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JPS4944083

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DESCRIPTION JPS4944083
1, the title of the invention]
Balanced nine reinforced polyethylene terephthalate film
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to polyethylene
terephthalate films and methods of making the same. More particularly, the present invention
relates to a polyethylene terephthalate film with increased tensile strength and a method for
producing the same. More particularly, the present invention relates to a reinforced polyethylene
terephthalate film having a balun EndPage: 1 property and a method of manufacturing the same.
The use of magnetic tapes used in audio, video and computers etc. in the past few years has
increased significantly. In line with this increase in the use of magnetic tapes, carrier films that
deposit magnetic coatings also progress rapidly to pass the stringent requirements of users of
magnetic tapes. Especially 1B film film substrate, to that film! ! It must not be strong enough to
withstand the high speed starts and stops required. In addition the film is also high temperature
Ki? Should have excellent dimensional stability. Furthermore, the film needs to have sufficient
dimensional stability when in contact with the solvent in the coating operation. However, it
should be noted that improving any of these properties will degrade the other properties. Among
the many polymeric films, polyester films, especially polyethylene terephthalate, film, and
illumine, are considered to be excellent polymeric% films for use in magnetic tapes. There are
many reasons for this, but the greatest strength is the extreme strength of polyethylene
terephthalate. However, because of the strict requirements for films used in magnetic tapes,
polyethylene terephthalate has been modified to increase its tensile strength. As a result, a group
of polyethylene terephthalate films, called "tgSsilized" polyester films, is rolled up. These films
generally have a tensile strength of about 88,000 psih or more. Conventional methods (by means
of a reinforced polyester film are certainly needed to make it stronger for magnetic tapes, but it
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is hard to say that other properties are balanced). The strength of the inside (ie, perpendicular to
the direction of travel) is significantly worse. This does not directly mean that the film having the
above-mentioned characteristics is not suitable for practical use, but in the case where the
characteristics of these films are well balanced and in contact with a solvent or high temperature
etc. Results in the loss of dimensional stability.
Deflection of the magnetic coating on the film means distortion of the magnetic coating, which
significantly reduces the efficiency of the magnetic tape as it only leads to rerecording or
reading. It is also well known that reinforced polyester film used in magnetic tape is applied as a
magnetic coating company slurry and is solvent VC # in the coating operation. Furthermore,
these reinforced films are exposed to high temperatures at various stages such as film handling
and solvent removal. Another drawback of conventional reinforced polyester films is that they
have relatively low tensile strength upon elongation. Is magnetic tape Ki in use? I, -t is always
slightly elongated NK. Therefore, in these applications more meaningful evaluations of
polyethylene terephthalate reinforced films are made with tensile sag at elongation rather than
normal tensile strength. The most common tensile strength test at extension is the F6 range. F,
melted 5 means the tensile strength at the time of ring extension. In the conventional method,
the FI 俸 Fi of the well-balanced polynistail film is 15. O o. p81であった。 Although this value
gives satisfactory results, it is an extremely superior film for use with magnetic tape that has an F
@ sensitivity beyond this value. The present invention relates to a reinforced polyethylene
terephthalate film having well-balanced properties, having excellent resistance to polyester film
wear tearing and the like when Fw @ at 54 elongation exceeds 15.000 psjTr. In addition, the
tensile strength of the film of the present invention is higher than that of the conventional strong
polyethylene terephthalate EndPage: 2 lay (the film is different from the tensile strength in the
longitudinal direction of the polyester ester film reinforced only in the longitudinal direction.
Furthermore, the tensile strength of the novel reinforced polyethylene terephthalate film of the
present invention at the 6 superior extension is the tough strength required for the conventional
reinforced polyethylene-reinforced polyethylene / tele 7 thallate film compared to that of the
conventional. It has superior transcendent ability to cope with. Furthermore, the polyethylene
terephthalate film of the present invention is excellent in dimensional stability when exposed to a
high temperature or a solvent as compared with conventional films. According to the present
invention, a polyethylene / terephthalate polymer film is obtained. The film is characterized in
that the tensile strength in the longitudinal and transverse directions both have a balanced
strength of 40.0009 s (more than that). Further, the tensile strength of the reinforced
polyethylene terephthalate 7 thallate film of the present invention when stretched by 5 憾 is both
to, ooopai or more in the longitudinal direction and the transverse direction.
