CN105056990B - Catalyst for preparing propylene with propane dehydrogenation and preparation method thereof - Google Patents
Catalyst for preparing propylene with propane dehydrogenation and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of catalyst for preparing propylene with propane dehydrogenation, the catalyst is to contain Ta molecular sieves of MCM 68 as carrier, using Pt as main active component, using Y as helping active component.Pt content is 0.1~1.0wt% of total catalyst weight in the catalyst, and the content of the Y is 0.4~4.0wt% of total catalyst weight, and Ta content is 0.2~5.0wt% of total catalyst weight.The invention further relates to the preparation method of above-mentioned catalyst, the present invention is used as catalyst carrier using the MCM 68 containing Ta, active component is used as using Pt, Y, introducing in advance for Ta can suppress the formation of Pt Ta alloys at reaction conditions, strengthen the interaction force between Pt and carrier simultaneously, improve the stability of catalyst reaction, and Y introducing is conducive to improving decentralization and valence stability of the precious metals pt in carrier surface, and the interaction between metal promoter carrier is further improved, so as to improve the reactivity and Propylene Selectivity of catalyst.
Description
Technical field
The present invention relates to a kind of catalyst for preparing propylene with propane dehydrogenation and preparation method thereof.
Background technology
Propylene is that consumption is only second to one of important alkene of ethene in petrochemical industry, in addition to for producing polypropylene, also
It is the master for producing the products such as acrylonitrile, expoxy propane, butanol, octanol, isopropanol, oxo-alcohols, isopropylbenzene, acrylic acid, nonyl phenol
Want raw material.In recent years, the fast development with petrochemical industry and the rapid growth of downstream derivative thing demand, global propylene consumption
Measure amplification and exceed ethene.It is one of its main path produced that propylene, which is made, by De-hydrogen Technology using propane cheap and easy to get,
But realize that the key of preparing propylene by dehydrogenating propane technology is that developing the propane with high stability, high activity and high selectivity takes off
Hydrogen catalyst.The dehydrogenation developed at present mainly using aluminum oxide as carrier and adds various metal promoters, this kind of catalyst
Selectivity is higher under some reaction conditions, but due to the easy carbon distribution inactivation of catalyst under hot conditions, causes the steady of catalytic reaction
Qualitative difference, service life is shorter.
The Chinese invention patent application of Publication No. 101066532《It is a kind of using ZSM-5 molecular sieve of the skeleton containing Sn as carrier
Preparing propylene by dehydrogenating propane catalyst》(application number：200710023431.X) disclose one kind preparing ZSM-5 molecular sieve mistake
Sn is doped with journey, while using new dehydrogenating propane of the platinum family element as main active component, using alkalinous metal as auxiliary agent
Catalyst for preparing propene, the catalyst has higher catalytic reaction activity and Propylene Selectivity, while carbon accumulation resisting ability is also stronger.
Notification number is 101972664 Chinese invention patent《A kind of catalyst and its system for preparing propylene by dehydrogenating propane
It is standby》(application number：201010510192.2) one kind is disclosed with skeleton bimetallic AlSn-SBA-15 dehydrogenating propanes containing Sn and Al
The catalyst of propylene processed, it is using skeleton bimetallic AlSn-SBA-15 molecular sieves containing Sn and Al as carrier, with platinum family element metal
For major catalyst, Group IV metal element or group ia or group iia metal element are auxiliary agent, be distributed infusion process prepare and
Into the catalyst has higher conversion of propane, Propylene Selectivity, reaction stability and excellent anti-carbon performance.
The content of the invention
The technical problems to be solved by the invention are the present situations for prior art, equally provide a kind of reactivity it is high,
Propylene Selectivity and the catalyst for preparing propylene with propane dehydrogenation that heat endurance is good, anti-carbon performance is strong.
Another technical problem to be solved by this invention is that the present situation for being directed to prior art takes off there is provided a kind of above-mentioned propane
The preparation method of hydrogen catalyst for preparing propene, this method step is simple, and prepared catalyst has higher conversion of propane, third
Alkane selectivity, reaction stability and anti-carbon.
The present invention solve the technical scheme that is used of above-mentioned technical problem for：A kind of catalyst for preparing propylene with propane dehydrogenation, its
It is characterised by：The catalyst is to contain Ta MCM-68 molecular sieves as carrier, using Pt as main active component, using Y as helping
Active component.
