IPC분류정보
국가/구분 |
United States(US) Patent
등록
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국제특허분류(IPC7판) |
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출원번호 |
US-0117714
(2002-04-05)
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발명자
/ 주소 |
- Buckanin, Richard S.
- Tan, Lian S.
- McAlister, E. Steven
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출원인 / 주소 |
- 3M Innovative Properties Company
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대리인 / 주소 |
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인용정보 |
피인용 횟수 :
29 인용 특허 :
21 |
초록
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The present invention provides a method of preparing an aqueous dispersion of poly(perfluorovinyl ether) homopolymers. The present invention further relates to a method of making an aqueous fluoropolymer dispersion comprising bicomponent particles of poly(perfluorovinyl ether) homopolymers and a sec
The present invention provides a method of preparing an aqueous dispersion of poly(perfluorovinyl ether) homopolymers. The present invention further relates to a method of making an aqueous fluoropolymer dispersion comprising bicomponent particles of poly(perfluorovinyl ether) homopolymers and a second fluoropolymer. The dispersions of the present invention may be used for rendering fibrous substrates oil repellent, water repellent and/or stain repellent without altering the looks and feel of the substrate.
대표청구항
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1. A method of making a bicomponent fluoropolymer dispersion comprising the steps of:a. pre-emulsifying an aqueous mixture of a perfluorovinyl ether monomer in the presence of a fluorochemical emulsifier to an average emulsion droplet size of one micron or less, andb. polymerizing said perfluoroviny
1. A method of making a bicomponent fluoropolymer dispersion comprising the steps of:a. pre-emulsifying an aqueous mixture of a perfluorovinyl ether monomer in the presence of a fluorochemical emulsifier to an average emulsion droplet size of one micron or less, andb. polymerizing said perfluorovinyl ether in the presence of a free-radical initiator at temperature and for a time sufficient to produce particles of poly(perfluorovinyl other),c. subsequently adding at least one additional fluorinated comonomer without additional emulsifier, andd. further polymerizing the resulting mixture. 2. The method of claim 1 wherein perfluorovinyl ether monomers are of the formula: 2 ═CF—R f wherein R f represents a perfluorinated organic group having a chain length of at least 2 atoms and having at least one carbon atom and at least one oxygen atom. 3. The method of claim 2 wherein said R f group is a perfluoroalkoxy group, a perfluoroether group or a perfluoropolyether group. 4. The method of claim 2 wherein R f group is of the formula: 1 f O) n (R 2 f O) m R 3 f wherein R 1 f , R 2 f each independently represents a linear or branched perfluoroalkylene group having 1 to 6 carbon atoms, R 3 f represents a linear, branched or cyclic perfluoroalkyl group having 1 to 6 carbon atoms and n and m each independently represents an integer of 0 to 10. 5. The method of claim 4 wherein at least one of n and in is different from 0. 6. The method of claim 4 wherein in is 0, n is 1, R 1 f is —CF 2 CF 2 —, —CF 2 CF(CF 3 )— or —CF 2 CF 2 CF 2 — and R 3 f represents a linear, branched or cyclic perfluoroalkyl group having 1 to 6 carbon atoms. 7. The method of claim 1 wherein said fluoropolymer comprise particles having an average size of 80 to 200 nanometers. 8. The method of claim 1 wherein the degree of conversion of said polymerisation in said first polymerisation step is at least 1 percent. 9. The method of claim 1 wherein the amount of said poly(perfluorovinyl ether) in said bicomponent particle is from 1 to 50 wt. %. 10. The method of claim 1 wherein the amount of said poly(perfluorovinyl ether) in said bicomponent particle is from 1 to 10 wt. %. 11. The method of claim 1 producing a bicomponent particle dispersion comprising a first fluoropolymer consisting essentially of polymerised monomer units of the formulaa second fluoropolymer in said dispersion, wherein R f represents a perfluorinated organic group having a chain length of at least 2 atoms and having at least one carbon atom and one oxygen atom. 12. The method of claim 11 wherein a core-shell polymer is produced comprising a core of said first fluoropolymer and a shell of said second fluoropolymer. 13. The method of claim 1 wherein said emulsifier is a salt of linear or branched perfluoroalkyl carboxylic and sulphonic acids having 4 to 11 carbon atoms in the perfluoroalkyl chain. 14. The method of claim 1 wherein said emulsifier comprises perfluoropolymers that comprise repeating units derivable from a monomer of the formula:wherein a is 0, 1 or 2, and t is an integer of 2 to 4, and G is a moiety containing one or more nonionic, anionic or cationic hydrophilic groups. 15. The method of claim 1 wherein said emulsifier is selected from f a —O—(CF 2 O) k (CF 2 CF 2 O) p (CF(CF 3 )CF 2 O) q -Q 1 -COOM or 1 -O—(CF 2 O) k (CF 2 CF 2 O) p (CF(CF 3 )CF 2 O) q -Q 2 -COOZwherein k, p and q each represent a value of 0 to 15, and the sum of k, p and q being such that the number average molecular weight is at least 200 g/mol, R f a represents a perfluoroalkyl group of 2 to 4 carbon atoms, M and Z each independently represent hydrogen or a cation and Q 1 and Q 2 each independently represents —CF 2 — or —CF(CF 3 )—. 16. The method of claim 15 further comprising an emulsifier of the formula 1 -O—(CF 2 O) k (CF 2 CF 2 O) p ( CF(CF 3 )CF 2 O) q -Q 2 -COOZwherein k, p and q each represent a value of 0 to 15, arid the sum of k, p and q being such that the number average molecular weight is al least 200 g/mol, R f a represents a perfluoroalkyl group of 2 to 4 carbon atoms, M and Z each independently represent hydrogen or a cation and Q 1 and Q 2 each independently represents —CF 2 — or —CF(CF 3 )—. 17. The method of claim 1 wherein said fluorinated comonomers comprise ethylenically-unsaturated fluoromonomer containing at least one fluorine atom substituent on a double-bonded carbon atom, and further substituted with a halogen atom, hydrogen, or a lower fluoroalkyl radical. 18. The method of claim 1 wherein said fluorinated comonomers are selected from tetrafluoroethylene, vinylidene fluoride, hexafluoropropene, chlorotrifluoroethylene, 2-chloropentafluoropropene, tetrafluoroethylene, 1-hydropentafluoropropene, dichlorodifluoroethylene, trifluoroethylene, 1,1-chlorofluoroethylene, and trichloroethylene. 19. The method of claim 1 wherein said second polymerisation step further comprises at least one non-fluorinated monomer selected from ethylene and propylene. 20. The method of claim 1 wherein said initiator comprises a water-soluble initiator. 21. The method of claim 20 wherein said water-soluble initiator is present in amounts from 0.01 to 2 weight percent, based on the total weight of the monomers. 22. The method of claim 1 wherein the temperature of said first polymerisation step is between 50 and 80° C. 23. The method of claim 1 wherein the degree of conversion is said first polymerisation step is at least 5%. 24. The method of claim 1 wherein the amount of emulsifier is from 0.01 to 10 weight percent, relative to the total weight of the monomer.
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