JPH05504786A - ポリエチレン合成の為のマルチステージプロセス - Google Patents
ポリエチレン合成の為のマルチステージプロセスInfo
- Publication number
- JPH05504786A JPH05504786A JP4501688A JP50168891A JPH05504786A JP H05504786 A JPH05504786 A JP H05504786A JP 4501688 A JP4501688 A JP 4501688A JP 50168891 A JP50168891 A JP 50168891A JP H05504786 A JPH05504786 A JP H05504786A
- Authority
- JP
- Japan
- Prior art keywords
- polymerization
- ethylene
- loop reactor
- reactor
- reaction
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F297/00—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer
- C08F297/06—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type
- C08F297/08—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type polymerising mono-olefins
- C08F297/083—Macromolecular compounds obtained by successively polymerising different monomer systems using a catalyst of the ionic or coordination type without deactivating the intermediate polymer using a catalyst of the coordination type polymerising mono-olefins the monomers being ethylene or propylene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/2435—Loop-type reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
- B01J8/18—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles
- B01J8/24—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with fluidised particles according to "fluidised-bed" technique
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F110/00—Homopolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F110/02—Ethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F210/00—Copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond
- C08F210/16—Copolymers of ethene with alpha-alkenes, e.g. EP rubbers
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10S526/00—Synthetic resins or natural rubbers -- part of the class 520 series
- Y10S526/905—Polymerization in presence of transition metal containing catalyst in presence of hydrogen
Abstract
(57)【要約】本公報は電子出願前の出願データであるため要約のデータは記録されません。
Description
【発明の詳細な説明】
ポリエチレン合成の為のマルチステージプロセス本発明は、マルチステージプロ
セスにおけるバイモーダル及び/あるいは広範な分子量分布を有するポリエチレ
ンを合成するためのプロセスに関する。
−チが示唆されている。
済的なものや非現実的なものにする。
ロセスの例としては、GB 1532231. US 4.368291.It
s 4309521. US 4368304おより283512があげられる
。
明確にするために、さらに詳細に再調査される。
US 4368291には2ステツプの液相−気相プロセスが開示されており、
ここでは、オレフィンは攪拌タンクタイプの反応器内で液状炭化水素媒体中で重
合され相プロセスにおいて使用される。これらの公報はプロセスそれ自身につい
ては同等有用な情報を提供していない。
に重合ステップである。ループ反応器が気相反応器に関連して言及されているた
めに、この特許公報はここで単に参照されている。
合を伴うスラリー相重合を使用することでは不可能であったものである。
反応混合物からのより良い熱移動を与え、それゆえより均一な温度特性と高スラ
リー密度を与え、そしてさらにそれゆえより良い混合を与えるためである。
選択のフレキシビリティを許す。
ンモノマーおよび任意に水素および/又はコモノマーの存在下で完結される。
チタンで、該触媒は非担持、あるいは無機担体、例えばシリカ、アルミナ、ある
いはシリカ−アルミナの様なものに担持されていてもよい。
好ましい触媒は、例えば、フィンランド特許出願905430.902123,
901895.900842.906323 、905703.895526.
