| 552 | 15 | 55 |
| 下载次数 | 被引频次 | 阅读次数 |
以重镁水(Mg(HCO3)2)溶液为原料,采用热解法制备碱式碳酸镁。用X射线衍射(XRD)、扫描电子显微镜、热重-差热分析(TG-DTA)和比表面积仪对其进行表征,研究了影响反应诱导期、重镁水分解率、碱式碳酸镁形貌和比表面积的因素。结果表明:提高反应温度、降低反应压力,可以缩短反应诱导期,促进重镁水分解。反应压力为0.10 MPa、反应温度为40℃、分解时间0.5 h时,重镁水分解率为30.51%;升高温度至70℃,分解率为66.43%,比表面积随温度升高先增大后减小;在0.03 MPa和70℃时,重镁水的分解率为91.2%,随温度升高产品比表面积减小,产品形貌变化趋势为:棒状-片状颗粒-花球状。XRD和TG-DTA表征显示产品化学组成为:4MgCO3·Mg(OH)2·4H_2O。
Abstract：Basic magnesium carbonate was prepared via pyrolyzing magnesium bicarbonate solution. The parameter influences on the induction period, decomposition rate of magnesium bicarbonate solution, morphology and specific surface area of basic magnesium carbonate were investigated. The prepared samples were characterized by X-ray diffraction(XRD), scanning electron microscopy and thermogravimetry-differential thermal analysis(TG-DTA) and specific surface area analysis, respectively. The results show that increasing the reaction temperature, and decreasing the reaction pressure can shorten the induction period and promote the decomposition of Mg(HCO3)2. The decomposition rate is 30.51% at 0.1 MPa and 40 °C for 0.5 h. When the temperature increases to 70 °C, the decomposition rate is 66.43 %. The specific surface area firstly increases and then decreases with the increase of temperature. The decomposition rate is 91.2% at 0.03 MPa and 70 °C. The specific surface area decreases and the product morphology becomes rod, flaky, and flower-globose when the temperature increases. Based on the analysis by XRD and TG-DTA, the chemical composition is 4 MgCO3·Mg(OH)2·4H_2O.
[1]HOLLINGBERY L A,HULL T R.The fire retardant behaviour of huntite and hydromagnesite-A review[J].Polymer Degrad Stab,2010,95(12):2213–2225.
[2]任宏瑞,陈镇,党杰,等.TG-DTG和FTIR法研究碳酸镁水合物的热分解[J].太原理工大学学报,2013,44(5):560–564.REN Hongrui,CHEN Zhen,DANG Jie,et al.J Taiyuan Univ Technol(in Chinese),2013,44(5):560–564.
[3]万建军,于博,刘安双.热解反应速率对轻质碳酸镁晶体形貌影响研究[J].盐业与化工,2013,42(2):28–30.WAN Jianjun,YU Bo,LIU Anshuang.J Salt Chem Ind(in Chinese),2013,42(2):28–30.
[4]杨晨,郑东,杨小波,等.特殊形貌碳酸镁用途、制备及表征[J].无机盐工业,2011,43(7):5–7.YANG Chen,ZHENG Dong,YANG Xiaobo,et al.Inorg Chem Ind(in Chinese),2011,43(7):5–7.
[5]郭小水,刘家祥,李敏,等.重镁水真空热解法制备高纯氧化镁[J].非金属矿,2008,31(3):33–34.GUO Xiaoshui,LIU Jiaxiang,LI Min,et al.Non-Met Mines(in Chinese),2008,31(3):33–34.
[6]张雨山,高春娟,黄西平.轻质碳酸镁研究现状及其发展前景[J].盐业与化工,2010,39(1):42–46.ZHANG Yushan,GAO Chunjuan,HUANG Xiping.J Salt Chem Ind(in Chinese),2010,39(1):42–46.
[7]王峻,王晶,柯庆,等.水热处理对无水碳酸镁微观结构的影响[J].硅酸盐学报,2015,43(3):327–333.WANG Jun,WANG Jing,KE Qing,et al.J Chin Ceram Soc,2015,43(3):327–333.
[8]袁春华.水氯镁石制备优质碱式碳酸镁及氧化镁的研究[D].青海:中国科学院盐湖研究所,2005.YUAN Chunhua.The study on preparation of the pure basic magnesium carbonate and magnesia by bischofite(in Chinese,dissertation).Qinghai:Qinghai Institute of Salt Lakes,Chinese Academy of Sciences,2005.
