EP0257611A2 — Polyester compositions, process for preparing the…

Claim 1

Independent Claim 128 words

A polyester composition comprising a polyester and 0.001 to 5% by weight of fine spherical silica particles obtained by subjecting alkoxysilane to hydrolysis and condensation reaction, said particles being substantially amorphous and having an average diameter of 0.01 to 3.0 u.m, and the diameter dispersion index of said particles represented by the formula (1) being in the range of 1.1 to 2.7: wherein d 10 is the diameter of the particle when the cumulative number thereof is 10% of the total number of said particles, d≠ is the diameter of the particle when the cumulative number thereof is 90% of the total number of said particles, and d,o and d 90 are measured under an electron microscope, said cumulative numbers being calculated beginning with the largest particle size.

Claim 2

Dependent Claim 128 words

A polyester composition comprising a polyester and 0.001 to 5% by weight of fine spherical silica particles obtained by subjecting alkoxysilane to hydrolysis and condensation reaction, said particles being substantially amorphous and having an average diameter of 0.01 to 3.0 u.m, and the diameter dispersion index of said particles represented by the formula (1) being in the range of 1.1 to 2.7: wherein d 10 is the diameter of the particle when the cumulative number thereof is 10% of the total number of said particles, d≠ is the diameter of the particle when the cumulative number thereof is 90% of the total number of said particles, and d,o and d 90 are measured under an electron microscope, said cumulative numbers being calculated beginning with the largest particle size.

Claim 3

Dependent Claim 18 words

The polyester composition according to claim 1, wherein said polyester comprises ethylene terephthalate unit as main repeating unit.

Claim 4

Dependent Claim 17 words

The polyester composition according to claim 1, wherein said polyester comprises ethylene-2,6-naphthalate unit as main repeating unit.

Claim 5

Dependent Claim 26 words

The polyester composition according to any of claims 1 to 3, wherein said fine spherical silica particles comprises 90% by weight or more of silicon dioxide.

Claim 6

Dependent Claim 63 words

The polyester composition according to any of claims 1 to 4, wherein the fine spherical silica particles have a volumetric shape parameter represented by the following formula (2): wherein φv is defined as φv = V/D 3 , wherein V is the volume of the particle (µm 3 ) and D is the maximum projected diameter (um) of the projection of the particle.

Claim 7

Dependent Claim 199 words

A process for preparing a polyester composition comprising a polyester mainly comprising ethylene terephthalate repeating unit and fine spherical silica particles, which comprises subjecting an aromatic dicarboxylic acid and ethylene glycol to an esterification reaction, subjecting the reaction product of said esterification reaction to polycondensation reaction an the presence of a polycondensation catalyst, and adding said fine spherical silica particles at any stage till the initial polycondensation reaction is completed in an amount of 0.001 to 5% by weight based on the polyester to be produced, said particles being substantially amorphous, being obtained by subjecting alkoxysilane to hydrolysis reaction and condensation reaction, and having an average diameter of 0.01 to 3.0 u.m, and the diameter dispersion index of said particles represented by the formula (1) being in the range of 1.1 to 2.7: wherein d,o is the diameter of the particle when the cumulative number thereof is 10% of the total number of said particles, d 90 is the diameter of the particle when the cumulative number thereof is 90% of the total number of said particles, and d,o and d 90 are measured under an electron microscope, said cumulative numbers being calculated beginning with the largest particle size.

Claim 8

Dependent Claim 199 words

A process for preparing a polyester composition comprising a polyester mainly comprising ethylene terephthalate repeating unit and fine spherical silica particles, which comprises subjecting an aromatic dicarboxylic acid and ethylene glycol to an esterification reaction, subjecting the reaction product of said esterification reaction to polycondensation reaction an the presence of a polycondensation catalyst, and adding said fine spherical silica particles at any stage till the initial polycondensation reaction is completed in an amount of 0.001 to 5% by weight based on the polyester to be produced, said particles being substantially amorphous, being obtained by subjecting alkoxysilane to hydrolysis reaction and condensation reaction, and having an average diameter of 0.01 to 3.0 u.m, and the diameter dispersion index of said particles represented by the formula (1) being in the range of 1.1 to 2.7: wherein d,o is the diameter of the particle when the cumulative number thereof is 10% of the total number of said particles, d 90 is the diameter of the particle when the cumulative number thereof is 90% of the total number of said particles, and d,o and d 90 are measured under an electron microscope, said cumulative numbers being calculated beginning with the largest particle size.

