以轻烧粉制备六方片状氢氧化镁
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摘要
主要以轻烧粉和硝酸铵为原料,经过蒸氨反应得到蒸氨精制液,不加任何添加剂,再以氨水为沉淀剂,制备高品质的六方片氢氧化镁。研究了蒸氨过程中镁离子浓度随蒸氨温度和蒸氨时间的变化规律以及在沉镁过程中,氨镁比、沉镁温度对氢氧化镁形貌和粒径的影响。结果表明:氨水法制备的氢氧化镁为规整六方片形、粒度在1～2μm之间,(001)面的X射线衍射强度远远大于(101)面,说明其表面极性较低、分散性较好,而且该产品分解温度为335.4℃,具有良好的热稳定性,可以用作工业级阻燃剂。
A high-quality hexagonal magnesium hydroxide was prepared using ammonia water as a precipitant, and light-burning powder and ammonium nitrate as raw materials without any additives.The evaporated ammonia refining solution was obtained by ammonia evaporation.The magnesium ion concentration changes with ammonia evaporation temperature and time in the ammonia evaporation process.The effects of ammonia-magnesium ratio and reaction temperature on the morphology and particle size of magnesium hydroxide in precipitation magnesium were investigated.The experimental results show that magnesium hydroxide prepared by ammonia water method is regular hexagonal plate with the size of 1–2 μm.The X-ray diffraction intensity of the(001)plane is greater than that of the(101) plane, indicating that the surface polarity is low.The product with the well-dispersibility and the decomposition temperature of 335.4 ℃ can be obtained,having a good thermal stability, and it can be used as an industrial grade flame retardant.
A high-quality hexagonal magnesium hydroxide was prepared using ammonia water as a precipitant, and light-burning powder and ammonium nitrate as raw materials without any additives.The evaporated ammonia refining solution was obtained by ammonia evaporation.The magnesium ion concentration changes with ammonia evaporation temperature and time in the ammonia evaporation process.The effects of ammonia-magnesium ratio and reaction temperature on the morphology and particle size of magnesium hydroxide in precipitation magnesium were investigated.The experimental results show that magnesium hydroxide prepared by ammonia water method is regular hexagonal plate with the size of 1–2 μm.The X-ray diffraction intensity of the(001)plane is greater than that of the(101) plane, indicating that the surface polarity is low.The product with the well-dispersibility and the decomposition temperature of 335.4 ℃ can be obtained,having a good thermal stability, and it can be used as an industrial grade flame retardant.
引文
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[2]赵丽,王立艳,肖姗姗,等.氢氧化镁阻燃剂制备研究进展[J].无机盐工业,2018,50(3):16-19.ZHAO Li,WANG Liyan,XIAO Shanshan,et al.Inorg Chem Ind(in Chinese),2018,50(3):16-19.
[3]杨华明,周灿伟,李云龙,等.氢氧化镁阻燃剂的现状和发展[J].中国非金属矿工业导刊,2004,13(5):81-84.YANG Huaming,ZHOU Canwei,LI Yunlong,et al.Chin Non-Met Min Ind(in Chinese),2004,13(5):81-84.
[4]陈晓浪,于杰,何敏,等.表面改性剂对聚丙烯/氢氧化镁复合材料燃烧性能和热稳定性及结晶行为的影响[J].高分子材料科学与工程,2009,25(5):60-63.CHEN Xiaolang,YU Jie,HE Min,et al.High Polym Mater Sci Eng(in Chinese),2009,25(5):60-63.
[5]LATTIMER R P,KROENKE W J.The Functional Role of MolybdenumTrioxide as a Smoke retarder additive in rigid poly(vinyl chloride)[J].J Appl Polym Sci,2010,26(4):1191-1210.
[6]CAMINO G,COSTA L,TROSSARELLI L,et al.Study of the mechanism of intumescence in fire retardant polymers:Part IV-Evidence of ester formation in ammoniu polyphosphatepentaerythritol mixtures[J].Polym Degrad Stab,1985,12(3):213-228.