Preferably, the polyethylene terephthalate film of the present invention, which is well-balanced,
has an inherent viscosity of about 0.64 to 0.84 d / l. In another embodiment of the present
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invention, the reinforced polyethylene terephthalate film of the present invention has a tensile
strength in the longitudinal direction and in the lateral direction of ag, ooops 4 or more, and a
tensile strength of 16.5 000 pm4 or more at the time of rolling 5 転 extension. . This film has an
intrinsic viscosity of about 0.60 to 0.70, a shrinkage factor of less than 10%, and a shrinkage
factor of about 8%-8% after standing at 150 ° C for 80 minutes. is there. The invention also
relates to a method of producing a balanced reinforced film according to the invention. Preferred
Method of Carrying Out the Invention-A balanced, reinforced polyethylene terephthalate film is
first stretched in the longitudinal direction, and the stretched film is further stretched in the
transverse direction to be biaxially oriented. Make it excerpt. However, according to the method
of the present invention, unlike the conventional method, the drawing ratio in the transverse
direction is 9 larger than the drawing ratio in the longitudinal direction. According to the
preferred practice, the longitudinal 'stretching ratio is 80-6.0 times its original length, and that of
the transverse direction is 08.2-5.2 times its original width. After the stretching operation in the
z-axis direction, the film is heat-set at 180 ° C.-260 ° C. under tension to make the upper eyelid
balanced and reinforced. The improved film of the present invention is prepared by the
polymerization of bis (2-hydroxy ethyl) terephthalate. Bis (2-hydroxyethyl) terephthalate itself is
produced in either of two different ways. One of them is a method of producing by direct
esterification reaction of bis (2-hydrocoethyl) terethal ヲ tere 7 tar acid with ethylene glycol (for
example, US Pat. No. 8,050,688). In the process, the reaction by-product is water, which is
removed from the reaction product by distillation. The ninety-one methods are dialkyl esters of
terephthalic acid (/ # to dimethyl tele 7 turret)! The process is prepared by transesterification
with 1 mol or about 2 mol or more of ethylene glycol in sonodial. In this reaction, it is preferable
to increase the ratio of ethylene glycol per dialkyl terephthalate, that is, to use 2 moles or more.
By doing so, the first step, the // sesterification reaction proceeds more rapidly and completely.
The esterification is carried out at high temperature (from the boiling point of the reaction
mixture to 250 ° C.), at atmospheric pressure, under 1E 111 or under reduced pressure.
If a portion of the transesterification reaction is used, methanol is removed from reaction
formation. Various known catalysts are favored for promoting the reaction. EndPage: 3 Bis (2hydroxyethyl) terebutrate is prepared and after good conditions this will promote the removal of
ethylene glycol or water, ethylene glycol or the boiling point of the reaction mixture or higher,
and if necessary, only 825 By heating to a temperature of up to ° C., it is converted into a block
copolymer of butylene terephthalate. It is important to reduce the pressure during heating, or at
least at one time during heating, to rapidly remove excess glycol or water, to obtain a preferred
polymerization product. The pressure is reduced gradually. That is, heating is initiated at normal
pressure, continued under reduced pressure, and completed at lower pressure. The final pressure
is preferably i which is about 1-11-1O. A catalyst for the esterification reaction may also be
present as a catalyst for the polymerization reaction. Preferably, the polymerization catalyst is an
antimony trioxide / some h is preferably a fy tymon compound such as an antimono acid, which
accelerates the conversion of bis (2-hydroxyethyl) terephthalate to polyethylene terephthalate
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and is measured in orthochlorophenol Give a polymer having an inherent viscosity [0,8 dec./f or
more, preferably, about 0.4-1.0 dec./f. More preferably, the polyethylenoterephthalate polymer
of the present invention has an inherent viscosity of about 0.62 to about 9 deciliter / l. The
heating of the polymerization reaction should be carried out under conditions that prevent
oxidation, ie, in the absence of any trace amount of oxygen. And, usually, inert gas such as
nitrogen, carbon dioxide, etc. is melted through the upper part of the melt 0 or "." The viscosity of
the melt gradually increases during heating and polymerization. Therefore, it is necessary to keep
the polymer at a sufficiently high temperature so as to always keep the molten 1ik throughout
the heating period. Heating takes place over the required property values and is continued until a
melt is obtained which can form a film whose melting point exceeds about 240.degree. C.,
preferably above 260.degree. When heating is complete, the product is used for film or other
production, or is taken out of the reaction vessel in the molten state and shaped into blocks,
chips and the like. The molten polyethylene / terephthalate polymerization product is extruded
through a die onto a chilled polishing gearing roll to form a polyethylene terephthalate film.
