TW202206568A - Epoxy adhesive composition, epoxy adhesive, and method for preparing epoxy adhesive - Google Patents
Epoxy adhesive composition, epoxy adhesive, and method for preparing epoxy adhesive Download PDFInfo
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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
- 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
- C08G59/5006—Amines aliphatic
- C08G59/5013—Amines aliphatic containing more than seven carbon atoms, e.g. fatty amines
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- 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
- 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
- C08G59/22—Di-epoxy compounds
- C08G59/223—Di-epoxy compounds together with monoepoxy compounds
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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
- 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
- C08G59/22—Di-epoxy compounds
- C08G59/24—Di-epoxy compounds carbocyclic
- C08G59/245—Di-epoxy compounds carbocyclic aromatic
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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
- 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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- 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
- 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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- 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
- 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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- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Adhesives Or Adhesive Processes (AREA)
Abstract
Description
本發明係關於黏著劑之領域。具體而言，本發明係關於環氧黏著劑組成物、環氧黏著劑、及用於製備該環氧黏著劑之方法。 The present invention relates to the field of adhesives. Specifically, the present invention relates to epoxy adhesive compositions, epoxy adhesives, and methods for preparing the epoxy adhesives.
隨著電子產品的快速發展，其精確度、整合性、藝術性、以及效率增加。同時，塑膠廣泛用以置換傳統的玻璃基材及金屬基材，以實現輕量的電子產品。許多小型塑膠組件(諸如，用於印刷電路板的保護板、磁鐵、及電子貨架標籤(electronic shelf label))需要藉由合適的黏著劑黏附至電子產品的特定位置。此外，一些特殊應用(諸如，電子產品之封裝及填縫)亦需要使用合適的黏著劑。 With the rapid development of electronic products, its precision, integration, artistry, and efficiency have increased. At the same time, plastics are widely used to replace traditional glass substrates and metal substrates to realize lightweight electronic products. Many small plastic components, such as protective plates for printed circuit boards, magnets, and electronic shelf labels, need to be attached to specific locations on electronic products by means of suitable adhesives. In addition, some special applications (such as packaging and caulking of electronic products) also require the use of suitable adhesives.
因為電子組件通常需要耐溫，一般使用可在低溫下固化的單部分式黏著劑以達成電子產品之精密點膠。目前，合適的黏著劑主要包括基於環氧硫醇之環氧黏著劑。然而，此類環氧黏著劑一般具有不良的抗水汽滲透性，且經常無法滿足實際應用之要求。 Because electronic components usually require temperature resistance, one-part adhesives that can be cured at low temperatures are generally used to achieve precise dispensing of electronic products. At present, suitable adhesives mainly include epoxy thiol-based epoxy adhesives. However, such epoxy adhesives generally have poor water vapor permeation resistance and often fail to meet practical application requirements.
因此，為了解決前述技術問題，必須開發具有良好的抗水汽滲透性的新穎黏著劑。 Therefore, in order to solve the aforementioned technical problems, it is necessary to develop novel adhesives with good water vapor permeability resistance.
本發明之一個目的係提供一種環氧黏著劑組成物及一種自該環氧黏著劑組成物製備之環氧黏著劑。環氧黏著劑組成物具有良好的加工性及固化程序可操作性。此外，環氧黏著劑在塑膠表面(尤其是聚對苯二甲酸乙二酯(PET)表面)上具有良好的T-剝離強度及良好的抗水汽滲透性。 An object of the present invention is to provide an epoxy adhesive composition and an epoxy adhesive prepared from the epoxy adhesive composition. The epoxy adhesive composition has good processability and curing procedure operability. In addition, epoxy adhesives have good T-peel strength and good water vapor permeation resistance on plastic surfaces, especially polyethylene terephthalate (PET) surfaces.
本發明之另一個目的係提供一種用於製備環氧黏著劑之方法。 Another object of the present invention is to provide a method for preparing an epoxy adhesive.
為此，在一個態樣中，本發明提供一種環氧黏著劑組成物，其包含：a)10至50重量份之雙酚A環氧樹脂、雙酚F環氧樹脂、或雙酚A環氧樹脂與雙酚F環氧樹脂之組合，其中該雙酚A環氧樹脂與該雙酚F環氧樹脂具有150至250g/Eq之環氧當量；b)20至50重量份之具有100至150g/Eq之環氧當量之二羥基酚環氧丙基醚環氧樹脂；c)1至5重量份之矽烷偶合劑；d)20至60重量份之聚醚胺固化劑；e)10至40重量份之填料；及f)0至10重量份之咪唑促進劑。 To this end, in one aspect, the present invention provides an epoxy adhesive composition comprising: a) 10 to 50 parts by weight of bisphenol A epoxy resin, bisphenol F epoxy resin, or bisphenol A ring A combination of oxygen resin and bisphenol F epoxy resin, wherein the bisphenol A epoxy resin and the bisphenol F epoxy resin have an epoxy equivalent of 150 to 250 g/Eq; b) 20 to 50 parts by weight have an epoxy equivalent of 100 to 150g/Eq of epoxy equivalent of dihydroxyphenol glycidyl ether epoxy resin; c) 1 to 5 parts by weight of silane coupling agent; d) 20 to 60 parts by weight of polyetheramine curing agent; e) 10 to 50 parts by weight 40 parts by weight of filler; and f) 0 to 10 parts by weight of imidazole accelerator.
根據本發明之某些技術方案，該雙酚A環氧樹脂、該雙酚F環氧樹脂、或該雙酚A環氧樹脂與該雙酚F環氧樹脂之該組合之含量係10至50重量份，較佳的是15至40重量份。 According to some technical solutions of the present invention, the content of the bisphenol A epoxy resin, the bisphenol F epoxy resin, or the combination of the bisphenol A epoxy resin and the bisphenol F epoxy resin is 10 to 50 parts by weight, preferably 15 to 40 parts by weight.
