摘要
以双酚A(BPA)酚醛树脂和六亚甲基二异氰酸酯(HDI)为原料,在二月桂酸二丁基锡(DBTDL)催化作用下合成了HDI-BPA酚醛树脂。采用FTIR、~1HNMR、GPC、有机元素分析等对HDI-BPA酚醛树脂的化学结构和相对分子质量进行了表征,结果表明目标产物成功制备,其Mw为3376。探讨了反应温度、反应时间、物料配比、催化剂用量等因素对目标产物中异氰酸酯基质量分数及接枝率的影响。通过建立异氰酸酯基质量分数和接枝率的二次回归方程,使用响应面分析法中的Box-Behnken Design(BBD)对HDI-BPA酚醛树脂的合成工艺进行了优化,最佳工艺条件为:反应温度32℃、反应时间为55min、m(BPA酚醛树脂)∶m(HDI)∶m(DBTDL)=0.2101∶1∶0.0025。在此条件下,合成产物中异氰酸酯基质量分数为25.51%,接枝率为48.929%。最后,在HDI-BPA酚醛树脂中加入E-51固化剂,制备出HDI-BPA酚醛树脂胶黏剂,其最大粘结力达283.69 N,相对于BPA酚醛树脂胶黏剂的性能提升了3.7倍,表明HDI的加入显著提高了BPA酚醛树脂对低极性皮革基材的粘结性能。同时,HDI-BPA酚醛树脂胶黏剂的接触角为93.5°,表现出较好的疏水和耐水性能。
HDI-BPA phenolic resin was synthesized from bisphenol A(BPA)phenolic resinand hexamethylene diisocyanate(HDI)in the presence of a catalytic amount of dibutyltindilaurate(DBTDL).The chemical structure and relative molecular mass of HDI-BPA phenolic resin were characterize by FTIR,~1 HNMR,GPC and element analysis.The results showed that the target product was successfully prepared and its Mw was 3376.In addition,the effects of reaction temperature,reaction time,material ratio and amount of catalyst on the content and grafting ratio of isocyanate groups in the target product were discussed.The synthesis process of HDI-BPA phenolic resin was optimized by Box-Behnken Design(BBD)in response surface methodology by establishing a quadratic regression equation of isocyanate content and grafting ratio.The optimum conditions were obtained as follows:reaction temperature 32℃,reaction time 55 min,m(BPA phenolic resin)∶m(HDI)∶m(DBTDL)=0.2101∶1∶0.0025.Under these conditions,the mass fraction and graft ratio of the isocyanate groups in the final product were 25.51%and 48.929%,respectively.Finally,HDI-BPA phenolic resin adhesive was prepare by adding E-51 curing agent to HDI-BPA phenolic resin.Its maximum adhesion was 283.69 N,which was 3.7 times higher than that of BPA phenolic resin adhesive,indicating that HDI modification can significantly improve the adhesion of BPA phenolic resin to low polarity leather substrates.At the same time,the HDI-BPA phenolic resin adhesive had a contact angle of 93.5°,which showed good hydrophobic properties and water resistance.
作者
郭睿
李秀环
何观伟
刘雪艳
霍文生
冯文佩
GUO Rui;LI Xiu-huan;HE Guan-wei;LIU Xue-yan;HUO Wen-sheng;FENG Wen-pei(MOE Key Laboratory of the Chemistry and Technology of Light Auxiliary Chemicals,Shaanxi University of Science&Technology,Xi'an 710021,Shaanxi,China;The Northwest Research Institute of Chemical Industry Co.,Ltd.,Xi'an 710061,Shaanxi,China)
出处
《精细化工》
EI
CAS
CSCD
北大核心
2019年第12期2503-2511,共9页
Fine Chemicals
基金
陕西省2017年重点研发计划项目(2017ZDXM-GY-087)
陕西省2017年重点研发计划项目(2017GY-185)
陕西省教育厅服务地方专项计划项目(15JF011)
