JP2016130289A - Rubber composition for water supply piping - Google Patents
Rubber composition for water supply piping Download PDFInfo
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Abstract
Description
本発明は、例えば上水道の配管に組み込んで使用される上水道配管用可とうゴム継手等の形成材料として用いる上水道配管用ゴム組成物に関するものである。 The present invention relates to a rubber composition for water supply piping used as a forming material for a flexible rubber joint for water supply piping used by being incorporated in, for example, water supply piping.
上記上水道配管用可とうゴム継手等の、上水道の配管に組み込んで用いる各種ゴム部品には、水道水中の塩素に対して劣化しにくいことが求められる。
そこで上記ゴム部品は、塩素に対する耐性に優れた架橋物を形成しうる、例えばエチレンプロピレンジエンゴム(EPDM)やスチレンブタジエンゴム(SBR)等をゴム分として含むゴム組成物によって形成するのが一般的である。
Various rubber parts used in water supply pipes such as the above-mentioned flexible rubber joints for water supply pipes are required to be hardly deteriorated by chlorine in tap water.
Therefore, the rubber component is generally formed of a rubber composition that can form a crosslinked product having excellent resistance to chlorine, such as ethylene propylene diene rubber (EPDM) or styrene butadiene rubber (SBR). It is.
また上記ゴム部品には、そのもとになるゴム組成物中に配合される架橋成分等の各種添加剤や架橋後のゴム部品中に残存する遊離炭素等の有機炭素が水道水中に浸出するのを抑制して、当該水道水の全有機炭素(TOC:Total Organic Carbon)をできるだけ低減できることも求められる。
具体的には、公益社団法人 日本水道協会が制定したJWWA Z108:2012「水道用資機材−浸出試験方法」に規定の測定方法に則って測定され、JWWA K156:2004「水道施設用ゴム材料」(一部改定後)において規定された全有機炭素が0.5mg/L以下、中でも0.2mg/L以下、特に不検出であるのが好ましい。
In addition, various additives such as crosslinking components blended in the rubber composition as a base and organic carbon such as free carbon remaining in the rubber component after crosslinking are leached into the tap water. It is also required that the total organic carbon (TOC: Total Organic Carbon) of the tap water can be reduced as much as possible.
Specifically, JWWA K156: 2004 “Rubber material for water supply facilities” was measured in accordance with the measurement method prescribed in JWWA Z108: 2012 “Water supply equipment and leaching test method” established by the Japan Water Works Association. It is preferable that the total organic carbon specified in (after partial revision) is 0.5 mg / L or less, particularly 0.2 mg / L or less, and particularly not detected.
しかし、ゴム分として例えばEPDMを含むゴム組成物からなるゴム部品では、上記ゴム分を架橋させるための架橋成分のうち特に促進剤が表面にブルームしやすいため、当該促進剤の水道水中への浸出とそれによるTOCの増加が懸念される。
そこで特許文献1では、ゴム部品としてのシール材の表面のうち水道水と直接に接触する可能性のある領域に超高分子量ポリエチレンを主成分とする樹脂フィルムをコーティングして有機炭素の水道水中への浸出を抑制することが提案されている。
However, in rubber parts made of a rubber composition containing, for example, EPDM as a rubber component, among the crosslinking components for crosslinking the rubber component, the accelerator is particularly likely to bloom on the surface, so that the accelerator is leached into tap water. There is concern about the increase in TOC.
Therefore, in Patent Document 1, a resin film mainly composed of ultrahigh molecular weight polyethylene is coated on an area of the surface of a sealing material as a rubber part that may be in direct contact with tap water, and then into organic carbon tap water. It has been proposed to suppress the leaching of slag.
しかし上記の構成では、促進剤をはじめとする水道水中への浸出が懸念される成分(有機炭素)の量が低減される訳ではないので、例えばゴム部品の構造上、その表面に樹脂フィルムをコーティングできない領域などを生じると、そこから有機炭素が水道水中に浸出してTOCが増加するおそれがある。
特許文献2には、ゴム分としてEPDMを含むゴム組成物をゴム部品の形状に成形するとともに一次架橋させたのち、さらに二次架橋させることが記載されている。
However, in the above configuration, the amount of the component (organic carbon) that is likely to be leached into tap water including the accelerator is not necessarily reduced. If an area that cannot be coated is generated, organic carbon may leach out into the tap water and the TOC may increase.
Patent Document 2 describes that a rubber composition containing EPDM as a rubber component is molded into the shape of a rubber part and subjected to primary crosslinking, followed by secondary crosslinking.
かかる構成では、有機炭素のうち一次架橋後にゴム部品中に残留する遊離炭素を二次架橋によってゴムの架橋物中に取り込んでTOCを低減できる。
また特許文献2には、架橋成分として有機過酸化物を用い、当該有機過酸化物のうち一次架橋時に未反応であった分を二次架橋時の熱によってゴム部品中から散逸させてTOCをさらに低減することも記載されている。
In such a configuration, it is possible to reduce the TOC by taking in free carbon remaining in the rubber component after the primary cross-linking among the organic carbon into the cross-linked product of the rubber by the secondary cross-linking.
Further, in Patent Document 2, an organic peroxide is used as a crosslinking component, and the TOC is obtained by dissipating the unreacted portion of the organic peroxide from the rubber component by the heat during the secondary crosslinking. Further reduction is also described.
ところが特許文献2の構成では、架橋成分として有機過酸化物でなく硫黄と促進剤とを組み合わせた場合、促進剤の浸出の問題は解消されないままである。
またゴム部品の製造に際してはゴム組成物の焼け(スコーチ)の防止も重要な課題であるが、特許文献2の構成ではかかる焼け防止についても十分に考慮されているとはいえない。
However, in the structure of Patent Document 2, when sulfur and an accelerator are combined as a crosslinking component instead of an organic peroxide, the problem of the leaching of the accelerator remains unresolved.
Further, in the production of rubber parts, prevention of scorching of the rubber composition is also an important issue, but in the configuration of Patent Document 2, it cannot be said that such prevention of scoring is sufficiently considered.
本発明の目的は、塩素に対する耐性に優れるとともに現状よりも水道水中のTOCを低減しうるゴム部品を形成できる上、現状よりも焼けを生じにくい上水道配管用ゴム組成物を提供することにある。 An object of the present invention is to provide a rubber composition for waterworks piping that is excellent in resistance to chlorine and that can form a rubber part that can reduce the TOC in tap water more than the current state, and that is less likely to be burned than the current state.
