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Method for preparing silanol by photocatalytic oxidation of silane

A technology for oxidizing silane and silanol, which is applied in the direction of silicon organic compounds, etc., can solve the problems of poor catalytic selectivity of precious metals, difficulty in preparing space silane, and unsuitability for industrial production, and achieve ultra-high activity and efficiency, high catalytic activity, and easy Separate reusable effects

Active Publication Date: 2022-04-01
XI AN JIAOTONG UNIV
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AI Technical Summary

Benefits of technology

This patented process allows for efficient use of expensive materials while also simplifying the overall procedure involved. By inducing chemical changes through UV radiation or other methods, it becomes possible to create new compounds from existing ones without losing any properties like reactivity or environmental impact. These novel products are useful intermediates for various industries including medicine, agriculture, electronics manufacturing, energy storage devices, biological researches, sensors, and electronic components.

Problems solved by technology

Technologies aim at developing new ways to make chemical substances like silicons through synthetic processes or natural sources such as silica gels. These techniques involve reactants made from different starting molecules called silans (Si), alkenyl groups on Si atoms) and other elements found naturally within these species. Current methods require complicated steps involving harsh treatments and often result in low yields and high manufacturing expenses. There is therefore a pressing need for improved methods for converting certain types of chemistry into more useful products while minimizing environmental concerns associated with existing methods.

Method used

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  • Method for preparing silanol by photocatalytic oxidation of silane
  • Method for preparing silanol by photocatalytic oxidation of silane
  • Method for preparing silanol by photocatalytic oxidation of silane

Examples

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preparation example Construction

[0041] 1) Carbon nitride g-C 3 N 4 The preparation method:

[0042] A certain amount of urea or melamine is calcined in air at 550°C for 3-6h, the heating rate is 5°C / min, and after cooling to room temperature, a pale yellow powder is obtained. spare.

[0043] 2) Preparation of carbon quantum dots:

[0044] A certain amount of citric acid was pyrolyzed at 180°C with a heating rate of 5°C / min. After pyrolysis for 40 hours, 5 mol / L NaOH was added to neutralize the solution, and then the brown-orange powder was obtained by freeze-drying. spare.

[0045] 3) Bismuth Vanadate BiVO 4 Doping state preparation method:

[0046] At a certain amount of BiVO 4 Add Pd, Cu, Ru, Ir, Re, Ag, Pt, Au or Rh element or its compound state with a mass fraction of 0.01%-1%, calcined in air at 400°C for 2 hours, and the heating rate is 5°C / min.

[0047] 4) Titanium dioxide TiO 2 Doping state preparation method:

[0048] First, add a certain amount of Pd, Cu, Ru, Ir, Re, Ag, Pt, Au or Rh elem...

Embodiment 1

[0049] Embodiment 1, the preparation of compound dimethylphenylsilanol

[0050] In a 10mL reaction flask, add 5mL water, add 50mM dimethylphenylsilane and 0.125mg Au-TiO 2 Under the induction of visible light, stir magnetically at room temperature for 30 minh. After the reaction, the catalyst was recovered by centrifugation, added 10ml of ethyl acetate for extraction, extracted twice, the organic phase was combined, the organic phase was distilled under reduced pressure at 30-40°C to remove the organic solvent, and the target compound dimethylbenzene was obtained by column chromatography elution Silanols (99% conversion, 98% selectivity). The column chromatography eluent adopts petroleum ether containing 10% ethyl acetate by volume, and the conversion rate of dimethylphenylsilane into dimethylphenylsilanol is as follows: figure 2 As shown, the gas chromatogram of the product is image 3 As shown in the figure, the retention times of dimethylphenylsilane, dimethylphenylsila...

Embodiment 2

[0052] Embodiment 2, the preparation of compound triphenylsilanol

[0053] In a 10 mL reaction flask, 1 mL of methanol was added, followed by 100 mM triphenylsilane and 1 mg of Au-ZnO, and magnetically stirred at room temperature for 1 h under the induction of visible light. After the reaction, the catalyst is recovered by centrifugation, the organic phase is distilled off under reduced pressure at 30-40°C to remove the organic solvent, and the target compound triphenylsilanol is obtained by column chromatography with petroleum ether containing 5% ethyl acetate by volume (99% conversion, 99% selectivity). The gas chromatogram of the product is as Figure 5 As shown, the retention times of triphenylsilane and triphenylsilanol are 7.71min and 8.42min, respectively. The structural formula of the product is as follows:

[0054]

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Abstract

The invention discloses a method for preparing silanol by photocatalytic oxidation of silane, which comprises the following steps: dissolving a silane substrate and a photocatalyst in a reaction solvent, and carrying out selective oxidation catalytic reaction under the induction of visible light to prepare silanol, the photocatalyst is prepared from zinc oxide (ZnO), cadmium sulfide (CdS), tin oxide (SnO2), titanium dioxide (TiO2), tungsten trioxide (WO3), zirconium dioxide (ZrO2), carbon nitride (g-C3N4), bismuth vanadate (BiVO4), carbon quantum dots, metal doping states of the carbon quantum dots and the like. The selected photocatalyst is simple to prepare, low in cost, easy to obtain, ultrahigh in activity and efficiency, easy to separate and reusable, mild in reaction condition, simple and convenient to operate, constant in material conservation and few in reaction by-products, the reaction can be expanded to a pure substrate system, and the method can be used for industrial large-scale production.

Description

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Claims

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Application Information

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Owner XI AN JIAOTONG UNIV
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