CN106861708A - It is a kind of to produce non-precious metal catalyst of hydrogen and preparation method thereof completely for hydrazine borine - Google Patents
It is a kind of to produce non-precious metal catalyst of hydrogen and preparation method thereof completely for hydrazine borine Download PDFInfo
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- CN106861708A CN106861708A CN201710140415.2A CN201710140415A CN106861708A CN 106861708 A CN106861708 A CN 106861708A CN 201710140415 A CN201710140415 A CN 201710140415A CN 106861708 A CN106861708 A CN 106861708A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/88—Molybdenum
- B01J23/885—Molybdenum and copper
Abstract
Non-precious metal catalyst of hydrogen and preparation method thereof is produced completely for hydrazine borine the invention provides a kind of.The catalyst is made up of base metal copper, nickel, molybdenum, is prepared by using a simple and effective stage reduction method, and with sodium borohydride as reducing agent, the mixed solution of direct-reduction copper source, nickel source and molybdenum source presoma different ratio is obtained.Non-precious metal catalyst boryl hydrolysis and diazanyl cracking of energy efficient catalytic hydrazine borine under 323K alkaline environments realizes that it produces hydrogen completely, and its transformation frequency (TOF) value has reached 108mol H2 mol metal‑1h‑1.The catalyst preparation is simple, cheap and with catalysis activity and stability very high, is a kind of very promising catalyst.
Description
Technical field
The inventive method is related to a kind of non-precious metal catalyst, more particularly to a kind of base metal for producing hydrogen completely for hydrazine borine
Catalyst and preparation method thereof, belongs to hydrogen storage material field.
Technical background
With increasingly sharpening for energy crisis and problem of environmental pollution, the clean energy resource of Development of Novel low-carbon (LC) is extremely urgent.Hydrogen Energy
Received much concern as a kind of cleaning, efficient, the safe and pollution-free energy.The utilization of Hydrogen Energy mainly includes the cheap system of hydrogen
Take, safe and efficient hydrogen storage and scale application, but the safe and efficient storage problem of hydrogen is always restriction Hydrogen Energy development and utilization
Bottleneck.High capacity solid hydrogen storage material has hydrogen storage mass fraction high and volume hydrogen-storage density, because it is in terms of hydrogen discharging performance
Significant advantage, cause the extensive interest of academia.
Hydrazine borine (N2H4BH3, HB), physicochemical properties stabilization, it is easy to prepare, its hydrogen storage content is up to 15.4wt%, exceeds well over
The requirement index (5.5wt%) of the hydrogen storage materials in 2017 that USDOE formulates, and hydrazine borine stablizes at room temperature, is easy to protect
Deposit with transport, it is a kind of solid-state hydrogen storage material with application potential to be recognized.The mode of hydrazine borine dehydrogenation mainly has pyrolysis
(J.Am.Chem.Soc.2009,131,7444) and hydrolysis (Energy Environ.Sci.2011,4,3355), pyrolysis needs
Temperature higher can just be carried out, and in the presence of suitable catalyst, the hydrolytic hydrogen production reaction of hydrazine borine is under mild conditions
Can be carried out.What is more important hydrazine borine is expected to be decomposed by the hydrolysis of boryl and diazanyl realize producing hydrogen completely, because
This in theory, 1 moles hydrazine borine is produced completely by hydrolyzing its boryl (reaction 1) and decomposing its diazanyl (reaction 2) realization
Hydrogen, can produce 5 moles of hydrogen and 1 mole of nitrogen.But, the decomposition of diazanyl is difficult, and has the generation of side reaction
(reaction 3).Therefore, catalysis hydrazine borine produces it is critical only that for hydrogen and prepares high activity, the catalyst of hydrogen selective high completely.
