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Preparation method for stannous methyl amino iodide-titanium dioxide visible light catalytic material

A technology of stannous iodide and methylamino is applied in the field of preparation of methylamino stannous iodide-titanium dioxide visible light catalytic materials, and can solve the problems of poor control of coating uniformity, inaccurate component stoichiometry, and increased Synthetic material cost and other issues, to achieve the effect of improving visible light catalytic activity, wide light response range and low cost

Inactive Publication Date: 2016-07-20
SHANGHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, since methylaminotin iodide (MASnI 3 ) small bandgap width, so that the photogenerated electrons and holes rapidly recombine, although the photoresponse range is widened, but its catalytic efficiency is not high
[0004] Currently, methylamino tin iodide (MASnI 3 ) The commonly used methods for material preparation are: normal temperature grinding method (see literature: ChungI., SongJ.-H., ImJ., et al. J.Am.Chem.Soc. 2012,134,8579.); high temperature mixing method (SchaeferF.C., HechenbleiknerI., etal. J.Am.Chem.Soc. 1959,81,1466.); liquid phase spin coating method (NamJJ., JunHN., YoungCK., etal. NatureMaterials. 2014,13,897.), among them, the materials synthesized by grinding and mixing methods have low purity, often contain impurities, and the stoichiometric ratio of components is not accurate, so that certain defects will appear in the materials
The material synthesized by the liquid phase spin coating method improves the purity of the material, but the uniformity of the coating layer is not well controlled during the spin coating process, which affects the performance of the material
Moreover, the above methods all need vacuum operation, which increases the cost of synthetic materials and makes the operation more complicated.

Method used

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  • Preparation method for stannous methyl amino iodide-titanium dioxide visible light catalytic material
  • Preparation method for stannous methyl amino iodide-titanium dioxide visible light catalytic material
  • Preparation method for stannous methyl amino iodide-titanium dioxide visible light catalytic material

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Embodiment 1

[0031]In this embodiment, the preparation method of methylamino tin iodide-titanium dioxide visible light catalytic material, the steps of the method are as follows:

[0032] (1), the preparation of methyl ammonium iodide (MAI), comprises the following steps:

[0033] 30mL methylamine (CH 3 NH 2 ) alcohol solution and 30mL hydrogen iodide (HI) aqueous solution were mixed, magnetically stirred, and reacted at 0°C for 3 hours to obtain a mixed solution; the mixed solution was rotary evaporated to obtain a white precipitate; the white precipitate was dissolved in a mixed solvent of ethanol and ether Carry out recrystallization operation, put the precipitate after recrystallization in 60 ℃ of vacuum oven and dry 24h, obtain the methyl ammonium iodide (MAI) of white dryness, use in the preparation of above-mentioned methyl ammonium iodide (MAI) Methylamine (CH 3 NH 2 ) alcoholic solution can be a commercially available product, and its purity is an analytically pure reagent;

...

Embodiment 2

[0049] Embodiment 2: The method of this embodiment 2 is basically the same as that of the above-mentioned embodiment 1, the difference is that step 4 described in this embodiment 2 is specifically as follows:

[0050] The methylamino tin iodide-titanium dioxide (MASnI) described in step 4 3 -TiO 2 ) The preparation of visible light catalytic material comprises the following steps:

[0051] (4-1). The methylamino tin iodide (MASnI) synthesized in the 3rd step of 0.637g 3 ) and 2.8mL tetrabutyl titanate (TBOT) were added to 50mL n-hexane to form a mixed solution, nitrogen (N 2 ) into the mixed solution so as to remove the air in the mixed solution, and the mixed solution was heated, stirred and refluxed at 70°C for 8 hours to form a suspension;

[0052] (4-2). Step (4-2) in the second embodiment and step (4-2) in the first embodiment;

[0053] (4-3). Step (4-3) in the second embodiment and step (4-3) in the first embodiment;

[0054] (4-4). The dry solid powder formed in th...

Embodiment 3

[0057] The third embodiment is basically the same as the method in the first embodiment above, the difference is that step 4 described in the third embodiment is specifically as follows:

[0058] The methylamino tin iodide-titanium dioxide (MASnI) described in step 4 3 -TiO 2 ) The preparation of visible light catalytic material comprises the following steps:

[0059] (4-1). The step (4-1) in the third embodiment is the same as the step (4-1) in the first embodiment;

[0060] (4-2). Step (4-2) in the third embodiment is the same as step (4-2) in the first embodiment;

[0061] (4-3). Add the pure solid obtained in step (2) to 50mL deionized water, fully hydrolyze under the condition of magnetic stirring, and then filter and wash to form a precipitate, and put the precipitate into a vacuum drying oven , dried at 80°C for 12 hours to obtain dry solid powder;

[0062] (4-4). The step (4-4) in the third embodiment is the same as the step (4-4) in the first embodiment.

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Abstract

The invention discloses a preparation method for a stannous methyl amino iodide-titanium dioxide visible light catalytic material. The preparation method comprises the following steps: 1) preparing ammonium methyl iodide; 2) preparing stannous iodide; 3) preparing stannous methyl amino iodide; 4) preparing the stannous methyl amino iodide-titanium dioxide visible light catalytic material: adding stannous methyl amino iodide and tetrabutyl titanate into normal hexane, mixing, heating and stirring at 70 DEG C for reaction under reflux, centrifugally separating turbid liquid by using a high speed centrifuge, adding into deionized water after centrifugal separation, magnetically stirring, filtering, washing and drying to obtain dry solid powder, and putting into a muffle furnace for roasting, thereby acquiring the methyl amino stannous iodide-titanium dioxide visible light catalytic material. The preparation method is simple and convenient in operation and low in cost; the photoproduction electron generated by the visible light catalytic material can quickly transfer to a TiO2 guide tape; the recombination rate of photoproduction electron and hole can be reduced; the separation of the photoproduction electron-hole on the material interface can be promoted; the visible light catalytic activity of the material is promoted.

Description

technical field [0001] The invention relates to the technical field of visible light catalytic materials, in particular to a method for preparing a methylamino tin iodide-titanium dioxide visible light catalytic material. Background technique [0002] Photocatalytic material is a potential and ideal environmental purification material, titanium dioxide (TiO 2 ) has become a versatile material for photocatalytic applications due to its unique properties. However, since titanium dioxide (TiO 2 ) has too large a bandgap width, and can only absorb ultraviolet light with a wavelength less than 387nm, and ultraviolet light only accounts for about 4% of the total energy of sunlight, thus greatly limiting its application in actual production and life. [0003] In recent years, the emergence of organic-inorganic hybrid perovskite-based materials as light absorber hole transport layer materials has made optoelectronic technology have a new development direction. Methylamino tin iod...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38
CPCB01J31/38B01J35/39
Inventor 王晓红张薇宁赵庆国
Owner SHANGHAI UNIV
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