CN105642284A - Catalyst for propane dehydrogenation to produce propylene and preparation method and application thereof - Google Patents
Catalyst for propane dehydrogenation to produce propylene and preparation method and application thereof Download PDFInfo
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- 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
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- 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
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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
- C07C5/3335—Catalytic processes with metals
- C07C5/3337—Catalytic processes with metals of the platinum group
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- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
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- C07C2523/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36
- C07C2523/56—Platinum group metals
- C07C2523/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tatalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- C07C2523/652—Chromium, molybdenum or tungsten
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
- C07C2523/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals
- C07C2523/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36
- C07C2523/56—Platinum group metals
- C07C2523/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tatalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- C07C2523/656—Manganese, technetium or rhenium
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- 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
A catalyst for propane dehydrogenation to produce propylene comprises the active components of Pt, a metal additive Sn-M and a mixed carrier Al2O3 / Cr2O3. M represents Mg or Mn in the metal additive Sn-M; Al2O3 and Cr2O3 in the mixed carrier have mass ratio of 1: 2; and the catalyst comprises 0.2-0.8 wt.% of Pt, 0.4-1.4 wt.% of Sn, 0.2-1.0 wt.% of M, and the balance of mixed carrier Al2O3 / Cr2O3. The catalyst is prepared by a successive impregnation method and is used for catalytic dehydrogenation of propane to produce propylene. The present invention has the advantages that: the preparation process is simple and easy to operate; the prepared catalyst for propane dehydrogenation to produce propylene has good selectivity, catalytic activity, stability and long life, and can significantly improve the conversion rate of propane dehydrogenation. The invention has remarkable technical and economic effect and is conducive to the industrialization promotion.
Description
Technical field
The present invention relates to the catalysis technique of preparing propylene by dehydrogenating propane, particularly a kind of Catalysts and its preparation method and application preparing propylene for propane catalytic dehydrogenation.
Background technology
Propylene is a kind of important industrial chemicals, it is possible to be used for synthesizing polypropylene, is also the main raw material of the derived product such as synthesis of acrylonitrile, butanols, isopropyl benzene and nonyl phenol simultaneously. In addition the oligopolymer of propylene, it is also possible to improve the octane value of gasoline. Therefore, the commercial value of propylene is self-evident, the whole world demand of propylene is surged and some country its demand rate of rise exceeded ethene. China's production of propylene can be divided into two classes according to raw material sources: petroleum base propylene and non-traditional raw material propylene. Petroleum base propylene is mainly derived from cracking propylene; Non-traditional raw material propylene is mainly separated by refinery gas. But, traditional process equipment is produced and has been difficult to meet the growing demand of propylene, and in order to meet industrial production demand as far as possible, the special new technology producing propylene of exploitation release is being made great efforts in many petro-chemical corporations and technological development commercial city. For now, steam cracking technology, catalytic cracking technology, dehydrogenating propane and disproportionation reaction technology are four kinds of propylene production technology of at present industrialization, and of greatest concern be exactly preparing propylene by dehydrogenating propane technology.
The technology that propane prepares propylene mainly contains three kinds: catalytic dehydrogenation, oxydehydrogenation and membrane reactor dehydrogenation. Dehydrogenation, cracking, addition, hydrogenolysis and long-pending carbon etc. can occur in dehydrogenating propane process, and reaction system more complicated, China there is no the report of propane anaerobic dehydrogenation industrialization. At present, the preparing propylene by dehydrogenating propane technology (PDH) succeeded in developing in the world mainly contains the technique of the Oleflex technique of UOP company, the Catofin technique of LummusTechnology company and Linde, Statoil and Borealis cooperative development, and the key distinction of above-mentioned preparing propylene by dehydrogenating propane technique is the design of catalyst preparing, reactor and the renovation process of catalyzer. The Oleflex technique of UOP company mainly adopts alumina base platinum catalyst, and LummusTechnology company adopts alumina-silica chrome catalysts. Pt series catalysts is remarkable to preparing propylene by dehydrogenating propane effect, and conversion of propane and the propylene selectivity of this catalyzer are higher, and stability better can effectively alleviate the impact of long-pending carbon, has good prospects for commercial application.
