JPS62207356A - Method of improving slipperiness - Google Patents
Method of improving slipperinessInfo
- Publication number
- JPS62207356A JPS62207356A JP61048456A JP4845686A JPS62207356A JP S62207356 A JPS62207356 A JP S62207356A JP 61048456 A JP61048456 A JP 61048456A JP 4845686 A JP4845686 A JP 4845686A JP S62207356 A JPS62207356 A JP S62207356A
- Authority
- JP
- Japan
- Prior art keywords
- polyester
- fine particles
- added
- particles
- particle size
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims description 21
- 239000002245 particle Substances 0.000 claims abstract description 38
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 11
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 8
- 229910052751 metal Inorganic materials 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 7
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 6
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 5
- 239000010419 fine particle Substances 0.000 claims description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 229920006267 polyester film Polymers 0.000 claims description 18
- 150000002902 organometallic compounds Chemical class 0.000 claims description 13
- 239000010936 titanium Substances 0.000 claims description 10
- 229910052845 zircon Inorganic materials 0.000 claims description 10
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 claims description 10
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 9
- 150000001875 compounds Chemical class 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 9
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 229910052809 inorganic oxide Inorganic materials 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 5
- 230000003301 hydrolyzing effect Effects 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 2
- 229920000728 polyester Polymers 0.000 abstract description 23
- 239000012798 spherical particle Substances 0.000 abstract description 7
- 125000000217 alkyl group Chemical group 0.000 abstract description 5
- 229910052726 zirconium Inorganic materials 0.000 abstract description 2
- 125000002524 organometallic group Chemical group 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000002904 solvent Substances 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- 239000000243 solution Substances 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 9
- 239000010408 film Substances 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 238000009826 distribution Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 4
- 238000006460 hydrolysis reaction Methods 0.000 description 4
- 238000006116 polymerization reaction Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000011859 microparticle Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 230000000704 physical effect Effects 0.000 description 3
- -1 silicon oxide-magnesium oxide compound Chemical class 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- PHTQWCKDNZKARW-UHFFFAOYSA-N isoamylol Chemical compound CC(C)CCO PHTQWCKDNZKARW-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- RYSXWUYLAWPLES-MTOQALJVSA-N (Z)-4-hydroxypent-3-en-2-one titanium Chemical compound [Ti].C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O.C\C(O)=C\C(C)=O RYSXWUYLAWPLES-MTOQALJVSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- KWKAKUADMBZCLK-UHFFFAOYSA-N 1-octene Chemical group CCCCCCC=C KWKAKUADMBZCLK-UHFFFAOYSA-N 0.000 description 1
- IHEDBVUTTQXGSJ-UHFFFAOYSA-M 2-[bis(2-oxidoethyl)amino]ethanolate;titanium(4+);hydroxide Chemical compound [OH-].[Ti+4].[O-]CCN(CC[O-])CC[O-] IHEDBVUTTQXGSJ-UHFFFAOYSA-M 0.000 description 1
- KTXWGMUMDPYXNN-UHFFFAOYSA-N 2-ethylhexan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCCC(CC)C[O-].CCCCC(CC)C[O-].CCCCC(CC)C[O-].CCCCC(CC)C[O-] KTXWGMUMDPYXNN-UHFFFAOYSA-N 0.000 description 1
- AIFLGMNWQFPTAJ-UHFFFAOYSA-J 2-hydroxypropanoate;titanium(4+) Chemical compound [Ti+4].CC(O)C([O-])=O.CC(O)C([O-])=O.CC(O)C([O-])=O.CC(O)C([O-])=O AIFLGMNWQFPTAJ-UHFFFAOYSA-J 0.000 description 1
- LYPJRFIBDHNQLY-UHFFFAOYSA-J 2-hydroxypropanoate;zirconium(4+) Chemical compound [Zr+4].CC(O)C([O-])=O.CC(O)C([O-])=O.CC(O)C([O-])=O.CC(O)C([O-])=O LYPJRFIBDHNQLY-UHFFFAOYSA-J 0.000 description 1
- DUFCMRCMPHIFTR-UHFFFAOYSA-N 5-(dimethylsulfamoyl)-2-methylfuran-3-carboxylic acid Chemical compound CN(C)S(=O)(=O)C1=CC(C(O)=O)=C(C)O1 DUFCMRCMPHIFTR-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- AEMRFAOFKBGASW-UHFFFAOYSA-M Glycolate Chemical compound OCC([O-])=O AEMRFAOFKBGASW-UHFFFAOYSA-M 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 150000001414 amino alcohols Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000011952 anionic catalyst Substances 0.000 description 1
- 229940111121 antirheumatic drug quinolines Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical class OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000008094 contradictory effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- XGZNHFPFJRZBBT-UHFFFAOYSA-N ethanol;titanium Chemical compound [Ti].CCO.CCO.CCO.CCO XGZNHFPFJRZBBT-UHFFFAOYSA-N 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000005457 ice water Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 239000010954 inorganic particle Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- ZEIWWVGGEOHESL-UHFFFAOYSA-N methanol;titanium Chemical compound [Ti].OC.OC.OC.OC ZEIWWVGGEOHESL-UHFFFAOYSA-N 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- DAWBXZHBYOYVLB-UHFFFAOYSA-J oxalate;zirconium(4+) Chemical compound [Zr+4].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O DAWBXZHBYOYVLB-UHFFFAOYSA-J 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 150000003248 quinolines Chemical class 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- QQQSFSZALRVCSZ-UHFFFAOYSA-N triethoxysilane Chemical compound CCO[SiH](OCC)OCC QQQSFSZALRVCSZ-UHFFFAOYSA-N 0.000 description 1
- JSPLKZUTYZBBKA-UHFFFAOYSA-N trioxidane Chemical class OOO JSPLKZUTYZBBKA-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は滑り性改良方法に関するものである。[Detailed description of the invention] (Industrial application field) The present invention relates to a method for improving slipperiness.
