JP2013527052A - 硬化性組成物、複合材製造のための前記組成物の使用プロセス、ならびに優れた表面仕上げおよび高い繊維固着を有する複合材の製造プロセス - Google Patents
硬化性組成物、複合材製造のための前記組成物の使用プロセス、ならびに優れた表面仕上げおよび高い繊維固着を有する複合材の製造プロセス Download PDFInfo
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- JP2013527052A JP2013527052A JP2013505025A JP2013505025A JP2013527052A JP 2013527052 A JP2013527052 A JP 2013527052A JP 2013505025 A JP2013505025 A JP 2013505025A JP 2013505025 A JP2013505025 A JP 2013505025A JP 2013527052 A JP2013527052 A JP 2013527052A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/32—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof from compositions containing microballoons, e.g. syntactic foams
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
- C08J9/228—Forming foamed products
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- 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
- B29C44/12—Incorporating or moulding on preformed parts, e.g. inserts or reinforcements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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Landscapes
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Composite Materials (AREA)
- Reinforced Plastic Materials (AREA)
- Moulding By Coating Moulds (AREA)
- Casting Or Compression Moulding Of Plastics Or The Like (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Laminated Bodies (AREA)
Abstract
Description
(a)熱硬化性樹脂組成物を、プレフォームを含む密閉金型内に用意するステップであって、それらの各々が任意に、体積膨張が可能な物質を有する、ステップ;
(b)金型の内部を、熱硬化性樹脂組成物でプレフォームを湿潤するのに十分な第1の高い温度および高い圧力に曝すステップ;および
(c)熱硬化性樹脂組成物で含浸されたプレフォームを、第2の高い温度で金型内で硬化させ、RTM製品を形成するステップ
を含む。ただし、当然ながら、体積膨張が可能な物質が繊維または熱硬化性樹脂組成物の少なくとも1つに存在する。
プレフォームを、任意に、体積膨張が可能な物質と共に、金型内に用意するステップ;
熱硬化性樹脂組成物を、その組成物がプレフォームを湿潤するのに十分な時間、第1の高い温度および減圧下で金型内に用意するステップであって、熱硬化性樹脂組成物は、任意に、体積膨張が可能な物質を含む、ステップ;および
熱硬化性樹脂組成物で湿潤されたプレフォームを含む金型を、前記組成物で湿潤されたプレフォームを金型内で硬化するのに十分な第2の高い温度に減圧下で曝してVaRTM製品を形成するステップ
を含む。
プレフォームを、フィルム状の熱硬化性樹脂組成物を含む密閉金型内に用意するステップであって、それらの各々が任意に、体積膨張が可能な物質を含む、ステップ;
プレフォームに熱硬化性樹脂組成物を注入するのに十分な時間、金型の内部を第1の高い温度および任意に減圧に曝すと同時に、金型の外部を高い圧力に曝すステップ;および
