CN105964288A - Method for preparing mesoporous carbon nitride loaded nano nickel phosphide - Google Patents
Method for preparing mesoporous carbon nitride loaded nano nickel phosphide Download PDFInfo
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- CN105964288A CN105964288A CN201610406785.1A CN201610406785A CN105964288A CN 105964288 A CN105964288 A CN 105964288A CN 201610406785 A CN201610406785 A CN 201610406785A CN 105964288 A CN105964288 A CN 105964288A
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- nickel
- phosphide
- nickel phosphide
- carbonitride
- mesoporous carbonitride
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title abstract 3
- 238000002360 preparation method Methods 0.000 claims abstract description 9
- FBMUYWXYWIZLNE-UHFFFAOYSA-N nickel phosphide Chemical compound [Ni]=P#[Ni] FBMUYWXYWIZLNE-UHFFFAOYSA-N 0.000 claims abstract description 5
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 27
- 239000003054 catalyst Substances 0.000 claims description 25
- 238000003756 stirring Methods 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 14
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 11
- ACVYVLVWPXVTIT-UHFFFAOYSA-M phosphinate Chemical compound [O-][PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-M 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 7
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- 229910052698 phosphorus Inorganic materials 0.000 claims description 2
- 239000011574 phosphorus Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 abstract description 10
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 7
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 abstract 1
- 230000000536 complexating effect Effects 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 229910001453 nickel ion Inorganic materials 0.000 abstract 1
- 238000004729 solvothermal method Methods 0.000 abstract 1
- 238000005119 centrifugation Methods 0.000 description 9
- 238000001816 cooling Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 238000001291 vacuum drying Methods 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 description 7
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 229910052723 transition metal Inorganic materials 0.000 description 6
- 150000003624 transition metals Chemical class 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000010189 synthetic method Methods 0.000 description 2
- JIHQDMXYYFUGFV-UHFFFAOYSA-N 1,3,5-triazine Chemical compound C1=NC=NC=N1 JIHQDMXYYFUGFV-UHFFFAOYSA-N 0.000 description 1
- BFCFYVKQTRLZHA-UHFFFAOYSA-N 1-chloro-2-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1Cl BFCFYVKQTRLZHA-UHFFFAOYSA-N 0.000 description 1
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
- B01J35/615—100-500 m2/g
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for preparing mesoporous carbon nitride loaded nano nickel phosphide. According to the method, graphite-like mesoporous carbon nitride high in specific surface area serves as a carrier, and loaded nickel phosphide is prepared through a low-temperature normal-pressure solvothermal method, wherein the specific surface area is 435 m<2>/g; a special N-rich body structure of carbon nitride is used for complexing and dispersing nickel ions, and accordingly high-dispersity nano nickel phosphide is prepared. The carbon nitride loaded nano nickel phosphide is used for catalytic nitrobenzene hydrogenation, and catalytic activity and stability are high. The nano nickel phosphide is mild in preparation conditions, simple in process, low in cost and capable of easily achieving industrial production.
Description
Technical field
The present invention relates to new transition metal catalysts and preparing technical field thereof, particularly to a kind of support type
The preparation method of nano nickel phosphide hydrogenation catalyst.
Background technology
Transition metal phosphide is that a big class is entered the compound that metal lattice is formed, this kind of chemical combination by phosphorus atoms
Thing Heat stability is good, hardness are big, antioxidation and corrosion resistance strong, and show the highest Adsorption
Density.Research finds, transition metal phosphide has the hydroprocessing activity of excellence, and hydrogen-consuming volume is few, necessarily
Alternative precious metals pt in degree, arouses great concern in new catalytic material field.At present
In the transition metal phosphide studied, nickel phosphide shows more superior hydrogenation activity, is expected to become new
Generation oil refining hydrotreating catalyst.
Many scholars start to be devoted to the research of transition metal phosphide, find that the size of its particle diameter directly restricts
The height of catalysis activity, the phosphide of high dispersive is the active center of reaction.And traditional temperature programmed reduction
Method is easily reunited due to temperature required higher (600-800 DEG C), the phosphide particle of preparation, its specific surface area
Typically smaller than 10m2/g.Although and solvent-thermal method mild condition conventional recently, prepared phosphide particle is relatively
Little, have bigger specific surface area.But, solvent-thermal method is usually static treatment in crystallizing kettle, instead
A large amount of gas can be produced during Ying kettle is damaged.It addition, people also attempt being come by variety carrier
Dispersion phosphide, such as SiO2, molecular sieve, high surface area carbon etc..But due to phosphide and carrier function power relatively
Weak make dispersion effect not ideal enough.Therefore, it is necessary to find more cheap, easy method and suitably
Carrier prepares high dispersive, high activity phosphide catalyst.