Claim 9

Dependent Claim 79 words

The process for preparing a polyester composition according to claim 6, wherein the polycondensation reaction is carried out in the presence of an antimony (Sb) compound and/or a magnesium (Mg) compound of an amount defined by the following formulae (4) - (6): wherein Sb is the total number of moles of the antimony compound per 10 grams of the polyester, and Mg is the total number of moles of the magnesium compound per 10 6 grams of the polyester.

Claim 10

Dependent Claim 26 words

The process for preparing a polyester composition according to claim 6, wherein the fine spherical silica particles comprises 90% by weight or more of silicon dioxide.

Claim 11

Dependent Claim 62 words

The process for preparing a polyester composition according to claim 6, wherein the fine spherical silica particles have a volumetric shape parameter defined by the following formula (2): wherein φv is defined as φv = V/D 3 , wherein V is the volume of particle (µm 3 ) and D is the maximum projected diameter (µm) of the projection of the particle.

Claim 12

Dependent Claim 128 words

A polyester film which contains 0.001 to 5% by weight of fine spherical silica particles obtained by subjecting alkoxysilane to hydrolysis reaction and condensation reaction, said silica particles being substantially amorphous and having an average diameter of 0.01 to 3.0 um, the diameter dispersion index of said particles represented by the following formula (1) being in the range of 1.1 to 2.7: wherein d,o is the diameter of the particle when the cumulative number thereof is 10% of the total number of said particles, d 90 is the diameter of the particle when the cumulative number thereof is 90% of the total number of said particles, and d,o and d 90 are measured under an electron microscope, said cumulative numbers being calculated beginning with the largest particle size.

Claim 13

Dependent Claim 128 words

A polyester film which contains 0.001 to 5% by weight of fine spherical silica particles obtained by subjecting alkoxysilane to hydrolysis reaction and condensation reaction, said silica particles being substantially amorphous and having an average diameter of 0.01 to 3.0 um, the diameter dispersion index of said particles represented by the following formula (1) being in the range of 1.1 to 2.7: wherein d,o is the diameter of the particle when the cumulative number thereof is 10% of the total number of said particles, d 90 is the diameter of the particle when the cumulative number thereof is 90% of the total number of said particles, and d,o and d 90 are measured under an electron microscope, said cumulative numbers being calculated beginning with the largest particle size.

Claim 14

Dependent Claim 22 words

The polyester film according to claim 10, wherein said fine spherical silica particles comprise 90% by weight or more of silicon dioxide.

Claim 15

Dependent Claim 56 words

The polyester film according to claim 10, wherein said fine spherical silica particles have a volumetric shape parameter defined bv the followina formula (2): wherein φv is defined as φv = V/D 3 wherein V is the volume of particle (µm 3 ) and D is maximum projected diameter (u.m) of the projection of the particle.

Claim 16

Dependent Claim 30 words

The polyester film according to claim 10, wherein said fine spherical silica particles have a specific surface area ratio (R) defined by the following formula (3) of 5.0 or above:

Claim 17

Dependent Claim 31 words

The polyester film according to claim 10, which contains the inactive particles (B-II) precipitated in the reaction system in an amount of 0.05 to 1.0% by weight based on the polyester.

Claim 18

Dependent Claim 36 words

The polyester film according to claim 14, wherein said inactive particles (B-II) are the particles containing calcium, lithium and phosphorus elements each in an amount of 1.0% by weight or more based on said inactive particles.

