CN107224981A - A kind of titanium dioxide hollow ball load PdNi alloy nano catalyst and its preparation method and application - Google Patents
A kind of titanium dioxide hollow ball load PdNi alloy nano catalyst and its preparation method and application Download PDFInfo
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- CN107224981A CN107224981A CN201710493032.3A CN201710493032A CN107224981A CN 107224981 A CN107224981 A CN 107224981A CN 201710493032 A CN201710493032 A CN 201710493032A CN 107224981 A CN107224981 A CN 107224981A
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
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- C01B3/068—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by reaction of inorganic compounds containing electro-positively bound hydrogen, e.g. water, acids, bases, ammonia, with inorganic reducing agents the hydrogen being generated from the water as a result of a cyclus of reactions, not covered by groups C01B3/063 or C01B3/105
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Abstract
The present invention provides a kind of titanium dioxide hollow ball load PdNi alloy nano catalyst and its preparation method and application, and the catalyst includes active component and carrier；The active component is PdNi alloy nano particles, and the particle diameter of the PdNi alloy nano particles is 4.1~5.5nm；The carrier is titanium dioxide hollow ball, and a diameter of 2.1~3.0 μm of the titanium dioxide hollow ball, aperture is 0.33~0.5 μm.The present invention is big with the specific surface area of prepared above-mentioned catalyst, and PdNi alloy nanos, which are supported on inside and outside hole, uniformly to be inlayed, and increases load capacity, and the particle diameter of PdNi alloy nano particles is small, and active site is more, can significantly improve the activity and stability of catalyst；The catalyst is released into hydrogen for ammonia borane hydrolysis：At room temperature, its maximum hydrogen discharging rate is up to 105.36mol H2min‑1(mol Pd)‑1, the activation energy of reaction is 24.86kJ mol‑1；The preparation method technique is simple, and raw material is easy to get, with low cost, it is easy to implement, and is suitable for industrialized production, has a extensive future.
Description
Technical field
Hydrogen catalyst technology is explained the present invention relates to catalytic water, and in particular to a kind of titanium dioxide hollow ball load PdNi is closed
Gold nano catalyst and its preparation method and application, belongs to hydrogen storage material field.
Background technology
How safely and efficiently Hydrogen Energy is considered as a kind of new cleaning fuel and has the green energy resource of broad prospect of application,
It is great challenge for researcher to produce and store hydrogen.In recent years, chemical hydride is because of its high hydrogen content and low molecule amount
As the hydrogen storage material for most having development potentiality.Wherein ammonia borine (NH3BH3, abbreviation AB) and there is relatively low molecular weight (30.87g/
MCl) and high quality hydrogen-storage density (19.6wt%) and as most promising solid hydrogen storage material.Ammonia borine performance is stable,
Production hydrogen can be hydrolyzed in the presence of catalyst, therefore, it is the key for realizing ammonia borane hydrolysis hydrogen manufacturing to explore efficient catalyst.
The document of catalysis ammonia borane hydrolysis hydrogen manufacturing so far has a lot, and research shows, it is adaptable to which ammonia borane hydrolysis reacts
Catalyst be mainly precious metals pt base and Ru base catalyst, (J Power Sources, 2006,156:190-4；
Inorg.Chem.2007,46:788-94；Microporous Mesoporous Mater.2016,225:1-8；Int J
Hydrogen Energy, 2015,40: 15521-8).Although Pt bases and Ru bases catalyst show significant catalytic activity, but
Its cost is high, abundance is low, it is difficult to realize industrialization.And precious metals pd price is relatively cheap, and non-noble metal Ni has preferably
Cooperative effect, catalytic activity is high, if by Pd and Ni concerted catalysis, can not only reduce production cost, and can significantly improve Pd's
Catalytic activity.Due to active relevant, the stability of metallic also with the distribution of particle size, avtive spot of metallic catalyst
Influence its catalytic life, thus possessing the carrier of big specific surface area and loose structure contributes to metallic to be uniformly dispersed, grain
Son is more stablized, and catalytic activity is higher.
