JPS59221354A - Oriented polyester film - Google Patents

Abstract

PURPOSE:To manufacture an oriented polyester film having excellent surface flatness and slippery as well as adhesivity, by using a polyester containing a specific inner particle source and a higher fatty acid compound. CONSTITUTION:The objective oriented polyester film having a surface roughness Ra of 0.003-0.025mum and a static friction coefficient mus of 0.10-0.70 is prepared from a polyester composed of (A) 100pts.wt. of a polyester, (B) 0.001- 1pt.wt. of inner particles or inert particles having an average particle diameter of 0.1-3mum and (B) 0.005-2pts.wt. of a metallic salt or a partial metallic compound composed mainly of a 18-33C higher fatty acid monocarboxylic acid or a higher fatty acid amide composed mainly of a 18-33C compound. The inner particle is the particle produced by the bonding of the component of the polyester with the Ca, Mg and/or Li compounds added to the reaction system in the synthesis of the polyester.

Description

DETAILED DESCRIPTION OF THE INVENTION [Technical Field of the Invention] The present invention relates to an oriented polyester film containing fine particles and having excellent surface flatness, slipperiness, and adhesiveness. More specifically, Catalyst 1 used during polyester synthesis
Part or all of the coloring inhibitor etc. is precipitated during the synthesis reaction process. So-called internal particles and/or inert particles, and finely dispersed particles containing specific amounts of metal salts of specific higher fatty acids and/or amide compounds of higher fatty acids. The present invention relates to an oriented polyester film that simultaneously satisfies specific ranges for surface roughness (Ra) and static friction coefficient (CμB), and has excellent adhesive properties.

[Prior art]

In recent years, oriented polyester films have made remarkable progress in fields such as magnetic recording media such as magnetic tapes and magnetic disks, capacitors, photographs, microfilms, and packaging.

In each application of this oriented polyester film, 9
Strict surface control is required. In other words, for magnetic recording media such as magnetic tapes and magnetic disks, '!' is used to prevent recording disturbances. ! Ta. Also for capacitors to prevent insulation defects.

The surface of oriented polyester film needs to be flat for use in photography and microfilm to prevent image quality from being disturbed, and for packaging to not impair transparency and aesthetics.

In addition, common to all of these applications, 9 workability and quality issues are required both during unwinding, processing, winding, and slitting when commercializing products for those applications, and when using them after commercialization. From both sides, the surface of the polyester film needs to be slippery.

Sweet. Smoothness is an important property when forming an oriented polyester film from the viewpoint of stable and economical production with less tearing. However, the long-awaited flatness and smoothness of the surface are inherently contradictory properties. In other words, it is extremely difficult to satisfy both properties at the same time; if flatness is prioritized, smoothness must be sacrificed to some extent; on the other hand, if smoothness is prioritized, flatness must be sacrificed to some extent.

Conventionally, the following technologies have been proposed for the purpose of achieving both flatness and smoothness.

(2) A method in which part or all of the catalyst 1 color inhibitor used during polyester synthesis is precipitated during the reaction process and present on the film surface as fine particles.C (hereinafter referred to as internal particle generation method).

■ Method of adding inert particles to the polyester synthesis reaction system such as titanium dioxide, talc, kaolinite, calcium carbonate, silicon oxide, etc. C (hereinafter referred to as external particle addition method) 0 ■ Combination of ■ and ■ ■ Neutral or partial A method of adding neutralized montan wax salt or montan wax ester salt (JP-A-56-139551) and a method of adding an ester product (JP-A-57-195143). Below C,
(referred to as organic lubricant addition method).

However, the oriented polyester film by such conventionally proposed technology is

(2) In the internal particle generation method, there are many coarse particles mixed in, probably due to the strong cohesive force between the nine particles, and the coarse particles deteriorate the flatness of the film surface.

Furthermore, it has the disadvantage of insufficient lubricity.

(2) The external particle addition method has the disadvantage that it is not possible to achieve both flatness and slipperiness because secondary agglomeration of the 9 particles, roughness of the average particle size, and inclusion of coarse particles are unavoidable.

■ Even if the internal particle generation method and the external particle addition method are used together, the drawbacks of each cannot be overcome.

■ Among organic lubricant addition methods, JP-A-56-13955
In the technique of Publication No. 1, the organic solvent bleeds out onto the film surface.

It has the disadvantage of lacking lubricity, and was published in JP-A-57-1951.
In the technology of Publication No. 45, if an organic lubricant is added at the time of polymerization, it will gel, and if it is added to the raw material after polymerization (or later added to the raw material after polymerization), it will not be added during melt extrusion. All have the disadvantage that satisfactory surface properties (flatness, smoothness) cannot be obtained because the viscosity drops rapidly.

Even if any of these films were used to make a magnetic tape, there was a drawback that the running properties of the magnetic tape and the electromagnetic conversion characteristics could not be achieved at the same time.

