Photothermally chemical process for synthesizing iodoperfluoroparaffin

An iodoperfluoroalkane, photothermal chemistry technology, applied in chemical instruments and methods, organic chemistry, halogenated hydrocarbon preparation, etc., can solve the problems of low photoreaction quantum efficiency, short reactor life, low reaction speed, etc. To achieve the effect of increased reaction speed, easy separation and extended service life

Inactive Publication Date: 2002-07-03
上海博纳科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the target product can be synthesized with high selectivity by this method, the reaction speed is too low, the quantum efficiency of the photoreaction is low (usually about 0.1), and the reactor needs to be equipped with a circulation pump or a rectification cycle to cause the reaction. Severe corrosion of the reactor and short life of the reactor

Method used

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  • Photothermally chemical process for synthesizing iodoperfluoroparaffin
  • Photothermally chemical process for synthesizing iodoperfluoroparaffin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Use as attached figure 1 The photothermochemical reactor shown. Depend on figure 1 It can be seen that the reactor consists of two interconnected cylindrical tubes. The reaction tube 1 is 900 mm long and its inner diameter is 60 mm. A 40W ozone-free low-pressure mercury lamp 3 is sealed in the middle, and a conductive tape is wrapped around the outside. The inner diameter of the heat circulation tube 2 is 40 mm. , the outside is also wrapped with conductive tape, and the terminal posts at both ends of the lamp tube are led out by wires and connected to the electronic ballast. On the upper end of the reaction tube 1, there are feeding port 4, vacuum system connection port 5, reaction tube 1 and thermal cycle tube 2 are equipped with a material inlet 4 in the middle, and a material outlet 6 and a receiver 7 are arranged at the lower end of the heat circulation pipe 2 .

[0024] Add 20 grams of C to receiver 7 4 f 9 I and C 6 f 13 I mixture (wherein C 4 17.5%, C 6 ...

Embodiment 2

[0026] The reactor and operation steps are the same as in Example 1, the reaction temperature is 200°C (reaction tube 1), the total pressure of the reaction system is controlled at 80Kpa, and C 2 f 4 with C 2 f 5 The total molar ratio of I was 2.92, and the reaction was finished after 13.5 hours, and the product taken out was analyzed by gas chromatography. After analysis, the C contained in the product 2 f 5 I.C 4 f 9 I.C 5 f 11 I.C 6 f 13 I.C 7 f 15 I.C 8 f 17 I.C 9 f 19 I.C 10 f 21 I.C 12 f 25 The weight percentage composition of I is: 0.91%, 6.17%, 0.49%, 41.79%, 0.82%, 35.62%, 0.41%, 10.58%, 2.30%. Calculated from the above data to get C 2 f 5 The weight conversion rate of I is 97.2%, C 4 f 9 I.C 6 f 13 I.C 8 f 17 I.C 10 f 21 I versus C 2 f 5 The weight yields in terms of conversion of I were 6.5%, 68.6%, 110.6%, 32.9%, 7.2%, respectively. The quantum efficiency of this reaction is 0.23. In addition there are small amounts of perfluoroalk...

Embodiment 3

[0028] The reactor and operation steps are the same as in Example 1, the reaction temperature is 250°C (reaction tube 1), the total pressure of the reaction system is controlled at 100Kpa, and C 2 f 4 with C 2 f 5 The total molar ratio of I was 2.94, and the reaction was terminated after 17 hours, and the product taken out was analyzed by gas chromatography. After analysis, the C contained in the product 2 f 5 I.C 4 f 9 I.C 5 f 11 I.C 6 f 13 I.C 7 f 15 I.C 8 f 17 I.C 9 f 19 I.C 10 f 21 I.C 12 f 25 The weight percentage composition of I is: 1.70%, 5.13%, 0.35%, 22.87%, 0.55%, 38.58%, 0.45%, 21.60%, 7.77%. Calculated from the above data to get C 2 f 5 The weight conversion rate of I is 96.2%, C 4 f 9 I.C 6 f 13 I.C 8 f 17 I.C 10 f 21 I versus C 2 f 5 The weight yields in terms of conversion of I were 9.5%, 41.7%, 88.9%, 49.8%, 17.9%, respectively. The quantum efficiency of this reaction is 0.99. In addition there are small amounts of perfluoroal...

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Abstract

A photothermal chemical process for synthesizing iodoperfluoroparaffin features use of low-carbon iodoperfluoroparaffin and tetrafluoroethylene as raw materials, use of ultraviolet ray as triggering light source of photothermal chemical reaction, and its novel telomerizing method. Its advantages include high conversion rate of raw materials, and controllable distribution of products, that is, the highest output rate of C8F17I and the lowest output rate of high-carbon by-product.

Description

technical field [0001] The present invention relates to a method for synthesizing iodoperfluoroalkane, in particular to a method for regulating polymerization by continuously initiating free radicals with an ultraviolet light source and using light and high heat as the chain growth mode, and more particularly relates to iodoperfluoroalkane with a low carbon number A method for synthesizing iodoperfluoroalkanes with a narrow distribution of carbon chains using tetrafluoroethylene as a raw material. Background technique [0002] Iodoperfluoroalkane is a class of monoiodoalkane compounds in which hydrogen atoms are replaced by fluorine atoms. Its molecules have perfluoroalkyl groups that provide high surface activity, high stability, and hydrophobic and oleophobic properties. Perfluoroalkane Perfluoroiodane with a carbon chain length of 6 to 12 has the highest surface activity, and is a kind of fluorine-based three-proof (waterproof, oil-proof, anti-fouling) finishing agent, fl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/269C07C19/08
Inventor 张临阳徐宏程存康张淑兰蔡振良夏科峰巫建国吴亚妮付菲古宏晨
Owner 上海博纳科技发展有限公司
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