CN109759068A - A kind of method that ultrasonic wave assisted infusion prepares Ni base catalyst - Google Patents
A kind of method that ultrasonic wave assisted infusion prepares Ni base catalyst Download PDFInfo
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- CN109759068A CN109759068A CN201910155336.8A CN201910155336A CN109759068A CN 109759068 A CN109759068 A CN 109759068A CN 201910155336 A CN201910155336 A CN 201910155336A CN 109759068 A CN109759068 A CN 109759068A
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- base catalyst
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- assisted infusion
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Abstract
The present invention provides a kind of methods that ultrasonic wave assisted infusion prepares Ni base catalyst characterized by comprising by Ni (NO3)26H2O is dissolved in deionized water, obtain maceration extract, carrier is added in maceration extract, 5~30min is shaken, is then placed in ultrasonic disperse instrument and carries out ultrasonic disperse, 50~150W of ultrasonic power, it is then allowed to stand 24-48 hours, dry 8 in 110~180 DEG C of drying boxes~for 24 hours, products therefrom is placed in 3~5h of Muffle kiln roasting, the high temperature process furnances for being placed on 500~600 DEG C in, be passed through H2With the mixed gas of Ar, 3~5h is restored, Ni base catalyst is obtained.Compared with traditional dipping technique, the catalyst that the present invention is obtained after being assisted using ultrasonic wave can significantly improve the dispersion degree of Ni, and reduce its crystallite dimension.
Description
Technical field
The present invention relates to a kind of loaded catalyst preparation methods, and in particular to ultrasonic wave assisted infusion preparation Ni base is urged
The method of agent, belongs to material and chemical field.
Background technique
In CO2In catalysis reduction, loaded catalyst is the most commonly used catalyst of research.CO2Add and is catalyzed in hydrogen methane
The catalyst of better performances has the noble metals such as Rh, Ru, Pd, Pt, Co, Mg, Ni or base metal, and common carrier has ZrO2、CeO2、
La2O3、γ-Al2O3, molecular sieve etc..From reactivity worth and economy comprehensive consideration, Ni is preferable catalyst, but due to system
The reasons such as Preparation Method cause Ni to be difficult uniformly to be supported on carrier.Current preparation method mainly has infusion process, deposition sedimentation
Method, sol-gel method and ion-exchange etc..Industrially it is divided into incipient impregnation using more still infusion process, infusion process
Method, excessive infusion process and multiple maceration.Excessive infusion process is difficult to ensure impregnation increment；Repeatedly dipping will lead to program complexity, add
Big cost input；Equi-volume impregnating is easy to cause load uneven due to contacting successive difference etc. with carrier maceration extract.
Conventional magnetic/mechanical stirring not can effectively solve this problem, and ultrasonic disperse instrument can increase dispersion degree, make Metal Supported
More evenly.
Chinese patent CN 201810166100.X proposes addition citric acid, oxalic acid, glycine, ethylenediamine and urea etc.
The stability and activity of nickel-base catalyst are improved for complexant.The patent step is various, increases preparation cost.Chinese patent
CN201611117360.5 proposes a kind of method of ultrasonic wave preparation catalyst, which filters suspension, cannot
Guarantee impregnation increment.
Summary of the invention
The object of the present invention is to provide a kind of methods that ultrasonic wave assisted infusion prepares Ni base catalyst.
In order to achieve the above object, the present invention provides the sides that a kind of ultrasonic wave assisted infusion prepares Ni base catalyst
Method characterized by comprising by Ni (NO3)26H2O is dissolved in deionized water, obtains maceration extract, and maceration extract is added in carrier
In, 5~30min is shaken, is then placed in ultrasonic disperse instrument and carries out ultrasonic disperse, 50~150W of ultrasonic power is then allowed to stand
24-48 hours, dry 8 in 110~180 DEG C of drying boxes~for 24 hours, products therefrom is placed in Muffle 3~5h of kiln roasting, later
It is placed in 500~600 DEG C of high temperature process furnances, is passed through H2With the mixed gas of Ar, 3~5h is restored, Ni base catalyst is obtained.
Preferably, the H2With H in the mixed gas of Ar2Volume ratio with Ar is 1:9.
Preferably, the Ni base catalyst is with Ni (NO3)26H2O is the source Ni, and load capacity is 3~30%.
Preferably, the sonication times are 0.2~1h.
Preferably, the maturing temperature is 350~500 DEG C, and temperature rise rate is 5~10 DEG C/min.
Preferably, the reduction temperature is 500~600 DEG C.
Preferably, the plasma water is measured with experimental titration method.
