JP5148845B2 - Method for bonding parts of electronic products including polymer PTC elements - Google Patents
Method for bonding parts of electronic products including polymer PTC elements Download PDFInfo
- Publication number
- JP5148845B2 JP5148845B2 JP2006165275A JP2006165275A JP5148845B2 JP 5148845 B2 JP5148845 B2 JP 5148845B2 JP 2006165275 A JP2006165275 A JP 2006165275A JP 2006165275 A JP2006165275 A JP 2006165275A JP 5148845 B2 JP5148845 B2 JP 5148845B2
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- polymer
- parts
- reactive silicon
- silicon group
- mass
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- 238000000034 method Methods 0.000 title claims description 21
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- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 36
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- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- MHVJRKBZMUDEEV-UHFFFAOYSA-N (-)-ent-pimara-8(14),15-dien-19-oic acid Natural products C1CCC(C(O)=O)(C)C2C1(C)C1CCC(C=C)(C)C=C1CC2 MHVJRKBZMUDEEV-UHFFFAOYSA-N 0.000 description 2
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- BKIMMITUMNQMOS-UHFFFAOYSA-N normal nonane Natural products CCCCCCCCC BKIMMITUMNQMOS-UHFFFAOYSA-N 0.000 description 1
- MCCIMQKMMBVWHO-UHFFFAOYSA-N octadecanoic acid;titanium Chemical compound [Ti].CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O.CCCCCCCCCCCCCCCCCC(O)=O MCCIMQKMMBVWHO-UHFFFAOYSA-N 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 125000001181 organosilyl group Chemical group [SiH3]* 0.000 description 1
- CFJYNSNXFXLKNS-UHFFFAOYSA-N p-menthane Chemical compound CC(C)C1CCC(C)CC1 CFJYNSNXFXLKNS-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- WVDDGKGOMKODPV-ZQBYOMGUSA-N phenyl(114C)methanol Chemical compound O[14CH2]C1=CC=CC=C1 WVDDGKGOMKODPV-ZQBYOMGUSA-N 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 235000014786 phosphorus Nutrition 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000001739 pinus spp. Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- MOVRCMBPGBESLI-UHFFFAOYSA-N prop-2-enoyloxysilicon Chemical compound [Si]OC(=O)C=C MOVRCMBPGBESLI-UHFFFAOYSA-N 0.000 description 1
- TVDSBUOJIPERQY-UHFFFAOYSA-N prop-2-yn-1-ol Chemical compound OCC#C TVDSBUOJIPERQY-UHFFFAOYSA-N 0.000 description 1
- HKJYVRJHDIPMQB-UHFFFAOYSA-N propan-1-olate;titanium(4+) Chemical compound CCCO[Ti](OCCC)(OCCC)OCCC HKJYVRJHDIPMQB-UHFFFAOYSA-N 0.000 description 1
- 229960004063 propylene glycol Drugs 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- GRWFGVWFFZKLTI-UHFFFAOYSA-N rac-alpha-Pinene Natural products CC1=CCC2C(C)(C)C1C2 GRWFGVWFFZKLTI-UHFFFAOYSA-N 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- IYMSIPPWHNIMGE-UHFFFAOYSA-N silylurea Chemical compound NC(=O)N[SiH3] IYMSIPPWHNIMGE-UHFFFAOYSA-N 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 235000019830 sodium polyphosphate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- TXDNPSYEJHXKMK-UHFFFAOYSA-N sulfanylsilane Chemical compound S[SiH3] TXDNPSYEJHXKMK-UHFFFAOYSA-N 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- UQMOLLPKNHFRAC-UHFFFAOYSA-N tetrabutyl silicate Chemical compound CCCCO[Si](OCCCC)(OCCCC)OCCCC UQMOLLPKNHFRAC-UHFFFAOYSA-N 0.000 description 1
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- ZQZCOBSUOFHDEE-UHFFFAOYSA-N tetrapropyl silicate Chemical compound CCCO[Si](OCCC)(OCCC)OCCC ZQZCOBSUOFHDEE-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 229940036248 turpentine Drugs 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 description 1
Description
本発明は、難燃性湿気硬化型接着剤組成物及び接着方法に関し、特に、難燃性を要求される電気製品もしくは精密機器の組立用等の接着剤、固着剤として優れた性能を有し、電池およびバッテリー部品の内部抵抗に影響を与えず、かつ低粘度でありながら長期保存安定性に優れた難燃性湿気硬化型組成物、該難燃性湿気硬化型組成物を有効成分とする難燃性湿気硬化型接着剤組成物、及びそれを用いた接着方法に関する。 The present invention relates to a flame retardant moisture curable adhesive composition and an adhesion method, and in particular, has excellent performance as an adhesive or an adhesive for assembly of electrical products or precision equipment that requires flame retardancy. In addition, the flame retardant moisture curable composition that does not affect the internal resistance of the battery and battery parts and has low viscosity but excellent long-term storage stability, the flame retardant moisture curable composition as an active ingredient The present invention relates to a flame retardant moisture curable adhesive composition and an adhesion method using the same.
近年、電気・電子市場、建築市場、土木市場等では難燃性を付与した接着剤、シーリング材、塗料、注型材が強く求められている。また接着剤及びシーリング材においては、近年、異種材料の接着における熱膨張の差を吸収する弾性接着剤が広く使われるようになってきており、熱膨張の差による歪みに追従し、クラックを防止する接着性、変位追従性の優れた組成物が求められている。 In recent years, adhesives, sealing materials, paints and casting materials imparted with flame retardancy have been strongly demanded in the electric / electronic market, the construction market, the civil engineering market, and the like. In recent years, in adhesives and sealants, elastic adhesives that absorb the difference in thermal expansion in the bonding of different materials have become widely used, and follow the strain caused by the difference in thermal expansion to prevent cracks. There is a need for a composition having excellent adhesion and displacement followability.
難燃性接着剤における難燃剤としては、一般にはリン系難燃剤、ハロゲン系難燃剤、金属水酸化物等が用いられている。この中で、ポリリン酸ナトリウム、ポリリン酸アンモニウム等のポリリン酸塩及び五酸化リン等のリン系難燃剤は、耐水性の低下や銅を腐食させるおそれがあった。また、デカブロモジフェニルエーテル及びテトラブロモビスフェノールＡ等の臭素系難燃剤に代表されるハロゲン系難燃剤は、金属腐食や大気汚染のおそれを指摘されている。このハロゲン系難燃剤は酸化アンチモンとの併用で難燃効果が大幅に向上するが、酸化アンチモンは毒性をもつため好ましくないという問題もあった。 As the flame retardant in the flame retardant adhesive, generally, a phosphorus flame retardant, a halogen flame retardant, a metal hydroxide, or the like is used. Among them, polyphosphates such as sodium polyphosphate and ammonium polyphosphate and phosphorus flame retardants such as phosphorus pentoxide have a risk of lowering water resistance and corroding copper. In addition, halogen-based flame retardants represented by brominated flame retardants such as decabromodiphenyl ether and tetrabromobisphenol A have been pointed out to cause metal corrosion and air pollution. This halogen-based flame retardant greatly improves the flame retardant effect when used in combination with antimony oxide, but there is also a problem that antimony oxide is not preferable because it has toxicity.
他方、金属水酸化物である水酸化アルミニウムや水酸化マグネシウムはノンハロゲンの難燃剤として、近年各種プラスチックの難燃化剤として使われている。
しかしながら、シリル基変性ポリエーテル型組成物の難燃化にこれらの金属水酸化物を適用した場合、当該組成物１００質量部に対して少なくとも３５０質量部以上添加しないとＵＬ９４Ｖ−０（試料厚さ１．５ｍｍ）相当の難燃性が発揮されず、各種プラスチックへの接着性が劣り、熱老化性が低い等の問題があった。
なお、家電製品の難燃規制はアメリカのＵＬ規格が基本になっており、多くの製品が規制対象となっている。ＵＬ９４は、電気製品およびプラスチック材料の中の難燃性を評価するものであり、その中でＵＬ９４Ｖ−０は最も難燃性の高いクラスとして、規定されている。
On the other hand, metal hydroxides such as aluminum hydroxide and magnesium hydroxide have been used as non-halogen flame retardants and in recent years as flame retardants for various plastics.
However, when these metal hydroxides are applied to flame retardancy of a silyl group-modified polyether type composition, it is necessary to add at least 350 parts by mass or more to UL94V-0 (sample thickness) with respect to 100 parts by mass of the composition. 1.5 mm), the flame retardancy was not exhibited, there were problems such as poor adhesion to various plastics and low heat aging properties.
In addition, the flame retardance regulation of home appliances is based on the US UL standard, and many products are regulated. UL94 evaluates flame retardancy in electrical products and plastic materials, and UL94V-0 is defined as the class with the highest flame retardancy.
特許文献１には、反応性珪素基を有するアクリル系共重合体と金属水酸化物を含む難燃性を有する湿気硬化型組成物が記載されているが、該湿気硬化型組成物は、小さい部品の接着や固定をするには粘度が非常に高く作業性に難がある。小さい部品の接着や固定は生産性の観点からも接着剤の作業性は非常に重要であることから、今日では接着剤の低粘度化やフロー性が求められている。また、該湿気硬化型組成物を低粘度にするため低粘度の液体を添加した組成物では電池やバッテリー内の部品の内部抵抗を上昇させてしまうという問題があることが判明した。 Patent Document 1 describes a moisture curable composition having flame retardancy containing an acrylic copolymer having a reactive silicon group and a metal hydroxide, but the moisture curable composition is small. Viscosity is very high for bonding and fixing parts, and workability is difficult. Adhesion and fixing of small parts are very important from the viewpoint of productivity, and the workability of the adhesive is very important. Therefore, today, it is required to reduce the viscosity and flow of the adhesive. Further, it has been found that the composition added with a low-viscosity liquid in order to make the moisture-curable composition low in viscosity has a problem of increasing the internal resistance of the battery and parts in the battery.
