JP7084384B2 - 膨張及び硬化が同時に起こる熱可塑性フォーム - Google Patents
膨張及び硬化が同時に起こる熱可塑性フォーム Download PDFInfo
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- JP7084384B2 JP7084384B2 JP2019517088A JP2019517088A JP7084384B2 JP 7084384 B2 JP7084384 B2 JP 7084384B2 JP 2019517088 A JP2019517088 A JP 2019517088A JP 2019517088 A JP2019517088 A JP 2019517088A JP 7084384 B2 JP7084384 B2 JP 7084384B2
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- 238000000071 blow moulding Methods 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- HHSPVTKDOHQBKF-UHFFFAOYSA-J calcium;magnesium;dicarbonate Chemical compound [Mg+2].[Ca+2].[O-]C([O-])=O.[O-]C([O-])=O HHSPVTKDOHQBKF-UHFFFAOYSA-J 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- ASZXWYYSSJWIPL-UHFFFAOYSA-N cyano pentaneperoxoate Chemical compound C(#N)OOC(CCCC)=O ASZXWYYSSJWIPL-UHFFFAOYSA-N 0.000 description 1
- 238000001739 density measurement Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- PWWSSIYVTQUJQQ-UHFFFAOYSA-N distearyl thiodipropionate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCSCCC(=O)OCCCCCCCCCCCCCCCCCC PWWSSIYVTQUJQQ-UHFFFAOYSA-N 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
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- 239000000835 fiber Substances 0.000 description 1
- 239000006261 foam material Substances 0.000 description 1
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- 150000002334 glycols Chemical class 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000008240 homogeneous mixture Substances 0.000 description 1
- 229920001519 homopolymer Polymers 0.000 description 1
- 229940042795 hydrazides for tuberculosis treatment Drugs 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
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- 238000009776 industrial production Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 description 1
- 238000013035 low temperature curing Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- ZQMHJBXHRFJKOT-UHFFFAOYSA-N methyl 2-[(1-methoxy-2-methyl-1-oxopropan-2-yl)diazenyl]-2-methylpropanoate Chemical compound COC(=O)C(C)(C)N=NC(C)(C)C(=O)OC ZQMHJBXHRFJKOT-UHFFFAOYSA-N 0.000 description 1
