CN105148956B - A kind of high efficiency photocatalysis decompose aquatic products hydrogen catalyst and preparation method thereof - Google Patents
A kind of high efficiency photocatalysis decompose aquatic products hydrogen catalyst and preparation method thereof Download PDFInfo
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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 phosphorized copper and the compound photocatalysis Decomposition aquatic products hydrogen catalyst of titanium dioxide nanocrystalline and preparation method thereof, belong to nanocatalyst technical field.It is to be prepared into Kocide SD by copper nitrate, and Kocide SD is calcined with sodium hypophosphite under uniform temperature and nitrogen protection again, then by product washing, centrifugation, dry product phosphorized copper；Phosphorized copper is uniformly prepared with the nanocrystalline mixed grinding of anatase titania again.The present invention can make photochemical catalyzing produce 0.74mmol h of the hydroformylation reaction rate by pure titinium dioxide‑1g‑1Bring up to 7.94mmol h‑1g‑1, improve more than 10 times.Therefore the present invention is a kind of with the solution potential industrial applicability of energy crisis, and is a kind of new technical meanses for producing the environment-friendly novel energy.
Description
Technical field
The invention belongs to nanocatalyst technical field, and in particular to a kind of copper phosphide is combined with titanium dioxide nanocrystalline
Type photocatalysis Decomposition aquatic products hydrogen catalyst and preparation method thereof.
Background technology
Titanium dioxide is a kind of excellent material of photocatalysis performance, and its not only nontoxic but also relative low price, raw material comes
Source is again very abundant, and abundance is higher in the earth, and its whiteness is very high.It is a kind of semi-conducting material of excellent performance, is in photodissociation
Most materials is applied in water hydrogen preparation field, is the ideal material for solving energy crisis and producing clean energy resource.But, reality is deposited
Situation be that titanium dioxide uses its photochemical catalyzing extremely inefficient as photochemical catalyst decomposition water, it is difficult to meet industrialization
It is required that, light induced electron that titanium dioxide excites under ultraviolet light and hole quickly compound are primarily due to, light is had
Being utilized for effect, causes photochemical catalyzing effect very undesirable, so needs make improvements and design.
The content of the invention
It is extremely low in order to solve the problems, such as the photochemical catalyzing hydrogen generation efficiency that titanium deoxide catalyst is present in the prior art,
The present invention has made intensive studies to the mechanism that optically catalytic TiO 2 decomposes aquatic products hydrogen, is paying substantial amounts of original work
Afterwards, and then the present invention is completed.
High efficiency photocatalysis of the present invention decompose aquatic products hydrogen catalyst, are to be prepared into Kocide SD, hydroxide by copper nitrate
Copper is calcined with sodium hypophosphite under uniform temperature and nitrogen protection again, then by product washing, dry product copper phosphide；
Copper phosphide is uniform with the nanocrystalline mixed grinding of anatase titania again.The present invention can make photochemical catalyzing produce hydrogen reaction
Speed by pure titinium dioxide 0.74mmol h-1g-1Bring up to 7.94mmol h-1g-1, performance improve exceeded 10 times.Therefore originally
Invention is a kind of with the solution potential industrial applicability of energy crisis, and is a kind of new technology hand for producing the environment-friendly novel energy
Section.
A kind of high efficiency photocatalysis of the present invention decompose the preparation method of aquatic products hydrogen catalyst, and its step is as follows：
(1) taking copper nitrate solid particle and being stirred in reaction vessel makes its dissolving complete for 10~50 minutes, under continuing to stir
0.2~0.6 mole every liter of 50~100 milliliters of the sodium hydroxide solution, copper nitrate is added to be with the mole dosage ratio of NaOH
1：2~5, it is further continued for stirring and obtains suspension in 2~5 hours；
(2) suspension that step (1) is obtained is washed with deionized centrifugation 3~5 times, then centrifugation 1~3 is washed with ethanol
It is secondary, dried 10~15 hours under 80~100 degrees celsius again after abandoning supernatant；
(3) desciccate for obtaining step (2) and sodium hypophosphite (NaH2PO2·H2O) solid powder in mass ratio 1：
Grinding is uniform after 5~10 ratio mixing；
(4) product obtained by step (3) is taken in nitrogen, argon gas or the argon-mixed protection of nitrogen, 300~350 degrees celsius
Lower roasting 1~2 hour；
(5) product is washed with deionized centrifugation 3~5 times after step (4) is calcined, then centrifugation 1~2 is washed with ethanol
Time, abandon dry copper phosphide (Cu after supernatant3P)；
(6) 2.0~2.8 grams of PEO-PPOXs-PEO triblock copolymer (P123) is added
To in 80~160 milliliters of diethylene glycol (DEG)s, 3~6 milliliters of titanium tetrachloride aqueous solution (mass concentrations of titanium tetrachloride are then added>
99%) 3~6 milliliters of concentrated ammonia liquor (aqueous solution of mass fraction containing ammonia 25%~28%), is finally added, is taken the photograph 200~230
Reacted 3~5 hours in the oil bath of family name's degree；
(7) to the acetone that 50~80 milliliters are added in the mixed liquor in step (6), then acetone washing centrifugation 4~6 times,
Dried 10~15 hours under 80~100 degrees celsius again after abandoning supernatant；
(8) desciccate in step (7) is calcined 2~5 hours under 450~650 degrees celsius, obtains anatase two
TiOx nano is brilliant (grain size is 10~20 nanometers (nm))；
(9) by the product (copper phosphide in the product (anatase titania is nanocrystalline) and step (5) in step (8)
(Cu3P)) with mass ratio 100：Grinding is uniform (45~60 minutes) after 0.1~15 ratio is mixed, of the present invention so as to obtain
Photocatalysis Decomposition aquatic products hydrogen catalyst.
