JP2019515125A - 変性重合開始剤の製造方法及び製造装置 - Google Patents
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Abstract
Description
第1流体流入口、第2流体流入口、変形部及び流出口が備えられた管状反応器を準備した。前記管状反応器の本体(body)の外径は1/4inchであり、前記第1流体流入口は、管状反応器の側部に備えられており、外径が1/8inchであり、前記第2流体流入口は、管状反応器の一側端部から変形部と流出口の連結部まで内部に挿入された形態に備えられ、かつ、前記変形部と流出口の連結部で離隔されており、外径が1/8inchであり、前記流出口は、管状反応器の他側端部に備えられており、外径が1/8inchであり、前記変形部は、反応器の第1流体流入口が備えられた地点から離隔され、管状反応器の外径から前記流出口の外径に外径が漸次減少する形態に流出口に連結されている。
前記実施例1で、ジメチルビニルベンジルアミン(DMVBA)が3.8重量%で、極性添加剤であるテトラメチルエチレンジアミン(TMEDA)が2.7重量%でn−ヘキサンに共に溶解された溶液に代えて、ジメチルビニルベンジルアミン(DMVBA)が4.9重量%で、極性添加剤であるテトラメチルエチレンジアミン(TMEDA)が2.7重量%でn−ヘキサンに共に溶解された溶液を投入したことを除き、前記実施例1と同様の方法で実施した。このとき、n−ブチルリチウムとジメチルビニルベンジルアミンのモル比は1:1.3であり、ジメチルビニルベンジルアミンとテトラメチルエチレンジアミンのモル比は1:0.77であった。
第1流体流入口、第2流体流入口及び流出口が備えられた管状反応器を準備した。前記管状反応器の本体(body)の外径は1/4inchであり、前記第1流体流入口は、管状反応器の側部に備えられており、外径が1/8inchであり、前記第2流体流入口は、管状反応器の一側端部に備えられており、外径が1/8inchであり、前記流出口は、管状反応器の他側端部に備えられており、外径が1/8inchである。
3Lサイズの温度調節が可能な回分式反応器にヘキサン600g、1.6Mのn−ブチルリチウム溶液32g、テトラメチルエチレンジアミン8.9gを入れた後、反応器の温度を10℃に維持した。以後、反応器を撹拌しながら、ジメチルビニルベンジルアミン12.3gを前記反応器の上部からドロップワイズ(drop wise)方式で一滴ずつ投入した。前記ジメチルビニルベンジルアミンの投入が完了して10分間撹拌した後、生成された変性重合開始剤化合物の一部を分取して過量のエタノールで水素化させ、ガスクロマトグラフィーで確認した結果、変性官能基含有化合物として投入されたジメチルビニルベンジルアミンは検出されず、変性重合開始剤化合物が99モル%以上の転換率で生成されたことを確認することができた。
前記実施例及び比較例の変性重合開始剤の転換率をガスクロマトグラフィーで分析した。
Claims (7)
- 第1官能基含有化合物を含む第1流体流入口と、第2官能基含有化合物を含む第2流体流入口とを備えた反応器内に、前記第1流体流入口へ第1流体を投入し、前記第2流体流入口へ第2流体を投入して、前記第1官能基含有化合物及び前記第2官能基含有化合物を反応させるステップ(S1)と、
前記(S1)ステップの反応で製造された変性重合開始剤を含む第3流体を前記反応器に備えられた流出口を介して収得するステップ(S2)とを含んでなり、
前記(S1)ステップ及び(S2)ステップは連続的に実施され、
前記(S1)ステップにおいて、前記第1流体と前記第2流体が混合される時点の前記第1流体及び前記第2流体の流量は一定に維持され、前記第1流体の流速は前記第1流体と前記第2流体が混合される時点に増加する変性重合開始剤の製造方法。 - 前記第1官能基含有化合物及び前記第2官能基含有化合物は、それぞれ変性官能基含有化合物及び重合開始官能基含有化合物であり、
前記第1官能基含有化合物が変性官能基含有化合物である場合、前記第2官能基含有化合物は重合開始官能基含有化合物であり、
前記第1官能基含有化合物が重合開始官能基化合物である場合、前記第2官能基含有化合物は変性官能基含有化合物である請求項1に記載の変性重合開始剤の製造方法。 - 前記(S1)ステップの前記第1流体及び前記第2流体が混合される時点で、前記第1流体及び前記第2流体は平行に会うものである請求項1に記載の変性重合開始剤の製造方法。
- 前記(S1)ステップの前記第1流体及び前記第2流体の投入時、前記第1流体及び前記第2流体それぞれの流動方向は、互いに垂直である請求項1に記載の変性重合開始剤の製造方法。
- 前記(S1)ステップで投入される前記第1官能基含有化合物と前記第2官能基含有化合物のモル比(第1官能基含有化合物:第2官能基含有化合物)は、10:1から1:10である請求項1に記載の変性重合開始剤の製造方法。
- 前記反応器の内部温度は、−50℃から50℃である請求項1に記載の変性重合開始剤の製造方法。
- 請求項1に記載の変性重合開始剤の製造方法を実施するための変性重合開始剤の製造装置であって、
第1流体流入口、第2流体流入口、第1流体の流速を増加させるための変形部、第1流体と第2流体が混合される混合部、及び第3流体が流出される流出口を備えた反応器である変性重合開始剤の製造装置。
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JP2022521400A (ja) * | 2019-10-11 | 2022-04-07 | エルジー・ケム・リミテッド | 変性開始剤の製造方法および製造装置 |
JP7448556B2 (ja) | 2019-10-11 | 2024-03-12 | エルジー・ケム・リミテッド | 変性開始剤の製造方法および製造装置 |
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US20190083949A1 (en) | 2019-03-21 |
WO2018117472A1 (ko) | 2018-06-28 |
EP3406332A1 (en) | 2018-11-28 |
JP7216687B2 (ja) | 2023-02-01 |
US10906019B2 (en) | 2021-02-02 |
KR102159608B1 (ko) | 2020-09-25 |
EP3406332A4 (en) | 2019-03-20 |
JP2020196894A (ja) | 2020-12-10 |
KR20180073319A (ko) | 2018-07-02 |
CN108778482B (zh) | 2021-11-19 |
JP7123353B2 (ja) | 2022-08-23 |
CN108778482A (zh) | 2018-11-09 |
EP3406332B1 (en) | 2021-02-17 |
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