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Method of preparing full-fluorine alkyl iodide

A perfluoroalkyl iodide and catalyst technology, which is applied in chemical instruments and methods, halogenated hydrocarbon preparation, organic chemistry, etc., can solve the problem of low selectivity of target products and low production capacity of reaction, and can not control high carbon number well By-products and molecular weight distribution, etc., to reduce time, avoid cyclopolymerization, and improve production capacity

Active Publication Date: 2007-03-14
SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

J.of FluorineChemistry.36(1987): 483-489 has introduced a kind of method that initiates preparation perfluoroalkyl iodide with metal copper powder catalysis, although this method can realize carrying out telomerization reaction at lower temperature, and Hydrocarbon groups are not introduced, but this method cannot well control the high-carbon number by-products and molecular weight distribution in the product, and the selectivity of the target product and the production capacity of the reaction are relatively low

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  • Method of preparing full-fluorine alkyl iodide
  • Method of preparing full-fluorine alkyl iodide

Examples

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Embodiment 1

[0022] Volume is 10L Hastelloy stainless steel vertical reaction kettle except moisture content, adds active palladium powder catalyst 15g. The kettle was sealed and evacuated, replaced with nitrogen several times to remove oxygen, and the oxygen content reached below 10ppm. Add C to the kettle with an auxiliary pump at room temperature 2 f 5 I 1500g, turn on the stirring, heat to 50°C, and pretreat the catalyst for 2 hours. Then slowly feed 15g of TFE monomer. When the temperature rises to 100°C, the pressure is about 2.0MP. When the pressure in the kettle drops to a certain level, 15g of TFE is fed again, and the TFE is repeatedly and slowly fed until the total mass of TFE is 450 grams, react until the pressure no longer changes, cool down, reclaim unreacted C 2 f 5 I, to obtain the product C 2 f 5 (CF 2 CF 2 ) n I total 874.5 grams, n≥1. Product is through alkaline washing, after dehydration treatment, see Table 1 with the ratio of each component in the product of...

Embodiment 2

[0025] 90g of active tantalum powder catalyst was added to a Hastelloy stainless steel horizontal reaction kettle with a volume of 10L except water. The kettle was sealed and evacuated, replaced with nitrogen several times to remove oxygen, and the oxygen content reached below 10ppm. Add CF to the kettle with an auxiliary pump at room temperature 3 I 900g, turn on the stirring, heat to 50°C, and activate the catalyst for 4 hours. Then slowly feed 25g of hexafluoropropylene monomer. When the temperature rises to 140°C, the pressure is about 2.5MP. Fluoropropylene until the total mass of hexafluoropropylene is 600 grams, react until the pressure no longer changes, lower the temperature, and reclaim unreacted CF 3 I, to obtain the product CF 3 (CFCF 3 CF 2 ) n I total 861.2 grams, n≥1. Product is through alkaline washing, after dehydration treatment, see Table 2 with the ratio of each component in the product of chromatographic analysis:

[0026] Chain length

Embodiment 3

[0028] The capacity is 10L Hastelloy stainless steel vertical reaction kettle except moisture content, add the active palladium powder catalyst 40g of load and alumina upper carrier. The kettle was sealed and evacuated, replaced with nitrogen several times to remove oxygen, and the oxygen content reached below 10ppm. Add C to the kettle with an auxiliary pump at room temperature 3 f 7 I 1800g, turn on the stirring, heat to 50°C, and activate the catalyst for 4 hours. Then slowly feed 20g of vinylidene fluoride monomer. When the temperature rises to 160°C, the pressure is about 2.5MP. When the pressure in the kettle drops to a certain level, 20g of vinylidene Vinyl fluoride until the total mass of vinylidene fluoride is 1000 grams, react until the pressure no longer changes, cool down, and reclaim unreacted C 3 f 7 I, to obtain the product C 3 f 7 (CH 2 CF 2 ) n I total 1235.8 grams, n≥1. Product is through alkali washing, after dehydration treatment, see Table 3 with...

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Abstract

The present invention relates to the telomerization process of perfluoro alkyl iodide in the general expression of Rf(CF2CF2)nI. By using fluoric olefin as the taxogen and RfI as the telogen, at the temperature of 60-160 deg.c and the system generated pressure, the present invention performs the telomerization reaction in perfluoro solvent under the initiation of the active Pd, Nd, Ta or their alloy catalyst. The active metal catalyst is prepared through activating the metal nitrate attached to carrier with hydrogen, and can control the carbon number of the product, raise selectivity on target product, raise the reaction rate and reduce the reaction period. The reaction is performed at relatively low temperature to avoid cyclopolymerization of tetrafluoroethylene and in a kettle type or tubular reactor for high production capacity of the target product.

Description

technical field [0001] The invention belongs to the field of perfluorofine chemical intermediates, and relates to a method for synthesizing perfluoroalkyl iodide compounds, in particular to a method for preparing perfluoroalkyl iodides by catalyzing telomerization with active metals. Background technique [0002] As we all know, perfluoroalkyl iodides are monoiodoperfluoroalkane compounds in which hydrogen atoms are completely replaced by fluorine atoms, and are generally composed of a series of perfluoroalkyl groups with different chain lengths. 6-12 perfluoroalkyl iodides, among which perfluorooctane iodide with 8 carbon atoms has the best performance. Perfluoroalkyl iodide is a key intermediate in the production of fluorine-containing finishing agents, fluorine-containing surfactants, and other fluorine-containing fine chemicals. Its downstream products are used in light water fire extinguishing agents, magnetic recording materials, and water- and oil-repellent fabric fin...

Claims

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Application Information

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IPC IPC(8): C07C17/269C07C19/16
Inventor 张永明王军高洪光苗忠杰
Owner SHANDONG HUAXIA SHENZHOU NEW MATERIAL
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