Preferably, the carrier is γ-Al2O3、ZrO2、CeO2、La2O3Or γ-Al2O3。
Compared with prior art, the beneficial effects of the present invention are:
Present invention employs ultrasonic disperse instrument instead of traditional magnetic agitation or mechanical stirring, auxiliary by ultrasonic disperse instrument
Equi-volume impregnating is helped, with Ni (NO3)26H2O is the presoma of Ni, prepares Ni base catalyst.Compared with traditional dipping technique,
It is more uniform that the catalyst that the present invention is obtained after being assisted using ultrasonic wave mixes Ni with carrier, can significantly improve the dispersion of Ni
Degree, and reduce its crystallite dimension.This reduces catalyst cost and improves CO for the utilization efficiency of raising W metal2Methanation
Efficiency all has very important significance and application value, for the CO for preparing Load Balanced2The loaded catalyst of methanation mentions
A kind of novel method is supplied.
Detailed description of the invention
Fig. 1 is the flow chart that ultrasonic wave assisted infusion prepares Ni base catalyst；
Each label meaning in figure:
Ni(NO3)2·6H2O 1, deionized water 2, beaker 3, carrier (such as γ-Al2O3、ZrO2Deng) 4, maceration extract 5, ultrasound
Sample 8, Muffle furnace 9, high temperature process furnances 10, H after separating apparatus 6, drying box 7, drying2 11、Ar 12。
Fig. 2 is gained sample Ni/ γ-Al in embodiment 12O3XRD diagram.
Fig. 3 is gained sample Ni/ZrO in embodiment 22XRD diagram.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
As shown in Figure 1, by 2.918g Ni (NO3)2·6H2O 1 is completely dissolved in 8.0ml deionized water 2, is impregnated
Liquid 5；Again by 4.000g γ-Al2O3Carrier 4 is added in above-mentioned maceration extract 5, fullys shake 10 minutes, is then placed in ultrasonic disperse instrument
100W ultrasonic wave disperses 15 minutes in 6, is then stored at room temperature 36 hours, 12 hours dry in 110 DEG C of drying boxes 7, in Muffle furnace
In 9 with the heating rate of 5 DEG C/min rise to 450 DEG C roast 3 hours, by gained sample 8 in 550 DEG C of high temperature process furnances 10 lead to
Enter H2The mixed gas of 11 and Ar 12, H2Volume ratio with Ar is 1:9, restores 3h, obtains the Ni/ γ-of 5g load capacity 15%
Al2O3Catalyst.
Embodiment 2
As shown in Figure 1, by 2.918g Ni (NO3)2·6H2O 1 is completely dissolved in 1.2ml deionized water 2, is impregnated
Liquid 5；Again by 0.300g ZrO2Carrier 4 is added in above-mentioned maceration extract 5, fullys shake 15 minutes, is then placed in ultrasonic disperse instrument 6
Middle 80W ultrasonic wave disperses 10 minutes, is then stored at room temperature 48 hours, 8 hours dry in 180 DEG C of drying boxes 7, in Muffle furnace 9
450 DEG C are risen to the heating rate of 8 DEG C/min to roast 4 hours, and gained sample 8 is passed through in 600 DEG C of high temperature process furnances 10
H2The mixed gas of 11 and Ar 12, H2Volume ratio with Ar is 1:9, restores 3h, obtains the Ni/ZrO of 5g load capacity 10%2It urges
Agent.
Embodiment 3
As shown in Figure 1, by 3.891g Ni (NO3)2·6H2O 1 is completely dissolved in 8.0ml deionized water 2, is impregnated
Liquid 5；Again by 4.000g γ-Al2O3Carrier 4 is added in above-mentioned maceration extract 5, fullys shake 20 minutes, is then placed in ultrasonic disperse instrument
50W ultrasonic wave disperses 20 minutes in 6, is then stored at room temperature 24 hours, 12 hours dry in 110 DEG C of drying boxes 7, in Muffle furnace
9, which rise to 500 DEG C with the heating rate of 5 DEG C/min, roasts 3 hours, and gained sample 8 is passed through in 550 DEG C of high temperature process furnances 10
H2The mixed gas of 11 and Ar 12, H2Volume ratio with Ar is 1:9, restores 4h, obtains the Ni/ γ-of 5g load capacity 20%
Al2O3Catalyst.
