JP5624982B2 - 熱可塑性分散体の無溶剤製造法 - Google Patents
熱可塑性分散体の無溶剤製造法 Download PDFInfo
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Description
この方法における圧力は窒素封入(nitrogen padding)により個々に制御/維持可能である。
大きなユニットでのEAA XUS60758.02L(60% M.I.、17% AA、Dow社から入手可能)の分散体の生成条件
大きなユニットでの、2つの組合せたEAA:60重量%のPrimacor 3440(MI10、9.7AA%、Dow Chemical Companyから入手可能)と40重量%のXUS60758.02L(60 MI、17%AA、Dow社から入手可能)との分散体の生成条件
大きなユニットでの、SISとEAA:67重量%のKraton D 1161(Kraton社から入手可能)と33重量%のPrimacor 5980(300 MI、2.5%AA、Dow社から入手可能)との分散体の生成条件
大きなユニットでの、ポリエステルとEAA:19重量%の商業的に入手可能なポリエステルと15重量%のPrimacorとの分散体の生成条件は、上記実施例3と基本的に同等であるように選択され得る。
2 1のための冷却/加熱手段
3 1の充填用開口部のカバー
4 1の下部弁
5 1における撹拌機の駆動モータ
6 1における撹拌機の軸
7 脱塩水管
8 加圧空気管
9 洗浄媒体のための管
10 1の主出口管
11 循環管
12 11のモータ
13 弁を備える出口管
14 ポンプ
15 予熱された水/アルカリのための入口管
16 圧力センサ
17 圧力センサ
18 2次撹拌機ユニット
19 18のモータ
20 ディスパックスチャンバ
21 18のバイパスライン
22 21の安全弁
23 再循環管
24 再循環支流
25 出口支流
26 24における弁
27 25における弁
28 1における23の流出口
29 貫流式冷却ユニット
30 第2の出口管
31 1への試薬入口管
32 10への試薬入口管
Claims (13)
- 第1の容積(1)および第2の容積(10、20、23、24)を有する反応容器(1、10、20、23、24)を用いる熱可塑性またはエラストマーポリマー分散体の製造方法であって、第1の撹拌機が前記第1の容積(1)内に配置され作動可能であり、第2の撹拌機(20)が前記第2の容積(10、20、23、24)内に配置され作動可能であり、第1の容積(1)は第2の容積(10、20、23、24)より少なくとも20倍大きく、これらの容積内の撹拌機は1000mPas以上の粘度に対処可能であり、前記方法は、
a.初期量のポリマーと任意で水および/または任意でアルカリとを容器の第1の容積(1)に充填する工程と、
b.80〜300℃の範囲の標的処理温度に第1の容積(1)を外部から加熱する工程と、
c.10〜100rpmの範囲の速度で少なくとも30分の間第1の容積(1)における第1の撹拌機を作動する工程とを含み、工程cは任意で工程bに付随して行われ、さらに、
d.第1の容積(1)に水および任意でアルカリを添加する工程と、
e.第2の容積(10、20、23、24)を第1の容積(1)に接続し、1000rpmを超える速度で第2の容積(10、20、23、24)における第2の撹拌機(20)を作動させ、前記第1の容積内の反応流体が前記第2の容積を通る回転率である再循環比が3を超える時間範囲の間、動作温度を基本的には一定に保ちながら、前記第2の撹拌機に反応生成物を通して再循環させて、分散体を形成する工程とを含む方法。 - 工程aにおいて、第1の容積には、基本的には水なしでポリマーまたはポリマー前駆体材料のみが添加され、
工程cに付随してあるいは重複して行われる工程bにおいて、第1の容積およびその中のポリマーは、液体状態のポリマー材料を生成する155〜180℃の範囲の処理温度に能動的に加熱され、