894266 、893621 、892153および872459に開示され
ているものがある。しかし、本発明によるプロセスは触媒特異プロセスではない
ことは注意すべきことであり、それゆえ適切な活性と制御可能な分子量を与える
どの様な触媒も本発明によるプロセスに於いて使用可能である。
本発明によるプロセスに於ける第一ステップは、ループ反応器内で成し遂げらね
〜その中に不活性炭化水素媒体、エチレン、水素、触媒、および任意のコモノマ
ーが供給される。ループ反応器は従来のデザインのものでよく、それは反応器へ
の様々な供給要素を供給するための部材、反応器を通ってポリマー−炭化水素サ
スペンションを循環させるための部材、重合の熱を取り除く熱伝達部材、および
反応器からポリマースラリーを放出するための部材を含んでいる。
重合媒体として、不活性低沸点炭化水素が使用可能である。該炭化水素の例とし
ては、プロパン、ブタン、ペンタン、ヘキサン、ヘプタン、オクタンのような脂
肪族炭化水素と、シクロヘキサン、シクロへブタンの様な脂環式炭化水素である
。上記のどの炭化水素の混合物も使用可能である。
触媒で好ましくは炭化水素スラリーとしてで助触媒を伴うもの、不活性炭化水素
媒体、エチレン、水素、および任意のコモノマーは連続的にループ反応器に供給
される。反応混合物は連続的に反応器を通って循環さね、それによって粒子状の
ポリエチレンと不活性炭化水素のスラリーが形成される。ループ反応器の条件は
、総生産の少なくとも20%、しかし好ましくは40〜90%か該ループ反応器
内で重合されるように選ばれる。温度は通常75〜110℃の間から選ばれ、好
ましくは85〜100℃である。普通の反応条件下で、温度がポリマーの融点以
下より低くなるようになされた、より高い温度も使用可能である。反応圧力は4
0〜90バールの間から選ぶことができ、好ましくは50〜65バールである。
滞留時間は少なくとも10分であるべきであり、しかし好ましくは1〜2時間の
間である。水素のエチレンに対するモル比は、所望する生成物のメルトインデッ
クスに依存するものの間から選ばれるが、バイモーダルポリエチレンの製造にお
いては、0〜1.0の間であろう。超臨界状態下で、不活性炭化水素媒体として
炭化水素、好ましくはプロパンが使用されたならば、特別な利点が達成される。
これは、反応がその様な状態で行わわ−そこでは温度と圧力が、エチレン、プロ
パン、水素、および任意のコモノマーによって形成される反応混合物の対応する
臨界点以上であるが、温度は形成されたポリマーの融点以下であることを意味す
る。それによって、ループ反応器内の温度は85〜110℃の間で、圧力は60
〜90バールの間である。
超臨界プロパン相を使用することによって、臨界以下の状態に於いであるいはイ
ソブタンあるいは他の炭化水素を使用することによって可能であるような、より
高い水素濃度を使用することが可能になる。その生成物は低い溶解性を有し、フ
ラッシング技術による炭化水素(プロパン)と水素の分離がより容易である。
超臨界状態においては、該反応器内には事実上ある単一の反応流体があり、そこ
には分れた液相および気相は検知できず、そしてこれは良い熱移送、流体中のガ
ス要素の混在フリー、および反応媒体の低粘度を与えるものである。反応混合物
はループ反応器から、従来の部材によって、連続的あるいは断続的に取り出され
る。不活性炭化水素混合物と同様にもしあればコモノマーと水素は従来の部材、
例えばフラッシング技術でポリマーから取り出される。炭化水素媒体、残ったモ
ノマー、および水素はループ反応器にリサイクルで戻される。
濃縮されたポリマー混合物はそれから気相反応器へと供給される。この反応器は
、他のタイプの気相反応器も使用可能であるが、通常の流動床反応器である。
該流動床反応器内では床は触媒要素と同様に形成され成長するポリマー粒子を含
んでいる。床は、ガス状の要素、粒子が液体の様に作動するに十分な速度でのエ
チレンモノマーの様なものを導入することによって流動の状態に保持されている
。
流動ガスはまた、窒素や水素、もし必要ならば修飾された要素としてのものの様
な、不活性キャリアガスを含むこともできる。
第二フェーズにおいて使用される気相反応器は60〜115℃、好ましくは70
〜110℃の温度範囲で操作される。圧力は、10〜25バールで、エチレン分
圧は1〜20バールである。水素のエチレンに対するモル比は、選択的にループ
反応器内よりも低い。それによって気相反応器内の水素濃度はO〜10加1%の
間である。
