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Materials Engineering

Synthesis of magnesium oxysulfate whiskers from bittern and post-sequence separation process

  • Xue BAI Hongfei GUO Xueqing CHEN Bin ZHAO Jilin CAO
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  • 1. College of Chemical Engineering and Technology, Hebei University of Technology, Tianjin 300130, China 2. Hebei Provincial Key Lab of Green Chemical Technology and High Efficient Energy Saving, Tianjin 300130, China

Received date: 2018-12-10

  Revised date: 2019-01-11

  Online published: 2019-08-15

Abstract

Based on the comprehensive utilization of bittern resources, the synthesis of magnesium oxysulfate whiskers from bittern and the separation of potassium salt and sodium salt in the subsequent process were studied. Magnesium oxysulfate whiskers were synthesized by hydrothermal reaction of bittern with NaOH. The effects of raw material ratio, reaction temperature, concentration of liquid alkali and reaction time on liquid phase composition and product morphology were investigated. The products were characterized by XRD and SEM. The optimum conditions were determined as follows: the raw material molar ratio of Mg2+ to OH? was 1:1.5, the concentration of liquid alkali was 4 mol/L, the reaction temperature was 200℃ and the reaction time was 7 h. The Mg2+ in the mother liquid was completely converted into magnesium hydroxide crystals with the theoretical molar ratio of Mg2+ to OH? of 1:2. According to the phase diagrams of Na+, K+//Cl?, SO42??H2O system at 0 and 25℃ and NaCl?KCl?H2O ternary system at 25 and 100℃, NaCl, Na2SO4?10H2O and KCl were separated from the remaining mother liquor by evaporation concentration crystallization and freezing crystallization.

Cite this article

Xue BAI Hongfei GUO Xueqing CHEN Bin ZHAO Jilin CAO . Synthesis of magnesium oxysulfate whiskers from bittern and post-sequence separation process[J]. The Chinese Journal of Process Engineering, 2019 , 19(4) : 817 -825 . DOI: 10.12034/j.issn.1009-606X.218328

