JP2019529625A - 発泡性ケーブル絶縁体用核形成剤 - Google Patents
発泡性ケーブル絶縁体用核形成剤 Download PDFInfo
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- JP2019529625A JP2019529625A JP2019512892A JP2019512892A JP2019529625A JP 2019529625 A JP2019529625 A JP 2019529625A JP 2019512892 A JP2019512892 A JP 2019512892A JP 2019512892 A JP2019512892 A JP 2019512892A JP 2019529625 A JP2019529625 A JP 2019529625A
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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Abstract
Description
(A)45〜95重量%のHDPEと、
(B)4〜54重量%のLDPEと、
(C)0.01〜2重量%の核形成剤であって、核形成剤の重量に基づいた重量%で、
(1)20〜80重量%のフッ素樹脂、および
(2)80〜20重量%の膨張性ポリマーマイクロスフェアを含む核形成剤と、を含む組成物である。
(A’)50〜95重量%の、HDPEおよびLDPEのうちの少なくとも1つと、
(C)5〜50重量%の核形成剤であって、核形成剤の重量に基づいた重量%で、
(1)20〜80重量%のフッ素樹脂、および
(2)80〜20重量%の膨張性ポリマーマイクロスフェアを含む核形成剤とを、含むマスターバッチである。
(1)押出区域において、(a)HDPE、(b)LDPE、および(c)核形成剤であって、核形成剤の重量に基づいた重量%で、
(i)20〜80重量%のフッ素樹脂、および
(ii)80〜20重量%の膨張性ポリマーマイクロスフェアを含む核形成剤の溶融ブレンドを調製するステップと、
(2)押出条件下で(1)の混合物をワイヤまたはケーブル上に押し出すステップと、を含むプロセスである。
米国特許実務の目的のため、任意の参照される特許、特許出願、または刊行物の内容は、特に定義の開示(本開示に具体的に提供されるあらゆる定義と矛盾しない程度に)および当該技術分野における一般的知識に関して、それらの全体が参照により組み込まれる(またはその同等の米国版が参照によりそのように組み込まれる)。
「高密度ポリエチレン」(または「HDPE」)は、少なくとも0.94g/cc、または少なくとも0.94g/cc〜0.98g/ccの密度を有するエチレン系ポリマーである。HDPEは、0.1g/10分〜25g/10分のメルトインデックスを有する。
LDPE樹脂は当該技術分野において周知であり、市販されており、チーグラーナッタ、メタロセンまたは幾何拘束型(CGC)などが触媒する溶液、気相またはスラリー相を含むがこれらに限定されない、多種多様なプロセスのうちのいずれか1つによって作製される。これらの樹脂は、0.91〜0.94g/cm3の範囲の密度を有し得る。様々な実施形態において、LDPEは、少なくとも0.915g/cm3であるが、0.94g/cm3未満、もしくは0.93g/cm3未満、または0.920〜0.925g/cm3の範囲内の密度を有し得る。本明細書に提供されるポリマー密度は、ASTM D792に従って決定される。使用に好適なLDPEは、20グラム/10分未満、もしくは0.1〜10g/10分、2〜8g/10分、4〜8g/10分の範囲のメルトインデックスI2(190℃/2.16kg)を有し得るか、または約6g/10分のI2を有する。本明細書に提供されるメルトインデックスは、ASTM方法D1238に従って決定される。一般に、LDPEは、広い分子量分布(「MWD」)を有し、比較的高い多分散性指数(「PDI」、つまり重量平均分子量対数平均分子量の比)をもたらす。LDPEは、ゲル浸透クロマトグラフィーによって決定された、1.0〜30.0の範囲内、または2.0〜15.0の範囲内の多分散指数(「PDI」)を有し得る。
HDPE/LDPEのブレンドは、典型的には、ブレンドの重量に基づいた重量パーセント(重量%)で、50、または60、または70、80、85パーセントを超えるHDPEを含み、ブレンドの残りはLDPEを含む。典型的には、HDPE/LDPEブレンドは、98、または95、または90重量パーセントを超えてはHDPEを含まず、ブレンドの残りはLDPEを含む。
ポリテトラフルオロエチレン(PTFE)