根據本發明之某些技術方案，該二羥基酚環氧丙基醚環氧樹脂係選自下列之群組之一或多者：苯基二酚環氧丙基醚環氧樹脂及萘基二酚環氧丙基醚環氧樹脂。 According to certain technical solutions of the present invention, the dihydroxyphenol glycidyl ether epoxy resin is selected from one or more of the following groups: phenyl diphenol glycidyl ether epoxy resin and naphthyl diphenyl ether epoxy resin Phenol glycidyl ether epoxy resin.
根據本發明之某些技術方案，該二羥基酚環氧丙基醚環氧樹脂之含量係20至50重量份，較佳的是30至45重量份。 According to some technical solutions of the present invention, the content of the dihydroxyphenol glycidyl ether epoxy resin is 20 to 50 parts by weight, preferably 30 to 45 parts by weight.
根據本發明之某些技術方案，該矽烷偶合劑係選自下列之群組之一或多者：環氧基封端之矽烷偶合劑、胺基封端之矽烷偶合劑、及硫醇封端之矽烷偶合劑。 According to certain technical solutions of the present invention, the silane coupling agent is selected from one or more of the following group: epoxy-terminated silane coupling agent, amine-terminated silane coupling agent, and thiol-terminated silane coupling agent silane coupling agent.
根據本發明之某些技術方案，該矽烷偶合劑之含量係1至5重量份，較佳的是2至4重量份。 According to some technical solutions of the present invention, the content of the silane coupling agent is 1 to 5 parts by weight, preferably 2 to 4 parts by weight.
根據本發明之某些技術方案，該聚醚胺固化劑係選自下列之群組之一或多者：雙官能性聚丙二醇聚醚胺、三官能性聚丙二醇聚醚胺、及雙官能性聚丁二醇聚醚胺。 According to certain technical solutions of the present invention, the polyetheramine curing agent is selected from one or more of the following groups: bifunctional polypropylene glycol polyetheramine, trifunctional polypropylene glycol polyetheramine, and bifunctional Polybutylene glycol polyetheramine.
根據本發明之某些技術方案，該聚醚胺固化劑之含量係20至60重量份，較佳的是40至60重量份。 According to some technical solutions of the present invention, the content of the polyetheramine curing agent is 20 to 60 parts by weight, preferably 40 to 60 parts by weight.
根據本發明之某些技術方案，該填料係選自下列之群組之一或多者：滑石粉末、聚烯烴粉末、矽灰石、石英粉末、及雲母粉末。 According to certain technical solutions of the present invention, the filler is selected from one or more of the following groups: talc powder, polyolefin powder, wollastonite, quartz powder, and mica powder.
根據本發明之某些技術方案，該填料之含量係10至40重量份，較佳的是15至30重量份。 According to some technical solutions of the present invention, the content of the filler is 10 to 40 parts by weight, preferably 15 to 30 parts by weight.
根據本發明之某些技術方案，該環氧黏著劑組成物在25℃下具有小於或等於2000mPa．s之黏度，且在25℃下具有大於或等於6小時之工作窗。 According to some technical solutions of the present invention, the epoxy adhesive composition has less than or equal to 2000mPa at 25°C. s viscosity, and has a working window of greater than or equal to 6 hours at 25°C.
根據本發明之某些技術方案，該咪唑促進劑係選自下列之群組之一或多者：N-甲基咪唑、1,2-二甲基咪唑、及2-乙基-4-甲基咪唑。 According to certain technical solutions of the present invention, the imidazole accelerator is selected from one or more of the following groups: N-methylimidazole, 1,2-dimethylimidazole, and 2-ethyl-4-methylimidazole imidazole.
根據本發明之某些技術方案，該咪唑促進劑之含量係2至5重量份。 According to some technical solutions of the present invention, the content of the imidazole accelerator is 2 to 5 parts by weight.
根據本發明之某些技術方案，該環氧黏著劑組成物具有小於或等於30分鐘之固化時間。 According to certain technical solutions of the present invention, the epoxy adhesive composition has a curing time of less than or equal to 30 minutes.
在另一個態樣中，本發明提供一種環氧黏著劑，其包含：根據本發明所提供之環氧黏著劑組成物之固化產物。 In another aspect, the present invention provides an epoxy adhesive comprising: a cured product of the epoxy adhesive composition provided by the present invention.
根據本發明之某些技術方案，該環氧黏著劑在聚對苯二甲酸乙二酯(PET)表面上具有大於或等於1.0N/mm的T-剝離強度，且在60℃下具有小於或等於6.0g mm/m2 24hr之水汽滲透率。 According to certain technical solutions of the present invention, the epoxy adhesive has a T-peel strength greater than or equal to 1.0 N/mm on a polyethylene terephthalate (PET) surface, and has a T-peel strength of less than or equal to 1.0 N/mm at 60° C. Equivalent to a water vapor permeability of 6.0 g mm/m 2 24hr.
在又另一個態樣中，本發明提供一種用於製備環氧黏著劑之方法，其包含下列步驟：將根據本發明所提供之環氧黏著劑組成物固化，以獲得該環氧黏著劑。 In yet another aspect, the present invention provides a method for preparing an epoxy adhesive, comprising the steps of: curing the epoxy adhesive composition provided by the present invention to obtain the epoxy adhesive.
根據本發明之一個實施例，本發明所提供之環氧黏著劑組成物具有良好的加工性及固化程序可操作性；且自該環氧黏著劑組成物製備之環氧黏著劑在塑膠表面上(尤其是在PET表面上)具有良好的剝離強度及良好的水汽滲透率。 According to an embodiment of the present invention, the epoxy adhesive composition provided by the present invention has good processability and curing procedure operability; and the epoxy adhesive prepared from the epoxy adhesive composition is on the plastic surface (especially on PET surface) has good peel strength and good water vapor permeability.
在下文中，將通過與本發明之實施方式之組合，更詳細地敘述本發明。 Hereinafter, the present invention will be described in more detail in combination with the embodiments of the present invention.
