【作者】 郭丽芬；

【导师】 张广立；

【作者基本信息】 东北大学 ， 冶金物理化学， 2005， 硕士

【摘要】 关于超细无定形硼粉的制备,实验室已经找出了最佳镁热还原工艺和湿法酸浸工艺,并且所得硼粉的主要技术指标达到了美军标SB Boron92标准。本论文主要是深入探讨小型酸浸工艺,并在此基础上进行工业试验研究,逐步将工艺推向生产,实现工业化。 通过对酸浸过程的动力学分析,根据计算的浸出反应的活化能值,综合考虑中试生产实际操作条件和浸出溶剂盐酸的挥发程度,不论是小试还是工业试验,浸出过程的温度以80℃为宜。浸出过程处于扩散区,扩散为控制步骤,强化过程的方法是加强搅拌以提高液流的速度和增大紊流程度,磨细被浸出物料。 本论文前期工作主要是对小型酸浸实验进行更详细深入地分析,探索生产不同品位硼粉的操作规程。分析结果表明,不同酸浸步骤可以得到不同品位的硼粉:一次酸浸B%=25.16%,二次酸浸B%=39.62%,三次酸浸B%=70.63%,四次酸浸B%=87.83%,五次酸浸B%=90.11%,六次酸浸B%=90.25%,最终产品B%=91.31%,根据市场不同的需求可以控制酸浸步骤,选取适当的酸浸工艺进行生产后期工作是进行中试试验研究。研究主要分两个阶段,一是分析中试生产中采用原酸浸工艺进行生产时B₂O₃和MgO的浸出率;第二阶段针对工厂实际生产的经济成本和收益、环境治理和综合利用以及生产中出现的过氧化氢不溶物含量超标等新问题,进行酸浸工艺的不断改进,通过试验得出可行的改进酸浸工艺为:先进行三次温度为80℃的热水洗,接着进行六次酸浸,然后进行一定次数的蒸馏水洗涤,最后在真空干燥箱中烘干,烘干温度60℃左右,时间为4-5小时,得到产物无定形硼粉。中试生产中环保治理和综合利用方面采取如下措施:酸浸设备为机械密封,减少盐酸的挥发损失;每一步酸浸、水洗后均及时对B₂O₃、MgCl₂进行回收,B₂O₃采用冷却结晶法回收,MgCl₂采用余热蒸发结晶法回收;生产中采用全流程闭路循环。 在生产过程中,出现了硼粉品位低的现象,总硼含量仅为88%,影更多还原

【Abstract】 Ultra fine amorphous boron powder has been prepared by a series of integrated methods including heating reduction with Magnesium and acid dissolution. Its main technologic standards have reached U.S.A. SB Boron 92（MIL-B-S1092）. At present, the task is realizing industrialization of acid soaking technology through putting industrial test into practice.The value of activation energy was obtained through kinetic calculation and analysis of acid soaking process. Considering activation energy, the operating conditions of industrialization and volatilization of hydrochloric acid, 80℃ was selected as the best temperature. As results, the controlling step is proliferation and the methods of strengthening this process are speeding up stirring or grinding reactants.The earlier task was seeking the operating instructions. It was found boron powder with different purity can be prepared by different acid dissolution step: content of boron is 25.16% under the first acid soaking phase, 39.62% under the second, 70.63% under the third, 87.83% under the forth, 90.11% under the fifth, 90.25% under the sixth and the final purity of production is 91.31%. These can meet all kinds of requires of markets. The next assignment was the study of industrial test. In these periods, considering the production cost, economic benefit, environmental protection, comprehensive utilization and other new problems such as the worse content of insoluble in H₂O₂ etc, the improved acid dissolution technology was achieved: first, three times hot water soaking at 80 ℃; second, six times hydrochloric acid soaking; third, several times distilled更多还原