もし必要ならば、様々なガス状コモノマーを気相反応器に供給することもできる
。これらのコモノマーは、例えばプロピレン、1−ブテン、ペンテン、1−ヘキ
セン、1−オクテン、あるいは4−メチル−1−ペンテンである。
ミキサーが取り付けられているような気相反応器を使用することも好ましい。
それは反応器表面を清浄に保ち、そして反応器内へのガス配分を改良する手助け
をする。
本発明は2ステージプロセスには限定されない。一つの気相反応器の代りに、2
あるいは3つの気相反応器をループ反応器の後に使用することさえも可能である
。
本発明によるプロセスの形態は、添付の図によってさらに説明さねへその中で、
ループ反応器は参照番号10によって示されている。触媒は、触媒貯蔵器11か
ら触媒供給器12の助けを借りて触媒移送ライン13を通り、ループ反応器10
へと供給される。ライン14からのエチレン、ライン15からの低沸点炭化水素
、ライン16からの水素、およびライン17からのコモノマーはループ反応器1
0にライン18を通って供給される。ループ反応器10内では、反応混合物が特
有の循環部材(図示せず)によって循環されており、同時に重合熱が冷却システ
ム(図示せず)での反応器あるいは反応媒体を冷却することによって取り除かれ
る。
ループ反応器10から、ポリマー−炭化水素混合物がフラッシュ分離器20に供
給され、それを通って一つあるいはそれ以上の放出バルブ19および生成物放出
ライン21に供給される。炭化水素媒体、残ったモノマーおよびコモノマーと、
ポリマー粒子から分離された水素は、ライン23を通ってフラッシュ分離器20
から、ライン24を通って希釈剤回収システム(図示せず)へ取り出されるか、
あるいはライン25を通ってループ反応器10にリサイクルで戻される。ポリマ
ー粒子はライン22を通ってフラッシュ分離器から気相反応器30へと取り出さ
れる。
気相反応器30の低部には、ポリマー粒子の床があり、それはライン32から反
応器10のそこへおよびガス分配プレート31を通ってのガス状モノマー、コモ
ノマー、および水素によって流動状態に保持されている。ガス状の要素は連続的
に反応器30の頂部から取り出さね、そして冷却装置35、コンプレッサー36
とライン37、およびライン32を通って反応器30の底部へ戻り、リサイクル
される。反応器はその表面を清浄な状態に保つために、機械的攪拌器38を備え
付けられている。生成物は断続的にあるいは連続的に気相反応器30からライン
39を通って生成物回収システム(図示せず)に取り出される。
図にはただ一つの気相反応器のみが説明されているが、本発明によるプロセスに
於いて、第一の重合ステップが請求の範囲によるループ反応器内で行われさえす
れば、2あるいは3つの気相反応器でさえ使用できることは明らかである。
本発明はさらに以下の例によって説明される。
実施例1〜8
エチレンの2相重合に於いて、約50kg/hの容量を持つ試験的なスケールの
ループ反応器と、ループ反応器から生成物がやってくることを含む、約75kg
/hの容量を持つ気相反応器が使用された。エチレンに加え、ループ反応器内で
はコモノマーとして1−ブテンが、また気相反応器内では1−ブテンおよび1−
ヘキセンが使用された。水素はモディファイア−として使用された。ループ反応
器に追加された触媒はPCT出1iF190100279の実施例1によって調
整された。プロパンとイソブチンはループ反応器内での反応媒体として使用され
た。
ループ反応器から来る生成物からのガス状要素はフラッシュタンクへと取り出さ
れ、その後に生成物は気相反応器へと移送されへそこで重合が続けられた。ルー
プ反応器での重合は実施例2. 3. 7および8のみで検討された。重合条件
と生成物の特性は以下の表に開示する。
表
本発明によるプロセスで、制御可能な分子量分布D (M、/M、)を有するノ
くイるプロセスに於いては、ループ反応器は狭い分子量分布を有する生成物を製
造する。実施例2および4で測定されたD値3.5−4.0は典型的な値である
。
れは良いパイプ強度を示すものである。ユニモーダルポリエチレンからは匹敵す
る特性を有するバイブを製造することはできない。
観察では、気泡の形成は認められな力じだ。メルトフローインデ・シクスMF
R2は特に問題無<260の高さと同等にまで成り得る(実施例3)。
した。イソブタンが希釈剤として使用された時には、実施例8に示されているよ
うに、メルトフローインデックスMFRIがより低い状態で(0,2) 、93
5kg/+a”の密度を達成することができた。
果ユ約二!
