JPH064728B2 - Self-extinguishing resin composition - Google Patents
Self-extinguishing resin compositionInfo
- Publication number
- JPH064728B2 JPH064728B2 JP59066534A JP6653484A JPH064728B2 JP H064728 B2 JPH064728 B2 JP H064728B2 JP 59066534 A JP59066534 A JP 59066534A JP 6653484 A JP6653484 A JP 6653484A JP H064728 B2 JPH064728 B2 JP H064728B2
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- Japan
- Prior art keywords
- resin
- brominated epoxy
- self
- resin composition
- epoxy resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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Description
【発明の詳細な説明】 〔発明の技術分野〕 本発明は，すぐれた難燃性を有する自消性樹脂組成物に
関するものである。Description: TECHNICAL FIELD OF THE INVENTION The present invention relates to a self-extinguishing resin composition having excellent flame retardancy.
従来，難燃性を有する熱可塑性樹脂組成物としては，例
えば特公昭５７−４６６５号公報や特公昭５７−１０８
９８号公報等が知られ，電線被覆材，シート，成形品等
として広く使用されている。Conventionally, as a flame-retardant thermoplastic resin composition, for example, Japanese Patent Publication No. 57-4665 and Japanese Patent Publication No. 57-108.
No. 98, etc. are known and are widely used as electric wire coating materials, sheets, molded products and the like.
しかし，このような従来の組成物から得られたシート，
成形品等は，燃焼試験で，難燃焼がまだ不十分なレベル
であり，完全に自消性とはならない欠点があった。However, sheets obtained from such conventional compositions,
In the combustion test, the molded products, etc. had a defect that the flame retardancy was still insufficient and they were not completely self-extinguishing.
本発明の目的は，上記欠点を解消せしめ，高度の難燃焼
を示し，米国のＵＬ規格Subgect94，等級Ｖ−０に合格
する自消性の樹脂組成物を提供せんとするものである。It is an object of the present invention to provide a self-extinguishing resin composition which overcomes the above-mentioned drawbacks, exhibits a high degree of flame retardancy, and passes the UL standard Subgect 94, grade V-0.
本発明は，上記目的を達成するため，次の構成すなわ
ち，エチレン系またはプロピレン系樹脂１００重量部
は，水酸化マグネシウムまたは水酸化アルミニウムより
なる充填剤を６０〜２５０重量部と，ビスフェノールＡ
系臭素化エポキシ樹脂の架橋物とを配合してなる自消性
樹脂組成物であって，かつ該ビスフェノールＡ系臭素化
エポキシ樹脂の架橋物の量が該自消性樹脂組成物に対し
て２〜１０重量％含有されてなる自消性樹脂組成物を特
徴とするものである。In order to achieve the above object, the present invention has the following constitution: 100 parts by weight of ethylene or propylene resin, 60 to 250 parts by weight of filler made of magnesium hydroxide or aluminum hydroxide, and bisphenol A.
A self-extinguishing resin composition comprising a cross-linked product of a system-based brominated epoxy resin, wherein the amount of the cross-linked product of the bisphenol A-based brominated epoxy resin is 2 with respect to the composition. It is characterized by a self-extinguishing resin composition containing 10 to 10% by weight.
本発明におけるエチレン系またはプロピレン系樹脂は、
周知のエチレン系またはプロピレン系樹脂で、具体的に
は、ポリエチレン、ポリプロピレン、等のホモポリマ
ー、エチレン−酢酸ビニル共重合体、エチレン−プロピ
レン共重合体等の共重合体、あるいはこれらの混合物よ
りなる。Ethylene-based or propylene-based resin in the present invention,
A well-known ethylene-based or propylene-based resin, specifically, a homopolymer such as polyethylene or polypropylene, a copolymer such as an ethylene-vinyl acetate copolymer, an ethylene-propylene copolymer, or a mixture thereof. .
これらのエチレン系またはプロピレン系樹脂は必要に応
じて相互にブレンドして用いることも可能である。These ethylene-based or propylene-based resins may be blended with each other if necessary.