更に詳しくは、ポリエステルフィルムの滑り性を向上さ
せる為に、特定の製法で得られた粒子径のそろった無機
酸化物球状微粒子をポリエステルに添加する滑り性改頁
方法に関するものである。More specifically, the present invention relates to a slipping property page breaking method in which inorganic oxide spherical fine particles of uniform particle size obtained by a specific manufacturing method are added to polyester film in order to improve the slipping property of the polyester film.
（従来の技術）
ポリエステルは優れた物理的・化学的性能を有しておシ
、それ故そのフィルムであるポリエステルフィルムは磁
気テープ用、光学写真用、蒸着用、コンデンサー用、包
装用等に広く用いられている。(Prior art) Polyester has excellent physical and chemical properties, and therefore its polyester film is widely used for magnetic tapes, optical photography, vapor deposition, capacitors, packaging, etc. It is used.
しかしながら、その優れた性能にもかかわらず、製造工
程中に種々の好ましくないトラブルが生じる場合がある
。これはポリエステルフィルムの清シ性の悪さに起因す
るものと考えられている。さらに、ポリエステルフィル
ムをその表面に磁性層を塗布して磁気テープとして用い
る場合には、特に滑υ性の良さが要求される。これは、
フィルムの滑り性が悪いとフィルム製造時、磁性層塗布
時あるいはその他フィルム取扱い時にフィルム表面に傷
・しわ等が発生し、その為ドロップ・アウトが起こシ磁
気テープの品質に問題が生じるからである。また、製品
としての磁気テープはテープ走行性の良さが不可欠であ
る為、良好な滑り性が求められる。However, despite its excellent performance, various undesirable troubles may occur during the manufacturing process. This is thought to be due to the poor cleanliness of the polyester film. Furthermore, when a polyester film is used as a magnetic tape by coating a magnetic layer on its surface, particularly good lubricity is required. this is,
If the slipperiness of the film is poor, scratches and wrinkles will occur on the film surface during film manufacturing, magnetic layer coating, or other film handling, which will cause dropouts and cause problems with the quality of the magnetic tape. . Furthermore, since it is essential for magnetic tapes to have good tape running properties, good slipping properties are required.
従来、ポリエステルフィルムの滑り性を向上させる方法
として、フィルム表面に凹凸を形成して摩擦係数を低下
させることが行われている。その為に大別すると、（１
）ポリエステル合成時に使用する触媒、着色防止剤など
の一部または全部を反応過程で析出せしめ微粒子として
存在させる方法、（２）ポリエステル合成時の任意の段
階で外部より無機微粒子を添加する方法が提案されてい
る。Conventionally, as a method of improving the slipperiness of a polyester film, forming irregularities on the film surface to lower the coefficient of friction has been carried out. For this reason, it can be roughly divided into (1)
2.) A method in which part or all of the catalyst, color inhibitor, etc. used during polyester synthesis is precipitated during the reaction process and exists as fine particles, and (2) A method in which inorganic fine particles are added externally at any stage during polyester synthesis. has been done.
しかし、（１）の方法はポリエステルの合成反応中に触
媒金属化合物に起因する粒子を生成させる方法である為
、粒子量や粒子径のコントロールが内患
難であり、麿大粒子の生成が避は難いなどの問題点があ
った。However, since method (1) generates particles caused by the catalytic metal compound during the polyester synthesis reaction, it is difficult to control the particle amount and particle size, and the generation of large particles is unavoidable. There were some problems, such as difficulty.
一方、（２）の方法で添加する無機微粒子として、シリ
カ、酸化チタン、硫酸バリウム、酸化ケイ素−酸化マグ
ネシウム化合物、シリカ−アルミナ化合物、アルミナ化
合物、ガラス粉末、炭酸カルシウム、クレイ、雲母、タ
ルク、リン酸カルシウム、リン酸マグネシウムなどが知
られておυ、その平均粒径が０．００１〜１０μｍのも
のがポリエステルフィルムの用途に応じて使い分けられ
ている（特公昭５９−８２１６号、特開昭５２−３６４
５号など）。On the other hand, as inorganic fine particles added in method (2), silica, titanium oxide, barium sulfate, silicon oxide-magnesium oxide compound, silica-alumina compound, alumina compound, glass powder, calcium carbonate, clay, mica, talc, calcium phosphate , magnesium phosphate, etc. are known, and those with an average particle size of 0.001 to 10 μm are used depending on the purpose of the polyester film (Japanese Patent Publication No. 59-8216, JP-A No. 52-364).
No. 5, etc.).
しかし、従来から用いられているこれらの無機微粒子は
、それらの製法に由来するのであるが、粒径分布が広く
、殆んどの粒子形状が不定形である。シリカ微粒子を例
にとると、ノ・ロゲン化ケイ素の熱分解法による平均−
次粒子径０．０２〜０．１μｍ九シリカなどで、いずれ
も電子顕微鏡観察によると、粒子形状が不定形であった
り、仮に球形に近いものでも粒径分布が非常に広いもの
であった。However, these conventionally used inorganic fine particles have a wide particle size distribution and most of the particle shapes are amorphous due to their manufacturing method. Taking silica fine particles as an example, the average -
9 silica having a particle size of 0.02 to 0.1 μm, and according to electron microscopic observation, the particle shape was irregular, and even if it was close to spherical, the particle size distribution was very wide.
さらに、近年ポリエステルフィルムの薄膜化が進み、特
に磁気記録の高密度化で一段と促進されるにつけ、ポリ
エステルフィルムの滑り性および耐摩耗性の改良が今ま
でより以上に強く要望されてきている。その為にポリエ
ステル中に不活性微粒子を添加する方法については、多
くの提案がなされてきてはいるが、上述したように添加
微粒子の物性面による制限から、電磁変換特性として必
要な均質微細で高密度な表面凹凸を与えるものではなく
、フィルムの製造工程、磁気テープ製造工程および磁気
テープ使用時の滑υ性や耐摩耗性を充分に満足しうるＫ
は至っていない。Furthermore, as polyester films have become thinner in recent years, and this has been further accelerated by the increasing density of magnetic recording, there has been a stronger demand than ever for improvements in the slipperiness and abrasion resistance of polyester films. For this reason, many proposals have been made regarding the method of adding inert fine particles to polyester, but as mentioned above, due to limitations due to the physical properties of the added fine particles, it is difficult to achieve the homogeneous, fine, and high quality required for electromagnetic conversion characteristics. K does not give dense surface irregularities, but satisfies lubricity and abrasion resistance during film manufacturing processes, magnetic tape manufacturing processes, and magnetic tape use.
has not yet been reached.
