高校化学工程学报
高校化學工程學報
고교화학공정학보
JOURNAL OF CHEMICAL ENGINEERING OF CHINESE UNIVERSITIES
2014年
4期
851-857
,共7页
杨军胜%许伟%郝丽芬%安秋凤
楊軍勝%許偉%郝麗芬%安鞦鳳
양군성%허위%학려분%안추봉
含氟无皂乳液%阳离子%核壳%制备
含氟無皂乳液%暘離子%覈殼%製備
함불무조유액%양리자%핵각%제비
fluorine-containing soap-free latex%cationic%core-shell%synthesis
采用半连续种子乳液聚合技术制备阳离子含氟核壳无皂乳液,对影响乳液聚合反应稳定性的主要因素进行探讨和优化;通过红外光谱(FT-IR)、核磁共振氢谱(1H-NMR)、透射电镜(TEM)、X 射线光电子能谱(XPS)、接触角测量仪表征共聚物化学组成、乳胶粒形貌、共聚物膜表面化学元素及其疏水性。结果表明,顺丁烯二酸-乙酯撑基[三甲基氯化铵]-十八烷基聚氧乙烯(20)醚酯(R303)用量为总单体质量3%,引发剂偶氮二异丁基脒盐酸盐(VA-50)用量为总单体质量0.7%,氟单体为总单体质量16.5%,反应温度T为70℃时,可以制得稳定的阳离子含氟核壳无皂乳液。FT-IR及1H-NMR测试结果证明氟单体完全参与共聚,TEM和XPS表征结果表明乳胶粒具有核壳结构,且氟元素在乳液成膜过程中容易迁移到涂膜表面并富集。与传统乳液聚合所得乳液相比,涂膜疏水性有一定提高。
採用半連續種子乳液聚閤技術製備暘離子含氟覈殼無皂乳液,對影響乳液聚閤反應穩定性的主要因素進行探討和優化;通過紅外光譜(FT-IR)、覈磁共振氫譜(1H-NMR)、透射電鏡(TEM)、X 射線光電子能譜(XPS)、接觸角測量儀錶徵共聚物化學組成、乳膠粒形貌、共聚物膜錶麵化學元素及其疏水性。結果錶明,順丁烯二痠-乙酯撐基[三甲基氯化銨]-十八烷基聚氧乙烯(20)醚酯(R303)用量為總單體質量3%,引髮劑偶氮二異丁基脒鹽痠鹽(VA-50)用量為總單體質量0.7%,氟單體為總單體質量16.5%,反應溫度T為70℃時,可以製得穩定的暘離子含氟覈殼無皂乳液。FT-IR及1H-NMR測試結果證明氟單體完全參與共聚,TEM和XPS錶徵結果錶明乳膠粒具有覈殼結構,且氟元素在乳液成膜過程中容易遷移到塗膜錶麵併富集。與傳統乳液聚閤所得乳液相比,塗膜疏水性有一定提高。
채용반련속충자유액취합기술제비양리자함불핵각무조유액,대영향유액취합반응은정성적주요인소진행탐토화우화;통과홍외광보(FT-IR)、핵자공진경보(1H-NMR)、투사전경(TEM)、X 사선광전자능보(XPS)、접촉각측량의표정공취물화학조성、유효립형모、공취물막표면화학원소급기소수성。결과표명,순정희이산-을지탱기[삼갑기록화안]-십팔완기취양을희(20)미지(R303)용량위총단체질량3%,인발제우담이이정기미염산염(VA-50)용량위총단체질량0.7%,불단체위총단체질량16.5%,반응온도T위70℃시,가이제득은정적양리자함불핵각무조유액。FT-IR급1H-NMR측시결과증명불단체완전삼여공취,TEM화XPS표정결과표명유효립구유핵각결구,차불원소재유액성막과정중용역천이도도막표면병부집。여전통유액취합소득유액상비,도막소수성유일정제고。
Cationic fluorine-containing soap-free latex with core-shell structure was synthesized by semicontinuous seeded emulsion polymerization. Effects of dosage of the maleic acid double ester-octadecyl poly(ethyleneoxy)20 ether-ethylene trimethyl ammonium chloride (R303), the initiator (VA-50) and the fluorine monomer as well as reaction temperature on stability of emulsion polymerization were discussed and optimized. The chemical components of copolymer, micro-morphology of latex particles, surface chemical composition and hydrophobicity of latex film were characterized by FT-IR, 1H-NMR, TEM, XPS, respectively. Results showed that the stable cationic emulsion could be obtained when the dosage of R303, VA-50 and fluorine monomer and the reaction temperature were adopted as 3%, 0.7% and 16.5% (on basis of the mass of total monomers) as well as 70℃. FT-IR and 1H-NMR spectra confirmed the fluorine monomer could be incorporated into the latex particles through emulsion polymerization. TEM observation identified the formation of the core-shell structure particles. XPS study further indicated that the fluorine groups had the tendency to migrate to the film-air surface. Hydrophobicity of the soap-free latex film showed some improvement compared to the general one.