摘要
采用溶液聚合法,以己二酸、聚乙二醇400(PEG 400)为原料,制备醇酸树脂。研究原料配比、反应温度、反应时间、升温方式、催化剂等条件对醇酸树脂产率与分子量的影响。优化得到醇酸树脂的最佳合成条件:PEG 400与己二酸的摩尔比为1.2:1,催化剂辛酸亚锡用量为8×10~(-3)mol/mol,140℃到190℃的升温期间采用非线性升温方式升温。
基于溶胶凝胶(sol-gel)工艺,采用两步法,以正硅酸乙酯(TEOS)、甲基三乙氧基硅烷(MTES)、醇酸树脂为原料,制备疏水型醇酸树脂/SiO_2有机无机杂化材料。MTES的Si-CH_3基团赋予材料的疏水性能,随着MTES含量的提高,接触角θ增大,当MTES wt%超过15%时,接触角θ增大不明显,并最终稳定在126°左右。红外图谱(FTIR)和x-射线光电子能谱(XPS)分析结果显示,硅溶胶与醇酸树脂间发生了的杂化反应,形成了Si-O-C键。DSC分析结果显示,随SiO_2wt%的提高,杂化材料的耐热性能提高。
采用复合乳化剂,结合溶剂挥发法,制备醇酸树脂/SiO_2乳液。探讨了乳化剂用量、复合乳化剂的组成以及搅拌速度等条件对醇酸树脂/SiO_2乳液的性能影响。在复合乳化剂中,阴离子型乳化剂为十二烷基苯磺酸钠,非离子型乳化剂由OP-10与司班-80构成,且OP-10/司班-80=1:2(wt/wt)。当阴/非离子型复合乳化剂的配比为35/65(wt/wt),用量为9%(wt/wt)时,醇酸树脂/SiO_2乳液的稳定性较好。随搅拌速率的增大,乳胶粒子半径减小,当搅拌速率超过500r/m,乳胶粒子半径变化较小。
Basing on solution polymerization method,adipic acid and polyethylene glycol 400(PEG400)are used to synthesize alkyd resin in this paper.The effects of material ratio,reaction time,reaction temperature,heating mode and catalyst etc. on yield and molecular weight of alkyd resin are investigated.The optimized synthesis parameters for alkyd resin are as follow:molar ratio of adipic acid/PEG400 is 1:1.2,molar ratio of catalyst(Tin(Ⅱ)octanoate)/reactant is 8×10~(-3), a non-linear heating mode from 140℃to 190℃is adopted.
Basing on sol-gel method,tetraethoxysilane(TEOS),methylethoxysilane (MTES),alkyd resin are used to synthesize hydrophobic alkyd resin/SiO_2 organic inorganic hybrid material by two-step method.The Si-methyl groups of MTES contribute to hydrophobicity of the hybrid material.The contact angleθon the surface of hybrid material increases with the increase of the MTES wt%and keeps stable at about 126°for MTES wt%＞15.The transform infrared spectroscopy (FTIR)and X-ray photoelectron spectroscopy(XPS)spectra show that alkyd resin can hybridize with silica sol and form Si-O-C bonds.Moreover,the differential scanning calorimetry(DSC)results show that the heat resistant property of the hydrophobic alkyd resin /SiO_2 organic inorganic hybrid material has being improved with the increase of the SiO_2wt%
Basing on solvent evaporation method,a compound emulsion agent is used to prepare alkyd resin/SiO_2 emulsion.The effects of the dosage and component of compound emulsion agent,stirring rate etc.on the properties of alkyd resin/SiO_2 emulsion are investigated.In compound emulsion agent,the anion emulsion agent is sodium dodecyl benzene sulfonate,while the non-ionic emulsion agent is composed of OP-10 and span-80(the weight ratio of OP-10/span-80 is 1:20).When the weight ratio of anion/non-ionic emulsion agent is 35/65 and the dosage of compound emulsion agent is 9wt%,the alkyd resin/SiO_2 emulsion is more stable. The emulsion particle size decreases with the increase of stirring rate and changes unobviously for stirring rate over 500r/m.
引文
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