Catalyst for synthesizing diethyl carbonate by oxidative carbonylation of ethanol and preparation method thereof
A technology for the oxidation of diethyl carbonate and ethanol, which is applied in the preparation of carbon monoxide and oxygen, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc. It can solve the problems of low catalytic efficiency and easy deactivation , to achieve the effect of good activity, high selectivity and mild conditions
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Embodiment 1
[0019] Step A: The quantitative relationship between different substances is x TEOS:(1-x)APS:(0.12-1)CTAB:(0.36-2)TMAOH. In this embodiment, 4g of cetyltrimethylammonium bromide was weighed and dissolved in deionized water, and stirred until completely dissolved; then 6g of tetramethylammonium hydroxide was added; 20g of ethyl orthosilicate was then added dropwise, and the stirring continued for a certain period of time. After that, 4g of 3-aminopropyltriethoxysilane was added dropwise, and the resulting suspension was stirred at room temperature, then transferred to a hydrothermal kettle, sealed and placed in an oven at room temperature to 200°C for static aging. After aging, the obtained sample was filtered with a sand core funnel, washed with deionized water until no white foam was produced, washed with absolute ethanol for the last time, and dried in an oven. The obtained white powder was refluxed and stirred in absolute ethanol and repeated 3 times to remove the template ...
Embodiment 2
[0024] Under the completely identical situation of experimental condition and embodiment 1, in the catalyst preparation process CuCl 2 with PdCl 2 The coordination order is adjusted to be with PdCl first 2 CuCl 2 Coordination, the catalyst support remains unchanged, as Schiff base-grafted mesoporous silica ImPy-SiO 2 , the prepared catalyst is recorded as Cu-Pd-ImPy-SiO 2 . Using the same evaluation process as in Example 1, the performance evaluation of the catalyst was carried out on a micro-tubular catalyst evaluation device to obtain 169mg·g -1 h -1 Ethanol space-time conversion rate and 77.5% diethyl carbonate selectivity.
Embodiment 3
[0026] Under the completely identical situation of experimental condition and embodiment 1, the prepared catalyst is carried out 2h pretreatment under the temperature of reaction and pressure under ethanol and (or) CO atmosphere, adopts the evaluation process completely identical with embodiment 1 afterwards , The performance evaluation of the catalyst was carried out on the micro-tubular catalyst evaluation device to obtain 162mg·g -1 h -1 Ethanol space-time conversion and 74.6% diethyl carbonate selectivity.
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