JPH0333373B2 - - Google Patents
Info
- Publication number
- JPH0333373B2 JPH0333373B2 JP61068771A JP6877186A JPH0333373B2 JP H0333373 B2 JPH0333373 B2 JP H0333373B2 JP 61068771 A JP61068771 A JP 61068771A JP 6877186 A JP6877186 A JP 6877186A JP H0333373 B2 JPH0333373 B2 JP H0333373B2
- Authority
- JP
- Japan
- Prior art keywords
- paddle
- container
- powder
- sets
- paddles
- 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.)
- Expired
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
- B01F27/625—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis the receptacle being divided into compartments, e.g. with porous divisions
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Mixers Of The Rotary Stirring Type (AREA)
Description
〔産業上の利用分野〕
本発明は撹拌装置に関するものである。更に詳
しくは、横型円筒状容器に多数のパドルが回転軸
に取り付けられた撹拌手段が内蔵されていると共
に、この回転軸と垂直に1つの固定堰が容器周壁
に固定されており、この固定堰を挟んで隣接する
パドルの取付けが特殊に構成されていて重合器、
後処理器、乾燥器、等として好適に使用される横
型一軸式の撹拌装置に関するものである。
〔従来の技術〕
横型円筒状容器に横型一軸式の撹拌手段が内蔵
された撹拌装置は以前からポリオレフイン等のポ
リマー粒子の撹拌装置として知られている。これ
らの撹拌装置の一つとして、ポリマー粒子や触媒
粒子等(以下、粉粒体と総称することがある)の
完全な混合、あるいは除熱効率の向上、更には粉
粒体の容器内での滞留時間分布(以下、RTDと
略記することがある)の幅を狭くすることすなわ
ち滞留時間の均一化(以下、RTDの向上と言う
ことがある)等を図るため、矩形状の平らなパド
ルが水平な回転軸上に多数取り付けられた横型一
軸式の撹拌手段に加えて、1以上の固定堰が回転
軸に対して垂直方向に容器内壁に固定された連続
処理のできうる撹拌装置が知られている(特公昭
59−21321参照)。
〔発明が解決しようとする問題点〕
しかしながら、この種の固定堰を単に従来の撹
拌手段に加えて内設して固定堰で区切られた各撹
拌ゾーン(以下、単にゾーンと言うことがある)
を構成しただけの撹拌装置では、混合あるいは除
熱効率の向上があつたとしても、RTDの充分な
向上は得られなかつた。今、固定堰を1つ内設し
て2つのゾーンが構成されている撹拌装置につい
て、その1つのゾーン内で、粉粒体がそのゾーン
内の平均滞留時間だけ撹拌された後に次の隣接ゾ
ーンへピストンフローで全量移送される場合すな
わち各ゾーンでバツチ運転して順次移送される場
合を仮定すると、ゾーン数が多い程撹拌効果は増
大する。このような効果を槽数効果と称し、この
効果に及ぼすゾーン1つ分の槽数効果を1とし、
全体の槽数効果をその和で表現するならば、上記
の如くゾーン2つの場合は全体で槽数効果は2で
ある。しかしながら単に従来の撹拌手段に加えて
固定堰を内設しただけの前記従来の撹拌装置を連
続運転した場合は、各ゾーンにシヨート・パス粒
子や長期滞留粒子が存在して槽数効果はゾーン1
つ分で1以下になり、全体で2に達しない。更に
は、完全な混合を得ようとして回転数を増加させ
た場合は、固定堰を1つ内設したにもかかわら
ず、粉粒体は流動状態となつて固定堰をその両側
から超えるものが多く、槽数効果は全体で1に近
づいて堰を設けた効果が殆んど表われないことも
あつた。
この様に、固定堰を単に従来の撹拌手段に加え
て内設しただけの従来の撹拌装置では、粉粒体の
RTDを向上させることは非常に困難である問題
点があつた。そして例えばオレフイン重合用やポ
リオレフインの乾燥用の撹拌装置内でシヨート・
パス粒子等が存在することは、得られたポリオレ
フインに品質不均一、物性低下、外観不良、等を
招いたので、上記従来技術の問題点の早期解決が
望まれていた。
〔問題点を解決するための手段〕
本発明は、上記の如き従来技術の問題点を解決
し、粉粒体の滞留時間を均一化した状態で行なう
連続撹拌を工業的規模において、長期間安定して
実施することのできる横型一軸式の撹拌装置を提
供することを目的に鋭意研究した結果成されたも
のである。
すなわち本発明は、一端に撹拌対象物の供給口
と他端に粉粒体の抜出し口とを有する横型円筒状
容器内に、水平な回転軸とその上の複数の各位置
にそれぞれ1枚以上の矩形状の平らなパドルが取
り付けられて成るパドル組の複数組とから成る撹
拌手段が内蔵されている横型一軸式の撹拌装置で
あつて、上記回転軸と垂直方向に容器内壁に固定
された1つの固定堰によつて容器内が2つの撹拌
ゾーンに分割されており、該固定堰を挟んで隣接
する2つのパドル組が以下の条件を満足すること
を特徴とする撹拌装置;
(i) 2つのパドル組のパドルの幅W及び枚数は互
に等しい。
(ii) β=0゜、
(iii) D/100≦l1≦D/20、
(iv) l2/l1≧1
(v) 1≦S2/S1≦20
[ここに
β:固定堰を挟んで隣接するパドル組間で各パド
ルが回転軸に対して垂直な投影面上で成す位相
角差、
D:横型円筒状の容器の内径(mm)、
l1:容器内壁と供給口側のパドル組のパドル先端
とのクリアランス(mm)、
l2:容器内壁と抜出し口側のパドル組のパドル先
端とのクリアランス(mm)、
S1:供給口側のパドル組のパドルと固定堰とのク
リアランス(mm)、
S2:抜出し口側のパドル組のパドルと固定堰との
クリアランス(mm)、]
に関するものである。
〔構成の説明〕
本発明に係る撹拌装置を図面によつて詳細に説
明する。
第1図は本発明装置の1実施例を模式的且つ透
視的に示す側面説明図、第2図は第1図中固定堰
を挟んで隣接する2組のパドル組(隣接パドル
組)の各パドルの位置を示すA−A線から矢印方
向に見た説明図、第3図はパドルの位相角差が
90゜のときの隣接パドル組を第2図と同じ位置で
見た説明図、第4図は第3図の状態から隣接パド
ル組を90゜回転させた状態を示す説明図、第5図
はパドル組が粉粒体を撹拌するときの回転に従つ
て変化する粉粒体堆積表面の高低を示す説明図、
第6図及び第7図はそれぞれ粉粒体を撹拌すると
きの固定堰付近における粉粒体堆積表面の高低変
化を第3図及び第4図に対応する2つの両極端の
場合についてパドル組の位置と共に示す側面説明
図、第8図、第9図及び第10図は本発明装置に
おける固定堰とこれを挟んで隣接するパドル組と
の配置状態の種々な態様と粉粒体堆積表面の形成
状態とを示す側面説明図である。
図面中、1は横型円筒状容器(直径D、長さ
L、L/D=3.0)であつて、第1図に示す如く、
一端に撹拌対象物の供給口2と他端に粉粒体の抜
出し口3とを有している。この横型円筒状容器
(以下単に容器と略称することがある)1内の筒
軸位置に水平な回転軸(直径d)4が設けられて
おり、この回転軸4上の複数の各位置に第1図及
び第2図に示す如くそれぞれ1枚以上(図例は揃
つて2枚)の矩形状の平らなパドル(幅W)が取
り付けられて成るパドル組5が回転軸4のほぼ全
長に亘つて複数組設けられていて回転軸4とで撹
拌手段を構成している。そしてこの撹拌手段とこ
れを内蔵する容器1とで横型一軸式の撹拌装置が
構成されている。各パドル組5のパドル数は図例
では揃つて2枚であるが、必ずしもその必要はな
く、例えば1枚、2枚、又は3枚等異なる枚数の
パドルから成るパドル組5が混在していても良
い。但し、後記する如く固定堰を挟んで隣接する
パドル組間ではパドル数は等しいことが必要であ
る。7は固定堰であつて、第1図及び第2図に示
す如く、回転軸4と垂直方向に容器1の長さLを
例えばほぼ同じ長さに分割する位置に上方に容器
内壁との間に半月形(円弧と弦とより成り、必ず
しも半円を意味しない)の開口部8を残して容器
内壁に固定されており、この固定堰7によつて容
器1内が2つの撹拌ゾーン(以下、供給口2側を
第1ゾーンと、又抜出し口3側を第2ゾーンと言
うことがある)に分割されている。
ところで本発明装置においては、この固定堰7
を挟んで隣接する2つのパドル組(以下、それぞ
れを隣接パドル組と称することがある)、すなわ
ち供給口2側(上流側)に位置する隣接パドル組
5aと抜出し口3側(下流側)に位置する隣接パ
ドル組5bとが、前記で示した条件(i)〜(v)を満足
するものであることが本発明の特徴である。
なお、本発明装置に使用される横型円筒状容器
