CN108786924A - A kind of Ni (OH)2The preparation method of/TpPa-2 materials - Google Patents
A kind of Ni (OH)2The preparation method of/TpPa-2 materials Download PDFInfo
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- CN108786924A CN108786924A CN201810739598.4A CN201810739598A CN108786924A CN 108786924 A CN108786924 A CN 108786924A CN 201810739598 A CN201810739598 A CN 201810739598A CN 108786924 A CN108786924 A CN 108786924A
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- 239000000463 material Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 238000005119 centrifugation Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 1
- 239000001257 hydrogen Substances 0.000 abstract description 28
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 28
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 27
- 230000001699 photocatalysis Effects 0.000 abstract description 16
- 238000006303 photolysis reaction Methods 0.000 abstract description 10
- 230000015843 photosynthesis, light reaction Effects 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract description 4
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 3
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract description 2
- 230000004044 response Effects 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 abstract 1
- 229910021508 nickel(II) hydroxide Inorganic materials 0.000 description 13
- 238000000034 method Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- BWAPJIHJXDYDPW-UHFFFAOYSA-N 2,5-dimethyl-p-phenylenediamine Chemical class CC1=CC(N)=C(C)C=C1N BWAPJIHJXDYDPW-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000003776 cleavage reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002431 hydrogen Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 230000007017 scission Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-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
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000007717 exclusion Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 150000002732 mesitylenes Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 description 1
- 229960001553 phloroglucinol Drugs 0.000 description 1
- 230000000258 photobiological effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000027756 respiratory electron transport chain Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- 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
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
-
- 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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- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Combustion & Propulsion (AREA)
- Catalysts (AREA)
Abstract
A kind of Ni (OH)2The preparation method of/TpPa-2 materials is related to a kind of Ni (OH)2The preparation method of/TpPa-2 materials.The present invention provides a kind of novel Ni (OH)2/ TpPa-2 materials, in order to solve the problems, such as that existing TpPa-2 photolysis water hydrogens material hydrogen production efficiency is not high.The preparation process of the present 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 low problem of TpPa-2 photolysis water hydrogen efficiency.The present invention is applied to photocatalysis hydrolytic hydrogen production field, and experiment shows Ni (OH)2/ TpPa-2 materials have good response performance to visible light, there is strong and wide absorption band in visible region, and it is 640nm or so to absorb band edge.At the same time, Ni (OH)2There is/TpPa-2 materials excellent photolysis water hydrogen performance, photocatalytic water hydrogen-producing speed can reach 1896 μm of ol g‑1•h‑1。
Description
Technical field
The present invention relates to a kind of Ni (OH)2The preparation method of/TpPa-2 materials is applied to photocatalysis hydrolytic hydrogen production field.
Background technology
The two big challenges that Global Sustainable Development faces are exactly energy and environmental problem, increasingly exhausted fossil energy and day
The serious environmental pollution that becomes drastically influences the survival and development of the mankind, finds and develop the renewable green of alternative fossil energy
The color energy becomes the hot spot of domestic and international using energy source and material science research.At present oneself exploitation new energy mainly include wind energy,
Geothermal energy, ocean energy, solar energy etc..Wherein, solar energy is due to having many advantages, such as that inexhaustible, nexhaustible is considered as most having
One of new energy of future.The utilization ratio for improving solar energy has own strategic significance to changing energy consumption structure.It utilizes
Solar energy realizes that photolysis water hydrogen will be the important channel for pushing hydrogen economy development, solving environment and energy crisis.It realizes too
There are many method that sun can crack aquatic products hydrogen, include to utilize solar energy electrolyzing water, photo-biological water-splitting, photocatalytic cleavage water system
Hydrogen.In these methods, the photocatalytic cleavage water of conductor photocatalysis system also originates in hydrogen（It can using Driven by Solar Energy thermodynamics
Back reaction generates hydrogen molecule）, become focus.
Phase earlier 1970s, Japanese Scientists Fujishima and Honda have found in laboratory in TiO2Monocrystalline
On electrode can photochemical catalyzing be made hydrogen, to disclose utilize the direct hydrogen production by water decomposition of solar energy possibility.But from
For sun light efficiency, however it remains many problems：On the one hand the photoresponse narrow scope of this kind of semi-conducting material is only rung
Answer 4% ultraviolet light, sun light utilization efficiency relatively low；On the other hand the combined efficiency of their photo-generate electron-hole pair is very high, amount
Son is less efficient, develops in photolysis water hydrogen field to limit it.For this purpose, researcher is successively from the new caltalyst of exploitation
All various aspects such as system, the absorptivity for changing sacrifice agent type, improving sunlight, the Schottky barrier for reducing electron transfer are to photodissociation
Water hydrogen producing technology is improved, and achieves significant effect.But many researchs also indicate that：Develop new caltalyst
It is, improves that the performance of original catalyst is still effectively improve photocatalytic conversion efficiency at present, reduce the main of catalyst cost
One of approach.
