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Method for continuous production of perfluoroalkyl iodide telomer

A technology of perfluoroalkyl and iodide, which is applied in organic chemical methods, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of insufficient catalytic activity and medium chain length telomerization compound selection Unsatisfactory performance and other problems, to achieve the effect of continuous and efficient production

Inactive Publication Date: 2004-10-06
DAIKIN IND LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] However, even when the above-mentioned various catalysts are used, their catalytic activity is still insufficient and the selectivity for medium-chain-length telomer compounds in which n is 4 or less is not satisfactory.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] A stainless steel pipe with an inner diameter of 3 / 8 inch was filled with 46 g of spherical copper powder (produced by Mitsui Mining & Smelting Co. Ltd., particle size 300 mesh or less, average particle diameter 19 μm) as a tubular reactor. Wherein tetrafluoroethylene (TFE) is dissolved in perfluoroethyl iodide (TFE concentration is TFE / (adjustment+TFE)=4.25mol%) initial solution is provided in the stainless steel tube continuously with the speed of 9.0ml / min, The telomerization reaction was carried out under the reaction pressure of 3Mpa (gauge pressure). The reaction is carried out at 60-120°C.

[0049] The reaction solution discharged from the stainless steel tube was cooled, and its composition was analyzed by gas chromatography. Table 1 lists the results.

[0050] temperature reflex

Embodiment 2

[0052] A stainless steel pipe with an inner diameter of 3 / 8 inch was filled with 46 g of spherical copper powder (produced by Mitsui Mining & Smelting Co. Ltd., particle size 300 mesh or less, average particle diameter 19 μm) as a tubular reactor. Wherein tetrafluoroethylene (TFE) is dissolved in the perfluoroethyl iodide (TFE concentration is TFE / (adjustment+TFE)=4.25mol%) initial solution is provided continuously in the stainless steel tube, with the reaction pressure of 3MPa ( gauge pressure) and a temperature of 120°C for telomerization. The starting solution was provided at a rate of 1.4ml / min, 4.4ml / min or 9ml / min.

[0053] The reaction solution discharged from the stainless steel tube was cooled, and its composition was analyzed by gas chromatography. Table 2 lists the results.

[0054] Extraction of the starting solution

Embodiment 3

[0056] A stainless steel pipe with an inner diameter of 3 / 8 inch was filled with 18 g of spherical copper powder (produced by Mitsui Mining & Smelting Co. Ltd., particle size 330 mesh or less, average particle diameter 19 μm) as a tubular reactor. The initial solution in which tetrafluoroethylene (TFE) is dissolved in perfluoroethyl iodide is continuously supplied to the stainless steel tube reactor at a rate of 4.4ml / min, and the reaction pressure (gauge pressure) of 4.5MPa and 120°C The telomerization reaction is carried out at the temperature. The concentration of tetrafluoroethylene (TFE) in the starting solution is 3.03 mol%, 7.06 mol%, 8.42 mol% or 11.35 mol%.

[0057] The reaction solution discharged from the stainless steel tube was cooled, and its composition was analyzed by gas chromatography. Table 3 lists the results.

[0058] TFE concentration

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Abstract

The present invention relates to a process for continuously producing a perfluoroalkyl iodide represented by the general formula Rf(CF2CF2)nI, wherein Rf is a C1-6 perfluoroalkyl and n is an integer from 1 to 4, the method comprising continuously supplying a perfluoroalkyl iodide as a telogen represented by the general formula RfI, wherein Rf is as defined above, and tetrafluoroethylene as a taxogen to a tubular reactor packed with a metal catalyst comprising a powdery spherical metal or a sintered metal; and conducting telomerization at a temperature of 60 to 160 DEG C. under a pressure of 0.1 to 5 MPa (gauge pressure). According to the present invention, medium-chain perfluoroalkyl iodides can be continuously and efficiently produced with little generation of impurities, such as hydrogen-containing organic compounds and the like.

Description

technical field [0001] The present invention relates to a process for the continuous production of perfluoroalkyl iodide telomers. Background of the invention [0002] Perfluoroalkyl iodides having about 6 to 12 carbon atoms are used as components of surfactants and components of water and oil repellents for fibers. [0003] For the production of perfluoroalkyl iodides, the industry uses the method of telomerization reaction, which is represented by the following reaction formula: [0004] <chemistry num="001"> <chem file="02808257_cml001.xml" / > < / chemistry> [0005] where R f is a perfluoroalkyl group having 1 to 6 carbon atoms, and n is an integer of 1 to 4. [0006] This reaction is known to be carried out under heating. For example, DE 1,443,517 discloses a process in which the reaction is carried out at 250-800° C. and a pressure of 2 mmHg-5 atmospheres, with a residence time of 1 hour or less. However, such a thermal reaction has a problem in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/14B01J23/72B01J23/825B01J23/835B01J35/00C07B61/00C07C17/278C07C19/16
CPCB01J35/023B01J23/72B01J23/14B01J23/835B01J35/1009B01J35/02B01J35/08C07C17/278B01J35/612B01J35/51B01J35/40C07C19/16B01J35/00B01J35/30
Inventor 舩越义郎三木淳
Owner DAIKIN IND LTD
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