JPH06322333A - Production of solvent-type rubber-based tack agent - Google Patents
Production of solvent-type rubber-based tack agentInfo
- Publication number
- JPH06322333A JPH06322333A JP11052993A JP11052993A JPH06322333A JP H06322333 A JPH06322333 A JP H06322333A JP 11052993 A JP11052993 A JP 11052993A JP 11052993 A JP11052993 A JP 11052993A JP H06322333 A JPH06322333 A JP H06322333A
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- Prior art keywords
- rubber
- solvent
- material components
- type
- sensitive adhesive
- 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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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、溶剤型ゴム系粘着剤の
製造方法に関し、さらに詳しくは、固形分濃度の高い溶
剤型ゴム系粘着剤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 solvent-type rubber-based pressure-sensitive adhesive, and more particularly to a method for producing a solvent-type rubber-based pressure-sensitive adhesive having a high solid content concentration.
【０００２】[0002]
【従来の技術】ゴム系粘着剤は、通常、ゴムに、粘着付
与樹脂、軟化剤、老化防止剤、充填剤等の各種成分を混
合したものであり、溶剤型で用いられている。この溶剤
型ゴム系粘着剤は、同粘着剤を構成する上記原料成分を
ヘキサン、ヘプタン、トルエン等の有機溶剤に溶解し、
ロールコーター等で基材に塗布後、乾燥機で溶剤を蒸発
させて粘着テープとするのに用いられている。2. Description of the Related Art A rubber-based pressure-sensitive adhesive is usually a mixture of rubber with various components such as a tackifying resin, a softening agent, an antiaging agent, and a filler, and is used in a solvent type. This solvent-based rubber-based pressure-sensitive adhesive, the raw material components constituting the pressure-sensitive adhesive is dissolved in an organic solvent such as hexane, heptane, toluene,
It is used to form an adhesive tape by coating a substrate with a roll coater or the like and then evaporating the solvent with a drier.
【０００３】従来、溶剤型ゴム系粘着剤の製造工程にお
いて、溶剤に、ゴム、粘着付与樹脂、軟化剤等の原料成
分を溶解させる際には、所定量の溶剤中に上記原料成分
をそれぞれ所要量投入し、十数時間から数十時間攪拌、
溶解した後に、ゴム系粘着剤を得ていた。Conventionally, in the process of producing a solvent-based rubber-based pressure-sensitive adhesive, when the raw material components such as rubber, tackifying resin, and softening agent are dissolved in the solvent, the above-mentioned raw material components are required in a predetermined amount of the solvent. Add the amount and stir for 10 to 10 hours.
After the dissolution, a rubber-based pressure-sensitive adhesive was obtained.
【０００４】ところで、近年の粘着剤業界においては、
その製造プロセス中で溶剤を可及的に削減することが求
められている。その為には、ゴムをより高濃度で溶剤に
溶解させる必要がある。By the way, in the recent adhesive industry,
It is required to reduce the solvent as much as possible in the manufacturing process. For that purpose, it is necessary to dissolve the rubber in a solvent at a higher concentration.
【０００５】しかし、上記のような従来の溶剤型ゴム系
粘着剤の製造方法では、ゴムを高濃度で溶解させようと
しても、ゴムの溶解に長時間を要したり、数十時間かけ
てもゴムが溶解せず、均一な粘着剤が得られなかった。However, in the conventional method for producing a solvent-based rubber-based pressure-sensitive adhesive as described above, even if an attempt is made to dissolve the rubber at a high concentration, it takes a long time to dissolve the rubber, or it takes several tens of hours. The rubber did not dissolve and a uniform adhesive could not be obtained.
【０００６】また、ゴムを高濃度で溶解させるために、
予め、ゴムの素練りを過度に行い、これによりゴム分子
を機械的に切断して分子量を小さくすることで、溶剤へ
の溶解性を向上させる方法が考えられる。Further, in order to dissolve rubber at a high concentration,
A method of improving solubility in a solvent by preliminarily masticating the rubber and mechanically cutting the rubber molecules thereby to reduce the molecular weight is considered.