また、復帰性を有し交換不要なサーミスターとして、正の温度特性（ＰＴＣ：Positive Temperature Coefficient）を有する導電性ポリマーを利用したポリマーＰＴＣ素子が知られているが（例えば、特許文献２及び３等）、前記湿気硬化型組成物を用いて、ポリマーＰＴＣ素子の接着やポリマーＰＴＣ素子と同一密閉空間中の部品の接着に用いた場合、ポリマーＰＴＣ素子の抵抗値に影響を与え、正常な作動をしない場合があることが判明した。
本発明は、難燃性を要求される電気製品もしくは精密機器の組立用等の接着剤、固着剤として優れた性能を有する難燃性湿気硬化型接着剤組成物及びそれを用いた接着方法を提供することを目的とする。 The present invention relates to a flame retardant moisture-curing adhesive composition having excellent performance as an adhesive for assembling an electrical product or precision instrument that requires flame retardancy, and a bonding method using the same. The purpose is to provide.
本発明者らは、上記課題を解決するために、鋭意研究を行った結果、反応性珪素基を有する有機重合体、金属水酸化物、粘度５００ｍＰａ・ｓ／２３℃以下でかつ誘電率５以上もしくは沸点１７０℃以下の液状化合物を組み合わせることによって、接着剤、固着剤としての基本的性能を満たした上で、ＵＬ９４Ｖ−０（試料厚さ１．５ｍｍ）に合格しうる難燃性を有する硬化物が得られ、かつ電気・電子部品に悪影響を与えることなく作業性・長期保存安定性に優れることを見出し、本発明を完成した。 As a result of intensive studies to solve the above problems, the present inventors have found that an organic polymer having a reactive silicon group, a metal hydroxide, a viscosity of 500 mPa · s / 23 ° C. or less, and a dielectric constant of 5 or more. Alternatively, by combining liquid compounds with a boiling point of 170 ° C. or lower, the cured product has flame retardancy that can pass UL94V-0 (sample thickness 1.5 mm) after satisfying the basic performance as an adhesive and fixing agent. The present invention was completed by finding that the product was obtained and that it was excellent in workability and long-term storage stability without adversely affecting electric / electronic components.
即ち、本発明のポリマーＰＴＣ素子を含む電子製品の部品の接着用難燃性湿気硬化型組成物は、（Ａ）反応性珪素基含有有機重合体、（Ｂ）平均粒径０．１〜２００μｍの金属水酸化物、及び（Ｃ）２３℃における粘度が５００ｍＰａ・ｓ以下である液状化合物であって、誘電率が５以上及び／又は沸点が１７０℃以下の液状化合物、を必須成分として含有し、前記液状化合物がアルコール類又はヘキサンであることを特徴とする。 That is, the flame-retardant moisture-curable composition for bonding electronic parts including the polymer PTC element of the present invention includes (A) a reactive silicon group-containing organic polymer, and (B) an average particle size of 0.1 to 200 μm. a metal hydroxide, and (C) a liquid compound viscosity at 23 ° C. is not more than 500 mPa · s, dielectric constant of 5 or more and / or a boiling point of 170 ° C. or less of the liquid compound, containing as essential components The liquid compound is an alcohol or hexane .
前記重合体（Ａ）が、反応性珪素基含有ポリオキシアルキレン系重合体、反応性珪素基含有（メタ）アクリル系重合体、反応性珪素基含有ポリイソブチレン系重合体からなる群から選択される１種又は２種以上であることが好ましい。なお、本発明において、アクリル又はメタクリルをあわせて（メタ）アクリルと記載する。 The polymer (A) is selected from the group consisting of a reactive silicon group-containing polyoxyalkylene polymer, a reactive silicon group-containing (meth) acrylic polymer, and a reactive silicon group-containing polyisobutylene polymer. It is preferable that it is 1 type or 2 types or more. In the present invention, acrylic or methacryl is collectively referred to as (meth) acrylic.
前記金属水酸化物（Ｂ）が、水酸化アルミニウム及び／又は水酸化マグネシウムであることが好ましい。特に、前記金属水酸化物（Ｂ）が、カップリング剤、脂肪酸又は樹脂酸で処理された金属水酸化物であることが好適である。該表面処理された金属水酸化物を使用すれば保存安定性における粘度上昇率や電気特性の改善もできる。 It is preferable that the metal hydroxide (B) is aluminum hydroxide and / or magnesium hydroxide. In particular, the metal hydroxide (B) is preferably a metal hydroxide treated with a coupling agent, a fatty acid or a resin acid. If the surface-treated metal hydroxide is used, the viscosity increase rate in storage stability and the electrical characteristics can be improved.
前記液状化合物（Ｃ）が、構造中に水酸基を有することが好ましい。また、前記液状化合物（Ｃ）が、炭素数１〜１０の炭化水素化合物であることが好適である。 The liquid compound (C) preferably has a hydroxyl group in the structure. Moreover, it is suitable that the said liquid compound (C) is a C1-C10 hydrocarbon compound.
本発明の難燃性湿気硬化型接着剤組成物は、（Ｄ）炭酸カルシウムをさらに含有することが好ましい。前記炭酸カルシウム（Ｄ）としては、表面処理された炭酸カルシウムが好ましく、脂肪酸もしくは樹脂酸で処理された表面処理炭酸カルシウムがより好ましい。 The flame retardant moisture curable adhesive composition of the present invention preferably further contains (D) calcium carbonate. As the calcium carbonate (D), surface-treated calcium carbonate is preferable, and surface-treated calcium carbonate treated with a fatty acid or a resin acid is more preferable.
本発明の難燃性湿気硬化型接着剤組成物は、（Ｅ）シリカをさらに含有することが好適である。前記シリカ（Ｅ）が親水性シリカであることが好ましい。 The flame retardant moisture curable adhesive composition of the present invention preferably further contains (E) silica. The silica (E) is preferably hydrophilic silica.
本発明の難燃性湿気硬化型接着剤組成物は、ポリマーＰＴＣ素子を含む電子製品の部品の接着に好適に用いられる。 The flame-retardant moisture-curable adhesive composition of the present invention is suitably used for bonding electronic product parts including polymer PTC elements.
本発明の接着方法は、本発明の難燃性湿気硬化型接着剤組成物を用いて難燃性を要求される製品の部品を接着することを特徴とする。
前記製品として、ポリマーＰＴＣ素子を含む電子製品が好適である。
The bonding method of the present invention is characterized in that a part of a product that requires flame retardancy is bonded using the flame-retardant moisture-curable adhesive composition of the present invention.
As the product, an electronic product including a polymer PTC element is suitable.
本発明の電子製品は、ポリマーＰＴＣ素子を含む電子製品であって、前記本発明方法により部品を接着されてなることを特徴とする。 The electronic product of the present invention is an electronic product including a polymer PTC element, and is characterized in that parts are bonded by the method of the present invention.
本発明の難燃性湿気硬化型接着剤組成物は、難燃性で無溶剤化が容易であり、高温で軟化せず、各種接着剤に対する接着性が良好でかつ保存安定性及び貯蔵安定性に優れており、難燃性を要求される電気製品もしくは精密機器の組立用の接着剤、固着剤として好適に用いられるという効果を奏する。さらに、本発明の難燃性湿気硬化型接着剤はポリマーＰＴＣ素子本体や同一密閉空間中の部品に用いられる接着剤として特に好適に用いられる。 The flame retardant moisture curable adhesive composition of the present invention is flame retardant and easy to be solvent-free, does not soften at high temperatures, has good adhesion to various adhesives, and has storage and storage stability. It is advantageous in that it is suitably used as an adhesive or an adhesive for assembling an electric product or precision instrument that requires flame retardancy. Furthermore, the flame retardant moisture curable adhesive of the present invention is particularly suitably used as an adhesive used for polymer PTC element bodies and parts in the same sealed space.
以下に本発明の実施の形態を説明するが、これら実施の形態は例示的に示されるもので、本発明の技術思想から逸脱しない限り種々の変形が可能なことはいうまでもない。 Embodiments of the present invention will be described below, but these embodiments are exemplarily shown, and it goes without saying that various modifications can be made without departing from the technical idea of the present invention.
本発明の難燃性湿気硬化型接着剤組成物は、下記成分（Ａ）、（Ｂ）及び（Ｃ）を必須成分として配合するものである。
（Ａ）反応性珪素基含有有機重合体、
（Ｂ）平均粒径０．１〜２００μｍの金属水酸化物、
（Ｃ）２３℃における粘度が５００ｍＰａ・ｓ以下である液状化合物であって、誘電率が５以上及び／又は沸点１７０℃以下の液状化合物。
The flame retardant moisture curable adhesive composition of the present invention contains the following components (A), (B) and (C) as essential components.
(A) a reactive silicon group-containing organic polymer,
(B) a metal hydroxide having an average particle size of 0.1 to 200 μm,
(C) A liquid compound having a viscosity at 23 ° C. of 500 mPa · s or less and having a dielectric constant of 5 or more and / or a boiling point of 170 ° C. or less.
