CN108786924B - A kind of Ni (OH)2Preparation method of/TpPa-2 material and hydrogen production by photolysis of water - Google Patents
A kind of Ni (OH)2Preparation method of/TpPa-2 material and hydrogen production by photolysis of water Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims description 9
- 239000001257 hydrogen Substances 0.000 title abstract description 32
- 229910052739 hydrogen Inorganic materials 0.000 title abstract description 32
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 title abstract description 31
- 238000006303 photolysis reaction Methods 0.000 title abstract description 14
- 230000015843 photosynthesis, light reaction Effects 0.000 title abstract description 14
- 238000002360 preparation method Methods 0.000 claims abstract description 13
- 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
- 239000002244 precipitate Substances 0.000 claims description 7
- BWAPJIHJXDYDPW-UHFFFAOYSA-N 2,5-dimethyl-p-phenylenediamine Chemical compound CC1=CC(N)=C(C)C=C1N BWAPJIHJXDYDPW-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- QCDYQQDYXPDABM-UHFFFAOYSA-N phloroglucinol Chemical compound OC1=CC(O)=CC(O)=C1 QCDYQQDYXPDABM-UHFFFAOYSA-N 0.000 claims description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims description 4
- JPYHHZQJCSQRJY-UHFFFAOYSA-N Phloroglucinol Natural products CCC=CCC=CCC=CCC=CCCCCC(=O)C1=C(O)C=C(O)C=C1O JPYHHZQJCSQRJY-UHFFFAOYSA-N 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 229960001553 phloroglucinol Drugs 0.000 claims description 3
- 239000013310 covalent-organic framework Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 12
- 238000010521 absorption reaction Methods 0.000 abstract description 4
- 230000007062 hydrolysis Effects 0.000 abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000003153 chemical reaction reagent Substances 0.000 abstract 1
- 239000011941 photocatalyst Substances 0.000 abstract 1
- 238000011161 development Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- AUHZEENZYGFFBQ-UHFFFAOYSA-N 1,3,5-trimethylbenzene Chemical compound CC1=CC(C)=CC(C)=C1 AUHZEENZYGFFBQ-UHFFFAOYSA-N 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-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
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 239000002211 L-ascorbic acid Substances 0.000 description 1
- 235000000069 L-ascorbic acid Nutrition 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 238000003421 catalytic decomposition reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 238000001291 vacuum drying Methods 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
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- 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
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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
- 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
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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
- 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
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- 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
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- 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
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Abstract
A kind of Ni (OH)2A preparation method of a TpPa-2 material relates to Ni (OH)2A preparation method of a TpPa-2 material. The invention provides a novel Ni (OH)2The material TpPa-2 aims to solve the problem that the hydrogen production efficiency of the existing material for producing hydrogen by photolyzing water by TpPa-2 is not high. The preparation process is simple and effective, the reagent consumption is low, and the yield is high; the photocatalyst provided by the invention can effectively improve the problem of low hydrogen production efficiency by photocatalytic water splitting of TpPa-2. The invention is applied to the field of hydrogen production by photocatalytic hydrolysis, and experiments show that Ni (OH)2The material/TpPa-2 has good response performance to visible light, and has a strong and wide absorption band in a visible light region, and the absorption band edge is about 640 nm. At the same time, Ni (OH)2The material TpPa-2 has excellent performance of hydrogen production by photolysis of water, and the hydrogen production rate by photolysis of water can reach 1896 mu mol g‑1·h‑1。
Description
Technical Field
The invention relates to a Ni (OH)2The preparation method of the TpPa-2 material is applied to the field of hydrogen production by photocatalytic hydrolysis.
Background
Two major challenges faced by global sustainable development are energy and environmental problems, the survival and development of human beings are seriously affected by the increasingly exhausted fossil energy and the increasingly serious environmental pollution, and the search and development of renewable green energy which can replace the fossil energy become hot spots for energy utilization and material science research at home and abroad. The new energy developed at present mainly comprises wind energy, geothermal energy, ocean energy, solar energy and the like. Among them, solar energy is considered as one of the most promising new energy sources because of its advantages such as inexhaustibility and inexhaustibility. The utilization efficiency of solar energy is improved, and the method has important strategic significance for changing energy consumption structures. The solar energy is utilized to realize hydrogen production by water photolysis, which is an important way for promoting the economic development of hydrogen energy and solving the environmental and energy crisis. The method for realizing hydrogen production by solar energy water splitting comprises the steps of water electrolysis by solar energy, water splitting by photogenerator and hydrogen production by photocatalytic water splitting. Among these methods, the photocatalytic water splitting reduction hydrogen production (hydrogen molecules produced by solar energy driven thermodynamic reversible reaction) of semiconductor photocatalytic systems is a focus of attention.
