CN106744677A - Use RhNiCo/CeO2@C3N4The method of nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation - Google Patents
Use RhNiCo/CeO2@C3N4The method of nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses one kind RhNiCo/CeO2@C3N4The method of nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation, belongs to technical field of chemistry and chemical engineering.The RhNiCo/CeO that the present invention will be prepared2@C3N4Nanocatalyst is placed in reactor, reactor is placed in uniform temperature is risen in oil bath, is reacted during hydrazine hydrate and NaOH mixed liquor then are added into reactor, and the hydrogen of generation is collected using drainage.The RhNiCo/CeO2@C3N4Nanocatalyst has activity and selectivity higher.Hydrazine hydrate dehydrogenation reaction is carried out using the catalyst, conversion rate of dehydrogenation and selectivity are 100%, and the TOF values of reaction are more than 650h‑1。
Description
Technical field
The invention belongs to technical field of chemistry and chemical engineering, and in particular to one kind RhNiCo/CeO2@C3N4Nanocatalyst is urged
The method for changing hydrazine hydrate dehydrogenation.
Background technology
The energy is one of critical elements necessary to human survival, is the important substance guarantee of social development.With society
The high speed development of meeting, people increasingly increase the demand of the energy, and fossil fuel constantly reduces energy crisis and its burning for bringing
Product is caused energy system at present based on fossil fuel is constantly proposed sternly with the environmental pollution that " haze " is representative
High challenge.The new renewable and clean energy resource of exploitation substitutes the inexorable trend that traditional fossil fuel is Future Social Development,
It is the main strategic selection of the mankind.
Hydrogen Energy is considered as the new energy for advancing 21 century energy revolution, and it is only water that it uses rear product as the energy, right
Environment, without any harm, is current country support and the clean energy resource direction developed energetically, but because hydrogen density is small, danger
Property it is high, the efficient storage for how realizing hydrogen be restrict present hydrogen large-scale use key.
Compared to other hydrogen storage materials, hydrazine hydrate has security higher and possesses hydrogen content higher in the application
(8.0wt%), CN105126884A is reported on containing nano metal phosphide MxPyThe ammonia borine or hydrazine hydrate of catalyst are urged
Change hydrolysis and release hydrogen system and its application, but catalyst activity in hydrazine hydrate dehydrogenation systems is not still high, it is necessary to further improve
The catalysis activity of catalyst.
The content of the invention
The purpose of the present invention is directed to the deficiencies in the prior art, there is provided one kind RhNiCo/CeO2@C3N4Nanocatalyst
The method of Compounds with Hydrazine Hydrate Catalyzed dehydrogenation, to the RhNiCo/CeO2@C3N4Nanocatalyst has good catalysis activity and selection
Property, the complete dehydrogenation of hydrazine hydrate is realized under the conditions of relatively mild.
The technical solution adopted for the present invention to solve the technical problems is as follows.
The RhNiCo/CeO that will be prepared2@C3N4Nanocatalyst is placed in reactor, reactor is placed in oil bath and is risen
It is then 1 by mol ratio to 20~60 DEG C:0.5~4 hydrazine hydrate and NaOH mixed liquor is carried out instead in adding reactor
Should, hydrogen product is obtained, wherein, the amount of the material of hydrazine hydrate is 0.01mol/g with the mass ratio of catalyst.
Described RhNiCo/CeO2@C3N4Nanocatalyst is through the following steps that prepared：
(1) by melamine and cerous nitrate according to mass ratio 1:0.03~0.1 dissolving is made into mixed solution, by above-mentioned mixing
Solution is stirred to drying at 80~120 DEG C, is transferred to tube furnace and is obtained CeO in 500~700 DEG C of 6~8h of roasting2@C3N4Carry
Body.
(2) it is 1 by mol ratio：0.5~3：0.1~0.5 Rh salt, Ni salt, Co salt and deionized water are configured in container,
Mixed solution is formed after being sufficiently stirred for, then CeO prepared by step (1)2@C3N4It is added in above-mentioned mixed solution, wherein, mixing
The amount and CeO of the material of salt2@C3N4The mass ratio of carrier is 0.2mmol/g.
(3) mixed solution of step (2) is placed in 0 DEG C of water-bath, with the sodium borohydride of 0.1mol/L~0.3mol/L
Reduction is dropwise added dropwise, and stirs 4~12h.
(4) dried after the solution filtering for obtaining step (3), that is, obtain RhNiCo/CeO2@C3N4Nanocatalyst.
Further, described RhNiCo/CeO2@C3N4Rh salt in the preparation process (2) of nanocatalyst is chlorination
Rhodium, Ni salt is nickel chloride, and Co salt is cobalt chloride.