【０００７】しかしながら、過度の素練りを行ったゴム
を用いた粘着剤は凝集力が低下し、粘着剤そのものの働
きを発現させにくくなる。However, the pressure-sensitive adhesive using rubber that has been excessively masticated has a reduced cohesive force, making it difficult to exert the function of the pressure-sensitive adhesive itself.
【０００８】また、高濃度粘着剤を得るために、従来の
粘着剤を濃縮させることもできるが、溶剤の総量は変ら
ないため、これは本質的な課題解決にならない。Further, in order to obtain a high-concentration pressure-sensitive adhesive, the conventional pressure-sensitive adhesive can be concentrated, but this does not solve the essential problem because the total amount of the solvent does not change.
【０００９】このように、従来技術においては、高濃度
のゴム系粘着剤を分子切断を起こすことなく製造する有
効な方法は、提案されていない。As described above, the prior art has not proposed an effective method for producing a high-concentration rubber-based pressure-sensitive adhesive without causing molecular cleavage.
【００１０】[0010]
【発明が解決しようとする課題】本発明の目的は、溶剤
型ゴム系粘着剤の製造工程において、高濃度の粘着剤を
ゴムの分子切断を起こすことなく、均一な粘着剤を製造
する方法を提供することにある。SUMMARY OF THE INVENTION An object of the present invention is to provide a method for producing a uniform pressure-sensitive adhesive in a process for producing a solvent-type rubber-based pressure-sensitive adhesive, without causing molecular cutting of a high-concentration pressure-sensitive adhesive. To provide.
【００１１】本発明者等は、前記従来技術の有する問題
点を克服すべく鋭意研究した結果、予め、ゴムを溶剤で
膨潤しておき、得られた膨潤ゴムに残余の成分を混練溶
解させることにより、均一な溶剤型ゴム系粘着剤を製造
できることを見い出し、その知見に基づいて本発明を完
成するに至った。As a result of intensive studies to overcome the problems of the prior art, the present inventors have swelled rubber with a solvent in advance, and knead and dissolve the remaining components in the obtained swollen rubber. As a result, they have found that a uniform solvent-type rubber-based pressure-sensitive adhesive can be produced, and have completed the present invention based on the findings.
【００１２】[0012]
【課題を解決するための手段】かくして本発明によれ
ば、ゴム系粘着剤を構成する原料成分を溶剤に溶解させ
るに当たり、予め、ゴムを溶剤で膨潤させておき、得ら
れた膨潤ゴムに残余の原料成分を加えて混練溶解させる
ことを特徴とする溶剤型ゴム系粘着剤の製造方法が提供
される。Thus, according to the present invention, when the raw material components constituting the rubber-based pressure-sensitive adhesive are dissolved in the solvent, the rubber is swollen in advance with the solvent, and the resulting swollen rubber is left with a residual substance. There is provided a method for producing a solvent-based rubber-based pressure-sensitive adhesive, which comprises adding the raw material components described above, kneading and dissolving.
【００１３】以下、本発明について詳述する。The present invention will be described in detail below.
【００１４】膨潤用の溶剤としては、一般に使用されて
いるノルマルヘキサン、ヘプタン、トルエン、トリクレ
ン、ゴム用揮発油等の有機溶剤が用いられる。As the swelling solvent, generally used organic solvents such as normal hexane, heptane, toluene, trichlene, and volatile oil for rubber are used.
【００１５】溶剤の使用量は、配合するゴムの種類、形
状、最終粘着剤の設計固形分濃度等に依存するが、特に
ゴムの配合量で大きく制約を受けるため、粘着剤中のゴ
ム配合量は６０重量％迄とされる必要がある。これ以上
ゴム濃度を上げると、ゴムの膨潤が不十分であり、残余
の原料成分と混合する時に、未溶解のゴム塊が生じてし
まい、目的の溶剤型粘着剤が得られなくなる。The amount of the solvent used depends on the type and shape of the rubber to be compounded, the designed solid content concentration of the final adhesive, etc., but the compounding amount of the rubber is particularly limited, so the amount of the rubber compounded in the adhesive is large. Must be up to 60% by weight. If the rubber concentration is further increased, the swelling of the rubber will be insufficient and undissolved rubber lumps will be formed when mixing with the remaining raw material components, whereby the intended solvent-based pressure-sensitive adhesive cannot be obtained.