本発明は、EPDMを含むゴム分、ならびに前記ゴム分を架橋させるための架橋成分としての硫黄および促進剤を含み、前記促進剤は分子量250以上、600以下のチアゾール系促進剤およびチウラム系促進剤からなる群より選ばれた少なくとも1種である上水道配管用ゴム組成物である。 The present invention includes a rubber component containing EPDM, sulfur as a crosslinking component for crosslinking the rubber component, and an accelerator, and the accelerator includes a thiazole accelerator and a thiuram accelerator having a molecular weight of 250 or more and 600 or less. It is the rubber composition for waterworks piping which is at least 1 sort (s) chosen from the group which consists of.
本発明によれば、塩素に対する耐性に優れるとともに現状よりも水道水中のTOCを低減しうるゴム部品を形成できる上、現状よりも焼けを生じにくい上水道配管用ゴム組成物を提供できる。 ADVANTAGE OF THE INVENTION According to this invention, while being excellent in the tolerance with respect to chlorine, the rubber component which can reduce TOC in tap water rather than the present condition can be formed, and the rubber composition for waterworks piping which does not produce a burning more easily than the present condition can be provided.
《上水道配管用ゴム組成物》
本発明は、EPDMを含むゴム分、ならびに前記ゴム分を架橋させるための架橋成分としての硫黄および促進剤を含み、前記促進剤は分子量250以上、600以下のチアゾール系促進剤およびチウラム系促進剤からなる群より選ばれた少なくとも1種である上水道配管用ゴム組成物である。
<< Rubber composition for waterworks piping >>
The present invention includes a rubber component containing EPDM, sulfur as a crosslinking component for crosslinking the rubber component, and an accelerator, and the accelerator includes a thiazole accelerator and a thiuram accelerator having a molecular weight of 250 or more and 600 or less. It is the rubber composition for waterworks piping which is at least 1 sort (s) chosen from the group which consists of.
架橋成分のうち硫黄は、架橋反応によってゴムの架橋物中に取り込まれて水道水中にはほとんど浸出しない上、そもそも有機炭素にはカウントされないため、当該水道水のTOCを増加させるおそれはない。
また分子量が上記範囲にある上記2種の促進剤はいずれも、分子量が250未満である同種の促進剤や、あるいは分子量が上記範囲にあっても上記2種以外の他種の促進剤、例えばジチオカルバミン酸塩系促進剤、スルフェンアミド系促進剤などと比べて架橋速度が速すぎないため焼けを生じにくい上、架橋後のゴム部品中から水道水中に浸出しにくいため、当該水道水のTOCを増加させるおそれはない。
Of the cross-linking components, sulfur is taken into the rubber cross-linked product by the cross-linking reaction and hardly leaches into tap water, and is not counted as organic carbon in the first place, so there is no risk of increasing the TOC of the tap water.
The two kinds of accelerators having a molecular weight in the above range are both the same kind of accelerator having a molecular weight of less than 250, or other kinds of accelerators other than the above two kinds even if the molecular weight is in the above range, for example, Compared to dithiocarbamate accelerators, sulfenamide accelerators, etc., the crosslinking rate is not too fast, so it is difficult to burn, and it is difficult to leach into tap water from the rubber parts after crosslinking. There is no risk of increasing.
したがって本発明によれば、塩素に対する耐性に優れたEPDMを含むゴム分、硫黄、ならびに上記特定の分子量を有するチアゾール系促進剤および/またはチウラム系促進剤を選択して使用することにより、塩素に対する耐性に優れるとともに現状よりも水道水中のTOCを低減しうるゴム部品を形成できる上、現状よりも焼けを生じにくい上水道配管用ゴム組成物を提供できる。 Therefore, according to the present invention, by selecting and using a rubber component containing EPDM excellent in resistance to chlorine, sulfur, and a thiazole accelerator and / or thiuram accelerator having the specific molecular weight described above, It is possible to provide a rubber composition for water supply piping that is excellent in resistance and can form a rubber part that can reduce the TOC in tap water more than the current state, and that is less likely to be burned than the current state.
さらに、分子量が上記範囲にある上記2種の促進剤はいずれも、分子量が600を超える同種または他種の促進剤に比べて架橋速度が遅すぎないため、架橋に長時間を要さずゴム部品の生産性を向上できるという利点もある。
〈ゴム分〉
ゴム分としては、上述したように塩素に対する耐性に優れた架橋物を形成しうるEPDMを少なくとも用いる。
Furthermore, since both of the two types of accelerators having a molecular weight in the above range are not too slow in crosslinking speed compared to the same or other kinds of accelerators having a molecular weight of more than 600, the rubber does not require a long time for crosslinking. There is also an advantage that the productivity of parts can be improved.
<Rubber>
As the rubber component, at least EPDM capable of forming a crosslinked product having excellent resistance to chlorine as described above is used.
(EPDM)
EPDMとしては、エチレンとプロピレンに第3成分(ジエン分)を加えることで主鎖中に二重結合を導入した種々のEPDMがいずれも使用可能である。
かかるEPDMとしては、例えば第3成分の種類や量の違いによる様々な製品が提供されている。代表的な第3成分としては、例えばエチリデンノルボルネン(ENB)、1,4−ヘキサジエン(1,4−HD)、ジシクロペンタジエン(DCP)等が挙げられる。
(EPDM)
As the EPDM, any of various EPDMs in which a double bond is introduced into the main chain by adding a third component (diene component) to ethylene and propylene can be used.
As such EPDM, for example, various products are provided depending on the type and amount of the third component. Representative examples of the third component include ethylidene norbornene (ENB), 1,4-hexadiene (1,4-HD), dicyclopentadiene (DCP), and the like.
特にEPDMとしては、上記ジエン分の含量(ジエン含量)が9質量%以上であるものを用いるのが好ましく、15質量%以下であるものを用いるのが好ましい。
硫黄架橋に関与するジエン含量が上記の範囲未満であるEPDMからなるゴム部品は架橋密度が小さく、架橋後に残存する遊離炭素が多く、そして水道水中に浸出する有機炭素量が多くなってTOCを増加させるおそれがある。
In particular, EPDM is preferably one having a diene content (diene content) of 9% by mass or more, and preferably 15% by mass or less.
