JPS5813645A - Resin composition containing organic peroxide in high concentration - Google Patents
Resin composition containing organic peroxide in high concentrationInfo
- Publication number
- JPS5813645A JPS5813645A JP11191781A JP11191781A JPS5813645A JP S5813645 A JPS5813645 A JP S5813645A JP 11191781 A JP11191781 A JP 11191781A JP 11191781 A JP11191781 A JP 11191781A JP S5813645 A JPS5813645 A JP S5813645A
- Authority
- JP
- Japan
- Prior art keywords
- organic peroxide
- resin
- vinyl acetate
- resin composition
- peroxide
- 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.)
- Pending
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- Compositions Of Macromolecular Compounds (AREA)
- Organic Insulating Materials (AREA)
Abstract
Description
【発明の詳細な説明】
この発明はパイプ、シート、容器などの成形品や被覆電
線を製造するlIK用いる有機過酸化物を高換11に含
有した樹脂組成物Kmするものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a resin composition containing an organic peroxide in high conversion 11, which is used for manufacturing molded products such as pipes, sheets, containers, and covered electric wires.
従来パイプ、シートや容器などの成形品あるい紘被!電
線Ojl造時に用−る有機過酸化物含有樹脂組成物とし
て紘樹脂100重量部に対して有機過酸化物を1〜2重
量部含むものが殆んどである。Conventional molded products such as pipes, sheets, containers, etc. Most organic peroxide-containing resin compositions used in the production of electric wires contain 1 to 2 parts by weight of organic peroxide per 100 parts by weight of the resin.
そしてそのような樹脂組成物によるパイプ、シートなど
の成形子被覆電線の製造法として11図に工程図として
示すようK。A method for manufacturing molded element-covered wires such as pipes and sheets using such a resin composition is shown in FIG. 11 as a process diagram.
(1) 定量の樹脂lに予め所定量を計量した有機過
酸化物2を混合して8のパンバリミキナー、オープンロ
ール、あるいは!軸押出機にて樹脂の一点以上、有機過
酸化物の分解温度以下で混練し、有機過酸化物を均一に
分散せしめAll、粒状成形品4を得る。(1) Mix a predetermined amount of organic peroxide 2 with a certain amount of resin 1, and mix it into a panburi mixer, an open roll, or! The resin is kneaded at one or more points in a axial extruder at a temperature below the decomposition temperature of the organic peroxide to uniformly disperse the organic peroxide to obtain a granular molded product 4.
(2) 次iで粒状成形品4を押出機6に供給し、架
橋可能な樹脂組成物である粒状成#−晶4からパイプ、
シートなどに成形する。あるiはこの粒状成形品を導体
上に押出して被覆電−を得る。(2) In the next step i, the granular molded product 4 is fed to the extruder 6, and from the granular molded product 4, which is a crosslinkable resin composition, a pipe is formed.
Form into sheets, etc. Some i extrude this granular molded product onto a conductor to obtain a coating.
(3) 上記樹脂組成物によるシート、パイプ等の成
形物あるいは被覆電llIを有機過酸化物が分解する温
度に加熱、架116し、成形品7を得る0が行なわれて
いる。(3) A molded article such as a sheet or pipe made of the resin composition or a coated electric material is heated to a temperature at which the organic peroxide decomposes and then racked (116) to obtain a molded article 7.
しかしてこのような従来の有機過酸化物含有樹脂組成物
を用いた場合、安定した被板電線を得ること社可能であ
るが、その製造工程においては必ず樹脂と有機過酸化物
を混練、混合する工程を必要とするため、設備費や加工
費が高くつくという欠点を有している。However, when using such conventional organic peroxide-containing resin compositions, it is possible to obtain stable covered electric wires, but the manufacturing process always requires kneading and mixing of the resin and organic peroxide. This method has the disadvantage that equipment costs and processing costs are high because it requires a process of
上記のような樹脂と有機過酸化物の混練、混合の工程を
省く方法としては、樹脂ペレットと有機過酸化物を計量
後両者を押出機ホッパーから同時に押出機内に投入し、
押出機内で両者を混線と同時に押出すという方法が考え
られる。As a method of omitting the kneading and mixing process of the resin and organic peroxide as described above, after weighing the resin pellets and the organic peroxide, both are fed into the extruder from the extruder hopper at the same time.