In numerous backing materials, TiO2Nontoxic, efficient, cheap, environment-friendly and chemical inertness, which turns into, most to be had
One of catalyst carrier of potentiality.And TiO2Hollow ball more shows the advantage of uniqueness：Big specific surface area, loose structure can be very
Good loading particle, the particle of load is more stablized, excellent electronics and optical property (J Alloy Compd.2014,612:
69-73；Chem.Soc.Rev.2015,44:1861-85).But in catalyst field, TiO2It is commonly used in photochemical catalyst, such as
Chinese invention patent (application number：201510082234.X, the applying date：2015.02.15 a kind of metal-nitrogen co-doped) is provided
Titanium dioxide hollow ball catalyst and preparation method thereof, the catalyst adulterates nickel and nitrogen in titanium dioxide hollow ball, is
A kind of photochemical catalyst.
According to literature survey, in TiO2PdNi alloy nano particles are loaded in hollow ball and catalyzing hydrolysis ammonia boron is used it for
The research of alkane is not reported also.
In view of this, the present invention proposes a kind of titanium dioxide hollow ball load PdNi alloy nanos catalyst and its preparation side
Method and application, to solve the above problems.
The content of the invention
It is an object of the invention to overcome the shortcomings of existing product, there is provided a kind of titanium dioxide hollow ball load PdNi alloys
Nanocatalyst and its preparation method and application.Using titanium dioxide hollow ball as carrier, and its specific surface area is big, and PdNi alloys are received
Rice, which is supported on inside and outside hole, uniformly to be inlayed, and increases load capacity, the particle diameter of PdNi alloy nano particles is small, active site
It is many, the activity and stability of catalyst can be significantly improved；The preparation method technique is simple, and raw material is easy to get, with low cost, it is easy to real
Apply, be suitable for industrialized production, have a extensive future.
In order to achieve the above object, the technical solution adopted in the present invention is：A kind of titanium dioxide hollow ball loads PdNi
Alloy nano catalyst, including active component and carrier；The active component is PdNi alloy nano particles, the PdNi alloys
The particle diameter of nano-particle is 4.1~5.5nm；The carrier is titanium dioxide hollow ball, the diameter of the titanium dioxide hollow ball
For 2.1~3.0 μm, aperture is 0.33~0.5 μm.
A kind of titanium dioxide hollow ball loads the preparation method of PdNi alloy nano catalyst, comprises the following steps：
(1) by titanium potassium oxalate K2TiO(C2O4)2·2H2O is dissolved in deionized water and obtains colourless transparent solution, into the solution successively
Add H2O2, hydrochloric acid, after stirring, be added in the stainless steel cauldron of polytetrafluoroethyllining lining seal, in constant temperature 160
12h is reacted under the conditions of DEG C, room temperature is naturally cooled to, filters, wash, be dried in vacuum overnight, obtain titanium dioxide hollow ball
(TiO2HS) white powder；
(2) by TiO obtained by above-mentioned steps (1)2HS is added in deionized water, then palladium salt and nickel salt solution is added dropwise, ultrasound
After 20min, continue magnetic agitation 5h, obtain suspension；
(3) by reducing agent NaBH4It is dissolved in deionized water, and is added dropwise in the suspension of step (2), after completion of dropping
Continue to stir 3h；Product is filtered, wash, is dried in vacuum overnight, PdNi/TiO is obtained2HS catalyst.
Further, titanium potassium oxalate, deionized water, H described in step (1)2O2Mol ratio with hydrochloric acid is 1：410：
72.3：11.9.
Further, the mol ratio of the nickel in the palladium and nickel salt described in step (2) in palladium salt is 1：0.6.
Further, palladium salt described in step (2) is H2PdCl4, described nickel salt is soluble nickel salt.
A kind of titanium dioxide hollow ball loads the application of PdNi alloy nano catalyst, and the catalyst is in catalysis ammonia borine water
Explain the application in hydrogen.
The beneficial effects of the invention are as follows：
1st, the TiO prepared by the present invention2HS has big surface area and pore space structure, and PdNi alloy nanos are supported on inside and outside hole
Uniformly inlay, increase load capacity, utilize synergy strong between Pd and Ni and PdNi alloy nano particles and TiO2HS
Between difunctional effect, so as to effectively increase Pd mithridatism, obtained the PdNi/ with good mithridatism and stability
TiO2HS catalyst.
2nd, by the PdNi/TiO2HS catalyst releases hydrogen for being catalyzed ammonia borane hydrolysis：At room temperature, its maximum hydrogen discharging rate
Up to 105.36mol H2min-1(mol Pd)-1, the activation energy of reaction is 24.86kJ mol-1。
3rd, the catalyst uses solwution method fabricated in situ, and technique is simple, with low cost, it is easy to implement, and is easy to push away on a large scale
Wide application.
