CN107456988A - A kind of molybdenum nitride hydrogenation deoxidation catalyst and its preparation method and application - Google Patents
A kind of molybdenum nitride hydrogenation deoxidation catalyst and its preparation method and application Download PDFInfo
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- C—CHEMISTRY; METALLURGY
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- C07C1/20—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon starting from organic compounds containing only oxygen atoms as heteroatoms
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
- C10G3/42—Catalytic treatment
- C10G3/44—Catalytic treatment characterised by the catalyst used
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
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Abstract
The present invention have studied a kind of support type Nitrides Catalysts and preparation method thereof.For carrier, using equi-volume impregnating, active component is supported on carrier with mesoporous carbon (MC) for described catalyst, and the presoma of catalyst is obtained after drying, and obtained presoma is first carbonized the Nitrides Catalysts for nitrogenizing loaded again.The catalyst that this method is prepared has higher activity to the reaction of guaiacol hydrogenation deoxidation, has higher selectivity to benzene.
Description
Technical field
It is used to be catalyzed guaiacol selective hydrogenation deoxidation the invention belongs to catalyst technical field, more particularly to a kind of
Catalyst.
Background technology
The non-renewable and its a large amount of consumption of fossil fuel causes energy resource supply to be becoming tight and the continuous deterioration of ecological environment,
Cause the concern of the environmentally friendly type regenerative resource research and development of people.In this context, to important renewable resource
The research of lignocellulose-like biomass be increasingly subject to pay attention to.Lignin is the main composition portion of lignocellulose-like biomass
Divide, be the Main By product of lignocellulose biomass by hydrolyzation fermentation ethanol industry processed and paper industry, due to that cannot fill
Divide and utilize, become environmental contaminants, seriously pollute environment.Therefore from environmental protection and the strategy of sustainable development, profit
Alkane fuel is produced with lignin, has the double meaning of efficent use of resources and Environment control concurrently.
Lignin is a kind of natural polymerses being made up of phenylpropyl alcohol alkyl structure, can be with by directional catalyzing cracking
Obtain the product liquid rich in aromatic rings.But wherein contain substantial amounts of containing oxygen derivative, especially substantial amounts of guaiacol base junction
The phenol derivatives compound of structure.Its temperature is low, viscosity is big, unstable, corrosivity by force can not directly as fuel oil substitute, because
This, efficient catalytic hydrogenation deoxidation PROCESS FOR TREATMENT (HDO) is carried out to lignin depolymerization product, be produce high-quality biological oil must be through
Approach.
In early days, the hydrogenation deoxidation handling process of bio oil is this to urge mainly using NiMo, CoMo of vulcanization as catalyst
Agent has good hydrogenation deoxidation effect, it is possible to achieve the General Promotion of bio oil performance indications.But the active metal of vulcanization
Catalyst has unstability, there is the generation of many accessory substances.And sulfide catalyst can introduce sulfur-containing compound so that production
Thing reduces, and to overcome the deficiency, researcher is by Rh, Pt, Pd etc. of noble metal alternatively thing, such as load, but noble metal price
It is expensive, widely using for it is limited to a certain extent.
The content of the invention
For shortcoming and defect existing for prior art, the present invention is prepared for a kind of relatively inexpensive transitional metal nitride molybdenum
Catalyst carries out hydrogenation deoxidation research to guaiacol, by using mesoporous carbon as carrier, thinking active component, using isometric leaching
Stain method, active component is supported on carrier, and the presoma of catalyst is obtained after drying, then that obtained presoma is first
Carbonization nitrogenizes to obtain Nitrides Catalysts again.Nitrides Catalysts prepared by the present invention are not only cheap, and with good
Hydrogenation deoxidation effect, there is very high productive value.
The present invention with to guaiacol compound (be can most represent lignin cracking compound characteristic containing oxygen derivative)
Progress hydrogenation deoxidation is target, by the use of the molybdenum nitride of synthesis as catalyst, can effectively improve the selectivity to benzene.
