CN112399994A - 用于与高压氢接触的挤出成型品的聚酰胺树脂组合物及使用该聚酰胺树脂组合物的挤出成型品 - Google Patents
用于与高压氢接触的挤出成型品的聚酰胺树脂组合物及使用该聚酰胺树脂组合物的挤出成型品 Download PDFInfo
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- CN112399994A CN112399994A CN201980045904.7A CN201980045904A CN112399994A CN 112399994 A CN112399994 A CN 112399994A CN 201980045904 A CN201980045904 A CN 201980045904A CN 112399994 A CN112399994 A CN 112399994A
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- ZWWQRMFIZFPUAA-UHFFFAOYSA-N dimethyl 2-methylidenebutanedioate Chemical compound COC(=O)CC(=C)C(=O)OC ZWWQRMFIZFPUAA-UHFFFAOYSA-N 0.000 description 1
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- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 description 1
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- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
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- OTCKOJUMXQWKQG-UHFFFAOYSA-L magnesium bromide Chemical compound [Mg+2].[Br-].[Br-] OTCKOJUMXQWKQG-UHFFFAOYSA-L 0.000 description 1
- 229910001623 magnesium bromide Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- BLQJIBCZHWBKSL-UHFFFAOYSA-L magnesium iodide Chemical compound [Mg+2].[I-].[I-] BLQJIBCZHWBKSL-UHFFFAOYSA-L 0.000 description 1
- 229910001641 magnesium iodide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 125000005439 maleimidyl group Chemical group C1(C=CC(N1*)=O)=O 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 235000002867 manganese chloride Nutrition 0.000 description 1
- QWYFOIJABGVEFP-UHFFFAOYSA-L manganese(ii) iodide Chemical compound [Mn+2].[I-].[I-] QWYFOIJABGVEFP-UHFFFAOYSA-L 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- NKHAVTQWNUWKEO-IHWYPQMZSA-N methyl hydrogen fumarate Chemical compound COC(=O)\C=C/C(O)=O NKHAVTQWNUWKEO-IHWYPQMZSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Chemical class OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N n-Octanol Natural products CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 1
- IPLJNQFXJUCRNH-UHFFFAOYSA-L nickel(2+);dibromide Chemical compound [Ni+2].[Br-].[Br-] IPLJNQFXJUCRNH-UHFFFAOYSA-L 0.000 description 1
- BFSQJYRFLQUZKX-UHFFFAOYSA-L nickel(ii) iodide Chemical compound I[Ni]I BFSQJYRFLQUZKX-UHFFFAOYSA-L 0.000 description 1
- SJYNFBVQFBRSIB-UHFFFAOYSA-N norbornadiene Chemical compound C1=CC2C=CC1C2 SJYNFBVQFBRSIB-UHFFFAOYSA-N 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920001643 poly(ether ketone) Polymers 0.000 description 1
- 229920000747 poly(lactic acid) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920005668 polycarbonate resin Polymers 0.000 description 1
- 239000004431 polycarbonate resin Substances 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920001955 polyphenylene ether Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 229910052903 pyrophyllite Inorganic materials 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
- 235000011150 stannous chloride Nutrition 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
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- 238000009864 tensile test Methods 0.000 description 1
