JP2006016624A - Manufacturing method of hydrogenated nbr mixture blended with reclaimed rubber - Google Patents
Manufacturing method of hydrogenated nbr mixture blended with reclaimed rubber Download PDFInfo
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Abstract
Description
本発明は、再生ゴム混合水素化ＮＢＲ混合物の製造方法に関する。更に詳しくは、実用に耐え得る再生ゴムを混合した再生ゴム混合水素化ＮＢＲ混合物の製造方法に関する。 The present invention relates to a method for producing a recycled rubber mixed hydrogenated NBR mixture. More specifically, the present invention relates to a method for producing a recycled rubber mixed hydrogenated NBR mixture in which a recycled rubber that can withstand practical use is mixed.
加硫スクラップゴムの再生には、オープンスチーム法(パン法)、ダイジェスター法(蒸解法)、メカニカル法(機械法)、ＵＨＦ加熱脱硫法等が従来から知られているが、これらの方法では脱硫缶、蒸解缶、リクレーメーター、スーパーミキサー、ＵＨＦ加熱処理装置等が用いられ、高温もしくは高圧条件下で処理するため、多大のエネルギー消費を必要とするばかりではなく、刺激臭や高温という作業環境の改善を求める声も大きい。 For the regeneration of vulcanized scrap rubber, the open steam method (bread method), digester method (digestion method), mechanical method (mechanical method), UHF heat desulfurization method, etc. have been conventionally known. Desulfurization cans, digesters, reclaim meters, super mixers, UHF heat treatment equipment, etc. are used, and because they are processed under high temperature or high pressure conditions, they not only require a lot of energy consumption, but also work of irritating odors and high temperatures There are also many calls for environmental improvements.
即ち、加硫ゴムを可塑化し、再生する方法では、しゃく解剤(分子を切断するように作用する化学的軟化剤；ペプタイザー)、オイル等の再生処理剤を用い、高温、高圧処理を行うため、再生工程で刺激臭があり、得られた再生ゴムをバージンゴムに混合すると、再生処理剤の混入を避けることができず、このため再生ゴムをバージンゴムに多量に混合すると物性の低下がみられ、再生ゴムを混合したゴム材料の使用用途が限定されることになる。 That is, in a method of plasticizing and regenerating vulcanized rubber, a reprocessing agent such as a peptizer (chemical softener that acts to cut molecules; a peptizer), oil, etc., is used for high temperature and high pressure processing If there is an irritating odor in the recycling process and the resulting recycled rubber is mixed with virgin rubber, it is not possible to avoid the mixing of the regeneration treatment agent. Therefore, the usage of the rubber material mixed with recycled rubber is limited.
また、加硫ゴムを可塑化し、再生する対象は、廃タイヤであることが多く、これらは天然ゴムやＳＢＲ等イオウ加硫されたゴムであり、しかるに一般に過酸化物架橋された水素化ＮＢＲの可塑化方法としては、前記各方法は適当な方法とはいえない。更に、水素化ＮＢＲは、それ自体高価格であり、その架橋ゴム廃棄物の有効利用は、コスト削減および環境問題の観点から、重要な課題となっている。 In addition, the object to plasticize and recycle vulcanized rubber is often waste tires, which are natural rubber and sulfur vulcanized rubber such as SBR, and are generally made of peroxide-crosslinked hydrogenated NBR. As a plasticizing method, the above-mentioned methods are not appropriate methods. Furthermore, hydrogenated NBR is itself expensive, and effective use of its crosslinked rubber waste is an important issue from the viewpoint of cost reduction and environmental problems.
本発明の目的は、実用に耐え得る再生ゴムを混合した水素化ＮＢＲ混合物の製造方法を提供することにある。 An object of the present invention is to provide a method for producing a hydrogenated NBR mixture in which a recycled rubber that can withstand practical use is mixed.