既知であるか、または今後発見される任意のフッ素樹脂が、本明細書で用いられ得る。好適なフッ素樹脂の例としては、ポリテトラフルオロエチレン(「PTFE」)、テトラフルオロエチレン−ペルフルオロアルキルビニルエーテルコポリマー(「PFA」)、エチレン−テトラフルオロエチレンコポリマー(「ETFE」)、テトラフルオロエチレン−ヘキサフルオロプロピレンコポリマー(「FEP」)、テトラフルオロエチレン−エチレンコポリマー、ポリフッ化ビニリデン(「PVdF」)、ポリクロロトリフルオロエチレン(「PCTFE」)、及びクロロトリフルオロエチレン−エチレンコポリマー(「ECTFE」)などが挙げられるが、これらに限定されず、PTFE、PFA、及びETFEが好ましい。1つ以上の実施形態において、フッ素樹脂は、PTFEを含む。1つ以上の実施形態において、フッ素樹脂は、PTFEからなる。
平均粒径(μm)=(ΣND3/ΣN)1/3
粒径の計算は、USP6,121,335に更に例証される。凝集体サイズの計算は、粒径決定について上述した様式と同じ様式で決定される。
米国特許第3,615,972号に記載の膨張性ポリマーミクロスフェアは、熱にさらされると劇的に膨張するのに適合している。これらのミクロスフェアは、揮発性流体を封入している樹脂材料の本体を含む単一セルの粒子である。加熱すると、熱可塑性ミクロスフェアの樹脂材料は軟化し、揮発性材料は膨張し、ミクロスフェア全体のサイズの実質的な増加を引き起こす。冷却すると、ミクロスフェアのシェル中の樹脂材料は流動を停止し、その大きくなった寸法を保持する傾向があり、ミクロスフェア内部の揮発性流体は収縮する傾向があり、ミクロスフェア内に圧力の低減を引き起こす。
発泡性ポリマーミクロスフェア対フッ素樹脂、好ましくはPTFEの重量比は、典型的には20:80〜70:30、およびさらにより典型的には20:80〜50:50である。ポリオレフィン組成物に添加されるフッ素樹脂およびミクロスフェアの量として表すと、ポリオレフィン組成物に十分なフッ素樹脂が添加されて、典型的には0.01〜1重量%、より典型的には0.05〜0.6重量%、さらにより典型的には0.1〜0.3重量%のポリオレフィン組成物を含むフッ素樹脂をもたらす。十分な膨張性ポリマーミクロスフェアをポリオレフィン組成物に添加して、典型的には300百万分率(ppm)〜5,000ppm、より典型的には500ppm〜5,000ppm、およびさらにより典型的には500ppm〜3,000ppmのポリオレフィン組成物を含むフッ素樹脂をもたらす。
抗酸化剤
一実施形態において、本発明の組成物は、1つ以上の抗酸化剤を含む。抗酸化剤の例としては、テトラキス[メチレン(3,5−ジ−tert−ブチル−4−ヒドロキシヒドロ−シンナメート)]メタンなどのヒンダードフェノール;ビス[(ベータ−(3,5−ジtert−ブチル−4−ヒドロキシベンジル)−メチル−カルボキシエチル)]スルフィド;4,4’−チオビス(2−メチル−6−tert−ブチル−フェノール);4,4’−チオビス(2−tert−ブチル−5−メチルフェノール);2,2’−チオビス(4−メチル−6−tert−ブチルフェノール);およびチオジエチレンビス(3,5−ジ−tert−ブチル−4−ヒドロキシ)ヒドロシンナメート;トリス(2,4−ジ−tert−ブチルフェニル)ホスファイトおよびジ−tert−ブチルフェニル−ホスホナイトなどのホスファイトおよびホスホナイト;ジラウリルチオジプロピオネート、ジミリスチルチオジプロピオネート、およびジステアリルチオジプロピオネートなどのチオ化合物;様々なシロキサン;重合2,2,4−トリメチル−1,2−ジヒドロキノリン;n、n’−ビス(1,4−ジメチルペンチル−p−フェニレンジアミン);アルキル化ジフェニルアミン、4,4’−ビス(アルファ,アルファ−ジメチルベンジル)ジフェニルアミン;ジフェニル−p−フェニレンジアミン、混合ジアリール−p−フェニレンジアミン、および他のヒンダードアミン抗劣化剤または安定剤が挙げられるが、これらに限定されない。抗酸化剤は、例えば、組成物の重量に基づいて、0.01〜5重量%、または0.01〜0.1重量%、または0.01〜0.3重量%の量で使用することができる。
一実施形態において、本発明の組成物は、1つ以上のセル安定剤を含む。セル安定剤の例としては、グリセロールモノステアレート(GMS)、グリセロールモノパルミテート(GMP)、パルミチドおよび/またはアミドが挙げられるが、これらに限定されない。好適なアミドとしては、ステアリルステアラミド、パルミチドおよび/またはステアラミドが挙げられるが、これらに限定されない。好適な混合物としては、GMSとGMPとの混合物、またはステアラミドとパルミタミドとを含む混合物が挙げられるが、これらに限定されない。セル安定剤は、例えば、組成物の重量に基づいて、0.01〜5重量%、または0.01〜0.1重量%、または0.01〜0.3重量%の量で使用することができる。
