CN104941640A - Catalyst for production of propylene through catalytic dehydrogenation of propane, and preparation method thereof - Google Patents

Catalyst for production of propylene through catalytic dehydrogenation of propane, and preparation method thereof Download PDF

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CN104941640A
CN104941640A CN201510287222.0A CN201510287222A CN104941640A CN 104941640 A CN104941640 A CN 104941640A CN 201510287222 A CN201510287222 A CN 201510287222A CN 104941640 A CN104941640 A CN 104941640A
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catalyst
preparation
propane
catalytic dehydrogenation
temperature
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吴世华
关允飞
张守民
王彦美
郭先芝
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Nankai University
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Nankai University
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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

A catalyst for production of propylene through catalytic dehydrogenation of propane adopts alumina-chrome oxide as a mixed carrier, metallic Pt as an active component and metallic Sn, La and Ca as assistants, the chemical formula of the catalyst is Pt-Sn-Ca/Cr2O3.Al2O3 and Pt-Sn-La-Ca/Cr2O3.Al2O3, and a mass ratio of Cr2O3 to Al2O3 in the mixed carrier is 2:1. A preparation method of the catalyst has the advantages of simple process and easy operation; a performance test result of the catalyst shows that the catalyst has high propane conversion rate, high activity, long service life and high propylene selectivity; and the initial conversion rate is about 48%, and the catalyst still has a high conversion rate of about 40% and high propylene selectivity of above 91% 4h later, so the catalyst has a great economic effect, and can be industrially popularized.