Thereafter, the amorphous film of the source is biaxially oriented by stretching in the
longitudinal direction and the transverse direction.
In the preferred practice, the film is stretched 8.0-6.0 times its original length in the length
direction. That is, it means that the ratio of the stretched film to that before stretching is 8.0: 1 to
5.0: 1. More preferably, the ratio is about 3.6: 1 to t5: 1. More preferably, the cast, i.e., iamorphous film is stretched longitudinally at a stretch ratio of 8.8: 1 to 4.2: 1. The preferred
stretching temperature is about 70 ° C to 100 ° C. More preferably, it is about 80785 ° C. In
the unique method of the present invention, it is carried out after stretching in the transverse
direction. Unlike the prior art methods, the transverse draw ratio is greater than that of the
longitudinal direction h0 In a preferred practice, the transverse draw ratio is about 8.2: 1 to 5 J:
1. Of course, the ratio is limited by the need for the transverse draw ratio to be greater than that
in the longitudinal direction. More preferably, the transverse draw ratio is about 8.7: 1 to 4.7: 1.
More preferably, this ratio is about 4.0: 1 to 4.4: 1. Also, the temperature at the time of
transverse stretching is about 90 to 11 ° C, more preferably about 96 to 110 ° C. After
longitudinal and transverse stretching and biaxial orientation of the film, the film is heat set
under elongation to further promote crystallization. In the preferred practice, the heat setting
temperature is about 180-250 ° C. Preferably about 180 ˜! ! It is 80 ° C, more preferably about
185-196 ° C. EndPage: 4 Polyethylene terephthalate capable of producing the balanced
reinforced film of the present invention is a high molecular weight polymer. In a preferred
embodiment, the polyethylene terephthalate polymer melt has an intrinsic viscosity of about 0.7
to 0.9 d / l, as measured in orthochlorophenol at 26 ° C. According to another preferred
embodiment, the intrinsic viscosity of the polyethylene terephthalate melt is about 0.61a-0.72. As
is well known, intrinsic viscosity 1 is commonly used as a measure of the molecular weight of the
polymer. It should also be noted that the intrinsic viscosity of the formed film is usually lower
than the intrinsic viscosity of the melt from which it was made. A balanced reinforced
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polyethylene terephthalate film is obtained by the above method. The polyethylene terephthalate
film of the present invention has an inherent viscosity of about 0.60 to 0.80 dllt as measured in
5C 26C orthochlorophenol, which also depends on its raw material, solid I gate 1 of Limer I.
In a preferred embodiment, the inherent viscosity is about 0.64 to 0.80 dl / y. More preferably,
the value is 0.66 to 0.70 di / v. In another preferred embodiment, the intrinsic viscosity of the
baled reinforced polyethylene terephthalate is about 0 JO-0,70. The polyethylene terephthalate
film of the present invention described in agriculture has a high strength. In the preferred
embodiment, the tensile strength is at least 40.000 jlss in both the longitudinal and transverse
directions. And in fact, it is about 40.000-50.00 (H + st or more). In addition, the tensile strength
at the time of 5 engagement extension in both directions is about 20.000 pm 4 or more.
Preferably, the [is about 20,000 to 26. 0001 at. The breaking elongation of the present invention
is about 50 to 601 G in both directions. The modulus of the polyethylene terephthalate melt is
600,000 p1 <or more in both directions. More preferably, it is about 650.000 to 800.000 F # i.
In another embodiment of the present invention, it is also possible to slightly reduce the degree
of pull by a slight degree so that the balanced contraction rate is extremely reduced. The intrinsic
viscosity of the polyethylene terephthalate melt used in this practice is about 0.62 to 0.72, and
that of the resulting film is O, SO to 0.70. Also this film's tension strength is about 詔, oo in both
directions. The tensile strength in both directions at 5 憾 extension is about 16.000 pajμ. The
contraction rate is about 8 to 8 in both directions. The invention will now be illustrated by means
of the following examples, but the invention is not limited thereto. EXAMPLE 1 A castery /
gaging drum maintained at 25 ° C. is a polyethylene terephthalate melt which has been
prepared according to the method described above and has an inherent viscosity of 0.75 deciliter
per gram (measured in 25 ° C. orthochlorophenol enol). The amorphous dye was extruded
through the dyestuff of Stretch the film in the length direction between the upstream and
downstream ports, and rotate the speed of the lower roll above the upstream roll so that the
length extension in the length direction is 40 times the unstretched length. The The film was held
at about 85 ° C. during the longitudinal stretching step. After the longitudinal stretching step,
the film was heated to 90 ° C. and stretched transversely in the chatter. The chamber was held
at 100 ° C. and the film was stretched laterally 4.2 times its original width.