Brief description of the drawings
Fig. 1 is the TiO prepared by embodiment one2The SEM figures of hollow ball；
Fig. 2 is the PdNi/TiO prepared by embodiment one2The TEM figures of HS catalyst；
Fig. 3 is the PdNi/TiO prepared by embodiment one2Pd XPS spectrum figure in HS catalyst；
Fig. 4 is the PdNi/TiO prepared by embodiment one2Ni XPS spectrum figure in HS catalyst；
Fig. 5 is the TiO prepared by embodiment one2HS and PdNi/TiO2Monometallic load prepared by HS catalyst, embodiment two
Mixed type (Pd/TiO2HS+Ni/TiO2HS) catalyst, the carrier-free PdNi nano-particles prepared by embodiment three are catalyzed ammonia respectively
Borane hydrolysis produces the rate diagram of hydrogen；
Fig. 6 is the PdNi/TiO prepared by embodiment one2HS catalyst is catalyzed ammonia boron at 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C of water-bath
The hydrogen discharging performance test of alkane hydrolysis and activation energy test chart one；
Fig. 7 is the PdNi/TiO prepared by embodiment one2HS catalyst is catalyzed ammonia boron at 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C of water-bath
The hydrogen discharging performance test of alkane hydrolysis and activation energy test chart two.
Embodiment
In order to be better understood from the present invention, below in conjunction with the accompanying drawings with the embodiment content that the present invention is furture elucidated, but this
The content of invention is not limited solely to the following examples.
Embodiment one：TiO2Hollow ball (TiO2HS)、PdNi/TiO2The preparation of HS loaded catalysts
(1) 1.8g titanium potassium oxalate K is weighed2TiO(C2O4)2·2H2In O, the beaker for adding it to 100mL, add into beaker
Enter 37.5mL deionized water, magnetic agitation until forming colourless transparent solution.Then 37.5mL H are sequentially added2O2With 5mL salt
Acid, is stirred for after about 5min, and being added to 100mL has in the stainless steel cauldron of polytetrafluoroethyllining lining, under the conditions of 160 DEG C
12h is reacted, natural cooling is filtered, washing, and 80 DEG C are dried in vacuum overnight, and obtain titanium dioxide hollow ball (TiO2HS) white powder
End.Wherein described H2O2Mass fraction be 30%, the mass fraction of the hydrochloric acid is 37%.
(2) 70.93mg PdCl is weighed2It is added in the small beaker for filling a small amount of concentrated hydrochloric acid, is stirred at room temperature to solid
Body is completely dissolved, and transfers it to constant volume in 100mL volumetric flasks, and 0.04mol/L H is made2PdCl4Solution.
(3) 100mg TiO are weighed2HS is added in 30mL deionized waters, adds 2.5mL 0.04mol/L H2PdCl4
With 1.5mL 0.04mol/L Ni (NO3)2·6H2Continue to stir 5h after O, ultrasonic 10min, obtain suspension.
(4) 50.0mg reducing agent NaBH is weighed4The solution is added dropwise to by solid dissolving in 10mL deionized waters
Continue to stir 3h after the metal ion being used in reducing solution in above-mentioned suspension, completion of dropping.Product is filtered, washed, very
Sky is dried overnight, and obtains PdNi/TiO2HS。
The TiO prepared to embodiment one2HS is scanned electronic microscope photos：It will be seen from figure 1 that the TiO of synthesis2Hollow ball
Diameter at 2.1~3.0 μm, aperture is 0.33~0.5 μm, and surface of shell is by many TiO2Nanometer rods are constituted.To embodiment one
The PdNi/TiO of preparation2HS catalyst carries out transmission electron microscope analysis：From figure 2 it can be seen that PdNi alloy nano particles are uniform
Ground is distributed in TiO2HS surface, particle diameter is 4.1~5.5nm.Fig. 3 and figure are PdNi/TiO2The XPS collection of illustrative plates of HS catalyst, from
As can be seen that the catalyst has Pd 3d signal peaks, at 335.6eV and 340.8eV in Fig. 3；It can be seen that from Fig. 4
Ni 2p signal peaks, positioned at 856.5eV, 862.4eV, 873.8eV, at 879.0eV.By Fig. 3 and Fig. 4 fully prove element palladium and
Nickel is successfully carried on TiO2On hollow ball.
