Study on Inspection of Synthetic Reaction for Preparation of N-(phosphonomethyl) iminodiacetic Acid with Iminodiacetic Acid by Precolumn Derivatization-HPLC

The derivatives of the reaction liquid for synthesizing N-（phosphonomethyl） iminodiacetic acid （PMIDA） were synthesized with 9-fluorenyl methyl chlomformate （FMOC-C1） as the derivatization reagent. The separation of the derivatives was performed on a Gemini C18 column at room temperature by isocratic elution. The mobile phase was composed of 60% 0.05 M Nail2 PO4 （pH = 3.5） and 40% CH3 CN at a flow rate of 1 ml/min. The injection volume was 10 td, and the detection wavelength was 265 nm. The linear ranges of the derivatives of iminodiacetonitrile, iminodiacetic acid （IDA） and ammonia were, respectively, 0.02-1.2, 0.02-1.2 and 0.1 -2. 0 mg/ml with correlation coefficients not smaller than 0. 999 8. The detection limits for the derivatives were, respectively, 0. 000 4, 0. 000 4 and 0.003 mg/ml. The average recoveries of 3 derivatives were respectively 99.96%, 99. 86% and 99.89%, respectively, with relative standard deviation values not smaller than 1.6%. The method developed in the present paper could be used for monitoring the reaction system for preparation of PMIDA by IDA.

双甘膦和草甘膦及副产物的高效液相色谱分析

利用高效液相色谱法,在Hpersil SAX色谱柱上对草甘膦、双甘膦及主要副产物采用外标法进行定性定量分析,流动相为含0.01mol/L磷酸二氢钾溶液,用磷酸(85%)调节pH值2.1,流速为1.0mL/min,柱温为26℃,紫外检测波长为200nm。结果表明:草甘膦、双甘膦及氨甲基磷酸的线性相关系数分别为0.9999、0.9994、0.99965,标准偏差分别为0.083%、0.089%、0.028%,相对标准偏差分别为0.142%、0.313%、2.57%。

草甘膦活性炭催化剂的失活与碱再生研究

[方法]通过反应底物模拟吸附实验和BET表征方法,对双甘膦催化氧化制备草甘膦活性炭催化剂的失活原因与碱再生方法进行了研究。[结果]实验得出催化剂失活的原因为催化剂吸附的双甘膦等物质造成微孔比表面积和微孔孔容积的减小,从而使催化剂的活性下降。[结论]根据失活机理,采用NaOH溶液对失活催化剂进行了再生,实验结果表明:反应温度为180℃、碱炭质量比为1∶10、处理时间为90 min时,催化剂的再生效率可达52.0%。