TW201905070A - 乙烯-乙烯醇系共聚物組成物、丸粒及多層結構體 - Google Patents
乙烯-乙烯醇系共聚物組成物、丸粒及多層結構體Info
- Publication number
- TW201905070A TW201905070A TW107122177A TW107122177A TW201905070A TW 201905070 A TW201905070 A TW 201905070A TW 107122177 A TW107122177 A TW 107122177A TW 107122177 A TW107122177 A TW 107122177A TW 201905070 A TW201905070 A TW 201905070A
- Authority
- TW
- Taiwan
- Prior art keywords
- evoh resin
- ethylene
- resin composition
- vinyl alcohol
- iron compound
- Prior art date
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 19
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 title claims description 164
- 239000008188 pellet Substances 0.000 title claims description 38
- 150000002506 iron compounds Chemical class 0.000 claims abstract description 57
- 229920001577 copolymer Polymers 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 125000003011 styrenyl group Chemical class [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims abstract 4
- 239000004715 ethylene vinyl alcohol Substances 0.000 claims description 155
- RZXDTJIXPSCHCI-UHFFFAOYSA-N hexa-1,5-diene-2,5-diol Chemical compound OC(=C)CCC(O)=C RZXDTJIXPSCHCI-UHFFFAOYSA-N 0.000 claims 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 abstract description 17
- 239000005977 Ethylene Substances 0.000 abstract description 16
- 238000010521 absorption reaction Methods 0.000 abstract description 16
- 239000006097 ultraviolet radiation absorber Substances 0.000 abstract description 4
- UFRKOOWSQGXVKV-UHFFFAOYSA-N ethene;ethenol Chemical compound C=C.OC=C UFRKOOWSQGXVKV-UHFFFAOYSA-N 0.000 description 151
- 229920005989 resin Polymers 0.000 description 111
- 239000011347 resin Substances 0.000 description 111
- 239000011342 resin composition Substances 0.000 description 96
- 238000000034 method Methods 0.000 description 60
- 239000010410 layer Substances 0.000 description 50
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 36
- 150000003440 styrenes Chemical class 0.000 description 34
- -1 Ethyl vinyl Chemical group 0.000 description 30
- 239000000243 solution Substances 0.000 description 24
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 21
- 229920001567 vinyl ester resin Polymers 0.000 description 19
- 238000002156 mixing Methods 0.000 description 18
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 16
- 239000002585 base Substances 0.000 description 15
- 150000003839 salts Chemical class 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- 239000005022 packaging material Substances 0.000 description 13
- WBYWAXJHAXSJNI-VOTSOKGWSA-M .beta-Phenylacrylic acid Natural products [O-]C(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-M 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 12
- 238000007127 saponification reaction Methods 0.000 description 12
- 239000004840 adhesive resin Substances 0.000 description 11
- 229920006223 adhesive resin Polymers 0.000 description 11
- 150000001875 compounds Chemical class 0.000 description 11
- 238000001035 drying Methods 0.000 description 10
- 229920005672 polyolefin resin Polymers 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- 239000002253 acid Substances 0.000 description 8
- 238000000071 blow moulding Methods 0.000 description 8
- 230000007423 decrease Effects 0.000 description 8
- 229910052742 iron Inorganic materials 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000000178 monomer Substances 0.000 description 8
- 239000012488 sample solution Substances 0.000 description 8
- 229920005992 thermoplastic resin Polymers 0.000 description 8
- 239000004743 Polypropylene Substances 0.000 description 7
- 238000004040 coloring Methods 0.000 description 7
