CN109433226A - With the method for NiAgPt/ porous C exCoyOz nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation - Google Patents
With the method for NiAgPt/ porous C exCoyOz nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation Download PDFInfo
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- CN109433226A CN109433226A CN201811525088.3A CN201811525088A CN109433226A CN 109433226 A CN109433226 A CN 109433226A CN 201811525088 A CN201811525088 A CN 201811525088A CN 109433226 A CN109433226 A CN 109433226A
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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
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8933—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/894—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals also combined with metals, or metal oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with rare earths or actinides
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- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
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Abstract
The invention discloses a kind of methods with NiAgPt/ porous C exCoyOz nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation, belong to technical field of chemistry and chemical engineering.The nanocatalyst prepared is placed in reactor by the present invention, and reactor is placed in water-bath and rises to certain temperature, and then hydrazine hydrate and sodium hydroxide mixed liquor are added in reactor and react, and the hydrogen of generation is collected using drainage.Unlike existing catalyst: according to the present invention, adjusting W metal in catalyst, the high activity for hydrazine hydrate dehydrogenation hydrogen, highly selective, high stability nanocatalyst can be made in the molar ratio of mole when support precursor cerous nitrate, cobalt nitrate and 2-methylimidazole of Ag, Pt.Hydrazine hydrate dehydrogenation reaction is carried out using the catalyst, conversion rate of dehydrogenation and selectivity are 100%, and the TOF value of reaction is greater than 880h‑1, 3h is recycled, the TOF value of reaction is still greater than 874h‑1。
Description
Technical field
The invention belongs to technical field of chemistry and chemical engineering, and in particular to be urged with NiAgPt/ porous C exCoyOz nanocatalyst
Change the method for hydrazine hydrate dehydrogenation.
Background technique
Heavy environmental pollution caused by the reserves of fossil resource are limited and its a large amount of use, seeks and explores Novel clean energy
Source is the important channel that the mankind solved the above problems and realized sustainable development.Currently, hydrogen produces after having from a wealth of sources, use
The advantages that object is only water and high energy density is known as the clean and effective new energy of 21 century.Developing efficient hydrogen storage material is
Promote hydrogen energy source in the key of the large-scale application of hydrogen fuel cell.
Hydrazine hydrate has very high mass energy density (8wt%), and is in a liquid state at room temperature, can safely store
And transport.There are mainly two types of approach for hydrazine hydrate decomposition at present: the product that approach one decomposes completely only has hydrogen and nitrogen, without it
His solid by-product；Two incomplete decomposing of approach generates nitrogen and ammonia, causes the waste of hydrazine hydrate.Therefore, exploitation is efficient
Hydrazine hydrate dehydrogenation is to hydrogen using most important.
What catalyst of heap of stone to alumina load platinum in 2014 carries out nickel and is modified, and effectively raises the transformation frequency of reaction
(TOF), 16.5h but has also been only reached-1, further increase big rule of the reaction transformation frequency (TOF) for hydrazine hydrate of catalyst
Mould practical application is of great significance.This patent proposes that the method for Ni doped alloys and carrier Optimal improvements technology combine pair
The catalytic performance of catalyst optimizes regulation, it is intended to improve the stability and activity of catalyst.
Summary of the invention
It is urged in view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of with exCoyOz nanometers of NiAgPt/ porous C
The method of agent Compounds with Hydrazine Hydrate Catalyzed dehydrogenation, to the NiAgPt/ porous C exCoyOz nanocatalyst under the conditions of relatively mild
Realize the complete dehydrogenation of hydrazine hydrate.
The technical solution adopted by the present invention to solve the technical problems is as follows.
With the method for NiAgPt/ porous C exCoyOz nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation, comprises the concrete steps that: will prepare
Good NiAgPt/ porous C exCoyOz nanocatalyst is placed in reactor, and reactor is placed in water-bath and rises to 15~60 DEG C,
Then by molar ratio be 1:(1.2~2.5) hydrazine hydrate and sodium hydroxide mixed liquor be added reactor in react, produced
Object hydrogen；The catalyst and mixed liquor mass ratio is 1:(30~70).
The NiAgPt/ porous C exCoyOz nanocatalyst includes Ni, Ag, Pt and porous C exCoyOz, wherein Ni
From nickel nitrate, Ag derives from silver nitrate, and Pt derives from chloroplatinic acid, and porous C exCoyOz is by cerous nitrate, cobalt nitrate and 2- first
Base imidazoles forms Ce-Co-MOF roasting and is made, and the molar ratio of nickel nitrate, silver nitrate and chloroplatinic acid is 1:(0.1~0.4): (0.05
~0.2)；The molar ratio of nickel nitrate and cerous nitrate, cobalt nitrate, 2-methylimidazole is 1:(1~3): (5~9): (12~21).
