JP7421307B2 - Composition for power transmission belts - Google Patents
Composition for power transmission belts Download PDFInfo
- Publication number
- JP7421307B2 JP7421307B2 JP2019197196A JP2019197196A JP7421307B2 JP 7421307 B2 JP7421307 B2 JP 7421307B2 JP 2019197196 A JP2019197196 A JP 2019197196A JP 2019197196 A JP2019197196 A JP 2019197196A JP 7421307 B2 JP7421307 B2 JP 7421307B2
- Authority
- JP
- Japan
- Prior art keywords
- composition
- ethylene
- power transmission
- olefin
- parts
- 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.)
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- 230000005540 biological transmission Effects 0.000 title claims description 43
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Description
本発明は、伝動ベルト用組成物に関する。 The present invention relates to a composition for power transmission belts.
伝動ベルトは、自動車用、自動二輪用および一般産業機械用に広く用いられている。伝動ベルトには、高ゴム弾性および耐摩耗性が必要とされている。前記性質を満たす伝動ベルトを製造するため、クロロプレンゴムが通常用いられている。ここで、耐熱性や耐寒性の改良、および軽量化の要求から、クロロプレンゴムにかえてエチレン・プロピレン・非共役ポリエン共重合体ゴムを用いることが検討されている(例えば、特許文献1~2参照)。 Transmission belts are widely used for automobiles, motorcycles, and general industrial machinery. Transmission belts are required to have high rubber elasticity and wear resistance. Chloroprene rubber is commonly used to manufacture power transmission belts that meet the above properties. Here, in order to improve heat resistance and cold resistance, and to reduce weight, the use of ethylene/propylene/non-conjugated polyene copolymer rubber instead of chloroprene rubber is being considered (for example, Patent Documents 1 to 2). reference).
本発明者らの検討によれば、エチレン・プロピレン・非共役ポリエン共重合体を用いた場合は、当該共重合体を含有する伝動ベルト用組成物から形成されたシート間の粘着力(タック)が不足し、したがって成形加工が困難となる傾向にある。本発明の課題は、粘着力が高く、したがって成形加工性に優れた伝動ベルト用組成物を提供することにある。 According to studies by the present inventors, when an ethylene-propylene-nonconjugated polyene copolymer is used, the adhesive force (tack) between sheets formed from a power transmission belt composition containing the copolymer There is a tendency for the molding process to become difficult. An object of the present invention is to provide a composition for power transmission belts that has high adhesive strength and therefore excellent moldability.
本発明者らは、前記課題を解決すべく鋭意検討を行ったところ、下記構成の伝動ベルト用組成物により前記課題を解決できることを見出し、本発明を完成するに至った。すなわち本発明は、例えば以下の[1]~[9]に関する。 The inventors of the present invention conducted extensive studies to solve the above-mentioned problems, and found that the above-mentioned problems could be solved by a composition for power transmission belts having the following structure, and thus completed the present invention. That is, the present invention relates to, for example, the following [1] to [9].
[1]エチレン[A1]に由来する構造単位と、炭素数4~20のα-オレフィン[A2]に由来する構造単位と、非共役ポリエン[A3]に由来する構造単位とを有し、下記(1)~(3)の要件を満たすエチレン・α-オレフィン・非共役ポリエン共重合体(A)100質量部と、カーボンブラック(B)0.1~200質量部とを含有する伝動ベルト用組成物。
(1)エチレン[A1]に由来する構造単位と、炭素数4~20のα-オレフィン[A2]に由来する構造単位とのモル比〔[A1]/[A2]〕が、40/60~90/10であり、
(2)非共役ポリエン[A3]に由来する構造単位の含有割合が、[A1]、[A2]および[A3]に由来する構造単位の合計を100モル%として、0.1~6.0モル%であり、
(3)下記式(i)で表されるB値が、1.20以上である。
B値=([EX]+2[Y])/〔2×[E]×([X]+[Y])〕・・・(i)
[ここで[E]、[X]および[Y]は、それぞれ、エチレン[A1]、炭素数4~20のα-オレフィン[A2]、および非共役ポリエン[A3]に由来する構造単位のモル分率を示し、[EX]はエチレン[A1]-炭素数4~20のα-オレフィン[A2]ダイアッド連鎖分率を示す。]
[2]前記共重合体(A)における炭素数4~20のα-オレフィン[A2]に由来する構造単位が、1-ブテンに由来する構造単位を含む前記[1]に記載の伝動ベルト用組成物。
[3]短繊維(C)をさらに含有し、前記短繊維(C)の含有量が、前記共重合体(A)100質量部に対して0.1~100質量部である前記[1]または[2]に記載の伝動ベルト用組成物。
[4]前記短繊維(C)が、アラミド繊維である前記[3]に記載の伝動ベルト用組成物。
[5]前記エチレン・α-オレフィン・非共役ポリエン共重合体(A)が、下記(4)の要件をさらに満たす前記[1]~[4]のいずれかに記載の伝動ベルト用組成物。
(4)100℃におけるムーニー粘度ML(1+4)100℃が、5~150である。
[6]2つ以上のエチレン性二重結合を有する架橋助剤をさらに含有する前記[1]~[5]のいずれかに記載の伝動ベルト用組成物。
[7]前記[1]~[6]のいずれかに記載の伝動ベルト用組成物から形成された成形体。
[8]前記[1]~[6]のいずれかに記載の伝動ベルト用組成物から形成された架橋成形体。
[9]前記[7]に記載の成形体または前記[8]に記載の架橋成形体を有する伝動ベルト。
[1] It has a structural unit derived from ethylene [A1], a structural unit derived from an α-olefin having 4 to 20 carbon atoms [A2], and a structural unit derived from a non-conjugated polyene [A3], and has the following: For power transmission belts containing 100 parts by mass of an ethylene/α-olefin/non-conjugated polyene copolymer (A) that satisfies requirements (1) to (3) and 0.1 to 200 parts by mass of carbon black (B) Composition.
(1) The molar ratio [[A1]/[A2]] of the structural unit derived from ethylene [A1] and the structural unit derived from α-olefin [A2] having 4 to 20 carbon atoms is 40/60 to 90/10,
(2) The content ratio of structural units derived from non-conjugated polyene [A3] is 0.1 to 6.0, assuming that the total of structural units derived from [A1], [A2] and [A3] is 100 mol%. is mole%,
(3) The B value represented by the following formula (i) is 1.20 or more.
B value = ([EX]+2[Y])/[2×[E]×([X]+[Y])]...(i)
[Here, [E], [X] and [Y] are moles of structural units derived from ethylene [A1], α-olefin having 4 to 20 carbon atoms [A2], and non-conjugated polyene [A3], respectively. [EX] indicates the ethylene [A1]-α-olefin [A2] dyad chain fraction having 4 to 20 carbon atoms. ]
[2] The power transmission belt according to [1] above, wherein the structural unit derived from the α-olefin [A2] having 4 to 20 carbon atoms in the copolymer (A) includes a structural unit derived from 1-butene. Composition.
[3] The above [1], further containing short fibers (C), wherein the content of the short fibers (C) is 0.1 to 100 parts by mass based on 100 parts by mass of the copolymer (A). Or the composition for power transmission belts according to [2].
[4] The composition for a power transmission belt according to [3] above, wherein the short fibers (C) are aramid fibers.
[5] The composition for a power transmission belt according to any one of [1] to [4], wherein the ethylene/α-olefin/nonconjugated polyene copolymer (A) further satisfies the following requirement (4).
(4) Mooney viscosity ML (1+4) at 100°C is 5 to 150.
[6] The composition for a power transmission belt according to any one of [1] to [5] above, further containing a crosslinking aid having two or more ethylenic double bonds.
[7] A molded article formed from the composition for a power transmission belt according to any one of [1] to [6] above.
[8] A crosslinked molded article formed from the composition for power transmission belts according to any one of [1] to [6] above.
[9] A power transmission belt comprising the molded article according to [7] or the crosslinked molded article according to [8].
本発明によれば、粘着力が高く、したがって成形加工性に優れた伝動ベルト用組成物を提供することができる。 According to the present invention, it is possible to provide a composition for a power transmission belt that has high adhesive strength and therefore excellent moldability.
本発明について詳細に説明する。
[伝動ベルト用組成物]
本発明の伝動ベルト用組成物(以下「本発明の組成物」ともいう)は、以下に説明するエチレン・α-オレフィン・非共役ポリエン共重合体(A)と、カーボンブラック(B)とを含有する。本発明の組成物は、短繊維(C)をさらに含有することが好ましい。
The present invention will be explained in detail.
[Composition for power transmission belt]
The power transmission belt composition of the present invention (hereinafter also referred to as "composition of the present invention") comprises an ethylene/α-olefin/non-conjugated polyene copolymer (A) and carbon black (B), which will be explained below. contains. It is preferable that the composition of the present invention further contains short fibers (C).
<エチレン・α-オレフィン・非共役ポリエン共重合体(A)>
エチレン・α-オレフィン・非共役ポリエン共重合体(A)は、エチレン[A1]に由来する構造単位と、炭素数4~20のα-オレフィン[A2]に由来する構造単位と、非共役ポリエン[A3]に由来する構造単位とを有し、下記(1)~(3)の要件を満たす。以下、前記(A)を「成分(A)」ともいう。成分(A)は、一実施態様において、後述する要件(4)または(4')を満たすことが好ましい。
<Ethylene/α-olefin/non-conjugated polyene copolymer (A)>
The ethylene/α-olefin/non-conjugated polyene copolymer (A) consists of a structural unit derived from ethylene [A1], a structural unit derived from an α-olefin having 4 to 20 carbon atoms [A2], and a non-conjugated polyene. It has a structural unit derived from [A3] and satisfies the following requirements (1) to (3). Hereinafter, the above (A) will also be referred to as "component (A)". In one embodiment, component (A) preferably satisfies requirement (4) or (4') described below.
なお、成分(A)は、エチレン[A1]に由来する構造単位と、少なくとも1種類の炭素数4~20のα-オレフィン[A2]に由来する構造単位と、少なくとも1種類の非共役ポリエン[A3]に由来する構造単位とを有することができる。
(1)エチレン[A1]に由来する構造単位と、炭素数4~20のα-オレフィン[A2]に由来する構造単位とのモル比〔[A1]/[A2]〕が、40/60~90/10である。
(2)非共役ポリエン[A3]に由来する構造単位の含有割合が、[A1]、[A2]および[A3]に由来する構造単位の合計を100モル%として、0.1~6.0モル%である。
(3)下記式(i)で表されるB値が、1.20以上である。
B値=([EX]+2[Y])/〔2×[E]×([X]+[Y])〕・・(i)
ここで[E]、[X]および[Y]は、それぞれ、エチレン[A1]、炭素数4~20のα-オレフィン[A2]、および非共役ポリエン[A3]に由来する構造単位のモル分率を示し、[EX]はエチレン[A1]-炭素数4~20のα-オレフィン[A2]ダイアッド連鎖分率を示す。
In addition, component (A) contains a structural unit derived from ethylene [A1], a structural unit derived from at least one type of α-olefin having 4 to 20 carbon atoms [A2], and at least one type of non-conjugated polyene [ A3].
(1) The molar ratio [[A1]/[A2]] of the structural unit derived from ethylene [A1] and the structural unit derived from α-olefin [A2] having 4 to 20 carbon atoms is 40/60 to It's 90/10.
(2) The content ratio of structural units derived from non-conjugated polyene [A3] is 0.1 to 6.0, assuming that the total of structural units derived from [A1], [A2] and [A3] is 100 mol%. It is mole%.
(3) The B value represented by the following formula (i) is 1.20 or more.
B value = ([EX]+2[Y])/[2×[E]×([X]+[Y])]...(i)
Here, [E], [X] and [Y] are the mole fraction of structural units derived from ethylene [A1], α-olefin having 4 to 20 carbon atoms [A2], and non-conjugated polyene [A3], respectively. [EX] indicates the ethylene [A1]-α-olefin [A2] dyad chain fraction having 4 to 20 carbon atoms.
炭素数4~20のα-オレフィン[A2]としては、例えば、1-ブテン、1-ペンテン、1-ヘキセン、1-ヘプテン、1-オクテン、1-ノネン、1-デセン、1-ノナデセン、1-エイコセン等の直鎖状α-オレフィン;4-メチル-1-ペンテン、9-メチル-1-デセン、11-メチル-1-ドデセン、12-エチル-1-テトラデセン等の側鎖含有α-オレフィンが挙げられる。これらの中でも、炭素数4~10のα-オレフィンが好ましく、1-ブテン、1-ヘキセン、1-オクテンがより好ましく、1-ブテンがさらに好ましい。 Examples of the α-olefin [A2] having 4 to 20 carbon atoms include 1-butene, 1-pentene, 1-hexene, 1-heptene, 1-octene, 1-nonene, 1-decene, 1-nonadecene, 1 -Linear α-olefins such as eicosene; α-olefins containing side chains such as 4-methyl-1-pentene, 9-methyl-1-decene, 11-methyl-1-dodecene, and 12-ethyl-1-tetradecene can be mentioned. Among these, α-olefins having 4 to 10 carbon atoms are preferred, 1-butene, 1-hexene, and 1-octene are more preferred, and 1-butene is even more preferred.
炭素数4~20のα-オレフィン[A2]は単独で、または2種以上組み合わせて用いることができる。
α-オレフィンがプロピレンであるエチレン・プロピレン・非共役ポリエン共重合体は、得られる組成物同士の粘着力が低く、したがって当該組成物の、成形体および架橋成形体(以下、これらをあわせて「(架橋)成形体」ともいう)への成形性が低い傾向にある。また、この共重合体は、短繊維(C)との混練性も低い傾向にある。
The α-olefin [A2] having 4 to 20 carbon atoms can be used alone or in combination of two or more.
