prepared using the method for co-precipitation.Catalyst is prepared by vacuum-impregnated method using this carrier, the active component in catalyst is Pt, Sn, K are modulating agent, and load capacity is respectively：Pt0.1~1.0wt.%, Sn0.2~5.0wt.%, K0.1~3wt.%, preferably load capacity are:Pt0.3~0.7wt.%, Sn0.5~3.0wt.%, K0.3~1.5wt.%.This catalyst is primarily useful in the reaction that C3-C6 dehydrating alkanes produce corresponding alkene.The iron more conventional alumina support of aluminium composite oxide carrier prepared by the present invention has significant raising in terms of reactivity, catalyst stability, and preferably activity and stability are also shown compared to commercialized aluminum oxide.
Description
Technical field
The present invention relates to a kind of preparation method of low-carbon alkane dehydrogenation catalyst carrier.This carrier is mainly used in low
Carbon alkane dehydrogenation is produced in the preparation process of the catalyst of corresponding alkene.
Background technology
During dehydrating alkanes produce corresponding alkene, generally from Al2O3As carrier, but due to oxygen
Changing has acid centre on aluminium, often cause and hydrogenolysis, isomerization, coking etc. occur during dehydrating alkanes
Side reaction, the selectivity for causing catalyst is reduced, carbon distribution is inactivated.The composite oxides for preparing Fe doping are carried
Body, can be with modulation Al2O3Acid centre, contribute to the dispersion of active component, it is possible to reduce side reaction
Occur, improve the activity and stability of catalyst.
Industrially during dehydrogenating low-carbon alkane, the platinum group catalyst of alumina load has been obtained widely
Using.However, due to there is the side reactions such as cracking, hydrogenolysis, isomerization, the dehydrogenation selection of these catalyst
Property is relatively low.In addition, these catalyst are also easily influenceed and are inactivated by the sintering of carbon distribution and the platinum particles of load.
Therefore, substantial amounts of research has been done on the dehydrogenation of catalyst around how improving.At present, it is widely used
Catalyst for dehydrogenation of low-carbon paraffin is generally platinum group catalyst, and carrier is generally aluminum oxide, and catalyst surface is due to a small amount of
The presence of middle strong acid, dehydrogenation reaction process is often accompanied by side reaction generation, causes area carbon, so that catalysis
Agent is inactivated.In catalyst preparation process, the general method being modified by catalyst surface is (as introduced alkali gold
Category auxiliary agent K, Na etc.) weaken the acid centre number of catalyst, suppress side reaction and improve to be catalyzed to reach
The purpose in agent life-span.Improved except adding metal component in the catalyst in addition to its catalytic performance, in aluminum oxide
Another oxide is added in carrier and has also obtained certain research preparing composite oxide carrier.In recent years,
Many research institutions report, and ZnO, MgO etc. are added in aluminum oxide and prepares composite oxide carrier,
During dehydrogenating low-carbon alkane, catalyst has activity and stability well.At present it has been reported that
The patent of alkane dehydrogenating catalyst support modification has a lot, such as：United States Patent (USP)：US2014275686-A1,
US2013072739-A1；European patent：EP2794091-A1,EP2712675-A1,
EP2689843-A1；Chinese patent：CN103990454-A,CN104289220-A,
CN103787810-A etc., and it is little about the patent of iron aluminium composite oxide carrier.It is de- from low-carbon alkanes
Domestic and international scientific research institution is can be seen that in the exploitation and development of hydrogen catalyst and studying height always using unit
The catalyst of catalysis activity and stability, but many research be only limitted to from the active component of catalyst load and
Carrying method is set about, and the selection of carrier is confined to the aluminum oxide of distinct methods preparation, and aluminum oxide is mixed
Miscellaneous modified research is less.
The content of the invention
It is an object of the invention to provide a kind of support preparation method of catalyst for dehydrogenation of low-carbon paraffin, present invention system
Standby catalyst carrier has more preferable compared with the catalyst of the regular oxidation alumina supporter prepared under the conditions of
Activity and stability.
A kind of preparation method of low-carbon alkane dehydrogenation catalyst carrier, the carrier of catalyst is prepared as iron aluminium and is combined
Prepared by salting liquid coprecipitation, comprise the following steps：
(1) soluble molysite and aluminum salt solution is prepared, a certain amount is taken and is placed in reactor, water-bath control
30-50 DEG C of reaction temperature processed；[Al/Fe] mol ratio is 20-200 in salting liquid.