在下文中，為了更清楚地敘述本發明，敘述了本發明之數種技術方案及數種用於比較之技術方案。然而，此部分僅例示一些請求保護的特定實施例，其中一或多種技術方案中所述之技術特徵可與任何一或多種技術方案組合，且只要不悖離本發明之精神，此等藉由組合而獲得之技術方案，亦落入本申請之保護範疇。 In the following, in order to describe the present invention more clearly, several technical solutions of the present invention and several technical solutions for comparison are described. However, this section only exemplifies some specific embodiments claimed, in which the technical features described in one or more technical solutions can be combined with any one or more technical solutions, and as long as it does not depart from the spirit of the present invention, these are achieved by The technical solutions obtained by combination also fall into the protection scope of the present application.
環氧黏著劑組成物 Epoxy Adhesive Composition
本發明提供之環氧黏著劑組成物包含：a)10至50重量份之雙酚A環氧樹脂、雙酚F環氧樹脂、或雙酚A環氧樹脂與雙酚F環氧樹脂之組合，其中其環氧當量係150至250g/Eq；b)20至50重量份之具有100至150g/Eq之環氧當量之二羥基酚環氧丙基醚環氧樹脂；c)1至5重量份之矽烷偶合劑；d)20至60重量份之聚醚胺固化劑；e)10至40重量份之填料；及f)0至10重量份之咪唑促進劑。 The epoxy adhesive composition provided by the present invention comprises: a) 10 to 50 parts by weight of bisphenol A epoxy resin, bisphenol F epoxy resin, or a combination of bisphenol A epoxy resin and bisphenol F epoxy resin , wherein its epoxy equivalent is 150 to 250 g/Eq; b) 20 to 50 parts by weight of a dihydroxyphenol glycidyl ether epoxy resin with an epoxy equivalent of 100 to 150 g/Eq; c) 1 to 5 parts by weight parts of a silane coupling agent; d) 20 to 60 parts by weight of a polyetheramine curing agent; e) 10 to 40 parts by weight of a filler; and f) 0 to 10 parts by weight of an imidazole accelerator.
在本發明中，該雙酚A環氧樹脂及該雙酚F環氧樹脂具有150至250g/Eq之環氧當量；雙酚A環氧樹脂及雙酚F環氧樹脂可調節環氧黏著劑之水汽滲透率。 In the present invention, the bisphenol A epoxy resin and the bisphenol F epoxy resin have an epoxy equivalent of 150 to 250 g/Eq; the bisphenol A epoxy resin and the bisphenol F epoxy resin can adjust the epoxy adhesive the water vapor permeability.
根據本發明之一個實施例，該雙酚A環氧樹脂、該雙酚F環氧樹脂、或該雙酚A環氧樹脂與該雙酚F環氧樹脂之該組合之含量係10至50重量份，較佳的是15至40重量份。 According to an embodiment of the present invention, the content of the bisphenol A epoxy resin, the bisphenol F epoxy resin, or the combination of the bisphenol A epoxy resin and the bisphenol F epoxy resin is 10 to 50 wt. parts, preferably 15 to 40 parts by weight.
根據本發明之一個實施例，該雙酚A環氧樹脂可選自於可購自Hexion Specialty Chemicals Co.,Ltd.(Columbus,USA)之EPON 826。 According to one embodiment of the present invention, the bisphenol A epoxy resin may be selected from EPON 826, which is available from Hexion Specialty Chemicals Co., Ltd. (Columbus, USA).
根據本發明之一個實施例，該雙酚F環氧樹脂可選自於可購自Huntsman Co.,Ltd.(Houston,USA)之Araldite GY 285。 According to one embodiment of the present invention, the bisphenol F epoxy resin may be selected from Araldite GY 285 available from Huntsman Co., Ltd. (Houston, USA).
在本發明中，該二羥基酚環氧丙基醚環氧樹脂不僅可調節環氧黏著劑之黏度，亦可調節其在塑膠表面(尤其是PET表面)上之剝離強度。 In the present invention, the dihydroxyphenol glycidyl ether epoxy resin can not only adjust the viscosity of the epoxy adhesive, but also adjust its peel strength on the plastic surface (especially the PET surface).
根據本發明之一個實施例，該二羥基酚環氧丙基醚環氧樹脂係選自下列之群組之一或多者：苯基二酚環氧丙基醚環氧樹脂及萘基二酚環氧丙基醚環氧樹脂。 According to an embodiment of the present invention, the dihydroxyphenol glycidyl ether epoxy resin is one or more selected from the group consisting of: phenyl diphenol glycidyl ether epoxy resin and naphthyl diphenol Glycidoxypropyl ether epoxy resin.
根據本發明之一個實施例，該二羥基酚環氧丙基醚環氧樹脂之含量係20至50重量份，較佳的是30至45重量份。 According to an embodiment of the present invention, the content of the dihydroxyphenol glycidyl ether epoxy resin is 20 to 50 parts by weight, preferably 30 to 45 parts by weight.
根據本發明之一個實施例，該苯基二酚環氧丙基醚環氧樹脂可選自於可購自Nagase America Corporation(New York City,USA)之Denacol EX-201 IM；且該萘基二酚環氧丙基醚環氧樹脂可選自於可購自DIC Co.,Ltd.(Tokyo,Japan)之HP4032D。 According to one embodiment of the present invention, the phenyldiphenol glycidyl ether epoxy resin may be selected from Denacol EX-201 IM available from Nagase America Corporation (New York City, USA); and the naphthyl diphenolate The phenolic glycidyl ether epoxy resin can be selected from HP4032D available from DIC Co., Ltd. (Tokyo, Japan).
在本發明中，該矽烷偶合劑可調節環氧黏著劑在塑膠表面(尤其是PET表面)上之剝離強度。 In the present invention, the silane coupling agent can adjust the peel strength of the epoxy adhesive on the plastic surface (especially the PET surface).
