JP6795403B2 - 接着剤組成物 - Google Patents
接着剤組成物 Download PDFInfo
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- JP6795403B2 JP6795403B2 JP2016575787A JP2016575787A JP6795403B2 JP 6795403 B2 JP6795403 B2 JP 6795403B2 JP 2016575787 A JP2016575787 A JP 2016575787A JP 2016575787 A JP2016575787 A JP 2016575787A JP 6795403 B2 JP6795403 B2 JP 6795403B2
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- IGALFTFNPPBUDN-UHFFFAOYSA-N phenyl-[2,3,4,5-tetrakis(oxiran-2-ylmethyl)phenyl]methanediamine Chemical compound C=1C(CC2OC2)=C(CC2OC2)C(CC2OC2)=C(CC2OC2)C=1C(N)(N)C1=CC=CC=C1 IGALFTFNPPBUDN-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000005077 polysulfide Substances 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 239000010902 straw Substances 0.000 description 1
- DDGDWXGKPCHUCI-UHFFFAOYSA-N strontium;hydrate Chemical compound O.[Sr] DDGDWXGKPCHUCI-UHFFFAOYSA-N 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000012747 synergistic agent Substances 0.000 description 1
- 229920002994 synthetic fiber Polymers 0.000 description 1
- 239000012209 synthetic fiber Substances 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- FAGUFWYHJQFNRV-UHFFFAOYSA-N tetraethylenepentamine Chemical compound NCCNCCNCCNCCN FAGUFWYHJQFNRV-UHFFFAOYSA-N 0.000 description 1
- 238000001757 thermogravimetry curve Methods 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000003190 viscoelastic substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
Classifications
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- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/182—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing using pre-adducts of epoxy compounds with curing agents
-
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/02—Polycondensates containing more than one epoxy group per molecule
-
- C—CHEMISTRY; METALLURGY
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/20—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the epoxy compounds used
- C08G59/32—Epoxy compounds containing three or more epoxy groups
- C08G59/3227—Compounds containing acyclic nitrogen atoms
-
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
-