The test of luxuriant and rich with fragrance Lay light system for producing hydrogen is moored through Beijing and Japanese Shimadzu GC-81 types chromatograph is detected, light prepared by the present invention
Catalyst is catalyzed the simple titanium dioxide of photocatalytic water speed ratio under conditions of triethanolamine does sacrifice agent and is obviously improved, property
The raising of energy has exceeded 10 times.
The present invention can greatly improve photochemical catalyzing efficiency, further meet industrial requirement.Composite
Catalyst system greatly inhibits under ultraviolet excitation the compound of light induced electron and hole in titanium dioxide, improves photoproduction load
The separative efficiency of son is flowed, is effectively utilized luminous energy, and then improve the speed of its photochemical catalyzing.Therefore it is of the invention
It is a very significant innovation and creation.
Brief description of the drawings
Fig. 1：Pure Cu3P、TiO2And 2wt%Cu3P-TiO2Digital pictures, it can be seen that sample appearance color occurs very big change
Change, black is that we prepare pure Cu3P samples, color more shallow we prepare pure TiO2, color is grey
It is the 2wt%Cu of our preparations3P-TiO2Sample, it is seen that a small amount of Cu3P has very big influence to the color of sample.
Fig. 2：Pure Cu3P、TiO2With 0.125~5wt%Cu3P-TiO2The hydrogen-producing speed phenogram of sample；Can be with from figure
It is clear that our modified sample hydrogen-producing speeds than simple Cu3P、TiO2It is greatly improved.
Fig. 3：0.5wt%Cu3P-TiO2Cyclical stability phenogram；As can be seen from the figure our properties of sample ten
Divide stabilization, do not decay by 5 loop test performances.
Fig. 4：Figure (a) and figure (b) are pure TiO2And 0.5wt%Cu3P-TiO2Sample transmission electron microscope；Can be with from figure (a)
Find out pure TiO2Grain size it is nanocrystalline for 10~20 nanometers (nm), it can be seen that spacing of lattice (d), d=from figure (b)
0.230nm is Cu3[202] crystal face of P, d=0.196nm is Cu3[113] crystal face of P, d=0.350nm is TiO2[101] it is brilliant
Face, it was demonstrated that Cu3P and TiO2It is fine that both hetero-junctions of formation are combined.
Fig. 5：Pure TiO2And 0.5wt%Cu3P-TiO2Fluorescence spectrum characterization figure；Photoluminescence spectrum intensity indicates us and is combined
Sample greatly suppress the compound of light induced electron and hole, so as to improve the utilization ratio of luminous energy.
Fig. 6：Sample 0.5wt%Cu3P-TiO2Element Surface scan (mapping) phenogram and tunnel scanning electron microscopy
Mirror figure (SEM)；Mapping figures are the patterns of correspondence SEM, and directly displayed Cu, P, Ti, O element in composite sample is all present
And its distribution situation is it is also clear that be Cu so as to further confirm our sample3P and TiO2It is compound.
Fig. 7：Cu3P and TiO2X-ray diffractometer (XRD) phenogram；As can be seen from the figure Cu3P and TiO2It is
Pure phase, corresponding PDF cards numbering：65-3628 and 21-1272.
