功能材料
功能材料
공능재료
JOURNAL OF FUNCTIONAL MATERIALS
2012年
17期
2363-2368
,共6页
多孔聚合物%聚酰亚胺微球%接枝单体%相分离
多孔聚閤物%聚酰亞胺微毬%接枝單體%相分離
다공취합물%취선아알미구%접지단체%상분리
porous polymer%polymer microspheres%graft monomer%phase separation
以3,5-二氨基苯甲酸与线性低聚物聚乙二醇单甲醚在催化剂存在的条件下发生酯化反应,得到了接枝单体。以接枝单体、3,5-二氨基苯甲酸以及均苯四甲酸二酐在非水乳液体系中发生聚合反应,经过两步亚胺化及热处理得到了多孔聚酰亚胺微球。通过实验确定了接枝单体的最优反应条件:酸醇摩尔比为1.3,催化剂、携水剂的用量与醇的质量比分别为4%、130%,反应时间为6h。实验结果表明,随着接枝单体在聚酰亚胺中浓度从20%~40%,粒径逐渐增大,粒径范围为9.5~15.7μm;而玻璃化温度从210℃降至178℃;同时在接枝单体浓度为40%时得到了孔结构,比表面积为148cm3/g;通过控制热处理时气体压力可以控制孔结构大小。
以3,5-二氨基苯甲痠與線性低聚物聚乙二醇單甲醚在催化劑存在的條件下髮生酯化反應,得到瞭接枝單體。以接枝單體、3,5-二氨基苯甲痠以及均苯四甲痠二酐在非水乳液體繫中髮生聚閤反應,經過兩步亞胺化及熱處理得到瞭多孔聚酰亞胺微毬。通過實驗確定瞭接枝單體的最優反應條件:痠醇摩爾比為1.3,催化劑、攜水劑的用量與醇的質量比分彆為4%、130%,反應時間為6h。實驗結果錶明,隨著接枝單體在聚酰亞胺中濃度從20%~40%,粒徑逐漸增大,粒徑範圍為9.5~15.7μm;而玻璃化溫度從210℃降至178℃;同時在接枝單體濃度為40%時得到瞭孔結構,比錶麵積為148cm3/g;通過控製熱處理時氣體壓力可以控製孔結構大小。
이3,5-이안기분갑산여선성저취물취을이순단갑미재최화제존재적조건하발생지화반응,득도료접지단체。이접지단체、3,5-이안기분갑산이급균분사갑산이항재비수유액체계중발생취합반응,경과량보아알화급열처리득도료다공취선아알미구。통과실험학정료접지단체적최우반응조건:산순마이비위1.3,최화제、휴수제적용량여순적질량비분별위4%、130%,반응시간위6h。실험결과표명,수착접지단체재취선아알중농도종20%~40%,립경축점증대,립경범위위9.5~15.7μm;이파리화온도종210℃강지178℃;동시재접지단체농도위40%시득도료공결구,비표면적위148cm3/g;통과공제열처리시기체압력가이공제공결구대소。
A new graft monomer as new diamine was synthesized by 3,5-diaminobenzoic acid(3,5-DBA) and methoxypolyethylene glycols(MPEG) through esterification reaction in the presence of catalyst.The porous polyimide microspheres was prepared by graft monomer and 3,5-DBA simultaneously with pyromellitic dianhydride(PMDA)in the non-aqueous emulsion polycondensation and then process traditional two steps imidization and the final thermal treatment.The optimal condition of esterification reaction was confirmed by experiments: n(acid)/n(alcohol) was 1.3,the content of catalyst and water carrying(to PMDA by weight) were 5% and 120% separately and reaction time was 6h.As the concentration of graft monomer in the PI increasing,the size of porous PI microspheres was increasing from 9.5 to 15.9μm;the value of glass transition temperature(Tg) was decreasing from 210 to 178℃.Porous PI microspheres with obvious and uniform porous structure were obtained when the concentration of graft monomer was 40% and the specific surface area was 148cm3/g;the porous size can be controlled by the pressure of the thermal treatment stage in the muffle furnace.