After stretching in the transverse direction, the biaxially oriented film was crystallized at high
temperature while maintaining tension. That is, the film was held and heated to the chaff 7 even
if no stretching occurred during the heat treatment. The temperature to which the film is
subjected at this heat setting step was EndPage: 5180 ° C. The physical properties of the
polyethylene terephthalate / terephthalate film produced according to the method of the present
invention were measured. The tensile strength in the longitudinal direction was 4 & 400 psi, and
the tensile strength in the lateral direction was 4 & 400 js <. The tension strength of the film is
perfectly balanced as a force. The tensile strength at 5 憾 extension in the longitudinal direction
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was 2o, ooop 8i. Tensile strength f (Fs) at the time of 5 憾 extension in the lateral direction! !
1.800paiであった。 The breaking elongation was 60 spit in the longitudinal direction
and 54 in the lateral direction. The intrinsic viscosity of the film measured in orthochlorophenol
at 26 ° C., which was 676.000 jsi in the longitudinal direction and in the lateral direction, and
684,000 pai, respectively, was 0.68 d / g. EXAMPLE 9 A second polyethylene / terephthalate
film is prepared from the same polyethylene terephthalate polymer melt from which the film of
Example 1 was formed. The melt having an intrinsic viscosity (175 d / g) was biaxially oriented
as in Example 1. In this example, the crystallization temperature is maintained at 186 ° C. from
180 ° C. in the case of Example 1 and circled. The physical properties of this film were as
determined in Example 1 as in Example 1. The tensile and tensile strengths of the polyethylene
terephthalate film in the longitudinal and transverse directions are 46,000 and 47.700 'p # i,
respectively, and the tensile strengths at the time of the extension in the longitudinal and lateral
directions of 6 and 7 are respectively * Zo, ooopai and 2zloopsi. Longitudinal eyebrows and
transverse rupture stretches were 58 sounds and 64 abbreviations, respectively. The longitudinal
modulus is 662.000 jlaj>! And the lateral no-modulus is nine in the 762.000'pa4. The intrinsic
viscosity of the final produced film was 069 d / g, measured in 2 g ° C orthochlorophenol. The
above two examples show that it is a highly reinforced polyethylene terephthalate film having
significantly balanced properties compared to conventional reinforced polyethylene
terephthalate films. The best reported example of a high molecular weight polyethylene
terephthalate film shouldering high tensile properties in two vertical directions would be US
Patent 8,482,691.
In this patent it is stated that the film has a tensile property of more than 40,000 pai. In
particular, Table X shows that Filml has a tensile strength in the longitudinal direction of 4α 000
pai and a tensile strength in the transverse direction [−4 I 44 60 60 psi. Judging from these b
values, this film is said to be balanced, but the film of the present invention is said to be much
more balanced. Also from the above fact, this patent seems to be aimed at a film with improved
strength in the thickness direction (direction perpendicular to both the longitudinal and
transverse directions). Another patent for reinforced polyethylene / terephthalate fil is US Patent
8,897,072. This patent describes a polyethylene / terephthalate reinforced film with a tensile
strength in the machine direction of greater than 40,000. However, this reinforced film is
distinguished from that of the present invention by the fact that its transverse strength is
extremely low (i.e., the tensile strength is 18.000 Fat5). That is, this film is characterized by being
unbalanced. Equally important is that the reinforced film of the present invention has a balanced
tensile strength of 20.0005 '# (or better) at 54 elongation. Patent US Pat. No. 8,482 for claiming
balanced tensile strength at the time of six-row extension. , 691 exist. See Table X again.
EndPage: 6 shows that the two samples of Film 1 and Film 3 are balanced in tensile strength at 6
憾 extension, but both s4 extension s4 extension 11)! ! The strength is smaller than wu 20-000
pat. U.S. Pat. Nos. 8,461,199 and 8,165,499 describe a 20.000 ps tensile strength at 5 憾
elongation (more than a strength-modified polyethylene terephthalate film). However, it is
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difficult to say that these films have a tensile strength at the time of elongation at 5 の み of only
ff1O, 0002 s (more than 虱 / − − − −). Example ■ Example of polyethylene terephthalate of
intrinsic viscosity 0.70 in orthochlorophenol prepared at 26 ° C as described above! Two rings
were stretched like. The film was then crystallized by exposure to 206 ° C. and temperatures
under tension. The reinforced film superior by this method has a proper term '[0, 66,-tensile
strength in the direction of swearing and in the lateral direction is 40,000 pai and sy, 5 oopsj].
