JPH08239484A - Production of rubber composition containing short reinforcing fiber - Google Patents
Production of rubber composition containing short reinforcing fiberInfo
- Publication number
- JPH08239484A JPH08239484A JP6691395A JP6691395A JPH08239484A JP H08239484 A JPH08239484 A JP H08239484A JP 6691395 A JP6691395 A JP 6691395A JP 6691395 A JP6691395 A JP 6691395A JP H08239484 A JPH08239484 A JP H08239484A
- Authority
- JP
- Japan
- Prior art keywords
- polymer
- short fibers
- fibers
- rubber composition
- reinforcing
- 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.)
- Granted
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は補強用短繊維を含有する
ゴム組成物の製造方法に係り、詳しくは補強用短繊維の
分散を良くしたゴム組成物の製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a rubber composition containing reinforcing short fibers, and more particularly to a method for producing a rubber composition in which reinforcing short fibers are dispersed well.
【０００２】[0002]
【従来の技術】補強用短繊維を含有するゴム組成物は、
短繊維による異方性、耐摩耗性等の特性を利用してＶベ
ルト、Ｖリブドベルト等の動力伝動用ベルトを始めとし
て種々の分野で利用されている。特に、繰り返し圧縮力
を受ける動力伝動用ベルトにおいて短繊維を分散させた
ゴム組成物を使用した場合には、短繊維の分散が悪く塊
で残っていると、その部分が亀裂の核となってベルト故
障の原因になっている。2. Description of the Related Art A rubber composition containing reinforcing short fibers is
It is used in various fields including power transmission belts such as V-belts and V-ribbed belts by utilizing properties such as anisotropy and wear resistance due to short fibers. In particular, when a rubber composition in which short fibers are dispersed in a power transmission belt that receives repeated compressive force is used, if the short fibers are poorly dispersed and remain in lumps, that portion becomes a nucleus of cracks. It is causing the belt failure.
【０００３】今日、密閉式混練機を用いて補強用短繊維
を含有するゴム組成物を練る方法としては、例えば
（１）まずポリマーと補強用短繊維を混合して短繊維混
入マスターバッチを作製した後、補強剤（カーボンブラ
ック等）、充填剤、軟化剤、老化防止剤、加硫促進剤、
加硫剤等を練り込んで所定のゴム組成物とする方法、
（２）マトリックスとなるコンパウンドを作製してお
き、そのコンパウンドに補強用短繊維を練り込んで所定
のゴム組成物とする方法、（３）補強用短繊維を少量の
ポリマー、軟化剤、補強剤と混合して高濃度の短繊維混
入マスターバッチを作製し、これをマトリックスとなる
コンパウンドと混合して分散させる方法がある。Today, as a method of kneading a rubber composition containing reinforcing short fibers by using a closed kneader, for example, (1) first, a polymer and reinforcing short fibers are mixed to prepare a short fiber-mixed master batch. After that, reinforcing agent (carbon black etc.), filler, softening agent, antioxidant, vulcanization accelerator,
A method of kneading a vulcanizing agent or the like into a predetermined rubber composition,
(2) A method of preparing a compound to be a matrix and kneading the reinforcing short fibers into the compound to obtain a predetermined rubber composition, (3) a small amount of reinforcing short fibers of a polymer, a softening agent, and a reinforcing agent. There is a method in which a high-concentration short fiber-mixed master batch is prepared by mixing with, and this is mixed with a compound serving as a matrix and dispersed.
【０００４】また、特公平４−１７９５０９号公報に
は、無撚り長繊維束をエラストマー溶液中に浸漬した
後、乾燥することで、エラストマーが内部まで浸入した
長繊維収束体を作製し、その後この長繊維収束体を切断
してエラストマー被覆短繊維をしたのち、これをマトリ
ックスとなるエラストマー中に混入し、分散して短繊維
の分散性を向上させた方法は開示されている。In Japanese Patent Publication No. 4-179509, untwisted long fiber bundles are dipped in an elastomer solution and then dried to prepare long fiber bundles in which the elastomer penetrates to the inside. A method has been disclosed in which long fiber bundles are cut into elastomer-coated short fibers, which are then mixed in an elastomer serving as a matrix and dispersed to improve the dispersibility of the short fibers.
