CN106582613B - A kind of catalyst of preparing propylene by dehydrogenating propane and its application - Google Patents
A kind of catalyst of preparing propylene by dehydrogenating propane and its application Download PDFInfo
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- CN106582613B CN106582613B CN201510677255.6A CN201510677255A CN106582613B CN 106582613 B CN106582613 B CN 106582613B CN 201510677255 A CN201510677255 A CN 201510677255A CN 106582613 B CN106582613 B CN 106582613B
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Abstract
The present invention provides a kind of catalyst of preparing propylene by dehydrogenating propane and its applications during preparing propylene by dehydrogenating propane, the catalyst includes: carrier and the active component being supported on carrier and auxiliary agent, wherein, the carrier is the aluminium oxide containing modifying agent, the modifying agent is one of rare earth component or a variety of, the active component is chromium, and the auxiliary agent contains boron and alkaline components or contains boron and alkaline earth metal component.When the catalyst of preparing propylene by dehydrogenating propane provided by the invention is used for preparing propylene by dehydrogenating propane reaction, available higher conversion of propane and Propylene Selectivity, and used catalyst stability with higher.
Description
Technical field
The present invention relates to a kind of catalyst of preparing propylene by dehydrogenating propane and its applications during preparing propylene by dehydrogenating propane.
Background technique
With the universal use of civil natural gas, the effective use of refinery's liquefied gas more and more attention has been paid to；Shale gas
The development also a large amount of lime set of by-product, main group become low-carbon alkanes, chemical utilization can efficent use of resources, also obtain people's
Common concern.Preparing propylene by dehydrogenating propane (PDH) is one of the important channel of liquefied gas and shale gas lime set production industrial chemicals.Third
Alkane anaerobic dehydrogenation propylene has at home and abroad realized industrialization, has nearly 20 covering device in industry park plan.Its catalytic body owner
It to be Cr series catalysts and Pt series catalysts, wherein Cr series catalysts are compared with noble metal catalyst, it is to impurity in raw material
It is required that it is relatively low and cheap, there is comparable competitive advantage.
In dehydrogenating propane technology, there are Lummus-Houdry company, referred to as ' Catofin work using chromium-based catalysts
Skill ', conversion of propane and Propylene Selectivity all preferably (respectively 45~60mol%, 87~94mol%), and have been carried out
Industrialized production, but consistent with other intelligencers is that chromium-based catalysts carbon distribution is serious, causes catalyst inactivation quickly, then
Raw frequently (regeneration period of Catofin technique is 15~30min or so, signal period reaction time only 7~9min), expends
Mass energy, therefore the stability for improving catalyst has great importance.
People have done numerous studies development from the factors such as carrier and auxiliary agent, it is expected to optimize the stabilization of catalyst
Property, and guarantee the yield of propylene.Cabrer etc. will have been investigated Sn being added to Cr2O3/Al2O3To reaction result in catalyst
It influences, it is found that the addition of Sn changes Cr2O3/Al2O3Activity, selectivity and the stability of catalyst.These in addition Sn are urged
The content of Cr is substantially change in agent, and coke content is also closely bound up with Sn content.When Sn content >=3 weight %, significantly
Reduce Cr2O3Content and coke content, to improve catalytic stability, but activity is declined.(Catal.Today, 2008,
133-135:800-804.)
Zhou Yuming etc. has investigated the reaction of the dehydrogenating propane on Pt catalyst, and it uses multiclass carriers, including regular oxidation
Aluminium, ZSM-5, SBA-15, meso-porous alumina etc., discovery ZSM-5 have highest stability, and reason may be since its is special
Cellular structure so that raw material and reaction product molecule in catalyst duct be easier spread, and have higher appearance carbon
Performance, but it is expensive due to Pt, and to increase cost, (Shi Junjun, Master's thesis, 2013, Southeast China University was mesoporous
The synthesis of alumina support and its application in dehydrogenating propane).
