CN109570523A - The preparation method of nanostructure based on porous rhodium - Google Patents
The preparation method of nanostructure based on porous rhodium Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B82—NANOTECHNOLOGY
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
Abstract
The preparation method of nanostructure based on porous rhodium, first by 50mg~1000mg cationic surfactant, 1mL~10mL concentration is the rhodium salt of 10mM~50mM, 1mL~10mL concentration is that the KI of 0.01M~0.1M is added sequentially in water, ultrasonic dissolution, obtain clear liquid, add the AA aqueous solution that 0.1mL~1mL concentration is 0.1M~1M, after mixing, aging 2h~10h at 50 DEG C~100 DEG C, generate black colloid product, the black colloid product is centrifuged at a high speed, and 4~8 times are washed with water until supernatant becomes colorless transparence, obtain final product.Porous Rh nanosphere prepared by the present invention has the nano-pore structure of high opening, ultra-thin substructure unit and active atomic highly exposed on the surface, shows fabulous catalytic performance in ammonia borane hydrolysis dehydrogenation reaction.
Description
Technical field
The present invention relates to field of material technology, and in particular to a kind of preparation method of the nanostructure based on porous rhodium.
Background technique
Precious metal catalyst has been developed as most heavy in modern organic synthesis and industrial production because of its unique catalytic activity
The a part wanted.The catalytic performance of noble metal nano structure and its pattern, size, structure and chemical composition etc. have essential
Connection, porous noble metal nano structure can not only provide very high specific surface area and Kong Rong, but also have abundant high living
The edge corner atom of property.Meanwhile interconnected porous duct can provide the mass transfer rate being exceedingly fast for reactant molecule, these
All impart the not expected catalytic performance of material.
Rhodium (Rh) all shows extraordinary catalysis in many important organic reactions as one of precious metal element
Property, such as in the selective hydrogenation of unsaturated compound, C-H priming reaction, formylation reaction, silylation and
Superior catalytic performance is shown in the dehydrogenation reaction of ammonia borine.Therefore, if mutually interconnected out in Rh nanoparticle internal invention
Logical mesopore orbit, resulting materials can not only provide more active sites, and can provide for reactant quickly
Mass transfer rate, these all will bring better catalytic activity for rhodium nano material.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of nanostructure based on porous rhodium, using surfactant
Soft template method synthesizes porous Rh nanostructure, these porous Rh nanospheres show superior urge in the dehydrogenation reaction of ammonia borine
Change performance.
The technical solution adopted by the present invention is that:
The preparation method of nanostructure based on porous rhodium, first by cationic surfactant, concentration be 10mM~
The rhodium salt of 50mM, the KI that concentration is 0.01M~0.1M are successively added to the water, and ultrasonic dissolution obtains clear liquid, adds
Concentration is the AA aqueous solution (i.e. ascorbic acid) of 0.1M~1M, and after mixing, aging 2h~10h at 50 DEG C~100 DEG C is raw
At black colloid product, which is centrifuged at a high speed, and is washed with water 4~8 times and becomes colorless to supernatant
Until transparence, final product is obtained.
Further, the dosage of the cationic surfactant is 50mg~1000mg, the dosage of rhodium salt be 1mL~
The dosage of 10mL, KI are 1mL~10mL, and the dosage of water is 2mL~10mL, and the dosage of AA aqueous solution is 0.1mL~1mL.
The preparation method of nanostructure based on porous rhodium, cationic surfactant is added to the water, and is stirred at room temperature
For 10min~60min to being completely dissolved, sequentially adding rhodium salt that concentration is 10mM~50mM and concentration is the of 10mM~50mM
Two metal salts, be rapidly added after mixing concentration be 0.1M~1M AA aqueous solution, then at 50 DEG C~100 DEG C aging 2h~
10h generates black colloid product, which is centrifuged at a high speed, and is washed with water 4~8 times to supernatant change
Until colorless and transparent, final product is obtained.
