氯化法制备高纯材料  

High Purity Materials Were Prepared by Chloride Method

作　　者：曾小东 徐成 胡丹 Zeng Xiaodong;Xu Cheng;Hu Dan(National Research Center of Rare Metals Engineering Technology,First Rare Materials Co.,Ltd.,Qingyuan 511517;Vital Microelectronics Technology Co.,Ltd.,Qingyuan 511517,China)

机构地区：[1]国家稀散金属工程技术研究中心广东先导稀材股份有限公司,广东清远511517 [2]广东先导微电子科技有限公司,广东清远511517

出　　处：《广东化工》2022年第22期279-282,共4页Guangdong Chemical Industry

摘　　要：氯化法制备高纯材料,可以分为几类,一类是直接生成高纯的氯化物材料,这一类包含有四氯化锡,三氯化镓,三氯化铟,四氯化碲,四氯化铪等;另一类是生成的氯化物经过提纯,再经过氢化还原生成高纯单质,这里包含有高纯砷,高纯锑,高纯磷等[1]。还有氯化后经过水解生成高纯的氧化物,比如氧化锗,氧化钛等。氯化法制备高纯材料中水、氯的影响不容忽视,其中氯化法制备高纯砷、高纯锑等高纯金属具有较好的适应性,氯气与粗砷等原料生产对应氯化物,由于氯气及环境中存在水汽,氯气在相应氯化物中的溶解较大,导致氯化物中的水、游离氯含量较高[2]。本文讨论了用浓硫酸及酸洗干燥剂对氯化物的除水效果以及游离氯的去除及再利用。氯化法对材料也有特殊的要求,在采用砷与氯气反应生产三氯化砷,精馏三氯化砷后进行还原制备的高纯砷的过程中,由于三氯化砷的强腐蚀性,以及超高纯砷的纯度的要求。本文讨论了砷和氯气的反应釜、三氯化砷的蒸馏精馏装置、三氯化砷的氢化还原装置、高纯砷的研磨破碎工具的材质选择及优缺点[3-4]。The preparation of high purity materials by chloride method can be divided into several categories.One is the direct generation of high purity chloride materials,which includes tin tetrachloride,gallium trichloride,indium trichloride,tellurium tetrachloride,hafnium tetrachloride,etc.The other kind of chloride is generated after purification,and then through hydrogenation reduction to generate high purity elemental,which contains high purity arsenic,high purity antimony,high purity phosphorus and so on.There are also chlorination after hydrolysis to generate high purity oxides,such as germanium oxide,titanium oxide and so on.Chlorination process of preparation of high purity water in the material,the influence of chlorine should not be ignored,the chlorination process of preparation of high purity,high purity antimony,arsenic,high purity metal has good adaptability,chlorine gas and crude arsenic corresponding chloride,such as raw material to produce because of chlorine gas and moisture environment,chlorine gas dissolved in the corresponding chloride is bigger,lead to chloride in water,free chlorine content is higher.This paper discusses the dewatering effect of concentrated sulfuric acid and acid pickling desiccant on chloride and the removal and reuse of free chlorine.The chlorination method also has special requirements on the material,in the use of arsenic and chlorine reaction production of arsenic trichloride,and then rectification of arsenic trichloride after reduction of high purity arsenic preparation,because of the strong corrosion of arsenic trichloride,as well as the purity of ultra-high purity arsenic requirements.In this paper,the material selection and advantages and disadvantages of the reaction kettle for arsenic and chlorine gas,distillation distillation unit for arsenic trichloride,hydrogenation reduction unit for arsenic trichloride,grinding and crushing tool for high purity arsenic are discussed.

关 键 词：氯化物 高纯材料 除氯、除水 耐腐材料 

分 类 号：TQ[化学工程]