Further, described RhNiCo/CeO2@C3N4Drying in the preparation process (4) of nanocatalyst is in an oven
Carry out, drying temperature is 80~120 DEG C, drying time is 12~24h.
Compared with prior art, the beneficial effects of the invention are as follows：
1st, the present invention uses immersion reduction method, and catalyst preparation is using cerous nitrate and melamine mixed liquor is fired obtains
CeO2@C3N4, the carrier of above-mentioned preparation is placed in the RhCl of certain content3·3H2O、NiCl2·6H2O and CoCl2·6H2O solution
In, dried through sodium borohydride solution reduction and prepare RhNiCo/CeO2@C3N4Nanocatalyst, the catalyst has activity higher
And selectivity.Hydrazine hydrate dehydrogenation reaction is carried out using the catalyst, conversion rate of dehydrogenation and selectivity are 100%, the TOF of reaction
Value is more than 650h-1。
2 from unlike traditional loaded catalyst：According to the present invention, metal Rh, Ni, Co in regulation catalyst
Mole when support C eO2@C3N4Composition high activity, high selectivity for hydrazine hydrate dehydrogenation hydrogen can be just obtained
RhNiCo/CeO2@C3N4Nanocatalyst.
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
By 2g melamines and 0.06g Ce (NO3)3·6H2O is dissolved in 200mL deionized waters, by above-mentioned mixed liquor 80
Drying is stirred well in DEG C water-bath, 8h after 500 DEG C of roastings is transferred in tube furnace, CeO is obtained after roasting2@C3N4, it is designated as
0.03CeO2@C3N4.By 6.6mg RhCl3·3H2O、3.0mg NiCl2·6H2O and 0.6mg CoCl2·6H2O is dissolved in 20mL steamings
Distilled water, then by 0.2g 0.03CeO2@C3N4Add in above-mentioned solution, after being sufficiently stirred for, a period of time stirred in 0 DEG C of ice bath,
0.1mol/L sodium borohydride solutions are added dropwise to reduce and stir 12h, 24h is dried in the drying box of 80 DEG C of filtering, catalyst is designated as
RhNi0.5Co0.1/0.03CeO2@C3N4, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in controlling reaction temperature in oil bath
It it is 20 DEG C, it is 1 that mol ratio is added dropwise thereto:0.5 hydrazine hydrate and NaOH mixed liquor 4ml, collects reacting gas, after reaction
It is 100% to measure the selectivity of hydrogen, and hydrazine hydrate conversion ratio is 100%, and the TOF values of reaction are 680h-1。
Embodiment 2
Prepare catalyst process
By 2g melamines and 0.2g Ce (NO3)3·6H2O is dissolved in 200mL deionized waters, by above-mentioned mixed liquor 120
Drying is stirred well in DEG C water-bath, 6h after 700 DEG C of roastings is transferred in tube furnace, CeO is obtained after roasting2@C3N4, it is designated as
0.1CeO2@C3N4.By 2.3mg RhCl3·3H2O、6.3mg NiCl2·6H2O and 1.1mg CoCl2·6H2O is dissolved in 20mL steamings
Distilled water, then by 0.2g 0.1CeO2@C3N4Add in above-mentioned solution, after being sufficiently stirred for, stirred in 0 DEG C of ice bath a period of time, drop
Plus 0.3mol/L sodium borohydride solutions are reduced and stir 4h, 12h is dried in the drying box of 120 DEG C of filtering, catalyst is designated as
RhNi3Co0.5/0.1CeO2@C3N4, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in controlling reaction temperature in oil bath
It it is 60 DEG C, it is 1 that mol ratio is added dropwise thereto:4 hydrazine hydrate and NaOH mixed liquor 4ml, collects reacting gas, is surveyed after reaction
The selectivity for obtaining hydrogen is 100%, and hydrazine hydrate conversion ratio is 100%, and the TOF values of reaction are 1280h-1。
Embodiment 3
Prepare catalyst process
By 2g melamines and 0.1g Ce (NO3)3·6H2O is dissolved in 200mL deionized waters, by above-mentioned mixed liquor 90
Drying is stirred well in DEG C water-bath, 7h after 600 DEG C of roastings is transferred in tube furnace, CeO is obtained after roasting2@C3N4, it is designated as
0.05CeO2@C3N4.By 4.8mg RhCl3·3H2O、4.3mg NiCl2·6H2O and 0.9mg CoCl2·6H2O is dissolved in 20mL steamings
