Synthetic method of perfluoropropanoyl fluoride and preparation method of catalyst applied to reaction

A technology of perfluoropropionyl fluoride and a synthesis method, which is applied in the field of fluorine-containing fine chemicals, can solve the problems of harsh reaction conditions, unfavorable industrialized production, complicated reactor design, etc., and achieves short reaction time, simple production steps and high efficiency. Yield effect

Inactive Publication Date: 2016-05-04
TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the conditions required for the above reaction are harsh and the design of the reactor is complicated, which is not conducive to industrial production.
In CN103145544A, organic amine compounds, five-membered or six-membered nitrogen-containing heterocyclic compounds or six-membered condensed ring-li

Method used

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  • Synthetic method of perfluoropropanoyl fluoride and preparation method of catalyst applied to reaction
  • Synthetic method of perfluoropropanoyl fluoride and preparation method of catalyst applied to reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0029] 1. Preparation of supported catalyst:

[0030] (1) Weighing 0.05 moles of cesium fluoride (CsF) to be configured into 1 L of aqueous solution with a concentration of 0.05 mol / L, adding 50 g of activated carbon to the above solution, fully stirring, the stirring time is 5 hours;

[0031] (2) Stop stirring, put the mixed solution in a muffle furnace, evaporate the water therein, the evaporation temperature is 150 degrees Celsius, and fully dry to constant weight under vacuum and room temperature conditions to obtain a black powdery catalyst;

[0032] (3) Weighing and calculating the loading of cesium fluoride (CsF) in the supported catalyst is 12%.

[0033] 2. Synthesis of perfluoropropionyl fluoride:

[0034] (1) First, activate the supported catalyst prepared above at high temperature, set the activation temperature to 400° C., and set the activation time to 12 hours. After the activation, the system is naturally cooled down to room temperature.

[0035] (2) Adding 10...

Embodiment 2

[0040] 1. Preparation of supported catalyst:

[0041] (1) Take 0.2 moles of potassium fluoride (KF) and configure it into 500 mL of an aqueous solution with a concentration of 0.4 mol / L, add 50 g of activated carbon to the above solution, stir fully, and the stirring time is 12 hours;

[0042] (2) Stop stirring, put the mixed solution in a muffle furnace, evaporate the water therein, the evaporation temperature is 150 degrees Celsius, and fully dry to constant weight under vacuum and room temperature conditions to obtain a black powdery catalyst;

[0043] (3) Weigh and calculate the loading capacity of potassium fluoride (KF) in the supported catalyst to be 16%.

[0044] 2. Synthesis of perfluoropropionyl fluoride:

[0045] (1) Activate the supported catalyst prepared above at high temperature, set the activation temperature to 200° C., and set the activation time to 5 hours. After the activation, the system is naturally cooled down to room temperature.

[0046] (2) Adding 10g...

Embodiment 3

[0051] In order to further confirm that high-purity perfluoropropionyl fluoride can be prepared by the synthetic method of the present invention, the obtained material can be used in subsequent reactions without further purification. This example is based on Example 2 and calculated according to the conventional reaction. Weigh the produced perfluoropropionyl fluoride product, carry out esterification reaction with methanol, the reaction temperature is 50 degrees Celsius, and the reaction time is 2 hours. The product is washed with water, left to stand for liquid separation, and distilled, and the collected fractions are weighed. And calculate the yield, the yield of the prepared ester is 89%, and the purity of the prepared ester through gas chromatography analysis is 98.8%.

[0052] Content (%)

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Abstract

The invention discloses a synthetic method of perfluoropropanoyl fluoride and a preparation method of a catalyst applied to a reaction. The synthetic method is innovatively characterized by comprising the steps that hexafluoropropylene oxide serves as the raw material and is subjected to a isomerization reaction at the proper reaction temperature and under the action of the catalyst, so that perfluoropropionyl chloride is generated. The preparation method of the catalyst is innovatively characterized by comprising the steps of weighing and compounding alkali metal fluoride into a solution with a certain concentration, adding activated carbon, placing mixed liquor into a muffle furnace, and conducting evaporation and sufficient drying till constant weight is reached. According to the preparation method, perfluor epoxypropane serves as the raw material to synthesize the perfluoropropionyl chloride, the hexafluoropropylene oxide is subjected to the isomerization reaction at the specific temperature and under the action of the alkali metal fluoride catalyst with the activated carbon as the carrier, so that the perfluoropropanoyl fluoride is generated, the raw material conversion rate and the product purity are high, the purity of an obtained product can reach 99% and above without being subjected to fractionation, and when the product is made to have a chemical reaction with alcohol, ester with the purity being 98.8% can be obtained.

Description

technical field [0001] The invention relates to a method for synthesizing perfluoropropionyl fluoride, and also relates to a method for preparing a catalyst for the reaction, belonging to the technical field of fluorine-containing fine chemicals. Background technique [0002] Perfluoropropionyl fluoride is also known as pentafluoropropionyl fluoride, molecular formula: CF 3 CF 2 COF is an important chemical synthesis intermediate. Using the alkoxy and acyl structures in its molecule, the compound can be subjected to reactions such as addition, decomposition, hydrolysis, aminolysis, and alcoholysis to obtain a variety of derivatives, such as perfluoropropionic acid, perfluoroalkoxyacyl High value-added fluorine-containing fine chemicals such as fluorine and perfluorohexanone are widely used in the fields of fluorine-containing medicines, fluorine-containing pesticides, electronics and precision instruments. Therefore, it is particularly important to produce perfluoropropio...

Claims

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Application Information

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IPC IPC(8): C07C51/58C07C53/50C07C67/14C07C69/63B01J27/12
CPCB01J27/12C07C51/58C07C67/14C07C53/50C07C69/63
Inventor 耿谦李景旺姚素梅高国红戴楠楠
Owner TIANJIN CHANGLU CHEM NEW MATERIAL CO LTD
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