In the early seventies of the twentieth century, Japanese scientists Fujishima and Honda found in TiO in the laboratory2The single crystal electrode can be used for photocatalytic decomposition of water to produce hydrogen, thereby revealing the possibility of directly decomposing water to produce hydrogen by using solar energy. However, there are still many problems in terms of the efficiency of using sunlight: on one hand, the photoresponse range of the semiconductor material is narrow, the semiconductor material only responds to 4% of ultraviolet light, and the sunlight utilization rate is low; on the other hand, the efficiency of photogenerated electron-hole pairs is high, and the quantum efficiency is low, so that the development of the photogenerated electron-hole pairs in the field of hydrogen production by water photolysis is limited. Therefore, researchers improve the hydrogen production technology by water photolysis from various aspects such as developing a new catalyst system, changing the types of sacrificial agents, improving the absorptivity of sunlight, reducing Schottky barrier of electron migration and the like, and obtain remarkable effects. However, numerous studies have also shown that: the development of a new catalyst system and the improvement of the performance of the original catalyst are still one of the main ways of effectively improving the photocatalytic conversion efficiency and reducing the cost of the catalyst at present.
Disclosure of Invention
The invention aims to solve the problem of low efficiency of hydrogen production by photolysis of water by the existing TpPa-2 material, and provides a Ni (OH)2Preparation method of/TpPa-2 materialThe method is carried out. A kind of Ni (OH)2The preparation of the material of the/TpPa-2 is completed according to the following steps: dispersing a proper amount of TpPa-2 in NaOH solution, carrying out ultrasonic treatment for 20-30 min under the condition that the ultrasonic frequency is 35-45 kHz, and dropwise adding Ni (NO) with different volumes3)2Reacting the solution for a period of time under the condition of magnetic stirring, centrifuging at 8000 r/min for 5min after reaction to obtain precipitate, washing with water for 3-5 times to neutrality, and finally drying in vacuum at 80 ℃ to obtain Ni (OH)2A material of TpPa-2;
ni (OH) mentioned above2The application of the material of TpPa-2 in the aspect of hydrogen production by photolysis of water.
The invention has the beneficial effects that:
the invention adopts a solvothermal method, takes 1,3, 5-trialdehyde phloroglucinol (Tp) and 2, 5-dimethyl-p-phenylenediamine (Pa-2) as raw materials, successfully synthesizes a covalent organic framework material TpPa-2, but the efficiency of photolysis of water to produce hydrogen under visible light is lower, and is only 72 mu mol h-1·g-1. The invention synthesizes a new material Ni (OH) based on the TpPa-2 material2TpPa-2, which effectively improves the hydrogen production performance of TpPa-2 by photolyzing water, Ni (OH)2The photolysis water hydrogen production efficiency of the/TpPa-2 material is 202-1896 mu mol-h-1·g-1。
Drawings
FIG. 1 shows (2.5 mol%) of Ni (OH) obtained in example 32The ultraviolet visible diffuse reflectance diagram of the material of the/TpPa-2;
FIG. 2 shows Ni (OH)2A graph of hydrogen production rate by photolysis of water with TpPa-2 material and TpPa-2.
Detailed Description
The invention is further illustrated by the following examples, which are merely illustrative of the process of the invention and are not intended to limit the scope of the invention in any way.
Example 1: ni (OH) according to the present embodiment2The preparation of the material of the/TpPa-2 is completed according to the following steps:
step one, preparation of TpPa-2: adding 1,3, 5-trialdehyde phloroglucinol (0.063 g) and 2, 5-dimethyl-p-phenylenediamine (0.048 g) into a heat-resistant glass tube, then adding a mixed solution of 1,3, 5-trimethylbenzene (1.5 mL), 1, 4-dioxane (1.5 mL) and acetic acid (0.5 mL and 3 mol/L), carrying out ultrasonic treatment for 30 min under the condition of ultrasonic frequency of 40 kHz, carrying out freeze-thaw cycle degassing for three times in a liquid nitrogen bath, heating for 72 h at 120 ℃ after sealing, filtering and washing for three times by tetrahydrofuran, and drying for 24 h in a vacuum drying box at 180 ℃;
step two, Ni (OH)2Preparation of a/TpPa-2 material: dispersing TpPa-2 in 30mL of 0.25 mol/L NaOH solution, carrying out ultrasonic treatment for 20-30 min under the condition that the ultrasonic frequency is 35-45 kHz, and dropwise adding 42 muL of Ni (NO)3)2Treating the solution for 6 h under the condition of magnetic stirring, centrifuging at 8000 r/min for 5min after reaction to obtain precipitate, washing with water for 3-5 times until the precipitate is neutral, and drying in vacuum at 80 ℃ to obtain (0.5 mol%) Ni (OH)2A material of TpPa-2;
example 2: this embodiment differs from example 1 in that: ni (NO) described in step two3)2The volume was 83 μ L, and other steps and parameters were the same as in example 1. To obtain (1 mol%) Ni (OH)2A material of TpPa-2.