Summary of the invention
The technical problem to be solved in the present invention is complicated, harsh for current transition metal phosphide preparation condition,
Cost is high, and particle agglomeration is serious, the problems such as support dispersion effect is not ideal enough, it is provided that a kind of synthetic method letter
List, mild condition, with low cost and can the support type nickel phosphide nanoparticle hydrogenation catalyst of high degree of dispersion
Method.
The technical solution adopted for the present invention to solve the technical problems is:
The present invention selects the mesoporous carbonitride of class graphite mould of high-ratio surface to be carrier, by low-temperature atmosphere-pressure solvent thermal
Method prepares loaded nano nickel phosphide, and the specific surface area of described mesoporous carbonitride is 435m2/g.Specifically according to
Following steps are carried out:
(1) weigh a certain amount of nickel source and mesoporous carbonitride joins in solvent, wherein nickel and the matter of carbonitride
Amount ratio is 1:20-1:6, is sufficiently stirred for；It is subsequently adding a certain amount of sodium dihydric hypophosphite, wherein the rubbing of phosphorus and nickel
That ratio is 2:1-5:1, stirs；
(2) by said mixture reflow treatment 5h in 150-200 DEG C of oil bath, naturally cool to after room temperature from
The heart separates, wash, be vacuum dried and i.e. obtain described catalyst.
As limitation of the invention, nickel source of the present invention is Nickel dichloride., nickel acetate or nickel sulfate；Described
Solvent be ethylene glycol, propylene glycol or glycerol.
In the present invention, use low-temperature atmosphere-pressure solvent structure nano nickel phosphide, on the one hand avoid traditional
Higher temperature needed for temperature programmed reduction method and the rigors to heating schedule；On the other hand normal pressure
Method can be avoided producing a large amount of gas in enclosed system and reaction vessel is caused damage.
The present invention selects the mesoporous carbonitride of class graphite mould of high-ratio surface to be carrier, utilizes in carbonitride main unit
Abundant N lone pair electrons, make presoma Ni element be dispersed in the " empty of 3 three s-triazine compositions by coordinate bond
Chamber " in, thus prepare the nickel phosphide of high degree of dispersion.
This synthetic method is simple to operate, mild condition and with low cost, it is easy to industrialized production.
Catalyst of the present invention shows good catalysis activity with multiple in the hydrogenation reaction of Nitrobenzol
The property used.
Detailed description of the invention
In conjunction with following example, the present invention is further illustrated below, however, it should be noted that these are real
Execute example only to illustrate and be used, and be not necessarily to be construed as the restriction that the present invention implements.
Embodiment 1
Weigh 0.2377g Nickel dichloride hexahydrate and the mesoporous carbonitride of 0.3522g join in 40ml ethylene glycol,
It is sufficiently stirred for 1h, is subsequently adding 0.2640g sodium dihydric hypophosphite and continues to stir 0.5h；By mixture at 170 DEG C
Reflow treatment 5h in oil bath, centrifugation after naturally cooling to room temperature, sample deionized water fully wash,
60 DEG C of vacuum drying, obtain described catalyst A.
Embodiment 2
Weigh 0.2377g Nickel dichloride hexahydrate and the mesoporous carbonitride of 0.7044g join in 40ml ethylene glycol,
It is sufficiently stirred for 1h, is subsequently adding 0.2640g sodium dihydric hypophosphite and continues to stir 0.5h；By mixture at 170 DEG C
Reflow treatment 5h in oil bath, centrifugation after naturally cooling to room temperature, sample deionized water fully wash,
60 DEG C of vacuum drying, obtain described catalyst B.
Embodiment 3
Weigh 0.2377g Nickel dichloride hexahydrate and the mesoporous carbonitride of 1.174g joins in 40ml ethylene glycol, fill
Divide stirring 1h, be subsequently adding 0.176g sodium dihydric hypophosphite and continue to stir 0.5h；By mixture at 170 DEG C
Reflow treatment 5h in oil bath, centrifugation after naturally cooling to room temperature, sample deionized water fully wash,