- 235000013305 food Nutrition 0.000 description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 7
- 229920001155 polypropylene Polymers 0.000 description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- 230000002745 absorbent Effects 0.000 description 6
- 239000002250 absorbent Substances 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 6
- 229920000098 polyolefin Polymers 0.000 description 6
- 239000002904 solvent Substances 0.000 description 6
- 239000004711 α-olefin Substances 0.000 description 6
- WBYWAXJHAXSJNI-SREVYHEPSA-N Cinnamic acid Chemical compound OC(=O)\C=C/C1=CC=CC=C1 WBYWAXJHAXSJNI-SREVYHEPSA-N 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 230000004888 barrier function Effects 0.000 description 5
- 229930016911 cinnamic acid Natural products 0.000 description 5
- 235000013985 cinnamic acid Nutrition 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000000314 lubricant Substances 0.000 description 5
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 description 5
- 238000000465 moulding Methods 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- 238000006116 polymerization reaction Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 4
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 4
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 4
- 239000006096 absorbing agent Substances 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 4
- 150000008064 anhydrides Chemical class 0.000 description 4
- 125000004432 carbon atom Chemical group C* 0.000 description 4
- 239000010941 cobalt Substances 0.000 description 4
- 229910017052 cobalt Inorganic materials 0.000 description 4
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 4
- 235000014113 dietary fatty acids Nutrition 0.000 description 4
- POULHZVOKOAJMA-UHFFFAOYSA-N dodecanoic acid Chemical compound CCCCCCCCCCCC(O)=O POULHZVOKOAJMA-UHFFFAOYSA-N 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 4
- 239000000806 elastomer Substances 0.000 description 4
- 150000002148 esters Chemical class 0.000 description 4
- 229930195729 fatty acid Natural products 0.000 description 4
- 239000000194 fatty acid Substances 0.000 description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 description 4
- 239000012086 standard solution Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- WBYWAXJHAXSJNI-VOTSOKGWSA-N trans-cinnamic acid Chemical compound OC(=O)\C=C\C1=CC=CC=C1 WBYWAXJHAXSJNI-VOTSOKGWSA-N 0.000 description 4
- 229910052723 transition metal Inorganic materials 0.000 description 4
- 150000003624 transition metals Chemical class 0.000 description 4
- 238000002834 transmittance Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 235000021355 Stearic acid Nutrition 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 238000004898 kneading Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 3
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 3
- 229920000768 polyamine Polymers 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 229920001225 polyester resin Polymers 0.000 description 3
- 229920002635 polyurethane Polymers 0.000 description 3
- 239000004814 polyurethane Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000008117 stearic acid Substances 0.000 description 3
- 125000001424 substituent group Chemical group 0.000 description 3
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 244000291564 Allium cepa Species 0.000 description 2
- 235000002732 Allium cepa var. cepa Nutrition 0.000 description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 239000004709 Chlorinated polyethylene Substances 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 2
- 239000004278 EU approved seasoning Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- 240000008415 Lactuca sativa Species 0.000 description 2