本発明における水酸化マグネシウムまたは水酸化アルミ
ニウムよりなる充填剤とは，分子中に結合水あるいは熱
分解して水分を発生することのでるき水酸基を含有する
化合物であることが必要条件であり，具体的な例とし
て，水酸化マグネシウム，水酸化アルミニウム，両者の
混合物、またはこれらにその他の水酸化無機化合物や結
晶水含有無機化合物、例えば、塩基性炭酸マグネシウム
等が添加されたもの等が挙げられる。The filler composed of magnesium hydroxide or aluminum hydroxide in the present invention is a necessary condition that it is a compound containing a bound hydroxyl group in the molecule which can generate bound water or thermal decomposition to generate water. Specific examples thereof include magnesium hydroxide, aluminum hydroxide, a mixture of both, or a compound obtained by adding other inorganic compound such as hydroxide inorganic compound or water of crystallization, for example, basic magnesium carbonate.
これらの水酸化マグネシウムまたは水酸化アルミニウム
よりなる充填剤の粒径は，成形時のフィルター目詰ま
り，分散性の点から，一般に0.01〜５０μ，好ましくは
0.1〜２０μのものが好ましい。また，これらの水酸化
マグネシウムまたは水酸化アルミニウムよりなる充填剤
は，樹脂との混合に先立ち，高級脂肪酸，高級脂肪酸
塩，シランカップリング剤，チタネート系表面処理剤，
難燃助剤等でコーティング処理されたものを用いるのが
望ましく，特にこれらの少なくとも１種で表面処理され
た水酸化マグネシウムおよび，もしくは水酸化アルミニ
ウムを用いるのが望ましい。The particle size of the filler made of magnesium hydroxide or aluminum hydroxide is generally 0.01 to 50 μ, preferably from the viewpoint of filter clogging during molding and dispersibility.
It is preferably 0.1 to 20 μm. In addition, these fillers made of magnesium hydroxide or aluminum hydroxide, prior to mixing with the resin, higher fatty acid, higher fatty acid salt, silane coupling agent, titanate surface treatment agent,
It is desirable to use those which have been coated with a flame retardant aid or the like, and it is particularly desirable to use magnesium hydroxide and / or aluminum hydroxide whose surface is treated with at least one of these.
本発明におけるビスフェノールＡ系臭素化エポキシ樹脂
とは，テトノラプロムビスフェノールＡのジグリシジル
エーテル（式１）またはこれを主体とする臭素化エポキ
シ樹脂（式２）がある。Examples of the bisphenol A-based brominated epoxy resin in the present invention include a diglycidyl ether of Tetonoraprom bisphenol A (formula 1) or a brominated epoxy resin mainly composed of this (formula 2).
（式１） （式２） 通常，これらのビスフェノールＡ系臭素化エポキシ樹脂
は，臭素含有率が１６〜６０重量％，エポキシ当量が２
００〜３０００，分子量が６５６〜６０００のものが使
用できる。(Equation 1) (Formula 2) Usually, these bisphenol A-based brominated epoxy resins have a bromine content of 16 to 60% by weight and an epoxy equivalent of 2
Those having a molecular weight of 00 to 3000 and a molecular weight of 656 to 6000 can be used.
これらの中でも，エポキシ当量の大きいもの，例えば，
エポキシ当量が８００以上のもの，さらに好ましくは１
２００以上のものより得た架橋物が，シート成形時のプ
リードアウトが少なく，ベース樹脂との混練性が良くな
る点から望ましい。Among these, those with a large epoxy equivalent, for example,
Epoxy equivalent of 800 or more, more preferably 1
A crosslinked product obtained from a resin having a viscosity of 200 or more is desirable because it has less bleed-out during sheet molding and improves kneading properties with the base resin.