In conclusion the raising of catalyst performance, which still has, chooses in the technical solution of existing preparing propylene by dehydrogenating propane
War property: under the premise of guaranteeing catalytic activity, the stability of catalyst is still to be improved.
Summary of the invention
During overcoming using existing chromium-based catalysts progress preparing propylene by dehydrogenating propane
The poor defect of the stability of catalyst provides a kind of catalyst of preparing propylene by dehydrogenating propane and its in preparing propylene by dehydrogenating propane mistake
Application in journey.
To achieve the goals above, the present invention provides a kind of catalyst of preparing propylene by dehydrogenating propane, which includes:
Carrier and the active component being supported on carrier and auxiliary agent, wherein the carrier is the aluminium oxide containing modifying agent, described to change
Property agent be one of rare earth component or a variety of, the active component is chromium, and the auxiliary agent contains boron and alkaline components
Or contain boron and alkaline earth metal component.
The present invention also provides application of catalyst during preparing propylene by dehydrogenating propane.
When carrying out preparing propylene by dehydrogenating propane using catalyst provided by the invention, the conversion ratio of obtained propane and propylene
Selectivity is high, and catalyst has good stability.
Other features and advantages of the present invention will the following detailed description will be given in the detailed implementation section.
Specific embodiment
Detailed description of the preferred embodiments below.It should be understood that described herein specific
Embodiment is merely to illustrate and explain the present invention, and is not intended to restrict the invention.
The present invention provides a kind of catalyst of preparing propylene by dehydrogenating propane, which includes: carrier and is supported on load
Active component and auxiliary agent on body, wherein the carrier is the aluminium oxide containing modifying agent, and the modifying agent is rare earth metal group
Point one of or it is a variety of, the active component is chromium, and the auxiliary agent contains boron and alkaline components or containing boron and alkaline earth
Metal component.
According to the present invention, on the basis of the total amount of the catalyst and based on the element, the content of the carrier can be 60-
90 weight %, preferably 73-89 weight %；The content of the active component can be 8-35 weight %, preferably 10-25 weight
Measure %, more preferably 12-20 weight %；The content of the auxiliary agent can be 0.2-6 weight %, preferably 0.5-2 weight %.
In the present invention, the content of the active component is that the present inventor obtains by a large amount of further investigation
, the inventors found that: when the content of active component is lower than 8 weight %, the activity of obtained catalyst is lower；And
When the content of active component is greater than 35 weight %, not only increase the cost of catalyst, but also catalyst can not be improved
Activity；In addition, present inventor has further discovered that when the content of active component be greater than 35 weight % when, the preparation difficulty of catalyst
Increase, such as forming process, this will make the commercialization of catalyst more difficult.
In the present invention, active component being loaded to the mode on carrier can be method commonly used in the art, example
It such as, can be infusion process, the precipitation method, deposition-precipitation, kneading method or sol-gel method, preferably infusion process.A kind of excellent
In the embodiment of choosing, by loading active component in the maceration extract of the presoma containing active component carrier impregnation
Onto carrier, wherein the presoma of the active component be salt or oxide containing active component, preferably chromium trioxide,
One of ammonium chromate, ammonium dichromate and chromic nitrate are a variety of, more preferably chromium trioxide.In addition, the present invention is to above-mentioned dipping
Condition there is no particular limitation, can be this field routine selection, for example, dipping temperature be room temperature, time 0.5-
2h。
According to the present invention, in the auxiliary agent, the molar ratios of boron and alkaline components can be 1:0.1-5, preferably 1:
0.3-2；The molar ratio of boron and alkaline earth metal component can be 1:0.1-5, preferably 1:0.3-2.
According to the present invention, the molar ratio of the boron and the active component that contain in the auxiliary agent can be 1:5-50.
According to the present invention, the alkaline components are one of Li, Na and K or a variety of, preferably K or Na；The alkali
Earth metal group is divided into one of Mg, Ca and Ba or a variety of, preferably Mg or Ca.
