CN104056631B - Method for activating Ni/AC catalyst in microwave heating way - Google Patents
Method for activating Ni/AC catalyst in microwave heating way Download PDFInfo
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- CN104056631B CN104056631B CN201410253994.8A CN201410253994A CN104056631B CN 104056631 B CN104056631 B CN 104056631B CN 201410253994 A CN201410253994 A CN 201410253994A CN 104056631 B CN104056631 B CN 104056631B
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Abstract
The invention provides a method for activating a Ni/AC catalyst in a microwave heating way. The method comprises the following steps of preparing a Ni/AC catalyst precursor; performing roasting; and performing microwave radiation. According to the method, the principle of absorbing microwaves to generate resonant heating by AC is used for providing heat for reaction; meanwhile, by virtue of a resonant effect of the microwaves on the AC and the influence of the microwaves on the dispersion of metal nickel as well as particle sizes and apertures thereof, the specific surface area of the catalyst is large, active ingredients can be uniformly dispersed, and the catalytic activity of the catalyst is high.
Description
Technical field
The invention belongs to activation of catalyst technical field, particularly to a kind of side of microwave heating activation Ni/AC catalyst
Method.
Background technology
The activation of catalyst typically adopts conventional electrical heating high-temperature hydrogen reduction method and sodium borohydride local reduction way.
The use of electrical heating high-temperature hydrogen reduction method is more generally it is adaptable to the reduction of most of catalyst, mainly right
Catalyst precursor passes through heat treated, so that complex catalyst precursor oxide body is combined with hydrogen, and reduction obtains with catalysis activity
Elemental metals and hydrone.
For the activation processing of noble metal catalyst, after noble metal hydrogen reducing is complete, active component activity is of a relatively high, exposes
Being exposed at easy and in the air the oxygen of in the air to combine, aoxidizing, so needing in high temperature reduction noble metal to be passivated locating
Reason, to ensure its activity, like this can lose it amount of activated.
Sodium borohydride reduction is used primarily in the reduction of noble metal, due to and sodium borohydride reduction utilizes sodium borohydride
Superpower reproducibility make metal-oxide reduce obtain elemental metals, the catalyst due to obtaining is present in aqueous solution, thus
It is difficult oxidized it is ensured that it is active, thus the multiplex sodium borohydride reduction of reduction of noble metal.
Although Ni/AC catalyst also can sodium borohydride reduction, for the larger nickel-base catalyst of load capacity,
One is sodium borohydride large usage quantity, than relatively hazardous.Two is that sodium borohydride reduction loading type nickel-based catalyst can cause substantial amounts of work
Property component run off, reduce catalyst activity.And there is reduction thoroughly in routine thermal reduction, the low problem of catalyst activity.
Content of the invention
In order to overcome the problem that in prior art, Ni/AC activation of catalyst exists, the invention provides a kind of microwave heating
The method of activation Ni/AC catalyst.
A kind of method of microwave heating activation Ni/AC catalyst, comprises the steps：
1) roasting：
Ni/AC catalyst precursor is positioned over 450 DEG C of roasting 4h in Muffle furnace, obtains the nickel of oxidation state；
2) microwave radiation：
By 1) in the material that obtains in presence of hydrogen, hydrogen flow rate is 60-100mL/min, heats up under microwave radiation
To 350-500 DEG C of reductase 12-4h, after cooling, obtain Ni/AC catalyst.
Preferably, step 2) in, microwave irradiation power is 1-1.5kW.
The present invention is the improvement to high-temperature hydrogen reduction method, is primarily directed to the reduction of Ni/AC catalyst, using AC's
Absorb the principle that microwave produces resonant heating, while providing heat for reaction, due to the resonance effect to AC for the microwave, to metallic nickel
Dispersion and its particle diameter and aperture impact, make the specific surface area of catalyst bigger, active component dispersion be more uniformly distributed, catalysis
Activity is higher.
Specific embodiment
Preparation 15%Ni/AC catalyst precursor：
Take 29g Nickelous nitrate hexahydrate deionized water constant volume in 50mL volumetric flask, take the bodies such as 10mL above-mentioned solution employing
The method of long-pending dipping is impregnated on 5g activated carbon, and stirring fully, stands 12h, 110 DEG C are dried 12h, are ground into powder, obtain
Ni/AC catalyst precursor.
The Ni/AC catalyst precursor mentioned in comparative example 1 and embodiment 1-3 is to be prepared according to the method described above.