Specific embodiment
Below by specific embodiment, the present invention is described in detail, but the purposes of these exemplary embodiments and
Purpose is only used for enumerating the present invention, not constitutes any type of any restriction to real protection scope of the invention, more non-to incite somebody to action
Protection scope of the present invention is confined to this.
Embodiment 1
(1) take during 0.4689 gram of copper nitrate is put into 250 milliliters of beakers and stir 10 minutes, then continue to be added under stirring condition
100 milliliters of 0.25 mole every liter of sodium hydroxide solution, continues to stir 2 hours；
(2) suspension of step (1) is washed with deionized centrifugation 3 times, supernatant is outwelled in ethanol washing centrifugation 2 times
It is put into afterwards in 80 degrees Celsius of baking oven and dries 12 hours；
(3) by step (2) dried product and the sodium hypophosphite (quality of sodium hypophosphite：Step (2) is dried
Quality=5 of product：1) grind uniform in mortar；
(4) take the product obtained by step (3) and be put into the tube furnace with nitrogen protection device the roasting under the conditions of 300 degree
1 hour；
(5) product after step (4) is calcined is washed with deionized centrifugation 3 times, and ethanol washing centrifugation 2 times obtains product
Copper phosphide (Cu3P), the Cu of pure phase is detected as through X-ray diffractometer (XRD)3P；
(6) by 2.4 grams of PEO-PPOX-PEO triblock copolymer P123) add 80 millis
Rise in diethylene glycol (DEG), then add 4 milliliters of titanium tetrachloride solution (mass concentration of titanium tetrachloride is 99.5%), then add again
Enter 4 milliliters of concentrated ammonia liquor (mass fraction containing ammonia is 25% aqueous solution), be subsequently placed into 220 degree of oil bath under agitation
Reaction 3 hours；
(7) to 80 milliliters of acetone is added in the mixed liquor in step (6), then with acetone centrifuge washing 4 times, place into
Dried 12 hours in 80 degree of baking ovens；
(8) will under the conditions of 450 degree of desciccate in step (7) be calcined 2 hours anatase titania it is nanocrystalline
(TiO2) TiO of pure phase is detected as through X-ray diffractometer (XRD)2, it is 10~20 to characterize particle diameter through transmission electron microscope (TEM)
The TiO of nanometer2It is nanocrystalline
(9) product in step (8) is mixed to form uniform suspension (0.1 gram, 90 milliliters of pure phase titanium dioxide nanocrystalline
Water, 10 milliliters of mass fractions are 99.5% triethanolamine) and step (5) in product be mixed to form uniform suspension, phosphatization
Cuprous 0.1 gram, 90 milliliters of water, the triethanolamine that 10 milliliters of mass fractions are 99.5%) moor luxuriant and rich with fragrance Lay light through Beijing respectively and produce hydrogen system
Unified test is tried and Japanese Shimadzu GC-81 types chromatograph detection.Pure titinium dioxide (TiO prepared by the present invention2) nanocrystalline catalysis photodissociation
Water hydrogen-producing speed is 0.74mmol h-1g-1；Pure phase copper phosphide (Cu3P) nanocrystalline catalysis photocatalytic water hydrogen-producing speed is
0.05mmol h-1g-1。
Embodiment 2
Step (1)~(8) with embodiment 1, by the product (pure phase titanium dioxide (TiO in step (8)2) nanocrystalline and step
Suddenly product (pure phase copper phosphide (Cu in (5)3P) mass ratio is the (quality of titanium dioxide：Quality=100 of copper phosphide：
0.125), grind to be well mixed for 45 minutes in mortar and obtain sample 0.125wt%Cu3P/TiO2；By 0.1 gram of catalyst,
90 milliliters of water, 10 milliliters of mass fractions are that 99.5% triethanolamine is mixed to form uniform suspension, moor luxuriant and rich with fragrance Lay light through Beijing and produce
Hydrogen system is tested and Japanese Shimadzu GC-81 types chromatograph detection.The catalysis photocatalytic water of photocatalysis Decomposition aqua prepared by the present invention
Speed is 7.149mmol h-1g-1, than simple titanium dioxide hydrogen-producing speed 0.74mmol h-1g-1It is obviously improved, improves
Effect has exceeded 9 times.