A possible method is to mix and extrude both in an extruder at the same time.
しかしながら、この方法では有機過酸化物が樹脂中和均
一に分散されないこと、さらに有機過酸化物が樹脂ペレ
ット表面を覆い、潤滑剤の如き役目を果すため樹脂ペレ
ットが、滑シ、押出量が安定しないなどといった欠点が
あ)、これも実用に至ってiない。However, with this method, the organic peroxide is not uniformly dispersed during resin neutralization, and furthermore, the organic peroxide covers the resin pellet surface and acts like a lubricant, so the resin pellet does not lubricate and the extrusion rate is stable. However, this has also not been put to practical use.
を丸別の方法として押出機の中で溶融樹脂と混練させる
有様過酸化物を押出機シリンダの数個所に設は丸柱入口
から圧入するという方法も提案されている。(%開昭5
3−75487号、同58−115079号)
この方法によると、有機過酸化物の分散や押出量は比較
的安定するが1.押出機シリンダに数個所の注入口を必
要とする丸め設備費が高価であること、さらに有機過酸
化物の樹脂に対する供給比率を一定圧することが難かし
いという欠点がある。As an alternative method, a method has been proposed in which a peroxide to be kneaded with the molten resin in the extruder is placed in several places in the extruder cylinder and then press-fitted from the round cylinder inlet. (% Kaisho 5
(No. 3-75487, No. 58-115079) According to this method, the dispersion and extrusion amount of the organic peroxide are relatively stable, but 1. There are disadvantages in that the extruder cylinder requires several injection ports and the rounding equipment is expensive, and furthermore, it is difficult to maintain a constant supply ratio of organic peroxide to resin.
この発明は上記した従来の方法における樹脂と有機過酸
化物との混線、成形時の種々の欠点を改良すべく鋭意検
討の結果なされたものである。This invention was made as a result of intensive studies in order to improve the various drawbacks during molding, such as crosstalk between resin and organic peroxide, in the conventional methods described above.
即ちこの発明は、押出機K11脂ペレツトとともに投入
する有機過酸化物を後述するような有機過酸化物高員度
含有樹脂組成物として、これを投入するならば有機轡・
酸化物が樹脂中に均一に分散され、また押出量も安定す
ることを見出したものである。That is, in this invention, the organic peroxide to be charged together with the extruder K11 fat pellets is a resin composition containing a high organic peroxide content as described below.
It was discovered that the oxide is uniformly dispersed in the resin and that the extrusion rate is also stable.
以下ζO発明である有機過酸化物高淡度含有樹脂組成物
(以下単に樹脂組成物と略記する)にりいて説明すると
、この樹脂組成物は、酢酸ビニルをムロ重量−以上含有
する樹脂100重量部に有機過酸化物を10重量部以上
配合し、オープンロールなどで混練混合することによっ
て得られるのである。ここで使用する樹脂中の酢酸ビニ
ルの含有量を15重量−以上と規定するのは、15重量
−以下の含有量では得られた樹脂組成物の保存中に有機
過酸化物が組成物粒土にブリードしやすく、このため樹
脂ペレットと同時投入による押出時に有機過酸化物が樹
脂ペレット中に均一に分散されKくく、また押出量も変
動し、実用に供せられなiためである。The following explanation will be based on a resin composition containing a high degree of organic peroxide (hereinafter simply referred to as a resin composition), which is the ζO invention. It is obtained by adding 10 parts by weight or more of an organic peroxide to each part and kneading and mixing with an open roll or the like. The reason why the content of vinyl acetate in the resin used here is defined as 15 weight or more is that if the content is 15 weight or less, organic peroxide may be dissolved in the composition particles during storage of the resulting resin composition. This is because organic peroxides tend to bleed easily, and as a result, it is difficult for the organic peroxide to be uniformly dispersed in the resin pellets during extrusion when they are added together with the resin pellets, and the amount of extrusion varies, making it impractical.