Comparative example 1：
The presoma of the Ni/AC catalyst being obtained using incipient impregnation, takes sample 1g to add using conventional electricity after roasting
The method of heat, in H2Under existence condition, hydrogen flow rate be 80mL/min, temperature control at 500 DEG C, constant temperature 4h, cooling obtain Ni/
AC catalyst.It is named as Ni/AC-Normal
Embodiment 1：
The presoma of the Ni/AC catalyst being obtained using incipient impregnation, takes sample 1g to adopt microwave radiation after roasting
Method, in H2Under existence condition, hydrogen flow rate is 80mL/min, and microwave emitter output is 1.5Kw, and temperature control exists
350 DEG C, constant temperature 2h, cooling obtains Ni/AC catalyst.Gained catalyst is named as Ni/AC-Microwave1.
Embodiment 2：
Method is 400 DEG C with embodiment 1, except for the difference that reduction temperature, and gained catalyst is named as Ni/AC-
Microwave2.
Embodiment 3：
Method is 500 DEG C with embodiment 1, except for the difference that reduction temperature, and the recovery time is 4h, and gained catalyst is named as
Ni/AC-Microwave3.
Application examples 1：
The product of comparative example and embodiment is used in the reaction that glucose hydrogenation prepares Sorbitol, takes 50mL10Wt% Portugal
Grape sugar juice is placed in 100mL high-temperature high-pressure reaction kettle, plus the catalyst of the above-mentioned gained of 0.5g, and reaction condition is initial H2Pressure
For 4Mpa, reaction temperature is 100 DEG C, reacts 2h, takes supernatant to do liquid chromatograph, compare Sorbitol yield.
| Catalyst | Inversion rate of glucose | Sorbitol yield |
| Ni/AC-Normal | 92.10% | 89.10% |
| Ni/AC-Microwave1 | 98.30% | 97.30% |
| Ni/AC-Microwave2 | 99.10% | 98.10% |
| Ni/AC-Microwave3 | 99.20% | 98.20% |
React under the same terms, compare Sorbitol yield it is found that the activity of the catalyst of microwave method activation is more conventional
The activity height being prepared by glucose hydrogenation to Sorbitol reaction of the catalyst that electrical heating activation obtains.
Application examples 2：
The product of comparative example and embodiment is used for furfuryl alcohol Hydrogenation in the reaction of tetrahydrofurfuryl alcohol, taking 50mL40Wt% bran
Alcoholic solution (methanol is as solvent) is placed in 100mL high-temperature high-pressure reaction kettle, plus the catalyst of the above-mentioned gained of 0.5g, reaction condition
For initial H2Pressure is 3Mpa, and reaction temperature is 120 DEG C, reacts 0.5h, takes supernatant to do liquid chromatograph, compare the conversion of furfuryl alcohol
Rate and the selectivity of tetrahydrofurfuryl alcohol.
Under identical reaction condition, the catalyst of microwave method activation is prepared in the reaction of tetrahydrofurfuryl alcohol for furfuryl alcohol no matter
Be the conversion ratio of furfuryl alcohol or the selectivity of tetrahydrofurfuryl alcohol all high than the catalyst that conventional heating mode obtains it can be seen that microwave
The reaction that the activity and selectivity of the catalyst of method activation prepares tetrahydrofurfuryl alcohol in furfuryl alcohol is an advantage over what conventional heating mode reduced
Catalyst.
Claims (1)
1. a kind of method of microwave heating activation Ni/AC catalyst it is characterised in that：Comprise the steps：1) roasting：By Ni/
AC catalyst precursor is positioned over 450 DEG C of roasting 4h in Muffle furnace, the nickel of the oxidation state obtaining being carried on AC；2) microwave spoke
Penetrate：By 1) in the material that obtains in presence of hydrogen, hydrogen flow rate is 60-100mL/min, is warming up to 350- under microwave radiation
500 DEG C of reductase 12-4h, obtain Ni/AC catalyst after cooling；Step 2) in, microwave irradiation power is 1-1.5kW.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410253994.8A CN104056631B (en) | 2014-06-10 | 2014-06-10 | Method for activating Ni/AC catalyst in microwave heating way |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410253994.8A CN104056631B (en) | 2014-06-10 | 2014-06-10 | Method for activating Ni/AC catalyst in microwave heating way |
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| Publication Number | Publication Date |
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| CN104056631A CN104056631A (en) | 2014-09-24 |
| CN104056631B true CN104056631B (en) | 2017-02-08 |
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| CN105032428B (en) * | 2015-07-10 | 2019-03-01 | 湖北大学 | A kind of preparation method of microwave heating synthetic catalyst and the method that catalyst one-step synthesis method cyclohexylamine is made based on the preparation method |
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| TWI318897B (en) * | 2006-06-01 | 2010-01-01 | Ritek Corp | Method of preparing catalyst for catalyzing carbon nanotubes growth |
| CN101323909B (en) * | 2008-07-17 | 2010-06-23 | 东北大学 | Method of microwave selective reduction roasting-dilute acid leaching nickel oxide ore |
| CN102029169B (en) * | 2009-09-29 | 2014-03-26 | 中国科学院大连化学物理研究所 | Method for preparing loaded transitional metal phosphide catalyst |
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Granted publication date: 20170208 |