かかる本発明の目的は、架橋した水素化ＮＢＲに過酸化水素を加え、加圧加熱処理し、好ましくはその後機械的せん断力を加えることにより得られた可塑化された再生水素化ＮＢＲをバージン水素化ＮＢＲに混合する再生ゴム混合水素化ＮＢＲ混合物の製造方法によって達成される。 An object of the present invention is to add virgin hydrogenated plasticized regenerated NBR obtained by adding hydrogen peroxide to cross-linked hydrogenated NBR, subjecting it to pressure heat treatment, and preferably applying mechanical shearing force thereafter. This is achieved by a method for producing a recycled rubber-mixed hydrogenated NBR mixture that is mixed with the hydrogenated NBR.
架橋水素化ＮＢＲ、特にパーオキサイド架橋水素化ＮＢＲは、しゃく解剤、オイル等の再生処理剤による可塑化が困難であり、またこれらの再生処理剤を加えて処理すると、再生前後でゴムの配合組成が変り、バージンゴムに再生ゴムを混合した場合物性等の特性が変り、ゴム製品の要求品質によっては再生ゴムの混合割合を増やすことができなくなる場合もあるが、本発明方法で用いられる再生ゴムは、これをバージンゴムと混合して架橋した場合にバージンゴム単体と同程度の品質を維持することができる。このことは、再生ゴムの使用用途の適用範囲を拡げるばかりではなく、廃棄物の有効利用およびコストの削減をも達成させる。 Cross-linked hydrogenated NBR, especially peroxide cross-linked hydrogenated NBR, is difficult to plasticize with regenerative treatment agents such as peptizers and oils. When the composition changes and when recycled rubber is mixed with virgin rubber, properties such as physical properties change, and depending on the required quality of the rubber product, it may not be possible to increase the mixing ratio of recycled rubber, but the recycled used in the method of the present invention The rubber can maintain the same quality as the virgin rubber alone when it is mixed with the virgin rubber and crosslinked. This not only expands the scope of application of recycled rubber, but also achieves effective use of waste and cost reduction.
かかる再生ゴム混合水素化ＮＢＲ混合物の使用用途としては、Oリング、パッキン等のシール材の成形材料としてだけではなく、水素化ＮＢＲが一般に用いられている各種用途への展開を可能とする。 The use of the recycled rubber mixed hydrogenated NBR mixture enables not only as a molding material for sealing materials such as O-rings and packings, but also to various uses where hydrogenated NBR is generally used.
可塑化処理される架橋水素化ＮＢＲは、水素化ＮＢＲを有機過酸化物またはイオウで架橋したものであり、水素化ＮＢＲとしては、分子主鎖中の不飽和結合量を約30%以下、好ましくは約10%以下にしたＮＢＲ水素化物であって、そのムーニー粘度ML１＋４(100℃)が約50〜85程度のものが一般に用いられるが、100以上のものも用いることができる。 The crosslinked hydrogenated NBR to be plasticized is obtained by crosslinking hydrogenated NBR with an organic peroxide or sulfur. As the hydrogenated NBR, the amount of unsaturated bonds in the molecular main chain is preferably about 30% or less, preferably Is an NBR hydride having a Mooney viscosity ML 1 + 4 (100 ° C.) of about 50 to 85, although it is generally about 10% or less, and 100 or more can also be used.
実際の処理対象物は、加硫成形した際のバリ、屑、不良成形品等であり、可塑化処理前に予め粉砕しておくと、取扱性が良くなるばかりではなく、可塑化に要する時間を短縮できるので好ましいことである。 Actual processing objects are burrs, scraps, defective molded products, etc. when vulcanized and molded, and if pulverized in advance before plasticizing treatment, not only will handling be improved, but also the time required for plasticization Can be shortened, which is preferable.