Embodiment 3
Step (1)~(8) with embodiment 1, by the product (pure phase titanium dioxide (TiO in step (8)2) nanocrystalline and step
Suddenly product (pure phase copper phosphide (Cu in (5)3P) mass ratio is the (quality of titanium dioxide：Quality=100 of copper phosphide：
0.5), grind to be well mixed for 45 minutes in mortar and obtain sample 0.5wt%Cu3P/TiO2；By 0.1 gram of catalyst, 90 millis
Rise the triethanolamine that water, 10 milliliters of mass fractions are 99.5% and be mixed to form uniform suspension, moor luxuriant and rich with fragrance Lay light through Beijing and produce hydrogen system
Unified test is tried and Japanese Shimadzu GC-81 types chromatograph detection.The catalysis photocatalytic water speed of photocatalysis Decomposition aqua prepared by the present invention
It is 7.939mmol h-1g-1, than simple titanium dioxide hydrogen-producing speed 0.74mmol h-1g-1It is obviously improved, improves effect
10 times are exceeded.
Embodiment 4
Step (1)~(8) with embodiment 1, by the product (pure phase titanium dioxide (TiO in step (8)2) nanocrystalline and step
Suddenly product (pure phase copper phosphide (Cu in (5)3P) mass ratio is the (quality of titanium dioxide：Quality=100 of copper phosphide：
1), grind to be well mixed for 45 minutes in mortar and obtain sample 1wt%Cu3P/TiO2；By 0.1 gram of catalyst, 90 milliliters
Water, 10 milliliters of mass fractions are that 99.5% triethanolamine is mixed to form uniform suspension, and luxuriant and rich with fragrance Lay light system for producing hydrogen is moored through Beijing
Test and Japanese Shimadzu GC-81 types chromatograph detection.The catalysis photocatalytic water speed of photocatalysis Decomposition aqua prepared by the present invention is
7.698mmol h-1g-1, than simple titanium dioxide hydrogen-producing speed 0.74mmol h-1g-1It is obviously improved, improves effect and surpass
10 times are crossed.
Embodiment 5
Step (1)~(8) with embodiment 1, by the product (pure phase titanium dioxide (TiO in step (8)2) nanocrystalline and step
Suddenly product (copper phosphide (pure phase Cu in (5)3P) mass ratio is the (quality of titanium dioxide：Quality=100 of copper phosphide：
2), grind to be well mixed for 45 minutes in mortar and obtain sample 2wt%Cu3P/TiO2；By 0.1 gram of catalyst and 90 milliliters
Water and 10 milliliters of mass fractions are that 99.5% triethanolamine is mixed to form uniform suspension, and luxuriant and rich with fragrance Lay light system for producing hydrogen is moored through Beijing
Test and Japanese Shimadzu GC-81 types chromatograph detection.The catalysis photocatalytic water speed of photocatalysis Decomposition aqua prepared by the present invention is
6.673mmol h-1g-1, than simple titanium dioxide hydrogen-producing speed 0.74mmol h-1g-1It is obviously improved, improves effect and surpass
9 times are crossed.
Embodiment 6
Step (1)~(8) with embodiment 1, by the product (pure phase titanium dioxide (TiO in step (8)2) nanocrystalline and step
Suddenly product (pure phase copper phosphide (Cu in (5)3P) mass ratio is the (quality of titanium dioxide：Quality=100 of copper phosphide：
5), grind to be well mixed for 45 minutes in mortar and obtain sample 5wt%Cu3P/TiO2；By 0.1 gram of catalyst and 90 milliliters
Water and 10 milliliters of mass fractions are that 99.5% triethanolamine is mixed to form uniform suspension, and luxuriant and rich with fragrance Lay light system for producing hydrogen is moored through Beijing
Test and Japanese Shimadzu GC-81 types chromatograph detection.The catalysis photocatalytic water speed of photocatalysis Decomposition aqua prepared by the present invention is
5.354mmol h-1g-1, than simple titanium dioxide hydrogen-producing speed 0.74mmol h-1g-1It is obviously improved, improves effect and surpass
7 times are crossed.
To sum up preparating example, we draw conclusion further below：
(1) mass ratio of titanium dioxide and copper phosphide has individual optimal value scope, the i.e. quality of titanium dioxide：Copper phosphide
Quality=100：0.125~5；
(2) purity of copper phosphide and the pattern of titanium dioxide nanocrystalline have material impact to the performance of the catalyst；
(3) addition of sacrifice agent triethanolamine plays good synergy to photochemical catalyzing performance.