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/68—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used
- C08G59/686—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the catalysts used containing nitrogen
-
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/24—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs
- C08J5/249—Impregnating materials with prepolymers which can be polymerised in situ, e.g. manufacture of prepregs characterised by the additives used in the prepolymer mixture
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09J109/00—Adhesives based on homopolymers or copolymers of conjugated diene hydrocarbons
- C09J109/02—Copolymers with acrylonitrile
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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- C09J5/00—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers
- C09J5/06—Adhesive processes in general; Adhesive processes not provided for elsewhere, e.g. relating to primers involving heating of the applied adhesive
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4246—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof polymers with carboxylic terminal groups
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- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
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- Engineering & Computer Science (AREA)
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Description
(a)少なくとも1種の芳香族エポキシ樹脂;
(b)エポキシ樹脂ゴム付加物;
(c)アミン硬化剤;
及び
(d)油吸収剤
(e)防錆剤
(f)ウロン系促進剤。
の1つ以上
を含む接着剤組成物を提供する
他の記載と重複するが、以下に本発明を示す。
[発明1]
(a)少なくとも1種の芳香族エポキシ樹脂;
(b)エポキシ樹脂ゴム付加物;
(c)任意に、アミン硬化剤;及び任意に
(d)油吸収剤
(e)防錆剤
(f)ウロン系促進剤
の1種以上
を含む接着剤組成物。
[発明2]
(a)がビスフェノールAエポキシ樹脂を含む、発明1に記載の組成物。
[発明3]
(b)がビスフェノールFエポキシ樹脂から形成される付加物を含む、発明1又は2に記載の組成物。
[発明4]
(b)がニトリルゴムを含む、発明1から3のいずれか一項に記載の組成物。
[発明5]
(d)が無機充填剤、好ましくは、CaCO 3 を含む、発明1から4のいずれか一項に記載の組成物。
[発明6]
(e)がCrを実質的に含まない、発明1から5のいずれか一項に記載の組成物。
[発明7]
(f)が4,4−メチレンジフェニレンビス(N,N−ジメチル尿素)を含む、発明1から6のいずれか一項に記載の組成物。
[発明8]
前記組成物がフェノールノボラックエポキシ樹脂を更に含む、発明1から7のいずれか一項に記載の組成物。
[発明9]
前記組成物がエチレン酢酸ビニルコポリマーを更に含む、発明1から8のいずれか一項に記載の組成物。
[発明10]
前記組成物が、150℃にて150秒以下、好ましくは、120秒以下で硬化性を有する、発明1から9のいずれか一項に記載の組成物。
[発明11]
