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Method for catalytic esterification of -SO3H-containing metal-organic framework compound

A metal-organic framework, -SO3H technology, applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., can solve problems such as difficult product separation, harsh reaction conditions, and large losses , to achieve the effect of strong controllability, simple separation and easy operation

Inactive Publication Date: 2013-05-01
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to overcome the shortcomings of the prior art, such as serious environmental pollution, harsh reaction conditions, difficult product separation, large losses in recycling, and provide a 3 Method for Catalyzed Esterification of H Metal Organic Framework Compounds

Method used

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  • Method for catalytic esterification of -SO3H-containing metal-organic framework compound
  • Method for catalytic esterification of -SO3H-containing metal-organic framework compound

Examples

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Effect test

Embodiment 1

[0015] Example 1: 10 mmol of n-butanol, 10 mmol of glacial acetic acid and 16 mg of IRMOF-3a were added to a 25 ml one-necked flask with a stirring bar and a reflux condenser. The reaction was vigorously stirred at 110°C for 45 minutes, cooled to room temperature and filtered. The filtrate was detected by gas chromatography with a conversion rate of 98%, a selectivity of 100%, and a yield of 98%. The filter residue was vacuum-dried at 120°C for 8 hours to remove water and then recycled.

Embodiment 2

[0016] Example 2: 10 mmol of n-octanol, 15 mmol of glacial acetic acid and 16 mg of IRMOF-3a were respectively added to a 25 ml one-necked flask equipped with a stirring bar and a reflux condenser. The reaction was vigorously stirred at 110°C for 60 minutes, cooled to room temperature and filtered. The filtrate was detected by gas chromatography with a conversion rate of 94%, a selectivity of 100%, and a yield of 94%. The filter residue was vacuum-dried at 120°C for 8 hours to remove water and then recycled.

Embodiment 3

[0017] Example 3: 20mol ethanol, 10mmol oxalic acid and 36mg IRMOF-3b were respectively added into a 25ml single-necked bottle with a stirring bar and a reflux condenser. The reaction was vigorously stirred at 110°C for 60 minutes, cooled to room temperature and filtered. The filtrate was detected by gas chromatography with a conversion rate of 92%, a selectivity of 100%, and a yield of 92%. The filter residue was vacuum-dried at 120°C for 8 hours to remove water and then recycled.

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Abstract

The invention provides a method for catalytic esterification of a -SO3H-containing metal-organic framework compound, and belongs to the technical field of organic synthesis chemistry. In esterification reaction, a molar ratio of alcohol to acid is 1:(1-2); based on -SO3H, the molar weight of the -SO3H-containing metal-organic framework compound is 8 percent of the alcohol; the reaction temperature is 110DEG C, the reaction time is 30 to 60 minutes, and the reaction pressure is one atmosphere; after reaction, the temperature is reduced to room temperature; and after filtration, the obtained -SO3H-containing metal-organic framework compound catalyst is subjected to vacuum drying at 120DEG C to be recycled. Compared with the traditional reaction process using protonic acid, Lewis acid and acidic ionic liquid as a catalyst, the method has the advantages that the catalytic activity is high, the using amount of the catalyst is small, the catalyst is easily separated from a reaction system, the catalyst can be recycled and the like.

Description

Technical field: [0001] The invention belongs to the technical field of organic chemical synthesis, in particular to a 3 Method for catalytic esterification of H metal organic framework compound. Background technique: [0002] Metal-organic frameworks (MOFs) are network-like frameworks formed by linking oxygen- or nitrogen-containing organic ligands with transition metals. It is mainly formed by the self-assembly of metal ions and organic ligands, with metal or metal clusters as vertices and connected by rigid or semi-rigid organic ligands. Compared with traditional solid catalytic materials (such as molecular sieves, activated carbon, oxides, etc.), metal-organic framework compounds have the following two significant advantages as catalysts or catalyst supports: (1) have high specific surface area (such as Langmuir of MIL-101 The specific surface area is 5900m 2 g -1 ; The Langmuir specific surface area of ​​IRMOF-3 is 2160m 2 g -1 ); (2) By modulating metal ions and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/08C07C69/14C07C69/36B01J31/22
CPCY02P20/584Y02P20/588Y02P20/50
Inventor 岳彩波伊廷锋
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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