熱硬化性樹脂組成物が注入されたプレフォームを、金型内で第2の高い温度で硬化させ、RFI製品を形成するステップを含む。ただし、当然ながら、体積膨張が可能な物質が繊維または熱硬化性樹脂組成物の少なくとも1つに存在する。
(a)繊維、例えば、層状の繊維を、任意に、体積膨張が可能な物質と共に、用意するステップ;
(b)熱硬化性樹脂組成物を、任意に、体積膨張が可能な物質と共に、用意するステップ;および
(c)プリプレグアセンブリを形成するために熱硬化性樹脂組成物と繊維とを接合し、得られたプリプレグアセンブリを、繊維に熱硬化性樹脂組成物を注入するのに十分な高い温度および圧力条件に曝してプリプレグを形成する、ステップ
を含む。
(a)繊維を、任意に、体積膨張が可能な物質と共に、用意するステップ;
(b)液状の熱硬化性樹脂組成物を、任意に、体積膨張が可能な物質と共に、用意するステップ;
(c)繊維に熱硬化性樹脂組成物を注入してプリプレグアセンブリを形成するために、繊維を、液体熱硬化性樹脂組成物中を通過させるステップ;および
(d)過剰の熱硬化性樹脂組成物をプリプレグアセンブリから取り除くステップ
を含む。
(a)熱硬化性樹脂組成物を、プレフォームを含む密閉金型内に用意するステップであって、それらの各々は任意に、体積膨張が可能な物質を含むか、または体積膨張が可能な物質と接触している、ステップ;
(b)金型の内部を、熱硬化性樹脂組成物でプレフォームを湿潤するのに十分な第1の高い温度および高い圧力に曝すステップ;および
(c)熱硬化性樹脂組成物が含浸されたプレフォームを、金型内で第2の高い温度で硬化し、RTM製品を形成するステップ
を含む。ただし、当然ながら、体積膨張が可能な物質が繊維または熱硬化性樹脂組成物の少なくとも1つに存在する。
(a)プレフォームを金型内に用意するステップであって、プレフォームは任意に体積膨張が可能な物質と接触している、ステップ;
(b)熱硬化性樹脂組成物を、プレフォームを湿潤するのに十分な時間、第1の高い温度および減圧下で金型内に用意するステップであって、熱硬化性樹脂組成物は任意に、体積膨張が可能な物質を含む、ステップ;および
(c)組成物で湿潤されたプレフォームを含む金型を、熱硬化性樹脂組成物で湿潤されたプレフォームを金型内で硬化するのに十分な第2の高い温度に減圧下で曝し、VaTRM製品を形成する、ステップ
を含む。
(a)プレフォームを、フィルム状の熱硬化性樹脂組成物を含む密閉金型内に用意するステップであって、それらの各々は任意に、体積膨張が可能な物質を含む、ステップ;
(b)プレフォームに熱硬化性樹脂組成物を注入するのに十分な時間、金型内部を第1の高い温度および任意に減圧に曝すと同時に金型外部を高い圧力に曝すステップ;および
(c)熱硬化性樹脂組成物が注入されたプレフォームを、金型内で第2の高い温度で硬化しRFI製品を形成する、ステップ
を含む。ただし、当然ながら、体積膨張が可能な物質が、繊維または熱硬化性樹脂組成物の少なくとも1つに存在する。これらの実施形態の特定の態様では、体積膨張が可能な物質はフィルム形態で存在する。すなわち、一般的に言うと、a.剥離紙;b.樹脂成分;およびc.膨張性物質を含む、フィルムが提供される。
a.プレフォームを金型内に用意するステップ;
b.フィルムを金型内に配置されたプレフォーム上に用意するステップ;
c.樹脂を金型内に用意するステップ;
d.複合材またはラミネート部品を形成するために、プレフォーム、フィルムおよび樹脂を、樹脂を硬化およびフィルムを膨張させるのに適した条件に曝すステップ;および
e.膨張されたフィルムを複合材またはラミネート部品から取り除き、表面仕上げおよび樹脂固着が改善された複合材またはラミネート部品を得るステップ
を含む。
RTMプロセスで使用するための樹脂を下の表に示す。試料No.2は本発明の樹脂(膨張性微小球を有する)を表し、試料No.1はコントロール(膨張性微小球を有しない)を表す。
・配合物を温度160°Fに予熱する。
・プレフォームを密閉金型内に挿入する。
・金型を温度250°Fに予熱する。
・金型を1時間減圧下に置き、プレフォームから揮発物を除去する。
・樹脂注入装置を温度235°Fに予熱する。
・事前加熱した配合物を注入装置に添加する。
・配合物が温度250°Fで平衡に達したら、15分間高真空下に置き空気を除去する。
・真空を解除する。
・約20psiの注入圧力によって、1分当たり約5から200ccの速度で配合物を注入する。注入全体を通して所望の流速を維持することが望まれる場合は、注入圧力を高めてもよい。