- 239000005639 Lauric acid Substances 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 244000294411 Mirabilis expansa Species 0.000 description 2
- 235000015429 Mirabilis expansa Nutrition 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 239000002216 antistatic agent Substances 0.000 description 2
- 238000004380 ashing Methods 0.000 description 2
- 235000013361 beverage Nutrition 0.000 description 2
- 239000002981 blocking agent Substances 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 150000001735 carboxylic acids Chemical class 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 229940114081 cinnamate Drugs 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000002537 cosmetic Substances 0.000 description 2
- 229910001882 dioxygen Inorganic materials 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001125 extrusion Methods 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 235000021107 fermented food Nutrition 0.000 description 2
- MSNWSDPPULHLDL-UHFFFAOYSA-K ferric hydroxide Chemical compound [OH-].[OH-].[OH-].[Fe+3] MSNWSDPPULHLDL-UHFFFAOYSA-K 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 235000011194 food seasoning agent Nutrition 0.000 description 2
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- 150000004679 hydroxides Chemical class 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229920000831 ionic polymer Polymers 0.000 description 2
- 229910000398 iron phosphate Inorganic materials 0.000 description 2
- 159000000014 iron salts Chemical class 0.000 description 2
- 229910000358 iron sulfate Inorganic materials 0.000 description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 2
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 description 2
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 description 2
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 2
- 238000010030 laminating Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 235000013372 meat Nutrition 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 2
- 235000013536 miso Nutrition 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012778 molding material Substances 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 2
- 239000004645 polyester resin Substances 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 229920002223 polystyrene Polymers 0.000 description 2
- 229920005990 polystyrene resin Polymers 0.000 description 2
- 229920000915 polyvinyl chloride Polymers 0.000 description 2
- 239000004800 polyvinyl chloride Substances 0.000 description 2
- 239000005033 polyvinylidene chloride Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 235000012045 salad Nutrition 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- 229920002554 vinyl polymer Polymers 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 description 1
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- 150000000180 1,2-diols Chemical group 0.000 description 1
- FJLUATLTXUNBOT-UHFFFAOYSA-N 1-Hexadecylamine Chemical compound CCCCCCCCCCCCCCCCN FJLUATLTXUNBOT-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- QLZJUIZVJLSNDD-UHFFFAOYSA-N 2-(2-methylidenebutanoyloxy)ethyl 2-methylidenebutanoate Chemical class CCC(=C)C(=O)OCCOC(=O)C(=C)CC QLZJUIZVJLSNDD-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- HOVLEIUJGCUOMI-UHFFFAOYSA-N 2-(butanoyloxymethyl)prop-2-enyl butanoate Chemical compound CCCC(=O)OCC(=C)COC(=O)CCC HOVLEIUJGCUOMI-UHFFFAOYSA-N 0.000 description 1
- SIWMBFPZQRYWLS-UHFFFAOYSA-N 2-methyl-1,3-dipropoxypropane Chemical compound CCCOCC(C)COCCC SIWMBFPZQRYWLS-UHFFFAOYSA-N 0.000 description 1