Ethylene-propylene-nonconjugated polyene copolymers in which the α-olefin is propylene have low adhesion between the resulting compositions, and therefore molded products and crosslinked molded products (hereinafter collectively referred to as " (also referred to as a "crosslinked) molded product" tends to have low moldability. Furthermore, this copolymer tends to have low kneading properties with short fibers (C).
一方、本発明では、ゴム成分として成分(A)を少なくとも用いる。成分(A)は、炭素数4~20のα-オレフィン[A2]に由来する構造単位を有しているので、得られる組成物同士の粘着力が高くなったと推察され、したがって当該組成物の、(架橋)成形体、特に伝動ベルトへの成形性が高い。また、成分(A)は、短繊維(C)との混練性にも優れている。 On the other hand, in the present invention, at least component (A) is used as a rubber component. Since component (A) has a structural unit derived from α-olefin [A2] having 4 to 20 carbon atoms, it is presumed that the adhesive strength between the resulting compositions is increased, and therefore the composition has a higher adhesive strength. , has high moldability into (crosslinked) molded bodies, especially power transmission belts. In addition, component (A) also has excellent kneading properties with short fibers (C).
非共役ポリエン[A3]としては、例えば、1,4-ヘキサジエン、1,6-オクタジエン、2-メチル-1,5-ヘキサジエン、6-メチル-1,5-ヘプタジエン、7-メチル-1,6-オクタジエン等の鎖状非共役ジエン;シクロヘキサジエン、ジシクロペンタジエン、メチルテトラヒドロインデン、5-ビニル-2-ノルボルネン、5-エチリデン-2-ノルボルネン、5-メチレン-2-ノルボルネン、5-イソプロピリデン-2-ノルボルネン、6-クロロメチル-5-イソプロペニル-2-ノルボルネン等の環状非共役ジエン;2,3-ジイソプロピリデン-5-ノルボルネン、2-エチリデン-3-イソプロピリデン-5-ノルボルネン、2-プロペニル-2,5-ノルボルナジエン、1,3,7-オクタトリエン、1,4,9-デカトリエン、4,8-ジメチル-1,4,8-デカトリエン、4-エチリデン-8-メチル-1,7-ノナジエン等のトリエンが挙げられる。これらの中でも、1,4-ヘキサジエン等の鎖状非共役ジエン、5-エチリデン-2-ノルボルネン、5-ビニル-2-ノルボルネン等の環状非共役ジエンが好ましく、環状非共役ジエンがより好ましく、5-エチリデン-2-ノルボルネン、5-ビニル-2-ノルボルネンがさらに好ましい。 Examples of the non-conjugated polyene [A3] include 1,4-hexadiene, 1,6-octadiene, 2-methyl-1,5-hexadiene, 6-methyl-1,5-heptadiene, 7-methyl-1,6 - Chain nonconjugated dienes such as octadiene; cyclohexadiene, dicyclopentadiene, methyltetrahydroindene, 5-vinyl-2-norbornene, 5-ethylidene-2-norbornene, 5-methylene-2-norbornene, 5-isopropylidene- Cyclic non-conjugated dienes such as 2-norbornene, 6-chloromethyl-5-isopropenyl-2-norbornene; 2,3-diisopropylidene-5-norbornene, 2-ethylidene-3-isopropylidene-5-norbornene, 2 -propenyl-2,5-norbornadiene, 1,3,7-octatriene, 1,4,9-decatriene, 4,8-dimethyl-1,4,8-decatriene, 4-ethylidene-8-methyl-1, Examples include trienes such as 7-nonadiene. Among these, linear non-conjugated dienes such as 1,4-hexadiene, cyclic non-conjugated dienes such as 5-ethylidene-2-norbornene and 5-vinyl-2-norbornene are preferred, and cyclic non-conjugated dienes are more preferred; -ethylidene-2-norbornene and 5-vinyl-2-norbornene are more preferred.
非共役ポリエン[A3]は単独で、または2種以上を組み合わせて用いることができる。
成分(A)としては、例えば、エチレン・1-ブテン・1,4-ヘキサジエン共重合体、エチレン・1-ペンテン・1,4-ヘキサジエン共重合体、エチレン・1-ヘキセン・1,4-ヘキサジエン共重合体、エチレン・1-へプテン・1,4-ヘキサジエン共重合体、エチレン・1-オクテン・1,4-ヘキサジエン共重合体、エチレン・1-ノネン・1,4-ヘキサジエン共重合体、エチレン・1-デセン・1,4-ヘキサジエン共重合体、エチレン・1-ブテン・1-オクテン・1,4-ヘキサジエン共重合体、エチレン・1-ブテン・5-エチリデン-2-ノルボルネン共重合体、エチレン・1-ペンテン・5-エチリデン-2-ノルボルネン共重合体、エチレン・1-ヘキセン・5-エチリデン-2-ノルボルネン共重合体、エチレン・1-へプテン・5-エチリデン-2-ノルボルネン共重合体、エチレン・1-オクテン・5-エチリデン-2-ノルボルネン共重合体、エチレン・1-ノネン・5-エチリデン-2-ノルボルネン共重合体、エチレン・1-デセン・5-エチリデン-2-ノルボルネン共重合体、エチレン・1-ブテン・1-オクテン・5-エチリデン-2-ノルボルネン共重合体、エチレン・1-ブテン・5-エチリデン-2-ノルボルネン・5-ビニル-2-ノルボルネン共重合体、エチレン・1-ペンテン・5-エチリデン-2-ノルボルネン・5-ビニル-2-ノルボルネン共重合体、エチレン・1-ヘキセン・5-エチリデン-2-ノルボルネン・5-ビニル-2-ノルボルネン共重合体、エチレン・1-へプテン・5-エチリデン-2-ノルボルネン・5-ビニル-2-ノルボルネン共重合体、エチレン・1-オクテン・5-エチリデン-2-ノルボルネン・5-ビニル-2-ノルボルネン共重合体、エチレン・1-ノネン・5-エチリデン-2-ノルボルネン・5-ビニル-2-ノルボルネン共重合体、エチレン・1-デセン・5-エチリデン-2-ノルボルネン・5-ビニル-2-ノルボルネン共重合体、エチレン・1-ブテン・1-オクテン・5-エチリデン-2-ノルボルネン・5-ビニル-2-ノルボルネン共重合体が挙げられる。
Non-conjugated polyene [A3] can be used alone or in combination of two or more types.
As component (A), for example, ethylene/1-butene/1,4-hexadiene copolymer, ethylene/1-pentene/1,4-hexadiene copolymer, ethylene/1-hexene/1,4-hexadiene copolymer, ethylene/1-heptene/1,4-hexadiene copolymer, ethylene/1-octene/1,4-hexadiene copolymer, ethylene/1-nonene/1,4-hexadiene copolymer, Ethylene/1-decene/1,4-hexadiene copolymer, ethylene/1-butene/1-octene/1,4-hexadiene copolymer, ethylene/1-butene/5-ethylidene-2-norbornene copolymer , ethylene/1-pentene/5-ethylidene-2-norbornene copolymer, ethylene/1-hexene/5-ethylidene-2-norbornene copolymer, ethylene/1-heptene/5-ethylidene-2-norbornene copolymer Polymer, ethylene/1-octene/5-ethylidene-2-norbornene copolymer, ethylene/1-nonene/5-ethylidene-2-norbornene copolymer, ethylene/1-decene/5-ethylidene-2-norbornene Copolymer, ethylene/1-butene/1-octene/5-ethylidene-2-norbornene copolymer, ethylene/1-butene/5-ethylidene-2-norbornene/5-vinyl-2-norbornene copolymer, Ethylene/1-pentene/5-ethylidene-2-norbornene/5-vinyl-2-norbornene copolymer, ethylene/1-hexene/5-ethylidene-2-norbornene/5-vinyl-2-norbornene copolymer, Ethylene/1-heptene/5-ethylidene-2-norbornene/5-vinyl-2-norbornene copolymer, ethylene/1-octene/5-ethylidene-2-norbornene/5-vinyl-2-norbornene copolymer , ethylene/1-nonene/5-ethylidene-2-norbornene/5-vinyl-2-norbornene copolymer, ethylene/1-decene/5-ethylidene-2-norbornene/5-vinyl-2-norbornene copolymer , ethylene/1-butene/1-octene/5-ethylidene-2-norbornene/5-vinyl-2-norbornene copolymer.
《要件(1)》
成分(A)は、(1)エチレン[A1]に由来する構造単位と、炭素数4~20のα-オレフィン[A2]に由来する構造単位とのモル比〔[A1]/[A2]〕が、40/60~90/10である。モル比が前記範囲にある成分(A)は、低温でのゴム弾性と常温での引張強度とのバランスに優れる。
《Requirement (1)》
Component (A) consists of (1) a molar ratio of structural units derived from ethylene [A1] and structural units derived from α-olefin [A2] having 4 to 20 carbon atoms [[A1]/[A2]]; is 40/60 to 90/10. Component (A) having a molar ratio within the above range has an excellent balance between rubber elasticity at low temperatures and tensile strength at room temperature.
[A1]/[A2]の下限は、好ましくは45/55、より好ましくは50/50、特に好ましくは55/45である。また、[A1]/[A2]の上限は、好ましくは80/20、より好ましくは75/25、さらに好ましくは70/30である。 The lower limit of [A1]/[A2] is preferably 45/55, more preferably 50/50, particularly preferably 55/45. Further, the upper limit of [A1]/[A2] is preferably 80/20, more preferably 75/25, and even more preferably 70/30.
《要件(2)》
成分(A)は、(2)非共役ポリエン[A3]に由来する構造単位の含有割合が、前記[A1]に由来する構造単位、前記[A2]に由来する構造単位および前記[A3]に由来する構造単位の合計を100モル%として、0.1~6.0モル%である。この含有割合が前記範囲にある成分(A)は、充分な架橋性および柔軟性を有する。
《Requirement (2)》
Component (A) has a content ratio of structural units derived from (2) non-conjugated polyene [A3], structural units derived from said [A1], structural units derived from said [A2], and said [A3]. It is 0.1 to 6.0 mol%, assuming the total derived structural units as 100 mol%. Component (A) whose content is within the above range has sufficient crosslinkability and flexibility.
前記[A3]に由来する構造単位の含有割合の下限は、好ましくは0.5モル%である。前記[A3]に由来する構造単位の含有割合の上限は、好ましくは4.0モル%、より好ましくは3.5モル%、さらに好ましくは3.0モル%である。 The lower limit of the content of the structural unit derived from [A3] is preferably 0.5 mol%. The upper limit of the content of the structural unit derived from [A3] is preferably 4.0 mol%, more preferably 3.5 mol%, and even more preferably 3.0 mol%.
《要件(3)》
成分(A)は、(3)前記式(i)で表されるB値が、1.20以上、好ましくは1.20~1.80、より好ましくは1.22~1.40である。
《Requirement (3)》
Component (A) has (3) a B value expressed by the above formula (i) of 1.20 or more, preferably 1.20 to 1.80, more preferably 1.22 to 1.40.
B値が1.20未満のエチレン・α-オレフィン・非共役ポリエン共重合体は、低温での圧縮永久ひずみが大きくなり、低温でのゴム弾性と常温での引張強度とのバランスに優れないおそれがある。B値が1.20以上である成分(A)は、共重合体を構成するモノマー単位の交互性が高く結晶性が低いため、得られる組成物の加工性が向上する。 Ethylene/α-olefin/non-conjugated polyene copolymers with a B value of less than 1.20 have a large compression set at low temperatures and may not have an excellent balance between rubber elasticity at low temperatures and tensile strength at room temperature. There is. Component (A) having a B value of 1.20 or more has high alternation of monomer units constituting the copolymer and low crystallinity, so that the processability of the resulting composition is improved.
なお、B値は、共重合体中における共重合モノマー連鎖分布のランダム性を示す指標であり、前記式(i)中の[E]、[X]、[Y]、[EX]は、13C-NMRスペクトルを測定し、J. C.Randall [Macromolecules, 15, 353 (1982)]、J. Ray [Macromolecules, 10, 773 (1977)]らの報告に基づいて求めることができる。一方、前記(1)~(2)における、エチレン[A1]に由来する構造単位、炭素数4~20のα-オレフィン[A2]に由来する構造単位および非共役ポリエン[A3]に由来する構造単位のモル量は、1H-NMRスペクトルメーターによる強度測定によって求めることができる。 The B value is an index indicating the randomness of the copolymerized monomer chain distribution in the copolymer, and [E], [X], [Y], and [EX] in the formula (i) are as follows: 13 It can be determined by measuring a C-NMR spectrum and based on the reports of JCRandall [Macromolecules, 15, 353 (1982)], J. Ray [Macromolecules, 10, 773 (1977)], etc. On the other hand, in (1) to (2) above, a structural unit derived from ethylene [A1], a structural unit derived from an α-olefin having 4 to 20 carbon atoms [A2], and a structure derived from a non-conjugated polyene [A3] The molar amount of the unit can be determined by intensity measurement using a 1 H-NMR spectrometer.
《要件(4)》
成分(A)は、(4)100℃におけるムーニー粘度ML(1+4)100℃が、好ましくは5~150、より好ましくは5~100、さらに好ましくは5~50である。ムーニー粘度が前記範囲にある成分(A)は、加工性および流動性が良好であり、また良好な後処理品質(リボンハンドリング性)を示すと共に優れたゴム物性を有する。
《Requirement (4)》
Component (A) has (4) a Mooney viscosity ML (1+4) at 100°C of preferably 5 to 150, more preferably 5 to 100, even more preferably 5 to 50. Component (A) having a Mooney viscosity within the above range has good processability and fluidity, exhibits good post-processing quality (ribbon handling properties), and has excellent rubber physical properties.