ビスフェノールＡ系臭素化エポキシ樹脂の具体的な市販
品として，住友化学工業(株)製“スミエポキシ”ＥＳＢ
−３４０，４００，５００，７００やダウ・ケミカル社
製“ＤＥＲ−５１１，５４２”等，シエル化学社製“１
０４５−Ｂ−８０”、ＤＸ−２４８−Ｂ−８０”等，さ
らに，坂本薬品工業（株）製“ＳＲ−ＴＢＡ−３５０，
４００”等がある。"Sumiepoxy" ESB manufactured by Sumitomo Chemical Co., Ltd. as a specific commercial product of bisphenol A-based brominated epoxy resin
-340,400,500,700 and "DER-511,542" manufactured by Dow Chemical Company, "1 manufactured by Ciel Chemical Company"
045-B-80 ″, DX-248-B-80 ″, etc., and “SR-TBA-350” manufactured by Sakamoto Yakuhin Kogyo Co., Ltd.
400 "etc.
なお，シート成形性，難燃剤のブリードアウトの点から
は，上述の臭素化エポキシ樹脂をプレポリマー化したも
のを架橋物として用いる必要がある。From the standpoints of sheet formability and bleed-out of flame retardant, it is necessary to use a prepolymerized brominated epoxy resin as a crosslinked product.
本発明でいうビスフェノールＡ系臭素化エポキシ樹脂架
橋物とは，ビスフェノールＡ系臭素化エポキシ樹脂単独
もしくは臭素含有率の異なるものを２種以上混合したも
の，あるいはこれらの臭素化エポキシ樹脂に周知のエポ
キシ樹脂用硬化剤で三次元架橋させて不溶・不融とした
ものである。The term "bisphenol A-based brominated epoxy resin cross-linked product" as used in the present invention means a bisphenol A-based brominated epoxy resin alone or a mixture of two or more kinds having different bromine contents, or a well-known epoxy for these brominated epoxy resins. It is insoluble and infusible by three-dimensional crosslinking with a resin curing agent.
ただし，上述の架橋物を難燃剤として，本発明のポリオ
レフィン系樹脂に含有せしめる場合，該臭素化エポキシ
樹脂の架橋物中に，一部，未架橋物，例えば，プレポリ
マーを含有していてもさしつかえない。However, when the above-mentioned crosslinked product is contained in the polyolefin resin of the present invention as a flame retardant, even if a part of the crosslinked product of the brominated epoxy resin contains an uncrosslinked product, for example, a prepolymer. I don't care.
さらに，臭素化エポキシ樹脂架橋物にプレポリマーおよ
び，モノマーを混合して用いることも可能である。Further, it is also possible to use a mixture of a brominated epoxy resin crosslinked product with a prepolymer and a monomer.
上記臭素化エポキシ樹脂の三次元架橋に必要な硬化剤と
しては，一般のエポキシ樹脂用の硬化剤であれば何でも
よく，具体例としては，エチレンジアミン，ジエチレン
トリアミン，トリエチレンテトラミン，メタフエニレン
ジアミン，４，４′−ジアミノジフエニルメタン，４，
４′−ジアミノジフエニルスルホン，三弗化ホウ素モノ
エチルアミン錯体等のアミン触媒，無水マレイン酸，無
水フタル酸，無水メチルハイミック酸等の酸無水物触
媒，その他ジシアンジアミド，イミダゾール，ポリアミ
ド樹脂等がある。特に三弗化ホウ素モノエチルアミン錯
体は好ましい硬化剤である。The curing agent required for three-dimensional crosslinking of the brominated epoxy resin may be any curing agent for general epoxy resins, and specific examples include ethylenediamine, diethylenetriamine, triethylenetetramine, metaphenylenediamine, 4 , 4'-diaminodiphenylmethane, 4,
There are amine catalysts such as 4'-diaminodiphenyl sulfone, boron trifluoride monoethylamine complex, etc., acid anhydride catalysts such as maleic anhydride, phthalic anhydride, methylhymic anhydride, etc., and other dicyandiamide, imidazole, polyamide resin, etc. . In particular, boron trifluoride monoethylamine complex is a preferred curing agent.
