CN110124746A - A kind of preparation of nickel phosphide/TpPa-2 composite material and photolysis water hydrogen - Google Patents
A kind of preparation of nickel phosphide/TpPa-2 composite material and photolysis water hydrogen Download PDFInfo
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- CN110124746A CN110124746A CN201910571474.4A CN201910571474A CN110124746A CN 110124746 A CN110124746 A CN 110124746A CN 201910571474 A CN201910571474 A CN 201910571474A CN 110124746 A CN110124746 A CN 110124746A
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- 239000002131 composite material Substances 0.000 title claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- FBMUYWXYWIZLNE-UHFFFAOYSA-N nickel phosphide Chemical compound [Ni]=P#[Ni] FBMUYWXYWIZLNE-UHFFFAOYSA-N 0.000 title claims abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 title abstract description 26
- 239000001257 hydrogen Substances 0.000 title abstract description 26
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title abstract description 24
- 238000006303 photolysis reaction Methods 0.000 title abstract description 12
- 230000015843 photosynthesis, light reaction Effects 0.000 title abstract description 11
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 7
- 229910021205 NaH2PO2 Inorganic materials 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 4
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000003786 synthesis reaction Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 6
- 229910000510 noble metal Inorganic materials 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000000354 decomposition reaction Methods 0.000 abstract description 3
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 3
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GDSOZVZXVXTJMI-SNAWJCMRSA-N (e)-1-methylbut-1-ene-1,2,4-tricarboxylic acid Chemical compound OC(=O)C(/C)=C(C(O)=O)\CCC(O)=O GDSOZVZXVXTJMI-SNAWJCMRSA-N 0.000 description 1
- BWAPJIHJXDYDPW-UHFFFAOYSA-N 2,5-dimethyl-p-phenylenediamine Chemical compound CC1=CC(N)=C(C)C=C1N BWAPJIHJXDYDPW-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013310 covalent-organic framework Substances 0.000 description 1
- 239000002178 crystalline material Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000008055 phosphate buffer solution Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/28—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of the platinum group metals, iron group metals or copper
-
- 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
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- 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
- C01B3/042—Decomposition of water
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2203/00—Integrated processes for the production of hydrogen or synthesis gas
- C01B2203/02—Processes for making hydrogen or synthesis gas
- C01B2203/0266—Processes for making hydrogen or synthesis gas containing a decomposition step
- C01B2203/0277—Processes for making hydrogen or synthesis gas containing a decomposition step containing a catalytic decomposition step
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Catalysts (AREA)
Abstract
A kind of preparation of nickel phosphide/TpPa-2 composite material and photocatalytic hydrogen production by water decomposition, are related to a kind of Ni2The preparation of P/TpPa-2 composite material and photocatalytic hydrogen production by water decomposition.The present invention provides a kind of Ni2P/TpPa-2 composite material, in order to solve the problems, such as to be currently used for photocatalysis hydrogen production material hydrogen production efficiency under the conditions of no noble metal not high.Method: the one, preparation of TpPa-2；Two, Ni2The preparation of P/TpPa-2 composite material.Preparation process of the invention is simple and effective, and reagent consumption is less and yield is high；And photochemical catalyst provided by the invention can effectively improve the problem of TpPa-2 photolysis water hydrogen low efficiency.The present invention is applied to photolysis water hydrogen field, and experiment shows that the composite material has excellent photolysis water hydrogen performance, and photocatalytic water hydrogen generation efficiency can reach 2.52 mmolg‑1·h‑1。
Description
Technical field
The present invention relates to a kind of preparation of nickel phosphide/TpPa-2 composite material and photolysis water hydrogens.
Background technique
For a long time, fossil energy sharply consumption so that the energy and environmental problem it is increasingly serious, force the mankind positive
Seek solution.Hydrogen Energy is 21 century most potential secondary clean energy, since it is close with high specific energy
The advantages that degree, calorific value are big, and combustion product only has water, will not cause any pressure to environment.Fujishima et al. is reported for the first time
Under ultraviolet light (UV), since n-type semiconductor titanium dioxide electrodes are applied to optical electro-chemistry decomposition water, recognize people
To the feasibility using solar photolysis water hydrogen.People can use solar energy, carry out the chemical conversion of luminous energy, to answer
For solving the problems, such as the utilization of new energy resources in human lives.
Existing photochemical catalyzing is mostly used noble metal platinum (Pt) as co-catalyst and solves light induced electron and hole-recombination
The high problem of rate.But in view of noble metal is scarce resource, and it is expensive, it is unfavorable for that photochemical catalyst is mass produced.Phosphatization
Nickel (Ni2P), as important a member of transition metal phosphide, it is not only good anticorrosive, wear-resistant, waterproof material,
And such as hydrodesulfurization/denitrogenation has extremely excellent potential using value in terms of catalysis.Nickel phosphide is as a kind of novel
Semiconductor nano material, also have very important potentiality application in terms of photocatalysis.
