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浙江大学学报(工学版)
J4  2011, Vol. 45 Issue (4): 765-769    DOI: 10.3785/j.issn.1008-973X.2011.04.029
    
Characterization of adductive crystal of terephthalic
acid and N-methyl pyrrolidone
PENG Ge1,2, GUO Xia2, CHENG You-wei2, LI Xi2
1. Chemical Engineering College, Ningbo University of Technology, Ningbo 315016, China;
2. Department of Chemical and Biochemical Engineering, Zhejiang University, Hangzhou 310027, China
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Abstract  

Adductive crystals formed by terephthalic acid (TA) and N-methyl pyrrolidone (NMP) were measured and characterized by using high performance liquid chromatography (HPLC), thermo gravimetric (TG), X-ray diffraction (XRD) and spectrophotometry. The adduct was a crystal consisting of one TA molecule and two NMP molecules tied by O—H…O hydrogen-bond. The crystal was unstable above 50 ℃ at which it is prone to decomposition to disengage the solvent. The computational hydrogen-bonding energy between TA and NMP is -87.8 KJ·mol-1, which can be categorized to the relatively strong hydrogen bond. Results show that the adductive crystallization is an effective separation method of recovering the terephthalic acid residue, by which 97% colored impurities in TA residue can be removed.

Published: 05 May 2011
CLC:  TQ 245.1  
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Cite this article:

PENG Ge, GUO Xia, CHENG You-wei, LI Xi. Characterization of adductive crystal of terephthalic
acid and N-methyl pyrrolidone. J4, 2011, 45(4): 765-769.

URL:

http://www.zjujournals.com/eng/10.3785/j.issn.1008-973X.2011.04.029     OR     http://www.zjujournals.com/eng/Y2011/V45/I4/765


TA与NMP形成的加合物晶体表征

 采用高效液相色谱(HPLC)、热重(TG)、X线衍射(XRD)、分光光度法等方法对溶剂N甲基吡咯烷酮（NMP）与对苯二甲酸（TA）形成的加合物晶体进行表征,所形成的加合物是1个TA分子与2个NMP分子通过O—H…O的氢键作用形成的结晶体,该晶体在50 ℃以上不稳定,易受热分解而脱除溶剂.通过计算得出,TA与NMP之间的氢键键能为-87.8 KJ/mol,属于较强类型的氢键作用.研究表明,加合结晶可以除去TA固体残渣中97%以上的有色杂质,是一种新型的结晶分离方法.

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