前記重合体（Ａ）としては、反応性珪素基を含有する有機重合体であれば特に限定されず、公知の重合体を広く使用可能である。前記反応性珪素基は、珪素原子に結合した水酸基又は加水分解性基を有し、シロキサン結合を形成することにより架橋しうる珪素含有基であり、下記式（Ｉ）で示される珪素含有官能基が好適である。
前記重合体（Ａ）が、反応性珪素基含有ポリオキシアルキレン系重合体、反応性珪素基含有（メタ）アクリル系重合体、反応性珪素基含有（メタ）アクリル変性ポリオキシアルキレン系重合体、反応性珪素基含有ポリイソブチレン系重合体、及びこれらの混合物であることが好ましい。 The polymer (A) is a reactive silicon group-containing polyoxyalkylene polymer, a reactive silicon group-containing (meth) acrylic polymer, a reactive silicon group-containing (meth) acryl-modified polyoxyalkylene polymer, A reactive silicon group-containing polyisobutylene polymer and a mixture thereof are preferable.
前記反応性珪素基含有ポリオキシアルキレン系重合体としては、特に限定されるものではないが、具体的には、特公昭４５−３６３１９号、特公昭４６−１２１５４号、特公昭４９−３２６７３号、特開昭５０−１５６５９９号の各公報等に記載の反応性珪素基を有するオキシアルキレン系重合体があげられる。 The reactive silicon group-containing polyoxyalkylene polymer is not particularly limited, and specifically, JP-B 45-36319, JP-B 46-12154, JP-B 49-32673, Examples thereof include oxyalkylene polymers having a reactive silicon group described in JP-A-50-156599.
前記反応性珪素基含有（メタ）アクリル系重合体としては、特に限定されるものではないが、具体的には、特開昭５９−１２２５４１号、特開昭６０−３１５５６号、特開昭６３−１１２６４２号、特開平１１−３１０６８２号の各公報等に記載の公知の反応性珪素基を有する（メタ）アクリル系重合体が挙げられ、反応性珪素基を有する（メタ）アクリル酸エステル系共重合体が好ましく、加水分解により架橋可能な反応性珪素基を有し、分子鎖が実質的に、（１）炭素数１〜８のアルキル基を有する（メタ）アクリル酸アルキルエステル単量体単位及び、（２）炭素数１０以上のアルキル基を有する（メタ）アクリル酸アルキルエステル単量体単位からなる共重合体（Ａ１）を用いることが特に好ましい。なお、分子中の反応性珪素基の位置は特に限定されないが、分子鎖末端に反応性珪素基を有する（メタ）アクリル系重合体が好ましい。 The reactive silicon group-containing (meth) acrylic polymer is not particularly limited. Specifically, JP-A-59-122541, JP-A-60-31556, JP-A-63. And (meth) acrylic polymers having a reactive silicon group described in JP-A-11-12642, JP-A-11-310682, and the like. (Meth) acrylic acid alkyl ester monomer unit having a reactive silicon group that can be cross-linked by hydrolysis, and a molecular chain substantially having (1) an alkyl group having 1 to 8 carbon atoms. And (2) It is particularly preferable to use a copolymer (A1) comprising a (meth) acrylic acid alkyl ester monomer unit having an alkyl group having 10 or more carbon atoms. The position of the reactive silicon group in the molecule is not particularly limited, but a (meth) acrylic polymer having a reactive silicon group at the molecular chain end is preferred.
前記反応性珪素基含有有機重合体（Ａ）の製造法は、特に限定されず、公知の合成法を利用することができる。前記反応性珪素基含有有機重合体として、反応性珪素基を含有し、主鎖がアクリル系重合体等のビニル系重合体であるものを用いる場合、ラジカル重合法で合成されたビニル系重合体を用いることが好ましい。 The manufacturing method of the said reactive silicon group containing organic polymer (A) is not specifically limited, A well-known synthesis method can be utilized. When the reactive silicon group-containing organic polymer contains a reactive silicon group and the main chain is a vinyl polymer such as an acrylic polymer, a vinyl polymer synthesized by a radical polymerization method is used. Is preferably used.
上記重合体（Ａ）のうち、上記反応性珪素基含有（メタ）アクリル系重合体、上記反応性珪素基を有するポリオキシアルキレン系重合体、及びこれらの混合物は、他の重合体に比べ耐熱性が優れている。また、上記反応性珪素基を有する（メタ）アクリル系重合体、上記反応性珪素基を有するポリオキシアルキレン系重合体、及びこれらの混合物は、上記反応基を有するシリコーン等に比べ、接点障害の要因となる低分子環状シロキサンを含有もしくは発生させない点で好適である。 Among the polymers (A), the reactive silicon group-containing (meth) acrylic polymer, the polyoxyalkylene polymer having the reactive silicon group, and a mixture thereof are more heat resistant than other polymers. The property is excellent. In addition, the (meth) acrylic polymer having the reactive silicon group, the polyoxyalkylene polymer having the reactive silicon group, and a mixture thereof are more resistant to contact failure than silicone having the reactive group. This is preferable in that it does not contain or generate a low-molecular cyclic siloxane as a factor.
また、上記反応性珪素基を有する（メタ）アクリル酸エステル系共重合体は、重合度３０００〜６０００程度では粘度が高いために、可塑剤、ポリエーテルポリオール及び溶剤等の液状物で希釈しないと作業性が悪い場合がある。
一方、反応性珪素基を有するポリオキシアルキレン系重合体は、（メタ）アクリル酸エステル系共重合体に比べて、同じ重合度で低粘度のものが得られる。したがって、塗布性等の作業性を改善する目的で、上記反応性珪素基を有する（メタ）アクリル酸エステル系共重合体と反応性珪素基を有するオキシアルキレン系重合体を併用することで無溶剤型の難燃性組成物を構成することができる。
Moreover, since the (meth) acrylic acid ester-based copolymer having a reactive silicon group has a high viscosity at a polymerization degree of about 3000 to 6000, it must be diluted with a liquid material such as a plasticizer, a polyether polyol and a solvent. Workability may be poor.
On the other hand, a polyoxyalkylene polymer having a reactive silicon group can have a low viscosity at the same degree of polymerization as compared to a (meth) acrylic acid ester copolymer. Therefore, for the purpose of improving workability such as coating properties, a solvent-free operation can be achieved by using the (meth) acrylic acid ester copolymer having a reactive silicon group and the oxyalkylene polymer having a reactive silicon group in combination. A mold flame retardant composition can be constructed.
前記重合体（Ａ）として、上記反応性珪素基を有する（メタ）アクリル酸エステル系共重合体と、反応性珪素基を有するポリオキシアルキレン系重合体とからなる混合物を用いる場合、両者の配合割合は特に限定されないが、上記反応性珪素基を有する（メタ）アクリル酸エステル系共重合体１００質量部に対して、上記反応性珪素基を有するポリオキシアルキレン系重合体を１０〜２００質量部配合することが好ましい。 In the case of using a mixture of the (meth) acrylic acid ester copolymer having a reactive silicon group and a polyoxyalkylene polymer having a reactive silicon group as the polymer (A), the combination of both Although the ratio is not particularly limited, 10 to 200 parts by mass of the polyoxyalkylene polymer having the reactive silicon group is used with respect to 100 parts by mass of the (meth) acrylic acid ester copolymer having the reactive silicon group. It is preferable to mix.
前記金属水酸化物（Ｂ）としては、水酸化アルミニウム、水酸化マグネシウムが好適に用いられる。金属水酸化物は表面処理せずに使用してもよく、カップリング剤、脂肪酸及び樹脂酸等の処理剤で表面処理したものを用いてもよい。これらは単独で用いてもよく、２種以上併用してもよい。 As the metal hydroxide (B), aluminum hydroxide and magnesium hydroxide are preferably used. The metal hydroxide may be used without surface treatment, or may be used after surface treatment with a treatment agent such as a coupling agent, a fatty acid and a resin acid. These may be used alone or in combination of two or more.