工程dは、以下の工程;
d1.少なくとも140℃に第1の容積内の温度を保ちながら、15〜60分の範囲、80〜95%の範囲の固形分となる量のアルカリと組合わせて第1の量の水を基本的に連続的にあるいは細かく分割された回分式で添加し、
その後、さらに10〜30分の間、対応する反応混合物を撹拌する任意の工程と、
d2.60〜120分間、非アルカリ水を連続的あるいは回分式に添加することで、50〜70%の範囲の固形分が得られる工程と、を含む、請求項1に記載の方法。 - 前記工程a〜工程eの後、固形分を30〜50%の範囲にするためにさらなる量の水が第1の容積および/または第2の容積に添加され、その後、反応混合物は任意で5〜30分撹拌され、その後、再循環ライン(23)が出力ライン(25)に転換され、反応混合物は、急冷工程において、20〜40℃の温度まで急速に冷却される、請求項1または2に記載の方法。
- 前記標的処理温度は100〜200℃の範囲であり、および/または前記第2の撹拌機はローターステーターポンプであり、かつ/または1次撹拌機の先端速度は、50km/h未満である、請求項1〜3のいずれかに記載の方法。
- 前記第1の容積は反応容器の下部に配置され、前記第2の容積は反応容器の上部に配置され、反応容器に充填する際、最初は第1の容積を形成する下部にのみ反応物を満たす、請求項1〜4のいずれかに記載の方法。
- 前記第2の撹拌機はローターステーターポンプであり、その入力側は調節弁を介して第1の容積の下部に接続され、その出力側は第1の容積の上部に接続され、工程dの後に、前記弁を開いて工程eにおける支援された再循環を開始する、請求項1〜5のいずれかに記載の方法。
- 工程cは、少なくとも1時間行われる、請求項1〜6のいずれかに記載の方法。
- 工程eは少なくとも5分間行われる、請求項1〜7のいずれかに記載の方法。
- 工程c〜工程eの間、反応容器における圧力は4〜20バールの範囲に維持される、請求項1〜8のいずれかに記載の方法。
- 工程eにおいて形成される分散体は、20μm未満の平均粒径を有する、請求項1〜9のいずれかに記載の方法。
- 工程eにおいて形成される分散体は、9未満のpH値を有する、請求項1〜10のいずれかに記載の方法。
- 工程aにおいて容器内に満たされるポリマーは、EAA(エチレンアクリル酸)、EMAA(エチレン/メタクリル酸)、オレイン、ステアリン、コロホニーなどのロジン、またはその混合物からなる第1のグループから、任意で、SIS(スチレン‐イソプレン‐スチレン)、SBS(スチレン‐ブタジエン‐スチレン)、SEBS(スチレン‐エチレン‐ブタジエン‐スチレン)、SES(スチレン‐エチレン‐スチレン)、EVA(エチレン‐酢酸ビニル)、PP(ポリプロピレン)、PE(ポリエチレン)、ポリエステル、PET(ポリエチレンテレフタレート)、PVC(ポリ塩化ビニル)、またはこれらの系の混合物からなる第2のグループから選択される系との混合物において、選択され、混合された系においては、第1のグループの熱可塑性/エラストマーポリマー部分は、少なくとも20容量パーセントとして存在する、請求項1〜11のいずれかに記載の方法。
- 反応容器の下部に配置され外部から加熱される第1の容積と、反応容器の上部に配置される第2の容積とを含み、あるいは第2の容積は第1の容積の反応流体を再循環させる撹拌手段を備える再循環配管システムによって与えられ、第1の容積は第2の容積の少なくとも20倍大きく、これらの容積における撹拌機は1000mPas以上の粘度に対処可能であり、第1の撹拌機が第1の容積内に配置され、第2の撹拌機が第2の容積内に配置され、第1の撹拌機および第2の撹拌機は、反応容器内に同軸上に設けられ異なった速度で動作可能であり、第2の撹拌機はディスパックスチャンバ(20)である、請求項1〜12のいずれかに記載の方法を実施するための反応容器。
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