In the present invention, boron is loaded to the mode on carrier can be for method commonly used in the art, for example, can be with
For infusion process, the precipitation method, deposition-precipitation, mediate method or sol-gel method, preferably infusion process.In a kind of preferred implementation
In mode, by loading to boron on carrier in the maceration extract of the presoma containing boron carrier impregnation, wherein the boron
Presoma be salt or acid containing active component, preferably one of boric acid, Boratex and potassium borate or a variety of, more preferably
For boric acid.In addition, there is no particular limitation for condition of the present invention to above-mentioned dipping, the condition of above-mentioned dipping can be used, herein
It repeats no more.
In the present invention, it can be commonly used in the art for alkali or alkaline earth metal being loaded to the mode on carrier
Method, for example, can be infusion process, the precipitation method, deposition-precipitation, kneading method or sol-gel method, preferably infusion process.In
In a kind of preferred embodiment, by the way that carrier impregnation is made in the maceration extract of the presoma containing alkali or alkaline earth metal
It obtains alkali or alkaline earth metal to load on carrier, wherein the presoma of the alkali or alkaline earth metal is to contain active group
Point salt or alkali, it is however preferred to have water-soluble nitrate, carbonate, villaumite, phosphate, sulfate, acetate, fluoride,
One of hydroxide is a variety of, more preferably potassium hydroxide, potassium nitrate, potassium carbonate, potassium acetate, potassium fluoride, potassium phosphate, hydrogen
Sodium oxide molybdena, sodium nitrate, sodium carbonate, sodium bicarbonate, sodium chloride, sodium sulphate, sodium acetate, calcium nitrate, calcium dihydrogen phosphate, magnesium nitrate,
One of magnesium phosphate, barium nitrate are a variety of.In addition, there is no particular limitation for condition of the present invention to above-mentioned dipping, can adopt
With the condition of above-mentioned dipping, details are not described herein.
According to the present invention, on the basis of the total amount of the carrier and based on the element, the content of the modifying agent can be
0.1-2 weight %, preferably 0.2-0.8 weight %.
According to the present invention, in situations where it is preferred, the modifying agent can be La or Ce, preferably La.
In the present invention, the aluminium oxide containing modifying agent can be made by the way that modifying agent to be supported on aluminium oxide
, the method for load can be method commonly used in the art, for example, can for infusion process, the precipitation method, deposition-precipitation,
Kneading method or sol-gel method, preferably infusion process.In a preferred embodiment, by containing carrier impregnation
In the maceration extract of the presoma of modifying agent modifying agent is loaded on carrier, wherein the presoma of the modifying agent be containing
The salt of active component, preferably nitrate or chloride, more preferably nitrate.In a kind of preferred embodiment of the invention
In, the presoma of the modifying agent is lanthanum nitrate.It, can be in addition, there is no particular limitation for condition of the present invention to above-mentioned dipping
Using the condition of above-mentioned dipping, details are not described herein.
According to the present invention, there is no particular limitation to the aluminium oxide by the present invention, and in the preferred case, the aluminium oxide can
Think δ-aluminium oxide and/or θ-aluminium oxide.There is no particular limitation in source of the present invention to the aluminium oxide, for example, can be
The commercially available various aluminium oxide for being suitble to be used as carrier, can also by nitric acid aluminum precipitation-roasting method, boehmite roasting method,
Aluminium oxide made from boehmite roasting method or Aluminum sol gel method.In addition, the present inventor be pointed out that as
It is known in those skilled in the art, pure δ-aluminium oxide or θ-aluminium oxide be difficult it is obtained, therefore, in the present invention,
δ-the aluminium oxide or θ-aluminium oxide refer to its content in the δ-aluminium oxide or θ-aluminium oxide of 90 weight %, preferably 95 weights
Measure % or more.
In a preferred embodiment of the invention, the catalyst can be prepared by following steps:
(1) alumina support is immersed in the maceration extract of the presoma containing modifying agent, is then dried and roasts,
Obtain catalyst precursor；
(2) catalyst precursor obtained by step (1) is successively immersed in the presoma containing active component and contained
The maceration extract of the presoma of auxiliary agent, is then dried and roasts.
