JP7383399B2 - Sound insulation sheets and laminates - Google Patents
Sound insulation sheets and laminates Download PDFInfo
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- JP7383399B2 JP7383399B2 JP2019095986A JP2019095986A JP7383399B2 JP 7383399 B2 JP7383399 B2 JP 7383399B2 JP 2019095986 A JP2019095986 A JP 2019095986A JP 2019095986 A JP2019095986 A JP 2019095986A JP 7383399 B2 JP7383399 B2 JP 7383399B2
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- 238000009413 insulation Methods 0.000 title claims description 60
- 239000004973 liquid crystal related substance Substances 0.000 claims description 92
- 229920005989 resin Polymers 0.000 claims description 91
- 239000011347 resin Substances 0.000 claims description 91
- 229920006038 crystalline resin Polymers 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 27
- 125000003118 aryl group Chemical group 0.000 claims description 25
- 239000011148 porous material Substances 0.000 claims description 17
- 239000000178 monomer Substances 0.000 claims description 16
- 238000002844 melting Methods 0.000 claims description 15
- 230000008018 melting Effects 0.000 claims description 15
- 239000004745 nonwoven fabric Substances 0.000 claims description 13
- 229920000728 polyester Polymers 0.000 claims description 12
- 229920006149 polyester-amide block copolymer Polymers 0.000 claims description 11
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 7
- 239000006260 foam Substances 0.000 claims description 7
- 125000004959 2,6-naphthylene group Chemical group [H]C1=C([H])C2=C([H])C([*:1])=C([H])C([H])=C2C([H])=C1[*:2] 0.000 claims description 6
- 239000011491 glass wool Substances 0.000 claims description 5
- 229920005672 polyolefin resin Polymers 0.000 claims 2
- -1 polybutylene terephthalate Polymers 0.000 description 30
- 238000000034 method Methods 0.000 description 21
- 238000006116 polymerization reaction Methods 0.000 description 17
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 10
- 230000005540 biological transmission Effects 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 7
- KAUQJMHLAFIZDU-UHFFFAOYSA-N 6-Hydroxy-2-naphthoic acid Chemical compound C1=C(O)C=CC2=CC(C(=O)O)=CC=C21 KAUQJMHLAFIZDU-UHFFFAOYSA-N 0.000 description 6
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 6
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 6
- 239000008188 pellet Substances 0.000 description 5
- 229920001707 polybutylene terephthalate Polymers 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- PLIKAWJENQZMHA-UHFFFAOYSA-N 4-aminophenol Chemical compound NC1=CC=C(O)C=C1 PLIKAWJENQZMHA-UHFFFAOYSA-N 0.000 description 4
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 4
- 238000010030 laminating Methods 0.000 description 4
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 description 4
- 239000011342 resin composition Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 238000001125 extrusion Methods 0.000 description 3
- 230000001771 impaired effect Effects 0.000 description 3
- 239000012774 insulation material Substances 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000007790 solid phase Substances 0.000 description 3
- 125000001424 substituent group Chemical group 0.000 description 3
- UPHOPMSGKZNELG-UHFFFAOYSA-N 2-hydroxynaphthalene-1-carboxylic acid Chemical class C1=CC=C2C(C(=O)O)=C(O)C=CC2=C1 UPHOPMSGKZNELG-UHFFFAOYSA-N 0.000 description 2
- VHYFNPMBLIVWCW-UHFFFAOYSA-N 4-Dimethylaminopyridine Chemical compound CN(C)C1=CC=NC=C1 VHYFNPMBLIVWCW-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
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- 150000004984 aromatic diamines Chemical class 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000013016 damping 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
- 239000000835 fiber Substances 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- RXOHFPCZGPKIRD-UHFFFAOYSA-N naphthalene-2,6-dicarboxylic acid Chemical compound C1=C(C(O)=O)C=CC2=CC(C(=O)O)=CC=C21 RXOHFPCZGPKIRD-UHFFFAOYSA-N 0.000 description 2
- MNZMMCVIXORAQL-UHFFFAOYSA-N naphthalene-2,6-diol Chemical compound C1=C(O)C=CC2=CC(O)=CC=C21 MNZMMCVIXORAQL-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 238000006068 polycondensation reaction Methods 0.000 description 2
- 235000011056 potassium acetate Nutrition 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 125000001140 1,4-phenylene group Chemical group [H]C1=C([H])C([*:2])=C([H])C([H])=C1[*:1] 0.000 description 1
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 1
- MCTWTZJPVLRJOU-UHFFFAOYSA-N 1-methyl-1H-imidazole Chemical compound CN1C=CN=C1 MCTWTZJPVLRJOU-UHFFFAOYSA-N 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- XBNGYFFABRKICK-UHFFFAOYSA-N 2,3,4,5,6-pentafluorophenol Chemical compound OC1=C(F)C(F)=C(F)C(F)=C1F XBNGYFFABRKICK-UHFFFAOYSA-N 0.000 description 1
- QTHMEINNGLIDSU-UHFFFAOYSA-N 2,5-dichloro-4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC(Cl)=C(O)C=C1Cl QTHMEINNGLIDSU-UHFFFAOYSA-N 0.000 description 1
- NEQFBGHQPUXOFH-UHFFFAOYSA-N 4-(4-carboxyphenyl)benzoic acid Chemical compound C1=CC(C(=O)O)=CC=C1C1=CC=C(C(O)=O)C=C1 NEQFBGHQPUXOFH-UHFFFAOYSA-N 0.000 description 1
- JTGCXYYDAVPSFD-UHFFFAOYSA-N 4-(4-hydroxyphenyl)benzoic acid Chemical group C1=CC(C(=O)O)=CC=C1C1=CC=C(O)C=C1 JTGCXYYDAVPSFD-UHFFFAOYSA-N 0.000 description 1
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 229920005830 Polyurethane Foam Polymers 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 125000001118 alkylidene group Chemical group 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- VCCBEIPGXKNHFW-UHFFFAOYSA-N biphenyl-4,4'-diol Chemical group C1=CC(O)=CC=C1C1=CC=C(O)C=C1 VCCBEIPGXKNHFW-UHFFFAOYSA-N 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
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- JAWGVVJVYSANRY-UHFFFAOYSA-N cobalt(3+) Chemical compound [Co+3] JAWGVVJVYSANRY-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- PNOXNTGLSKTMQO-UHFFFAOYSA-L diacetyloxytin Chemical compound CC(=O)O[Sn]OC(C)=O PNOXNTGLSKTMQO-UHFFFAOYSA-L 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000012765 fibrous filler Substances 0.000 description 1
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000005165 hydroxybenzoic acids Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229940046892 lead acetate Drugs 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- UEGPKNKPLBYCNK-UHFFFAOYSA-L magnesium acetate Chemical compound [Mg+2].CC([O-])=O.CC([O-])=O UEGPKNKPLBYCNK-UHFFFAOYSA-L 0.000 description 1
- 239000011654 magnesium acetate Substances 0.000 description 1
- 229940069446 magnesium acetate Drugs 0.000 description 1
- 235000011285 magnesium acetate Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 239000006082 mold release agent Substances 0.000 description 1
- PCILLCXFKWDRMK-UHFFFAOYSA-N naphthalene-1,4-diol Chemical compound C1=CC=C2C(O)=CC=C(O)C2=C1 PCILLCXFKWDRMK-UHFFFAOYSA-N 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- IZUPBVBPLAPZRR-UHFFFAOYSA-N pentachloro-phenol Natural products OC1=C(Cl)C(Cl)=C(Cl)C(Cl)=C1Cl IZUPBVBPLAPZRR-UHFFFAOYSA-N 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000011496 polyurethane foam Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 125000001501 propionyl group Chemical group O=C([*])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 238000005809 transesterification reaction Methods 0.000 description 1
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- Laminated Bodies (AREA)
- Soundproofing, Sound Blocking, And Sound Damping (AREA)
Description
本発明は、遮音シート及び積層体に関する。 The present invention relates to a sound insulating sheet and a laminate.
