绿色溶剂中苯乙烯-马来酸酐无规共聚物的合成及表征
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摘要
使用绿色溶剂碳酸二甲酯(DMC)代替传统溶剂丙酮,在120℃、苯乙烯与马来酸酐配比为9:1及氮气环境下,以溶液聚合法制备了苯乙烯-马来酸酐无规共聚物(R-SMA),通过红外光谱、核磁共振、化学滴定等表征方法确证产物为R-SMA,并研究了两种溶剂及其用量对R-SMA组成、结构、分子量、转化率等的影响。结果表明:DMC作溶剂时,R-SMA以苯乙烯作为分子主链,其中SSM、MSS、MSM三种结构在分子链中随机分布,呈无规排列;随着DMC用量的增加,R-SMA的分子量降低,转化率先升高后降低,马来酸酐含量变化不大;与丙酮作溶剂相比,DMC作溶剂时,产物的分子量及马来酸酐含量均较低,耐热性更好。
The random copolymer of styrene-maleic anhydride(R-SMA) was prepared by solution copolymerization with dimethyl carbonate(DMC) as a green solvent instead of acetone at 120℃, the ratio of styrene to maleic anhydride was 9:1 and nitrogen atmosphere. The product was confirmed to be R-SMA by IR, NMR and chemical titration. The effects of two solvents and their dosage on the composition, structure, molecular weight and conversion of R-SMA were studied. The results show that when DMC is used as solvent, R-SMA takes styrene as its main molecular chain. The three structures of SSM, MSS and MSM are randomly distributed in the molecular chain and arranged randomly. With the increase of DMC dosage, the molecular weight of R-SMA decreases, the conversion rate increases first and then decreases, and the content of maleic anhydride does not change much. Compared with acetone, the molecular weight and maleic anhydride content of the product are lower and the heat resistance is better when DMC is used as solvent.
The random copolymer of styrene-maleic anhydride(R-SMA) was prepared by solution copolymerization with dimethyl carbonate(DMC) as a green solvent instead of acetone at 120℃, the ratio of styrene to maleic anhydride was 9:1 and nitrogen atmosphere. The product was confirmed to be R-SMA by IR, NMR and chemical titration. The effects of two solvents and their dosage on the composition, structure, molecular weight and conversion of R-SMA were studied. The results show that when DMC is used as solvent, R-SMA takes styrene as its main molecular chain. The three structures of SSM, MSS and MSM are randomly distributed in the molecular chain and arranged randomly. With the increase of DMC dosage, the molecular weight of R-SMA decreases, the conversion rate increases first and then decreases, and the content of maleic anhydride does not change much. Compared with acetone, the molecular weight and maleic anhydride content of the product are lower and the heat resistance is better when DMC is used as solvent.
引文
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[3]P T Anastas,J C Warner.Green chemistry:Theory and practice[M].Oxford:Oxford University Press,2000.
[4]Prat D,Wells A,Hayler J,et al.CHEM21 selection guide of classical-and less classical-solvents[J].Green Chem,2016,18:288-296.
[5]Byrne F P,Jin S,Paggiola G,et al.Tools and techniques for solvent selection:Green solvent selection guides[J].Sustainable Chemical Processes,2016,DOI:10.1186/s40508-016-0051-z.