Summary of the invention
The present invention be directed to above-mentioned technical Analysis and existing problems, a kind of Catalysts and its preparation method for propane catalytic dehydrogenation propylene and application are provided, the method technique is simple, lower cost, the catalyzer of preparation has higher conversion of propane, well active, longer work-ing life, can improve the selectivity of propylene.
The technical scheme of the present invention:
For a catalyzer for preparing propylene by dehydrogenating propane, by active ingredient Pt, metal promoter Sn-M and mixed carrier Al2O3/Cr2O3Composition, the M in metal promoter Sn-M is Mg or Mn, Al in mixed carrier2O3With Cr2O3Mass ratio be 1:2, in catalyzer, the mass percent of each component is: Pt0.2-0.8%, Sn0.4-1.4%, M0.2-1.0%, mixed carrier Al2O3/Cr2O3For surplus.
A preparation method for the described catalyzer for preparing propylene by dehydrogenating propane, adopts the preparation of continuous impregnating method, and step is as follows:
1) by analytical pure Cr (NO3)3��6H2O and analytical pure Al (NO3)3Being dissolved in deionized water, dripping while vigorous stirring that to add concentration be ammonia soln to the pH value of 25-28wt% is 4.8-5.1, centrifugal after leaving standstill 15min, by throw out deionized water wash 2 times, then at 80 DEG C, dry 8-12h, at temperature 550 DEG C, calcine 4h, after grinding, obtain Al2O3/Cr2O3Mixed carrier;
2) by the Al of preparation2O3/Cr2O3Mixed carrier H2PtCl6Aqueous impregnation, then add deionized water, stir 8-12h, then at 80 DEG C, dry 8-12h, at temperature is 550 DEG C, calcine 4h after grinding, after grinding, obtain calcined material;
3) by above-mentioned calcined material SnCl2Ethanolic soln floods, then adds ethanol, stirs 8-12h, then dries 8-12h at 80 DEG C, calcine 4h after grinding at temperature is 550 DEG C, obtained Pt-Sn/Al after grinding2O3/Cr2O3;
4) by above-mentioned Pt-Sn/Al2O3/Cr2O3With Mg (NO3)2Or MnCl2Aqueous impregnation, then add deionized water, stir 8-12h, then at 80 DEG C, dry 8-12h, after grinding, at temperature is 550 DEG C, calcine 4h, obtained catalyst Pt-Sn-Mg/Al after grinding2O3/Cr2O3Or Pt-Sn-Mn/Al2O3/Cr2O3��
Described step 1) in Al (NO3)3��Cr(NO3)3It is 5.5188g:7.8953g:150mL with the amount ratio of deionized water.
Described step 2) in H2PtCl6The concentration of the aqueous solution is 0.019mol/L, mixed carrier Al2O3/Cr2O3��H2PtCl6The amount ratio of the aqueous solution and deionized water is 2.0g:2-3mL:20-40mL.
Described step 3) in SnCl2The concentration of ethanolic soln is 0.10mol/L, calcined material, SnCl2The amount ratio of ethanolic soln and ethanol is 2.0g:1-2mL:20-40mL.
Described step 4) in Mg (NO3)2The concentration 0.1716mol/L of the aqueous solution, Pt-Sn/Al2O3/Cr2O3��Mg(NO3)2The amount ratio of the aqueous solution and deionized water is 1.5g:0.72-3.63mL:15-30mL; MnCl2The concentration 0.110mol/L of the aqueous solution, Pt-Sn/Al2O3/Cr2O3��MnCl2The amount ratio of the aqueous solution and deionized water is 1.5g:0.5-2.5mL:15-30mL.