- JFFYKITVXPZLQS-UHFFFAOYSA-N 2-methylidenepropane-1,3-diol Chemical compound OCC(=C)CO JFFYKITVXPZLQS-UHFFFAOYSA-N 0.000 description 1
- AUZRCMMVHXRSGT-UHFFFAOYSA-N 2-methylpropane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CC(C)CS(O)(=O)=O AUZRCMMVHXRSGT-UHFFFAOYSA-N 0.000 description 1
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
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- FFHDFBALZJMPST-UHFFFAOYSA-N 3-ethoxy-2-(ethoxymethyl)prop-1-ene Chemical compound CCOCC(=C)COCC FFHDFBALZJMPST-UHFFFAOYSA-N 0.000 description 1
- OFNISBHGPNMTMS-UHFFFAOYSA-N 3-methylideneoxolane-2,5-dione Chemical compound C=C1CC(=O)OC1=O OFNISBHGPNMTMS-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
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- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 description 1
- 239000005695 Ammonium acetate Substances 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 235000021357 Behenic acid Nutrition 0.000 description 1
- CCTSBABCCIPBKG-UHFFFAOYSA-N CC=CCCCCCCCCCCCCCCCCCN Chemical compound CC=CCCCCCCCCCCCCCCCCCN CCTSBABCCIPBKG-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 244000223760 Cinnamomum zeylanicum Species 0.000 description 1
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical group ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 1
- UAUDZVJPLUQNMU-UHFFFAOYSA-N Erucasaeureamid Natural products CCCCCCCCC=CCCCCCCCCCCCC(N)=O UAUDZVJPLUQNMU-UHFFFAOYSA-N 0.000 description 1
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 1
- 229910021577 Iron(II) chloride Inorganic materials 0.000 description 1
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- 150000003609 titanium compounds Chemical class 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/02—Homopolymers or copolymers of unsaturated alcohols
- C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B9/00—Making granules
- B29B9/12—Making granules characterised by structure or composition
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B25/042—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material of natural rubber or synthetic rubber
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B25/08—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/14—Layered products comprising a layer of natural or synthetic rubber comprising synthetic rubber copolymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
本發明提供一種乙烯-乙烯醇系共聚物組成物,以作為即便不摻合公知的紫外線吸收劑仍具有良好的紫外線吸收能力,熱穩定性優異,且著色受到抑制的乙烯-乙烯醇系共聚物組成物,其含有乙烯-乙烯醇系共聚物(A)、苯乙烯衍生物(B)及鐵化合物(C),且每單位重量之乙烯-乙烯醇系共聚物組成物中,該鐵化合物(C)之含量以金屬換算計為0.01~5ppm。
Description
本發明係關於以乙烯-乙烯醇系共聚物(以下有時簡稱為「EVOH樹脂」。)作為主成分之EVOH樹脂組成物、及由其構成之丸粒、及具有由其構成之層之多層結構體,更詳言之,係關於具有紫外線吸收能力之EVOH樹脂組成物、由該EVOH樹脂組成物構成之丸粒、及具有由EVOH樹脂組成物構成之層之多層結構體。
EVOH樹脂的透明性、氧氣等之氣體阻隔性、保香性、耐溶劑性、耐油性、機械強度等優異,人們將其成形為薄膜、片、瓶等並廣泛使用作為食品包裝材料、醫藥品包裝材料、工業藥品包裝材料、農藥包裝材料等各種包裝材料。
不過,食品、藥品等中會因紫外線而劣化、變質者為多數,而有其包裝材須具有紫外線吸收能力之需求。就賦予包裝材料紫外線吸收能力之方法而言,一般會在作為包裝材料使用的樹脂中摻合紫外線吸收劑。例如有人提案一種疊層結構體,係將由聚烯烴與EVOH樹脂構成之層疊層而得,並對於其一部分之層或全部之層混入紫外線吸收劑,從而使紫外線之穿透率減低(例如參照專利文獻1)。 [先前技術文獻] [專利文獻]
[專利文獻1]日本特開2008-230112號公報
[發明所欲解決之課題]
然而,紫外線吸收劑一般為低分子化合物,故成為成形品後容易在樹脂中遷移,而有使用中遷移至層表面而與內容物接觸、或使表面發黏之問題點。又,為了獲得充分的紫外線吸收能力,須在樹脂中摻合大量之紫外線吸收劑,結果有使樹脂特性降低之傾向。
本案發明人等在解決該課題並獲得即便不摻合公知的紫外線吸收劑仍具有良好的紫外線吸收能力的EVOH樹脂組成物之際,想到使用鐵化合物。然而,EVOH樹脂組成物中摻合鐵化合物時,紫外線吸收能力及熱穩定性會與摻合量成比例地提升,但熔融成形時有著色之傾向。
亦即,本發明提供即便不摻合公知的紫外線吸收劑仍具有紫外線吸收能力,熱穩定性優異,且著色受到抑制的EVOH樹脂組成物、丸粒及多層結構體。 [解決課題之手段]
本案發明人等鑑於上述實情努力進行探討,結果發現藉由對於EVOH樹脂併用特定微量的鐵化合物與苯乙烯衍生物(B),獲得的樹脂組成物具有紫外線吸收能力,熱穩定性優異,且著色受到抑制,乃完成本發明。
亦即,本發明之第1要旨為一種EVOH樹脂組成物,含有EVOH樹脂(A)、苯乙烯衍生物(B)及鐵化合物(C),其特徵為:每單位重量之EVOH樹脂組成物中,該鐵化合物(C)之含量以金屬換算計為0.01~5ppm。又,本發明之第2要旨為一種丸粒,係由上述EVOH樹脂組成物構成。又,本發明之第3要旨為一種多層結構體,具有由上述EVOH樹脂組成物構成之層。 [發明之效果]
本發明之EVOH樹脂組成物含有EVOH樹脂(A)、苯乙烯衍生物(B)及鐵化合物(C),且每單位重量之EVOH樹脂組成物中,該鐵化合物(C)之含量以金屬換算計為0.01~5ppm。因此,本發明之EVOH樹脂組成物,不使用有表面遷移、妨礙樹脂特性之疑慮之紫外線吸收劑而仍具有紫外線吸收能力,熱穩定性優異,而且可抑制加熱時之著色。