In addition, the longitudinal and lateral tensions at the 6 憾 extension were 9,900 psi and 16,800
p * << respectively. The contraction rate after holding for 150 minutes at 150 ′ tl: is 4.6 り in
the lengthwise direction, and in the horizontal direction. It was 4.01 in the monkey. Films
produced according to US Pat. No. 8,482,591 show greater shrinkage as summarized in Table-X
(film 1) and it is clear that they are not balanced compared to the films of the side layers is there.
The present invention has been described above by the examples. It is a matter of course that
these improvements or variations are the present invention OIl! The present invention is not
limited by this embodiment. The embodiment and the details of the present invention are as
follows. 1, A tensile strength of 40,000 psi or more in both longitudinal and transverse
directions, and a tensile strength of 20,000 psi or more at 5 憾 elongation in both longitudinal
and transverse directions, balanced in biaxial orientation Polyethylene terephthalate film. 2
Intrinsic viscosity 0.64 to 0.80 dllt t, b a film of paragraph 1. The film according to claim 2,
wherein the tensile strength in the longitudinal direction and the transverse direction is about
40,000 to 50,000 pg <and the tensile strength in both directions at the time of 6-width
elongation is about 20,000 to 25,000 ps. 4. The film according to claim 2, wherein the intrinsic
viscosity is about 0.68 to 0.70 dllt. 6, The film according to claim 2, wherein the longitudinal and
transverse moduli exceed 600,0001 si. 6, the breaking extension rate is 6 (l in both the
transverse direction and the longitudinal direction, and now the sixth film. 7, Longitudinal and
lateral tensile strength of the paper, about oo. or less, tensile strength at 5% elongation in both
longitudinal and transverse directions is about 16,000 pgj or more, j? a biaxially oriented wellbalanced polyethylene terephthalate film characterized in that the shrinkage ratio at 80 ° C. for
150 minutes at 150 ° C. is about 8 to 8 in both directions. 8. "7 + 7) film with an intrinsic
viscosity of about 0.60-0.70 dllt. Extrude the polyethylene terephthalate film from the die
according to the method for producing a 9.2 axis-oriented balanced polyethylene terephthalate
film: cool the melt on a casting drum to form a polyethylene terephthalate film; EndPage: 7 The
film is stretched in the lengthwise direction so that the ratio of the length after stretching to the
length before stretching is about & O: 1-5.0: 1; the film stretched in the lengthwise direction is
stretched in the transverse direction The ratio of the width after stretching to the width before
stretching is about [2: l-6, 2: 1 (in this case, the ratio of after stretching to during stretching in
the lateral direction is the length after stretching in the lengthwise direction and before
stretching Stretched to a ratio greater than the length) to form a biaxially oriented film: and heat
setting the biaxially oriented film under tension at a temperature of about 180 ° C. to 250 ° C
.: each The Wherein the consisting-up.
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The method of Claim 9 wherein 1 G, the extruded melt has an inherent viscosity of about 0.62 to
0.90-dVt. 11. The film has a stretch ratio relative to the lengthwise direction of 8, 5: 1 to 4 J): a
stretch ratio relative to 11 of the lateral direction of 8, 7: 1 to 4, 7: 1 (in this case, the lateral
direction stretch ratio) The method according to claim 9, wherein the film is stretched at about
180 ° C. to 280 ° C. in a method of drawing in which 12, stretch in the longitudinal direction
at a stretch ratio of 8.8: 1 to 4.2: 1 and then in the transverse direction at a stretch ratio of 4.0: 1
to 4.4: 1 (where the transverse stretch ratio The method of paragraph U wherein the heat is fixed
at a temperature of 186 ° C. to 195 ° C. under tension, which is large compared to the draw
ratio in the longitudinal direction. % Pertinent Applicants Celanese, シ ョ / シ ョ Attorney, 瀬 代
理人 Attorney Attorney Takano Yoshino 6, List of attached documents (1) 1 statement (2) power
of attorney and 1 translation each (3) priority certificate Honors and Translations 1- each 7
inventors, inventors and agents other than the above (1) Inventors address United States of
America South Carolina Spatanbound Lake Drive Route 3 Names William, Barry, Mody (2) Agent
Name Patent Attorney (6706 ) Takano Yoshino-EndPage: 8
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