JP2006307219A - 高められた温度で加硫するオルガノポリシロキサン組成物の連続製造法 - Google Patents
高められた温度で加硫するオルガノポリシロキサン組成物の連続製造法 Download PDFInfo
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Abstract
【解決手段】少なくとも500Pa・sの25℃で測定された粘度を有する、高められた温度で加硫するオルガノポリシロキサン組成物(MH)を連続的に製造するにあたり、高粘性のオルガノポリシロキサン(OH)と架橋性添加剤(H)とを、一列に隣り合って配置された少なくとも2つの混練室を有し、それらの混練室がそれぞれ同方向又は逆方向に駆動可能な軸平行の2つの混練工具を有し、かつ該混練工具の軸に対して横方向に通過可能な開口を通じて互いに接続されていて、第一の混練室が供給口を有し、かつ最後の混練室が排出口を有する混練カスケード中で混合及び均質化し、その際、架橋性添加剤(H)を含んでいる混練室中の温度を高くても95℃とする。
【選択図】図1
Description
R1 aR2 bSiO(4−a−b)/2 (1)
[式中、
基R1は、同一又は異なって、Siに結合した、−H、−OH、−ORから選択される一価の基であり、その際、Rは、C1〜C10−炭化水素基を示し、かつハロゲン置換又はシアノ置換されたもしくは置換されていない、二価の有機基を介してケイ素に結合されてよいC1〜C10−炭化水素基を示し、これらの炭化水素基は脂肪族の炭素−炭素多重結合を少なくとも1つ有し、
基R2は、同一又は異なって、Siに結合した、ハロゲン置換又はシアノ置換されたもしくは置換されていない一価のC1〜C10−炭化水素基であり、これらの炭化水素基は脂肪族の炭素−炭素多重結合を有さず、
aは、0〜1の負数でない数であり、かつ
bは、1〜2.1の負数でない数である]に相当する。
−(O)p[(CH2)qO]r− (2)
[式中、
pは、0又は1、特に0の値を意味し、
qは、1〜4、特に1又は2の値を意味し、かつ
rは、1〜20、特に1〜5の値を意味する]のオキシアルキレン単位から構成される。一般式(2)のオキシアルキレン単位は、その左側でケイ素原子に結合されている。
Viは、ビニル基を意味し、かつMeは、メチル基を意味し、負数でない整数c、d、e及びfは以下の関係を満たす:
c+d≧1、c+f=2、1000<(d+e)<9000、有利には3000<(d+e)<7000、そして
0<(d+1)/(d+e)<1、有利には0<(d+1)/(d+e)<0.1]に相当する、ビニル基を有するオルガノポリシロキサン(OH)を使用することが特に好ましい。
HTVゴムA:BET表面積少なくとも200m2/gの補強性ケイ酸40部を、平均重合度5500を有するポリジメチルシロキサン100部に対して有し、殆ど架橋性ビニル基を有さず、かつ加工助剤を含有する高粘性の固形ゴム混合物。このHTV混合物は、約40のムーニーによる粘度(ML(1+4分)23℃;DIN53523)を有し、そして、例えばペルオキシドによる加硫の後に、ショアAによる硬度60が生ずる。
該方法を図1をもとに説明する:
混合のために、IKA Maschinebau Junke & Kunkel GmbH & Co.KG社(シュタウフェン在)のConterna(登録商標)混練カスケード(2)を使用した。混練カスケード(2)は、それぞれ5lまでの容量の6つの混練室を有し、それらは個別に制御可能な羽根ブロック(blade block)を有する。全処理量は、添加物中の油割合に応じて150〜250kg/hであった。オルガノポリシロキサン(OH)と充填剤とからなる混合物の供給(1)と、オルガノポリシロキサン組成物(MH)の排出あるいは成形(6)のために、それぞれColmec社(イタリア・ミラノ在)の円錐二軸押出機CTE75をそれぞれ使用した。そこに、添加物のペーストを、PLSの制御下に、傍心軸ポンプ(eccentric screw pump)と圧力モニタを有するViscoTec社(テーギンク/ドイツ在)のドラム型圧出装置(drum expression apparatus)(3)を介して供給した。