[Purpose of the invention]

The object of the present invention is to provide an oriented polyester film that does not have the above-mentioned drawbacks, that is, is excellent in all of the following six properties: surface flatness, smoothness, and adhesion.

[Structure of the invention]

The present invention uses 100 parts by weight of polyester.

A. 0001 to 1 part by weight of inert particles having internal particles or an average particle size of 01 to 6 μm.

B, at least one metal salt or partial metal salt compound of a compound whose main component is a higher fatty acid monocarboxylic acid having 18 to 66 carbon atoms, or C, whose main component is 18 to 66 carbon atoms;
Contains 0.005 to 2 parts by weight of higher fatty acid amide of ~36, and has a surface roughness Ra of 0.0 [13
~0,025μm, static friction coefficientμday is 0.10~0,7
The film is characterized by an oriented polyester film having an orientation of 0.

The polyester in the present invention is a polyester containing an aromatic dicarboxylic acid as a main acid component and an alkylene glycol as a main glycol component.

Specific examples of 6-aromatic dicarboxylic acids include terephthalic acid,
Isophthalic acid, naphthalene dicarboxylic acid.

Diphenoxyethane dicarboxylic acid, diphenyl dicarboxylic acid, diphenyl ether dicarboxylic acid.

Diphenylsulfone dicarboxylic acid, diphenylketone dicarboxylic acid, anthracene dicarboxylic acid.

α,β-bis(2-chlorophenoxy)ethane-4,4
'-dicarboxylic acids and the like. Among these, terephthalic acid is particularly desirable.

Specific examples of alkylene glycol include ethylene glycol, trimethylene glycol, tetramethylene glycol, pentamethylene glycol, hexamethylene glycol, hexylene glycol, and the like. Among these, ethylene glycol is particularly desirable.

Of course, these polyesters may be homopolyesters or copolyesters (copolymerized polyesters), and examples of copolymerized components include diethylene glycol, propylene glycol, neopentyl glycol, polyalkylene glycol, p -xylylene glycol, 1,4-cyclohexanedimethanol. Diol components such as 5-sodium sulforesorcin.

Adipic acid, sebacic acid, phthalic acid, isophthalic acid, 2
．． Examples include dicarboxylic acid components such as 6-naphthalene dicarboxylic acid and 5-sodium isophthalic acid, polyfunctional dicarboxylic acid components such as trimellitic acid and pyromellitic acid, and oxycarboxylic acid components such as p-oxyethoxybenzoic acid.

It should be noted that, of course, known additives such as antistatic agents, heat stabilizers, and ultraviolet absorbers may be added to the polyester in amounts that do not impair the effects of the present invention.

The internal particles in the present invention are particles produced by the combination of at least one compound among calcium compounds, magnesium compounds, and lithium compounds added during polyester synthesis and components constituting the polyester.

Note that the internal particles of the present invention may contain elemental phosphorus and trace amounts of other metal components, such as zinc, cobalt, antimony, germanium, titanium, etc., to the extent that the effects of the present invention are not impaired. .

An example of a method for measuring the content of internal particles will be explained.

Wash the polyethylene terephthalate thoroughly with methanol to remove surface deposits, wash with water 1~, dry, and add 300 g (
D Sample Ko - Add 2.7 bags of chlorophenol and raise the temperature to 100°C while stirring, and after raising the temperature, continue to heat for 1 hour.
1. So-called it is released and the polyethylene terephthalate partial tone m is interpreted. However, if the polyethylene terephthalate portion does not dissolve, such as when it is highly crystallized, the above-mentioned dissolution operation is performed after melting and quenching.

Next, coarse insoluble materials such as dust contained in PolyT and Cilente 7/phthalate are separated and removed using a G-1 glass filter, and the weight of this furnace material is subtracted from the sample weight.

Hitachi Separation Ultracentrifuge ADp type rotor J (P)
After injecting 30Ω of the solution after separating the glass 9-filter into each cell 9, turn the rotor 4
After rotating at 5.0 rpm and confirming that there are no rotation abnormalities, the rotor is evacuated and the rotor is rotated to 30,000 rpm.
The rotation speed is increased to 1, and the particles are centrifuged at this rotation speed.

Separation is completed after approximately 40 minutes, and this can be confirmed, if necessary, by checking that the light transmittance of the liquid after separation at 375 mμ becomes a constant value higher than that before separation.

After separation, the two-layer liquid is removed by decanting to obtain separated particles.

Separated particles may contain polyester components due to insufficient separation, so the collected particles may be heated to zero at room temperature.
- After adding chlorophenol and suspending it almost uniformly, perform the ultracentrifuge treatment again.

This operation must be repeated until a melting peak corresponding to the polymer can no longer be detected by drying the particles, which will be described later, and then subjecting them to full-scanning differential calorimetry analysis of the core particles. Finally, the thus obtained separated particles are vacuum dried at 120'c for 16 hours and weighed.

