# US 11,028,199 B2 · Fluoropolymer powder and method for producing same

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- Number: US 11,028,199 B2
- Document ID: US11028199B2
- Status: Granted
- Kind: B2
- Application number: 16/341,527
- Filed: 2017-10-11
- Published: 2019-12-12
- Granted: 2021-06-08
- Earliest claimed: 2016-10-14
- Assignees: Daikin Industries, Ltd.
- Applicants: Daikin Industries, Ltd.
- Inventors: Yuki Yotsumoto; Tadashi Ino; Kazuhiro Ohtsuka; Noriyuki Shinoki; Masaharu Nakazawa; Takashi Yoshimura; Masahiro Kondo
- Web page: https://patentgrep.com/patent/US11028199B2

## CPC

- C08F 214/26: Tetrafluoroethene
- C08F 2/001: {Multistage polymerisation processes characterised by a change in reactor conditions without deactivating the intermediate polymer (C08F295/00, C08F297/00 take precedence)}
- C08F 2/22: Emulsion polymerisation
- C08F 2/26: anionic
- C08F 8/12: Hydrolysis
- C08F 8/44: Preparation of metal salts or ammonium salts
- C08F 214/262: {with fluorinated vinyl ethers}
- C08F 216/1408: {Monomers containing halogen}
- C08J 3/16: by coagulating dispersions {(C08J3/122 takes precedence)}
- C08J 7/14: with acids, their salts or anhydrides
- C09D 127/18: Homopolymers or copolymers of tetrafluoroethene
- C08F 216/1475: {Monomers containing sulfur and oxygen}
- C08F 2800/20: as weight or mass percentages
- C08F 2810/00: Chemical modification of a polymer
- C08F 2810/50: wherein the polymer is a copolymer and the modification is taking place only on one or more of the monomers present in minority
- C08F: MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29)
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)

## Abstract

The invention provides a powder that is easily redispersible in a liquid medium such as water. The powder contains a fluoropolymer. The fluoropolymer contains at least one group A selected from the group consisting of —SO2Y, —COOR, —SO3X, —SO2NR12, and —COOX, wherein Y is a halogen atom; R is a C1-C4 alkyl group; X is M1/L or NR14, where M is a hydrogen atom or an L-valent metal, the L-valent metal being a metal in group 1, group 2, group 4, group 8, group 11, group 12, or group 13 of the periodic table; and R1s are each individually a hydrogen atom or a C1-C4 alkyl group. The powder exhibits a dispersion of 50% or higher. The dispersion is calculated by filtering a composition obtainable by mixing the powder with water through a mesh having an opening of 20 μm.

## Claims

### Claim 1

A powder comprising a fluoropolymer and having an aspect ratio of 3 or lower,
the fluoropolymer containing at least one group A selected from the group consisting of —SO2Y, —COOR, —SO3X, —SO2NR12, and —COOX,
wherein Y is a halogen atom; R is a C1-C4 alkyl group; X is M1/L or NR14, where M is a hydrogen atom or an L-valent metal, the L-valent metal being a metal in group 1, group 2, group 4, group 8, group 11, group 12, or group 13 of the periodic table; and R1s are each individually a hydrogen atom or a C1-C4 alkyl group,
the powder exhibiting a dispersion of 50% or higher, the dispersion being calculated by filtering a composition obtained by mixing the powder with water through a mesh having an opening of 20 μm,
wherein the powder has an average primary particle size of greater than 30 nm to 300 nm.

### Claim 2 (depends on 1)

The powder according to claim 1,
wherein the powder contains 0 to 20% by mass of volatile matter.

### Claim 3 (depends on 1)

The powder according to claim 1,
wherein the fluoropolymer contains a constitutional unit derived from a fluoromonomer represented by the following formula (I):
CF2═CF—(O)n1—(CF2CFY1—O)n2—(CFY2)n3-A (I)
wherein Y1 is a halogen atom or a perfluoroalkyl group; n1 is an integer of 0 or 1; n2 is an integer of 0 to 3; n2 Y1s are the same as or different from each other; Y2 is a halogen atom; n3 is an integer of 1 to 8; n3 Y2s are the same as or different from each other; and A is the same as the group A.

### Claim 4 (depends on 3)

The powder according to claim 3,
wherein the fluoropolymer is a copolymer of two or more monomers and contains a constitutional unit derived from a fluoromonomer represented by the formula (I) and a constitutional unit derived from a different fluorine-containing ethylenic monomer.

### Claim 5 (depends on 4)

The powder according to claim 4,
wherein the fluorine-containing ethylenic monomer is at least one species of monomers represented by the following formula (II):
CF2═CF—Rf1 (II)
wherein Rf1 is a fluorine atom, a chlorine atom, Rf2, or ORf2, where Rf2 is a C1-C9 linear or branched perfluoroalkyl group optionally containing an ether bond.

### Claim 6 (depends on 5)

The powder according to claim 5,
wherein any or all of the monomers represented by the formula (II) are tetrafluoroethylene.

### Claim 7 (depends on 3)

The powder according to claim 3,
wherein in the formula (I), Y1 is a trifluoromethyl group, Y2 is a fluorine atom, n1 is 1, n2 is 0 or 1, and n3 is 2.

### Claim 8 (depends on 1)

A method for producing the powder according to claim 1, comprising:
a step (1) of preparing an aqueous dispersion (a) by emulsion polymerization, the aqueous dispersion (a) containing a fluoropolymer that contains at least one group selected from the group consisting of —SO2Y and —COOR, wherein Y is a halogen atom; and R is a C1-C4 alkyl group;
a step (2) of adding an alkali or an acid to the aqueous dispersion (a) to provide an aqueous dispersion (b), the aqueous dispersion (b) containing a fluoropolymer that contains at least one group selected from the group consisting of —SO3X, —SO2NR12, and —COOX, wherein X is M1/L or NR14, where M is a hydrogen atom or an L-valent metal, the L-valent metal being a metal in group 1, group 2, group 4, group 8, group 11, group 12, or group 13 of the periodic table; and les are each individually a hydrogen atom or a C1-C4 alkyl group;
a step (3) of filtering the aqueous dispersion (b) and collecting a residue; and
a step (4) of drying the residue at a work of 200 W or lower to provide a powder containing 0 to 20% by mass of volatile matter.