Covalent organic machine frame (COFs) material is to be formed by light atom (hydrogen, boron, carbon, nitrogen etc.) by covalently key connection
Highly porous organic polymer crystalline material with two dimensional topology, because it is with good visible absorption, regular duct
The advantages that structure and suitable forbidden bandwidth, become a kind of very potential conductor photocatalysis material, but light induced electron with
The easily compound disadvantage in hole keeps photocatalysis effect not satisfactory.Therefore developing a kind of material that photolysis water hydrogen is high-efficient becomes
Research hotspot.
Summary of the invention
The invention aims to solve, current material photolysis water hydrogen is inefficient under the conditions of no noble metal to be asked
Topic, and a kind of Ni is provided2The preparation method of P/TpPa-2 composite material.
A kind of Ni of the invention2The preparation method of P/TpPa-2 composite material is completed by the following steps:
One, the preparation of TpPa-2；
Two, Ni2The preparation of P/TpPa-2: by the TpPa-2 and NiCl of above-mentioned synthesis2·6H2O、NaH2PO2·H2O is placed in mortar
Uniformly, it is subsequently transferred to Ci Zhouzhong, be warming up to 200 DEG C with tube furnace under nitrogen atmosphere and keeps 1h, is centrifuged with water and ethyl alcohol
It washs for several times, in 80 DEG C of oven drying 10h up to Ni2P/TpPa-2 composite material；
NiCl described in step 22·6H2O and NaH2PO2·H2The mass ratio of O is 1:5；
The heating rate of tube furnace described in step 2 is 5 DEG C/min；
Above-mentioned Ni2Application of the P/TpPa-2 composite material in terms of photolysis water hydrogen.
Beneficial effects of the present invention:
The present invention uses solvent-thermal method, and with 2,5- dimethyl-p-phenylenediamine and 1,3,5- tri- aldehyde radical phloroglucins are raw material, success
A kind of two-dimentional organic material (TpPa-2) has been synthesized, but photocatalytic water hydrogen generation efficiency is lower under visible light for the material, only
0.08mmol·g-1·h-1.Therefore the invention has synthesized a kind of new composite material Ni again on the basis of TpPa-22P/TpPa-2,
The material effectively raises the photolysis water hydrogen performance of TpPa-2, Ni2The photocatalytic water hydrogen generation efficiency of P/TpPa-2 composite material
For 1.51~2.52mmolg-1·h-1。
Detailed description of the invention
Fig. 1 is Ni2The X-ray powder diffraction figure of P/TpPa-2 material；
Fig. 2 is Ni2Scanning electron microscope (SEM) figure of P/TpPa-2 material；
Fig. 3 is Ni2The photodissociation aquatic products hydrogen figure of P/TpPa-2 material.
Specific embodiment
With embodiment, invention is further explained below, these embodiments only say method of the invention
It is bright, it is without any restrictions to the scope of application of the invention.
Specific embodiment 1: a kind of Ni of present embodiment2The preparation of P/TpPa-2 material is to complete according to the following steps
:
Step 1: the preparation of TpPa-2；
Step 2: Ni2The preparation of P/TpPa-2: by TpPa-2 (60mg) and NiCl2·6H2O(1.98mg)、NaH2PO2·H2O
(9.9mg) is placed in mortar uniformly, is subsequently transferred to Ci Zhouzhong, is warming up to 200 DEG C of (heating speed with tube furnace under nitrogen atmosphere
Rate is 5 DEG C/min) and keep 1h, for several times with water and ethyl alcohol centrifuge washing, in 80 DEG C of oven drying 10h up to Ni2P/TpPa-2
(mass ratio 1:100) composite material；
Specific embodiment 2: the present embodiment is different from the first embodiment in that: described in step 2
NiCl2·6H2The quality of O is 6mg, NaH2PO2·H2The quality of O is 30mg, other steps and parameter and specific embodiment one
It is identical.Obtain Ni2P/TpPa-2 (mass ratio 3:100) composite material；
Specific embodiment 3: the present embodiment is different from the first and the second embodiment in that: described in step 3
NiCl2·6H2The quality of O is 10mg, NaH2PO2·H2The quality of O is 50mg, other steps and parameter and specific embodiment one
Or two is identical.Obtain Ni2P/TpPa-2 (mass ratio 5:100) composite material；
Following tests is carried out for verifying beneficial effects of the present invention:
To investigate Ni2Aquatic products hydrogen effect is catalytically decomposed in P/TpPa-2 material, carries out visible light photocatalysis production to it by the following method