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Chemical class CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- KOECRLKKXSXCPB-UHFFFAOYSA-K triiodobismuthane Chemical compound I[Bi](I)I KOECRLKKXSXCPB-UHFFFAOYSA-K 0.000 description 1
- KLNPWTHGTVSSEU-UHFFFAOYSA-N undecane-1,11-diamine Chemical compound NCCCCCCCCCCCN KLNPWTHGTVSSEU-UHFFFAOYSA-N 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
- 229940102001 zinc bromide Drugs 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
本发明的目的是提供可以获得挤出成型性、滞留稳定性优异,可以将成型品的厚度不均抑制得小,即使反复进行高压氢的填充和放压也能够抑制缺陷点产生的挤出成型品的聚酰胺树脂组合物。因此,提供一种用于与高压氢接触的挤出成型品的聚酰胺树脂组合物,其特征在于,相对于聚酰胺6树脂(A)70~99重量份与耐冲击材料(B)1~30重量份的合计100重量份,混配有金属卤化物(C)0.005~1重量份,上述聚酰胺树脂组合物的在260℃的温度下测定时的熔融张力为20mN以上,并且在260℃的温度下测定时的断裂时牵引速度为30m/min以上。
Description
技术领域
本发明涉及混配特定量的聚酰胺6树脂、耐冲击材料、和金属卤化物,并被控制为特定的熔融张力、断裂时牵引速度的、用于与高压氢接触的挤出成型品的聚酰胺树脂组合物以及将其成型而成的挤出成型品。
背景技术
近年来,为了应对石油燃料的枯竭、有害气体排出量的减少的要求,将使氢气与空气中的氧气进行电化学反应而发电的燃料电池搭载于汽车,将燃料电池发电的电供给到电动机而成为驱动力的燃料电池电动汽车受到关注。作为燃料电池电动汽车搭载用的高压氢用罐,研究了将树脂制的内衬的外侧用碳纤维增强树脂加强而成的树脂制罐。然而,由于氢分子尺寸小,因此与分子尺寸较大的天然气等相比,易于从树脂中透过,以及高压氢与常压的氢相比,在树脂中蓄积的量变多等,因此迄今为止的树脂制罐具有如果反复进行高压氢的填充和放压,则发生罐的变形、破坏的课题。
作为阻气性优异、即使在低温下也具有优异的耐冲击性的氢罐内衬用材料,研究了例如,由包含聚酰胺6、共聚聚酰胺、和耐冲击材料的聚酰胺树脂组合物形成的氢罐内衬用材料(例如,参照专利文献1)。
此外,作为阻气性优异的气体储存罐用内衬,研究了例如,含有包含聚酰胺、成核剂和耐冲击性改良剂的聚合物组合物的气体储存罐用内衬(例如,参照专利文献2)。
现有技术文献
专利文献
专利文献1:日本特开2009-191871号公报
专利文献2:日本特表2014-501818号公报
发明内容
发明所要解决的课题
与高压氢接触的成型品的制造方法可举出注射成型、挤出成型、吹塑成型等。其中,在成型长条的罐内衬时,有时通过挤出成型而成型出罐内衬的主体部,但有时在挤出成型时发生下垂(drawdown),不能获得成型品,有时壁厚变得不均匀。因此,为了挤出成型长条的罐内衬的主体部而要求耐下垂性等挤出成型性优异的材料。
进一步,挤出成型与注射成型相比,具有成型时的滞留时间变长的倾向,有时在滞留时树脂分解,韧性降低。因此,对挤出成型用的树脂组合物要求在滞留时不易分解的材料。进一步,即使获得了挤出成型品,如果所得的挤出成型品的厚度不均产生,则在反复进行高压氢的填充和放压时,有时也从厚度薄的位置产生缺陷点、裂缝。因此,对与高压氢接触的挤出成型用的树脂组合物要求在成型后不产生厚度不均。在挤出成型中,如果挤出/牵引变得不均匀,则易于产生厚度不均。挤出/牵引变得不均匀的因素之一可举出熔融张力低。
然而,专利文献1所记载的氢罐内衬具有易于发生氢气的透过,易于发生氢在树脂中的溶解,如果反复进行高压氢的填充和放压,则氢罐内衬产生缺陷点的课题。此外,具有聚酰胺树脂组合物的熔融张力低,耐下垂性差,得不到挤出成型品的课题。
此外,专利文献2所记载的气体储存罐用内衬虽然氦气耐透过性优异,但是具有易于发生氢气的透过、氢在树脂中的溶解,如果反复进行高压氢的填充和放压,则氢罐内衬产生缺陷点的课题。此外,具有聚酰胺树脂组合物的熔融张力低,耐下垂性差,得不到挤出成型品的课题。
本发明鉴于上述现有技术的课题,其课题是提供可以获得挤出成型性、滞留稳定性优异,并且,成型品的厚度不均被抑制得小,即使反复进行高压氢的填充和放压也抑制了缺陷点产生的挤出成型品的聚酰胺树脂组合物。
用于解决课题的方法
为了达到上述目的,本发明具有以下构成。
一种用于与高压氢接触的挤出成型品的聚酰胺树脂组合物,其特征在于,相对于聚酰胺6树脂(A)70~99重量份与耐冲击材料(B)1~30重量份的合计100重量份,混配有金属卤化物(C)0.005~1重量份,上述聚酰胺树脂组合物的在260℃的温度下测定时的熔融张力为20mN以上,并且在260℃的温度下测定时的断裂时牵引速度为30m/min以上。
进一步为,树脂浓度0.01g/ml的98%硫酸溶液的25℃的温度下的聚酰胺6树脂(A)的相对粘度(ηr)为3.3~7.0的用于挤出成型品的聚酰胺树脂组合物。作为上述耐冲击材料(B),使用不饱和羧酸和/或其衍生物改性乙烯/α-烯烃共聚物。进一步为,相对于不饱和羧酸和/或其衍生物改性乙烯/α-烯烃共聚物100重量份,来源于改性而被导入的不饱和羧酸和/或其衍生物部分为0.1~3.0重量份的用于挤出成型品的聚酰胺树脂组合物。
本发明包含由上述聚酰胺树脂组合物形成的与高压氢接触的挤出成型品。
发明的效果
本发明的用于与高压氢接触的挤出成型品的聚酰胺树脂组合物由于熔融张力高,耐下垂性优异,此外,能够承受快的牵引速度,因此可以提供厚度不均小,挤出成型性优异,进一步,在成型后厚度不均不易产生,即使反复进行高压氢的填充和放压也抑制缺陷点产生,滞留稳定性也优异的挤出成型品。
本发明的挤出成型品由于厚度不均被抑制得小,因此发挥即使反复进行高压氢的填充和放压也不易产生缺陷点,滞留稳定性优异的特长,能够作为与高压氢接触的用途所使用的挤出成型品而有用地展开。
具体实施方式
以下,进一步详细地说明本发明。
本发明的用于与高压氢接触的挤出成型品的聚酰胺树脂组合物(以下,有时记载为“聚酰胺树脂组合物”)是下述用于与高压氢接触的挤出成型品的聚酰胺树脂组合物,其特征在于,相对于聚酰胺6树脂(A)70~99重量份与耐冲击材料(B)1~30重量份的合计100重量份,混配有金属卤化物(C)0.005~1重量份,上述聚酰胺树脂组合物的在260℃的温度下测定时的熔融张力为20mN以上,并且在260℃的温度下测定时的断裂时牵引速度为30m/min以上,即,将聚酰胺树脂组合物在260℃的温度下熔融进行排出时,能够不断裂地牵引直到牵引速度为30m/min。
首先,对本发明中的聚酰胺6树脂(A)和耐冲击材料(B)的特征说明概略。
聚酰胺6树脂(A)的成型性、阻气性、刚性和韧性的平衡优异。聚酰胺6树脂(A)可以承受快的牵引速度,但如果为了提高熔融张力而使相对粘度过高,则易于发生混炼不良。进一步,可以提供下述聚酰胺树脂组合物:由于结晶度高,可以抑制氢气的透过、氢在树脂中的溶解,因此可以获得即使反复进行高压氢的填充、放压也不易产生缺陷点的挤出成型品。
