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A kind of preparation method of high-efficiency photolysis water composite catalyst

A technology of composite catalyst and photolysis of water, which is applied in the field of energy and environmental materials, can solve the problems of complicated steps and low efficiency of photohydrogen production, and achieve the effect of simple device, good water solubility and improved utilization rate

Active Publication Date: 2017-01-04
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Most of the reported Au / semiconductor heterodimer structure nanocrystals are prepared in organic sol, which requires phase transfer between different sol phases, and the steps are complicated
In addition, in the few reported Au / semiconductor heterodimer structure nanocrystals prepared in aqueous sol, the semiconductor layer is mostly amorphous or polycrystalline, and because of the directionality enhanced by surface plasmons, each Au / semiconductor cannot be Surface plasmon-enhanced effects in semiconducting heterodimer-structured nanocrystals, resulting in low photohydrogen production efficiency

Method used

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  • A kind of preparation method of high-efficiency photolysis water composite catalyst
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  • A kind of preparation method of high-efficiency photolysis water composite catalyst

Examples

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preparation example Construction

[0036] (1) Preparation method of sulfur precursor solution

[0037] Take 3mL of n-dodecanethiol and 7mL of toluene, add them in turn to a 20mL polytetrafluoroethylene reactor, stir evenly to form a solution c, weigh 38.79mg of sulfur powder and add it to the above solution c, stir at room temperature for 2min, seal it, and React in an oven at 100°C for 15 hours, and take it out as a sulfur precursor for later use.

[0038] (2) The preparation method of selenium precursor solution

[0039] Take 3mL of octadecene and 7mL of toluene, add them in turn to a 20mL polytetrafluoroethylene reactor, stir evenly to form a solution d, weigh 134.5mg of selenium dioxide and add it to the above solution d, stir at room temperature for 2min, seal it, and It was reacted in an oven at ℃ for 15 hours, and then taken out as a selenium precursor for later use.

[0040] (3) Preparation method of gold nanoparticle hydrosol

[0041] Take 1.25mL 0.001mol / L chloroauric acid solution and 2.5mL 0.15mo...

Embodiment 1

[0045] (1) Take 30mL of the aqueous sol of the gold nanoparticles in a 50mL centrifuge tube, centrifuge and wash at 7000rpm for 10min, discard the supernatant, and redisperse the lower gold nanoparticles in 10mL of 0.025mol / L hexadecyltrimethyl Ammonium bromide (CTAB) solution, add 0.7mL 0.1mol / L ascorbic acid (A.A), 0.2mL 0.01mol / L silver nitrate (AgNO 3 ) solution, adding 1.0mL of 0.1mol / L sodium hydroxide (NaOH) to adjust the pH of the solution to 10, and standing in a water bath at 30°C for 1h to obtain the Au / Ag core-shell structure nanocrystalline sol with a concentration of 0.005mol / L.

[0046] (2) Take 15mL of the above-mentioned Au / Ag core-shell structure nanocrystalline sol and add it to a 20mL polytetrafluoroethylene reactor, then add 60uL of the sulfur precursor solution, mix well, seal it, and put it in an oven at 80°C for reaction At the end of 1h, wash with deionized water at a volume ratio of 1:1, centrifuge at 7000rpm for 10min, discard the supernatant, and ...

Embodiment 2

[0050] (1) Take 30mL of the aqueous sol of the gold nanoparticles in a 50mL centrifuge tube, centrifuge and wash at 7000rpm for 10min, discard the supernatant, and redisperse the lower gold nanoparticles in 10mL of 0.025mol / L hexadecyltrimethyl Ammonium bromide (CTAB) solution, add 0.7mL 0.1mol / L ascorbic acid (A.A), 0.35mL 0.01mol / L silver nitrate (AgNO 3 ) solution, adding 1.0mL of 0.1mol / L sodium hydroxide (NaOH) to adjust the pH of the solution to 10, and standing in a water bath at 30°C for 1h to obtain the Au / Ag core-shell structure nanocrystalline sol with a concentration of 0.005mol / L.

[0051] (2) Take 15mL of the above-mentioned Au / Ag core-shell structure nanocrystalline sol and add it to a 20mL polytetrafluoroethylene reactor, then add 80uL of the sulfur precursor solution, mix well, seal it, and put it in an oven at 80°C for reaction At the end of 1h, wash with deionized water at a volume ratio of 1:1, centrifuge at 7000rpm for 10min, discard the supernatant, and...

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Abstract

The invention relates to preparation and high-efficiency hydrogen production of a novel surface plasma enhanced high-efficiency photocatalytic water splitting composite catalyst Au / CdX (X refers to S, Se and the like). The Au / Cd core-shell structure nanocrystalline consists of Au particles serving as a core and a CdX semiconductor serving as a shell layer, wherein the size of the Au particles is 20-45nm; the CdX shell layer is a single crystalline layer of 2-12nm; and the crystal form is a hexagonal phase of wurtzite. The preparation method comprises the following steps: adding a precursor into hydrosol of the Au / Ag nanoparticles to be converted into Au / AgX; adding a cadmium salt and a phosphine ligand, reacting at the temperature of 50 to 80 DEG C to generate the Au / CdX catalyst. The photocatalytic water splitting hydrogen production efficiency of the catalyst is 20-30mol / g / h and is higher than that of pure CdS quantum dots of the same mass by over 1000 times. The water solubility is high, the inverted phase is not needed during the test, the operating device is simplified, and the time is shortened. Meanwhile, the material utilization rate is improved, the synthesis condition is mild, and the catalyst is environmentally friendly, feasible and low in cost and has wide application prospects in the field of photocatalysis.

Description

technical field [0001] The invention belongs to the field of energy and environmental materials, and specifically relates to a highly efficient photolysis of water to produce hydrogen Au / CdX (X represents S, Se and the composite of S and Se) core-shell structure nanocrystal catalyst and a preparation method thereof. [0002] technical background [0003] At present, the world is facing severe challenges such as energy shortage, environmental degradation and climate warming. Finding, developing and utilizing clean and renewable energy is an effective means to solve the above problems. Solar photocatalytic water splitting hydrogen production technology has become a research hotspot due to its advantages of no pollution, easy operation, and the ability to directly convert solar energy into clean hydrogen energy. At present, the main problem restricting the development of photocatalytic materials is that the current photocatalytic materials have poor separation efficiency of phot...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/04B01J27/057C01B3/04
CPCY02E60/36
Inventor 张加涛桂晶赵倩张清华陈涛
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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