Claim 19

Dependent Claim 38 words

The polyester film according to claim 10, wherein the number of interference fringes of n-th order (H n , per 1 cm 2 ) as measured by double beam interference. method, satisfies the following formulae (8) and (9):

Claim 20

Dependent Claim 52 words

The polyester film according to claim 10, which contains in addition to the fine spherical silica particles (hereinafter referred to as fine particles (A)), 0.005 to 1.0% by weight of fine particles (B-I) having (D 2 /D 1 ) defined by the following formula of in the range of 1.1 to 3.0:

Claim 21

Dependent Claim 20 words

The polyester film according to claim 17, where the Mohs hardness of said fine particles (B-I) is 4.0 or below.

Claim 22

Dependent Claim 25 words

The polyester film according to claim 10, wherein the F s value of the film in the machine direction is 12 kg/mm 2 or above.

Claim 23

Dependent Claim 16 words

The polyester film according to claim 10, wherein the film is a biaxially stretched polyester film.

Claim 24

Dependent Claim 133 words

A polyester film for magnetic recording media, which contains 0.001 to 5% by weight of fine spherical silica particles obtained by subjecting alkoxysilane to hydrolysis and condensation reaction, said silica particles being substantially amorphous and having an average diameter of 0.01 to 3.0 µm, the diameter dispersion index of said particles represented by the following formula (1) being in the range of 1.1 to 2.7: wherein d, a is the diameter of the particle when the cumulative number thereof is 10% of the total number of said particles, d 90 is the diameter of the particle when the cumulative number thereof is 90% of the total number of said particles, and d 10 and d 90 are measured under an electron microscope, said cumulative numbers being calculated beginning with the largest particle size.

Claim 25

Dependent Claim 133 words

A polyester film for magnetic recording media, which contains 0.001 to 5% by weight of fine spherical silica particles obtained by subjecting alkoxysilane to hydrolysis and condensation reaction, said silica particles being substantially amorphous and having an average diameter of 0.01 to 3.0 µm, the diameter dispersion index of said particles represented by the following formula (1) being in the range of 1.1 to 2.7: wherein d, a is the diameter of the particle when the cumulative number thereof is 10% of the total number of said particles, d 90 is the diameter of the particle when the cumulative number thereof is 90% of the total number of said particles, and d 10 and d 90 are measured under an electron microscope, said cumulative numbers being calculated beginning with the largest particle size.

Claim 26

Dependent Claim 25 words

The polyester film for magnetic recording media according to claim 21, wherein said fine silica particles comprise 90% by weight or more of silicon dioxide.

Claim 27

Dependent Claim 62 words

The polyester film for magnetic recording media according to claim 21, wherein the fine spherical silica particles have a volumetric shape parameter defined by the following formula (2): wherein φv is defined as φv = V/D 3 , wherein V is the volume of particle (µm 3 ) and D is the maximum projected diameter (µm) of the projection of the parficle.

Claim 28

Dependent Claim 26 words

The polyester film for magnetic recording media according to claim 21, wherein the specific resistance [ρν] in molten state of the film satisfies the following formula:

Claim 29

Dependent Claim 43 words

The polyester film for magnetic recording media according to claim 21, wherein the film surface roughness (Ra), double refractive index (An) and the number of broken protuberances per 1 mm 2 (Bp) on the film surface satisfy the following formulae (14) - (16):

Claim 30

Dependent Claim 32 words

The polyester film for magnetic recording media according to claim 21, wherein said film has a thickness of 4 to 30 µm and is used as a base film for magnetic tapes.

Claim 31

Dependent Claim 32 words

The polyester film for magnetic recording media according to claim 21, wherein said film has a thickness of 30 to 100 um and is used as a base film for magnetic discs.

Claim 32

Dependent Claim 61 words

The polyester film for magnetic recording media according to claim 21, wherein the number of coarse protuberances having a height of 0.81 u.m or greater on the film surface is 10 or less per 25 cm 2 and the number of coarse protuberances having a height of 0.54 u.m to less than 0.81 u.m is 50 or less per 25 cm2.

