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A method for continuously preparing ishikawa fluorinating agent and a reaction device for realizing the method

A fluorinating agent and two-stage injection technology, which is applied in the direction of condensation/addition reaction to prepare amino compounds, organic chemistry, etc., can solve the problems of local heat release, heat removal, long reaction time, etc., and achieve production efficiency High, efficiency-enhancing, fast-response effects

Active Publication Date: 2017-01-11
SHANDONG GUOBANG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the intense heat release in this reaction process, the reaction is more sensitive to temperature, the problem of local heat release is more difficult to solve, there are many side reactions, and the heat in the whole reaction process is difficult to remove, so the reaction time is very long

Method used

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  • A method for continuously preparing ishikawa fluorinating agent and a reaction device for realizing the method
  • A method for continuously preparing ishikawa fluorinating agent and a reaction device for realizing the method

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Reaction device for realizing the method of continuous preparation of Ishikawa fluorinating agent, such as figure 1 As shown, it includes a primary jet mixer 1, a primary cooler 2, a secondary jet mixer 3, a static mixer 4 and a secondary cooler 5 arranged sequentially from front to back according to the process route. The first-stage jet mixer 1 and the second-stage jet mixer 3 have the same structure and are all existing products. For example, products such as SX / SK / SV / SL that can be produced by Qidong Mixer Factory Co., Ltd. can be adopted, and its structure is not described here. To repeat, the first-stage jet mixer 1 and the second-stage jet mixer 3 are each provided with two liquid inlets and one liquid outlet. The primary cooler 2 and the secondary cooler 5 have the same structure and are existing products. The primary cooler 2 and the secondary cooler 5 are each provided with a liquid inlet and a liquid outlet. heat exchangers, plate heat exchangers and other f...

Embodiment 2

[0026] Feed dichloromethane into the primary jet mixer with a flow rate of 600g / h, and feed diethylamine with a flow rate of 65g / h simultaneously, and dichloromethane and diethylamine are mixed in the primary jet mixer to form a mixed solution, After the mixed liquid is sprayed from the primary jet mixer, it directly enters the primary cooler and is rapidly cooled to below -20°C to form a cooled mixed liquid; then, the cooled mixed liquid directly enters the secondary jet mixer, and at the same time, it is cooled at a rate of 160g / h The flow rate conveys hexafluoropropylene to the secondary jet mixer, thereby forming a premixed liquid of cooling mixed liquid and hexafluoropropylene in the secondary jet mixer; the premixed liquid is sprayed from the secondary jet mixer and directly enters the static mixer, pre The mixed liquid is subjected to strong mixing and continuous reaction in the static mixer, the heat generated by the reaction is quickly removed by the cooling device in ...

Embodiment 3

[0028] Feed dichloromethane into the primary jet mixer with a flow rate of 700g / h, and feed diethylamine with a flow rate of 85g / h simultaneously, and dichloromethane and diethylamine are mixed in the primary jet mixer to form a mixed solution, After the mixed liquid is sprayed from the primary jet mixer, it directly enters the primary cooler and is rapidly cooled to below -25°C to form a cooled mixed liquid; then, the cooled mixed liquid directly enters the secondary jet mixer, and at the same time, it is cooled at a rate of 165g / h The flow rate sends hexafluoropropylene to the secondary jet mixer, thereby forming a premixed liquid of cooling mixed liquid and hexafluoropropylene in the secondary jet mixer; the premixed liquid is sprayed from the secondary jet mixer and directly enters the static mixer. The mixed liquid is strongly mixed and continuously reacted in the static mixer, the heat generated by the reaction is quickly removed by the cooling device in the static mixer,...

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Abstract

The invention discloses a method and a reaction device for continuously preparing an Ishikawa fluorinating agent. The method comprises the following steps of mixing dichloromethane and diethylamine by virtue of a jet mixer to obtain a mixture, cooling the mixture by virtue of a cooler, mixing the cooled mixture and hexafluoropropylene by virtue of a jet mixer and fully reacting in a static mixer and rapidly cooling by virtue of a cooler. The entire process is rapidly completed in a few seconds and the problems of long reaction time and multiple side reactions are effectively solved. The reaction device comprises a primary jet mixer, a primary cooler, a secondary jet mixer, the static mixer and a secondary cooler which are sequentially arranged and has the advantages of simplicity in structure and convenience in use.

Description

technical field [0001] The invention relates to a method for continuously preparing Ishikawa fluorinating agent and a reaction device for realizing the method. Background technique [0002] Ishikawa fluorinating agent referred to as PPDA, is C 3 f 5 NET 2 and C 3 f 6 NET 2 The mixture is an effective fluorinating agent for the substitution of hydroxyl groups in alcohols and carboxylic acids. PPDA as a fluorinating reagent was proposed by Ishikawa and his collaborators in 1979 based on the study of Yarovenko's reagent. Yarovenko reagent is the product generated by the reaction of diethylamine and chlorofluoroethylene. The product is an alkylamine, and the reaction conditions are very harsh. PPDA is a product produced by the reaction of diethylamine and hexafluoropropylene. Its reaction conditions are much milder than those of Yarovenko reagent, and the product is very stable. It will not deteriorate even if it is sealed at room temperature for several months. Advantag...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C209/60C07C211/15
Inventor 廖仕学梁永江李琦斌孟德伟陈林静徐登清安守明
Owner SHANDONG GUOBANG PHARMA
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