聚甲氧基二甲醚缩合产物的气相色谱分析

石油炼制与化工 ›› 2022, Vol. 53 ›› Issue (3): 104-109.

聚甲氧基二甲醚缩合产物的气相色谱分析

梁琳琳^1,2,雷骞^1,2,邓聪迩^1,2,陈洪林^1,2

1. 中国科学院成都有机化学有限公司
2. 成都中科凯特科技有限公司

收稿日期:2021-04-01 修回日期:2021-12-13 出版日期:2022-03-12 发布日期:2022-03-03
通讯作者: 陈洪林 E-mail:hlchen@cioc.ac.cn
基金资助:
国家重点研发计划项目

^,MEASUREMENT OF POLYOXYMETHYLENE DIMETHYL ETHERS PRODUCTS COMPOSITION BY GAS CHROMATOGRAPHY

Received:2021-04-01 Revised:2021-12-13 Online:2022-03-12 Published:2022-03-03
Contact: Hong-Lin Chen E-mail:hlchen@cioc.ac.cn

摘要/Abstract

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、PODE2和PODE3为基准物，通过外推法计算得到PODE4~10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、PODE2和PODE3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。

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

Abstract: 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), PODE2 and PODE3 used as primary standard materials, the relative mass correction factors of PODE4-10 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.

Key words: polyoxymethylene dimethyl ethers, gas chromatography, hemiacetal, quantitative analysis

梁琳琳雷骞邓聪迩陈洪林. 聚甲氧基二甲醚缩合产物的气相色谱分析[J]. 石油炼制与化工, 2022, 53(3): 104-109.

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