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有机硅废触体的综合利用
冯亮
学位类型硕士
导师高林
2014-05-28
学位授予单位中国科学院大学
学位授予地点北京
学位专业有机化学
关键词有机硅废触体 氯化铜 硅粉 氧化铜 氧化亚铜
摘要

合成有机硅单体时随着反应的进行硅粉和铜催化剂形成的触体活性降低,需要排出的未反应的硅粉和废催化剂的混合物称为有机硅废触体。由于Rochow反应合成有机硅单体生产技术的发明,促进了有机硅工业的快速发展,同时也产生了大量的有机硅废触体。为有效回收利用这些资源和防止污染环境,我们利用氧化酸浸法对有机硅废触体进行处理。首先采用1mol/L的盐酸和质量分数为27%的双氧水对10g废触体中的催化剂氧化成二价铜再酸溶解得到氯化铜盐,通过正交实验法测定各因素的最佳用量:双氧水用量为2mL,盐酸用量为11mL,反应时间3h,溶液总量为30mL,以及各因素对实验影响大小的顺序为:双氧水的量>溶液总量>盐酸的量>时间。铜盐回收率达98%。利用各物质密度的不同用钨酸钠配制密度为1.30g/mL的重液除去碳粉等杂质得到纯度为99%的高纯硅粉。再利用所回收的铜盐采用沉淀法制备了纳米氧化铜和纳米氧化亚铜等不同类型的铜催化剂,通过X射线衍射仪,扫描电镜,红外,比表面积分析仪,热重分析对其结构和形貌进行表征。然后将纳米氧化铜和纳米氧化亚铜分别用于纳米氧化铜对双氧水的分解和纳米氧化亚铜对甲基橙的光解,催化性能与商业铜催化剂和商业铜氧化物进行比较。催化结果表明,回收铜盐和商业铜盐制备的纳米氧化铜对双氧水催化分解的效果明显优于商业氧化铜;回收铜盐和商业铜盐制备的纳米氧化亚铜对甲基橙光解的效率也远远高于商业氧化亚铜。

其他摘要
The spent silicon contact mass is the mixture of unreacted silicon powder and spent catalyst, as the activity of contact is reduced when the reaction proceeds. Since the reaction of Rochow that synthesize the organic silicon monomer, so the silicone industry can be rapidly developed, at the same time, large amounts of spent silicon contact mass was produced. For the effective recycling of resources and prevention of environmental pollution, we use the method of acid leaching to handle the spent silicon contact mass. Firstly, 10g spent silicon contact mass was oxidized by 27ω% H2O2 and acid leached by 1mol/L HCl to the obtain CuCl2 from the Cu catalyst. The optimum reaction situations (H2O2 : 2mL, HCl : 11mL, reaction time : 3h, total volume of the solution : 30mL) were determined by the orthogonal experimental method .The best order of each factor for the experimental impact are as follows: Volume of H2O2, Total volume of the solution, Volume of HCl, Reaction time. 98% of the copper were recycled to prepare the related catalyst. Finally the carbon was removed by sodium tungstate solution (density 1.30g/mL) to get high-purity silicon (99%) according to the different density of different substance. And then, we prepared nano-CuO and nano-Cu2O by the recovered copper chloride, and characterized the structure and morphology of copper oxide nanoparticles and cuprous oxide nanoparticles by XRD, SEM, BET, TGA,IR. The catalytic effect of CuO was measured by Hydrogen peroxide decomposition rate and the catalytic effect of Cu2O measured by Photocatalytic decomposition of methyl orange, the catalytic effect compared with commercial CuO and CuO prepared by commercial CuCl2, as the same of Cu2O. The results show that the catalytic effect of CuO prepared by recycled CuCl2 and CuO prepared by commercial CuCl2 is the same, and their catalytic effect were far superior to the CuO. The catalytic effect of Cu2O is all so like that.
文献类型学位论文
条目标识符http://ir.xjipc.cas.cn/handle/365002/3422
专题资源化学研究室
作者单位中国科学院新疆理化技术研究所
推荐引用方式
GB/T 7714
冯亮. 有机硅废触体的综合利用[D]. 北京. 中国科学院大学,2014.
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