【００１６】溶剤によるゴムの膨潤は、静置槽にて行う
ことも可能であるが、均一な膨潤ゴムを得るためには、
位置交換の機構をもった、ニーダー型、プロペラ式、回
転式等の種々のタイプのミキサーを用いることが好まし
い。 膨潤ゴムと残余原料成分の混合は、ニーダー型ミ
キサー、連続混練機、エクストルーダ等の種々のタイプ
のミキサーを用いて行うことができる。The swelling of rubber with a solvent can be carried out in a stationary tank, but in order to obtain a uniform swelling rubber,
It is preferable to use various types of mixers such as a kneader type, a propeller type, and a rotary type having a position exchange mechanism. The swelling rubber and the remaining raw material components can be mixed with each other by using various types of mixers such as a kneader type mixer, a continuous kneader, and an extruder.
【００１７】ゴムとしては、天然ゴム、ポリイソプレン
ゴム、ポリブタジエンゴム、スチレンブタジエンゴム、
スチレン−イソプレン−スチレンやスチレン−ブタジエ
ン−スチレンゴム等のブロック共重合体ゴム等を例示す
ることができる。As the rubber, natural rubber, polyisoprene rubber, polybutadiene rubber, styrene-butadiene rubber,
Examples thereof include block copolymer rubbers such as styrene-isoprene-styrene and styrene-butadiene-styrene rubber.
【００１８】粘着付与樹脂としては、汎用のものが使用
でき、例えば、ロジン系、クマロン−インデン系、テル
ペン系、石油系、スチレン系、フェノール系、キシレン
系等を挙げることができる。As the tackifying resin, general-purpose resins can be used, and examples thereof include rosin-based, coumarone-indene-based, terpene-based, petroleum-based, styrene-based, phenol-based and xylene-based resins.
【００１９】軟化剤としては、例えば、ポリブテン、ポ
リイソプレン、プロセスオイル、ナフテン系オイル等を
挙げることができる。Examples of the softening agent include polybutene, polyisoprene, process oil, naphthenic oil and the like.
【００２０】老化防止剤としては、汎用のフェノール
系、アミン系安定剤を用いることが可能である。As the antiaging agent, a general-purpose phenol-based or amine-based stabilizer can be used.
【００２１】充填剤としては、亜鉛華、炭酸カルシウ
ム、クレー、タルク等、顔料としては、チタン白、カー
ボンブラック等を例示することができる。Examples of the filler include zinc white, calcium carbonate, clay, talc and the like, and examples of the pigment include titanium white and carbon black.
【００２２】架橋剤としては、チウラム系、フェノール
系、イソシアネート系等を用いることができる。As the cross-linking agent, thiuram type, phenol type, isocyanate type and the like can be used.
【００２３】これらの原料成分は、使用目的に応じて適
宜選択して用いられる。These raw material components are appropriately selected and used according to the purpose of use.
【００２４】ゴム系粘着剤を構成する原料成分の配合
は、たとえば下記の割合で行われる。 天然ゴム ：１００重量部 粘着付与樹脂：６０〜１２０重量部 軟化剤 ：０〜６０重量部 老化防止剤 ：０〜５重量部The raw material components constituting the rubber-based pressure-sensitive adhesive are compounded in the following proportions, for example. Natural rubber: 100 parts by weight Tackifying resin: 60 to 120 parts by weight Softener: 0 to 60 parts by weight Anti-aging agent: 0 to 5 parts by weight
【００２５】[0025]
【作用】前記したように、一般に溶剤型ゴム系粘着剤の
製造工程では、配合設計に従って、所定量の溶剤中に、
粘着剤を構成する原料成分であるゴム、粘着付与樹脂、
軟化剤等を所要量投入し、攪拌溶解する手法が用いられ
ている。As described above, generally, in the process of producing a solvent-based rubber-based pressure-sensitive adhesive, a predetermined amount of solvent is added in accordance with the compounding design.
Rubber, a tackifying resin, which is a raw material component of the adhesive,
A method is used in which a required amount of a softening agent or the like is added and dissolved by stirring.