《要件(4')》
成分(A)は、(4')125℃におけるムーニー粘度ML(1+4)125℃が、好ましくは3~100、より好ましくは3~70、さらに好ましくは3~30である。ムーニー粘度が前記範囲にある成分(A)は、加工性および流動性が良好であり、また良好な後処理品質(リボンハンドリング性)を示すと共に優れたゴム物性を有する。
《Requirement (4')》
Component (A) has a (4') Mooney viscosity ML (1+4) at 125°C of preferably 3 to 100, more preferably 3 to 70, even more preferably 3 to 30. Component (A) having a Mooney viscosity within the above range has good processability and fluidity, exhibits good post-processing quality (ribbon handling properties), and has excellent rubber physical properties.
本発明の組成物は、1種の成分(A)を含有してもよく、2種以上の成分(A)を含有してもよい。
本発明の組成物中の成分(A)の含有割合は、通常は20質量%以上、好ましくは30~90質量%である。
The composition of the present invention may contain one type of component (A), or may contain two or more types of components (A).
The content of component (A) in the composition of the present invention is usually 20% by mass or more, preferably 30 to 90% by mass.
《成分(A)の製造方法》
成分(A)は、メタロセン触媒を用いた従来公知の製造方法で得ることができる。メタロセン触媒および当該触媒を用いた製造方法としては、例えば、国際公開第2015/122415号、特に当該公報の段落[0249]~[0320]に記載の例を採用することができる。
《Production method of component (A)》
Component (A) can be obtained by a conventionally known production method using a metallocene catalyst. As the metallocene catalyst and the production method using the catalyst, for example, the examples described in International Publication No. 2015/122415, particularly paragraphs [0249] to [0320] of the publication can be adopted.
具体的には、
下記式(a)で表される遷移金属化合物(a)と、
有機金属化合物(b-1)、有機アルミニウムオキシ化合物(b-2)、および遷移金属化合物(a)と反応してイオン対を形成する化合物(b-3)から選ばれる少なくとも1種の化合物(b)と
を含むオレフィン重合用触媒の存在下において、エチレン[A1]と炭素数4~20のα-オレフィン[A2]と非共役ポリエン[A3]とを共重合することにより、成分(A)を得ることができる。
in particular,
A transition metal compound (a) represented by the following formula (a),
At least one compound selected from the organometallic compound (b-1), the organoaluminumoxy compound (b-2), and the compound (b-3) that reacts with the transition metal compound (a) to form an ion pair ( By copolymerizing ethylene [A1], an α-olefin having 4 to 20 carbon atoms [A2], and a non-conjugated polyene [A3] in the presence of an olefin polymerization catalyst containing b), component (A) can be obtained.
上記式(a)について説明する。
Mは、チタン原子、ジルコニウム原子またはハフニウム原子である。
Rは、それぞれ独立に、アリール基の水素原子の一つ以上をハメット則の置換基定数σが-0.2以下の電子供与性基で置換してなる置換アリール基である。前記置換アリール基が電子供与性基を複数個有する場合、それぞれの電子供与性基は同一でも異なっていてもよい。
The above formula (a) will be explained.
M is a titanium atom, a zirconium atom or a hafnium atom.
R's are each independently a substituted aryl group in which one or more hydrogen atoms of the aryl group are substituted with an electron-donating group having a Hammett's substituent constant σ of −0.2 or less. When the substituted aryl group has a plurality of electron donating groups, each electron donating group may be the same or different.
Qは、ハロゲン原子、炭素数1~20の炭化水素基、アニオン配位子および孤立電子対で配位可能な中性配位子から同一のまたは異なる組合せで選ばれ、好ましくはハロゲン原子である。 Q is selected from the same or different combinations from a halogen atom, a hydrocarbon group having 1 to 20 carbon atoms, an anionic ligand, and a neutral ligand capable of coordinating with a lone pair of electrons, and is preferably a halogen atom. .
jは、1~4の整数であり、好ましくは2である。
Rにおけるアリール基としては、例えば、フェニル基、1-ナフチル基、2-ナフチル基、アントラセニル基、フェナントレニル基、テトラセニル基、クリセニル基、ピレニル基、インデニル基、アズレニル基、ピロリル基、ピリジル基、フラニル基、チオフェニル基が挙げられ、フェニル基が好ましい。
j is an integer from 1 to 4, preferably 2.
Examples of the aryl group in R include phenyl group, 1-naphthyl group, 2-naphthyl group, anthracenyl group, phenanthrenyl group, tetracenyl group, chrysenyl group, pyrenyl group, indenyl group, azulenyl group, pyrrolyl group, pyridyl group, furanyl group. and thiophenyl group, with phenyl group being preferred.
ハメット則の置換基定数σが-0.2以下の電子供与性基は、以下のように定義および例示される。ハメット則はベンゼン誘導体の反応または平衡に及ぼす置換基の影響を定量的に論ずるために1935年L. P. Hammettにより提唱された経験則であるが、これは今日広く妥当性が認められている。ハメット則で求められた置換基定数にはベンゼン環のパラ位に置換した際のσpおよびメタ位に置換した際のσmがあり、これらの値は多くの一般的な文献に見出すことができる。例えば、HanschおよびTaftによる文献[Chem. Rev., 91, 165 (1991)]には非常に広範な置換基について詳細な記載がなされている。ただし、これらの文献に記載されているσpおよびσmは、同じ置換基であっても文献によって値が僅かに異なる場合がある。本明細書ではこのような状況によって生じる混乱を回避するために、記載のある限りの置換基においてはHanschおよびTaftによる文献[Chem. Rev., 91, 165 (1991)]のTable 1(168-175頁)に記載された値をハメット則の置換基定数σpおよびσmと定義する。本明細書においてハメット則の置換基定数σが-0.2以下の電子供与性基とは、電子供与性基がフェニル基のパラ位(4位)に置換している場合はσpが-0.2以下の電子供与性基であり、フェニル基のメタ位(3位)に置換している場合はσmが-0.2以下の電子供与性基である。また、電子供与性基がフェニル基のオルト位(2位)に置換している場合、またはフェニル基以外のアリール基の任意の位置に置換している場合は、σpが-0.2以下の電子供与性基である。 Electron-donating groups having a substituent constant σ of Hammett's rule of -0.2 or less are defined and exemplified as follows. Hammett's rule is an empirical rule proposed by L. P. Hammett in 1935 to quantitatively discuss the influence of substituents on the reaction or equilibrium of benzene derivatives, and its validity is widely recognized today. The substituent constants determined by Hammett's rule include σp when substituted at the para position of the benzene ring and σm when substituted at the meta position, and these values can be found in many general literature. For example, the article by Hansch and Taft [Chem. Rev., 91, 165 (1991)] provides a detailed description of a very wide range of substituents. However, the values of σp and σm described in these documents may differ slightly depending on the document even if the substituents are the same. In order to avoid confusion caused by such a situation, in this specification, as far as the substituents are mentioned, Table 1 (168-1) of the literature by Hansch and Taft [Chem. The values described on page 175 are defined as the substituent constants σp and σm of Hammett's rule. In this specification, an electron-donating group with Hammett's substituent constant σ of -0.2 or less means that when the electron-donating group is substituted at the para-position (4-position) of a phenyl group, σp is -0. It is an electron-donating group with a value of .2 or less, and when it is substituted at the meta-position (3-position) of a phenyl group, it is an electron-donating group with a σm of -0.2 or less. In addition, if the electron donating group is substituted at the ortho position (2nd position) of the phenyl group or at any position of the aryl group other than the phenyl group, σp is −0.2 or less. It is an electron donating group.
ハメット則の置換基定数σpまたはσmが-0.2以下の電子供与性基としては、例えば、p-アミノ基(4-アミノ基)、p-ジメチルアミノ基(4-ジメチルアミノ基)、p-ジエチルアミノ基(4-ジエチルアミノ基)、m-ジエチルアミノ基(3-ジエチルアミノ基)等の窒素含有基;p-メトキシ基(4-メトキシ基)、p-エトキシ基(4-エトキシ基)等の酸素含有基;p-t-ブチル基(4-t-ブチル基)等の三級炭化水素基;p-トリメチルシロキシ基(4-トリメチルシロキシ基)等のケイ素含有基が挙げられる。 Examples of electron-donating groups with Hammett's substituent constant σp or σm of -0.2 or less include p-amino group (4-amino group), p-dimethylamino group (4-dimethylamino group), p-dimethylamino group (4-dimethylamino group), - Nitrogen-containing groups such as diethylamino group (4-diethylamino group) and m-diethylamino group (3-diethylamino group); oxygen such as p-methoxy group (4-methoxy group) and p-ethoxy group (4-ethoxy group) Containing groups; tertiary hydrocarbon groups such as pt-butyl group (4-t-butyl group); silicon-containing groups such as p-trimethylsiloxy group (4-trimethylsiloxy group).
Rは、それぞれ独立に、前記電子供与性基としての窒素含有基および酸素含有基から選ばれる基を含む置換フェニル基であることが好ましい。
前記置換アリール基は、ハメット則の置換基定数σが-0.2以下の電子供与性基以外の、炭素数1~20の炭化水素基、ケイ素含有基、窒素含有基、酸素含有基、ハロゲン原子およびハロゲン含有基から選ばれる他の置換基を有していてもよい。前記置換アリール基が他の置換基を複数個有する場合、それぞれの他の置換基は同一でも異なっていてもよい。
It is preferable that each R is independently a substituted phenyl group containing a group selected from a nitrogen-containing group and an oxygen-containing group as the electron-donating group.
The substituted aryl group is a hydrocarbon group having 1 to 20 carbon atoms, a silicon-containing group, a nitrogen-containing group, an oxygen-containing group, or a halogen group, other than an electron-donating group having a Hammett's substituent constant σ of -0.2 or less. It may also have other substituents selected from atoms and halogen-containing groups. When the substituted aryl group has a plurality of other substituents, each of the other substituents may be the same or different.
一つの置換アリール基に含まれるハメット則の置換基定数σが-0.2以下の電子供与性基および他の置換基の各々のハメット則の置換基定数σの総和は-0.15以下であることが好ましい。このような置換アリール基としては、例えば、m,p-ジメトキシフェニル基(3,4-ジメトキシフェニル基)、p-(ジメチルアミノ)-m-メトキシフェニル基(4-(ジメチルアミノ)-3-メトキシフェニル基)、p-(ジメチルアミノ)-m-メチルフェニル基(4-(ジメチルアミノ)-3-メチルフェニル基)、p-メトキシ-m-メチルフェニル基(4-メトキシ-3-メチルフェニル基)、p-メトキシ-m,m-ジメチルフェニル基(4-メトキシ-3,5-ジメチルフェニル基)が挙げられる。 The sum of the Hammett's rule substituent constants σ of each of the electron-donating groups and other substituents whose Hammett's rule substituent constant σ is −0.2 or less contained in one substituted aryl group is −0.15 or less. It is preferable that there be. Examples of such substituted aryl groups include m,p-dimethoxyphenyl group (3,4-dimethoxyphenyl group), p-(dimethylamino)-m-methoxyphenyl group (4-(dimethylamino)-3- methoxyphenyl group), p-(dimethylamino)-m-methylphenyl group (4-(dimethylamino)-3-methylphenyl group), p-methoxy-m-methylphenyl group (4-methoxy-3-methylphenyl group) p-methoxy-m,m-dimethylphenyl group (4-methoxy-3,5-dimethylphenyl group).
Qにおいて、ハロゲン原子としては、フッ素、塩素、臭素、ヨウ素が例示され;炭素数1~20の炭化水素基としては、炭素数1~10のアルキル基、炭素数3~10のシクロアルキル基が例示され;アニオン配位子としては、アルコキシ基、アリーロキシ基、カルボキシレート基、スルホネート基が例示され;孤立電子対で配位可能な中性配位子としては、トリメチルホスフィン、トリエチルホスフィン、トリフェニルホスフィン、ジフェニルメチルホスフィン等の有機リン化合物、テトラヒドロフラン、ジエチルエーテル、ジオキサン、1,2-ジメトキシエタン等のエーテル化合物が例示される。 In Q, examples of the halogen atom include fluorine, chlorine, bromine, and iodine; examples of the hydrocarbon group having 1 to 20 carbon atoms include an alkyl group having 1 to 10 carbon atoms, and a cycloalkyl group having 3 to 10 carbon atoms. Examples of anionic ligands include alkoxy groups, aryloxy groups, carboxylate groups, and sulfonate groups; examples of neutral ligands that can coordinate with lone pairs include trimethylphosphine, triethylphosphine, and triphenyl Examples include organic phosphorus compounds such as phosphine and diphenylmethylphosphine, and ether compounds such as tetrahydrofuran, diethyl ether, dioxane, and 1,2-dimethoxyethane.
遷移金属化合物(a)としては、例えば、[ビス(4-メトキシフェニル)メチレン(η5-シクロペンタジエニル)(η5-2,3,6,7-テトラメチルフルオレニル)]ハフニウムジクロリドが挙げられる。 Examples of the transition metal compound (a) include [bis(4-methoxyphenyl)methylene(η 5 -cyclopentadienyl)(η 5 -2,3,6,7-tetramethylfluorenyl)]hafnium dichloride. can be mentioned.