耐冲击材料(B)与聚酰胺6树脂(A)的相容性良好,在与聚酰胺6树脂(A)进行了混炼时,期望耐冲击材料(B)的分散直径小,深入研究的结果发现,聚酰胺树脂组合物在高温下的熔融张力能够成为指标。在本发明中,包含聚酰胺6树脂(A)和耐冲击材料(B)的聚酰胺组合物的熔融张力变高,其结果,耐下垂性优异,即使为快的牵引速度流动性也充分,厚度不均不易产生。此外,通过在这样的聚酰胺6树脂(A)中混配特定量的耐冲击材料(B),可以使韧性提高。与高压氢接触的用途所使用的挤出成型品通过高压氢的填充、放压,从而反复收缩、膨胀,易于产生裂缝。通过混配特定量的耐冲击材料(B),即使反复进行这样的由高压氢的填充、放压引起的收缩、膨胀也可以抑制裂缝。
进一步,通过混配特定量的金属卤化物(C),可以使滞留稳定性提高。与高压氢接触的用途所使用的挤出成型品在挤出成型时滞留时间变长,韧性易于降低。通过混配特定量的金属卤化物(C),从而即使这样的在挤出成型时滞留时间变长也可以抑制韧性的降低。
(关于聚酰胺6树脂(A))
本发明所使用的所谓聚酰胺6树脂(A),是以6-氨基己酸和/或ε-己内酰胺作为主要原料的聚酰胺树脂。在不损害本发明的目的的范围内,可以共聚其它单体。这里,所谓“主要原料”,是指在构成聚酰胺树脂的单体单元的合计100摩尔%中,包含来源于6-氨基己酸的单元或来源于ε-己内酰胺的单元合计50摩尔%以上。更优选包含来源于6-氨基己酸的单元或来源于ε-己内酰胺的单元70摩尔%以上,进一步优选包含90摩尔%以上。
作为被共聚的其它单体,可举出例如,11-氨基十一烷酸、12-氨基十二烷酸、对氨基甲基苯甲酸等氨基酸、ω-十二内酰胺等内酰胺;1,4-丁二胺、1,5-戊二胺、1,6-己二胺、2-甲基-1,5-戊二胺、1,11-十一烷二胺、1,12-十二烷二胺、2,2,4-/2,4,4-三甲基-1,6-己二胺、5-甲基-1,9-壬二胺等脂肪族二胺;间苯二甲胺、对苯二甲胺等芳香族二胺;1,3-双(氨基甲基)环己烷、1,4-双(氨基甲基)环己烷、1-氨基-3-氨基甲基-3,5,5-三甲基环己烷、双(4-氨基环己基)甲烷、双(3-甲基-4-氨基环己基)甲烷、2,2-双(4-氨基环己基)丙烷、双(氨基丙基)哌嗪、氨基乙基哌嗪等脂环族二胺;己二酸、辛二酸、壬二酸、癸二酸、十二烷二酸等脂肪族二羧酸;对苯二甲酸、间苯二甲酸、2-氯对苯二甲酸、2-甲基对苯二甲酸、5-甲基间苯二甲酸、间苯二甲酸5-磺酸钠、六氢对苯二甲酸、六氢间苯二甲酸等芳香族二羧酸;1,4-环己烷二甲酸、1,3-环己烷二甲酸、1,2-环己烷二甲酸、1,3-环戊烷二甲酸等脂环族二羧酸。可以将它们共聚2种以上。
对聚酰胺6树脂(A)的聚合度没有特别限制,但在树脂浓度0.01g/ml的98%浓硫酸溶液中,在25℃的温度下测定的相对粘度优选为3.3~7.0的范围。如果相对粘度为3.3以上,则挤出成型时的聚酰胺树脂组合物的熔融张力适度变高,可以使下垂性更加提高。进一步,相对粘度更优选为4.0以上。另一方面,如果相对粘度为7.0以下,则聚酰胺树脂组合物的挤出成型时的熔融粘度适度变低,可以使挤出成型性更加提高。
对聚酰胺6树脂(A)的氨基末端基量没有特别限制,但优选为1.0×10-5~10.0×10-5mol/g的范围。如果氨基末端基量为1.0×10-5~10.0×10-5mol/g的范围,则可以获得充分的聚合度,使挤出成型品的机械强度提高。这里,聚酰胺6树脂(A)的氨基末端基量可以通过将聚酰胺6树脂(A)溶解于苯酚/乙醇混合溶剂(83.5:16.5(体积比)),使用0.02N盐酸水溶液进行滴定而求出。
(关于耐冲击材料(B))
作为本发明所使用的耐冲击材料(B),是指玻璃化转变温度为0℃以下的聚合物。这里所谓玻璃化转变温度,可以利用差示扫描量热计(DSC),使测定开始温度为-70℃,以20℃/min的升温速度升温,由此时产生的拐点求出。可举出例如,烯烃系树脂、丙烯酸系橡胶、有机硅系橡胶、氟系橡胶、苯乙烯系橡胶、腈系橡胶、乙烯基系橡胶、氨基甲酸酯系橡胶、聚酰胺弹性体、聚酯弹性体、离子交联聚合物等。可以将它们混配2种以上。
它们之中,从与聚酰胺6树脂(A)的相容性优异,韧性改良效果高考虑,优选使用烯烃系树脂。烯烃系树脂为将乙烯、丙烯、丁烯、异戊二烯、戊烯等烯烃单体聚合而获得的热塑性树脂。可以为2种以上烯烃单体的共聚物,也可以为这些烯烃单体与其它单体的共聚物。作为烯烃系树脂的具体例,可举出聚乙烯、聚丙烯、聚苯乙烯、聚1-丁烯、聚1-戊烯、聚甲基戊烯等聚合物或它们的共聚物;乙烯/α-烯烃共聚物、乙烯/α,β-不饱和羧酸酯共聚物、α-烯烃/α,β-不饱和羧酸酯共聚物、将[(乙烯和/或丙烯)与乙烯醇酯的共聚物]的至少一部分水解而获得的聚烯烃、(乙烯和/或丙烯)与(不饱和羧酸和/或不饱和羧酸酯)的共聚物、将[(乙烯和/或丙烯)与(不饱和羧酸和/或不饱和羧酸酯)的共聚物]的羧基的至少一部分进行金属盐化而获得的聚烯烃、共轭二烯与乙烯基芳香族烃的嵌段共聚物或其氢化物等。它们之中,更优选为乙烯/α-烯烃共聚物、乙烯/α,β-不饱和羧酸酯共聚物,进一步优选为乙烯/α-烯烃共聚物。
此外,期望上述烯烃系树脂被不饱和羧酸和/或其衍生物改性。如上所述,耐冲击材料(B)与聚酰胺6树脂(A)的相容性良好,在与聚酰胺6树脂(A)混炼时,期望耐冲击材料(B)的分散直径小,但为了使分散直径小,与聚酰胺6树脂(A)的混合量、和耐冲击材料(B)的弹性体的种类成为要点。例如,被不饱和羧酸和/或其衍生物改性了的耐冲击材料与聚酰胺6树脂的反应性良好,与聚酰胺6树脂的相容性提高。
这里,所谓不饱和羧酸的衍生物,是将不饱和羧酸的羧基的羟基部分用其它取代基置换了而得的化合物,是不饱和羧酸的金属盐、酰基卤、酯、酸酐、酰胺和酰亚胺等。通过使用这样的改性烯烃系树脂,从而与聚酰胺6树脂(A)的相容性更加提高,可以使挤出成型性更加提高。作为不饱和羧酸及其衍生物,可举出例如,丙烯酸、甲基丙烯酸、马来酸、富马酸、衣康酸、巴豆酸、甲基马来酸、甲基富马酸、中康酸、柠康酸、戊烯二酸和这些羧酸的金属盐;马来酸氢甲酯、衣康酸氢甲酯、丙烯酸甲酯、丙烯酸乙酯、丙烯酸丁酯、丙烯酸2-乙基己酯、丙烯酸羟基乙酯、甲基丙烯酸甲酯、甲基丙烯酸2-乙基己酯、甲基丙烯酸羟基乙酯、甲基丙烯酸氨基乙酯、马来酸二甲酯、衣康酸二甲酯等不饱和羧酸酯;马来酸酐、衣康酸酐、柠康酸酐、内二环-(2,2,1)-5-庚烯-2,3-二甲酸、内二环-(2,2,1)-5-庚烯-2,3-二甲酸酐等酸酐;马来酰亚胺、N-乙基马来酰亚胺、N-丁基马来酰亚胺、N-苯基马来酰亚胺、丙烯酸缩水甘油酯、甲基丙烯酸缩水甘油酯、乙基丙烯酸缩水甘油酯、衣康酸缩水甘油酯、柠康酸缩水甘油酯、5-降冰片烯-2,3-二甲酸等。它们之中,优选为不饱和二羧酸及其酸酐,特别优选为马来酸或马来酸酐。
作为将这些不饱和羧酸或其衍生物导入到烯烃系树脂的方法,可以举出例如,将烯烃单体与不饱和羧酸和/或其衍生物共聚的方法、使用自由基引发剂向未改性烯烃系树脂接枝导入不饱和羧酸和/或其衍生物的方法等。
导入了一部分不饱和羧酸和/或其衍生物成分的烯烃系树脂除了耐冲击性改善以外,也兼有还有助于聚酰胺6树脂中的弹性体的分散而减少将该组合物制成成型品时的厚度不均的作用。
