Supported quaternary ammonium catalyst, its preparation method and application

A catalyst, supported technology, applied in the preparation of oxygen-containing compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of poor catalyst stability and easy loss of active components.

Active Publication Date: 2018-02-13
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] One of the technical problems to be solved by the present invention is that the prior art has the problems of poor catalyst stability and easy loss of active components, and a new supported quaternary ammonium catalyst is provided

Method used

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  • Supported quaternary ammonium catalyst, its preparation method and application
  • Supported quaternary ammonium catalyst, its preparation method and application
  • Supported quaternary ammonium catalyst, its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0102] Magnetic Fe 3 O 4 Preparation of nanoparticles: 14.12g Fe(acac) 3 Dissolved in a mixed solution composed of 200 mL of oleylamine and 200 mL of dibenzyl ether, the solution was treated at 110 °C for 1 hour under nitrogen protection, and then continued to be treated at 300 °C for 2 hours under nitrogen protection, and 100 mL of ethanol was added. The solid was washed three times with acetone, 100 mL each time, and the obtained solid was dried in a vacuum oven to obtain magnetic Fe 3 O 4 Nanoparticle A1 was characterized by transmission electron microscope and found that the average particle size of the nanoparticle was 9.5 nm.

[0103] Treatment of chlorosilicates: 10.0 g of magnetic Fe 3 O 4 Nanoparticle A1 was placed in a 500mL three-neck flask, and then 200mL anhydrous toluene, 2.0g γ-chloropropyl triethoxysilane (γ-chloropropyl triethoxysilane, CPTES, C 3 H 6 ClSi(OC 2 H 5 ) 3 ), refluxed at 110 °C for 24 hours, filtered, washed with absolute ethanol for 3 t...

Embodiment 2

[0107] Magnetic Fe 3 O 4 Preparation of nanoparticles: 14.12g Fe(acac) 3 Dissolved in a mixed solution composed of 400 mL of oleylamine and 50 mL of dibenzyl ether, the solution was treated at 80 °C for 5 hours under nitrogen protection, and then continued to be treated at 350 °C for 4 hours under nitrogen protection, and 100 mL of ethanol was added. The solid was washed three times with acetone, 100 mL each time, and the obtained solid was dried in a vacuum oven to obtain magnetic Fe 3 O 4 Nanoparticle A2 was characterized by transmission electron microscope and found that the average particle size of the nanoparticle was 5.9 nm.

[0108] Treatment of chlorosilicates: 10.0 g of magnetic Fe 3 O 4 Nanoparticle A2 was placed in a 500mL three-neck flask, and then 200mL anhydrous toluene, 0.2g γ-chloropropyl triethoxysilane (γ-chloropropyl triethoxysilane, CPTES, C 3 H 6 ClSi(OC 2 H 5 ) 3), filtered after refluxing for 6 hours, washed 3 times with absolute ethanol, and d...

Embodiment 3

[0112] Magnetic Fe 3 O 4 The preparation method of nanoparticles A2 is the same as [Example 2], and the process of chlorosilicate treatment is the same as that of [Example 1], except that the chlorosilicate used is CPTMS: 3-chloropropyl trimethoxysilane (3-chloropropyl trimethoxysilane) trimethoxysilane), the structural formula is ClC 3 H 6 Si(OCH 3 ) 3 , the carrier B3 was obtained. After weighing, it was found that B3 contained chlorosilicate and magnetic Fe. 3 O 4 The weight ratio of nanoparticles was 0.069.

[0113] The quaternization process is the same as the quaternization process described in [Example 1], except that the tertiary amine used is tributylamine, and the obtained Cl - Type-loaded quaternary ammonium salt C3.

[0114] Cl - The transformation of the supported quaternary ammonium salt is the same as the process described in [Example 1] to obtain catalyst D3, wherein the weight content of the quaternary ammonium salt component is 11.2%, and the rest is...

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Abstract

The invention relates to a supported quaternary ammonium catalyst, its preparation method and application, and mainly solves the problems of poor catalyst stability and easy loss of active components in the prior art. The supported quaternary ammonium catalyst of the present invention has the following average structural formula (1): it can be used in the industrial production of dialkyl carbonate prepared by transesterification.

Description

technical field [0001] The present invention relates to a supported quaternary ammonium catalyst, its preparation method and its application. Background technique [0002] Dimethyl carbonate (DMC) has active chemical properties, excellent physical properties, and is non-toxic and easily biodegradable. It is a new low-pollution, environmentally friendly green basic chemical raw material, which can be used as solvent, gasoline additive, lithium-ion battery Electrolytes and carbonylation, methylation and carbonylmethoxylation reagents are widely used in chemical and chemical fields. At present, countries are actively researching green chemical processes based on DMC, an environmentally friendly chemical raw material. Among them, the transesterification method has become a method with great industrial prospects due to its mild reaction conditions, high yield and co-production of ethylene glycol or propylene glycol. [0003] In general, alkali metal hydroxides, alkali metal car...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28C07C27/00C07C29/128C07C31/20C07C68/06C07C69/96
CPCY02P20/52
Inventor 陈梁锋何文军
Owner CHINA PETROLEUM & CHEM CORP
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