有機金属化合物(b-1)(ただし、有機アルミニウムオキシ化合物(b-2)を除く)としては、例えば、トリメチルアルミニウム、トリエチルアルミニウム、トリイソブチルアルミニウム、トリn-オクチルアルミニウム等のトリアルキルアルミニウム、トリシクロアルキルアルミニウム、イソブチルアルミニウムジクロリド、ジエチルアルミニウムクロリド、エチルアルミニウムジクロリド、エチルアルミニウムセスキクロリド、メチルアルミニウムジクロリド、ジメチルアルミニウムクロリド、ジイソブチルアルミニウムハイドライドなどの有機アルミニウム化合物が挙げられる。 Examples of the organometallic compound (b-1) (excluding the organoaluminumoxy compound (b-2)) include trialkylaluminum such as trimethylaluminum, triethylaluminum, triisobutylaluminum, and tri-n-octylaluminum; Examples include organoaluminum compounds such as cycloalkylaluminum, isobutylaluminum dichloride, diethylaluminium chloride, ethylaluminum dichloride, ethylaluminum sesquichloride, methylaluminum dichloride, dimethylaluminum chloride, and diisobutylaluminum hydride.
有機アルミニウムオキシ化合物(b-2)としては、例えば、従来公知のアルミノキサンが挙げられる。
遷移金属化合物(a)と反応してイオン対を形成する化合物(b-3)としては、例えば、特表平1-501950号公報、特表平1-502036号公報、特開平3-179005号公報、特開平3-179006号公報、特開平3-207703号公報、特開平3-207704号公報、USP-5321106号、国際公開第2015/122415号などに記載されたルイス酸、イオン性化合物、ボラン化合物およびカルボラン化合物が挙げられる。
Examples of the organoaluminumoxy compound (b-2) include conventionally known aluminoxane.
Examples of the compound (b-3) that reacts with the transition metal compound (a) to form an ion pair include those disclosed in Japanese Patent Publication No. 1-501950, Japanese Patent Publication No. 1-502036, and Japanese Patent Application Laid-open No. 3-179005. Lewis acids, ionic compounds described in publications, JP-A-3-179006, JP-A-3-207703, JP-A-3-207704, USP-5321106, International Publication No. 2015/122415, etc. Examples include borane compounds and carborane compounds.
オレフィン重合用触媒は、必要に応じて担体(c)を含むことができる。担体(c)は、無機化合物または有機化合物であって、顆粒状ないしは微粒子状の固体である。このうち無機化合物としては、多孔質酸化物、無機ハロゲン化物、粘土、粘土鉱物またはイオン交換性層状化合物が好ましい。 The olefin polymerization catalyst may contain a carrier (c) if necessary. The carrier (c) is an inorganic compound or an organic compound, and is a granular or particulate solid. Among these, preferred inorganic compounds are porous oxides, inorganic halides, clays, clay minerals, and ion exchange layered compounds.
重合方法としては、溶液(溶解)重合、懸濁重合等の液相重合法または気相重合法のいずれにおいても実施可能である。重合温度は、通常は-50~+200℃、好ましくは0~200℃である。重合圧力は、通常は常圧~10MPaゲージ圧、好ましくは常圧~5MPaゲージ圧である。重合反応は、回分式、半連続式、連続式のいずれの方法においても行うことができる。さらに重合を反応条件の異なる2段以上に分けて行うことも可能である。 As the polymerization method, any of liquid phase polymerization methods such as solution (dissolution) polymerization and suspension polymerization, or gas phase polymerization methods can be used. The polymerization temperature is usually -50 to +200°C, preferably 0 to 200°C. The polymerization pressure is usually normal pressure to 10 MPa gauge pressure, preferably normal pressure to 5 MPa gauge pressure. The polymerization reaction can be carried out in any of the batch, semi-continuous and continuous methods. Furthermore, it is also possible to carry out the polymerization in two or more stages with different reaction conditions.
<カーボンブラック(B)>
カーボンブラック(B)は、例えば、得られる(架橋)成形体の機械的強度、モジュラス、耐摩耗性の向上に寄与する成分である。
<Carbon black (B)>
Carbon black (B) is, for example, a component that contributes to improving the mechanical strength, modulus, and abrasion resistance of the obtained (crosslinked) molded product.
カーボンブラック(B)としては、例えば、SRF、GPF、FEF、MAF、HAF、ISAF、SAF、FT、MTが挙げられる。カーボンブラックの表面はシランカップリング剤で処理されていてもよい。市販されているカーボンブラックとしては、例えば、「旭#55G」、「旭#50HG」、「旭#60G」、「旭#60UG」(商品名、旭カーボン社製)、「シーストV」、「シーストSO」(商品名、東海カーボン社製)が挙げられる。 Examples of carbon black (B) include SRF, GPF, FEF, MAF, HAF, ISAF, SAF, FT, and MT. The surface of carbon black may be treated with a silane coupling agent. Commercially available carbon blacks include, for example, "Asahi #55G", "Asahi #50HG", "Asahi #60G", "Asahi #60UG" (trade name, manufactured by Asahi Carbon Co., Ltd.), "Seest V", " SEAST SO" (trade name, manufactured by Tokai Carbon Co., Ltd.).
本発明の組成物は、1種のカーボンブラック(B)を含有してもよく、2種以上のカーボンブラック(B)を含有してもよい。
本発明の組成物におけるカーボンブラック(B)の含有量は、成分(A)100質量部に対して、0.1~200質量部であり、好ましくは10~200質量部、より好ましくは20~100質量部である。このような態様であると、得られる(架橋)成形体の機械的強度と、本発明の組成物の加工性との観点から好ましい。
The composition of the present invention may contain one type of carbon black (B), or may contain two or more types of carbon black (B).
The content of carbon black (B) in the composition of the present invention is 0.1 to 200 parts by weight, preferably 10 to 200 parts by weight, more preferably 20 to 200 parts by weight, based on 100 parts by weight of component (A). It is 100 parts by mass. Such an embodiment is preferable from the viewpoints of the mechanical strength of the (crosslinked) molded product obtained and the processability of the composition of the present invention.
<短繊維(C)>
本発明の組成物は、短繊維(C)をさらに含有することが好ましい。短繊維(C)を用いることにより、前記組成物から形成される(架橋)成形体のモジュラス、機械的強度を改善することができる。成分(A)は短繊維(C)との混練性にも優れているので、本発明の組成物は、短繊維(C)を含有したとしても、成形加工性に優れる傾向にある。
<Short fiber (C)>
It is preferable that the composition of the present invention further contains short fibers (C). By using short fibers (C), the modulus and mechanical strength of the (crosslinked) molded article formed from the composition can be improved. Since component (A) also has excellent kneadability with short fibers (C), the composition of the present invention tends to have excellent moldability even if it contains short fibers (C).
短繊維(C)としては、例えば、ポリアミド、ポリイミド、ポリエステル、ポリビニルアルコール、レーヨン、ポリオレフィン、ポリアリレート、ポリフェニレンサルファイド、ポリエーテルエーテルケトン、ポリパラフェニレンベンゾビスオキサゾール、フッ素系ポリマー等の合成樹脂からなる繊維;綿、木材セルロース繊維等の天然繊維が挙げられる。これらの中でも、合成樹脂からなる短繊維が好ましく、ポリアミドからなる短繊維がより好ましい。短繊維(C)は、通常、成分(A)から形成された短繊維ではない。 The short fibers (C) are made of synthetic resins such as polyamide, polyimide, polyester, polyvinyl alcohol, rayon, polyolefin, polyarylate, polyphenylene sulfide, polyetheretherketone, polyparaphenylenebenzobisoxazole, and fluorine-based polymers. Fibers: Natural fibers such as cotton and wood cellulose fibers can be mentioned. Among these, short fibers made of synthetic resin are preferred, and short fibers made of polyamide are more preferred. Short fibers (C) are usually not short fibers formed from component (A).
ポリアミドとしては、例えば、ポリカプラミド、ポリ-ω-アミノヘプタン酸、ポリ-ω-アミノノナン酸、ポリウンデカンアミド、ポリエチレンジアミンアジパミド、ポリテトラメチレンアジパミド、ポリヘキサメチレンアジパミド、ポリヘキサメチレンセバカミド、ポリヘキサメチレンドデカミド、ポリオクタメチレンアジパミド、ポリデカメチレンアジパミド等の脂肪族ポリアミド;ポリパラフェニレンテレフタラミド(商品名「ケブラー」、東レ・デュポン社製)、ポリメタフェニレンイソフタラミド、コポリパラフェニレン-3,4'-オキシジフェニレンテレフタラミド、ポリメタキシリレンアジパミド、ポリメタキシリレンピメラミド、ポリメタキシリレンアゼラミド、ポリパラキシリレンアゼラミド、ポリパラキシリレンデカナミド等の芳香族ポリアミド(アラミド)が挙げられる。 Examples of the polyamide include polycapramide, poly-ω-aminoheptanoic acid, poly-ω-aminononanoic acid, polyundecaneamide, polyethylenediamine adipamide, polytetramethylene adipamide, polyhexamethylene adipamide, and polyhexamethylene. Aliphatic polyamides such as sebaamide, polyhexamethylene dodecamide, polyoctamethylene adipamide, and polydecamethylene adipamide; polyparaphenylene terephthalamide (trade name "Kevlar", manufactured by DuPont-Toray), poly Metaphenylene isophthalamide, copolyparaphenylene-3,4'-oxydiphenyleneterephthalamide, polymethaxylylene adipamide, polymethaxylylene pimeramide, polymethaxylylene azeramide, polyparaxylylene azeramide, poly Examples include aromatic polyamides (aramids) such as paraxylylene decanamide.
短繊維(C)としては、得られる(架橋)成形体の引張応力および引裂強さをより向上させるという観点から、芳香族ポリアミドからなる短繊維、すなわちアラミド短繊維が好ましく、ポリパラフェニレンテレフタラミド短繊維、ポリメタフェニレンイソフタラミド短繊維、コポリパラフェニレン-3,4'-オキシジフェニレンテレフタラミド短繊維がより好ましい。 The short fibers (C) are preferably short fibers made of aromatic polyamide, that is, aramid short fibers, from the viewpoint of further improving the tensile stress and tear strength of the resulting (crosslinked) molded product, and polyparaphenylene terephthalate is preferable. More preferred are lamid staple fibers, polymetaphenylene isophthalamide staple fibers, and copolyparaphenylene-3,4'-oxydiphenylene terephthalamide staple fibers.
短繊維(C)の平均繊維長は、通常は0.1~50mm、好ましくは0.5~10mm、より好ましくは0.5~6mmである。短繊維(C)の繊維径は、通常は0.1~100μm、好ましくは0.1~25μm、より好ましくは1~20μmである。 The average fiber length of the short fibers (C) is usually 0.1 to 50 mm, preferably 0.5 to 10 mm, and more preferably 0.5 to 6 mm. The fiber diameter of the short fibers (C) is usually 0.1 to 100 μm, preferably 0.1 to 25 μm, and more preferably 1 to 20 μm.
短繊維(C)の平均繊維長は、例えば、光学顕微鏡により短繊維の写真撮影を行い、得られた写真において無作為に選んだ100個の短繊維の長さを測定し、これを算術平均することにより求めることができる。 The average fiber length of the short fibers (C) can be determined by, for example, taking a photograph of the short fibers using an optical microscope, measuring the lengths of 100 randomly selected short fibers in the photograph, and calculating the arithmetic average. It can be found by
短繊維(C)は、チョップドファイバー(カットファイバー)状短繊維でも、フィブリルを有するパルプ状短繊維でもよい。
本発明の組成物は、1種の短繊維(C)を含有してもよく、2種以上の短繊維(C)を含有してもよい。
The short fibers (C) may be chopped fibers (cut fibers) or pulp-like short fibers having fibrils.
The composition of the present invention may contain one type of short fiber (C), or may contain two or more types of short fiber (C).
本発明の組成物における短繊維(C)の含有量は、成分(A)100質量部に対して、通常は0.1~100質量部、好ましくは0.1~30質量部、より好ましくは3~20質量部である。このような態様であると、得られる(架橋)成形体のモジュラス、機械的強度の観点から好ましい。 The content of short fibers (C) in the composition of the present invention is usually 0.1 to 100 parts by mass, preferably 0.1 to 30 parts by mass, and more preferably The amount is 3 to 20 parts by mass. Such an embodiment is preferable from the viewpoint of the modulus and mechanical strength of the (crosslinked) molded product obtained.
<その他の成分>
本発明の組成物は、架橋剤をさらに含有することが好ましい。本発明の組成物は、架橋助剤、軟化剤、無機充填剤、補強剤、老化防止剤、加工助剤、活性剤、吸湿剤、帯電防止剤、着色剤、滑剤および増粘剤から選ばれる少なくとも1種をさらに含有することができる。本発明の組成物は、成分(A)以外の他のポリマー、例えばエラストマーおよび/またはゴムをさらに含有することができる。以下に説明する各成分は、それぞれ1種単独で用いてもよく、2種以上を用いてもよい。
<Other ingredients>
It is preferable that the composition of the present invention further contains a crosslinking agent. The composition of the invention is selected from crosslinking aids, softeners, inorganic fillers, reinforcing agents, anti-aging agents, processing aids, activators, moisture absorbers, antistatic agents, colorants, lubricants and thickeners. It can further contain at least one kind. The compositions of the invention may further contain other polymers than component (A), such as elastomers and/or rubbers. Each of the components described below may be used alone or in combination of two or more.
