| 钼系催化体系制备高乙烯基含量丁苯共聚物的研究 |
| Study on Preparation of Bd-St Copolymer with High Vinyl Content by Molybdenum Catalytic System |
| 投稿时间：2020-02-18 修订日期：2020-02-18 |
| DOI：10.12136/j.issn.1000-890X.2021.01.0031 |
| 中文关键词: 钼系催化剂 丁苯共聚物 乙烯基含量 配位聚合 聚合活性 特性粘数 相对分子质量 |
| 英文关键词: molybdenum catalyst butadiene-styrene copolymer vinyl content coordination polymerization polymerization activity intrinsic viscosity relative molecular weight |
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| 中文摘要: |
| 以磷酸三丁酯（TBP）为配体改性的五氯化钼（MoCl5）为主催化剂，二丁基镁[Mg（Bu）2]为助催化剂组成二元催化体系，在丁二烯（Bd）物质的量浓度为2.6×103 mol·L-1和Bd/苯乙烯（St）质量比为3的条件下进行丁苯共聚物的配位聚合，研究催化体系和聚合条件对聚合反应的影响，并采用凝胶渗透色谱、傅里叶变换红外光谱、核磁共振氢谱、差示扫描量热法等对共聚物的微观结构进行分析。试验得出的最佳反应条件为：TBP/MoCl5物质的量比 2，MoCl5/单体物质的量比 1×10-3，Mg（Bu）2/MoCl5物质的量比 3，聚合温度 70 ℃，聚合时间 12 h。在该条件下，Bd和St聚合活性较高，丁苯共聚物的数均相对分子质量为1.24×105，相对分子质量分布较宽，Bd结构单元中1，2-结构物质的量分数大于0.85，聚合产物为高乙烯基含量无规丁苯共聚物。 |
| 英文摘要: |
| The coordination polymerization of butadiene（bd） and styrene（St） was carried out with binary molybdenum catalystic system which consists of the main catalyst of MoCl5 seasoning modified by tributyl phosphate（TBP） ligands and cocatalyst butyl magnesium[Mg（Bu）2] under the mass concentration of Bd was 2.6 mol·mL-1 and the mass ratio of Bd/St was 3.The effects of the cocatalyst system and polymerization condition on the polymerization reaction were investigated.Furthermore，the microstructure of the copolymer were analyzed by GPC，FTIR，1H MNR and DSC.The results showed that，the optimum reaction conditions were as follows：the mole ratio of TBP/MoCl5 was 2，the mole ratio of MoCl5/ monomer was 1×10-3，the mole ratio of Mg（Bu）2/MoCl5 was 3，the polymerization temperature was 70 ℃，and the polymerization time was 12 h. Under these conditions，the copolymerization activity of Bd and St was higher，the number average molecular weight of the copolymer was up to 1.24×105，and the relative molecular weight distribution was broader，the butadiene unit was mainly 1，2-structure with mole fraction of over 0.85.The polymerization product was random Bd/St copolymer with high vinyl content. |
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