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建立了齐格勒-纳塔催化剂中2-羟基苯甲酸乙酯、苯甲酸乙酯、邻苯二甲酸二异丁酯、邻苯二甲酸二丁酯、2-异丙基-2-异戊基-1,3-二甲氧基丙烷、2-氰基-2,3-二异丙基丁二酸二乙酯、2,4-戊二醇二苯甲酸酯和3,5-庚二醇二苯甲酸酯内给电子体的气相色谱-质谱联用分析方法。样品经水分散,乙酸乙酯萃取后,气相色谱-质谱法测定。8种内给电子体化合物含量在1~10 mg/L范围内线性关系良好(R2>0.998),苯甲酸乙酯、邻苯二甲酸二丁酯、邻苯二甲酸二异丁酯检出限(S/N=3)为0.05 g/kg,2-羟基苯甲酸乙酯、2-异丙基-2-异戊基-1,3-二甲氧基丙烷、2-氰基-2,3-二异丙基丁二酸二乙酯、2,4-戊二醇二苯甲酸酯、3,5-庚二醇二苯甲酸酯检出限(S/N=3)为0.1 g/kg;添加水平为5 g/kg的加标回收率为90.2%~120.9%,添加水平为20 g/kg的加标回收率为92.0%~98.8%,相对标准偏差(RSD,n=3)小于11%。方法有效减小催化剂基质的干扰,为齐格勒-纳塔催化剂内给电子体的研发和产品质量控制提供科学数据。
In the Ziegler-Natta catalyst, ethyl 2-hydroxybenzoate, ethyl benzoate, diisobutyl phthalate, dibutyl phthalate, 2-isopropyl-2- 1,3-dimethoxypropane, diethyl 2-cyano-2,3-diisopropylsuccinate, 2,4-pentanediol dibenzoate and 3,5- Analysis of Internal Electron Donor Derivatives of Glycol Dibenzoate by Gas Chromatography - Mass Spectrometry. Samples were water-dispersed, extracted with ethyl acetate and analyzed by gas chromatography-mass spectrometry. The linearity of the 8 internal electron donor compounds was in the range of 1 ~ 10 mg / L (R2> 0.998). The detection limits of ethyl benzoate, dibutyl phthalate and diisobutyl phthalate (S / N = 3) of 0.05 g / kg, ethyl 2-hydroxybenzoate, 2-isopropyl-2-isopentyl-1,3-dimethoxypropane, The detection limit (S / N = 3) of 3-diisopropylsuccinate, 2,4-pentanediol dibenzoate and 3,5-heptanediol dibenzoate were 0.1 The recoveries were 90.2% ~ 120.9% at 5 g / kg and 92.0% ~ 98.8% at 20 g / kg. The relative standard deviations (RSD, n = 3) less than 11%. The method can effectively reduce the interference of the catalyst matrix and provide scientific data for the development and product quality control of the electron donor in the Ziegler-Natta catalyst.