Molybdenum nitride hydrogenation deoxidation catalyst provided by the invention, the catalyst is using mesoporous carbon (MC) as carrier, with nitrogen
Change molybdenum as active component, wherein, active component accounts for the 5%~50% of catalyst quality in terms of molybdenum trioxide quality.
Present invention also offers a kind of preparation method of Nitrides Catalysts, the preparation method uses incipient impregnation
Method, the salting liquid of molybdenum is supported on the carrier of catalyst, by drying, being first carbonized, it is obtained to nitrogenize again.
Described equi-volume impregnating prepares comprising the following steps that for Nitrides Catalysts：
A. mesoporous carbon is handled with 2M concentrated hydrochloric acids in advance, then the water absorption rate according to mesoporous carbon (MC) accurately weighs Jie
Hole carbon, impregnated carrier is used as after drying and roasting；
B. ammonium molybdate is dissolved in pure water, obtains maceration extract；
C. the impregnated carrier incipient impregnation that maceration extract step (b) obtained obtains with step (a), impregnates at room temperature
12h, the presoma of catalyst is obtained after drying；
D. catalyst precursor step (c) obtained, which is first carbonized, to be nitrogenized to obtain Nitrides Catalysts again；
Wherein, in catalyst of the present invention, carrier mesoporous carbon (MC), SBA-15, Ce-SBA-15 can use existing commercially available business
Product, it can also be prepared by prior art.
Drying condition described in step (c) is：1~12h is dried in drying box at 100~120 DEG C；
The multi-stage procedure Elevated Temperature Conditions nitrogenized again that are first carbonized of presoma described in step (d) are：Under the atmosphere of hydrogen
Temperature rate is that 5~10 DEG C/min rises to 350 DEG C from room temperature, and 450 are warming up to from 350 DEG C using heating rate as 0.5~1 DEG C/min
DEG C, 650 DEG C~750 DEG C ammonification final temperatures are risen to as 2~10 DEG C/min from 450 DEG C using heating rate, hydrogen is now converted into ammonia
Gas, 1 is kept in nitridation final temperature~5 hours.
The hydrogenation deoxidation that Nitrides Catalysts prepared by the present invention are used for guaiacol reacts, and its step is as follows：More to create
Wooden phenol is raw material, under the conditions of existing for solvent and catalyst, adds hydrogen and carries out catalytic reaction.
Preferably, described reaction condition is：Reaction temperature is 300~400 DEG C, and hydrogen reaction pressure is 2~5MPa.
Preferably, described solvent is decane, the mass ratio of guaiacol and decane is 1: 50~1: 100.
Preferably, the liquid hourly space velocity (LHSV) (LHSV) of reaction raw materials is 2~10h-1。
Beneficial effects of the present invention：
1st, the catalyst in the present invention is by the way that in hydrogen reduction, Mo reacts Mr. with the C in carrier mesoporous carbon
Into molybdenum carbide, hydrogen is then converted into ammonia during final temperature, molybdenum carbide is converted into the higher molybdenum nitride of activity, in the system of catalyst
Mesoporous carbon is both used as carrier during standby, is used as reactant again, therefore obtained catalyst reaction activity is higher, to guaiacol
With good hydrogenation deoxidation effect, there is higher selectivity to benzene.
2nd, the present invention rises to 650 DEG C~750 DEG C ammonification final temperatures as 2~10 DEG C/min using heating rate from 450 DEG C, this temperature
Degree scope ensure that molybdenum carbide can effectively be converted into molybdenum nitride, while also make the molybdenum nitride of generation that there is higher reaction to live
Property.
3rd, the catalyst carrier in the present invention selects mesoporous carbon, and its suitable duct is advantageous to reduce inside diffusional resistance, carries
High reaction rate；Active component molybdenum nitride has the property of class noble metal, and hydrogenation deoxidation activity is high, good to the selectivity of benzene.