（発明が解決しようとする問題点）
本発明者らは、ポリエステルフィルム表面が平滑である
が滑υ性も満足するという一見あい入れない特性の要求
に対して、従来技術での問題点が添加微粒子の性状に基
くものと考え、鋭意検討した結果本発明に至ったもので
ある。(Problems to be Solved by the Invention) The present inventors have discovered that the problems with the prior art have been added to meet the seemingly contradictory requirements of having a polyester film surface that is smooth and also satisfies lubricity. We believe that this is based on the properties of the fine particles, and as a result of intensive study, we have arrived at the present invention.
（問題点を解決するための手段および作用）本発明は、
有機金属化合物をアルコール性溶液中で加水分解して製
造された平均粒子径が０．０５〜２μｍの範囲でかつ粒
子径の標準偏差値が１〜１．５の範囲にある無機酸化物
球状微粒子を、ポリエステルに対して０．０１〜５重量
％添加することを特徴とするポリエステルフィルムの滑
り性改良方法に関するものである。(Means and effects for solving the problems) The present invention has the following features:
Inorganic oxide spherical fine particles with an average particle diameter in the range of 0.05 to 2 μm and a standard deviation value of the particle diameter in the range of 1 to 1.5, produced by hydrolyzing an organometallic compound in an alcoholic solution. The present invention relates to a method for improving the slipperiness of a polyester film, which comprises adding 0.01 to 5% by weight of the following to polyester.
本発明に用いられる無機酸化物球状微粒子（以下、これ
を球状微粒子囚という。）の原料である有機金属化合物
は、加水分解性有機基を含有するシリコン、チタン、ジ
ルコン等の金属化合物で、加水分解して無機酸化物を形
成しうるものであれば良く、工業的に入手しやすく安価
であるものとして金属アルコキシドが好適に用いられる
。それらは一般式Ｍ（ＯＲ）４ （但し、ＭはＳｉ、
ＴｉまたはＺｒであり、Ｒはアルキル基を表わす。）で
示されるが、好ましくは上記アルキル基は炭素数８まで
の低級アルキル基が用いられる。具体的にはテトラメト
キシシラン、テトラエトキシシラン、テトライソプロポ
キシチタン、テトラブトキシシラン、テトラメトキシチ
タン、テトラエトキシチタン、テトライソプロポキシチ
タン、テトラブトキシチタン、テトラメトキシジルコン
、テトラエトキシジルコン、テトライソプロポキシジル
コン、テトラブトキシジルコン、テトラ（２−エチルヘ
キシル）チタネートなどが掲げられるが、ジメトキシジ
ェトキシシラン、ジェトキシジブトキシチタンなどの如
く複数のアルキル基の化合物であっても良い。The organometallic compound that is the raw material for the inorganic oxide spherical fine particles (hereinafter referred to as spherical fine particles) used in the present invention is a metal compound such as silicon, titanium, or zircon that contains a hydrolyzable organic group. Any material may be used as long as it can be decomposed to form an inorganic oxide, and metal alkoxides are preferably used because they are industrially easily available and inexpensive. They have the general formula M(OR)4 (where M is Si,
Ti or Zr, and R represents an alkyl group. ), but preferably the alkyl group is a lower alkyl group having up to 8 carbon atoms. Specifically, tetramethoxysilane, tetraethoxysilane, tetraisopropoxytitanium, tetrabutoxysilane, tetramethoxytitanium, tetraethoxytitanium, tetraisopropoxytitanium, tetrabutoxytitanium, tetramethoxyzircone, tetraethoxyzircone, tetraisopropoxyzircone. , tetrabutoxyzircon, tetra(2-ethylhexyl)titanate, etc., but compounds having a plurality of alkyl groups such as dimethoxyjethoxysilane, jetoxydibutoxytitanium, etc. may also be used.
また、他の好ましい有機金属化合物として金属アルコキ
シドの誘導体がある。−例として、前記一般式Ｍ （Ｏ
Ｒ） ４のうち３つまでのフルコキシド基（ＯＲ）がカ
ルボキシル基あるいはβ−ジカルボニル基で置換された
化合物、あるいは金属アルコキシドまたは上記アルコキ
シド置換化合物を部分的に加水分解して得られる低縮合
物などである。Other preferred organometallic compounds include metal alkoxide derivatives. - As an example, the general formula M (O
R) Compounds in which up to three of the flukoxide groups (OR) of 4 are substituted with carboxyl groups or β-dicarbonyl groups, or low condensates obtained by partially hydrolyzing metal alkoxides or the above alkoxide-substituted compounds. etc.
その他の有機金属化合物としては、例えばジルコニウム
アセテート、ジルコニウムオキサレート、ジルコニウム
ラクテート、チタンラクテートなどのチタンまたはジル
コンの７シレート化合物；チタンアセチルアセトナート
、ジルコンアセチルアセトナート、チタンオクチレング
リコラート、ジルコンアセチルアセトナート、チタント
リエタノールアミネートなどのチタンまたはジルコンの
グリコール、β−ジケトン、ヒドロキシカルボン酸、ケ
トエステル、ケトアルコール、アミノアルコール、キノ
リンなどのキレート化合物などが挙げられる。Other organometallic compounds include, for example, titanium or zircon heptacylate compounds such as zirconium acetate, zirconium oxalate, zirconium lactate, titanium lactate; titanium acetylacetonate, zircon acetylacetonate, titanium octylene glycolate, zircon acetylacetonate; Examples include glycols of titanium or zircon such as titanium triethanolaminate, and chelate compounds such as β-diketones, hydroxycarboxylic acids, ketoesters, ketoalcohols, aminoalcohols, and quinolines.