又,本發明之中,尤其每單位重量之EVOH樹脂組成物中上述苯乙烯衍生物(B)之含量為1~1000ppm的話,可成為具有更優異之紫外線吸收能力及熱穩定性,且加熱時之著色更受到抑制者。
而且,本發明之中,尤其上述苯乙烯衍生物(B)之含量相對於上述鐵化合物(C)之金屬換算含量之重量比為0.2~50000的話,可成為具有更優異之紫外線吸收能力及熱穩定性,且加熱時之著色更受到抑制者。
又,由本發明之EVOH樹脂組成物構成之丸粒,具有紫外線吸收能力,熱穩定性優異,且加熱時之著色受到抑制,故可適用作為包裝材料之原料。
而且,具有含有本發明之EVOH樹脂組成物之層之多層結構體,具有紫外線吸收能力,熱穩定性優異,且加熱時之著色受到抑制,故作為食品之包裝材料係特別有用。
以下針對本發明之構成詳細地說明,但該等係展示理想實施態樣之一例,並不限於該等內容。
本發明之EVOH樹脂組成物係以EVOH樹脂(A)作為主成分,並含有苯乙烯衍生物(B)及鐵化合物(C)。本發明之EVOH樹脂組成物的基礎樹脂為EVOH樹脂(A)。亦即,EVOH樹脂組成物中之EVOH樹脂(A)之含量通常為70重量%以上,較佳為80重量%以上,更佳為90重量%以上,特佳為95重量%以上。 以下針對各成分進行說明。
[EVOH樹脂(A)] 本發明使用之EVOH樹脂(A),通常為將係為乙烯與乙烯酯系單體之共聚物的乙烯-乙烯酯系共聚物予以皂化而得之樹脂,為非水溶性之熱塑性樹脂。就上述乙烯酯系單體而言,考量經濟方面,一般會使用乙酸乙烯酯。 就乙烯與乙烯酯系單體之聚合法而言,可使用公知的任意聚合法,例如溶液聚合、懸浮聚合、乳化聚合等並實施,一般會使用以甲醇作為溶劑之溶液聚合。得到的乙烯-乙烯酯系共聚物之皂化亦能以公知的方法實施。 以上述方式製造之EVOH樹脂(A),係以來自乙烯之結構單元與乙烯醇結構單元為主,並含有未皂化而殘存之些許量之乙烯酯結構單元。
作為上述乙烯酯系單體,考量市場取得性、製造時之雜質處理效率佳之觀點,典型會使用乙酸乙烯酯。作為其它乙烯酯系單體,例如可列舉甲酸乙烯酯、丙酸乙烯酯、戊酸乙烯酯、丁酸乙烯酯、異丁酸乙烯酯、三甲基乙酸乙烯酯、癸酸乙烯酯、月桂酸乙烯酯、硬脂酸乙烯酯、叔碳酸乙烯酯等脂肪族乙烯酯、苯甲酸乙烯酯等芳香族乙烯酯等,可使用通常為碳數3~20,較佳為碳數4~10,特佳為碳數4~7之脂肪族乙烯酯。該等通常單獨使用,但視需要也可同時使用多種。
EVOH樹脂(A)中之乙烯結構單元之含量,可利用使乙烯酯系單體與乙烯進行共聚合時之乙烯之壓力進行控制,通常為20~60莫耳%,較佳為25~50莫耳%,特佳為28~45莫耳%。該含量過低時,有高濕下之氣體阻隔性、延伸性降低之傾向;反之過高時,有氣體阻隔性降低之傾向。 另外,該乙烯結構單元之含量可根據ISO14663進行測定。
EVOH樹脂(A)中之乙烯酯成分之皂化度,可利用將乙烯-乙烯酯系共聚物進行皂化時之皂化觸媒(通常使用氫氧化鈉等鹼性觸媒)之量、溫度、時間等進行控制,通常為90~100莫耳%,較佳為95~100莫耳%,特佳為99~100莫耳%。該皂化度過低時,有氣體阻隔性、熱穩定性、耐濕性等降低之傾向。 該EVOH樹脂(A)之皂化度可根據JIS K6726(惟,EVOH樹脂係以使其均勻地溶解於水/甲醇溶劑而成之溶液的形式使用)進行測定。
又,該EVOH樹脂(A)之熔體流動速率(MFR)(210℃,荷重2160g),通常為0.5~100g/10分鐘,較佳為1~50g/10分鐘,特佳為3~35g/10分鐘。該MFR過大時,有損及製膜時之穩定性之傾向;過小時,有黏度變得過高而熔融擠製變得困難之傾向。 該MFR係為EVOH樹脂之聚合度之指標,可藉由將乙烯與乙烯酯系單體進行共聚合時之聚合起始劑之量、溶劑之量進行調整。
本發明使用之EVOH樹脂(A)中,也可在不妨礙本發明之效果之範圍(例如EVOH樹脂(A)之10莫耳%以下)更含有來自以下所示之共聚單體之結構單元。 就前述共聚單體而言,可列舉:丙烯、1-丁烯、異丁烯等烯烴類、3-丁烯-1-醇、3-丁烯-1,2-二醇、4-戊烯-1-醇、5-己烯-1,2-二醇等含羥基之α-烯烴類或其酯化物、醯基化物等衍生物;2-亞甲基丙烷-1,3-二醇、3-亞甲基戊烷-1,5-二醇等羥烷基亞乙烯類;1,3-二乙醯氧基-2-亞甲基丙烷、1,3-二丙醯氧基-2-亞甲基丙烷、1,3-二丁醯氧基-2-亞甲基丙烷等二乙酸羥烷基亞乙烯酯類;丙烯酸、甲基丙烯酸、巴豆酸、苯二甲酸(酐)、馬來酸(酐)、伊康酸(酐)等不飽和酸類或其鹽或其碳數1~18之單或二烷基酯類;丙烯醯胺、碳數1~18之N-烷基丙烯醯胺、N,N-二甲基丙烯醯胺、2-丙烯醯胺丙烷磺酸或其鹽、丙烯醯胺丙基二甲基胺或其酸鹽或其4級鹽等丙烯醯胺類;甲基丙烯醯胺、碳數1~18之N-烷基甲基丙烯醯胺、N,N-二甲基甲基丙烯醯胺、2-甲基丙烯醯胺丙烷磺酸或其鹽、甲基丙烯醯胺丙基二甲基胺或其酸鹽或其4級鹽等甲基丙烯醯胺類;N-乙烯基吡咯烷酮、N-乙烯基甲醯胺、N-乙烯基乙醯胺等N-乙烯基醯胺類;丙烯腈、甲基丙烯腈等氰化乙烯類;碳數1~18之烷基乙烯醚、羥烷基乙烯醚、烷氧烷基乙烯醚等乙烯醚類;氯乙烯、偏二氯乙烯、氟乙烯、偏二氟乙烯、溴乙烯等鹵化乙烯化合物類;三甲氧基乙烯基矽烷等乙烯基矽烷類;乙酸烯丙酯、氯丙烯等鹵化烯丙基化合物類;烯丙醇、二甲氧基烯丙醇等烯丙醇類;三甲基-(3-丙烯醯胺-3-二甲基丙基)-氯化銨、丙烯醯胺-2-甲基丙烷磺酸等共聚單體。可將它們單獨使用或併用2種以上。
尤其,考量保持氣體阻隔性且同時二次成形性為良好之觀點,於側鏈具有1級羥基之EVOH樹脂為較佳,其中,又以經共聚合含羥基之α-烯烴類而得之EVOH樹脂較佳,於側鏈具有1,2-二醇結構之EVOH樹脂尤佳。 尤其,為於側鏈具有1級羥基之EVOH樹脂時,來自具有該1級羥基之單體之結構單元之含量,通常為EVOH樹脂之0.1~20莫耳%,更佳為0.5~15莫耳%,特佳為1~10莫耳%。
又,本發明使用之EVOH樹脂(A)也可為經胺甲酸酯化、縮醛化、氰乙基化、氧伸烷基化等「後改性」而得者。
再者,本發明使用之EVOH樹脂(A)也可為和不同的其它EVOH樹脂之混合物,作為該其它EVOH樹脂可列舉乙烯結構單元之含量不同者、皂化度不同者、聚合度不同者、共聚合成分不同者等。
[苯乙烯衍生物(B)] 本發明使用之苯乙烯衍生物(B),係指具有將自由基予以共振穩定化並捕捉之能力之芳香族化合物,具體而言,為具有苯乙烯分子結構作為分子骨架的化合物。較佳為在α位或β位具有取代基的苯乙烯化合物。
例如,在α位具有取代基之苯乙烯化合物,就利用苄基位將自由基予以共振穩定化之觀點為較佳,具體可列舉2,4-二苯基-4-甲基-1-戊烯等。在β位具有取代基之苯乙烯化合物為在β位具有羰基之苯乙烯化合物時,就具有烯酮(enone)結構將自由基予以共振穩定化之觀點為較佳,例如可列舉桂皮酸、桂皮酸醇、桂皮酸酯、桂皮酸鹽等桂皮酸衍生物。其中又以使用桂皮酸為最理想。
上述苯乙烯衍生物(B)之分子量通常為100~100000,較佳為100~10000,特佳為100~1000,極佳為130~300。分子量為上述範圍內時,有更有效地獲得本發明之效果之傾向。
相對於本發明之EVOH樹脂組成物全體,苯乙烯衍生物(B)之含量以重量基準計通常為1~1000ppm,較佳為10~800ppm,特佳為50~600ppm。過多時,有生產性降低之傾向;過少時,有熱穩定性降低之傾向。
另外,成為上述苯乙烯衍生物(B)之含有比例之基準的EVOH樹脂組成物,為含有EVOH樹脂(A)、苯乙烯衍生物(B)、鐵化合物(C)、視需要而摻合之各種添加劑等的作為最終製品的EVOH樹脂組成物。
本發明之EVOH樹脂組成物中之苯乙烯衍生物(B)之含量,例如可使用液體層析質量分析法(LC/MS/MS)並根據下列程序進行測定。另外,下列程序係以使用桂皮酸之情形為例進行記載,但針對其它苯乙烯衍生物(B)也能以同樣的程序進行測定。
<苯乙烯衍生物(B)之含量之測定方法> [標準溶液之製備] 將桂皮酸(10.89mg)秤量於10mL定量瓶中,將其溶解於甲醇而製成10mL溶液(標準原液;1089μg/mL)。接著,將製備而得之標準原液以甲醇稀釋,製備多個濃度(0.109μg/mL、0.218μg/mL、0.545μg/mL、1.09μg/mL、2.18μg/mL)的各混合標準溶液。使用該等混合標準溶液實施LC/MS/MS分析,製作成檢量線。