Embodiment
In order to further illustrate the present invention, following examples are enumerated.
Embodiment 1
The preparation of catalyst
Water absorption rate according to mesoporous carbon (MC) (mesoporous carbon is handled with 2M concentrated hydrochloric acids in advance) accurately weighs carrier, is roasted through drying
Impregnated carrier is used as after burning, 0.27g ammonium molybdates are dissolved in pure water, obtain maceration extract；By the body such as maceration extract and impregnated carrier
Product dipping, impregnates 12h at room temperature, and the presoma of catalyst is obtained after drying；The presoma that will be obtained, carry out multistage journey
Sequence temperature reaction；Under the atmosphere of hydrogen temperature rate be 5 DEG C/min rise to 350 DEG C from room temperature, using warm speed as 1 DEG C/min from
350 DEG C are warming up to 450 DEG C, and 700 DEG C of final temperatures are risen to from 450 DEG C by 5 DEG C/min of heating rate, hydrogen now is converted into ammonia
Gas, kept for 2 hours in final temperature, obtain 10%MoN/MC catalyst.
In fixed bed reactors, 10%MoN/MC catalyst 2ml, the liquid hourly space velocity (LHSV) of reaction raw materials are added
(LHSV)3h-1, being filled with hydrogen makes the reaction pressure of reaction system reach 2.0MPa, and heating reaction furnace makes reaction temperature
Reach 300 DEG C of reactions, reaction product is finally taken out, using gas chromatographic analysis.
Embodiment 2
0.27g ammonium molybdates in embodiment 1 are replaced with 0.54g ammonium molybdates, other steps are the same as embodiment 1.
Embodiment 3
0.27g ammonium molybdates in embodiment 1 are replaced with 0.82g ammonium molybdates, other steps are the same as embodiment 1.
Embodiment 4
0.27g ammonium molybdates in embodiment 1 are replaced with 1.08g ammonium molybdates, other steps are the same as embodiment 1.
Comparative example 1
The preparation of catalyst
Water absorption rate according to SBA-15 accurately weighs carrier, impregnated carrier is used as after drying and roasting, by 0.27g ammonium molybdates
It is dissolved in pure water, obtains maceration extract；By maceration extract and impregnated carrier incipient impregnation, 12h is impregnated at room temperature, after drying i.e.
Obtain the presoma of catalyst；The presoma that will be obtained, carry out multi-stage procedure temperature reaction；The temperature speed under the atmosphere of hydrogen
Rate is that 5 DEG C/min rises to 350 DEG C from room temperature, 450 DEG C is warming up to from 350 DEG C using warm speed as 1 DEG C/min, using heating rate as 5
DEG C/min rises to 700 DEG C of final temperatures from 450 DEG C, and hydrogen now is converted into ammonia, kept for 2 hours in final temperature, obtain 10%MoN/
SBA-15 catalyst.
In fixed bed reactors, 10%MoN/SBA-15 catalyst 2ml, the liquid hourly space velocity (LHSV) (LHSV) of reaction raw materials are added
3h-1, being filled with hydrogen makes the reaction pressure of reaction system reach 2.0MPa, and heating reaction furnace makes reaction temperature reach 300 DEG C of reactions,
Reaction product is finally taken out, using gas chromatographic analysis.
Comparative example 2
0.27g ammonium molybdates in comparative example 1 are replaced with 0.54g ammonium molybdates, other steps are the same as comparative example 1.
Comparative example 3
0.27g ammonium molybdates in comparative example 1 are replaced with 0.82g ammonium molybdates, other steps are the same as comparative example 1.
Comparative example 4
0.27g ammonium molybdates in comparative example 1 are replaced with 1.08g ammonium molybdates, other steps are the same as comparative example 1.