Invention content
The invention aims to solve the problems, such as that existing TpPa-2 materials photolysis water hydrogen is inefficient, and provide a kind of
Ni(OH)2The preparation method of/TpPa-2 materials.A kind of Ni (OH)2The preparation of/TpPa-2 materials, is completed according to the following steps：
Appropriate TpPa-2 is dispersed in NaOH solution, 20 ~ 30min of ultrasound under conditions of supersonic frequency is 35 ~ 45KHz adds dropwise
Enter the Ni (NO of different volumes3)2Solution reacts a period of time under conditions of magnetic agitation, is centrifuged in 8000r/min after reaction
5min is precipitated, and is washed with water 3 ~ 5 times to neutrality, and last 80 DEG C of vacuum drying obtain Ni (OH)2/ TpPa-2 materials；
Above-mentioned Ni (OH)2/ TpPa-2 materials in terms of the photolysis water hydrogen in application.
Beneficial effects of the present invention：
The present invention uses solvent-thermal method, with 1,3,5- tri- aldehyde radical phloroglucin, 2,5- dimethyl-p-phenylenediamines for raw material, successfully closes
At a kind of covalent organic frame material（TpPa-2）, but photocatalytic water hydrogen generation efficiency is relatively low under visible light for the material, only
72 µmol·h-1·g-1.The present invention has synthesized a kind of new material Ni (OH) again on the basis of TpPa-2 materials2/ TpPa-2,
The material effectively increases TpPa-2 photolysis water hydrogen performances, Ni (OH)2The photocatalytic water hydrogen generation efficiency of/TpPa-2 materials be 202 ~
1896 µmol·h-1·g-1。
Description of the drawings
Fig. 1 is what embodiment 3 obtained（2.5mol%）Ni(OH)2The UV-vis DRS figure of/TpPa-2 materials；
Fig. 2 is Ni (OH)2/ TpPa-2 materials and TpPa-2 photocatalytic water hydrogen-producing speed figures.
Specific implementation mode
Using embodiment below, invention is further explained, these embodiments only say the method for the present invention
It is bright, it is without any restrictions to the scope of application of the present invention.
Embodiment 1：A kind of Ni (OH) of present embodiment2The preparation of/TpPa-2 materials is completed according to the following steps：
Step 1: the preparation of TpPa-2：By tri- aldehyde radical phloroglucins of 1,3,5-（0.063g）With 2,5- dimethyl-p-phenylenediamines
（0.048g）It is added in heat-resistant glass tube, then adds 1,3,5- trimethylbenzenes（1.5mL）, 1,4- dioxane（1.5mL）With
Acetic acid（0.5mL,3mol/L）Mixed solution, supersonic frequency be 40KHz under conditions of be ultrasonically treated 30min, in liquid nitrogen bath
Frozen-thawed cycled deaerates three times for middle progress, heats 72h after sealing in 120 DEG C, filters and washed three times with tetrahydrofuran, in 180
In DEG C vacuum drying chamber it is dry for 24 hours；
Step 2: Ni (OH)2The preparation of/TpPa-2：0.05g TpPa-2 are dispersed in 30mL 0.25mol/L NaOH solutions
In, 42 μ L 0.05mol/L Ni (NO are added dropwise in 20 ~ 30min of ultrasound under conditions of supersonic frequency is 35 ~ 45KHz3)2It is molten
Liquid handles 6h under conditions of magnetic agitation, is precipitated in 8000r/min centrifugations 5min after reaction, and be washed with water 3 ~ 5 times
To neutrality, 80 DEG C of vacuum drying obtain（0.5mol%）Ni(OH)2/ TpPa-2 materials；
Embodiment 2：Present embodiment is as different from Example 1：Ni (NO are added dropwise described in step 23)2Volume be
83 μ L, other steps and parameter are same as Example 1.It obtains（1mol%）Ni(OH)2/ TpPa-2 materials.
Embodiment 3：Present embodiment is unlike embodiment 1 or 2：Ni (NO are added dropwise described in step 23)2's
Volume is 208 μ L, other steps and parameter are identical as embodiment 1 or 2.It obtains（2.5mol%）Ni(OH)2/ TpPa-2 materials.
Embodiment 4：Present embodiment is unlike embodiment 1 to 3：Ni (NO are added dropwise described in step 23)2's
Volume is 333 μ L, other steps and parameter are identical as embodiment 1 to 3.It obtains（4mol%）Ni(OH)2/ TpPa-2 materials.
Embodiment 5：Present embodiment is unlike embodiment 1 to 4：Ni (NO are added dropwise described in step 23)2
Volume be 416 μ L, other steps and parameter are identical as embodiment 1 to 4.It obtains（5mol%）Ni(OH)2/ TpPa-2 materials.
Following tests is carried out for verification beneficial effects of the present invention：
Fig. 1 illustrates what embodiment 3 obtained（2.5mol%）Ni(OH)2The UV-vis DRS figure of/TpPa-2 materials.From figure
In it is observed that there is strong and wide absorption band in visible region.It is 640nm or so to absorb band edge, it was demonstrated that（2.5mol%）Ni
(OH)2/ TpPa-2 materials have good response performance to visible light.