球状微粒子（５）は、上記したシリコン、チタンおよび
／またはジルコンの有機金属化合物を主原料とするもの
であるが、それ以外にナトリウム、カリウム、ルビジウ
ム、セシウム、マグネシウム、カルシウム、ストロンチ
ウム、バリウム、ホウ素、アルミニウム、ガリウム、イ
ンジウムなどの有機金属化合物または無機塩を共存せし
めて加水分解することにより、シリコン、チタンおよび
／またはジルコンの酸化物と上記金属の酸化物の複合体
微粒子とすることもできる。その際、球状微粒子回申の
シリコン、チタンおよび／−１！たはジルコンの酸化物
の割合を原子比で７０％以上とするのが好ましい。The spherical fine particles (5) are mainly made from the organometallic compound of silicon, titanium, and/or zircon, but also contain sodium, potassium, rubidium, cesium, magnesium, calcium, strontium, barium, and boron. By hydrolysis in the coexistence of organometallic compounds or inorganic salts such as aluminum, gallium, and indium, fine particles of a composite of silicon, titanium, and/or zircon oxides and oxides of the above metals can be obtained. At that time, silicon, titanium and /-1! It is preferable that the proportion of oxide of zircon or zircon be 70% or more in terms of atomic ratio.
上記した有機金属化合物はアルコール性溶液中に添加混
合して加水分解されるが、その添加方法は一括、分割な
ど任意の方法がとシうる。その際有機金属化合物の溶液
の最終濃度は０．７ ｍｏ Ｉ ／ １以下にするのが
好ましい。The above-mentioned organometallic compound is added and mixed into an alcoholic solution and hydrolyzed, and the addition method can be any method such as all at once or divided. In this case, the final concentration of the solution of the organometallic compound is preferably 0.7 mo I/1 or less.
この濃度が０．７ｍｏｌ／ｌを超えると、本発明に有効
な前記した粒子径範囲の球状微粒子（２）が、安定に得
られなくなることがある。If this concentration exceeds 0.7 mol/l, it may become impossible to stably obtain spherical fine particles (2) having the particle size range described above, which are effective in the present invention.
アルコール性溶液中のアルコールは、メタノール、エタ
ノール、イングロバノール、ブタノール、イソアミルア
ルコール、エチレングリコール、フロピレンゲリコール
などが単一でまたは混合物で用いられる。該溶液中にジ
オキサン、ジエチルエーテル、酢酸エチル、ベンゼン、
トルエン、ヘキサンなどの有機溶媒を一部混合すること
もできる。As the alcohol in the alcoholic solution, methanol, ethanol, inglobanol, butanol, isoamyl alcohol, ethylene glycol, phlopylene gellicol, etc. are used singly or in a mixture. Dioxane, diethyl ether, ethyl acetate, benzene,
It is also possible to partially mix organic solvents such as toluene and hexane.
アルコール性溶液中には加水分解に必要な水を！
共存せしめる。この水含量は、粒子の形状１粒子径に影
響を及ぼすので、好ましい量に制御する必要があるが、
有機金属化合物の金属の種類および化合物の種類によっ
て変化する。また、この水ははそのアルコール溶液を上
記アルコール性溶液中に添加し、０〜５０℃の範囲、好
ましくは室温下３０分〜１００時間撹拌することによっ
て行われる。Water necessary for hydrolysis is included in the alcoholic solution! Let them coexist. This water content affects the shape and diameter of the particles, so it needs to be controlled to a preferable amount.
It varies depending on the type of metal in the organometallic compound and the type of compound. Further, this water and alcohol solution is added to the above-mentioned alcoholic solution, and the mixture is stirred at a temperature of 0 to 50°C, preferably at room temperature, for 30 minutes to 100 hours.
その際、加水分解速度をフントロールする目的で、ＮＨ
４、Ｎａ などのカチオンや８０４’ 、 Ｈ２Ｐ
Ｏ４−などのアニオンの触媒成分を添加することができ
るされる。At that time, for the purpose of controlling the hydrolysis rate, NH
4. Cations such as Na, 804', H2P
Anionic catalyst components such as O4- can be added.
このようにして有機金属化合物をアルコール性溶液中で
適切な条件の元で加水分解すれば、球状微粒千人は、球
形でしかも粒径分布中の非常に小さい無機酸化物微粒子
として溶液中に析出する。In this way, if an organometallic compound is hydrolyzed in an alcoholic solution under appropriate conditions, spherical microparticles will be precipitated in the solution as spherical and very small inorganic oxide microparticles with a particle size distribution. do.
この析出粒子には原料に由来する有機基が一部残存して
結合していることもある。該析出粒子を溶液中より濾過
、遠心分離、溶媒蒸発など従来公知の方法で分離した後
、乾燥または場合によ９３００〜１０００℃で焼成して
、目的とする球状微粒千人とすることができる。また、
球状微粒千人のポリエステル中での分散性を高めるため
に、粒子間の凝集を極力防ぎ単分散させることが重要で
ある。Some of the organic groups derived from the raw materials may remain and bond to these precipitated particles. The precipitated particles can be separated from the solution by conventionally known methods such as filtration, centrifugation, and solvent evaporation, and then dried or optionally calcined at 9300 to 1000°C to obtain the desired spherical fine particles. . Also,
In order to improve the dispersibility of the spherical fine particles in the polyester, it is important to prevent agglomeration between the particles as much as possible and to achieve monodispersion.
そのために、ポリエステルへの添加に先立って捕潰機、
ボールミル、ジェット粉砕機等通常の方法で凝集粒子を
ときほぐすことは有効である。For this purpose, a crusher,
It is effective to loosen agglomerated particles using a conventional method such as a ball mill or a jet pulverizer.