可塑化処理に用いられる過酸化水素としては、約３〜40%の濃度のものが用いられ、一般には35%過酸化水素水が用いられる。35%過酸化水素水の場合、それは架橋水素化ＮＢＲ100重量部当り約10重量部以上、好ましくは約20〜100重量部の割合で用いられる。過酸化水素水の量がこれよりも少ないと、可塑化時間を長くする必要があり、一方これ以上の割合で用いられると、可塑化時間は短かくできるものの、再生ゴム中に含まれる水分量が多くなり、それの乾燥に時間がかかるようになる。また、過酸化水素水の濃度の大小についても、同様の傾向がみられる。 As the hydrogen peroxide used for the plasticizing treatment, those having a concentration of about 3 to 40% are used, and generally 35% hydrogen peroxide water is used. In the case of 35% hydrogen peroxide solution, it is used at a ratio of about 10 parts by weight or more, preferably about 20 to 100 parts by weight per 100 parts by weight of the crosslinked hydrogenated NBR. If the amount of hydrogen peroxide solution is less than this, it is necessary to lengthen the plasticizing time. On the other hand, if it is used at a higher rate, the amount of water contained in the recycled rubber can be shortened. And it will take longer to dry. Moreover, the same tendency is seen also about the magnitude | size of the concentration of hydrogen peroxide water.
過酸化水素は、加熱処理により水と活性酸素とに分解し、その過程で架橋水素化ＮＢＲを分解し、可塑化、軟化させる。この過酸化水素水による可塑化処理は、加圧加熱条件下で行われる。加圧は、オートクレーブ等の密閉容器を用い、それを加熱することにより加圧された状態で用いられる。密閉容器内の圧力は、用いられた過酸化水素水の量が多い程高くなるが、5Kg/cm２程度でも十分に可塑化することができ、一般には約2〜50Kg/cm２の圧力が適用される。加熱条件は、約100〜200℃で約5〜48時間、好ましくは約120〜180℃で約10〜24時間程度であり、加熱温度を高くすれば加熱時間を短かくすることができる。 Hydrogen peroxide is decomposed into water and active oxygen by heat treatment, and in the process, the crosslinked hydrogenated NBR is decomposed and plasticized and softened. The plasticizing treatment with the hydrogen peroxide solution is performed under pressure and heating conditions. The pressurization is performed in a pressurized state by using a closed container such as an autoclave and heating it. The pressure inside the sealed container increases as the amount of the hydrogen peroxide solution used increases, but it can be sufficiently plasticized even at about 5 kg / cm 2 , and generally the pressure is about 2 to 50 kg / cm 2 . Applied. The heating conditions are about 100 to 200 ° C. for about 5 to 48 hours, preferably about 120 to 180 ° C. for about 10 to 24 hours. If the heating temperature is increased, the heating time can be shortened.
可塑化処理後、ゴムに水を多く含む場合には、機械的脱水処理あるいは恒温槽やオーブン等による乾燥処理が行われる。水を多く含まない場合には、水の除去処理を行うことなく、そのまま用いることもできる。 When the rubber contains a large amount of water after the plasticizing process, a mechanical dehydration process or a drying process using a thermostat or oven is performed. When not containing much water, it can be used as it is without removing the water.
可塑化処理を終えたゴムには、ロール、押出機等を用いて機械的せん断を加えることが好ましい。ロールとしては、高炭素クロム軸受鋼ドリルド構造を有するリファイナーロールが、また押出機としては２軸押出機が好んで用いられる。このような機械的せん断力を適用すると、可塑化および軟化した表面が平滑な再生ゴムが得られるようになる。 The rubber after the plasticizing treatment is preferably subjected to mechanical shearing using a roll, an extruder or the like. A refiner roll having a high carbon chromium bearing steel drilled structure is preferably used as the roll, and a twin-screw extruder is preferably used as the extruder. When such a mechanical shear force is applied, a recycled rubber having a smooth plasticized and softened surface can be obtained.
このようにして得られる再生ゴム中には、架橋反応を阻害するような成分が含まれていないため、そこに有機過酸化物等の架橋剤や架橋促進剤を新たに加えることにより、バージンゴムと同様に再架橋することができる。 Since the recycled rubber obtained in this way does not contain any components that inhibit the crosslinking reaction, a virgin rubber can be added by newly adding a crosslinking agent such as an organic peroxide or a crosslinking accelerator. It can be re-crosslinked in the same way.