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- WVFLGSMUPMVNTQ-UHFFFAOYSA-N n-(2-hydroxyethyl)-2-[[1-(2-hydroxyethylamino)-2-methyl-1-oxopropan-2-yl]diazenyl]-2-methylpropanamide Chemical compound OCCNC(=O)C(C)(C)N=NC(C)(C)C(=O)NCCO WVFLGSMUPMVNTQ-UHFFFAOYSA-N 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 150000002832 nitroso derivatives Chemical class 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 238000010943 off-gassing Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- NFHFRUOZVGFOOS-UHFFFAOYSA-N palladium;triphenylphosphane Chemical compound [Pd].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 NFHFRUOZVGFOOS-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920002959 polymer blend Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229940088417 precipitated calcium carbonate Drugs 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 125000002572 propoxy group Chemical group [*]OC([H])([H])C(C([H])([H])[H])([H])[H] 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000010561 standard procedure Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 239000004634 thermosetting polymer Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 125000005591 trimellitate group Chemical group 0.000 description 1
- 239000010456 wollastonite Substances 0.000 description 1
- 229910052882 wollastonite Inorganic materials 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/06—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent
- C08J9/10—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a chemical blowing agent developing nitrogen, the blowing agent being a compound containing a nitrogen-to-nitrogen bond
- C08J9/102—Azo-compounds
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- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/02—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles for articles of definite length, i.e. discrete articles
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- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
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- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29K2101/00—Use of unspecified macromolecular compounds as moulding material
- B29K2101/12—Thermoplastic materials
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
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- C08J2201/00—Foams characterised by the foaming process
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- C08J2201/026—Crosslinking before of after foaming
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Description
a)ラジカル反応によって架橋可能な、20~85重量%の少なくとも1つの熱可塑性ポリマーP;
b)2~15重量%の少なくとも1つのアゾラジカル開始剤I;
c)0~25重量%の少なくとも1つの接着促進剤AD;
d)0~10重量%の少なくとも1つの粘着性付与剤T;
e)0~2.5重量%の少なくとも1つの酸化防止剤AO;
f)2,500g/モル未満の分子量を有する、0~2.5重量%の少なくとも1つのポリアクリレートAC
を含む、熱膨張性組成物であって、
全ての個々の量が膨張前の全組成物を基準とする組成物を提供することによって独立クレーム1の特徴でこの目的を達成する。
60~75重量%の前記熱可塑性ポリマーP;
