Preparation of Potassium Borohydride by Reactive Crystallization

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Abstract

As for the existing problems for the production of alkali metal borohydride via Schlesinger method, to illustrate, high costs for the cycle of mother liquor, lower quality for product caused by the accumulation of by-products, preparation of potassium borohydride by reactive crystallization was established to dispose of the crystallization mother liquor from the production and increase the yield for alkali metal borohydride while maintaining moderate economic benefits. Iodometric method from volumetric analysis, optical microscopy, Malvern Mastersizer 3000 and X-ray diffraction were employed to test the influence of various operating conditions on the product. The result shows that controlling the molar ratio between 1.05 and 1.10, reaction temperature 50℃, cooling rate 10℃·h^-1, keeping temperature 0℃, can ensure the product meet the standards of the chemical industry.

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	Articles by authors
	Wang Zelin
	Wang Rijie
	Yang Xiaoxia

Keywords： sodium borohydride； potassium borohydride； reactive crystallization； cooling crystallization

Received 2016-03-16;

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Wang Zelin, Wang Rijie, Yang Xiaoxia.Preparation of Potassium Borohydride by Reactive Crystallization[J] Chemcial Industry and Engineering, 2018,V35(4): 52-57

[1] Schlesinger H I, Brown H C. Methods of preparing alkali metal borohydrides:US, 2534533[P]. 1950-12-19
[2] Banus M D, Gibb T R P. Method of purifying borohydrides of the alkali metals:US, 2542746[P]. 1951-02-20
[3] Martelli P, Caputo R, Remhof A, et al. Stability and decomposition of NaBH₄[J]. Journal of Physical Chemistry C, 2010, 114(15):7173-7177
[4] Minkina V, Shabunya S, Kalinin V, et al. Long-Term stability of sodium borohydrides for hydrogen generation[J]. International Journal of Hydrogen Energy, 2008, 33(20):5629-5635
[5] Churikov A V, Gamayunova I M, Zapsis K V, et al. Influence of temperature and alkalinity on the hydrolysis rate of borohydride ions in aqueous solution[J]. International Journal of Hydrogen Energy, 2012, 37(1):335-344
[6] Fournier M C, Falk L, Villermaux J. A new parallel competing reaction system for assessing micromixing efficiency——Experimental approach[J]. Chemical Engineering Science, 1996, 51(22):5053-5064
[7] ljuki? B, Santos D M F, Sequeira C A C, et al. Analytical monitoring of sodium borohydride[J]. Analytical Methods, 2013, 5(4):829-839
[8] 张忠林, 赵以芳, 段东红. 电化学法测定硼氢化钠浓度的研究[J]. 山西化工, 2011, 31(6):30-31 Zhang Zhonglin, Zhao Yifang, Duan Donghong. Determination of the borohydride concentration using electrochemical methods[J]. Shanxi Chemical Industry, 2011, 31(6):30-31(in Chinese)
[9] 刘毅敏, 覃军, 王祥智, 等. 硼氢化钠样品纯度的测定[J]. 理化检验:化学分册, 2003, 39(9):555-556 Liu Yimin, Tan Jun, Wang Xiangzhi. Determination of the of purity of sodium borohydride[J]. Physical Testing and Chemical Analysis, 2003, 39(9):555-556(in Chinese)
[10] 车瀛照,庄英俊. 一种定量分析碱金属硼氢化物的方法:CN, 102901793A[P]. 2013-01-30 Che Yingzhao, Zhuang Yingjun. Method for quantitative analysis of alkali metal borohydride:CN, 102901793A[P]. 2013-01-30(in Chinese)
[11] Lyttle D, Jensen E, Struck W. Simple volumetric assay for sodium borohydride[J]. Analytical Chemistry, 1952, 24(11):1843-1844
[12] Chaikin S W. Direct volumetric assay of sodium borohydride and potassium borohydride[J]. Analytical Chemistry, 1953, 25(5):831-832
[13] 中国石油和化学工业联合会. HG/T 3584-2011硼氢化钾[S]. 北京:化学工业出版社, 2012 China Petroleum and Chemical Industry Federation. HG/T 3584-2011 Potassium borohydride[S]. Beijing:Chemical Industry Press, 2012(in Chinese)
[14] 中国石油和化学工业协会. HG/T 3585-2009工业硼氢化钠[S]. 北京:化学工业出版社, 2010 China Petroleum and Chemical Industry Federation. HG/T 3585-2009 Industrial sodium borohydride[S]. Beijing:Chemical Industry Press, 2010(in Chinese)
[15] 杨裴, 范国强, 白莹, 等. 硼氢化钾分析方法改进[J]. 无机盐工业, 2012, 44(6):52-53 Yang Pei, Fan Guoqiang, Bai Ying, et al. Improvement on analytical method for potassium borohydride[J]. Inorganic Chemicals Industry, 2012, 44(6):52-53(in Chinese)
[16] 陆思伟. 硼氢化钾化工行业标准简介[J]. 化工标准化与质量监督, 2000, 8:1-2 Lu Siwei. Brief introduction of potassium hydrogen chemical industry standard[J]. Chemical Industry Standardization and Quality Supervision, 2000, 8:1-2(in Chinese)
[17] 中国石油和化学工业联合会. HG/T 3584-1999硼氢化钾[S]. 北京:化学工业出版社, 1999 China Petroleum and Chemical Industry Federation. HG/T 3584-1999 Potassium borohydride[S]. Beijing:Chemical Industry Press, 1999(in Chinese)
[18] Brown J, Svensson M. Additions and corrections:The stability of potassium borohydride in alkaline solutions[J]. Journal of the American Chemical Society, 1957, 79(24):6581-6581
[19] Brown J B, Svensson M. The stability of potassium borohydride in alkaline solutions[J]. Journal of the American Chemical Society, 1957, 79(15):4241-4242
[20] Churikov A V, Zapsis K V, Khramkov V V, et al. Temperature-induced transformation of the phase diagrams of ternary systems NaBO₂+NaOH+H₂O and KBO₂+KOH+H₂O[J]. Journal of Chemical & Engineering Data, 2011, 56(3):383-389