種々の防音目的で、例えば、自動車のエンジン、家電製品等からの騒音が外部に到達するのを防止するため、又は、騒音が建築物の外部から内部に侵入するのを防止するため、様々な防音材が用いられている。例えば、特許文献１には、融点２００℃以上の熱可塑性重合体、具体的には、ポリブチレンテレフタレートを用いた吸音材が開示されている。 For various soundproofing purposes, for example, to prevent noise from car engines, home appliances, etc. from reaching the outside, or to prevent noise from entering a building from the outside. Soundproofing materials are used. For example, Patent Document 1 discloses a sound absorbing material using a thermoplastic polymer having a melting point of 200° C. or higher, specifically, polybutylene terephthalate.
しかし、本発明者らの検討によれば、従来の防音材では、特定の膜厚以下で、音の周波数によって、コインシデンス効果による透過損失の低減が著しく、遮音効果が十分でないことが判明した。コインシデンス効果とは、特定の周波数の音が防音材に入射する際に、共振が生じ、当該周波数付近で透過損失が低下する現象をいう。 However, according to studies conducted by the present inventors, it has been found that with conventional soundproofing materials, the reduction in transmission loss due to the coincidence effect is significant depending on the sound frequency when the film thickness is below a certain level, and the soundproofing effect is not sufficient. The coincidence effect refers to a phenomenon in which resonance occurs when sound at a specific frequency is incident on a soundproofing material, and transmission loss decreases around the frequency.
本発明は、かかる事情に鑑みてなされたものであり、コインシデンス効果が抑制され、遮音性に優れる遮音シートを提供することを目的とする。 The present invention has been made in view of the above circumstances, and an object of the present invention is to provide a sound insulating sheet that suppresses the coincidence effect and has excellent sound insulating properties.
本発明者らは、特定の液晶性樹脂を含み、膜厚及び面密度の各々が特定の範囲内である液晶性樹脂フィルムを遮音シートに用いることで上記の課題を解決できることを見出した。具体的には、本発明は、以下のようなものを提供する。 The present inventors have discovered that the above problem can be solved by using a liquid crystal resin film containing a specific liquid crystal resin and having a film thickness and areal density each within specific ranges for a sound insulation sheet. Specifically, the present invention provides the following.
（１） 少なくとも１層の液晶性樹脂フィルムを備える遮音シートであって、
前記少なくとも１層の液晶性樹脂フィルムは、融点が２５０℃以上４００℃以下である液晶性樹脂を含み、膜厚が５～５００μｍ、面密度が０．０００７～０．０７ｇ／ｃｍ２である遮音シート。
(1) A sound insulation sheet comprising at least one layer of liquid crystal resin film,
The at least one layer of liquid crystalline resin film includes a liquid crystalline resin having a melting point of 250°C or more and 400°C or less, has a thickness of 5 to 500μm, and has an areal density of 0.0007 to 0.07g/cm 2 . sheet.
（２） 前記液晶性樹脂が、芳香族ヒドロキシカルボン酸に由来する構成単位を全構成単位に対し４０～１００モル％含む全芳香族ポリエステル又は全芳香族ポリエステルアミドである、（１）に記載の遮音シート。 (2) The liquid crystal resin according to (1) is a wholly aromatic polyester or a wholly aromatic polyester amide containing 40 to 100 mol% of constitutional units derived from aromatic hydroxycarboxylic acid based on the total constitutional units. Sound insulation sheet.
（３） 前記液晶性樹脂が、２，６－ナフチレン基を有する構成単位を全構成単位に対し０．１～３０モル％含む、（１）又は（２）に記載の遮音シート。 (3) The sound insulation sheet according to (1) or (2), wherein the liquid crystalline resin contains 0.1 to 30 mol% of a structural unit having a 2,6-naphthylene group based on the total structural units.
（４） 前記液晶性樹脂が、非対称な分子構造を有するモノマーに由来する構成単位を全構成単位に対し９０～１００モル％含む、（１）～（３）のいずれかに記載の遮音シート。 (4) The sound insulation sheet according to any one of (1) to (3), wherein the liquid crystal resin contains 90 to 100 mol% of structural units derived from monomers having an asymmetric molecular structure based on the total structural units.
（５） 前記非対称な分子構造を有するモノマーに由来する構成単位が、下記構造式（Ｉ）で表される構成単位、下記構造式（ＩＩ）で表される構成単位、下記構造式（ＩＩＩ）で表される構成単位、及び下記構造式（ＩＶ）で表される構成単位からなる群から選択される少なくとも１種である、（１）～（４）のいずれかに記載の遮音シート。
（６） 更に、少なくとも１層の多孔質層を備える、（１）～（５）のいずれかに記載の遮音シートであって、
前記少なくとも１層の多孔質層は、多孔質材料を含む遮音シート。
(6) The sound insulation sheet according to any one of (1) to (5), further comprising at least one porous layer,
The at least one porous layer is a sound insulation sheet containing a porous material.
（７） 前記多孔質材料が、フェルト、グラスウール、フォーム、及び不織布からなる群より選ばれる少なくとも１種である、（６）に記載の遮音シート。 (7) The sound insulation sheet according to (6), wherein the porous material is at least one selected from the group consisting of felt, glass wool, foam, and nonwoven fabric.
（８） １層の液晶性樹脂フィルムと、
少なくとも１層の多孔質層、及び／又は、少なくとも１層の別の液晶性樹脂フィルムと、
を備える積層体であって、
前記１層の液晶性樹脂フィルム又は前記少なくとも１層の別の液晶性樹脂フィルムは、融点が２５０℃以上４００℃以下である液晶性樹脂を含み、膜厚が５～５００μｍ、面密度が０．０００７～０．０７ｇ／ｃｍ２であり、
前記少なくとも１層の多孔質層は、多孔質材料を含む積層体。
(8) One layer of liquid crystal resin film,
at least one porous layer and/or at least one other liquid crystal resin film;
A laminate comprising:
The one layer of liquid crystal resin film or the at least one layer of another liquid crystal resin film includes a liquid crystal resin having a melting point of 250° C. or more and 400° C. or less, has a film thickness of 5 to 500 μm, and has an areal density of 0. 0007~0.07g/ cm2 ,
The at least one porous layer is a laminate containing a porous material.
（９） 前記液晶性樹脂が、芳香族ヒドロキシカルボン酸に由来する構成単位を全構成単位に対し４０～１００モル％含む全芳香族ポリエステル又は全芳香族ポリエステルアミドである、（８）に記載の積層体。 (9) The liquid crystal resin according to (8) is a wholly aromatic polyester or a wholly aromatic polyester amide containing 40 to 100 mol% of constitutional units derived from aromatic hydroxycarboxylic acid based on the total constitutional units. laminate.
（１０） 前記液晶性樹脂が、２，６－ナフチレン基を有する構成単位を全構成単位に対し０．１～３０モル％含む、（８）又は（９）に記載の積層体。 (10) The laminate according to (8) or (9), wherein the liquid crystal resin contains a structural unit having a 2,6-naphthylene group in an amount of 0.1 to 30 mol% based on the total structural units.
（１１） 前記液晶性樹脂が、非対称な分子構造を有するモノマーに由来する構成単位を全構成単位に対し９０～１００モル％含む、（８）～（１０）のいずれかに記載の積層体。 (11) The laminate according to any one of (8) to (10), wherein the liquid crystal resin contains 90 to 100 mol% of structural units derived from monomers having an asymmetric molecular structure based on the total structural units.
（１２） 前記非対称な分子構造を有するモノマーに由来する構成単位が、下記構造式（Ｉ）で表される構成単位、下記構造式（ＩＩ）で表される構成単位、下記構造式（ＩＩＩ）で表される構成単位、及び下記構造式（ＩＶ）で表される構成単位からなる群から選択される少なくとも１種である、（８）～（１１）のいずれかに記載の積層体。
（１３） 前記多孔質材料が、フェルト、グラスウール、フォーム、及び不織布からなる群より選ばれる少なくとも１種である、（８）～（１２）のいずれかに記載の積層体。 (13) The laminate according to any one of (8) to (12), wherein the porous material is at least one selected from the group consisting of felt, glass wool, foam, and nonwoven fabric.
（１４） 前記積層体が遮音シートとして用いられる、（８）～（１３）のいずれかに記載の積層体。 (14) The laminate according to any one of (8) to (13), wherein the laminate is used as a sound insulation sheet.
本発明によれば、コインシデンス効果が抑制され、遮音性に優れる遮音シートを提供することができる。 According to the present invention, it is possible to provide a sound insulating sheet that suppresses the coincidence effect and has excellent sound insulating properties.