Rubber parts made of EPDM whose diene content involved in sulfur cross-linking is less than the above range have low cross-linking density, a large amount of free carbon remaining after cross-linking, and a large amount of organic carbon leached into tap water, increasing TOC There is a risk of causing.
一方、ジエン含量が上記の範囲を超えるEPDMからなるゴム部品は逆に架橋密度が大きくなって硬くなったり、伸びが小さくなったりするおそれがある。
これに対し、EPDMのジエン含量を上記の範囲とすることにより、ゴム部品の適度な硬さや良好な伸びを維持しながら水道水中のTOCの増加を抑制できる。
ちなみにゴム部品が前述した上水道配管用可とうゴム継手である場合、そのゴム硬さは、温度23±2℃の環境下、日本工業規格JIS K6253−3:2012「加硫ゴム及び熱可塑性ゴム−硬さの求め方−第3部:デュロメータ硬さ」所載の測定方法に則って測定されるタイプAデュロメータ硬さで表して60以上であるのが好ましく、75以下であるのが好ましい。
On the other hand, a rubber part made of EPDM having a diene content exceeding the above range, on the other hand, may have a high crosslinking density and become hard or may have a small elongation.
On the other hand, by setting the diene content of EPDM within the above range, it is possible to suppress an increase in TOC in tap water while maintaining an appropriate hardness and good elongation of the rubber part.
Incidentally, when the rubber part is the above-described flexible rubber joint for water supply pipes, the rubber hardness is as follows : Japanese Industrial Standard JIS K6253-3 : 2012 “Vulcanized rubber and thermoplastic rubber— The hardness is preferably 60 or more, more preferably 75 or less in terms of type A durometer hardness measured in accordance with the measurement method described in “Method of obtaining hardness—Part 3: Durometer hardness”.
また上記上水道配管用可とうゴム継手は、温度23±2℃の環境下、日本工業規格JIS K6251:2010「加硫ゴム及び熱可塑性ゴム−引張特性の求め方」所載の測定方法に則って測定される切断時伸びEb(%)が400%以上、特に450%以上であるのが好ましく、引張強さTS(MPa)が14MPa以上、特に16MPa以上であるのが好ましい。 In addition, the above flexible rubber joint for waterworks piping is in accordance with the measurement method described in Japanese Industrial Standard JIS K6251 : 2010 “How to Obtain Vulcanized Rubber and Thermoplastic Rubber-Tensile Properties” in an environment of a temperature of 23 ± 2 ° C. The measured elongation at break E b (%) is preferably 400% or more, particularly 450% or more, and the tensile strength TS (MPa) is preferably 14 MPa or more, particularly preferably 16 MPa or more.
またEPDMとしては、伸展油を加えて柔軟性を調整した油展タイプのものと加えない非油展タイプのものとがあるが、伸展油は有機炭素として水道水中へ浸出してTOCを増加させる原因となるため、当該TOCを極力低減することを考慮すると、EPDMとしては伸展油を含まない非油展タイプのEPDMが好ましい。
これらEPDMの1種または2種以上を使用できる。
In addition, there are two types of EPDM: oil-extended type that has been adjusted for flexibility by adding extender oil and non-oil-extended type that does not add, but extender oil leaches into tap water as organic carbon to increase TOC. Therefore, in consideration of reducing the TOC as much as possible, the EPDM is preferably a non-oil-extended EPDM that does not contain an extending oil.
One or more of these EPDMs can be used.
(他のゴム分)
ゴム分としてはEPDMを単独(2種以上のEPDMを併用する場合を含む。)で使用してもよいが、他のゴムを併用してもよい。
特にEPDMはタック性が小さく、混練工程においてオープンロールに巻き付きにくい、成形工程で金型への充てん時にゴム組成物同士の貼り合わせが難しいといった問題があるため、これらの問題を解消してゴム組成物の加工性を向上できるタック性のよいゴムと併用するのが好ましい。
(Other rubber)
As the rubber component, EPDM may be used alone (including the case where two or more kinds of EPDM are used in combination), but other rubber may be used in combination.
In particular, EPDM has a low tackiness, is difficult to wind around an open roll in a kneading process, and has a problem that it is difficult to bond rubber compositions together when filling a mold in a molding process. It is preferable to use in combination with a rubber having good tackiness that can improve the workability of the product.
かかる他のゴム分としては、EPDMとともに硫黄によって架橋できる種々のゴムが使用可能であるが、特に前述したように塩素に対する耐性に優れた架橋物を形成できるSBRが好ましい。
SBRとしては、スチレンと1,3−ブタジエンとを乳化重合法、溶液重合法等の重合法によって共重合させて合成される種々のSBRがいずれも使用可能である。
As such other rubber components, various rubbers that can be crosslinked with sulfur together with EPDM can be used, but SBR that can form a crosslinked product excellent in resistance to chlorine as described above is particularly preferable.
As the SBR, any of various SBRs synthesized by copolymerizing styrene and 1,3-butadiene by a polymerization method such as an emulsion polymerization method or a solution polymerization method can be used.
またSBRとしては、スチレン含量によって分類される高スチレンタイプ、中スチレンタイプ、および低スチレンタイプのSBRがあるがこのいずれも使用可能である。
さらにSBRとしては、伸展油を加えて柔軟性を調整した油展タイプのものと加えない非油展タイプのものとがあるが、前述したように伸展油は有機炭素として水道水中へ浸出してTOCを増加させる原因となるため、当該TOCを極力低減することを考慮すると、SBRとしては伸展油を含まない非油展タイプのSBRが好ましい。
SBR includes high styrene type, medium styrene type, and low styrene type SBR classified by styrene content, and any of these can be used.
In addition, SBR is classified into an oil-extended type in which flexibility is adjusted by adding extender oil and a non-oil-extended type in which extensibility is not added. As described above, extender oil leaches into tap water as organic carbon. In view of reducing the TOC as much as possible, the SBR is preferably a non-oil-extended type SBR that does not include an extended oil.
これらSBRの1種または2種以上を使用できる。
(配合割合)
ゴム分としてEPDMとSBRの2種を併用する場合、SBRの配合割合は、両ゴムの総量100質量部中の20質量部以上であるのが好ましく、40質量部以下であるのが好ましい。
One or more of these SBRs can be used.
(Mixing ratio)
When two types of EPDM and SBR are used in combination as the rubber component, the blending ratio of SBR is preferably 20 parts by mass or more, and preferably 40 parts by mass or less in a total amount of 100 parts by mass of both rubbers.
