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以氯化钾和四氯化铪为原料,通过气-固反应直接制备出了氯铪酸钾。首先考察了氯化钾与四氯化铪混合同一坩埚内加热及分别放入不同的坩埚加热两种加料方式对产物的影响,结果表明采取后一种加料方式反应较充分;之后分析原料配比、反应温度及时间对产物的影响,并对得到的产物进行XRD、EDS及SEM分析。XRD结果表明,产物为氯铪酸钾,由EDS分析可知,产物中钾原子与铪原子的摩尔比为2.11(nK:nHf=2.11),与纯氯铪酸钾中钾与铪的摩尔比2:1接近,说明产物中大部分为氯铪酸钾。制备氯铪酸钾较理想的反应条件为:采用分开放料的加料方式,氯化钾与四氯化铪的质量比为1:2,反应温度为450℃,反应时间为3 h。
With potassium chloride and hafnium tetrachloride as raw materials, potassium hafnate is prepared directly by gas-solid reaction. First of all, the effects of heating with potassium chloride and hafnium tetrachloride in the same crucible and heating in two different crucibles separately on the products were investigated. The results showed that the reaction of one feeding method was more adequate after that. After that, , The reaction temperature and time on the product, and the product obtained by XRD, EDS and SEM analysis. The results of XRD showed that the product was potassium chlorochromate. The EDS showed that the molar ratio of potassium to hafnium in the product was 2.11 (nK: nHf = 2.11), and the molar ratio of potassium to hafnium in pure potassium chlorochromate was 2 : 1 close, indicating that most of the product is potassium chlorite hafnate. The optimum reaction conditions for the preparation of potassium hafnate are as follows: the mass ratio of potassium chloride to hafnium tetrachloride is 1: 2, the reaction temperature is 450 ℃ and the reaction time is 3 h.