Hydrogen performance test.Test process is as follows: Photocatalyzed Hydrogen Production experiment is carried out in photocatalytic activity evaluation on-line analysis system, and reaction is opened
Before beginning, cooling recirculation system is opened, to ensure that light-catalyzed reaction temperature is maintained at steady temperature (4 DEG C), and is excluded with vacuum pump
Air in system.The Xe lamp (>=420nm) of 300W is used as light source, with Ni2P/TpPa-2 (10mg) is used as photochemical catalyst, and L- is anti-bad
Hematic acid sodium (100mg) is sacrifice agent, and phosphate buffer solution (50mL) is reaction solution, in the item that supersonic frequency is 35~45KHz
30min is ultrasonically treated under part to be allowed to form uniform suspension.As shown, TpPa-2 photocatalytic water hydrogen generation efficiency under visible light
It is lower, only 0.08mmolh-1·g-1；And novel Ni2P/TpPa-2 composite material presents good photocatalysis hydrolysis system
The performance of hydrogen, photocatalytic water hydrogen generation efficiency are 1.51~2.52mmolh-1·g-1。
Claims (4)
1. a kind of preparation of nickel phosphide/TpPa-2 composite material, it is characterised in that this method sequentially includes the following steps:
One, the preparation of TpPa-2；
Two, Ni2The preparation of P/TpPa-2: by the TpPa-2 and NiCl of above-mentioned synthesis2·6H2O、NaH2PO2·H2O is placed in mortar
Uniformly, be subsequently transferred to Ci Zhouzhong, be warming up to 200 DEG C with tube furnace under nitrogen atmosphere and keep 1 h, with water and ethyl alcohol from
The heart washs for several times, in 80 DEG C of 10 h of oven drying up to Ni2P/TpPa-2 composite material；
NiCl described in step 22·6H2O and NaH2PO2·H2The mass ratio of O is 1:5；
The heating rate of tube furnace described in step 2 is 5 DEG C/min.
2. a kind of Ni according to claim 12The preparation of P/TpPa-2 composite material, it is characterised in that described in step 2
Ni2The quality of P is 1. 98 ~ 10 mg.
3. a kind of Ni according to claim 12The preparation of P/TpPa-2 composite material, it is characterised in that described in step 2
NiCl2·6H2O and NaH2PO2·H2The mass ratio of O is 1:5.
4. a kind of Ni according to claim 12The preparation of P/TpPa-2 composite material, it is characterised in that described in step 2
The heating rate of tube furnace is 5 DEG C/min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910571474.4A CN110124746A (en) | 2019-06-26 | 2019-06-26 | A kind of preparation of nickel phosphide/TpPa-2 composite material and photolysis water hydrogen |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910571474.4A CN110124746A (en) | 2019-06-26 | 2019-06-26 | A kind of preparation of nickel phosphide/TpPa-2 composite material and photolysis water hydrogen |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114425375A (en) * | 2022-01-24 | 2022-05-03 | 辽宁大学 | Ni12P5TpPa-1-COF photocatalyst, preparation method thereof and application thereof in photocatalytic water decomposition |
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|---|---|---|---|---|
| CN104525168A (en) * | 2014-12-18 | 2015-04-22 | 黑龙江大学 | Method for synthesizing anatase/brookite nano composite material for photocatalytic decomposition of water into hydrogen through one-step hydrothermal method |
| CN107349961A (en) * | 2017-06-27 | 2017-11-17 | 哈尔滨理工大学 | A kind of NH2The preparation of the composites of 66@TpPa of UIO 1 and photolysis water hydrogen |
| CN108837841A (en) * | 2018-06-29 | 2018-11-20 | 哈尔滨理工大学 | A kind of CD@NH2-UiO-66/g-C3N4The preparation of composite material and photolysis water hydrogen |
-
2019
- 2019-06-26 CN CN201910571474.4A patent/CN110124746A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104525168A (en) * | 2014-12-18 | 2015-04-22 | 黑龙江大学 | Method for synthesizing anatase/brookite nano composite material for photocatalytic decomposition of water into hydrogen through one-step hydrothermal method |
| CN107349961A (en) * | 2017-06-27 | 2017-11-17 | 哈尔滨理工大学 | A kind of NH2The preparation of the composites of 66@TpPa of UIO 1 and photolysis water hydrogen |
| CN108837841A (en) * | 2018-06-29 | 2018-11-20 | 哈尔滨理工大学 | A kind of CD@NH2-UiO-66/g-C3N4The preparation of composite material and photolysis water hydrogen |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114425375A (en) * | 2022-01-24 | 2022-05-03 | 辽宁大学 | Ni12P5TpPa-1-COF photocatalyst, preparation method thereof and application thereof in photocatalytic water decomposition |
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