本発明は、マルチステップシーケンスにおけるエチレン重合触媒システムの存在
下で、バイモーダルおよび/または広範な分子量分布を有するポリエチレンを製
造するためのマルチステージプロセスに関連し、ここにおいて、第一反応ステッ
プが液相重合ステップで、第二反応ステップが一つあるいはそれ以上の気相重合
ステップによって形成されている。本発明のプロセスによれば、第一反応ステッ
プにおいて、エチレンはループ反応器(10)内で、不活性低沸点炭化水素媒体
中で、滞留時間少なくとも10分間で重合さべ反応混合物は該ループ反応器(1
0)から放出さ娠そして少なくとも該不活性炭化水素混合物の実質的な一部か分
割さへそして該ポリマーが一つあるいはそれ以上の気相反応器(30)へと移送
され、ここにおいて重合がエチレンおよび任意に水素およびコモノマーの存在下
で完了される。
該ループ反応器(工0)内での不活性炭化水素媒体としてはプロパンか使用でき
、不活性炭化水素、七ツマー1水素および任意のコモノマーの混合物か超臨界状
態下にあるように重合か遂行される。
1際調査報告
国際調査報告
Claims (8)
- 1.マルチステップシーケンスにおけるエチレン重合触媒システムの存在下で、 バイモーダルおよび/または広範な分子量分布を有するポリエチレンを製造する ためのマルチステージプロセスで、ここにおいて、第一反応ステップが液相重合 ステップで、第二反応ステップが一つあるいはそれ以上の気相重合ステップによ って形成されており、それが、第一反応ステップに於いて、エチレンがループ反 応器(10)内で、不活性低沸点炭化水素媒体中で、滞留時間少なくとも10分 間で重合され、反応混合物が該ループ反応器(10)から放出され、そして少な くとも該不活性炭化水素混合物の実質的な一部が分割され、そして該ポリマーが 一つあるいはそれ以上の気相反応器(30)へと移送され、ここにおいて重合が エチレンおよび任意に水素およびコモノマーの存在下で完了されることを特徴と するプロセス。
- 2.該第一ステップに於ける重合が、増加したメルトインデックスを有するポリ マーを生成するよう行われ、そしてその後のステップに於いて、エチレンあるい はエチレンとコモノマーは低メルトフローインデックスおよび低密度を有するエ チレンホモポリマーあるいはコポリマーを生成するよう重合されることを特徴と する請求の範囲1によるプロセス。
- 3.水素のエチレンに対する比が0〜1mol/molの範囲内、好ましくは0 〜0.5mol/molの範囲内であることを特徴とする請求の範囲2によるプ ロセス。
- 4.該不活性炭化水素媒体が、プロパン、ブタン、ペンタン、ヘキサン、ヘプタ ン、およびオクタンを含む群から選ばれることを特徴とする先の請求の範囲のい ずれかによるプロセス。
- 5.該不活性炭化水素媒体が、プロパンであることを特徴とする請求の範囲4に よるプロセス。
- 6.該ループ反応器(10)における重合が、温度75〜110℃、圧力が60 〜90バールで行われることを特徴とする先の請求の範囲のいずれかによるプロ セス。
- 7.該ループ反応器(10)における重合が、超臨界状態下で行われ、それによ って重合温度および圧力が炭化水素媒体、モノマー、水素、および任意のコモノ マーによって形成される混合物の対応する臨界点以上であり、そして重合温度が 形成されるポリマーの融点よりも低いことを特徴とする先の請求の範囲のいずれ かによるプロセス。
- 8.該ループ反応器(10)における重合が、温度85〜110℃、圧力が60 〜90バールで行われることを特徴とする請求の範囲8によるプロセス。
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FI906428 | 1990-12-28 | ||
FI906428A FI86867C (fi) | 1990-12-28 | 1990-12-28 | Flerstegsprocess foer framstaellning av polyeten |
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EP (1) | EP0517868B1 (ja) |
JP (1) | JP2529923B2 (ja) |
AT (1) | ATE130316T1 (ja) |
DE (2) | DE69114696T2 (ja) |
DK (1) | DK0517868T3 (ja) |
ES (1) | ES2079844T3 (ja) |
FI (1) | FI86867C (ja) |
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1990