Comparative example 5
The preparation of catalyst
Water absorption rate according to Ce-SBA-15 accurately weighs carrier, impregnated carrier is used as after drying and roasting, by 0.27g molybdenums
Sour ammonium is dissolved in pure water, obtains maceration extract；By maceration extract and impregnated carrier incipient impregnation, 12h is impregnated at room temperature, is dried
Obtain the presoma of catalyst afterwards；The presoma that will be obtained, carry out multi-stage procedure temperature reaction；It is warm under the atmosphere of hydrogen
Degree speed is that 5 DEG C/min rises to 350 DEG C from room temperature, 450 DEG C is warming up to from 350 DEG C using warm speed as 1 DEG C/min, with heating rate
700 DEG C of final temperatures are risen to from 450 DEG C for 5 DEG C/min, hydrogen is now converted into ammonia, is kept for 2 hours in final temperature, obtains 10%
MoN/Ce-SBA-15 catalyst.
In fixed bed reactors, 10%MoN/Ce-SBA-15 catalyst 2ml, the liquid hourly space velocity (LHSV) of reaction raw materials are added
(LHSV)3h-1, being filled with hydrogen makes the reaction pressure of reaction system reach 2.0MPa, and heating reaction furnace makes reaction temperature reach 300
DEG C reaction, reaction product is finally taken out, using gas chromatographic analysis.
Comparative example 6
0.27g ammonium molybdates in comparative example 5 are replaced with 0.54g ammonium molybdates, other steps are the same as comparative example 5.
Comparative example 7
0.27g ammonium molybdates in comparative example 5 are replaced with 0.82g ammonium molybdates, other steps are the same as comparative example 5.
Comparative example 8
0.27g ammonium molybdates in comparative example 5 are replaced with 1.08g ammonium molybdates, other steps are the same as comparative example 5.
Comparative example 9
The preparation of catalyst
Water absorption rate according to mesoporous carbon (MC) (mesoporous carbon is handled with 2M concentrated hydrochloric acids in advance) accurately weighs carrier, is roasted through drying
Impregnated carrier is used as after burning, 0.27g ammonium molybdates are dissolved in pure water, obtain maceration extract；By the body such as maceration extract and impregnated carrier
Product dipping, impregnates 12h at room temperature, and the presoma of catalyst is obtained after drying；The presoma that will be obtained, carry out multistage journey
Sequence temperature reaction；Under the atmosphere of hydrogen temperature rate be 5 DEG C/min rise to 350 DEG C from room temperature, using warm speed as 1 DEG C/min from
350 DEG C are warming up to 450 DEG C, and 500 DEG C of final temperatures are risen to from 450 DEG C by 5 DEG C/min of heating rate, hydrogen now is converted into ammonia
Gas, kept for 2 hours in final temperature, obtain 10%MoN/MC catalyst.
In fixed bed reactors, 10%MoN/MC catalyst 2ml, liquid hourly space velocity (LHSV) (LHSV) 3h of reaction raw materials are added-1,
Being filled with hydrogen makes the reaction pressure of reaction system reach 2.0MPa, and heating reaction furnace makes reaction temperature reach 300 DEG C of reactions, finally
Reaction product is taken out, using gas chromatographic analysis.
Comparative example 10
The preparation of catalyst
Water absorption rate according to mesoporous carbon (MC) (mesoporous carbon is handled with 2M concentrated hydrochloric acids in advance) accurately weighs carrier, is roasted through drying
Impregnated carrier is used as after burning, 0.27g ammonium molybdates are dissolved in pure water, obtain maceration extract；By the body such as maceration extract and impregnated carrier
Product dipping, impregnates 12h at room temperature, and the presoma of catalyst is obtained after drying；The presoma that will be obtained, carry out multistage journey
Sequence temperature reaction；Under the atmosphere of hydrogen temperature rate be 5 DEG C/min rise to 350 DEG C from room temperature, using warm speed as 1 DEG C/min from
350 DEG C are warming up to 450 DEG C, and 600 DEG C of final temperatures are risen to from 450 DEG C by 5 DEG C/min of heating rate, hydrogen now is converted into ammonia
Gas, kept for 2 hours in final temperature, obtain 10%MoN/MC catalyst.