【０００５】[0005]
【発明が解決しようとする課題】しかし、（１）の方法
のようにポリマーと短繊維だけを練る場合、短繊維の分
散を良くするために、練り時間を長くすれば、混合物の
温度が上がり、そのためポリマーの粘度が落ちて短繊維
に剪断力がかからなくなり、短繊維の分散は良くならな
い。また、短繊維の長さが長くなるにしたがい、短繊維
がほぐれていく過程で綿状の塊になりやすく、一度この
塊となれば、練り時間を長くしても塊はなかなかほぐれ
なくなる問題があった。However, when only the polymer and the short fibers are kneaded as in the method (1), the temperature of the mixture is increased by prolonging the kneading time in order to improve the dispersion of the short fibers. Therefore, the viscosity of the polymer is reduced and the shearing force is not applied to the short fibers, so that the dispersion of the short fibers is not good. In addition, as the length of the short fibers becomes longer, it tends to become a cotton-like lump in the process of loosening the short fibers, and once it becomes this lump, even if the kneading time is lengthened, the lump does not easily come loose. there were.
【０００６】また、（２）の方法のようにマトリックス
となるコンパウンドに短繊維を練り込む場合、上記
（１）の方法に比べて短繊維に剪断力がかかりやすくな
るが、温度上昇が大きく、粘度も大きく低下する結果、
短繊維に充分な剪断力がかからなくなるばかりでなく、
硫黄変成タイプのクロロプレンゴムのように熱だけで加
硫してしまうものでは、練り−冷却のサイクルを繰り返
す必要があり、多大の労力を要していた。When the short fibers are kneaded into the matrix compound as in the method (2), the short fibers are more likely to be subjected to shearing force than the method (1), but the temperature rise is large. As a result of a large decrease in viscosity,
Not only does the short fiber not have sufficient shearing force,
In the case of a sulfur-modified type chloroprene rubber that is vulcanized only by heat, it is necessary to repeat the kneading-cooling cycle, which requires a great deal of labor.
【０００７】また、（３）の方法のように高濃度の短繊
維混入マスターバッチを作製する方法では、マスターバ
ッチを作製する過程では前述のような（１）あるいは
（２）の方法による問題が生じる。また、高濃度の短繊
維混入マスターバッチとこれと混合するコンパウンドの
粘度が大きく異なる場合には、マスターバッチがコンパ
ウンド中に均一に分散しないという問題があった。更
に、カーボンブラックを短繊維と同時に投入した場合に
は、繊維の間に入り込んだカーボンブラックがゴム中に
均一に分散せず、カーボンブラックと短繊維が固まった
塊が残ることになる。Further, in the method for producing a high-concentration short fiber-mixed masterbatch as in the method (3), the problems due to the method (1) or (2) described above occur in the process of producing the masterbatch. Occurs. Further, when the viscosity of the high-concentration short fiber-mixed master batch and the compound mixed therewith are greatly different, there is a problem that the master batch is not uniformly dispersed in the compound. Furthermore, when carbon black is added at the same time as the short fibers, the carbon black that has entered between the fibers is not uniformly dispersed in the rubber, and a lump in which the carbon black and the short fibers are solidified remains.
【０００８】本発明はこのような問題点を改善するもの
であり、補強用短繊維を含有するゴム組成物を練る際
に、出来るだけ労力をかけずに短繊維の分散を良くした
補強用短繊維を含有するゴム組成物の製造方法を提供す
ることを目的とする。The present invention is intended to solve such problems, and when kneading a rubber composition containing reinforcing short fibers, the short reinforcing fibers are dispersed with the least effort as much as possible. An object of the present invention is to provide a method for producing a rubber composition containing fibers.