根據本發明之一個實施例，該矽烷偶合劑係選自下列之群組之一或多者：環氧基封端之矽烷偶合劑、胺基封端之矽烷偶合劑、及硫醇封端之矽烷偶合劑。 According to one embodiment of the present invention, the silane coupling agent is selected from one or more of the following group: epoxy terminated silane coupling agent, amine terminated silane coupling agent, and thiol terminated silane coupling agent Silane coupling agent.
根據本發明之一個實施例，該矽烷偶合劑之含量係1至5重量份，較佳的是2至4重量份。 According to an embodiment of the present invention, the content of the silane coupling agent is 1 to 5 parts by weight, preferably 2 to 4 parts by weight.
根據本發明之一個實施例，該矽烷偶合劑可選自於可購自Dowcorning Co.,Ltd.(Midland,USA)之Z6040。 According to one embodiment of the present invention, the silane coupling agent may be selected from Z6040 which is available from Dowcorning Co., Ltd. (Midland, USA).
在本發明中，該聚醚胺固化劑不僅可促進環氧黏著劑組成物之固化，亦可調節環氧黏著劑之黏度及在塑膠表面(尤其是聚對苯二甲酸乙二酯(PET)表面)上之剝離強度。 In the present invention, the polyetheramine curing agent can not only promote the curing of the epoxy adhesive composition, but also adjust the viscosity of the epoxy adhesive and adjust the viscosity of the epoxy adhesive on the surface of plastics (especially polyethylene terephthalate (PET). surface) peel strength.
根據本發明之一個實施例，該聚醚胺固化劑係選自下列之群組之一或多者：雙官能性聚丙二醇聚醚胺、三官能性聚丙二醇聚醚胺、及雙官能性聚丁二醇聚醚胺。 According to an embodiment of the present invention, the polyetheramine curing agent is selected from one or more of the following groups: bifunctional polypropylene glycol polyetheramine, trifunctional polypropylene glycol polyetheramine, and bifunctional polyetheramine Butylene glycol polyetheramine.
根據本發明之一個實施例，該聚醚胺固化劑之含量係20至60重量份，較佳的是30至50重量份。 According to an embodiment of the present invention, the content of the polyetheramine curing agent is 20 to 60 parts by weight, preferably 30 to 50 parts by weight.
根據本發明之一個實施例，該雙官能性聚丙二醇聚醚胺固化劑可選自於可購自Huntsman Co.,Ltd.(Houston,USA)之D230及D400；且該三官能性聚丙二醇聚醚胺固化劑可選自於可購自Huntsman Co.,Ltd.(Houston,USA)之T403。 According to an embodiment of the present invention, the bifunctional polypropylene glycol polyetheramine curing agent can be selected from D230 and D400 which can be purchased from Huntsman Co., Ltd. (Houston, USA); and the trifunctional polypropylene glycol polymer The etheramine curing agent can be selected from T403 available from Huntsman Co., Ltd. (Houston, USA).
在本發明中，該填料可調節環氧黏著劑之水汽滲透率。根據本發明之一個實施例，該填料係選自下列之群組之一或多者：滑石粉末、聚烯烴粉末、矽灰石、石英粉末、及雲母粉末。 In the present invention, the filler can adjust the water vapor permeability of the epoxy adhesive. According to one embodiment of the present invention, the filler is one or more selected from the group consisting of talc powder, polyolefin powder, wollastonite, quartz powder, and mica powder.
根據本發明之一個實施例，該填料之含量係10至40重量份，較佳的是15至30重量份。 According to an embodiment of the present invention, the content of the filler is 10 to 40 parts by weight, preferably 15 to 30 parts by weight.
根據本發明之一個實施例，該滑石粉末可選自於可購自Quartz Industry Materials(Shanghai)Co.,Ltd.(Shanghai,China)之AH51210；且該聚烯烴粉末可選自於可購自Lyondell Bassell Chemical Company(Houston,USA)之MICROTHENE F FA 700-00。 According to one embodiment of the present invention, the talc powder can be selected from AH51210 available from Quartz Industry Materials (Shanghai) Co., Ltd. (Shanghai, China); and the polyolefin powder can be selected from available from Lyondell MICROTHENE F FA 700-00 from Bassell Chemical Company (Houston, USA).
在本發明中，將咪唑促進劑可選地添加至環氧黏著劑組成物以縮短其固化時間，從而改善固化程序可操作性。 In the present invention, an imidazole accelerator is optionally added to the epoxy adhesive composition to shorten its curing time, thereby improving curing procedure operability.
根據本發明之一個實施例，該咪唑促進劑係選自下列之群組之一或多者：N-甲基咪唑、1,2-二甲基咪唑、及2-乙基-4-甲基咪唑。 According to an embodiment of the present invention, the imidazole accelerator is selected from one or more of the following group: N-methylimidazole, 1,2-dimethylimidazole, and 2-ethyl-4-methyl imidazole.
根據本發明之一個實施例，該咪唑促進劑之含量係0至10重量份，較佳的是2至5重量份。 According to an embodiment of the present invention, the content of the imidazole accelerator is 0 to 10 parts by weight, preferably 2 to 5 parts by weight.
根據本發明之一個實施例，N-甲基咪唑及2-乙基-4-甲基咪唑可商購自Shikoku Chemicals Corporation(Chiba City,Japan)；且1,2-二甲基咪唑可商購自Ningxia Joie Material Co.,Ltd.(Ningxia,China)。根據本發明之一個實施例，該環氧黏著劑組成物在25℃下具有小於或等於2000mPa．s之黏度，且在25℃下具有大於或等於6小時之工作窗。 According to one embodiment of the present invention, N-methylimidazole and 2-ethyl-4-methylimidazole are commercially available from Shikoku Chemicals Corporation (Chiba City, Japan); and 1,2-dimethylimidazole is commercially available From Ningxia Joie Material Co., Ltd. (Ningxia, China). According to an embodiment of the present invention, the epoxy adhesive composition at 25 ° C has less than or equal to 2000mPa. s viscosity, and has a working window of greater than or equal to 6 hours at 25°C.
