Composite solid acid as well as preparation method and application thereof

A technology for compounding solid acids and solids, which is applied in the preparation of carboxylic acid esters, the preparation of organic compounds, chemical instruments and methods, etc. The effect of high atomic economy, less three wastes and high yield

Active Publication Date: 2021-12-07
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The technical problem to be solved by the present invention is that the existing difluoroacetate synthesis method and complex production process, equipment corrosion, low yield and three wastes (waste solid, air, water) etc.

Method used

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  • Composite solid acid as well as preparation method and application thereof
  • Composite solid acid as well as preparation method and application thereof
  • Composite solid acid as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Preparation of Type I Composite Solid Acid I-A: Add 40.3g (1.0mol) of magnesium oxide and 84.0g (1.0mol) of aluminum fluoride to 500mL of deionized water, stir for half an hour, let stand, filter to obtain powder block solid, under nitrogen condition , heated to 300°C, kept at the temperature for 24 hours, cooled to room temperature, and ground into 100-200 mesh powder to prepare composite solid acid I-A.

Embodiment 2

[0056] Preparation of Type I Composite Solid Acid I-B: Add 79.9g (1.0mol) of titanium dioxide and 62.3g (1.0mol) of magnesium fluoride to 500mL of deionized water, stir for half an hour, let stand, filter to obtain powder block solid, under argon condition , heated to 250°C, kept at the temperature for 36 hours, cooled down to room temperature, and ground into 300-400 mesh powder to prepare composite solid acid I-B.

Embodiment 3

[0058] Preparation of Type I Composite Solid Acid I-C: Add 101.9g (1.0mol) of alumina and 62.3g (1.0mol) of magnesium fluoride to 500mL deionized water, stir for half an hour, let stand, filter to obtain powder block solid, under argon condition , heated to 300°C, kept at the temperature for 24 hours, cooled down to room temperature, and ground into 100-200 mesh powder to prepare composite solid acid I-C.

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Abstract

The invention discloses composite solid acid as well as a preparation method and application thereof. The preparation method of the composite solid acid disclosed by the invention comprises the following steps: adding an oxide and a fluoride into water, filtering to obtain a solid, and heating the obtained solid at the temperature of 150-350 DEG C for 12-100 hours to obtain the composite solid acid, wherein the oxide is one or more of magnesium oxide, aluminum oxide, zinc oxide, iron oxide, copper oxide, titanium dioxide, zirconium dioxide, silicon dioxide, diatomite and montmorillonite; and the fluoride is one or more of magnesium fluoride, calcium fluoride, zinc fluoride, copper fluoride and aluminum fluoride. The composite solid acid can be applied to preparation of difluoroacetate compounds, and the preparation method is high in atom economy, simple in preparation step, suitable for continuous channelization reaction in preparation process, safe in technological process, short in reaction time, high in yield and few in three wastes, and is an environment-friendly preparation method.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a composite solid acid, its preparation method and application. Specifically, it relates to a "one-pot method" synthesis method for the preparation of difluoroacetate by promoting the defluorination and rearrangement reaction of 1,1,2,2-tetrafluoroethyl alkyl ether with composite solid acid. Background technique [0002] As an important fluorine-containing fine chemical, difluoroacetate is widely used in pesticides, medicines and organic synthesis (J. Jaunzems and M. Braun, Org. Process Res. Dev. 2014, 18, 1055). Among them, ethyl difluoroacetate is also called ethyl difluoroacetate, molecular formula C 4 h 6 f 2 o 2 , is a colorless transparent liquid with a boiling point of 99°C. It is commonly used as an important reagent and synthetic building block containing difluoromethylene; ethyl difluoroacetate can undergo reactions such as reduction, condensation, and amid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/125B01J27/135B01J27/138C07C67/00C07C69/63
CPCB01J27/138B01J27/135B01J27/125C07C67/00C07C69/63
Inventor 赵刚孙磊杰孙家乐陈君花文杰陆颖鹏
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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