N2H4BH3(s)+3H2O(l)→N2H4(l)+H3BO3(l)+3H2(g) (1)
N2H4(l)→N2(g)+2H2(g) (2)
3N2H4(l)→4NH3(g)+N2(g) (3)
The single-metal reforming catalyst of report can not be catalyzed the boryl hydrolysis of hydrazine borine and diazanyl decomposes and realizes completing to produce hydrogen at present
(Int.J.Hydrogen Energy 2011,36,4958；Sci.Rep.2014,4,7597).So far, had been reported that
Produce the catalyst of hydrogen completely for being catalyzed hydrazine borine, all contain precious metals pt or Rh (ACS Catal.2014,4,4261；
J.Mater.Chem.A 2015,3,23520), so far there are no has been reported that hydrazine borine produces the non-precious metal catalyst of hydrogen completely.By
It is rare, expensive in Precious Metals Resources, it is unfavorable for practical application.Therefore, cheap, efficient non-precious metal catalyst reality is developed
The hydrogen of product completely of existing hydrazine borine has very important theory significance and practical value.
The content of the invention
Non-precious metal catalyst of hydrogen and preparation method thereof is produced completely for hydrazine borine it is an object of the invention to provide a kind of.
The catalyst for producing hydrogen completely for hydrazine borine of the present invention is made up of base metal copper, nickel, molybdenum.
The non-precious metal catalyst for producing hydrogen completely for hydrazine borine of the present invention is with sodium borohydride as reducing agent under 298K
The mixed solution of direct-reduction copper source, nickel source and molybdenum source presoma different ratio is obtained, and specifically includes following steps：
1) soluble copper source presoma and nickel source presoma, ultrasound 5 minutes are added in 5 ml of water；
2) to step 1) molybdenum source presoma is added, stir 2 minutes；
3) to step 2) reaction solution that obtains adds reducing agent sodium borohydride, and reaction 20 minutes is stirred vigorously under 298K, obtain
To required catalyst.
Step 1) described in copper source presoma be copper chloride dihydrate, nitrate trihydrate copper or cupric sulfate pentahydrate；Before described nickel source
Drive body is six water nickel chlorides, six water nickel nitrates or six water sulfuric acid acid nickel.
Step 1) described in middle copper source presoma and nickel source presoma mol ratio (nCu/nNi) it is 0.43~1.5.
Step 2) described in molybdenum source presoma be Sodium Molybdate Dihydrate, ammonium molybdate tetrahydrate or molybdenum pentachloride.
Step 2) described in molybdenum source presoma and copper source presoma and nickel source presoma mol ratio (nMo/nCu+Ni) for 0.4~
1.4。
Step 3) described in sodium borohydride consumption be 10~25mg.
Non-precious metal catalyst of the present invention is a kind of powdery amorphous material, and particle diameter is about 6nm or so, with
The features such as grain is small, active site is more.
It is an advantage of the invention that：(1) transition metal copper that is used, nickel, molybdenum are cheap and easy to get.(2) catalyst prepared by is mesh
Preceding the first can realize that hydrazine borine produces the non-precious metal catalyst of hydrogen completely.(3) catalyst performance prepared by is excellent, in 323K alkali
Efficient catalytic hydrazine borine produces hydrogen completely under property environment, and its transformation frequency (TOF) value has reached 108mol H2mol metal-1h-1,
And the catalyst recycles 10 performance tests, its H2Selectivity and catalysis activity do not have substantially reduction.Such catalysis
Agent aboundresources, with low cost, excellent performance, good stability, are a kind of very promising catalyst.