Note that the separated particles obtained by the above operation contain both internal particles 10- and external particles. For this reason, it is necessary to determine the amount of internal particles and the amount of external particles separately. First, quantitative analysis of the metal content of the separated particles is performed to determine the amount of Ca, Li, etc.
The content of metals other than Ca and Li are determined in advance. Next, the separated particles are heated under reflux for 6 hours or more in 3 times the molar amount of ethylene glycol, and then the ethylene glycol is distilled off to a temperature of 200° C. or higher for depolymerization, so that only the internal particles are dissolved. The separated particles obtained by centrifuging the remaining particles are dry-weighed and taken as the external particle amount, and the difference from the initial total separated particle amount is taken as the internal particle amount.

In addition, in order to confirm whether the depolymerization has been completely carried out, the separated particles after depolymerization are quantitatively analyzed for metal content, and by repeating these operations, the accuracy of particle amount measurement can be improved.

In the present invention, the inert particles are chemically inert particles selected from oxides or inorganic salts of elements of Groups I, I, and IV of the Periodic Table of the Elements.

For example, calcium carbonate, wet silica (silicon dioxide), dry silica (silicon dioxide), aluminum silicate (kaolinite), barium sulfate, calcium phosphate, which can be obtained synthetically or naturally.

Examples include talc, titanium dioxide, aluminum oxide, aluminum hydroxide, calcium terephthalate, and calcium silicate. The average particle size of the inert particles is 0.
Must be 1 to 6 μm.

Preferably it is 0.1 to 2 μm. If it is less than 0.1 μm, the film has insufficient lubricity; if it exceeds 9.6 μm, the film has poor flatness.

In addition, removal of coarse particles and particle size adjustment of inert particles are performed in step 1.
Various methods 1 can be carried out, for example, air classification, pulverization and/or classification treatment methods such as natural sedimentation, centrifugal sedimentation, and sand mill pulverization as an ethylene glycol slurry or water slurry.

In the present invention, it must contain at least one of the above-mentioned amount of internal particles or the above-mentioned inert particles. In the case of only either internal particles or inert particles, the content is o, o, based on 100 parts by weight of polyester.
Must be oi~1 part by weight, preferably 001~
It is 0.5 part by weight.

In addition, if it contains both internal particles and inert particles, 1
The total content of both is 0.001 to 2 parts by weight, preferably 0, OO2 to 1 per 100 parts by weight of polyester.
Parts by weight are preferred. If the content is less than the lower limit of the above range, the coefficient of friction between films or between films and metal will increase, resulting in poor lubricity; on the other hand, if the content exceeds the upper limit of the above range, , the generation of coarse particles increases, 9 surface roughness increases, and flatness deteriorates. If a magnetic tape is made using a film with a content outside the appropriate range as described above, running properties and electromagnetic conversion characteristics will not be compatible.

The metal salt compound or partial metal salt compound C of a compound consisting of a higher aliphatic monocarboxylic acid having 18 to 36 carbon atoms as a main component in the present invention.

Specific examples of higher fatty acid metal salt compounds include stearic acid, nonadecanoic acid, and arachidic acid.

Examples include carnaubic acid, lignoceric acid, cerotic acid, montanic acid, petroselic acid, oleic acid, erucic acid, linoleic acid, and acid mixtures containing these, and metal species include alkali and /''!.

Bamboo alkaline earth metals such as lithium, potassium, barium, magnesium, calcium,
Examples include strontium, and particularly preferred compounds include magnesium stearate, calcium montanate,
Examples include sodium montanate and sodium erucate.

Here, the term "main component" refers to a composition containing 800 parts by weight of the compound.

In addition, if the fatty acid of the higher fatty acid metal salt compound has less than 18 carbon atoms, bleed-out to the film surface will be severe and the adhesion will be extremely poor, and if the number of carbon atoms exceeds 63, lubricity will not be obtained. .

The content of the higher fatty acid metal salt compound is as follows: polyester 1
It needs to be 0.005 to 2 parts by weight, preferably 001 to 1 part by weight.

More preferably, ld is 0.05 to 0.5 parts by weight. If the above content is less than 0.005 parts by weight, the flatness and slipperiness of the film will hardly be obtained, and if it exceeds 2 parts by weight, bleed-out to the film surface will be severe and the adhesion will be significantly poor. Put it away.

In the present invention. Higher fatty acid amide is a higher fatty acid amide whose main component has 18 to 33 carbon atoms, and specific examples include stearic acid amide, oleic acid amide, erucic acid amide, and behenic acid amide, and in particular,
Erucic acid amide is preferred. Here, the main component refers to a product containing 800 parts by weight of higher fatty acids having 18 to 3 carbon atoms. In addition to the above specific examples, substituted fatty acid amides may be represented by the general formula [wherein R1 is an alkyl, alkenyl or cycloalkenyl group, and R2 is H or an alkyl group].

R□ may contain an alkyl group, R1 as well as an R, trioxy group or an alkoxy group. however.

A compound having a total number of carbon atoms of 18 to 63 may be used. Specific examples include acetic acid-N-stearylamide, propionic acid-N-methyl-N-stearylamide, and the like.

