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作 者:施建奎 宋琴珑 顾克军 SHI Jiankui;SONG Qinlong;GU Kejun(Zhonghua High-Performance Fiber Material Co.,Ltd.,Yangzhou Jiangsu 211400,China)
机构地区:[1]中化高性能纤维材料有限公司,江苏扬州211400
出 处:《石油化工应用》2023年第6期104-106,109,共4页Petrochemical Industry Application
摘 要:固体光气在N,N-二甲基甲酰胺为催化剂的条件下,以间苯二甲酸为原料,一步合成间苯二甲酰氯,考察了反应温度、催化剂用量、间苯二甲酸浓度、固体光气用量对反应的影响。结果表明,以氯化苯为溶剂,间苯二甲酸浓度为50%,固体光气与间苯二甲酸的摩尔比为0.8∶1,反应温度为60℃,DMF用量为间苯二甲酸的10%时,间苯二甲酰氯收率达96.8%,精制后,产品总收率达91.0%,产品纯度可达99.96%。In the presence of solid phosgene in N,N-dimethylformamide as catalyst,isophthalic acid as raw material was used to synthesize isophthalic acid chloride in one step,the reaction temperature,the amount of catalys,isophthalic acid concentration and triphosgene dosage were investigated.The results show that with chlorinated benzene as the solvent,the reaction concentration of isophthalic acid is 50%,the molar ratio of triphosgene to isophthalic acid is 0.8∶1,the reaction temperature is 60℃,the dosage of DMF is 10%of the weight of isophthalic acid,the yield of isophthalyl chloride reaches 96.8%,and after refining,the yield and purity of isophthaloyl chloride was reaches 91.0%and 99.96%,respectively.
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