【０００９】[0009]
【課題を解決するための手段】即ち、本発明と特徴とす
るところは、予めポリマー、補強用短繊維と軟化剤を混
練し、補強用短繊維をポリマー中に分散させた後、しか
る後再度上記マスターバッチに補強剤、充填剤、老化防
止剤、加硫促進剤、加硫剤等を練り込む補強用短繊維を
含有するゴム組成物の製造方法にある。また、本発明は
ポリマー、補強用短繊維と軟化剤を混練し、補強用短繊
維をポリマー中に分散させた後、いったん得られた混練
物のマスターバッチを冷却する工程も含む。また、ポリ
マーがクロロプレンゴムに限定される場合も含む。Means for Solving the Problems That is, the present invention is characterized in that a polymer, a reinforcing short fiber and a softening agent are kneaded in advance to disperse the reinforcing short fiber in the polymer, and then again. It is a method for producing a rubber composition containing reinforcing short fibers in which a reinforcing agent, a filler, an antioxidant, a vulcanization accelerator, a vulcanizing agent and the like are kneaded into the masterbatch. The present invention also includes a step of kneading the polymer, the reinforcing short fibers and the softening agent, dispersing the reinforcing short fibers in the polymer, and then cooling the masterbatch of the once kneaded product. It also includes the case where the polymer is limited to chloroprene rubber.
【００１０】本発明では、ポリマーと補強用短繊維を混
練する際に、軟化剤を添加することにより、短繊維とポ
リマーのなじみが良くなり、ポリマー中への分散が良く
なるばかりか、短繊維自体が絡み合って綿状になるのを
防ぐ効果がある。即ち、軟化剤が短繊維に浸透し、素繊
維同士の絡み合いがほぐれるための潤滑剤としての役割
をはたし、短繊維が綿状になるの阻止し、かつ短繊維と
ポリマーのなじみが良くなって短繊維の分散が良くな
る。In the present invention, by adding a softening agent when the polymer and the reinforcing short fibers are kneaded, the short fibers and the polymer are made to fit well and the dispersion in the polymer is improved, and the short fibers are also improved. It has the effect of preventing itself from becoming entangled and becoming cotton-like. That is, the softening agent penetrates into the short fibers, plays a role as a lubricant for loosening the entanglement of the elementary fibers, prevents the short fibers from becoming cotton-like, and well fits the short fibers and the polymer. The dispersion of short fibers is improved.
【００１１】本発明で使用するポリマーとしては、天然
ゴム、ＳＢＲ（スチレン・ブタジエンゴム）、硫黄変性
または非硫黄変性のクロロプレンゴム、アクリロニトリ
ル・ブタジエンゴム、ＨＮＢＲ（水素化ニトリルゴ
ム）、ＥＰＤＭ（エチレン・プロピレン・ジエンモノマ
ー）、あるいはオレフィン系、エステル系、ウレタン系
の熱可塑性エラストマーが使用される。The polymers used in the present invention include natural rubber, SBR (styrene-butadiene rubber), sulfur-modified or non-sulfur-modified chloroprene rubber, acrylonitrile-butadiene rubber, HNBR (hydrogenated nitrile rubber), EPDM (ethylene-butadiene rubber). Propylene / diene monomer), or an olefin-based, ester-based, or urethane-based thermoplastic elastomer is used.
【００１２】また、補強用短繊維としては、アラミド、
ナイロン、ポリエステル、ビニロン、レーヨン、綿等で
ある。通常、この短繊維の長さは０．１〜１０ｍｍであ
り、素繊維径が数μ〜数１０μｍであるが、特に本発明
では素繊維径が細く、かつ繊維長が長くて、繊維同士が
絡まり綿状になりやすい短繊維に有効である。As the reinforcing short fibers, aramid,
Examples include nylon, polyester, vinylon, rayon, and cotton. Usually, the length of this short fiber is 0.1 to 10 mm, and the diameter of the elementary fiber is several μm to several tens of μm. In particular, in the present invention, the elementary fiber diameter is small and the fiber length is long, and the fibers are Effective for short fibers that tend to become entangled and cotton-like.