Brief description of the drawings
Fig. 1 is that the present invention implements the gained Cu of row 10.4Ni0.6Mo1.0The transmission electron microscope picture of non-precious metal catalyst；
Fig. 2 is that the present invention implements the gained Cu of row 10.4Ni0.6Mo1.0The selected diffraction figure of non-precious metal catalyst；
Fig. 3 is that the present invention implements the gained Cu of row 10.4Ni0.6Mo1.0The EDS energy spectrum diagrams of non-precious metal catalyst；
Fig. 4 is the Cu that the present invention implements row 1 and 6-8 gained difference Cu and Ni mol ratiosxNi1-xMo1.0Non-precious metal catalyst
Hydrazine borane hydrolysis are catalyzed under 323K puts hydrogen test performance test chart；
Fig. 5 is the Cu that the present invention implements row 1 and 11-15 gained difference Mo contents0.4Ni0.6MoyNon-precious metal catalyst exists
Hydrazine borane hydrolysis are catalyzed under 323K puts hydrogen test performance test chart；
Fig. 6 is that the present invention implements the gained Cu of row 10.4Ni0.6Mo1.0 non-precious metal catalyst is catalyzed hydrazine borane hydrolysis under 323K
Recycle performance test chart.
Specific embodiment
Embodiment 1：
1) 0.04mmol copper chloride dihydrates and the water nickel chlorides of 0.06mmol six, ultrasound 5 minutes are added in 5 ml of water；
2) to step 1) 0.10mmol Sodium Molybdate Dihydrates are added, stir 2 minutes；
3) to step 2) mixed solution that obtains adds 25mg sodium borohydrides, stirring reaction 20 minutes, and obtaining metal component is
Cu0.4Ni0.6Mo1.0Non-precious metal catalyst.
Embodiment 2：
By step 1 in embodiment 1) copper chloride dihydrate is changed to nitrate trihydrate copper, other the step of with embodiment 1, obtain metal group
It is divided into Cu0.4Ni0.6Mo1.0Non-precious metal catalyst.
Embodiment 3：
By step 1 in embodiment 1) copper chloride dihydrate is changed to cupric sulfate pentahydrate, other the step of with embodiment 1, obtain metal group
It is divided into Cu0.4Ni0.6Mo1.0Non-precious metal catalyst.
Embodiment 4：
By step 1 in embodiment 1) six water nickel chlorides are changed to six water nickel nitrates, other the step of with embodiment 1, obtain metal group
It is divided into Cu0.4Ni0.6Mo1.0Non-precious metal catalyst.
Embodiment 5：
By step 1 in embodiment 1) six water nickel chlorides are changed to nickel sulfate hexahydrate, other the step of with embodiment 1, obtain metal group
It is divided into Cu0.4Ni0.6Mo1.0Non-precious metal catalyst.
Embodiment 6：
By step 1 in embodiment 1) add 0.04mmol copper chloride dihydrates and the water nickel chlorides of 0.06mmol six to be changed to 0.03mol bis-
Water copper chloride and the water nickel chlorides of 0.07mol six, other the step of with embodiment 1, obtain metal component for Cu0.3Ni0.7Mo1.0It is non-
Noble metal catalyst.
Embodiment 7：
By step 1 in embodiment 1) add 0.04mmol copper chloride dihydrates and the water nickel chlorides of 0.06mmol six to be changed to 0.05mol bis-
Water copper chloride and the water nickel chlorides of 0.05mol six, other the step of with embodiment 1, obtain metal component for Cu0.5Ni0.5Mo1.0It is non-
Noble metal catalyst.
Embodiment 8：
By step 1 in embodiment 1) add 0.04mmol copper chloride dihydrates and the water nickel chlorides of 0.06mmol six to be changed to 0.06mol bis-
Water copper chloride and the water nickel chlorides of 0.04mol six, other the step of with embodiment 1, obtain metal component for Cu0.6Ni0.4Mo1.0It is non-
Noble metal catalyst.
Embodiment 9：
By step 2 in embodiment 1) Sodium Molybdate Dihydrate is changed to ammonium molybdate tetrahydrate, other the step of with embodiment 1, obtain metal group
It is divided into Cu0.4Ni0.6Mo1.0Non-precious metal catalyst.
Embodiment 10：
By step 2 in embodiment 1) Sodium Molybdate Dihydrate is changed to molybdenum pentachloride, other the step of with embodiment 1, obtain metal component
It is Cu0.4Ni0.6Mo1.0Non-precious metal catalyst.
