JP2020510746A - 炭素繊維製造用アクリロニトリル系重合体の製造方法 - Google Patents
炭素繊維製造用アクリロニトリル系重合体の製造方法 Download PDFInfo
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Abstract
Description
本発明は、2017年9月29日に出願された韓国特許出願第10−2017−0127936号及び2018年9月17に出願された韓国特許出願第10−2018−0110670号に基づいた優先権の利益を主張し、当該韓国特許出願の文献に開示された全ての内容を本明細書の一部として含む。
本発明の一実施形態による炭素繊維製造用アクリロニトリル系重合体の製造方法は、(1)(メタ)アクリロニトリル系単量体及び第1反応溶媒を含む反応溶液を準備する段階、(2)前記反応溶液に開始剤を1次投入して重合を開始する段階、及び、(3)重合転換率が70から80%である時点に到達した時、開始剤を2次投入して重合を行う段階を含む。
先ず、(メタ)アクリロニトリル系単量体及び第1反応溶媒を含む反応溶液を準備する。
次に、前記反応溶液に開始剤を1次投入して重合を開始する。
次に、1次開始剤投入後に重合が進行され重合転換率が70から80%である時点に到達した時、開始剤を2次に投入し、重合反応を進行させる。
以下、本発明の属する技術分野で通常の知識を有する者が容易に実施できるように、本発明の実施形態に対して詳しく説明する。しかし、本発明は、色々と異なる形態に具現されてよく、ここで説明する実施形態に限定されない。
[実施例1]
ジメチルスルホキシド365重量部に、アクリロニトリルとメチルアクリレートとイタコン酸を97:2:1のモル比で混合した単量体混合物100重量部を均一に溶解し反応溶液を準備した。ジメチルスルホキシド5重量部にラジカル重合開始剤としてアゾビスイソブチロニトリル0.2重量部を均一に溶解しラジカル重合開始剤溶液を準備した。
6時間の間溶液重合を行った後、前記ラジカル重合開始剤溶液の全量を一括投入(重合転換率が75%である時点)したことを除いては、実施例1と同一の方法でアクリロニトリル系重合体溶液を収得した。
7時間の間溶液重合を行った後、前記ラジカル重合開始剤溶液の全量を一括投入(重合転換率が80%である時点)したことを除いては、実施例1と同一の方法でアクリロニトリル系重合体溶液を収得した。
アゾビスイソブチロニトリルの代わりに、ジメチル2,2’−アゾビス(2−メチルプロピオネート)を均一に溶解したラジカル重合開始剤溶液を投入したことを除いては、実施例1と同一の方法でアクリロニトリル系重合体溶液を収得した。
アゾビスイソブチロニトリルの代わりに、2,2’−アゾビス(2−メチルブチロニトリル)を均一に溶解したラジカル重合開始剤溶液を投入したことを除いては、実施例3と同一の方法でアクリロニトリル系重合体溶液を収得した。
4.9時間の溶液重合を行った後、前記ラジカル重合開始剤溶液の全量を一括投入(重合転換率が69%である時点)したことを除いては、実施例1と同一の方法でアクリロニトリル系重合体溶液を収得した。
7.2時間の溶液重合を行った後、前記ラジカル重合開始剤溶液の全量を一括投入(重合転換率が81%である時点)したことを除いては、実施例1と同一の方法でアクリロニトリル系重合体溶液を収得した。
ジメチルスルホキシド370重量部に、アクリロニトリルとメチルアクリレートとイタコン酸を97:2:1のモル比で混合した単量体混合物100重量部を均一に溶解し反応溶液を準備した。
ジメチルスルホキシド365重量部に、アクリロニトリルとメチルアクリレートとイタコン酸を97:2:1のモル比で混合した単量体混合物100重量部を均一に溶解し反応溶液を準備した。
ジメチルスルホキシド370重量部に、アクリロニトリルとメチルアクリレートとイタコン酸を97:2:1のモル比で混合した単量体混合物100重量部を均一に溶解し反応溶液を準備した。
実施例1、比較例1から比較例3のアクリロニトリル系重合体の重合転換率、分子量分布(PDI:Mw/Mn)を測定しており、重合体溶液の粘度を測定し下記表1に記載した。