- 1990-12-28 FI FI906428A patent/FI86867C/fi not_active IP Right Cessation
-
1991
- 1991-12-20 AT AT92900629T patent/ATE130316T1/de not_active IP Right Cessation
- 1991-12-20 DE DE69114696T patent/DE69114696T2/de not_active Expired - Lifetime
- 1991-12-20 DK DK92900629.4T patent/DK0517868T3/da active
- 1991-12-20 JP JP4501688A patent/JP2529923B2/ja not_active Expired - Lifetime
- 1991-12-20 US US07/920,569 patent/US5326835A/en not_active Expired - Lifetime
- 1991-12-20 WO PCT/FI1991/000406 patent/WO1992012182A1/en active IP Right Grant
- 1991-12-20 EP EP92900629A patent/EP0517868B1/en not_active Expired - Lifetime
- 1991-12-20 ES ES92900629T patent/ES2079844T3/es not_active Expired - Lifetime
- 1991-12-20 DE DE199292900629T patent/DE517868T1/de active Pending
-
1992
- 1992-08-26 NO NO923334A patent/NO179286C/no not_active IP Right Cessation
-
1996
- 1996-01-25 GR GR950403657T patent/GR3018786T3/el unknown
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2002519496A (ja) * | 1998-07-06 | 2002-07-02 | ボレアリス テクノロジー オイ | パイプ用ポリマー組成物 |
JP2003509543A (ja) * | 1999-09-10 | 2003-03-11 | フイナ・リサーチ・ソシエテ・アノニム | ポリオレフィンの製造法 |
JP4683805B2 (ja) * | 1999-09-10 | 2011-05-18 | トータル・ペトロケミカルズ・リサーチ・フエリユイ | ポリオレフィンの製造法 |
JP2006504821A (ja) * | 2002-10-30 | 2006-02-09 | ボレアリス テクノロジー オイ | オレフィン重合体を製造する方法および装置 |
Also Published As
Publication number | Publication date |
---|---|
DE517868T1 (de) | 1993-07-22 |
JP2529923B2 (ja) | 1996-09-04 |
DE69114696T2 (de) | 1996-04-11 |
DE69114696D1 (de) | 1995-12-21 |
NO179286B (no) | 1996-06-03 |
NO923334D0 (no) | 1992-08-26 |
FI906428A0 (fi) | 1990-12-28 |
NO179286C (no) | 1996-09-11 |
GR3018786T3 (en) | 1996-04-30 |
FI86867B (fi) | 1992-07-15 |
US5326835A (en) | 1994-07-05 |
EP0517868A1 (en) | 1992-12-16 |
FI906428A (fi) | 1992-06-29 |
WO1992012182A1 (en) | 1992-07-23 |
EP0517868B1 (en) | 1995-11-15 |
NO923334L (no) | 1992-08-26 |
ES2079844T3 (es) | 1996-01-16 |
DK0517868T3 (da) | 1996-03-18 |
FI86867C (fi) | 1992-10-26 |
ATE130316T1 (de) | 1995-12-15 |
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