上記カップリング剤としては、例えば、有機チタネート化合物、有機アルミニウム化合物、有機ジルコニウム化合物、アルコキシシランなどが挙げられる。具体的な有機チタネート化合物として、例えば、テトラプロポキシチタン、テトラブトキシチタン、テトラキス（２−エチルヘキシルオキシ）チタン、テトラステアリルオキシチタン、ジプロキシ・ビス（アセチルアセトナト）チタン、チタニウムプロポキシオクチレングリコレート、チタニウムステアレート、イソプロピルトリイソステアロイルチタネート、イソプロピルトリドデシルベンゼンスルホニルチタネート、イソプロピルトリス（ジオクチルパイロホスフェート）チタネート、テトライソプロピルビス（ジオクチルホスファイト）チタネート、テトラオクチルビス（ジトリデシルホスファイト）チタネート、テトラ（２，２−ジアリルオキシメチル−１−ブチル）ビス（ジートリデシル）ホスファイトチタネート、ビス（ジオクチルパイロホスフェート）オキシアセテートチタネート、トリス（ジオクチルパイロホスフェート）エチレンチタネートなどが挙げられる。アセトアルコキシアルミニウムジイソプロピレートなどの有機アルミニウム化合物やジルコニウムブチレート、ジルコニウムアセチルアセトネート、アセチルアセトンジルコニウムブチレート、ジルコニウムラクテート、ステアリン酸ジルコニウムブチレートなどの有機ジルコニウム化合物が使用できる。また、シラン化合物としては、例えば、ビニルトリメトキシシラン、ビニルトリエトキシシラン、ビストリス（２−メトキシエトキシ）シラン、Ｎ−（２−アミノエチル）３−アミノプロピルメチルジメトキシシラン、Ｎ−（２−アミノエチル）３−アミノプロピルメチルトリメトキシシラン、３−アミノプロピルトリメトキシシラン、３−アミノプロピルトリエトキシシラン、３−グリシドキシプロピルトリメトキシシラン、３−グリシドキシプロピルメチルジメトキシシラン、２−（３，４−エポキシシクロヘキシル）エチルトリメトキシシラン、３−クロロプロピルトリメトキシシラン、３−クロロプロピルメチルジメトキシシラン、３−メタクリロキシプロピルトリメトキシシラン、３−メルカプトプロピルトリメトキシシラン、ヘキサメチルジシラザンなどが挙げられる。 Examples of the coupling agent include organic titanate compounds, organoaluminum compounds, organozirconium compounds, and alkoxysilanes. Specific organic titanate compounds include, for example, tetrapropoxy titanium, tetrabutoxy titanium, tetrakis (2-ethylhexyloxy) titanium, tetrastearyloxy titanium, diproxy bis (acetylacetonato) titanium, titanium propoxyoctylene glycolate, titanium Stearate, isopropyltriisostearoyl titanate, isopropyltridodecylbenzenesulfonyl titanate, isopropyltris (dioctylpyrophosphate) titanate, tetraisopropylbis (dioctylphosphite) titanate, tetraoctylbis (ditridecylphosphite) titanate, tetra (2, 2-diallyloxymethyl-1-butyl) bis (ditridecyl) phosphite titanate, bis (diocyl) Le) oxyacetate titanate, tris (dioctyl pyrophosphate) ethylene titanate. Organoaluminum compounds such as acetoalkoxyaluminum diisopropylate and organozirconium compounds such as zirconium butyrate, zirconium acetylacetonate, acetylacetone zirconium butyrate, zirconium lactate and zirconium stearate butyrate can be used. Examples of the silane compound include vinyltrimethoxysilane, vinyltriethoxysilane, bistris (2-methoxyethoxy) silane, N- (2-aminoethyl) 3-aminopropylmethyldimethoxysilane, and N- (2-amino). Ethyl) 3-aminopropylmethyltrimethoxysilane, 3-aminopropyltrimethoxysilane, 3-aminopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3-glycidoxypropylmethyldimethoxysilane, 2- ( 3,4-epoxycyclohexyl) ethyltrimethoxysilane, 3-chloropropyltrimethoxysilane, 3-chloropropylmethyldimethoxysilane, 3-methacryloxypropyltrimethoxysilane, 3-mercaptopropyltrimethoxysilane, Such support hexamethyldisilazane and the like.
上記脂肪酸としては、例えば、カプリル酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、アラギン酸などの飽和脂肪酸、オレイン酸、エライジン酸、リノーリ酸、リシノール酸などの不飽和脂肪酸、ナフテン酸などの脂環族カルボン酸が挙げられる。
上記樹脂酸としては、例えば、アビチエン酸、ピマル酸、パラストリン酸、ネオアビエチン酸等が挙げられる。
Examples of the fatty acid include saturated fatty acids such as caprylic acid, lauric acid, myristic acid, palmitic acid, stearic acid, and alginic acid, unsaturated fatty acids such as oleic acid, elaidic acid, linoleic acid, and ricinoleic acid, and naphthenic acid. An alicyclic carboxylic acid is mentioned.
Examples of the resin acid include abithienic acid, pimaric acid, parastrinic acid, neoabietic acid, and the like.
水酸化アルミニウム、水酸化マグネシウム又はその混合物は高分子材料の分解温度と一致する約１８０〜３２０℃で構造水を放出するため、炎の着火、延焼を防ぐことが出来、優れた難燃性を発揮することができる。
また、上記金属水酸化物が芳香族アミン、フェノール、ナフトール類もしくは活性メチレン化合物などで処理されたカップリング剤、脂肪酸または樹脂酸で表面処理されたものを使用した場合、多少難燃効果は薄れるが、粘度安定性及び電気特性が向上する。
Aluminum hydroxide, magnesium hydroxide, or a mixture thereof releases structural water at about 180 to 320 ° C., which matches the decomposition temperature of the polymer material, so that flame ignition and fire spread can be prevented, and excellent flame retardancy is achieved. It can be demonstrated.
In addition, when the above metal hydroxide is treated with a coupling agent treated with an aromatic amine, phenol, naphthols or active methylene compound, a surface treated with a fatty acid or a resin acid, the flame retardant effect is somewhat diminished. However, viscosity stability and electrical properties are improved.
上記金属水酸化物の粒径は０．１μｍ〜２００μｍが用いられるが、０．３μｍ〜１００μｍが更に好ましく、０．３μｍ〜３０μｍが最も好ましい。
該金属水酸化物の粒径が、０．１μｍより小さいと、組成物粘度が著しい高くなり作業性が悪くなる問題があり、一方２００μｍより大きいと、微量定量吐出の場合に針先や装置嵌合部で詰まる問題がある。
The particle size of the metal hydroxide is 0.1 μm to 200 μm, more preferably 0.3 μm to 100 μm, and most preferably 0.3 μm to 30 μm.
If the particle size of the metal hydroxide is smaller than 0.1 μm, there is a problem that the viscosity of the composition is remarkably increased and workability is deteriorated. There is a problem of clogging at joints.
金属水酸化物の量は、重合体（Ａ）１００質量部に対して１５０質量部〜３５０質量部が配合されることが好ましく、１７０質量部〜２８０質量部が更に好ましく、１９０質量部〜２５０質量部が最も好ましい。この金属水酸化物の量が、１５０質量部より少ないと、充分な難燃性が得られず、例えば着火すると延焼し続けたりポリマーが解重合し液状化することがあり、一方３５０質量部を超えると、組成物粘度が高くなり作業性が悪くなる問題の他、接着強さ等の基本的物性が保てなくなる場合がある。また金属水酸化物の粒径によっても難燃効果は多少異なる。
上記のハロゲン系、リン系、酸化アンチモン等の難燃剤は通常の使用において上述したような問題があるが、本発明においては、これらの難燃剤を金属水酸化物と併用することも可能である。この他に、硼酸亜鉛、錫酸亜鉛等も発煙量の低減効果が有るため、添加することができる。
The amount of the metal hydroxide is preferably 150 to 350 parts by mass, more preferably 170 to 280 parts by mass, and 190 to 250 parts by mass with respect to 100 parts by mass of the polymer (A). Part by mass is most preferred. When the amount of the metal hydroxide is less than 150 parts by mass, sufficient flame retardancy cannot be obtained. For example, when ignited, the flame may continue to spread or the polymer may be depolymerized and liquefied. If it exceeds, the composition viscosity becomes high and the workability becomes worse, and the basic physical properties such as adhesive strength may not be maintained. In addition, the flame retardant effect varies somewhat depending on the particle size of the metal hydroxide.
Flame retardants such as the above halogen-based, phosphorus-based, and antimony oxide have the above-described problems in normal use. In the present invention, these flame retardants can be used in combination with metal hydroxides. . In addition, zinc borate, zinc stannate and the like can be added because they have an effect of reducing the amount of smoke generated.
前記液状化合物（Ｃ）は、２３℃の粘度が５００ｍＰａ・ｓ以下の液状化合物であり、且つ（１）誘電率５以上、（２）沸点１７０℃以下、の一方又は両方の条件を満たすものでる。これらは単独で用いられてもよく、２種以上が併用されてもよい。
前記液状化合物（Ｃ）の２３℃での粘度が５０ｍＰａ・ｓ以下であることが好ましく、３０ｍＰａ・ｓ以下であることがより好ましい。粘度の下限は特に限定されないが、０．０１ｍＰａ・ｓ以上であることが好適である。
前記液状化合物（Ｃ）の誘電率が１０以上であることが好ましく、２０以上であることがより好ましい。誘電率の上限は特に限定されないが、５０以下が好適である。
前記液状化合物（Ｃ）の沸点が１００℃以下であることが好ましい。沸点の下限は特に限定されないが、４０℃以上であることが好適である。
The liquid compound (C) is a liquid compound having a viscosity at 23 ° C. of 500 mPa · s or less, and satisfies one or both conditions of (1) a dielectric constant of 5 or more and (2) a boiling point of 170 ° C. or less. . These may be used independently and 2 or more types may be used together.
The viscosity of the liquid compound (C) at 23 ° C. is preferably 50 mPa · s or less, and more preferably 30 mPa · s or less. Although the minimum of a viscosity is not specifically limited, It is suitable that it is 0.01 mPa * s or more.
The dielectric constant of the liquid compound (C) is preferably 10 or more, and more preferably 20 or more. The upper limit of the dielectric constant is not particularly limited, but is preferably 50 or less.
The boiling point of the liquid compound (C) is preferably 100 ° C. or lower. Although the minimum of a boiling point is not specifically limited, It is suitable that it is 40 degreeC or more.