When the number of carbon atoms in the fatty acid is less than 18, bleed-out to the film surface is severe and the adhesion is extremely poor, while when the number of carbon atoms exceeds 35, the adhesiveness cannot be obtained.

The content of the higher fatty acid amide needs to be 0.005 to 2 parts by weight, preferably 0.01 to 1 part by weight, based on 100 parts by weight of the polyester.

More preferably, it is 0.05 to 0.5 part by weight.

If the content is less than 0.0 parts by weight of O5, the flatness and slipperiness of the film will be poor, and if it exceeds 2 parts by weight, bleed-out to the film surface will be severe and the adhesiveness will be poor.

In the present invention, unless at least one of the above-mentioned higher fatty acid metal salt compound and the above-mentioned higher fatty acid amide is contained in a specified amount, the effects of the present invention will not be exhibited, and the running properties when made into a magnetic tape will be The electromagnetic conversion characteristics are no longer compatible. In addition, when containing both a higher fatty acid metal salt compound and a higher fatty acid amide, the total content of both is 0.005 to 25 parts by weight per 100 parts by weight of polyester.
The amount is preferably 0.002 to 1 part by weight.

As mentioned above, the oriented polyester film of the present invention is as follows.

(A) internal particles (hereinafter referred to as C), simply referred to as ■) or inert particles (hereinafter referred to as C, simply referred to as ■); and (B) higher fatty acid metal salt compounds (hereinafter referred to as C, simply referred to as ■)). and particles c or less in the above A term.

(simply referred to as particle source (A)) and inclusions C and below in section B.

It is necessary that both of them (simply referred to as higher fatty acid compound (B)) be contained. If only the particle source (A) or only the higher fatty acid compound (B) is contained, the effects of the present invention will not be exhibited. In other words, it is an oriented polyester film containing a specific amount of one particle source (A) and a higher fatty acid compound (B), and having a specific surface roughness and coefficient of static friction. Preferred particle source (A).

-1;'- The combinations of higher fatty acid compounds CB) are ■10■10■, ■+
■Ten+■, ■ten■, ■ten■, ■+■ (here,
10” means to be used together).

The reason that both the 9-particle source (A) and the higher fatty acid compound (B) must be contained is that the higher fatty acid compound (B) is ultrafinely dispersed in the 1-particle source (A) in the polyester. This is because there is a reciprocal effect.

The surface roughness Ral in the present invention is measured by the method described below, and its range is 0. It needs to be OO3 to 0.025 μm, preferably 0.005 to 0.023 μm.

More preferably, it is 0,005 to 0.005 μm, most preferably 0,005 to 0.014 μm. If the surface roughness (Ra) is less than 0.003 μm, it will be too flat and scratches will easily occur. On the other hand, when Ra exceeds 0.025μ, flatness is poor. If Ra deviates from the preferred range as described above, the magnetic tape u,'x magnetic conversion characteristics and runnability are not compatible with each other using the film.

The static friction coefficient cμB) in the present invention is measured by the method described below in 18-1, and its range is as follows:
Must be between 010 and 070, please select ' [0,
20-0.60. Favorable to f L < u mouth, ro 0-0
It is 55.

If the static friction coefficient (μs) is less than 0.10, loose winding occurs during operation. On the other hand, if it exceeds 0.70, lubricity is insufficient and high-speed running performance during processing deteriorates.

In the present invention, the film must be oriented. If it is not an oriented film, it will be difficult to keep both the surface roughness and the coefficient of static friction within the above ranges, and the thickness unevenness and rigidity 1-dimensional stability will be fatally poor. Forms of orientation include -axis orientation, biaxial orientation, etc.

Although any known orientation format can be selected, a biaxial orientation format is preferred. The degree of orientation is 1-plane birefringence Δn7 in the case of -axis orientation.
5EO~0. ．． 15, preferably [the sum of the 0, 0, and 10° in-plane refractive indices is 3.2 to 3.42, and the thickness direction refractive index ratio is desirably 0.935 to 0.980. The in-plane birefringence Δn here refers to the refractive index in the vertical direction, horizontal direction, and thickness direction of the film measured at 25° 0.65% RH with an Atsube refractometer using sodium D line. It is the absolute value of the difference between the refractive index in the vertical direction and the horizontal direction, and it is also the sum of the in-plane refractive index and the sum of the refractive index in the vertical direction and the refractive index in the horizontal direction, which is 1 dimension. The refractive index in the thickness direction is the ratio of the refractive index (p) in the thickness direction of the film to the refractive index (Q) in the thickness direction of an amorphous film that is rapidly cooled in 10"C water after melt-pressing the film. .

In other words, (P) / (Q). If the degree of orientation deviates from the above-mentioned preferred range, it is undesirable because it becomes difficult to achieve both flatness and lubricity of the film, and it becomes difficult to achieve both runnability and electromagnetic conversion characteristics of a magnetic tape using the film.