SBRの配合割合がこの範囲未満では、当該SBRを併用することによる、ゴム組成物の加工性を向上する効果が十分に得られないおそれがある。
一方、SBRの配合割合が上記の範囲を超える場合には、引張特性の良いEPDMの割合が相対的に少なくなるため前述した伸びEb(%)や引張強さTS(MPa)が低下する傾向がある。またSBRは。EPDMと違って主鎖に二重結合を有するため水道水中の残留塩素によって主鎖の分子切断を生じやすく、分子切断を生じると水道水中に浸出する有機炭素量が多くなってTOCが増加する傾向がある。
When the blending ratio of SBR is less than this range, the effect of improving the processability of the rubber composition by using the SBR together may not be sufficiently obtained.
On the other hand, when the blending ratio of SBR exceeds the above range, the ratio of EPDM having good tensile properties is relatively decreased, and thus the above-described elongation E b (%) and tensile strength TS (MPa) tend to decrease. There is. Also SBR. Unlike EPDM, it has a double bond in the main chain, so it tends to cause molecular cleavage of the main chain due to residual chlorine in tap water. If molecular cleavage occurs, the amount of organic carbon leached into tap water tends to increase and TOC tends to increase. There is.
これに対しSBRの配合割合を上記の範囲とすることにより、良好な引張特性を維持し、かつ水道水中のTOCの増加を抑制しながらゴム組成物の加工性を向上できる。
〈架橋成分〉
上記ゴム分を架橋させる架橋成分としては、前述したように硫黄と、分子量250以上、600以下のチアゾール系促進剤および/またはチウラム系促進剤を用いる。この理由は先に説明したとおりである。
On the other hand, by making the blending ratio of SBR within the above range, it is possible to maintain good tensile properties and improve the processability of the rubber composition while suppressing an increase in TOC in tap water.
<Crosslinking component>
As the crosslinking component for crosslinking the rubber component, as described above, sulfur and a thiazole accelerator and / or thiuram accelerator having a molecular weight of 250 to 600 are used. The reason for this is as described above.
このうち硫黄としては、ゴム分の架橋剤として機能しうる例えば粉末硫黄等が挙げられる。
上記硫黄の配合割合は、ゴム分の総量100質量部あたり1質量部以上であるのが好ましく、3質量部以下であるのが好ましい。
硫黄の配合割合がこの範囲未満ではゴム部品の架橋密度が小さく、架橋後に残存する遊離炭素が多く、そして水道水中に浸出する有機炭素量が多くなってTOCが増加するおそれがある。
Among these, as sulfur, powder sulfur etc. which can function as a crosslinking agent for rubber are mentioned.
The mixing ratio of the sulfur is preferably 1 part by mass or more and preferably 3 parts by mass or less per 100 parts by mass of the total amount of rubber.
If the blending ratio of sulfur is less than this range, the crosslinking density of rubber parts is small, there is a large amount of free carbon remaining after crosslinking, and the amount of organic carbon leached into tap water may increase and TOC may increase.
一方、硫黄の配合割合が上記の範囲を超える場合にはゴム部品の架橋密度が大きくなって前述した伸びEb(%)が低下する傾向がある。
これに対し、硫黄の配合割合を上記の範囲とすることにより、ゴム部品の良好な伸びを維持しながら水道水中のTOCの増加を抑制できる。
またチアゾール系促進剤および/またはチウラム系促進剤の分子量は、水道水中への浸出を抑制してTOCをより一層良好に低減するとともに、架橋速度を抑えて焼けをより一層生じにくくすることを考慮すると、上記の範囲でも300以上であるのが好ましい。
On the other hand, when the compounding ratio of sulfur exceeds the above range, the crosslinking density of the rubber part increases and the above-described elongation E b (%) tends to decrease.
On the other hand, the increase of the TOC in tap water can be suppressed, maintaining the favorable elongation of rubber parts by making the compounding ratio of sulfur into the above range.
In addition, the molecular weight of thiazole accelerator and / or thiuram accelerator is considered to suppress leaching into tap water to further reduce TOC, and to suppress cross-linking rate to make it more difficult to cause burning. Then, it is preferable that it is 300 or more also in said range.
分子量が250以上、600以下であるチアゾール系促進剤としては、例えば2−メルカプトベンゾチアゾールのシクロヘキシルアミン塩〔M−60OT、分子量:266.43〕、2−(4′−モルホリノジチオ)ベンゾチアゾール〔MDB、分子量:284.43〕、ジ−2−ベンゾチアゾリルジスルフィド〔DM、分子量:332.49〕、2−メルカプトベンゾチアゾールの亜鉛塩〔MZ、分子量:397.86〕等の1種または2種以上が挙げられる。 Examples of thiazole accelerators having a molecular weight of 250 or more and 600 or less include, for example, cyclohexylamine salt of 2-mercaptobenzothiazole [M-60OT, molecular weight: 266.43], 2- (4′-morpholinodithio) benzothiazole [ MDB, molecular weight: 284.43], di-2-benzothiazolyl disulfide [DM, molecular weight: 332.49], zinc salt of 2-mercaptobenzothiazole [MZ, molecular weight: 397.86] or the like or Two or more types can be mentioned.
特に分子量が300以上で、かつ金属を含まないジ−2−ベンゾチアゾリルジスルフィドが好ましい。
また分子量が250以上、600以下であるチウラム系促進剤としては、例えばテトラエチルチウラムジスルフィド〔TET、分子量:296.54〕、ジペンタメチレンチウラムテトラスルフィド〔TRA、分子量:384.69〕、テトラブチルチウラムジスルフィド〔TBT、分子量:408.75〕、テトラベンジルチウラムジスルフィド〔TBZTD、分子量:544.8〕等の1種または2種以上が挙げられる。
In particular, di-2-benzothiazolyl disulfide having a molecular weight of 300 or more and containing no metal is preferable.
Examples of the thiuram accelerator having a molecular weight of 250 or more and 600 or less include, for example, tetraethylthiuram disulfide [TET, molecular weight: 296.54], dipentamethylene thiuram tetrasulfide [TRA, molecular weight: 384.69], tetrabutylthiuram. One type or two or more types of disulfide [TBT, molecular weight: 408.75], tetrabenzylthiuram disulfide [TBZTD, molecular weight: 544.8] and the like can be mentioned.