前記液状化合物（Ｃ）において、２３℃での粘度が５００ｍＰａ・ｓ以下で且つ誘電率５以上の液状化合物としては、例えば、構造中に極性基を有する液状化合物が好ましく、ＯＨ基を有する液状化合物やアセテート類等が好適に用いられるが、ＯＨ基を有する液状化合物がより好ましい。
具体的には、メタノール、エタノール、１−プロパノール、２−プロパノール（イソプロピルアルコール）、１−ブタノール、２−ブタノール、イソブチルアルコール、tert−ブチルアルコール、１−ペンタノール、２−ペンタノール、３−ペンタノール、２−メチル−１−ブタノール、イソペンチルアルコール、tert−ペンチルアルコール、３−メチル−２−ブタノール、ネオペンチルアルコール、１−ヘキサノール、２−メチル−１−ペンタノール、４−メチル−２−ペンタノール、２−エチル−１−ブタノール、１−ヘプタノール、２−ヘプタノール、３−ヘプタノール、１−オクタノール、２−オクタノール、２−エチル−１ヘキサノール、１−ノナノール、３，３，５−トリメチル−１−ヘキサノール、１−デカノール、１−ウンデカノール、１−ドデカノール、アリルアルコール、プロパルギルアルコール、ベンジルアルコール、シクロヘキサノール、１−メチルシクロヘキサノール、２−メチルシクロヘキサノール、３−メチルシクロヘキサノール、４−メチルシクロヘキサノール、１，２−エタンジオール、１，２−プロパンジオール、１，３−プロパンジオール、１，２−ブタンジオール、１，３−ブタンジオール、１，４−ブタンジオール、２，３−ブタンジオール、１，５−ペンタンジオール、２−ブテン−１，４−ジオール、２−メチル−２，４−ペンタンジオール、２−エチル−１，３−ヘキサンジオール、２−エチル−２−（ヒドロキシメチル）−１，３−プロパンジオール、１，２，６−ヘキサントリオール、３−メトキシ−３−メチル−１−ブタノール、３−メチル−１，３−ブタンジオール、２−メチル−１，３−プロパンジオールなどのアルコール類、並びに３−メトキシ−３−メチル−ブチルアセテート、プロピレングリコールモノメチルエーテルアセテートなどのアセテート類等が挙げられ、中でも分子量１００以下のメタノール、エタノール、イソプロピルアルコールなどのアルコール類が好適に用いられる。これらは単独で用いられてもよく、２種以上が併用されてもよい。
In the liquid compound (C), as the liquid compound having a viscosity at 23 ° C. of 500 mPa · s or less and a dielectric constant of 5 or more, for example, a liquid compound having a polar group in its structure is preferable, and a liquid compound having an OH group And acetates are preferably used, but a liquid compound having an OH group is more preferable.
Specifically, methanol, ethanol, 1-propanol, 2-propanol (isopropyl alcohol), 1-butanol, 2-butanol, isobutyl alcohol, tert-butyl alcohol, 1-pentanol, 2-pentanol, 3-pen Tanol, 2-methyl-1-butanol, isopentyl alcohol, tert-pentyl alcohol, 3-methyl-2-butanol, neopentyl alcohol, 1-hexanol, 2-methyl-1-pentanol, 4-methyl-2- Pentanol, 2-ethyl-1-butanol, 1-heptanol, 2-heptanol, 3-heptanol, 1-octanol, 2-octanol, 2-ethyl-1-hexanol, 1-nonanol, 3,3,5-trimethyl- 1-hexanol, 1-decanol, 1-unde 1-dodecanol, allyl alcohol, propargyl alcohol, benzyl alcohol, cyclohexanol, 1-methylcyclohexanol, 2-methylcyclohexanol, 3-methylcyclohexanol, 4-methylcyclohexanol, 1,2-ethanediol, 1 , 2-propanediol, 1,3-propanediol, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, 2,3-butanediol, 1,5-pentanediol, 2- Butene-1,4-diol, 2-methyl-2,4-pentanediol, 2-ethyl-1,3-hexanediol, 2-ethyl-2- (hydroxymethyl) -1,3-propanediol, 1, 2,6-hexanetriol, 3-methoxy-3-methyl-1-butanol , Alcohols such as 3-methyl-1,3-butanediol and 2-methyl-1,3-propanediol, and acetates such as 3-methoxy-3-methyl-butyl acetate and propylene glycol monomethyl ether acetate Among them, alcohols such as methanol, ethanol and isopropyl alcohol having a molecular weight of 100 or less are preferably used. These may be used independently and 2 or more types may be used together.
前記液状化合物（Ｃ）において、２３℃での粘度が５００ｍＰａ・ｓ以下で且つ沸点が１７０以下の液状化合物としては、例えば、炭素数１〜１０の炭化水素化合物が好ましい。
具体的には、ヘキサン、２−メチルペンタン、２，２−ジメチルブタン、２，３−ジメチルブタン、ヘプタン、オクタン、２，２，３−トリメチルペンタン、イソオクタン、ノナン、２，２，５−トリメチルヘキサン、１−ヘキセン、１−ヘプテン、１−オクテン、１−ノネン、ベンゼン、トルエン、キシレン、エチルベンゼン、クメン、メシチレン、tert−ブチルベンゼン、スチレン、シクロペンタン、メチルシクロペンタン、シクロヘキサン、メチルシクロヘキサン、エチルシクロヘキサン、P-メンタン、シクロヘキセン、α−ピネン、テレビン油などの炭化水素化合物などが挙げられる。特に誘電率が５未満の場合、沸点１００℃以下が好ましく、具体的にはヘキサンが好適に用いられる。これらは単独で用いられてもよく、２種以上が併用されてもよい。
In the liquid compound (C), as the liquid compound having a viscosity at 23 ° C. of 500 mPa · s or less and a boiling point of 170 or less, for example, a hydrocarbon compound having 1 to 10 carbon atoms is preferable.
Specifically, hexane, 2-methylpentane, 2,2-dimethylbutane, 2,3-dimethylbutane, heptane, octane, 2,2,3-trimethylpentane, isooctane, nonane, 2,2,5-trimethyl Hexane, 1-hexene, 1-heptene, 1-octene, 1-nonene, benzene, toluene, xylene, ethylbenzene, cumene, mesitylene, tert-butylbenzene, styrene, cyclopentane, methylcyclopentane, cyclohexane, methylcyclohexane, ethyl And hydrocarbon compounds such as cyclohexane, P-menthane, cyclohexene, α-pinene, and turpentine. In particular, when the dielectric constant is less than 5, the boiling point is preferably 100 ° C. or lower, and specifically, hexane is preferably used. These may be used independently and 2 or more types may be used together.
前記液状化合物（Ｃ）の配合割合は特に限定されないが、重合体（Ａ）１００質量部に対して１〜３０質量部が好ましく、３〜３０質量部配合がより好ましく、５〜３０質量部がさらに好ましい。該液状化合物（Ｃ）の配合により、減粘効果が得られ、低粘度化が可能となるが、３０質量部をこえると体積変化が大きくなったり、長期保存安定性（ブリードアウト）が低下する場合がある。前記液状化合物（Ｃ）は単独で用いてもよく、２種以上用いてもよい。 The blending ratio of the liquid compound (C) is not particularly limited, but is preferably 1 to 30 parts by weight, more preferably 3 to 30 parts by weight, and more preferably 5 to 30 parts by weight with respect to 100 parts by weight of the polymer (A). Further preferred. By blending the liquid compound (C), a viscosity-reducing effect can be obtained and the viscosity can be lowered. However, if the amount exceeds 30 parts by mass, the volume change becomes large, and long-term storage stability (bleed out) decreases. There is a case. The liquid compound (C) may be used alone or in combination of two or more.
本発明の難燃性湿気硬化型接着剤組成物には、さらに（Ｄ）炭酸カルシウムを配合することが好ましい。該炭酸カルシウム（Ｄ）の粒径は特に限定されないが、平均粒径０．０１〜１０μｍが好ましく、０．０１〜０．０５μｍがより好ましく、０．０１〜０．０３μｍがさらに好ましい。
前記炭酸カルシウム（Ｄ）は表面処理された炭酸カルシウムと無処理の炭酸カルシウムもいずれも使用できるが、表面処理された炭酸カルシウムがより好ましい。
It is preferable to further add (D) calcium carbonate to the flame-retardant moisture-curable adhesive composition of the present invention. The particle size of the calcium carbonate (D) is not particularly limited, but the average particle size is preferably 0.01 to 10 μm, more preferably 0.01 to 0.05 μm, and still more preferably 0.01 to 0.03 μm.
As the calcium carbonate (D), both surface-treated calcium carbonate and untreated calcium carbonate can be used, but surface-treated calcium carbonate is more preferable.
前記表面処理された炭酸カルシウムの表面処理剤としては、具体的には、カプリル酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、アラギン酸などの飽和脂肪酸、オレイン酸、エライジン酸、リノーリ酸、リシノール酸などの不飽和脂肪酸、ナフテン酸などの脂環族カルボン酸、アビチエン酸、ピマル酸、パラストリン酸、ネオアビエチン酸などの樹脂酸などが挙げられる。またスルホン酸類、アルカリ金属塩、アルカリ土類金属塩、アンモニウム塩、アミン塩で処理された炭酸カルシウムも使用でき、さらにはアニオン性、カチオン性、ノニオン性の界面活性剤で処理された炭酸カルシウムも使用できる。 Specific examples of the surface treatment agent for the surface-treated calcium carbonate include saturated fatty acids such as caprylic acid, lauric acid, myristic acid, palmitic acid, stearic acid, and alginic acid, oleic acid, elaidic acid, linoleic acid, Examples thereof include unsaturated fatty acids such as ricinoleic acid, alicyclic carboxylic acids such as naphthenic acid, and resin acids such as abithienic acid, pimaric acid, parastrinic acid, and neoabietic acid. In addition, calcium carbonate treated with sulfonic acids, alkali metal salts, alkaline earth metal salts, ammonium salts, and amine salts can be used, and calcium carbonate treated with anionic, cationic, and nonionic surfactants can also be used. Can be used.