Claims (7)
1. a kind of high efficiency photocatalysis decompose the preparation method of aquatic products hydrogen catalyst, and its step is as follows：
(1) taking copper nitrate solid particle and being stirred in reaction vessel makes its dissolving complete for 10~50 minutes, continues to stir lower addition
50~100 milliliters of 0.2~0.6 mole every liter of sodium hydroxide solution, copper nitrate is 1 with the mole dosage ratio of NaOH：2~
5, it is further continued for stirring and obtains suspension in 2~5 hours；
(2) suspension that step (1) is obtained is washed with deionized centrifugation 3~5 times, then centrifugation 1~3 time is washed with ethanol,
Dried after abandoning supernatant；
(3) desciccate for obtaining step (2) and sodium hypophosphite solid powder in mass ratio 1：After 5~10 ratio mixing
Grinding is uniform；
(4) step (3) products therefrom is calcined under nitrogen, argon gas or the argon-mixed protection of nitrogen；
(5) product is washed with deionized centrifugation 3~5 times after step (4) is calcined, then centrifugation 1~2 time is washed with ethanol, does
Copper phosphide Cu is obtained after dry3P；
(6) 2.0~2.8 grams of PEO-PPOX-PEO triblock copolymer P123s are added to 80~
In 160 milliliters of diethylene glycol (DEG), 3~6 milliliters of titanium tetrachloride solutions are then added, finally add 3~6 milliliters of concentrated ammonia liquor,
Reacted 3~5 hours in 200~230 degrees Celsius of oil bath；
(7) to the acetone that 50~80 milliliters are added in the mixed liquor in step (6), then acetone washing centrifugation 4~6 times, then
Dried 10~15 hours under 80~100 degrees celsius；
(8) desciccate in step (7) is calcined, is obtained anatase titania nanocrystalline；
(9) by the product in the product in step (8) and step (5) with mass ratio 100：Grinding is equal after 0.1~15 ratio is mixed
The even high efficiency photocatalysis that obtain decompose aquatic products hydrogen catalyst.
2. a kind of high efficiency photocatalysis as claimed in claim 1 decompose the preparation method of aquatic products hydrogen catalyst, it is characterised in that：Step
Suddenly (2) are dried 10~15 hours under 80~100 degrees celsius.
3. a kind of high efficiency photocatalysis as claimed in claim 1 decompose the preparation method of aquatic products hydrogen catalyst, it is characterised in that：Step
Suddenly (4) are calcined 1~2 hour under 300~350 degrees celsius.
4. a kind of high efficiency photocatalysis as claimed in claim 1 decompose the preparation method of aquatic products hydrogen catalyst, it is characterised in that：Step
Suddenly (8) are calcined 2~5 hours under 450~650 degrees celsius.
5. a kind of high efficiency photocatalysis as claimed in claim 1 decompose the preparation method of aquatic products hydrogen catalyst, it is characterised in that：Step
Suddenly the milling time of (9) is 45 minutes~60 minutes.
6. a kind of high efficiency photocatalysis as claimed in claim 1 decompose the preparation method of aquatic products hydrogen catalyst, it is characterised in that：Step
Suddenly the mass ratio of titanium dioxide and copper phosphide is 100 in (9)：0.125~5.
7. a kind of high efficiency photocatalysis decompose aquatic products hydrogen catalyst, it is characterised in that：It is as described in claim 1~6 any one
Method prepare.
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| CN105903482B (en) * | 2016-05-20 | 2018-09-28 | 宁夏大学 | A kind of CoP/TiO2Composite photo-catalyst and its preparation and application |
| CN107376957B (en) * | 2017-06-27 | 2020-01-24 | 青岛鲁润能源环境有限公司 | Preparation method and application of red phosphorus-coated titanium dioxide nanofiber photocatalytic material |
| CN109865524A (en) * | 2017-12-05 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of carbon support transition metal phosphide produces hydrogen elctro-catalyst and preparation method thereof |
| CN108193219B (en) * | 2017-12-27 | 2019-05-28 | 黄河科技学院 | Phosphorized copper modified titanic oxide optoelectronic pole and preparation method thereof and the application in photoelectrocatalysis decomposition water |
| CN108483404A (en) * | 2018-04-20 | 2018-09-04 | 中国科学技术大学 | A kind of preparation method of unformed metal hydroxides nanometer sheet and phosphide nanometer sheet |
| CN110252359B (en) * | 2019-06-17 | 2020-04-03 | 四川大学 | Preparation method of catalyst for photolysis of water to produce hydrogen by using cadmium sulfide-containing heterojunction |
| CN112774732B (en) * | 2021-01-29 | 2023-04-11 | 江西新节氢能源科技有限公司 | Ti-MOF/Rh-Al 2 O 3 Preparation method of composite catalyst |
| CN115449630A (en) * | 2022-08-12 | 2022-12-09 | 上海师范大学 | Method for selective metal leaching of photocatalysis nitrile-amine-containing solution system |
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