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磷酸锆是一种耐高温耐辐射的无机离子交换剂,本工作找到了较好的磷酸锆制备条件。ZrOCl_2·8H_2O与H_3PO_4的克分子比为3.84。ZrOCl_2·8H_2O的浓度为40克/升,磷酸浓度为含PO_4≡80克/升,在1N HCl溶液中沉淀得到离子交换剂。中性溶液中总交换容量~4毫克当量/克干交换剂。第一次再生总交换容量降低10—15%,以后再生就不会降低。锆与磷酸的比例在1:3到1:5之间,总交换容量较高。制备时盐酸浓度与总交换容量无关。磷酸浓度最好为60—80克/升。沉淀应洗至pH=3。在60℃烘干,烘干温度不可太高。随着锆与磷酸比例变大时产品的粒度变细。磷酸锆能耐6N HCl的腐蚀,但在在0.1N NaOH中会遭破坏。络合能力较强的络合剂如乙二胺四乙酸二钠、草酸、酒石酸鲫钠对它有显著破坏作用。由pH滴定曲线证明为多元弱酸型离子交换剂。差热分析证明在130°—260℃有脱水现象。X射线粉末法分析说明基本上属无定形;但制备条件改变可得到不完整晶形;高温处理后均变为无定形。结构可能是-[(Zr-O)_x-(P-O)_y]-(其中x与y为可变数)结成网状,在锆与磷上连有活性基团-OH,其中的氢离子可进行交换。磷酸锆离子交换剂在最初半小时内能交换总交换容量的60%,以后却进行得非常缓慢。对U-Ux_1及Fe_~(+++)-Ni~(++)离子对的分离较好,而对Ca~(++)-Mg~(++)、Th~(+4)-Ce~(+3)、Th~(+4)-Sm~(+3)能进行交换,但由于淋洗条件尚未选择好,未能达到彼此分离。
Zirconium phosphate is a high temperature resistant inorganic ion exchangers, the work to find a better preparation conditions of zirconium phosphate. The molar ratio of ZrOCl 2 · 8H 2 O to H 3 PO 4 was 3.84. The concentration of ZrOCl 2 · 8H 2 O was 40 g / L, and the concentration of phosphoric acid was PO 4 ≡ 80 g / L. The ion exchanger was precipitated in 1N HCl solution. Total exchange capacity in neutral solution ~ 4 meq / g dry exchanger. The first exchange of renewable exchange capacity reduced by 10-15%, after the regeneration will not be reduced. The ratio of zirconium to phosphoric acid is between 1: 3 and 1: 5 and the total exchange capacity is higher. Preparation of hydrochloric acid concentration and the total exchange capacity has nothing to do. The concentration of phosphoric acid is preferably from 60 to 80 g / l. The precipitate should be washed to pH = 3. Drying at 60 ℃, the drying temperature can not be too high. As the ratio of zirconium to phosphoric becomes larger, the particle size of the product becomes smaller. Zirconium phosphate is resistant to corrosion by 6N HCl but is destroyed in 0.1N NaOH. Complexing ability of complexing agents such as disodium ethylenediaminetetraacetate, oxalic acid, crucian carp Carassius auratus have a significant role in the destruction. The pH titration curve proved to be a multi-weak acid-type ion exchanger. Differential thermal analysis showed dehydration at 130 ° -260 ° C. X-ray powder analysis shows that basically amorphous; but the preparation conditions can be obtained incomplete crystal form; after high-temperature treatment have become amorphous. The structure may be - [(Zr-O) _x- (PO) _y] - (where x and y are variable numbers) to form a network with an active group -OH attached to zirconium and phosphorus, Exchange. Zirconium phosphate ion exchangers can exchange 60% of the total exchange capacity in the first half-hour and then proceed very slowly. The separation of U ~ Ux_1 and Fe_ ~ (+++) - Ni ~ (++) ion pairs was good, while the Ca ~ (++) - Mg ~ (++), Th ~ (+4) -Ce ~ (+3), Th ~ (+4) -Sm ~ (+3) can be exchanged, but because the elution conditions have not been selected, they can not be separated from each other.