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Preparation and characterization of 10B boric acid with high purity for nuclear industry

机译:核工业用高纯度10B硼酸的制备与表征

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摘要

Boric acid is often added into coolant as neutron capture agent for pressurized water reactor, whose amount is influenced by its abundance and purity. Therefore, the preparation of enriched 10B boric acid with high purity is beneficial to nuclear industry. 10B is also used in developing tumor-specific boronated drugs in boron neutron capture therapy. The boronated drug can be administered to patient intravenously, intratumorally, or deposited at tumor site in surgical excision. Thus, enriched 10B boric acid is of practical significance in the field of medicine. Self-made boron trifluoride–methanol-complex solution was selected as one of the experimental reagents, and the preparation of 10B acid was realized by one-step reaction for the complexes with water and calcium chloride. The determination of electrical conductivity in reaction process proves that the optimum reaction time was 16–20 h. Furthermore, the effect of reaction time, ratio of calcium chloride to complex as well as the amount of water on the purity and yield of boric acid was investigated. Finally, the optimum reaction time was 20 h, the optimal solid–liquid ratio (molar ratio) was 3:1, and the amount of water was 1 L of deionized water for each mol of the complex. H2O2 was added in the reaction process to remove Fe2+. After recrystallization, IR spectra of 10B boric acid was measured and compared with standard to verify the product of boric acid. The feasibility of the preparation method was determined by the detection of XRD of boric acid. To observe the morphology by polarizing microscope, crystal structure was obtained. The purity of the final product is 99.95 %, and the yield is 96.47 %. The ion concentration of boric acid accords with the national standard of high purity, which was determined by ICP.
机译:硼酸通常作为中子俘获剂添加到冷却剂中,用于压水堆,其量受其丰度和纯度影响。因此,制备高纯度的富集 10 B硼酸对核工业有利。 10 B还用于在硼中子捕获疗法中开发肿瘤特异性的含硼药物。含硼的药物可以静脉内,肿瘤内或手术切除后沉积在肿瘤部位。因此,富集的 10 硼酸在医学领域具有实际意义。选择自制的三氟化硼-甲醇配合物溶液作为实验试剂之一,通过与水和氯化钙的配合物一步反应实现了 10 B酸的制备。反应过程中电导率的确定证明最佳反应时间为16–20 h。此外,研究了反应时间,氯化钙与配合物的比例以及水的量对硼酸纯度和产率的影响。最后,最佳反应时间为20小时,最佳固液比(摩尔比)为3:1,每摩尔配合物的水量为1 L去离子水。反应过程中加入H2O2去除Fe 2 + 。重结晶后,测量 10 B硼酸的红外光谱,并与标准品进行比较,以验证硼酸的产物。通过检测硼酸的XRD确定了该制备方法的可行性。为了通过偏光显微镜观察形态,获得了晶体结构。最终产品的纯度为99.95%,产率为96.47%。硼酸的离子浓度符合ICP测定的高纯度国家标准。

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