不饱和羧酸和/或其衍生物成分的导入量例如相对于烯烃系树脂100重量份,优选使不饱和羧酸和/或其衍生物为0.1~3重量份。具体而言,在通过不饱和羧酸和/或其衍生物而导入不饱和羧酸和/或其衍生物,该不饱和羧酸和/或其衍生物改性乙烯/α-烯烃共聚物的重量为100重量份时,优选被导入的不饱和羧酸和/或其衍生物改性部的重量为0.1重量~3.0重量份。进一步,更优选不饱和羧酸和/或其衍生物改性部的重量为0.3重量份~2.5重量份。
在上述不饱和羧酸和/或其衍生物改性部的重量份范围中,在将聚酰胺6树脂(A)与耐冲击材料(B)进行了混炼时,耐冲击材料(B)的粒子分散直径变小。下面对分散直径进行描述。
作为效果,通过为0.1重量份以上,从而与聚酰胺6树脂(A)的相容性提高,耐冲击材料(B)的分散直径小,熔融张力变高,在挤出成型时不易发生下垂的问题。进一步,断裂时牵引速度变高,不易发生挤出成型品的壁厚变得不均匀的问题,是优选的。通过为3重量份以下,从而抑制与聚酰胺6树脂(A)的异常反应发生而凝胶化,熔融流动性降低,从而在挤出成型时不易发生负荷变大而机械停止的问题。进一步,断裂时牵引速度变高,不易发生挤出成型品的壁厚变得不均匀的问题,是优选的。
作为乙烯/α-烯烃共聚物,优选为乙烯与碳原子数3~20的α-烯烃的共聚物。作为碳原子数3~20的α-烯烃,具体而言,可举出丙烯、1-丁烯、1-戊烯、1-己烯、1-庚烯、1-辛烯、1-壬烯、1-癸烯、1-十一碳烯、1-十二碳烯、1-十三碳烯、1-十四碳烯、1-十五碳烯、1-十六碳烯、1-十七碳烯、1-十八碳烯、1-十九碳烯、1-二十碳烯、3-甲基-1-丁烯、3-甲基-1-戊烯、3-乙基-1-戊烯、4-甲基-1-戊烯、4-甲基-1-己烯、4,4-二甲基-1-己烯、4,4-二甲基-1-戊烯、4-乙基-1-己烯、3-乙基-1-己烯、9-甲基-1-癸烯、11-甲基-1-十二碳烯、12-乙基-1-十四碳烯等。可以将它们使用2种以上。在这些α-烯烃中,碳原子数3~12的α-烯烃从机械强度的提高的观点考虑是优选的。进一步,可以共聚1,4-己二烯、二环戊二烯、2,5-降冰片二烯、5-亚乙基降冰片烯、5-乙基-2,5-降冰片二烯,5-(1’-丙烯基)-2-降冰片烯等非共轭二烯的至少1种。被不饱和羧酸和/或其衍生物改性了的乙烯与碳原子数3~12的α-烯烃的共聚物可以使与聚酰胺6树脂(A)的相容性更加提高,使挤出成型性、韧性更加提高,因此是更优选的。此外,即使用更高压的氢反复进行填充和放压,也可以抑制缺陷点产生。乙烯/α-烯烃共聚物中的α-烯烃含量优选为1~30摩尔%,更优选为2~25摩尔%,进一步优选为3~20摩尔%。
耐冲击材料(B)的微粒的构成和结构没有特别限定,可以为例如,由由橡胶形成的至少1个层、与由与其不同种类的聚合物形成的1个以上层构成的被称为所谓核壳型的多层结构体。构成多层结构体的层的数只要为2层以上即可,可以为3层以上或4层以上,但优选在内部具有1层以上橡胶层(核心层)。构成多层结构体的橡胶层的橡胶的种类没有特别限定,可举出例如,使丙烯酸系成分、有机硅成分、苯乙烯成分、腈成分、共轭二烯成分、氨基甲酸酯成分、乙烯成分、丙烯成分、异丁烯成分等聚合而获得的橡胶。构成多层结构体的橡胶层以外的层的不同种类的聚合物的种类只要是具有热塑性的聚合物,就没有特别限定,但优选为与橡胶层相比玻璃化转变温度高的聚合物。另外,在作为耐冲击材料而使用的共聚组成、改性量、结构中,只要玻璃化转变温度为0℃以下即可。作为具有热塑性的聚合物,可举出例如,含有不饱和羧酸烷基酯单元、不饱和羧酸单元、含有不饱和缩水甘油基的单元、不饱和二羧酸酐单元、脂肪族乙烯基单元、芳香族乙烯基单元、氰化乙烯基单元、马来酰亚胺单元、不饱和二羧酸单元和其它乙烯基单元等的聚合物。
(关于金属卤化物(C))
作为本发明所使用的金属卤化物(C),可举出例如,碘化锂、碘化钠、碘化钾、溴化锂、溴化钠、溴化钾、氯化锂、氯化钠、氯化钾等碱金属卤化物、碘化镁、碘化钙、溴化镁、溴化钙、氯化镁、氯化钙等碱土金属卤化物;碘化锰(II)、溴化锰(II)、氯化锰(II)等第VIIB族金属卤化物;碘化铁(II)、溴化铁(II)、氯化铁(II)等第VIII族第1列金属卤化物;碘化钴(II)、溴化钴(II)、氯化钴(II)等第VIII族第2列金属卤化物;碘化镍(II)、溴化镍(II)、氯化镍(II)等第VIII族第3列金属卤化物;碘化铜(I)、溴化铜(I)、氯化铜(I)等第IB族金属卤化物;碘化锌、溴化锌、氯化锌等第IIB族金属卤化物;碘化铝(III)、溴化铝(III)、氯化铝(III)等第IIIA族金属卤化物;碘化锡(II)、溴化锡(II)、氯化锡(II)等第IVA族金属卤化物;三碘化锑、三溴化锑、三氯化锑、碘化铋(III)、溴化铋(III)、和氯化铋(III)等第VA族金属卤化物等。可以将它们并用2种以上。
它们之中,从获得容易、在聚酰胺6树脂(A)中的分散性优异,与自由基的反应性更高、并且使滞留稳定性更加提高这样的观点考虑,优选为碱金属卤化物和/或碘化铜。从使气体产生量减少这样的观点考虑,在碱金属卤化物中更优选使用碱金属碘化物。
(关于聚酰胺树脂组合物)
本发明的聚酰胺树脂组合物相对于聚酰胺6树脂(A)70~99重量份与耐冲击材料(B)1~30重量份的合计100重量份,混配有金属卤化物(C)0.005~1重量份。
如果聚酰胺6树脂(A)的混配量少于70重量份,则由所得的聚酰胺树脂组合物形成的挤出成型品的阻气性降低,如果用高压的氢反复进行填充和放压则产生缺陷点。聚酰胺6树脂(A)的混配量优选为75重量份以上,更优选为80重量份以上。另一方面,如果聚酰胺6树脂(A)的混配量多于99重量份,则由所得的聚酰胺树脂组合物形成的挤出成型品的韧性降低,如果用高压的氢反复进行填充和放压则产生裂缝。聚酰胺6树脂(A)的混配量优选为97重量份以下,更优选为95重量份以下。
耐冲击材料(B)的混配量为1~30重量份,优选为3重量份以上,更优选为5重量份以上。此外,优选为25重量份以下,更优选为20重量份以下。如果耐冲击材料(B)的混配量少于1重量份,则由所得的聚酰胺树脂组合物形成的挤出成型品的韧性降低,如果用高压的氢反复进行填充和放压则产生裂缝。另一方面,如果耐冲击材料(B)的混配量多于30重量份,则由所得的聚酰胺树脂组合物形成的挤出成型品的阻气性降低,如果用高压的氢反复进行填充和放压则产生缺陷点。
相对于聚酰胺6树脂(A)与耐冲击材料(B)的合计100重量份,金属卤化物(C)的混配量优选为0.005~1重量份,如果金属卤化物(C)的混配量少于0.005重量份,则所得的聚酰胺树脂组合物的挤出成型时的滞留稳定性降低,挤出成型品的韧性降低。从使滞留稳定性更加提高这样的观点考虑,金属卤化物(C)的混配量优选为0.02重量份以上,更优选为0.04重量份以上。另一方面,如果金属卤化物(C)的混配量多于1重量份,则金属卤化物(C)的自凝集进行从而分散直径变得粗大,由所得的聚酰胺树脂组合物形成的挤出成型品的机械物性降低。此外,通过变为粗大分散从而表面积降低,金属卤化物(C)与自由基的反应降低,因此所得的聚酰胺树脂组合物的挤出成型时的滞留稳定性降低,挤出成型品的韧性降低。金属卤化物(C)的混配量优选为0.5重量份以下,更优选为0.3重量份以下。