In such scheme, Pt content is 0.1~1.0wt% of total catalyst weight in the catalyst, and the Y's contains
0.4~4.0wt% for total catalyst weight is measured, the content of the Ta is 0.2~5.0wt% of total catalyst weight.
A kind of preparation method of catalyst for preparing propylene with propane dehydrogenation, it is characterised in that comprise the following steps：
(1) take Ludox to be dissolved in ethanol water, then by it with aluminium hydroxide, contain TaCl5Ethanol solution mix
Close, be stirring evenly and then adding into potassium hydroxide and continue to stir, be eventually adding template and be stirred until homogeneous, gained is mixed
Thing is fitted into hydrothermal reaction kettle the Crystallizing treatment at 130~180 DEG C and taken out after 10~15 days, is placed in after being washed through cooling, suction filtration, alcohol
3~5h of drying process at 90~120 DEG C, by dried material, 5~8h of calcination process obtains Ta-MCM- at 450~650 DEG C
68 molecular sieve carriers；
(2) Ta-MCM-68 molecular sieve carriers obtained by step (1) are put into the aqueous solution containing Pt presomas and Y presomas
In, the system is placed under 10~20T ultrastrong magnetic field, 20~60min is handled under the synergy of ultrasonic wave, then should
System is warming up to 105~120 DEG C, and moisture of the drying process into above-mentioned system is all evaporated, that is, has obtained supporting Pt and Y
Pt-Y-Ta-MCM-68 catalyst；
(3) by Pt-Y-Ta-MCM-68 catalyst obtained by step (2) in air atmosphere at 500~700 DEG C at roasting
2~4h is managed, final catalyst is obtained.
In such scheme, the mol ratio of each material is in the reaction system in step (1) in reactor：n(SiO2):n
(Al(OH)3):n(KOH):N (template):n(H2O):N (ethanol)=1.0:0.1:0.38:(0.1~0.5):30:30.
As an improvement, described template is AEO and 1- methyl -3- propane sulfonic acid base imidazoles phosphorus tungsten
In the mixture of hydrochlorate, and the mixture, the AEO and 1- methyl -3- propane sulfonic acid base imidazoles phosphotungstic acids
The mass ratio of salt is 1:1.
Preferably, the frequency setting of supersonic generator described in step (2) is 30~100KHz.
Preferably, described Pt presomas are one kind in potassium platinic chloride, ammonium chloroplatinate, acetylacetone,2,4-pentanedione platinum.
Preferably, described Y presomas are yttrium nitrate or yttrium chloride.
In above-mentioned each preferred scheme, in the aqueous solution of the Pt presomas and Y presomas, Pt concentration for 0.01~
0.1mol/L, Y concentration are 0.05~0.5mol/L.
Pt content is 0.1~1.0wt% in Pt-Y-Ta-MCM-68 catalyst obtained by step (3), and the content of the Y is
0.4~4.0wt%, the Ta content are 0.2~5.0wt%.
Compared with prior art, the advantage of the invention is that：
The catalyst of the present invention directly introduces Ta in carrier MCM-68 molecular sieve situs, and element T a can be in very great Cheng
Reactivity and carbon accumulation resisting ability of the catalyst during dehydrogenating propane are improved on degree, while coordinate with active component Pt, Y,
Make catalyst that integrally there is higher conversion of propane, and because MCM-68 molecular sieves have larger specific surface area in itself, make
Obtain active component to be uniformly dispersed on a catalyst support, further increase the catalytic activity of catalyst；
The preparation method of the present invention is using mass ratio as 1:1 AEO and 1- methyl -3- propane sulfonic acid bases
The mixture of imidazoles phosphotungstate MCM-68 molecular sieves containing Ta in skeleton as the step fabricated in situ of template one, use fat
The mixture of fat alcohol APEO and 1- methyl -3- propane sulfonic acid base imidazoles phosphotungstates is used as both template, one side
The meso-hole structure of new amphipathic pore creating material and induced synthesis high-sequential, another aspect 1- first can be cooperatively formed
Base -3- propane sulfonic acid base imidazoles phosphotungstates can be with TaCl5Complex compound is formed, is conducive to Ta uniform on molecular sieve carrier
Distribution；
The preparation method of invention is used as catalyst carrier, using Pt, Y as active component, Ta's using the MCM-68 for containing Ta
The formation of Pt-Ta alloys can be suppressed at reaction conditions by introducing in advance, while strengthen the interaction force between Pt and carrier,
The stability of catalyst reaction is improved, and Y introducing is conducive to improving decentralization and valence state of the precious metals pt in carrier surface
Stability, and the interaction between metal-auxiliary agent-carrier is further improved, so as to extend the service life of catalyst；
The present invention introduces ultrastrong magnetic field and ultrasonication technology when preparing catalyst in dipping process, the two
Collaboration auxiliary can not only drive active component to rapidly enter inside the duct of catalyst and obtain dispersed, and can contract
The drying process time of shot-catalyst agent；Meanwhile, the energy that ultrastrong magnetic field and ultrasonic wave are provided can make between each active component, living
Property component and carrier between occur reciprocation so that accelerate reaction and diffusion process, improve catalyst reactivity and third
Alkene selectivity.