(2) to ammoniacal liquor being added dropwise in reactor and stirring, regulation system pH value to 8-12, stop that ammonia is added dropwise
Water, continues to stir 30-60 minutes, stops stirring aging 2-6 hours again, plastic.
(3) after cemented into bundles, through filtering, washing, dries and roasting is obtained iron aluminium composite oxide
(Fe-Al-O) carrier.
Step 1) the soluble iron salting liquid be Fe (NO3)3Or FeCl3Aqueous solution one kind therein or two
Kind, step 1) the soluble aluminum salting liquid be Al (NO3)3Or AlCl3One or two in the aqueous solution,
Iron ion and aluminum ions concentration are 1.0-3.0mol/L in molysite and aluminum salt solution., in salting liquid [Al/Fe]
Mol ratio is preferably 25-65.
When molysite and aluminium salt mixed solution volume be 0.5-1.5L when, step 2) described in ammoniacal liquor with 80-200
The speed of drop/minute is added drop-wise in composite compaction technique.
Step 2) described in ammoniacal liquor mass concentration be 3%-15%, preferably 5%-10%.
Step 2) aging temperature is stood for 30-50 DEG C.
Step 3) after the solution gel filtration, after the wet glue of gained is washed with deionized water or ethanol, place
4-16h, 2-10 hours prepared carrier of 500-700 DEG C of roasting are dried in 100-130 DEG C of baking oven.
Step 2) described in ammoniacal liquor preferred mass concentration be 8%.
The present invention is used as the dehydrogenation of low-carbon alkanes using iron aluminium composite oxide prepared by coprecipitation
Carrier；Catalyst constitutes percentage by weight：Pt0.1~1.0wt.%, Sn0.2~5.0wt.%, K0.1~3wt.%,
Preferably load capacity is:Pt0.3~0.7wt.%, Sn0.5~3.0wt.%, K0.3~1.5wt.%.Remaining is iron
Aluminum oxide.
The preparation method of catalyst of the present invention is as follows：
Catalyst is prepared using infusion process：
(1) resulting vehicle will be prepared to be placed in vacuum impregnation device, carries out vacuum pre-treatment；
(2) appropriate hydrochloric acid solution is added to be made leaching after mixing platinum salt, stannous chloride, Klorvess Liquid
Stain liquid.
After impregnation drying, by the sample after roasting, hydrogen is also in reduction furnace under 400-600 DEG C of constant temperature
It is former 1-5 hours, the gas hourly space velocity 5000-15000h of hydrogen-1, hydrogen is aqueous less than 20ppm, pure
Degree>99.9%.The catalyst that corresponding alkene is produced for dehydrogenating low-carbon alkane can be prepared after reduction.
The present invention is a kind of catalyst carrier for C3-C6 dehydrogenating low-carbon alkanes, with ammoniacal liquor as precipitating reagent,
Prepared using coprecipitation method.Carrier is iron aluminium composite oxide, using this carrier by vacuum-impregnated
Method prepares catalyst, and the active component in catalyst is Pt, and Sn, K are modulating agent, and load capacity is respectively：
Pt0.1~1.0wt.%, Sn0.2~5.0wt.%, K0.1~3wt.%, preferably load capacity
For:Pt0.3~0.7wt.%, Sn0.5~3.0wt.%, K0.3~1.5wt.%.This catalyst is mainly used in low-carbon (LC)
During the corresponding alkene of alkane (C3-C6) dehydrogenation system.The iron aluminium composite oxide prepared using the present invention
During as catalyst carrier compared with same method prepare aluminum oxide be used as carrier when catalyst reactivity,
Catalyst stability aspect has significant raising.Preferable work is also shown compared to commercialized aluminum oxide
Property and stability.
Brief description of the drawings
Fig. 1 is the yield anaplasia at any time of the catalyst preparing isobutene through dehydrogenation of iso-butane described in embodiment 8
Change figure, ordinate is respectively the yield of isobutene, and abscissa is the time, and unit is hour (h).
Fig. 2 is that catalyst n-hexane conversion rate of dehydrogenation changes over time figure described in embodiment 9, indulges and sits
The conversion ratio of n-hexane is designated as, abscissa is the time, and unit is hour (h).
