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Loaded dual-function catalyst and preparation method and use thereof

A bifunctional catalyst, supported technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of amino hydroxy compounds, etc., can solve the problems of easy loss and singleness of ionic liquids, and achieve relatively high loss of active components and operation. Simple, convenient, and highly reproducible results

Inactive Publication Date: 2009-03-25
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But currently using chemical bonds to There are very few studies on the immobilization of acidic ionic liquids on solid supports. Qiao et al. Contains [CF 3 SO 3 ] - The acidic ionic liquid is immobilized on the surface of mercapto-functionalized silica gel. This system can be used as an effective solid-phase catalyst for esterification and nitration reactions. The stability of the catalyst is enhanced, and the separation of products is easier, but it is only a single catalyst
[0006] because In acidic ionic liquid immobilization, there is a problem that ionic liquid is easy to be lost by using physical methods. Therefore, how to firmly immobilize acidic ionic liquid on the surface of silica gel, and then support metal platinum on it is the key to the preparation of bifunctional catalysts.

Method used

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  • Loaded dual-function catalyst and preparation method and use thereof
  • Loaded dual-function catalyst and preparation method and use thereof
  • Loaded dual-function catalyst and preparation method and use thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Synthesis of acidic ionic liquid 1-vinyl-3-sulfobutylimidazolium bisulfate:

[0031]① Take 0.50mol of 1-vinylimidazole and 0.5-0.55mol of 1,4-butane sultone, put them in a 250ml three-necked flask, and react at room temperature to 50°C for 12-96 hours to obtain a white The zwitterionic solid was washed sequentially with toluene and anhydrous ether, and then dried in vacuum at 40°C to constant weight to obtain the zwitterionic 1-vinyl-3-sulfobutylimidazolium salt.

[0032] ②Take 0.50mol of 1-vinyl-3-sulfobutylimidazolium salt into a four-necked flask, and slowly add 0.48-0.52mol of concentrated sulfuric acid (95%- 98%, the same below), and then reacted at room temperature to 40°C for 3 to 6 hours, washed the reaction solution with toluene and anhydrous ether in sequence, and then vacuum-dried to constant weight at 40°C to obtain the target product acidic ionic liquid 1-vinyl-3-sulfobutylimidazolium hydrogen sulfate. The molecular weight is 328.

[0033] FT-IR(KBr): υ ...

Embodiment 2

[0038] In the first step, 10g of HV-01 SiO produced by Tianjin Research Institute of Chemical Industry 2 Add to 200ml (2mol·L -1 ) in the hydrochloric acid solution for 2 hours, and the filtered precipitate was then stirred for 0.5 hour in the mixed solution of concentrated sulfuric acid and concentrated nitric acid (65-68% by mass, the same as in the following examples) at a volume ratio of 1:1 in 100ml, Then rinse with deionized water to pH = 7.0, and vacuum dry at 80 °C to obtain acid-washed SiO 2 ;

[0039] In the second step, the 2.0g SiO obtained in the first step by pickling 2 0.1mol·L added to 100ml -1 In the chloroform solution of 3-mercaptopropyltrimethoxysilane (MPS), react under reflux for 12 hours, let stand and age for 36 hours, then wash with chloroform, toluene and anhydrous ether in sequence, and vacuum dry at 60°C to obtain MPS modified silica gel.

[0040] In the third step, 2.0 g of the MPS modified silica gel prepared in the second step is added to a ...

Embodiment 3

[0044] In the first step, 10g of HV-01 SiO produced by Tianjin Research Institute of Chemical Industry 2 Add to 200ml (2mol·L -1 ) in hydrochloric acid solution for 4 hours, and the filtered precipitate was then stirred in 100ml of a mixed solution of concentrated sulfuric acid and concentrated nitric acid with a volume ratio of 4:1 for 0.5 hours, then rinsed with deionized water until pH = 7.0, at 80°C Vacuum-drying, obtains the SiO2 that pickling is handled;

[0045] In the second step, the 2.0g SiO obtained in the first step by pickling 2 0.4mol·L added to 100ml -1 In the chloroform solution of 3-mercaptopropyltrimethoxysilane (MPS), react under reflux for 24 hours, let stand and age for 36 hours, then wash with chloroform, toluene and anhydrous ether in sequence, and vacuum dry at 60°C to obtain MPS modified silica gel.

[0046] In the third step, 2.0 g of the MPS modified silica gel prepared in the second step is added to a 250ml garden-necked flask with magnetic stir...

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Abstract

The invention provides a supported bi-functional catalyst as well as a preparation method and applications thereof, belonging to the catalyst containing platinum and an organic compound simultaneously. The catalyst has the compositions: an acidic ionic liquid of 1-vinyl-3-sulfobutyl imidazole hydrosulfate ([HSO3-bvim]HSO4), an active metal Pt and a carrier silica gel. The preparation method comprises the steps: the acidic ionic liquid of 1-vinyl-3-sulfobutyl imidazole hydrosulfate and the modified silica gel are added in a weight ratio of 0.05 to 1:1, then a mixed solution of solvent and deionized water as well as azo-bis-isobutryonitrile (AIBN) are added thereto, and then the [HSO3-bvim]HSO4 / SiO2 solid-acid catalyst is obtained after the reaction; and finally the target product of supported bi-functional catalyst is obtained after the reaction by adding chloroplatinic acid and an alcohol-water mixed solution in a weight ratio of 0.0001 to 0.01:1 of the metal platinum to the solid-acid catalyst. The supported bi-functional catalyst is used in the nitrobenzene catalytic hydrogenation synthesis p-aminophenol reaction, and has advantages of extreme high stability, high mechanical strength, abrasion resistance and low loss of active components.

Description

technical field [0001] The technical scheme of the invention relates to a catalyst containing platinum and an organic compound, specifically a preparation method and application of a supported dual-function catalyst. technical background [0002] Immobilizing homogeneous precursors on solid supports is an important route to develop and prepare heterogeneous catalysts. Immobilized catalysts have the advantages of easy separation, recovery and recycling. [0003] Room temperature ionic liquids have the characteristics of non-volatility, high thermal stability, and designability, and are widely used in catalysis, organic synthesis, extraction and separation, and other fields. Many researchers have attempted to load ionic liquids on inorganic porous materials or organic polymer materials to prepare heterogeneous catalysts. But as far as the immobilization of ionic liquids is concerned, this is a new field of research on ionic liquids. [0004] Functional Acidic ionic liquids...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/02C07C215/76C07C213/00B01J23/42
Inventor 王延吉崔咏梅赵新强
Owner HEBEI UNIV OF TECH
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