In the present invention, the drying can adopt and implement with the conventional methods in the field, such as rotary evaporation seasoning；Institute
Stating roasting can also conventionally implement, and implementation condition may include: that maturing temperature is 400-900 DEG C, and the time is
2-4 hours.
The present invention also provides application of above-mentioned catalyst during preparing propylene by dehydrogenating propane.
In the present invention, catalyst provided by the invention is applied to need before preparing propylene by dehydrogenating propane reaction in hydrogen
In the presence of, active component is subjected to reduction activation, there is no particular limitation for condition of the present invention to the reduction activation, such as can
With are as follows: reduction temperature is 400-600 DEG C；The reduction activation can carry out in pure hydrogen atmosphere, can also be in hydrogen and lazy
It carries out, such as can be carried out in hydrogen with the mixed atmosphere of nitrogen and/or argon gas in the mixed atmosphere of property gas.
The present invention will be described in detail by way of examples below.
In the following Examples and Comparative Examples:
The content of active component, modifying agent and auxiliary agent is measured using X-ray fluorescence spectra analysis method；The crystalline substance of carrier
Mutually it is measured using XRD method.
Embodiment 1
The present embodiment is for illustrating dehydrogenation provided by the invention and preparation method thereof.
(1) preparation of carrier
The aqueous solution of nitric acid 0.20L of 1.0mol/L is taken, lanthanum nitrate 1.5g is added, 100g boehmite is added and 200g is thin
It in diaspore, is added in kneader and mediates 30min, subsequent extrusion is 3mm strip, and after dry, 900 DEG C of roastings obtain catalyst load
Body Z1, on the basis of the total amount of the carrier and based on the element, the quality group of carrier Z1 becomes 0.2%La-Al2O3, the carrier
It is detected by XRD, Crystallization is δ and θ type, wherein the content of δ and θ type aluminium oxide is greater than 95%.
(2) preparation of catalyst
50g chromium trioxide and 1g potassium nitrate are added in 110mL water, maceration extract is made, by the above-mentioned carrier Z1 of 150g in room
It is immersed in 0.5h in maceration extract under temperature, then roasts 3h at 720 DEG C, obtains catalyst precursor.
2g boric acid is added in 105mL hot water, maceration extract is made, above-mentioned catalyst precursor is immersed at room temperature
0.5h in stain liquid obtains catalyst A1 in 500 DEG C of roastings after drying, on the basis of the total amount of the catalyst and based on the element,
The quality group of catalyst A1 becomes Z1/17%Cr/0.24%B-0.26%K.
(3) it detects
Preparing propylene by dehydrogenating propane reaction is carried out in fixed bed reactors.Catalyst A1 is loaded, filling volume is 10mL, is adopted
It is diluted with 2:1 quartz sand, the temperature of the air speed of propane feed, the time of reaction and reactor is as shown in table 1；Start in reaction
Before, using pure hydrogen reducing catalyst A1, reduction temperature is 575 DEG C, time 2h, the content of propane used be 99.9% with
On, reaction carries out under normal pressure.Dehydrogenating propane product is analyzed using HP7890 gas-chromatography.Testing result such as 1 institute of table
Show.
Embodiment 2
The present embodiment is for illustrating dehydrogenation provided by the invention and preparation method thereof.
(1) preparation of carrier
The aqueous solution of nitric acid 0.20L of 1.0mol/L is taken, cerous nitrate 1.4g is added, 100g boehmite is added and 200g is thin
It in diaspore, is added in kneader and mediates 30min, subsequent extrusion is 3mm strip, and after dry, 900 DEG C of roastings obtain catalyst load
Body Z2, on the basis of the total amount of the carrier and based on the element, the quality group of carrier Z2 becomes 0.2%Ce-Al2O3The load
Body is detected by XRD, and Crystallization is δ and θ type, wherein the content of δ and θ type aluminium oxide is greater than 95%.