Example 3: this embodiment differs from embodiment 1 or 2 in that: ni (NO) described in step two3)2The volume is 208 mu L, and other steps and parameters are the same as those of the embodiment 1 or 2. To obtain (2.5 mol%) Ni (OH)2A material of TpPa-2.
Example 4: this embodiment differs from specific examples 1 to 3 in that: ni (NO) described in step two3)2The volume is 333 mu L, and other steps and parameters are the same as those of the examples 1 to 3. To obtain (4 mol%) Ni (OH)2A material of TpPa-2.
Example 5: this embodiment differs from examples 1 to 4 in that: ni (NO) described in step two3)2The volume was 416 μ L, and other steps and parameters were the same as in examples 1 to 4. Obtaining (5 mol%) Ni (OH)2A material of TpPa-2.
To verify the beneficial effects of the present invention, the following tests were performed:
FIG. 1 shows (2.5 mol%) Ni (OH) obtained in example 32/TpPa-2 ultraviolet-visible diffuse reflectance pattern of material. From fig. 1, it can be observed that there is a strong and wide absorption band in the visible region. Absorption band edge of about 640nm, confirmed (2.5 mol%) Ni (OH)2The material of the/TpPa-2 has good corresponding performance to visible light.
To investigate Ni (OH)2The catalytic decomposition water hydrogen production effect of the TpPa-2 material is tested according to the following method. The test procedure was as follows: the photocatalytic hydrogen production experiment is carried out in a photocatalytic activity evaluation online analysis system, before the reaction starts, a condensation system is started, and air in the system is removed through a vacuum pump. The xenon lamp of 300W is used as the light source (more than or equal to 420 nm). 0.1g L-ascorbic acid as sacrificial agent, 50mL water as reaction solution, 0.01g Ni (OH)2the/TpPa-2 is used as a catalyst for hydrogen production by water photolysis, and 1 is a TpPa-2 material as shown in figure 2; 2 is (0.5 mol%) Ni (OH) obtained in example 12A material of TpPa-2; 3 is (1 mol%) Ni (OH) obtained in example 22A material of TpPa-2; 4 is (2.5 mol%) Ni (OH) obtained in example 32A material of TpPa-2; 5 is (4 mol%) Ni (OH) obtained in example 42A material of TpPa-2; 6 is (5 mol%) Ni (OH) obtained in example 52A material of TpPa-2. The hydrogen efficiency of the water photolyzed by the TpPa-2 under visible light is low and is only 72 mu mol.h-1·g-1(ii) a And new Ni (OH)2The material/TpPa-2 shows a good performance of photocatalytic hydrolysis hydrogen production, and the efficiency of photocatalytic hydrolysis hydrogen production is 202-1895 mu mol.h-1·g-1The performance of hydrogen production by photolysis of water of the TpPa-2 material is effectively improved.
Claims (6)
1. A kind of Ni (OH)2The preparation method of the material/TpPa-2 is completed according to the following steps: synthesizing a covalent organic framework material TpPa-2 by using 1,3, 5-trialdehyde phloroglucinol and 2, 5-dimethyl-p-phenylenediamine as raw materials, dispersing a proper amount of TpPa-2 in NaOH solution, carrying out ultrasonic treatment for 20-30 min under the condition that the ultrasonic frequency is 35-45 kHz, and dropwise adding Ni (NO) with different volumes3)2The solution is reacted for a period of time under the condition of magnetic stirring, after the reaction, the solution is centrifuged for 5min at 8000 r/min to obtain a precipitate, the precipitate is washed by water for 3 to 5 times until the precipitate is neutral, and finally the precipitate is vacuum-dried at 80 DEG CAir-drying to obtain Ni (OH)2A material of TpPa-2.
2. A Ni (OH) according to claim 12The preparation method of the TpPa-2 material is characterized in that the dosage of the TpPa-2 is 0.04-0.06 g.
3. A Ni (OH) according to claim 12The preparation method of the/TpPa-2 material is characterized in that the concentration of NaOH used is 0.2-0.25 mol/L.
4. A Ni (OH) according to claim 12The preparation method of the TpPa-2 material is characterized in that the volume ratio of the mass of the TpPa-2 to the volume of NaOH is 0.05 g: 20-30 mL.
5. A Ni (OH) according to claim 12Method for producing a TpPa-2 material, characterized in that said Ni (NO)3)2The concentration of (b) is 0.04-0.05 mol/L.
6. A Ni (OH) according to claim 12A method for preparing a TpPa-2 material, characterized in that said TpPa-2 mass is related to Ni (NO)3)2The volume ratio is 0.05g to 40-450 mu L.
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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 |
| CN110624610B (en) * | 2019-10-29 | 2021-06-01 | 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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