Embodiment
The present invention is described in further detail with reference to embodiments.
Embodiment 1：
The preparation method of catalyst for preparing propylene with propane dehydrogenation comprises the following steps in the present embodiment：
(1) according to the 3.0wt% that the content of Ta in catalyst is total catalyst weight, Ludox is taken to be dissolved in ethanol water
In, then by it with aluminium hydroxide, contain TaCl5Ethanol solution mixing, be stirring evenly and then adding into potassium hydroxide and continue to stir
Mix uniform, be eventually adding template and be stirred until homogeneous, gained mixture is fitted into hydrothermal reaction kettle at 130 DEG C at crystallization
Reason is taken out after 15 days, and drying process 5h at 90 DEG C is placed in after being washed through cooling, suction filtration, alcohol, dried material is roasted at 450 DEG C
Burn processing 8h and obtain Ta-MCM-68 molecular sieve carriers；
The mol ratio of each material is in reaction system in the step in reactor：n(SiO2):n(Al(OH)3):n
(KOH):N (template):n(H2O):N (ethanol)=1.0:0.1:0.38:0.5:30:30, wherein, template is that mass ratio is
1:The mixture of 1 AEO and 1- methyl -3- propane sulfonic acid base imidazoles phosphotungstates；
(2) according to the 0.5wt% that the content of Pt in catalyst is total catalyst weight, Y content is total catalyst weight
4.0wt%, Ta-MCM-68 molecular sieve carriers obtained by step (1) are put into the aqueous solution of potassium platinic chloride and yttrium nitrate, will
The system is placed under 10T ultrastrong magnetic field, the processing 60min under frequency setting is 40KHz supersonic generator effect, then
The system is warming up to 105 DEG C, moisture of the drying process into above-mentioned system is all evaporated, that is, has obtained supporting Pt and Y Pt-
Y-Ta-MCM-68 catalyst；
In the step in the aqueous solution of Pt potassium platinic chlorides and yttrium nitrate, Pt concentration is 0.01mol/L, and Y concentration is
0.05mol/L；
(3) by Pt-Y-Ta-MCM-68 catalyst obtained by step (2) in air atmosphere in calcination process 4h at 500 DEG C,
Obtain final catalyst.