＜遮音シート＞
本発明に係る遮音シートは、少なくとも１層の液晶性樹脂フィルムを備え、前記少なくとも１層の液晶性樹脂フィルムは、融点が２５０℃以上４００℃以下である液晶性樹脂を含み、膜厚が５～５００μｍ、面密度が０．０００７～０．０７ｇ／ｃｍ２である。本発明に係る遮音シートは、上記の構成を備えることにより、コインシデンス効果が抑制され、遮音性に優れる。音が上記遮音シートに入射して振動が発生すると、当該遮音シート中の液晶性樹脂は、この振動を熱エネルギーに変換する特性に優れているため、上記振動が低減される結果、コインシデンス効果が抑制され、遮音性に優れると考えられる。上記遮音シートが２層以上の液晶性樹脂フィルムを備える場合、液晶性樹脂フィルム同士は、同一でも異なっていてもよい。
<Sound insulation sheet>
The sound insulation sheet according to the present invention includes at least one layer of liquid crystalline resin film, and the at least one layer of liquid crystalline resin film includes a liquid crystalline resin having a melting point of 250° C. or higher and 400° C. or lower, and has a film thickness of 5° C. ~500μm, and the areal density is 0.0007~0.07g/ cm2 . The sound insulation sheet according to the present invention has the above-mentioned configuration, thereby suppressing the coincidence effect and exhibiting excellent sound insulation properties. When sound enters the sound insulation sheet and generates vibration, the liquid crystal resin in the sound insulation sheet has an excellent property of converting this vibration into thermal energy, so the vibration is reduced and the coincidence effect is reduced. It is considered to have excellent sound insulation properties. When the sound insulation sheet includes two or more layers of liquid crystal resin films, the liquid crystal resin films may be the same or different.
［液晶性樹脂フィルム］
（液晶性樹脂）
本発明で使用する液晶性樹脂とは、光学異方性溶融相を形成し得る性質を有する溶融加工性ポリマーを指す。異方性溶融相の性質は、直交偏光子を利用した慣用の偏光検査法により確認することが出来る。より具体的には、異方性溶融相の確認は、Ｌｅｉｔｚ偏光顕微鏡を使用し、Ｌｅｉｔｚホットステージに載せた溶融試料を窒素雰囲気下で４０倍の倍率で観察することにより実施できる。本発明に適用できる液晶性樹脂は直交偏光子の間で検査したときに、たとえ溶融静止状態であっても偏光は通常透過し、光学的に異方性を示す。
[Liquid crystal resin film]
(liquid crystal resin)
The liquid crystalline resin used in the present invention refers to a melt-processable polymer having the property of forming an optically anisotropic melt phase. The nature of the anisotropic melt phase can be confirmed by conventional polarization testing using crossed polarizers. More specifically, the anisotropic melt phase can be confirmed by observing a molten sample placed on a Leitz hot stage at 40x magnification under a nitrogen atmosphere using a Leitz polarization microscope. When inspected between orthogonal polarizers, the liquid crystalline resin applicable to the present invention normally transmits polarized light even when it is in a molten, stationary state, and exhibits optical anisotropy.
上記のような液晶性樹脂の種類としては、融点が２５０℃以上４００℃以下である限り、特に限定されず、芳香族ポリエステル及び／又は芳香族ポリエステルアミドであることが好ましい。また、芳香族ポリエステル及び／又は芳香族ポリエステルアミドを同一分子鎖中に部分的に含むポリエステルもその範囲にある。液晶性樹脂としては、６０℃でペンタフルオロフェノールに濃度０．１質量％で溶解したときに、好ましくは少なくとも約２．０ｄｌ／ｇ、更に好ましくは２．０～１０．０ｄｌ／ｇの対数粘度（Ｉ．Ｖ．）を有するものが好ましく使用される。なお、液晶性樹脂は、融点が２５０℃以上４００℃以下であると、取り扱い性、加工性等が良好となりやすい。 The type of liquid crystal resin as described above is not particularly limited as long as it has a melting point of 250° C. or more and 400° C. or less, and aromatic polyester and/or aromatic polyester amide are preferable. Further, polyesters partially containing aromatic polyesters and/or aromatic polyesteramides in the same molecular chain are also within this range. The liquid crystalline resin preferably has a logarithmic viscosity of at least about 2.0 dl/g, more preferably from 2.0 to 10.0 dl/g when dissolved in pentafluorophenol at 60° C. at a concentration of 0.1% by mass. (I.V.) is preferably used. Note that when the liquid crystal resin has a melting point of 250° C. or more and 400° C. or less, handling properties, processability, etc. tend to be good.
本発明に適用できる液晶性樹脂としての芳香族ポリエステル又は芳香族ポリエステルアミドは、特に好ましくは、芳香族ヒドロキシカルボン酸に由来する構成単位を構成成分として有する芳香族ポリエステル又は芳香族ポリエステルアミドである。 The aromatic polyester or aromatic polyester amide as the liquid crystal resin applicable to the present invention is particularly preferably an aromatic polyester or aromatic polyester amide having a structural unit derived from an aromatic hydroxycarboxylic acid as a constituent component.
より具体的には、
（１）主として芳香族ヒドロキシカルボン酸及びその誘導体の１種又は２種以上に由来する構成単位からなるポリエステル；
（２）主として（ａ）芳香族ヒドロキシカルボン酸及びその誘導体の１種又は２種以上に由来する構成単位と、（ｂ）芳香族ジカルボン酸、脂環族ジカルボン酸、及びそれらの誘導体の１種又は２種以上に由来する構成単位と、（ｃ）芳香族ジオール、脂環族ジオール、脂肪族ジオール、及びそれらの誘導体の少なくとも１種又は２種以上に由来する構成単位、とからなるポリエステル；
（３）主として（ａ）芳香族ヒドロキシカルボン酸及びその誘導体の１種又は２種以上に由来する構成単位と、（ｂ）芳香族ヒドロキシアミン、芳香族ジアミン、及びそれらの誘導体の１種又は２種以上に由来する構成単位と、（ｃ）芳香族ジカルボン酸、脂環族ジカルボン酸、及びそれらの誘導体の１種又は２種以上に由来する構成単位、とからなるポリエステルアミド；
（４）主として（ａ）芳香族ヒドロキシカルボン酸及びその誘導体の１種又は２種以上に由来する構成単位と、（ｂ）芳香族ヒドロキシアミン、芳香族ジアミン、及びそれらの誘導体の１種又は２種以上に由来する構成単位と、（ｃ）芳香族ジカルボン酸、脂環族ジカルボン酸、及びそれらの誘導体の１種又は２種以上に由来する構成単位と、（ｄ）芳香族ジオール、脂環族ジオール、脂肪族ジオール、及びそれらの誘導体の少なくとも１種又は２種以上に由来する構成単位、とからなるポリエステルアミド等が挙げられる。更に上記の構成成分に必要に応じ分子量調整剤を併用してもよい。
More specifically,
(1) Polyester mainly consisting of structural units derived from one or more aromatic hydroxycarboxylic acids and their derivatives;
(2) Mainly (a) structural units derived from one or more aromatic hydroxycarboxylic acids and derivatives thereof, and (b) one type of aromatic dicarboxylic acids, alicyclic dicarboxylic acids, and derivatives thereof. or a polyester consisting of a structural unit derived from two or more types, and (c) a structural unit derived from at least one type or two or more types of aromatic diols, alicyclic diols, aliphatic diols, and derivatives thereof;
(3) Mainly (a) structural units derived from one or more aromatic hydroxycarboxylic acids and derivatives thereof, and (b) one or two aromatic hydroxyamines, aromatic diamines, and derivatives thereof. A polyesteramide consisting of a structural unit derived from at least one species, and (c) a structural unit derived from one or more of aromatic dicarboxylic acids, alicyclic dicarboxylic acids, and derivatives thereof;
(4) Mainly (a) structural units derived from one or more aromatic hydroxycarboxylic acids and derivatives thereof, and (b) one or two aromatic hydroxyamines, aromatic diamines, and derivatives thereof. (c) structural units derived from one or more types of aromatic dicarboxylic acids, alicyclic dicarboxylic acids, and derivatives thereof; and (d) aromatic diols, alicyclic Examples include polyesteramides comprising structural units derived from at least one or two or more of group diols, aliphatic diols, and derivatives thereof. Furthermore, if necessary, a molecular weight regulator may be used in combination with the above components.