1としてはその直径Dに対する長さLの比L/D
が1.0以上のものが好ましい。又、固定堰7の開
口部8の面積は容器断面積1/4πD2の30%よりも
大きくないことが好ましい。又、開口部8の形状
としては基本的に第2図に示す半月形が好ましい
が、開口部8の周縁の一部として容器周壁の円弧
が含有されていること以外に特別の制限はない。
〔作用〕
以下、本発明装置の作用を本発明装置開発の経
緯と共に説明する。
1つの固定堰7が設けられている横型一軸式の
撹拌装置であつても、隣接パドル組5a,5bに
ついての上記条件を満足していない場合、例え
ば、両隣接パドル組5a,5bのパドル数が異な
る場合、又は同じであつても両隣接パドル組5
a,5bの少なくとも一部のパドルの位相角差β
が0゜でない場合(前者の場合はパドルの位相角差
については当然に後者の場合と同じになる)は、
粉粒体が固定堰7上方の開口部8を通過する軸方
向へのフローパターンは一方方向ではなく、下流
側のパドル組5bによつてかき上げられた粉粒体
が固定堰7を越して逆移動するものもある。固定
堰7上方の開口部8において、粉粒体が第1ゾー
ンから第2ゾーンへの移動のみであれば、槽数効
果がある程度表われるが、上記条件を満足してい
ない場合、第2ゾーンから第1ゾーンへ逆移動も
あり、この逆移動分だけ第1ゾーンから第2ゾー
ンへの粉粒体移動量が増して、シヨート・パス分
が増すこととなり、滞留時間を不均一にする。
又、単位時間当りの逆移動量は回転数の増加とと
もに増加し、はなはだしい場合は、固定堰7を内
設したにもかからず、その効果は殆んど表われな
い。
これらの現象について、種々検討した結果を第
3図〜第7図により詳しく説明する。第3図に示
す固定堰7を挟んだ両隣接パドル組5a,5b
は、それぞれのパドル数は同じ2枚であつて各隣
接パドル組5a,5bそれぞれにおいて隣接パド
ル組5aのパドル6aと6a、及び隣接パドル組
5bのパドル6bと6bとの成す開き角α゜は共に
180゜にとつてある。両隣接パドル組5a,5b間
には各パドル6aと6b1枚づつの組2組につい
て位相角差βが存在するが、上例では位相角差β
は0゜でない場合の例として2組共90゜にとつてあ
る。これらのパドル組5a,5bは第3図の位置
から90゜回転すると第4図の位置になる。一般に、
撹拌装置に粉粒体を適当量(装置の約60容量%の
場合が多い)保有させておいてパドル組5を回転
させてゆくと、粉粒体堆積表面の傾斜は変化し、
その頂部一帯の高さは上下に変化する。その変化
状態は粉粒体の性状、回転数、保有量等によつて
異なるが、パドル組5がほぼ第5図に示す回転位
置近辺で安息角に達し、このとき粉粒体堆積表面
の頂部一帯は最も高いレベル(HLで表わす)に
なる。更にパドル組5が第5図に示す回転位置よ
り開き角αの1/2(図例では90゜)回転した時(パ
ドル組5の回転位置は図示せず)に、粉粒体堆積
表面の頂部一帯は最も低いレベル(LLで表わす)
になる。また、パドル組5が上記2つの回転位置
の中間では粉粒体堆積表面の頂部一帯はHLとLL
との平均的なレベル(ALで表わす)になる。従
つて、粉粒体堆積の頂部一帯のレベルはパドル組
5の回転中にHL→AL→LL→AL→HLのように
変化する。ここで第3図、第4図に示す如く隣接
パドル組間の位相角差βが90゜であつて且つその
他の互に隣接するパドル組間の位相角差も90゜の
場合について上記結果により検討すると、第6図
及び第7図に示す如く、固定堰7の両側で隣接パ
ドル組5a,5bのいずれか一方の域の粉粒体堆
積表面の頂部一帯がレベルHLにある時点で他方
の隣接パドル組5a又は5bの域の粉粒体堆積表
面の頂部一帯のレベルは必ずLLである。
従つて回転軸4を連続回転させて粉粒体を撹拌
する場合、隣接パドル組5a,5bが第3図に示
す位置(隣接パドル組5aは第5図のパドル組5
と同じ位置)に来た時は、第6図に示すように、
隣接パドル組5a域の粉粒体堆積表面の頂部一帯
はレベルHLにあり、隣接パドル組5b域の粉粒
体堆積表面の頂部一帯はレベルLLにある。粉粒
体の軸方向への移動は高いレベルHLから低いレ
ベルLL方向に流動するから、第6図の場合、粉
粒体は自然に固定堰7を越して第1ゾーンから第
2ゾーンに移動する。
更に回転軸4が回転して隣接パドル組5a及び
5bが第4図に示す位置に来た時は、第7図に示
すように、隣接パドル組5a,5b各域の粉粒体
堆積表面の頂部一帯のレベルは第7図に示す如く
HLとLLとは逆転し、粉粒体は固定堰7を越して
第2ゾーンから第1ゾーンに逆移動することにな
る。
このレベルHL,LLの逆転現象は位相角差βと
パドルの開き角αとの関係から上例では時間的等
間隔で起るが、不等間隔で起きる場合についても
粉粒体の移動状態については基本的に同じであ
る。
このように固定堰7を挟んで隣接するパドル組
5a,5b各域の粉粒体堆積表面間で頂部一帯の
レベルの高低が交互に逆転する場合は、必ず粉粒
体の逆移動現象が起こり、一面で長期滞留粒子従
つて反面ではシヨート・パス粒子を多く発生させ
て滞留時間を不均一にさせていたことが判つた。
この逆移動現象を少なくするために更に検討を進
めた結果、回転中の隣接パドル組5a,5bのパ
ドル6aと6b、により掻き上げられる粉粒体堆
積表面の頂部一帯のそれぞれのレベルが同時刻に
おいて同じであつて差を生じさせないパドル6
a,6bの配置が重要なのであるとの認識に達し
た。そしてそのための条件を、隣接パドル組5
a,5bのパドル6aと6bとが同一幅Wを有す
る矩形状であり、第8図に示す如く、容器1の内
壁とのクリアランスl1及びl2(第8図中のl1,l2は、
パドル6a,6bの先端と容器内壁とのクリアラ
ンスをやゝ斜めに見たものであるから、その位置
のみを示すものである。第9図及び第10図にお
いても同じ。)が等しく、且つ固定堰7とのクリ
アランスS1及びS2も等しい場合について検討した
ところ、下記に示す条件が滞留時間均一化の基本
条件であると認められた。
(i) 両隣接パドル組5a,5b間でパドル6a,
6bの数が等しい。
(ii) 両隣接パドル組5a,5b間で各パドル6
a,6bの位相角差βが0゜。
条件(ii)は、換言すれば、両隣接パドル組5a,
5bのパドル6a,6bの各1枚から成る1組2
枚の各パドル6a,6bは回転軸4の方向に見れ
ば第2図の如く一致することを意味するが、必ず
し各開き角αが等しいことを要しない。この場
合、両隣接パドル組5a,5b各域の粉粒体堆積
表面の頂部一帯のレベルがHLからLLまでのどの
状態にあつても、例えばHLの場合について第8
図に示す如く、供給口2からの粉粒体の供給がな
い限り、固定堰7上方の開口部8における粉粒体
堆積表面の傾斜は固定堰7の両側に同じであつて
粉圧はバランスしており、両側傾斜面の交差する
谷部P′は固定堰7の真上に形成されて固定堰7の
上方延長面P上にあり、この固定堰7を越す粉粒
体の移動は起らない。このような固定堰7及び隣
接パドル組5a,5bの配置においては、供給口
2からの粉粒体の供給がある場合、第1ゾーンで
の増加分だけがわずかなレベル差となり、粉粒体
は第1ゾーンから第2ゾーンへの移動のみのフロ
ーパターンを示すのである。
次に両隣接パドル組5a,5b間でパドル6
a,6bの枚数が等しく且つ位相角差βが0゜であ
つても、固定堰7の開口部8の面積が大きい場
合、回転数が高い場合、及び粉粒体の保有量が多
い場合などには粉粒体の軸方向への飛散程度が増
加し、飛散によるシヨート・パス及び逆移動の防
止は必ずしも充分でない。この様な飛散あるいは
逆移動の防止について種々検討した結果、種々な
場合を総合して、両隣接パドル組5a,5bのパ
ドル6a,6bの幅Wが同じで(以下の説明にお
いてこの条件は変わらないものとし、逐一示すこ
とは省略する)、l2/l1≧1で且つS2/S1≧1の場
合に防止効果が充分にあることが認められた。
l2/l1=1、S2/S1=1の場合は先に第8図で見
た通りである。l2/l1>1、S2/S1=1の場合は
第9図に、又l2/l1=1、S2/S1>1の場合は第
10図にそれぞれ粉粒体堆積表面の頂部一帯の形
成状態を示す。第9図及び第10図においてはい
ずれの場合も両隣接パドル組5a,5bそれぞれ
の域の粉粒体堆積表面が接して形成する谷部P′が
固定堰7の上方延長面Pより第2ゾーン側に在
り、谷部P′と面Pとの軸方向の距離Hsの存在が
認められる。この距離Hsが第2ゾーン側に存在
することは面Pにおける粉圧が第1ゾーンから第
2ゾーンに向くことを意味し、そしてHsが大き
いほど粉粒体の逆移動は生じ難いことになる。
次にl1が容器1の内径Dに対して実際的にどの
範囲に定めるのが良いかを数多くの実験により経
験的に求めたところ、l1の適切な範囲は、
(iii) D/100≦l1≦D/20、
であることが判つた。
又、S2/S1は大きければ大きいほど逆移動防止
には有効であるが、反面大き過ぎるとそのクリア
ランスS2における粉粒体の撹拌状態が悪化し、は
なはだしい場合はデツド・スペースとなる。この
点についても経験的に
(v) 1≦S2/S1≦20
が適切な範囲として得られた。
以上の如くにして本発明に係る撹拌装置が構成
されたのである。
次にl2/l1及びS2/S1について更に数多くの実
験により検討を進めた結果、
(iv) 1≦l2/l1≦3