特に分子量が300以上で、かつ適度の架橋速度を有するテトラブチルチウラムジスルフィドが好ましい。
上記チアゾール系促進剤および/またはチウラム系促進剤の配合割合は、ゴム分の総量100質量部あたり1質量部以上であるのが好ましく、2.5質量部以下であるのが好ましい。
In particular, tetrabutyl thiuram disulfide having a molecular weight of 300 or more and an appropriate crosslinking rate is preferable.
The blending ratio of the thiazole accelerator and / or the thiuram accelerator is preferably 1 part by mass or more and preferably 2.5 parts by mass or less per 100 parts by mass of the total amount of rubber.
促進剤の配合割合がこの範囲未満ではゴム部品の架橋密度が小さく、架橋後に残存する遊離炭素が多く、そして水道水中に浸出する有機炭素量が多くなってTOCが増加するおそれがある。
一方、促進剤の配合割合が上記の範囲を超える場合にはゴム部品の架橋密度が大きくなって前述した伸びEb(%)が低下したり、水道水中に浸出する有機炭素量が多くなってTOCが増加したりする傾向がある。
When the blending ratio of the accelerator is less than this range, the crosslinking density of the rubber part is small, there is a large amount of free carbon remaining after the crosslinking, and the amount of organic carbon leached into the tap water increases, which may increase the TOC.
On the other hand, when the blending ratio of the accelerator exceeds the above range, the crosslinking density of the rubber parts is increased and the above-described elongation E b (%) is decreased, or the amount of organic carbon leached into the tap water is increased. There is a tendency for TOC to increase.
これに対し、促進剤の配合割合を上記の範囲とすることにより、ゴム部品の良好な伸びを維持しながら水道水中のTOCの増加を抑制できる。
なお促進剤の配合割合は、2種以上のチアゾール系促進剤および/またはチウラム系促進剤を併用する場合はその合計の配合割合を上記の範囲とするのが好ましい。
〈その他の成分〉
本発明の上水道配管用ゴム組成物には、さらに必要に応じてカーボンブラックなどの補強剤、オイル等の軟化剤、酸化亜鉛やステアリン酸等の促進助剤などの種々の添加剤を、適宜の割合で配合してもよい。
On the other hand, by setting the blending ratio of the accelerator within the above range, it is possible to suppress an increase in TOC in tap water while maintaining good elongation of the rubber parts.
It should be noted that the blending ratio of the accelerator is preferably set to the above range when the two or more thiazole accelerators and / or thiuram accelerators are used in combination.
<Other ingredients>
The rubber composition for water supply pipes of the present invention may further contain various additives such as a reinforcing agent such as carbon black, a softening agent such as oil, and an auxiliary promoter such as zinc oxide and stearic acid as necessary. You may mix | blend in a ratio.
上記本発明の上水道配管用ゴム組成物は、例えば上記各成分のうちゴム分に、まず架橋成分以外の成分を配合して混練したのち、架橋成分を加えて混練する等して調製できる。
《ゴム部品》
本発明の上水道配管用ゴム組成物は、前述した上水道配管用可とうゴム継手の形成材料として好適に使用できる。かかる上水道配管用可とうゴム継手は、例えば両端に金属等からなるフランジが連結されるとともに内部に布等からなる補強層が埋設された略筒状等に形成される。
The rubber composition for water supply piping of the present invention can be prepared, for example, by first mixing and kneading components other than the crosslinking component to the rubber component of the above components, and then kneading the mixture by adding the crosslinking component.
<Rubber parts>
The rubber composition for water supply piping of the present invention can be suitably used as a material for forming the above-described flexible rubber joint for water supply piping. Such a flexible rubber joint for water supply piping is formed, for example, in a substantially cylindrical shape in which flanges made of metal or the like are connected to both ends and a reinforcing layer made of cloth or the like is embedded therein.
また本発明の上水道配管用ゴム組成物は、上記上水道配管用可とうゴム継手以外の種々の、上水道の配管に組み込んで使用するゴム部品の形成材料として用いることもできる。
かかる他のゴム部品としては、例えば上水道配管の管継手部やバルブ等に組み込まれるシール材やパッキン、あるいはバルブの弁体やダイヤフラム等が挙げられる。
上水道配管用可とうゴム継手等のゴム部品はいずれも、上記本発明の上水層配管用ゴム組成物を用いること以外は従来同様にして製造できる。
The rubber composition for water supply piping of the present invention can also be used as a material for forming rubber parts that are incorporated into various types of water supply piping other than the above flexible rubber joint for water supply piping.
Examples of such other rubber parts include seal materials and packings incorporated into pipe joints and valves of water supply pipes, valve bodies and diaphragms of valves, and the like.
Any rubber parts such as flexible rubber joints for water supply piping can be produced in the same manner as in the prior art except that the rubber composition for water supply piping according to the present invention is used.
すなわち上水道配管用ゴム組成物をプレス成形法、押出成形法、射出成型法等の任意の成形法によって所定のゴム部品の形状に成形するとともにゴム分を架橋させることでゴム部品が製造される。 That is, a rubber component is produced by forming a rubber composition for water supply piping into a predetermined rubber component shape by an arbitrary molding method such as a press molding method, an extrusion molding method, or an injection molding method and crosslinking the rubber component.
〈実施例1〉
ゴム分としてはEPDM〔住友化学(株)製のエスプレン(登録商標)505A、非油展タイプ、ジエン含量:9.5質量%、エチレン含量:50質量%〕70質量部、およびSBR〔JSR(株)製のJSR(登録商標)1502〕30質量部を用いた。
上記ゴム分の総量100質量部を、バンバリミキサを用いて素練りしながら下記表1に示す各成分のうち粉末硫黄と促進剤DM以外の各成分を加えて150℃で5分間混練したのち、さらに2軸オープンロールを用いて、粉末硫黄および促進剤を加えて70℃で5分間混練して水道配管用ゴム組成物を調製した。
<Example 1>
The rubber content is 70 parts by weight of EPDM (Esprene (registered trademark) 505A manufactured by Sumitomo Chemical Co., Ltd., non-oil-extended type, diene content: 9.5% by mass, ethylene content: 50% by mass), and SBR [JSR ( Co., Ltd. JSR (registered trademark) 1502] 30 parts by mass was used.
After kneading 100 parts by mass of the total amount of the rubber component using a Banbury mixer and adding components other than powdered sulfur and accelerator DM among the components shown in Table 1 below, kneading at 150 ° C. for 5 minutes, and further Using a biaxial open roll, powdered sulfur and an accelerator were added and kneaded at 70 ° C. for 5 minutes to prepare a water pipe rubber composition.