本発明で使用されるポリオレフィン組成物は、必要に応じてまたは所望のように1つ以上の他の添加剤を含有してもよい。代表的なこれらの他の添加剤としては、加工助剤、潤滑剤、発泡剤、界面活性剤、流動助剤、粘度制御剤、着色剤、金属阻害剤などが挙げられるが、これらに限定されない。これらの添加剤は、加工前または加工中のいずれかでポリマー(複数可)に添加され得る。ポリオレフィン組成物中の任意の特定の添加剤の量は、典型的には、0.01〜1重量%、より典型的には0.01〜0.5重量%、およびさらにより典型的には0.01〜0.3重量%であり、ポリオレフィン組成物中のこれらの他の添加剤の総量は、少しでも存在する場合、典型的には0.01〜5重量%、より典型的には0.01〜2重量%、およびさらにより典型的には0.01〜1重量%である。
本発明のブレンド組成物の配合は、当業者に既知の標準的な手段によって実施することができる。配合装置の例は、BANBURY(商標)、またはBOLLING(商標)内部混合機などの内部バッチ混合機である。あるいは、FARREL(商標)連続混合機、WERNERおよびPFLEIDERER(商標)二軸スクリュー混合機、またはBUSS(商標)混錬連続押出機などの、連続単軸または二軸スクリュー混合機を使用してもよい。利用される混合機の種類、および混合機の操作条件は、粘度、体積抵抗率、および押出表面の滑らかさなどの組成物の特性に影響を及ぼし得る。
一実施形態において、本発明は、キャリア樹脂としてHDPEおよびLDPEのうちの1つ以上と、核形成剤としてフッ素樹脂、特にPTFEと膨張性ポリマーミクロスフェアとの混合物とを含むマスターバッチである。一実施形態において、本発明は、マスターバッチであって、マスターバッチの重量に基づいた重量パーセントで、
(A’)50〜95重量%の、HDPEおよびLDPEのうちの少なくとも1つと、
(C)5〜50重量%の核形成剤であって、核形成剤の重量に基づいた重量%で、
(1)20〜80重量%のPTFE、および
(2)80〜20重量%の膨張性ポリマーマイクロスフェアを含む核形成剤と、を含むマスターバッチである。
発泡剤は、押出温度、発泡条件、及び発泡体形成法などにとって好適な1つ以上のものである。最終形態の絶縁発泡体層が押出形成と同時に形成される場合、例えば、窒素、炭素ガス(例えば、CO、CO2など)、ヘリウム、及びアルゴンなどの不活性気体、メタン、プロパン、ブタン、及びペンタンなどの炭化水素、例えば、ジクロロジフルオロメタン、ジクロロモノフルオロメタン、モノクロロジフルオロメタン、トリクロロモノフルオロメタン、モノクロロペンタフルオロエタン、及びトリクロロトリフルオロエタンなどのハロゲン化炭化水素が使用される。使用される発泡剤の量は、変動し得る。典型的には、それは、100重量部の発泡されるポリオレフィン組成物当たり0.001〜0.1重量部、より典型的には0.005〜0.05重量部である。発泡剤は、発泡される有機ポリマーと事前に混合されてもよく、または押出機のバレル上に形成されている発泡剤供給口から押出機内に供給されてもよい。
本発明のポリオレフィン組成物は、既知の方法および既知の装置を使用して発泡させる。典型的には、発泡体は、核剤を含有するポリオレフィン組成物を、組成物が高圧区域にある間に、例えば、発泡剤の注入などの発泡押出条件下で操作される押出機を使用して押出し、次いで組成物を低圧区域に押し出すことによって生成される。発泡プロセスは、C.P.Park in Polyolefin Foam,Chapter9,Handbook of Polymer Foams and Technology,edited by D.Klempner and K.C.Frisch,Hanser Publishers(1991)にさらに記載されている。
(1)押出区域において、(a)HDPE、(b)LDPE、および(c)核形成剤であって、核形成剤の重量に基づいた重量%で、
(i)20〜80重量%のPTFE、および
(ii)80〜20重量%の膨張性ポリマーマイクロスフェアを含む核形成剤の溶融ブレンドを調製するステップと、
(2)押出条件下で(1)の混合物をワイヤまたはケーブル上に押し出すステップと、を含むプロセスである。
これらの実施例で使用した材料を表1に記載する。
物理的発泡実験を、ガス注入システムを備えた単軸スクリュー押出機で行った。スクリュー直径は、L/D比40で50mmである。ガス注入点は、発泡剤としてCO2を用いるスクリューの中間に位置する。温度プロファイルは、140/175/180(気体注入)/170/145(静的混合機)/143(ダイ)である。HDPE、LDPE、および核形成剤MBをまず乾燥ブレンドし、次いで押出機の上流に供給する。あるいは、AXELERON(商標)CX A−6944NT、AXELERON(商標)CX B−1258NT、および核形成剤マスターバッチを「オールインワン」配合物へと配合し、次いでガス注入押出機で発泡させる。
空隙率
膨張比を、発泡前後の試料の密度に基づいて計算した。発泡物品および固体プラークの密度を、ASTM D792に従って測定した。