Embodiment 2：
The preparation method of catalyst for preparing propylene with propane dehydrogenation comprises the following steps in the present embodiment：
(1) according to the 4.5wt% that the content of Ta in catalyst is total catalyst weight, Ludox is taken to be dissolved in ethanol water
In, then by it with aluminium hydroxide, contain TaCl5Ethanol solution mixing, be stirring evenly and then adding into potassium hydroxide and continue to stir
Mix uniform, be eventually adding template and be stirred until homogeneous, gained mixture is fitted into hydrothermal reaction kettle at 180 DEG C at crystallization
Reason is taken out after 10 days, drying process 3h at 120 DEG C is placed in after being washed through cooling, suction filtration, alcohol, by dried material at 650 DEG C
Calcination process 5h obtains Ta-MCM-68 molecular sieve carriers；
The mol ratio of each material is in reaction system in the step in reactor：n(SiO2):n(Al(OH)3):n
(KOH):N (template):n(H2O):N (ethanol)=1.0:0.1:0.38:0.5:30:30, wherein, template is that mass ratio is
1:The mixture of 1 AEO and 1- methyl -3- propane sulfonic acid base imidazoles phosphotungstates；
(2) according to the 0.8wt% that the content of Pt in catalyst is total catalyst weight, Y content is total catalyst weight
3.8wt%, Ta-MCM-68 molecular sieve carriers obtained by step (1) are put into the aqueous solution of ammonium chloroplatinate and yttrium nitrate, will
The system is placed under 20T ultrastrong magnetic field, the processing 40min under frequency setting is 80KHz supersonic generator effect, then
The system is warming up to 120 DEG C, moisture of the drying process into above-mentioned system is all evaporated, that is, has obtained supporting Pt and Y Pt-
Y-Ta-MCM-68 catalyst；
In the step in the aqueous solution of ammonium chloroplatinate and yttrium nitrate, Pt concentration is 0.08mol/L, and Y concentration is
0.5mol/L；
(3) by Pt-Y-Ta-MCM-68 catalyst obtained by step (2) in air atmosphere in calcination process 2h at 700 DEG C,
Obtain final catalyst.
Embodiment 3：
The preparation method of catalyst for preparing propylene with propane dehydrogenation comprises the following steps in the present embodiment：
(1) according to the 0.2wt% that the content of Ta in catalyst is total catalyst weight, Ludox is taken to be dissolved in ethanol water
In, then by it with aluminium hydroxide, contain TaCl5Ethanol solution mixing, be stirring evenly and then adding into potassium hydroxide and continue to stir
Mix uniform, be eventually adding template and be stirred until homogeneous, gained mixture is fitted into hydrothermal reaction kettle at 150 DEG C at crystallization
Reason is taken out after 13 days, drying process 4h at 100 DEG C is placed in after being washed through cooling, suction filtration, alcohol, by dried material at 550 DEG C
Calcination process 6h obtains Ta-MCM-68 molecular sieve carriers；
The mol ratio of each material is in reaction system in the step in reactor：n(SiO2):n(Al(OH)3):n
(KOH):N (template):n(H2O):N (ethanol)=1.0:0.1:0.38:0.1:30:30, wherein, template is that mass ratio is
1:The mixture of 1 AEO and 1- methyl -3- propane sulfonic acid base imidazoles phosphotungstates；
(2) according to the 1.0wt% that the content of Pt in catalyst is total catalyst weight, Y content is total catalyst weight
0.4wt%, Ta-MCM-68 molecular sieve carriers obtained by step (1) are put into the aqueous solution of acetylacetone,2,4-pentanedione platinum and yttrium chloride, will
The system is placed under 15T ultrastrong magnetic field, the processing 30min under frequency setting is 100KHz supersonic generator effect, so
The system is warming up to 110 DEG C afterwards, moisture of the drying process into above-mentioned system is all evaporated, that is, obtains supporting Pt and Y
Pt-Y-Ta-MCM-68 catalyst；
In the step in the aqueous solution of acetylacetone,2,4-pentanedione platinum and yttrium chloride, Pt concentration is 0.1mol/L, and Y concentration is
0.2mol/L；
(3) by Pt-Y-Ta-MCM-68 catalyst obtained by step (2) in air atmosphere in calcination process 3h at 600 DEG C,
Obtain final catalyst.
