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Catalyst for oxidative carbonylation of ethanol to synthesize diethyl carbonate and preparation method thereof

A technology for the oxidation of diethyl carbonate and ethanol, which is applied in the preparation of organic compounds, carbonate/haloformate preparation, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of low catalytic efficiency and easy Inactivation and other issues, to achieve the effect of good activity, high selectivity, mild conditions

Active Publication Date: 2019-09-20
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology allows for efficient preparation of dimethylether (C2H5OH) from alcohol by means of an oxygenated intermediate that forms two types of ester compounds - one being more stable than another type called monoether or trioxane. These ester groups are then used to create other chemicals like diacetone acrylate.

Problems solved by technology

This patented technical problem addressed in this patents relates to finding an efficient way to produce highly active but stable catalyst that could achieve higher yields than current processes such as those based on fossil resources or redoxy chemistry.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to a catalyst for oxidative carbonylation of ethanol to synthesize diethyl carbonate and a preparation method thereof, belonging to the technical field of oxidative carbonylation of alcohol and the gas phase synthesis catalytic technology of diethyl carbonate. The catalyst consists of uniformly distributed Cu ions, Pd ion active sites and silica carrier. The invention has the advantages that the relative distribution structure of the Cu ion and the Pd ion center is adjustable, and the electronic structure of the Cu and Pd centers is adjustable. The catalyst is used in the oxidative carbonylation of ethanol, a miniature fixed bed reactor is adopted and the conditions are mild. The catalyst has high activity and high selectivity to diethyl carbonate. Under stable conditions, the space-time conversion rate of ethanol reaches 298 mg.g/1.h-1. The selectivity of diethyl carbonate is 85.1%.

Description

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Claims

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Application Information

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Owner BEIJING UNIV OF CHEM TECH
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