高分散型六角片状氢氧化镁的制备与表征
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摘要
利用X射线衍射仪(XRD)、扫描隧道显微镜(SEM)、红外(FTIR)和热重(TG)等技术对制备所得的Mg(OH)2固体进行表征。研究了水热温度、水热时间、水热介质溶液的浓度、表面活性剂的种类以及含量对制备六角片状纳米氢氧化镁的影响。实验研究表明,升温或延长水热时间都能使氢氧化镁的形貌趋向六角片状并提高颗粒的分散性。实验中使用的四种表面活性剂中,在使用量为Mg(OH)2质量的4%时,PVP对Mg(OH)2颗粒的改性效果较佳。
The prepared magnesium hydroxide was characterized with X-ray diffractometer( XRD),scanning tunneling microscopy( SEM),fourier transform infrared spectrometer( FTIR spectrometer) and thermogravimetric analysis( TG). The effect of hydrothermal temperature,hydrothermal time,concentration of hydrothermal solvent,the type and concentration of surfactant on the preparation of hexagonal flaky magnesium hydroxide was studied. The result showed that the crystal shape and dispersion of particles can be improved with increasing the temperature and prolonging hydrothermal time. Among the three surfactant used in the experiment,,the modified effect of PVP on Mg( OH)2 particles is better when added 4% quality of magnesium hydroxide in the experiment.
The prepared magnesium hydroxide was characterized with X-ray diffractometer( XRD),scanning tunneling microscopy( SEM),fourier transform infrared spectrometer( FTIR spectrometer) and thermogravimetric analysis( TG). The effect of hydrothermal temperature,hydrothermal time,concentration of hydrothermal solvent,the type and concentration of surfactant on the preparation of hexagonal flaky magnesium hydroxide was studied. The result showed that the crystal shape and dispersion of particles can be improved with increasing the temperature and prolonging hydrothermal time. Among the three surfactant used in the experiment,,the modified effect of PVP on Mg( OH)2 particles is better when added 4% quality of magnesium hydroxide in the experiment.
引文
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[18]D.Zhu,X.Nai,S.Lan,S.Bian,Xin Liu,W.Li,Surface modification of magnesium hydroxide sulfate hydrate whiskers using a silane coupling agent by dry process[J].Appl.Surf.Sci.2016(390):25-30.
[19]Haibo Dong,Zhiping Du,Yonghong Zhao,Dapeng,Zhou Preparation of surface modified nano-Mg(OH)2via precipitation method[J].Powder Technology.2010(198):325-329.
[20]Yongbin Chen,Tao Zhou,Huaxiong Fang,Simin Li,Yuting Yao,Bailin Fan,Jian Wang.A novel preparation of nanosized hexagonal Mg(OH)2as a flame retardant[J].Particuology.2016(24):177-182.
[21]苏明阳,李姗姗.双柱沉淀——水热处理法制备高分散氢氧化镁[J].盐业与化工(现《盐科学与化工》),2015,44(2):23-26.
[22]逯登琴,王余庆,刘国旺,等.氢氧化镁阻燃剂改性研究现状[J].盐业与化工(现《盐科学与化工》),2016,45(10):9-16.
[2]L.Liu,J.Hu,J.Zhuo,C.Jiao,X.Chen,S.Li.Synergistic flame retardant effects between hollow glass microspheres and magnesium hydroxide in ethylene-vinyl acetate composites[J].Polym.Degrad.Stab.2014(87):87-94.
[3]H.Ma,Z.Chen,Z.Mao.Controlled growth of magnesium hydroxide crystals and its effect on the high-temperature properties of cotton/magnesium hydroxide composites[J].Vacuum 95.2013(95):1-5.
[4]F.He witt,D.E.Rhebat,A.Witkows ki,T.R.Hull.An experimental and numericalmodel for the release of acetone from decomposing EVA containing aluminium,magnesium or calcium hydroxidefire Retardants[J].Polym.Degrad.Stab.2016(65):65-78.