[試樣溶液之製備] (1)將經粉碎之本發明之EVOH樹脂組成物之丸粒(1g)秤量於10mL定量瓶中,然後加入甲醇9mL。 (2)實施120分鐘超音波處理後,於室溫(25℃)放置冷卻。 (3)加入甲醇並定容至10mL(試樣溶液(I))。 (4)取試樣溶液(I)1mL於10mL定量瓶中,然後加入甲醇並定容至10mL(試樣溶液(II))。 (5)將試樣溶液(I)或試樣溶液(II)經以PTFE過濾器(0.45μm)過濾而得之液體作為測定溶液而供於LC/MS/MS分析。 從經LC/MS/MS分析檢測而得之峰部面積值、與標準溶液之檢量線算出桂皮酸之檢測濃度。
[LC/MS/MS測定條件] LC系統: LC-20A[島津製作所公司製] 質量分析計: API4000[AB/MDS Sciex] 分析管柱: Scherzo SM-C18(3.0×75mm,3μm) 管柱溫度: 45℃ 移動相: A 10mmol/L 乙酸銨水溶液 B 甲醇 時間程序: 0.0→5.0min B%=30%→95% 5.0→10.0min B%=95% 10.1→15.0min B%=30% 流量: 0.4mL/min 切換閥: 2.0 to 6.0min:to MS 注入量: 5μL 離子化: ESI法 檢測: 負離子檢測(SRM法) 監測離子: Q1=147.0→Q3=102.9(CE:-15eV)
[鐵化合物(C)] 本發明之特徵為:含有EVOH樹脂(A)、苯乙烯衍生物(B)及鐵化合物(C),且鐵化合物(C)之摻合量為特定微量。發現藉由採用該構成,獲得的樹脂組成物具有紫外線吸收能力,熱穩定性優異,且著色受到抑制。
另外,該鐵化合物(C),在EVOH樹脂組成物中除了以氧化物、氫氧化物、氯化物、鐵鹽之形式存在之情況以外,也可以例如離子化之狀態、或與樹脂、其它配位子相互作用而成之錯合物之狀態存在。作為上述氧化物,例如可列舉氧化鐵(III)、四氧化三鐵、氧化亞鐵等。作為上述氯化物,例如可列舉氯化鐵(II)、氯化鐵(III)等。作為上述氫氧化物,例如可列舉氫氧化鐵(II)、氫氧化鐵(III)等。作為上述鐵鹽,例如可列舉磷酸鐵、硫酸鐵等無機鹽、羧酸(乙酸、丁酸、硬脂酸等)鐵等有機鹽。可將它們單獨使用或併用2種以上。
考量在EVOH樹脂組成物中之分散性之觀點,鐵化合物(C)宜為水溶性。又,考量分散性與生產性之觀點,其分子量通常為100~10000,較佳為100~1000,特佳為100~500。
本發明之EVOH樹脂組成物之特徵為:每單位重量之EVOH樹脂組成物中,鐵化合物(C)之含量以金屬換算計為0.01~5ppm。該鐵化合物之含量較佳為0.05~3ppm,特佳為0.08~1ppm。 鐵化合物之含量過少的話,有紫外線吸收能力降低之傾向;過多的話,有成形物著色之傾向。
在此,鐵化合物(C)之含量係指利用下列方法進行測定而得者。 <鐵化合物(C)之分析> 將EVOH樹脂組成物丸粒之粉碎物0.5g利用紅外線加熱爐在氧氣氣流中於650℃進行1小時灰化處理,然後將灰分溶解於酸並以純水定容,將其作為試樣溶液。將該溶液利用Agilent Technologies公司製 ICP質量分析裝置 7500ce型,依ICP-MS標準添加法進行測定。
本發明之EVOH樹脂組成物中前述苯乙烯衍生物(B)之含量相對於上述鐵化合物(C)之金屬換算含量之重量比,通常為0.2~50000,較佳為1~20000,特佳為100~10000,極佳為1000~8000。該值過大時,有紫外線吸收能力變低之傾向;過小時,有成形物著色之傾向。
[其它熱塑性樹脂] 本發明之EVOH樹脂組成物中,可在不妨礙本發明之效果之範圍(例如通常為EVOH樹脂組成物之30重量%以下,較佳為20重量%以下,特佳為10重量%以下)含有EVOH樹脂(A)以外之熱塑性樹脂。 就其它熱塑性樹脂而言,可使用公知的熱塑性樹脂。例如可具體列舉:聚醯胺系樹脂、聚烯烴系樹脂、聚酯系樹脂、聚苯乙烯系樹脂、聚氯乙烯系樹脂、聚碳酸酯系樹脂、聚丙烯酸系樹脂、離子聚合物、乙烯-丙烯酸共聚物、乙烯-丙烯酸酯共聚物、乙烯-甲基丙烯酸共聚物、乙烯-甲基丙烯酸酯共聚物、聚偏二氯乙烯、乙烯酯系樹脂、聚酯彈性體、聚胺甲酸酯彈性體、氯化聚乙烯、氯化聚丙烯等。可將它們單獨使用或併用2種以上。
[其它摻合劑] 又,本發明之EVOH樹脂組成物中,也可在不妨礙本發明之效果之範圍含有一般摻合於EVOH樹脂之摻合劑。例如也可摻合無機複鹽(例如菱水鎂鋁石等)、塑化劑(例如乙二醇、甘油、己二醇等脂肪族多元醇等)、氧吸收劑[例如:鋁粉、亞硫酸鉀、光觸媒氧化鈦等無機系氧吸收劑;抗壞血酸、再者其脂肪酸酯或金屬鹽等、氫醌、没食子酸、含羥基之酚醛樹脂等多元酚類、雙水楊醛-亞胺鈷、四亞乙基五胺鈷、鈷-希夫鹼錯合物、卟啉類、大環狀聚胺錯合物、聚乙烯亞胺-鈷錯合物等含氮化合物與鐵以外之過渡金屬的配位結合體、萜烯化合物、胺基酸類與含羥基之還原性物質之反應產物、三苯基甲基化合物等有機化合物系氧吸收劑;含氮樹脂與鐵以外之過渡金屬的配位結合體(例如間二甲苯二胺(MXD)尼龍與鈷的組合)、含三級氫之樹脂與鐵以外之過渡金屬的混摻物(例如聚丙烯與鈷的組合)、含碳-碳不飽和鍵之樹脂與鐵以外之過渡金屬的混摻物(例如聚丁二烯與鈷的組合)、光氧化降解性樹脂(例如聚酮)、蔥醌聚合物(例如聚乙烯蔥醌)等、進一步於該等之摻合物添加光起始劑(二苯甲酮等)、上述以外之抗氧化或消臭劑(活性碳等)而成者等高分子系氧吸收劑]、熱穩定劑、光穩定劑、紫外線吸收劑、著色劑、抗靜電劑、界面活性劑(惟,作為潤滑劑使用者除外)、抗菌劑、防黏連劑、填充材(例如無機填料等)等。可將該等化合物單獨使用或併用2種以上。
[EVOH樹脂組成物之製造方法] 就製造本發明之EVOH樹脂組成物之方法而言,例如可列舉乾式混摻法、熔融混合法、溶液混合法、含浸法等公知的方法,也可將該等方法任意地組合。
就乾式混摻法而言,例如可列舉:(i)使用滾筒等將EVOH樹脂(A)丸粒、苯乙烯衍生物(B)及鐵化合物(C)予以乾式混摻之方法等。
就熔融混合法而言,例如可列舉:(ii)將EVOH樹脂(A)丸粒、苯乙烯衍生物(B)及鐵化合物(C)之乾式混摻物進行熔融混練,並得到丸粒或成形物之方法;(iii)於熔融狀態之EVOH樹脂(A)添加苯乙烯衍生物(B)、鐵化合物(C)後進行熔融混練,並得到丸粒或成形物之方法等。
就溶液混合法而言,例如可列舉:(iv)使用市售之EVOH樹脂(A)丸粒來製備溶液,於此溶液摻合苯乙烯衍生物(B)及鐵化合物(C)中之至少一者,予以凝固成形並造粒,進行固液分離後予以乾燥之方法;(v)在EVOH樹脂(A)之製造過程中,使皂化前之乙烯-乙烯酯系共聚物溶液、EVOH樹脂之均勻溶液(水/醇溶液等)含有苯乙烯衍生物(B)及鐵化合物(C)中之至少一者,然後予以凝固成形並造粒,進行固液分離後予以乾燥之方法等。
就含浸法而言,例如可列舉:(vi)使EVOH樹脂(A)丸粒與含有苯乙烯衍生物(B)及鐵化合物(C)中之至少一者之水溶液接觸,使EVOH樹脂(A)丸粒中含有苯乙烯衍生物(B)及鐵化合物(C)中之至少一者後,予以乾燥之方法等。
又,可列舉:(vii)利用齒輪泵等來輸送含有高濃度之非氧化性之酸(例如鹽酸、乙酸)的EVOH樹脂(A)之甲醇溶液,藉此使微量之鐵化合物(C)從齒輪泵之驅動部之不銹鋼溶出,而對於EVOH樹脂(A)摻合微量之鐵化合物(C)。從該處理後之EVOH樹脂(A)之甲醇溶液得到含有EVOH樹脂(A)及鐵化合物(C)之EVOH樹脂(A)丸粒,將該含鐵化合物(C)之EVOH樹脂(A)丸粒與苯乙烯衍生物(B)進行乾式混摻及熔融混練中之至少一者,而獲得丸粒之方法;或利用含浸法使上述含鐵化合物(C)之EVOH樹脂(A)丸粒含有苯乙烯衍生物(B),然後予以乾燥而獲得丸粒之方法等。
本發明中,可組合上述不同的方法。其中,考量生產性之觀點,宜使皂化前之乙烯-乙烯酯系共聚物溶液含有苯乙烯衍生物(B),利用常法進行皂化,針對得到的EVOH樹脂(A)溶液視需要使用水來調整溶劑,並將該EVOH樹脂(A)溶液供於(vii)之方法。再者,考量生產性、獲得本發明之效果更為顯著的樹脂組成物之觀點,熔融混合法較佳,(ii)之方法尤佳。
另外,利用上述各方法獲得之本發明之EVOH樹脂組成物丸粒、各方法中使用之EVOH樹脂(A)丸粒的形狀為任意。例如有球形、卵形、圓柱形、立方體形、長方體形等,通常為卵形、或圓柱形,就其大小而言,考量後續作為成形材料使用時之便利性之觀點,為卵形時短徑通常為1~10mm,較佳為2~6mm,更佳為2.5~5.5mm,長徑通常為1.5~30mm,較佳為3~20,更佳為3.5~10mm。又,為圓柱形時底面之直徑通常為1~6mm,較佳為2~5mm,長度通常為1~6mm,較佳為2~5mm。