The NiAgPt/ porous C exCoyOz nanocatalyst is through the following steps that prepared:
(1) cerous nitrate, cobalt nitrate and 2-methylimidazole are dissolved in methanol solution and form uniform solution, at 18~30 DEG C
It is lower stirring 16~for 24 hours, centrifugation obtain Ce-Co-MOF；
(2) Ce-Co-MOF is transferred to tube furnace, roasting obtains porous C exCoyOz；
(3) the porous C exCoyOz that roasting obtains is placed in nickel nitrate, silver nitrate and platinum acid chloride solution, at 3~12 DEG C
3.5~6h is restored using ammonia Borane solution, centrifugal drying obtains NiAgPt/ porous C exCoyOz nanocatalyst.
As a kind of optimization, in the preparation step (2) of the NiAgPt/ porous C exCoyOz nanocatalyst: tubular type
Furnace maturing temperature is 460~530 DEG C, 2.5~5.4h of calcining time, calcination atmosphere O2/N2, wherein O2Volume accounting be
18%~25%.
As a kind of optimization, in the preparation step (3) of the NiAgPt/ porous C exCoyOz nanocatalyst: ammonia boron
Alkane concentration is 0.06~0.12mol/L.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention uses immersion reduction method synthetic catalyst that is easy to operate, being easy to industrial applications, catalyst carrier
Preparation is presoma using cerous nitrate cheap and easy to get, cobalt nitrate and 2-methylimidazole, and it is molten to be dissolved in methanol by certain mol proportion
Uniform solution is formed in liquid, reacts certain time under mild reaction conditions, centrifugation obtains Ce-Co-MOF, by Ce-Co-MOF
It is transferred to tube furnace, roasting obtains porous C exCoyOz under certain roasting condition and atmosphere, roasting is obtained porous
CexCoyOz is placed in the nickel nitrate, silver nitrate and platinum acid chloride solution of definite composition, in a mild condition also using ammonia Borane solution
Former a period of time, centrifugal drying obtain the NiAgPt/ porous C exCoyOz nano-catalytic with high dispersancy nano particle
Agent.
2, NiAgPt/ porous C exCoyOz nanocatalyst activity with higher to hydrazine hydrate dehydrogenation reaction, selection
Property and stability.Hydrazine hydrate dehydrogenation under temperate condition can be realized using the catalyst, and conversion rate of dehydrogenation and selectivity are
100%, the TOF value of reaction is greater than 880h-1, 3h is recycled, the TOF value of reaction is still greater than 874h-1。
Specific implementation method
The present invention is described in further details below by embodiment.But the example is not constituted to limit of the invention
System.
Embodiment 1
Prepare catalyst process
1mmol cerous nitrate, 5mmol cobalt nitrate and 12mmol 2-methylimidazole are dissolved in and is dissolved in 200mL methanol and is formed
One solution stirs for 24 hours at 18 DEG C, and centrifugation obtains Ce-Co-MOF, and Ce-Co-MOF is transferred to tube furnace, roasts at 460 DEG C
Time 5.4h, calcination atmosphere 25%O2/N2, roast and porous C exCoyOz be made, porous C exCoyOz obtained is placed in and is contained
In 1mmol nickel nitrate, 0.1mmol silver nitrate and 0.05mmol platinum acid chloride solution, using the ammonia Borane solution of 0.06mol/L 12
DEG C reduction 6h, obtain catalyst, be denoted as NiAg0.1Pt0.05/ porous C e1Co5Oz nanocatalyst, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in water-bath and controls reaction temperature
It is 60 DEG C, hydrazine hydrate and sodium hydroxide mixed liquor 1.5g that molar ratio is 1:2.5 is added dropwise thereto, collects reaction gas, reaction
The selectivity for measuring hydrogen afterwards is 100%, and the conversion ratio of hydrazine hydrate is 100%, and the TOF value of reaction is 1220h-1, it is recycled
The TOF value of 3h, reaction are still greater than 1215h-1。
Embodiment 2
Prepare catalyst process
3mmol cerous nitrate, 9mmol cobalt nitrate and 21mmol 2-methylimidazole are dissolved in and is dissolved in 200mL methanol and is formed
One solution stirs 16h at 30 DEG C, and centrifugation obtains Ce-Co-MOF, Ce-Co-MOF is transferred to tube furnace, roasts at 530 DEG C
Time 2.5h, calcination atmosphere 18%O2/N2, roast and porous C exCoyOz be made, porous C exCoyOz obtained is placed in and is contained