(2) preparation of catalyst
50g chromium trioxide and 2.4g magnesium nitrate are added in 110mL water, maceration extract is made, by the above-mentioned carrier Z2 of 150g in
It is immersed in 0.5h in maceration extract at room temperature, then roasts 3h at 720 DEG C, obtains catalyst precursor.
2g boric acid is added in 105mL hot water, maceration extract is made, above-mentioned catalyst precursor is immersed at room temperature
0.5h in stain liquid obtains catalyst A2 in 500 DEG C of roasting 3h after drying, on the basis of the total amount of the catalyst and with element
The quality group of meter, catalyst A2 becomes Z2/17%Cr/0.24%B-0.26%Mg.
(3) it detects
Preparing propylene by dehydrogenating propane reaction is carried out in fixed bed reactors.Catalyst A2 is loaded, filling volume is 10mL, is adopted
It is diluted with 2:1 quartz sand, the temperature of the air speed of propane feed, the time of reaction and reactor is as shown in table 1；Start in reaction
Before, using pure hydrogen reducing catalyst A2, reduction temperature is 575 DEG C, time 2h, the content of propane used be 99.9% with
On, reaction carries out under normal pressure.Dehydrogenating propane product is analyzed using HP7890 gas-chromatography.Testing result such as 1 institute of table
Show.
Embodiment 3
The present embodiment is for illustrating dehydrogenation provided by the invention and preparation method thereof.
(1) preparation of carrier
The aqueous solution of nitric acid 0.20L of 1.0mol/L is taken, lanthanum nitrate 3.0g is added, 100g boehmite is added and 200g is thin
It in diaspore, is added in kneader and mediates 30min, subsequent extrusion is 3mm strip, and after dry, 900 DEG C of roastings obtain catalyst load
Body Z3, on the basis of the total amount of the carrier and based on the element, the quality group of carrier Z3 becomes 0.4%La-Al2O3, the carrier
It is detected by XRD, Crystallization is δ and θ type, wherein the content of δ and θ type aluminium oxide is greater than 95%.
(2) preparation of catalyst
23g chromium trioxide and 3.9g sodium nitrate are added in 110mL water, maceration extract is made, by the above-mentioned carrier Z1 of 150g in
It is immersed in 1h in maceration extract at room temperature, then roasts 3h at 720 DEG C, obtains catalyst precursor.
2.5g boric acid is added in 105mL hot water, maceration extract is made, above-mentioned catalyst precursor is immersed at room temperature
1h in maceration extract obtains catalyst A3 in 500 DEG C of roastings after drying, on the basis of the total amount of the catalyst and based on the element,
The quality group of catalyst A3 becomes Z3/8%Cr/0.3%B-0.7%Na.
(3) it detects
Preparing propylene by dehydrogenating propane reaction is carried out in fixed bed reactors.Catalyst A3 is loaded, filling volume is 10mL, is adopted
It is diluted with 2:1 quartz sand, the temperature of the air speed of propane feed, the time of reaction and reactor is as shown in table 1；Start in reaction
Before, using pure hydrogen reducing catalyst A3, reduction temperature is 575 DEG C, time 2h, the content of propane used be 99.9% with
On, reaction carries out under normal pressure.Dehydrogenating propane product is analyzed using HP7890 gas-chromatography.Testing result such as 1 institute of table
Show.
Embodiment 4
The present embodiment is for illustrating dehydrogenation provided by the invention and preparation method thereof.
(1) preparation of carrier
The aqueous solution of nitric acid 0.20L of 1.0mol/L is taken, lanthanum nitrate 3.0g is added, 100g boehmite is added and 200g is thin
It in diaspore, is added in kneader and mediates 30min, subsequent extrusion is 3mm strip, and after dry, 900 DEG C of roastings obtain catalyst load
Body Z4, on the basis of the total amount of the carrier and based on the element, the quality group of carrier Z4 becomes 0.8%La-Al2O3, the carrier
It is detected by XRD, Crystallization is δ and θ type, wherein the content of δ and θ type aluminium oxide is greater than 95%.
