Synthesis and purification of [60] PCBM

doi:10.11949/j.issn.0438-1157.20151495

Abstract

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

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

CLC Number:

O625.52

HU Hongchao, CUI Yingde. Synthesis and purification of [60] PCBM[J]. CIESC Journal, 2015, 66(S2): 461-465.

胡洪超, 崔英德. [60]PCBM的合成及纯化工艺[J]. 化工学报, 2015, 66(S2): 461-465.

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