この再生ゴムには、バージンゴムが混合されて用いられる。この再生ゴムをバージンゴム100重量部当り5〜300重量部、好ましくは5〜150重量部混合して用いても、バージンゴム単体から得られた架橋物と比較して、加硫物性や耐熱性の点で何ら遜色のない架橋物を得ることができる。 This recycled rubber is used by mixing virgin rubber. Even if this recycled rubber is used in a mixture of 5 to 300 parts by weight, preferably 5 to 150 parts by weight, per 100 parts by weight of virgin rubber, compared with a crosslinked product obtained from a virgin rubber alone, vulcanized physical properties and heat resistance In this respect, it is possible to obtain a crosslinked product that is inferior to that of the other.
次に、実施例について本発明を説明する。 Next, the present invention will be described with reference to examples.
実施例
水素化ＮＢＲ(日本ゼオン製品ゼットポール1020) 100重量部
ＳＲＦカーボンブラック 30 〃
酸化亜鉛 5 〃
ステアリン酸 0.5 〃
1,2-ポリブタジエン(MW2000) 2 〃
アジピン酸系エーテルエステル可塑剤(粘度20cps) 5 〃
ジフェニルアミン系老化防止剤 1.5 〃
イミダゾール系老化防止剤 1.5 〃
ジクミルパーオキサイド 8 〃
以上の各成分を3Lニーダおよびオープンロールを用いて混練し、混練物について180℃、６分間のプレス加硫を行ない、加硫バリをロール間隔を0.1mm、ロール温度を40℃に調整した10インチ型リファイナーロール機に10回程度通し、粗粉砕を行った。
Example Hydrogenated NBR (Nippon Zeon product Zetpol 1020) 100 parts by weight SRF carbon black 30 〃
Zinc oxide 5 〃
Stearic acid 0.5 〃
1,2-polybutadiene (MW2000) 2 〃
Adipic acid ether plasticizer (viscosity 20cps) 5 〃
Diphenylamine anti-aging agent 1.5 〃
Imidazole-based anti-aging agent 1.5 〃
Dicumyl peroxide 8 〃
The above components were kneaded using a 3 L kneader and an open roll, and the kneaded product was subjected to press vulcanization at 180 ° C. for 6 minutes. The coarse pulverization was performed about 10 times through an inch type refiner roll machine.
この粗粉砕架橋水素化ＮＢＲ100重量部に対して35%過酸化水素水40重量部を加えた後オートクレーブ中に入れ、150℃で15時間の加熱処理を行った。加熱処理後オートクレーブを開放し、空冷もしくは水冷する。 After adding 40 parts by weight of 35% aqueous hydrogen peroxide to 100 parts by weight of the coarsely pulverized crosslinked hydrogenated NBR, the mixture was placed in an autoclave and heat-treated at 150 ° C. for 15 hours. After the heat treatment, open the autoclave and cool with air or water.
このようにして可塑化処理を終えたゴムを、120℃の恒温槽で15分間乾燥した後、ロール間隔を0.1mm、ロール温度を40℃に調整した10インチ型リファイナーロール機に20回通し、その後ロールに巻き付け、５分間の切り返しを行ない、練りを加えた。ロール間隔を1mmにして分出しを行った結果、バージンゴムシートと同様の表面状態を有する再生ゴムシートが得られた。この再生ゴムシートの刺激臭は、少なかった。 After the rubber thus plasticized was dried for 15 minutes in a constant temperature bath at 120 ° C., it was passed 20 times through a 10-inch refiner roll machine in which the roll interval was adjusted to 0.1 mm and the roll temperature was adjusted to 40 ° C. Then, it was wound around a roll, turned back for 5 minutes, and kneaded. As a result of dispensing with a roll interval of 1 mm, a recycled rubber sheet having the same surface state as the virgin rubber sheet was obtained. The irritating odor of this recycled rubber sheet was small.
得られた再生ゴムの可塑化の程度を評価するため、レオメーターＯＤＲ(180℃)の最低トルク値を測定すると、11Kgf・cmという値が得られた。 When the minimum torque value of the rheometer ODR (180 ° C.) was measured to evaluate the degree of plasticization of the obtained recycled rubber, a value of 11 kgf · cm was obtained.