Further, the dosage of the cationic surfactant is 50mg~1000mg, the dosage of rhodium salt be 0.1mL~
1mL, the dosage of the second metal salt are 0.1mL~1mL, and the dosage of water is 1mL~10mL, the dosage of AA aqueous solution be 0.1mL~
1mL。
Further, the cationic surfactant is selected from one of CTAC, OTAB, OTAC, DTAB, DTAC, HDPC (ten
Six alkyl trimethyl ammonium bromides (CTAB), hexadecyltrimethylammonium chloride (CTAC), n-octyltrimethylammonium ammonium bromide (OTAB),
N-octyltrimethylammonium ammonium chloride (OTAC), dodecyl trimethyl ammonium bromide (DTAB), dodecyl trimethyl ammonium chloride
(DTAC), hexadecylpyridinium chloride (HDPC)).
Further, the rhodium salt is RhCl3。
Further, second metal salt is selected from Na2PdCl4、H2PtCl6、CoCl2、NiCl2、Cu(CH3COO)2One of.
Wherein, Na2PdCl4(chlorine palladium acid sodium) is as second of metal precursor in rhodium-palladium bimetallic porous nanometer structure synthesis, shape
At using Pd nanoparticle as core, using porous Rh as the core-shell type bimetal nano material of shell, the effect machine of other several metal salts
It manages identical.
Beneficial effects of the present invention:
The present invention uses traditional cation surfactant as structure directing agent, rhodium salt or rhodium salt and the second metal salt
Mixture as presoma, ascorbic acid as reducing agent, by prepared after water-heat process, high speed centrifugation a series of patterns and
The highly homogeneous porous nanometer structure of partial size, the structure have the nano-pore of high opening, ultra-thin substructure unit and adjustable
The partial size and pore size of control.The soft template method synthesizes porous rhodium nanostructure, have the advantages that it is economical, efficient, flexible, can be with
It avoids synthesizing using complicated, time-consuming self-corrosion, de- alloy, the hard templates such as synthesis that are restricted based on conventional porous materials
The deficiency of method.
The forming process of porous Rh nanosphere of the invention is related to one and is typically formed crystal seed-crystal seed epitaxial growth machine
Reason, wherein surfactant (being illustrated by taking CTAB as an example) and iodide ion play the role of conclusive, the induction of CTAB molecule
The formation of Rh porous structure, and iodide ion help to obtain more regular pattern and is distributed more uniform partial size, meanwhile, porous Rh
The formation of nanostructure needs a slow rate of reduction, and ascorbic acid (AA) solution is weak reductant, can just be mentioned
For slow growth rate.
For surfactant, being oriented to method has versatility, can be used not only for the preparation of porous Rh nanosphere, can be with
The how metal porous nanostructure being used to prepare based on Rh；And iodide ion, when synthesizing porous rhodium (Rh) nanosphere iodine from
Son can reinforce the electrostatic interactions between ammonium salt class surfactant molecule and precious metal ion, can obtain having rule
The nano particle of pattern, size uniformity；And when synthesizing bimetallic porous nanometer structure, then it can be added without iodide ion, utilized
The growth of second of the metal inducement Rh introduced uses cation surface activating for preparing Pd@Rh bimetal nanostructure
Agent hexadecylpyridinium chloride (HDPC) is used as structure directing agent, radium chloride (RhCl3) and chlorine palladium acid sodium (Na2PdCl4) as gold
Belong to presoma, due to Pd reducing electrode potential ratio Rh it is low, Pd is first reduced, formed Pd nanoparticle, then Pd nanometers
The growth that particle is re-used as crystal seed induction Rh eventually forms under the guiding role of surfactant HDPC with Pd nanoparticle
For core and using porous Rh as the core-shell type bimetal nano material of shell.
The method of the present invention can go out interconnected mesopore orbit in rhodium (Rh) nanoparticle internal invention, and resulting materials are not
It is only capable of providing more active sites, and quick mass transfer rate can be provided for reactant, these features are all material
Bring not expected catalytic activity.
Porous Rh nanosphere prepared by the present invention have high opening nano-pore structure, ultra-thin substructure unit and
Highly exposed active atomic on the surface shows fabulous catalytic performance, TOF in ammonia borane hydrolysis dehydrogenation reaction
Value is much higher than most of monometallic nanocatalyst, or even is higher than some bimetal nanos based on noble metal and urges
Agent.