液体窒素を利用して、得られたPE発泡試料を破砕し、次いで異なる倍率で得たIR走査電子顕微鏡(SEM)画像によって被覆した。SEM写真の分析を通して平均セルサイズを得た。
Claims (15)
- 組成物であって、前記組成物の重量に基づいた重量パーセントで、
(A)45〜95重量%のHDPEと、
(B)4〜54重量%のLDPEと、
(C)0.01〜2重量%の核形成剤であって、前記核形成剤の重量に基づいた重量%で、
(1)20〜80重量%のフッ素樹脂、および
(2)80〜20重量%の膨張性ポリマーマイクロスフェアを含む核形成剤と、を含む、組成物。 - 前記フッ素樹脂が、ポリテトラフルオロエチレン(「PTFE」)、テトラフルオロエチレン−パーフルオロアルキルビニルエーテルコポリマー(「PFA」)、またはエチレン−テトラフルオロエチレンコポリマー(「ETFE」)のうちの1つを含む、請求項1に記載の組成物。
- 前記HDPEが二峰性である、請求項1に記載の組成物。
- 抗酸化剤およびセル安定剤のうちの少なくとも1つをさらに含む、請求項1〜3のいずれか一項に記載の組成物。
- マスターバッチであって、前記マスターバッチの重量に基づいた重量パーセントで、
(A’)50〜95重量%の、HDPEおよびLDPEのうちの少なくとも1つと、
(C)5〜50重量%の核形成剤であって、前記核形成剤の重量に基づいた重量%で、
(1)20〜80重量%のフッ素樹脂、および
(2)80〜20重量%の膨張性ポリマーマイクロスフェアを含む核形成剤と、を含む、マスターバッチ。 - HDPEとLDPEの両方を含む、請求項5に記載のマスターバッチ。
- 前記フッ素樹脂が、ポリテトラフルオロエチレン(「PTFE」)、テトラフルオロエチレン−パーフルオロアルキルビニルエーテルコポリマー(「PFA」)、またはエチレン−テトラフルオロエチレンコポリマー(「ETFE」)のうちの1つを含む、請求項5に記載のマスターバッチ。
- 前記HDPEが二峰性である、請求項5〜7のいずれか一項に記載のマスターバッチ。
- 発泡性ポリエチレン組成物でワイヤまたはケーブルを被覆するプロセスであって、
(1)押出区域において、(a)HDPE、(b)LDPE、および(c)核形成剤であって、前記核形成剤の重量に基づいた重量%で、
(i)20〜80重量%のフッ素樹脂、および
(ii)80〜20重量%の膨張性ポリマーマイクロスフェアを含む核形成剤の溶融ブレンドを調製するステップと、
(2)押出条件下で(1)の前記混合物をワイヤまたはケーブル上に押し出すステップと、を含むプロセス。 - 前記フッ素樹脂が、ポリテトラフルオロエチレン(「PTFE」)、テトラフルオロエチレン−パーフルオロアルキルビニルエーテルコポリマー(「PFA」)、またはエチレン−テトラフルオロエチレンコポリマー(「ETFE」)のうちの1つを含む、請求項9に記載のプロセス。
- 前記HDPEが二峰性である、請求項9に記載のプロセス。
- 前記発泡性組成物が、抗酸化剤およびセル安定剤のうちの1つ以上をさらに含む、請求項9〜11のいずれか一項に記載のプロセス。
- 前記HDPE、LDPEおよび核形成剤が、押出区域の外側で予備配合される、請求項12に記載のプロセス。
- 前記核形成剤が、マスターバッチの一部として押出区域に供給される、請求項12に記載のプロセス。
- 前記HDPE、LDPEおよび核形成剤が、予備配合ペレットとして押出区域に供給される、請求項12に記載のプロセス。
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US20190203011A1 (en) | 2019-07-04 |
US10858492B2 (en) | 2020-12-08 |
KR20190055094A (ko) | 2019-05-22 |
BR112019003983A2 (pt) | 2019-05-28 |
BR112019003983B1 (pt) | 2022-09-13 |
WO2018049555A1 (en) | 2018-03-22 |
MX2019002857A (es) | 2019-07-15 |
EP3512912B1 (en) | 2021-10-20 |
EP3512912A4 (en) | 2020-05-06 |
CN109689767B (zh) | 2022-02-18 |
KR102589718B1 (ko) | 2023-10-18 |
CA3036390A1 (en) | 2018-03-22 |
CN109689767A (zh) | 2019-04-26 |
JP6860654B2 (ja) | 2021-04-21 |
EP3512912A1 (en) | 2019-07-24 |
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