合成二乙烯三胺五甲叉膦酸的质谱分析及其阻垢性能

ES-MS analysis of synthesis products diethylene triamine pentamethylene phosphonic acid and its scale inhibition of sodium salt

采用一锅法以二乙烯三胺、甲醛、亚磷酸为原料在盐酸作催化剂的条件下合成了二乙烯三胺五甲叉膦酸（DETPMP）.对不同反应时间下合成的二乙烯三胺五甲叉膦酸的产物进行了电喷雾质谱分析.通过质谱峰及实验和理论的同位素分析对产物中DETPMP的相对含量进行了分析发现：在二乙烯三胺、甲醛、亚磷酸按照摩尔比1∶10∶5,温度100～105℃,反应时间4 h可得到DETPMP百分含量较高的混合物.用40%的氢氧化钠溶液对反应混合液进行处理得到钠盐（DETPMPS）.研究了不同浓度的DETPMP和DETPMPS对硫酸钙的阻垢性能的影响,结果表明：在含1.51 g/L的钙离子溶液中加入10 mg/L DETPMPS,其阻垢率达到94.55%.

The synthesis of diethylenetriamine pentamethylene phosphonic acid（DETPMP） was carried out by one-pot reaction of diethylene triamine, formaldehyde and phosphorous acid under the catalysis of hydrochloric acid. The synthesized DETPMP products at different reaction times were analyzed by ES-MS mass spectroscopy and isotope analysis. The relative content of DETPMP in the reaction mixture was obtained by analyzing the mass spectra and comparing experimental and theoretical isotope spectra. The optimum conditions for obtaining the products containing more DETPMP molecules are： 1∶10∶5 mole ratio of diethylenetriamine,formaldehyde and phosphorous acid, temperature 100-105 ℃ and reaction time 4 h. And the sodium salt（DETPMPS） of DETPMP was obtained by mixing DETPMP with 40% sodium hydroxide solution. Moreover,the effect of the concentration of the synthesized DETPMPS and DETPMP on the inhibition rate to calcium sulfate was studied. The results show that the inhibition rate of DETPMPS is 94.55% after adding the 10 mg/L DETPMPS in the solution containing calcium 1.51 g / L.