In fixed bed reactors, 10%MoN/MC catalyst 2ml, liquid hourly space velocity (LHSV) (LHSV) 3h of reaction raw materials are added-1,
Being filled with hydrogen makes the reaction pressure of reaction system reach 2.0MPa, and heating reaction furnace makes reaction temperature reach 300 DEG C of reactions, finally
Reaction product is taken out, using gas chromatographic analysis.
Comparative example 11
The preparation of catalyst
Water absorption rate according to mesoporous carbon (MC) (mesoporous carbon is handled with 2M concentrated hydrochloric acids in advance) accurately weighs carrier, is roasted through drying
Impregnated carrier is used as after burning, 0.27g ammonium molybdates are dissolved in pure water, obtain maceration extract；By the body such as maceration extract and impregnated carrier
Product dipping, impregnates 12h at room temperature, and the presoma of catalyst is obtained after drying；The presoma that will be obtained, carry out multistage journey
Sequence temperature reaction；Under the atmosphere of hydrogen temperature rate be 5 DEG C/min rise to 350 DEG C from room temperature, using warm speed as 1 DEG C/min from
350 DEG C are warming up to 450 DEG C, and 800 DEG C of final temperatures are risen to from 450 DEG C by 5 DEG C/min of heating rate, hydrogen now is converted into ammonia
Gas, kept for 2 hours in final temperature, obtain 10%MoN/MC catalyst.
In fixed bed reactors, 10%MoN/MC catalyst 2ml, liquid hourly space velocity (LHSV) (LHSV) 3h of reaction raw materials are added-1,
Being filled with hydrogen makes the reaction pressure of reaction system reach 2.0MPa, and heating reaction furnace makes reaction temperature reach 300 DEG C of reactions, finally
Reaction product is taken out, using gas chromatographic analysis.
Comparative example 12
The preparation of catalyst
Water absorption rate according to mesoporous carbon (MC) (mesoporous carbon is handled with 2M concentrated hydrochloric acids in advance) accurately weighs carrier, is roasted through drying
Impregnated carrier is used as after burning, 0.27g ammonium molybdates are dissolved in pure water, obtain maceration extract；By the body such as maceration extract and impregnated carrier
Product dipping, impregnates 12h at room temperature, and the presoma of catalyst is obtained after drying；The presoma that will be obtained, carry out multistage journey
Sequence temperature reaction；It is 1 in nitrogen and hydrogen volume:Temperature rate is that 5 DEG C/min rises to 350 DEG C from room temperature under 3 atmosphere, with temperature
Speed is that 1 DEG C/min is warming up to 450 DEG C from 350 DEG C, 700 DEG C of final temperatures is risen to from 450 DEG C by 5 DEG C/min of heating rate, now
Hydrogen is converted into ammonia, is kept for 2 hours in final temperature, obtains 10%MoN/MC catalyst.
In fixed bed reactors, 10%MoN/MC catalyst 2ml, liquid hourly space velocity (LHSV) (LHSV) 3h of reaction raw materials are added-1,
Being filled with hydrogen makes the reaction pressure of reaction system reach 2.0MPa, and heating reaction furnace makes reaction temperature reach 300 DEG C of reactions, finally
Reaction product is taken out, using gas chromatographic analysis.
Performance comparision of the catalyst to guaiacol hydrogenation deoxidation made from the embodiment of table 1 and comparative example
It is higher that table 1 illustrates that support type Nitrides Catalysts prepared by this method have to the reaction of guaiacol hydrogenation deoxidation
Activity and there is higher selectivity to benzene.