(v) 1≦S2/S1≦12
の場合は比較的粒度分布の狭い粉粒体の撹拌に、
また、
(iv) l2/l1=1
(v) 1≦S2/S1≦3
の場合は上記の粉粒体の他に球形に近い形状の粉
粒体の撹拌にも、それぞれ特に好適であることが
認められた。
〔使用方法〕
本発明装置の用途は特に限定されないが、炭素
数2〜6のα−オレフインを遷移金属化合物を含
む触媒と共に気相重合させるときの気相重合装
置、気相重合後の後処理装置としての気相反応装
置、ポリマーの乾燥装置、等として好ましく使用
される。
このようにして本発明装置を使用して例えばオ
レフインの気相重合等を実施する場合、下記に示
すフルード数(Fr)が0.05〜3.0の範囲、好まし
くは0.2〜2.0の範囲となるように回転させるのが
良い。
Fr=Rω2/g
ここに
R:回転軸センターからパドル先端までの長さ、
ω:角速度(=2πN、Nは回転数rps)
g:重力加速度
また、容器内保有量は10〜80容量%で、連続処
理するのが好ましい。この場合、第1ゾーン及び
第2ゾーン各々の保有量を等しくするか、あるい
は第2ゾーンの保有量が第1ゾーンのそれより若
干少ないことが逆移動防止を一層確実にするのに
好ましい。
撹拌対象がポリマーであるとき、その種類を例
示すると、エチレンポリマー、プロピレンポリマ
ー、ブテンポリマー、エチレン−プロピレンコポ
リマー、エチレン−ブテン−1コポリマー、プロ
ピレン−ブテン1コポリマー、プロピレン−ブテ
ン1−エチレンコポリマー、等があげられる。
〔効果〕
本発明に係る撹拌装置を使用すれば、ポリマー
粒子等のシヨート・パス量は極端に減少させて粉
粒体の滞留時間を均一化することができ、連続重
合あるいは連続処理にも拘わらず、粉粒体の
RTDはバツチ重合あるいはバツチ処理のRTDに
近似させることができ、従つて撹拌対象の品質、
物性等を向上させることができる。
〔実施例、比較例〕
以下、実施例、比較例により、本発明を具体的
に説明する。
実施例1、比較例1〜3
内径Dが430mm、長さLが1320(L/D=3)の
横型円筒状容器内に、径dが110mmの回転軸に幅
wが50mmのパドルが取り付けられた種々な態様の
本発明装置と、固定堰の有無又はパドルの取付け
態様において本発明の範囲外の横型一軸式撹拌装
置とを使用し、メジアン径が600μ、かさ密度が
0.5g/cm3の比較的粒度分布が狭いポリプロピレ
ンの不活性粉体を15Kg/hrで連続供給しながら回
転数60rpm(Fr=0.826)で連続撹拌し、定常運転
時の粉粒体保有量を装置容量の60容量%に保つ
た。この場合、装置の実容積は179であるから、
平均滞留時間φは3.58時間(215分)である。
この定常運転中にトレーサーとして同じポリプ
ロピレンの着色粉体270g(保有量の0.5重量%相
当量)を粉粒体の供給口にインパルス的に投入
し、粉粒体の抜出し口において抜出しポリマー中
のトレーサーの濃度を経時的に測定してその変化
(以下、インパルス応答と称することがある。)を
調べた。
このインパルス応答により各実施例、比較例に
おける粉粒体の滞留時間の均一性について検討し
た。
実施例 1
容器の長さLを2等分する位置に面積140cm2の
半月形開口部を上方に残して固定堰が1枚内設さ
れており、すべてのパドル組はパドル数が2枚で
その開き角αが180゜であり、固定堰の両側の各ゾ
ーンにおいて互い隣接するパドル組間のパドルの
位相角差が90゜で、容器内壁と各パドル先端との
クリヤランスlがすべて5.0mmであり、固定堰を
挟んで隣接する両隣接パドル組において、
l1=l2=5.0mm
〔従つて、l2/l1=1、D/100(=4.3)<l1<
D/20(=21.5)〕
S1=S2=8.0mm〔従つてS2/S1=1〕
β=0゜
である本発明装置の場合。
比較例 1
固定堰を有せず、すべての互に隣接するパドル
組間において位相角差が90゜である以外は実施例
1と同様の撹拌装置の場合。
比較例 2
両隣接パドル組間においてもβ=90゜である以
外は実施例1と同様の撹拌装置の場合。
比較例 3
下流側の隣接パドル組のパドル数が3枚で各開
き角αが120゜であり、上流側の隣接パドル組との
間で1枚のパドルについてβ=0゜であるが他のパ
ドルについてはβ=0゜となるパドルがない(従つ
て回転軸方向に見て一致するパドルが1組しかな
く、また、下流側の撹拌ゾーンにおいて隣接パド
ル組とその下流側に隣接するパドル組との間でパ
ドルの位相角差が必ずしも90゜となつていない)
以外は実施例1と同様の撹拌装置の場合。
インパルス応答はサンプリング時間関数t/φ
に対するトレーサー濃度関数e/e0の変化で示
す。ここで、tはトレーサー投入から粉粒体抜出
し口でサンプリングするまでの経過時間(サンプ
リング時間)すなわちトレーサーの容器内実滞留
時間、φは平均滞留時間、eは粉粒体抜出し口に
おけるt時のトレーサー濃度(重量%)、e0は投
入トレーサー量の容器内ポリマー保有量に対する
トレーサー濃度である。
[Industrial Field of Application] The present invention relates to a stirring device. More specifically, a horizontal cylindrical container has a built-in stirring means in which many paddles are attached to a rotating shaft, and a fixed weir is fixed to the peripheral wall of the container perpendicularly to this rotating shaft. The installation of the adjacent paddles across the polymerization vessel is specially configured.
The present invention relates to a horizontal uniaxial stirring device suitable for use as a post-processor, dryer, etc. [Prior Art] A stirring device in which a horizontal uniaxial stirring means is built into a horizontal cylindrical container has long been known as a stirring device for polymer particles such as polyolefin. As one of these stirring devices, it is used to completely mix polymer particles, catalyst particles, etc. (hereinafter sometimes referred to as powder and granules), improve heat removal efficiency, and further improve the retention of powder and granules in a container. In order to narrow the width of the time distribution (hereinafter sometimes abbreviated as RTD), that is, to make the residence time uniform (hereinafter sometimes referred to as improving RTD), the rectangular flat paddle is placed horizontally. In addition to horizontal uniaxial stirring means installed in large numbers on a rotating shaft, there is also known a stirring device capable of continuous processing in which one or more fixed weirs are fixed to the inner wall of a container in a direction perpendicular to the rotating shaft. There is (Tokuko Akira)
59-21321). [Problems to be Solved by the Invention] However, this type of fixed weir is simply added to the conventional stirring means and is internally installed in each stirring zone (hereinafter sometimes simply referred to as zone) separated by the fixed weir.