さらに樹脂に配合する有機過酸化物の量を10重量部以
上とするのは、これが10重量部以下では有機過酸化物
を含まない組成物(例えにケーブル被覆組成物)中に一
定の有機過酸化物を添加する際に有機過酸化物含有樹脂
組成物を樹脂ベレットに対してかなシ多量に添加せねば
ならない九め、材料コストが高くつくからである。□
しかしてこの発明の有機過酸化物高濃度含有樹脂思成物
を使用した場合のパイプ、シートなどの成形や被覆電線
の製造工程を第2図にて説明すると、樹脂ペレッ) 1
1とそれに対して所要量の有機過酸化物高鎖度含有樹脂
組成物1tvt同時に押出機18に投入し、両者の均一
な分散とともKPk畳形状の押出成形を行い、次いで加
熱架*141゜て成形品15を得るのである。Furthermore, the reason why the amount of organic peroxide to be added to the resin is 10 parts by weight or more is that if it is less than 10 parts by weight, a certain amount of organic peroxide will be added to the composition (for example, a cable coating composition) that does not contain organic peroxide. This is because when adding the oxide, a large amount of the organic peroxide-containing resin composition must be added to the resin pellet, which increases the material cost. □ However, the process of forming pipes, sheets, etc. and manufacturing covered wires when using the resin composition containing a high concentration of organic peroxide of the present invention is explained with reference to Fig. 2.Resin pellets) 1
1 and the required amount of organic peroxide high chain degree-containing resin composition 1 tvt were simultaneously charged into the extruder 18, both were uniformly dispersed and extruded into a KPk tatami shape, and then heated on a heating rack*141° A molded article 15 is obtained.
以上のように、この発明の有機過駿化物高am含有樹脂
組成物として有機過酸化物を使用することkよって押出
機内で有機過酸化物が樹脂ペレット中に均一に分散され
ることとな〉、従来の樹脂ペレットと有機過酸化物を用
いる場合における樹脂ベレットの融点以上で混練すると
iう工程を全く省略することが可能でToll、工程の
短縮とそれに伴なうコスト低減忙大きな効果をも九らす
のである。As described above, by using an organic peroxide as the organic persulfide-rich am-containing resin composition of the present invention, the organic peroxide is uniformly dispersed in the resin pellets in the extruder. In the case of using conventional resin pellets and organic peroxide, it is possible to completely omit the step of kneading at a temperature higher than the melting point of the resin pellets, which has the effect of shortening the process and reducing costs accordingly. It's nine.
このような有機過酸化物高鎖度含有樹脂組成物と樹脂ペ
レッ)Kよる成形製品としては被覆電−、パイプ、シー
ト、テープ、容器などの成形品が挙けられる。Examples of molded products made from such a resin composition containing a high organic peroxide chain degree and resin pellets include molded products such as coated electrical conductors, pipes, sheets, tapes, and containers.
この発明において使用する酢酸ビニルを15重量−以上
含有する樹脂としては、エチレン−酢酸ビニル共重合体
のような酢酸ビニルの共重合体およびプラスチックにポ
リ酢酸ビニルを酢酸ビニルが15重量−以上となるよう
ブレンドしたものなどがあるが、なかでもエチレン−酢
酸ビニル共重合体が最も好ましい。The resin containing 15 weight or more of vinyl acetate used in this invention includes copolymers of vinyl acetate such as ethylene-vinyl acetate copolymer, and polyvinyl acetate in plastics containing 15 weight or more of vinyl acetate. Among them, ethylene-vinyl acetate copolymer is most preferred.