表1中の各成分は下記のとおり。また表中の質量部はゴム分の総量100質量部あたりの質量部を示す。
粉末硫黄:鶴見化学工業(株)製
促進剤DM:ジ−2−ベンゾチアゾリルジスルフィド、チアゾール系、分子量:332.49、大内新興化学工業(株)製のノクセラー(登録商標)DM
酸化亜鉛2種:三井金属鉱業(株)製
ステアリン酸:日油(株)製の商品名つばき
カーボンブラック:HAF、東海カーボン(株)製のシースト3
オイル:出光興産(株)製のダイアナ(登録商標)プロセスオイルPW380
〈実施例2〉
促進剤DMに代えて、同量の促進剤TBT〔テトラブチルチウラムジスルフィド、チウラム系、分子量:408.75、大内新興化学工業(株)製のノクセラーTBT−N〕を配合したこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
Each component in Table 1 is as follows. Moreover, the mass part in a table | surface shows the mass part per 100 mass parts of total amounts of rubber | gum content.
Powder sulfur: Tsurumi Chemical Co., Ltd. accelerator DM: Di-2-benzothiazolyl disulfide, thiazole, molecular weight: 332.49, Nouchira (registered trademark) DM manufactured by Ouchi Shinsei Chemical Co., Ltd.
2 types of zinc oxide: manufactured by Mitsui Mining & Smelting Co., Ltd. Stearic acid: Tsubaki, manufactured by NOF Corporation Carbon black: HAF, Seast 3 manufactured by Tokai Carbon Co., Ltd.
Oil: Diana (registered trademark) process oil PW380 manufactured by Idemitsu Kosan Co., Ltd.
<Example 2>
Implemented except that the same amount of accelerator TBT [tetrabutylthiuram disulfide, thiuram, molecular weight: 408.75, Noxeller TBT-N manufactured by Ouchi Shinsei Chemical Co., Ltd.] was used instead of the accelerator DM. In the same manner as in Example 1, a rubber composition for water pipes was prepared.
〈実施例3〉
促進剤DMに代えて、同量の促進剤TET〔テトラエチルチウラムジスルフィド、チウラム系、分子量:296.54、大内新興化学工業(株)製のノクセラーTET〕を配合したこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
〈実施例4〉
EPDMとして、住友化学(株)製のエスプレン501A〔非油展タイプ、ジエン含量:4質量%、エチレン含量:52質量%〕を同量配合したこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
<Example 3>
Example 1 except that the same amount of accelerator TET [tetraethylthiuram disulfide, thiuram, molecular weight: 296.54, Noxeller TET manufactured by Ouchi Shinsei Chemical Co., Ltd.] was used instead of the accelerator DM. Similarly, a rubber composition for water pipes was prepared.
<Example 4>
EPDM 501A manufactured by Sumitomo Chemical Co., Ltd. (non-oil-extended type, diene content: 4% by mass, ethylene content: 52% by mass) was used as EPDM in the same manner as in Example 1 except for the same amount. A rubber composition was prepared.
〈実施例5〜9〉
促進剤DMの配合割合を、ゴム分の総量100質量部あたり0.5質量部(実施例5)、1.0質量部(実施例6)、2.5質量部(実施例7)、3.0質量部(実施例8)、および4.0質量部(実施例9)としたこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
<Examples 5-9>
The mixing ratio of the accelerator DM is 0.5 parts by mass (Example 5), 1.0 part by mass (Example 6), 2.5 parts by mass (Example 7) per 100 parts by mass of the total amount of rubber. A rubber composition for water supply piping was prepared in the same manner as in Example 1 except that the content was 0.0 parts by mass (Example 8) and 4.0 parts by mass (Example 9).
〈実施例10〜13〉
粉末硫黄の配合割合を、ゴム分の総量100質量部あたり0.5質量部(実施例10)、1.0質量部(実施例11)、3.0質量部(実施例12)、および3.5質量部(実施例13)としたこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
〈実施例14〉
EPDMの配合割合を90質量部、SBRの配合割合を10質量部としたこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
<Examples 10 to 13>
The blending ratio of powder sulfur is 0.5 parts by mass (Example 10), 1.0 part by mass (Example 11), 3.0 parts by mass (Example 12), and 3 parts per 100 parts by mass of the total amount of rubber. A rubber composition for water pipes was prepared in the same manner as in Example 1 except that the content was 5 parts by mass (Example 13).
<Example 14>
A rubber composition for water supply piping was prepared in the same manner as in Example 1 except that the blending ratio of EPDM was 90 parts by mass and the blending ratio of SBR was 10 parts by mass.
〈実施例15〉
EPDMの配合割合を80質量部、SBRの配合割合を20質量部としたこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
〈実施例16〉
EPDMの配合割合を60質量部、SBRの配合割合を40質量部としたこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
<Example 15>
A rubber composition for water supply piping was prepared in the same manner as in Example 1 except that the blending ratio of EPDM was 80 parts by mass and the blending ratio of SBR was 20 parts by mass.
<Example 16>
A rubber composition for water supply piping was prepared in the same manner as in Example 1 except that the blending ratio of EPDM was 60 parts by mass and the blending ratio of SBR was 40 parts by mass.
〈実施例17〉
EPDMの配合割合を50質量部、SBRの配合割合を50質量部としたこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
〈比較例1〉
促進剤DMに代えて、同量の促進剤M〔2−メルカプトベンゾチアゾール、チアゾール系、分子量:167.25、大内新興化学工業(株)製のノクセラーM〕を配合したこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
<Example 17>
A rubber composition for water supply piping was prepared in the same manner as in Example 1 except that the blending ratio of EPDM was 50 parts by mass and the blending ratio of SBR was 50 parts by mass.
<Comparative example 1>
Example except that the same amount of the promoter M [2-mercaptobenzothiazole, thiazole, molecular weight: 167.25, Noxeller M manufactured by Ouchi Shinsei Chemical Industry Co., Ltd.] was blended in place of the promoter DM. In the same manner as in No. 1, a rubber composition for water pipes was prepared.