さらに、前記炭酸カルシウムが、ＢＥＴ比表面積２０〜１００ｍ2／ｇの炭酸カルシウムを脂肪酸で表面処理した炭酸カルシウムであることが好ましい。前記脂肪酸による表面処理は不飽和脂肪酸と飽和脂肪酸で行うことが好ましく、該不飽和脂肪酸及び飽和脂肪酸は、酸の形態でも使用可能であるが、金属塩及び／又はエステルの形態で用いてもよい。不飽和脂肪酸と飽和脂肪酸を併用する場合、両者の混合割合は特に限定されないが、不飽和脂肪酸／飽和脂肪酸が０．５〜１．９であることが好ましい。また、水銀圧入法による空隙径分布曲線における最多確率空隙径のピークが０．０３μｍ未満であり、且つ最多確率空隙容量が０．０５〜０．５ｃｍ3／ｇであることが好ましい。このような表面処理炭酸カルシウムとしては、具体的には、特開２００３−１７１１２１号等に記載の炭酸カルシウムが挙げられる。 Further, the calcium carbonate is preferably calcium carbonate obtained by surface-treating calcium carbonate having a BET specific surface area of 20 to 100 m 2 / g with a fatty acid. The surface treatment with the fatty acid is preferably performed with an unsaturated fatty acid and a saturated fatty acid. The unsaturated fatty acid and the saturated fatty acid can be used in the form of an acid, but may be used in the form of a metal salt and / or an ester. . When the unsaturated fatty acid and the saturated fatty acid are used in combination, the mixing ratio of the two is not particularly limited, but the unsaturated fatty acid / saturated fatty acid is preferably 0.5 to 1.9. Moreover, it is preferable that the peak of the most probable void diameter in the void diameter distribution curve by the mercury intrusion method is less than 0.03 μm, and the most probable void volume is 0.05 to 0.5 cm 3 / g. Specific examples of such surface-treated calcium carbonate include calcium carbonate described in JP-A No. 2003-171121.
前記炭酸カルシウム（Ｄ）の配合割合は特に限定されないが、重合体（Ａ）１００質量部に対して１〜５０質量部配合されることが好ましく、３〜４０質量部が更に好ましく、５〜３０質量部が最も好ましい。炭酸カルシウムが５０質量部を超えると、十分な難燃性は得られるものの、組成物の粘度が高粘度となり作業性に問題が生じる場合がある。 Although the blending ratio of the calcium carbonate (D) is not particularly limited, it is preferably 1 to 50 parts by weight, more preferably 3 to 40 parts by weight, with respect to 100 parts by weight of the polymer (A). Part by mass is most preferred. When the calcium carbonate exceeds 50 parts by mass, sufficient flame retardancy can be obtained, but the viscosity of the composition becomes high and there may be a problem in workability.
本発明の難燃性湿気硬化型接着剤組成物には、さらに（Ｅ）シリカを配合することが好ましい。該シリカは親水性シリカと疎水性シリカのいずれも使用できるが、親水性シリカがより好ましい。これらは単独で用いられてもよく、２種類以上が併用されてもよい。
前記シリカ（Ｅ）の粒径は特に限定されないが、微粉末シリカが好ましい。
前記シリカ（Ｅ）の配合割合は特に限定されないが、重合体（Ａ）１００質量部に対して１〜２０質量部配合されることが好ましく、２〜１０質量部配合されることがより好ましい。
It is preferable that (E) silica is further blended in the flame-retardant moisture-curable adhesive composition of the present invention. As the silica, either hydrophilic silica or hydrophobic silica can be used, and hydrophilic silica is more preferable. These may be used alone or in combination of two or more.
The particle size of the silica (E) is not particularly limited, but fine powder silica is preferable.
Although the compounding ratio of the silica (E) is not particularly limited, it is preferably 1 to 20 parts by mass and more preferably 2 to 10 parts by mass with respect to 100 parts by mass of the polymer (A).
本発明の難燃性湿気硬化型接着剤組成物には、必要に応じて、種々の添加剤を添加してもよい。添加剤としては、例えば、水分吸収剤、接着付与剤、硬化触媒、充填剤、難燃助剤、紫外線吸収剤、老化防止剤、着色剤などが挙げられる。 Various additives may be added to the flame-retardant moisture-curable adhesive composition of the present invention as necessary. Examples of the additive include a moisture absorbent, an adhesion-imparting agent, a curing catalyst, a filler, a flame retardant aid, an ultraviolet absorbent, an antiaging agent, and a colorant.
前記水分吸収剤としては組成物の水分を吸収したり、水分と反応するものであれば特に限定されない。例えば、メチルシリケート、エチルシリケート、プロピルシリケート、ブチルシリケートに代表されるシリケート化合物類およびそのオリゴマー類、ビニルシラン類、酸化カルシウムなどが挙げられる。これらは単独で用いられてもよく、２種以上が併用されてもよい。 The moisture absorbent is not particularly limited as long as it absorbs moisture of the composition or reacts with moisture. Examples thereof include silicate compounds represented by methyl silicate, ethyl silicate, propyl silicate, butyl silicate and oligomers thereof, vinyl silanes, calcium oxide and the like. These may be used independently and 2 or more types may be used together.
前記接着付与剤としては、例えば、ビニルシラン、エポキシシラン、スチリルシラン、メタクリロキシシラン、アクリロキシシラン、アミノシラン、ウレイドシラン、クロロプロピルシラン、メルカプトシラン、スルフィドシラン及びイソシアネートシランなどが挙げられる。これらは単独で用いられてもよく、２種類以上が併用されてもよい。 Examples of the adhesion-imparting agent include vinyl silane, epoxy silane, styryl silane, methacryloxy silane, acryloxy silane, amino silane, ureido silane, chloropropyl silane, mercapto silane, sulfide silane, and isocyanate silane. These may be used alone or in combination of two or more.
前記硬化触媒としては、前記重合体（Ａ）を架橋させる触媒であれば特に限定されない。具体的には、ジブチル錫ジラウレート、ジブチル錫オキサイド、ジブチル錫ジアセテート、ジブチル錫ジステアレート、ジブチル錫ラウレートオキサイド、ジブチル錫ジアセチルアセトナート、ジブチル錫ジオレイルマレート、ジブチル錫オクトエート、ジオクチル錫オキサイド、ジオクチル錫ジラウレート等の錫化合物；金属錯体としてはテトラ−ｎ−ブトキシチタネート、テトライソプロポキシチタネート等のチタネート系化合物；オクチル酸鉛、ナフテン酸鉛、ナフテン酸ニッケル、ナフテン酸コバルト、亜鉛系化合物、鉄系化合物、ビスマス等のカルボン酸金属塩；アルミニウムアセチルアセトナート錯体、バナジウムアセチルアセトナート錯体等の金属アセチルアセトナート錯体が挙げられる。またジブチルアミン−２−エチルヘキソエート等のアミン塩や、モノメチル燐酸、ジ−ｎ−ブチル燐酸などの有機燐酸化合物や他の酸性触媒及び塩基性触媒等も使用することができる。これらは単独で用いられてもよく、２種類以上が併用されてもよい。 The curing catalyst is not particularly limited as long as it is a catalyst that crosslinks the polymer (A). Specifically, dibutyltin dilaurate, dibutyltin oxide, dibutyltin diacetate, dibutyltin distearate, dibutyltin laurate oxide, dibutyltin diacetylacetonate, dibutyltin dioleyl malate, dibutyltin octoate, dioctyltin oxide, dioctyl Tin compounds such as tin dilaurate; Titanate compounds such as tetra-n-butoxy titanate and tetraisopropoxy titanate as metal complexes; lead octylate, lead naphthenate, nickel naphthenate, cobalt naphthenate, zinc-based compounds, iron-based compounds Compound, carboxylic acid metal salt such as bismuth; metal acetylacetonate complex such as aluminum acetylacetonate complex and vanadium acetylacetonate complex. Also, amine salts such as dibutylamine-2-ethylhexoate, organic phosphoric acid compounds such as monomethyl phosphoric acid and di-n-butyl phosphoric acid, other acidic catalysts and basic catalysts, and the like can be used. These may be used alone or in combination of two or more.
前記充填剤としては、各種形状の有機又は無機のものが挙げられるが、タルク、クレー、炭酸マグネシウム、無水珪素、含水珪素、珪酸カルシウム、シラスバルーン、ガラスバルーン等の無機物が好ましく、このような無機物を添加した場合、難燃性や作業性が向上することがある。 Examples of the filler include organic or inorganic materials of various shapes, but inorganic materials such as talc, clay, magnesium carbonate, anhydrous silicon, hydrated silicon, calcium silicate, shirasu balloon, glass balloon and the like are preferable. In some cases, flame retardancy and workability may be improved.
前記難燃助剤としては、特に限定されないが、難燃剤として市販されているシリコーン化合物が好ましく、ノンハロゲンの難燃助剤として用いることができる。 Although it does not specifically limit as said flame retardant adjuvant, The silicone compound marketed as a flame retardant is preferable, and it can use as a flame retardant adjuvant of a non-halogen.
また、本発明の難燃性湿気硬化型接着剤組成物にさらにエポキシ樹脂を併用すると、残炭率が向上してドリップ性（燃焼中に落下すること）が改善するため、金属水酸化物の配合量を低減できる。 Further, when an epoxy resin is further used in combination with the flame-retardant moisture-curable adhesive composition of the present invention, the residual carbon ratio is improved and the drip property (falling during combustion) is improved. The blending amount can be reduced.
本発明の難燃性湿気硬化型接着剤組成物は、必要に応じて１液型とすることも可能であるし、２液型とすることも可能である。本発明の難燃性湿気硬化型接着剤組成物は、接着剤や固着剤としての使用が最も適しているが、必要に応じて、シーリング材、粘着材、コーティング材、ポッティング材等としても使用可能である。本発明の難燃性湿気硬化型接着剤組成物は、各種電気・電子分野用、建築物用、自動車用、土木用等に使用可能である。 The flame retardant moisture curable adhesive composition of the present invention can be a one-component type or a two-component type as required. The flame retardant moisture curable adhesive composition of the present invention is most suitable for use as an adhesive or a sticking agent, but also used as a sealing material, an adhesive material, a coating material, a potting material, etc. Is possible. The flame-retardant moisture-curable adhesive composition of the present invention can be used for various electric / electronic fields, buildings, automobiles, civil engineering, and the like.