To investigate Ni (OH)2Aquatic products hydrogen effect is catalytically decomposed in/TpPa-2 materials, by the following method to its visible light photocatalysis
H2-producing capacity is tested.Test process is as follows：Photocatalyzed Hydrogen Production experiment is carried out in photocatalytic activity evaluation on-line analysis system,
Before reaction starts, condenser system is opened, air in vacuum pump exclusion system is passed through.The xenon lamp of 300W is as light source（≥420nm）.
Using 0.1g L-AAs sodium as sacrifice agent, 50mL water is as reaction solution, 0.01g Ni (OH)2/ TpPa-2 is as photocatalytic water system
Hydrogen catalyst, as shown in Figure 2：1 is TpPa-2 materials；2 be what embodiment 2 obtained（0.5mol%）Ni(OH)2/ TpPa-2 materials；
3 be what embodiment 3 obtained（1mol%）Ni(OH)2What/TpPa-2 materials, 4 obtained for embodiment 4（2.5mol%）Ni(OH)2/
TpPa-2 materials；5 be what embodiment 5 obtained（4mol%）Ni(OH)2/ TpPa-2 materials；6 be what embodiment 6 obtained（5mol%）
Ni(OH)2/ TpPa-2 materials.TpPa-2 photocatalytic waters hydrogen generation efficiency is relatively low under visible light, only 72 μm of olh-1·g-1；And it is new
Type Ni (OH)2/ TpPa-2 materials present the performance of a good photocatalysis hydrolytic hydrogen production, and photocatalytic water hydrogen generation efficiency is
202~1896 µmol·h-1·g-1, effectively raise the photolysis water hydrogen performance of TpPa-2 materials.
Claims (6)
1. a kind of Ni (OH)2The preparation method of/TpPa-2 materials, is completed according to the following steps：Appropriate TpPa-2 is dispersed in
In NaOH solution, the Ni (NO of different volumes are added dropwise in 20 ~ 30min of ultrasound under conditions of supersonic frequency is 35 ~ 45KHz3)2
Solution reacts a period of time under conditions of magnetic agitation, is precipitated in 8000r/min centrifugations 5min after reaction, water is used in combination
3 ~ 5 times extremely neutrality, last 80 DEG C of vacuum drying of washing obtain Ni (OH)2/ TpPa-2 materials.
2. a kind of Ni (OH) according to claim 12The preparation method of/TpPa-2 materials, it is characterised in that the TpPa-2
Dosage be 0.04 ~ 0.06g.
3. a kind of Ni (OH) according to claim 12The preparation method of/TpPa-2 materials, it is characterised in that described to use
A concentration of 0.2 ~ 0.25mol/L of NaOH.
4. a kind of Ni (OH) according to claim 12The preparation method of/TpPa-2 materials, it is characterised in that the TpPa-2
Quality is 0.05g with NaOH volume ratios：20~30mL.
5. a kind of Ni (OH) according to claim 12The preparation method of/TpPa-2 materials, it is characterised in that the Ni
(NO3)2A concentration of 0.04 ~ 0.05mol/L.
6. a kind of Ni (OH) according to claim 12The preparation method of/TpPa-2 materials, it is characterised in that the TpPa-2
Quality and Ni (NO3)2Volume ratio is 0.05g：40~450µL.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810739598.4A CN108786924B (en) | 2018-07-06 | 2018-07-06 | A kind of Ni (OH)2Preparation method of/TpPa-2 material and hydrogen production by photolysis of water |
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| CN201810739598.4A CN108786924B (en) | 2018-07-06 | 2018-07-06 | A kind of Ni (OH)2Preparation method of/TpPa-2 material and hydrogen production by photolysis of water |
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| Publication Number | Publication Date |
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| CN108786924A true CN108786924A (en) | 2018-11-13 |
| CN108786924B CN108786924B (en) | 2021-02-02 |
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| CN110227548A (en) * | 2019-06-26 | 2019-09-13 | 哈尔滨理工大学 | A kind of preparation of the titanium dioxide TpPa-1 composite material being covalently keyed and photolysis water hydrogen |
| CN110624610A (en) * | 2019-10-29 | 2019-12-31 | 福州大学 | Visible light photocatalyst for synthesizing water gas and preparation and application thereof |
| CN113318788A (en) * | 2021-06-25 | 2021-08-31 | 哈尔滨理工大学 | Cu-NH2Preparation of-MIL-125/TpPa-2 composite material and hydrogen production by photolysis of water |
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| CN113318788A (en) * | 2021-06-25 | 2021-08-31 | 哈尔滨理工大学 | Cu-NH2Preparation of-MIL-125/TpPa-2 composite material and hydrogen production by photolysis of water |
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Inventor after: Zhang Fengming Inventor after: Meng Xiangbin Inventor after: Sheng Jingli Inventor after: Li Jing Inventor after: Yu Taoyuan Inventor before: Meng Xiangbin Inventor before: Zhang Fengming Inventor before: Sheng Jingli Inventor before: Li Jing Inventor before: Yu Taoyuan |
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