Embodiment two：Monometallic load mixed type (Pd/TiO2HS+Ni/TiO2HS) the preparation of catalyst
Weigh the TiO prepared by 100mg above-described embodiments one2HS is added in 30mL deionized waters, adds 2.5mL
0.04mol/L H2PdCl4, continue after ultrasonic 10min to stir 5h, obtain suspension.Then 50.0mg reducing agent is weighed
NaBH4The solution is added dropwise to the metal in above-mentioned suspension in reducing solution by solid dissolving in 10mL deionized waters
Continue to stir 3h after ion, completion of dropping.Product is filtered, wash, is dried in vacuum overnight, Pd/TiO is obtained2HS catalyst.
Weigh the TiO of 100mg above-described embodiments one2HS is added in 30mL deionized waters, adds 1.5mL 0.04
mol/L Ni(NO3)2·6H2Continue to stir 5h after O, ultrasonic 10min, obtain suspension.Then 50.0mg reducing agent is weighed
NaBH4The solution is added dropwise to the metal in above-mentioned suspension in reducing solution by solid dissolving in 10mL deionized waters
Continue to stir 3h after ion, completion of dropping.Product is filtered, wash, is dried in vacuum overnight, Ni/TiO is obtained2HS catalyst.
Weigh same amount of Pd/TiO2HS and Ni/TiO2HS is mixed, and obtains monometallic load mixed type (Pd/
TiO2HS +Ni/TiO2HS) catalyst.
Embodiment three：The preparation of DNAcarrier free PdNi nano-particles
Measure 2.5mL 0.04mol/L H2PdCl4With 1.5mL 0.04mol/L Ni (NO3)2·6H2O be added to 30mL go from
In sub- water, ultrasound obtains dispersed solution after 10 minutes.Then, by 50.0mg NaBH4Solid is dissolved in 10mL deionizations
In water, the solution is added dropwise to after above-mentioned solution, completion of dropping and continues to stir 3h.Product is filtered, washed, 80 DEG C true
Sky is dried overnight, and obtains PdNi NPs catalyst.
Catalyst prepared by embodiment one, embodiment two and embodiment three is tested ammonia borane hydrolysis H2-producing capacity and living
Change can be tested
Catalyst prepared by embodiment one, embodiment two and embodiment three is catalyzed ammonia borane hydrolysis respectively, its reaction is determined
Speed：Take 18.5mg ammonia borines to be placed in 50mL round-bottomed flasks bottom, at 25 DEG C of water-bath, 20mL deionized waters are added, in stirring
Under the conditions of add the above-mentioned catalyst of 10mg, be catalyzed ammonia borane hydrolysis, with drainage measure hydrogen desorption capacity, and every 30 seconds record produce
The volume of hydrogen.Fig. 5 is to the gained TiO of embodiment one2HS and PdNi/TiO2HS, the gained monometallic of embodiment two load mixed type
(Pd/TiO2HS+Ni/TiO2HS), the gained PdNi nano-particles of embodiment three carry out catalysis ammonia borane hydrolysis and release hydrogen experiment, it is seen that
Bimetal supported catalyst PdNi/TiO2The hydrogen discharging rate of HS catalysis ammonia borane hydrolysis is maximum, with highest catalytic activity.
It is computed, catalyst PdNi/TiO2HS TOF values are 105.36mol H2min-1(mol Pd)-1。
Fig. 6-7 is the PdNi/TiO for preparing embodiment one2HS catalyst is urged at 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C of water-bath
Change hydrogen discharging performance test and the activation energy test chart of ammonia borane hydrolysis.It can be seen that, temperature is higher, and it is faster that ammonia borine releases hydrogen speed, by
Release hydrogen speed and the activation energy (Ea) of catalytic reaction is obtained for 24.86kJ mol according to Arrhenius formula calculating-1, it is seen that it is lived
Changing can be relatively low, is conducive to the quick progress of catalytic reaction.
The PdNi/TiO prepared using embodiment one2HS catalyst carries out recycling performance test, at 25 DEG C, when urging
After change ammonia borane hydrolysis is complete, then toward ammonia borine (18.5mg) test of addition equivalent in round-bottomed flask, after 5 times circulate,
Catalyst PdNi/TiO2HS catalytic activity is respectively 100%, 87.5%, 77.8%, 70.0% and 64.0%, it is seen then that this is urged
Agent has very high activity and stability.
Above-described embodiment is elaborated to the present invention.Certainly, described above not limitation of the present invention, the present invention
It is also not limited to above-mentioned example, person skilled change made in the essential scope of the present invention, retrofits, adds and add deduct
Less, replace, fall within protection scope of the present invention.