・プレフォームを完全に含浸させ、金型樹脂出口部を閉じる。
・金型を100psiに加圧し、その圧力で約10分間保持する。
・1分当たり3°Fで金型温度を350°Fに上げる。
・配合物がゲル化したら、加えている圧力を解除する。
・3時間、温度350°Fに保持する。
・温度を120°Fに下げる。
・金型を開き、硬化部品を取り出す。
繊維とのプリプレグ化プロセスにおいて、特定の量の記載された成分と共に使用する樹脂を以下の表に示す。
成分としてビスフェノール−A系エポキシ樹脂、エポキシ付加物、疎水性ヒュームドシリカ、4,4−ジアミノジフェニルスルホンおよびジシアンジアミドを含む組成物からフィルム層を製造した。これらの成分を混合し、次いで厚さ0.1mmのフィルムへの成形を膨張性物質としてEXPANCEL 091 DU 80を10重量%使用して行った。
Claims (43)
- (a)熱硬化性樹脂組成物を、任意に、膨張が可能な物質と共に、プレフォームを含む密閉金型内に用意するステップ;
(b)金型の内部を、プレフォームを熱硬化性樹脂組成物で湿潤するのに十分な第1の高い温度および高い圧力に曝すステップ;および
(c)熱硬化性樹脂組成物が含浸されたプレフォームを、前記金型内で第2の高い温度で硬化して樹脂トランスファー成形製品を形成するステップ
を含み、
前記熱硬化性樹脂組成物は(i)熱硬化性樹脂を含み、かつ前記熱硬化性樹脂組成物または前記プレフォームの少なくとも1つは膨張が可能な物質を含む、
樹脂トランスファー成形プロセス。 - 前記熱硬化性樹脂組成物が、さらに(ii)強化剤成分を含む、請求項1に記載の樹脂トランスファー成形プロセス。
- 前記熱硬化性樹脂組成物が、エポキシ、エピスルフィド、オキサジン、オキサゾリン、シアネートエステル、マレイミド、ナジミド、イタコンイミド、フェノール、チオフェノール樹脂およびそれらの組合せからなる群より選択される、請求項1に記載の樹脂トランスファー成形プロセス。
- 前記熱硬化性樹脂組成物が、樹脂注入温度において10から3000センチポアズの範囲にある粘度を有する、請求項1に記載の樹脂トランスファー成形プロセス。
- 前記熱硬化性樹脂組成物の粘度がプロセス条件下で100%増加する間の時間が、注入温度で30分から10時間の範囲にある、請求項1に記載の樹脂トランスファー成形プロセス。
- 複数の織物層または一方向層が、ガラス、炭素、アラミドおよびセラミックから選択される繊維を含む、請求項1に記載の樹脂トランスファー成形プロセス。
- 前記膨張が可能な物質が、複数の膨張性微小球である、請求項1に記載の樹脂トランスファー成形プロセス。
- 請求項1から7に記載のプロセスによって製造された樹脂トランスファー成形製品。
- (a)複数の織物層または一方向層;
(b)前記複数の織物層または一方向層に付与された、(i)オキサジン成分を含む熱硬化性バインダー組成物;および
(c)体積膨張が可能な物質
を含み、前記物質は、(a)または(b)の少なくとも1つと共に、または(a)または(b)の少なくとも1つの中にそれぞれ存在する、
樹脂トランスファー成形プレフォーム。 - 前記熱硬化性バインダー組成物が、さらに任意に、熱可塑性材料、ゴム、金属、炭素、コアシェル、セラミックおよびそれらの組合せから構成される粒子からなる群より選択されるスペーサーを含む、請求項9に記載の樹脂トランスファー成形プレフォーム。
- (a)任意に、膨張が可能な物質を含むプレフォームを、金型内に用意するステップ;
(b)熱硬化性樹脂組成物を、前記組成物でプレフォームを湿潤させるのに十分な時間、第1の高い温度および減圧下で金型内に用意するステップであってここで前記樹脂組成物が含まれるステップ;および
(c)組成物で湿潤されたプレフォームを含む金型を、減圧下、熱硬化性樹脂組成物で湿潤されたプレフォームを金型内で硬化するのに十分な第2の高い温度に曝し、樹脂トランスファー成形製品を形成するステップ
を含み、前記熱硬化性樹脂組成物は(i)オキサジン成分を含み、かつ、前記プレフォームまたは前記熱硬化性樹脂組成物の少なくとも1つは膨張が可能な物質を含む、
減圧補助樹脂トランスファー成形プロセス。 - 前記プレフォームを用意した後、分散媒体がその上に提供される、請求項11に記載の減圧補助樹脂トランスファー成形プロセス。
- 前記熱硬化性樹脂組成物が、さらに(ii)強化剤成分を含む、請求項11に記載の減圧補助樹脂トランスファー成形プロセス。