Embodiment 4：
The preparation method of catalyst for preparing propylene with propane dehydrogenation comprises the following steps in the present embodiment：
(1) according to the 5.0wt% that the content of Ta in catalyst is total catalyst weight, Ludox is taken to be dissolved in ethanol water
In, then by it with aluminium hydroxide, contain TaCl5Ethanol solution mixing, be stirring evenly and then adding into potassium hydroxide and continue to stir
Mix uniform, be eventually adding template and be stirred until homogeneous, gained mixture is fitted into hydrothermal reaction kettle at 170 DEG C at crystallization
Reason is taken out after 12 days, drying process 4h at 105 DEG C is placed in after being washed through cooling, suction filtration, alcohol, by dried material at 500 DEG C
Calcination process 7h obtains Ta-MCM-68 molecular sieve carriers；
The mol ratio of each material is in reaction system in the step in reactor：n(SiO2):n(Al(OH)3):n
(KOH):N (template):n(H2O):N (ethanol)=1.0:0.1:0.38:0.4:30:30, wherein, template is that mass ratio is
1:The mixture of 1 AEO and 1- methyl -3- propane sulfonic acid base imidazoles phosphotungstates；
(2) according to the 0.1wt% that the content of Pt in catalyst is total catalyst weight, Y content is total catalyst weight
3.0wt%, Ta-MCM-68 molecular sieve carriers obtained by step (1) are put into the aqueous solution of ammonium chloroplatinate and yttrium chloride, will
The system is placed under 12T ultrastrong magnetic field, the processing 50min under frequency setting is 90KHz supersonic generator effect, then
The system is warming up to 100 DEG C, moisture of the drying process into above-mentioned system is all evaporated, that is, has obtained supporting Pt and Y Pt-
Y-Ta-MCM-68 catalyst；
In the step in the aqueous solution of ammonium chloroplatinate and yttrium chloride, Pt concentration is 0.05mol/L, and Y concentration is
0.5mol/L；
(3) by Pt-Y-Ta-MCM-68 catalyst obtained by step (2) in air atmosphere in calcination process 3h at 600 DEG C,
Obtain final catalyst.
Embodiment 5：
The preparation method of catalyst for preparing propylene with propane dehydrogenation comprises the following steps in the present embodiment：
(1) according to the 2.0wt% that the content of Ta in catalyst is total catalyst weight, Ludox is taken to be dissolved in ethanol water
In, then by it with aluminium hydroxide, contain TaCl5Ethanol solution mixing, be stirring evenly and then adding into potassium hydroxide and continue to stir
Mix uniform, be eventually adding template and be stirred until homogeneous, gained mixture is fitted into hydrothermal reaction kettle at 180 DEG C at crystallization
Reason is taken out after 11 days, and drying process 5h at 95 DEG C is placed in after being washed through cooling, suction filtration, alcohol, dried material is roasted at 620 DEG C
Burn processing 5h and obtain Ta-MCM-68 molecular sieve carriers；
The mol ratio of each material is in reaction system in the step in reactor：n(SiO2):n(Al(OH)3):n
(KOH):N (template):n(H2O):N (ethanol)=1.0:0.1:0.38:0.3:30:30, wherein, template is that mass ratio is
1:The mixture of 1 AEO and 1- methyl -3- propane sulfonic acid base imidazoles phosphotungstates；
(2) according to the 0.8wt% that the content of Pt in catalyst is total catalyst weight, Y content is total catalyst weight
0.4wt%, Ta-MCM-68 molecular sieve carriers obtained by step (1) are put into the aqueous solution of acetylacetone,2,4-pentanedione platinum and yttrium nitrate, will
The system is placed under 18T ultrastrong magnetic field, the processing 60min under frequency setting is 60KHz supersonic generator effect, then
The system is warming up to 110 DEG C, moisture of the drying process into above-mentioned system is all evaporated, that is, has obtained supporting Pt and Y Pt-
Y-Ta-MCM-68 catalyst；
In the step in the aqueous solution of acetylacetone,2,4-pentanedione platinum and yttrium nitrate, Pt concentration is 0.1mol/L, and Y concentration is
0.05mol/L；
(3) by Pt-Y-Ta-MCM-68 catalyst obtained by step (2) in air atmosphere in calcination process 3h at 700 DEG C,
Obtain final catalyst.
Catalyst prepared by the various embodiments described above is ground, tabletting and screening, then in 600 in nitrogen atmosphere
Activation process 3h under the conditions of DEG C；Reaction evaluating is carried out to the catalyst being disposed, appreciation condition is：By 0.50g catalyst
Sample is fitted into isothermal reactor, and regulation propane mass space velocity is 4h-1, reaction temperature is 600 DEG C, and reaction pressure is 0.1MPa,
Hydrogen/propane molar ratio is 1:4.5, the reaction time is 300h.Specific evaluation result is shown in Table 1.