Claims (6)
1. a kind of titanium dioxide hollow ball loads PdNi alloy nano catalyst, it is characterised in that including active component and carrier；
The active component is PdNi alloy nano particles, and the particle diameter of the PdNi alloy nano particles is 4.1~5.5nm；It is described to carry
Body is titanium dioxide hollow ball, a diameter of 2.1~3.0 μm of the titanium dioxide hollow ball, and aperture is 0.33~0.5 μm.
2. a kind of titanium dioxide hollow ball according to claim 1 loads the preparation method of PdNi alloy nano catalyst,
It is characterised in that it includes following steps：
(1) titanium potassium oxalate is dissolved in deionized water and obtains colourless transparent solution, H is sequentially added into the solution2O2, hydrochloric acid, stirring
After uniform, it be added in the stainless steel cauldron of polytetrafluoroethyllining lining and seal, 12h is reacted under the conditions of 160 DEG C of constant temperature, from
Room temperature so is cooled to, filters, wash, be dried in vacuum overnight, titanium dioxide hollow ball white powder is obtained；
(2) titanium dioxide hollow ball obtained by above-mentioned steps (1) is added in deionized water, then palladium salt is added dropwise and nickel salt is molten
After liquid, ultrasonic 20min, continue magnetic agitation 5h, obtain suspension；
(3) by reducing agent NaBH4It is dissolved in deionized water, and is added dropwise in the suspension of step (2), after completion of dropping
Continue to stir 3h；Product is filtered, wash, is dried in vacuum overnight, PdNi/TiO is obtained2HS catalyst.
3. a kind of titanium dioxide hollow ball loads the preparation method of PdNi alloy nano catalyst according to claim 2, its
It is characterised by, titanium potassium oxalate, deionized water, H described in step (1)2O2Mol ratio with hydrochloric acid is 1：410：72.3：11.9.
4. a kind of titanium dioxide hollow ball loads the preparation method of PdNi alloy nano catalyst according to Claims 2 or 3,
Characterized in that, the mol ratio of the nickel in palladium and nickel salt described in step (2) in palladium salt is 1：0.6.
5. a kind of titanium dioxide hollow ball loads the preparation method of PdNi alloy nano catalyst according to claim 4, its
It is characterised by, palladium salt described in step (2) is H2PdCl4, described nickel salt is soluble nickel salt.
6. a kind of titanium dioxide hollow ball according to claim 1 loads the application of PdNi alloy nano catalyst, it is special
Levy and be, application of the catalyst in catalysis ammonia borane hydrolysis releases hydrogen.
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| CN111569904A (en) * | 2020-06-02 | 2020-08-25 | 辽宁石油化工大学 | Hollow sphere photocatalyst and preparation method and application thereof |
| CN111569904B (en) * | 2020-06-02 | 2023-09-22 | 辽宁石油化工大学 | Hollow sphere photocatalyst and preparation method and application thereof |
| CN111686752A (en) * | 2020-07-20 | 2020-09-22 | 浙江大学 | Taraxacum-shaped load type amorphous alloy catalyst and preparation method and application thereof |
| CN112717952A (en) * | 2021-02-25 | 2021-04-30 | 郑州大学 | Catalyst PtNiOx/TiO for ammonia borane hydrogen evolution by hydrolysis2-VO and preparation method thereof |
| CN112717952B (en) * | 2021-02-25 | 2022-10-25 | 郑州大学 | Catalyst PtNiO for ammonia borane hydrogen evolution by hydrolysis x /TiO 2 -V O And method for preparing the same |
| CN114050281A (en) * | 2021-11-02 | 2022-02-15 | 湖北大学 | Hollow carbon nanosphere composite catalyst and preparation method and application thereof |
| CN114050281B (en) * | 2021-11-02 | 2023-12-15 | 湖北大学 | Hollow carbon nano sphere composite catalyst and preparation method and application thereof |
| CN114377691A (en) * | 2022-01-24 | 2022-04-22 | 桂林电子科技大学 | Doughnut-shaped hollow porous Pt-Ni nanoparticle-loaded titanium oxide material and preparation method thereof |
| CN114377691B (en) * | 2022-01-24 | 2024-04-05 | 桂林电子科技大学 | Doughnut-shaped hollow porous Pt-Ni nanoparticle-loaded titanium oxide material and preparation method thereof |
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