《架橋剤》
架橋剤としては、ゴムを架橋する際に一般的に使用される架橋剤が挙げられ、例えば、有機過酸化物、硫黄系化合物、フェノール樹脂、ヒドロシリコーン系化合物、アミノ樹脂、キノンまたはその誘導体、アミン系化合物、アゾ系化合物、エポキシ系化合物、イソシアネート系化合物が挙げられる。これらの中でも、有機過酸化物、硫黄系化合物が好ましい。
《Crosslinking agent》
Examples of the crosslinking agent include crosslinking agents commonly used when crosslinking rubber, such as organic peroxides, sulfur compounds, phenolic resins, hydrosilicone compounds, amino resins, quinones or derivatives thereof, Examples include amine compounds, azo compounds, epoxy compounds, and isocyanate compounds. Among these, organic peroxides and sulfur compounds are preferred.
有機過酸化物としては、例えば、ジクミルパーオキサイド、ジ-tert-ブチルパーオキサイド、2,5-ジ-(tert-ブチルパーオキシ)ヘキサン、2,5-ジメチル-2,5-ジ-(tert-ブチルパーオキシ)ヘキサン、2,5-ジメチル-2,5-ジ-(tert-ブチルパーオキシ)ヘキシン-3、1,3-ビス(tert-ブチルパーオキシイソプロピル)ベンゼン、1,1-ビス(tert-ブチルパーオキシ)-3,3,5-トリメチルシクロヘキサン、n-ブチル-4,4-ビス(tert-ブチルパーオキシ)バレレート、ベンゾイルパーオキサイド、p-クロロベンゾイルパーオキサイド、2,4-ジクロロベンゾイルパーオキサイド、tert-ブチルパーオキシベンゾエート、tert-ブチルパーオキシイソプロピルカーボネート、ジアセチルパーオキサイド、ラウロイルパーオキサイド、tert-ブチルクミルパーオキサイドが挙げられる。 Examples of organic peroxides include dicumyl peroxide, di-tert-butyl peroxide, 2,5-di-(tert-butylperoxy)hexane, 2,5-dimethyl-2,5-di-( tert-butylperoxy)hexane, 2,5-dimethyl-2,5-di-(tert-butylperoxy)hexyne-3, 1,3-bis(tert-butylperoxyisopropyl)benzene, 1,1- Bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane, n-butyl-4,4-bis(tert-butylperoxy)valerate, benzoyl peroxide, p-chlorobenzoyl peroxide, 2,4 -dichlorobenzoyl peroxide, tert-butyl peroxybenzoate, tert-butyl peroxyisopropyl carbonate, diacetyl peroxide, lauroyl peroxide, and tert-butyl cumyl peroxide.
本発明の組成物において、架橋剤として有機過酸化物を用いる場合、有機過酸化物の含有量は、成分(A)および必要に応じて配合される架橋が必要な他のポリマー(ゴム等)の合計100質量部に対して、通常は0.1~20質量部、好ましくは0.2~15質量部、さらに好ましくは0.5~10質量部である。 In the composition of the present invention, when an organic peroxide is used as a crosslinking agent, the content of the organic peroxide is the same as that of component (A) and other polymers (rubber, etc.) that require crosslinking and are blended as necessary. The amount is usually 0.1 to 20 parts by weight, preferably 0.2 to 15 parts by weight, and more preferably 0.5 to 10 parts by weight, based on a total of 100 parts by weight.
架橋剤として有機過酸化物を用いる場合、架橋助剤を併用することが好ましい。この場合、架橋助剤をさらに含有する本発明の組成物を用い、当該組成物に、架橋工程前に有機過酸化物を配合し、架橋工程を行ってもよい。 When using an organic peroxide as a crosslinking agent, it is preferable to use a crosslinking aid together. In this case, the composition of the present invention further containing a crosslinking aid may be used, an organic peroxide may be added to the composition before the crosslinking step, and the crosslinking step may be performed.
架橋助剤としては、例えば、イオウ;p-キノンジオキシム等のキノンジオキシム系架橋助剤;2つ以上のエチレン性二重結合を有する架橋助剤;マレイミド系架橋助剤;酸化亜鉛(例えば、ZnO#1・酸化亜鉛2種(JIS規格(K-1410))、ハクスイテック社製)、酸化マグネシウム、亜鉛華(例えば、「META-Z102」(商品名;井上石灰工業社製)などの酸化亜鉛)等の金属酸化物が挙げられ、2つ以上のエチレン性二重結合を有する架橋助剤が好ましい。 Examples of crosslinking aids include sulfur; quinonedioxime crosslinking aids such as p-quinonedioxime; crosslinking aids having two or more ethylenic double bonds; maleimide crosslinking aids; zinc oxide (e.g. , ZnO#1, zinc oxide type 2 (JIS standard (K-1410), manufactured by Hakusui Tech Co., Ltd.), magnesium oxide, zinc white (for example, "META-Z102" (trade name; manufactured by Inoue Lime Industry Co., Ltd.), etc.) Examples include metal oxides such as zinc), and crosslinking aids having two or more ethylenic double bonds are preferred.
2つ以上のエチレン性二重結合を有する架橋助剤中のエチレン性二重結合数は、好ましくは2~6、より好ましくは2~4である。前記架橋助剤を用いることにより、例えば共重合体(A)と短繊維(C)との間で良好にネットワークを形成することができると考えられる。2つ以上のエチレン性二重結合を有する架橋助剤としては、例えば、エチレングリコールジ(メタ)アクリレート、トリメチロールプロパントリ(メタ)アクリレート等の(メタ)アクリル系架橋助剤;ジアリルフタレート、トリアリルイソシアヌレート等のアリル系架橋助剤;ジビニルベンゼン等のビニル系架橋助剤が挙げられる。これらの中でも、(メタ)アクリル系架橋助剤が好ましく、エチレングリコールジメタクリレートがより好ましい。 The number of ethylenic double bonds in the crosslinking auxiliary agent having two or more ethylenic double bonds is preferably 2 to 6, more preferably 2 to 4. It is thought that by using the crosslinking aid, a network can be formed favorably between, for example, the copolymer (A) and the short fibers (C). Examples of crosslinking aids having two or more ethylenic double bonds include (meth)acrylic crosslinking aids such as ethylene glycol di(meth)acrylate and trimethylolpropane tri(meth)acrylate; diallyl phthalate, and tri(meth)acrylate; Examples include allyl crosslinking aids such as allyl isocyanurate; vinyl crosslinking aids such as divinylbenzene. Among these, (meth)acrylic crosslinking aids are preferred, and ethylene glycol dimethacrylate is more preferred.
本発明の組成物が架橋助剤を含有する場合、架橋助剤の含有量は、有機過酸化物1モルに対して、通常は0.5~10モル、好ましくは0.5~7モル、より好ましくは1~5モルである。 When the composition of the present invention contains a crosslinking auxiliary agent, the content of the crosslinking auxiliary agent is usually 0.5 to 10 mol, preferably 0.5 to 7 mol, per 1 mol of organic peroxide. More preferably, it is 1 to 5 mol.
架橋剤として硫黄系化合物を用いる場合、その具体例としては、硫黄、塩化硫黄、二塩化硫黄、モルフォリンジスルフィド、アルキルフェノールジスルフィド、テトラメチルチウラムジスルフィド、ジチオカルバミン酸セレンが挙げられる。 When a sulfur compound is used as a crosslinking agent, specific examples include sulfur, sulfur chloride, sulfur dichloride, morpholine disulfide, alkylphenol disulfide, tetramethylthiuram disulfide, and selenium dithiocarbamate.
本発明の組成物において、架橋剤として硫黄系化合物を用いる場合、硫黄系化合物の含有量は、成分(A)および必要に応じて配合される架橋が必要な他のポリマー(ゴム等)の合計100質量部に対して、通常は0.3~10質量部、好ましくは0.5~7.0質量部、さらに好ましくは0.7~5.0質量部である。 In the composition of the present invention, when a sulfur-based compound is used as a crosslinking agent, the content of the sulfur-based compound is the sum of component (A) and other polymers (rubber, etc.) that require crosslinking and are blended as necessary. The amount is usually 0.3 to 10 parts by weight, preferably 0.5 to 7.0 parts by weight, and more preferably 0.7 to 5.0 parts by weight per 100 parts by weight.
架橋剤として硫黄系化合物を用いる場合、加硫促進剤を併用することが好ましい。加硫促進剤としては、例えば、N-シクロヘキシル-2-ベンゾチアゾールスルフェンアミド、N-オキシジエチレン-2-ベンゾチアゾールスルフェンアミド、N,N'-ジイソプロピル-2-ベンゾチアゾールスルフェンアミド、2-メルカプトベンゾチアゾール、2-(4-モルホリノジチオ)ペンゾチアゾール)、2-(2,4-ジニトロフェニル)メルカプトベンゾチアゾール、2-(2,6-ジエチル-4-モルフォリノチオ)ベンゾチアゾール、ジベンゾチアジルジスルフィド等のチアゾール系加硫促進剤;ジフェニルグアニジン、トリフェニルグアニジン、ジオルソトリルグアニジン等のグアニジン系加硫促進剤;アセトアルデヒド・アニリン縮合物、ブチルアルデヒド・アニリン縮合物等のアルデヒドアミン系加硫促進剤;2-メルカプトイミダゾリン等のイミダゾリン系加硫促進剤;ジエチルチオウレア、ジブチルチオウレア等のチオウレア系加硫促進剤;テトラメチルチウラムモノスルフィド、テトラメチルチウラムジスルフィド、テトラエチルチウラムジスルフィド、テトラブチルチウラムジスルフィド、ジペンタメチレンチウラムテトラスルフィド等のチウラム系加硫促進剤;ジメチルジチオカルバミン酸亜鉛、ジエチルジチオカルバミン酸亜鉛、ジブチルジチオカルバミン酸亜鉛、ジエチルジチオカルバミン酸テルル等のジチオ酸塩系加硫促進剤;エチレンチオ尿素(例えば、サンセラー22C(商品名;三新化学工業社製))、N,N'-ジエチルチオ尿素、N,N'-ジブチルチオ尿素等のチオウレア系加硫促進剤;ジブチルキサトゲン酸亜鉛等のザンテート系加硫促進剤;その他、亜鉛華が挙げられる。 When using a sulfur-based compound as a crosslinking agent, it is preferable to use a vulcanization accelerator together. Examples of the vulcanization accelerator include N-cyclohexyl-2-benzothiazolesulfenamide, N-oxydiethylene-2-benzothiazolesulfenamide, N,N'-diisopropyl-2-benzothiazolesulfenamide, 2 -Mercaptobenzothiazole, 2-(4-morpholinodithio)penzothiazole), 2-(2,4-dinitrophenyl)mercaptobenzothiazole, 2-(2,6-diethyl-4-morpholinothio)benzothiazole, Thiazole-based vulcanization accelerators such as dibenzothiazyl disulfide; guanidine-based vulcanization accelerators such as diphenylguanidine, triphenylguanidine, and diorthotolylguanidine; aldehyde amine-based vulcanization accelerators such as acetaldehyde/aniline condensates, butyraldehyde/aniline condensates, etc. Vulcanization accelerator: Imidazoline vulcanization accelerator such as 2-mercaptoimidazoline; Thiourea vulcanization accelerator such as diethylthiourea, dibutylthiourea; Tetramethylthiuram monosulfide, tetramethylthiuram disulfide, tetraethylthiuram disulfide, tetrabutylthiuram Thiuram-based vulcanization accelerators such as disulfide, dipentamethylene thiuram tetrasulfide; dithioate-based vulcanization accelerators such as zinc dimethyldithiocarbamate, zinc diethyldithiocarbamate, zinc dibutyldithiocarbamate, tellurium diethyldithiocarbamate; ethylenethiourea ( For example, thiourea-based vulcanization accelerators such as Suncella 22C (trade name; manufactured by Sanshin Kagaku Kogyo Co., Ltd.), N,N'-diethylthiourea, N,N'-dibutylthiourea; xanthate-based vulcanization accelerators such as zinc dibutylxatogenate. Vulcanization accelerator; other examples include zinc white.
本発明の組成物が加硫促進剤を含有する場合、加硫促進剤の含有量は、成分(A)および必要に応じて配合される架橋が必要な他のポリマー(ゴム等)の合計100質量部に対して、通常は0.1~20質量部、好ましくは0.2~15質量部、さらに好ましくは0.5~10質量部である。 When the composition of the present invention contains a vulcanization accelerator, the content of the vulcanization accelerator is 100% in total of component (A) and other polymers (rubber, etc.) that require crosslinking and are blended as necessary. The amount is usually 0.1 to 20 parts by weight, preferably 0.2 to 15 parts by weight, and more preferably 0.5 to 10 parts by weight.
加硫助剤は、架橋剤が硫黄系化合物である場合に好ましく用いることができ、例えば、酸化亜鉛(例えば、ZnO#1・酸化亜鉛2種、ハクスイテック社製)、酸化マグネシウム、亜鉛華(例えば、「META-Z102」(商品名;井上石灰工業社製)等の酸化亜鉛)が挙げられる。 The vulcanization aid can be preferably used when the crosslinking agent is a sulfur-based compound, such as zinc oxide (e.g., ZnO #1, zinc oxide 2, manufactured by Hakusui Tech), magnesium oxide, zinc white (e.g. , "META-Z102" (trade name; manufactured by Inoue Lime Industry Co., Ltd.) and other zinc oxides).
本発明の組成物が加硫助剤を含有する場合、加硫助剤の含有量は、成分(A)および必要に応じて配合される架橋が必要な他のポリマー(ゴム等)の合計100質量部に対して、通常は1~20質量部である。 When the composition of the present invention contains a vulcanization aid, the content of the vulcanization aid is a total of 100 It is usually 1 to 20 parts by mass.