本発明の樹脂組成物は，上記したとおり，水酸化マグネ
シウムまたは水酸化アルミニウムよりなる充填剤ととも
に，ビスフェノールＡ系臭素化エポキシ樹脂の架橋物を
配合したものであるが，該樹脂組成物中にビスフェノー
ルＡ系臭素化エポキシ樹脂の架橋物中の臭素が２〜１０
重量％，好ましくは２〜８重量％含有させることが必要
である。As described above, the resin composition of the present invention contains a cross-linked product of a bisphenol A-based brominated epoxy resin together with a filler made of magnesium hydroxide or aluminum hydroxide. Bromine in the crosslinked product of the A-based brominated epoxy resin is 2 to 10
It is necessary that the content be wt%, preferably 2 to 8 wt%.
これが２重量％未満では，難燃性が不十分となり好まし
くない。一方，１０重量％を超えると成形品表面への臭
素化エポキシ樹脂の架橋物のブリードアウトおよび燃焼
時の発煙がひどくなるので好ましくない。If it is less than 2% by weight, the flame retardance is insufficient, which is not preferable. On the other hand, if it exceeds 10% by weight, bleeding out of the cross-linked product of the brominated epoxy resin on the surface of the molded article and smoke generation during combustion become severe, which is not preferable.
なお，本発明の樹脂組成物は，上記成分以外に本発明の
目的をそこなわない範囲であれば三酸化アンチモン等の
難燃助剤，他種難燃剤，熱安定剤，紫外線吸収剤，可塑
剤，滑剤，顔料，帯電防止剤，分散剤等の添加剤を配合
することができる。In addition to the above components, the resin composition of the present invention is a flame retardant aid such as antimony trioxide, other flame retardants, heat stabilizers, ultraviolet absorbers, plasticizers, etc., as long as the object of the present invention is not impaired. Additives such as agents, lubricants, pigments, antistatic agents, and dispersants can be added.
次に，本発明の樹脂組成物の製造方法の一例について説
明する。まず，上記のエチレン系またはプロピレン系樹
脂に水酸化マグネシウムまたは水酸化アルミニウムより
なる充填剤とビスフェノールＡ系臭素化エポキシ樹脂の
架橋物を所定の量配合し、溶融混練する。この混練法
は，あらかじめ，マスターバッチを製造して後，混合し
ても良いし，一度に溶融混練してもよい。Next, an example of the method for producing the resin composition of the present invention will be described. First, a predetermined amount of a filler made of magnesium hydroxide or aluminum hydroxide and a cross-linked product of a bisphenol A-based brominated epoxy resin is mixed with the above ethylene-based or propylene-based resin, and melt-kneaded. In this kneading method, the masterbatch may be manufactured in advance and then mixed, or the melt kneading may be performed all at once.
なお，混練装置は，周知のもの，すなわち，バンバリミ
キサー，加圧式ニーダー，ロールミキシング，一軸押出
機，二軸押出機等適当なものを用いることができる。As the kneading device, a known device such as Banbury mixer, pressure kneader, roll mixing, single-screw extruder, twin-screw extruder can be used.
こうして溶融混練して得られた組成物は，通常押出機に
よってペレットの形状に加工され，成形用樹脂（通常密
度1.0g／cc以上）として提供される。The composition thus obtained by melt-kneading is usually processed into pellets by an extruder and provided as a molding resin (usually having a density of 1.0 g / cc or more).
上述のペレットは，一般的には直径２〜６mm，長さ３〜
１０mm程度の円柱形状で利用されることが多いが，これ
ら限定されない。The above pellets generally have a diameter of 2 to 6 mm and a length of 3 to
It is often used in a cylindrical shape of about 10 mm, but is not limited to these.
本発明の組成物から得たシート成形品を電子線照射して
架橋させることもできる。The sheet molded article obtained from the composition of the present invention can be irradiated with an electron beam to be crosslinked.
また，本発明の組成物中に化学架橋剤を配合して成形
後，加熱架橋させることもできる。Further, a chemical crosslinking agent may be added to the composition of the present invention, and the composition may be molded and then heat-crosslinked.
本発明の組成物は，電線被覆材のような電気絶縁材料や
フィルム，シート類，さらにラジオやテレビ等のキャビ
ネットその他電気機器等の成形材料，建材，内装材，自
動車部品のような難燃用材料等，高度の難燃性が要求さ
れる分野で広く利用できる。INDUSTRIAL APPLICABILITY The composition of the present invention is used for electric insulation materials such as electric wire coating materials, films, sheets, and molding materials for cabinets such as radios and televisions and other electric devices, building materials, interior materials, flame retardants such as automobile parts. It can be widely used in fields such as materials where high flame retardancy is required.