本発明に適用できる液晶性樹脂を構成する具体的化合物の好ましい例としては、ｐ－ヒドロキシ安息香酸、６－ヒドロキシ－２－ナフトエ酸等の芳香族ヒドロキシカルボン酸、２，６－ジヒドロキシナフタレン、１，４－ジヒドロキシナフタレン、４，４’－ジヒドロキシビフェニル、ハイドロキノン、レゾルシン、下記一般式（Ｉ）で表される化合物、及び下記一般式（ＩＩ）で表される化合物等の芳香族ジオール；テレフタル酸、イソフタル酸、４，４’－ジフェニルジカルボン酸、２，６－ナフタレンジカルボン酸、及び下記一般式（ＩＩＩ）で表される化合物等の芳香族ジカルボン酸；ｐ－アミノフェノール、ｐ－フェニレンジアミン等の芳香族アミン類が挙げられる。
本発明で使用する液晶性樹脂は、得られる液晶性樹脂フィルムの制振性が向上しやすいことから、２，６－ナフチレン基を有する構成単位を全構成単位に対し０．１～３０モル％含むことが好ましく、１～３０モル％含むことがより好ましい。２，６－ナフチレン基を有する構成単位としては、例えば、６－ヒドロキシ－２－ナフトエ酸に由来する構成単位、２，６－ナフタレンジカルボン酸に由来する構成単位、２，６－ジヒドロキシナフタレンに由来する構成単位が挙げられ、制振性の点で、６－ヒドロキシ－２－ナフトエ酸に由来する構成単位が好ましい。 The liquid crystal resin used in the present invention contains 0.1 to 30 mol% of structural units having a 2,6-naphthylene group based on the total structural units, since the vibration damping properties of the obtained liquid crystal resin film are likely to be improved. It is preferably contained, and more preferably 1 to 30 mol%. Examples of the structural unit having a 2,6-naphthylene group include a structural unit derived from 6-hydroxy-2-naphthoic acid, a structural unit derived from 2,6-naphthalene dicarboxylic acid, and a structural unit derived from 2,6-dihydroxynaphthalene. From the viewpoint of vibration damping properties, structural units derived from 6-hydroxy-2-naphthoic acid are preferred.
中でも、製膜性の観点から、本発明で使用する液晶性樹脂は、非対称な分子構造を有するモノマーに由来する構成単位を全構成単位に対し９０～１００モル％含むことが好ましく、９２～１００モル％含むことがより好ましい。非対称な分子構造を有するモノマーに由来する構成単位を含む液晶性樹脂としては、例えば、以下の（１）又は（２）に示すような液晶性樹脂を挙げることができる。 Among these, from the viewpoint of film-forming properties, the liquid crystal resin used in the present invention preferably contains 90 to 100 mol% of structural units derived from monomers having an asymmetric molecular structure, and 92 to 100 mol% of the total structural units. It is more preferable to include mol%. Examples of the liquid crystal resin containing a structural unit derived from a monomer having an asymmetric molecular structure include liquid crystal resins as shown in (1) or (2) below.
（１）主として非対称な分子構造を有する芳香族ヒドロキシカルボン酸及びその誘導体の１種又は２種以上からなるポリエステル。 (1) A polyester mainly composed of one or more aromatic hydroxycarboxylic acids and derivatives thereof having an asymmetric molecular structure.
非対称な分子構造とは、図１に示すように分子骨格は対称であるが置換基（Ｒ１、Ｒ２）を考慮すると非対称となる分子構造をいう。ここで分子骨格とは、例えば、図１の分子構造の場合、置換基（Ｒ１、Ｒ２）を除いた残りの原子団（即ち、１，４－フェニレン基）が分子骨格である。 The asymmetric molecular structure refers to a molecular structure whose molecular skeleton is symmetrical, but becomes asymmetrical when substituents (R 1 , R 2 ) are taken into consideration, as shown in FIG. Here, the molecular skeleton is, for example, in the case of the molecular structure shown in FIG. 1, the atomic group (ie, 1,4-phenylene group) remaining after substituents (R 1 , R 2 ) are removed.
非対称な分子構造を有する芳香族ヒドロキシカルボン酸としては、従来公知のものを使用することができる。例えば、芳香族ヒドロキシカルボン酸としては、ヒドロキシ安息香酸及びそのエステル誘導体、ヒドロキシナフトエ酸及びそのエステル誘導体が挙げられる。
より具体的には以下の化合物を挙げることができる。
４－ヒドロキシ安息香酸等のヒドロキシ安息香酸；
２，５－ジクロロ－４－ヒドロキシ安息香酸等のヒドロキシ安息香酸のハロゲン置換体等；
６－ヒドロキシ－２－ナフトエ酸等のヒドロキシナフトエ酸；
４－カルボキシ－４’－ヒドロキシビフェニル、４－カルボキシ－４’－ヒドロキシジフェニルエーテル、４－カルボキシ－４’－ヒドロキシジフェニルメタン、４－カルボキシ－４’－ヒドロキシジフェニルスルフィド等のジフェニル化合物等が挙げられる。
As the aromatic hydroxycarboxylic acid having an asymmetric molecular structure, conventionally known ones can be used. For example, aromatic hydroxycarboxylic acids include hydroxybenzoic acid and its ester derivatives, and hydroxynaphthoic acid and its ester derivatives.
More specifically, the following compounds can be mentioned.
Hydroxybenzoic acids such as 4-hydroxybenzoic acid;
Halogen substituted products of hydroxybenzoic acid such as 2,5-dichloro-4-hydroxybenzoic acid;
Hydroxynaphthoic acids such as 6-hydroxy-2-naphthoic acid;
Examples include diphenyl compounds such as 4-carboxy-4'-hydroxybiphenyl, 4-carboxy-4'-hydroxydiphenyl ether, 4-carboxy-4'-hydroxydiphenylmethane, and 4-carboxy-4'-hydroxydiphenyl sulfide.
（２）主として（２－Ａ）非対称な分子構造を有する芳香族ヒドロキシカルボン酸及びその誘導体の１種又は２種以上と、（２－Ｂ）非対称な分子構造を有する芳香族ヒドロキシアミン及びその誘導体の１種又は２種以上と、からなるポリエステルアミド； (2) Mainly (2-A) one or more aromatic hydroxycarboxylic acids and derivatives thereof having an asymmetric molecular structure, and (2-B) aromatic hydroxyamines and derivatives thereof having an asymmetric molecular structure. A polyester amide consisting of one or more of the following;
（２－Ａ）非対称な分子構造を有する芳香族ヒドロキシカルボン酸及びその誘導体は、（１）で説明したものと同様であるため説明を省略する。 (2-A) The aromatic hydroxycarboxylic acid and its derivatives having an asymmetric molecular structure are the same as those explained in (1), so the explanation will be omitted.
（２－Ｂ）非対称な分子構造を有する芳香族ヒドロキシアミン及びその誘導体について説明する。 (2-B) Aromatic hydroxyamine and its derivatives having an asymmetric molecular structure will be explained.
芳香族ヒドロキシアミンは、非対称な分子構造を有するものであればよい。非対称な分子構造は上記で説明したものと同義である。芳香族ヒドロキシアミンの具体例としては、４－アミノフェノール、４－アセトアミドフェノール、４－アミノ－４’－ヒドロキシジフェニル、４－アミノ－４’－ヒドロキシジフェニルエーテル、４－アミノ－４’－ヒドロキシジフェニルメタン、４－アミノ－４’－ヒドロキシジフェニルスルフィド等が挙げられる。これら芳香族ヒドロキシアミンのエステル誘導体及び／又はアミド誘導体としては、アセチル、プロピオニル等の誘導体が挙げられる。 The aromatic hydroxyamine may have an asymmetric molecular structure. Asymmetric molecular structure has the same meaning as explained above. Specific examples of aromatic hydroxyamines include 4-aminophenol, 4-acetamidophenol, 4-amino-4'-hydroxydiphenyl, 4-amino-4'-hydroxydiphenyl ether, 4-amino-4'-hydroxydiphenylmethane, Examples include 4-amino-4'-hydroxydiphenyl sulfide. Examples of the ester derivatives and/or amide derivatives of these aromatic hydroxyamines include derivatives of acetyl, propionyl, and the like.
