化工学报 ›› 2015, Vol. 66 ›› Issue (S2): 461-465.DOI: 10.11949/j.issn.0438-1157.20151495

• 材料化学工程与纳米技术 • 上一篇    下一篇

[60]PCBM的合成及纯化工艺

胡洪超1, 崔英德2   

  1. 1. 西北工业大学材料学院, 陕西西安 710072;
    2. 广州科技职业技术学院, 广东广州 510550
  • 收稿日期:2015-07-25 修回日期:2015-07-29 出版日期:2015-08-31 发布日期:2015-08-31
  • 通讯作者: 崔英德

Synthesis and purification of [60] PCBM

HU Hongchao1, CUI Yingde2   

  1. 1. Northwestern Polytechnical University, Xi'an 710072, Shaanxi, China;
    2. Guangzhou Vocational College of Science and Technology, Guangzhou 510550, Guangdong, China
  • Received:2015-07-25 Revised:2015-07-29 Online:2015-08-31 Published:2015-08-31

摘要:

以C60,对甲苯磺酰肼和4-苯甲酰基丁酸为原料,通过一锅法多步骤合成了[60] PCBM,用硅胶柱为载体,甲苯为洗脱剂获得初步纯化的[60] PCBM。经红外光谱图和1H NMR谱图表征,证明合成产物为目标产物。为进一步纯化产物,结合HPLC分离技术,获得99.5%纯度的[60] PCBM。通过将副产物及回收的C60重新投入合成体系,抑制了新的副产物产生,使得新鲜C60转化为[60]PCBM的收率提高到93.3%。这些措施为降低高纯度[60] PCBM的成本奠定良好的基础。

关键词: 制备, 合成, 纯化, PCBM, HPLC

Abstract:

Using C60, p-toluene sulfonyl hydrazide and 4-benzoyl butyric acid as raw material, [60] PCBM was synthesized by one pot method by multiple steps, obtain the preliminary purification of [60] PCBM using silica gel as the carrier, toluene as the eluent. The structure of product is verified by IR and 1H NMR.For further purification of the product, combined with HPLC separation technology, get 99.5% purity of [60] PCBM. Through the by-products and the recycling of C60 back into synthetic system, inhibit by-products of new generation, make fresh C60 transformation to [60] PCBM to yield of 93.3%. These technology lay the foundation for high purity [60] PCBM costing reduction.

Key words: preparation, synthesis, purification, PCBM, HPLC

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