Specific embodiment
Below by embodiment further instruction is given to technology of the invention.
Embodiment 1：The preparation of alumina support
Take the Al (NO that molar concentration is 2mol/L3)3Solution 600mL is added in the reactor of 2000mL,
Maintain temperature constant at 40 DEG C, (300r/min) is constantly stirred under suitable rotating speed using agitating paddle,
Take the concentrated ammonia liquor that mass fraction is 25%, dilute three times, during it slowly to pump into mixing salt solution, speed
Control is in or so 100 drop/minutes.Until pH value of solution reaches 10, stop that ammoniacal liquor is added dropwise, stirring stablizes 60
Minute, solution is filtered after 40 DEG C of aging 4h of standing after stopping stirring, and is repeatedly washed with deionized water
Wash.Then 12h is dried at 120 DEG C, dried solid is in Muffle furnace with the heating rate of 5 DEG C/min
Constant temperature calcining 4h is obtained respective carrier after rising to 600 DEG C.
Embodiment 2：It is prepared by composite oxide carrier one
Take the Al (NO of 660mL1.33mol/L3)3Solution, the Fe (NO of 4.6mL1.23mol/L3)3Solution,
It is added in the reactor of 2000mL, maintains temperature constant at 40 DEG C, is suitably being turned using agitating paddle
(300r/min) is constantly stirred under speed, takes the concentrated ammonia liquor that mass fraction is 25%, three times is diluted, by it
Slowly pump into mixing salt solution, speed control is in or so 100 drop/minutes.Until pH value of solution reaches
10, stop that ammoniacal liquor is added dropwise, stirring is stablized 60 minutes, and solution stands aging 4h at 40 DEG C after stopping stirring
After filter, and repeatedly washed with deionized water.Then 12h, dried solid are dried at 120 DEG C
Constant temperature calcining 4h is obtained corresponding compound after rising to 600 DEG C with the heating rate of 5 DEG C/min in Muffle furnace
Oxide carrier one.
Embodiment 3：It is prepared by composite oxide carrier two
Take the Al (NO of 600mL1.32mol/L3)3Solution, the Fe (NO of 17.1mL1.23mol/L3)3It is molten
Liquid, is added in the reactor of 2000mL, maintains temperature constant at 40 DEG C, using agitating paddle suitable
Rotating speed under (300r/min) constantly stir, take the concentrated ammonia liquor that mass fraction is 25%, dilute three times,
It is slowly pumped into mixing salt solution, speed control is in or so 100 drop/minutes.Until pH value of solution reaches
To 10, stop that ammoniacal liquor is added dropwise, stirring is stablized 60 minutes, and solution is aging in 40 DEG C of standings after stopping stirring
Filtered after 4h, and repeatedly washed with deionized water.Then 12h is dried at 120 DEG C, it is dried
Constant temperature calcining 4h is obtained accordingly after solid rises to 600 DEG C in Muffle furnace with the heating rate of 5 DEG C/min
Composite oxide carrier two.
Embodiment 4：Aluminum oxide is the preparation of the catalyst of carrier
The alumina support grinding that will be obtained in embodiment 1, screening obtains the particle of 20~40 mesh.Weigh
The 5g alumina particles are placed in vacuum impregnation device, while taking the chloroplatinic acid aqueous solution of the grams per milliliter of platiniferous 0.06
0.42 milliliter, 0.4 milliliter of concentrated hydrochloric acid, 0.75 milliliter of the stannous chloride aqueous solution of stanniferous 0.1 grams per milliliter,
1.25 milliliters of the potassium chloride solution containing the grams per milliliter of potassium 0.02, above-mentioned maceration extract is added to equipped with the true of carrier
In empty infuser, the uniform rear 120 DEG C of dryings of dipping 2 hours, 580 DEG C are calcined 4 hours in Muffle furnace,
With the aqueous pure hydrogen (purity less than 20ppm>99.9%), in 530 DEG C of reductase 12s hour.Gained is catalyzed
Agent is constituted：Platinum：0.5%, tin：1.5%, potassium：0.5% (to vehicle weight).
Embodiment 5：The preparation of the correspondence catalyst of composite oxide carrier one
The composite oxide carrier grinding that will be obtained in embodiment 2, screening obtains the particle of 20~40 mesh.