Detailed description of the invention
Fig. 1 is the porous rhodium nanosphere low power transmission electron microscope photo of embodiment 1；
Fig. 2 is the porous rhodium nanosphere dark field transmission electromicroscopic photograph and high-resolution-ration transmission electric-lens photo of embodiment 1；
Fig. 3 is the porous rhodium nanosphere wide-angle powder X-ray diffractogram of embodiment 1, and abscissa is 2 θ (°), ordinate
For intensity (a.u.)；
Fig. 4 is that rhodium-palladium bimetallic porous nanometer structure transmission electron microscope photo of embodiment 8 and dark field transmission Electronic Speculum are shone
Piece, a. rhodium-palladium bimetallic porous nanometer structure transmission electron microscope photo, b. rhodium-palladium bimetallic porous nanometer structure dark field are saturating
Penetrate electromicroscopic photograph, c. rhodium-palladium bimetallic porous nanometer structure high-resolution-ration transmission electric-lens photo, palladium bimetallic is porous receives for d. rhodium-
The dark field transmission electromicroscopic photograph of rice structure, e. rhodium-palladium bimetallic porous nanometer structure Pd nuclear element are distributed photo, f. rhodium-palladium
The porous rhodium shell Elemental redistribution photo of bimetallic porous nanometer structure.
Specific embodiment
Below with reference to embodiment, the invention will be further described.
Embodiment 1
By 200mg CTAB, 8mL RhCl3(30mM), 3mL KI (0.01M) and 10mL water are successively added to the molten of 30mL
In agent bottle, ultrasonic dissolution obtains red clear liquid, adds pre-prepared AA aqueous solution (0.2M, 0.5mL),
After mixing, in 60 DEG C of aging 5h, black colloid product generated is by being centrifuged at a high speed, and with a large amount of water washing
4 times.
Embodiment 2
Difference with embodiment 1 is that the dosage of CTAB is 50mg, and other conditions are identical, not enough fill in the usage amount of CTAB
When foot (50mg), the porous Rh nanostructure of lower quality, and the porous degree inside this Rh nano particle can only obtain
It is very low.
Embodiment 3
Difference with embodiment 1 is to change CTAB into PVP (polyvinylpyrrolidone), other conditions are identical, the present embodiment
Only obtain some extra small Rh nanoparticles.
Embodiment 4
Difference with embodiment 1 is that iodide ion is not introduced in synthetic system, and other conditions are identical, obtained porous rhodium
Nano particle has irregular pattern and particle size distribution range is also very wide, meanwhile, each porous rhodium nanoparticles only has
Several branches' (substructure unit), and assemble very serious.
Embodiment 5
Difference with embodiment 1 is that weak reductant AA is replaced with the stronger NaBH of reproducibility4Aqueous solution, other conditions
It is identical, it is only capable of obtaining the Rh nanoparticle of about 5nm.
Embodiment 6
Difference with embodiment 1 is, by RhCl3Concentration 90mM is progressively increased to by 30mM, other conditions are identical, obtain
The average grain diameter of porous rhodium nanosphere increases, meanwhile, the unordered worm meso-porous structure of script direction arbitrary arrangement, which is transformed into, to be had
The divergence expression meso-hole structure of sequence.
The synthesis of 7 Pt Rh bimetallic porous nanometer structure of embodiment
50mg Surfactant CTAB is added in 10mL water, 10min is stirred at room temperature to being completely dissolved, then is successively added
The RhCl of 1mL 10mM3, 1mL 0.1M KI and 1mL 50mM H2PtCl6, it is rapidly added the AA of 1mL 0.1M after mixing
Solution, then in 50 DEG C of aging 10h, black colloid product generated, which passes through, to be centrifuged at a high speed, and with a large amount of water washing 4 times
It is colorless and transparent to supernatant.
The synthesis of 8 rhodiums of embodiment-palladium bimetallic porous nanometer structure
500mg surfactant HDPC is added in 10mL water, 60min is stirred at room temperature to being completely dissolved, then successively plus
Enter the RhCl of 1mL 50mM3With the Na of 1mL 50mM2PdCl4, it is rapidly added the AA solution of 1mL 1.0M after mixing, then
100 DEG C of aging 2h, black colloid product generated is by being centrifuged at a high speed, and with a large amount of water washing 8 times to supernatant
It is colorless and transparent.
By the Na in embodiment 82PdCl4Change CoCl into2、NiCl2、Cu(CH3COO)2One of, it is more to obtain different bimetallics
Hole nanostructure.