- 前記熱硬化性樹脂組成物が、エポキシ、エピスルフィド、オキサジン、オキサゾリン、シアネートエステル、マレイミド、ナジミド、イタコンイミド、フェノール、チオフェノール樹脂およびそれらの組合せからなる群より選択される、請求項11に記載の減圧補助樹脂トランスファー成形プロセス。
- 前記熱硬化性樹脂組成物が、トランスファー成形温度において10から2000センチポアズの範囲の粘度を有する、請求項11に記載の減圧補助樹脂トランスファー成形プロセス。
- 前記熱硬化性樹脂組成物の粘度が、プロセス条件下で100%増加する間の時間が、樹脂トランスファー温度で30分から10時間の範囲にある、請求項11に記載の減圧補助樹脂トランスファー成形プロセス。
- 前記プレフォームが、ガラス、炭素、アラミド、セラミックおよびそれらの組合せから選択される繊維を含む、請求項11に記載の減圧補助樹脂トランスファー成形プロセス。
- 請求項11から17に記載のプロセスによって製造された減圧補助樹脂トランスファー成形製品。
- (a)任意に、膨張が可能な物質を有する、複数の織物層または一方向層;および
(b)前記複数の織物層または一方向層に付与され、任意に、膨張が可能な物質を有する、熱硬化性バインダー組成物
を含み、前記熱硬化性バインダー組成物は(i)オキサジン成分を含み、かつ、前記複数の織物層または一方向層または熱硬化性バインダー組成物の少なくとも1つは、膨張が可能な物質を含む、
減圧補助樹脂トランスファー成形プレフォーム。 - 前記熱硬化性バインダー組成物が、さらに(ii)強化剤成分を含む、請求項19に記載の減圧補助樹脂トランスファー成形プレフォーム。
- 前記熱硬化性バインダー組成物が、エポキシ、エピスルフィド、オキサジン、オキサゾリン、シアネートエステル、マレイミド、ナジミド、イタコンイミド、フェノール、チオフェノール樹脂およびそれらの組合せからなる群より選択される、請求項19に記載の減圧補助樹脂トランスファー成形プレフォーム。
- 前記熱硬化性バインダー組成物が、さらに任意に、熱可塑性材料、ゴム、金属、炭素、コアシェル、セラミックおよびそれらの組合せから構成される粒子からなる群より選択されるスペーサーを含む、請求項19に記載の減圧補助樹脂トランスファー成形プレフォーム。
- 前記複数の織物層または一方向層が、ガラス、炭素、アラミド、セラミックおよびそれらの組合せから選択される繊維を含む、請求項19に記載の減圧補助樹脂トランスファー成形プレフォーム。
- (a)各々が膨張が可能な物質である、フィルム状の熱硬化性樹脂組成物を含む密閉金型に、プレフォームを用意するステップ;
(b)熱硬化性樹脂組成物をプレフォームに注入するのに十分な時間、金型の内部を第1の高い温度および任意に減圧に曝すと同時に、金型の外部を高い圧力に曝すステップ;および
(c)熱硬化性樹脂組成物が注入されたプレフォームを、金型内で第2の高い温度で硬化して樹脂トランスファー成形製品を形成するステップ
を含み、前記熱硬化性樹脂組成物は(i)オキサジン成分を含み、かつ、前記プレフォームまたは前記フィルム状の熱硬化性樹脂組成物の少なくとも1つは、膨張が可能な物質を含む、
樹脂フィルム注入プロセス。 - 前記熱硬化性樹脂組成物が、さらに(ii)強化剤成分を含む、請求項24に記載の樹脂フィルム注入プロセス。
- 前記熱硬化性樹脂組成物が、エポキシ、エピスルフィド、オキサジン、オキサゾリン、シアネートエステル、マレイミド、ナジミド、イタコンイミド、フェノール、チオフェノール樹脂およびそれらの組合せからなる群より選択される、請求項24に記載の樹脂フィルム注入プロセス。
- 前記熱硬化性樹脂組成物が、注入温度で10から5000センチポアズの範囲にある粘度を有する、請求項24に記載の樹脂フィルム注入プロセス。
- 前記熱硬化性樹脂組成物の粘度が、プロセス条件下で100%増加する時間が、注入温度で30分から10時間の範囲にある、請求項24に記載の樹脂フィルム注入プロセス。
- 前記プレフォームが、ガラス、炭素、アラミド、セラミックおよびそれらの組合せから選択される繊維を含む、請求項24に記載の樹脂フィルム注入プロセス。
- 請求項24から29に記載のプロセスによって製造される、樹脂フィルム注入製品。
- 熱硬化性樹脂組成物が注入された繊維を含むプリプレグであって、樹脂成分を含み、前記繊維または樹脂成分の少なくとも1つは膨張が可能な物質を含む、プリプレグ。
- 複数の繊維を用意するステップ;
樹脂成分を含む熱硬化性樹脂組成物を用意するステップ;
膨張が可能な物質を用意するステップ
を含み、前記繊維の少なくとも1つは、膨張が可能な物質を前記繊維の層上または繊維の層周囲に含む、
プリプレグプロセス。 - 前記繊維が、層状に配向している、請求項31に記載のプリプレグ。