〈比較例2〉
促進剤DMに代えて、促進剤TOT−N〔テトラキス(2−エチルヘキシル)チウラムジスルフィド、チウラム系、分子量:633.18、大内新興化学工業(株)製のノクセラーTOT−N〕をゴム分の総量100質量部あたり3.0質量部配合したこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
<Comparative example 2>
Instead of the accelerator DM, the accelerator TOT-N [tetrakis (2-ethylhexyl) thiuram disulfide, thiuram, molecular weight: 633.18, NOCELLER TOT-N manufactured by Ouchi Shinsei Chemical Co., Ltd.] A rubber composition for water supply piping was prepared in the same manner as in Example 1 except that 3.0 parts by mass per 100 parts by mass of the total amount was blended.
〈比較例3〉
促進剤DMに代えて、促進剤TS〔テトラメチルチウラムモノスルフィド、チウラム系、分子量:208.37、大内新興化学工業(株)製のノクセラーTS〕をゴム分の総量100質量部あたり0.5質量部配合したこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
<Comparative Example 3>
In place of the accelerator DM, an accelerator TS [tetramethylthiuram monosulfide, thiuram, molecular weight: 208.37, Noxeller TS manufactured by Ouchi Shinsei Chemical Co., Ltd.] is added to the rubber content of 100 parts by mass. A rubber composition for water supply piping was prepared in the same manner as in Example 1 except that 5 parts by mass was blended.
〈比較例4〉
促進剤DMに代えて、促進剤BZ〔ジブチルジチオカルバミン酸亜鉛、ジチオカルバミン酸塩系、分子量:474.15、大内新興化学工業(株)製のノクセラーBZ〕をゴム分の総量100質量部あたり1.0質量部配合したこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
<Comparative example 4>
Instead of the accelerator DM, the accelerator BZ [zinc dibutyldithiocarbamate, dithiocarbamate, molecular weight: 474.15, Noxeller BZ manufactured by Ouchi Shinsei Chemical Co., Ltd.] is added per 100 parts by mass of the total rubber content. A rubber composition for water supply piping was prepared in the same manner as in Example 1 except that 0.0 part by mass was blended.
〈比較例5〉
促進剤DMに代えて、促進剤MSA〔N−オキシジエチレン−2−ベンゾチアゾリルスルフェンアミド、スルフェンアミド系、分子量:252.36、大内新興化学工業(株)製のノクセラーMSA−G〕をゴム分の総量100質量部あたり1.0質量部配合したこと以外は実施例1と同様にして水道配管用ゴム組成物を調製した。
<Comparative Example 5>
In place of the accelerator DM, the accelerator MSA [N-oxydiethylene-2-benzothiazolylsulfenamide, sulfenamide-based, molecular weight: 252.36, Noxeller MSA-G manufactured by Ouchi Shinsei Chemical Co., Ltd. A rubber composition for water supply piping was prepared in the same manner as in Example 1 except that 1.0 part by mass per 100 parts by mass of the total amount of rubber was blended.
〈スコーチタイム〉
各実施例、比較例で調製した未架橋の水道配管用ゴム組成物について、焼けの生じにくさの基準であるスコーチタイムを、日本工業規格JIS K6300−1:2013「未加硫ゴム−物理特性−第1部:ムーニー粘度計による粘度及びスコーチタイムの求め方」所載の測定方法に則って測定した。
スコーチタイムはスコーチタイム10分未満、または測定不能を「×」、10分以上、15分未満を「○」、15分以上を「◎」と評価した。
<Scorch time>
With respect to the rubber composition for uncrosslinked water pipes prepared in each example and comparative example, the scorch time, which is a standard for the difficulty of burning, was determined according to Japanese Industrial Standard JIS K6300-1: 2013 “Unvulcanized Rubber—Physical Properties —Part 1: Measurement of viscosity and scorch time using Mooney viscometer ”.
The scorch time was evaluated as a scorch time of less than 10 minutes, or an unmeasurable value of “×”, 10 minutes or more, less than 15 minutes as “◯”, and 15 minutes or more as “◎”.
〈引張特性〉
各実施例、比較例で調製した未架橋の水道配管用ゴム組成物をシート状に成形し、140℃×50分間プレス架橋させてシート状のサンプルを作製した。
<Tensile properties>
The uncrosslinked rubber composition for water pipes prepared in each Example and Comparative Example was formed into a sheet shape, and press-crosslinked at 140 ° C. for 50 minutes to prepare a sheet-like sample.
次いでこのサンプルを打ち抜いて、前出の日本工業規格JIS K6251:2010「加硫ゴム及び熱可塑性ゴム−引張特性の求め方」において規定されたダンベル状3号形試験片を作製し、温度23±2℃の環境下、同規格に規定された引張試験をして切断時伸びEb(%)、および引張強さTS(MPa)を求めた。
切断時伸びEbは400%未満を「×」、400%以上、450%未満を「○」、450%以上を「◎」と評価した。
また引張強さTSは14MPa未満を「×」、14MPa以上、16MPa未満を「○」、16MPa以上を「◎」と評価した。
Next, this sample was punched out to produce a dumbbell-shaped No. 3 test piece defined in the above-mentioned Japanese Industrial Standard JIS K6251 : 2010 “vulcanized rubber and thermoplastic rubber—how to obtain tensile properties”, and a temperature of 23 ± Under an environment of 2 ° C., a tensile test defined in the same standard was performed to determine elongation at break E b (%) and tensile strength TS (MPa).
The elongation at break Eb was evaluated as “x” when less than 400%, “◯” when 400% or more, less than 450%, and “◎” when 450% or more.
In addition, the tensile strength TS was evaluated as “x” when less than 14 MPa, “◯” when less than 14 MPa, “◯” when less than 16 MPa, and “◎” when more than 16 MPa.
〈ゴム硬さ〉
上記シート状のサンプルのタイプAデュロメータ硬さを、温度23±2℃の環境下、前出の日本工業規格JIS K6253−3:2012「加硫ゴム及び熱可塑性ゴム−硬さの求め方−第3部:デュロメータ硬さ」所載の測定方法に則って測定した。
タイプAデュロメータ硬さは60未満または75超をいずれも「×」、60〜75を「◎」と評価した。
<Rubber hardness>
The type A durometer hardness of the above sheet-like sample was measured under the environment of a temperature of 23 ± 2 ° C. The above-mentioned Japanese Industrial Standard JIS K6253-3 : 2012 “Vulcanized rubber and thermoplastic rubber—How to obtain hardness—No. It was measured according to the measurement method described in “Part 3: Durometer hardness”.
The type A durometer hardness was evaluated as “x” when less than 60 or more than 75, and “◎” when 60-75.
