环氧树脂的水性化改性及其复合涂层的性能研究
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摘要
水性环氧树脂体系避免了挥发性有机物(VOC)的大量使用，具有显著的环保特点和实际应用价值，因此环氧树脂的水性化及其应用研究成为近些年来备受关注的热点领域之一。
本文采用化学改性法对环氧树脂E-51进行水性化改性，首先用丙烯酸和环氧树脂反应得到环氧丙烯酸树脂，然后用顺丁烯二酸酐和环氧丙烯酸树脂中的侧羟基反应，得到含有亲水性羧基和可交联固化的不饱和双键的改性树脂，用有机碱进行中和成盐，加水制得稳定的乳液体系；确定了最佳的合成反应条件；并对乳液的稳定性进行讨论；选择了合适的固化体系和固化条件。另外，通过乳液聚合法制备了聚苯胺和聚苯胺—二氧化硅（SiO_2／PANI）复合粒子，并对水性环氧复合涂层进行性能测试。
实验结果表明：改性树脂结构与目标产物一致，热稳定性良好；反应物的物质的量比为：n（EpA）：n（酸酐）=1:2，用有机碱中和改性树脂，中和温度为60℃左右，体系固含量较高时可以形成较稳定的乳液体系。室温下过氧化苯甲酰—N,N-二甲基苯胺固化体系涂层优于过硫酸钠—亚硫酸氢钠固化体系涂层；中温下（100℃～120℃）采用分阶段固化（50℃／1h+100℃／1h）可以得到较好的固化效果；聚苯胺包覆二氧化硅比聚苯胺的热稳定性提高，复合粒子涂层在涂层耐水性、铅笔硬度、涂层附着力及耐盐雾腐蚀等方面比纯聚苯胺涂层性能较好。
The water-based epoxy reasin can be prepared and used with very little or withoutorganic compound(VOC), therefore, it is environment-friendly and very attractive in manyapplication fields. In recent years, much more attention has been paid to preparation andapplication of the water-based epoxy reasin.
This thesis adopts chemical modified method to prepare water-based resins of theepoxy resin E-51. Firstly, epoxy resin was used to react with acrylic to produce epoxyacrylate, then the products side hydroxyl of epoxy acrylic resin was used to react withemaleic anhydride to produce the modified resin containing hydrophilic carboxyl andunsaturated double bonds(EpB). EpB can be crosslinked, neutralized to salt by addingorganic base, and then water was added into the EpB salts solution to produce stableemulsion system. The optimal reaction conditions were optimized, and the stability ofemulsion was discussed, and the appropriate curing system and curing conditions wasoptimized also. Polyaniline (PANI) and SiO2/PANI composite particles were prepared byemulsion polymerization, and the properties of epoxy composite coatings were tested.
The results showed that the structure of the modified resins is the target product, andthe products have good thermal stability. With molar ratio of n(EpA):n (anhydride)=1:2,and with organic base to neutralize at60℃, the stable emulsion system can be formedwith higher solid content. Under room temperature, the coatings cured with benzoylperoxide-N,N-dimethyl aniline system is superior to that cured with sodium persulfate-sodium bisulfite system; better curing effect can be reached under median temperature(100℃~120℃) under phased curing (50℃/1h+100℃/1h). Polyaniline coated onsilica surface (SiO_2/PANI) has a higher thermal stability than polyaniline. The coatingmodified with composite particles has better performance than that modified with purepolyaniline in the aspects of water-resistant, pencil hardness, coating adhesion andresistance to salt spray corrosion.
