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A kind of preparation method of 1,1-difluoro-2-iodoethylene

A technology of vinyl iodide and vinylidene fluoride, applied in the field of preparation of fluorine-containing elastomers, can solve the problems of high price of raw material ICl, difficult to obtain and store, complicated operating conditions, etc., and achieves overcoming safety risks, high price, low cost, simple craftsmanship

Active Publication Date: 2022-05-17
JUHUA GROUP TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although this type of method can obtain products, there are raw material ICl that is expensive (the market price is about 1 million / ton), difficult to obtain and store, low total yield (≤85%), high cost, and complex operating conditions.

Method used

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  • A kind of preparation method of 1,1-difluoro-2-iodoethylene
  • A kind of preparation method of 1,1-difluoro-2-iodoethylene

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) 316L material tubular reactor (Changsha Yuchuang Instrument Equipment Co., Ltd.) has an inner diameter of 5cm, a wall thickness of 8mm, and a tube length of 120cm. The effective height of the glass filler filled inside is 100cm, the particle size of the filler is 2mm, and the effective filler at the entrance is 30cm. As the raw material preheating section, the remaining 70cm of effective packing is used as the reaction section. The reactor is controlled by three-stage electric heating to control the temperature of the preheating section to 60°C and the temperature of the reaction section to 60°C. Control vinylidene fluoride with a flow rate of 640g / h (10mol / h) and chlorine gas into the tubular reactor with a flow rate of 710g / h (10mol / h) through a mass flowmeter, and the reaction product is condensed through a condenser, and the crude product 1,2 -Dichloro-1,1-difluoroethane was condensed into the crude product receiving bottle, and the tail gas was absorbed by 30wt...

Embodiment 2

[0037] (1) Hastelloy tubular reactor (Changsha Yuchuang Instrument Equipment Co., Ltd.) has an inner diameter of 5cm, a wall thickness of 8mm, and a tube length of 120cm. The effective height of the glass filler filled inside is 100cm, and the particle size of the filler is 2mm. 30cm is used as the raw material preheating section, and the remaining 70cm of effective packing is used as the reaction section. The reactor is controlled by three-stage electric heating to control the temperature of the preheating section to 60°C and the temperature of the reaction section to 100°C. Vinylidene fluoride is controlled by a mass flow meter with a flow rate of 640g / h (10mol / h), and chlorine gas is simultaneously passed into the tubular reactor with a flow rate of 640g / h (9mol / h). The reaction product is condensed by a condenser, and the crude product 1,2 -Dichloro-1,1-difluoroethane was condensed into the crude product receiving bottle, and the tail gas was absorbed by 30wt% KOH aqueous ...

Embodiment 3

[0041] (1) 304 stainless steel tubular reactor (Changsha Yuchuang Instrument Equipment Co., Ltd.) has an inner diameter of 5cm, a wall thickness of 8mm, and a tube length of 120cm. The effective height of the glass filler filled inside is 100cm, the particle size of the filler is 2mm, and the effective filler at the entrance is 30cm. , as the raw material preheating section, and the remaining 70cm of effective packing is used as the reaction section. The reactor is controlled by three-stage electric heating to control the temperature of the preheating section to 60°C and the temperature of the reaction section to 130°C. Control vinylidene fluoride with flow rate 640g / h (10mol / h) by mass flow meter, chlorine gas is passed in the tubular reactor simultaneously with flow rate 674.5g / h (9.5mol / h), reaction product is condensed by condenser, crude product 1 , 2-dichloro-1,1-difluoroethane was condensed into the crude product receiving bottle, and the tail gas was absorbed by 30wt% ...

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Abstract

The invention discloses a preparation method of 1,1-difluoro-2-iodoethylene, comprising: (1) feeding vinylidene fluoride and chlorine into a tubular reactor for reaction, condensing and collecting the reaction product to obtain 1 , 2-dichloro-1,1-difluoroethane; (2) reacting the above-mentioned 1,2-dichloro-1,1-difluoroethane with KI in a solvent, after the reaction is completed, cooling and discharging, Evaporate the reaction solution to dryness, and rectify the obtained distillate to obtain 1-chloro-1,1-difluoro-2-iodoethane; (3) obtain 1-chloro-1,1-difluoro-2 ‑Iodoethane is reacted under the action of a magnetic catalyst. After the reaction is completed, the temperature is lowered and the material is discharged. The reaction solution is placed in an external magnetic field to separate the catalyst and rectified to obtain the 1,1‑difluoro‑2‑iodoethylene product. The invention has the advantages of simple process, readily available raw materials, high yield and environmental protection.

Description

technical field [0001] The invention relates to a preparation method of fluorine-containing elastomer, in particular to a preparation method of 1,1-difluoro-2-iodoethylene. Background technique [0002] Fluorine-containing elastomer is a kind of synthetic polymer elastomer containing fluorine atoms on the main chain or side chain carbon atoms. It is widely used in aerospace, aviation, military industry, national defense, automobile and other fields, especially in sealing. DuPont introduced iodine-containing vulcanization point monomers into fluoroelastomers in the 1990s, which can significantly improve the low-temperature performance and mechanical properties of vulcanizates. 1,1-Difluoro-2-iodoethylene is used as a The introduction of an important monomer with a vulcanization point into the body has attracted the attention of various companies, and its preparation method has become a research hotspot. [0003] At present, 1,1-difluoro-2-iodoethylene generally adopts the ad...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C17/25C07C21/18
CPCC07C17/04C07C17/25C07C19/16C07C21/18Y02P20/584
Inventor 吕杨黄明星
Owner JUHUA GROUP TECH CENT
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