It should be appreciated that for those of ordinary skills, can according to the above description be improved or converted,
And all these modifications and variations should all belong to the protection domain of appended claims of the present invention.
Claims (7)
- A kind of 1. molybdenum nitride hydrogenation deoxidation catalyst, it is characterised in that：The catalyst is using mesoporous carbon as carrier, with molybdenum nitride As active component, wherein, active component accounts for the 5~50% of catalyst gross mass in terms of molybdenum trioxide quality.
- A kind of 2. preparation method of molybdenum nitride hydrogenation deoxidation catalyst as claimed in claim 1, it is characterised in that：The preparation Method comprises the following steps that：A. mesoporous carbon is handled with 2M concentrated hydrochloric acids in advance, then the water absorption rate according to mesoporous carbon accurately weighs mesoporous carbon, passes through Impregnated carrier is used as after drying and roasting；B. ammonium molybdate is dissolved in pure water, obtains maceration extract；C. the impregnated carrier incipient impregnation that maceration extract step (b) obtained obtains with step (a), impregnates 12h at room temperature, The presoma of catalyst is obtained after drying；D. the presoma of catalyst step (c) obtained, first it is carbonized and nitrogenizes to obtain Nitrides Catalysts again.
- 3. the preparation method of molybdenum nitride hydrogenation deoxidation catalyst as claimed in claim 2, it is characterised in that：Institute in step (c) The drying condition stated is：1~12h is dried in drying box at 100~120 DEG C.
- 4. the preparation method of molybdenum nitride hydrogenation deoxidation catalyst as claimed in claim 2, it is characterised in that：Institute in step (d) Stating the presoma condition nitrogenized again that is first carbonized is：Temperature rate is that 5~10 DEG C/min rises to 350 from room temperature under the atmosphere of hydrogen DEG C, 450 DEG C are warming up to from 350 DEG C using heating rate as 0.5~1 DEG C/min, is 2~10 DEG C/min from 450 DEG C using heating rate 650 DEG C~750 DEG C final temperatures are risen to, hydrogen is now converted into ammonia, are kept for 1~5 hour in final temperature.
- A kind of 5. application of molybdenum nitride hydrogenation deoxidation catalyst as claimed in claim 1, it is characterised in that：The catalyst is used It is as follows in the hydrogenation deoxidation reaction of catalysis guaiacol, its method：Using guaiacol as raw material, it is catalyzed in solvent and hydrogenation deoxidation Under the conditions of agent is existing, adds hydrogen and carry out hydrogenation deoxidation reaction.
- 6. the application of molybdenum nitride hydrogenation deoxidation catalyst as claimed in claim 5, it is characterised in that：The hydrogenation deoxidation reaction Condition is：Reaction temperature is 300~400 DEG C, and Hydrogen Vapor Pressure is 1~4MPa.
- 7. the application of molybdenum nitride hydrogenation deoxidation catalyst as claimed in claim 5, it is characterised in that：The solvent is positive ten The mass ratio of alkane, guaiacol and decane is 1: 50~1: 100.
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| CN109482212A (en) * | 2018-11-12 | 2019-03-19 | 大连理工大学 | A kind of preparation and its biomass hydrogenation deoxidation application of low temperature self assembly molybdenum carbide nano-wire catalyst |
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| CN110606800A (en) * | 2019-09-27 | 2019-12-24 | 常州大学 | Method for preparing phenol from guaiacol by taking spherical nano carbon-coated molybdenum nitride as catalyst |
| CN111229283A (en) * | 2020-03-04 | 2020-06-05 | 常州大学 | Noble metal modified Mo2Preparation method of N/OMC catalyst and application of N/OMC catalyst in biomass oil hydrodeoxygenation |
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| CN115025801A (en) * | 2022-06-08 | 2022-09-09 | 中国矿业大学 | Nitrogen-doped carbon-supported CoMoS catalyst and preparation method and application thereof |
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