Distilled water, then by 0.2g 0.05CeO2@C3N4Add in above-mentioned solution, after being sufficiently stirred for, a period of time stirred in 0 DEG C of ice bath,
0.2mol/L sodium borohydride solutions are added dropwise to reduce and stir 6h, 16h is dried in the drying box of 110 DEG C of filtering, catalyst is designated as
RhNiCo0.2/0.05CeO2@C3N4, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in controlling reaction temperature in oil bath
It it is 50 DEG C, it is 1 that mol ratio is added dropwise thereto:3 hydrazine hydrate and NaOH mixed liquor 4ml, collects reacting gas, is surveyed after reaction
The selectivity for obtaining hydrogen is 100%, and hydrazine hydrate conversion ratio is 100%, and the TOF values of reaction are 820h-1。
Embodiment 4
Prepare catalyst process
By 2g melamines and 0.16g Ce (NO3)3·6H2O is dissolved in 200mL deionized waters, and above-mentioned mixed liquor is existed
Drying is stirred well in 100 DEG C of water-baths, 6h after 550 DEG C of roastings is transferred in tube furnace, CeO is obtained after roasting2@C3N4, note
It is 0.08CeO2@C3N4.By 3.6mg RhCl3·3H2O、4.9mg NiCl2·6H2O and 1.3mg CoCl2·6H2O is dissolved in 20mL
Distilled water, then by 0.2g 0.08CeO2@C3N4In adding above-mentioned solution, after being sufficiently stirred for, when stirring one section in 0 DEG C of ice bath
Between, 0.15mol/L sodium borohydride solutions are added dropwise and reduce and stirs 9h, 18h, catalyst note are dried in the drying box of 100 DEG C of filtering
It is RhNi1.5Co0.4/0.08CeO2@C3N4, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in controlling reaction temperature in oil bath
It it is 40 DEG C, it is 1 that mol ratio is added dropwise thereto:2 hydrazine hydrate and NaOH mixed liquor 4ml, collects reacting gas, is surveyed after reaction
The selectivity for obtaining hydrogen is 100%, and hydrazine hydrate conversion ratio is 100%, and the TOF values of reaction are 760h-1。
Embodiment 5
Prepare catalyst process
By 2g melamines and 0.12g Ce (NO3)3·6H2O is dissolved in 200mL deionized waters, and above-mentioned mixed liquor is existed
Drying is stirred well in 115 DEG C of water-baths, 8h after 650 DEG C of roastings is transferred in tube furnace, CeO is obtained after roasting2@C3N4, note
It is 0.06CeO2@C3N4.By 4.6mg RhCl3·3H2O、4.1mg NiCl2·6H2O and 1.2mg CoCl2·6H2O is dissolved in 20mL
Distilled water, then by 0.2g 0.06CeO2@C3N4In adding above-mentioned solution, after being sufficiently stirred for, when stirring one section in 0 DEG C of ice bath
Between, 0.25mol/L sodium borohydride solutions are added dropwise and reduce and stirs 11h, 20h, catalyst note are dried in the drying box of 105 DEG C of filtering
It is RhNiCo0.3/0.06CeO2@C3N4, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in controlling reaction temperature in oil bath
It it is 30 DEG C, it is 1 that mol ratio is added dropwise thereto:1 hydrazine hydrate and NaOH mixed liquor 4ml, collects reacting gas, is surveyed after reaction
The selectivity for obtaining hydrogen is 100%, and hydrazine hydrate conversion ratio is 100%, and the TOF values of reaction are 710h-1。
Embodiment 6
Prepare catalyst process
By 2g melamines and 0.14g Ce (NO3)3·6H2O is dissolved in 200mL deionized waters, and above-mentioned mixed liquor is existed
Drying is stirred well in 105 DEG C of water-baths, 8h after 550 DEG C of roastings is transferred in tube furnace, CeO is obtained after roasting2@C3N4, note
It is 0.07CeO2@C3N4.By 4.8mg RhCl3·3H2O、3.5mg NiCl2·6H2O and 1.7mg CoCl2·6H2O is dissolved in 20mL
Distilled water, then by 0.2g 0.07CeO2@C3N4In adding above-mentioned solution, after being sufficiently stirred for, when stirring one section in 0 DEG C of ice bath
Between, 0.2mol/L sodium borohydride solutions are added dropwise and reduce and stirs 9h, 14h is dried in the drying box of 105 DEG C of filtering, catalyst is designated as
RhNi0.8Co0.4/0.07CeO2@C3N4, closed preservation.