（１）又は（２）の液晶性樹脂においては、更に上記の構成成分（モノマー）に必要に応じ分子量調整剤を併用してもよい。 In the liquid crystal resin (1) or (2), a molecular weight regulator may be used in combination with the above-mentioned constituent components (monomers), if necessary.
非対称な分子構造を有するモノマーに由来する構成単位は、製膜性の観点から、下記構造式（Ｉ）で表される構成単位、下記構造式（ＩＩ）で表される構成単位、下記構造式（ＩＩＩ）で表される構成単位、及び下記構造式（ＩＶ）で表される構成単位からなる群から選択される少なくとも１種であることが、特に好ましい。 From the viewpoint of film formability, the structural units derived from monomers having an asymmetric molecular structure include the structural units represented by the following structural formula (I), the structural units represented by the following structural formula (II), and the structural units shown below. Particularly preferred is at least one selected from the group consisting of the structural unit represented by (III) and the structural unit represented by the following structural formula (IV).
本発明に用いられる液晶性樹脂の調製は、上記のモノマー化合物（又はモノマーの混合物）から直接重合法やエステル交換法を用いて公知の方法で行うことができ、通常は溶融重合法、溶液重合法、スラリー重合法、固相重合法等、又はこれらの２種以上の組み合わせが用いられ、溶融重合法、又は溶融重合法と固相重合法との組み合わせが好ましく用いられる。エステル形成能を有する上記化合物類はそのままの形で重合に用いてもよく、また、重合の前段階で前駆体から該エステル形成能を有する誘導体に変性されたものでもよい。これらの重合に際しては種々の触媒の使用が可能であり、代表的なものとしては、酢酸カリウム、酢酸マグネシウム、酢酸第一錫、テトラブチルチタネート、酢酸鉛、酢酸ナトリウム、三酸化アンチモン、トリス（２，４－ペンタンジオナト）コバルト（ＩＩＩ）等の金属塩系触媒、Ｎ－メチルイミダゾール、４－ジメチルアミノピリジン等の有機化合物系触媒が挙げられる。触媒の使用量は一般にはモノマーの全質量に対して約０．００１～１質量％、特に約０．０１～０．２質量％が好ましい。これらの重合方法により製造されたポリマーは更に必要があれば、減圧又は不活性ガス中で加熱する固相重合により分子量の増加を図ることができる。 The liquid crystalline resin used in the present invention can be prepared by a known method using a direct polymerization method or a transesterification method from the above monomer compounds (or a mixture of monomers), and is usually a melt polymerization method or a solution polymerization method. Polymerization, slurry polymerization, solid phase polymerization, etc., or a combination of two or more of these methods are used, and melt polymerization, or a combination of melt polymerization and solid phase polymerization is preferably used. The above-mentioned compounds having an ester-forming ability may be used in the polymerization as they are, or may be modified from a precursor into a derivative having the ester-forming ability in a pre-polymerization step. Various catalysts can be used for these polymerizations, and typical examples include potassium acetate, magnesium acetate, stannous acetate, tetrabutyl titanate, lead acetate, sodium acetate, antimony trioxide, and tris(2). , 4-pentanedionato) cobalt (III), and organic compound catalysts such as N-methylimidazole and 4-dimethylaminopyridine. The amount of catalyst used is generally about 0.001 to 1% by weight, particularly about 0.01 to 0.2% by weight, based on the total weight of monomers. If necessary, the molecular weight of the polymers produced by these polymerization methods can be increased by solid phase polymerization by heating under reduced pressure or in an inert gas.
上記のような方法で得られた液晶性樹脂の溶融粘度は特に限定されない。一般には成形温度での溶融粘度が剪断速度１０００ｓｅｃ－１で３Ｐａ・ｓ以上５００Ｐａ・ｓ以下のものが使用可能である。しかし、それ自体あまり高粘度のものは流動性が非常に悪化するため好ましくない。なお、上記液晶性樹脂は２種以上の液晶性樹脂の混合物であってもよい。 The melt viscosity of the liquid crystalline resin obtained by the above method is not particularly limited. Generally, those having a melt viscosity at a molding temperature of 3 Pa·s or more and 500 Pa·s or less at a shear rate of 1000 sec −1 can be used. However, if the viscosity itself is too high, the fluidity will be extremely poor, which is not preferable. Note that the liquid crystal resin may be a mixture of two or more types of liquid crystal resins.
液晶性樹脂フィルムにおいて、液晶性樹脂の含有量は、例えば、５０～１００質量％でよく、７０～１００質量％でもよく、９０～１００質量％でもよく、１００質量％でもよい。 In the liquid crystal resin film, the content of the liquid crystal resin may be, for example, 50 to 100% by mass, 70 to 100% by mass, 90 to 100% by mass, or 100% by mass.
（その他の成分）
液晶性樹脂フィルムは、本発明の目的を損なわない範囲で、液晶性樹脂の他に、液晶性樹脂以外の重合体、繊維状充填剤、板状充填剤、粒状充填剤、核剤、カーボンブラック、無機焼成顔料等の顔料、酸化防止剤、安定剤、可塑剤、滑剤、離型剤、及び難燃剤のうちの１種以上を配合してもよい。
(Other ingredients)
The liquid crystal resin film may contain, in addition to the liquid crystal resin, a polymer other than the liquid crystal resin, a fibrous filler, a plate filler, a granular filler, a nucleating agent, and carbon black, as long as the object of the present invention is not impaired. , pigments such as inorganic fired pigments, antioxidants, stabilizers, plasticizers, lubricants, mold release agents, and flame retardants.
（液晶性樹脂フィルムの製造方法）
液晶性樹脂フィルムは、例えば、液晶性樹脂を押出成形して、又は、液晶性樹脂とその他の成分とを含む液晶性樹脂組成物を押出成形して得られる。押出成形としては、特に限定されず、Ｔダイ法、ラミネート体延伸法、インフレーション法等が挙げられる。押出成形後に、及び／又は、押出成形時に、必要に応じ、延伸を行ってもよい。延伸としては、特に限定されず、一軸延伸でも二軸延伸でもよい。二次延伸は、同時二軸延伸でも逐次二軸延伸でもよい。
(Method for manufacturing liquid crystal resin film)
The liquid crystal resin film is obtained, for example, by extruding a liquid crystal resin or by extruding a liquid crystal resin composition containing a liquid crystal resin and other components. Extrusion molding is not particularly limited, and examples include a T-die method, a laminate stretching method, and an inflation method. Stretching may be performed after extrusion molding and/or during extrusion molding, if necessary. Stretching is not particularly limited, and may be uniaxial or biaxial stretching. The secondary stretching may be simultaneous biaxial stretching or sequential biaxial stretching.
なお、上記液晶性樹脂組成物の製造方法は、液晶性樹脂とその他の成分とを均一に混合できれば特に限定されず、従来知られる樹脂組成物の製造方法から適宜選択することができる。例えば、１軸又は２軸押出機等の溶融混練装置を用いて、各成分を溶融混練して押出した後、得られた液晶性樹脂組成物を粉末、フレーク、ペレット等の所望の形態に加工する方法が挙げられる。 The method for producing the liquid crystal resin composition is not particularly limited as long as the liquid crystal resin and other components can be mixed uniformly, and can be appropriately selected from conventionally known methods for producing resin compositions. For example, after melt-kneading and extruding each component using a melt-kneading device such as a single-screw or twin-screw extruder, the resulting liquid crystal resin composition is processed into a desired form such as powder, flakes, or pellets. One method is to do so.
（膜厚）
液晶性樹脂フィルムの膜厚は、５～５００μｍであり、好ましくは１０～４００μｍであり、より好ましくは５０～３００μｍである。液晶性樹脂フィルムの膜厚が上記範囲内であると、得られる遮音シートは、遮音性に優れたものとなりやすい。
(film thickness)
The thickness of the liquid crystal resin film is 5 to 500 μm, preferably 10 to 400 μm, and more preferably 50 to 300 μm. When the thickness of the liquid crystal resin film is within the above range, the resulting sound insulation sheet tends to have excellent sound insulation properties.