本発明の組成物は，難燃剤として臭素化エポキシ樹脂の
架橋物を用いることにより，燃焼時に，他の難燃剤では
得られなかったポリマの炭化促進作用を示す結果，ドリ
ップ現象が起らない特徴を有する。さらに，水酸化マグ
ネシウムまたは水酸化アルミニウムよりなる充填剤との
併用により，可燃性のエチレン系またはプロピレン系樹
脂を完全に自消性となし、かつ燃焼時の発煙も少ないも
のとなる特徴があるため，高度の難燃性が必要とされる
部材用として極めて有用である。The composition of the present invention uses a cross-linked product of a brominated epoxy resin as a flame retardant, and exhibits a carbonization-promoting action of a polymer which cannot be obtained by other flame retardants at the time of combustion, resulting in no drip phenomenon. Have. In addition, when used in combination with a filler made of magnesium hydroxide or aluminum hydroxide, it has the characteristics that the flammable ethylene-based or propylene-based resin is completely self-extinguishing and emits less smoke during combustion. , It is extremely useful for parts that require high flame retardancy.
なお、本発明の測定値は次の測定法による。 The measured value of the present invention is based on the following measuring method.
(1)臭素含有率：プレスシートから切りだした小片を精
秤する。この試料をフラスコ燃焼法で分解し，その吸収
液を銀電極を用いて硝酸銀溶液で電位滴定する。この滴
定曲線より臭素量を求めて含有量（重量％）を算出し
た。(1) Bromine content: A small piece cut from a press sheet is precisely weighed. This sample is decomposed by the flask combustion method, and the absorption liquid is subjected to potentiometric titration with a silver nitrate solution using a silver electrode. The bromine content was calculated from this titration curve to calculate the content (% by weight).
(2)難燃性：米国のＵＬ規格，Subgect94の方法に準じて
測定した。(2) Flame retardancy: Measured according to the method of US UL standard, Subgect 94.
以下，実施例に基づいて本発明の一実施態様を説明す
る。An embodiment of the present invention will be described below based on examples.
実施例１〜２，比較例１〜８ エチレン系またはプロピレン系樹脂として，低密度ポリ
エチレン（ＬＤＰＥ），エチレン一酢ビ共重合体（ＥＶ
Ａ）（酢ビ含有２６％）、ポリプロピレン（ＰＰ）を１
００重量部に対し水酸化マグネシウムまたは水酸化アル
ミニウムよりなる充填剤として，水酸化マグネシウム
（Mg(OH)2）を、難燃剤としてビスフェノールＡ系臭素
化エポキシ樹脂の架橋物（ＴＢＡ−４００，１２００，
１５００）およびそのプレポリマ（ＴＢＡ−４００−Ｐ
−１），デカブロモジフェニルエーテル（ＤＢＥ）を各
々表１に示した割合でブレンドし，加圧式ニーダーを使
って１４０〜１５０゜Cで溶融混練したものを１５０×１
５０角，厚さ3.2mmのシートをプレス成形した。このシ
ートから長さ１２７mm，幅１２．７mmの試験片を切り出
して難燃性を評価した。Examples 1-2 and Comparative Examples 1-8 As ethylene-based or propylene-based resins, low density polyethylene (LDPE), ethylene-vinyl acetate copolymer (EV
A) (26% vinyl acetate content), polypropylene (PP) 1
Magnesium hydroxide (Mg (OH) 2 ) is used as a filler composed of magnesium hydroxide or aluminum hydroxide per 100 parts by weight, and a cross-linked product of bisphenol A-based brominated epoxy resin (TBA-400, 1200,
1500) and its prepolymer (TBA-400-P
-1) and decabromodiphenyl ether (DBE) were blended in the proportions shown in Table 1 and melt-kneaded at 140 to 150 ° C using a pressure kneader to obtain 150 x 1
A 50-mm square sheet having a thickness of 3.2 mm was press-molded. A test piece having a length of 127 mm and a width of 12.7 mm was cut out from this sheet to evaluate the flame retardancy.