进一步,作为获得具有高熔融张力和高断裂时牵引速度的聚酰胺树脂组合物的方法,期望耐冲击材料(B)的分散直径小。作为使耐冲击材料(B)的分散直径小的方法,例如,优选作为树脂温度,将温度控制为比较高温的235℃~330℃的范围进行混炼。另外,这里所谓树脂温度,是向模孔直接插入接触型的树脂温度计而进行了测定的值。可以将在聚酰胺树脂组合物中分散的耐冲击材料(B)的分散直径微细地控制,聚酰胺6树脂(A)与耐冲击材料(B)的界面增加,熔融张力变高,并且能够均匀地被挤出/牵引,因此可以承受快的断裂时牵引速度,是优选的。这里,在聚酰胺树脂组合物中分散的耐冲击材料(B)的平均分散直径优选为0.01μm以上且0.5μm以下,更优选为0.02μm以上且0.3μm以下,进一步优选为0.05μm以上且0.2μm以下。
耐冲击材料(B)的平均分散直径例如为可以从聚酰胺树脂组合物颗粒切出超薄的切片,对该截面切片进行耐冲击材料(B)的染色,使用透射型电子显微镜进行观察,利用图像解析而算出分散了的粒子的直径。另外,在粒子不是正圆的情况下算出长径和短径的平均值,作为长径和短径的平均值,算出平均分散直径。
在本发明的聚酰胺树脂组合物中,在不损害其特性的范围内,可以根据需要混配除上述成分(A)、(B)和(C)以外的其它成分。作为其它成分,可以举出例如,填充材料、上述(A)以外的热塑性树脂类、各种添加剂类。
例如,通过混配填充材料,可以使成型品的强度和尺寸稳定性等提高。填充材料的形状可以为纤维状也可以为非纤维状,可以将纤维状填充材料与非纤维状填充材料组合使用。作为纤维状填充材料,可举出例如,玻璃纤维、玻璃研磨纤维、碳纤维、钛酸钾晶须、氧化锌晶须、硼酸铝晶须、芳族聚酰胺纤维、氧化铝纤维、碳化硅纤维、陶瓷纤维、石棉纤维、石膏纤维、金属纤维等。作为非纤维状填充材料,可举出例如,硅灰石、沸石、绢云母、高岭土、云母、粘土、叶蜡石、膨润土、石棉、滑石、硅酸铝等硅酸盐、氧化铝、氧化硅、氧化镁、氧化锆、氧化钛、氧化铁等金属氧化物、碳酸钙、碳酸镁、白云石等金属碳酸盐、硫酸钙、硫酸钡等金属硫酸盐、氢氧化镁、氢氧化钙、氢氧化铝等金属氢氧化物、玻璃珠、陶瓷珠、氮化硼和碳化硅等,它们可以为中空。此外,将这些纤维状和/或非纤维状填充材料用偶联剂进行预处理而使用在获得更优异的机械特性的意图下是优选的。作为偶联剂,可举出例如,异氰酸酯系化合物、有机硅烷系化合物、有机钛酸酯系化合物、有机硼烷系化合物、环氧化合物等。
作为热塑性树脂类,可举出例如,除上述聚酰胺6树脂(A)以外的聚酰胺树脂、聚酯树脂、聚苯硫醚树脂、聚苯醚树脂、聚碳酸酯树脂、聚乳酸树脂、聚缩醛树脂、聚砜树脂、四氟化聚乙烯树脂、聚醚酰亚胺树脂、聚酰胺酰亚胺树脂、聚酰亚胺树脂、聚醚砜树脂、聚醚酮树脂、聚硫醚酮树脂、聚醚醚酮树脂、聚苯乙烯树脂、ABS树脂等苯乙烯系树脂、聚氧化烯树脂等。也能够将这样的热塑性树脂类混配2种以上。另外,在混配除上述聚酰胺6树脂(A)以外的聚酰胺树脂的情况下,相对于聚酰胺6树脂(A)100重量份,优选为4重量份以下。
作为各种添加剂类,可举出例如,着色防止剂、受阻酚、受阻胺等抗氧化剂、亚乙基双硬脂基酰胺、高级脂肪酸酯等脱模剂、增塑剂、热稳定剂、润滑剂、紫外线防止剂、着色剂、阻燃剂、发泡剂等。
本发明的聚酰胺树脂组合物在260℃的温度下测定时的熔融张力为20mN以上,并且在260℃的温度下测定时的断裂时牵引速度为30m/min以上。聚酰胺树脂组合物如果在260℃的温度下测定时的熔融张力为20mN以上,并且在260℃的温度下测定时的断裂时牵引速度为30m/min以上,则在挤出成型时易于均匀地被延长,可以将厚度不均抑制得小,在反复进行高压氢的填充和放压时可以抑制缺陷点、裂缝的产生。
本发明的聚酰胺树脂组合物优选熔融张力为20~500mN,更优选为25~500mN,进一步优选为30~300mN。如果聚酰胺树脂组合物在260℃的温度下测定时的熔融张力为20mN以上,则可以抑制挤出成型时的下垂,可以获得挤出成型品。此外,如果聚酰胺树脂组合物在260℃的温度下测定时的熔融张力为500mN以下,则抑制拉伸性的降低,挤出成型性优异。
本发明的聚酰胺树脂组合物优选断裂时牵引速度为30m/min以上,更优选为50m/min以上,进一步优选为70m/min以上。如果聚酰胺树脂组合物的在260℃的温度下测定时的断裂时牵引速度为30m/min以上,则能够获得壁厚均匀的挤出成型品,残留应变少,此外,可以抑制反复进行高压氢的填充和放压时的应力集中,因此可以抑制缺陷点、裂缝产生。
另外,在本发明中,聚酰胺树脂组合物的熔融张力是如下那样操作而测定的。使用东洋精机制作所制キャピログラフ1C(料筒内径9.55mm,孔(orifice)的长度10.0mm,内径1.0mm),将试验温度设定为260℃。通过在料筒中填充聚酰胺树脂组合物,压紧而保持20分钟从而使其熔融后,使活塞速度为10mm/min而将260℃的熔融树脂从孔口条状地挤出。使该线料从下方的张力检测用滑轮的圆形引导件通过而以10m/min的牵引速度卷绕,将检测到的张力设为聚酰胺树脂组合物的熔融张力。
作为使聚酰胺树脂组合物的熔融张力为上述范围的方法,只要可获得那样的聚酰胺树脂组合物,就没有特别限制,优选使用下述方法:使用在树脂浓度0.01g/ml的98%浓硫酸溶液中,在25℃的温度下测定的相对粘度为3.3~7.0的范围的聚酰胺6树脂(A)的方法;使用不饱和羧酸和/或其衍生物改性乙烯/α-烯烃共聚物作为耐冲击材料(B)的方法。进而,优选使用下述方法:使用相对于乙烯/α-烯烃共聚物100重量份,利用不饱和羧酸和/或其衍生物0.1~3重量份改性而得的乙烯/α-烯烃共聚的方法。具体而言,优选使用相对于不饱和羧酸和/或其衍生物改性乙烯/α-烯烃共聚物100重量份,来源于改性而被导入的不饱和羧酸和/或其衍生物部分为0.1~3重量份的、耐冲击材料(B)。
在本发明中,聚酰胺树脂组合物的断裂时牵引速度是如下那样操作而测定的。使用东洋精机制作所制キャピログラフ1C(料筒内径9.55mm,孔(orifice)的长度10.0mm,内径1.0mm),将试验温度设定为260℃。在料筒中填充聚酰胺树脂组合物,压紧而保持20分钟从而使其熔融后,使活塞速度为10mm/min而将260℃的熔融树脂从孔口条状地挤出。使该线料从下方的张力检测用滑轮的圆形引导件通过而以10m/min的牵引速度卷绕,使检测到的张力稳定。在稳定后,一边以400m/min2的加速度使牵引速度加速一边卷绕,将线料断裂的时刻的牵引速度设为聚酰胺树脂组合物的断裂时牵引速度。另外,上述测定方法中的聚酰胺树脂组合物的断裂时牵引速度的测定的极限值为200m/min,但如果使用其它测定法则有时为200m/min以上。
在本发明中,如果为30m/min以上,则能够获得壁厚均匀的挤出成型品,厚度不均小,此外,可以抑制反复进行了高压氢的填充和放压时的应力集中,可以抑制缺陷点、裂缝产生。
作为使聚酰胺树脂组合物的断裂时牵引速度为上述范围的方法,只要可获得那样的聚酰胺树脂组合物,就没有特别限制,优选使用下述方法:使用不饱和羧酸和/或其衍生物改性乙烯/α-烯烃共聚物作为耐冲击材料(B)的方法。进而,优选使用下述方法:使用相对于乙烯/α-烯烃共聚物100重量份,利用不饱和羧酸和/或其衍生物0.1~3重量份改性而得的、改性乙烯/α-烯烃共聚的方法。具体而言,优选为使用相对于不饱和羧酸和/或其衍生物改性乙烯/α-烯烃共聚物100重量份,来源于改性而被导入了的不饱和羧酸和/或其衍生物0.1~3.0重量份的、耐冲击材料(B)的方法。
