CAJ | 학술논문

为了制备高活性聚氨酯交联固化剂,用2,4-二异氰酸基甲苯(TDI)三元聚合反应合成了具有3个活性异氰酸根的六元环结构异氰脲酸酯.用红外光谱、凝胶色谱(GPC)及化学分析法对反应条件进行了优化研究,并对产物进行了表征.利用凝胶色谱法对TDI三聚体及多聚体的形成过程进行过程跟踪,并对TDI三聚体的稳定性进行了研究.结果表明:采用Cat-3作催化剂,在(60±2)℃下反应,可制得分子量为530～550,Mw/Mn=1.10,NCO质量分数为(25.0±0.5)%窄分子量分布的TDI三聚体;随着反应时间延长,TDI会进一步多元聚合生成多聚结构;而加入质量分数为0.4%的苯甲酰氯作为稳定剂,可有效抑制多元聚合的发生,所制备的TDI三聚体稳定性可在半年以上.
위료제비고활성취안지교련고화제,용2,4-이이청산기갑분(TDI)삼원취합반응합성료구유3개활성이청산근적륙원배결구이청뇨산지.용홍외광보、응효색보(GPC)급화학분석법대반응조건진행료우화연구,병대산물진행료표정.이용응효색보법대TDI삼취체급다취체적형성과정진행과정근종,병대TDI삼취체적은정성진행료연구.결과표명:채용Cat-3작최화제,재(60±2)℃하반응,가제득분자량위530～550,Mw/Mn=1.10,NCO질량분수위(25.0±0.5)%착분자량분포적TDI삼취체;수착반응시간연장,TDI회진일보다원취합생성다취결구;이가입질량분수위0.4%적분갑선록작위은정제,가유효억제다원취합적발생,소제비적TDI삼취체은정성가재반년이상.
For the production of reactive polyurethane cross-linkinger and curing agents, 2, 4-diisocyanate toluene (TDI) terpolymer, which possesses the rigid structures of hexatomic ring and three reactive functional groups, was synthesized and characterized by the Fourier transform infrared (FTIR), the gel permeation chromatography (GPC) and the chemical analysis methods. The reaction conditions were studied and optimized.A tracking research on the polymerization process of TDI was taken by using the GPC. The formation processes of the terpolymer, oligomers and higher-polymers were also dealt with. Results show that the TDI terpolymer can be prepared in the presence of Cat-3 catalyst and at the reaction temperature of (60 ± 2)℃. The reaction time is short, its outcomes have narrow molecular weights distribution, namely molecular weights from 530 to 550, Mw/Mn = 1.10, and the mass fraction of NCO is (25.0 ± 0. 5) %. With the reaction time prolonging,however, TDI can be further higher-polymerized to form higher-polymers. Benzoyl chloride (0. 4%, mass fraction), as the stabilizing agent, can effectively inhibit the occurrence of higher-polymerization. The obtained TDI terpolymer can be stable for more than half a year.