JP6334064B2 - エチレンの重合方法 - Google Patents
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Description
本発明は、(a)Ti、Mg、ハロゲン及び任意に電子供与体を含む固体触媒成分、(b)アルミニウムアルキル化合物、及び(c)特定のハロゲン化アルコールを含む触媒の存在下で行われる、エチレン及びそのオレフィンCH2=CHR(ここで、Rは、炭素数1〜12のアルキル、シクロアルキル又はアリール基である)との混合物の気相重合方法に関するものである。本方法は、エタン形成の程度が低減されることを特徴とする。
a)水素、及び(A)二塩化マグネシウム上に担持されたチタン化合物を含む固体触媒成分及び(B)アルミニウムアルキル化合物を含む触媒系の存在下で、気相反応器で、エチレンを任意に一つ以上のコモノマーと共に重合する工程;
b)工程a)より少ない量の水素及び工程(a)で定義された触媒系の存在下で、他の気相反応器で、エチレンを任意に一つ以上のコモノマーと共に重合する工程;
前記気相反応器のうち少なくとも一つにおいて、成長する重合体粒子が高速流動化又は輸送条件下では、第1重合区域(上昇部)を通って上方に流れ、前記上昇部から出た後、第2重合区域(下降部)に入り、前記第2重合区域の重力の作用下で下方に流れ、前記下降部から出た後、上昇部内に再び投入することで、前記2個の重合区域の間で重合体の循環を確立し、前記反応器のうちの少なくとも一つにおいて、重合は、更に(C)式AOHのハロゲン化アルコール(ここで、Aは、水素原子の少なくとも一つが塩素で置換されたC1−C10飽和又は不飽和炭化水素基である)の存在下で行われる。第1重合区域(上昇部)では、一つ以上のオレフィン(エチレン及びコモノマー)を含む気体混合物を重合体粒子の輸送速度より速い速度で供給することで、高速流動化条件が確立される。前記気体混合物の速度は、好ましくは、0.5〜15m/s、より好ましくは、0.8〜5m/sである。用語「輸送速度」及び「高速流動化条件」とは、当該技術分野で周知である;その定義は、例えば、文献「D. Geldart, Gas Fluidisation Technology, page 155 et seq., J. Wiley & Sons Ltd., 1986」を参照されたい。
実施例
特性化
MIE流動指数:ASTM−D 1238 条件E
MIF流動指数:ASTM−D 1238 条件F
MIP流動指数:ASTM−D 1238 条件P
嵩密度:DIN−53194
固体触媒成分(A)の製造方法
重合工程は、連続的に作動し、基本的に小型反応器(予備接触ポット)付きプラントで行った。ここで触媒成分が混合されて触媒系を形成し、前の反応器で形成された触媒系を受ける第2輸送容器及び前の反応器から出てくる触媒混合物を受け入るプロパンを有する流動化条件下で維持された一つの流動床反応器(重合反応器)を含む。
前述のように製造された固体触媒成分
希釈剤としての液体プロパン
TIBAL溶液
約3モルのアルコールを含有する塩化マグネシウム及びアルコール付加物は、10000RPMの代わりに2000RPMで作動することを除いては、アメリカ特許第4,399,054号の実施例2に記載された方法に従って製造した。この付加物をアルコールの重量含量24.4%に達するまで窒素気流流下で50〜150℃の温度範囲で熱処理した。
Claims (8)
- (A)二塩化マグネシウム上に担持されたチタン化合物を含む固体触媒成分、(B)アルミニウムアルキル化合物、及び(C)式AOHのハロゲン化アルコール(ここで、Aは、水素原子の少なくとも一つが、塩素で置換されたC 2 −C10飽和炭化水素基である)を含む触媒系の存在下で、エチレン、水素、不活性流動化ガス及び任意に一つ以上のアルファオレフィンCH2=CHR(ここで、Rは、C1−C10炭化水素基である)を含むガス混合物を重合する工程を含むエチレン(共)重合体の製造方法において、
前記方法がハロゲン化アルコール(C)の不在下で同じ重合条件下で生成された量より低い量のエタンを生成することを特徴とする製造方法。 - A基が、4個以下の炭素原子を有する飽和直鎖炭化水素基である請求項1に記載の方法。
- 前記塩素原子が、ヒドロキシル基に対して、アルファ位の炭素原子上に連結された一つ以上の水素を置換する請求項1に記載の方法。
- 前記化合物(C)が、2,2,2−トリクロロエタノールである請求項1〜3のいずれか1項に記載の方法。
- ハロゲン化アルコール(C)が、モル比(C)/Tiが0.1〜10の範囲の量で使用され、ここで、Tiが、成分(A)内のチタンモル量である請求項1に記載の方法。
- 固体触媒成分(A)が、例えば、エーテル、エステル、アミン及びケトンの中から選ばれる内部供与体(ID)を更に含む請求項1に記載の方法。
- 以下の工程を任意の相互順序で含む方法:
a)水素、及び(A)二塩化マグネシウム上に担持されたチタン化合物を含む固体触媒成分及び(B)アルミニウムアルキル化合物を含む触媒系の存在下で、気相反応器で、エチレンを任意に一つ以上のコモノマーと共に重合する工程;
b)工程a)より少ない量の水素及び工程(a)で定義された触媒系の存在下で、他の気相反応器で、エチレンを任意に一つ以上のコモノマーと共に重合する工程;
前記気相反応器のうち少なくとも一つにおいて、成長する重合体粒子が高速流動化又は輸送条件下では、第1重合区域(上昇部)を通って上方に流れ、前記上昇部から出た後、第2重合区域(下降部)に入り、前記第2重合区域の重力の作用下で下方に流れ、前記下降部から出た後、上昇部内に再び投入することで、前記2個の重合区域の間で重合体の循環を確立し、前記反応器のうちの少なくとも一つにおいて、重合は、更に(C)式AOHのハロゲン化アルコール(ここで、Aは、水素原子の少なくとも一つが塩素で置換されたC 2 −C10飽和炭化水素基である)の存在下で行われる。 - (A)二塩化マグネシウム上に担持されたチタン化合物を含む固体触媒成分及び(B)アルミニウムアルキル化合物を含む触媒系の存在下で、エチレン、水素、不活性流動化ガス及び任意に一つ以上のアルファオレフィンCH2=CHR(ここで、Rは、C1−C10炭化水素基である)を含む気体混合物の重合を含む重合工程でエタン生成を低減させる方法において、
前記方法が、更に式AOHのハロゲン化アルコール(ここで、Aは、水素原子の少なくとも一つが塩素で置換されたC 2 −C10飽和炭化水素基である)の存在下で行われる方法。
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EP14196869.3 | 2014-12-09 | ||