実施例１〜２はいずれも本発明の要件をすべて満たして
いるため，難燃性に優れ，すべてＶ−０であった。Since all of Examples 1 and 2 satisfied all the requirements of the present invention, they were excellent in flame retardancy and were all V-0.
一方，比較例１〜３はいずれも水酸化マグネシウムまた
は水酸化アルミニウムよりなる充填剤の添加量が少なく
本発明の要件を満たしていないため，比較例４，５はビ
スフェノールＡ系臭素化エポキシ樹脂の架橋物が含まれ
ていないため，いずれも難燃性の評価結果が実施例に比
べて劣っておりＶ−１，Ｖ−２のレベルであった。On the other hand, in Comparative Examples 1 to 3, since the addition amount of the filler made of magnesium hydroxide or aluminum hydroxide is small and does not satisfy the requirements of the present invention, Comparative Examples 4 and 5 are bisphenol A-based brominated epoxy resins. Since the crosslinked product was not contained, the flame retardancy evaluation results were inferior to those of the examples, and the levels were V-1 and V-2.
なお、比較例６、７、８は、ビスフェノールＡ系臭素化
エポキシ樹脂がプレポリマーであるので、ＵＬ９４垂直
試験では、確かにＶ−０の評価を得ているものの、ドリ
ップ現象が認められるので、十分な難燃性を有するもの
ではない。In Comparative Examples 6, 7, and 8, since the bisphenol A-based brominated epoxy resin is a prepolymer, the UL94 vertical test certainly gives V-0, but the drip phenomenon is recognized. It does not have sufficient flame retardancy.
Claims (1)
重量部に、水酸化マグネシウムまたは水酸化アルミニウ
ムよりなる充填剤を６０〜２５０重量部と、ビスフェノ
ールＡ系臭素化エポキシ樹脂の架橋物を配合してなる自
消性樹脂組成物であって、かつ該ビスフェノールＡ系臭
素化エポキシ樹脂の架橋物の量が該自消性樹脂組成物に
対して２〜１０重量％含有されてなる自消性樹脂組成
物。1. An ethylene-based or propylene-based resin 100
A self-extinguishing resin composition comprising 60 parts by weight to 250 parts by weight of a filler made of magnesium hydroxide or aluminum hydroxide, and a cross-linked product of a bisphenol A-based brominated epoxy resin. A self-extinguishing resin composition comprising a cross-linked product of a bisphenol A-based brominated epoxy resin in an amount of 2 to 10% by weight based on the self-extinguishing resin composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59066534A JPH064728B2 (en) | 1984-04-03 | 1984-04-03 | Self-extinguishing resin composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59066534A JPH064728B2 (en) | 1984-04-03 | 1984-04-03 | Self-extinguishing resin composition |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60210665A JPS60210665A (en) | 1985-10-23 |
| JPH064728B2 true JPH064728B2 (en) | 1994-01-19 |
Family
ID=13318651
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59066534A Expired - Lifetime JPH064728B2 (en) | 1984-04-03 | 1984-04-03 | Self-extinguishing resin composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH064728B2 (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07103273B2 (en) * | 1987-02-02 | 1995-11-08 | 三菱化学株式会社 | Self-extinguishing polymer composition |
| JP2738104B2 (en) * | 1990-01-31 | 1998-04-08 | 大日本インキ化学工業株式会社 | Flame retardant masterbatch |
| CN102276791B (en) * | 2011-07-08 | 2013-02-27 | 绵阳惠利电子材料有限公司 | Flame-retardant epoxy resin compound |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57115432A (en) * | 1981-01-08 | 1982-07-17 | Furukawa Electric Co Ltd:The | Highly-inorganic-filled foam of high expansion ratio and its manufacutre |
-
1984
- 1984-04-03 JP JP59066534A patent/JPH064728B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60210665A (en) | 1985-10-23 |
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