こうして得られた球状微粒子図は、平均粒径が０．０５
〜２μｍの範囲でかつ粒子径の標準偏差値が１〜１．５
、より好ましくは１〜１．３の範囲にある粒径分布が非
常にシャープなものである。粒径が０．０５μｍより小
さければ添加による滑り性改良の効果が少なく、また、
２．０μｍより大きければ薄膜フィルムには表面の凹凸
が大き過ぎて問題となる。The spherical particle diagram obtained in this way has an average particle size of 0.05
~2μm range and standard deviation value of particle size is 1~1.5
, more preferably one with a very sharp particle size distribution in the range of 1 to 1.3. If the particle size is smaller than 0.05 μm, the effect of improving slipperiness by addition is small;
If it is larger than 2.0 μm, the surface unevenness will be too large for a thin film, causing a problem.
本発明におけるポリエステルとは、テレフタル酸または
そのエステル形成性誘導体を主たるジカルボン酸成分と
し、エチレングリコール、１．４−ブタンジオールなど
のジグリコールまたはそのエステル形成性誘導体を主た
るグリコール成分とするポリエステルであるが、組成、
製法などに限定されるものではなく、弛めポリエステル
を配合したものであってもよい。The polyester in the present invention is a polyester having terephthalic acid or its ester-forming derivative as the main dicarboxylic acid component and a diglycol such as ethylene glycol or 1,4-butanediol or its ester-forming derivative as the main glycol component. However, the composition
It is not limited to the manufacturing method, and may be one in which loose polyester is blended.
ポリエステル中に球状微粒子図を添加する時期は、ポリ
エステル重合前、重合中あるいは重合終卜
７後ベレット化する時でも良く、更にクー説伏に溶融押
出しする際に添加しても良い。The spherical particles may be added to the polyester before or during the polyester polymerization, or during pelletization after the end of the polymerization, or even during melt extrusion.
球状微粒子図は通常粉末状で添加されるが、ポリエステ
ルへの添加時期がポリエステル重合前または重合中とす
る場合には、エチレングリコールなど重合仕込時に液状
であるポリエステル原料の一部あるいは全量中にあらか
じめ上記微粒子を混合、高分散せしめて、スラリー状ま
たはゾル状で添加することはポリエステル中にも高分散
され、結果としてフィルム中に均一に分散し均一な凹凸
を形成せしめることができるので好ましい。液状ポリエ
ステル原料中に上記微粒子を高分散させるには、湿式ボ
ールミル、超音波など従来公知の方法が用いられる。Spherical microparticles are usually added in powder form, but if they are added to polyester before or during polyester polymerization, they can be added in advance to some or all of the polyester raw materials that are liquid at the time of polymerization, such as ethylene glycol. It is preferable to mix and highly disperse the above-mentioned fine particles and add them in the form of a slurry or sol, since this will also result in a high degree of dispersion in the polyester, resulting in uniform dispersion and formation of uniform irregularities in the film. In order to highly disperse the fine particles in the liquid polyester raw material, conventionally known methods such as wet ball milling and ultrasonic waves are used.
また、ポリエステルへの添加に際し、シランカップリン
グ剤、チタンカップリング剤、界面活性剤などを用いて
、分散性を高めてもよい。Further, when added to polyester, a silane coupling agent, a titanium coupling agent, a surfactant, etc. may be used to improve dispersibility.
球状微粒子図の添加量は、ポリエステルに対して０．０
１〜５重ｆｉｋｓの範囲とする。添加量が０．０１重ｔ
％よりも少なければ滑り性に対する効果が不充分であり
、また、５重量％よりも多い場合はフィルムの破断強度
などの物性の低下があり好ましくない。The amount of spherical particles added is 0.0 to polyester.
The range is 1 to 5 fiks. Added amount is 0.01 weight t
If the amount is less than 5% by weight, the effect on slip properties is insufficient, and if it is more than 5% by weight, the physical properties such as the breaking strength of the film may deteriorate, which is not preferable.
なお、本発明でいう平均粒子径および標準偏差値は下記
の方法により求めた。Note that the average particle diameter and standard deviation value as used in the present invention were determined by the following method.
１０万倍の電子顕微鏡撮影像の任意の粒子１００個の粒
子径を実測して求め、平均粒子径、標準偏差値を下記の
式により求めた。The particle size of 100 arbitrary particles in an image taken with an electron microscope at a magnification of 100,000 times was determined by actual measurement, and the average particle size and standard deviation value were determined using the following formula.
（但し、Ｘｉはｂ個目の粒子径を示し、ルは１００であ
る。）
（発明の効果）
特定された製法によυ得られた、粒子が球状で粒子径分
布が非常にシャープな無機酸化物球状微粒子をポリエス
テルに添加することを特徴とする本発明の方法によれば
、ポリエステルフィルム表面に均質微細な凹凸を確実か
つ容易に形成することができ、表面が実質上平滑でしか
も滑υ性に優れたポリエステルフィルムを得ることがで
きる。(However, Xi indicates the b-th particle diameter, and Le is 100.) (Effect of the invention) Inorganic particles with spherical particles and a very sharp particle size distribution obtained by the specified manufacturing method According to the method of the present invention, which is characterized in that oxide spherical fine particles are added to polyester, homogeneous fine irregularities can be reliably and easily formed on the surface of a polyester film, and the surface is substantially smooth and slippery. A polyester film with excellent properties can be obtained.
したがって、本発明の方法で得られたポリエステルフィ
ルムは、耐摩耗性や磁気テープとする時の磁性層の塗布
性にもすぐれておシ、特に電磁変換特性にすぐれた磁気
テープ製造に好適なものである。Therefore, the polyester film obtained by the method of the present invention has excellent abrasion resistance and coatability of the magnetic layer when it is made into a magnetic tape, and is particularly suitable for manufacturing magnetic tapes with excellent electromagnetic conversion characteristics. It is.
（実施例）
以下、実施例によシ本発明を詳述するが、この実施例に
より本発明の範囲が何ら制限されるものではない。(Examples) Hereinafter, the present invention will be explained in detail with reference to Examples, but the scope of the present invention is not limited by these Examples in any way.