（面密度）
液晶性樹脂フィルムの面密度は、０．０００７～０．０７ｇ／ｃｍ２であり、好ましくは０．００１４～０．０５６ｇ／ｃｍ２であり、より好ましくは０．００７～０．０４２ｇ／ｃｍ２である。液晶性樹脂フィルムの面密度が上記範囲内であると、得られる遮音シートは、遮音性に優れたものとなりやすい。
(area density)
The areal density of the liquid crystal resin film is 0.0007 to 0.07 g/cm 2 , preferably 0.0014 to 0.056 g/cm 2 , more preferably 0.007 to 0.042 g/cm 2 It is. When the areal density of the liquid crystalline resin film is within the above range, the resulting sound insulation sheet tends to have excellent sound insulation properties.
［多孔質層］
本発明に係る遮音シートは、更に、少なくとも１層の多孔質層を備えてもよく、前記少なくとも１層の多孔質層は、多孔質材料を含む。これにより、上記遮音シートは、遮音性が更に向上しやすくなり、また、優れた吸音性を発現しやすくなる。上記遮音シートが２層以上の多孔質層を備える場合、多孔質層同士は、同一でも異なっていてもよい。
[Porous layer]
The sound insulation sheet according to the present invention may further include at least one porous layer, and the at least one porous layer includes a porous material. As a result, the sound insulation sheet can easily further improve its sound insulation properties, and can also easily exhibit excellent sound absorption properties. When the sound insulation sheet includes two or more porous layers, the porous layers may be the same or different.
（多孔質材料）
多孔質材料としては、特に限定されず、例えば、フェルト、グラスウール、フォーム、不織布等が挙げられる。フォームとしては、特に限定されず、例えば、ポリウレタンフォーム、メラミンフォーム等が挙げられる。不織布を構成する繊維は、特に限定されず、天然繊維でも合成繊維でもよい。多孔質材料は、１種単独で用いても、２種以上を併用してもよい。
(Porous material)
The porous material is not particularly limited, and examples thereof include felt, glass wool, foam, nonwoven fabric, and the like. The foam is not particularly limited, and examples thereof include polyurethane foam, melamine foam, and the like. The fibers constituting the nonwoven fabric are not particularly limited, and may be natural fibers or synthetic fibers. Porous materials may be used alone or in combination of two or more.
（その他の成分）
多孔質層は、本発明の目的を損なわない範囲で、多孔質材料の他に、着色剤、難燃剤等のその他の成分を含んでもよい。
(Other ingredients)
In addition to the porous material, the porous layer may contain other components such as a colorant and a flame retardant, as long as the object of the present invention is not impaired.
（厚み）
多孔質層の厚みは、得られる遮音シートの遮音性、吸音性等の観点から、好ましくは２０００～５００００μｍであり、より好ましくは２０００～３００００μｍである。
(thickness)
The thickness of the porous layer is preferably 2,000 to 50,000 μm, more preferably 2,000 to 30,000 μm from the viewpoint of sound insulation, sound absorption, etc. of the resulting sound insulation sheet.
（多孔質層の製造方法）
多孔質層の製造方法は、特に限定されず、多孔質層を構成する多孔質材料に応じて、適宜、公知の製造方法から選択すればよい。
(Method for manufacturing porous layer)
The method for manufacturing the porous layer is not particularly limited, and may be appropriately selected from known manufacturing methods depending on the porous material that constitutes the porous layer.
［その他の層］
本発明に係る遮音シートは、本発明の目的を損なわない範囲で、液晶性樹脂フィルム及び多孔質層以外に、その他の層を備えてもよい。その他の層としては、特に限定されず、液晶性樹脂フィルム以外の樹脂フィルム、紙、織物等が挙げられる。
[Other layers]
The sound insulation sheet according to the present invention may include other layers in addition to the liquid crystal resin film and the porous layer, as long as the object of the present invention is not impaired. Other layers are not particularly limited, and include resin films other than liquid crystal resin films, paper, textiles, and the like.
［遮音シートの構成］
遮音シートの構成は、特に限定されず、例えば、下記の構成が挙げられる。
（ａ）１層の液晶性樹脂フィルムのみからなる遮音シート
（ｂ）２層以上の液晶性樹脂フィルムのみからなる遮音シート
（ｃ）少なくとも１層の液晶性樹脂フィルムと少なくとも１層の多孔質層とがこの順序で積層してなる遮音シート
（ｄ）少なくとも１層の液晶性樹脂フィルムと少なくとも１層の多孔質層と少なくとも１層の液晶性樹脂フィルムとがこの順序で積層してなる遮音シート
（ｅ）少なくとも１層の多孔質層と少なくとも１層の液晶性樹脂フィルムと少なくとも１層の多孔質層とがこの順序で積層してなる遮音シート
[Sound insulation sheet configuration]
The structure of the sound insulation sheet is not particularly limited, and examples thereof include the following structure.
(a) Sound insulation sheet consisting of only one layer of liquid crystal resin film (b) Sound insulation sheet consisting of only two or more layers of liquid crystal resin film (c) At least one layer of liquid crystal resin film and at least one porous layer (d) A sound insulation sheet formed by laminating in this order: (d) A sound insulation sheet formed by laminating at least one layer of liquid crystalline resin film, at least one layer of porous layer, and at least one layer of liquid crystalline resin film in this order. (e) A sound insulation sheet formed by laminating at least one porous layer, at least one liquid crystal resin film, and at least one porous layer in this order.
［遮音シートの製造方法］
遮音シートの製造方法は、特に限定されず、遮音シートの構成に応じて、適宜、選択すればよい。遮音シートが１層の液晶性樹脂フィルムのみからなる場合は、液晶性樹脂フィルムの製造方法と同じである。遮音シートが２層以上の液晶性樹脂フィルムのみからなる場合や、遮音シートが少なくとも１層の液晶性樹脂フィルムと少なくとも１層の多孔質層とを備える場合は、例えば、重ね合わせた層同士を、接着及び／又は融着等の公知の接合方法で、互いに接合する方法が挙げられる。
[Method for manufacturing sound insulation sheet]
The method for manufacturing the sound insulation sheet is not particularly limited, and may be selected as appropriate depending on the configuration of the sound insulation sheet. When the sound insulating sheet consists of only one layer of liquid crystal resin film, the method for manufacturing the liquid crystal resin film is the same. When the sound insulation sheet consists of only two or more layers of liquid crystal resin films, or when the sound insulation sheet includes at least one layer of liquid crystal resin film and at least one porous layer, for example, the stacked layers may be Examples include a method of joining them together by a known joining method such as adhesion and/or fusion.
［用途］
本発明に係る遮音シートは、コインシデンス効果が抑制され、遮音性に優れるので、遮音性を要する用途に用いることができる。例えば、騒音等の侵入、流出等を防止するために、車両、船舶、航空機等の内装材；電気冷蔵庫、掃除機、エアーコンディショナー等の家電製品の内部に設置される遮音材；建築物の壁材；土木工事等における遮音壁；電動工具、油圧工具等の内部に設置される遮音材；原動機、発電機等の周囲に設置される遮音材として用いられる。その際、本発明に係る遮音シートは、適宜、所望のサイズや形状に加工され、必要に応じ、他の材料や部材とともに用いられる。
[Application]
The sound insulation sheet according to the present invention suppresses the coincidence effect and has excellent sound insulation properties, so it can be used in applications requiring sound insulation properties. For example, interior materials for vehicles, ships, aircraft, etc. to prevent the intrusion and outflow of noise, etc.; sound insulation materials installed inside home appliances such as electric refrigerators, vacuum cleaners, and air conditioners; walls of buildings; Used as a sound insulation wall in civil engineering work, etc.; a sound insulation material installed inside electric tools, hydraulic tools, etc.; a sound insulation material installed around prime movers, generators, etc. At that time, the sound insulating sheet according to the present invention is appropriately processed into a desired size and shape, and is used together with other materials and members as necessary.