The thickness of the film of the present invention is preferably 3 to 125 μm, preferably 4 to 80 μm, and more preferably 4 to 70 μm.

The film of the present invention has a surface tension (γC) of 9.

A range of 50 to 60 d, yne/cm is an important range in terms of improving slipperiness and adhesion.

It is desirable to provide a magnetic layer on at least one side of the film of the present invention to form a magnetic recording medium. This magnetic layer is a well-known magnetic layer made of γ-Fe20. , Co-doped γ-
Powdered magnetic material such as Fe, O, Cry, or ferromagnetic alloy is dispersed in an organic binder and
A magnetic layer formed by a method of coating Fθ, Go, Ni and other ferromagnetic metals or magnetic alloys containing them in a thickness of 10 m by a method such as FC, vacuum evaporation, sputtering, ion blating, electroplating, etc. Although any magnetic layer formed with a thickness of 10 DO nm may be used, it is preferable to provide the latter magnetic layer in order to advantageously exhibit the effects of the present invention and improve the accuracy of the magnetic recording medium.

Next, a summary of the method for manufacturing the oriented film and magnetic recording medium of the present invention will be described. However, it is not limited to this.

For simplicity, explanation will be given using polyethylene terephthalate as an example of polyester.

(1) Method for producing oriented film: First, the method for producing internal particles will be described. The internal particles are produced through the process of ■ polycondensation through direct esterification of terephthalic acid and ethylene glycol 21- or ■
In the process of polycondensation through the transesterification reaction of terephthalic acid with dimethyl terephthalate and ethylene glycol, "I-soluble calcium compounds,
At least one of a magnesium compound, a manganese compound, a lithium compound, and preferably a phosphorus acid and/or
! It is produced by adding a bamboo ester compound in an appropriate manner. The addition of the compound for producing internal particles starts from the point at which the esterification reaction or transesterification reaction is substantially completed and starts the polycondensation reaction! Calcium compounds,
It is preferable to add at least one lithium compound to the reaction system as a glycol solution.

Calcium and magnesium can be used here.

Compounds of manganese and lithium include halides,
Inorganic acid salts such as nitrates, sulfates, and acetates.

Organic acid salts such as oxalates and benzoates, and glycol-soluble compounds such as hydrides and oxides are most preferably used, but two or more of them may be used in combination.

In addition, phosphorus compounds include phosphoric acid and phosphorous acid.

Phosphonic acid and one or more of these esters are used.

Next, a method for adding inert particles and higher fatty acid compounds will be described. These may be added at any time before the polymerization reaction of polyethylene terephthalate, during one polymerization reaction, and once after the completion of the polymerization reaction during melt extrusion molding. However, in the case of inert particles, the special It is preferable to add a slurry dispersed in ethylene glycol or ethylene glycol before or during the polymerization reaction.

In order to improve the 9-dispersibility of the higher fatty acid compound, among the methods described in 2., the method of adding the higher fatty acid compound during the 9-polymerization reaction is particularly important.

2. In the present invention, polyethylene terephthalate containing internal particles or inert particles is separately produced and kneaded with a higher fatty acid compound in a melting process, or internal particles and/or crushed inert particles and higher A method of diluting a highly concentrated mask containing a large amount of fatty acid compounds with polyethylene terephthalate is also widely adopted.

Thus, polyethylene terephthalate containing a specific particle source (7V) and a specific amount of higher fatty acid compound CB) is melt-extruded in an extruder, cast into a sheet, and stretched and oriented using a well-known method. The stretching method is not particularly limited, but examples of uniaxial stretching methods for obtaining a -axis orientation include vertical stretching in one direction using rolls and horizontal stretching in one direction using clips. Examples of biaxial stretching methods to obtain a biaxially oriented format include simultaneous biaxial stretching, vertical→horizontal, vertical→
Horizontal → Vertical, Horizontal → Vertical, 2nd vertical → Horizontal, 2nd vertical →
Examples include horizontal → vertical, 2-stage vertical → horizontal → 2 axes at the same time.

Then, if necessary, heat treatment is performed while providing appropriate relaxation.

Then, if necessary, at least one side is subjected to well-known corona discharge treatment, plasma treatment, etc., and then wound up.

(2) Method for manufacturing a magnetic recording medium: The above-mentioned magnetic layer is formed on one side of the oriented film obtained as described in Section 2 to produce, for example, a magnetic tape.

[Effects and uses of the invention]

The oriented polyester film of the present invention has internal particles and/-! l: inert particles having a specific average particle size;
It is characterized by containing a specific amount of a specific higher fatty acid metal salt and/or a specific higher fatty acid amide, respectively, and having a surface roughness and a coefficient of static friction within specific ranges. It has the effect of being both excellent in lubricity.

At the same time, it has the effect of having excellent adhesion to metals such as aluminum and printing ink.