また有機過酸化物としては、ジクミルパーオキサイド、
ジターシャリ−ブチルパーオキサイド、2.5−ジメチ
ル2.5−ジ(タークヤクープチルパーオキク)ヘキサ
ント、l、8−ビス(ターフヤリ−ブチ、I& 、<−
オキクイソプロビル)ベンゼン、2.5−ジメチル2.
5−ジ(ハイドロパーオキン)ヘキサンなどが挙げられ
るが、ジクミルパーオキサイドが
(υ 安価であること、
Q) 分解半減期が10時間の・ときの温度は116℃
であり、ポリエチレンは約1200で成形加工されるの
でジクミルパーオキサイド(DCP)の分解による、い
わゆる焼けの発生が少なく、架橋時例えば蒸気架橋なら
、約200℃の温度で架橋されるので十分な一連で架橋
できる。In addition, examples of organic peroxides include dicumyl peroxide,
Ditertiary-butyl peroxide, 2,5-dimethyl 2,5-di(tertiarybutylperoxide)hexant, l,8-bis(tertiarybutylperoxide, I&,<-
Oxyquiisopropyl)benzene, 2,5-dimethyl2.
Examples include 5-di(hydroperoquine)hexane, but dicumyl peroxide has a decomposition half-life of 10 hours (116°C).
Since polyethylene is molded at a temperature of about 1,200°C, so-called burning due to the decomposition of dicumyl peroxide (DCP) is less likely to occur, and when crosslinking, for example, with steam crosslinking, it is crosslinked at a temperature of about 200°C, which is sufficient. Can be crosslinked in series.
などの点で最も好ましい。It is most preferable because of the following points.
これはDCPよシも温度が高いと、(半減期10hrs
)架橋時に焼けが発生しやすく、逆KDCPの温度より
低いと、架橋時間が長くな)、生産速度が遅くなってし
まうためである。This is true for DCP as well, when the temperature is high (half-life: 10 hrs).
) Burning is likely to occur during crosslinking, and if the temperature is lower than that of reverse KDCP, the crosslinking time will be long () and the production rate will be slow.
次忙この発明を実施例によシ詳細に説明する。This invention will be explained in detail by way of examples.
実施例
有機過敏化物としてジクミルパーオキサイド(DCP)
を用い、第1表に示すよりな@1ilK配合し、夫々を
オープンロールで混練混合してベレット化した。次いで
これらを常温で1週間放置し、樹脂ベレット表面にジク
ミルパーオキナイドが滲出してくるブリード量の絢定を
行つ九。結果社第1表に示した。Example Dicumyl peroxide (DCP) as an organic sensitizer
Using @1ilK as shown in Table 1, each was kneaded and mixed using an open roll to form pellets. Next, these were left at room temperature for one week, and the amount of dicumyl peroxinide oozed out on the surface of the resin pellet was determined.9. The results are shown in Table 1.
なお比較例として酢酸ビニル含有量16%以下の樹脂や
低密度ポリエチレンKDCPを配合し丸もOKついて−
同じようにブリード量O媚定を行った。As a comparative example, a resin with a vinyl acetate content of 16% or less and a low-density polyethylene KDCP were blended and the circle was OK.
Bleed amount O was determined in the same manner.
注:*1 ブリード量は上表の配合したam組zooべ
vット表面をメタノールテ洗。Note: *1 The amount of bleed is determined by washing the surface of the AM set zoo bed with the formulation shown in the table above with methanol.
浄したのち、メタノールでソックスレ
ー抽出を行ない、抽出液を液体クロマ
ドグ2フで分析す−る−こと−によって、ベレット中の
残存DCP量を求めブリー
ド量を計算した。またブリード量の
wt9GはDCPの配合iLK対する割合である。After cleaning, the pellet was subjected to Soxhlet extraction with methanol, and the extract was analyzed with a liquid chromagraph to determine the amount of DCP remaining in the pellet and calculate the amount of bleed. In addition, the bleeding amount wt9G is the ratio of DCP to the blended iLK.
