高比表面积黄色氧化钨制备工艺研究

Preparation Technology of Yellow Tungsten Oxide with High Specific Surface Area

以蒸发结晶生产的仲钨酸铵(APT)为原料,采用高温煅烧法制备了催化剂、太阳能电池用的优质原料——高比表面积黄色氧化钨,研究了进料端温度、煅烧温度、炉管转速、给料速度、炉内压力和不同原料对黄色氧化钨比表面积的影响。运用扫描电镜、费氏粒度仪、比表面积仪等检测设备,对黄色氧化钨进行了表征。研究结果表明:采用6带加热氧化钨回转炉,以连续结晶母液再结晶生产的APT为原料,控制进料端温度为580~620℃、出料端温度为620~680℃、炉管转速为2.0~2.2 r/min、进料速度为150~200 kg/h、炉内压力为-100 Pa,可以制取高比表面积的黄色氧化钨。该黄色氧化钨晶体形貌多呈方形和斜方形,晶粒表面更致密,裂纹更少,几乎无晶体团聚现象。

With ammonium paratungstate(APT)produced by evaporation and crystallization as raw material,a high-quality raw material with high specific surface area for catalysts and solar cells was prepared by high-temperature calcination method.The effects of feed end temperature,calcination temperature,furnace tube speed,feeding speed,furnace pressure and different raw materials on the specific surface area of yellow tungsten oxide were studied.The yellow tungsten oxide was characterized by scanning electron microscope,Fischer particle size analyzer and specific surface area meter.The research results show that yellow tungsten oxide with high specific surface area can be prepared by using 6-belt heated tungsten oxide rotary furnace,taking APT produced by recrystallization of continuous crystalli-zation mother liquor as raw material,and controlling feed end temperature of 580-620℃,discharge end temperature of 620-680℃,furnace tube speed of 2.0-2.2 r/min,feed rate of 150-200 kg/h and furnace pressure of‒100 Pa.The morphol-ogy of the yellow tungsten oxide crystal is mostly square and oblique square,and the crystal surface is denser,with fewer cracks and almost no crystal agglomeration.