作为本发明的聚酰胺树脂组合物的制造方法,可举出熔融状态下的制造、溶液状态下的制造等。从生产性的观点考虑,可以优选使用熔融状态下的制造。关于熔融状态下的制造,可以使用采用挤出机、班伯里密炼机、捏合机、混合辊的熔融混炼等,从生产性方面考虑,可以优选使用采用能够连续制造的挤出机的熔融混炼。作为挤出机,可举出单螺杆挤出机、双螺杆挤出机、四螺杆挤出机等多螺杆挤出机、双螺杆单螺杆复合挤出机等。可以将这些挤出机多个组合。从混炼性、反应性、生产性的提高方面考虑,优选为双螺杆挤出机、四螺杆挤出机等多螺杆挤出机,更优选为双螺杆挤出机。
作为使用了双螺杆挤出机的熔融混炼方法,可举出例如,将聚酰胺6树脂(A)、耐冲击材料(B)、金属卤化物(C)和根据需要的除(A)(B)(C)以外的成分进行预混合而供给到料筒温度被设定为聚酰胺6树脂(A)的熔点以上的双螺杆挤出机进行熔融混炼的方法。对原料的混合顺序没有特别限制,可以使用将全部原料通过上述方法进行熔融混炼的方法、将一部分原料通过上述方法进行熔融混炼并进一步混配剩下的原料进行熔融混炼的方法、或在将一部分原料进行熔融混炼中使用侧进料机混合剩下的原料的方法等中的任一方法。此外也优选使用在挤出机中途将暴露于真空状态而产生的气体除去的方法。
作为使用了双螺杆挤出机的熔融混炼时的树脂温度,优选控制为235℃~330℃的范围。通过将熔融混炼时的树脂温度控制为235℃以上,从而可以将在聚酰胺树脂组合物中分散的耐冲击材料(B)的分散直径微细地控制,聚酰胺6树脂(A)与耐冲击材料(B)的界面增加,熔融张力变高,并且易于均匀地被延长,因此可以承受快的断裂时牵引速度,是优选的。此外,通过将熔融混炼时的树脂温度控制为330℃以下,从而抑制聚酰胺6树脂(A)和耐冲击材料(B)的分解,熔融张力更加变高,并且均匀地被挤出/牵引,因此可以承受快的断裂时牵引速度,是优选的。另外,这里所谓树脂温度,是向模孔直接插入接触型的树脂温度计而进行了测定的值。
本发明的聚酰胺树脂组合物能够进行挤出成型而获得成型品。作为成型形状,可举出例如,颗粒状、板状、纤维状、条状、膜或片状、管状、中空状的形状,优选使用作为管状的挤出成型品。
上述管状的挤出成型品优选将挤出成型品沿圆周方向分割成4份后各份的厚度的标准偏差σ为0.1以下。如果将管状的挤出成型品沿圆周方向分割成4份后各份的厚度的标准偏差大于0.1,则挤出成型品的壁厚不均匀,因此残留应变变大,此外,反复进行了高压氢的填充和放压时的应力集中变大,因此缺陷点、裂缝易于产生。
此外,从即使反复进行更高压的氢的填充和放压,也可以抑制缺陷点、裂缝产生方面考虑,管状的挤出成型品沿圆周方向分割成4份后各份的厚度的标准偏差优选为0.09以下,更优选为0.08以下。
这里,关于管状的挤出成型品的厚度,使用点测头测微计(Point micrometer)测定将管状的挤出成型品沿圆周方向分割成4份后的挤出成型品片各自的弧的中心。厚度的标准偏差σ可以使用所得的厚度xk,通过下述式算出。
式1)x=(1/4)∑xk(k=1~4)
式2)V=(1/4)∑(xk-x)2(k=1~4)
x:4个位置的厚度的平均
xk:各个位置的厚度(mm)
V:厚度的分散
σ:厚度的标准偏差。
将管状的挤出成型品沿圆周方向分割成4份后各份的厚度的标准偏差σ为0.1以下的挤出成型品的厚度没有特别限制,但优选为0.5mm~5mm的范围,更优选为1.0mm~4mm的范围。另外,挤出成型品的厚度为使用上述式1而求出的厚度。
为了使将这样的挤出成型品沿圆周方向分割成4份后各份的厚度的标准偏差为0.1以下,可举出例如,使用上述在260℃的温度下测定时的熔融张力为20mN以上,并且在260℃的温度下测定时的断裂时牵引速度为30m/min以上的聚酰胺树脂组合物的方法。
本发明的挤出成型品发挥即使反复进行高压氢的填充和放压也抑制缺陷点产生的优异特征,用于与高压氢接触的挤出成型品。这里所谓与高压氢接触的挤出成型品,是与常压以上的压力的氢接触的挤出成型品。从发挥抑制反复进行高压氢的填充和放压时的缺陷点产生的效果考虑,优选用于与压力20MPa以上的氢接触的挤出成型品用途,更优选用于与30MPa以上的氢接触的挤出成型品用途。另一方面,优选用于与压力200MPa以下的氢接触的挤出成型品用途,更优选用于与150MPa以下的氢接触的挤出成型品用途,进一步优选用于与100MPa以下的氢接触的挤出成型品用途。作为与高压氢接触的挤出成型品,可举出例如,高压氢用软管、高压氢用罐、高压氢用罐内衬、高压氢用管(pipe)、高压氢用压力传感器、高压氢用泵、高压氢用管(tube)、高压氢用膜、高压氢用片、高压氢用纤维等。其中,可以优选用于高压氢用罐、高压氢用罐内衬等高压氢容器。
实施例
以下,举出实施例进一步具体地说明本发明的效果。另外,本发明不限定于下述实施例。各实施例和比较例中的评价通过下述方法进行。
(1)高压氢的填充和放压反复特性(缺陷点)
对通过实施例1~4和比较例4、5、7、8而获得的挤出成型品进行X射线CT解析,观察了缺陷点的有无。将没有缺陷点的挤出成型品加入到高压釜后,在高压釜中经5分钟注入氢气直到20MPa,保持1小时后,经5分钟而减压直到变为常压。将其作为1个循环而反复进行100个循环。关于100个循环反复后的试验片,使用ヤマト科学(株)制TDM1000-IS进行X射线CT解析,观察10μm以上缺陷点的有无,将不存在缺陷点的情况设为“无”,将存在缺陷点的情况设为“有”。
(2)拉伸伸长率(韧性)
关于从通过实施例1~4和比较例4、5、7、8而获得的挤出成型品(厚度约3mm)以高度100mm、宽度5mm且以挤出成型方向成为高度方向的方式切出的试验片5条,在温度23℃、湿度50%的条件下调湿30分钟后,以夹盘间距离50mm、10mm/分钟的速度实施拉伸试验,评价了拉伸伸长率。将测定5条的平均值设为拉伸伸长率。另外,挤出成型品的拉伸伸长率为50%以上表示即使在受到挤出成型时施加的热后也维持韧性,热稳定性高。
(3)熔融张力
对于通过各实施例和比较例而获得的颗粒,使用东洋精机制作所制キャピログラフ1C(料筒内径9.55mm,孔(orifice)的长度10.0mm,内径1.0mm),在将试验温度设定为260℃的料筒中填充聚酰胺树脂组合物,压紧而保持20分钟从而使其熔融后,使活塞速度为10mm/min而将260℃的熔融树脂从孔口条状地挤出。使该线料从下方的张力检测用滑轮的圆形引导件通过而以10m/min的牵引速度卷绕,将检测到的张力设为熔融张力。
(4)断裂时牵引速度
对于通过各实施例和比较例获得的颗粒,使用东洋精机制作所制キャピログラフ1C(料筒内径9.55mm,孔(orifice)的长度10.0mm,内径1.0mm),在将试验温度设定为260℃的料筒中填充聚酰胺树脂组合物,压紧而保持20分钟从而使其熔融后,使活塞速度为10mm/min而将260℃的熔融树脂从孔口条状地挤出。使该线料从下方的张力检测用滑轮的圆形引导件通过而以10m/min的牵引速度卷绕,使检测到的张力稳定。在稳定后,一边以400m/min2的加速度使牵引速度加速一边卷绕,将线料断裂的时刻的牵引速度设为断裂时牵引速度。
(5)将挤出成型品沿圆周方向分割成4份后各份的厚度的标准偏差(挤出成型品厚度的标准偏差)
关于通过实施例1~4和比较例4、5、7、8而获得的挤出成型品,使用点测头测微计测定沿圆周方向分割成4份后的挤出成型品片各自的弧的中心,由所得的厚度xk,通过下述式算出厚度的标准偏差σ。
式1)x=(1/4)∑xk(k=1~4)
式2)V=(1/4)∑(xk-x)2(k=1~4)
x:4个位置的厚度的平均