Weigh the 5g composite oxide particles to be placed in vacuum impregnation device, while taking the chlorine platinum of the grams per milliliter of platiniferous 0.06
0.42 milliliter of aqueous acid, 0.4 milliliter of concentrated hydrochloric acid, the stannous chloride aqueous solution 0.75 of stanniferous 0.1 grams per milliliter
Be added to above-mentioned maceration extract equipped with load by milliliter, 1.25 milliliters of the potassium chloride solution containing the grams per milliliter of potassium 0.02
In the vacuum impregnation device of body, the uniform rear 120 DEG C of dryings of dipping 2 hours, 580 DEG C of roastings 4 in Muffle furnace
Hour, with the aqueous pure hydrogen (purity less than 20ppm>99.9%), in 530 DEG C of reductase 12s hour.Institute
Obtaining catalyst composition is：Platinum：0.5%, tin：1.5%, potassium：0.5% (to vehicle weight).
Embodiment 6：The preparation of the correspondence catalyst of composite oxide carrier two
The composite oxide carrier grinding that will be obtained in embodiment 3, screening obtains the particle of 20~40 mesh.
Weigh the 5g composite oxide particles to be placed in vacuum impregnation device, while taking the chlorine platinum of the grams per milliliter of platiniferous 0.06
0.42 milliliter of aqueous acid, 0.4 milliliter of concentrated hydrochloric acid, the stannous chloride aqueous solution 0.75 of stanniferous 0.1 grams per milliliter
Be added to above-mentioned maceration extract equipped with load by milliliter, 1.25 milliliters of the potassium chloride solution containing the grams per milliliter of potassium 0.02
In the vacuum impregnation device of body, the uniform rear 120 DEG C of dryings of dipping 2 hours, 580 DEG C of roastings 4 in Muffle furnace
Hour, with the aqueous pure hydrogen (purity less than 20ppm>99.9%), in 530 DEG C of reductase 12s hour.Institute
Obtaining catalyst composition is：Platinum：0.5%, tin：1.5%, potassium：0.5% (to vehicle weight).
Embodiment 7：Commercial oxidation aluminium is the preparation of the catalyst of carrier
The grinding of commercial oxidation alumina supporter, screening are obtained into the particle of 20~40 mesh.Weigh the 5g aluminum oxide
Particle is placed in vacuum impregnation device, while 0.42 milliliter of the chloroplatinic acid aqueous solution of the grams per milliliter of platiniferous 0.06 is taken,
0.4 milliliter of concentrated hydrochloric acid, 0.75 milliliter of the stannous chloride aqueous solution of stanniferous 0.1 grams per milliliter, containing 0.02 gram of potassium
1.25 milliliters of the potassium chloride solution of/milliliter, above-mentioned maceration extract is added in the vacuum impregnation device equipped with carrier,
The uniform rear 120 DEG C of dryings of dipping 2 hours, 580 DEG C are calcined 4 hours in Muffle furnace, are less than with aqueous
Pure hydrogen (the purity of 20ppm>99.9%), in 530 DEG C of reductase 12s hour.Gained catalyst is constituted：Platinum：
0.5%, tin：1.5%, potassium：0.5% (to vehicle weight).
Embodiment 8：Dehydrogenation of isobutane catalyst reaction Performance
To embodiment 4, embodiment 5, embodiment 6 and embodiment 7 on quartz tube type fixed bed reactors
The catalyst of preparation carries out dehydrogenation of isobutane reactivity worth evaluation.Loaded catalyst 0.3g (0.6mL),
In H2Under the conditions of, 580 DEG C are warming up to the heating rate of 5 DEG C/min, reductase 12 hour is passed through afterwards
Iso-butane, reaction condition is：580 DEG C of temperature, pressure is normal pressure, WHSV=2h-1, H/C=1.Reaction is produced
Thing passes through gas-chromatography Agilent 7890A on-line analyses, and chromatographic condition is：180 DEG C of injector temperature, post
105 DEG C of case temperature, 200 DEG C of fid detector temperature, chromatographic column HP-Al/KCl.Catalyst isobutyl
The isobutene yield relation of changing with time of alkane dehydrogenation reaction is shown in Fig. 1.