An application for the described catalyzer for preparing propylene by dehydrogenating propane, for propane catalytic dehydrogenation propylene, the processing condition of its catalytic dehydrogenation are: temperature 550-630 DEG C, pressure 0.1Mp, reaction volume air speed (GHSV) 2600-3900h-1��
It is an advantage of the invention that:
This preparation method's technique is simple, be easy to operation, and the catalyzer of preparation is used for preparing propylene by dehydrogenating propane and has good selectivity, stability and catalytic activity, it may also be useful to the life-span is long, and can significantly improve dehydrogenating propane transformation efficiency; The conversion rate of dehydrogenation initial value of propane can be reached more than 50% by this catalyzer, even if through long-time reaction, its final transformation efficiency still can maintain the level of about 40%, and technology and obvious economic, be conducive to industrialization promotion.
Accompanying drawing explanation
Fig. 1 be preparation catalyzer to the conversion rate curve of propane catalytic dehydrogenation, in figure: (a) is Pt-Sn-Mg/Al2O3/Cr2O3; B () is Pt-Sn-Mn/Al2O3/Cr2O3��
Fig. 2 be preparation catalyzer to the selectivity curve of propane catalytic dehydrogenation, in figure: (a) is Pt-Sn-Mg/Al2O3/Cr2O3;B () is Pt-Sn-Mn/Al2O3/Cr2O3��
Embodiment
The synthesis preparation method of catalyzer is described below by way of concrete example.
Embodiment 1:
For a catalyzer for preparing propylene by dehydrogenating propane, by active ingredient Pt, metal promoter Sn-Mg and mixed carrier Al2O3/Cr2O3Composition, Al in mixed carrier2O3With Cr2O3Mass ratio be 1:2, in catalyzer, the mass percent of each component is: Pt0.4%, Sn0.6%, Mg0.6%, mixed carrier Al2O3/Cr2O3For surplus.
The preparation method of the described catalyzer for preparing propylene by dehydrogenating propane, adopts the preparation of continuous impregnating method, and step is as follows:
1) by 7.8953g analytical pure Cr (NO3)3��6H2O and 5.5188g analytical pure Al (NO3)3It is dissolved in 150mL deionized water, dripping while vigorous stirring that to add concentration be ammonia soln to the pH value of 25wt% is 5.1, leave standstill after 15min centrifugal, by throw out deionized water wash 2 times, then at 80 DEG C, 12h is dried, at temperature is 550 DEG C, calcine 4h after grinding, after grinding, obtain composite oxides Al2O3/Cr2O3Mixed carrier;
2) in round-bottomed flask, by above-mentioned 2.0gAl2O3/Cr2O3Mixed carrier 2.17mL, concentration are the H of 0.019mol/L2PtCl6Aqueous impregnation, then add 35mL deionized water, stir 12h, then at 80 DEG C, dry 12h, at temperature is 550 DEG C, calcine 4h after grinding, after grinding, obtain calcined material;
3) by above-mentioned 2.0g calcined material, it is the SnCl of 0.100mol/L by 1.02mL, concentration2Ethanolic soln floods, then adds 35mL ethanol, stirs 12h, then dries 12h at 80 DEG C, calcine 4h after grinding at temperature is 550 DEG C, obtained Pt-Sn/Al after grinding2O3/Cr2O3��
4) by above-mentioned 2.0g calcined material, it is Mg (the NO of 0.1716mol/L by 2.89mL, concentration3)2Aqueous impregnation, then add 35mL deionized water, stir 12h, then at 80 DEG C, dry 12h, after grinding, at temperature is 550 DEG C, calcine 4h, obtained catalyst Pt-Sn-Mg/Al after grinding2O3/Cr2O3��
Embodiment 2:
For a catalyzer for preparing propylene by dehydrogenating propane, by active ingredient Pt, metal promoter Sn-Mn and mixed carrier Al2O3/Cr2O3Composition, Al in mixed carrier2O3With Cr2O3Mass ratio be 1:2, in catalyzer, the mass percent of each component is: Pt0.7%, Sn0.6%, Mn0.4%, mixed carrier Al2O3/Cr2O3For surplus.