Even if mixing or heat removal efficiency could be improved with a stirring device consisting of only 1, a sufficient improvement in RTD could not be obtained. Now, regarding an agitation device that has one fixed weir inside and is configured with two zones, in one zone, after the powder is agitated for the average residence time in that zone, it is transferred to the next adjacent zone. Assuming that the entire amount is transferred by piston flow, that is, that each zone is batch-operated and transferred sequentially, the greater the number of zones, the greater the stirring effect. This effect is called the tank number effect, and the tank number effect for one zone on this effect is 1,
If the overall tank number effect is expressed as the sum, in the case of two zones as described above, the total tank number effect is 2. However, when the above-mentioned conventional stirring device, which is simply equipped with a fixed weir in addition to the conventional stirring means, is operated continuously, short pass particles and long-term residence particles exist in each zone, and the effect of the number of tanks is limited to zone 1.
The number is less than 1 in parts, and the number does not reach 2 in total. Furthermore, when the rotational speed is increased in an attempt to achieve complete mixing, the powder and granules become fluid and the amount of material that exceeds the fixed weir from both sides becomes fluid even though one fixed weir is installed. In many cases, the overall effect of the number of tanks approached 1, meaning that the effect of installing a weir was hardly noticeable. In this way, with conventional stirring devices that simply incorporate a fixed weir in addition to conventional stirring means, powder and granule material
There was a problem that it was very difficult to improve RTD. For example, in stirring equipment for olefin polymerization or polyolefin drying,
The presence of pass particles and the like causes nonuniform quality, deterioration of physical properties, poor appearance, etc. in the obtained polyolefin, and therefore, an early solution to the problems of the above-mentioned prior art has been desired. [Means for Solving the Problems] The present invention solves the problems of the prior art as described above, and makes it possible to perform continuous stirring with uniform residence time of powder and granules on an industrial scale for a long period of time. This was achieved as a result of intensive research with the aim of providing a horizontal, single-shaft stirring device that can be used as a stirrer. That is, the present invention provides a horizontal cylindrical container having a supply port for the material to be stirred at one end and an outlet for the powder or granular material at the other end, and one or more sheets at each of a plurality of positions on the horizontal rotation shaft. A horizontal uniaxial stirring device having a built-in stirring means consisting of a plurality of paddle sets each having rectangular flat paddles attached thereto, the stirring device being fixed to the inner wall of the container in a direction perpendicular to the rotation axis. (i) A stirring device characterized in that the interior of the container is divided into two stirring zones by one fixed weir, and two paddle sets adjacent to each other across the fixed weir satisfy the following conditions; (i) The width W and number of paddles of the two paddle sets are equal to each other. (ii) β=0゜, (iii) D/100≦l 1 ≦D/20, (iv) l 2 /l 1 ≧1 (v) 1≦S 2 /S 1 ≦20 [here β: fixed Phase angle difference between adjacent paddle sets across the weir on the projection plane perpendicular to the axis of rotation of each paddle, D: Inner diameter of horizontal cylindrical container (mm), l 1 : Inner wall of container and supply port Clearance between the paddle tip of the paddle group on the side (mm), l 2 : Clearance between the inner wall of the container and the tip of the paddle of the paddle group on the outlet side (mm), S 1 : Paddle of the paddle group on the supply port side and the fixed weir (mm), S 2 : Clearance (mm) between the paddle of the paddle assembly on the outlet side and the fixed weir (mm). [Description of Configuration] The stirring device according to the present invention will be explained in detail with reference to the drawings. FIG. 1 is a side explanatory view schematically and transparently showing one embodiment of the device of the present invention, and FIG. 2 is a diagram showing each of two adjacent paddle groups (adjacent paddle groups) in FIG. 1 with a fixed weir in between. An explanatory diagram viewed in the direction of the arrow from line A-A indicating the position of the paddle, Figure 3 shows the phase angle difference of the paddle.
An explanatory diagram showing the adjacent paddle set at 90 degrees at the same position as in Figure 2, Figure 4 is an explanatory diagram showing the adjacent paddle set rotated 90 degrees from the state in Figure 3, and Figure 5 is An explanatory diagram showing the height of the powder/granular material accumulation surface that changes as the paddle set rotates when stirring the powder/granular material;
Figures 6 and 7 show the position of the paddle set for the two extreme cases corresponding to Figures 3 and 4, respectively, showing changes in height of the powder and granule accumulation surface near the fixed weir when stirring the powder and granules. The side explanatory views, FIGS. 8, 9, and 10 shown together with the figures show various aspects of the arrangement of the fixed weir and the adjacent paddle set on both sides of the fixed weir in the device of the present invention, and the formation of the powder deposition surface. FIG. In the drawings, 1 is a horizontal cylindrical container (diameter D, length L, L/D=3.0), as shown in FIG.
It has a supply port 2 for the material to be stirred at one end and a discharge port 3 for the powder and granular material at the other end. A horizontal rotating shaft (diameter d) 4 is provided at the cylindrical axis position in this horizontal cylindrical container (hereinafter sometimes simply referred to as a container) 1, and a horizontal rotating shaft (diameter d) 4 is provided at each of a plurality of positions on this rotating shaft 4. As shown in FIGS. 1 and 2, a paddle set 5 consisting of one or more rectangular flat paddles (width W) each extending over almost the entire length of the rotating shaft 4 (two paddles in the example shown) is attached. A plurality of sets are provided, and the rotating shaft 4 constitutes a stirring means. This stirring means and the container 1 containing it constitute a horizontal uniaxial stirring device. Although the number of paddles in each paddle set 5 is two in the illustrated example, this is not necessarily necessary; for example, paddle sets 5 consisting of different numbers of paddles, such as one, two, or three, may be mixed. Also good. However, as will be described later, it is necessary that the number of paddles be equal between adjacent paddle sets across the fixed weir. Reference numeral 7 denotes a fixed weir, as shown in FIGS. 1 and 2, which is located above and between the inner wall of the container at a position that divides the length L of the container 1 into approximately the same length in the direction perpendicular to the rotating shaft 4. is fixed to the inner wall of the container leaving a half-moon-shaped opening 8 (consisting of an arc and a chord, not necessarily a semicircle), and this fixed weir 7 creates two stirring zones (hereinafter referred to as , the supply port 2 side is sometimes referred to as a first zone, and the extraction port 3 side is sometimes referred to as a second zone). By the way, in the device of the present invention, this fixed weir 7
Two adjacent paddle sets (hereinafter, each may be referred to as adjacent paddle sets), that is, the adjacent paddle set 5a located on the supply port 2 side (upstream side) and the adjacent paddle set 5a located on the extraction port 3 side (downstream side). A feature of the present invention is that the adjacent paddle set 5b located therein satisfies the conditions (i) to (v) shown above. The horizontal cylindrical container 1 used in the device of the present invention has a ratio L/D of length L to diameter D.
is preferably 1.0 or more. Further, it is preferable that the area of the opening 8 of the fixed weir 7 is not larger than 30% of the cross-sectional area of the container 1/4πD 2 . The shape of the opening 8 is basically preferably a half-moon shape as shown in FIG. 2, but there is no particular restriction other than that the arc of the container peripheral wall is included as part of the periphery of the opening 8. [Function] Hereinafter, the function of the device of the present invention will be explained together with the history of development of the device of the present invention. Even if it is a horizontal uniaxial stirring device provided with one fixed weir 7, if the above conditions for adjacent paddle sets 5a, 5b are not satisfied, for example, the number of paddles of both adjacent paddle sets 5a, 5b is are different, or even if they are the same, both adjacent paddle sets 5
Phase angle difference β between at least some of the paddles a and 5b
is not 0° (in the former case, the paddle phase angle difference is naturally the same as in the latter case), then
The flow pattern in the axial direction in which the powder and granules pass through the opening 8 above the fixed weir 7 is not unidirectional, but the powder and granules scraped up by the paddle set 5b on the downstream side pass over the fixed weir 7. Some move backwards. At the opening 8 above the fixed weir 7, if the granular material only moves from the first zone to the second zone, the effect of the number of tanks will appear to some extent, but if the above conditions are not satisfied, the second zone There is also a reverse movement from the first zone to the first zone, and the amount of granular material movement from the first zone to the second zone increases by this reverse movement, resulting in an increase in the short pass, making the residence time non-uniform.