又,上述各方法中使用之鐵化合物(C),如前述宜使用水溶性之鐵化合物,例如可列舉:氧化鐵(III)、四氧化三鐵、氧化亞鐵等氧化物、氯化鐵(II)、氯化鐵(III)等氯化物、氫氧化鐵(II)、氫氧化鐵(III)等氫氧化物、磷酸鐵、硫酸鐵等無機鹽、羧酸(乙酸、丁酸、硬脂酸等)鐵等有機鹽等鐵鹽。另外,該鐵化合物(C),如前述在EVOH樹脂組成物中除了以上述鹽之形式存在之情況以外,也可以離子化之狀態、或以將樹脂、其它化合物作為配位子而成之錯合物之狀態存在。
又,就上述(vi)之方法中使用之含有鐵化合物(C)之水溶液而言,可使用上述鐵化合物(C)之水溶液、藉由將鐵鋼材料浸漬於含有各種藥劑之水中而使鐵離子溶出而成者。另外,此時EVOH樹脂組成物中之鐵化合物(C)之含量(金屬換算),可藉由浸漬EVOH樹脂(A)丸粒之水溶液中之鐵化合物之濃度、浸漬溫度、浸漬時間等進行控制。上述浸漬時間通常為0.5~48小時,較佳為1~36小時,上述浸漬溫度通常為10~40℃,較佳為20~35℃。 將該EVOH樹脂組成物丸粒利用公知的方法進行固液分離,並以公知的乾燥方法進行乾燥。該乾燥方法可採用各種之乾燥方法,可為靜置乾燥、流動乾燥中之任一者。又,也可將該等組合並實施。
本發明之EVOH樹脂組成物丸粒之含水率,通常為0.01~0.5重量%,較佳為0.05~0.35重量%,特佳為0.1~0.3重量%。
另外,本發明之EVOH樹脂組成物丸粒之含水率係利用以下方法測定、算出。 利用電子天秤秤量EVOH樹脂組成物丸粒之乾燥前重量(W1),使其於150℃之熱風乾燥機中乾燥5小時並於乾燥器中放置冷卻30分鐘後秤量重量(W2),依下式算出。 含水率(重量%)=[(W1-W2)/W1]×100
以此方式得到的EVOH樹脂組成物之丸粒可直接供於熔融成形,但考量使熔融成形時之饋料性穩定之觀點,也宜使公知的潤滑劑附著於丸粒的表面。就潤滑劑之種類而言,例如可列舉:碳數12以上之高級脂肪酸(例如月桂酸、肉豆蔻酸、棕櫚酸、硬脂酸、二十二酸、油酸等)、高級脂肪酸酯(例如高級脂肪酸之甲酯、異丙酯、丁酯、辛酯等)、高級脂肪醯胺(例如月桂醯胺、肉豆蔻醯胺、棕櫚醯胺、硬脂醯胺、二十二醯胺等飽和高級脂肪醯胺;油醯胺、芥醯胺等不飽和高級脂肪醯胺、伸乙基雙硬脂醯胺、伸乙基雙油醯胺、伸乙基雙芥醯胺、伸乙基雙月桂醯胺等雙高級脂肪醯胺等)、低分子量聚烯烴(例如分子量約500~10000之低分子量聚乙烯或低分子量聚丙烯等、或其酸改性品)、碳數6以上之高級醇、酯寡聚物、氟化乙烯樹脂等。可將該等化合物單獨使用或併用2種以上。又,該潤滑劑之含量通常為EVOH樹脂組成物之5重量%以下,較佳為1重量%以下。
將以此方式得到的本發明之EVOH樹脂組成物製備成丸粒、或粉末狀、液體狀等各式各樣形態之EVOH樹脂組成物,並提供作為各種成形物的成形材料。尤其本發明中,提供作為熔融成形用之材料時,有更有效地獲得本發明之效果之傾向,較為理想。另外,本發明之EVOH樹脂組成物也包含混合本發明之EVOH樹脂組成物中使用之EVOH樹脂(A)以外之樹脂而得之樹脂組成物。
而且,就該成形物而言,能以使用本發明之EVOH樹脂組成物成形而得之單層薄膜之形式、具有使用本發明之EVOH樹脂組成物成形而得之層的多層結構體之形式供於實用。
[多層結構體] 本發明之多層結構體具有由上述本發明之EVOH樹脂組成物構成之層。含有本發明之EVOH樹脂組成物之層(以下簡單稱為「EVOH樹脂組成物層」。),藉由和以本發明之EVOH樹脂組成物以外之熱塑性樹脂作為主成分之其它基材(以下有時將基材中使用之樹脂簡稱為「基材樹脂」。)疊層,可進一步賦予強度、保護EVOH樹脂組成物層不受水分等之影響、或賦予其它機能。
作為上述基材樹脂,例如可列舉:包括直鏈狀低密度聚乙烯、低密度聚乙烯、超低密度聚乙烯、中密度聚乙烯、高密度聚乙烯、乙烯-丙烯(嵌段及無規)共聚物、乙烯-α-烯烴(碳數4~20之α-烯烴)共聚物等聚乙烯系樹脂、聚丙烯、丙烯-α-烯烴(碳數4~20之α-烯烴)共聚物等聚丙烯系樹脂、聚丁烯、聚戊烯、聚環狀烯烴系樹脂(於主鏈及側鏈之至少一者具有環狀烯烴結構的聚合物)等(未改性)聚烯烴系樹脂、該等聚烯烴類經以不飽和羧酸或其酯接枝改性而得之不飽和羧酸改性聚烯烴系樹脂等改性烯烴系樹脂的廣義的聚烯烴系樹脂、離子聚合物、乙烯-乙酸乙烯酯共聚物、乙烯-丙烯酸共聚物、乙烯-丙烯酸酯共聚物、聚酯系樹脂、聚醯胺系樹脂(亦包括共聚合聚醯胺)、聚氯乙烯、聚偏二氯乙烯、丙烯酸系樹脂、聚苯乙烯系樹脂、乙烯酯系樹脂、聚酯系彈性體、聚胺甲酸酯系彈性體、聚苯乙烯系彈性體、氯化聚乙烯、氯化聚丙烯等鹵化聚烯烴、芳香族或脂肪族聚酮類等。
該等之中,係疏水性樹脂的聚醯胺系樹脂、聚烯烴系樹脂、聚酯系樹脂、聚苯乙烯系樹脂為較佳,更佳為聚乙烯系樹脂、聚丙烯系樹脂、聚環狀烯烴系樹脂及它們的不飽和羧酸改性聚烯烴系樹脂等聚烯烴系樹脂。
多層結構體之層構成,令本發明之EVOH樹脂組成物層為a(a1、a2、・・・)、基材樹脂層為b(b1、b2、・・・)時,可為a/b、b/a/b、a/b/a、a1/a2/b、a/b1/b2、b2/b1/a/b1/b2、b2/b1/a/b1/a/b1/b2等任意之組合。又,令將製造該多層結構體之過程中產生之端部、不良品等予以再熔融成形而得之含有本發明之EVOH樹脂組成物與本發明之EVOH樹脂組成物以外之熱塑性樹脂之混合物的再生層為R時,也可為b/R/a、b/R/a/b、b/R/a/R/b、b/a/R/a/b、b/R/a/R/a/R/b等。多層結構體之層數以總數計通常為2~15,較佳為3~10。視需要也可使含有黏著性樹脂的黏著性樹脂層介隔於上述層構成之各層間。
上述黏著性樹脂可使用公知者,因應基材樹脂「b」中使用之熱塑性樹脂之種類適當地選擇即可。典型可列舉利用加成反應、接枝反應等使不飽和羧酸或其酐化學性地鍵結於聚烯烴系樹脂而得之含羧基之改性聚烯烴系聚合物。作為上述含羧基之改性聚烯烴系聚合物,例如可列舉:馬來酸酐接枝改性聚乙烯、馬來酸酐接枝改性聚丙烯、馬來酸酐接枝改性乙烯-丙烯(嵌段及無規)共聚物、馬來酸酐接枝改性乙烯-丙烯酸乙酯共聚物、馬來酸酐接枝改性乙烯-乙酸乙烯酯共聚物、馬來酸酐改性聚環狀烯烴系樹脂、馬來酸酐接枝改性聚烯烴系樹脂等。而且,可使用選自於該等中之1種或2種以上之混合物。
在多層結構體中,於本發明之EVOH樹脂組成物層與基材樹脂層之間使用黏著性樹脂層時,黏著性樹脂層位在EVOH樹脂組成物層之兩側,故宜使用疏水性優異之黏著性樹脂。
上述基材樹脂、黏著性樹脂中,也可在不妨礙本發明之要旨之範圍(例如相對於樹脂全體為30重量%以下,較佳為10重量%以下)含有習知的塑化劑、填料、黏土(蒙脫石等)、著色劑、抗氧化劑、抗靜電劑、潤滑劑、成核劑、防黏連劑、蠟等。可將它們單獨使用或併用2種以上。
本發明之EVOH樹脂組成物層與上述基材樹脂層之疊層(包括使黏著性樹脂層介隔之情形)可利用公知的方法實施。例如可列舉:將基材樹脂熔融擠製層合於本發明之EVOH樹脂組成物之薄膜、片等之方法;將本發明之EVOH樹脂組成物熔融擠製層合於基材樹脂層之方法;將EVOH樹脂組成物與基材樹脂進行共擠製之方法;使用有機鈦化合物、異氰酸酯化合物、聚酯系化合物、聚胺甲酸酯化合物等公知的黏著劑將EVOH樹脂組成物(層)與基材樹脂(層)予以乾層合之方法;於基材樹脂上塗覆EVOH樹脂組成物之溶液後將溶劑除去之方法等。該等之中,考量成本、環境之觀點,又以進行共擠製之方法較佳。
如上述的多層結構體,視需要可接著施以(加熱)延伸處理。延伸處理可為單軸延伸、雙軸延伸中之任一者,雙軸延伸時可為同時延伸,也可為逐次延伸。又,就延伸方法而言,也可採用輥延伸法、拉幅機延伸法、管狀延伸法、延伸吹塑法、真空壓空成形等當中之延伸倍率較高者。延伸溫度為多層結構體之熔點附近之溫度,通常選自約40~170℃之範圍,較佳為選自約60~160℃之範圍。延伸溫度過低時,延伸性變得不良;過高時,難以維持穩定之延伸狀態。
另外,為了於延伸後賦予尺寸穩定性,也可實施熱固定。熱固定可利用周知的手段實施,例如對於上述延伸薄膜邊使其保持緊張狀態邊於通常80~180℃,較佳為100~165℃,實施通常約2~600秒之熱處理。又,將由本發明之EVOH樹脂組成物得到的多層延伸薄膜作為收縮用薄膜使用時,為了賦予熱收縮性,不實施上述熱固定,而實施例如對於延伸後之薄膜吹送冷風而予以冷卻固定等處理即可。
又,視情況也可使用本發明之多層結構體來獲得杯、盤狀之多層容器。此時,通常會採用抽拉成形法,具體可列舉:真空成形法、壓空成形法、真空壓空成形法、柱塞輔助式真空壓空成形法等。再者,從多層型坏(吹塑前的中空管狀的預成形物)獲得管、瓶狀之多層容器(疊層體結構)時會採用吹塑成形法。具體可列舉:擠製吹塑成形法(雙頭式、模具移動式、型坏移動式、旋轉式、蓄積式、水平型坏式等)、冷型坯式吹塑成形法、射出吹塑成形法、雙軸延伸吹塑成形法(擠製式冷型坯雙軸延伸吹塑成形法、射出式冷型坯雙軸延伸吹塑成形法、射出成形內嵌式雙軸延伸吹塑成形法等)等。得到的疊層體視需要可實施熱處理、冷卻處理、壓延處理、印刷處理、乾層合處理、溶液或熔融塗層處理、製袋加工、深抽拉加工、箱形加工、管狀加工、分切加工等。