前記組成物が、23℃にてISO527に準拠して6MPaより高いラップせん断強度を有する硬化生成物を形成する硬化性を有する、発明1から10のいずれか一項に記載の組成物。
[発明12]
前記組成物が、前記組成物の全重量に基づいて、
(a)40から60重量%の芳香族エポキシ樹脂;及び/又は
(b)20から35重量%のエポキシ樹脂ゴム付加物;及び/又は
(c)3から7重量%のアミン硬化剤;及び/又は
(d)8から12重量%の油吸収剤;及び/又は
(e)0.1から2重量%の防錆剤;及び/又は
(f)2から6重量%のウロン系促進剤
を含む、発明1から11のいずれか一項に記載の組成物。
[発明13]
前記組成物が、40℃にて少なくとも110,000Pa.s、そして好ましくは、40℃にて120,000から200,000Pa.s、好ましくは130,000から350,000Pa.sの範囲、及び/又は前記範囲の組合せの粘度を有し(粘度は規定の温度にてASTM D445に準拠して測定する)、40℃以下にてフィルム又は半固体の形態である、発明1から12のいずれか一項に記載の組成物。
[発明14]
80℃における前記接着剤組成物の粘度が、100から1000Pa.s、好ましくは150から900Pa.s、より好ましくは250から800Pa.sの範囲、及び/又は前記値及び範囲の組合せである(粘度は規定の温度にてASTM D445に準拠して測定する)、発明1から13のいずれか一項に記載の組成物。
[発明15]
前記組成物を150℃に、210秒以下又は200秒以下、又は180秒以下又は150秒以下、好ましくは120秒以下の間、加熱する段階を含む、発明1から14のいずれか一項に記載の接着剤組成物を硬化する方法。
[発明16]
前記生成物が、少なくとも95%の硬化度、好ましくは、95から97%の間の硬化度に硬化される、発明15に記載の方法により得ることができる硬化生成物。
[発明17]
2つの表面を結合する方法であって、第1表面を、発明1から14のいずれか一項に記載の組成物に接触させる段階、及び前記組成物を、第2表面に接触させて硬化させる段階、を含む方法。
[発明18]
前記硬化させる段階が、150℃に、210秒以下又は200秒以下、又は180秒以下又は150秒以下、好ましくは、120秒以下の間、加熱する段階を含む、発明17に記載の方法。
[発明19]
前記第1表面及び第2表面の少なくとも1つが金属、好ましくは、鋼又はアルミニウムである、発明18又は17に記載の方法。
[発明20]
前記表面が油で汚染されている、発明17から19のいずれか一項に記載の方法。
[発明21]
発明17から20のいずれか一項に記載の方法により得ることができる複合物品。
[発明22]
繊維強化材と、発明1から14のいずれか一項に記載の組成物を含むプリプレグ。
[発明23]
複合材料を金属表面に結合するための、発明1から14のいずれか一項に記載の接着剤組成物の使用。
[発明24]
前記複合材料が強化樹脂マトリクス(rrm)を含む、発明23に記載の接着剤組成物の使用。
[発明25]
前記接着剤組成物と前記rrmを、同じ硬化段階で完全に硬化させる、発明24に記載の接着剤組成物の使用。
[発明26]
(a)少なくとも1種の芳香族エポキシ樹脂;
(b)エポキシ樹脂ゴム付加物;
(c)アミン硬化剤;
(d)ウロン系促進剤
を含む接着剤組成物であって、前記接着剤組成物が、150℃にて180秒で硬化して、本明細書に記載した方法に従って油が付着した鋼上で20MPaより高いラップせん断強度を示すことができる、接着剤組成物。
[発明27]
前記組成物が、触媒能を有する一成分接着剤組成物、好ましくは、触媒能を有するエポキシ系一成分接着剤組成物である、発明1から14のいずれか一項に記載の接着剤組成物。
(a)少なくとも1種の芳香族エポキシ樹脂;
(b)エポキシ樹脂ゴム付加物;
(c)アミン硬化剤;及び任意に、
(d)任意に、油吸収剤
(e)任意に、防錆剤
(f)ウロン系促進剤。
の1つ以上
を含む接着剤組成物が提供される。
(a)40から60重量%の芳香族エポキシ樹脂;及び
(b)20から35重量%のエポキシ樹脂ゴム付加物;及び
(c)3から7重量%のアミン硬化剤;及び
(d)8から12重量%の油吸収剤;及び
(e)0.1から2重量%の防錆剤;及び
(f)2から6重量%のウロン系促進剤。
(a)40から60重量%の芳香族エポキシ樹脂;
(b)20から35重量%のエポキシ樹脂ゴム付加物;
(c)3から7重量%のアミン硬化剤;
(d)8から12重量%の油吸収剤;
(e)0.1から2重量%の防錆剤;
(f)2から6重量%のウロン系促進剤。
