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Method of making fluoropolymers

A technology of fluoropolymers and polymers, which is applied in the fields of surface coating liquid devices, bulk chemical production, coating, etc., and can solve problems such as the polymerization of fluoromonomers that are not mentioned

Inactive Publication Date: 2007-05-16
THE UNIV OF NORTH CAROLINA AT CHAPEL HILL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] V.Krukonis and M.McHugh described the fractionation of perfluoroalkyl polyether oils and chlorotrifluoroethylene oligomers in supercritical carbon dioxide in "Supercritical Fluid Extraction" pages 156-158, but did not mention fluorinated Polymerization of Monomers in Supercritical Carbon Dioxide

Method used

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  • Method of making fluoropolymers
  • Method of making fluoropolymers
  • Method of making fluoropolymers

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Experimental program
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Effect test

Embodiment 1-17

[0053] Solubility, Polymerization and Copolymerization of Fluoroacrylate Monomers

Embodiment 1

[0055] Experimental procedure

[0056] Material. The five fluoromonomers illustrated by Formula (II) and Table 1 and Formula (III) and Table 2 were kindly provided by Minnesota Mining and Manufacturing Company (3M). MeFOSEA, EtFOSEA and EtFOSEMA were purified by recrystallization in methanol. By passing through Al 2 o 3 The column removes the inhibitor to purify 1,1-dihydroperfluorooctyl acrylate (FOA). AIBN (Kodak) was recrystallized twice from methanol. Carbon dioxide (Matheson, 99.99%) was passed through a copper oxide catalyst column to remove traces of oxygen followed by a molecular sieve (3A) column to remove traces of moisture. Freon-113 (CF 2 ClCFCl 2 ) Fractional distillation. Methanol (Mallinckrodt) was used as received.

[0057]

[0058] Table 1 Fluorinated monomers of formula (II)

[0059] name

R

R’

MeFOSEA

EtFOSEA

MeFOSEMA

EtFOSEMA

h

h

CH 3

CH 3

CH 3

CH 2 CH ...

Embodiment 3

[0073] Solubility evaluation in carbon dioxide

[0074] The solubility of poly(EtFOSEA) and poly(MeFOSEA) in carbon dioxide was tested using a flow system, and the results are listed in Table 4. Poly(EtFOSEA) was found to be very soluble (about 25 wt%) in both liquid and supercritical carbon dioxide. Poly(MeFOSEA) dissolved in liquid CO at room temperature at 3000 psi 2 . The view cell studies discussed below demonstrate that the polymer is 2 is also soluble in

[0075] For comparison, poly(methyl methacrylate) (PMMA) in liquid and supercritical CO 2 Solubility in. Quite the opposite is that even PMMA, which has a lower molecular weight than the two fluoropolymers discussed above, is insoluble in carbon dioxide at pressures of 2000-5000 psi and temperatures of room temperature - 160°C.

[0076]To ensure that the fluoropolymers form a homogeneous solution with carbon dioxide, the solubility of the five fluoropolymers was also tested using a viewing chamber...

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Abstract

A process for making a fluoropolymer is disclosed. The process comprises solubilizing a fluoromonomer in solvent comprising a carbon dioxide fluid, and then polymerizing the fluoromonomer to produce a fluoropolymer. A preferred solvent for carrying out the process is supercritical carbon dioxide; preferred fluoromonomers for carrying out the process are fluoroacrylate monomers such as 1,1-dihydroperfluorooctyl acrylate. The polymerization step is preferably carried out in the presence of an initiator such as azobisisobutyronitrile.

Description

[0001] Cross-references to related applications [0002] This application is a continuation-in-part of co-pending U.S. Application Serial No. 08 / 529,873, filed September 18, 1995, which is a continuation-in-part of U.S. Patent Application Serial No. 08 / 302,642, filed September 27, 1994, which follows The latter, pursuant to 35 U.S.C. § 371, is a continuation of PCT application PCT / US93 / 01626, filed February 26, 1993, the last application being part of US application serial number 07 / 858,150, filed and abandoned on March 27, 1992 continue. field of invention [0003] The present invention relates to a process for the manufacture of fluoropolymers, including copolymers thereof, in a solvent comprising a carbon dioxide fluid, such as supercritical carbon dioxide. Background of the invention [0004] Chlorofluorocarbons (CFCs) have been considered to be one of the main causes of atmospheric ozone depletion. Accordingly, considerable efforts have been directed at finding replac...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F16/24C08F14/18C08F20/22C08F12/20C08F2/06C08F2/04B05D1/02B05D5/08C08F2/00C08F6/12C08F16/22C08F20/24C08F20/28C08F20/38C08J3/02
CPCC08F16/24C08F12/20C08F16/22C08F20/22C08F6/12B05D1/025C08J2327/12C08J3/02C08F14/18B05D5/083Y02P20/54C08F2/04C08L27/12
Inventor 约瑟夫·M·德西蒙
Owner THE UNIV OF NORTH CAROLINA AT CHAPEL HILL