＜積層体＞
本発明に係る積層体は、１層の液晶性樹脂フィルムと、少なくとも１層の多孔質層、及び／又は、少なくとも１層の別の液晶性樹脂フィルムと、を備え、前記１層の液晶性樹脂フィルム又は前記少なくとも１層の別の液晶性樹脂フィルムは、融点が２５０℃以上４００℃以下である液晶性樹脂を含み、膜厚が５～５００μｍ、面密度が０．０００７～０．０７ｇ／ｃｍ２であり、前記少なくとも１層の多孔質層は、多孔質材料を含む。ここで、前記１層の液晶性樹脂フィルム又は前記少なくとも１層の別の液晶性樹脂フィルムは、遮音シートの必須の構成要素として液晶性樹脂フィルムについて上述した通りである。また、前記少なくとも１層の多孔質層は、遮音シートの任意の構成要素として多孔質層について上述した通りである。本発明に係る積層体は、遮音シートとして好適に用いられる。
<Laminated body>
The laminate according to the present invention includes one layer of liquid crystal resin film, at least one porous layer, and/or at least one other layer of liquid crystal resin film, The resin film or the at least one layer of another liquid crystal resin film contains a liquid crystal resin having a melting point of 250° C. or more and 400° C. or less, has a thickness of 5 to 500 μm, and an areal density of 0.0007 to 0.07 g/ cm 2 and the at least one porous layer includes a porous material. Here, the one layer of liquid crystal resin film or the at least one layer of another liquid crystal resin film is as described above for the liquid crystal resin film as an essential component of the sound insulation sheet. Further, the at least one porous layer is as described above regarding the porous layer as an optional component of the sound insulation sheet. The laminate according to the present invention is suitably used as a sound insulation sheet.
積層体の構成は、特に限定されず、例えば、下記の構成が挙げられる。
（ｂ’）２層以上の液晶性樹脂フィルムのみからなる積層体
（ｃ’）少なくとも１層の液晶性樹脂フィルムと少なくとも１層の多孔質層とがこの順序で積層してなる積層体
（ｄ’）少なくとも１層の液晶性樹脂フィルムと少なくとも１層の多孔質層と少なくとも１層の液晶性樹脂フィルムとがこの順序で積層してなる積層体
（ｅ’）少なくとも１層の多孔質層と少なくとも１層の液晶性樹脂フィルムと少なくとも１層の多孔質層とがこの順序で積層してなる積層体
The configuration of the laminate is not particularly limited, and examples thereof include the following configurations.
(b') A laminate consisting only of two or more layers of liquid crystalline resin films (c') A laminate consisting of at least one layer of liquid crystalline resin film and at least one porous layer laminated in this order (d ') A laminate in which at least one liquid crystal resin film, at least one porous layer, and at least one liquid crystal resin film are laminated in this order (e') At least one porous layer; A laminate formed by laminating at least one layer of liquid crystalline resin film and at least one porous layer in this order.
以下に実施例を挙げて、本発明を更に詳しく説明するが、本発明はこれら実施例のみに限定されるものではない。 The present invention will be explained in more detail with reference to Examples below, but the present invention is not limited only to these Examples.
［実施例１］
重合容器に下記の原料を仕込んだ後、反応系の温度を１４０℃に上げ、１４０℃で１時間反応させた。その後、更に３３０℃まで３．５時間かけて昇温し、そこから１５分かけて１０Ｔｏｒｒ（即ち１３３０Ｐａ）まで減圧して、酢酸、過剰の無水酢酸、及びその他の低沸分を留出させながら重縮合を行った。撹拌トルクが所定の値に達した後、窒素を導入して減圧状態から常圧を経て加圧状態にして、重合容器の下部からポリマーを排出し、ストランドをペレタイズして融点が３２２℃のペレットを得た。得られたペレットを溶融押出し、インフレーション成形法により、膜厚が２３０μｍ、面密度が０．０３２ｇ／ｃｍ２の液晶性樹脂フィルム（以下、「ＬＣＰフィルム」ともいう。）を得た。
（原料）
４－ヒドロキシ安息香酸（ＨＢＡ）；２５２４ｇ（７９．３モル％）
２－ヒドロキシ－６－ナフトエ酸（ＨＮＡ）；８６７ｇ（２０モル％）
テレフタル酸（ＴＡ）；２７ｇ（０．３モル％）
金属触媒（酢酸カリウム触媒）；１５０ｍｇ
アシル化剤（無水酢酸）；２３３６ｇ
[Example 1]
After charging the following raw materials into a polymerization vessel, the temperature of the reaction system was raised to 140°C, and the reaction was carried out at 140°C for 1 hour. Thereafter, the temperature was further increased to 330°C over 3.5 hours, and the pressure was then reduced to 10 Torr (i.e. 1330 Pa) over 15 minutes, while acetic acid, excess acetic anhydride, and other low-boiling components were distilled out. Polycondensation was performed. After the stirring torque reaches a predetermined value, nitrogen is introduced and the pressure is increased from a reduced pressure state to a normal pressure state to a pressurized state, the polymer is discharged from the bottom of the polymerization vessel, and the strands are pelletized to form pellets with a melting point of 322°C. I got it. The obtained pellets were melt-extruded and subjected to inflation molding to obtain a liquid crystalline resin film (hereinafter also referred to as "LCP film") having a film thickness of 230 μm and an areal density of 0.032 g/cm 2 .
(material)
4-hydroxybenzoic acid (HBA); 2524g (79.3 mol%)
2-hydroxy-6-naphthoic acid (HNA); 867g (20 mol%)
Terephthalic acid (TA); 27g (0.3 mol%)
Metal catalyst (potassium acetate catalyst); 150mg
Acylating agent (acetic anhydride); 2336g
［比較例１］
重合容器に下記の原料を仕込んだ後、反応系の温度を２１０℃まで２時間かけて昇温し、エステル化反応を進行させた。その後、更に２５０℃まで３０分かけて昇温し、そこから２０分かけて０．５Ｔｏｒｒ（即ち６６．５Ｐａ）まで減圧して、メタノール、過剰の１，４－ブタンジオール、及びその他の低沸分を留出させながら重縮合を行った。撹拌トルクが所定の値に達した後、窒素を導入して減圧状態から常圧を経て加圧状態にして、重合容器の下部からポリマーを排出し、ストランドをペレタイズして融点が２２４℃のペレットを得た。得られたペレットを溶融押出し、インフレーション成形法により、膜厚が１９０μｍ、面密度が０．０２５ｇ／ｃｍ２のポリブチレンテレフタレートフィルム（以下、「ＰＢＴフィルム」ともいう。）を得た。
（原料）
テレフタル酸ジメチル；２２０４ｇ（４０モル％）
１，４－ブタンジオール；１５３５ｇ（６０モル％）
金属塩系触媒（チタン酸ブチル触媒）；１２５０ｍｇ
[Comparative example 1]
After charging the following raw materials into a polymerization container, the temperature of the reaction system was raised to 210° C. over 2 hours to advance the esterification reaction. Thereafter, the temperature was further increased to 250°C over 30 minutes, and the pressure was then reduced to 0.5 Torr (i.e. 66.5 Pa) over 20 minutes to remove methanol, excess 1,4-butanediol, and other low-boiling materials. Polycondensation was carried out while distilling off the components. After the stirring torque reaches a predetermined value, nitrogen is introduced and the pressure is increased from a reduced pressure state to a normal pressure state and then a pressurized state, the polymer is discharged from the bottom of the polymerization vessel, and the strands are pelletized to form pellets with a melting point of 224°C. I got it. The obtained pellets were melt-extruded and subjected to inflation molding to obtain a polybutylene terephthalate film (hereinafter also referred to as "PBT film") having a film thickness of 190 μm and an areal density of 0.025 g/cm 2 .
(material)
Dimethyl terephthalate; 2204g (40 mol%)
1,4-butanediol; 1535g (60 mol%)
Metal salt catalyst (butyl titanate catalyst); 1250 mg
［透過損失の測定］
ブリュエル・ケアー製４２０６Ｔ型透過損失管キット（５０Ｈｚ－６．４ｋＨｚ）を用いて、図２に模式的に示す通りに、試料として実施例１又は比較例１のフィルムを設置した後、スピーカから音波を発生させ、マイクロホン１～４により音圧を測定した結果から、透過損失を決定した。なお、周波数が５０Ｈｚ～１．６ｋＨｚの範囲では、内径１００ｍｍの太管を用い、周波数が５００Ｈｚ～６．４ｋＨｚの範囲では、内径２９ｍｍの細管を用いた。結果を図３（ａ）及び図３（ｂ）に示す。
[Measurement of transmission loss]
Using a Brüel & Kjær model 4206T transmission loss tube kit (50Hz-6.4kHz), as schematically shown in Figure 2, after installing the film of Example 1 or Comparative Example 1 as a sample, a sound wave was emitted from the speaker. was generated and the sound pressure was measured using microphones 1 to 4. From the results, the transmission loss was determined. Note that in the frequency range of 50 Hz to 1.6 kHz, a thick tube with an inner diameter of 100 mm was used, and in the frequency range of 500 Hz to 6.4 kHz, a thin tube with an inner diameter of 29 mm was used. The results are shown in FIGS. 3(a) and 3(b).