本発明の接着剤組成物には、少なくとも1種の芳香族エポキシ樹脂が含まれる。本明細書中で言う芳香族エポキシ樹脂は、主鎖又は存在する場合には側鎖に少なくとも1種の芳香族単位を含有するエポキシ樹脂である。典型的には、芳香族エポキシ樹脂には、少なくとも1種の芳香族エポキシド、例えばグリシジルエーテルが、好ましくは、樹脂の主鎖又は存在する場合には側鎖の端部にて含まれる。使用することができる芳香族エポキシ樹脂には、例えば、フェノール(フェノール及びホルムアルデヒド)とエピクロロヒドリン、過酸エポキシ、グリシジルエステル、グリシジルエーテルの反応生成物、エピクロロヒドリンとアミノフェノールの反応生成物、エピクロロヒドリンとグリオキサールテトラフェノールの反応生成物等が含まれる。上記で言うフェノールには、多核フェノール(即ち、少なくとも2つのフェノール官能基を有する化合物)が含まれる。多核フェノールの典型的な例は、ビスフェノールである。
更に、本発明の接着剤組成物には、エポキシ樹脂ゴム付加物が含有される。エポキシ樹脂ゴム付加物が存在すると、エポキシ樹脂ゴム付加物が存在しない組成物と比較すると、硬化した場合に組成物のラップせん断強度が増加する。更に、エポキシゴム付加物は、ゴム成分と関連する大きい非極性領域をもたらし、これらは、油性汚染物を吸着し、且つ結合表面からそれらを除去することができる。従って、エポキシ樹脂付加物も、油吸収機能を提供する。
本発明の接着剤組成物には、硬化性エポキシ樹脂を架橋することができる少なくとも1種以上硬化剤が含まれる。典型的に、これらの薬剤(硬化剤)は、第一級又は第二級アミンである。アミンは、1つ以上のアミノ部分を有する脂肪族、脂環式、芳香族、又は芳香族構造体であってもよい。
任意に、接着剤組成物は、充填剤等の特性改良添加剤を含むことができる。これらは、接着を促進し、耐食性を改良し、熱又は電気の伝導性を改良し、接着剤のレオロジー特性を制御し、及び/又は硬化の間の収縮を低減させるために添加することができる。充填剤には、シリカゲル、カルシウムのケイ酸塩、リン酸塩、モリブデン酸塩、ヒュームドシリカ、非晶質シリカ、非晶質溶融シリカ、ベントナイト、有機粘土等の粘土、アルミニウム三水和物、中空ガラス微小球、中空高分子微小球及び炭酸カルシウムを含めることができる。充填剤を、流れ特性を改良し、そして組成物の嵩を増すために、本発明の接着剤組成物に有利に添加することができる。好ましい充填剤は、CaCO3、TiO(酸化チタン)、シリカ、マイクロバルーン、タルク、コロイドシリカ、カオリン、マイクロファイバー又はWest Epoxyから供給されるMicrolight(商標)から選択することができる。更に、組成物には、グルーライン厚さを制御可能とするために、充填剤粒子を含有させることができる。これらの粒子は、ガラスビーズ、酸化シリカ又はマイクロバルーンとすることができる。粒子のサイズは、50ミクロンから500ミクロン、好ましくは、100から200ミクロンの範囲とすることができる。本発明の実施態様では、接着剤組成物には、発泡剤を含めることができる。
油吸収剤には、直鎖脂肪族非極性付加物を有するエポキシ成分又は樹脂が含まれてもよい。油吸収剤には、前述したように、エポキシゴム付加物が含まれてもよい。我々は、これらのエポキシ樹脂成分又は樹脂が、本発明の組成物の好適な油吸収剤として作用することを発見した。
更に、接着剤組成物には、エポキシ成分に加えて、1種以上の防錆剤が含まれてもよく、これは、硬化した場合に防錆剤として機能する。追加的な防錆剤には、結合ラインで起こる腐食を抑制するための付加的な利益をもたらすことができる。典型的に、抑制剤は、潜在的な将来の環境規制に適合するようにCrを実質的に含まない。任意の適切な無機塩を、防錆剤として使用してもよい。抑制剤には、リン酸塩、リンケイ酸塩、チタン酸塩、亜鉛塩、ケイ酸塩、及びこれらの混合物が含まれてもよい。好ましい防錆剤は、ポリリン酸アルミニウムストロンチウム水和物である。更に、防錆剤には、相乗剤が含まれてもよい。好ましくは、防錆剤は、組成物中に、組成物の全重量に基づいて、0.1から12%重量%の量で、好ましくは、組成物の全重量に基づいて、0.5から2重量%の量で存在する。
接着剤組成物を、担体材料上で薄いフィルムに流延することができる。担体材料は、接着剤組成物を結合すべき表面に塗布した後、除去される紙又はポリマーの裏紙であってもよい。あるいは、担体は、2つの結合表面の間で、その場所に残っていてもよい。これには、異なる電極電位を有する2つの表面を絶縁する効果があり、従って、電解腐食を抑制する。電解腐食を抑制するための好適な担体には、ガラス繊維、熱可塑性樹脂及び天然材料のいずれかを含むシート、布及びベールが含まれる。
本発明の組成物は、150℃にて、150秒以下、好ましくは、120秒以下で硬化性である。この文脈において、「硬化性」は、本発明の組成物が、完全に硬化した組成物と比べて、硬化度のレベルが少なくとも95%に硬化することを意味する。硬化度のレベルは、以下のように測定することができる。
更に、本発明は、繊維強化材及び接着剤組成物を含むプリプレグを提供する。更に、本発明の接着剤組成物は、本発明とは異なる組成物の樹脂マトリクスを含むプリプレグに塗布した表面層として提供することができる。このような樹脂組成物は、以下では、強化樹脂マトリクス(rrm)と称する。