参考例１
撹拌機、滴下口、温度計を備えた３０１のガラス製反応
器にエタノール１６１と２８％アンモニア水溶液２．７
ｉ＜９を添加して混合した。該混合液を２０℃±０．
５℃に調整し撹拌しながら、テトラエトキシシラン１．
０ユをエタノール２１に希釈した溶液を滴下口より１時
間かけて滴下し、滴下後も２時間撹拌を続け、加水分解
を行い懸濁液を得た。Reference Example 1 161 parts of ethanol and 2.7 parts of a 28% ammonia aqueous solution were placed in a 301 glass reactor equipped with a stirrer, a dropping port, and a thermometer.
i<9 was added and mixed. The mixture was heated to 20°C±0.
While adjusting the temperature to 5°C and stirring, add tetraethoxysilane 1.
A solution prepared by diluting 0 U of ethanol with 21 L of ethanol was added dropwise from the dropping port over a period of 1 hour, and stirring was continued for 2 hours after the addition to effect hydrolysis and obtain a suspension.
この時の最終溶液全量に対する各原料の濃度はテトラエ
トキシシラン０．２２モル／ｌ、−ｙンモニア２．０２
モル／ｌｌ氷水、９１モル／ｌであった。次いで、上記
懸濁液を蒸発缶に移し、缶温度４０℃で減圧下にアンモ
ニア、水およびエタノールを溜去して、粉末状のシリカ
微粒子（１ａ）を得た。このシリカ微粒子（１ａ）を空
気中５００℃で焼成して、シリカ微粒子（１ｂ）を得た
。At this time, the concentration of each raw material with respect to the total amount of the final solution was 0.22 mol/l of tetraethoxysilane and 2.02 mol/l of -ymmonia.
Mol/l ice water, 91 mol/l. Next, the suspension was transferred to an evaporator, and ammonia, water and ethanol were distilled off under reduced pressure at a temperature of 40° C. to obtain powdery silica particles (1a). The silica particles (1a) were fired in air at 500°C to obtain silica particles (1b).
得られたシリカ微粒子（１ａ）および（１ｂ）の平均粒
子径、粒子径由、粒子径の標準偏差値および比表面積を
測定し、その結果を第１表に示した。The average particle diameter, particle diameter, standard deviation of particle diameter, and specific surface area of the obtained silica fine particles (1a) and (1b) were measured, and the results are shown in Table 1.
また、これらの電子顕微鏡撮影像によれば、球形の微粒
子であった。Moreover, according to these electron microscope images, they were spherical fine particles.
参考例２〜６
有機金属化合物の種類、アルコールの種類、最終溶液全
量に対する各原料”の濃度および焼成温度を第１表に示
した通りとする以外は参考例１と同様にして、シリカ微
粒子（２）〜（３）、チタニア微粒子（４）、ジルコニ
ア微粒子（５）およびチタニア−ジルコニア化合物微粒
子（６）を得た。これらの微粒子の平均粒子径等の物性
測定結果を第１表に示した。Reference Examples 2 to 6 Silica fine particles ( 2) to (3), titania fine particles (4), zirconia fine particles (5), and titania-zirconia compound fine particles (6) were obtained.The physical property measurement results such as the average particle diameter of these fine particles are shown in Table 1. .
実施例１
参考例１〜６で得られたシリカ微粒子（１ａ）、（２）
、（３）、チタニア微粒子（４）、ジルコニア微粒子（
５）およびチタニア−ジルコニア化合物微粒子（６）の
それぞれ０．５重量部をエチレングリコール１００重量
部に添加し、ボールミルにかけて微粒子のエチレングリ
コール高分散体を得た。次にジメチルテレフタレート１
００重量部および微粒子のエチレングリコール高分散体
８０１ｉ量部に酢酸亜鉛０．０１重量部を加えて、最終
減圧下２８０℃まで昇温して重縮合を行った後、２９０
℃に設定された押出機でシート化し、続いて１００℃で
縦および横方向に３．５倍延伸し、２１０℃で１０秒間
熱処理を行って、厚さ４０μｍのポリエステルフィルム
を得た。Example 1 Silica fine particles (1a) and (2) obtained in Reference Examples 1 to 6
, (3), titania fine particles (4), zirconia fine particles (
0.5 parts by weight of each of 5) and titania-zirconia compound fine particles (6) were added to 100 parts by weight of ethylene glycol, and the mixture was ball milled to obtain a high dispersion of fine particles of ethylene glycol. Next, dimethyl terephthalate 1
0.01 parts by weight of zinc acetate was added to 0.00 parts by weight and 801 parts by weight of fine particle ethylene glycol high dispersion, and the temperature was raised to 280°C under final reduced pressure to perform polycondensation.
It was formed into a sheet using an extruder set at .degree. C., then stretched 3.5 times in the longitudinal and transverse directions at 100.degree. C., and heat-treated at 210.degree. C. for 10 seconds to obtain a polyester film with a thickness of 40 .mu.m.
また、参考例１で得られたシリカ微粒子（１ｂ）につい
ては、エチレングリコールの分散体とする前に、シリカ
微粒子（Ｉｂ） ０．５重量部に対して０．０５重量部
のｒ−アミノプロピルトリエトキシシランで処理した他
は、上記の方法と同様にして、無機酸化物球状微粒子を
含むポリエステルフィルムを得た。Furthermore, regarding the silica fine particles (1b) obtained in Reference Example 1, 0.05 parts by weight of r-aminopropyl was added to 0.5 parts by weight of the silica fine particles (Ib) before making it into an ethylene glycol dispersion. A polyester film containing inorganic oxide spherical fine particles was obtained in the same manner as above except that it was treated with triethoxysilane.
これらのポリエステルフィルムについて、 ＡＳＴｈｉ
−Ｄ −１８９４Ｂ法に従って、静摩擦係数を測定した
ところ、すべて１．０以下であり、優れた滑り性を有し
ていた。About these polyester films, ASThi
When the static friction coefficient was measured according to the -D-1894B method, all the coefficients of static friction were 1.0 or less, indicating excellent slipperiness.