[7]刘志启,李丽娟,张东生,等.气液接触法制备球形氢氧化镁[J].无机化学学报,2014,30(3):705-709.LIU Zhiqi,LI Lijuan,ZHANG Dongsheng,et al.Chin J Inorg Chem(in Chinese)2014,30(3):705-709.
[8]王伟,顾惠敏,翟玉春,等.球形氢氧化镁的制备及其晶体生长动力学[J].材料研究学报,2008,22(6):585-588.WANG Wei,GU Huimin,QU Yuchun,et al.Chin J Mater Res(in Chinese),2008,22(6):585-588.
[9]张琴,赵娜,翟俊,等.卤水-氨水制备超细Mg(OH)2及超声处理对其影响[J].盐业与化工,2014,43(10):12-15.ZHANG Qin,ZHAO Na,QU Jun,et al.J Salt Chem Ind(in Chinese),2014,43(10):12-15.
[10]韩丰,王朝乾.卤水法超细氢氧化镁生产工艺研究[J].盐科学与化工,2017,46(8):14-17.HAN Feng,WANG Chaoqian.J Salt Sci Chem Ind(in Chinese),2017,46(8):14-17.
[11]刘立华.卤水-氨水法制备氢氧化镁阻燃剂的实验研究[J].化工科技市场,2010,33(1):14-16.LIU Lihua.Chem Technol Marker(in Chinese),2010,33(1):14-16.
[12]宋雪雪,李丽娟,刘志启,等.氨气法制备氢氧化镁工艺研究[J].化学工程,2014(6):74-78.SONG Xuexue,LI Lijuan,LIU Zhiqi,et al.Chem Eng(in Chinese),2014,6:74-78.
[13]徐嘉欣,颜粉鸽,黄建翠,等.高分散型六角片状氢氧化镁的制备与表征[J].盐科学与化工,2018,47(3):14-21.XU Jiaxin,YAN Fenge,HUANG Jiancui,et al.J Salt Sci Chem Ind(in Chinese),2018,47(3):14-21.
[14]杜以波.均质流体法制备纳米氢氧化镁[P].CN Patent,1332116.2002-01-23.DU Yibo.Preparation of nanometer magnesium hydroxide by homogeneous fluid method(in Chinese).CN Patent,1332116.2002-01-23.
[15]易求实.反向沉淀法制备纳米Mg(OH)2阻燃剂的研究[J].化学试剂,2001,23(4):197-199.YI Qiushi.Chem Reagents(in Chinese),2001,23(4):197-199.
[16]范天博,李雪,马超,等.氯化镁溶液氨气鼓泡反应制备纳米氢氧化镁[J].化工学报,2012,61(11):3025-3032.FAN Tianbo,LI Xue,MA Chao et al.J Chem Ind Eng(in Chinese),2012,61(11):3025-3032.
[17]向兰,金永成,金涌.氢氧化钠溶液中氢氧化镁的水热改性[J].过程工程学报,2003,3(2):116-120.XIANG Lan,JIN Yongcheng,JIN Yong.Chin J Process Eng(in Chinese),2003,3(2):116-120.
[18]于雪峰,朱秀丽,师敏,等.探究温度对氨法制备氢氧化镁阻燃剂的影响[J].化学工程与装备,2011(3):33-35.YU Xuefeng,ZHU Xiuli,SHI Min,et al.Chem Eng Equip(in Chinese),2011(3):33-35.
[19]程沛,李雪,裴冰野,等.阴离子对Mg(OH)2晶体生长及形貌的影响机理[J].化工学报,2017,68(10):3985-3992.CHENG Pei,LI Xue,PEI Bingye,et al.J Chem Ind Eng(in Chinese),2017,68(10):3985-3992.
[20]李雪,张滢,侯睿,等.轻烧粉蒸氨液中杂离子对氢氧化镁晶体的影响[J].无机盐工业,2016,48(10):23-25.LI Xue,ZHANG Ying,HOU Rui,et al.Inorg Chem Ind(in Chinese),2016,48(10):23-25.