Embodiment 9：N-hexane dehydrogenation reactivity worth is investigated
1.26 grams of the catalyst (1.5mL) of embodiment 6 and embodiment 7 is weighed, loads reactor, in H2
Under the conditions of, 530 DEG C are warming up to, reduce 6 hours, GHSV=2000h-1.Start to pump into n-hexane afterwards,
Reacted, reaction condition is：530 DEG C of temperature, pressure 0.1MPa, the volume space velocity during liquid of n-hexane
It is 5h-1, H2It is 2 with the mol ratio of n-hexane.Maintain the hexane conversion rate 20% of each catalyst with
Under conditions of upper, the service life of each catalyst is investigated.The conversion ratio of catalyst n-hexane dehydrogenation reaction
See Fig. 2.
Claims (6)
1. a kind of preparation method of low-carbon alkane dehydrogenation catalyst carrier, it is characterised in that：Catalyst
Carrier is prepared as the preparation of iron aluminium composite compaction technique coprecipitation, comprises the following steps：
(1) soluble molysite and aluminum salt solution is prepared, is placed in reactor, water-bath control reaction
30-50 DEG C of temperature；[Al/Fe] mol ratio is 20-200 in salting liquid；
(2) to ammoniacal liquor being added dropwise in reactor and stirring, regulation system pH value to 8-12, drop is stopped
Ammonification water, continues to stir 30-60 minutes, then aging 2-6 hours, plastic；
(3) after cemented into bundles, through filtering, washing, dries and roasting is obtained iron aluminium composite oxide
Carrier.
2. according to the preparation method of catalyst carrier described in claim 1, it is characterised in that：Step 1)
The soluble iron salting liquid is Fe (NO3)3Or FeCl3The aqueous solution it is therein one or two, it is soluble
Aluminum salt solution is Al (NO3)3Or AlCl3One or two in the aqueous solution, iron in molysite and aluminum salt solution
Ion and aluminum ions concentration are respectively 1.0-3.0mol/L.
3. according to the preparation method of catalyst carrier described in claim 1 or 2, it is characterised in that：
[Al/Fe] mol ratio is preferably 25-65 in salting liquid.
4. according to the preparation method of catalyst carrier described in claim 1, it is characterised in that：Work as molysite
When with the volume of aluminium salt mixed solution being 0.5-1.5L, step 2) described in ammoniacal liquor with 80-200 drops/point
The speed of clock is added drop-wise in composite compaction technique；Ammoniacal liquor mass concentration is 3%-15%, preferably 5%-10%.
5. according to the preparation method of catalyst carrier described in claim 1, it is characterised in that：Step 2)
It is 30-50 DEG C to stand aging temperature.
6. according to the preparation method of catalyst carrier described in claim 1, it is characterised in that：Step 3)
After the gel filtration, after the wet glue of gained is washed with deionized water or ethanol, 100-130 DEG C of baking is positioned over
4-16h, 2-10 hours prepared carrier of 500-700 DEG C of roasting are dried in case.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103394349A (en) * | 2013-07-26 | 2013-11-20 | 中国石油大学(华东) | Catalyst for dehydrogenation of light alkane and preparation method of catalyst |
| CN103990454A (en) * | 2014-05-20 | 2014-08-20 | 南京沃来德能源科技有限公司 | Low-carbon alkane dehydrogenation catalyst as well as preparation method and low-carbon alkane dehydrogenation process thereof |
| CN104923227A (en) * | 2015-05-29 | 2015-09-23 | 南开大学 | Relatively high-stability catalyst for propylene preparation by propane dehydrogenation and preparation method for catalyst |
-
2015
- 2015-12-13 CN CN201510919711.3A patent/CN106861765A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103394349A (en) * | 2013-07-26 | 2013-11-20 | 中国石油大学(华东) | Catalyst for dehydrogenation of light alkane and preparation method of catalyst |
| CN103990454A (en) * | 2014-05-20 | 2014-08-20 | 南京沃来德能源科技有限公司 | Low-carbon alkane dehydrogenation catalyst as well as preparation method and low-carbon alkane dehydrogenation process thereof |
| CN104923227A (en) * | 2015-05-29 | 2015-09-23 | 南开大学 | Relatively high-stability catalyst for propylene preparation by propane dehydrogenation and preparation method for catalyst |
Non-Patent Citations (1)
| Title |
|---|
| SHINGO KOBAYASHI ET AL.: "Effect of iron oxide on isobutane dehydrogenation over Pt/Fe2O3-Al2O3 catalyst", 《APPLIED CATALYSIS A: GENERAL》 * |
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Application publication date: 20170620 |