Claim 33

Dependent Claim 38 words

The polyester film for magnetic recording media according to claim 21, wherein the average refractive index n of the film and refractive index na in the thicknesswise direction of the film satisfy the following formulae (10) and (11):

Claim 34

Dependent Claim 33 words

The polyester film for magnetic recording media according to claim 21, wherein the spherical silica particles have a specific surface area ratio (R) defined by the following formula (3) of 5.0 or above:

Claim 35

Dependent Claim 75 words

The polyester film for magnetic recording media according to claim 21, wherein the average surface roughness Ra (µm) of the film and the ratio of the maximum height of protuberance Rt (um) of the film to Ra satisfy the following formulae (17) and (18), respectively, and the number of broken protuberances on the film surface is 20 or less per mm 2 : 0.003 ≦ Ra ≦ 0.015 (17) 5 ≦ Rt/Ra ≦ 20 (18)

Claim 36

Dependent Claim 20 words

The polyester film for magnetic recording media according to claim 21, wherein the film is a biaxially stretched polyester film.

Claim 37

Dependent Claim 29 words

The polyester film for magnetic recording mediam according to claim 21, wherein the F s value of the film in the machine direction is 12 kg/mm 2 or above.

Claim 38

Dependent Claim 129 words

A polyester film for capacitors, which contains 0.001 to 5% by weight of fine spherical silica particles obtained by subjecting alkoxysilane to hydrolysis and condensation reaction, said silica particles being substantially amorphous and having an average diameter of 0.01 to 3.0 u.m, the diameter dispersion index of said particles represented by the following formula (1) being in the range of 1.1 to 2.7: wherein d,o is the diameter of the particle when the cumulative number thereof is 10% of the total number of said particles, d 90 is the diameter of the particle when the cumulative number thereof is 90% of the total number of said particles, and d,o and d 90 are measured under an electron microscope, said cumulative numbers being calculated beginning with the largest particle size.

Claim 39

Dependent Claim 129 words

A polyester film for capacitors, which contains 0.001 to 5% by weight of fine spherical silica particles obtained by subjecting alkoxysilane to hydrolysis and condensation reaction, said silica particles being substantially amorphous and having an average diameter of 0.01 to 3.0 u.m, the diameter dispersion index of said particles represented by the following formula (1) being in the range of 1.1 to 2.7: wherein d,o is the diameter of the particle when the cumulative number thereof is 10% of the total number of said particles, d 90 is the diameter of the particle when the cumulative number thereof is 90% of the total number of said particles, and d,o and d 90 are measured under an electron microscope, said cumulative numbers being calculated beginning with the largest particle size.

Claim 40

Dependent Claim 26 words

The polyester film for capacitors according to calim 34, wherein said fine silica particles are the particles comprise 90% by weight or more of silicon dioxide.

Claim 41

Dependent Claim 26 words

The polyester film for capacitors according to calim 34, wherein said fine silica particles are the particles comprise 90% by weight or more of silicon dioxide.

Claim 42

Dependent Claim 59 words

The polyester film for capacitors according to claim 34, wherein said fine spherical silica particles have a volumetric shape parameter defined by the following formula (2): wherein φv is defined as φv = V/D 3 , wherein V is the volume of particle (µm 3 ) and D is maximum projected diameter (µm) of the projection of the particles.

Claim 43

Dependent Claim 26 words

The polyester film for capacitors according to claim 34, wherein the specific resistance in molten state of the film is 2.0 x 10' (Ω·cm) or above.

Claim 44

Dependent Claim 51 words

The polyester film for capacitors according to claim 34, wherein the number of protuberances on the film surface is 1.0 x 10 3 or more per mm 2 , and the difference Ad between micrometric film thickness as measured by 10-ply lamination and gravimetric film thickness satisfies the following formula (19):

Claim 45

Dependent Claim 32 words

The polyester film for capacitors according to claim 34, wherein the fine spherical silica particles have a specific surface area ratio (R) defined by the following formula (3) of 5.0 or above:

Claim 46

Dependent Claim 18 words

The polyester film for capacitors according to claim 34, wherein the film is a biaxially stretched polyester film.

Polyester compositions, process for preparing the same, polyester films, polyester films for magnetic recording media and films for capacitors produced therefrom

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