2.5~10重量%の前記アゾラジカル開始剤I;
10~20重量%の前記接着促進剤AD;
5~8重量%の前記粘着性付与剤T;
0.5~1.5重量%の前記酸化防止剤AO;
0.5~1.5重量%の前記ポリアクリレートAC
を含む。
1.1.組成
いくつかの実施例本発明組成物(C-1~C-16)を、以下に示される手順に従って調製した。組成物の総重量を基準とするそれらのそれぞれの成分の重量当たりの部(「重量部」、「ppw」と略記される)単位での正確な個々の組成を表1~3に示す。これらの値は、組成の全重量部を100%に設定する場合、重量%に容易に変換することができる。
全組成物を、ローラーローターを備えたHAAKE(商標)Rheomix Lab Mixerにおいて調製した。このミキサーを95℃に予熱した後、ポリマーP、接着促進剤AD及び粘着性付与剤Tを添加し、50rpmで5分にわたって混合した。その後温度を70℃及び5rpmに設定し、その後放冷した(アゾラジカル開始剤I1を含む実験については70~75℃、I2及びI4については80℃、I3については85℃)。ポリアクリレートACを60℃に予熱し、アゾラジカル開始剤上へ滴らせた。それらを、10rpmで1分にわたって分割して混合物に添加し、これに、1~2分長さの混合が続いた。最後に、溶融物をミキサーから取り出し、75℃で30秒間ホットプレスを用いてプレスして試料形状にした。
膨張及び膨張安定性を、オーブン中で30分間の様々な温度での個々の試料の熱処理(ベーキング)によって全試料で試験した。室温(23℃)からそれぞれのベーキング温度までの加熱ランプは、常に10分であった。温度及び対応するベーキング温度での膨張の大きさ(膨張前の元の体積を基準とする%単位での)を表5及び6に示す。
本発明組成物C-8(表2を参照されたい)を使用してUV照射によって誘発される膨張を試験した。このために、一連の試験試料を、2~4mmの範囲の異なる試料厚さで調製した。試料のコア温度を監視するために、UV活性化用の各試料は、熱電対線を含有した。このようにして調製された試料を、周囲面からの加熱及びUVランプによって発生する熱を最小限にするために、UV源から25cmの距離で空気中に固定した。UV活性化のために、F-エミッター(300~400nm)を備えたHoenle UVASPOT 400 Wランプ(Hoenle UV Technology,Germany)を使用した。
本発明の態様として、以下の態様を挙げることができる:
《態様1》
全ての個々の量が膨張前の全組成物を基準として、以下を含む、熱膨張性組成物:
a)ラジカル反応によって架橋可能な、20~85重量%の少なくとも1つの熱可塑性ポリマーP;
b)2~15重量%の少なくとも1つのアゾラジカル開始剤I;
c)0~25重量%の少なくとも1つの接着促進剤AD;
d)0~10重量%の少なくとも1つの粘着性付与剤T;
e)0~2.5重量%の少なくとも1つの酸化防止剤AO;
f)2,500g/モル未満の分子量を有する、0~2.5重量%の少なくとも1つのポリアクリレートAC。
《態様2》
前記組成物が、過酸化物、重炭酸塩、アゾジカーボンアミド、又は4,4’-オキシビス(ベンゼンスルホニルヒドラジド)を含まない、態様1に記載の熱膨張性組成物。
《態様3》
前記ポリマーPが、エチレン酢酸ビニル及び/又はエチレンブチルアクリレートを含み、前記ポリマーP又はその混合物が、10~100g/10分のASTM D1238によるメルトフローインデックスを示す、態様1又は2に記載の熱膨張性組成物。
《態様4》
前記アゾラジカル開始剤Iが、55~120℃でのトルエン中で10h半減期を有するアゾニトリル化合物、アルキルアゾ化合物、及びアゾアミド化合物からなる群から選択される、態様1~3のいずれか一項に記載の熱膨張性組成物。
《態様5》
前記接着促進剤ADが、グリシジルメタクリレート基を有し、かつ3~10g/10分のASTM D1238によるメルトフローインデックスを示す熱可塑性ポリマーを含む、態様1~4のいずれか一項に記載の熱膨張性組成物。
《態様6》
前記粘着性付与剤Tが、芳香族変性されていてもよいC5炭化水素樹脂を含む、態様1~5のいずれか一項に記載の熱膨張性組成物。
《態様7》
前記酸化防止剤AOが、少なくとも110℃の融点を有する、立体障害のあるフェノール化合物を含む、態様1~6のいずれか一項に記載の熱膨張性組成物。
《態様8》
前記ポリアクリレートACが、少なくとも4つのアクリレート官能価を有する、態様1~7のいずれか一項に記載の熱膨張性組成物。
《態様9》
全ての個々の重量%値の合計が100重量%を超えないように選択されるように、以下を含む、態様1~8のいずれか一項に記載の熱膨張性組成物:
60~75重量%の前記熱可塑性ポリマーP;
2.5~10重量%の前記アゾラジカル開始剤I;
10~20重量%の前記接着促進剤AD;
5~8重量%の前記粘着性付与剤T;
0.5~1.5重量%の前記酸化防止剤AO;
0.5~1.5重量%の前記ポリアクリレートAC。
《態様10》
中空構造物用のバッフル要素及び/又は強化要素であって、前記要素が、態様1~9のいずれか一項に記載の熱膨張性組成物を含むか又はそれから本質的になる、バッフル要素及び/又は強化要素。
《態様11》
前記要素が、キャリアを含み、前記キャリアの上に前記熱膨張性組成物が堆積させられているか又は取り付けられており、前記キャリアが、熱可塑性材料でできており、好ましくは、エポキシ樹脂、エチレン-酢酸ビニル、ポリウレタン、ポリオレフィン、又はそれらの誘導体若しくは混合物から選択される少なくとも1つの熱可塑性ポリマーでできている、態様10に記載のバッフル要素及び/又は強化要素。
《態様12》