〈TOC〉
上記シート状のサンプルのTOCを、温度23±2℃の環境下、前出のJWWA Z108:2012「水道用資機材−浸出試験方法」に則って測定し、JWWA K156:2004「水道施設用ゴム材料」(一部改定後)の規定に従って0.5mg/L超を「×」、0.5mg/L以下で0.2mg/L超を「○」、0.2mg/L以下または不検出を「◎」と評価した。
<TOC>
The TOC of the sheet-like sample was measured in an environment of a temperature of 23 ± 2 ° C. in accordance with the above-mentioned JWWA Z108: 2012 “Water Supply Equipment / Leaching Test Method”. JWWA K156: 2004 “Rubber for Water Supply Facilities” In accordance with the provisions of “Materials” (after partial revision), over 0.5 mg / L is “x”, 0.5 mg / L or less is over 0.2 mg / L is “O”, 0.2 mg / L or less or no detection Evaluated as “◎”.
以上の結果を表2〜表5に示す。 The above results are shown in Tables 2 to 5.
表2〜表5の実施例1〜17、比較例1〜5の結果より、塩素に対する耐性に優れるとともに現状よりも水道水中のTOCを低減しうるゴム部品を、焼けを生じることなく形成するためには、架橋成分として硫黄と、分子量250以上、600以下のチアゾール系促進剤および/またはチウラム系促進剤とを併用する必要があることが判った。
また実施例1〜3の結果より、上記効果をより一層向上するためには、チアゾール系促進剤および/またはチウラム系促進剤の分子量は上記範囲でも300以上であるのが好ましいこと、チアゾール系促進剤としてはジ−2−ベンゾチアゾリルジスルフィドが好ましいこと、チウラム系促進剤としてはテトラブチルチウラムジスルフィドが好ましいことが判った。
From the results of Examples 1 to 17 and Comparative Examples 1 to 5 in Tables 2 to 5, in order to form a rubber component that is excellent in resistance to chlorine and can reduce TOC in tap water more than the current state without causing burning. It has been found that it is necessary to use sulfur as a crosslinking component in combination with a thiazole accelerator and / or a thiuram accelerator having a molecular weight of 250 or more and 600 or less.
In addition, from the results of Examples 1 to 3, in order to further improve the above effect, the molecular weight of the thiazole accelerator and / or thiuram accelerator is preferably 300 or more in the above range, and the thiazole accelerator. It was found that di-2-benzothiazolyl disulfide is preferable as the agent, and tetrabutylthiuram disulfide is preferable as the thiuram accelerator.
実施例1、4の結果より、ゴム部品の適度な硬さや良好な伸びを維持しながら水道水中のTOCの増加を抑制するためには、EPDMのジエン含量が9質量%以上であるのが好ましく、15質量%以下であるのが好ましいことが判った。
また実施例1、5〜9の結果より、ゴム部品の良好な伸びを維持しながら水道水中のTOCの増加を抑制するためには、分子量250以上、600以下のチアゾール系促進剤および/またはチウラム系促進剤の配合割合は、ゴム分の総量100質量部あたり1質量部以上であるのが好ましく、2.5質量部以下であるのが好ましいことが判った。
From the results of Examples 1 and 4, the diene content of EPDM is preferably 9% by mass or more in order to suppress the increase in TOC in tap water while maintaining appropriate hardness and good elongation of rubber parts. It was found that the content is preferably 15% by mass or less.
From the results of Examples 1 and 5 to 9, in order to suppress the increase in TOC in tap water while maintaining good elongation of rubber parts, a thiazole accelerator having a molecular weight of 250 or more and 600 or less and / or thiuram. It was found that the blending ratio of the system accelerator is preferably 1 part by mass or more per 100 parts by mass of the total amount of rubber, and preferably 2.5 parts by mass or less.
さらに実施例1、10〜13の結果より、ゴム部品の良好な伸びを維持しながら水道水中のTOCの増加を抑制するためには、硫黄の配合割合は、ゴム分の総量100質量部あたり1質量部以上であるのが好ましく、3質量部以下であるのが好ましいことが判った。
そして実施例1、14〜17の結果より、ゴム分としてEPDMとSBRを併用した系では、良好な引張特性を維持し、かつ水道水中のTOCの増加を抑制しながらゴム組成物の加工性を向上するために、SBRの配合割合が、両ゴムの総量100質量部中の20質量部以上であるのが好ましく、40質量部以下であるのが好ましいことが判った。
Furthermore, from the results of Examples 1 and 10 to 13, in order to suppress the increase in TOC in tap water while maintaining good elongation of rubber parts, the mixing ratio of sulfur is 1 per 100 parts by mass of the total amount of rubber. It was found that the amount was preferably not less than part by mass, and preferably not more than 3 parts by mass.
And from the results of Examples 1 and 14 to 17, in the system using both EPDM and SBR as rubber components, the processability of the rubber composition is maintained while maintaining good tensile properties and suppressing the increase in TOC in tap water. In order to improve, it turned out that it is preferable that the mixture ratio of SBR is 20 mass parts or more in 100 mass parts of total amount of both rubbers, and it is preferable that it is 40 mass parts or less.
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JPS6053547A (en) * | 1983-09-05 | 1985-03-27 | Bridgestone Corp | Low-odor rubber |
JPH09157447A (en) * | 1995-12-08 | 1997-06-17 | Inoac Corp | Rubber compound, molded rubber article, ring-shaped water-stopping material and production of ring-shaped water-stopping material |
JP2005068271A (en) * | 2003-08-22 | 2005-03-17 | Tazaki Asahi:Kk | Rubber composition stable to chlorine water |
JP2013035964A (en) * | 2011-08-09 | 2013-02-21 | Sumitomo Rubber Ind Ltd | Rubber composition for tire and pneumatic tire |
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JPS6053547A (en) * | 1983-09-05 | 1985-03-27 | Bridgestone Corp | Low-odor rubber |
JPH09157447A (en) * | 1995-12-08 | 1997-06-17 | Inoac Corp | Rubber compound, molded rubber article, ring-shaped water-stopping material and production of ring-shaped water-stopping material |
JP2005068271A (en) * | 2003-08-22 | 2005-03-17 | Tazaki Asahi:Kk | Rubber composition stable to chlorine water |
JP2013035964A (en) * | 2011-08-09 | 2013-02-21 | Sumitomo Rubber Ind Ltd | Rubber composition for tire and pneumatic tire |
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