次に、バージンゴム153.5重量部に対して40重量部または80重量部の再生ゴムを配合し、混練、プレス加硫(180℃、６分間)したものについて、常態物性の測定ならびに空気加熱老化試験(120℃、70時間後の常態物性の変化)を行ない、次のような結果を得た。
測定・試験項目 バージンゴム 再生ゴム40部 再生ゴム80部
[常態物性]
硬さ (JIS A) 75 77 78
引張強さ (MPa) 22.8 24.7 24.5
伸び (%) 238 236 246
[空気加熱老化試験]
硬さ変化 (ポイント) +7 +5 +6
引張強さ変化率 (%) +12 +10 +16
伸び変化率 (%) -10 -15 -15
Next, 40% by weight or 80% by weight of recycled rubber is blended with 153.5 parts by weight of virgin rubber, kneaded and press vulcanized (180 ° C., 6 minutes), and measurement of normal properties and air heat aging test (Changes in normal physical properties after 120 hours at 120 ° C.) were performed, and the following results were obtained.
Measurement / Test Items Virgin rubber recycled rubber 40 parts Recycled rubber 80 parts
[Normal physical properties]
Hardness (JIS A) 75 77 78
Tensile strength (MPa) 22.8 24.7 24.5
Elongation (%) 238 236 246
[Air heating aging test]
Change in hardness (points) +7 +5 +6
Tensile strength change rate (%) +12 +10 +16
Elongation change rate (%) -10 -15 -15
参考例１
実施例において、オートクレーブ中での加熱処理条件を120℃、15時間に変更した。再生ゴムシートの刺激臭は少なく、ＯＤＲ(180℃)最低トルク値は40Kgf・cmであった。
Reference example 1
In the examples, the heat treatment conditions in the autoclave were changed to 120 ° C. for 15 hours. The recycled rubber sheet had little irritating odor, and the ODR (180 ° C.) minimum torque value was 40 kgf · cm.
参考例２
実施例において、オートクレーブ中での加熱処理条件を150℃、5時間に変更した。再生ゴムシートの刺激臭は少なく、ＯＤＲ(180℃)最低トルク値は25Kgf・cmであった。
Reference example 2
In the examples, the heat treatment conditions in the autoclave were changed to 150 ° C. for 5 hours. The recycled rubber sheet had little irritating odor, and the ODR (180 ° C.) minimum torque value was 25 kgf · cm.
参考例３
水素化ＮＢＲ(ゼットポール1020) 100重量部
ＦＥＦカーボンブラック 40 〃
酸化亜鉛 5 〃
ステアリン酸 0.5 〃
ジフェニルアミン系老化防止剤 1.5 〃
イオウ 0.5 〃
チウラム系加硫促進剤（大内新興化学製品ノクセラーTRA） 0.7 〃
チウラム系加硫促進剤（同社製品ノクセラーTT） 0.7 〃
チアゾール系加硫促進剤（同社製品ノクセラーM） 0.5 〃
以上の各成分を実施例１と同様に混練し、160℃、14分間プレス加硫を行った後、以下実施例１と同様の条件で粉砕、加圧加熱処理およびリファイナーロールによる練りが行われた。再生ゴムシートの刺激臭は少なく、ＯＤＲ(180℃)最低トルク値は15Kgf・cmであった。
Reference example 3
Hydrogenated NBR (Zetpole 1020) 100 parts by weight FEF carbon black 40 〃
Zinc oxide 5 〃
Stearic acid 0.5 〃
Diphenylamine anti-aging agent 1.5 〃
Sulfur 0.5 〃
Thiuram vulcanization accelerator (Ouchi Emerging Chemicals Noxeller TRA) 0.7 〃
Thiuram accelerator (Noxeller TT product) 0.7 同 社
Thiazole-based vulcanization accelerator (Noxeller M, the company's product) 0.5 〃
The above components were kneaded in the same manner as in Example 1 and press vulcanized at 160 ° C. for 14 minutes. It was. The recycled rubber sheet had little irritating odor, and the ODR (180 ° C.) minimum torque value was 15 kgf · cm.