Further, the amount of reverse movement per unit time increases as the number of rotations increases, and in extreme cases, even if the fixed weir 7 is installed internally, its effect will hardly be seen. The results of various studies regarding these phenomena will be explained in detail with reference to FIGS. 3 to 7. Both adjacent paddle sets 5a and 5b sandwiching the fixed weir 7 shown in FIG.
The number of paddles is the same, two, and the opening angle α° between the paddles 6a and 6a of the adjacent paddle set 5a and the paddles 6b and 6b of the adjacent paddle set 5b in each of the adjacent paddle sets 5a and 5b is both
It is set at 180°. There is a phase angle difference β between both adjacent paddle sets 5a and 5b for two sets each consisting of one paddle 6a and one paddle 6b, but in the above example, the phase angle difference β
As an example where is not 0°, both sets are set at 90°. When these paddle sets 5a and 5b are rotated 90 degrees from the position shown in FIG. 3, they will be in the position shown in FIG. 4. in general,
When the stirring device holds an appropriate amount of powder (often about 60% by volume of the device) and the paddle set 5 is rotated, the slope of the surface on which the powder is deposited changes.
The height of its top area varies up and down. Although the state of change differs depending on the properties of the powder, the number of revolutions, the amount held, etc., the paddle set 5 reaches the angle of repose approximately near the rotational position shown in FIG. The area will be at the highest level (denoted by HL). Furthermore, when the paddle set 5 is rotated by 1/2 of the opening angle α (90° in the example shown) from the rotation position shown in FIG. 5 (the rotation position of the paddle set 5 is not shown), the surface of the powder deposited The area around the top is the lowest level (represented by LL)
become. In addition, when the paddle set 5 is in the middle of the above two rotational positions, the entire top area of the powder accumulation surface is HL and LL.
and the average level (expressed as AL). Therefore, the level over the top of the granular material accumulation changes as HL→AL→LL→AL→HL during the rotation of the paddle set 5. Here, as shown in Figs. 3 and 4, when the phase angle difference β between adjacent paddle sets is 90°, and the phase angle difference between other mutually adjacent paddle sets is also 90°, based on the above results, When examined, as shown in FIGS. 6 and 7, when the entire top area of the powder accumulation surface of either one of the adjacent paddle sets 5a, 5b on both sides of the fixed weir 7 is at the level HL, the other The level of the entire top area of the powder/grain material deposition surface in the area of the adjacent paddle set 5a or 5b is always LL. Therefore, when stirring the powder by continuously rotating the rotating shaft 4, the adjacent paddle sets 5a and 5b are placed in the position shown in FIG. 3 (the adjacent paddle set 5a is in the position shown in FIG.
), as shown in Figure 6,
The entire top area of the powder/granular material accumulation surface in the adjacent paddle group 5a area is at level HL, and the entire top area of the powder/granular material accumulation surface in the adjacent paddle group 5b area is at level LL. Since the granular material moves in the axial direction from the high level HL to the low level LL direction, in the case of Fig. 6, the granular material naturally moves over the fixed weir 7 from the first zone to the second zone. do. When the rotating shaft 4 further rotates and the adjacent paddle sets 5a and 5b come to the position shown in FIG. 4, as shown in FIG. The level of the entire top area is shown in Figure 7.
HL and LL are reversed, and the granular material crosses the fixed weir 7 and moves backward from the second zone to the first zone. This reversal phenomenon of levels HL and LL occurs at equal intervals in time in the above example due to the relationship between the phase angle difference β and the paddle opening angle α, but even when it occurs at unequal intervals, the state of movement of the powder and granules may be affected. are basically the same. In this way, when the height of the level of the entire top area is alternately reversed between the powder and granule accumulation surfaces of the adjacent paddle sets 5a and 5b with the fixed weir 7 in between, a reverse movement phenomenon of the powder and granules always occurs. It was found that on the one hand, long-term residence particles were generated, and on the other hand, many short-pass particles were generated, making the residence time uneven.
As a result of further studies in order to reduce this reverse movement phenomenon, it was found that the respective levels of the top area of the powder and granular material accumulation surface scraped up by the rotating paddles 6a and 6b of the adjacent paddle sets 5a and 5b at the same time. Paddle 6 that is the same and does not cause a difference in
We have come to the realization that the arrangement of a and 6b is important. Then, the conditions for that are 5 adjacent paddle groups.
Paddles 6a and 6b of a and 5b have a rectangular shape with the same width W, and as shown in FIG. 8, clearances l 1 and l 2 (l 1 and l 2 in FIG. teeth,
Since this is a slightly oblique view of the clearance between the tips of the paddles 6a, 6b and the inner wall of the container, only their positions are shown. The same applies to FIGS. 9 and 10. ) are equal and the clearances S 1 and S 2 with the fixed weir 7 are also equal, and the following conditions were recognized as the basic conditions for equalizing residence time. (i) Paddle 6a between both adjacent paddle sets 5a and 5b,
The numbers of 6b are equal. (ii) Each paddle 6 between both adjacent paddle sets 5a and 5b.
The phase angle difference β between a and 6b is 0°. In other words, condition (ii) means that both adjacent paddle sets 5a,
1 set 2 consisting of one each of paddles 6a and 6b of 5b
This means that the paddles 6a, 6b coincide as shown in FIG. 2 when viewed in the direction of the rotating shaft 4, but it is not necessarily necessary that the opening angles α are equal. In this case, even if the level of the top area of the powder/grain material accumulation surface in each region of both adjacent paddle sets 5a and 5b is in any state from HL to LL, for example, in the case of HL, the
As shown in the figure, unless powder is supplied from the supply port 2, the slope of the powder accumulation surface at the opening 8 above the fixed weir 7 is the same on both sides of the fixed weir 7, and the powder pressure is balanced. The trough P' where the slopes on both sides intersect is formed directly above the fixed weir 7 and is on the upward extension surface P of the fixed weir 7, and the movement of powder and granules over the fixed weir 7 does not occur. No. In such an arrangement of the fixed weir 7 and the adjacent paddle sets 5a and 5b, when powder and granular material is supplied from the supply port 2, only the increase in the first zone results in a slight level difference, and the powder and granular material indicates a flow pattern of movement only from the first zone to the second zone. Next, the paddle 6 is moved between both adjacent paddle sets 5a and 5b.
Even if the number of sheets a and 6b are equal and the phase angle difference β is 0°, when the area of the opening 8 of the fixed weir 7 is large, when the rotation speed is high, when there is a large amount of powder and granular material, etc. In this case, the degree of scattering of powder particles in the axial direction increases, and prevention of short passes and reverse movement due to scattering is not always sufficient. As a result of various studies on preventing such scattering or reverse movement, we found that the width W of the paddles 6a and 6b of both adjacent paddle sets 5a and 5b is the same (this condition will not be changed in the following explanation). It was recognized that there is a sufficient preventive effect when l 2 /l 1 ≧1 and S 2 /S 1 ≧1.