60 DEG C of vacuum drying, obtain described catalyst C.
Embodiment 4
Weigh 0.2377g Nickel dichloride hexahydrate and the mesoporous carbonitride of 0.7044g join in 40ml propylene glycol,
It is sufficiently stirred for 1h, is subsequently adding 0.264g sodium dihydric hypophosphite and continues to stir 0.5h；By mixture at 170 DEG C
Reflow treatment 5h in oil bath, centrifugation after naturally cooling to room temperature, sample deionized water fully wash,
60 DEG C of vacuum drying, obtain described catalyst D.
Embodiment 5
Weigh 0.2377g Nickel dichloride hexahydrate and the mesoporous carbonitride of 0.7044g joins in 40ml glycerol, fill
Divide stirring 1h, be subsequently adding 0.264g sodium dihydric hypophosphite and continue to stir 0.5h；By mixture at 170 DEG C
Reflow treatment 5h in oil bath, centrifugation after naturally cooling to room temperature, sample deionized water fully wash,
60 DEG C of vacuum drying, obtain described catalyst E.
Embodiment 6
Weigh 0.2377g Nickel dichloride hexahydrate and the mesoporous carbonitride of 0.7044g join in 40ml ethylene glycol,
It is sufficiently stirred for 1h, is subsequently adding 0.44g sodium dihydric hypophosphite and continues to stir 0.5h；By mixture at 200 DEG C
Reflow treatment 5h in oil bath, centrifugation after naturally cooling to room temperature, sample deionized water fully wash,
60 DEG C of vacuum drying, obtain described catalyst F.
Embodiment 7
Weigh 0.2377g Nickel dichloride hexahydrate and the mesoporous carbonitride of 0.7044g join in 40ml ethylene glycol,
It is sufficiently stirred for 1h, is subsequently adding 0.264g sodium dihydric hypophosphite and continues to stir 0.5h；By mixture at 150 DEG C
Reflow treatment 5h in oil bath, centrifugation after naturally cooling to room temperature, sample deionized water fully wash,
60 DEG C of vacuum drying, obtain described catalyst G.
Embodiment 8
Weigh 0.1768g nickel acetate and the mesoporous carbonitride of 0.7044g joins in 40ml ethylene glycol, fully stir
Mix 1h, be subsequently adding 0.264g sodium dihydric hypophosphite and continue to stir 0.5h；By mixture 170 DEG C of oil baths
Middle reflow treatment 5h, centrifugation after naturally cooling to room temperature, sample deionized water fully wash, 60 DEG C
Vacuum drying, obtains described catalyst H.
Embodiment 9
Weigh 0.2628g nickel sulfate and the mesoporous carbonitride of 0.7044g joins in 40ml ethylene glycol, fully stir
Mix 1h, be subsequently adding 0.264g sodium dihydric hypophosphite and continue to stir 0.5h；By mixture 170 DEG C of oil baths
Middle reflow treatment 5h, centrifugation after naturally cooling to room temperature, sample deionized water fully wash, 60 DEG C
Vacuum drying, obtains described catalyst I.
During catalyst in above-described embodiment is applied to hydrogenation of chloronitrobenzene, reaction condition is as follows:
Solvent: ethanol；Catalyst: 10mg；Nitrobenzol: 0.5mL；Hydrogen Vapor Pressure: 1.0MPa；Instead
Answer temperature: 100 DEG C；Response time: 1h, its catalytic performance is as shown in table 1:
The catalytic performance of table 1 catalyst
| Catalyst | Nitrobenzene conversion rate (%) | Aniline selectivity (%) |
| A | 92.3 | 99.7 |
| B | 98.7 | 100 |
| C | 90.1 | 99.7 |
| D | 93.6 | 99.8 |
| E | 86.5 | 98.9 |
| F | 85.1 | 98.6 |
| G | 92.6 | 99.8 |
| H | 98.5 | 100 |
| I | 95.9 | 100 |
As it can be seen from table 1 catalyst of the present invention to be used for the hydrogenation of Nitrobenzol, at 100 DEG C,
Reacting 1h under 1.0MPa hydrogen pressure, Nitrobenzol maximum conversion is up to 98.7%, and aniline selectivity is up to 100%.
