Process for preparing perfluoroalkyl group by telomerization

A perfluoroalkyl iodide and perfluoroalkyl technology, which is applied in the field of telomerization to synthesize perfluoroalkyl iodide, can solve the problems of wide carbon chain distribution of telomer products, difficulty in telomerization degree in tank reactors, and tubular reactors. Low reaction efficiency and other problems, to achieve the effect of no hydrogen-containing by-products, simple production equipment, and high product purity

Inactive Publication Date: 2008-11-19
JUHUA GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The degree of telomerization in the tank reactor is difficult to control, and the carbon chain distribution of the obtained telomer product is very wide; the reaction efficiency of the tubular reactor is low

Method used

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  • Process for preparing perfluoroalkyl group by telomerization

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Effect test

Embodiment 1

[0024]The telomerization test was carried out in an extraction tower reactor composed of a stainless steel reflux cooling tube with an inner diameter of 10mm and a height of 800mm; an extraction tower with an inner diameter of 40mm and a height of 400mm, and a product collection tank with a volume of 1.2L. The catalyst packing is a 5-mesh spherical active copper catalyst, and the height of the catalyst bed is 300 mm. The reflux cooling pipe is equipped with an outer jacket, which is cooled by a refrigerant inside, and the extraction tower and product collection kettle are also equipped with an outer jacket, and are heated by low-pressure steam. During the reaction, add 1500g C to the product collection kettle earlier. 2 f 5 I. Then pass industrial water to the jacket of the reflux cooling pipe, and pass low-pressure water vapor to the jacket of the extraction tower and the product collector, and control the temperatures of the middle part of the reflux cooling pipe, the extr...

Embodiment 2

[0026] The telomerization test was carried out in an extraction tower reactor composed of a stainless steel reflux cooling pipe with an inner diameter of 10mm and a height of 1500mm; an extraction tower with an inner diameter of 10mm and a height of 1300mm, and a product collection tank with a volume of 1.2L. The catalyst packing is a 50-mesh spherical active copper catalyst, and the height of the catalyst bed is 1000mm. The reflux cooling pipe is equipped with an outer jacket, which is cooled by refrigerant inside, and the extraction tower and product collection kettle are also equipped with outer jacket pipes, which are heated by low-pressure steam. Add 1500g C from the top of the tower 2 f 5 I. Industrial water is passed through the jacket of the reflux cooling pipe, and low-pressure water vapor is passed through the jacket of the extraction tower and product collection kettle. Then add C at a rate of 30g / h 2 f 4 , Continue feeding for 4h, stop the reaction after 2h of...

Embodiment 3

[0028] The telomerization test was carried out in an extraction tower reactor composed of a stainless steel reflux cooling tube with an inner diameter of 10mm and a height of 800mm; an extraction tower with an inner diameter of 40mm and a height of 400mm, and a product collection tank with a volume of 1.2L. The catalyst filler is a 10-mesh spherical active copper-nickel alloy catalyst, the mass ratio of copper to nickel is 3:7, and the height of the catalyst bed is 300mm. The reflux cooling pipe is equipped with an outer jacket tube, which is cooled by a refrigerant inside, and the extraction tower and product collection kettle are also equipped with an outer jacket tube, which is heated by low-pressure steam. After replacing the oxygen in the system with high-purity nitrogen, add 800g C from the top of the tower 2 f 5 I. Industrial water is passed through the jacket of the reflux cooling pipe, and low-pressure water vapor is passed through the jacket of the extraction tower...

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Abstract

The invention discloses a method for synthesizing perfluoro-alkyl iodide through telomerization. The method is as follows: short-carbon chain perfluoro-alkyl iodide and tetrafluoroethylene are added in an extraction column reactor filled with catalyst filler inside an extraction tower or a rectification tower reactor taking catalyst as filler so as to carry out reaction with the molar ratio between short-carbon chain perfluoro-alkyl iodide and tetrafluoroethylene of between 3:1 and 50:1 at a reaction temperature of between 40 and 200 DEG C, thereby obtaining perfluoro-alkyl iodide. The method takes the lead in taking the extraction column filled with catalyst filler inside the extraction tower or the rectification tower taking catalyst as filler as a reactor which is used in the telomerization of perfluoro-alkyl iodide; moreover, compared with the prior disclosed art, the method has the advantages of simple production equipment, easily controlled technological parameter, better operational safety, ideal reaction selectivity, high product purity and no hydrogen-containing byproducts, etc.

Description

technical field [0001] The invention relates to a polymerization reaction, in particular to a method for synthesizing perfluoroalkyl iodide by telomerization. Background technique [0002] Straight-chain perfluoroalkyl iodide R with carbon number 6-12 f (CF 2 CF 2 ) n I is a key intermediate in the production of fluorine-containing surfactants, fluorine-containing finishing agents and other fluorine-containing fine chemicals. Its downstream products have the characteristics of high surface activity, high thermal stability, high chemical stability and excellent water and oil repellency. [0003] Perfluoroalkyl iodide R f (CF 2 CF 2 ) n I is usually composed of a short carbon chain perfluoroalkyl iodide R f It is formed by telomerization of I and tetrafluoroethylene. where R f for C 1-6 Perfluoroalkyl, n is an integer of 1-4. [0004] The telomerization reaction can be carried out thermally, photo-initiated, catalyst-initiated or initiator-initiated. [0005] The...

Claims

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Application Information

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IPC IPC(8): C07C19/16C07C17/37
Inventor 周强吴周安王树华叶志翔
Owner JUHUA GRP
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