In 1mmol nickel nitrate, 0.4mmol silver nitrate and 0.2mmol platinum acid chloride solution, using the ammonia Borane solution of 0.12mol/L at 3 DEG C
3.5h is restored, catalyst is obtained, is denoted as NiAg0.4Pt0.2/ porous C e3Co9Oz nanocatalyst, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in water-bath and controls reaction temperature
It is 15 DEG C, hydrazine hydrate and sodium hydroxide mixed liquor 3.5g that molar ratio is 1:1.2 is added dropwise thereto, collects reaction gas, reaction
The selectivity for measuring hydrogen afterwards is 100%, and the conversion ratio of hydrazine hydrate is 100%, and the TOF value of reaction is 920h-1, it is recycled
The TOF value of 3h, reaction are still greater than 914h-1。
Embodiment 3
Prepare catalyst process
2mmol cerous nitrate, 7mmol cobalt nitrate and 16mmol 2-methylimidazole are dissolved in and is dissolved in 200mL methanol and is formed
One solution stirs 23h at 24 DEG C, and centrifugation obtains Ce-Co-MOF, Ce-Co-MOF is transferred to tube furnace, roasts at 480 DEG C
Time 3.4h, calcination atmosphere 23%O2/N2, roast and porous C exCoyOz be made, porous C exCoyOz obtained is placed in and is contained
In 1mmol nickel nitrate, 0.2mmol silver nitrate and 0.15mmol platinum acid chloride solution, using the ammonia Borane solution of 0.08mol/L 10
DEG C reduction 5h, obtain catalyst, be denoted as NiAg0.2Pt0.15/ porous C e2Co7Oz nanocatalyst, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in water-bath and controls reaction temperature
It is 25 DEG C, hydrazine hydrate and sodium hydroxide mixed liquor 2.5g that molar ratio is 1:1.4 is added dropwise thereto, collects reaction gas, reaction
The selectivity for measuring hydrogen afterwards is 100%, and the conversion ratio of hydrazine hydrate is 100%, and the TOF value of reaction is 1023h-1, it is recycled
The TOF value of 3h, reaction are still greater than 1019h-1。
Embodiment 4
Prepare catalyst process
3mmol cerous nitrate, 8mmol cobalt nitrate and 19mmol 2-methylimidazole are dissolved in and is dissolved in 200mL methanol and is formed
One solution stirs 18h at 24 DEG C, and centrifugation obtains Ce-Co-MOF, Ce-Co-MOF is transferred to tube furnace, roasts at 520 DEG C
Time 4.8h, calcination atmosphere 21%O2/N2, roast and porous C exCoyOz be made, porous C exCoyOz obtained is placed in and is contained
In 1mmol nickel nitrate, 0.3mmol silver nitrate and 0.1mmol platinum acid chloride solution, using the ammonia Borane solution of 0.09mol/L at 9 DEG C
4h is restored, catalyst is obtained, is denoted as NiAg0.3Pt0.1/ porous C e3Co8Oz nanocatalyst, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in water-bath and controls reaction temperature
It is 45 DEG C, hydrazine hydrate and sodium hydroxide mixed liquor 2g that molar ratio is 1:2.3 is added dropwise thereto, reaction gas is collected, after reaction
The selectivity for measuring hydrogen is 100%, and the conversion ratio of hydrazine hydrate is 100%, and the TOF value of reaction is 1056h-1, 3h is recycled,
The TOF value of reaction is still greater than 1052h-1。
Embodiment 5
Prepare catalyst process
2mmol cerous nitrate, 9mmol cobalt nitrate and 20mmol 2-methylimidazole are dissolved in and is dissolved in 200mL methanol and is formed
One solution stirs 22h at 18 DEG C, and centrifugation obtains Ce-Co-MOF, Ce-Co-MOF is transferred to tube furnace, roasts at 520 DEG C
Time 3.5h, calcination atmosphere 22%O2/N2, roast and porous C exCoyOz be made, porous C exCoyOz obtained is placed in and is contained
In 1mmol nickel nitrate, 0.25mmol silver nitrate and 0.15mmol platinum acid chloride solution, using the ammonia Borane solution of 0.07mol/L 7
DEG C reduction 4.5h, obtain catalyst, be denoted as NiAg0.25Pt0.15/ porous C e2Co9Oz nanocatalyst, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in water-bath and controls reaction temperature
It is 55 DEG C, hydrazine hydrate and sodium hydroxide mixed liquor 3g that molar ratio is 1:1.9 is added dropwise thereto, reaction gas is collected, after reaction
The selectivity for measuring hydrogen is 100%, and the conversion ratio of hydrazine hydrate is 100%, and the TOF value of reaction is 1217h-1, 3h is recycled,
The TOF value of reaction is still greater than 1214h-1。
