低游離度TDI三聚體的合成

jiabeneryiqingsuanzhi(tdi)zaicuihuazuoyongxiakeyifashengsanjufanying，xingchenghanyiqingniaosuanzhihuandesanjuti。tdisanjutijuyouhuifaxingdi、duxingxiao、guannengdugao、rewendingxinghao、naifushixinghaodengyoudian，changzuoweijuanzhiguhuajibeiguangfanyingyongzaituliao、zhanhejizhong。zai20shiji70niandai，guowaiduojiagongsikaishigongyehuashengchanyingyongzheleichanpin，rubayer、basf、dowdeng。muqiangaoxingneng、diyoulidantidetdisanjutirengranxuyaodaliangyilaijinkou。

benyanjiuyicuihuaji nt cat p100hecheng tdi sanjutijuanzhiguhuaji，shiyanjieguobiaoming: gaicuihuajijuyoucuihuasulvkuai、huoxinggao、fanyingwendudidengyoudian。zai40 ℃xia，yidijiafangshicuihuafanying，8 h jiukeyidadaofanyingzhongdian，dedaodiyoulidantihanliang tdi sanjuti。

原料及試劑

jiabeneryiqingsuandantitdi(80/20):gongyepin，basf；cusuandingzhi:fenxichun，guangzhoufanyuliqianghuagongchang；nt cat dmp-30:gongyepin，xindianhuaxue；nt cat k-15:gongyepin，xindianhuaxue；nt cat p100: xindianhuaxue；

合成工藝

zaidanqibaohudetiaojianxia，wangzhuangyoujiaoban、wendujiyijihuiliulengningguandeganzaosikouyuandishaopingzhongjiaru tdi( 80/20) danti 100 g，cusuandingzhi100 g。jiaoban5 ～10 min，jiareshengwenzhi40 ℃，dijia0. 5 gcuihuajidecusuandingzhirongye( cusuandingzhi10 ml) 。dijiawanbihou，kongzhiwenduzai40 ～80 ℃zhijian，baowenfanyingyue8 h，meige1 hcedingyicifanyingrongyede—ncozhi，dang—ncohanliangjiangdidao8.5% ～ 9% shi，jiaru1 gbenjiaxianlv，jixufanying0.5 h，tingzhijiarejiaoban，jiangwenchuliao，dedaoqianhuangsetoumingyeti。

zaishangshugongyijichushang，dijiayushedingliangdechun，baowenfanying30 ～60 min，dui tdi sanjutijinxinggaixingchuli。

催化劑種類、用量及滴加方式的影響

cuihuajidexuanzeshitdisanjufanyingdeguanjian。changyongdetdisanjucuihuajibaokuoshuan、youjijinshuhuahewu、youjilinhuahewu、jianjinshusuosuanyandeng。xuanyongdmp－30、k-15hep100dui50%cusuandingzhidetdirongyefenbiecuihuafanying，jieguorubiao1hetu2suoshi。

表1 不同催化劑（0.5%添加量）對TDI三聚反應的影響

youbiao1hetu2kejian，bujiacuihuajideqingkuangxia，tdidesanjufanyingbufasheng；k-15cuihuasanjudexiaoguojiaocha，wendujiaogao、fanyingshijianchang，rongyichanshenggengduodeduojutijiegou；junweishuanleicuihuajidedmp－30hep100cuihuaxiaoguojiaohao，xiangbizhixiap100decuihuaxingnenggengqiang，duanshijianneijiunengxunsufanying，jiangdi—ncozhi，erqieshiyanhuanbiaomingzai40 ℃xiaqirengranjuyouhengaodecuihuahuoxing。yinci，xuanyongp100zuoweicuihuaji。tu3ship100cuihuajiyongliangfenbiezhantdidantizongzhiliangde2%、0.5%ji0.8%shiduitdisanjufanyingdeyingxiang。

圖2 3 種催化劑的催化效率對比

diyoulidutdisanjutidehecheng

congtu3kandao，zaiqitatiaojianxiangtongdeqingkuangxia，suizhup100yongliangdezengjia，fanyingsulvjiakuai，tongshi—ncojituanhanliangyousuojianshao。cuihuajiyongliangtaishaoshi，jishiyanchangfanyingshijian，—ncohanliangrenggaoyu12%；ercuihuajiyongliangguogaoshi，daliangcanliudecuihuajizaiyidingchengdushangyingxianglechanpindexingneng。shiyanbiaoming，p100yongliangwei0.5%jiaoheshi。

圖3 催化劑用量對TDI三聚反應的影響

diyoulidutdisanjutidehecheng

lingwai，cuihuajidedijiafangshiyehuiyingxiangsanjufanying。shiyanbiaoming，ruoyicixingjiarucuihuaji，dantimashangjuliefanying，daliangfangre，jubuwendukeshangsheng10 ℃，fanyingwuhuoxingdezengjiakenengdaozhichanwudexiangduifenzizhiliangzengjia、fenbubiankuan，shengchengdaliangdegaojuwu，shichanwudenianduzengjia、yansejiashen、chanpinxingnengxiajiang。ercaiyongcusuandingzhixishicuihuajihouzhudidijiadefangshi，nenghenhaodikongzhifanyingwendu。

結論

caiyongp100weicuihuajihechengtdisanjuti，shiyanbiaominggaicuihuajicuihuahuoxinggao、cuihuasulvkuai，cuihuaxiaoguojiao dmp－30 hek-15hao。