《軟化剤》
軟化剤としては、例えば、プロセスオイル、潤滑油、パラフィン油、流動パラフィン、石油アスファルト、ワセリン等の石油系軟化剤;コールタール等のコールタール系軟化剤;ヒマシ油、アマニ油、ナタネ油、大豆油、ヤシ油等の脂肪油系軟化剤;蜜ロウ、カルナウバロウ等のロウ類;リシノール酸、パルミチン酸、ステアリン酸、ステアリン酸バリウム、ステアリン酸カルシウム等の脂肪酸またはその塩;ナフテン酸、パイン油、ロジンまたはその誘導体;テルペン樹脂、石油樹脂、クマロンインデン樹脂等の合成高分子物質;ジオクチルフタレート、ジオクチルアジペート等のエステル系軟化剤;その他、マイクロクリスタリンワックス、液状ポリブタジエン、変性液状ポリブタジエン、炭化水素系合成潤滑油、トール油、サブ(ファクチス)が挙げられ、石油系軟化剤が好ましく、プロセスオイルがより好ましい。
《Softener》
Examples of softeners include process oil, lubricating oil, paraffin oil, liquid paraffin, petroleum asphalt, petroleum softeners such as vaseline; coal tar softeners such as coal tar; castor oil, linseed oil, rapeseed oil, and Fatty oil-based softeners such as bean oil and coconut oil; waxes such as beeswax and carnauba wax; fatty acids or their salts such as ricinoleic acid, palmitic acid, stearic acid, barium stearate, and calcium stearate; naphthenic acid, pine oil, rosin or derivatives thereof; synthetic polymer substances such as terpene resins, petroleum resins, coumaron indene resins; ester softeners such as dioctyl phthalate and dioctyl adipate; others, microcrystalline wax, liquid polybutadiene, modified liquid polybutadiene, hydrocarbon synthesis Examples include lubricating oil, tall oil, and sub(factice), with petroleum softeners being preferred and process oils being more preferred.
本発明の組成物が軟化剤を含有する場合、軟化剤の含有量は、成分(A)および必要に応じて配合される他のポリマー(エラストマー、ゴム等)の合計100質量部に対して、通常は2~100質量部、好ましくは5~100質量部である。 When the composition of the present invention contains a softener, the content of the softener is based on a total of 100 parts by mass of component (A) and other polymers (elastomer, rubber, etc.) blended as necessary. It is usually 2 to 100 parts by weight, preferably 5 to 100 parts by weight.
《無機充填剤》
無機充填剤としては、例えば、軽質炭酸カルシウム、重質炭酸カルシウム、タルク、クレーが挙げられる。これらの中でも、重質炭酸カルシウムが好ましい。
《Inorganic filler》
Examples of the inorganic filler include light calcium carbonate, heavy calcium carbonate, talc, and clay. Among these, heavy calcium carbonate is preferred.
本発明の組成物が無機充填剤を含有する場合、無機充填剤の含有量は、成分(A)および必要に応じて配合される他のポリマー(エラストマー、ゴム等)の合計100質量部に対して、通常は2~50質量部、好ましくは5~50質量部である。 When the composition of the present invention contains an inorganic filler, the content of the inorganic filler is based on a total of 100 parts by mass of component (A) and other polymers (elastomer, rubber, etc.) blended as necessary. The amount is usually 2 to 50 parts by weight, preferably 5 to 50 parts by weight.
《補強剤》
補強剤としては、例えば、シリカ、炭酸カルシウム、活性化炭酸カルシウム、微粉タルク、微分ケイ酸が挙げられ、ただし、前述したカーボンブラック(B)を除く。
《Reinforcer》
Examples of the reinforcing agent include silica, calcium carbonate, activated calcium carbonate, finely divided talc, and differential silicic acid, excluding the carbon black (B) mentioned above.
本発明の組成物が補強剤を含有する場合、補強剤の含有量は、成分(A)および必要に応じて配合される他のポリマー(エラストマー、ゴム等)の合計100質量部に対して、通常は0.1~100質量部、好ましくは5~30質量部である。 When the composition of the present invention contains a reinforcing agent, the content of the reinforcing agent is based on a total of 100 parts by mass of component (A) and other polymers (elastomer, rubber, etc.) blended as necessary. It is usually 0.1 to 100 parts by weight, preferably 5 to 30 parts by weight.
《老化防止剤(安定剤)》
本発明の組成物は、老化防止剤(安定剤)を含有することにより、当該組成物から形成される(架橋)成形体の寿命を長くすることができる。老化防止剤としては、例えば、アミン系老化防止剤、フェノール系老化防止剤、イオウ系老化防止剤が挙げられる。
《Anti-aging agent (stabilizer)》
By containing the anti-aging agent (stabilizer), the composition of the present invention can extend the life of a (crosslinked) molded article formed from the composition. Examples of anti-aging agents include amine-based anti-aging agents, phenol-based anti-aging agents, and sulfur-based anti-aging agents.
アミン系老化防止剤としては、例えば、フェニルブチルアミン、N,N-ジ-2-ナフチル-p―フェニレンジアミン等の芳香族第2アミン系老化防止剤が挙げられる。フェノール系老化防止剤としては、例えば、ジブチルヒドロキシトルエン、ペンタエリトリトールテトラキス[3-(3,5-ジ-tert-ブチル-4-ヒドロキシフェニル)プロピオナート]が挙げられる。イオウ系老化防止剤としては、例えば、ビス[2-メチル-4-(3-n-アルキルチオプロピオニルオキシ)-5-t-ブチルフェニル]スルフィド等のチオエーテル系老化防止剤;ジブチルジチオカルバミン酸ニッケル等のジチオカルバミン酸塩系老化防止剤;2-メルカプトベンゾイルイミダゾール、2-メルカプトベンゾイミダゾール、2-メルカプトベンゾイミダゾールの亜鉛塩、ジラウリルチオジプロピオネート、ジステアリルチオジプロピオネートが挙げられる。 Examples of the amine antioxidant include aromatic secondary amine antioxidants such as phenylbutylamine and N,N-di-2-naphthyl-p-phenylenediamine. Examples of the phenolic anti-aging agent include dibutylhydroxytoluene and pentaerythritol tetrakis [3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]. Examples of sulfur-based anti-aging agents include thioether-based anti-aging agents such as bis[2-methyl-4-(3-n-alkylthiopropionyloxy)-5-t-butylphenyl] sulfide; nickel dibutyldithiocarbamate, etc. Dithiocarbamate-based anti-aging agents; examples include 2-mercaptobenzoylimidazole, 2-mercaptobenzimidazole, zinc salt of 2-mercaptobenzimidazole, dilaurylthiodipropionate, and distearylthiodipropionate.
本発明の組成物が老化防止剤を含有する場合、老化防止剤の含有量は、成分(A)および必要に応じて配合される他のポリマー(エラストマー、ゴム等)の合計100質量部に対して、通常は0.3~10質量部、好ましくは0.5~7.0質量部である。 When the composition of the present invention contains an anti-aging agent, the content of the anti-aging agent is based on a total of 100 parts by mass of component (A) and other polymers (elastomer, rubber, etc.) blended as necessary. The amount is usually 0.3 to 10 parts by weight, preferably 0.5 to 7.0 parts by weight.
《加工助剤》
加工助剤としては、一般的に加工助剤としてゴムに配合されるものを広く用いることができる。加工助剤としては、例えば、リシノール酸、ステアリン酸、パルミチン酸、ラウリン酸、ステアリン酸バリウム、ステアリン酸亜鉛、ステアリン酸カルシウム、エステル類が挙げられる。これらの中でも、ステアリン酸が好ましい。
《Processing aid》
As the processing aid, a wide variety of processing aids that are generally blended into rubber can be used. Examples of processing aids include ricinoleic acid, stearic acid, palmitic acid, lauric acid, barium stearate, zinc stearate, calcium stearate, and esters. Among these, stearic acid is preferred.
本発明の組成物が加工助剤を含有する場合、加工助剤の含有量は、成分(A)および必要に応じて配合される他のポリマー(エラストマー、ゴム等)の合計100質量部に対して、通常は10質量部以下、好ましくは8.0質量部以下である。 When the composition of the present invention contains a processing aid, the content of the processing aid is based on a total of 100 parts by mass of component (A) and other polymers (elastomer, rubber, etc.) blended as necessary. The amount is usually 10 parts by mass or less, preferably 8.0 parts by mass or less.
《活性剤》
活性剤としては、例えば、ジ-n-ブチルアミン、ジシクロヘキシルアミン、モノエラノールアミン等のアミン類;ジエチレングリコール、ポリエチレングリコール、レシチン、トリアリルートメリレート、脂肪族カルボン酸または芳香族カルボン酸の亜鉛化合物等の活性剤;過酸化亜鉛調整物;クタデシルトリメチルアンモニウムブロミド、合成ハイドロタルサイト、特殊四級アンモニウム化合物が挙げられる。
《Activator》
Examples of the activator include amines such as di-n-butylamine, dicyclohexylamine, and monoelanolamine; diethylene glycol, polyethylene glycol, lecithin, triaryl utmerate, and zinc compounds of aliphatic carboxylic acids or aromatic carboxylic acids. Activators; zinc peroxide preparations; tadecyltrimethylammonium bromide, synthetic hydrotalcites, special quaternary ammonium compounds.
本発明の組成物が活性剤を含有する場合、活性剤の含有量は、成分(A)および必要に応じて配合される他のポリマー(エラストマー、ゴム等)の合計100質量部に対して、通常は0.2~10質量部、好ましくは0.3~5質量部である。 When the composition of the present invention contains an active agent, the content of the active agent is based on a total of 100 parts by mass of component (A) and other polymers (elastomer, rubber, etc.) blended as necessary. It is usually 0.2 to 10 parts by weight, preferably 0.3 to 5 parts by weight.
《吸湿剤》
吸湿剤としては、例えば、酸化カルシウム、シリカゲル、硫酸ナトリウム、モレキュラーシーブ、ゼオライト、ホワイトカーボンが挙げられる。
本発明の組成物が吸湿剤を含有する場合、吸湿剤の含有量は、成分(A)および必要に応じて配合される他のポリマー(エラストマー、ゴム等)の合計100質量部に対して、通常は0.5~15質量部、好ましくは1.0~12質量部である。
《Moisture absorbent》
Examples of the moisture absorbent include calcium oxide, silica gel, sodium sulfate, molecular sieve, zeolite, and white carbon.
When the composition of the present invention contains a hygroscopic agent, the content of the hygroscopic agent is based on a total of 100 parts by mass of component (A) and other polymers (elastomer, rubber, etc.) blended as necessary. It is usually 0.5 to 15 parts by weight, preferably 1.0 to 12 parts by weight.
《他のポリマー》
本発明の組成物は、成分(A)以外の他のポリマーをさらに含有することができる。
架橋が必要な他のポリマーとしては、例えば、天然ゴム、イソプレンゴム、ブタジエンゴム、スチレン-ブタジエンゴム、クロロプレンゴム、ニトリルゴム、ブチルゴム、アクリルゴム、シリコーンゴム、フッ素ゴム、ウレタンゴム等のゴムが挙げられる。
《Other polymers》
The composition of the present invention may further contain other polymers than component (A).
Examples of other polymers that require crosslinking include rubbers such as natural rubber, isoprene rubber, butadiene rubber, styrene-butadiene rubber, chloroprene rubber, nitrile rubber, butyl rubber, acrylic rubber, silicone rubber, fluororubber, and urethane rubber. It will be done.
架橋が不要な他のポリマーとしては、例えば、スチレンとブタジエンとのブロック共重合体(SBS)、ポリスチレン-ポリ(エチレン-ブチレン)-ポリスチレン(SEBS)、ポリスチレン-ポリ(エチレン-プロピレン)-ポリスチレン(SEPS)等のスチレン系熱可塑性エラストマー(TPS)、オレフィン系熱可塑性エラストマー(TPO)、塩ビ系エラストマー(TPVC)、エステル系熱可塑性エラストマー(TPC)、アミド系熱可塑性エラストマー(TPA)、ウレタン系熱可塑性エラストマー(TPU)、その他の熱可塑性エラストマー(TPZ)等のエラストマーが挙げられる。
本発明の組成物が他のポリマーを含有する場合、他のポリマーの含有量は、成分(A)100質量部に対して、通常は100質量部以下、好ましくは80質量部以下である。
Examples of other polymers that do not require crosslinking include block copolymers of styrene and butadiene (SBS), polystyrene-poly(ethylene-butylene)-polystyrene (SEBS), polystyrene-poly(ethylene-propylene)-polystyrene ( Styrene thermoplastic elastomer (TPS) such as SEPS), olefin thermoplastic elastomer (TPO), polyvinyl chloride elastomer (TPVC), ester thermoplastic elastomer (TPC), amide thermoplastic elastomer (TPA), urethane thermoplastic elastomer Examples include elastomers such as plastic elastomer (TPU) and other thermoplastic elastomers (TPZ).
When the composition of the present invention contains other polymers, the content of the other polymers is usually 100 parts by mass or less, preferably 80 parts by mass or less, based on 100 parts by mass of component (A).
<組成物の調製>
本発明の組成物は、成分(A)と、カーボンブラック(B)と、必要に応じて配合される短繊維(C)、その他の成分とを、例えば、ミキサー、ニーダー、ロール等の混練機を用いて所望の温度で混練することにより調製することができる。
<Preparation of composition>
The composition of the present invention is prepared by mixing component (A), carbon black (B), short fibers (C) blended as necessary, and other components in a kneading machine such as a mixer, kneader, or roll. It can be prepared by kneading at a desired temperature using.
