水热法制备MF树脂微球工艺研究
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摘要
采用水热法制备MF树脂微球,讨论了反应体系pH值、水热时间、三聚氰胺质量分数等因素对MF树脂微球理化性质的影响。利用扫描电镜(SEM)、红外光谱(FTIR)、热重(TG)等方法对微球的粒径、形貌、结构和热稳定性进行了测试和分析。研究结果表明:在pH值为11、水热温度160℃、水热时间12h和三聚氰胺质量分数1%条件下,能够制备出表面光滑和球形度好的平均粒径为5μm左右的MF树脂微球。
The MF resin microspheres are prepared by hydrothermal method, and the effects of the p H value of the reaction system, hydrothermal time, mass fraction of melamine on the physical and chemical properties of microspheres are discussed. The particle size, morphology, structure and thermal stability of the product are tested and analyzed by means of SEM, FTIR and TG. The results show that the MF resin microspheres with smooth surface and good sphericity are prepared with an average particle size of about 5μm when the p H vale is 11, hydrothermal temperature is 160 ℃, hydrothermal time is 12h and the melamine mass fraction is 1%.
The MF resin microspheres are prepared by hydrothermal method, and the effects of the p H value of the reaction system, hydrothermal time, mass fraction of melamine on the physical and chemical properties of microspheres are discussed. The particle size, morphology, structure and thermal stability of the product are tested and analyzed by means of SEM, FTIR and TG. The results show that the MF resin microspheres with smooth surface and good sphericity are prepared with an average particle size of about 5μm when the p H vale is 11, hydrothermal temperature is 160 ℃, hydrothermal time is 12h and the melamine mass fraction is 1%.
引文
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[14]WU Y, LI Y, XU J, et al. Incorporating fluorescent dyes into monodisperse melamine-formaldehyde resin microspheres via an organic sol-gel process:a pre-polymer doping strategy[J].Journal of Materials Chemistry B, 2014, 2:5837.
[15]ZHOU H, XU S, SU H, et al. Facile preparation and ultra-microporous structure of melamine-resorcinol-formaldehyde polymeric microspheres[J]. Chemical Communications, 2013, 49:3763~3765.
[16]LU W, QIAN C, BI L, et al. Biomolecule-based formaldehyde resin microspheres loaded with Au nanoparticles:a novel immunoassay for detection of tumor markers in human serum[J].Biosensors and Bioelectronics, 2014, 53:346~354.
[2]WU Y, LI Y, XU J, et al. Incorporating fluorescent dyes into monodisperse melamine-formaldehyde resin microspheres via an organic sol-gel process:a pre-polymer doping strategy[J]. Journal of Materials Chemistry B, 2014, 2(35):5837~5846.
[3]SCHWARZ D, WEBER J. Synthesis of mesoporous poly(melamineformaldehyde)particles by inverse emulsion polymerization[J].Journal of Colloid&Interface Science,2017, 498:335~342.
[4]WANG Y, LI Y, LIU S, et al. Fabrication of chitin microspheres and their multipurpose application as catalyst support and adsorbent[J]. Carbohydrate polymers, 2015, 120:53~59.
[5]AGRAWAL A, SAH U K K. Separation and recovery of lead from a mixture of some heavy metals using Amberlite IRC 718 chelating resin[J]. Journal of hazardous materials, 2006,133:299~303.
[6]WANG S, WANG K, DAI C, ET AL. Adsorption of Pb2+on aminofunctionalized core-shell magnetic mesoporous SBA-15silica composite[J]. Chemical Engineering Journal, 2015, 262:897~903.
[7]ZHOU X, SU Y, ZHAO S. Preparation of chitosan-quercetin resin microspheres and its adsorption properties for flavonoids[J].Separation Science and Technology, 2013, 48:941~946.
[8]LI M, ZHANG Y, YANG L, et al. Hollow melamine resin-based carbon spheres/graphene composite with excellent performance for supercapacitors[J]. Electrochimica Acta, 2015, 166:310~319.
[9]REN S, WANG M, JIA C, et al. Fabrication of supercapacitors using carbon microspheres synthesized from resorcinol-formaldehyde resin[J]. Energy Technology, 2013,1:332~337.
[10]LIU H, LI H, DING Z, et al. Preparation of porous hollow SiO2spheres by a modified St觟ber process using MF microspheres as templates[J]. Journal of Cluster Science, 2011, 23:273~285.
[11]WU Y, LI Y, QIN L, et al. Monodispersed or narrow-dispersed melamine-formaldehyde resin polymer colloidal spheres:preparation, sizecontrol, modification, bioconjugation and particle formation mechanism[J]. Journal of Materials Chemistry B, 2013,1:204~212.
[12]DAIGUJI H, MAKUTA T, KINOSHITA H, et al. Fabrication of hollow melamine-formaldehyde microcapsules from microbubble templates[J].The Journal of Physical Chemistry B, 2007, 111:8879~8884.
[13]RAZALI R, ZAK A K, MAJID W H A, et al. Solvothermal synthesis of microsphere ZnO nanostructures in DEA media[J].Ceramics International, 2011, 37:3657~3663.
[14]WU Y, LI Y, XU J, et al. Incorporating fluorescent dyes into monodisperse melamine-formaldehyde resin microspheres via an organic sol-gel process:a pre-polymer doping strategy[J].Journal of Materials Chemistry B, 2014, 2:5837.
[15]ZHOU H, XU S, SU H, et al. Facile preparation and ultra-microporous structure of melamine-resorcinol-formaldehyde polymeric microspheres[J]. Chemical Communications, 2013, 49:3763~3765.
[16]LU W, QIAN C, BI L, et al. Biomolecule-based formaldehyde resin microspheres loaded with Au nanoparticles:a novel immunoassay for detection of tumor markers in human serum[J].Biosensors and Bioelectronics, 2014, 53:346~354.