JP7300384B2 - ポリウレタンホットメルト接着剤、それを用いた積層体及び積層体の製造方法 - Google Patents
ポリウレタンホットメルト接着剤、それを用いた積層体及び積層体の製造方法 Download PDFInfo
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- JP7300384B2 JP7300384B2 JP2019535084A JP2019535084A JP7300384B2 JP 7300384 B2 JP7300384 B2 JP 7300384B2 JP 2019535084 A JP2019535084 A JP 2019535084A JP 2019535084 A JP2019535084 A JP 2019535084A JP 7300384 B2 JP7300384 B2 JP 7300384B2
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- JP
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- Prior art keywords
- melt adhesive
- polyurethane hot
- polyurethane
- temperature
- melt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/76—Polyisocyanates or polyisothiocyanates cyclic aromatic
- C08G18/7657—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings
- C08G18/7664—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups
- C08G18/7671—Polyisocyanates or polyisothiocyanates cyclic aromatic containing two or more aromatic rings containing alkylene polyphenyl groups containing only one alkylene bisphenyl group
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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Description
(株)東洋精機製作所製のキャピログラフ1C(キャピラリーレオメータ)を用いて溶融粘度測定を行った。具体的には、内径9.55mm, 有効長35mmの円筒状のチャンバーの底部に1mmφx10mmのキャピラリーをセットした。そして、所定の温度に加熱したチャンバー内に、粉砕したポリウレタンホットメルト接着剤を所定量充填し、ポリウレタンホットメルト接着剤を溶融させた。そして、チャンバー内にせん断速度6.08/sec~121.6/secの範囲でピストンを進行させ、そのときの応力から溶融粘度を測定した。そして、各温度における溶融粘度のせん断速度依存性のチャートから、各温度においてせん断速度12.1/secのときの溶融粘度が2.0×103Pa・sになる温度(℃)をX、1.0×105 Pa・sになる温度(℃)をYとして特定した。
幅25mm×長さ15cm×厚さ100μmのポリウレタンホットメルト接着剤のフィルムを製造した。そして、JIS K7311に準拠した引張試験機(テンシロン オリエンテック(株)製)を用いて、ヘッドスピード:100mm/分の条件でフィルムの100%モジュラスを測定した。
幅25mm×長さ15cmのサイズで、厚さ1.0mm、見掛け密度0.6g/cm3の立毛調人工皮革(スエード調人工皮革)と、同じサイズで厚さ3.0mm、見掛け密度0.3g/cm3のダブルラッセルタイプのメッシュ編物とを準備した。そして、立毛調人工皮革とメッシュ編物との間に、厚さ100μmのポリウレタンホットメルト接着剤のフィルムを介在させ、80℃~160℃の間で5℃毎の温度にそれぞれ設定した加温平板プレス機を用いて、圧力:6kgf/cm2、加圧時間:60秒間の条件で熱接着した。そして、室温で1日間冷却して積層体を得た。そして、引張試験機(テンシロン オリエンテック(株))を用いて積層体の接着強力を測定した。そして、積層体の接着強力が2.5kg/cm以上となったときの温度の範囲を特定し、その温度幅を接着良好温度幅とした。
幅25mm×長さ15cmのサイズで、厚さ1.0mm、見掛け密度0.6g/cm3の立毛調人工皮革片同士の間に、厚さ100μmのポリウレタンホットメルト接着剤のフィルムを介在させた積重体を形成した。そして、前述の〈繊維構造体の接着良好温度幅〉の測定において最高の接着強力を達成したときの温度に設定した加温平板プレス機を用いて、圧力:6kgf/cm2、加圧時間:60秒間の条件で積重体を熱プレスした後、室温で1日間放置して積層体を得た。そして、引張試験機(テンシロン オリエンテック(株))を用いて積層体の接着強力(S0)を測定した。また、同様に作成した積層体を、温度70℃、相対湿度95%の恒温恒湿槽内に3週間放置した。そして、恒温恒湿槽から積層体を取り出し、同様に接着強力(S1)を測定した。そして、接着強力の保持率(%)をS1/S0×100の式から求めた。