The catalyst B obtaining above-described embodiment 2 carries out multiplexing performance investigation, and this catalyst is centrifugal to be reclaimed also
With three dried multiplexings of washing with alcohol, performance is as shown in table 2:
The multiplexing performance of table 2 catalyst B
| Multiplexing number | Nitrobenzene conversion rate (%) | Aniline selectivity (%) |
| 1 | 98.7 | 100 |
| 2 | 98.2 | 100 |
| 3 | 98.3 | 100 |
| 4 | 98.0 | 100 |
| 5 | 98.2 | 100 |
| 6 | 97.9 | 100 |
Table 2 shows that catalyst is active almost without decline after using 6 times, and multiplexing performance is good.
With the above-mentioned desirable embodiment according to the present invention for enlightenment, by above-mentioned description, related work
Personnel can carry out various change and amendment completely in the range of without departing from this invention technological thought.
The content that the technical scope of this invention is not limited in description, it is necessary to according to right
Determine its technical scope.
Claims (4)
1. the preparation method of a mesoporous carbonitride load nano nickel phosphide, it is characterised in that select high-ratio surface
The mesoporous carbonitride of long-pending rich N agent structure is carrier, prepares loaded nano by low-temperature atmosphere-pressure solvent-thermal method
Nickel phosphide, the specific surface area of described mesoporous carbonitride is 435m2/g。
The preparation method of a kind of mesoporous carbonitride the most according to claim 1 load nano nickel phosphide, its
It is characterised by that the method is carried out as steps described below:
(1) weigh a certain amount of nickel source and mesoporous carbonitride joins in solvent, wherein nickel and the matter of carbonitride
Amount ratio is 1:20-1:6, is sufficiently stirred for；It is subsequently adding a certain amount of sodium dihydric hypophosphite, wherein the rubbing of phosphorus and nickel
That ratio is 2:1-5:1, stirs；
(2) by said mixture reflow treatment 5h in 150-200 DEG C of oil bath, naturally cool to after room temperature from
The heart separates, wash, be vacuum dried and i.e. obtain described catalyst.
The preparation method of a kind of mesoporous carbonitride the most according to claim 2 load nano nickel phosphide, its
It is characterised by that the nickel source described in step (1) is Nickel dichloride., nickel acetate or nickel sulfate.
The preparation method of a kind of mesoporous carbonitride the most according to claim 2 load nano nickel phosphide, its
It is characterised by that the solvent described in step (1) is ethylene glycol, propylene glycol or glycerol.
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Cited By (12)
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| CN107312199A (en) * | 2017-06-09 | 2017-11-03 | 福州大学 | A kind of hypo-aluminum orthophosphate Hybrid fire retardant and preparation method thereof |
| CN107694584A (en) * | 2017-10-15 | 2018-02-16 | 华东师范大学 | A kind of self-supporting catalyst of phosphatizing nickel and its preparation method and application |
| CN109107597A (en) * | 2018-08-31 | 2019-01-01 | 华南农业大学 | A kind of transition metal phosphide/g-C3N4Composite material and preparation method and application |
| CN109160500A (en) * | 2018-09-28 | 2019-01-08 | 常州大学 | A method of control synthesis different phase nano nickel phosphide |
| CN110813352A (en) * | 2019-10-31 | 2020-02-21 | 润泰化学（泰兴）有限公司 | Ni2Preparation method of P/NC catalyst, Ni2P/NC catalyst and application thereof |
| CN112090434A (en) * | 2020-09-16 | 2020-12-18 | 常州大学 | Preparation method of supported nickel phosphide for catalyzing selective hydrogenation of furfural to prepare furfuryl alcohol |
| CN112201782A (en) * | 2020-10-16 | 2021-01-08 | 西南大学 | Nickel phosphide/carbon/nickel phosphide composite material and preparation method and application thereof |
| CN112588310A (en) * | 2020-12-02 | 2021-04-02 | 江苏大学 | Preparation method of visible light response nickel-phosphorized carbon nitride photocatalyst |
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| CN114768855A (en) * | 2022-05-10 | 2022-07-22 | 安徽工业技术创新研究院 | Heterojunction composite photocatalyst with atomic-level channel, preparation method and application |
| CN115475648A (en) * | 2022-10-09 | 2022-12-16 | 陕西师范大学 | Internal and external surface simultaneously loaded with Ni 2 Preparation method of mesoporous P-doped carbon nitride hollow sphere catalyst of P |
| WO2024036756A1 (en) * | 2022-08-19 | 2024-02-22 | 台州学院 | Multifunctional phosphorus and nickel doped graphite-like carbon nitride nanosheet, preparation method therefor, and abs material |
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