根據本發明之一個實施例，該環氧黏著劑組成物可在小於或等於-20℃之條件下儲存。 According to an embodiment of the present invention, the epoxy adhesive composition can be stored at a temperature of less than or equal to -20°C.
環氧黏著劑 epoxy adhesive
本發明所提供之環氧黏著劑包含：根據本發明所提供之環氧黏著劑組成物之固化產物。關於環氧黏著劑組成物中所包括之各組分的細節，參見本說明書之「環氧黏著劑組成物(epoxy adhesive composition)」一節，其將不會在本文中再次敘述。 The epoxy adhesive provided by the present invention includes: a cured product of the epoxy adhesive composition provided by the present invention. For details of each component included in the epoxy adhesive composition, see the section "epoxy adhesive composition" of this specification, which will not be described again herein.
根據本發明之一個實施例，該環氧黏著劑在聚對苯二甲酸乙二酯(PET)表面上具有大於或等於1.0N/mm的T-剝離強度，且在60℃下具有小於或等於6.0g mm/m2 24hr之水汽滲透率。 According to an embodiment of the present invention, the epoxy adhesive has a T-peel strength greater than or equal to 1.0 N/mm on a polyethylene terephthalate (PET) surface, and has a T-peel strength of less than or equal to 60° C. Water vapor permeability of 6.0g mm/m 2 24hr.
用於製備環氧黏著劑之方法 Method for preparing epoxy adhesive
本發明所提供之用於製備環氧黏著劑之方法包含下列步驟：將根據本發明所提供之環氧黏著劑組成物固化，以獲得環氧黏著劑。關於環氧黏著劑組成物中所包括之各組分的細節，參見本說明書之「環氧黏著劑組成物(epoxy adhesive composition)」一節，其將不會在本文中再次敘述。 The method for preparing an epoxy adhesive provided by the present invention includes the following steps: curing the epoxy adhesive composition provided by the present invention to obtain an epoxy adhesive. For details of each component included in the epoxy adhesive composition, see the section "epoxy adhesive composition" of this specification, which will not be described again herein.
特別地，根據本發明之一個實施例，該製備方法可包含下列步驟： In particular, according to an embodiment of the present invention, the preparation method may comprise the following steps:
步驟1，將本發明所提供之環氧黏著劑組成物之雙酚A環氧樹脂及/或雙酚F環氧樹脂、二羥基酚環氧丙基醚環氧樹脂、及矽烷偶合劑在室溫(25℃)之條件下混合，以獲得第一混合物； Step 1, the epoxy adhesive composition provided by the present invention is bisphenol A epoxy resin and/or bisphenol F epoxy resin, dihydroxyphenol glycidyl ether epoxy resin, and silane coupling agent in the room Mixing under warm (25°C) conditions to obtain a first mixture;
步驟2，將本發明所提供之環氧黏著劑組成物之填料添加至該第一混合物，以獲得第二混合物；及 Step 2, adding the filler of the epoxy adhesive composition provided by the present invention to the first mixture to obtain a second mixture; and
步驟3：將本發明所提供之環氧黏著劑組成物之聚醚胺固化劑與咪唑促進劑添加至該第二混合物，隨後固化以獲得該環氧黏著劑。 Step 3: adding the polyetheramine curing agent and imidazole accelerator of the epoxy adhesive composition provided by the present invention to the second mixture, followed by curing to obtain the epoxy adhesive.
根據本發明之一個實施例，在步驟2中，本發明所提供之環氧黏著劑組成物之填料可在高速分散混合之後添加至該第一混合物，其經受至少三次之三輥碾磨以獲得該第二混合物。 According to an embodiment of the present invention, in step 2, the filler of the epoxy adhesive composition provided by the present invention can be added to the first mixture after high-speed dispersing and mixing, which is subjected to at least three times of three-roll milling to obtain the second mixture.
根據本發明之一個實施例，在步驟3中，在添加本發明所提供之環氧黏著劑組成物之聚醚胺固化劑及咪唑促進劑至該第二混合物之前，可將該第二混合物冷卻至10℃或更低。 According to an embodiment of the present invention, in step 3, before adding the polyetheramine curing agent and imidazole accelerator of the epoxy adhesive composition provided by the present invention to the second mixture, the second mixture can be cooled to 10°C or lower.
根據本發明之一個實施例，在步驟3中，在添加本發明所提供之環氧黏著劑組成物之聚醚胺固化劑及咪唑促進劑至該第二混合物之後，可在低溫(<10℃)下充分混合混合物，且該混合物接著經受足夠的真空消泡以獲得該環氧黏著劑。 According to an embodiment of the present invention, in step 3, after adding the polyetheramine curing agent and imidazole accelerator of the epoxy adhesive composition provided by the present invention to the second mixture, it can be heated at a low temperature (<10° C. ) and the mixture is then subjected to sufficient vacuum defoaming to obtain the epoxy adhesive.
實例example
在下文中，將提供較佳實例以更佳地理解本發明。然而，下列實例僅用於說明性目的，且使所屬技術領域中具有通常知識者更佳地理解本發明，且本發明不應受限於此等實例。 Hereinafter, preferred examples will be provided for better understanding of the present invention. However, the following examples are only for illustrative purposes and to enable those having ordinary skill in the art to better understand the present invention, and the present invention should not be limited by these examples.
1.原料 1. Raw materials
(1)雙酚A環氧樹脂 (1) Bisphenol A epoxy resin
EPON 826，其係具有178至186g/Eq之環氧當量之雙酚A環氧樹脂，可商購自Hexion Specialty Chemicals Co.,Ltd.(Columbus,USA)。 EPON 826, which is a bisphenol A epoxy resin having an epoxy equivalent weight of 178 to 186 g/Eq, is commercially available from Hexion Specialty Chemicals Co., Ltd. (Columbus, USA).
(2)雙酚F環氧樹脂 (2) Bisphenol F epoxy resin
Araldite GY 285，其係具有164至173g/Eq之環氧當量之雙酚F環氧樹脂，可商購自Huntsman Co.,Ltd.(Houston,USA)。 Araldite GY 285, which is a bisphenol F epoxy resin having an epoxy equivalent weight of 164 to 173 g/Eq, is commercially available from Huntsman Co., Ltd. (Houston, USA).