Dehydrogenation reaction process
The above-mentioned catalyst of 50mg is filled in tubular reactor, then tubular reactor is placed in controlling reaction temperature in oil bath
It it is 60 DEG C, it is 1 that mol ratio is added dropwise thereto:4 hydrazine hydrate and NaOH mixed liquor 4ml, collects reacting gas, is surveyed after reaction
The selectivity for obtaining hydrogen is 100%, and hydrazine hydrate conversion ratio is 100%, and the TOF values of reaction are 1210h-1。
Claims (3)
1. RhNiCo/CeO is used2@C3N4The method of nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation, it is characterised in that：By RhNiCo/
CeO2@C3N4Nanocatalyst is placed in reactor, reactor is placed in oil bath and rises to 20~60 DEG C, is then by mol ratio
1:0.5~4 hydrazine hydrate and NaOH mixed liquor is reacted in adding reactor, obtains hydrogen product, wherein：Hydrazine hydrate
The mass ratio of amount and catalyst of material be 0.01mol/g；
Described RhNiCo/CeO2@C3N4Nanocatalyst is through the following steps that prepared：
(1) by melamine and cerous nitrate according to mass ratio 1:0.03~0.1 dissolving is made into mixed solution, by above-mentioned mixed solution
Stirred to drying at 80~120 DEG C, be transferred to tube furnace and obtain CeO in 500~700 DEG C of 6~8h of roasting2@C3N4Carrier；
(2) it is 1 by mol ratio：0.5~3：0.1~0.5 Rh salt, Ni salt, Co salt and deionized water are configured in container, fully
Mixed solution is formed after stirring, then CeO prepared by step (1)2@C3N4Carrier is added in above-mentioned mixed solution, wherein：Mixing
The amount and CeO of the material of salt2@C3N4The mass ratio of carrier is 0.2mmol/g；
(3) mixed solution that step (2) is obtained is placed in 0 DEG C of water-bath, is dropwise dripped with the sodium borohydride of 0.1~0.3mol/L
Plus reduction, and stir 4~12h；
(4) dried after the solution filtering for obtaining step (3), that is, obtain RhNiCo/CeO2@C3N4Nanocatalyst.
2. RhNiCo/CeO is used as claimed in claim 12@C3N4The method of nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation, its feature
It is, described RhNiCo/CeO2@C3N4Rh salt in the preparation process (2) of nanocatalyst is radium chloride, and Ni salt is chlorination
Nickel, Co salt is cobalt chloride.
3. RhNiCo/CeO is used as claimed in claim 12@C3N4The method of nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation, its feature
It is, described RhNiCo/CeO2@C3N4Drying in the preparation process (4) of nanocatalyst is carried out in an oven, dries temperature
It is 80~120 DEG C to spend, and drying time is 12~24h.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109433226A (en) * | 2018-12-13 | 2019-03-08 | 安徽工业大学 | With the method for NiAgPt/ porous C exCoyOz nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation |
| CN109499584A (en) * | 2018-12-13 | 2019-03-22 | 安徽工业大学 | With the method for NiPd/ porous C exCoyOz nanocatalyst catalysis formaldehyde dehydrogenation |
| CN109569654A (en) * | 2018-12-17 | 2019-04-05 | 安徽工业大学 | With the method for NiPdPt/ porous C exCoyOz nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation |
| CN109647435A (en) * | 2018-12-17 | 2019-04-19 | 安徽工业大学 | With the method for CuPd/ porous C exCoyOz nanocatalyst catalysis formaldehyde dehydrogenation |
| CN114669319A (en) * | 2022-04-19 | 2022-06-28 | 南京航空航天大学 | Nano cobaltosic oxide-carbon nitrogen composite catalyst and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109433226A (en) * | 2018-12-13 | 2019-03-08 | 安徽工业大学 | With the method for NiAgPt/ porous C exCoyOz nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation |
| CN109499584A (en) * | 2018-12-13 | 2019-03-22 | 安徽工业大学 | With the method for NiPd/ porous C exCoyOz nanocatalyst catalysis formaldehyde dehydrogenation |
| CN109569654A (en) * | 2018-12-17 | 2019-04-05 | 安徽工业大学 | With the method for NiPdPt/ porous C exCoyOz nanocatalyst Compounds with Hydrazine Hydrate Catalyzed dehydrogenation |
| CN109647435A (en) * | 2018-12-17 | 2019-04-19 | 安徽工业大学 | With the method for CuPd/ porous C exCoyOz nanocatalyst catalysis formaldehyde dehydrogenation |
| CN114669319A (en) * | 2022-04-19 | 2022-06-28 | 南京航空航天大学 | Nano cobaltosic oxide-carbon nitrogen composite catalyst and preparation method and application thereof |
| CN114669319B (en) * | 2022-04-19 | 2023-06-23 | 南京航空航天大学 | Nanometer cobaltosic oxide-carbon nitrogen composite catalyst and preparation method and application thereof |
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