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Preparation method of 1, 1, 2, 2-tetrahydric perfluoro alkyl iodide

A technology of tetrahydroperfluoroalkyl and iodide, which is applied in 1 field, can solve the problems of high cost and high price of organic peroxide, and achieve the effects of improving efficiency, improving uniformity and stability, and low cost

Active Publication Date: 2013-11-06
太仓中化环保化工有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among the two methods, the former uses a noble metal catalyst, which is costly; the organic peroxide used in the latter is expensive and non-reusable, so the cost is high. In addition, it is dangerous and may introduce impurities into the reaction product
Therefore, both methods have certain limitations

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] This embodiment provides a C 4 f 9 CH 2 CH 2 The preparation method of I, concrete steps are as follows:

[0024] (1), add 15g 300 mesh copper powders in the vertical stainless steel reactor of 5L, seal and vacuumize the reactor. Replace with high-purity nitrogen so that the oxygen content in the kettle is less than 10ppm, and the moisture content is less than 100ppm. Then the reactor was evacuated to -0.1MPa, and 3kg of perfluorobutyl iodide (C 4 f 9 1) join in the reactor. Start stirring and heat up to 80°C, continue stirring for 60 minutes to obtain a suspension;

[0025] (2), slowly feed 31.5g ethylene gas into the reaction kettle through step (1), continue to heat up and control the reaction temperature to be 135°C, when the reaction pressure no longer changes, feed ethylene gas again, at this temperature Continue the reaction until the pressure no longer drops. The ethylene addition process was repeated until a total of 94.5 g was added until no ethylene ...

Embodiment 2

[0027] This embodiment provides a C 4 f 9 CH 2 CH 2 The preparation method of I, concrete steps are as follows:

[0028] (1) Add 30g of 300-mesh tin powder into a 5L vertical stainless steel reactor, seal the reactor and evacuate it. Replace with high-purity nitrogen so that the oxygen content in the kettle is less than 10ppm, and the moisture content is less than 100ppm. The reactor was then evacuated to -0.1 MPa, and 3 kg of perfluorobutyl iodide was added into the reactor through an auxiliary pump. Start stirring and heat up to 80°C, continue stirring for 60 minutes to obtain a suspension;

[0029] (2), slowly feed 39.3g ethylene gas into the reaction kettle through step (1), continue to heat up and control the reaction temperature to be 135°C, when the reaction pressure no longer changes, feed ethylene gas again, at this temperature Continue the reaction until the pressure no longer drops. The ethylene addition process was repeated until a total of 118 g was added u...

Embodiment 3

[0031] This embodiment provides a C 4 f 9 CH 2 CH 2 The preparation method of I, concrete steps are as follows:

[0032] (1) Add 60 g of 300-mesh copper-zinc mixed powder (mass ratio of copper to zinc: 65:35) into a 5L vertical stainless steel reactor, seal the reactor and evacuate it. Replace with high-purity nitrogen so that the oxygen content in the kettle is less than 10ppm, and the moisture content is less than 100ppm. The reactor was then evacuated to -0.1 MPa, and 3 kg of perfluorobutyl iodide was added into the reactor through an auxiliary pump. Turn on stirring and heat up to 80°C, continue stirring for 60 minutes to obtain a suspension;

[0033] (2), slowly feed 26.2g ethylene gas into the reaction kettle through step (1), continue to heat up and control the reaction temperature to be 135°C, when the reaction pressure no longer changes, feed ethylene gas again, at this temperature Continue the reaction until the pressure no longer drops. The ethylene addition ...

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Abstract

The invention relates to a preparation method of 1, 1, 2, 2-tetrahydric perfluoro alkyl iodide. Rf I and ethene have addition reaction under the existence of one or more of copper, nickel, tin, zinc, magnesium, iron or alloy thereof to obtain the 1, 1, 2, 2-tetrahydric perfluoro alkyl iodide, wherein the Rf is the perfluoro alkyl which has carbon numbers of 4-12 and has the structure of linear chain or branched chain. The preparation method comprises the following steps of: (1) adding catalytic agent into the Rf I, and stirring for 20-200min under the constant temperature of 50-150 DEG C to obtain suspension liquid; and (2) flowing the ethene into the suspension liquid to perform the addition reaction, wherein the reaction temperature is 50-250 DEG C, the pressure is a system self-generated pressure, the use amount of the catalytic agent is 0.1-5% of the mass of the feeding material of the Rf I, and the feeding material mole ratio of the ethene to the Rf I is 1:1-5. The method has lower cost, can obtain the 1, 1, 2, 2-tetrahydric perfluoro alkyl iodide with the content more than 98%, and has the yield reaching up to 95%.

Description

technical field [0001] The invention belongs to the field of perfluorinated fine chemical intermediates, in particular to a preparation method of 1,1,2,2-tetrahydroperfluoroalkyl iodide. Background technique [0002] At present, 1,1,2,2-tetrahydroperfluoroalkyliodides are widely used in the production of fluorine-containing finishing agents, fluorine-containing surfactants and other fluorine-containing fine chemicals. Compared with perfluoroalkyl iodide, the iodine on 1,1,2,2-tetrahydroperfluoroalkyl iodide is more likely to undergo substitution reaction to prepare corresponding polyfluoroalcohol, polyfluoroalkylthiol, polyfluoroalkane Various fluorine-containing intermediates such as carboxylic acid and polyfluoroalkylsulfonyl chloride. [0003] In the prior art, 1,1,2,2-tetrahydroperfluoroalkyl iodide is mainly prepared by addition reaction, specifically initiated under light, heat, free radical or catalyst conditions, and the reaction equation is as follows: [0004] R ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C19/16C07C17/275B01J23/72B01J23/14B01J23/80B01J27/138
Inventor 郭艳红胡开达梁成锋王军张海兵
Owner 太仓中化环保化工有限公司
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