本発明の接着方法は、前記難燃性湿気硬化型接着剤組成物を用いて難燃性を要求される製品の部品接着を行うものである。該難燃性を要求される製品としては、電気製品、例えば、ＰＴＣ素子を含む電子製品、スピーカー、ビデオカセットプレイヤー、テレビ、ラジオ、自動販売機、冷蔵庫、パーソナルコンピューター、カード型電池、ビデオカメラ等やカメラ、自動車部品及び精密機器等を挙げることができる。前記ＰＴＣ素子がポリマーＰＴＣ素子であることが好適である。ＰＴＣ素子は、例えば、電池パック、回路保護素子、温度感応スイッチなど、さらに具体的には、トランス、モーターの加熱保護、回路のＩＣ、ＬＳＩの加熱、過電流保護、電池パックの加熱、過電流保護、コンピュータおよび周辺機器の加熱、過電流保護などに好適に用いられる。ポリマーＰＴＣ素子を含む電子製品としては、例えば、コンピュータ及び周辺機器、携帯電話の電池パック、通信及びネットワーク機器、電源、産業用コントローラ、自動車、民生用機器等が挙げられる。 The bonding method of the present invention is to perform component bonding of products that require flame retardancy using the flame retardant moisture curable adhesive composition. The products requiring flame retardancy include electrical products such as electronic products including PTC elements, speakers, video cassette players, televisions, radios, vending machines, refrigerators, personal computers, card-type batteries, video cameras, etc. And cameras, automobile parts and precision equipment. The PTC element is preferably a polymer PTC element. PTC elements include, for example, battery packs, circuit protection elements, temperature sensitive switches, and more specifically, transformers, motor heating protection, circuit ICs, LSI heating, overcurrent protection, battery pack heating, overcurrent It is suitably used for protection, heating of computers and peripheral devices, overcurrent protection and the like. Examples of electronic products including polymer PTC elements include computers and peripheral devices, battery packs for mobile phones, communication and network devices, power supplies, industrial controllers, automobiles, consumer devices, and the like.
本発明の接着方法は、これらに加えて、高圧部品、高圧となりうる回路やその周辺で使用される部品の接着、長時間連続運転される電器製品内の接着にも適用することができる。これらの部品の具体例としては、コネクター、スイッチ、リレー、電線ケーブル、フライバックトランス、偏向ヨーク等を挙げることができる。特に、ポリマーＰＴＣ素子やポリマーＰＴＣ素子と同一密閉空間内の他の部品の接着に好適に用いることができ、該他の部品はＰＴＣ素子に接触していてもよく、接触していなくてもよい。 In addition to these, the bonding method of the present invention can also be applied to bonding of high-voltage components, circuits capable of becoming high voltage and components used in the vicinity thereof, and bonding in electrical products that are operated continuously for a long time. Specific examples of these parts include connectors, switches, relays, electric cables, flyback transformers, deflection yokes, and the like. In particular, it can be suitably used for adhesion of a polymer PTC element or other parts in the same sealed space as the polymer PTC element, and the other parts may or may not be in contact with the PTC element. .
以下に実施例をあげて本発明をさらに具体的に説明するが、これらの実施例は例示的に示されるもので限定的に解釈されるべきでないことはいうまでもない。 The present invention will be described more specifically with reference to the following examples. However, it is needless to say that these examples are shown by way of illustration and should not be construed in a limited manner.
（実施例１）
表１に示した配合（単位：質量部）で成分（Ａ）〜（Ｅ）をプラネタリーミキサーに入れて１００℃で１時間混合した後、２０℃に冷却し、水分吸収剤、硬化触媒及び接着付与剤を入れて、１０分間真空減圧混合し、室温湿気硬化型組成物を得た。
Example 1
After mixing components (A) to (E) in a planetary mixer with the formulation shown in Table 1 (unit: parts by mass) and mixing at 100 ° C. for 1 hour, the mixture was cooled to 20 ° C., and the moisture absorbent, curing catalyst, and An adhesion-imparting agent was added and mixed under vacuum for 10 minutes to obtain a room temperature moisture-curable composition.
（実施例２〜１０及び比較例１〜４）
表１及び表２に示した如く、配合物質を変更した以外は実施例１と同様に室温湿気硬化型組成物を調製した。
(Examples 2 to 10 and Comparative Examples 1 to 4)
As shown in Tables 1 and 2, room temperature moisture-curable compositions were prepared in the same manner as in Example 1 except that the compounding substances were changed.
表１及び表２中の各配合物質は次の通りである。
＊１）ＭＡ４５０：（株）カネカ製、ポリオキシアルキレン重合体とアクリル系重合体との混合物
＊２）ハイジライトＨ４２：昭和電工（株）製、水酸化アルミニウム（平均粒径１．１μｍ）
＊３）ハイジライトＨ４２Ｓ：昭和電工（株）製、表面脂肪酸処理水酸化アルミニウム（平均粒径１．１μｍ）
＊４）白艶華ＣＣＲ：白石工業（株）製、表面処理炭酸カルシウム（平均粒径０．０８μｍ）
＊５）ビスコエクセル３０：白石工業（株）製、表面処理炭酸カルシウム（平均粒径０．０３μｍ）
＊６）シリカ：（株）トクヤマ製、商品名レオロシールＱＳ−２０〔親水性シリカ〕
＊７）水分吸収剤：エチルシリケート
＊８）硬化触媒：ジブチル錫ジラウレート
＊９）接着付与剤：東レダウコーニングシリコーン（株）製、商品名ＳＨ６０２０〔γ−（２−アミノエチル）アミノプロピルトリメトキシシラン〕
＊１０）ＰＰＧ：三井化学ポリウレタン（株）製、商品名ＳＨＰ−２５５０
Each compounding substance in Table 1 and Table 2 is as follows.
* 1) MA450: manufactured by Kaneka Corporation, a mixture of polyoxyalkylene polymer and acrylic polymer * 2) Heidilite H42: manufactured by Showa Denko KK, aluminum hydroxide (average particle size 1.1 μm)
* 3) Heidilite H42S: manufactured by Showa Denko KK, surface fatty acid-treated aluminum hydroxide (average particle size 1.1 μm)
* 4) Shiraka Hana CCR: Shiraishi Kogyo Co., Ltd., surface treated calcium carbonate (average particle size 0.08 μm)
* 5) Bisco Excel 30: manufactured by Shiraishi Kogyo Co., Ltd., surface treated calcium carbonate (average particle size 0.03 μm)
* 6) Silica: manufactured by Tokuyama Co., Ltd., trade name Leoroseal QS-20 [hydrophilic silica]
* 7) Moisture absorbent: ethyl silicate * 8) Curing catalyst: Dibutyltin dilaurate * 9) Adhesive agent: Toray Dow Corning Silicone Co., Ltd., trade name SH6020 [γ- (2-aminoethyl) aminopropyltrimethoxy Silane]
* 10) PPG: manufactured by Mitsui Chemicals Polyurethanes Co., Ltd., trade name SHP-2550
成分（Ｃ）として用いたメタノール、イソプロピルアルコール、オクタノール、ノルマルヘキサン及びエチレングリコール、並びに比較例３〜５で用いたデカン、グリセリン及びＰＰＧの２３℃における粘度、誘電率、沸点及び分子量をそれぞれ表３に示した。 Table 3 shows the viscosity, dielectric constant, boiling point, and molecular weight of methanol, isopropyl alcohol, octanol, normal hexane, and ethylene glycol used as component (C), and decane, glycerin, and PPG used in Comparative Examples 3 to 5 at 23 ° C. It was shown to.
前記得られたそれぞれの室温湿気硬化型組成物を接着剤として使用し、下記性能評価を行った。結果を表４及び５に示す。 Each of the obtained room temperature moisture-curable compositions was used as an adhesive, and the following performance evaluation was performed. The results are shown in Tables 4 and 5.
１）難燃性
接着剤を、シリコーン離型紙間で１．５ｍｍのスペーサーを用いてシートを作製した。２０℃７日後、離型紙から剥がし、１．５×１３×１３０ｍｍの硬化シートを作製した。得られた硬化シートに対し、ＵＬ９４Ｖ−０規格に基づき試験を行い、難燃性を評価した。
具体的には以下の各項目を全て満たすものを合格、一つでも満たさないものを不合格とした。
ａ）各試料の残炎時間ｔ１またはｔ２が「１０秒以下」
ｂ）全ての処理による各組の残炎時間の合計（５枚の試料のｔ１＋ｔ２）が「５０秒以下」
ｃ）第２回接炎の各試料の残炎時間と残じん時間の合計（ｔ２＋ｔ３）が「３０秒以下」
ｄ）各試料の保持クランプまでの残炎または残じんが「無い事」
ｅ）発炎物質または滴下物による標識用綿の着火が「無い事」
ｔ１〜ｔ３は下記の通りである。
ｔ１：第１回接炎の試料の残炎時間（秒）
ｔ２：第２回接炎の試料の残炎時間（秒）
ｔ３：第２回接炎の試料の残じん時間（秒）
1) Flame retardance A sheet was prepared using an adhesive with a 1.5 mm spacer between silicone release papers. After 7 days at 20 ° C., the film was peeled off from the release paper to prepare a cured sheet of 1.5 × 13 × 130 mm. The obtained cured sheet was tested based on the UL94V-0 standard to evaluate flame retardancy.