[5]李三喜,任晓宇,王松.水热改性对氢氧化镁的影响[J].沈阳工业大学学报,2015,37(4):372-376.
[6]张玉星,陈建铭,宋云华.氧化镁两步法制备阻燃型氢氧化镁[J].无机化学学报,2014,30(4):860-866.
[7]王明帆,马祥伟,游轻寒,等.活性氢氧化镁水热改性制备分散性氢氧化镁[J].无机盐工业,2015,47(7):29-31.
[8]赵卓雅.六角片状氢氧化镁阻燃剂的制备及其应用性能研究[D].天津:天津大学,2014.
[9]赵卓雅,李祥高,王世荣,等.六角片状氢氧化镁(001)晶面优先生长条件的研究[J].人工晶体学报,2014,43(7):1 611-1 619.
[10]D.Zhang,P.Zhang,S.Song,Q.Yuan,P.Yang,X.Ren.Simulation of magnesium hy-droxide surface and interface,J.Alloys Compd.2014(612):315-322.
[11]Q.Wang,C..Li,M.Guo,L.Sun,C.Hu,Hydrothermal synthesis of hexagonal magnesium hydroxide nano flakes[J],Mater.Res.Bull.2014:35-39.
[12]陈建铭,张兆震,宋云华.水热反应条件对氢氧化镁微观内应变的影响[J].人工晶体学报,2011,40(2):396-399.
[13]W.Gong,D.Wu,Z.Cheng,H.Pang,Y.Lin,G.Ning.Direct synthesis of porous Mg(OH)2nanoplates from natural brucite[J].Mater.Res.Bull.2013(48):1 333-1 337.
[14]Y.Chen,T.Zhou,H.Fang,S.Li,Y.Yao,B.Fan,J.Wang.A novel preparation of nanosized hexagonal Mg(OH)2as a flame retardant[J].Particuology 2016(24):177-182.
[15]Huaxiong Fang,Tao Zhou,Xiangping Chen,Simin Li,Guangshan Shen,Xiaoyan Liao.Controlled preparation and characterization of nano-sized hexagonal Mg(OH)2flame retardant[J].Particuology.Particuology.2014(14):51-56.
[16]Silva,M.F.,da Silva,C.A.,Fogo,F.C.,Pineda,E.A.G.,&Hechenleitner,A.A.W..Thermal and FTIR study of polyvinylpyrrolidone/lignin blends[J].Thermal Analysis and Calorimetry,2005(79):367-370.
[17]A.Pilarska,M.Wysokowski,E.Markiewicz,T.Jesionowski,Synthesis of magnesiumhydroxide and its calcinates by precipitation method with the use of magnesiumsulfate and poly(ethylene glycols)[J].Powder Technol.2013:148-157.
[18]D.Zhu,X.Nai,S.Lan,S.Bian,Xin Liu,W.Li,Surface modification of magnesium hydroxide sulfate hydrate whiskers using a silane coupling agent by dry process[J].Appl.Surf.Sci.2016(390):25-30.
[19]Haibo Dong,Zhiping Du,Yonghong Zhao,Dapeng,Zhou Preparation of surface modified nano-Mg(OH)2via precipitation method[J].Powder Technology.2010(198):325-329.
[20]Yongbin Chen,Tao Zhou,Huaxiong Fang,Simin Li,Yuting Yao,Bailin Fan,Jian Wang.A novel preparation of nanosized hexagonal Mg(OH)2as a flame retardant[J].Particuology.2016(24):177-182.
[21]苏明阳,李姗姗.双柱沉淀——水热处理法制备高分散氢氧化镁[J].盐业与化工(现《盐科学与化工》),2015,44(2):23-26.
[22]逯登琴,王余庆,刘国旺,等.氢氧化镁阻燃剂改性研究现状[J].盐业与化工(现《盐科学与化工》),2016,45(10):9-16.