Find out from the porous rhodium nanosphere transmission electron microscope photo of Fig. 1 and Fig. 2, the porous rhodium nanosphere of embodiment 1 has
Quasi- spherical morphology, average grain diameter are about 44nm, also with the nano-pore structure of high opening, ultra-thin substructure unit and in table
Highly exposed active atomic on face.It can further be found from its TEM photo compared with high power, each porous rhodium nanometer
Ball all has meso-hole structure abundant and ultra-thin substructure unit, and the direction of these nano-pores is arbitrary arrangement, each
Porous rhodium nanosphere is made of about 18 ultra-thin substructure units, and high-resolution TEM photo further shows this sub- knot
The size of structure unit is about 2.5nm~3.5nm, and mesoporous pore size is about 2.0nm~5.0nm.Therefore, with commercialized rhodium/carbon
(Rh/C) catalyst is compared with traditional rhodium (Rh) nanoparticle, and porous rhodium nanosphere is capable of providing more active sites and non-
Often fast mass transfer rate, and extraordinary catalytic performance will be shown.
As can be seen from Figure 3, the porous rhodium nanosphere of embodiment 1 is at 41.1 °, 47.8 °, 69.9 °, 84.4 ° and 89.1 ° in 2 θ
There is a series of sharp diffraction peak, this can be attributed to respectively face-centered cubic Rh (JCPDS no.05-0685) (111),
(200), (220), (311) and (211) diffraction crystal face, the prepared porous rhodium nanosphere of this further proof are with higher
Crystallinity.
As can be seen from Figure 4, each particle is made of a solid core and a porous shell, corresponding dark field transmission
Electromicroscopic photograph (HAADF-STEM) further demonstrates this structure, from the point of view of the Elemental redistribution of corresponding single particle, element Pd
It is all distributed across the inside of particle, and element Rh is largely distributed across the outside of particle, this illustrates internal solid particle
It is Pd, external porous shell is Rh, and corresponding high-resolution TEM photo further proves that Rh is fixed on above Pd nanoparticle
, corresponding nano pore is also high-visible.These results clearly prove, pass through the side of current surfactant guiding
Porous Rh can be successfully grown on other metal nanoparticles with different-shape and structure, to obtain core-shell structure copolymer by method
The porous bimetal nanostructure of type.
The catalyst that 1 embodiment 1 of table obtains is to the expression activitiy in the hydrolysis/dehydrogenation reaction of ammonia borine with different catalysts
Ammonia borine (NH3BH3, AB) because having very high storing hydrogen ability, and it is regarded as most promising chemistry storage
One of hydrogen material releases whole H by hydrolyzing ammonia borine energy solution2.In general, the nanoparticle based on Pd and Pt is recognized
To be a kind of efficient catalyst, very high H can be obtained under conditions of quite mild2Rate of release.The present invention passes through assessment
The ability of dehydrogenation of porous rhodium nanosphere in the hydrolysis/dehydrogenation reaction of ammonia borine verifies its catalytic performance.It is sent out in evaluation procedure
Existing, prepared porous rhodium nanosphere can release 100% H in 7.0min2(H2/ AB ≈ 3), and commercialized 5%
Rh/C catalyst then needs 8.5min, and the Rh nanoparticle of 20nm needs 18min, and commercialized 5%Pd/C catalyst even more exists
67% H can only be released in 35min2。
These results clearly prove that porous rhodium nanosphere has higher catalytic activity, although the grain of porous rhodium nanosphere
Diameter will be far longer than conventional Rh nanocatalyst (partial size of Rh/C catalyst Rh is about 1-3nm) in 40nm, but ultra-thin
Substructure unit and atom highly exposed on the surface provide more active sites, so that porous rhodium nanosphere is shown
Higher catalytic activity.