秦20・・・DCPのブリード量10%以下を良とした
。Hata 20: DCP bleeding amount of 10% or less was considered good.
×・・・DCPのブリード量10% 以上□
を不良とした。×・・・DCP bleed amount 10% or more □
was considered defective.
次に第2表に示すように低密度ポリエチレン100宜友
部に対して!1重結合の有機過酸化物−含有am組成物
を有機過酸化物量が〜2重量部[するように夫々を混合
したのち、50■押出根ホツパーよシ投入し、押出量の
経時変化を絢定し九〇その結果は第2表の過多であった
。Next, as shown in Table 2, for 100 parts of low density polyethylene! After mixing the single bond organic peroxide-containing am composition so that the amount of organic peroxide was ~2 parts by weight, it was poured into a 50 cm extrusion root hopper to observe the change in extrusion amount over time. The results were as shown in Table 2.
ま九押出成形した樹脂棒を押出成形2時間後に5初/−
の高圧蒸気中で80分間加熱架橋したのち、この架橋押
出成形&H1m棹16について第8図に示すようにiT
himA、 B、 Cおよび中央りの4点におけるゲル
分率(120℃キシレン不溶分)の測定結果をも第2表
に示した。After 2 hours of extrusion molding the extruded resin rod
After heating and crosslinking in high pressure steam for 80 minutes, this crosslinked extrusion & H1m rod 16 was subjected to iT as shown in Figure 8.
Table 2 also shows the measurement results of the gel fraction (xylene insoluble content at 120°C) at four points: himA, B, C, and the center.
上記第1表および第2表から、この発明の実施hK>い
てはDCPのブリードが少なく、また押出量の変動が少
ないのに比べ、比較例は何れもDCPのブリードが多く
、押出量も少なくなシ且つ変動も大きくて実用的でない
ことが実証され友。From the above Tables 1 and 2, it can be seen that in the implementation of the present invention, DCP bleed is small and the extrusion amount fluctuates less, whereas in the comparative examples, DCP bleed is large and the extrusion amount is small. It has been proven that this method is impractical due to its large size and large fluctuations.
またこのほかに、押出機ホッパーから低密度ポリエチレ
ンとDCPとを直接投入することも試みたが、押出機内
で材料が滑シ、5分後には押出しできなかった。In addition, an attempt was made to directly feed low-density polyethylene and DCP from the extruder hopper, but the materials slipped in the extruder and could not be extruded after 5 minutes.
さらに1低密度ポリエチレン100重量部にDCP2重
量部をオープンロールでポリエチレンの融点以上で混線
混合したのちペレット化し、押出機に供給することも試
みたが、押出量が押出直後: 161F、10分後:
1621F、80分後: 1482゜1時間i: 16
0f、2時間後:151F、平均=160.8f、押出
量の最大と最小の差6tという結果が得られ、上記この
発明の実施例が従来と同等の加工性を有することが誌め
られた。Furthermore, we tried mixing 100 parts by weight of DCP with 100 parts by weight of low-density polyethylene using an open roll at a temperature above the melting point of polyethylene, pelletizing it, and feeding it to the extruder, but the extrusion amount was immediately after extrusion: 161F, 10 minutes later. :
1621F, 80 minutes later: 1482° 1 hour i: 16
0f, 2 hours later: 151F, average = 160.8f, and the difference between the maximum and minimum extrusion amount was 6t, indicating that the above embodiment of the present invention had workability equivalent to the conventional one. .