Embodiment 11：
By step 2 in embodiment 1) Sodium Molybdate Dihydrate consumption is changed to 0.04mmol, other the step of with embodiment 1, obtain metal
Component is Cu0.4Ni0.6Mo0.4Non-precious metal catalyst.
Embodiment 12：
By step 2 in embodiment 1) Sodium Molybdate Dihydrate consumption is changed to 0.06mmol, other the step of with embodiment 1, obtain metal
Component is Cu0.4Ni0.6Mo0.6Non-precious metal catalyst.
Embodiment 13：
By step 2 in embodiment 1) Sodium Molybdate Dihydrate consumption is changed to 0.08mmol, other the step of with embodiment 1, obtain metal
Component is Cu0.4Ni0.6Mo0.8Non-precious metal catalyst.
Embodiment 14：
By step 2 in embodiment 1) Sodium Molybdate Dihydrate consumption is changed to 0.12mmol, other the step of with embodiment 1, obtain metal
Component is Cu0.4Ni0.6Mo1.2Non-precious metal catalyst.
Embodiment 15：
By step 2 in embodiment 1) Sodium Molybdate Dihydrate consumption is changed to 0.14mmol, other the step of with embodiment 1, obtain metal
Component is Cu0.4Ni0.6Mo1.4Non-precious metal catalyst.
Embodiment 16：
By step 3 in embodiment 1) sodium borohydride consumption is changed to 10, other the step of with embodiment 1, obtaining metal component is
Cu0.4Ni0.6Mo1.0Non-precious metal catalyst.
Embodiment 17：
By step 3 in embodiment 1) sodium borohydride consumption is changed to 15mg, other the step of with embodiment 1, obtaining metal component is
Cu0.4Ni0.6Mo1.0Non-precious metal catalyst.
Embodiment 18：
By step 3 in embodiment 1) sodium borohydride consumption is changed to 20mg, other the step of with embodiment 1, obtaining metal component is
Cu0.4Ni0.6Mo1.0Non-precious metal catalyst.
Embodiment 19-22：
Using the Cu of the gained of embodiment 1,6,7,8xNi1-xMo1.0Non-precious metal catalyst catalysis hydrazine borine (N2H4BH3, HB) and hydrolysis
Hydrogen manufacturing (19,20,21,22), catalyst is placed in the two mouthfuls of flasks of 50ml containing 5ml ultra-pure waters, is subsequently adding 2.0M NaOH,
It is eventually adding hydrazine borine.Reacted under 323K (produce hydrogen figure as shown in Figure 4), following result (table one) is obtained after terminating：
Table one
Embodiment 23-28：
Using the Cu of the gained of embodiment 1,11,12,13,14,150.6Ni0.4MoyNon-precious metal catalyst is catalyzed hydrazine borine
(N2H4BH3, HB) and hydrolytic hydrogen production (corresponding to embodiment 23,24,25,26,27,28 respectively), catalyst is placed in ultra-pure water containing 5ml
Two mouthfuls of flasks of 50ml in, be subsequently adding 2.0M NaOH, be eventually adding hydrazine borine.Reacted under 323K and (produced hydrogen figure as schemed
Shown in 5), following result (table two) is obtained after terminating：
Table two
Embodiment 29：
Using the Cu of the gained of embodiment 10.4Ni0.6Mo1.0Non-precious metal catalyst is circulated performance test, hydrazine borine water
After solution is complete, the hydrazine borine test Cu of equivalent is added toward two mouthfuls of flasks0.4Ni0.6Mo1.0Non-precious metal catalyst is catalyzed hydrazine boron
The recycling performance of alkane hydrolytic hydrogen production, refers to Fig. 6.Multiple loop test shows synthesized Cu0.4Ni0.6Mo1.0Base metal
Catalyst has good recycling.
Claims (7)
1. a kind of non-precious metal catalyst for producing hydrogen completely for hydrazine borine, it is characterised in that described catalyst is by non-noble
Metallic copper, nickel, molybdenum composition, its structural formula is CuNiMo.