Claims (1)
て製造された平均粒子径が０．０５〜２μｍの範囲でか
つ粒子径の標準偏差値が１〜１．５の範囲にある無機酸
化物球状微粒子を、ポリエステルに対して０．０１〜５
重量％添加することを特徴とするポリエステルフィルム
の滑り性改良方法。 ２、有機金属化合物が金属アルコキシドまたはその誘導
体である特許請求の範囲第１項記載の滑り性改良方法。 ３、有機金属化合物がシリコン、チタンおよび／または
ジルコンの化合物を主成分とし、無機酸化物シリカ、チ
タニア、ジルコニアまたはそれらの複合酸化物を主成分
とする特許請求の範囲第１項記載の滑り性改良方法。[Claims] 1. A product produced by hydrolyzing an organometallic compound in an alcoholic solution and having an average particle diameter in the range of 0.05 to 2 μm and a standard deviation value of the particle diameter of 1 to 1.5. Inorganic oxide spherical fine particles within the range of 0.01 to 5
A method for improving the slipperiness of a polyester film, characterized by adding % by weight. 2. The method for improving slipperiness according to claim 1, wherein the organometallic compound is a metal alkoxide or a derivative thereof. 3. Slip properties according to claim 1, wherein the organometallic compound is mainly composed of a compound of silicon, titanium and/or zircon, and the main component is an inorganic oxide silica, titania, zirconia or a composite oxide thereof. Improvement method.
Priority Applications (10)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61048456A JPS62207356A (en) | 1986-03-07 | 1986-03-07 | Method of improving slipperiness |
| DE3751849T DE3751849T2 (en) | 1986-03-07 | 1987-03-05 | Process for improving the lubricity of polyester film |
| DE8787103111T DE3784357T2 (en) | 1986-03-07 | 1987-03-05 | MONODISPERSE GLYCOL SUSPENSION OF FEI INORGANIC OXIDE PARTICLES WITH EXCELLENT DISPERSION STABILITY AND METHOD FOR IMPROVING THE SLIP RESISTANCE OF POLYESTER FILM USING THE MONODISPERS SUSPENSION. |
| EP87103111A EP0236945B1 (en) | 1986-03-07 | 1987-03-05 | Monodispersed glycol suspension of fine inorganic oxide particles having excellent dispersion stability and method of improving the slipperiness of polyester film using the monodispersed suspension |
| EP92100741A EP0479774B1 (en) | 1986-03-07 | 1987-03-05 | Method of improving the slipperiness of polyester film |
| KR1019870002058A KR910008721B1 (en) | 1986-03-07 | 1987-03-07 | Monodispersed glycol sospension of fine inorganic oxide particles having excellent dispersion stability and method of improving the slipperiness of polyester film using the monodispersed suspension |
| US07/322,185 US5316714A (en) | 1986-03-07 | 1989-03-13 | Method of improving slipperiness of polyester film using a monodispersed glycol suspension of inorganic oxide particles |
| US07/731,259 US5236622A (en) | 1986-03-07 | 1991-07-17 | Process for producing a monodispersed glycol suspension of fine inorganic oxide particles having excellent dispersion stability |
| US07/925,424 US5304324A (en) | 1986-03-07 | 1992-08-10 | Monodispersed glycol suspension of fine inorganic oxide particles having excellent dispersion stability |
| US08/201,406 US5863647A (en) | 1986-03-07 | 1994-02-24 | Monodispersed glycol suspension of fine inorganic oxide particles having excellent dispersion stability and a polyester film containing said particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61048456A JPS62207356A (en) | 1986-03-07 | 1986-03-07 | Method of improving slipperiness |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4096476A Division JPH0791400B2 (en) | 1992-04-16 | 1992-04-16 | Polyester film for magnetic tape |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62207356A true JPS62207356A (en) | 1987-09-11 |
| JPH0578585B2 JPH0578585B2 (en) | 1993-10-29 |
Family
ID=12803856
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61048456A Granted JPS62207356A (en) | 1986-03-07 | 1986-03-07 | Method of improving slipperiness |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62207356A (en) |
Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63108037A (en) * | 1986-08-27 | 1988-05-12 | Teijin Ltd | Biaxially oriented polyester film |
| JPS63128030A (en) * | 1986-11-18 | 1988-05-31 | Toyobo Co Ltd | Oriented polyester film |
| JPS63168818A (en) * | 1987-01-07 | 1988-07-12 | Teijin Ltd | Magnetic recording medium |
| JPS63220417A (en) * | 1987-03-10 | 1988-09-13 | Teijin Ltd | Biaxially oriented polyester film for magnetic recording medium |
| JPS63234038A (en) * | 1987-03-23 | 1988-09-29 | Teijin Ltd | Biaxially oriented polyester film |
| JPS63235343A (en) * | 1987-03-25 | 1988-09-30 | Teijin Ltd | Biaxially oriented polyester film |
| JPS63286440A (en) * | 1987-05-19 | 1988-11-24 | Toyobo Co Ltd | Oriented polyester film |
| JPS63317533A (en) * | 1987-06-19 | 1988-12-26 | Diafoil Co Ltd | Polyester film |
| JPS6411135A (en) * | 1987-07-03 | 1989-01-13 | Toyo Boseki | Thermoplastic film |
| JPH01161025A (en) * | 1987-12-18 | 1989-06-23 | Teijin Ltd | Biaxially oriented polyester film |
| JPH01188553A (en) * | 1988-01-22 | 1989-07-27 | Kanegafuchi Chem Ind Co Ltd | Improve aromatic polyester film |
| JPH01266145A (en) * | 1988-04-19 | 1989-10-24 | Teijin Ltd | Thermoplastic polymer film |
| JPH02120221A (en) * | 1988-10-31 | 1990-05-08 | Nippon Steel Chem Co Ltd | Production of silica particle |