参考比較例１
実施例１の粗粉砕架橋水素化ＮＢＲ100重量部にトルクレジルホスフェート可塑剤40重量部を加え、実施例１と同様な可塑化処理を行った。得られた再生ゴムシートの表面には凹凸があり、また再生ゴムには大きな刺激臭がみられた。なお、ＯＤＲ(180℃)最低トルク値の測定は不可能であった。
Reference Comparative Example 1
40 parts by weight of torque resilate phosphate plasticizer was added to 100 parts by weight of the coarsely pulverized crosslinked hydrogenated NBR of Example 1, and the same plasticizing treatment as in Example 1 was performed. The surface of the obtained recycled rubber sheet was uneven, and the recycled rubber had a large irritating odor. Note that it was impossible to measure the ODR (180 ° C.) minimum torque value.
参考比較例２
比較例１において、更に混合ジアリルジスルフィドしゃく解剤(精工化学製品MR-906)が添加して用いられたが、全く同様な結果しか得られなかった。
Reference Comparative Example 2
In Comparative Example 1, a mixed diallyl disulfide peptizer (Seiko Chemical Product MR-906) was added and used, but only the same results were obtained.
参考比較例３
比較例１において、トリクレジルホスフェートの代りに同量の蒸留水が用いられた。得られた再生ゴムシート表面の凹凸は大で、ただし再生ゴムの刺激臭は少なかった。なお、ＯＤＲ(180℃)最低トルク値の測定は不可能であった。
Reference Comparative Example 3
In Comparative Example 1, the same amount of distilled water was used instead of tricresyl phosphate. The surface of the recycled rubber sheet obtained was large, but the irritating odor of the recycled rubber was small. Note that it was impossible to measure the ODR (180 ° C.) minimum torque value.
参考比較例４
実施例１において、過酸化水素水を加えての加熱処理が行われなかった。得られた再生ゴムシート表面の凹凸は大で、ただし再生ゴムの刺激臭は少なかった。なお、ＯＤＲ(180℃)最低トルク値の測定は不可能であった。
Reference Comparative Example 4
In Example 1, the heat treatment with the addition of hydrogen peroxide water was not performed. The surface of the recycled rubber sheet obtained was large, but the irritating odor of the recycled rubber was small. Note that it was impossible to measure the ODR (180 ° C.) minimum torque value.
Claims (3)
A recycled rubber mixed hydrogenated NBR mixture obtained by the method according to claim 1 or 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2005281708A JP4207945B2 (en) | 2005-09-28 | 2005-09-28 | Method for producing hydrogenated NBR mixture containing recycled rubber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2005281708A JP4207945B2 (en) | 2005-09-28 | 2005-09-28 | Method for producing hydrogenated NBR mixture containing recycled rubber |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21219798A Division JP3870567B2 (en) | 1998-07-28 | 1998-07-28 | Method for producing crosslinked hydrogenated NBR recycled rubber |
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| JP2006016624A true JP2006016624A (en) | 2006-01-19 |
| JP4207945B2 JP4207945B2 (en) | 2009-01-14 |
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| JP2005281708A Expired - Fee Related JP4207945B2 (en) | 2005-09-28 | 2005-09-28 | Method for producing hydrogenated NBR mixture containing recycled rubber |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009131410A (en) * | 2007-11-29 | 2009-06-18 | Shiseido Co Ltd | Packing of container for cosmetics |
| JP2012116987A (en) * | 2010-12-02 | 2012-06-21 | Ube Industries Ltd | Method for producing epoxidized diene-based rubber, and rubber composition containing the rubber |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009131410A (en) * | 2007-11-29 | 2009-06-18 | Shiseido Co Ltd | Packing of container for cosmetics |
| JP2012116987A (en) * | 2010-12-02 | 2012-06-21 | Ube Industries Ltd | Method for producing epoxidized diene-based rubber, and rubber composition containing the rubber |
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| JP4207945B2 (en) | 2009-01-14 |
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