(3)二羥基酚環氧丙基醚環氧樹脂 (3) Dihydroxyphenol glycidyl ether epoxy resin
Denacol EX-201 IM，其係具有120至135g/Eq之環氧當量之苯基二酚環氧丙基醚環氧樹脂，可商購自Nagase America Corporation(New York City,USA)。 Denacol EX-201 IM, which is a phenyldiphenol glycidyl ether epoxy resin having an epoxy equivalent weight of 120 to 135 g/Eq, is commercially available from Nagase America Corporation (New York City, USA).
HP4032D，其係具有140g/Eq之環氧當量之萘基二酚環氧丙基醚環氧樹脂，可商購自DIC Co.,Ltd.(Tokyo,Japan)。 HP4032D, which is a naphthyl diphenol glycidyl ether epoxy resin having an epoxy equivalent weight of 140 g/Eq, is commercially available from DIC Co., Ltd. (Tokyo, Japan).
(4)其他環氧樹脂 (4) Other epoxy resins
AFG-90，其係具有105至115g/Eq之環氧當量之胺基酚三官能性環氧樹脂，可商購自ShangHai HuaYi Resins Co.,Ltd.(Shanghai,China)。 AFG-90, which is an aminophenol trifunctional epoxy resin having an epoxy equivalent weight of 105 to 115 g/Eq, is commercially available from ShangHai HuaYi Resins Co., Ltd. (Shanghai, China).
DY-D，其係具有118至125g/Eq之環氧當量之丁二醇二環氧丙基醚環氧樹脂，可商購自Huntsman Co.,Ltd.(Houston,USA)。 DY-D, which is a butanediol diglycidyl ether epoxy resin having an epoxy equivalent weight of 118 to 125 g/Eq, is commercially available from Huntsman Co., Ltd. (Houston, USA).
(5)矽烷偶合劑 (5) Silane coupling agent
Z6040，其係環氧基封端之矽烷偶合劑，可商購自Dowcorning Co.,Ltd.(Midland,USA)。 Z6040, which is an epoxy-terminated silane coupling agent, is commercially available from Dowcorning Co., Ltd. (Midland, USA).
(6)聚醚胺固化劑 (6) Polyetheramine curing agent
D230，其係具有60g/Eq之活性氫當量之雙官能性聚丙二醇聚醚胺固化劑，可商購自Huntsman Co.,Ltd.(Houston,USA)。 D230, which is a bifunctional polypropylene glycol polyetheramine curing agent with an active hydrogen equivalent of 60 g/Eq, is commercially available from Huntsman Co., Ltd. (Houston, USA).
D400，其係具有115g/Eq之活性氫當量之雙官能性聚丙二醇聚醚胺固化劑，可商購自Huntsman Co.,Ltd.(Houston,USA)。 D400, which is a bifunctional polypropylene glycol polyetheramine curing agent having an active hydrogen equivalent weight of 115 g/Eq, is commercially available from Huntsman Co., Ltd. (Houston, USA).
T403，其係具有80g/Eq之活性氫當量之三官能性聚丙二醇聚醚胺固化劑，可商購自Huntsman Co.,Ltd.(Houston,USA)。 T403, which is a trifunctional polypropylene glycol polyetheramine curing agent with an active hydrogen equivalent of 80 g/Eq, is commercially available from Huntsman Co., Ltd. (Houston, USA).
(7)填料 (7) Packing
AH51105，其係滑石粉末，可商購自Quartz Industry Materials(Shanghai)Co.,Ltd.(Shanghai,China)； AH51105, which is a talc powder, commercially available from Quartz Industry Materials (Shanghai) Co., Ltd. (Shanghai, China);
WSE600，其係矽灰石，可商購自Quartz Industry Materials(Shanghai)Co.,Ltd.(Shanghai,China)； WSE600, which is a wollastonite, commercially available from Quartz Industry Materials (Shanghai) Co., Ltd. (Shanghai, China);
MICROTHENE F FA 700-00，其係聚烯烴粉末，可商購自Lyondell Bassell Chemical Company(Houston,USA)。 MICROTHENE F FA 700-00, which is a polyolefin powder, is commercially available from Lyondell Bassell Chemical Company (Houston, USA).
(8)基材 (8) Substrate
PET基材，可商購自REIKO Company(Tokyo,Japan)。 PET substrate, commercially available from REIKO Company (Tokyo, Japan).
(9)咪唑促進劑 (9) Imidazole accelerator
N-甲基咪唑，可商購自Shikoku Chemicals Corporation(Chiba City,Japan)； N-methylimidazole, commercially available from Shikoku Chemicals Corporation (Chiba City, Japan);
1,2-二甲基咪唑，可商購自Ningxia Joie Material Co.,Ltd.(Ningxia,China)； 1,2-Dimethylimidazole, commercially available from Ningxia Joie Material Co., Ltd. (Ningxia, China);
2-乙基-4-甲基咪唑，可商購自Shikoku Chemicals Corporation(Chiba City,Japan)。 2-ethyl-4-methylimidazole, commercially available from Shikoku Chemicals Corporation (Chiba City, Japan).
2.測試方法 2. Test method
(1)加工性測試 (1) Processability test
此測試使用黏度計(型號DV2TLV，可商購自Brookfield Company,Middleboro,USA)以測試本發明之實例及比較例中所提供之黏著劑組成物之黏度。特定測試步驟如下： This test uses a viscometer (model DV2TLV, commercially available from Brookfield Company, Middleboro, USA) to test the viscosity of the adhesive compositions provided in the inventive examples and comparative examples. The specific test steps are as follows:
步驟1：從冷凍庫移除黏著劑組成物，且記錄移除時之時間為T0，且接著該黏著劑組成物係經自然回溫至25℃且係呈液態。 Step 1: Remove the adhesive composition from the freezer, and record the time of removal as T 0 , and then the adhesive composition is naturally warmed to 25° C. and is in a liquid state.