Embodiment 4
As shown in Figure 1, by 1.946g Ni (NO3)2·6H2O 1 is completely dissolved in 8.0ml deionized water 2, is impregnated
Liquid 5；Again by 4.000g γ-Al2O3Carrier 4 is added in above-mentioned maceration extract 5, fullys shake 10 minutes, is then placed in ultrasonic disperse instrument
100W ultrasonic wave disperses 15 minutes in 6, is then stored at room temperature 36 hours, 12 hours dry in 110 DEG C of drying boxes 7, in Muffle furnace 9
In with the heating rate of 10 DEG C/min rise to 450 DEG C roast 3 hours, by gained sample 8 in 550 DEG C of high temperature process furnances 10 lead to
Enter H2The mixed gas of 11 and Ar 12, H2Volume ratio with Ar is 1:9,5h is restored, the Ni/ γ-of 5g load capacity 10% is obtained
Al2O3Catalyst.
Embodiment 5
As shown in Figure 1, by 1.167g Ni (NO3)2·6H2O 1 is completely dissolved in 4.8ml deionized water 2, is impregnated
Liquid 5；Again by 0.300g γ-Al2O3Carrier is added in above-mentioned maceration extract 5, fullys shake 15 minutes, is then placed in ultrasonic disperse instrument 6
Middle 80W ultrasonic wave disperses 10 minutes, is then stored at room temperature 48 hours, 8 hours dry in 110 DEG C of drying boxes 7, in Muffle furnace 9
450 DEG C are risen to the heating rate of 8 DEG C/min to roast 4 hours, by gained sample 8 at 550 DEG C, are passed through H211 and Ar's 12 is mixed
Close gas, H2Volume ratio with Ar is 1:9, restores 3h, obtains the Ni/ γ-Al of 3g load capacity 10%2O3Catalyst.
The above description is only an embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright specification is applied directly or indirectly in other relevant technical fields,
Similarly it is included within the scope of the present invention.
Claims (8)
1. a kind of method that ultrasonic wave assisted infusion prepares Ni base catalyst characterized by comprising by Ni (NO3)26H2O
It is dissolved in deionized water, obtains maceration extract, carrier is added in maceration extract, shake 5~30min, be then placed in ultrasonic disperse
Ultrasonic disperse is carried out in instrument, 50~150W of ultrasonic power is then allowed to stand 24-48 hours, is done in 110~180 DEG C of drying boxes
Dry 8~for 24 hours, products therefrom is placed in Muffle 3~5h of kiln roasting, the high temperature process furnances for being placed on 500~600 DEG C in, lead to
Enter H2With the mixed gas of Ar, 3~5h is restored, Ni base catalyst is obtained.
2. the method that ultrasonic wave assisted infusion as described in claim 1 prepares Ni base catalyst, which is characterized in that described
H2With H in the mixed gas of Ar2Volume ratio with Ar is 1:9.
3. the method that ultrasonic wave assisted infusion as described in claim 1 prepares Ni base catalyst, which is characterized in that described
Ni base catalyst is with Ni (NO3)26H2O is the source Ni, and load capacity is 3~30%.
4. the method that ultrasonic wave assisted infusion as described in claim 1 prepares Ni base catalyst, which is characterized in that described
Sonication times are 0.2~1h.
5. the method that ultrasonic wave assisted infusion as described in claim 1 prepares Ni base catalyst, which is characterized in that described
Maturing temperature is 350~500 DEG C, and temperature rise rate is 5~10 DEG C/min.
6. the method that ultrasonic wave assisted infusion as described in claim 1 prepares Ni base catalyst, which is characterized in that described
Reduction temperature is 500~600 DEG C.
7. the method that ultrasonic wave assisted infusion as described in claim 1 prepares Ni base catalyst, which is characterized in that described
Plasma water is measured with experimental titration method.
8. the method that ultrasonic wave assisted infusion as described in claim 1 prepares Ni base catalyst, which is characterized in that described
Carrier is γ-Al2O3、ZrO2、CeO2、La2O3Or γ-Al2O3。
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Cited By (4)
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| CN110961109A (en) * | 2019-12-10 | 2020-04-07 | 盐城工学院 | Ultrasonic-microwave synergistic auxiliary preparation of Ni-Al2O3Method for preparing catalyst and its application in CO2Application in hydrogenation |
| CN112246245A (en) * | 2020-09-16 | 2021-01-22 | 华南理工大学 | Supported nickel-based catalyst and preparation method and application thereof |
| CN112973803A (en) * | 2021-03-16 | 2021-06-18 | 河南神马催化科技股份有限公司 | Catalyst impregnation roasting device |
| CN113368867A (en) * | 2021-06-24 | 2021-09-10 | 新疆至臻化工工程研究中心有限公司 | Catalyst for ultrasonic-assisted synthesis of methyl glycolate and preparation method thereof |
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| CN113368867A (en) * | 2021-06-24 | 2021-09-10 | 新疆至臻化工工程研究中心有限公司 | Catalyst for ultrasonic-assisted synthesis of methyl glycolate and preparation method thereof |
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