The preparation method of the described catalyzer for preparing propylene by dehydrogenating propane, step 1) 2) 3) substantially the same manner as Example 1, difference is step 4) as follows:
4) by the 2.0gPt-Sn/Al of above-mentioned preparation2O3/Cr2O3It is the MnCl of 0.110mol/L by 1.33mL, concentration2Aqueous impregnation, then add 35mL deionized water, stir 12h, then at 80 DEG C, dry 12h, after grinding, at temperature is 550 DEG C, calcine 4h, obtained catalyst Pt-Sn-Mn/Al after grinding2O3/Cr2O3��
The application of a kind of prepared catalyzer for preparing propylene by dehydrogenating propane, for propane catalytic dehydrogenation propylene, reaction carries out in the fixed bed of catalytic evaluation device, outer connection gas-chromatography, the catalytic effect that sample carrys out evaluate catalysts is entered by timing, the processing condition of its catalytic dehydrogenation are: temperature 550-630 DEG C, pressure 0.1Mp, reaction volume air speed (GHSV) 2600-3900h-1. This catalyzer improves the long-pending carbon impact of catalyzer, improve stability and the activity of catalyzer, especially significantly improve the dehydrogenating propane transformation efficiency of catalyzer, initial conversion can be increased to more than 50%, even if reacting after 4 hours, its transformation efficiency is still about 40%.
Fig. 1 be preparation catalyzer to the conversion rate curve of propane catalytic dehydrogenation, in figure: (a) is Pt-Sn-Mg/Al2O3/Cr2O3;B () is Pt-Sn-Mn/Al2O3/Cr2O3. Figure shows: with Al2O3/Cr2O3After making mixed carrier load auxiliary agent Sn, Mg and Sn, Mn, dehydrogenating propane transformation efficiency initial value all reaches more than 45%, and after 4 hours, transformation efficiency is still very high. Particularly b catalyzer, transformation efficiency is significantly increased.
Fig. 2 be preparation catalyzer to the selectivity curve of propane catalytic dehydrogenation, in figure: (a) is Pt-Sn-Mg/Al2O3/Cr2O3; B () is Pt-Sn-Mn/Al2O3/Cr2O3. Showing in figure: along with the carrying out in reaction times, the selectivity of propylene progressively improves, and finally reaches more than 92%. Particularly a catalyzer, its selectivity is always higher more stable.
Claims (7)
1. the catalyzer for preparing propylene by dehydrogenating propane, it is characterised in that: by active ingredient Pt, metal promoter Sn-M and mixed carrier Al2O3/Cr2O3Composition, the M in metal promoter Sn-M is Mg or Mn, Al in mixed carrier2O3With Cr2O3Mass ratio be 1:2, in catalyzer, the mass percent of each component is: Pt0.2-0.8%, Sn0.4-1.4%, M0.2-1.0%, mixed carrier Al2O3/Cr2O3For surplus.
2. one kind as claimed in claim 1 for the preparation method of catalyzer of preparing propylene by dehydrogenating propane, it is characterised in that adopting the preparation of continuous impregnating method, step is as follows:
1) by analytical pure Cr (NO3)3��6H2O and analytical pure Al (NO3)3Being dissolved in deionized water, dripping while vigorous stirring that to add concentration be ammonia soln to the pH value of 25-28wt% is 4.8-5.1, centrifugal after leaving standstill 15min, by throw out deionized water wash 2 times, then at 80 DEG C, dry 8-12h, at temperature 550 DEG C, calcine 4h, after grinding, obtain Al2O3/Cr2O3Mixed carrier;
2) by the Al of preparation2O3/Cr2O3Mixed carrier H2PtCl6Aqueous impregnation, then add deionized water, stir 8-12h, then at 80 DEG C, dry 8-12h, at temperature is 550 DEG C, calcine 4h after grinding, after grinding, obtain calcined material;
3) by above-mentioned calcined material SnCl2Ethanolic soln floods, then adds ethanol, stirs 8-12h, then dries 8-12h at 80 DEG C, calcine 4h after grinding at temperature is 550 DEG C, obtained Pt-Sn/Al after grinding2O3/Cr2O3;
4) by above-mentioned Pt-Sn/Al2O3/Cr2O3With Mg (NO3)2Or MnCl2Aqueous impregnation, then add deionized water, stir 8-12h, then at 80 DEG C, dry 8-12h, after grinding, at temperature is 550 DEG C, calcine 4h, obtained catalyst Pt-Sn-Mg/Al after grinding2O3/Cr2O3Or Pt-Sn-Mn/Al2O3/Cr2O3��
3. according to claim 2 for the preparation method of catalyzer of preparing propylene by dehydrogenating propane, it is characterised in that: described step 1) in Al (NO3)3��Cr(NO3)3It is 5.5188g:7.8953g:150mL with the amount ratio of deionized water.