Specifically, those that satisfy all the following items were accepted, and those that did not meet even one were rejected.
a) After flame time t1 or t2 of each sample is “10 seconds or less”
b) The total after flame time of each set by all treatments (t1 + t2 of 5 samples) is “50 seconds or less”
c) The total after flame time and residual time (t2 + t3) of each sample of the second flame contact is “30 seconds or less”
d) “No residual flame or dust” up to the holding clamp of each sample.
e) There shall be no ignition of the marking cotton by the flaming substance or dripping material.
t1 to t3 are as follows.
t1: Afterflame time of the first flame contact sample (seconds)
t2: Afterflame time of the second flame contact sample (seconds)
t3: Residual time of the second flame contact sample (seconds)
２）保存安定性
接着剤を１３５ｍＬラミネートチューブに充填し、５０℃で６０日間放置し、液状分のブリードアウトを観察した。
〈評価基準〉
○：チューブよりの吐出時にブリードアウトなし
×：チューブよりの吐出時にブリードアウトあり
2) Storage stability The adhesive was filled in a 135 mL laminated tube and left at 50 ° C. for 60 days, and bleed out of the liquid was observed.
<Evaluation criteria>
○: No bleed-out when discharging from the tube ×: Bleed-out when discharging from the tube
３）粘度及び貯蔵安定性
各接着剤を２３℃５０％ＲＨ環境下で２４時間放置した後、Ｂ型粘度計（東機産業製、ＢＨローター７番、回転速度２０ｒｐｍ、測定上限値２００ｐａ・ｓ）を使用し、粘度を測定した。その結果を初期粘度とした。その後、５０℃乾燥機中に３０日間放置した後、２３℃５０％ＲＨ環境下で２４時間放置し、液温が２３℃になるように調整し、同様に粘度測定を行った。望ましい粘度は、３０〜１５０ｐａ・ｓである。
貯蔵安定性は「５０℃３０日後の粘度／初期粘度」の値により下記の基準で評価した。
○：２未満、△：２以上３未満、×：３以上。
また、粘度が高く粘度計で測定不能だった場合を測定不能として示した。
3) Viscosity and storage stability Each adhesive was allowed to stand in an environment of 23 ° C. and 50% RH for 24 hours, and then a B-type viscometer (manufactured by Toki Sangyo Co., Ltd., BH rotor No. 7, rotation speed 20 rpm, measurement upper limit 200 pa · s ) Was used to measure the viscosity. The result was taken as the initial viscosity. Then, after leaving it in a 50 ° C. dryer for 30 days, it was left in an environment of 23 ° C. and 50% RH for 24 hours to adjust the liquid temperature to 23 ° C., and the viscosity was measured in the same manner. A desirable viscosity is 30 to 150 pa · s.
The storage stability was evaluated according to the following criteria based on the value of “viscosity after 30 days at 50 ° C./initial viscosity”.
○: Less than 2, Δ: 2 or more and less than 3, ×: 3 or more.
Moreover, the case where the viscosity was high and measurement with a viscometer was impossible was shown as impossible.
４）抵抗値の変化率
ポリスイッチ（タイコエレクトロニクスレイケム（株）製）の表面に接着剤３ｇを直接塗布し密封状態にて２３℃５０％ＲＨ環境下で２１日放置し、デジタルオームメータにて抵抗値を測定し、初期値からの抵抗値変化率を調べた。なお、ポリスイッチとは、２枚の金属電極箔で導電性ポリマーのシートを挟み込んだ構造を有する、ポリマー系のＰＴＣサーミスターである。
評価基準は下記の通りである。また、初期値とは接着剤を塗布する前のポリスイッチの抵抗値である。
○：初期値の±２０％以内、×：初期値の±２０％以外。
4) Change rate of resistance value 3g of adhesive was directly applied to the surface of PolySwitch (manufactured by Tyco Electronics Raychem Co., Ltd.) and left in a sealed state at 23 ° C and 50% RH for 21 days. The resistance value was measured, and the resistance value change rate from the initial value was examined. The polyswitch is a polymer PTC thermistor having a structure in which a conductive polymer sheet is sandwiched between two metal electrode foils.
The evaluation criteria are as follows. The initial value is the resistance value of the polyswitch before applying the adhesive.
○: Within ± 20% of initial value, ×: other than ± 20% of initial value.
５）作業性
カートリッジに前記接着剤を３３３ｍＬ充填し、２３℃５０％ＲＨ環境下で２４時間放置した後、エアーガン（ノズル直径３ｍｍ、エアー圧３ｋｇ／ｃｍ2）を使用して該接着剤を３３３ｍＬ吐出するのに要した時間を測定した。評価基準は下記の通りである。
◎：所要時間９０秒以下、○：所要時間９０秒を超えて１８０秒以下、×：１８０秒を超えても３３３ｍＬ吐出できなかったもの。
5) Workability The cartridge was filled with 333 mL of the above-mentioned adhesive and left in an environment of 23 ° C. and 50% RH for 24 hours, and then 333 mL of the adhesive was used using an air gun (nozzle diameter 3 mm, air pressure 3 kg / cm 2 ). The time required to discharge was measured. The evaluation criteria are as follows.
A: Required time of 90 seconds or less, O: Required time exceeding 90 seconds and 180 seconds or less, X: 333 mL could not be discharged even after exceeding 180 seconds.
６）接着強度
軟鋼板（１．６×２５×１００ｍｍ）に各接着剤を２５×２５ｍｍの接着面積で接着剤を２００μｍ厚に塗布し、オープンタイムを３分とって貼り合わせ、２３℃５０％ＲＨ環境下で７日養生し、引っ張り速さ５０ｍｍ／分で接着強さを測定した。
6) Adhesive strength Each adhesive was applied to a mild steel plate (1.6 × 25 × 100 mm) with a bonding area of 25 × 25 mm to a thickness of 200 μm, and bonded for 3 minutes at an open time of 23 ° C. and 50%. It was cured for 7 days under an RH environment, and the adhesive strength was measured at a pulling speed of 50 mm / min.
表４及び５の結果から明らかなように、実施例１〜１０は、接着強度等、接着剤として好適な優れた特性を有し、且つＵＬ９４Ｖ−０規格に合格し得る、著しい難燃性を示し、更にはポリスイッチの抵抗値に悪影響を与えることなく作業性にも優れ、保存安定性及び貯蔵安定性に優れていた。
As is clear from the results in Tables 4 and 5, Examples 1 to 10 have excellent flame retardancy that has excellent properties suitable as an adhesive, such as adhesive strength, and can pass the UL94V-0 standard. Furthermore, the workability was excellent without adversely affecting the resistance value of the polyswitch, and the storage stability and storage stability were excellent.
Claims (10)
（Ｂ）平均粒径０．１〜２００μｍの金属水酸化物、及び
（Ｃ）２３℃における粘度が５００ｍＰａ・ｓ以下である液状化合物であって、誘電率が５以上及び／又は沸点が１７０℃以下の液状化合物、
を必須成分として含有し、
前記液状化合物がアルコール類又はヘキサンであり、
前記金属水酸化物（Ｂ）が、前記重合体（Ａ）１００質量部に対して１５０質量部〜３５０質量部、
前記液状化合物（Ｃ）が、前記重合体（Ａ）１００質量部に対して１〜３０質量部、
配合されてなるポリマーＰＴＣ素子を含む電子製品の部品の接着用難燃性湿気硬化型接着剤組成物を用いてポリマーＰＴＣ素子を含む電子製品の部品を接着することを特徴とする接着方法。 (A) a reactive silicon group-containing organic polymer,
(B) a metal hydroxide having an average particle size of 0.1 to 200 μm, and (C) a liquid compound having a viscosity at 23 ° C. of 500 mPa · s or less, having a dielectric constant of 5 or more and / or a boiling point of 170 ° C. The following liquid compounds,
As an essential component,
The liquid compound Ri alcohol or hexane der,
The metal hydroxide (B) is 150 parts by mass to 350 parts by mass with respect to 100 parts by mass of the polymer (A).
The liquid compound (C) is 1 to 30 parts by mass with respect to 100 parts by mass of the polymer (A),
Bonding method characterized by bonding the components of electronic products, including polymer PTC element using an adhesive flame retardant moisture-curing adhesive composition of components of the electronic product comprising a polymer PTC element comprising blended.
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| WO2010035614A1 (en) * | 2008-09-26 | 2010-04-01 | 日本ゼオン株式会社 | Thermally conductive pressure-sensitive adhesive composition, thermally conductive pressure-sensitive adhesive sheet, and electronic component |
| JP5388121B2 (en) * | 2009-10-27 | 2014-01-15 | セメダイン株式会社 | Speaker assembly method |
| JPWO2011089987A1 (en) * | 2010-01-20 | 2013-05-23 | コニシ株式会社 | Flame retardant moisture curable resin composition, flame retardant moisture curable adhesive containing the composition, and bonding method using the adhesive |
| JP2011225695A (en) * | 2010-04-19 | 2011-11-10 | Three Bond Co Ltd | Fire-retardant moisture-curable resin composition |
| JP5823099B2 (en) * | 2010-06-16 | 2015-11-25 | セメダイン株式会社 | Flame retardant heat transfer curable composition |
| JP6427995B2 (en) * | 2013-07-16 | 2018-11-28 | セメダイン株式会社 | Curable composition |
| JP2014132100A (en) * | 2014-04-16 | 2014-07-17 | Cemedine Co Ltd | Method for producing flame-retardant heat-conductive curable composition excellent in storage stability |
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