【００１３】軟化剤としては、一般的なゴム用の可塑
剤、例えばジブチルフタレート（ＤＢＰ）、ジオクチル
フタレート（ＤＯＰ）等のフタレート系、ジオクチルア
ジペート（ＤＯＡ）等のアジペート系、ジオクチルセバ
ケート（ＤＯＳ）等のセバケート系、トリクレジルホス
フェート等のホスフェートなど、あるいは一般的な石油
系の軟化剤が含まれる。上記軟化剤の添加量は、短繊維
の１０ｖｏｌ％以上、好ましくは短繊維の３０ｖｏｌ％
以上である。１０ｖｏｌ％未満の場合には、軟化剤が短
繊維全体に行き渡らず、分散の悪い部分が生じる可能性
がある。As the softening agent, a general plasticizer for rubber, for example, phthalate type such as dibutyl phthalate (DBP) and dioctyl phthalate (DOP), adipate type such as dioctyl adipate (DOA), dioctyl sebacate (DOS). Such as sebacate type, tricresyl phosphate and other phosphates, and general petroleum type softeners. The amount of the softening agent added is 10 vol% or more of the short fibers, preferably 30 vol% of the short fibers.
That is all. If it is less than 10 vol%, the softening agent may not spread over the entire short fibers, and a portion with poor dispersion may occur.
【００１４】更に、本発明のゴム組成物には、カーボン
ブラックからなる補強剤、充填剤、老化防止剤、加硫促
進剤、加硫剤等が添加される。Further, a reinforcing agent made of carbon black, a filler, an antioxidant, a vulcanization accelerator, a vulcanizing agent and the like are added to the rubber composition of the present invention.
【００１５】本発明では、まず第１ステップのマスター
バッチ練りとして、バンバリミキサーのような密閉式混
練機に、ポリマー１００重量部に１０〜４０重量部の補
強用短繊維と１〜１０重量部の軟化剤を投入して混練し
た後、混練したマスターバッチをいったん放出し、これ
を２０〜５０°Ｃまで冷却する。これはクロロプレンゴ
ムのスコーチを防止するためである。次いで、得られた
マスターバッチに所定量の補強剤、充填剤、老化防止
剤、加硫促進剤、加硫剤等をバンバリミキサー、オープ
ンロールを用いて仕上げ練りする。しかし、ポリマーに
よっては混練したマスターバッチをいったん放出し、冷
却する必要はなく、連続して仕上げ練りを行うことも可
能である。In the present invention, as the first step of masterbatch kneading, in a closed kneader such as a Banbury mixer, 10-40 parts by weight of reinforcing short fibers and 1-10 parts by weight of 100 parts by weight of polymer are used. After adding a softening agent and kneading, the kneaded master batch is once discharged and cooled to 20 to 50 ° C. This is to prevent scorch of the chloroprene rubber. Then, the obtained masterbatch is subjected to finish kneading with a predetermined amount of a reinforcing agent, a filler, an antioxidant, a vulcanization accelerator, a vulcanizing agent and the like using a Banbury mixer and an open roll. However, depending on the polymer, it is not necessary to discharge the kneaded masterbatch once and to cool it, and it is also possible to carry out finish kneading continuously.
【００１６】[0016]
【実施例】以下、本発明を実施例にて詳細に説明する。 実施例１〜２、比較例１〜２（配合Ａ） 実施例３〜４、比較例３〜４（配合Ｂ） 表１に示す配合Ａ、Ｂを下記の方法により混練してゴム
組成物を得た。The present invention will be described below in detail with reference to examples. Examples 1-2, Comparative Examples 1-2 (Compound A) Examples 3-4, Comparative Examples 3-4 (Compound B) Compounds A and B shown in Table 1 were kneaded by the following method to give a rubber composition. Obtained.