- 前記繊維層が、一方向繊維から製造される、請求項9に記載のプリプレグ。
- 前記繊維層が、繊維織物から製造される、請求項9に記載のプリプレグ。
- (a)繊維層を用意するステップ;
(b)液状の熱硬化性樹脂組成物を用意するステップ;
(c)繊維層に熱硬化性樹脂組成物を注入することによりプリプレグアセンブリを形成するために、繊維層を、液体の熱硬化性樹脂組成物中を通過させるステップ;および
(d)過剰の熱硬化性樹脂組成物をプリプレグアセンブリから取り除くステップ
を含み、前記熱硬化性樹脂組成物は(i)オキサジン成分を含み、かつ、前記繊維層または前記熱硬化性樹脂組成物の少なくとも1つは、膨張が可能な物質を含む、
プリプレグを製造するためのプロセス。 - 前記プリプレグアセンブリが、高い温度および圧力条件に曝される、請求項36に記載のプロセス。
- 請求項32に記載のプロセスによって製造されるプリプレグ。
- 請求項36に記載のプロセスによって製造されるプリプレグ。
- 請求項38に記載のプリプレグの硬化反応製品。
- 請求項39に記載のプリプレグの硬化反応製品。
- a.剥離紙、
b.樹脂成分、および
c.膨張性物質
を含む、フィルム。 - a.金型内にプレフォームを用意するステップ;
b.金型内に配置されたプレフォーム上に、請求項42に記載のフィルムを用意するステップ;
c.金型内に樹脂を用意するステップ;
d.プレフォーム、フィルムおよび樹脂を、樹脂を硬化してフィルムを膨張させるのに適した条件に曝し、複合材またはラミネート部品を形成するステップ;および
e.複合材またはラミネートから膨張フィルムを取り除き、表面仕上げおよび樹脂固着が改善された複合材またはラミネート部品を得るステップ
を含む、複合材またはラミネート部品の表面仕上げおよび複合材またはラミネート部品における樹脂固着を改善するためのプロセス。
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WO2017099060A1 (ja) * | 2015-12-10 | 2017-06-15 | 三菱レイヨン株式会社 | トウプリプレグ、複合材料補強圧力容器および複合材料補強圧力容器の製造方法 |
JP6222387B1 (ja) * | 2015-12-10 | 2017-11-01 | 三菱ケミカル株式会社 | トウプリプレグ、複合材料補強圧力容器および複合材料補強圧力容器の製造方法 |
US10889695B2 (en) | 2015-12-10 | 2021-01-12 | Mitsubishi Chemical Corporation | Tow prepreg, composite material-reinforced pressure vessel, and method of producing composite material-reinforced pressure vessel |
Also Published As
Publication number | Publication date |
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WO2011130188A2 (en) | 2011-10-20 |
US20130035013A1 (en) | 2013-02-07 |
JP6253979B2 (ja) | 2017-12-27 |
WO2011130188A3 (en) | 2012-04-19 |
EP2558266B1 (en) | 2020-10-21 |
JP2016026239A (ja) | 2016-02-12 |
CN103201079B (zh) | 2015-09-09 |
CN105108929A (zh) | 2015-12-02 |
US20160009891A1 (en) | 2016-01-14 |
CN105108929B (zh) | 2021-06-22 |
ES2851010T3 (es) | 2021-09-02 |
EP2558266A4 (en) | 2017-09-06 |
JP6167145B2 (ja) | 2017-07-19 |
CN103201079A (zh) | 2013-07-10 |
US9168703B2 (en) | 2015-10-27 |
EP2558266A2 (en) | 2013-02-20 |
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