| JPH03115437A (en) * | 1989-09-29 | 1991-05-16 | Toray Ind Inc | Biaxially oriented polyester film |
| JPH03192131A (en) * | 1989-12-21 | 1991-08-22 | Toray Ind Inc | Biaxially oriented thermoplastic resin film |
| JPH03234739A (en) * | 1990-02-09 | 1991-10-18 | Toyobo Co Ltd | Biaxially oriented polyester film |
| JPH03250043A (en) * | 1990-02-27 | 1991-11-07 | Toray Ind Inc | Production of polyester composition |
| JPH05156042A (en) * | 1992-04-16 | 1993-06-22 | Nippon Shokubai Co Ltd | Polyester film |
| US5316714A (en) * | 1986-03-07 | 1994-05-31 | Nippon Shokujai Kagaku Kogyo Co., Ltd. | Method of improving slipperiness of polyester film using a monodispersed glycol suspension of inorganic oxide particles |
| US5429855A (en) * | 1992-04-30 | 1995-07-04 | Diafoil Hoescht Company, Limited | Biaxially oriented laminated polyester film for magnetic recording media |
| US5670236A (en) * | 1992-09-29 | 1997-09-23 | Diafoil Hoechst Company, Ltd. | Biaxially oriented polyester film for magnetic recording medium |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52133356A (en) * | 1976-04-29 | 1977-11-08 | Ici Ltd | Polyeser film or sheet |
| JPS552225A (en) * | 1978-06-19 | 1980-01-09 | Konishiroku Photo Ind Co Ltd | Cleaning device |
| JPS59100156A (en) * | 1982-11-30 | 1984-06-09 | Teijin Ltd | Production of polyester composition |
| JPS60166203A (en) * | 1984-02-09 | 1985-08-29 | Dainippon Ink & Chem Inc | Preparation of fine ceramic powder |
-
1986
- 1986-03-07 JP JP61048456A patent/JPS62207356A/en active Granted
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS52133356A (en) * | 1976-04-29 | 1977-11-08 | Ici Ltd | Polyeser film or sheet |
| JPS552225A (en) * | 1978-06-19 | 1980-01-09 | Konishiroku Photo Ind Co Ltd | Cleaning device |
| JPS59100156A (en) * | 1982-11-30 | 1984-06-09 | Teijin Ltd | Production of polyester composition |
| JPS60166203A (en) * | 1984-02-09 | 1985-08-29 | Dainippon Ink & Chem Inc | Preparation of fine ceramic powder |
Cited By (26)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5316714A (en) * | 1986-03-07 | 1994-05-31 | Nippon Shokujai Kagaku Kogyo Co., Ltd. | Method of improving slipperiness of polyester film using a monodispersed glycol suspension of inorganic oxide particles |
| JPS63108037A (en) * | 1986-08-27 | 1988-05-12 | Teijin Ltd | Biaxially oriented polyester film |
| JPS63128030A (en) * | 1986-11-18 | 1988-05-31 | Toyobo Co Ltd | Oriented polyester film |
| JPS63168818A (en) * | 1987-01-07 | 1988-07-12 | Teijin Ltd | Magnetic recording medium |
| JPS63220417A (en) * | 1987-03-10 | 1988-09-13 | Teijin Ltd | Biaxially oriented polyester film for magnetic recording medium |
| JPS63234038A (en) * | 1987-03-23 | 1988-09-29 | Teijin Ltd | Biaxially oriented polyester film |
| JPH0513976B2 (en) * | 1987-03-23 | 1993-02-23 | Teijin Ltd | |
| JPH054414B2 (en) * | 1987-03-25 | 1993-01-20 | Teijin Ltd | |
| JPS63235343A (en) * | 1987-03-25 | 1988-09-30 | Teijin Ltd | Biaxially oriented polyester film |
| JPS63286440A (en) * | 1987-05-19 | 1988-11-24 | Toyobo Co Ltd | Oriented polyester film |
| JPS63317533A (en) * | 1987-06-19 | 1988-12-26 | Diafoil Co Ltd | Polyester film |
| JPS6411135A (en) * | 1987-07-03 | 1989-01-13 | Toyo Boseki | Thermoplastic film |
| JPH01161025A (en) * | 1987-12-18 | 1989-06-23 | Teijin Ltd | Biaxially oriented polyester film |
| JPH01188553A (en) * | 1988-01-22 | 1989-07-27 | Kanegafuchi Chem Ind Co Ltd | Improve aromatic polyester film |
| JPH0747645B2 (en) * | 1988-04-19 | 1995-05-24 | 帝人株式会社 | Thermoplastic polymer film |
| JPH01266145A (en) * | 1988-04-19 | 1989-10-24 | Teijin Ltd | Thermoplastic polymer film |
| JPH052607B2 (en) * | 1988-10-31 | 1993-01-12 | Shinnittetsu Kagaku | |
| JPH02120221A (en) * | 1988-10-31 | 1990-05-08 | Nippon Steel Chem Co Ltd | Production of silica particle |
| JPH03115437A (en) * | 1989-09-29 | 1991-05-16 | Toray Ind Inc | Biaxially oriented polyester film |
| JPH03192131A (en) * | 1989-12-21 | 1991-08-22 | Toray Ind Inc | Biaxially oriented thermoplastic resin film |
| JPH03234739A (en) * | 1990-02-09 | 1991-10-18 | Toyobo Co Ltd | Biaxially oriented polyester film |
| JPH03250043A (en) * | 1990-02-27 | 1991-11-07 | Toray Ind Inc | Production of polyester composition |
| JPH05156042A (en) * | 1992-04-16 | 1993-06-22 | Nippon Shokubai Co Ltd | Polyester film |
| JPH0791400B2 (en) * | 1992-04-16 | 1995-10-04 | 株式会社日本触媒 | Polyester film for magnetic tape |
| US5429855A (en) * | 1992-04-30 | 1995-07-04 | Diafoil Hoescht Company, Limited | Biaxially oriented laminated polyester film for magnetic recording media |
| US5670236A (en) * | 1992-09-29 | 1997-09-23 | Diafoil Hoechst Company, Ltd. | Biaxially oriented polyester film for magnetic recording medium |
Also Published As
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|---|---|
| JPH0578585B2 (en) | 1993-10-29 |
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Legal Events
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| EXPY | Cancellation because of completion of term |