多層結構體(包括經延伸者)之厚度,再者構成多層結構體之EVOH樹脂組成物層、基材樹脂層及黏著性樹脂層之厚度,會因層構成、基材樹脂之種類、黏著性樹脂之種類、用途或包裝形態、所要求之物性等而異,無法一概而論,多層結構體(包括經延伸者)之厚度通常為10~5000μm,較佳為30~3000μm,特佳為50~2000μm。EVOH樹脂組成物層通常為1~500μm,較佳為3~300μm,特佳為5~200μm,基材樹脂層通常為5~3000μm,較佳為10~2000μm,特佳為20~1000μm,黏著性樹脂層通常為0.5~250μm,較佳為1~150μm,特佳為3~100μm。
再者,多層結構體中EVOH樹脂組成物層相對於基材樹脂層之厚度比(EVOH樹脂組成物層/基材樹脂層),各層存在有多數層時則以厚度最厚的層彼此的厚度比計,通常為1/99~50/50,較佳為5/95~45/55,特佳為10/90~40/60。又,多層結構體中EVOH樹脂組成物層相對於黏著性樹脂層之厚度比(EVOH樹脂組成物層/黏著性樹脂層),各層存在有多數層時則以厚度最厚的層彼此的厚度比計,通常為10/90~99/1,較佳為20/80~95/5,特佳為50/50~90/10。
由如上述獲得之薄膜、片、延伸薄膜構成的袋及杯、盤、管、瓶等所構成的容器、蓋材,除了作為一般的食品之包裝材料容器係有用以外,作為美乃滋、調味醬等調味料、味噌等發酵食品、沙拉油等油脂食品、飲料、化妝品、醫藥品等各種之包裝材料容器亦為有用。 尤其,由本發明之EVOH樹脂組成物構成之層,具有優異的紫外線吸收能力,故作為食品之包裝材料,尤其作為紫外線所致之變色容易成為問題的精肉、火腿、香腸等畜肉用之包裝材料特別有用。 [實施例]
以下,舉實施例具體說明本發明,但本發明只要不超過其要旨,不限於實施例之記載。 另外,例中所記載之「份」除非事先說明否則意指重量基準。
[紫外線吸收能力] 使用EVOH樹脂組成物,製備濃度5重量%之水/異丙醇(4/6)溶液。然後,使用UV-VIS SPECTROPHOTOMETER(SHIMADZU公司製,UV-2600)測定該溶液之紫外線穿透率(波長300nm)。可藉由對於EVOH樹脂組成物在均勻溶液狀態下測定紫外線穿透率,來評價純粹樹脂組成物本身的紫外線穿透率。該值越低,意指紫外線吸收能力越高。
[著色] 使用手動油壓真空加熱壓製機(井元製作所公司製,IMC-11FD-A型)將EVOH樹脂組成物進行熱成形(210℃,熔融時間5分鐘,壓縮時間30秒),藉此獲得厚度2mm之樹脂板。使用色差計(日本電色工業公司製,SE 6000)測定獲得之樹脂板之YI值。
[熱穩定性] 對於EVOH樹脂組成物5mg,使用熱重量測定裝置(Perkin Elmer公司製,Pyris 1 TGA),於氮氣環境下:20mL/分鐘、升溫速度:10℃/分鐘、溫度範圍:30℃~550℃之條件,測定重量減少至測定前重量之95%之時點之溫度。
<實施例1> 使用乙烯結構單元之含量44莫耳%、皂化度99.6莫耳%、MFR12g/10分鐘(210℃,荷重2160g)之乙烯-乙烯醇共聚物作為EVOH樹脂(A)。對於該EVOH樹脂(A)之甲醇溶液(樹脂成分濃度36重量%)摻合乙酸水溶液,使乙酸相對於EVOH樹脂(A)100份成為1.5份。以齒輪泵輸送該甲醇溶液,並將其從圓形之模口擠壓至水中而成為股線狀,予以切斷而製作成圓柱形之丸粒。
使得到的丸粒以浴比2.5於35℃接觸乙酸水溶液(乙酸濃度2200ppm)3小時後,在氮氣氣流中於100℃進行36小時之乾燥,得到乙烯結構單元之含量44莫耳%、皂化度99.6莫耳%、MFR12g/10分鐘(210℃,荷重2160g)之EVOH樹脂(A)之丸粒。
[鐵化合物(C)之分析] 將上述EVOH樹脂(A)之丸粒經粉碎而成之樣品0.5g於紅外線加熱爐進行灰化處理(氧氣氣流中650℃,1小時),然後將灰分溶解於酸並以純水定容,將其作為試樣溶液。對於該溶液利用ICP-MS(Agilent Technologies公司製 ICP質量分析裝置 7500ce型)依標準添加法進行測定。結果鐵化合物(C)之含量以金屬換算計為0.1ppm。
利用塑性測定儀(Brabender公司製)將上述得到的EVOH樹脂(A)之丸粒100份、作為苯乙烯衍生物(B)之反式桂皮酸(和光純藥工業公司製)0.05份於210℃預熱5分鐘後予以熔融混練5分鐘,將得到的混練物冷卻後,實施粉碎處理,獲得EVOH樹脂組成物。 針對該EVOH樹脂組成物進行上述評價。將結果示於後述表1。
<比較例1> 使用乙烯結構單元之含量29莫耳%、皂化度99.6莫耳%、MFR3.9g/10分鐘(210℃,荷重2160g)之乙烯-乙烯醇共聚物(鐵化合物(C)之含量以金屬換算計為0ppm)作為EVOH樹脂(A),除此以外,以和實施例1同樣的方式獲得EVOH樹脂組成物。針對獲得之EVOH樹脂組成物同樣地進行評價。將結果示於後述之表1。
<比較例2> 將實施例1中使用之EVOH樹脂(A)之丸粒100份、作為苯乙烯衍生物(B)之反式桂皮酸(和光純藥工業公司製)0.05份、作為鐵化合物(C)之磷酸鐵(III)n水合物(和光純藥工業公司製,230℃乾燥減量 20.9重量%)0.0034份利用塑性測定儀(Brabender公司製)於210℃熔融混練5分鐘,將得到的混練物冷卻後,實施粉碎處理,獲得EVOH樹脂組成物。針對獲得的EVOH樹脂組成物同樣地進行評價。將結果示於後述表1。
<比較例3> 不摻合反式桂皮酸,除此以外,以和實施例1同樣的方式獲得EVOH樹脂組成物。針對獲得的EVOH樹脂組成物同樣地進行評價。將結果示於後述表1。
<比較例4> 不摻合反式桂皮酸,除此以外,以和比較例2同樣的方式獲得EVOH樹脂組成物。針對獲得的EVOH樹脂組成物同樣地進行評價。將結果示於下列表1。
【表1】
將含有鐵化合物(C)且不含有苯乙烯衍生物(B)的比較例3與比較例4進行對比的話,可得知紫外線吸收能力與鐵化合物(C)之摻合量成比例地提升,熱穩定性與鐵化合物(C)之摻合量成比例地提升。又,將比較例2與比較例4進行對比的話,可得知含有鐵化合物(C)10ppm且併用苯乙烯衍生物(B)之情況,獲得更良好的紫外線吸收能力,熱穩定性亦同等良好,但YI值高,因加熱而導致著色。
反觀使用了本發明之EVOH樹脂組成物的實施例1,儘管鐵化合物(C)係微量的0.1ppm,但紫外線吸收能力係和比較例2同等程度,而且著色更受到抑制,熱穩定性更為提升。另一方面,含有苯乙烯衍生物(B)且不含有鐵化合物(C)的比較例1,和實施例1相比紫外線吸收能力較差。又,比較例1和實施例1相比YI值較高,因加熱而導致著色,而且熱穩定性亦較差。
又,儘管在不含有苯乙烯衍生物(B)的比較例3、4中鐵化合物(C)之摻合量減少的話則熱穩定性降低,但在存在有苯乙烯衍生物(B)的實施例1中獲得了即便鐵化合物(C)之摻合量低也不損及熱穩定性甚至更為提升之無法預期的效果。可知唯有將苯乙烯衍生物(B)與微量之鐵化合物(C)併用方能獲得該效果。
上述實施例已揭示本發明之具體形態,但上述實施例僅為例示,不做限定性解釋。對於該技術領域中具有通常知識者而言為明顯的各種變形意欲包括在本發明之範圍內 [產業上利用性]
本發明之EVOH樹脂組成物,不摻合一般的紫外線吸收劑而仍具有紫外線吸收能力,熱穩定性優異,且著色受到抑制,故除了可適用作為各種食品之包裝材料以外,也可適用作為美乃滋、調味醬等調味料、味噌等發酵食品、沙拉油等油脂食品、飲料、化妝品、醫藥品等各種之包裝材料。
Claims (5)
- 一種乙烯-乙烯醇系共聚物組成物,含有乙烯-乙烯醇系共聚物(A)、苯乙烯衍生物(B)及鐵化合物(C),其特徵為:每單位重量之該乙烯-乙烯醇系共聚物組成物中,該鐵化合物(C)之含量以金屬換算計為0.01~5ppm。
- 如申請專利範圍第1項之乙烯-乙烯醇系共聚物組成物,其中,每單位重量之該乙烯-乙烯醇系共聚物組成物中,該苯乙烯衍生物(B)之含量為1~1000ppm。
- 如申請專利範圍第1或2項之乙烯-乙烯醇系共聚物組成物,其中,該苯乙烯衍生物(B)之含量相對於該鐵化合物(C)之金屬換算含量之重量比為0.2~50000。
- 一種丸粒,係由如申請專利範圍第1至3項中任一項之乙烯-乙烯醇系共聚物組成物構成。
- 一種多層結構體,含有由如申請專利範圍第1至3項中任一項之乙烯-乙烯醇系共聚物組成物構成之層。
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