実施例1のHTVゴムAの代わりに、220kg/hのHTVゴムBを混練カスケード(2)の供給押出機(1)を介して供給するが、ドラム型送出ステーション(3)を介して、シリコーンゴム中の2,5−ジ−t−ブチル−ペルオキシ−2,5−ジメチルヘキサンの45%ペースト(Peroxid−Chemie社からDHBP−45−PSIとして市販されている)の1.2%を供給した。着色のために、8.8kg/hの着色造粒物Elastosil(登録商標)FG Schwarz−9005を、Flexwall供給装置(Brabender社)を介して、第二の混練室の導入漏斗中に直接添加し、これを同様に最後の混練室の出口で均質に混和した。実施例1に加えて、篩交換アタッチメントを有する冷却された歯車ポンプGP112(Colmec社/ミラノ在)を、円錐型供給押出機(6)の出口で、製品形に成形する前に取り付けるため、ここでも100μmのストレーナを取り付けることができた。10×40mmの有孔板を介して、60℃未満の温度で、いわゆるL8−連続ストリップ(continuous strip)を製造し、これは品質試験の結果(165℃/10分間での圧縮;加硫測定器試験のためのバッチ装填物の複数の試料:T90値は測定安全範囲内)によれば均質に混合された。この高充填されたHTV混合物は高い油成分を有する。
実施例2に記載される架橋活性の安全ケーブル混合物の同じ成分を良く冷却された1メートルトンミキサ、例えば水冷シグマ混練機中で混合する場合に、少なくとも4時間の混合時間と排出時間が必要であるのは、部分的な加硫の回避のために内部温度を100℃未満に維持せねばならないからである。1人の装置操業者で少なくとも1時間の1メートルトンミキサの装填時間と、後続の100μmのストレーナ過程のための作業時間(1メートルトンにつき少なくとも約2〜3時間)とで、ここでは充填までに130〜140kg/hだけの全生産性のみが得られたに過ぎない。
非常に反応性の架橋剤の混和のための古典的な方法では、120kgのHTVゴムAを、水冷された2つの鋼製ロール(それぞれ550mmの直径、2m長)の大きな標準的ロール混練機において、実施例1でのように1.8%のジ(4−メチルベンゾイル)ペルオキシド(=2.16kgのペースト、シリコーン油中50%)及び1.2%の液状着色ペーストFL Blau−5015と混合した。添加物の油状の粘稠性に基づいて、これらを少しずつ分出シート(milled sheet)に添加しても、異なる回転数で回転するロールからゴムの剥離と減量は生じなかった。少なくとも20分の添加時間後に、更に15分の固有均質化時間を開始し、次いでまず後接続されたストレーナ押出機に取り出した。100μmの洗浄工程と、実施例1と同様に切断された供給形の包装は更に25〜30分かかり、それによりこの架橋系の臨界ゴム温度65℃を超える局所的な加熱が生じる、すなわち架橋活性のMH製品の部分的な加硫を回避できる。標準的ロール混練機の平均的な生産性は、従ってかかる良く作用する添加剤を用いて125kg/hである。単位時間あたりのより高い混合量では、商品における不均一性と、ひいては押出使用における、すなわち顧客での加工問題に危険性がある。これは、品質制御において、特にバッチの種々のロール混合物の加硫測定器値(迅速試験としての架橋速度)の特異的な比較において確認することもできる。
Claims (9)
- 高められた温度で加硫する、25℃で測定された粘度少なくとも500Pa・sを有するオルガノポリシロキサン組成物(MH)の連続的な製造方法であって、高粘性のオルガノポリシロキサン(OH)及び架橋性添加剤(H)を、少なくとも2つの一列に並んで配置された混練室を有し、そのそれぞれが2つの軸平行な同方向又は逆方向に駆動可能な混練工具を有し、かつ混練工具の軸に対して横方向に通過可能な開口部を通じて互いに接続されていて、第一の混練室が供給口を有し、そして最後の混練室が排出口を有している混練カスケードにおいて混合及び均質化し、その際、架橋性添加剤(H)を収容する混練室中の温度が高くても95℃である方法。
- オルガノポリシロキサン(OH)及び架橋性添加剤(H)及び場合によりその他の添加剤(Z)を一定の質量比で混合及び均質化する、請求項1記載の方法。
- 添加剤(Z)が、促進剤、抑制剤、安定化剤、顔料、着色ペースト、難燃性又は伝熱性の金属酸化物添加剤、電気的特性の改善剤、充填剤、オルガノポリシロキサン改質剤、ストラクチャ改善剤、加工助剤、分散助剤、疎水化剤、解ストラクチャ試薬、可塑剤、定着剤、熱安定剤及び酸化防止剤から選択される、請求項1又は2記載の方法。
- 混練カスケードが3〜10個の混練室からなる、請求項1から3までのいずれか1項記載の方法。
- オルガノポリシロキサン組成物(MH)の充填剤含量が5〜80質量%である、請求項1から4までのいずれか1項記載の方法。
- 架橋性添加剤(H)として、アルキルペルオキシド、ケタールペルオキシド及びアロイルペルオキシドから選択されるペルオキシド架橋剤を混加する、請求項1から6までのいずれか1項記載の方法。
- 架橋性添加剤(H)として、H−Si官能性のシロキサン並びに白金触媒又はロジウム触媒及び抑制剤を混加する、請求項1から6までのいずれか1項記載の方法。
- オルガノポリシロキサン(MH)を最後の混練室後に成形用排出装置に送る、請求項1から8までのいずれか1項記載の方法。