xk:各个位置的厚度(mm)
V:厚度的分散
σ:厚度的标准偏差。
以下显示各实施例和比较例所使用的原料和缩写。
(聚酰胺6树脂(A)的原料和缩写)
PA6(ηr2.7):聚酰胺6树脂(树脂浓度0.01g/ml的98%浓硫酸溶液中25℃的温度下的相对粘度2.70)
PA6(ηr3.0):聚酰胺6树脂(树脂浓度0.01g/ml的98%浓硫酸溶液中25℃的温度下的相对粘度3.00)
PA6(ηr4.4):聚酰胺6树脂(树脂浓度0.01g/ml的98%浓硫酸溶液中25℃的温度下的相对粘度4.40)
PA6/PA66共聚物:聚酰胺6/聚酰胺66共聚物(熔点190℃,树脂浓度0.01g/ml的98%浓硫酸溶液中25℃的温度下的相对粘度4.20)。
(耐冲击材料(B)的原料和缩写)
耐冲击材料1:乙烯/1-丁烯共聚物(MFR(190℃,2160g荷重)0.5g/10分钟,密度0.862g/cm3)。
耐冲击材料2:相对于MFR(190℃,2160g荷重)0.5g/10分钟,密度0.862g/cm3的乙烯/1-丁烯共聚物100重量份,混合马来酸酐1.05重量份、过氧化物(日油(株)制,商品名パーヘキシン25B)0.04重量份,使用双螺杆挤出机在料筒温度230℃的温度下熔融挤出而获得耐冲击材料2。所得的耐冲击材料2为被马来酸酐改性了的乙烯/1-丁烯共聚物,相对于乙烯/1-丁烯共聚物100重量份的改性量为1.0重量份。具体而言,在侧链的一部分被马来酸酐改性,导入不饱和羧酸的乙烯/1-丁烯共聚物的重量为100重量份时,被导入的不饱和羧酸改性部的重量为1.0重量份。
关于各重量份的测定,将乙烯/1-丁烯共聚物100重量份与马来酸酐1.05重量份熔融混炼,测定所得的导入了不饱和羧酸的乙烯/1-丁烯共聚物的颗粒的重量。关于不饱和羧酸改性部的重量,将不饱和羧酸利用二甲苯在130℃的温度下溶解,对于滴定液调整氢氧化钾的0.02mol/L乙醇溶液(アルドリッチ社制)滴定液,对于指示剂调整酚酞1%乙醇溶液,将通过滴定而获得的不饱和羧酸的摩尔浓度换算为质量。进而,将不饱和羧酸改性乙烯/1-丁烯共聚物的重量换算为每100重量份,设为“被导入了的不饱和羧酸改性部的重量”。
耐冲击材料3:相对于MFR(190℃,2160g荷重)0.5g/10分钟,密度0.862g/cm3的乙烯/1-丁烯共聚物100重量份,混合马来酸酐2.1重量份、过氧化物(日油(株)制,商品名パーヘキシン25B)0.1重量份,使用双螺杆挤出机在料筒温度230℃的温度下熔融挤出而获得耐冲击材料3。所得的耐冲击材料3为被马来酸酐改性了的乙烯/1-丁烯共聚物,相对于乙烯/1-丁烯共聚物100重量份的改性量为2.0重量份。具体而言,在侧链的一部分被马来酸酐改性,导入不饱和羧酸的乙烯/1-丁烯共聚物的重量为100重量份时,被导入的不饱和羧酸改性部的重量为2.0重量份。
耐冲击材料4:相对于MFR(190℃,2160g荷重)0.5g/10分钟,密度0.862g/cm3的乙烯/1-丁烯共聚物100重量份,混合马来酸酐3.68重量份、过氧化物(日油(株)制,商品名パーヘキシン25B)0.3重量份,使用双螺杆挤出机在料筒温度230℃的温度下熔融挤出而获得耐冲击材料4。所得的耐冲击材料4为被马来酸酐改性了的乙烯/1-丁烯共聚物,相对于乙烯/1-丁烯共聚物100重量份的改性量为3.5重量份。具体而言,在侧链的一部分被马来酸酐改性,导入不饱和羧酸的乙烯/1-丁烯共聚物的重量为100重量份时,被导入的不饱和羧酸改性部的重量为3.5重量份。
(金属卤化物(C)的原料和缩写)
金属卤化物1:碘化铜(I)(和光纯药工业(株)制)
金属卤化物2:碘化钾(和光纯药工业(株)制)。
[实施例1~4、比较例4、5]
将表1、2记载的各原料供给到将料筒温度设定为240℃、设为设置了1个捏合区域的螺杆排列、使螺杆转速为150rpm的双螺杆挤出机(JSW社制TEX30α-35BW-7V)(L/D=45(另外,这里的L为从原料供给口到排出口的长度,D为螺杆的直径。))而进行了熔融混炼。使以20kg/h的速度从模排出的条状物从填充了温调为10℃的水的冷却浴中经10秒通过从而进行了骤冷后,用线料切粒机制成粒状,获得了颗粒。将所得的颗粒用真空干燥机在温度80℃的温度下真空干燥12小时,获得了干燥后颗粒。从所得的颗粒,使用挤出机,在挤出温度260℃的条件下从模挤出,使其通过整形模后冷却,挤出成型出大约外径100mm、内径94mm的管状的挤出成型品。关于厚度,由式1)求出平均厚度x,将结果记载于表1、2中。使用将所得的挤出成型品切出为200mm长度的挤出成型品,通过上述方法进行了评价,将所得的结果记载于表1、2中。
实施例1中,以作为聚酰胺6树脂(A)的PA6(ηr=4.4)85重量份、15重量份耐冲击材料2和0.1重量份金属卤化物1的组成进行了混炼。熔融混炼时的树脂温度为265℃。所得的颗粒的耐冲击材料2的平均分散直径为0.13μm,微细地分散了。此外,所得的颗粒的熔融张力为70mN,断裂时牵引速度为150m/min,是良好的。挤出成型品也没有缺陷点,挤出成型品厚度的标准偏差为0.046,是良好的。
实施例2中,将实施例1的耐冲击材料2变更为耐冲击材料3,除此以外,与实施例1同样。熔融混炼时的树脂温度为272℃。所得的颗粒的熔融张力为85mN,断裂时牵引速度为107m/min,是良好的。挤出成型品也没有缺陷点,挤出成型品厚度的标准偏差为0.043,是良好的。
实施例3中,除了金属卤化物1以外还加入了金属卤化物2,除此以外,与实施例1同样。熔融混炼时的树脂温度为267℃。所得的颗粒的熔融张力为73mN,断裂时牵引速度为165m/min,是良好的。挤出成型品也没有缺陷点,挤出成型品厚度的标准偏差为0.044,是良好的。
实施例4中,变更了PA6与耐冲击材料2的比率,除此以外,与实施例1同样。熔融混炼时的树脂温度为258℃。所得的颗粒的熔融张力为31mN,断裂时牵引速度超过200m/min,是良好的。挤出成型品也没有缺陷点,挤出成型品厚度的标准偏差为0.061,是没有问题的范围。
另一方面,比较例4中,使用了耐冲击材料4(相对于乙烯/1-丁烯共聚物100重量份的改性量为3.5重量份)。所得的颗粒的熔融张力98mN,断裂时牵引速度低至27m/min。挤出成型品产生缺陷点,挤出成型品厚度的标准偏差大至0.122。比较例5中,没有金属卤化物(C),挤出成型品中虽然没有缺陷点,但是发生了灼烧。
[比较例1~3、6]
将表2记载的各原料供给到将料筒温度设定为240℃、设为设置了1个捏合区域的螺杆排列、使螺杆转速为150rpm的双螺杆挤出机(JSW社制TEX30α-35BW-7V)(L/D=45(另外,这里的L为从原料供给口到排出口的长度,D为螺杆的直径。))而进行了熔融混炼。使以20kg/h的速度从模排出的条状物从填充了温调为10℃的水的冷却浴中经10秒通过从而进行了骤冷后,用线料切粒机制成粒状,获得了颗粒。所得的颗粒用真空干燥机在温度80℃的温度下真空干燥12小时,获得了干燥后颗粒。从所得的颗粒,使用挤出机,在挤出温度260℃的条件下从模挤出时,发生下垂,不能获得挤出成型品。
另外,在比较例1和2中,使用了PA6(ηr=2.7)。所得的颗粒的熔融张力在比较例1中小到9mN,在比较例2中小到14mN,断裂时牵引速度超过200m/min。