構造的な用途の場合、一般的に、繊維は、一方向に配向していると好ましい。一方向繊維層を使用する場合、繊維の配向は、プリプレグスタック全体では変えることができる。しかし、これは、一方向繊維層のスタックに対する多くの可能な配向の一つに過ぎない。例えば、隣接する層の一方向繊維は、互いに直角に、所謂、0°−90°配置に配置してもよく、これは、隣接する繊維層間の角を示す。他の配置、例えば、多くの他の配置で、0°−+45°、−45°、−90°も勿論可能である。
ラップせん断試験を、グリース及び汚れのない表面を得るために、揮発性溶剤(アセトン)で清浄化したHot Dip亜鉛めっき鋼(Hot Dip galvanized steel)上で行った。その後、清浄化した表面に、防錆油、Anticorit PL3802−39S(Fuchs)を適用して、3g/m2のコーティングを得た。これを、ラップせん断試験用の基体として使用した。接着剤組成物を、油が付着した表面に塗布し、そして第2の油が付着した鋼ピースを適用して、ラップせん断接合の他の側を形成した。
例7、8及び9について、全組成物に基づく重量%による組成を表6に示す。
Claims (26)
- 接着剤組成物であって、前記組成物の全重量に基づいて、
(a)40から60重量%の芳香族エポキシ樹脂;
(b)20から35重量%のエポキシ樹脂ゴム付加物;
(c)3から7重量%のアミン硬化剤;
(d)8から12重量%の油吸収剤;
(e)0.1から2重量%の防錆剤;及び
(f)2から6重量%のウロン系促進剤
を含む接着剤組成物。 - (a)がビスフェノールAエポキシ樹脂を含む、請求項1に記載の組成物。
- (b)がビスフェノールFエポキシ樹脂から形成される付加物を含む、請求項1又は2に記載の組成物。
- (b)がニトリルゴムを含む、請求項1から3のいずれか一項に記載の組成物。
- (d)が無機充填剤を含む、請求項1から4のいずれか一項に記載の組成物。
- (e)がCrを実質的に含まない、請求項1から5のいずれか一項に記載の組成物。
- (f)が4,4−メチレンジフェニレンビス(N,N−ジメチル尿素)を含む、請求項1から6のいずれか一項に記載の組成物。
- 前記組成物がフェノールノボラックエポキシ樹脂を更に含む、請求項1から7のいずれか一項に記載の組成物。
- 前記組成物がエチレン酢酸ビニルコポリマーを更に含む、請求項1から8のいずれか一項に記載の組成物。
- 前記組成物が、150℃にて150秒以下で硬化性を有する、請求項1から9のいずれか一項に記載の組成物。
- 前記組成物が、23℃にてISO527に準拠して6MPaより高いラップせん断強度を有する硬化生成物を形成する硬化性を有する、請求項1から10のいずれか一項に記載の組成物。
- 前記組成物が、40℃にて少なくとも110,000Pa.sの粘度を有し(粘度は規定の温度にてASTM D445に準拠して測定する)、40℃以下にてフィルム又は半固体の形態である、請求項1から11のいずれか一項に記載の組成物。
- 80℃における前記接着剤組成物の粘度が、100から1000Pa.sの範囲である(粘度は規定の温度にてASTM D445に準拠して測定する)、請求項1から12のいずれか一項に記載の組成物。
- 前記組成物を150℃に、210秒以下又は200秒以下の間、加熱する段階を含む、請求項1から13のいずれか一項に記載の接着剤組成物を硬化する方法。
- 前記生成物が、少なくとも95%の硬化度に硬化される、請求項14に記載の方法により得ることができる硬化生成物。
- 2つの表面を結合する方法であって、第1表面を、請求項1から13のいずれか一項に記載の組成物に接触させる段階、及び前記組成物を、第2表面に接触させて硬化させる段階、を含む方法。
- 前記硬化させる段階が、150℃に、210秒以下の間、加熱する段階を含む、請求項16に記載の方法。
- 前記第1表面及び第2表面の少なくとも1つが金属である、請求項16又は17に記載の方法。
- 前記表面が油で汚染されている、請求項16から18のいずれか一項に記載の方法。
- 請求項16から19のいずれか一項に記載の方法により得ることができる複合物品。
- 繊維強化材と、請求項1から13のいずれか一項に記載の組成物を含むプリプレグ。
- 複合材料を金属表面に結合するための、請求項1から13のいずれか一項に記載の接着剤組成物の使用。
- 前記複合材料が強化樹脂マトリクス(rrm)を含む、請求項22に記載の接着剤組成物の使用。
- 前記接着剤組成物と前記rrmを、同じ硬化段階で完全に硬化させる、請求項23に記載の接着剤組成物の使用。
- 請求項1に記載の接着剤組成物であって、前記接着剤組成物が、150℃にて180秒で硬化して、本明細書に記載した方法に従って油が付着した鋼上で20MPaより高いラップせん断強度を示すことができる、接着剤組成物。
- 前記組成物が、触媒能を有する一成分接着剤組成物である、請求項1から13のいずれか一項に記載の接着剤組成物。