[9]邵平平,李志宝,密建国.碳酸镁水合物在283-363 K范围内的晶体组成及晶型[J].过程工程学报,2009,9(3):520–524.SHAO Pingping,LI Zhibao,MI Jianguo.Chin J Process Eng(in Chinese),2009,9(3):520–524.
[10]陈白珍,江剑兵,徐徽,等.热解法制备碱式碳酸镁[J].中南大学学报,2008,39(5):907–910.CHEN Baizhen,JIANG Jianbing,XU Hui,et al.J Cent South Univ:Sci Technol(in Chinese),2008,39(5):907–910.
[11]秦志扬,秦麟卿,张联盟,等.XRD,TG,DSC和FTIR法研究碱式碳酸镁的热分解[J].非金属矿,2012,35(4):52–53.QIN Zhiyang,QIN Linqing,ZHANG Lianmeng,et al.Non-Met Mines(in Chinese),2012,35(4):52–53.
[12]陈侠,于博,周秀云,等.重镁水热解工艺研究[J].盐业与化工,2012,41(6):12–14.CHEN Xia,YU Bo,ZHOU Xiuyun,et al.J Salt Chem Ind(in Chinese),2012,41(6):12–14.
[13]欧龙,刘家祥.重镁水中通入空气制备三水碳酸镁晶须[J].硅酸盐学报,2016,44(1):107–110.OU Long,LIU Jiaxiang.J Chin Ceram Soc,2016,44(1):107–110.
[14]李彩虹.一种制备单分散纳米粉体的液相沉淀法及其结晶动力学[D].天津:天津大学,2004.LI Caihong.A liquid precipitation method for preparing mono-dispersed nanoparticles and Its crystallization kinetics(in Chinese,dissertation).Tianjin:Tianjin University,2004.
[15]王志强,刘家祥,饶发明.以轻烧白云石为原料二次碳化法制备高纯碱式碳酸镁[J].硅酸盐学报,2013,41(10):1437–1441.WANG Zhiqiang,LIU Jiaxiang,RAO Faming.J Chin Ceram Soc,2013,41(10):1437–1441.
[16]宋兴福,杨晨,汪瑾,等.玫瑰花状多孔碱式碳酸镁微球的合成[J].无机化学学报,2011,27(5):1008–1014.SONG Xing Fu,YANG Chen,WANG Jin,et al.Chin J Inorg Chem(in Chinese),2011,27(5):1008–1014.
[17]郑亚君,党利琴,张智平,等.搅拌时间对水合碳酸镁形貌和组成的影响[J].精细化工,2007,24(9):836–838.ZHENG Yajun,DANG Liqin,ZHANG Zhiping,et al.Fine Chem(in Chinese),2007,24(9):836–838.
[18]袁春华,李海民.碱式碳酸镁的应用及合成方法[J].盐湖研究,2005,13(2):40–42.YUAN Chunhua,LI Haimin.J Salt Lake Res(in Chinese),2005,13(2):40–42.
[19]陈敏,李月圆,王健东,等.利用菱镁矿制备碳酸镁晶须[J].硅酸盐学报,2009,37(10):1649–1653.CHEN Min,LI Yueyuan,WANG Jiandong,et al.J Chin Ceram Soc,2009,37(10):1649–1653.
[20]闫小星,李云飞,薛冬峰,等.基于水合碳酸镁结晶过程的化学键分析(英文)[J].人工晶体学报,2007,36(5):992–999.YAN Xiaoxing,LI Yunfei,XUE Dongfeng,et al.J Synth Cryst(in Chinese),2007,36(5):992–999.
[21]GRAVNER Janko,GRIFFEATH David.Modeling snow crystal growthП:A mesoscopic lattice map with plausible dynamics[J].Phys D:Nonlinear Phenom,2008,237(3):385–404.
[22]王春迎,杜志明,丛晓民,等.碱式碳酸镁的热分解研究[J].应用化工,2008,37(6):658–660.WANG Chunying,DU Zhiming,CONG Xiaomin,et al.Appl Chem Ind(in Chinese),2008,37(6):658–660.
基本信息:
DOI：10.14062/j.issn.0454-5648.2018.07.06
中图分类号:TQ132.2
引用信息:
[1]常睿璇,丁珂,孙晓君,等.热解法制备不同形貌碱式碳酸镁[J].硅酸盐学报,2018,46(07):922-928.DOI:10.14062/j.issn.0454-5648.2018.07.06.
基金信息:
辽宁省自然科学基金项目(L2015020609);; 辽宁省创新团队项目(LT2013010);; 沈阳市科技局项目(F16-208-6-00)
2017-11-22
2017
2018-06-05
2018
1
2018-06-05
2018-06-05
2018-06-05