【００１７】[0017]
【表１】 [Table 1]
【００１８】マスターバッチ練りを行うため、表２に示
す配合物をＢＲバンバリミキサーに投入し、ラムウエイ
トを下げて加圧し、回転数４０ｒｐｍで１８０秒混練し
た後、ラムウエイトを上げて掃除を行い、更にラムウエ
イトを下げて１８０秒間混練し、混練物のマスターバッ
チを落下させた。この時、落下したマスターバッチの表
面状態を観察した。落下したマスターバッチを４０°Ｃ
まで冷却した。そして、仕上げ練りを行うため、上記冷
却したマスターバッチを表２に示す配合により同じＢＲ
バンバリミキサーに投入して、先ず６０秒間混練し、更
にカーボンブラック等を添加して１８０秒間混練し、更
に加硫剤、加硫促進剤を添加して１２０秒間混練してゴ
ム組成物を落下させた。得られたゴム組成物の物性評価
と得られたゴム組成物の短繊維の塊残り数を調べた。短
繊維の塊残り数の測定では、３ｃｍ×１４ｃｍの試料を
１６０°Ｃ、２０分で加硫し、この表面をグライダーで
研磨し、表面に存在する１ｍｍ以上の短繊維の塊残り数
を計数した。この結果を表４に示す。In order to carry out masterbatch kneading, the compounds shown in Table 2 were put into a BR Banbury mixer, the ram weight was lowered and pressurized, and after kneading at a rotation speed of 40 rpm for 180 seconds, the ram weight was raised to perform cleaning. Then, the ram weight was further lowered and kneading was performed for 180 seconds, and the master batch of the kneaded product was dropped. At this time, the surface state of the dropped masterbatch was observed. 40 ° C of the falling masterbatch
Cooled down. Then, in order to perform finish kneading, the cooled masterbatch was blended in the same BR with the formulation shown in Table 2.
Pour into a Banbury mixer, first knead for 60 seconds, further add carbon black etc. and knead for 180 seconds, further add vulcanizing agent and vulcanization accelerator and knead for 120 seconds to drop the rubber composition. It was The physical properties of the obtained rubber composition were evaluated, and the number of short fiber lumps remaining in the obtained rubber composition was examined. In the measurement of the number of remaining short fiber lumps, a sample of 3 cm × 14 cm was vulcanized at 160 ° C. for 20 minutes, the surface was ground by a glider, and the number of remaining short fiber lumps of 1 mm or more was counted. did. Table 4 shows the results.
【００１９】[0019]
【表２】 [Table 2]
【００２０】[0020]
【表３】 [Table 3]
【００２１】[0021]
【表４】 [Table 4]
【００２２】この結果、実施例の方法によって得られた
ゴム組成物は、短繊維の塊の残り数が少なく、短繊維の
分散が良好であることが判る。As a result, it can be seen that the rubber compositions obtained by the methods of Examples have a small number of short fiber lumps remaining, and that the short fibers are well dispersed.
【００２３】実施例５〜７、比較例５〜７（練り時間の
効果） 表５に示すように、マスターバッチの練り時間を変化さ
せて、実施例１と同様にゴム組成物を得た。得られたゴ
ム組成物の短繊維の塊残り数を調べた。短繊維の塊残り
数の測定では、３ｃｍ×１４ｃｍの試料を１６０°Ｃ、
２０分で加硫し、この表面をグライダーで研磨し、表面
に存在する直径１ｍｍ以上の短繊維の塊残り数を計数し
た。その結果を表５に併記する。Examples 5 to 7 and Comparative Examples 5 to 7 (Effect of kneading time) As shown in Table 5, the kneading time of the master batch was changed to obtain rubber compositions in the same manner as in Example 1. The number of remaining short fibers in the obtained rubber composition was examined. For the measurement of the number of remaining short fiber lumps, a sample of 3 cm × 14 cm was measured at 160 ° C.
After 20 minutes of vulcanization, the surface was ground with a glider, and the number of lumps of short fibers having a diameter of 1 mm or more present on the surface was counted. The results are also shown in Table 5.
【００２４】[0024]
【表５】 [Table 5]
【００２５】この結果、練り時間を長くすると、短繊維
の塊の残り数が少なく、短繊維の分散が良好になるが、
実施例にようにマスターバッチの練り段階でポリマー、
短繊維、軟化剤を混練する方法で練った方が比較例より
も明らかに良い水準を維持していることが判る。As a result, when the kneading time is increased, the number of remaining short fiber lumps is small and the short fibers are well dispersed.