Description

A kind of Catalysts and its preparation method for Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane
Technical field
The present invention relates to the correlation technique that propylene is prepared in propane catalytic dehydrogenation, especially a kind of Catalysts and its preparation method for Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane.
Background technology
Propylene is a kind of important industrial chemicals, can be used for synthesizing polypropylene, is also the primary raw material of the downstream product such as synthesis of acrylonitrile, butanols, isopropylbenzene and nonyl phenol simultaneously, in addition, as the oligomer of propylene, can also improves the octane number of gasoline.Therefore, the commercial value of propylene is self-evident, and the demand of the whole world to propylene is surged and exceeded ethene in the rate of rise of some its demand of country.China's production of propylene can be divided into two classes according to raw material sources: petroleum base propylene and unconventional feedstocks propylene.Petroleum base propylene is mainly derived from cracking propylene and cracking of ethylene; Unconventional feedstocks propylene is mainly separated by refinery gas.But, traditional process equipment is produced and has been difficult to meet the growing demand of propylene, through prediction, 2012 ~ 2017 years, propylene will continue the situation that supply falls short of demand, in order to meet industrial production demand as far as possible, the special new technology of 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 disproportionated reaction technology are current industrialized four kinds of propylene production technology, and of greatest concern be exactly preparing propylene by dehydrogenating propane technology.
Dehydrogenating propane technology mainly contains three classes: oxidative dehydrogenation, inorganic film reactor dehydrogenation and catalytic dehydrogenation.Although oxidative dehydrogenation of propane achieves certain progress, from industrialization, also there is a big difference; Inorganic film reactor dehydrogenation is selective good, and saturating amounts of hydrogen is large, and keeping the restriction can ignoring kinetic balance under catalyst greater activity and selective prerequisite, has a extensive future, but a lot of Basic Problems waits to solve, and is difficult to suitability for industrialized production; And propane catalytic dehydrogenation technology prepares carrier by synthesis, supported active metals, achieve industrialization, weak point is that the restriction of thermodynamics chemical balance makes it be difficult to the lifting of higher conversion of propane, carbon distribution causes the inactivation of catalyst, pyroreaction power consumption is huge, also needs to improve and improve such catalyst further.The device of Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane mainly contains and adopts the Catofin technology of ABB Lumkus company and the Oleflex technology of Uop Inc. in the world at present, adopts Pt series catalysts and Cr series catalysts respectively.Pt series catalysts heat endurance is high, can bear comparatively exacting terms, reaction time sustainable 7h and propane initial conversion also reaches 40%; Cr series catalysts is Cr 2o 3/ Al 2o 3catalyst, conversion per pass is up to 48-56%, but easy inactivation, only there is 15-30min reaction time.
In a word, preparing propylene by dehydrogenating propane technology suitability for industrialized production, but it is not high to there is Catalyst Conversion, poor stability, the defects such as easy in inactivation, also requires further improvement and perfect.
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 Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane is provided, catalyst prepared by the method has higher conversion of propane, higher activity, longer service life, and propylene is selective higher.
Technical scheme of the present invention:
For a catalyst for Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane, using alumina chromia as mixed carrier, Pt metal is active component, metal Sn, La and Ca are auxiliary agent, and its chemical formula is Pt-Sn-Ca/Cr 2o 3al 2o 3and Pt-Sn-La-Ca/Cr 2o 3al 2o 3, Cr in mixed carrier 2o 3with Al 2o 3mass ratio be the load capacity 0.4-1.5wt% of the load capacity 0.2-1.0wt% of 2:1, Pt, Sn, the load capacity 0.2-1.0wt% of the load capacity 0.4-1.4wt% of La, Ca.
A described preparation method for the catalyst of Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane, step is as follows:
1) coprecipitation method is adopted to prepare carrier
By Al (NO 3) 39H 2o and Cr (NO 3) 39H 2o adds deionized water, and stirring and dissolving is placed on ultrasonic 15min in ultrasonic cleaning machine, and dropping precipitant concentration is ammoniacal liquor to the pH value of 25-28wt% is while stirring 4.8-5.1; Sediment centrifugation is also used absolute ethanol washing 1-2 time, then sediment is transferred in crucible, at 80 DEG C, dries 8h in an oven, in Muffle furnace, at temperature is 550 DEG C, calcine 4h, obtained mixed carrier Cr 2o 3al 2o 3;
2) Pt-Sn/Cr 2o 3al 2o 3preparation
At Cr 2o 3al 2o 3in carrier, add the aqueous solution that concentration is the chloroplatinic acid of 0.00189mol/L, stir 12h, directly dry or revolve after steaming is dried and calcine 4h at temperature is 550 DEG C; Then, add the ethanolic solution that concentration is the stannous chloride of 0.01mol/L, stir 12h, directly dry or revolve after steaming is dried and at temperature is 550 DEG C, calcine 4h, obtained Pt-Sn/Cr 2o 3al 2o 3;
3) Pt-Sn-Ca/Cr 2o 3al 2o 3preparation
At catalyst Pt-Sn/Cr 2o 3al 2o 3in, add the Ca (NO that concentration is 0.01mol/L 3) 2the aqueous solution, stirs 12h, directly dries or revolve after steaming is dried to calcine 4h at temperature is 550 DEG C; Obtain catalyst a and Pt-Sn-Ca/Cr for Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane 2o 3al 2o 3;
4) Pt-Sn-La-Ca/Cr 2o 3al 2o 3preparation
At catalyst Pt-Sn/Cr 2o 3al 2o 3in, add the La (NO that concentration is 0.0359mol/L 3) 36H 2the O aqueous solution stirs 12h, directly dries or revolve after steaming is dried at temperature is 550 DEG C, to calcine 4h, obtained Pt-Sn-La/Cr 2o 3al 2o 3; Then Ca (the NO that concentration is 0.01mol/L is added 3) 2the aqueous solution stirs 12h, directly dries or revolve after steaming is dried to calcine 4h at temperature is 550 DEG C, obtains catalyst b and Pt-Sn-La-Ca/Cr for Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane 2o 3al 2o 3.
Described step 1) middle Al (NO 3) 39H 2o, Cr (NO 3) 39H 2the amount ratio of O and deionized water is 7.8953g:5.5188g:150mL.
A kind of method of testing of catalyst catalytic performance of prepared Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane, take 0.3g solid catalyst, quartz glass tube is proceeded to by funnel, and fixing in fixed bed, test condition is: temperature 550-630 DEG C, pressure 0.1Mpa, reaction volume air speed 2600-3900h -1, reaction time is 4 hours, between the stage of reaction every 1 hour sample introduction once, read and record the experiment response data of gas chromatograph.
Advantage of the present invention is:
Preparation method's technique is simple, and be easy to operation, the performance test of catalyst shows that it has higher conversion of propane, higher activity and longer service life, and Propylene Selectivity is higher; Initial conversion is about 48%, and still has the higher conversion of about 40% through the rear catalyst of 4h, and Propylene Selectivity maintains higher more than 91%.Predict that it has good economic effect, be conducive to industrialization promotion.
Accompanying drawing explanation
Fig. 1 is catalyst a, b conversion rate curve to propane catalytic dehydrogenation.
Fig. 2 is catalyst a, b selectivity curve to propane catalytic dehydrogenation.
Detailed description of the invention
The preparation method of catalyst is described below by way of concrete example.
Embodiment 1:
A kind of preparation method of the catalyst for preparing propylene by dehydrogenating propane, using alumina chromia as mixed carrier, take Pt metal as active component, with metal Sn and Ca for auxiliary agent, by continuous impregnating method loaded metal ion Sn and Ca, in catalyst, each component percentages is: Pt 0.4%, Sn 0.6%, Ca 0.5%, preparation process is as follows:
1) 7.8953g is analyzed pure Cr (NO 3) 36H 2o and 5.5188g analyzes pure Al (NO 3) 3be dissolved in 150mL deionized water, while vigorous stirring, dropping concentration is ammonia spirit to the pH value of 25-28wt% is 5.1, centrifugal after leaving standstill 15min, sediment is spent deionized water 2 times, then at 80 DEG C, 8h is dried, at temperature is 550 DEG C, calcine 4h after grinding, after grinding, can Cr be obtained 2o 3-Al 2o 3mixed carrier;
2) in round-bottomed flask, by above-mentioned 2.0g Cr 2o 3al 2o 3mixed carrier 2.17mL, concentration are the H of 0.019mol/L 2ptCl 6aqueous impregnation, then add 35mL deionized water, stir 12h, then at 80 DEG C, dry 8h, after grinding, at temperature is 550 DEG C, calcine 4h, after grinding, obtained Pt-Sn/Cr 2o 3al 2o 3;
3) by above-mentioned 2.0g calcined material, be the SnCl of 0.100mol/L by 1.02mL, concentration 2ethanolic solution floods, then adds 35mL ethanol, stirs 12h, then at 80 DEG C, dries 8h, calcine 4h after grinding at temperature is 550 DEG C, after grinding, and obtained Pt-Sn/Cr 2o 3al 2o 3.
4) by the 1.5g Pt-Sn/Cr of above-mentioned preparation 2o 3al 2o 3with the Ca (NO that 0.88mL, concentration are 0.01mol/L 3) 2aqueous impregnation, then add 35mL deionized water, stir 12h, then at 80 DEG C, dry 8h, after grinding, at temperature is 550 DEG C, calcine 4h, after grinding, catalyst a and Pt-Sn-Ca/Cr for Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane can be obtained 2o 3al 2o 3.
Embodiment 2:
A kind of preparation method of the catalyst for preparing propylene by dehydrogenating propane, using alumina chromia as mixed carrier, take Pt metal as active component, with metal Sn, La and Ca for auxiliary agent, by continuous impregnating method loaded metal ion Sn, La and Ca, in catalyst, each component percentages is: Pt 0.4%, Sn 0.6%, La1.1%, Ca 0.2%, preparation process 1) 2) 3) identical with embodiment 1, increase step 4) 5) as follows:
4) by the 1.5g Pt-Sn/Cr of above-mentioned preparation 2o 3al 2o 3with the La (NO that 3.35mL concentration is 0.0359mol/L 3) 3aqueous impregnation, then add 35mL deionized water, stir 12h, then at 80 DEG C, dry 8h, after grinding, at temperature is 550 DEG C, calcine 4h, after grinding, obtained catalyst Pt-Sn-La/Cr 2o 3al 2o 3.；
5) by the 1.0g Pt-Sn-La/Cr of above-mentioned preparation 2o 3al 2o 3with the Ca (NO that 5.01mL, concentration are 0.01mol/L 3) 2aqueous impregnation, then add 35mL deionized water, stir 12h, then at 80 DEG C, dry 8h, after grinding, at temperature is 550 DEG C, calcine 4h, after grinding, obtain catalyst b and Pt-Sn-La-Ca/Cr for Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane 2o 3al 2o 3.
The catalytic performance method of testing of the catalyst for preparing propylene by dehydrogenating propane of preparation, testing arrangement carries out in fixed bed, outer connection gas-chromatography, the catalytic effect of evaluate catalysts is carried out by every 1 hour timing sampling, the process conditions of its catalytic dehydrogenation are: temperature 550-630 DEG C, pressure 0.1Mp, reaction volume air speed (GHSV) 2600-3900h -1.Catalyst prepared by the method improves the surface acidity of catalyst, reduce carbon distribution impact, improve the activity of catalyst, especially while significantly improving the dehydrogenating propane conversion ratio of catalyst, higher Propylene Selectivity is maintained, initial conversion is about 48%, and Propylene Selectivity is all more than 91%, even if reaction is after 4 hours, its conversion of propane is still more than 40%, and Propylene Selectivity maintains more than 91%.
Fig. 1 is the conversion rate curve of obtained catalyst a, b propane catalytic dehydrogenation, shows: with Cr in figure 2o 3/ Al 2o 3after making mixed carrier load auxiliary agent Sn, La, Ca, propane initial conversion is all more than 46%, and after 4 hours, conversion ratio is still very high.
Fig. 2 be obtained catalyst a, b to the selectivity curve of propane catalytic dehydrogenation, show in figure: along with reaction is carried out, the selective of propylene maintains higher level always, more than 91%.