(2) preparation of catalyst
100g chromium trioxide and 9.8g calcium nitrate are added in 110mL water, maceration extract is made, by the room 150g above-mentioned carrier Z4
It is immersed in 2h in maceration extract under temperature, then roasts 3h at 720 DEG C, obtains catalyst precursor.
3.4g boric acid is added in 105mL hot water, maceration extract is made, above-mentioned catalyst precursor is immersed at room temperature
2h in maceration extract obtains catalyst A4 in 500 DEG C of roastings after drying, on the basis of the total amount of the catalyst and based on the element,
The quality group of catalyst A4 becomes Z4/35%Cr/0.4%B-1.6%Ca.
(3) it detects
Preparing propylene by dehydrogenating propane reaction is carried out in fixed bed reactors.Catalyst A4 is loaded, filling volume is 10mL, is adopted
It is diluted with 2:1 quartz sand, the temperature of the air speed of propane feed, the time of reaction and reactor is as shown in table 1；Start in reaction
Before, using pure hydrogen reducing catalyst A4, reduction temperature is 575 DEG C, time 2h, the content of propane used be 99.9% with
On, reaction carries out under normal pressure.Dehydrogenating propane product is analyzed using HP7890 gas-chromatography.Testing result such as 1 institute of table
Show.
Comparative example 1
Catalyst is prepared according to the same manner as in Example 1, the difference is that, carrier is not in the dipping containing boric acid
It is impregnated in liquid, obtains catalyst D1.
Detection method is same as Example 1, and testing result is as shown in table 1.
Comparative example 2
Catalyst is prepared according to the same manner as in Example 1, the difference is that, it is not added in the preparation process of carrier
Lanthanum nitrate obtains catalyst D1.
Detection method is same as Example 1, and testing result is as shown in table 1.
Comparative example 3
Catalyst is prepared according to the same manner as in Example 1, the difference is that, carrier is not in the leaching containing potassium nitrate
It is impregnated in stain liquid, obtains catalyst D3.
Detection method is same as Example 1, and testing result is as shown in table 1.
Table 1
By by the Comparative result of embodiment 1-4 and comparative example 1-3 it is found that dehydrogenation provided by the invention is to aoxidize
Aluminium is carrier, using chromium as active component, using boron and alkaline components or boron and alkaline earth metal component as auxiliary agent, is urged using this
When agent carries out preparing propylene by dehydrogenating propane reaction, available higher conversion of propane and Propylene Selectivity, and the catalysis
Agent has good stability.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, it can be combined in any appropriate way.In order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (6)
1. a kind of catalyst of preparing propylene by dehydrogenating propane, which includes: carrier and the active component that is supported on carrier
And auxiliary agent, which is characterized in that the carrier is the aluminium oxide containing modifying agent, and the modifying agent is La or Ce, with the carrier
Total amount on the basis of and based on the element, the content of the modifying agent is 0.1-2 weight %；The active component is chromium, the auxiliary agent
Containing boron and alkaline components or contain boron and alkaline earth metal component, the alkaline components are K or Na, the alkaline-earth metal
Group is divided into Mg or Ca；
Wherein, on the basis of the total amount of the catalyst and based on the element, the content of the carrier is 73-89 weight %；The work
Property component content be 10-25 weight %；The content of the auxiliary agent is 0.5-2 weight %；
In the auxiliary agent, the molar ratio of boron and alkaline components is 1:0.3-2；The molar ratio of boron and alkaline earth metal component is 1:
0.3-2。
2. catalyst according to claim 1, wherein the molar ratio of the boron and the active component that contain in the auxiliary agent
For 1:5-50.
3. catalyst according to claim 1, wherein described to change on the basis of the total amount of the carrier and based on the element
Property agent content be 0.2-0.8 weight %.
4. catalyst according to claim 1, wherein the modifying agent is La.
5. catalyst according to claim 1, wherein the aluminium oxide is δ-aluminium oxide and/or θ-aluminium oxide.
6. application of catalyst during preparing propylene by dehydrogenating propane described in any one of claim 1-5.
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