Discovery is calculated, transformation frequency (TOF) value of porous rhodium nanosphere has reached 47.3molH2·molcat -1·min-1,
This is a very high numerical value in all catalyst reported at present, to be significantly larger than some commercialized noble metals and urge
Agent (is shown in Table 1), such as the black (16.8mol of PtH2·molcat -1·min-1), the black (0.81mol of PdH2·molcat -1·min-1),
Porous Al2O3Au (the 0.33mol of loadH2·molcat -1·min-1), porous Al2O3Pd (the 1.69mol of loadH2·molcat -1·min-1) etc., also it is higher than the Ru nanocatalyst (31.5mol of some autonomous Design preparationsH2·molcat -1·min-1),
Also it is higher than the homogeneous catalyst of some Rh and the Rh catalyst of other porous material loadings simultaneously, for example, Rh (1,5-COD)
The TOF value of (μ-Cl) is 13.5molH2·molcat -1·min-1, the TOF value of Rh catalyst of zeolite molecular sieve load is
13.6molH2·molcat -1·min-1.It is some by noble metal based on bimetal nano catalyst in, porous rhodium nanosphere
Activity also rank among the best, TOF value is apparently higher than AuCo (16.58molH2·molcat -1·min-1), PdCo
(28.2molH2·molcat -1·min-1) etc. bimetallic catalysts.
These results explanation, in the hydrolysis/dehydrogenation reaction of ammonia borine, porous rhodium nanosphere is an excellent catalyst,
Compared with commercialized rhodium/carbon (Rh/C) catalyst and traditional rhodium (Rh) nanoparticle, with higher conversion ratio and more preferably
Selectivity, in the chemical hydrogen storage in future and the building of fuel cell have biggish application potential.
Claims (7)
1. the preparation method of the nanostructure based on porous rhodium, which is characterized in that be by cationic surfactant, concentration first
The rhodium salt of 10mM~50mM, the KI that concentration is 0.01M~0.1M are added sequentially in water, and ultrasonic dissolution obtains clear liquid,
The AA aqueous solution that concentration is 0.1M~1M is added, after mixing, aging 2h~10h at 50 DEG C~100 DEG C generates black
The black colloid product is centrifuged at a high speed by colloid product, and is washed with water 4~8 times and becomes colorless transparence to supernatant
Until, obtain final product.
2. the preparation method of the nanostructure as described in claim 1 based on porous rhodium, which is characterized in that the cation form
The dosage of face activating agent is 50mg~1000mg, and the dosage of rhodium salt is 1mL~10mL, and the dosage of KI is 1mL~10mL, the use of water
Amount is 2mL~10mL, and the dosage of AA aqueous solution is 0.1mL~1mL.
3. the preparation method of the nanostructure based on porous rhodium, which is characterized in that cationic surfactant is added to the water,
10min~60min is stirred at room temperature to being completely dissolved, sequentially add rhodium salt that concentration is 10mM~50mM and concentration be 10mM~
The second metal salt of 50mM is rapidly added the AA aqueous solution that concentration is 0.1M~1M after mixing, then at 50 DEG C~100 DEG C
Aging 2h~10h generates black colloid product, which is centrifuged at a high speed, and be washed with water 4~8 times extremely
Supernatant becomes colorless until transparence, obtains final product.
4. the preparation method of the nanostructure as claimed in claim 3 based on porous rhodium, which is characterized in that the cation form
The dosage of face activating agent is 50mg~1000mg, and the dosage of rhodium salt is 0.1mL~1mL, the dosage of the second metal salt be 0.1mL~
1mL, the dosage of water are 1mL~10mL, and the dosage of AA aqueous solution is 0.1mL~1mL.
5. the preparation method of the nanostructure based on porous rhodium as described in Claims 1 to 4 is any, which is characterized in that described
Cationic surfactant is selected from one of CTAC, OTAB, OTAC, DTAB, DTAC, HDPC.
6. the preparation method of the nanostructure based on porous rhodium as described in Claims 1 to 4 is any, which is characterized in that described
Rhodium salt is RhCl3。
7. the preparation method of the nanostructure based on porous rhodium as described in claim 3 or 4, which is characterized in that described second
Metal salt is selected from Na2PdCl4、H2PtCl6、CoCl2、NiCl2、Cu(CH3COO)2One of.
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| CN112520692A (en) * | 2020-11-10 | 2021-03-19 | 大连理工大学 | Method for catalyzing ammonia borane hydrolysis hydrogen release by nano porous palladium catalyst |
| CN114010785A (en) * | 2021-11-23 | 2022-02-08 | 中国科学技术大学 | Porous rhodium nano material, preparation method and anti-tumor application thereof |
| CN114010785B (en) * | 2021-11-23 | 2022-10-28 | 中国科学技术大学 | Porous rhodium nano material, preparation method and anti-tumor application thereof |
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