【００２６】しかし、この手法では、溶剤に粘着剤を高
濃度で溶解させようとしても、ゴムを十分に溶解させる
だけの溶剤が混合系中になく、ゴムが溶解せずに残って
しまう。However, in this method, even if an attempt is made to dissolve the pressure-sensitive adhesive in a solvent at a high concentration, there is no solvent in the mixing system to sufficiently dissolve the rubber, and the rubber remains without being dissolved.
【００２７】また、この粘着剤は、残った未溶解ゴムに
攪拌機による剪断力をかけていくには、高濃度の溶剤型
粘着剤と言えども粘度が低すぎ、攪拌機による剪断力を
ゴム塊に伝えることができず、残ったゴムを溶解させる
ことができない。Further, this adhesive is too low in viscosity to apply a shearing force to the remaining undissolved rubber by a stirrer, even though it is a high-concentration solvent-type adhesive, and the shearing force of the stirrer is applied to the rubber block. I can't tell and I can't dissolve the remaining rubber.
【００２８】一方、本発明の方法によれば、予め、所要
量のゴムと所定量の溶剤の一部または全部を混合し、ゴ
ムを溶剤で膨潤させる。すなわち、まず、溶剤を最も溶
解困難な高分子量のゴムの膨潤に使い、十分にゴム塊の
中に溶剤を染み込ませる。このことにより、膨潤された
ゴム塊は、わずかな剪断力で簡単に流動性を発現するこ
とができる。On the other hand, according to the method of the present invention, a predetermined amount of rubber and a predetermined amount of a solvent are partially or wholly mixed and the rubber is swollen with the solvent. That is, first, the solvent is used for swelling the most difficult-to-dissolve high-molecular-weight rubber, and the solvent is sufficiently soaked in the rubber block. As a result, the swollen rubber mass can easily exhibit fluidity with a slight shearing force.
【００２９】次に、この流動性の付与された膨潤ゴムに
残余の原料成分を投入し、膨潤ゴムを混練溶解させ、目
的の溶剤型粘着剤を得る。Next, the remaining raw material components are added to the swelling rubber to which the fluidity is imparted, and the swelling rubber is kneaded and dissolved to obtain the desired solvent-type pressure-sensitive adhesive.
【００３０】ここで、残余の原料成分も予め溶剤に溶解
しておくと、さらに混練時間の短縮化が図れる。If the remaining raw material components are also dissolved in the solvent in advance, the kneading time can be further shortened.
【００３１】[0031]
【実施例】以下に実施例および比較例を挙げて本発明に
ついて更に具体的に説明する。EXAMPLES The present invention will be described more specifically with reference to Examples and Comparative Examples below.
【００３２】実施例１ 天然ゴム（ＲＳＳ１）１００重量部に対して、トルエン
２３０重量部を加え６時間静置し、ゴムを膨潤させた。
次に、得られた膨潤ゴムを２０リットルの双腕型ニーダ
ーに投入し、３０分間攪拌した後、この膨潤ゴムに、粘
着付与樹脂（クイントンＡ−１００：日本ゼオン社製）
１００重量部と、ナフテン系オイル３０重量部を加え、
３０分間攪拌混合し、固形分濃度５０重量％の粘着剤溶
液を得た。このようにして得られた溶剤型粘着剤をアプ
リケーターを用いてポリエステルフィルム上へ塗布し、
１２０℃のオーブンで３分間乾燥させ、粘着剤層の厚み
３０〜３５μｍの粘着テープを得た。Example 1 To 100 parts by weight of natural rubber (RSS1), 230 parts by weight of toluene was added and left standing for 6 hours to swell the rubber.
Next, the obtained swelling rubber was put into a 20 liter double-arm kneader and stirred for 30 minutes, and then the swelling rubber was tackified with a resin (Quinton A-100: manufactured by Nippon Zeon Co., Ltd.).
Add 100 parts by weight and 30 parts by weight of naphthenic oil,
The mixture was stirred and mixed for 30 minutes to obtain an adhesive solution having a solid content concentration of 50% by weight. The solvent-type pressure-sensitive adhesive thus obtained was applied onto a polyester film using an applicator,
It was dried in an oven at 120 ° C. for 3 minutes to obtain an adhesive tape having an adhesive layer with a thickness of 30 to 35 μm.