The case of l 2 /l 1 =1 and S 2 /S 1 =1 is as seen earlier in FIG. When l 2 /l 1 > 1 and S 2 /S 1 = 1, the powder and granular material is shown in Figure 9, and when l 2 /l 1 = 1, S 2 /S 1 > 1, it is shown in Figure 10. The formation state of the entire top area of the deposition surface is shown. 9 and 10, in both cases, the trough P' formed by the contact between the powder and granular material accumulation surfaces in the areas of both adjacent paddle sets 5a and 5b is 2nd It is located on the zone side, and the existence of an axial distance Hs between the valley P' and the plane P is recognized. The existence of this distance Hs on the second zone side means that the powder pressure on the plane P is directed from the first zone to the second zone, and the larger Hs is, the harder it is for the powder to move backwards. . Next, we empirically determined in many experiments what range l 1 should practically be set in relation to the inner diameter D of container 1, and found that the appropriate range for l 1 is (iii) D/100 It was found that ≦l 1 ≦D/20. Further, the larger S 2 /S 1 is, the more effective it is in preventing reverse movement, but on the other hand, if it is too large, the state of stirring of the powder and granular material in the clearance S 2 will deteriorate, and if it is too large, it will become a dead space. Regarding this point as well, it was empirically determined that (v) 1≦S 2 /S 1 ≦20 is an appropriate range. The stirring device according to the present invention was constructed as described above. Next, we further investigated l 2 /l 1 and S 2 /S 1 through many experiments, and found that (iv) 1≦l 2 /l 1 ≦3 (v) 1≦S 2 /S 1 ≦12. When stirring powder and granular materials with a relatively narrow particle size distribution,
In addition, in the case of (iv) l 2 /l 1 =1 (v) 1≦S 2 /S 1 ≦3, in addition to the above-mentioned powder and granules, it is also particularly important to agitate powder and granules with a shape close to spherical. It was found to be suitable. [Method of Use] Applications of the device of the present invention are not particularly limited, but include a gas phase polymerization device for gas phase polymerization of α-olefin having 2 to 6 carbon atoms together with a catalyst containing a transition metal compound, and post-treatment after gas phase polymerization. It is preferably used as a gas phase reaction device, a polymer drying device, etc. When carrying out gas phase polymerization of olefins using the apparatus of the present invention in this manner, the rotation is performed so that the Froude number (Fr) shown below is in the range of 0.05 to 3.0, preferably in the range of 0.2 to 2.0. It is better to let Fr=Rω 2 /g where R: length from the center of the rotation axis to the tip of the paddle, ω: angular velocity (=2πN, N is the rotation speed rps) g: gravitational acceleration Also, the amount held in the container is 10 to 80% by volume It is preferable to carry out continuous treatment. In this case, it is preferable that the amount held in the first zone and the second zone be equal, or that the amount held in the second zone be slightly smaller than that in the first zone to further ensure prevention of reverse migration. When the object to be stirred is a polymer, examples of the types include ethylene polymer, propylene polymer, butene polymer, ethylene-propylene copolymer, ethylene-butene-1 copolymer, propylene-butene-1 copolymer, propylene-butene-1-ethylene copolymer, etc. can be given. [Effect] By using the stirring device according to the present invention, the amount of shots and passes of polymer particles, etc. can be extremely reduced and the residence time of powder and granules can be made uniform. of powder and granules
RTD can be approximated to batch polymerization or batch processing RTD, and therefore the quality of the stirred object,
Physical properties etc. can be improved. [Examples and Comparative Examples] The present invention will be specifically described below using Examples and Comparative Examples. Example 1, Comparative Examples 1 to 3 A paddle with a width w of 50 mm is attached to a rotating shaft with a diameter d of 110 mm in a horizontal cylindrical container with an inner diameter D of 430 mm and a length L of 1320 mm (L/D = 3). Using the present invention apparatus of the various embodiments described above and a horizontal uniaxial stirring apparatus which is outside the scope of the present invention in terms of the presence or absence of a fixed weir or the manner in which paddles are attached,
Inert polypropylene powder with a relatively narrow particle size distribution of 0.5 g/cm 3 was continuously fed at 15 kg/hr and continuously stirred at a rotation speed of 60 rpm (Fr = 0.826) to calculate the amount of powder retained during steady operation. The device capacity was kept at 60% by volume. In this case, the actual volume of the device is 179, so
The average residence time φ is 3.58 hours (215 minutes). During this steady operation, 270 g of the same colored polypropylene powder (equivalent to 0.5% by weight of the amount held) as a tracer was injected into the supply port of the powder and granules, and the tracer in the polymer was extracted at the outlet of the powder and granules. The concentration of was measured over time and its change (hereinafter sometimes referred to as impulse response) was investigated. Based on this impulse response, the uniformity of the residence time of the powder and granular material in each Example and Comparative Example was investigated. Example 1 A fixed weir is installed inside the container at a position that divides the length L of the container into two, leaving a half-moon-shaped opening with an area of 140 cm 2 above, and all paddle sets have two paddles. The opening angle α is 180°, the phase angle difference of the paddles between adjacent paddle sets in each zone on both sides of the fixed weir is 90°, and the clearance l between the inner wall of the container and the tip of each paddle is all 5.0 mm. Yes, in both adjacent paddle sets that are adjacent across the fixed weir, l 1 = l 2 = 5.0 mm [Therefore, l 2 /l 1 = 1, D/100 (= 4.3) < l 1 <
D/20 (=21.5)] S 1 =S 2 =8.0 mm [Hence, S 2 /S 1 =1] In the case of the device of the present invention where β=0°. Comparative Example 1 A stirring device similar to Example 1 except that it does not have a fixed weir and the phase angle difference between all adjacent paddle sets is 90°. Comparative Example 2 A stirring device similar to Example 1 except that β = 90° between both adjacent paddle sets. Comparative Example 3 The number of paddles in the adjacent paddle set on the downstream side is 3 and each opening angle α is 120°, and β = 0° for one paddle with the adjacent paddle set on the upstream side, but the other Regarding the paddles, there is no paddle for which β = 0° (therefore, there is only one set of paddles that match when viewed in the direction of the rotation axis, and in the downstream stirring zone, the adjacent paddle set and the adjacent paddle set on the downstream side) (The phase angle difference of the paddles is not necessarily 90° between the two.)
Other than that, the same stirring device as in Example 1 was used. Impulse response is sampling time function t/φ
It is shown as the change in the tracer concentration function e/e 0 with respect to Here, t is the elapsed time (sampling time) from the injection of the tracer until sampling at the powder outlet, that is, the actual residence time of the tracer in the container, φ is the average residence time, and e is the tracer at time t at the powder outlet. Concentration (% by weight), e 0 is the tracer concentration relative to the amount of tracer input relative to the amount of polymer held in the container.
【表】
一般に、t/φが約0.2以下においてe/e0が
大きいほどシヨート・パス分が多く、e/e0のピ
ーク値がt/φの比較的大きい領域にあるほど、
相対的にシヨート・パス分は少なくなる傾向であ
る。
第1表より、固定堰を有しない比較例1は勿論
であるが、単に固定堰が内設されているだけの比
較例2に比べても、隣接パドル組間でのパドルの
位相角差βがすべて0゜の実施例1ではシヨート・
パス分は圧倒的に少なく、粉粒体の滞留時間が均
一化していることが判る。又、比較例3から、両
隣接パドル組間でのパドルの一部がβ=0゜である
だけでは効果のないことが判る。
実施例 2〜4
実施例 2
下流側の隣接パドル組においてl2=15.0mm(従
つてl2/l1=3)である以外は実施例1と同様の
本発明装置の場合。
実施例 3
下流側の隣接パドル組においてS2=24.0mm(従
つてS2/S1=3)である以外は実施例1と同様の
本発明装置の場合。
実施例 4
下流側の隣接パドル組においてl2=15.0mm、S2
=24.0mm(従つてl2/l1>1且つS2/S1>1)で
ある以外は、実施例1と同様の本発明装置の場
合。
インパルス応答を第2表に示す。[Table] Generally, when t/φ is about 0.2 or less, the larger e/e 0 is, the more short passes there are, and the more the peak value of e/e 0 is in the relatively large region of t/φ, the more
The number of short passes tends to decrease relatively. From Table 1, it can be seen that not only Comparative Example 1 which does not have a fixed weir, but also Comparative Example 2 which simply has a fixed weir installed, the paddle phase angle difference β between adjacent paddle sets is In Example 1 where all are 0°, short
It can be seen that the number of passes is overwhelmingly small, and the residence time of the powder and granules is uniform. Furthermore, from Comparative Example 3, it is clear that there is no effect if only a portion of the paddles between both adjacent paddle sets have β=0°. Examples 2 to 4 Example 2 The device of the present invention is the same as in Example 1 except that l 2 =15.0 mm (therefore, l 2 /l 1 =3) in the downstream adjacent paddle set. Example 3 The device of the present invention is the same as Example 1 except that S 2 =24.0 mm (therefore, S 2 /S 1 =3) in the adjacent paddle set on the downstream side. Example 4 l 2 = 15.0 mm, S 2 in the adjacent paddle group on the downstream side
= 24.0 mm (therefore, l 2 /l 1 >1 and S 2 /S 1 >1), except that the device of the present invention is the same as in Example 1. The impulse response is shown in Table 2.