幅25mm×長さ15cmのサイズで、厚さ1.0mmの、ポリエーテルポリウレタン(大日精化工業(株)製のレザミン ME-1085EA)のフィルムを銀面層として有した見掛け密度0.5g/cm3の銀付調人工皮革を準備した。そして、その銀付調人工皮革の銀面層同士を、厚さ100μmの各ポリウレタンホットメルト接着剤のフィルムを介在させ、前述の〈繊維構造体の接着良好温度幅〉の測定において最高の剥離強力を達成したときの温度に設定した加温平板プレス機を用いて、圧力:6kgf/cm2、加圧時間:60秒間の条件で熱接着した。そして、室温で1日間冷却させた後、その後、引張試験機を用いて接着強力を測定した。
ソフトネステスター(皮革ソフトネス計測装置ST300:英国、MSAエンジニアリングシステム社製)を用いて剛軟度を測定した。具体的には、直径25mmの所定のリングを装置の下部ホルダーにセットした後、下部ホルダーに上記〈繊維構造体の接着良好温度幅〉の測定で作成したものと同じ構成の積層体をセットした。そして、上部レバーに固定された金属製のピン(直径5mm)を積層体に向けて押し下げた。そして、上部レバーを押し下げて上部レバーがロックしたときの数値を異なる5カ所で測定し、その平均値を読み取った。なお、数値は侵入深さを表し、数値が大きいほどしなやかであることを表す。
数平均分子量4000のポリプロピレングリコール(以下PPG4000とも称する、水酸基価28mgKOH/g) 40質量部と、数平均分子量1000のポリプロピレングリコール(以下PPG1000とも称する、水酸基価112mgKOH/g) 100質量部と、4,4‘-ジフェニルメタンジイソシアネート(以下、MDIとも称する) 60質量部と鎖伸長剤である1,4-ブタンジオール(以下、1,4-BDとも称する) 12.5質量部とを反応容器に仕込み、140℃で3時間加熱してブロック状の熱可塑性ポリウレタンを得た。そして、得られた熱可塑性ポリウレタンを粉砕し、Tダイ溶融押出成形法によって厚さ100μmのポリウレタンホットメルト接着剤のフィルムを作成した。そして、得られたポリウレタンホットメルト接着剤を用いて、上記評価方法に従って評価した。結果を表1に示す。
PPG4000 20質量部と、PPG1000 40質量部と、数平均分子量2000のポリエチレンプロピレンアジペート(以下PEPA2000とも称する、水酸基価56mgKOH/g) 40質量部と、MDI 50質量部と、1,4-BD 13.1質量部とを反応容器に仕込み、140℃で3時間加熱してブロック状の熱可塑性ポリウレタンを得た。そして、得られた熱可塑性ポリウレタンを粉砕し、Tダイ溶融押出成形法によって厚さ100μmのポリウレタンホットメルト接着剤のフィルムを作成した。そして、得られたポリウレタンホットメルト接着剤を用いて、上記評価方法に従って評価した。結果を表1に示す。
数平均分子量3000のポリプロピレングリコール(以下PPG3000とも称する、水酸基価37mgKOH/g) 20質量部と、数平均分子量500のポリプロピレングリコール(以下PPG500とも称する、水酸基価223mgKOH/g) 90質量部と、MDI 80質量部と、1,4-BD 12.5質量部とを反応容器に仕込み、140℃で3時間加熱してブロック状の熱可塑性ポリウレタンを得た。そして、得られた熱可塑性ポリウレタンを粉砕し、Tダイ溶融押出成形法によって厚さ100μmのポリウレタンホットメルト接着剤のフィルムを作成した。そして、得られたポリウレタンホットメルト接着剤を用いて、上記評価方法に従って評価した。結果を表1に示す。
数平均分子量2000のポリプロピレングリコール(以下PPG2000とも称する、水酸基価56mgKOH/g)50質量部と、PPG1000 50質量部と、MDI 40質量部と、1,4-BD 10質量部とを反応容器に仕込み、140℃で3時間加熱してブロック状の熱可塑性ポリウレタンを得た。そして、得られた熱可塑性ポリウレタンを粉砕し、Tダイ溶融押出成形法によって厚さ100μmのポリウレタンホットメルト接着剤のフィルムを作成した。そして、得られたポリウレタンホットメルト接着剤を用いて、上記評価方法に従って評価した。結果を表1に示す。
PPG3000 130質量部と、PPG1000 50質量部と、MDI 50質量部と1,4-BD 12質量部とを反応容器に仕込み、140℃で3時間加熱してブロック状の熱可塑性ポリウレタンを得た。そして、得られた熱可塑性ポリウレタンを粉砕し、Tダイ溶融押出成形法によって厚さ100μmのポリウレタンホットメルト接着剤のフィルムを作成した。そして、得られたポリウレタンホットメルト接着剤を用いて、上記評価方法に従って評価した。結果を表1に示す。