Moreover, it has the effect of being excellent in the durability of lubricity and abrasion resistance. Furthermore, 9 surface roughness is small, so transparency is good (
This also has the effect of reducing film haze. Because it has even better friction coefficient.

It has the advantage of good runnability and ease of handling in the film forming/slitting winding/unwinding process and post-product processing process, as well as the absence of disturbances, scratches, and protrusion transfer.

Because of the above effects, the polyester film of the present invention is suitable for base films for magnetic recording media such as magnetic tapes and floppy disks, optical base films, capacitor base films, graphic base films, and packaging base films. In particular, it is suitable for use as magnetic recording media bases such as video tape recorders and magnetic recording disks, which have recently been required to be smaller and lighter, and as bases for vapor-deposited foil-wound capacitors.

Furthermore, 9% of magnetic recording media are suitable for metal tapes that require higher density, tapes and disks made by vapor deposition or sputtering, and the most suitable ones are those with thin magnetic layers. This is a vapor-deposited tape application where runnability is important.

In addition, when used as a magnetic recording medium, the film of the present invention has both flatness and smoothness, so it is said that it has superior electromagnetic conversion characteristics and running consistency compared to conventionally known magnetic recording media. effect can be obtained.

The effective magnetic recording medium using the film of the present invention can be used as a magnetic tape, magnetic card, or magnetic disk for computers, audio, video, and measurement applications, and is particularly preferably used for video applications. .

[Measurement method and evaluation criteria of characteristics]

The characteristics measurement method and evaluation criteria in the present invention are as follows.

(1) Particle diameter φ (μm) of inert particles: The inert particles were measured as an ethylene glycol or water slurry using a centrifugal sedimentation type particle size distribution analyzer and expressed as an average particle diameter.

(2) Surface roughness Fta (μm): Shows the value measured by a stylus type surface roughness meter (cutoff 0.
25mm, measured value at 4 anus. However, J engineering 5-B-06
01).

(3) Static friction coefficient, μ8: Measured using a slip tester according to ASTM-D-1894B-65.

f41 Critical surface tension, γc (dyn eAl)
: By ASTM-D-2578-67T method.

Measurement was performed at 20°C under a 65% atmosphere.

(5) Adhesion (5)-8 Aluminum evaporation power Bell jar type high vacuum evaporation equipment (KBH- made by Japan Vacuum Technology ■)
6) at a vacuum level of approximately 1 x 10 mmHg.
/f was deposited to a thickness of about 1 [] Onm, and a commercially available cellophane adhesive tape manufactured by Nichiban Co., Ltd. was pasted on the deposition surface.
0 Evaluation was made based on the area of As present and adhered after peeling.

The criteria for evaluation are as follows.

If the index is 3 or more, it is sufficient for practical adhesive strength.

(5)-B Adhesion of magnetic coating film A commercially available cellophane adhesive tape manufactured by Nichiban Co., Ltd. was pasted on the coated side of a sample coated with magnetic paint, and evaluated by the remaining adhesion area of the magnetic coating film after peeling off for 90 minutes. . The evaluation was based on the same 5-level index as the aluminum vapor deposition power above.

5-C Printing Ink Adhesion Strength Use a metering bar to apply printing ink for cellophane [“CC-S T” white, manufactured by Toyo Ink Co., Ltd.] to the film so that the solid content is approximately 5 g/m”. Coat and dry with hot air at 60℃ for 1 minute, same as the aluminum evaporation power test above.

A cellophane adhesive tape peel test was conducted and evaluation was made using a 5-level index.

(6) Film runnability, μ = A load of 100 g was applied to a film slit to a width of 172 inches in an environment of 25° C. and 85% RH.

The tension T on the winding side when pulled at a take-off speed of 1cIII/SeC was determined, and μk was calculated using a linear equation.

1 μk = −log− π 10〇29− For magnetic tapes, μ is preferably 0.65 or less, more preferably ld: 0.30 or less, and even more preferably ld: 0.26 or less.

(7) Durability of lubricity: The surface of the tape-shaped film was repeatedly brought into contact with a metal (SUS) fixed guide (5 eaves φ) 500 times, and then μθ as described in (3) above was measured. μS at the start of running is also 0
．． If the difference is within 1, the durability is good (○), and the difference is 0.1.
If it exceeds , the durability is evaluated as poor (×).

(8) Abrasion resistance: After repeatedly touching and running the surface of a tape-shaped film against a metal (SUs) fixed guide (5rm] φ), the amount of scratches adhered to the film was observed, and the number of scratches was measured. The evaluation was made as follows, depending on the degree of difficulty.

(9) Running properties of magnetic tape A sample magnetic tape on which a signal of near 000 Hz was recorded was loaded into a tape recorder, and the tape was run at a running speed of 100 m/SeC while repeatedly starting and stopping running.