Table 1
| Conversion of propane/% | Propylene Selectivity/% | |
| Embodiment 1 | 30.4 | 97.5 |
| Embodiment 2 | 30.8 | 98.1 |
| Embodiment 3 | 31.5 | 96.8 |
| Embodiment 4 | 29.8 | 98.3 |
| Embodiment 5 | 30.6 | 97.1 |
Claims (9)
1. a kind of catalyst for preparing propylene with propane dehydrogenation, it is characterised in that：The catalyst is divided with the MCM-68 that Ta is introduced on skeleton
Son sieve is as carrier, using Pt as main active component, using Y as helping active component.
2. catalyst for preparing propylene with propane dehydrogenation according to claim 1, it is characterised in that：Pt content in the catalyst
For 0.1~1.0wt% of total catalyst weight, the content of the Y is 0.4~4.0wt% of total catalyst weight, the Ta's
Content is 0.2~5.0wt% of total catalyst weight.
3. a kind of preparation method of catalyst for preparing propylene with propane dehydrogenation, it is characterised in that comprise the following steps：
(1) take Ludox to be dissolved in ethanol water, then by it with aluminium hydroxide, contain TaCl5Ethanol solution mixing, stir
Mix uniform rear addition potassium hydroxide and continue to stir, be eventually adding template and be stirred until homogeneous, gained mixture is filled
Enter in hydrothermal reaction kettle that Crystallizing treatment takes out after 10~15 days at 130~180 DEG C, it is placed in 90 after being washed through cooling, suction filtration, alcohol~
3~5h of drying process at 120 DEG C, by dried material, 5~8h of calcination process obtains Ta-MCM-68 points at 450~650 DEG C
Son sieve carrier；Described template is the mixed of AEO and 1- methyl -3- propane sulfonic acid base imidazoles phosphotungstates
In compound, and the mixture, the quality of the AEO and 1- methyl -3- propane sulfonic acid base imidazoles phosphotungstates
Than for 1:1；
(2) Ta-MCM-68 molecular sieve carriers obtained by step (1) are put into the aqueous solution containing Pt presomas and Y presomas, will
The system is placed under 10~20T ultrastrong magnetic field, in supersonic generator effect 20~60min of lower processing, then by the system
105~120 DEG C are warming up to, moisture of the drying process into above-mentioned system is all evaporated, that is, have obtained supporting Pt and Y Pt-Y-
Ta-MCM-68 catalyst；
(3) by Pt-Y-Ta-MCM-68 catalyst obtained by step (2) in air atmosphere in calcination process 2 at 500~700 DEG C~
4h, obtains final catalyst.
4. the preparation method of catalyst for preparing propylene with propane dehydrogenation according to claim 3, it is characterised in that：In step (1)
The mol ratio of each material is in reaction system in reactor：n(SiO2):n(Al(OH)3):n(KOH):N (template):n
(H2O):N (ethanol)=1.0:0.1:0.38:(0.1~0.5):30:30.
5. the preparation method of catalyst for preparing propylene with propane dehydrogenation according to claim 3, it is characterised in that：In step (2)
The frequency setting of the supersonic generator is 30~100KHz.
6. the preparation method of catalyst for preparing propylene with propane dehydrogenation according to claim 3, it is characterised in that：Before described Pt
Drive body is one kind in potassium platinic chloride, ammonium chloroplatinate, acetylacetone,2,4-pentanedione platinum.
7. the preparation method of catalyst for preparing propylene with propane dehydrogenation according to claim 3, it is characterised in that：Before described Y
It is yttrium nitrate or yttrium chloride to drive body.
8. the preparation method of catalyst for preparing propylene with propane dehydrogenation according to claim 3, it is characterised in that：The Pt forerunner
In the aqueous solution of body and Y presomas, Pt concentration is 0.01~0.1mol/L, and Y concentration is 0.05~0.5mol/L.
9. the preparation method of catalyst for preparing propylene with propane dehydrogenation according to claim 3, it is characterised in that：Step (3) institute
The content for obtaining Pt in Pt-Y-Ta-MCM-68 catalyst is 0.1~1.0wt%, and the content of the Y is 0.4~4.0wt%, described
Ta content is 0.2~5.0wt%.
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| CN110614116A (en) * | 2018-06-20 | 2019-12-27 | 中国石油化工股份有限公司 | Non-noble metal low-carbon alkane dehydrogenation catalyst, preparation method thereof and method for preparing low-carbon olefin by low-carbon alkane dehydrogenation |
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