本文采用化学改性法对环氧树脂E-51进行水性化改性，首先用丙烯酸和环氧树脂反应得到环氧丙烯酸树脂，然后用顺丁烯二酸酐和环氧丙烯酸树脂中的侧羟基反应，得到含有亲水性羧基和可交联固化的不饱和双键的改性树脂，用有机碱进行中和成盐，加水制得稳定的乳液体系；确定了最佳的合成反应条件；并对乳液的稳定性进行讨论；选择了合适的固化体系和固化条件。另外，通过乳液聚合法制备了聚苯胺和聚苯胺—二氧化硅（SiO_2／PANI）复合粒子，并对水性环氧复合涂层进行性能测试。
实验结果表明：改性树脂结构与目标产物一致，热稳定性良好；反应物的物质的量比为：n（EpA）：n（酸酐）=1:2，用有机碱中和改性树脂，中和温度为60℃左右，体系固含量较高时可以形成较稳定的乳液体系。室温下过氧化苯甲酰—N,N-二甲基苯胺固化体系涂层优于过硫酸钠—亚硫酸氢钠固化体系涂层；中温下（100℃～120℃）采用分阶段固化（50℃／1h+100℃／1h）可以得到较好的固化效果；聚苯胺包覆二氧化硅比聚苯胺的热稳定性提高，复合粒子涂层在涂层耐水性、铅笔硬度、涂层附着力及耐盐雾腐蚀等方面比纯聚苯胺涂层性能较好。
The water-based epoxy reasin can be prepared and used with very little or withoutorganic compound(VOC), therefore, it is environment-friendly and very attractive in manyapplication fields. In recent years, much more attention has been paid to preparation andapplication of the water-based epoxy reasin.
This thesis adopts chemical modified method to prepare water-based resins of theepoxy resin E-51. Firstly, epoxy resin was used to react with acrylic to produce epoxyacrylate, then the products side hydroxyl of epoxy acrylic resin was used to react withemaleic anhydride to produce the modified resin containing hydrophilic carboxyl andunsaturated double bonds(EpB). EpB can be crosslinked, neutralized to salt by addingorganic base, and then water was added into the EpB salts solution to produce stableemulsion system. The optimal reaction conditions were optimized, and the stability ofemulsion was discussed, and the appropriate curing system and curing conditions wasoptimized also. Polyaniline (PANI) and SiO2/PANI composite particles were prepared byemulsion polymerization, and the properties of epoxy composite coatings were tested.
The results showed that the structure of the modified resins is the target product, andthe products have good thermal stability. With molar ratio of n(EpA):n (anhydride)=1:2,and with organic base to neutralize at60℃, the stable emulsion system can be formedwith higher solid content. Under room temperature, the coatings cured with benzoylperoxide-N,N-dimethyl aniline system is superior to that cured with sodium persulfate-sodium bisulfite system; better curing effect can be reached under median temperature(100℃~120℃) under phased curing (50℃/1h+100℃/1h). Polyaniline coated onsilica surface (SiO_2/PANI) has a higher thermal stability than polyaniline. The coatingmodified with composite particles has better performance than that modified with purepolyaniline in the aspects of water-resistant, pencil hardness, coating adhesion andresistance to salt spray corrosion.
引文
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[20]丁莉,王贵友,胡春圃,等.接枝环氧树脂水分散液的合成、分离与表征[J].功能高分子学报,2004,17(02):165-170.
[21] Kojima S, Watanable Y. Development of High Performance Waterborne Coating (part):Emulsifycation of Epoxy Resin[J]. Polymer English and Science,1993,33(5):253-259.
[22]施雪珍,海特.食品罐内壁涂料用水性环氧涂料的研制[J].涂料工业,2003,(12):18-21.
[23]何青峰,陈志明,巫峡.水性环氧乳液及其固化机理研究进展[J].涂料工业,2004,(06):23-24.
[24]邱东,袁才登,徐涛,等.环保型环氧树脂涂料[J].热固性树脂,2005,(06):15.
[25]陶永忠,陈铤,顾国芳. Ⅰ型水性环氧树脂固化剂及其涂料性能[J].建筑材料学报,2000,3(04):349-354.
[26]武龙,沈宁祥.水性环氧树脂研究进展[J].化学与粘合,2001,(06):268-270
[27] Stark C J(Shell Oil Co). Aqueous Dispersions of Epoxy Resin[P]. USA, US5602193,1997.
[28]陈铤,顾国芳. Ⅱ型水性环氧树脂乳液及其固化过程的研究[J].建筑材料学报，2001,4(04):356-361.
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