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Solid borne ionic liquid Cu salt catalyst as well as preparation method thereof and application in synthesis of dimethyl carbonate

A technology of ionic liquid and catalyst, which is applied in the field of immobilized ionic liquid Cu salt catalyst and its preparation, can solve problems such as no reports, and achieve the effects of reducing equipment corrosion, avoiding large dosage, and high catalytic activity

Inactive Publication Date: 2009-10-21
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there has not been any report on the application of solid-supported ionic liquid Cu salt catalyst system in the oxidative carbonylation of methanol

Method used

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  • Solid borne ionic liquid Cu salt catalyst as well as preparation method thereof and application in synthesis of dimethyl carbonate
  • Solid borne ionic liquid Cu salt catalyst as well as preparation method thereof and application in synthesis of dimethyl carbonate
  • Solid borne ionic liquid Cu salt catalyst as well as preparation method thereof and application in synthesis of dimethyl carbonate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] In the immobilized ionic liquid Cu salt catalyst represented by structural formula (1), the carrier is B-type silica gel, n is 3, and R is CH 3 , X is Br. The preparation method of the immobilized ionic liquid Cu salt catalyst of this structural formula is as follows:

[0029] 1. Preparation of pyridine ionic liquid

[0030]Add 59.62g of 3-chloropropyltrimethoxysilane and 47.46g of pyridine into a three-necked flask, the molar ratio of 3-chloropropyltrimethoxysilane to pyridine is 1:2, react at 95°C for 24 hours in an Ar atmosphere, Stand still, extract three times with 1,1,1-trichloroethane, and evaporate in a rotary evaporator to prepare trimethoxysilylpropylpyridinium chloride ionic liquid.

[0031] 2. Preparation of Immobilized Ionic Liquid Matrix

[0032] Add 6g of B-type silica gel and 3g of trimethoxysilyl propylpyridinium chloride ionic liquid into a three-necked flask, then add 54g of acetonitrile, in an Ar atmosphere, react at 70°C for 24 hours, filter with...

Embodiment 2

[0036] In the immobilized ionic liquid Cu salt catalyst represented by structural formula (1), the carrier is B-type silica gel, n is 3, and R is CH 3 , X is Br. The preparation method of the immobilized ionic liquid Cu salt catalyst of this structural formula is as follows:

[0037] In step 1 of the preparation method of the present invention, 19.87g of 3-chloropropyltrimethoxysilane and 7.91g of pyridine were added to a three-necked flask, and the molar ratio of 3-chloropropyltrimethoxysilane to pyridine was 1:1. React at 80°C for 48 hours in an Ar atmosphere, let stand, extract 3 times with 1,1,1-trichloroethane, evaporate in a rotary evaporator, and prepare trimethoxysilylpropylpyridinium chloride ionic liquid . In step 2 of the preparation method of the present invention, 6 g of B-type silica gel and 1.8 g of trimethoxysilylpropylpyridinium chloride ionic liquid were added to a three-necked flask, and then 32.4 g of acetonitrile were added, and reacted at 60 ° C for 20 ...

Embodiment 3

[0039] In the immobilized ionic liquid Cu salt catalyst represented by structural formula (1), the carrier is B-type silica gel, n is 3, and R is CH 3 , X is Br. The preparation method of the immobilized ionic liquid Cu salt catalyst of this structural formula is as follows:

[0040] In step 1 of the preparation method of the present invention, 19.87g of 3-chloropropyltrimethoxysilane and 23.73g of pyridine were added to a three-necked flask, and the molar ratio of 3-chloropropyltrimethoxysilane to pyridine was 1:3. React at 110°C for 20 hours in an Ar atmosphere, let stand, extract three times with 1,1,1-trichloroethane, evaporate in a rotary evaporator, and prepare trimethoxysilylpropylpyridinium chloride ionic liquid. In step 2 of the preparation method of the present invention, 3 g of B-type silica gel and 3 g of trimethoxysilylpropylpyridinium chloride ionic liquid were added to a three-necked flask, and then 54 g of acetonitrile was added, and reacted at 80° C. for 16 h...

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Abstract

The invention provides a compound, the constitutional formula is shown as (1), in formula (1) the carrier is one of B type silicon gel and SBA-15 molecular sieve, n is 1-3, R is any one of CH3 and CH2CH3, X is any one of Cl, Br, I, Ac, NO3. The preparation method of the compound comprises the steps of preparing pyridine ionic liquid, preparing solid borne ionic liquid matrix and preparing solid borne ionic liquid Cu salt catalyst. The application of the solid borne ionic liquid Cu salt catalyst in the synthesis of dimethyl carbonate is further provided in the invention. The catalytic activity of the catalyst of the invention is improved, and the loss of the active center Cu ion and corrosion of equipment are reduced; with the catalyst prepared by the invention adopted in the synthesis of dimethyl carbonate, the conversion rate of the methyl alcohol achieves 17%, and the selectivity of the dimethyl carbonate achieves 97.6%.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to an immobilized ionic liquid Cu salt catalyst, a preparation method thereof and an application of the catalyst. Background technique [0002] As a green organic solvent and catalyst, ionic liquid has attracted much attention due to its low vapor pressure, good solubility, thermal stability and chemical stability (J.F.Brennecke, AIChE J., 2001, 47: 2384-2389). Due to its unique properties, it has gradually replaced traditional volatile organic solvents in recent years and has been used in the fields of organic synthesis, separation and purification, and catalytic chemistry (M.H.Valkenberg, Appl.Catal.A: General, 2001, 215, 185-190) . Ionic liquids provide an environment different from traditional molecular solvents for chemical reactions, and can change the reaction mechanism to make the catalytic activity better. Due to the low vapor pressure and wide liquid temper...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/30B01J31/28B01J31/02B01J37/00C07C69/96C07C68/00
Inventor 董文生王晖刘春玲
Owner SHAANXI NORMAL UNIV
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