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US7943697B2 (en) | 2005-07-11 | 2011-05-17 | Saint-Gobain Performance Plastics Corporation | Radiation resistant silicone formulations and medical devices formed of same |
US7939014B2 (en) | 2005-07-11 | 2011-05-10 | Saint-Gobain Performance Plastics Corporation | Radiation resistant silicone formulations and medical devices formed of same |
US9133340B2 (en) | 2005-07-11 | 2015-09-15 | Saint-Gobain Performance Plastics Corporation | Radiation resistant silicone formulations and medical devices formed of same |
US20080166509A1 (en) * | 2007-01-08 | 2008-07-10 | Saint-Gobain Performance Plastics Corporation | Silicone tubing formulations and methods for making same |
DE102007031989A1 (de) | 2007-07-10 | 2009-01-15 | Contitech Vibration Control Gmbh | Vorrichtung zur Herstellung von Elastomermischungen |
DE102008055035A1 (de) * | 2008-12-19 | 2010-07-01 | Wacker Chemie Ag | Kontinuierliches Verfahren zur Herstellung von Grundmassen für Siliconzusammensetzungen mit verbesserter Stabilität |
KR101311189B1 (ko) * | 2011-12-23 | 2013-09-26 | 강윤정 | 방화재용 실리콘 고분자 조성물 및 그 제조방법 |
FI20155022A (fi) * | 2015-01-13 | 2016-07-14 | Oy Pro-Hydro Ab | Menetelmä ja laitejärjestely silikonimassan sekoittamiseksi |
FR3093457A1 (fr) * | 2019-03-06 | 2020-09-11 | Compagnie Generale Des Etablissements Michelin | Machine de Mélangeage et d’Extrusion à Bi-Vis avec Éléments Amovibles |
CN112123619B (zh) * | 2020-09-08 | 2022-04-05 | 湖南连心科技有限公司 | 一种用于粉末涂料制备的挤出机进料装置 |
EP4063091A1 (de) * | 2021-03-26 | 2022-09-28 | Starlinger & Co Gesellschaft m.b.H. | Vorrichtung und verfahren zur wärmebehandlung von thermoplastischen kunststoffschmelzen |
CN114701099B (zh) * | 2022-04-07 | 2023-08-08 | 华南理工大学 | 一种模块化高分子材料双转子泵式输运设备及输运方法 |
CN115814669A (zh) * | 2023-02-13 | 2023-03-21 | 山东轩友新材料科技有限公司 | 硅酮胶连续化着色*** |
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US20060247406A1 (en) | 2006-11-02 |
CN100519659C (zh) | 2009-07-29 |
EP1717002A1 (de) | 2006-11-02 |
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