步驟2：將回溫之黏著劑組成物裝入材料杯，且將該黏度計歸零及校準。 Step 2: Load the rewarmed adhesive composition into the material cup, and zero and calibrate the viscometer.
步驟3：選擇合適的轉子，其對應的黏度值係以黏度計測試並記錄，且確保力矩在10%至90%的範圍內。 Step 3: Select a suitable rotor, and its corresponding viscosity value is tested and recorded with a viscometer, and ensure that the torque is within the range of 10% to 90%.
步驟4：在一定的時間間隔之後，測試黏著劑組成物的黏度值，且將黏著劑組成物的黏度達到10000mPa．s時的時間記錄為T1。假設黏著劑組成物之工作窗係T，則T=T1-T0。 Step 4: After a certain time interval, test the viscosity value of the adhesive composition, and make the viscosity of the adhesive composition reach 10000mPa. The time at s is recorded as T 1 . Assuming that the working window of the adhesive composition is T, then T=T 1 -T 0 .
當環氧黏著劑組成物之所測量之黏度小於或等於2000mPa．s，且環氧黏著劑組成物在25℃下之工作窗T係大於或等於6小時，表示該環氧黏著劑組成物具有良好的加工性。當環氧黏著劑組成物之所測量之黏度小於或等於1000mPa．s，且環氧黏著劑組成物在25℃下之工作窗T係大於或等於8小時，表示該環氧黏著劑組成物具有優異的加工性。 When the measured viscosity of the epoxy adhesive composition is less than or equal to 2000mPa. s, and the working window T of the epoxy adhesive composition at 25°C is greater than or equal to 6 hours, indicating that the epoxy adhesive composition has good processability. When the measured viscosity of the epoxy adhesive composition is less than or equal to 1000mPa. s, and the working window T of the epoxy adhesive composition at 25°C is greater than or equal to 8 hours, indicating that the epoxy adhesive composition has excellent processability.
(2)T-剝離強度測試 (2) T-peel strength test
此測試係根據測試標準ASTM D1876，且在聚對苯二甲酸乙二酯(PET)基材表面上以100mm/分鐘之拉伸速率進行，以測量本發明之實例及比較例中所提供之黏著劑在PET表面上的T-剝離強度。 This test was performed according to the test standard ASTM D1876 and was performed on the surface of a polyethylene terephthalate (PET) substrate at a tensile rate of 100 mm/min to measure the adhesion provided in the inventive examples and comparative examples T-peel strength of the agent on the PET surface.
當所測量之T-剝離強度大於或等於1.0N/mm時，表示該黏著劑具有良好的T-剝離強度；且當所測量之T-剝離強度大於或等於1.5N/mm時，表示該黏著劑具有優異的T-剝離強度。 When the measured T-peel strength is greater than or equal to 1.0N/mm, it means that the adhesive has a good T-peel strength; and when the measured T-peel strength is greater than or equal to 1.5N/mm, it means the adhesive The agent has excellent T-peel strength.
(3)抗水汽滲透性之測試 (3) Test of water vapor permeability resistance
此測試係根據ASTM F-1249測量本發明之實例及比較例中所提供之黏著劑(1mm厚)在60℃下之水汽滲透率，測試條件為「60℃、100%濕度」，且測試結果之單位為g．mm/m2．24hr。 This test is based on ASTM F-1249 to measure the water vapor permeability of the adhesives (1mm thick) provided in the examples of the present invention and the comparative examples at 60°C. The test conditions are "60°C, 100% humidity", and the test results The unit is g. mm/m 2 ． 24hr.
當所測量之水汽滲透率小於或等於6.0g．mm/m2．24hr時，表示黏著劑具有良好的抗水汽滲透性；且當所測量之水汽滲透率小於或等於5.5g．mm/m2．24hr時，表示黏著劑具有優異的抗水汽滲透性。 When the measured water vapor permeability is less than or equal to 6.0g. mm/m 2 ． 24hr, it means that the adhesive has good water vapor permeability resistance; and when the measured water vapor permeability is less than or equal to 5.5g. mm/m 2 ． At 24hr, it indicates that the adhesive has excellent resistance to water vapor permeation.
(4)固化速度測試 (4) Curing speed test
此測試使用流變儀(型號ARES G2，可商購自TA Instruments,USA)以測試本發明之實例及比較例中所提供之黏著劑組成物之固化速度。測試步驟如下： This test uses a rheometer (model ARES G2, commercially available from TA Instruments, USA) to test the cure speed of the adhesive compositions provided in the inventive examples and comparative examples. The test steps are as follows:
步驟1：從冷凍庫移除黏著劑組成物，且接著該黏著劑組成物係經自然回溫至25℃且係呈液態。 Step 1: The adhesive composition is removed from the freezer, and then the adhesive composition is naturally warmed to 25°C and is in a liquid state.
步驟2：選擇25mm測試鋁盤且將其安裝在流變儀上，隨後歸零，且將操作程式設定為70℃之測試溫度、5.0 1/s之剪切速率、及5400s之總測試持續時間。 Step 2: A 25mm test aluminum pan was selected and mounted on the rheometer, then zeroed, and the operating program was set to a test temperature of 70°C, a shear rate of 5.0 1/s, and a total test duration of 5400s .
步驟3：將回溫至25℃之黏著劑組成物作為測試樣本，且放置在測試鋁盤上。將鋁盤之高度下降至0.5mm(亦即，測試樣本之厚度為0.5mm)。關閉保溫爐，隨後測量樣本之固化時間(在70℃下)。測試樣本之儲存模數曲線及損耗模數曲線相交之位置所對應的時間係固化時間。 Step 3: The adhesive composition heated to 25° C. is used as a test sample, and placed on a test aluminum pan. The height of the aluminum pan was lowered to 0.5 mm (ie, the thickness of the test sample was 0.5 mm). The holding oven was turned off and the curing time (at 70°C) of the samples was then measured. The time corresponding to the intersection of the storage modulus curve and the loss modulus curve of the test sample is the curing time.