本発明の組成物の一実施態様は、例えば以下のように調製される。成分(A)と、カーボンブラック(B)と、必要に応じて短繊維(C)と、所定のその他の成分とを、混練機に投入して所定の加熱条件(例えば80~200℃で3~30分)で混練して均一化する(A練り)。なお、A練りでは、A練りの加熱温度まで加熱すると成分(A)を架橋させる、架橋剤等は投入されない。A練りで混練された混合物の温度を、次いで、架橋剤の架橋温度未満(例えば、130℃以下)まで下げた後、A練りで添加されなかった架橋剤等を前記混合物に添加し、所定の加熱条件(例えばロール温度30~80℃で1~30分間)でさらに混練して均一化し(B練り)、本発明の組成物を得ることができる。 One embodiment of the composition of the invention is prepared, for example, as follows. Component (A), carbon black (B), short fibers (C) if necessary, and other predetermined components are put into a kneader and heated under predetermined heating conditions (e.g., 80 to 200°C for 30 minutes). -30 minutes) to make it homogeneous (Kneading A). In addition, in the A kneading, no crosslinking agent or the like is added, which crosslinks the component (A) when heated to the heating temperature of the A kneading. After the temperature of the mixture kneaded in A-kneading is then lowered to below the crosslinking temperature of the crosslinking agent (for example, 130°C or lower), the crosslinking agent etc. that were not added in A-kneading are added to the mixture, and a predetermined amount is obtained. The composition of the present invention can be obtained by further kneading and homogenizing under heating conditions (for example, roll temperature of 30 to 80°C for 1 to 30 minutes) (Kneading B).
本発明の組成物は、架橋剤を配合する前の組成(A練り)において、125℃におけるムーニー粘度ML(1+4)が、通常は10~250、好ましくは10~100、より好ましくは10~50である。ムーニー粘度が前記範囲にある組成物は、良好な後処理品質を示すと共に優れたゴム物性を有する。 The composition of the present invention has a Mooney viscosity ML (1+4) at 125°C of usually 10 to 250, preferably 10 to 100, more preferably 10 ~50. A composition having a Mooney viscosity within the above range exhibits good post-treatment quality and has excellent rubber physical properties.
[(架橋)成形体、伝動ベルト]
本発明の組成物から、(架橋)成形体を得ることができる。本発明の組成物は、例えば、押出成形、射出成形、プレス成形、カレンダー成形、トランスファー成形、発泡成形等の熱成形方法によって成形できる。本発明において、前記組成物の架橋温度は、通常は140℃以上、好ましくは150~220℃、より好ましくは160~200℃である。また、この架橋反応は、空気中で行うことができる。
[(Crosslinked) molded body, power transmission belt]
A (crosslinked) molded article can be obtained from the composition of the present invention. The composition of the present invention can be molded by thermoforming methods such as extrusion molding, injection molding, press molding, calendar molding, transfer molding, and foam molding. In the present invention, the crosslinking temperature of the composition is usually 140°C or higher, preferably 150 to 220°C, more preferably 160 to 200°C. Moreover, this crosslinking reaction can be performed in air.
本発明では、前記(架橋)成形体は、伝動ベルトの構成部材として好適に用いることができる。例えば、本発明の組成物は、成形加工性に適した高い粘着力を有しており、ベルト加工性に優れている。また、本発明の組成物を用いることにより、高ゴム弾性、耐摩耗性、耐熱性および耐寒性に優れた、伝動ベルトの構成部材を製造することができる。 In the present invention, the (crosslinked) molded body can be suitably used as a component of a power transmission belt. For example, the composition of the present invention has high adhesive strength suitable for molding processability and is excellent in belt processability. Further, by using the composition of the present invention, it is possible to produce a component for a power transmission belt that has high rubber elasticity, excellent abrasion resistance, heat resistance, and cold resistance.
本発明の伝動ベルトは、本発明の組成物から形成された(架橋)成形体を有する。
本発明の伝動ベルトとしては、例えば、Vベルト、Vリブドベルト等の摩擦伝動ベルト;タイミングベルト等のかみ合い伝動ベルトが挙げられる。伝動ベルトは、例えば、自動車用伝動ベルト、自動二輪用伝動ベルト、一般産業機械用伝動ベルトである。Vベルトとしては、例えば、ラップドベルト、ローエッジベルトが挙げられる。
The power transmission belt of the present invention has a (crosslinked) molded body formed from the composition of the present invention.
Examples of the power transmission belt of the present invention include friction power transmission belts such as V belts and V-ribbed belts; interlocking power transmission belts such as timing belts. The transmission belt is, for example, a transmission belt for automobiles, a transmission belt for motorcycles, or a transmission belt for general industrial machinery. Examples of the V-belt include a wrapped belt and a raw-edge belt.
伝動ベルトの一実施形態は、例えば、心線が埋設された接着ゴム部を有しており、さらに、前記接着ゴム部の下面に形成された底ゴム部を有することができる。前記伝動ベルトは、必要に応じて、接着ゴム部上に形成された上部帆布、および/または底ゴム部下に形成された下部帆布を有することができる。本発明の組成物は、例えば、接着ゴム部および/または底ゴム部を形成するために好適に用いられる。具体的には、接着ゴム部および/または底ゴム部として、本発明の組成物から形成された架橋成形部が好適に用いられる。 One embodiment of the power transmission belt has, for example, an adhesive rubber part in which a core wire is embedded, and can further include a bottom rubber part formed on the lower surface of the adhesive rubber part. The transmission belt may have an upper canvas formed on the adhesive rubber part and/or a lower canvas formed under the bottom rubber, as necessary. The composition of the present invention is suitably used, for example, to form an adhesive rubber part and/or a bottom rubber part. Specifically, a crosslinked molded part formed from the composition of the present invention is preferably used as the adhesive rubber part and/or the bottom rubber part.
伝動ベルトの抗張部材である心線は、接着ゴム部において、ベルトの長手方向に延在する。心線としては、例えば、ポリエステル系コードが挙げられる。接着ゴム部は、心線を取り囲み、かつ心線に接着されている。一実施形態では、例えば、本発明の組成物を心線周りに配置して架橋することにより、心線に接着された接着ゴム部を形成することができる。帆布としては、例えば、綿、綿とポリエステルとの混紡からなるもの、綿とポリアミドとの混紡からなるものが挙げられる。 The core wire, which is a tensile member of the power transmission belt, extends in the longitudinal direction of the belt at the adhesive rubber portion. Examples of the core wire include polyester cords. The adhesive rubber portion surrounds the core wire and is bonded to the core wire. In one embodiment, for example, the composition of the present invention may be placed around the core wire and crosslinked to form an adhesive rubber portion adhered to the core wire. Examples of the canvas include those made of cotton, a blend of cotton and polyester, and those made of a blend of cotton and polyamide.
以下、実施例に基づいて本発明をさらに具体的に説明するが、本発明はこれら実施例に限定されるものではない。特に言及しない限り「部」は「質量部」を表す。
[エチレン・α-オレフィン・非共役ポリエン共重合体の物性]
<エチレンに由来する構造単位、α-オレフィンに由来する構造単位、および非共役ポリエンに由来する構造単位のモル量>
前記モル量は、1H-NMRスペクトルメーターによる強度測定によって求めた。測定条件の詳細は、国際公開第2015/122415号に記載されている。
Hereinafter, the present invention will be explained in more detail based on Examples, but the present invention is not limited to these Examples. Unless otherwise specified, "parts" represent "parts by mass."
[Physical properties of ethylene/α-olefin/nonconjugated polyene copolymer]
<Molar amount of structural units derived from ethylene, structural units derived from α-olefin, and structural units derived from non-conjugated polyene>
The molar amount was determined by intensity measurement using a 1 H-NMR spectrometer. Details of the measurement conditions are described in International Publication No. 2015/122415.
<ムーニー粘度>
ムーニー粘度(ML(1+4)100℃、125℃)は、ムーニー粘度計(島津製作所社製SMV202型)を用いて、JIS K6300(1994)に準じて測定した。
<Mooney viscosity>
Mooney viscosity (ML (1+4) 100°C, 125°C) was measured using a Mooney viscometer (SMV202 model manufactured by Shimadzu Corporation) according to JIS K6300 (1994).
<B値>
o-ジクロロベンゼン-d4/ベンゼン-d6(4/1[v/v])を測定溶媒とし、測定温度120℃にて、13C-NMRスペクトル(100MHz、日本電子製ECX400P)を測定し、下記式(i)に基づき算出した。
B値=([EX]+2[Y])/〔2×[E]×([X]+[Y])〕・・・(i)
ここで[E]、[X]および[Y]は、それぞれ、エチレン[A1]、炭素数4~20のα-オレフィン[A2]、および非共役ポリエン[A3]に由来する構造単位のモル分率を示し、[EX]はエチレン[A1]-炭素数4~20のα-オレフィン[A2]ダイアッド連鎖分率を示す。
<B value>
Using o-dichlorobenzene-d 4 /benzene-d 6 (4/1 [v/v]) as the measurement solvent, the 13 C-NMR spectrum (100 MHz, JEOL ECX400P) was measured at a measurement temperature of 120°C. , calculated based on the following formula (i).
B value = ([EX]+2[Y])/[2×[E]×([X]+[Y])]...(i)
Here, [E], [X] and [Y] are the mole fraction of structural units derived from ethylene [A1], α-olefin having 4 to 20 carbon atoms [A2], and non-conjugated polyene [A3], respectively. [EX] indicates the ethylene [A1]-α-olefin [A2] dyad chain fraction having 4 to 20 carbon atoms.
[エチレン・α-オレフィン・非共役ポリエン共重合体]
国際公開第2015/122415号の[合成例C1]の記載に準じて、下記の物性を有するエチレン/1-ブテン/5-エチリデン-2-ノルボルネン(ENB)共重合体を得た。以下、これを「EBDM-1」と記載する。
EBDM-1の構成および物性は、以下のとおりである。
エチレンに由来する構造単位:67.7モル%
1-ブテンに由来する構造単位:30.0モル%
ENBに由来する構造単位:2.3モル%
ムーニー粘度ML(1+4)100℃:30
ムーニー粘度ML(1+4)125℃:22
B値:1.3
[Ethylene/α-olefin/non-conjugated polyene copolymer]
According to the description in [Synthesis Example C1] of International Publication No. 2015/122415, an ethylene/1-butene/5-ethylidene-2-norbornene (ENB) copolymer having the following physical properties was obtained. Hereinafter, this will be referred to as "EBDM-1".
The structure and physical properties of EBDM-1 are as follows.
Structural unit derived from ethylene: 67.7 mol%
Structural unit derived from 1-butene: 30.0 mol%
Structural unit derived from ENB: 2.3 mol%
Mooney viscosity ML (1+4) 100℃: 30
Mooney viscosity ML (1+4) 125℃: 22
B value: 1.3
[実施例1]
MIXTRON BB MIXER(神戸製鋼所社製、BB-2型、容積1.7L、ローター2WH)を用いて、100部のEBDM-1に対して、架橋助剤としてZnO#1・酸化亜鉛2種(JIS規格(K-1410))を5部、加工助剤としてステアリン酸を1部、カーボンブラックとして旭#60UGを40部、シリカとしてシリカVN3を10部、老化防止剤としてサンダントMB(2-メルカプトベンゾイミダゾール)を4部、老化防止剤としてイルガノックス1010(ペンタエリトリトールテトラキス[3-(3,5-ジ-tert-ブチル-4-ヒドロキシフェニル)プロピオナート])を2部、軟化剤としてダイアナプロセスオイルPW-380(パラフィン系プロセスオイル)を10部の配合量で配合した後混練し、配合物1を得た。
[Example 1]
Using MIXTRON BB MIXER (manufactured by Kobe Steel, BB-2 type, volume 1.7L, rotor 2WH), ZnO #1 and two types of zinc oxide ( 5 parts of JIS standard (K-1410)), 1 part of stearic acid as a processing aid, 40 parts of Asahi #60UG as carbon black, 10 parts of Silica VN3 as silica, and Sandant MB (2-mercapto) as an anti-aging agent. benzimidazole), 2 parts of Irganox 1010 (pentaerythritol tetrakis [3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate]) as an anti-aging agent, Diana Process Oil as a softener. PW-380 (paraffinic process oil) was blended in an amount of 10 parts and then kneaded to obtain a blend 1.
配合物1調製時の混練条件は、ローター回転数が40rpm、フローティングウェイト圧力が3kg/cm2、混練時間が5分間で行い、混練排出温度は144℃であった。
配合物1のムーニー粘度ML(1+4)125℃を、ムーニー粘度計(島津製作所社製SMV202型)を用いて、JIS K6300(1994)に準じて測定した。
The kneading conditions for preparing Compound 1 were as follows: rotor rotation speed was 40 rpm, floating weight pressure was 3 kg/cm 2 , kneading time was 5 minutes, and the kneading discharge temperature was 144°C.
The Mooney viscosity ML (1+4) 125° C. of Formulation 1 was measured using a Mooney viscometer (Model SMV202 manufactured by Shimadzu Corporation) according to JIS K6300 (1994).
次いで、配合物1が温度40℃となったことを確認した後、6インチロールを用いて、配合物1に、架橋剤としてカヤクミルDCP-40C(ジクミルパーオキサイド40質量%)を6.8部の配合量で添加して混練し、配合物2を得た。 Next, after confirming that the temperature of Formulation 1 reached 40°C, using a 6-inch roll, 6.8% of Kayakumil DCP-40C (40% by mass of dicumyl peroxide) was added to Formulation 1 as a crosslinking agent. The mixture was added and kneaded in an amount of 100% to obtain a blend 2.
配合物2調製時の混練条件は、ロール温度を前ロール/後ロール=50℃/50℃、ロール周速さを前ロール/後ロール=18rpm/15rpm、ロール間隙を3mmとして、混練時間8分間で分出しし、配合物2を得た。 The kneading conditions when preparing Compound 2 were: roll temperature: front roll/rear roll = 50°C/50°C, roll circumferential speed: front roll/rear roll = 18 rpm/15 rpm, roll gap: 3 mm, kneading time: 8 minutes. Compound 2 was obtained.
