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用改进的方法合成了对甲苯磺酰肼基二硫代甲酸钾(化合物1).以它作模型化合物,在酸性条件下加热分解,放出二硫化碳,被二乙胺及醋酸铜的混合液吸收,生成黄色荒氨酸铜,在430nm波长比色,从而建立了定量测定磺酰肼基二硫代甲酸基团的方法.并首次合成了苯磺酰肼基二硫代甲酸钾(化合物2)和对甲苯磺酰肼基二硫代甲酸三乙胺盐(化合物3)的纯品,与化合物1—起作标样,用外标法对测定方法进行了验证.测得二硫化碳回收率为99.2—100.5%,相对标准偏差≤2.0%.以此方法测定了用交联度和颗粒度不同的两种聚苯乙烯白球在相同条件下合成的聚苯乙烯磺酰肼基二硫代甲酸盐树脂的功能化程度,分别为1.62mmol·g~(-1)及1.29mmol·g~(-1).
A p-toluenesulfonylhydrazidyl dithioformate (compound 1) was synthesized by a modified method. It was used as a model compound and was decomposed by heating under acidic conditions to release carbon disulfide which was absorbed by a mixture of diethylamine and copper acetate. A yellow diorganic acid copper was synthesized and characterized at 430 nm wavelength to establish a method for the quantitative determination of sulfonylhydrazino dithiocarbamate groups. The synthesis of potassium benzenesulfonylhydrazidyl dithioformate (compound 2) and The tosylate hydrazinium dithioformate triethylamine salt (compound 3) of the pure product, with the compound 1 as a standard sample, the external standard method was used to test the determination of the measured carbon disulfide recovery of 99.2- 100.5%, the relative standard deviation was less than or equal to 2.0% .This method was used to determine the polystyrene sulfonylhydrazin dithiocarbamate resin synthesized under the same conditions with two kinds of polystyrene white balls with different degrees of crosslinking and particle size The degree of functionalization was 1.62 mmol · g -1 and 1.29 mmol · g -1, respectively.