【表】
第2表及び第1表実施例1の欄よりl2/l1(実施
例)あるいはS2>S1(実施例3)であれば粉粒体
の滞留時間の均一化には一層効果があり、又、l2
>l1且つS2>S1(実施例4)であれば更に相乗効
果のあることが判る。
実施例5〜7、比較例4
実施例 5
各隣接パドル組のパドル数が3枚で開き角αが
すべて120゜以外は、実施例1と同様(従つて上記
以外のパドル組のパドル数が2枚で開き角αが
180゜)の本発明装置の場合。
実施例 6
両隣接パドル組以外のパドル組のパドル数も3
枚で開き角αが120゜であつて、互に隣接するパド
ル組間(両隣接パドル組間を除く)でパドルの位
相角差が60゜である以外は、実施例5と同様の本
発明装置の場合。
実施例 7
各隣接パドル組のパドル数が3枚で各開き角
α1が120゜である以外は、実施例4と同様(従つて
上記以外のパドル組はすべてパドル数が2枚で開
き角αが180゜であり、l2=15.0mm、S2=24.0mm)の
本発明装置の場合。
比較例 4
両隣接パドル組のパドルの数及び位相角差βは
比較例3と同様(従つて各隣接パドル組のパドル
1枚についてはβ=0であるが、他のパドルには
β=0となるものがない)であり、その他は実施
例7と同様の撹拌装置の場合。
インパルス応答を第3表に示す。[Table] From the column of Table 2 and Example 1 of Table 1, if l 2 /l 1 (Example) or S 2 > S 1 (Example 3), it is possible to equalize the residence time of powder and granular material. It is more effective and l 2
> l 1 and S 2 > S 1 (Example 4), it can be seen that there is a further synergistic effect. Examples 5 to 7, Comparative Example 4 Example 5 Same as Example 1 except that the number of paddles in each adjacent paddle group is 3 and the opening angle α is all 120° (therefore, the number of paddles in the paddle groups other than the above is With two pieces, the opening angle α is
180°) for the device of the present invention. Example 6 The number of paddles in paddle groups other than both adjacent paddle groups is also 3
The present invention is the same as in Example 5, except that the opening angle α is 120° and the phase angle difference between the paddles is 60° between adjacent paddle sets (excluding both adjacent paddle sets). For equipment. Example 7 Same as Example 4 except that each adjacent paddle group has 3 paddles and each opening angle α1 is 120° (therefore, all paddle groups other than the above have 2 paddles and the opening angle α is 180°, l 2 = 15.0 mm, S 2 = 24.0 mm). Comparative Example 4 The number of paddles and the phase angle difference β in both adjacent paddle sets are the same as in Comparative Example 3 (therefore, β = 0 for one paddle in each adjacent paddle set, but β = 0 for the other paddles). ), otherwise the stirring device was the same as in Example 7. The impulse response is shown in Table 3.
【表】
第3表より、両隣接パドル組を含めて各パドル
組のパドル数が3枚の場合(実施例6)も2枚の
場合と同様に粉粒体滞留時間の均一化の効果があ
り、又、両隣接パドル組のパドル数や開き角αが
その他のパドル組のそれと異なつていても、前者
が本発明の条件を満足する限り(実施例5)、本
発明の上記効果のあることが判る。
更に、実施例7と比較例4との比較から、l1と
l2との関係及びS1とS2との関係を実施例4と同様
に好ましい態様としても、両隣接パドル組間でパ
ドルの位相角差βが本発明の条件を満足しないと
きは、効果のないことが判る。
実施例 8
実施例1と同じ撹拌装置を気相重合器として使
用し、これにエチレンとプロピレンとの混合モノ
マーを触媒と共に導入しながら、重合圧力20Kg/
cm3、重合温度60℃の条件下で回転数40rpm(Fr=
0.367)の撹拌を続ける連続重合を長期間実施し
て、エチレン−プロピレンコポリマー(エチレン
含量12重量%)を製造した。これから得られた成
形品の物性は良好で、とくに低温衝撃性は良好で
あつた。
実施例 9
実施例4と同じ撹拌装置を気相重合器として使
用し、実施例8と同じ混合モノマーを同じ条件下
で長期間連続重合してエチレン−プロピレンコポ
リマーを製造した。かくして得られた成形品の物
性、とくに低温衝撃性は著しく向上し、バツチ重
合で得られたエチレン−プロピレンコポリマーの
低温衝撃性と同等であつた。[Table] From Table 3, it can be seen that when the number of paddles in each paddle set is 3, including the adjacent paddle sets on both sides (Example 6), the effect of equalizing the residence time of the powder and granular material is the same as when there are 2 paddles. Also, even if the number of paddles and the opening angle α of both adjacent paddle sets are different from those of other paddle sets, as long as the former satisfies the conditions of the present invention (Example 5), the above effects of the present invention can be achieved. It turns out that there is something. Furthermore, from the comparison between Example 7 and Comparative Example 4, l 1 and
Even if the relationship with l 2 and the relationship between S 1 and S 2 are as preferred as in Example 4, if the paddle phase angle difference β between both adjacent paddle sets does not satisfy the conditions of the present invention, the effect It turns out that there is no. Example 8 The same stirring device as in Example 1 was used as a gas phase polymerization vessel, and while a mixed monomer of ethylene and propylene was introduced together with a catalyst, a polymerization pressure of 20 kg/
cm 3 , polymerization temperature 60℃, rotation speed 40rpm (Fr=
0.367) was carried out for a long period of time with continuous stirring to produce an ethylene-propylene copolymer (ethylene content 12% by weight). The physical properties of the molded product obtained from this were good, especially the low-temperature impact resistance. Example 9 Using the same stirring device as in Example 4 as a gas phase polymerization vessel, the same mixed monomers as in Example 8 were continuously polymerized for a long period of time under the same conditions to produce an ethylene-propylene copolymer. The physical properties of the thus obtained molded article, particularly the low-temperature impact properties, were significantly improved and were comparable to the low-temperature impact properties of the ethylene-propylene copolymer obtained by batch polymerization.
第1図は本発明装置の1例を模式的且つ透視的
に示す側面説明図、第2図は第1図中固定堰を挟
んで隣接する2組のパドル組(隣接パドル組)の
各パドルの位置を示すA−A線から矢印方向に見
た説明図、第3図はパドルの位相角差が90゜のと
きの隣接パドル組を第2図と同じ位置で見た説明
図、第4図は第3図の状態から隣接パドル組を
90゜回転させた状態を示す説明図、第5図はパド
ル組が粉粒体を撹拌するときの回転に従つて変化
する粉粒体堆積表面の高低を示す説明図、第6図
及び第7図はそれぞれ粉粒体を撹拌するときの固
定堰付近における粉粒体堆積表面の高低変化を第
3図及び第4図に対応する2つの両極端の場合に
ついてパドル組の位置と共に示す側面説明図、第
8図、第9図及び第10図は本発明装置の固定堰
とこれを挟んで隣接するパドル組との配置状態の
種々な態様と粉粒体堆積表面の形成状態とを示す
側面説明図である。
1……横型円筒状容器(容器)、2……供給口、
3……抜出し口、4……回転軸、5……パドル
組、5a……固定堰を挟んで隣接するパドル組
(隣接パドル組)中の供給口(上流)側のパドル
組、5b……隣接パドル組中の抜出し口(下流)
側のパドル組、6……パドル、6a……隣接パド
ル組中の供給口(上流)側のパドル組のパドル、
6b……隣接パドル組中の抜出し口(下流)側の
パドル組のパドル、7……固定堰、8……開口
部、D……容器の直径、d……回転軸の直径、
Hs……粉粒体堆積表面の谷部と固定堰の上方延
長面との軸方向の距離、L……容器の長さ、l…
…容器内壁とパドル先端とのクリアランス、l1…
…容器内壁と供給口(上流)側の隣接パドル組の
パドル先端とのクリアランス、l2……容器内壁と
抜出し口(下流)側の隣接パドル組のパドル先端
とのクリアランス、AL……粉粒体堆積表面の頂
部一帯の平均的なレベル、HL……粉粒体堆積表
面の頂部一帯の最も高いレベル、LL……粉粒体
堆積表面の頂部一帯の最も低いレベル、P……固
定堰の上方延長面、P′……谷部、S1……固定堰と
供給口(上流)側の隣接パドル組のパドルとのク
リアランス、S2……固定堰と抜出し口(下流)側
の隣接パドル組のパドルとのクリアランス、W…
…パドルの幅、α……開き角、β……隣接パドル
組間でのパドルの位相角差。
Fig. 1 is a side view schematically and transparently showing an example of the device of the present invention, and Fig. 2 shows each paddle of two adjacent paddle sets (adjacent paddle sets) across the fixed weir in Fig. 1. Figure 3 is an explanatory diagram of the adjacent paddle set viewed from the same position as Figure 2 when the phase angle difference of the paddles is 90°, Figure 4 is an explanatory diagram of the position of The figure shows the adjacent paddle groups from the state shown in Figure 3.
An explanatory diagram showing a state rotated by 90 degrees, Fig. 5 is an explanatory diagram showing the height of the powder/granular material accumulation surface that changes as the paddle set rotates when stirring the powder/granular material, Figs. 6 and 7 The figures are side explanatory views showing the height changes of the powder and granular material accumulation surface near the fixed weir when stirring the powder and granular materials, together with the position of the paddle set, for two extreme cases corresponding to FIGS. 3 and 4, respectively; FIGS. 8, 9, and 10 are side explanatory views showing various arrangements of the fixed weir of the device of the present invention and adjacent paddle sets on both sides thereof, and the formation state of the powder and granular material deposition surface. It is. 1... Horizontal cylindrical container (container), 2... Supply port,
3... Extraction port, 4... Rotating shaft, 5... Paddle group, 5a... Paddle group on the supply port (upstream) side of adjacent paddle groups (adjacent paddle groups) across the fixed weir, 5b... Extraction port in adjacent paddle set (downstream)
side paddle group, 6...paddle, 6a... paddle of the supply port (upstream) side paddle group in the adjacent paddle group,
6b... Paddle of the paddle group on the extraction port (downstream) side in the adjacent paddle group, 7... Fixed weir, 8... Opening, D... Diameter of container, d... Diameter of rotating shaft,
Hs...Distance in the axial direction between the valley part of the powder accumulation surface and the upwardly extending surface of the fixed weir, L...Length of the container, l...