2)分子量分布(PDI):収得された重合体溶液1gを下記条件でGPC(Gel Permeation Chromatography)を用いて重量平均分子量(Mw)と数平均分子量(Mn)を測定し、分子量分布を算出した。
3)粘度:下記条件でブルックフィールド(Brookfield)を用いて測定した。
Claims (10)
- (メタ)アクリロニトリル系単量体及び第1反応溶媒を含む反応溶液を準備する段階と、
前記反応溶液に開始剤を1次投入して重合を開始する段階と、
重合転換率が70から80%である時点に到達した時、開始剤を2次投入して重合を行う段階とを含む炭素繊維用アクリロニトリル系共重合体の製造方法。 - 前記1次投入された開始剤と2次投入された開始剤の重量比が1:1から10:1のものである、請求項1に記載の炭素繊維用アクリロニトリル系共重合体の製造方法。
- 前記2次投入された開始剤は、第2反応溶媒と混合された状態で投入されるものである、請求項1に記載の炭素繊維製造用アクリロニトリル系共重合体の製造方法。
- 前記第2反応溶媒は、第1反応溶媒と同一のものである、請求項3に記載の炭素繊維製造用アクリロニトリル系共重合体の製造方法。
- 前記2次投入された開始剤と第2反応溶媒は、1:15から1:35の重量比で混合されるものである、請求項3に記載の炭素繊維製造用アクリロニトリル系共重合体の製造方法。
- 前記第2反応溶媒は、前記第1反応溶媒100重量部に対して1から10重量部である、請求項3に記載の炭素繊維製造用アクリロニトリル系共重合体の製造方法。
- 前記1次投入された開始剤と2次投入された開始剤の全体含量は、前記(メタ)アクリロニトリル系単量体100重量部に対して0.2から2重量部のものである、請求項1に記載の炭素繊維製造用アクリロニトリル系共重合体の製造方法。
- 前記開始剤を1次投入する前に、前記反応溶液を50から70℃に昇温させる段階をさらに含む、請求項1に記載の炭素繊維製造用アクリロニトリル系共重合体の製造方法。
- 前記反応溶液は、カルボン酸系共単量体及び(メタ)アクリレート系単量体でなる群から選択される1種以上の共単量体をさらに含むものである、請求項1に記載の炭素繊維製造用アクリロニトリル系共重合体の製造方法。
- 前記共単量体は、前記(メタ)アクリロニトリル系単量体100重量部に対して1から10重量部で含まれるものである、請求項9に記載の炭素繊維製造用アクリロニトリル系共重合体の製造方法。
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KR20170127936 | 2017-09-29 | ||
KR10-2017-0127936 | 2017-09-29 | ||
KR1020180110670A KR102156109B1 (ko) | 2017-09-29 | 2018-09-17 | 탄소섬유 제조용 아크릴로니트릴계 중합체의 제조방법 |
KR10-2018-0110670 | 2018-09-17 | ||
PCT/KR2018/011007 WO2019066360A1 (ko) | 2017-09-29 | 2018-09-18 | 탄소섬유 제조용 아크릴로니트릴계 중합체의 제조방법 |
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US20190375870A1 (en) | 2019-12-12 |
EP3536717A4 (en) | 2019-12-04 |
KR20190038336A (ko) | 2019-04-08 |
EP3536717B1 (en) | 2021-04-07 |
CN110062774B (zh) | 2021-09-14 |
WO2019066360A1 (ko) | 2019-04-04 |
US11427659B2 (en) | 2022-08-30 |
KR102156109B1 (ko) | 2020-09-15 |
EP3536717A1 (en) | 2019-09-11 |
CN110062774A (zh) | 2019-07-26 |
JP7037585B2 (ja) | 2022-03-16 |
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