References

[1]袁俊生, 吴举, 邓会宁, 等.中国海盐苦卤综合利用技术的开发进展[J].盐业与化工, 2006, 35(4):33-37 [2]Yuan J S, Ju W U, Deng H N, et al.Evolution of Development of Technologies for Bittern Utilization in China[J].Journal of Salt and Chemical Industry, 2006, 35(4):33-37 [3]Ding Y, Zhao H, Sun Y, et al.Superstructured magnesium hydroxide sulfate hydrate fibres Photoluminescence study[J].Int. J. Inorg. Mater., 2001, 3(2):151-156 [4]Zhao W, Gao C, Wang T, et al.Effect of alcohols additives on hydrothermal formation of magnesium hydroxide sulfate hydrate whiskers[J].Cryst. Res. Technol., 2015, 50(8):676-681 [5]Liu B, Zhang Y, Wan C, et al.Thermal stability,flame retardancy and rheological behavior of ABS filled with magnesium hydroxide sulfate hydrate whisker[J].Polym. Bull., 2007, 58(4):747-755 [6]Kim E S, Ye C K, Park J, et al.Mechanical properties and flame retardancy of surface modified magnesium oxysulfate (5Mg(OH)2 ·MgSO4·3H2O) whisker for polypropylene composites[J].J. Materiom., 2018, 4(2):149-156 [7]王路明.料浆沉降过滤性能的改善[J].海湖盐与工业, 2002, 31(6):22-25 [8]Wang L M.Improvement of performance of Sedimentation Filtration of Mg(OH)2 Slurry[J].Sea-lake Salt and Chemical Industry, 2002, 31(6):22-25 [9]韩利华, 芮玉兰, 梁英华, 等.苦卤提镁制备氢氧化镁工业中的问题与对策[J].无机盐工业, 2006, 38(1):32-34 [10]Han L H, Rui Y L, Liang Y H, et al.Problems and solving measures for the preparation of magnesium hydroxide from brine[J].Inorganic Chemicals Industry, 2006, 38(1):32-34 [11]Alamdari A.Rahimpour M R,Esfandiari N,et alKinetics of magnesium hydroxide precipitation from sea bittern[J].Chem. Eng. Process., 2008, 47(2):215-221 [12]Chen X L, Yu J, Guo S Y, et al.Surface modification of magnesium hydroxide and its application in flame retardant polypropylene composites[J].J. Mater. Sci., 2009, 44(5):1324-1332 [13]Wu J M, Hong Y, Zhang X H, et al.Magnesium hydroxide nanoparticles synthesized in water-in-oil microemulsions[J].J. Colloid Interf. Sci., 2008, 324(1):167-171 [14]Wang M, Zeng X F, Chen J Y, et al.Magnesium hydroxide nanodispersion for polypropylene nanocomposites with high transparency and excellent fire-retardant properties Polym. Degrad. Stabil.,2017,146: 327-333.[J].Polymer Degradation and Stability, 2017, 146(0):327-333 [15]胡晓瑜, 韩充, 朱晓龙, 等.氢氧化镁晶须制备表征及改性研究[J].无机盐工业, 2013, 45(9):15-17 [16]Hu X Y, Han C, ?Zhu X L, et al.Preparation,characterization,and modification of magnesium hydroxide whiskers[J].Inorganic Chemicals Industry, 2013, 45(9):15-17 [17]郭淑元, 张雨山, 黄西平, 等.碱式硫酸镁晶须的制备[J].化学工业与工程, 2011, 28(2):35-39 [18]Guo S Y, Zhang Y S, Huang X P, et al.Preparation of Basic Magnesium Sulfate Whisker[J].Chemical Industry and Engineering, 2011, 28(2):35-39 [19]吴建松, 黄雪清, 邓国丽, 等.徐闻盐场苦卤制备碱式硫酸镁晶须[J].无机盐工业, 2015, 47(12):53-55 [20]Wu J S, Huang X Q, Deng G L, et al.Preparation of oxysulfate magnesium whiskers from brine in Xuwen salt field[J].Inorganic Chemicals Industry, 2015, 47(12):53-55 [21]张琳娜, 刘有智, 焦纬洲, 等.卤水提溴技术的发展与研究现状[J].盐湖研究, 2009, 17(1):68-72 [22]Zhang L N, Liu Y Z, Jiao W Z, et al.Development and research status of bromine extracting technology from the brine[J].Journal of Salt Lake Research, 2009, 17(1):68-72 [23]刘峰, 向兰, 金涌.水热法制备碱式硫酸镁晶须的过程机制[J].无机材料学报, 2004, 19(4):784-788 [24]Liu F, Xiang L, Jin Y.Hydrothermal Synthesis Process of Magnesium Oxysulfate Whiskers[J].Journal of Inorganic Materials, 2004, 19(4):784-788 [25]高传慧, 许军, 王传兴, 等.碱式硫酸镁晶须的一步法水热合成及生长机理[J].硅酸盐学报, 2011, 39(5):773-778 [26]Gao C H, Xu J, Wang C X, et al.Hydrothermal Synthesis and Growth Mechanism of Magnesium Hydroxide Sulfate Hydrate Whiskers by the One-Step Procedure[J].Journal of the Chinese Ceramic Society, 2011, 39(5):773-778 [27]Kang K H, Lee D K.Synthesis of magnesium oxysulfate whiskers using triethanolamine as a morphology control agent[J].J. Ind. Eng. Chem., 2014, 20(4):2580-2583 [28]Xiang L, Liu F, Li J, et al.Hydrothermal formation and characterization of magnesium oxysulfate whiskers[J].Mater. Chem. Phys., 2004, 87(2):424-429 [29]Gao C H, Ding L, Wu Y M, et al.Low-Cost Synthesis and Morphology Control of Magnesium Oxysulfate Hydrate Whiskers[J].Advanced Materials Research, 2014, 936(0):986-991 [30]朱黎霞, 岳涛, 高世扬, 等.的水热合成及反应时间对其形貌的影响英文[J].无机化学学报, 2003, 19(1):99-102 [31]Zhu L X, Yue T, Gao S Y, et al.Hydrothermal synthesis and the effect of reaction time on morphology of MgSO4·5Mg(OH)·3H2O[J].Chinese Journal of Inorganic Chemistry, 2003, 19(1):99-102 [32]Ding Y, Zhang G T, Wu H, et al.Nanoscale Magnesium Hydroxide and Magnesium Oxide Powders:? Control over Size,Shape,and Structure via Hydrothermal Synthesis[J].Chemistry of Materials, 2001, 13(2):435-440 [33]李艳丽, 彭建平, 倪平, 等.晶种和絮凝剂对氢氧化镁沉降的影响[J].无机盐工业, 2008, 40(11):26-27 [34]Li Y L, Peng J P, Ni P, et al.Effect of adding seed crystal and flocculant on magnesium hydrate deposition[J].Inorganic Chemicals Industry, 2008, 40(11):26-27 [35]Stephen H, ?Stephen T, Solubilities of Inorganic and Organic compounds [M].New York: Pergamon?Press, 1979.
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