図３（ａ）及び図３（ｂ）の結果から分かる通り、同程度の膜厚及び面密度を有するＬＣＰフィルム及びＰＢＴフィルム同士を比較したところ、ＰＢＴフィルムでは、コインシデンス効果がより強く生じて透過損失が著しく低減したが、ＬＣＰフィルムでは、コインシデンス効果が生じても透過損失の低減が抑えられており、優れた遮音性を有することが確認された。 As can be seen from the results in Figures 3(a) and 3(b), when LCP films and PBT films with similar film thicknesses and areal densities were compared, the coincidence effect was stronger in the PBT film, resulting in less transmission. Although the loss was significantly reduced, it was confirmed that the LCP film suppressed the reduction in transmission loss even when a coincidence effect occurred, and had excellent sound insulation properties.
Claims (18)
前記少なくとも１層の液晶性樹脂フィルムは、不織布ではなく、融点が２５０℃以上４００℃以下である液晶性樹脂を含み、オレフィン系樹脂を含まず、膜厚が５～５００μｍ、面密度が０．０００７～０．０７ｇ／ｃｍ２である遮音シート。 A sound insulation sheet comprising at least one layer of liquid crystalline resin film,
The at least one layer of liquid crystal resin film is not a nonwoven fabric, but contains a liquid crystal resin having a melting point of 250° C. or more and 400° C. or less, does not contain an olefin resin, has a thickness of 5 to 500 μm, and has an areal density of 0. A sound insulation sheet with a weight of 0007 to 0.07 g/cm 2 .
前記少なくとも１層の液晶性樹脂フィルムは、不織布ではなく、融点が２５０℃以上４００℃以下である液晶性樹脂を含み、前記液晶性樹脂は、下記構造単位（ＩＩＩ’）を含まず、膜厚が５～５００μｍ、面密度が０．０００７～０．０７ｇ／ｃｍ２である遮音シート。
The at least one layer of liquid crystal resin film is not a nonwoven fabric, but contains a liquid crystal resin having a melting point of 250° C. or more and 400° C. or less, and the liquid crystal resin does not contain the following structural unit (III') and has a film thickness of A sound insulation sheet with a surface density of 5 to 500 μm and an areal density of 0.0007 to 0.07 g/cm 2 .
前記少なくとも１層の液晶性樹脂フィルムは、不織布ではなく、融点が２５０℃以上４００℃以下である液晶性樹脂を含み、前記液晶性樹脂フィルムにおいて、前記液晶性樹脂の含有量は、７０～１００質量％であり、膜厚が５～５００μｍ、面密度が０．０００７～０．０７ｇ／ｃｍ２である遮音シート。 A sound insulation sheet comprising at least one layer of liquid crystalline resin film,
The at least one layer of liquid crystal resin film is not a nonwoven fabric, but contains a liquid crystal resin having a melting point of 250° C. or more and 400° C. or less, and the content of the liquid crystal resin in the liquid crystal resin film is 70 to 100° C. % by mass, a film thickness of 5 to 500 μm, and an areal density of 0.0007 to 0.07 g/cm 2 .
前記少なくとも１層の多孔質層は、多孔質材料を含む遮音シート。 The sound insulation sheet according to any one of claims 1 to 7, further comprising at least one porous layer,
The at least one porous layer is a sound insulation sheet containing a porous material.
少なくとも１層の多孔質層、及び／又は、少なくとも１層の別の液晶性樹脂フィルムと、
を備える積層体であって、
前記１層の液晶性樹脂フィルム又は前記少なくとも１層の別の液晶性樹脂フィルムは、不織布ではなく、融点が２５０℃以上４００℃以下である液晶性樹脂を含み、オレフィン系樹脂を含まず、膜厚が５～５００μｍ、面密度が０．０００７～０．０７ｇ／ｃｍ２であり、
前記少なくとも１層の多孔質層は、多孔質材料を含む積層体。 One layer of liquid crystal resin film,
at least one porous layer and/or at least one other liquid crystal resin film;
A laminate comprising:
The one layer of liquid crystal resin film or the at least one layer of another liquid crystal resin film is not a nonwoven fabric, contains a liquid crystal resin having a melting point of 250°C or more and 400°C or less, does not contain an olefin resin, and is not a nonwoven fabric. The thickness is 5 to 500 μm, the areal density is 0.0007 to 0.07 g/cm 2 ,
The at least one porous layer is a laminate containing a porous material.
少なくとも１層の多孔質層、及び／又は、少なくとも１層の別の液晶性樹脂フィルムと、
を備える積層体であって、
前記１層の液晶性樹脂フィルム又は前記少なくとも１層の別の液晶性樹脂フィルムは、不織布ではなく、融点が２５０℃以上４００℃以下である液晶性樹脂を含み、前記液晶性樹脂は、下記構造単位（ＩＩＩ’）を含まず、膜厚が５～５００μｍ、面密度が０．０００７～０．０７ｇ／ｃｍ２であり、
前記少なくとも１層の多孔質層は、多孔質材料を含む積層体。
at least one porous layer and/or at least one other liquid crystal resin film;
A laminate comprising:
The one layer of liquid crystal resin film or the at least one layer of another liquid crystal resin film is not a nonwoven fabric , and includes a liquid crystal resin having a melting point of 250° C. or more and 400° C. or less, and the liquid crystal resin has the following structure. Does not contain unit (III'), has a film thickness of 5 to 500 μm, and an areal density of 0.0007 to 0.07 g/cm 2 ,
The at least one porous layer is a laminate containing a porous material.
少なくとも１層の多孔質層、及び／又は、少なくとも１層の別の液晶性樹脂フィルムと、
を備える積層体であって、
前記１層の液晶性樹脂フィルム又は前記少なくとも１層の別の液晶性樹脂フィルムは、不織布ではなく、融点が２５０℃以上４００℃以下である液晶性樹脂を含み、前記液晶性樹脂フィルムにおいて、前記液晶性樹脂の含有量は、７０～１００質量％であり、膜厚が５～５００μｍ、面密度が０．０００７～０．０７ｇ／ｃｍ２であり、
前記少なくとも１層の多孔質層は、多孔質材料を含む積層体。 One layer of liquid crystal resin film,
at least one porous layer and/or at least one other liquid crystal resin film;
A laminate comprising:
The one layer of liquid crystal resin film or the at least one layer of another liquid crystal resin film is not a nonwoven fabric and contains a liquid crystal resin having a melting point of 250° C. or more and 400° C. or less, and in the liquid crystal resin film, the The content of the liquid crystal resin is 70 to 100% by mass, the film thickness is 5 to 500 μm, the areal density is 0.0007 to 0.07 g/cm 2 ,
The at least one porous layer is a laminate containing a porous material.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2001089581A (en) | 1999-09-22 | 2001-04-03 | Toray Ind Inc | Sheet and its production |
| JP2002105250A (en) | 2000-10-02 | 2002-04-10 | Toray Ind Inc | Polyolefin resin composition and sheet |
| WO2018225568A1 (en) | 2017-06-08 | 2018-12-13 | クラレクラフレックス株式会社 | Fiber structure, molded body and sound-absorbing material |
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| JP2001089581A (en) | 1999-09-22 | 2001-04-03 | Toray Ind Inc | Sheet and its production |
| JP2002105250A (en) | 2000-10-02 | 2002-04-10 | Toray Ind Inc | Polyolefin resin composition and sheet |
| WO2018225568A1 (en) | 2017-06-08 | 2018-12-13 | クラレクラフレックス株式会社 | Fiber structure, molded body and sound-absorbing material |
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