EP14196869 | 2014-12-09 | ||
PCT/EP2015/078127 WO2016091644A1 (en) | 2014-12-09 | 2015-12-01 | Process for the polymerization of ethylene |
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JP (1) | JP6334064B2 (ja) |
KR (1) | KR101851523B1 (ja) |
CN (1) | CN107001519B (ja) |
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CA3162303A1 (en) * | 2019-12-19 | 2021-06-24 | Angela I. Padilla-Acevedo | Gas-phase biphenylphenol polymerization catalysts |
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US4954470A (en) * | 1988-01-14 | 1990-09-04 | Mobil Oil Corporation | Chlorinated alcohol-containing catalyst composition for polymerizing alpha-olefins |
US5093443A (en) * | 1988-01-14 | 1992-03-03 | Mobil Oil Corporation | Alpha-olefins polymerization with chlorinated alcohol-containing catalyst composition |
US4849389A (en) * | 1988-01-14 | 1989-07-18 | Mobil Oil Corporation | Catalyst composition for polymerizing alpha-olefin polymers of narrow molecular weight distribution |
JP2782537B2 (ja) * | 1989-08-28 | 1998-08-06 | 東燃株式会社 | オレフィン重合用触媒成分の製造方法 |
US5070057A (en) * | 1990-04-02 | 1991-12-03 | Union Carbide Chemicals And Plastics Technology Corporation | Simplified polyethylene catalyst system |
FR2666337B1 (fr) | 1990-08-31 | 1994-04-08 | Bp Chemicals Snc | Procede regule de polymerisation d'olefine en phase gazeuse effectue a l'aide d'un catalyseur de type ziegler-natta. |
FR2680793B1 (fr) | 1991-08-30 | 1994-09-09 | Bp Chemicals Snc | Procede de fabrication d'un polymere de l'ethylene. |
JP3539873B2 (ja) * | 1998-07-29 | 2004-07-07 | 出光石油化学株式会社 | エチレン系重合体製造用触媒及び該触媒を用いるエチレン系重合体の製造方法 |
WO2002048207A1 (fr) | 2000-12-15 | 2002-06-20 | China Petro-Chemical Corporation | Catalyseur spherique pour (co)polymerisation d'ethylene, sa preparation et son utilisation |
KR100522617B1 (ko) | 2000-12-15 | 2005-10-19 | 차이나 페트로-케미칼 코포레이션 | 에틸렌 (공)중합용 담지촉매, 그 제조 방법 및 이용 방법 |
US6660817B2 (en) * | 2001-07-24 | 2003-12-09 | Eastman Chemical Company | Process for the polymerization of ethylene and interpolymers thereof |
US20090318643A1 (en) | 2005-10-31 | 2009-12-24 | China Petroleum & Chemical Corporation | Catalyst Component for Ethylene Polymerization, Preparation Thereof and Catalyst Comprising the Same |
CN102432709B (zh) * | 2010-09-29 | 2013-06-05 | 中国石油化工股份有限公司 | 一种用于乙烯聚合含钛球型催化剂组分及催化剂 |
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US10077322B2 (en) | 2018-09-18 |
US20170327603A1 (en) | 2017-11-16 |
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JP2017535660A (ja) | 2017-11-30 |
RU2660910C1 (ru) | 2018-07-11 |
EP3230324A1 (en) | 2017-10-18 |
KR20170084244A (ko) | 2017-07-19 |
CN107001519A (zh) | 2017-08-01 |
BR112017010681A2 (pt) | 2017-12-26 |
WO2016091644A1 (en) | 2016-06-16 |
BR112017010681B1 (pt) | 2022-04-12 |
KR101851523B1 (ko) | 2018-04-24 |
EP3230324B1 (en) | 2018-09-12 |
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