结晶法从含氟废水中合成粗颗粒冰晶石
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摘要
以颗粒粒径和含水率为考察指标,研究了结晶法从含氟废水中合成粗颗粒冰晶石的可行性。实验结果表明,在废水氟质量浓度低于4.5 g/L、废水流量为1.3 L/h、结晶反应pH为4.1～6.6、反应温度为45℃条件下,延长晶种停留时间可以有效增大冰晶石的粒径,降低冰晶石含水率,氟回收率稳定在80%左右。采用沉淀与固液分离一体化反应器对氟质量浓度为4.0 g/L的废水进行了连续处理,在废水流量为20 L/h、结晶反应pH为4.0～7.0、反应温度为45℃条件下,合理控制晶种停留时间,依靠停留在反应器底部晶种的作用,可以合成得到含水质量分数低于30%、粒径满足要求的冰晶石产品。
Taking the particle size and water content as indicators,the feasibility for synthesis of big-size cryolite from fluorine-containing wastewater by the crystallization process was studied.The experimental results showed that under the condition that the wastewater fluorine concentration was lower than 4.5 g/L,the wastewater flow rate was 1.3 L/h,the crystallization reaction pH was 4.1 to 6.6 and the reaction temperature was 45 ℃,prolonging the seed residence time was favor for increasing particle size and reducing water content of cryolite,and the fluorine recovery rate was stable at about 80%.The wastewater with a fluorine concentration of 4.0 g/L was treated by a precipitation and solid-liquid separation integrated reactor continuously,under the condition of wastewater flow rate of 20 L/h,crystallization pH of 4.0 to 7.0,reaction temperature of 45 ℃,reasonable control of seed residence time,and depending on the effect of the seed crystals remaining at the bottom of the reactor,it was possible to synthesize cryolite products with low water content(<30%) and particle sizes satisfying the requirements.
Taking the particle size and water content as indicators,the feasibility for synthesis of big-size cryolite from fluorine-containing wastewater by the crystallization process was studied.The experimental results showed that under the condition that the wastewater fluorine concentration was lower than 4.5 g/L,the wastewater flow rate was 1.3 L/h,the crystallization reaction pH was 4.1 to 6.6 and the reaction temperature was 45 ℃,prolonging the seed residence time was favor for increasing particle size and reducing water content of cryolite,and the fluorine recovery rate was stable at about 80%.The wastewater with a fluorine concentration of 4.0 g/L was treated by a precipitation and solid-liquid separation integrated reactor continuously,under the condition of wastewater flow rate of 20 L/h,crystallization pH of 4.0 to 7.0,reaction temperature of 45 ℃,reasonable control of seed residence time,and depending on the effect of the seed crystals remaining at the bottom of the reactor,it was possible to synthesize cryolite products with low water content(<30%) and particle sizes satisfying the requirements.
引文
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[14]Jiang K,Zhou K,Yang Y,et al.A pilot-scale study of cryolite precipitation from high fluoride-containing wastewater in a reactionseparation integrated reactor[J].Journal of Environmental Sciences,2013,25(7):1331-1337.
[15]CJ/T 221-2005城市污水处理厂污泥检验方法[S].
[16]国家环保局《水和废水监测分析方法》编委会.水和废水监测分析方法[M].4版.北京:中国环境科学出版社,2002.
[2]吴海峰,侯利芳.无机氟化工氟资源综合利用发展现状与建议[J].无机盐工业,2011,43(12):9-11.
[3]雷绍民,郭振华.氟污染的危害及含氟废水处理技术研究进展[J].金属矿山,2012(4):152-155.
[4]梁俊,范灵凯.某双氟化工有限公司仓库工程职业病危害控制效果评价[J].中国卫生工程学,2017,16(3):305-307.
[5]曹烨.中国主要化工矿产矿床类型划分方案[J].地质论评,2016,62(增刊):256-258.
[6]Aldaco R,Garea A,Fernández I,et al.Resources reduction in the fluorine industry:fluoride removal and recovery in a fluidized bed crystallizer[J].Clean Technologies and Environmental Policy,2008,10(2):203-210.
[7]刘海霞.氟硅酸综合利用工艺技术研究进展[J].无机盐工业,2017,49(3):9-13.
[8]王春梅,黄小卫,崔大立,等.利用氟铝络合物溶液合成冰晶石的研究[J].稀有金属,2009,33(5):737-741.
[9]刘晓红,章小明,程淑莲,等.回收废液制取冰晶石---废液与氨水反应生成铝、氟复合物[J].轻金属,2011(7):15-18.
[10]茆卫兵.控制合成冰晶石中杂质SiO2含量的研究[J].无机盐工业,1996(5):11-12.
[11]王化章,李治国.砂状冰晶石比常规氟盐在铝电解生产上应用的优势[J].轻金属,1996(9):22-24.
[12]周康根,姜科,杨有才,等.一种沉淀反应与固液分离一体化装置:中国,102657960A[P].2012-09-12.
[13]Jiang K,Zhou K.Recovery of cryolite with high molar ratio from high fluorine-containing wastewater[J].Euro-Mediterranean Journal for Environmental Integration,2017,2(1):22.
[14]Jiang K,Zhou K,Yang Y,et al.A pilot-scale study of cryolite precipitation from high fluoride-containing wastewater in a reactionseparation integrated reactor[J].Journal of Environmental Sciences,2013,25(7):1331-1337.
[15]CJ/T 221-2005城市污水处理厂污泥检验方法[S].
[16]国家环保局《水和废水监测分析方法》编委会.水和废水监测分析方法[M].4版.北京:中国环境科学出版社,2002.