Polymer in the kneading stage of the masterbatch, as in the examples
It can be seen that the kneading by the method of kneading the short fibers and the softening agent clearly maintains a better level than the comparative example.
【００２６】[0026]
【発明の効果】以上のように本発明では、ポリマーと補
強用短繊維を混練する際に、軟化剤を添加することによ
り、短繊維とポリマーのなじみが良くなり、ポリマー中
への分散が良くなるばかりか、短繊維自体の絡み合って
綿状になるのを防ぐ効果がある。As described above, in the present invention, when the polymer and the reinforcing short fibers are kneaded, by adding a softening agent, the short fibers and the polymer are well-familiarized and well dispersed in the polymer. In addition, it has the effect of preventing the short fibers themselves from becoming entangled and becoming cotton-like.
Claims (3)
混練し、補強用短繊維をポリマー中に分散させた後、し
かる後再度上記マスターバッチに補強剤、充填剤、老化
防止剤、加硫促進剤、加硫剤等を練り込むことを特徴と
する補強用短繊維を含有するゴム組成物の製造方法。1. A polymer, reinforcing short fibers and a softening agent are kneaded in advance to disperse the reinforcing short fibers in the polymer, and then the master batch is again added with a reinforcing agent, a filler, an antioxidant and an additive. A process for producing a rubber composition containing reinforcing short fibers, which comprises kneading a vulcanization accelerator, a vulcanizing agent and the like.
し、補強用短繊維をポリマー中に分散させた後、いった
ん得られた混練物のマスターバッチを冷却する請求項１
記載の補強用短繊維を含有するゴム組成物の製造方法。2. The polymer, the reinforcing short fibers and the softening agent are kneaded, the reinforcing short fibers are dispersed in the polymer, and then the masterbatch of the kneaded product once obtained is cooled.
A method for producing a rubber composition containing the reinforcing short fiber described above.
項１または２記載の補強用短繊維を含有するゴム組成物
の製造方法。3. The method for producing a rubber composition containing reinforcing short fibers according to claim 1, wherein the polymer is chloroprene rubber.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6691395A JP2963639B2 (en) | 1995-02-28 | 1995-02-28 | Method for producing rubber composition containing short reinforcing fibers |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6691395A JP2963639B2 (en) | 1995-02-28 | 1995-02-28 | Method for producing rubber composition containing short reinforcing fibers |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08239484A true JPH08239484A (en) | 1996-09-17 |
| JP2963639B2 JP2963639B2 (en) | 1999-10-18 |
Family
ID=13329693
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6691395A Expired - Fee Related JP2963639B2 (en) | 1995-02-28 | 1995-02-28 | Method for producing rubber composition containing short reinforcing fibers |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2963639B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013015373A1 (en) | 2011-07-28 | 2013-01-31 | 日本ゼオン株式会社 | Nitrile-group-containing highly saturated copolymer rubber composition |
| US10215257B2 (en) | 2014-04-17 | 2019-02-26 | Asahi Kasei Kabushiki Kaisha | Short rubber reinforcement fiber, rubber composition containing said short fiber, and power transmission belt |
-
1995
- 1995-02-28 JP JP6691395A patent/JP2963639B2/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013015373A1 (en) | 2011-07-28 | 2013-01-31 | 日本ゼオン株式会社 | Nitrile-group-containing highly saturated copolymer rubber composition |
| KR20140047656A (en) | 2011-07-28 | 2014-04-22 | 제온 코포레이션 | Nitrile-group-containing highly saturated copolymer rubber composition |
| US10988609B2 (en) | 2011-07-28 | 2021-04-27 | Zeon Corporation | Nitrile group-containing highly saturated copolymer rubber composition |
| US10215257B2 (en) | 2014-04-17 | 2019-02-26 | Asahi Kasei Kabushiki Kaisha | Short rubber reinforcement fiber, rubber composition containing said short fiber, and power transmission belt |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2963639B2 (en) | 1999-10-18 |
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