The test was conducted until the running time reached 100 hours while simultaneously measuring the output. If the tape runs smoothly throughout the period without sticking to the guide roller and the output decreases less than 2.0 a B after 100 hours, it is considered "good running performance." Otherwise, it is considered "poor running performance." OQ electromagnetic conversion characteristics: If the output signal is strong and the signal waveform is flat when looking at one screen of the output signal when reproducing the sample magnetic recording medium, the output signal is "good". If the signal was weak or the signal waveform was deformed, it was judged as "defective."

(Ill film haze measured according to ASTM-D-1003-52.15
Transparency is good if it is 3.5% or less in terms of μm thickness film.

〔Example〕

Hereinafter, one embodiment of the present invention will be described based on Examples.

Examples 1-10. Comparative Examples 1 to 18 A transesterification reaction was carried out by a conventional method using 10.0 parts by weight of dimethyl terephthalate and 62 parts by weight of ethylene glycol using 0.06 parts by weight of calcium acetate as a catalyst, and the product was mixed with 0.04 li of antimony trioxide. 0.07 parts by weight of lithium acetate and 0.04 parts by weight of calcium acetate, followed by addition of 0.02 parts by weight of phosphorous acid and 0.10 parts by weight of trimethyl phosphate, followed by 9-polycondensation,
Intrinsic viscosity 0.61B.

A polymer containing an internal particle amount of 0.65 parts by weight c to 100 parts by weight of polyester was obtained. The internal particles contained 1.2 parts by weight of calcium element, 1.9 parts by weight of lithium element, and 49 parts by weight of phosphorus element (polyester: A).

A slurry was prepared by kneading 100 parts by weight of terephthalic acid and 43 parts by weight of ethylene glycol. The slurry is continuously added at a constant rate to a reactant of 50 parts by weight of terephthalic acid and 21.5 parts by weight of ethylene glycol stored at 245°C in a reactor, and an esterification reaction is carried out at 245°C under normal pressure to produce the slurry. Water was continuously distilled out of the system from the rectification column.

The supply time of the slurry was completed in 6 hours and 30 minutes, and the esterification reaction was completed in 4 hours. From the obtained reaction product, the esterification reaction product corresponding to 100 parts by weight of terephthalic acid was transferred to a polymerization apparatus, and phosphoric acid was added. 2.3 parts by weight was added as an ethylene glycol slurry, and a polycondensation reaction was carried out according to a conventional method. The resulting polymer had an intrinsic viscosity of 0.615'i, no internal particles as defined in the present invention, and contained 2 parts by weight of calcium carbonate (Polyester 2B).

33- A polymer with an intrinsic viscosity of 0.62 without the addition of inert particles was obtained in the same manner as Polyester 2B (Polyester:
C).

In the same manner as polyester B, 1.0 weight of dry silica (S1O,) ("Aerosil" TT-600 manufactured by Nippon Aerosil ■) with an average particle size of 0.7μ was added to 100 parts by weight of polyethylene terephthalate instead of calcium carbonate. % (polyester: D) was obtained.

On the other hand, polyester 2E) containing 3 parts by weight of kaolinite having an average particle size of 18μ.

Polyesters A, B, C, and D thus obtained.

Select appropriate amounts of E, combine and blend, and dry under reduced pressure (1
After 70°0, 2 hours), sodium montanate, calcium montanate, magnesium stearate, and sodium behenate were further added as higher fatty acid compounds, and erucic acid amide, melisic acid amide, and acetic acid-N-stearylamide were added. were added, respectively, and 10 types were prepared from Example 1 to Example 10, each having the composition shown in Table 1. In addition, as comparative examples, 18 types of compositions shown in Table 1 were prepared from Comparative Example 1 to Comparative Example 18.

When preparing the compositions of these comparative examples, the polyesters A, B, C, and D described above were used.

In addition to E, polyester containing 6 parts by weight of calcium carbonate with an average particle size of 4.0 μm and 6 parts by weight of kaolinite with an average particle size of 2.0/1 m were prepared in the same manner as polyesters B, D, and E. Made of polyester.

In addition to the higher fatty acid compounds used in the examples, sodium palmitate and palmitic acid amide were used.

The composition was melt-extruded at 285°C, cast on a cooling drum at 60°C to form a non-stretched sheet, and then first stretched into a pair of sheets with a one-peripheral speed difference by a conventional sequential biaxial stretching method. It was stretched 3.3 times in the longitudinal direction at 90'c between rolls. The refractive index is in the vertical direction.

The values were 1.64 and 1.54 in the horizontal direction, respectively, and the in-plane birefringence Δn was 0.10. Next, it was fed into a tenter and stretched 3.5 times in the horizontal (C) direction at 95°C while holding both ends with clips, and then at 218°C for 5 seconds while being relaxed in the width direction in the same tenter. It was heat treated 4 times.

The biaxially oriented film that came out of the tenter was
0W-+n]. Both surfaces were subjected to corona discharge treatment with an energy of n/ml and wound up nine times to obtain a polyethylene terephthalate 1-2111 oriented film with a thickness of 15 μm. The windability of these films was very good. This film is vertical and horizontal. Therefore, in-plane birefringence Δn is 0
03. The sum of the in-plane refractive indices is 329. Thickness direction refractive index ratio 0
It was 95.