Embodiment 6
Prepare catalyst process
1mmol cerous nitrate, 6mmol cobalt nitrate and 18mmol 2-methylimidazole are dissolved in and is dissolved in 200mL methanol and is formed
One solution stirs for 24 hours at 30 DEG C, and centrifugation obtains Ce-Co-MOF, and Ce-Co-MOF is transferred to tube furnace, roasts at 490 DEG C
Time 4.4h, calcination atmosphere 21%O2/N2, roast and porous C exCoyOz be made, porous C exCoyOz obtained is placed in and is contained
In 1mmol nickel nitrate, 0.3mmol silver nitrate and 0.15mmol platinum acid chloride solution, using the ammonia Borane solution of 0.11mol/L 7
DEG C reduction 4.5h, obtain catalyst, be denoted as NiAg0.3Pt0.15/ porous C e1Co6Oz nanocatalyst, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in water-bath and controls reaction temperature
It is 35 DEG C, hydrazine hydrate and sodium hydroxide mixed liquor 2.4g that molar ratio is 1:1.8 is added dropwise thereto, collects reaction gas, reaction
The selectivity for measuring hydrogen afterwards is 100%, and the conversion ratio of hydrazine hydrate is 100%, and the TOF value of reaction is 946h-1, it is recycled
The TOF value of 3h, reaction are still greater than 942h-1。
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
A specific embodiment of the invention is only limitted to this, for those of ordinary skill in the art to which the present invention belongs, is not taking off
Under the premise of from present inventive concept, several simple deductions and replacement can also be made, all shall be regarded as belonging to the present invention by institute
Claims of submission determine the protection scope of patent.
Claims (3)
1. with the method for NiAgPt/ porous C exCoyOz nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation, it is characterised in that: will prepare
NiAgPt/ porous C exCoyOz nanocatalyst be placed in reactor, reactor is placed in water-bath and rises to 15~60 DEG C, is connect
By molar ratio be 1:(1.2~2.5) hydrazine hydrate and sodium hydroxide mixed liquor be added reactor in react, obtain product
Hydrogen；
The catalyst and mixed liquor mass ratio is 1:(30~70)；
The NiAgPt/ porous C exCoyOz nanocatalyst includes Ni, Ag, Pt and porous C exCoyOz, wherein the source Ni
In nickel nitrate, Ag derives from silver nitrate, and Pt derives from chloroplatinic acid, and porous C exCoyOz is by cerous nitrate, cobalt nitrate and 2- methyl miaow
Azoles forms Ce-Co-MOF roasting and is made, and the molar ratio of nickel nitrate, silver nitrate and chloroplatinic acid is 1:(0.1~0.4): (0.05~
0.2)；The molar ratio of nickel nitrate and cerous nitrate, cobalt nitrate, 2-methylimidazole is 1:(1~3): (5~9): (12~21)；
The NiAgPt/ porous C exCoyOz nanocatalyst is through the following steps that prepared:
(1) cerous nitrate, cobalt nitrate and 2-methylimidazole are dissolved in methanol solution and form uniform solution, stirred at 18~30 DEG C
Mix 16~for 24 hours, centrifugation obtains Ce-Co-MOF；
(2) Ce-Co-MOF is transferred to tube furnace, roasting obtains porous C exCoyOz；
(3) the porous C exCoyOz that roasting obtains is placed in nickel nitrate, silver nitrate and platinum acid chloride solution, is used at 3~12 DEG C
Ammonia Borane solution restores 3.5~6h, and centrifugal drying obtains NiAgPt/ porous C exCoyOz nanocatalyst.
2. the method for using NiAgPt/ porous C exCoyOz nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation as described in claim 1,
It is characterized in that, in the preparation step (2) of the NiAgPt/ porous C exCoyOz nanocatalyst: tube furnace maturing temperature is
460~530 DEG C, 2.5~5.4h of calcining time, calcination atmosphere O2/N2, wherein O2Volume accounting be 18%~25%.
3. the method for using NiAgPt/ porous C exCoyOz nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation as described in claim 1,
It is characterized in that, in the preparation step (3) of the NiAgPt/ porous C exCoyOz nanocatalyst: ammonia borane concentration is 0.06
~0.12mol/L.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110026242A (en) * | 2019-05-10 | 2019-07-19 | 上海纳米技术及应用国家工程研究中心有限公司 | A kind of preparation method of Co/Ce bimetallic MOF base ozone catalyst and products thereof and application |
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