配合物2に対して、プレス成形機を用いて170℃で15分間プレス処理を行って、厚さ2mmの架橋シートを作製した。得られた架橋シートについて、後述する硬度試験、引張試験、耐熱老化性試験およびゲーマン捻り試験を行った。 Compound 2 was pressed using a press molding machine at 170° C. for 15 minutes to produce a crosslinked sheet with a thickness of 2 mm. The obtained crosslinked sheet was subjected to a hardness test, a tensile test, a heat aging resistance test, and a Gehman twist test, which will be described later.
配合物2に対して、円柱状の金型がセットされたプレス成形機を用いて170℃で20分間プレス処理を行って、厚さ12.7mm、直径29mmの直円柱形の試験片を作製し、圧縮永久歪み(CS)測定用試験片を得た。 Compound 2 was pressed at 170°C for 20 minutes using a press molding machine equipped with a cylindrical mold to produce a right cylindrical test piece with a thickness of 12.7 mm and a diameter of 29 mm. A test piece for compression set (CS) measurement was obtained.
[実施例2~3、比較例1~3]
表2に記載した組成および硬化系に基づいたこと以外は実施例1と同様に行った。
実施例および比較例で用いた材料を以下の表1に示す。
[Examples 2-3, Comparative Examples 1-3]
The same procedure as in Example 1 was conducted except that the composition and curing system were based on those listed in Table 2.
Materials used in Examples and Comparative Examples are shown in Table 1 below.
[比重]
原料ポリマーまたは配合物1(A練り)を1g切り取り、試験片を作製した。試験片を25℃雰囲気下で自動比重計(東洋精機製作所製:M-1型)に取り付け、空気中および純水中の質量の差から比重測定を行った。表2中におけるraw polymerはクロロプレンゴム、2060MまたはEBDM-1(原料ポリマー)を指し、compoundは配合物1を指す。
[specific gravity]
A test piece was prepared by cutting out 1 g of the raw material polymer or Blend 1 (Kneading A). The test piece was attached to an automatic hydrometer (Model M-1, manufactured by Toyo Seiki Seisakusho) in an atmosphere of 25° C., and the specific gravity was measured from the difference in mass in air and in pure water. In Table 2, raw polymer refers to chloroprene rubber, 2060M or EBDM-1 (raw material polymer), and compound refers to Blend 1.
[プローブタック試験]
プローブタックは、配合物1に対して、JIS Z3284に準拠しRHESCA社製 TAC-IIを用いて測定した。条件は温度25℃、Immersion speed:120mm/min、Preload:600gf、Test speed:120mm/min、Press time:60sとした。
[Probe tack test]
Probe tack was measured for Formulation 1 using TAC-II manufactured by RHESCA in accordance with JIS Z3284. The conditions were: temperature 25°C, immersion speed: 120mm/min, preload: 600gf, test speed: 120mm/min, press time: 60s.
[コンパウンド同士の粘着性]
配合物1(A練り)に対して、50トンプレス成形機を用いて190℃で10分間プレス処理を行って、厚さ2mmのシートを作製した。前記シート2枚を貼り合わせ、軽く手で圧をかけた。貼り合わせた2枚のシートを手で剥がしたときの状況を以下の通り分類した。
[Adhesiveness between compounds]
Compound 1 (Kneading A) was subjected to a press treatment at 190° C. for 10 minutes using a 50-ton press molding machine to produce a sheet with a thickness of 2 mm. The two sheets were pasted together and pressure was applied lightly by hand. The situation when two sheets pasted together were peeled off by hand was classified as follows.
<評価>
◎:手で剥がそうとしても剥がれず基材破壊する。
〇:手で剥がそうとしても剥がれづらいが粘着面で剥がれる。
△:剥がそうとした際に手に圧を感じるが剥がれる。
×:剥がそうとした際に手にほぼ圧を感じず剥がれる。
<Evaluation>
◎: Even if you try to peel it off by hand, it will not peel off and the base material will be destroyed.
○: It is difficult to remove even if you try to remove it by hand, but it can be removed with the adhesive surface.
△: When I try to peel it off, I feel pressure on my hand, but it peels off.
×: When trying to peel it off, it peels off without feeling almost any pressure on the hand.
[硬度試験(Durometer-A)]
厚さ2mmの前記架橋シートの平らな部分を重ねて厚さ12mmのシートとし、JIS K6253に従い、硬度(JIS-A)を測定した。
[Hardness test (Durometer-A)]
The flat parts of the 2 mm thick crosslinked sheets were stacked to form a 12 mm thick sheet, and the hardness (JIS-A) was measured according to JIS K6253.
[引張試験:モジュラス、引張破断点応力、引張破断点伸び]
厚さ2mmの前記架橋シートを打抜いてJIS K6251(1993)に記載されている3号形ダンベル試験片を作製し、この試験片を用いてJIS K6251第3項に規定される方法に従い、測定温度25℃、引張速度500mm/分の条件で引張試験を行い、伸び率が25%であるときの引張応力(25%モジュラス(M25))、引張破断点応力(TB)および引張破断点伸び(EB)を測定した。
[Tensile test: modulus, tensile stress at break, tensile elongation at break]
A No. 3 dumbbell test piece described in JIS K6251 (1993) was prepared by punching out the crosslinked sheet with a thickness of 2 mm, and measurements were performed using this test piece according to the method specified in JIS K6251 Section 3. A tensile test was conducted at a temperature of 25°C and a tensile speed of 500 mm/min, and the tensile stress (25% modulus (M25)), tensile stress at break (TB), and tensile elongation at break ( EB) was measured.
[圧縮永久歪み試験]
圧縮永久歪み(CS)測定用試験片について、JIS K6262(1997)に従って、-20℃×22時間処理後または180℃×70時間処理後の圧縮永久歪みを測定した。圧縮永久歪みは小さいことが望ましい。
[Compression set test]
Regarding the test pieces for compression set (CS) measurement, the compression set was measured after treatment at -20°C for 22 hours or at 180°C for 70 hours, according to JIS K6262 (1997). It is desirable that the compression set is small.
[耐熱性試験(耐熱老化性試験)]
厚さ2mmの前記架橋シートを、JIS K6257に従い、180℃で70時間保持する熱老化試験を行った。熱老化試験後のシートの硬度、TBおよびEBを、前記硬度試験および引張試験の項目と同様の方法で測定した。
熱老化試験前後の硬度の差より、AH(Duro-A)を求め、熱老化試験前後のTBおよびEBから、熱老化試験前の値に対する試験後の変化率をそれぞれ、Ac(TB)、Ac(EB)として求めた。
[Heat resistance test (heat aging resistance test)]
A heat aging test was conducted on the crosslinked sheet having a thickness of 2 mm by holding it at 180° C. for 70 hours in accordance with JIS K6257. The hardness, TB and EB of the sheet after the heat aging test were measured in the same manner as in the hardness test and tensile test items.
AH (Duro-A) is determined from the difference in hardness before and after the heat aging test, and from TB and EB before and after the heat aging test, the rate of change after the test with respect to the value before the heat aging test is calculated as Ac (TB) and Ac, respectively. (EB).
[ゲーマン捻り試験(低温捻り試験)]
低温捻り試験は、JIS K6261(1993)に従って、ゲーマン捻り試験機を用いて、厚さ2mmの前記架橋シートのT2(℃)、T5(℃)、T10(℃)およびT100(℃)を測定した。これらの温度は、架橋ゴムの低温柔軟性の指標となる。例えばT2が低いほど、低温柔軟性が良好である。
[Gehman twist test (low temperature twist test)]
The low-temperature torsion test was performed using a Gehman torsion tester in accordance with JIS K6261 (1993) to determine T 2 (°C), T 5 (°C), T 10 (°C) and T 100 (°C) of the crosslinked sheet with a thickness of 2 mm. ) was measured. These temperatures are indicators of the low temperature flexibility of the crosslinked rubber. For example, the lower the T2 , the better the low temperature flexibility.
Claims (8)
カーボンブラック(B)0.1~200質量部と、
短繊維(C)と、
を含有し、
前記短繊維(C)の平均繊維長が1~20μmであり、
前記短繊維(C)の含有量は、前記共重合体(A)100質量部に対して、3~20質量部であり、
JIS Z3284に準拠し、温度25℃、Immersion speed:120mm/min、Preload:600gf、Test speed:120mm/min、Press time:60sの条件で測定したときのプローブタック試験のピーク値が394gf以上である、伝動ベルト用組成物。
(1)エチレン[A1]に由来する構造単位と、炭素数4~20のα-オレフィン[A2]に由来する構造単位とのモル比〔[A1]/[A2]〕が、40/60~90/10であり、
(2)非共役ポリエン[A3]に由来する構造単位の含有割合が、[A1]、[A2]および[A3]に由来する構造単位の合計を100モル%として、0.1~6.0モル%であり、
(3)下記式(i)で表されるB値が、1.20以上であり、
B値=([EX]+2[Y])/〔2×[E]×([X]+[Y])〕・・・(i)
[ここで[E]、[X]および[Y]は、それぞれ、エチレン[A1]、炭素数4~20のα-オレフィン[A2]、および非共役ポリエン[A3]に由来する構造単位のモル分率を示し、[EX]はエチレン[A1]-炭素数4~20のα-オレフィン[A2]ダイアッド連鎖分率を示す。]
(4’)125℃におけるムーニー粘度ML (1+4) 125℃が、3~70である。 It has a structural unit derived from ethylene [A1], a structural unit derived from an α-olefin having 4 to 20 carbon atoms [A2], and a structural unit derived from a non-conjugated polyene [A3], and has the following (1) ~100 parts by mass of an ethylene/α-olefin/non-conjugated polyene copolymer (A) that satisfies the requirements of (3) and (4') ;
0.1 to 200 parts by mass of carbon black (B) ,
short fibers (C);
Contains
The average fiber length of the short fibers (C) is 1 to 20 μm,
The content of the short fiber (C) is 3 to 20 parts by mass based on 100 parts by mass of the copolymer (A),
In accordance with JIS Z3284, the peak value of the probe tack test is 394 gf or more when measured under the conditions of temperature 25 ° C, Immersion speed: 120 mm/min, Preload: 600 gf, Test speed: 120 mm/min, Press time: 60 s. , a composition for power transmission belts.
(1) The molar ratio [[A1]/[A2]] of the structural unit derived from ethylene [A1] and the structural unit derived from α-olefin [A2] having 4 to 20 carbon atoms is 40/60 to 90/10,
(2) The content ratio of structural units derived from non-conjugated polyene [A3] is 0.1 to 6.0, assuming that the total of structural units derived from [A1], [A2] and [A3] is 100 mol%. is mole%,
(3) The B value represented by the following formula (i) is 1.20 or more,
B value = ([EX]+2[Y])/[2×[E]×([X]+[Y])]...(i)
[Here, [E], [X] and [Y] are moles of structural units derived from ethylene [A1], α-olefin having 4 to 20 carbon atoms [A2], and non-conjugated polyene [A3], respectively. [EX] indicates the ethylene [A1]-α-olefin [A2] dyad chain fraction having 4 to 20 carbon atoms. ]
(4') Mooney viscosity ML (1+4) at 125°C is 3 to 70.
(4)100℃におけるムーニー粘度ML(1+4)100℃が、5~150である。 The composition for a power transmission belt according to any one of claims 1 to 3 , wherein the ethylene/α-olefin/nonconjugated polyene copolymer (A) further satisfies the following requirement (4).
(4) Mooney viscosity ML (1+4) at 100°C is 5 to 150.
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Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2001310951A (en) | 2000-04-27 | 2001-11-06 | Bando Chem Ind Ltd | Short fiber reinforced elastomer composition for transmission belt and transmission belt |
JP2012214576A (en) | 2011-03-31 | 2012-11-08 | Mitsui Chemicals Inc | Ethylene-based copolymer, crosslinked ethylene-based copolymer and molded product thereof |
WO2016152711A1 (en) | 2015-03-20 | 2016-09-29 | 三井化学株式会社 | THERMOPLASTIC ELASTOMER COMPOSITION, USE THEREOF, METHOD FOR PRODUCING SAME, ETHYLENE/α-OLEFIN/UNCONJUGATED POLYENE COPOLYMER AND USE THEREOF |
WO2016194371A1 (en) | 2015-06-04 | 2016-12-08 | バンドー化学株式会社 | Transmission belt |
JP2018172553A (en) | 2017-03-31 | 2018-11-08 | 三井化学株式会社 | Thermoplastic elastomer composition |
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JP2001310951A (en) | 2000-04-27 | 2001-11-06 | Bando Chem Ind Ltd | Short fiber reinforced elastomer composition for transmission belt and transmission belt |
JP2012214576A (en) | 2011-03-31 | 2012-11-08 | Mitsui Chemicals Inc | Ethylene-based copolymer, crosslinked ethylene-based copolymer and molded product thereof |
WO2016152711A1 (en) | 2015-03-20 | 2016-09-29 | 三井化学株式会社 | THERMOPLASTIC ELASTOMER COMPOSITION, USE THEREOF, METHOD FOR PRODUCING SAME, ETHYLENE/α-OLEFIN/UNCONJUGATED POLYENE COPOLYMER AND USE THEREOF |
WO2016194371A1 (en) | 2015-06-04 | 2016-12-08 | バンドー化学株式会社 | Transmission belt |
JP2018172553A (en) | 2017-03-31 | 2018-11-08 | 三井化学株式会社 | Thermoplastic elastomer composition |
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