4. according to claim 2 for the preparation method of catalyzer of preparing propylene by dehydrogenating propane, it is characterised in that: described step 2) in H2PtCl6The concentration of the aqueous solution is 0.019mol/L, mixed carrier Al2O3/Cr2O3��H2PtCl6The amount ratio of the aqueous solution and deionized water is 2.0g:2-3mL:20-40mL.
5. according to claim 2 for the preparation method of catalyzer of preparing propylene by dehydrogenating propane, it is characterised in that: described step 3) in SnCl2The concentration of ethanolic soln is 0.10mol/L, calcined material, SnCl2The amount ratio of ethanolic soln and ethanol is 2.0g:1-2mL:20-40mL.
6. according to claim 2 for the preparation method of catalyzer of preparing propylene by dehydrogenating propane, it is characterised in that: described step 4) in Mg (NO3)2The concentration 0.1716mol/L of the aqueous solution, Pt-Sn/Al2O3/Cr2O3�� Mg(NO3)2The amount ratio of the aqueous solution and deionized water is 1.5g:0.72-3.63mL:15-30mL;MnCl2The concentration 0.110mol/L of the aqueous solution, Pt-Sn/Al2O3/Cr2O3��MnCl2The amount ratio of the aqueous solution and deionized water is 1.5g:0.5-2.5mL:15-30mL.
7. one kind as claimed in claim 1 for the application of catalyzer of preparing propylene by dehydrogenating propane, it is characterized in that: for propane catalytic dehydrogenation propylene, the processing condition of its catalytic dehydrogenation are: temperature 550-630 DEG C, pressure 0.1Mp, reaction volume air speed (GHSV) 2600-3900h-1��
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106483242A (en) * | 2016-12-16 | 2017-03-08 | 西安凯立新材料股份有限公司 | A kind of device for evaluating performance of preparing propylene by dehydrogenating propane catalyst and evaluation method |
| CN110139709A (en) * | 2016-12-13 | 2019-08-16 | Smh有限公司 | Hydrocarbon conversion catalyst system |
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| CN103977797A (en) * | 2014-05-20 | 2014-08-13 | 南开大学 | Preparation method and application of catalyst for preparing propylene by propane dehydrogenation |
| 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 |
| CN104941640A (en) * | 2015-05-29 | 2015-09-30 | 南开大学 | Catalyst for production of propylene through catalytic dehydrogenation of propane, and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103977797A (en) * | 2014-05-20 | 2014-08-13 | 南开大学 | Preparation method and application of catalyst for preparing propylene by propane dehydrogenation |
| 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 |
| CN104941640A (en) * | 2015-05-29 | 2015-09-30 | 南开大学 | Catalyst for production of propylene through catalytic dehydrogenation of propane, and preparation method thereof |
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| 余长林: "丙烷脱氢铂催化剂与反应性能的研究", 《中国博士学位论文全文数据库 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110139709A (en) * | 2016-12-13 | 2019-08-16 | Smh有限公司 | Hydrocarbon conversion catalyst system |
| CN106483242A (en) * | 2016-12-16 | 2017-03-08 | 西安凯立新材料股份有限公司 | A kind of device for evaluating performance of preparing propylene by dehydrogenating propane catalyst and evaluation method |
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