【００３３】実施例２ 膨潤ゴムへの粘着付与樹脂およびナフテン系オイル添加
後の攪拌を６０分とし、固形分濃度を７０重量％とした
点を除いて、実施例１と同じ操作を行い、やはり粘着剤
層の厚み３０〜３５μｍの粘着テープを得た。Example 2 The same operation as in Example 1 was carried out, except that the stirring after adding the tackifying resin to the swelling rubber and the naphthenic oil was 60 minutes and the solid content concentration was 70% by weight. An adhesive tape having an adhesive layer with a thickness of 30 to 35 μm was obtained.
【００３４】比較例１ トルエン７００重量部を２０リットルの双腕型ニーダー
に投入し、さらに、天然ゴム（ＲＳＳ１）１００重量
部、実施例１のものと同じ粘着付与樹脂１００重量部、
およびナフテン系オイル３０重量部を投入し、２４時間
攪拌し、固形分濃度２５重量％の粘着剤溶液を得た。こ
のようにして得られた溶剤型粘着剤を用い、実施例１と
同じ手法で、粘着剤層の厚み３０〜３５μｍの粘着テー
プを得た。Comparative Example 1 700 parts by weight of toluene was charged into a 20-liter double-arm kneader, and 100 parts by weight of natural rubber (RSS1), 100 parts by weight of the same tackifying resin as in Example 1,
Then, 30 parts by weight of naphthenic oil was added and stirred for 24 hours to obtain an adhesive solution having a solid content concentration of 25% by weight. Using the solvent-type pressure-sensitive adhesive thus obtained, a pressure-sensitive adhesive tape having a pressure-sensitive adhesive layer having a thickness of 30 to 35 μm was obtained in the same manner as in Example 1.
【００３５】比較例２ トルエンの使用量を２３０重量部とし、固形分濃度を５
０重量％とした点を除いて、比較例１と同じ操作を行
い、溶剤型粘着剤を得た。これは、ゴム塊が残り、均一
な粘着剤溶液ではなかった。Comparative Example 2 The amount of toluene used was 230 parts by weight, and the solid content concentration was 5
A solvent-type pressure-sensitive adhesive was obtained by performing the same operation as in Comparative Example 1 except that the content was 0% by weight. This was not a uniform adhesive solution, leaving a rubber lump.
【００３６】[0036]
【表１】 注１．均一性の評価は、粘着剤を薄膜に延ばし、目視観
察で未溶解物の有無を評価した。[Table 1] Note 1. To evaluate the uniformity, the adhesive was spread on a thin film, and the presence or absence of undissolved substances was evaluated by visual observation.
【００３７】注２．ＳＰ粘着力の測定は、温度２３℃、
湿度６５％ＲＨの恒温恒湿下で、幅１５ｍｍに粘着テー
プを切断し、これを鋼板（ＳＵＳ）に２ｋｇローラーに
て圧着し、１８０度の角度に３００ｍｍ／分の速度で剥
離したときの強度を測定することによって行った。Note 2. The SP adhesive strength is measured at a temperature of 23 ° C,
Strength when a pressure-sensitive adhesive tape was cut into a width of 15 mm under a constant temperature and humidity of 65% RH and pressure-bonded to a steel plate (SUS) with a 2 kg roller, and peeled at an angle of 180 degrees at a speed of 300 mm / min. Was measured.
【００３８】注３．ＳＰ保持力の測定は、ＪＩＳ Ｚ０
２３７に従い、温度２３℃、湿度６５％ＲＨ、の恒温恒
湿下で、鋼板（ＳＵＳ）に粘着テープを２５ｍｍ×２５
ｍｍの接着面積になるように、２ｋｇローラーにて圧着
した試験片を４０℃に保たれたオーブン内に３０分間放
置後、１ｋｇの荷重をかけ落下するまでの時間を測定す
ることによって行った。Note 3. Measurement of SP holding force is performed according to JIS Z0
In accordance with 237, the adhesive tape is 25 mm × 25 on a steel plate (SUS) under a constant temperature and humidity of 23 ° C. and a humidity of 65% RH.