PPG2000 20質量部と、PPG500 80質量部と、MDI 80質量部と、1,4-BD 12.5質量部とを反応容器に仕込み、140℃で3時間加熱してブロック状の熱可塑性ポリウレタンを得た。そして、得られた熱可塑性ポリウレタンを粉砕し、Tダイ溶融押出成形法によって厚さ100μmのポリウレタンホットメルト接着剤のフィルムを作成した。そして、得られたポリウレタンホットメルト接着剤を用いて、上記評価方法に従って評価した。結果を表1に示す。
PPG4000 20質量部と、PPG500 30質量部と、MDI 45質量部と、1,4-BD 10質量部とを反応容器に仕込み、140℃で3時間加熱してブロック状の熱可塑性ポリウレタンを得た。そして、得られた熱可塑性ポリウレタンを粉砕し、Tダイ溶融押出成形法によって厚さ100μmのポリウレタンホットメルト接着剤のフィルムを作成した。そして、得られたポリウレタンホットメルト接着剤を用いて、上記評価方法に従って評価した。結果を表1に示す。
PPG4000 30質量部と、PPG1000 30質量部と、PEPA2000 60質量部と、MDI 50質量部と、1,4-BD 12.5質量部とを反応容器に仕込み、140℃で3時間加熱し、ブロック状の熱可塑性ポリウレタンを得た。そして、得られた熱可塑性ポリウレタンを粉砕し、Tダイ溶融押出成形法によって厚さ100μmのポリウレタンホットメルト接着剤のフィルムを作成した。そして、得られたポリウレタンホットメルト接着剤を用いて、上記評価方法に従って評価した。結果を表1に示す。
数平均分子量3000のポリエチレンプロピレンアジペート(PEPA3000と称する、水酸基価37mgKOH/g) 60質量部と、数平均分子量1000のポリエチレンプロピレンアジペート(PEPA1000と称する、水酸基価112mgKOH/g)100質量部と、MDI 55質量部と1,4-BD 11.5質量部を反応容器に仕込み、140℃で3時間加熱してブロック状の熱可塑性ポリウレタンを得た。そして、得られた熱可塑性ポリウレタンを粉砕し、Tダイ溶融押出成形法によって厚さ100μmのポリウレタンホットメルト接着剤のフィルムを作成した。そして、得られたポリウレタンホットメルト接着剤を用いて、上記評価方法に従って評価した。結果を表1に示す。
PPG3000 100質量部と、MDI 35質量部と、1,4-BD 9.5質量部とを反応容器に仕込み、140℃で3時間加熱してブロック状の熱可塑性ポリウレタンを得た。そして、得られた熱可塑性ポリウレタンを粉砕し、Tダイ溶融押出成形法によって厚さ100μmのポリウレタンホットメルト接着剤のフィルムを作成した。そして、得られたポリウレタンホットメルト接着剤を用いて、上記評価方法に従って評価した。結果を表1に示す。
PPG3000 160質量部と、PPG1000 40質量部と、MDI 45質量部と、1,4-BD 12質量部とを反応容器に仕込み、140℃で3時間加熱してブロック状の熱可塑性ポリウレタンを得た。そして、得られた熱可塑性ポリウレタンを粉砕し、Tダイ溶融押出成形法によって厚さ100μmのポリウレタンホットメルト接着剤のフィルムを作成した。そして、得られたポリウレタンホットメルト接着剤を用いて、上記評価方法に従って評価した。結果を表1に示す。
2,3,4,5 部材
10 ポリウレタンホットメルト接着剤のフィルム
Claims (9)
- 高分子ポリオールとポリイソシアネートと鎖伸長剤とを含む原料の反応物である熱可塑性ポリウレタンを含み、
前記高分子ポリオールは、互いに数平均分子量が1000以上異なる少なくとも2種のポリプロピレングリコールを60質量%以上含有し、
溶融粘度が2.0×103Pa・sになる温度(℃)をX、1.0×105Pa・sになる温度をYとしたときに、X-Y≧15であり、
100%モジュラスが2.5MPa以上であるポリウレタンホットメルト接着剤。 - X-Y≧19である請求項1に記載のポリウレタンホットメルト接着剤。
- X≧135、130≧Yである請求項1または2に記載のポリウレタンホットメルト接着剤。
- 前記少なくとも2種のポリプロピレングリコールの数平均分子量が500~5000の範囲である請求項1~3の何れか1項に記載のポリウレタンホットメルト接着剤。
- 100%モジュラスが2.5~6.0MPaである請求項1~4の何れか1項に記載のポリウレタンホットメルト接着剤。
- フィルムである請求項1~5の何れか1項に記載のポリウレタンホットメルト接着剤。
- 基材の表面に、請求項1~6の何れか1項に記載のポリウレタンホットメルト接着剤で接着された少なくとも2枚の部材を積層した積層体。
- 前記基材は繊維構造体であり、
前記2枚の部材は、互いに織編構造が異なる繊維構造体である請求項7に記載の積層体。 - 基材の表面に、接着剤を介して、織編構造が互いに異なる少なくとも2枚の繊維構造体を配した積重体を形成する工程と、
前記積重体を熱プレスして積層体を形成する工程と、を備え、
前記接着剤が請求項1~7の何れか1項に記載のポリウレタンホットメルト接着剤である積層体の製造方法。
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