當所測得之固化時間小於或等於30分鐘時，表示測試樣本具有良好的固化程序可操作性。 When the measured curing time is less than or equal to 30 minutes, it means that the test sample has good operability of the curing procedure.
實例E1 instance E1
將21g EPON 826、9g Araldite GY 285、30g Denacol EX-201 IM、15g HP4032D、及2g Z6040添加至250ml反應容器。接著，在25℃的條件下，將上述以每分鐘1000轉之旋轉速度攪拌，直到獲得均質的第一混合物。 21 g EPON 826, 9 g Araldite GY 285, 30 g Denacol EX-201 IM, 15 g HP4032D, and 2 g Z6040 were added to a 250 ml reaction vessel. Next, the above was stirred at a rotational speed of 1000 revolutions per minute at 25° C. until a homogeneous first mixture was obtained.
將20g之填料(WSE600)添加至第一溶液。接著，將上述機械攪拌，直到充分分散，且產生第二混合物。 20 g of filler (WSE600) was added to the first solution. Next, the above is mechanically stirred until well dispersed and a second mixture is produced.
用可商購自EXAKT Advanced Technology Company,Norderstedt,Germany的型號50之三輥碾磨機將第二混合物碾磨三次，以確保該第二混合物之平均粒徑係控制在50微米或更小。 The second mixture was milled three times with a three roll mill, model 50, commercially available from EXAKT Advanced Technology Company, Norderstedt, Germany, to ensure that the average particle size of the second mixture was controlled at 50 microns or less.
將第二混合物冷卻至10℃或更低，且將20g D230及40g D400添加至其中。接著，在真空之條件下，將上述以每分鐘1000轉之旋轉速度攪拌，直到獲得均勻的環氧黏著劑組成物。較佳地，環氧黏著劑組成物可在小於或等於-20℃下經密封並儲存。 The second mixture was cooled to 10°C or lower, and 20 g of D230 and 40 g of D400 were added to it. Next, under the condition of vacuum, the above is stirred at a rotation speed of 1000 revolutions per minute until a uniform epoxy adhesive composition is obtained. Preferably, the epoxy adhesive composition can be sealed and stored at less than or equal to -20°C.
將環氧黏著劑組成物加熱至70℃，固化1小時，且在室溫(25℃)下放置3天以完全固化，從而獲得環氧黏著劑。 The epoxy adhesive composition was heated to 70° C., cured for 1 hour, and left at room temperature (25° C.) for 3 days to be completely cured, thereby obtaining an epoxy adhesive.
根據本文中所述之測試方法使環氧黏著劑組成物經受加工性測試，且使環氧黏著劑經受T-剝離強度測試及抗水汽滲透性之測試。測試結果係列在表1中。 The epoxy adhesive compositions were subjected to the processability test according to the test methods described herein, and the epoxy adhesives were subjected to the T-peel strength test and the water vapor permeation resistance test. The test results series are in Table 1.
實例E2至E7 Instances E2 to E7
實例E2至E7之環氧黏著劑係以與實例E1之相同方式製備，除了用以製備環氧黏著劑之環氧黏著劑組成物之組分及量不同。其組分及量係具體列在表1中。 The epoxy adhesives of Examples E2 to E7 were prepared in the same manner as Example E1, except that the components and amounts of the epoxy adhesive compositions used to prepare the epoxy adhesives were different. Its components and amount series are specifically listed in Table 1.
根據在本文中所述之測試方法使實施例E2至E7所提供之環氧黏著劑組成物經受加工性測試，並使環氧黏著劑經受T-剝離強度測試及抗水汽滲透性之測試。測試結果係列在表1中。 The epoxy adhesive compositions provided in Examples E2-E7 were subjected to the processability test according to the test methods described herein, and the epoxy adhesives were subjected to the T-peel strength test and the water vapor permeation resistance test. The test results series are in Table 1.
比較例C1至C5 Comparative Examples C1 to C5
比較例C1至C5之環氧黏著劑係以與實例E1之相同方式製備，除了用以製備環氧黏著劑之環氧黏著劑組成物之組分及量不同。其組分及量係具體列在表2中。 The epoxy adhesives of Comparative Examples C1 to C5 were prepared in the same manner as Example E1, except that the components and amounts of the epoxy adhesive compositions used to prepare the epoxy adhesives were different. Its components and amount series are specifically listed in Table 2.
根據在本文中所述之測試方法使比較例C1至C5所提供之環氧黏著劑組成物經受加工性測試，並使環氧黏著劑經受T-剝離強度測試及抗水汽滲透性之測試。測試結果係列在表2中。 The epoxy adhesive compositions provided in Comparative Examples C1-C5 were subjected to the processability test according to the test methods described herein, and the epoxy adhesives were subjected to the T-peel strength test and the water vapor permeation resistance test. The test results series are in Table 2.
實例E8至E11 Instances E8 to E11
實例E8至E11之環氧黏著劑係以與實例E1之相同方式製備，除了添加聚醚胺固化劑亦添加咪唑促進劑，及用以製備環氧黏著劑之環氧黏著劑組成物之組分及量不同。其組分及量係具體列在表3中。 The epoxy adhesives of Examples E8 to E11 were prepared in the same manner as Example E1, except that the polyetheramine curing agent was added and the imidazole accelerator was added, and the components of the epoxy adhesive composition used to prepare the epoxy adhesives And the amount is different. Its components and amount series are specifically listed in Table 3.
根據在本文中所述之測試方法使實施例E8至E11所提供之環氧黏著劑組成物經受加工性測試，並使環氧黏著劑經受T-剝離強度測試及抗水汽滲透性之測試。測試結果係列在表3中。 The epoxy adhesive compositions provided in Examples E8 to E11 were subjected to the processability test according to the test methods described herein, and the epoxy adhesives were subjected to the T-peel strength test and the water vapor permeation resistance test. The test results series are in Table 3.
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