比较例3中,使用了耐冲击材料1(无不饱和羧酸改性)。比较例6中,使用PA6(ηr=3.0)与PA6/PA66共聚物(ηr=4.2)、耐冲击材料2,变更了它们各自的比率。所得的颗粒的熔融张力小到18mN,断裂时牵引速度为180m/min。
[比较例7]
将表2记载的各原料供给到将料筒温度设定为225℃、设为设置了1个捏合区域的螺杆排列、使螺杆转速为100rpm的双螺杆挤出机(JSW社制TEX30α-35BW-7V)(L/D=45(另外,这里的L为从原料供给口到排出口的长度,D为螺杆的直径。))而进行了熔融混炼。使以20kg/h的速度从模排出的条状物从填充了温调为10℃的水的冷却浴中经10秒通过从而进行了骤冷后,用线料切粒机制成粒状,获得了颗粒。所得的颗粒用真空干燥机在温度80℃的温度下真空干燥12小时,获得了干燥后颗粒。从所得的颗粒,使用挤出机,在挤出温度260℃的条件下从模挤出,使其通过整形模后冷却,挤出成型出大约外径100mm、内径94mm的管状的挤出成型品。关于厚度,由式1)求出平均厚度x,将结果记载于表2中。使用将所得的挤出成型品切出为200mm长度的挤出成型品,通过上述方法进行了评价,将所得的结果记载于表2中。
比较例7中,树脂组成与实施例1同样,但熔融时的树脂温度低至232℃。所得的颗粒的熔融张力低至19mN,断裂时牵引速度为65m/min。所得的颗粒的耐冲击材料2的平均分散直径为0.62μm,粗大地分散了,挤出成型品中产生缺陷点,挤出成型品厚度的标准偏差为0.12,偏差大。
[比较例8]
将表2记载的各原料供给到将料筒温度设定为300℃、设为设置了3个捏合区域的螺杆排列、使螺杆转速为300rpm的双螺杆挤出机(JSW社制TEX30α-35BW-7V)(L/D=45(另外,这里的L为从原料供给口到排出口的长度,D为螺杆的直径。))而进行了熔融混炼。使以20kg/h的速度从模排出的条状物从填充了温调为10℃的水的冷却浴中经10秒通过从而进行了骤冷后,用线料切粒机制成粒状,获得了颗粒。所得的颗粒用真空干燥机在温度80℃的温度下真空干燥12小时,获得了干燥后颗粒。从所得的颗粒,使用挤出机,在挤出温度260℃的条件下从模挤出,使其通过整形模后冷却,挤出成型出大约外径100mm、内径94mm的管状的挤出成型品。关于厚度,由式1)求出平均厚度x,将结果记载于表2中。使用将所得的挤出成型品切出为200mm长度的挤出成型品,通过上述方法进行了评价,将所得的结果记载于表2中。
比较例8中,树脂组成与实施例1同样,但熔融时的树脂温度高达340℃。所得的颗粒的熔融张力低至19mN,断裂时牵引速度为72m/min。挤出成型品中产生缺陷点,挤出成型品厚度的标准偏差为0.118,偏差大。
表1
根据以上结果,是混配聚酰胺6树脂(A)、耐冲击材料(B)和金属卤化物(C)而获得的聚酰胺树脂组合物,且聚酰胺树脂组合物在260℃的温度下测定时的熔融张力为20mN,并且在260℃的温度下测定时的断裂时牵引速度为30m/min的聚酰胺树脂组合物的熔融张力高,耐下垂性优异,此外,能够承受快的牵引速度,因此厚度不均少,挤出成型性优异。
可知将这样的聚酰胺树脂组合物成型而获得的挤出成型品可以将厚度不均抑制得小,即使反复进行高压氢的填充和放压也抑制缺陷点产生,并且滞留稳定性也优异。
产业可利用性
本发明的聚酰胺树脂组合物由于熔融张力高,耐下垂性优异,此外,能够承受快的牵引速度,因此挤出成型性优异,进一步,可以将成型品的厚度不均抑制得小,因此即使反复进行高压氢的填充和放压也抑制缺陷点产生,进一步滞留稳定性也优异。将本发明的聚酰胺树脂组合物挤出成型而成的挤出成型品可以发挥这些特性而广泛用于与高压氢接触的挤出成型品。
Claims (9)
1.一种用于与高压氢接触的挤出成型品的聚酰胺树脂组合物,其中,相对于聚酰胺6树脂A 70~99重量份与耐冲击材料B1~30重量份的合计100重量份,混配有金属卤化物C0.005~1重量份,所述聚酰胺树脂组合物的在260℃的温度下测定时的熔融张力为20mN以上,并且在260℃的温度下测定时的断裂时牵引速度为30m/min以上。
2.根据权利要求1所述的用于与高压氢接触的挤出成型品的聚酰胺树脂组合物,树脂浓度0.01g/ml的98%硫酸溶液的25℃的温度下的聚酰胺6树脂A的相对粘度ηr为3.3~7.0。
3.根据权利要求1或2所述的用于与高压氢接触的挤出成型品的聚酰胺树脂组合物,作为所述耐冲击材料B,使用不饱和羧酸和/或其衍生物改性乙烯/α-烯烃共聚物。
4.根据权利要求3所述的用于与高压氢接触的挤出成型品的聚酰胺树脂组合物,在所述不饱和羧酸和/或其衍生物改性乙烯/α-烯烃共聚物中,相对于不饱和羧酸和/或其衍生物改性乙烯/α-烯烃共聚物100重量份,来源于改性而被导入的不饱和羧酸和/或其衍生物部分为0.1~3重量份。
5.根据权利要求1~4中任一项所述的用于与高压氢接触的挤出成型品的聚酰胺树脂组合物,其特征在于,所述金属卤化物C包含碱金属卤化物和/或碘化铜(I)。
6.一种与高压氢接触的挤出成型品,其由权利要求1~5中任一项所述的聚酰胺树脂组合物形成。
7.根据权利要求6所述的与高压氢接触的挤出成型品,所述挤出成型品为管状。
8.根据权利要求7所述的与高压氢接触的挤出成型品,其特征在于,将所述管状的挤出成型品沿圆周方向分割成4份后各份的厚度的标准偏差为0.1以下。
9.一种高压氢罐内衬的制造方法,其包含下述工序:将权利要求1~5中任一项所述的聚酰胺树脂组合物挤出成型而获得挤出成型品,接着将该挤出成型品与由树脂组合物形成的成型品熔接的工序。
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- 2019-07-29 KR KR1020207035607A patent/KR20210040285A/ko not_active Application Discontinuation
- 2019-07-29 EP EP19843906.9A patent/EP3816230B1/en active Active
- 2019-07-29 CN CN201980045904.7A patent/CN112399994B/zh active Active
- 2019-07-29 CA CA3102986A patent/CA3102986A1/en active Pending
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JPWO2020027032A1 (ja) | 2020-08-06 |
JP6690785B1 (ja) | 2020-04-28 |
WO2020027032A1 (ja) | 2020-02-06 |
CN112399994B (zh) | 2023-05-09 |
US11261326B2 (en) | 2022-03-01 |
EP3816230B1 (en) | 2022-08-17 |
EP3816230A1 (en) | 2021-05-05 |
US20210246307A1 (en) | 2021-08-12 |
CA3102986A1 (en) | 2020-02-06 |
EP3816230A4 (en) | 2021-07-21 |
KR20210040285A (ko) | 2021-04-13 |
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