The test piece pressed by a 2 kg roller so as to have an adhesion area of mm was left in an oven kept at 40 ° C. for 30 minutes, and then a time of dropping a load of 1 kg was measured.
【００３９】表１から明らかなように、従来の溶剤型粘
着剤の製造方法では溶解困難であった高濃度粘着剤を、
物性を損うことなく、製造することができる。As is clear from Table 1, the high-concentration pressure-sensitive adhesive, which was difficult to dissolve in the conventional solvent-type pressure-sensitive adhesive manufacturing method,
It can be manufactured without impairing the physical properties.
【００４０】このように、実施例１では固形分濃度５０
重量％、実施例２では固形分濃度７０重量％の溶剤型粘
着剤の製造が可能である。As described above, in Example 1, the solid content concentration was 50.
%, And in Example 2, it is possible to produce a solvent-based pressure-sensitive adhesive having a solid content concentration of 70% by weight.
【００４１】また、溶解時間に関しても、膨潤ゴムを用
いる製造方法では、従来技術に比べて時間短縮が可能で
ある。Regarding the dissolution time, the manufacturing method using swelling rubber can shorten the time as compared with the prior art.
【００４２】[0042]
【発明の効果】本発明により、高濃度の溶剤型ゴム系粘
着剤を製造することが可能となり、粘着剤製造プロセス
での溶剤使用量を削減することができる。EFFECTS OF THE INVENTION According to the present invention, it is possible to manufacture a high concentration solvent-type rubber-based pressure-sensitive adhesive, and it is possible to reduce the amount of solvent used in the pressure-sensitive adhesive manufacturing process.
Claims (1)
に溶解させるに当たり、予めゴムを溶剤で膨潤させてお
き、得られた膨潤ゴムに残余の原料成分を加えて混練溶
解させることを特徴とする溶剤型ゴム系粘着剤の製造方
法。1. When dissolving raw material components constituting a rubber-based pressure-sensitive adhesive in a solvent, the rubber is swollen in advance with the solvent, and the remaining raw material components are added to the obtained swollen rubber and kneaded and dissolved. And a method for producing a solvent-based rubber-based adhesive.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11052993A JPH06322333A (en) | 1993-05-12 | 1993-05-12 | Production of solvent-type rubber-based tack agent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11052993A JPH06322333A (en) | 1993-05-12 | 1993-05-12 | Production of solvent-type rubber-based tack agent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06322333A true JPH06322333A (en) | 1994-11-22 |
Family
ID=14538125
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11052993A Pending JPH06322333A (en) | 1993-05-12 | 1993-05-12 | Production of solvent-type rubber-based tack agent |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06322333A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003261740A (en) * | 2002-03-11 | 2003-09-19 | Nippon Zeon Co Ltd | Method for producing elastomer composition |
| JP2007507367A (en) * | 2003-10-01 | 2007-03-29 | フラテッリ・マリス・ソシエタ・ペル・アチオニ | Improved continuous production process for compositions containing rubber, hydrocarbon resin and solvent |
| JP4833352B2 (en) * | 2007-05-31 | 2011-12-07 | ソシエテ ド テクノロジー ミシュラン | Tire repair with cure patch |
| JP2017210526A (en) * | 2016-05-24 | 2017-11-30 | 旭化成株式会社 | Method for producing conjugated diene polymer composition |
-
1993
- 1993-05-12 JP JP11052993A patent/JPH06322333A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003261740A (en) * | 2002-03-11 | 2003-09-19 | Nippon Zeon Co Ltd | Method for producing elastomer composition |
| JP2007507367A (en) * | 2003-10-01 | 2007-03-29 | フラテッリ・マリス・ソシエタ・ペル・アチオニ | Improved continuous production process for compositions containing rubber, hydrocarbon resin and solvent |
| JP4833352B2 (en) * | 2007-05-31 | 2011-12-07 | ソシエテ ド テクノロジー ミシュラン | Tire repair with cure patch |
| JP2017210526A (en) * | 2016-05-24 | 2017-11-30 | 旭化成株式会社 | Method for producing conjugated diene polymer composition |
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