前記熱膨張性組成物が、前記キャリア上へ射出成形されるか、又は前記キャリアと共押出される、態様11に記載のバッフル要素及び/又は強化要素の製造方法。
《態様13》
態様1~9のいずれか一項に記載の熱膨張性組成物の発泡方法であって、前記熱膨張性組成物を、10~60分間で120~200℃の温度に付し、かつ/又は1~60分間で前記組成物の表面に少なくとも2.5mW/cm -2 のUV強度でUV照射に付す、方法。
《態様14》
騒音、振動、湿気、及び/若しくは熱の伝達が低減するように、かつ/又は前記空洞を取り囲む物体が機械的に強化されるように、陸上車両、水上車両、又は航空機の空洞若しくは中空構造物を密封し、好ましくは自動車車両の空洞若しくは中空構造物を密封し、かつ/若しくは建物の空洞を密封し、遮断し、又は強化するための態様10又は11のいずれか一項に記載のバッフル要素及び/又は強化要素の使用。
《態様15》
態様1~9のいずれか一項に記載の熱膨張性組成物を含む要素を、前記空洞若しくは中空構造に導入し、その後、熱及び/若しくはUV処理によって膨張させて、それにより前記空洞若しくは中空構造を、膨張した組成物によって少なくとも部分的に満たす、空洞若しくは中空構造の密封、遮断及び/若しくは強化方法。
Claims (15)
- 全ての個々の量が膨張前の全組成物を基準として、以下を含む、熱膨張性組成物:
a)ラジカル反応によって架橋可能な、20~85重量%の少なくとも1つの熱可塑性ポリマーP;
b)2~15重量%の少なくとも1つのアゾラジカル開始剤I;
c)0~25重量%の少なくとも1つの接着促進剤AD;
d)0~10重量%の少なくとも1つの粘着性付与剤T;
e)0~2.5重量%の少なくとも1つの酸化防止剤AO;
f)2,500g/モル未満の分子量を有する、0.1~2.5重量%の少なくとも1つのポリアクリレートAC;
ここで、前記組成物は、過酸化物、重炭酸塩、アゾジカーボンアミド、又は4,4’-オキシビス(ベンゼンスルホニルヒドラジド)を含まず、かつ
前記少なくとも1つのアゾラジカル開始剤Iは、アゾビスイソブチロニトリル、1,1’-アゾビス(シクロヘキサン-1-カルボニトリル)、及び2,2’-アゾビス[2-メチル-N-(2-ヒドロキシエチル)プロピオンアミド]からなる群から選択される。 - 前記ポリアクリレートACが、1,000g/モル未満の分子量を有し、かつ少なくとも2若しくは3のアクリレート官能価を示す、請求項1に記載の熱膨張性組成物。
- 前記ポリマーPが、エチレン酢酸ビニル及び/又はエチレンブチルアクリレートを含み、前記ポリマーP又はその混合物が、10~100g/10分のASTM D1238によるメルトフローインデックスを示す、請求項1又は2に記載の熱膨張性組成物。
- 前記アゾラジカル開始剤Iが、55~120℃でのトルエン中で10h半減期を有する化合物からなる群から選択される、請求項1~3のいずれか一項に記載の熱膨張性組成物。
- 前記接着促進剤ADが、グリシジルメタクリレート基を有し、かつ3~10g/10分のASTM D1238によるメルトフローインデックスを示す熱可塑性ポリマーを含む、請求項1~4のいずれか一項に記載の熱膨張性組成物。
- 前記粘着性付与剤Tが、芳香族変性されていてもよいC5炭化水素樹脂を含む、請求項1~5のいずれか一項に記載の熱膨張性組成物。
- 前記酸化防止剤AOが、少なくとも110℃の融点を有する、立体障害のあるフェノール化合物を含む、請求項1~6のいずれか一項に記載の熱膨張性組成物。
- 前記ポリアクリレートACが、少なくとも4つのアクリレート官能価を有する、請求項1~7のいずれか一項に記載の熱膨張性組成物。
- 全ての個々の重量%値の合計が100重量%を超えないように選択されるように、以下を含む、請求項1~8のいずれか一項に記載の熱膨張性組成物:
60~75重量%の前記熱可塑性ポリマーP;
2.5~10重量%の前記アゾラジカル開始剤I;
10~20重量%の前記接着促進剤AD;
5~8重量%の前記粘着性付与剤T;
0.5~1.5重量%の前記酸化防止剤AO;
0.5~1.5重量%の前記ポリアクリレートAC。 - 中空構造物用のバッフル要素及び/又は強化要素であって、前記要素が、請求項1~9のいずれか一項に記載の熱膨張性組成物を含むか又はそれから本質的になる、バッフル要素及び/又は強化要素。
- 前記要素が、キャリアを含み、前記キャリアの上に前記熱膨張性組成物が堆積させられているか又は取り付けられており、前記キャリアが、熱可塑性材料でできている、請求項10に記載のバッフル要素及び/又は強化要素。
- 前記熱膨張性組成物が、前記キャリア上へ射出成形されるか、又は前記キャリアと共押出される、請求項11に記載のバッフル要素及び/又は強化要素の製造方法。
- 請求項1~9のいずれか一項に記載の熱膨張性組成物の発泡方法であって、前記熱膨張性組成物を、10~60分間で120~200℃の温度に付し、かつ/又は1~60分間で前記組成物の表面に少なくとも2.5mW/cm-2のUV強度でUV照射に付す、方法。
- 騒音、振動、湿気、及び/若しくは熱の伝達が低減するように、かつ/又は前記空洞を取り囲む物体が機械的に強化されるように、陸上車両、水上車両、又は航空機の空洞若しくは中空構造物、及び/又は建物の空洞を、密封し、遮断し、又は強化するための請求項10又は11に記載のバッフル要素及び/又は強化要素の使用。
- 請求項1~9のいずれか一項に記載の熱膨張性組成物を含む要素を、前記空洞若しくは中空構造に導入し、その後、熱及び/若しくはUV処理によって膨張させて、それにより前記空洞若しくは中空構造を、膨張した組成物によって少なくとも部分的に満たす、空洞若しくは中空構造の密封、遮断及び/若しくは強化方法。
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