Table 1 shows the results of measuring and evaluating the properties of these films. The film properties showed the same values and results on both sides.

From the results in Table 1, each film of Examples 1 to 10 has flatness (Ra), slipperiness (μs), and transparency (haze).
, adhesion (Al vapor deposition strength, printing ink adhesive strength), runnability (
It can be seen that the material is also excellent in terms of lubricity, durability, and abrasion resistance. On the other hand, Comparative Example 1 did not contain internal particles, inert particles, and higher fatty acid metal salt compounds,
Since it contains only higher fatty acid amides, it has poor lubricity and poor running properties. In addition, each of the films of Comparative Examples 2 to 18 did not meet any of the requirements of the claims of the present invention, and therefore any of the film characteristic items was poor.

Next, regarding the films of each example and each comparative example,
A magnetic paint was applied to one side of the tape using the primary method to obtain a magnetic tape. Namely.

Ferromagnetic alloy powder (Fθ-C○) 600 parts by weight Zinc powder (average particle size 2 μm) 25 Cellulose acetate butyrate 60 Epoxy resin
25 〃Silicone oil
4 〃Lecithin 5 ”
A composition consisting of 200 parts of toluene (solvent), 200 parts of methyl ethyl ketone (solvent), and 100 parts of ethyl acetate (solvent) was placed in a ball mill and thoroughly kneaded, then 180 parts by weight of a polyisocyanate compound (Desmodeur L-75) was added and filtered. After stirring and mixing for 0 minutes, the mixture was coated on one side of a two-dimensional polyethylene terephthalate film to a dry thickness of 4 μm while applying a magnetic field, and dried. After that.

After being hardened and mirror-finished, it was slit into a 172-inch width to make a videotape.

Table 1 also shows the results of evaluating the magnetic tape properties of the film thus obtained.

From the measurement evaluation results of magnetic tape characteristics in Table 1.

Tapes using each film of Examples 1 to 10 are as follows.

It can be seen that the magnetic film adhesion, magnetic tape running properties, and N magnetic conversion characteristics are all good.

On the other hand, Comparative Example 1 had good magnetic film adhesion strength and electromagnetic conversion characteristics, but poor magnetic tape running properties. Further, each of the films of Comparative Examples 2 to 1B does not meet any of the requirements of the claims of the present invention.

One of the magnetic tape characteristics items has deteriorated.

Example 11 One side of the film of Example 8 was coated with co-N as a magnetic layer.
i alloy was vacuum deposited to a thickness of 1100 nm,
The tape was slit to a width of /2 inches to obtain a vapor-deposited magnetic tape. The results of measuring and evaluating this magnetic tape.

Adhesion of the magnetic layer to the film, running properties of the magnetic tape.

Both electromagnetic conversion characteristics were good.

Although the above description has mainly focused on a single-layer film, the single-layer film may be coated as a coating layer on both or one side of an oriented base film made of another composition to form an oriented composite film.

In addition, it is preferable that the thickness of the coating layer is in the range of 0.1 to 5 μm. In addition, when the coating layer is single-sided coating, the roughness Ra of the exposed surface of the base (the side on which the coating layer is not provided) is 0.0.
The magnetic layer is preferably provided on the exposed surface side.

39- 壬 [kushiu i: Neyama -+TL'? Mr. Kazuo Wakasugi, Commissioner of the Bow Patent Office1, Indication of the case 1982 Patent Application No. 965622, Title of invention: Oriented Polyester Film3, Related Ministry case for amendment Patent No. 9' [Applicant 41, Tokyo Metropolitan Government] Chuo-ku [1 Honbashi Muromachi 2-2 Voluntary 5, No number of inventions increased by amendment 6, Column 7 of Detailed explanation of one invention in the amended pair or specification I, Contents of amendment (1) Specification No. Page 17, line 11, ``abbreviated)'' is corrected to ``1 abbreviated)'' or higher fatty acid amide (hereinafter abbreviated as ■ in A)''.

(2) Same page 19, lines 15 to 16 [In the case of -axis orientation, in-plane birefringence Δn] is changed to ``In the case of -axis orientation, in-plane birefringence Δn is 0.02 to 0.25, preferably 0.06~0.
2 is desirable, and in the case of biaxial orientation, it is corrected as in-plane birefringence Δn.

38

Claims (1)

[Claims] (1) 100 parts by weight of polyester. A. 0.001 to 1 part by weight of internal particles or inert particles having an average particle size of 0.1 to 6 μm. B. At least one metal salt or partial metal salt compound of a compound whose main component is a higher fatty acid monocarboxylic acid having 18 to 53 carbon atoms, or a higher fatty acid amide having 18 to 36 carbon atoms as a main component. .005 to 2 parts by weight, and the surface roughness Ra is 0.003 to 0.
．． 025 μm, and a static friction coefficient μs of 0.10 to 0.70.