2. a kind of preparation method of the non-precious metal catalyst for producing hydrogen completely for hydrazine borine according to claim 1, its
It is characterised by, there is provided prepared by an a kind of simple and effective stage reduction method, specifically include following steps：
1) soluble copper source presoma and nickel source presoma, ultrasound 5 minutes are added in 5 ml of water；
2) to step 1) molybdenum source presoma is added, stir 2 minutes；
3) to step 2) reaction solution that obtains adds reducing agent sodium borohydride, and reaction 20 minutes is stirred vigorously under 298K, obtain
To required non-precious metal catalyst.
3. the preparation method that hydrazine borine produces the non-precious metal catalyst of hydrogen completely is used for according to claim 2, and its feature exists
In step 1) described in copper source presoma be copper chloride dihydrate, nitrate trihydrate copper or cupric sulfate pentahydrate；Described nickel source forerunner
Body is six water nickel chlorides, six water nickel nitrates or six water sulfuric acid acid nickel.
4. the preparation method that hydrazine borine produces the non-precious metal catalyst of hydrogen completely is used for according to claim 2, and its feature exists
In step 1) described in middle copper source presoma and nickel source presoma mol ratio (nCu/nNi) it is 0.43~1.5.
5. the preparation method that hydrazine borine produces the non-precious metal catalyst of hydrogen completely is used for according to claim 2, and its feature exists
In step 2) described in molybdenum source presoma be Sodium Molybdate Dihydrate, ammonium molybdate tetrahydrate or molybdenum pentachloride.
6. the preparation method that hydrazine borine produces the non-precious metal catalyst of hydrogen completely is used for according to claim 2, and its feature exists
In step 2) described in molybdenum source presoma and copper source presoma and nickel source presoma mol ratio (nMo/nCu+Ni) for 0.4~
1.4。
7. the preparation method that hydrazine borine produces the non-precious metal catalyst of hydrogen completely is used for according to claim 2, and its feature exists
In step 3) described in sodium borohydride consumption be 10~25mg.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108745403A (en) * | 2018-06-12 | 2018-11-06 | 吉林大学 | A kind of preparation method and application of boron nitride load Ni-MoOx nanocatalysts |
| CN110180552A (en) * | 2019-06-28 | 2019-08-30 | 武汉工程大学 | Copper/cuprous oxide/molybdenum dioxide electrocatalysis material and preparation method thereof, application |
| CN117443461A (en) * | 2023-12-22 | 2024-01-26 | 苏州大学 | Catalyst of boron-containing solid hydrogen storage material, preparation method and catalyst precursor |
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| CN103949272A (en) * | 2014-05-21 | 2014-07-30 | 江西师范大学 | NiPt@RGO composite nano catalyst for producing hydrogen by using hydrazine borane and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108745403A (en) * | 2018-06-12 | 2018-11-06 | 吉林大学 | A kind of preparation method and application of boron nitride load Ni-MoOx nanocatalysts |
| CN108745403B (en) * | 2018-06-12 | 2021-07-09 | 吉林大学 | Preparation method and application of boron nitride loaded Ni-MoOx nano catalyst |
| CN110180552A (en) * | 2019-06-28 | 2019-08-30 | 武汉工程大学 | Copper/cuprous oxide/molybdenum dioxide electrocatalysis material and preparation method thereof, application |
| CN110180552B (en) * | 2019-06-28 | 2022-05-10 | 武汉工程大学 | Copper/cuprous oxide/molybdenum dioxide electrocatalytic material and preparation method and application thereof |
| CN117443461A (en) * | 2023-12-22 | 2024-01-26 | 苏州大学 | Catalyst of boron-containing solid hydrogen storage material, preparation method and catalyst precursor |
| CN117443461B (en) * | 2023-12-22 | 2024-04-05 | 苏州大学 | Catalyst of boron-containing solid hydrogen storage material, preparation method and catalyst precursor |
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