…Clearance between the inner wall of the container and the tip of the paddle, l 1 …
...Clearance between the inner wall of the container and the paddle tip of the adjacent paddle group on the supply port (upstream) side, l 2 ...Clearance between the inner wall of the container and the paddle tip of the adjacent paddle group on the extraction port (downstream) side, AL...Powder grain average level over the top area of the particle accumulation surface, HL...highest level across the top area of the particle accumulation surface, LL...lowest level across the top area of the particle accumulation surface, P...of the fixed weir. Upper extension surface, P′...trough, S 1 ... Clearance between the fixed weir and the paddle of the adjacent paddle group on the supply port (upstream) side, S 2 ... Fixed weir and the adjacent paddle on the outlet (downstream) side Clearance with the pair of paddles, W...
...paddle width, α...opening angle, β...paddle phase angle difference between adjacent paddle sets.
Claims (1)
抜出し口とを有する横型円筒状容器内に、水平な
回転軸とその上の複数の各位置にそれぞれ1枚以
上の矩形状の平らなパドルが取り付けられて成る
パドル組の複数組とから成る撹拌手段が内蔵され
ている横型一軸式の撹拌装置であつて、上記回転
軸と垂直方向に容器内壁に固定された1つの固定
堰によつて容器内が2つの撹拌ゾーンに分割され
ており、該固定堰を挟んで隣接する2つのパドル
組が以下の条件を満足することを特徴とする撹拌
装置; (i) 2つのパドル組のパドルの幅W及び枚数は互
に等しい。 (ii) β=0゜、 (iii) D/100≦l1≦D/20、 (iv) l2/l1≧1 (v) 1≦S2/S1≦20 [ここに β:固定堰を挟んで隣接するパドル組間の各パド
ルが回転軸に対して垂直な投影面上で成す位相
角差、 D:横型円筒状の容器の内径(mm)、 l1:容器内壁と供給口側のパドル組のパドル先端
とのクリアランス(mm)、 l2:容器内壁と抜出し口側のパドル組のパドル先
端とのクリアランス(mm)、 S1:供給口側のパドル組のパドルと固定堰とのク
リアランス(mm)、 S2:抜出し口側のパドル組のパドルと固定堰との
クリアランス(mm)。] 2 l1とl2とが (iv) 1≦l2/l1≦3 の関係にあり、 S1とS2とが (v) 1≦S2/S1≦12 の関係にある特許請求の範囲第1項に記載の撹拌
装置。 3 l1とl2とが (iv) l2/l1=1 の関係にあり、 S1とS2とが (v) 1≦S2/S1≦3 の関係にある特許請求の範囲第1項に記載の撹拌
装置。 4 l1とl2とが (iv) l2/l1>1 の関係にあり、 S1とS2とが (v) 1<S2/S1≦20 の関係にある特許請求の範囲第1項に記載の撹拌
装置。 5 横型円筒状容器の供給口が、該容器の内部で
連続的に気相重合されて固定堰に至るまでに粉粒
体となる重合性単量体と重合触媒との混合物を供
給するための供給口である特許請求の範囲第1項
から第4項までのいずれか1項に記載の撹拌装
置。[Claims] 1. In a horizontal cylindrical container that generally has a supply port for the material to be stirred and a powder outlet at the other end, one sheet is placed at each of a plurality of positions on the horizontal rotation shaft. It is a horizontal uniaxial stirring device that has a built-in stirring means consisting of a plurality of paddle sets each having the rectangular flat paddles attached thereto, and is fixed to the inner wall of the container in a direction perpendicular to the rotation axis. A stirring device characterized in that the inside of the container is divided into two stirring zones by one fixed weir, and two sets of paddles adjacent to each other across the fixed weir satisfy the following conditions; ) The width W and number of paddles of the two paddle sets are equal to each other. (ii) β=0゜, (iii) D/100≦l 1 ≦D/20, (iv) l 2 /l 1 ≧1 (v) 1≦S 2 /S 1 ≦20 [here β: fixed Phase angle difference between adjacent paddle sets across the weir on a projection plane perpendicular to the axis of rotation, D: Inner diameter of horizontal cylindrical container (mm), l 1 : Inner wall of container and supply port Clearance between the paddle tip of the paddle group on the side (mm), l 2 : Clearance between the inner wall of the container and the tip of the paddle of the paddle group on the outlet side (mm), S 1 : Paddle of the paddle group on the supply port side and the fixed weir clearance (mm), S 2 : Clearance (mm) between the paddle of the paddle assembly on the outlet side and the fixed weir. ] 2 A patent in which l 1 and l 2 are in the relationship (iv) 1≦l 2 /l 1 ≦3, and S 1 and S 2 are in the relationship (v) 1≦S 2 /S 1 ≦12 A stirring device according to claim 1. 3 Claims in which l 1 and l 2 have a relationship of (iv) l 2 /l 1 = 1, and S 1 and S 2 have a relationship of (v) 1≦S 2 /S 1 ≦3 The stirring device according to item 1. 4 Claims in which l 1 and l 2 have a relationship of (iv) l 2 /l 1 > 1, and S 1 and S 2 have a relationship of (v) 1<S 2 /S 1 ≦20 The stirring device according to item 1. 5 The supply port of the horizontal cylindrical container is for supplying a mixture of a polymerizable monomer and a polymerization catalyst that is continuously polymerized in the gas phase inside the container and becomes a powder by the time it reaches the fixed weir. The stirring device according to any one of claims 1 to 4, which is a supply port.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61068771A JPS62227431A (en) | 1986-03-28 | 1986-03-28 | Agitator |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61068771A JPS62227431A (en) | 1986-03-28 | 1986-03-28 | Agitator |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62227431A JPS62227431A (en) | 1987-10-06 |
| JPH0333373B2 true JPH0333373B2 (en) | 1991-05-16 |
Family
ID=13383328
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61068771A Granted JPS62227431A (en) | 1986-03-28 | 1986-03-28 | Agitator |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62227431A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101379097B (en) | 2006-02-03 | 2011-08-03 | 日本聚丙烯公司 | Propylene-based polymer and its preparation method, propylene-based polymer composition and shaped articles made from the composition |
-
1986
- 1986-03-28 JP JP61068771A patent/JPS62227431A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS62227431A (en) | 1987-10-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3354136A (en) | Material treatment methods | |
| FI96745C (en) | Process for olefin polymerization in fluidized bed polymerization reactor | |
| CA2312988C (en) | Agitator for subfluidized particulate bed in quench-cooled vapor phase polymerization reactors | |
| US4101289A (en) | Horizontal reactor for the vapor phase polymerization of monomers | |
| US3469948A (en) | Paddle-type polymerization reactor | |
| JPS5921321B2 (en) | Monomer vapor phase polymerization method and polymerization reactor used therein | |
| US7459506B2 (en) | Segmented agitator reactor | |
| US4535134A (en) | Method and apparatus for controlling the discharge of product from vapor phase polymerization of monomers in a horizontal stirred-bed reactor | |
| KR930010921B1 (en) | Process for producing styrene-based polymers and apparatus for producing said polymers | |
| EP1133350B1 (en) | Prepolymerisation reactor | |
| EP1663476B1 (en) | Process with a loop reactor with varying diameter for olefin polymerization | |
| JPH0333373B2 (en) | ||
| JPH025450B2 (en) | ||
| JPH0331094B2 (en) | ||
| JPH0227011B2 (en) | ||
| JPH0333374B2 (en) | ||
| US3749555A (en) | Polymerization reactor | |
| JPS63223001A (en) | Horizontal reactor | |
| US8383740B1 (en) | Horizontal agitator | |
| US4727132A (en) | Method of continuous manufacturing of polymers or copolymers of trioxane | |
| KR20170112626A (en) | Stirring apparatus | |
| JPH0113547Y2 (en) | ||
| JPS60150821A (en) | Stirring apparatus of horizontal-type uniaxial cylindrical vessel | |
| JPS61146328A (en) | Process for operating stirring device | |
| JP2952834B2 (en) | Method for producing polyoxymethylene |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| EXPY | Cancellation because of completion of term |