第1図は従来の樹脂ペレットと有機過・酸化物を用いえ
押出成形の工程図、第2図はこの発明の有機過酸化物高
濃度含有樹脂組成物と樹脂ベレットによる押出成形の工
程図、第3図は架橋押出成形した樹脂棒におけるゲル分
率測定個所を示す#樹脂棒の斜REである。
特許出願人 住友電気工業株式会社同 代
理人 弁理士和1) 昭第1図 第
2図
第3図
手続補正書印発)
昭和57年4 月13日
特許庁長官 島田春樹 殿
1、事件の表示
昭和56年 特許 願第111917号2、発明の名称
有機過酸化物高濃度含有樹脂組成物3、 補正をす
る者
事件との関係 特許出願人
住 所 大阪市東区北浜5丁l」15番地エ ゎ、
□)(213) 住友電気工業株式会社4、代理人
6、補正により増加する尭−の数
7、補正の対象
補正の内容
1、明細書第8頁4〜7行目
「これは・・・・・・しまうためである。」を[これは
DCPよジも分解半減期10時間における温度が低い有
機過酸化物を用いると、(半減期10 hrs )架橋
時に焼けが発生しやすく、逆にDCPの分解半減期10
時間における温度より高い有機過酸化物を用いると、架
橋時間が長くなり、生産速度が遅くなってしまうためで
ある。」と訂正します。Fig. 1 is a process diagram of extrusion molding using conventional resin pellets and organic peroxide, and Fig. 2 is a process diagram of extrusion molding using a resin composition containing a high concentration of organic peroxide and resin pellets of the present invention. FIG. 3 is a diagonal RE of #resin rod showing the gel fraction measurement points in the crosslinked extrusion molded resin rod. Patent applicant: Sumitomo Electric Industries, Ltd. Agent: Patent Attorney Kazu1) Figure 1, Figure 2, Figure 3, Procedural amendments stamped) April 13, 1980 Commissioner of the Japan Patent Office Haruki Shimada, 1, Indication of the case 1981 Patent Application No. 111917 2, Title of invention: Resin composition containing high concentration of organic peroxide 3, Relationship to the case of the person making the amendment Patent applicant address: 15-15 Kitahama 5-chome, Higashi-ku, Osaka ,
□) (213) Sumitomo Electric Industries, Ltd. 4, Agent 6, Number of 庭-s increased by amendment 7, Contents of amendment subject to amendment 1, Page 8 of the specification, lines 4-7, “This... This is because if an organic peroxide with a low temperature at a decomposition half-life of 10 hours (half-life of 10 hrs) is used for DCP, burns are likely to occur during crosslinking; Degradation half-life of DCP 10
This is because if an organic peroxide is used at a temperature higher than that for the time, the crosslinking time becomes longer and the production rate becomes slower. ” I am corrected.
Claims (3)
重量部に有機過酸化物を10重量部以上配合したことを
特徴とする有機過酸化物高鎖度含有樹脂組成物。(1) Resin 100 containing 15 weight or more of #identical vinyl
A resin composition containing a high chain degree of organic peroxide, which contains 10 parts by weight or more of an organic peroxide.
してエチレン−酢酸ビニル共重合樹脂を用いることを特
徴とする特許請求の範囲第1項記載の有機過酸化物高鎖
度含有樹脂組成物。(2) The organic peroxide high chain degree-containing resin composition according to claim 1, wherein an ethylene-vinyl acetate copolymer resin is used as the resin containing 16 weight or more of vinyl acetate.
を用−ること10黴とする特許請求の範囲第1項記載の
有機過酸化物高111ffi含有樹脂鑑成物。(3) A resin product containing an organic peroxide with a high 111ffi content as set forth in claim 1, wherein dicumyl peroxide is used as the organic peroxide.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP11191781A JPS5813645A (en) | 1981-07-16 | 1981-07-16 | Resin composition containing organic peroxide in high concentration |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP11191781A JPS5813645A (en) | 1981-07-16 | 1981-07-16 | Resin composition containing organic peroxide in high concentration |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS5813645A true JPS5813645A (en) | 1983-01-26 |
Family
ID=14573347
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP11191781A Pending JPS5813645A (en) | 1981-07-16 | 1981-07-16 | Resin composition containing organic peroxide in high concentration |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS5813645A (en) |
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1981
- 1981-07-16 JP JP11191781A patent/JPS5813645A/en active Pending
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