Claims (4)

1. for a catalyst for Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane, it is characterized in that: using alumina chromia as mixed carrier, Pt metal is active component, metal Sn, La and Ca are auxiliary agent, and its chemical formula is Pt-Sn-Ca/Cr 2o 3al 2o 3and Pt-Sn-La-Ca/Cr 2o 3al 2o 3, Cr in mixed carrier 2o 3with Al 2o 3mass ratio be the load capacity 0.4-1.5wt% of the load capacity 0.2-1.0wt% of 2:1, Pt, Sn, the load capacity 0.2-1.0wt% of the load capacity 0.4-1.4wt% of La, Ca.
2., as claimed in claim 1 for a preparation method for the catalyst of Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane, it is characterized in that step is as follows:
1) coprecipitation method is adopted to prepare carrier
By Al (NO 3) 39H 2o and Cr (NO 3) 39H 2o adds deionized water, and stirring and dissolving is placed on ultrasonic 15min in ultrasonic cleaning machine, and dropping precipitant concentration is ammoniacal liquor to the pH value of 25-28wt% is while stirring 4.8-5.1; Sediment centrifugation is also used absolute ethanol washing 1-2 time, then sediment is transferred in crucible, at 80 DEG C, dries 8h in an oven, in Muffle furnace, at temperature is 550 DEG C, calcine 4h, obtained mixed carrier Cr 2o 3al 2o 3;
2) Pt-Sn/Cr 2o 3al 2o 3preparation
At Cr 2o 3al 2o 3in carrier, add the aqueous solution that concentration is the chloroplatinic acid of 0.00189mol/L, stir 12h, directly dry or revolve after steaming is dried and calcine 4h at temperature is 550 DEG C; Then, add the ethanolic solution that concentration is the stannous chloride of 0.01mol/L, stir 12h, directly dry or revolve after steaming is dried and at temperature is 550 DEG C, calcine 4h, obtained Pt-Sn/Cr 2o 3al 2o 3;
3) Pt-Sn-Ca/Cr 2o 3al 2o 3preparation
At catalyst Pt-Sn/Cr 2o 3al 2o 3in, add the Ca (NO that concentration is 0.01mol/L 3) 2the aqueous solution, stirs 12h, directly dries or revolve after steaming is dried to calcine 4h at temperature is 550 DEG C; Obtain catalyst a and Pt-Sn-Ca/Cr in Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane 2o 3al 2o 3;
4) Pt-Sn-La-Ca/Cr 2o 3al 2o 3preparation
At catalyst Pt-Sn/Cr 2o 3al 2o 3in, add the La (NO that concentration is 0.0359mol/L 3) 36H 2the O aqueous solution stirs 12h, directly dries or revolve after steaming is dried at temperature is 550 DEG C, to calcine 4h, obtained Pt-Sn-La/Cr 2o 3al 2o 3; Then Ca (the NO that concentration is 0.01mol/L is added 3) 2the aqueous solution stirs 12h, directly dries or revolve after steaming is dried to calcine 4h at temperature is 550 DEG C, obtains catalyst b and Pt-Sn-La-Ca/Cr in Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane 2o 3al 2o 3.
3. according to claim 2 for the preparation method of Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane, it is characterized in that: described step 1) middle Al (NO 3) 39H 2o, Cr (NO 3) 39H 2the amount ratio of O and deionized water is 7.8953g:5.5188g:150mL.
4. the method for testing of the catalyst effect of the Trends In Preparation of Propene By Catalytic Dehydrogenation of Propane prepared by a claim 2, it is characterized in that: take 0.3g solid catalyst, quartz glass tube is proceeded to by funnel, and fixing in fixed bed, test condition is: temperature 550-630 DEG C, pressure 0.1Mpa, reaction volume air speed 2600-3900h -1, reaction time is 4 hours, between the stage of reaction every 1 hour sample introduction once, read and record the experiment response data of gas chromatograph.
CN201510287222.0A 2015-05-29 2015-05-29 Catalyst for production of propylene through catalytic dehydrogenation of propane, and preparation method thereof Pending CN104941640A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105642284A (en) * 2015-12-18 2016-06-08 南开大学 Catalyst for propane dehydrogenation to produce propylene and preparation method and application thereof
CN109320392A (en) * 2018-11-15 2019-02-12 西南化工研究设计院有限公司 A kind of fixed fluidized bed reaction of preparing propylene by dehydrogenating propane and regeneration technology
CN110139709A (en) * 2016-12-13 2019-08-16 Smh有限公司 Hydrocarbon conversion catalyst system
CN116474771A (en) * 2023-04-24 2023-07-25 厦门大学 Alumina-supported ternary PtSnNa catalyst, and preparation method and application thereof

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105642284A (en) * 2015-12-18 2016-06-08 南开大学 Catalyst for propane dehydrogenation to produce propylene and preparation method and application thereof
CN105642284B (en) * 2015-12-18 2018-08-21 南开大学 A kind of catalyst and its preparation method and application for preparing propylene by dehydrogenating propane
CN110139709A (en) * 2016-12-13 2019-08-16 Smh有限公司 Hydrocarbon conversion catalyst system
CN109320392A (en) * 2018-11-15 2019-02-12 西南化工研究设计院有限公司 A kind of fixed fluidized bed reaction of preparing propylene by dehydrogenating propane and regeneration technology
CN116474771A (en) * 2023-04-24 2023-07-25 厦门大学 Alumina-supported ternary PtSnNa catalyst, and preparation method and application thereof

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Application publication date: 20150930