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GB0817795D0 (en) | 2008-09-30 | 2008-11-05 | 3M Innovative Properties Co | Fast curing oil-uptaking epozxy-based structural adhesives |
JP6007914B2 (ja) * | 2010-11-08 | 2016-10-19 | 東レ株式会社 | 真空成形用プリプレグ、繊維強化複合材料およびその製造方法 |
US20120129980A1 (en) * | 2010-11-19 | 2012-05-24 | Ppg Industries Ohio, Inc. | Structural adhesive compositions |
US8895148B2 (en) * | 2011-11-09 | 2014-11-25 | Cytec Technology Corp. | Structural adhesive and bonding application thereof |
SI2850119T1 (sl) * | 2012-05-18 | 2018-10-30 | Hexcel Composites Limited | Hitro strdljive epoksi smole in iz njih pridobljeni prepregi |
GB2510835A (en) * | 2013-02-13 | 2014-08-20 | Hexcel Composites Ltd | Fire retardant epoxy resin formulations and their use |
WO2014172128A1 (en) * | 2013-04-19 | 2014-10-23 | Dow Global Technologies Llc | Adhesive compositions, manufacture and use thereof |
-
2014
- 2014-06-30 GB GBGB1411586.9A patent/GB201411586D0/en not_active Ceased
-
2015
- 2015-06-30 GB GB1511458.0A patent/GB2528779B/en not_active Expired - Fee Related
- 2015-06-30 CN CN201580034940.5A patent/CN106459378B/zh active Active
- 2015-06-30 JP JP2016575787A patent/JP6795403B2/ja active Active
- 2015-06-30 US US15/315,918 patent/US9932503B2/en active Active
- 2015-06-30 EP EP15734628.9A patent/EP3161035B1/en active Active
- 2015-06-30 KR KR1020167036997A patent/KR20170023028A/ko not_active Application Discontinuation
- 2015-06-30 WO PCT/EP2015/064881 patent/WO2016001245A1/en active Application Filing
- 2015-06-30 CA CA2953447A patent/CA2953447A1/en not_active Abandoned
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Publication number | Publication date |
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CN106459378A (zh) | 2017-02-22 |
GB201411586D0 (en) | 2014-08-13 |
KR20170023028A (ko) | 2017-03-02 |
EP3161035A1 (en) | 2017-05-03 |
GB201511458D0 (en) | 2015-08-12 |
JP2017527645A (ja) | 2017-09-21 |
GB2528779B (en) | 2017-10-04 |
CA2953447A1 (en) | 2016-01-07 |
EP3161035B1 (en) | 2020-08-12 |
CN106459378B (zh) | 2019-12-06 |
US9932503B2 (en) | 2018-04-03 |
WO2016001245A1 (en) | 2016-01-07 |
US20170107409A1 (en) | 2017-04-20 |
GB2528779A (en) | 2016-02-03 |
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