聚甲氧基二甲醚缩合产物的气相色谱分析  

MEASUREMENT OF POLYOXYMETHYLENE DIMETHYL ETHERS PRODUCTS COMPOSITION BY GAS CHROMATOGRAPHY

作　　者：梁琳琳[1,2] 雷骞 邓聪迩[1,2] 陈洪林 Liang Linlin;Lei Qian;Deng Conger;Chen Honglin(Chengdu Organic Chemicals Co.,Ltd.,Chinese Academy of Sciences,Chengdu 610041;Chengdu Zhongke Catalysis Technology Co.,Ltd.)

机构地区：[1]中国科学院成都有机化学有限公司,成都610041 [2]成都中科凯特科技有限公司

出　　处：《石油炼制与化工》2022年第3期104-109,共6页Petroleum Processing and Petrochemicals

基　　金：国家重点研发计划项目(2018YFB0604900)。

摘　　要：建立了一种采用气相色谱测定聚甲氧基二甲醚(PODE)缩合产物组成的分析方法,以乙二醇二乙醚(EGDE)为内标物测定了甲醇、甲酸甲酯、三聚甲醛及PODE_(n)(n≤3)的相对质量校正因子;以甲缩醛、PODE_(2)和PODE_(3)为基准物,通过外推法计算得到PODE_(4~10)各组分的相对质量校正因子;根据有效碳数法计算了聚甲氧基半缩醛(HF_(n))的相对质量校正因子。精密度与加标回收试验结果表明,甲醇、甲酸甲酯、三聚甲醛、甲缩醛、PODE_(2)和PODE_(3)重复测定的相对标准偏差均小于2%,加标回收率在99%~104%之间,满足不同含水量原料合成PODE的产物组成定量分析要求。A gas chromatography method for determination of polyoxymethylene dimethyl ethers products composition was developed.The relative mass correction factors of methanol(MeOH),methyl formate(MF),trioxane(TOX)and polyoxymethylene dimethyl ethers(PODE_(n),n≤3)were determined by using ethylene glycol diethyl ether as internal standard.From dimethoxymethane(DMM),PODE_(2) and PODE_(3) used as primary standard materials,the relative mass correction factors of PODE_(4~10) components were extrapolated.The relative mass correction factors of hemiacetal(HF_(n))were calculated by effective carbon number method.The results of precision and recovery showed that the relative standard deviations were less than 2.0%,and the recovery rate ranged between 99%-104%,which could meet the requirements of the quantitative analysis for polyoxymethylene dimethyl ethers product from different water content of raw materials.

关 键 词：聚甲氧基二甲醚 气相色谱法 聚甲氧基半缩醛 定量分析 

分 类 号：O657.71[理学—分析化学] TQ317.2[理学—化学]