小型高壓(ya)反(fan)應釜(fu)用連續(xu)加(jia)料法制備聚醚多元醇,其(qi)特(te)征(zheng)在于將環氧單體70-90.起始劑10-30.催(cui)化(hua)劑30-200×10↑［-6］和質子酸0-100×10↑［-6］利(li)用如 下步驟制備,其(qi)中(zhong)的含量均為重量百分(fen)比:
步驟(zou)1:按(an)配方稱(cheng)取質子(zi)酸.起(qi)始劑.催化劑在容(rong)器(qi)中混(hun)和(he)均(jun)勻(yun),并轉入高壓反(fan)應釜(fu)內,高壓反(fan)應釜(fu)密封;含(han)量均(jun)為(wei)重 量百(bai)分比(bi);
步(bu)驟2:連(lian)(lian)(lian)(lian)接(jie)(jie)氮(dan)氣(qi)(qi)瓶(ping)與(yu)(yu)(yu)加料(liao)罐(guan)(guan),先打開(kai)(kai)(kai)氮(dan)氣(qi)(qi)瓶(ping)閥(fa),調氮(dan)氣(qi)(qi)瓶(ping)減壓(ya)(ya)(ya)(ya)表壓(ya)(ya)(ya)(ya)為0.5-1MPA;接(jie)(jie)著打開(kai)(kai)(kai)加料(liao)罐(guan)(guan)與(yu)(yu)(yu)氮(dan)氣(qi)(qi)瓶(ping)連(lian)(lian)(lian)(lian)接(jie)(jie)閥(fa),再打開(kai)(kai)(kai)加料(liao)罐(guan)(guan)與(yu)(yu)(yu)高(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)反應(ying) 釜(fu)(fu)連(lian)(lian)(lian)(lian)接(jie)(jie)進料(liao)閥(fa),用(yong)氮(dan)氣(qi)(qi)置換3-5次(ci)排除高(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)反應(ying)釜(fu)(fu)內空(kong)(kong)氣(qi)(qi)后(hou),關(guan)閉加料(liao)罐(guan)(guan)與(yu)(yu)(yu)高(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)反應(ying)釜(fu)(fu)連(lian)(lian)(lian)(lian)接(jie)(jie)進料(liao)閥(fa),關(guan)閉加料(liao)罐(guan)(guan)與(yu)(yu)(yu)氮(dan)氣(qi)(qi)瓶(ping)連(lian)(lian)(lian)(lian)接(jie)(jie)閥(fa);設定(ding)高(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)反應(ying)釜(fu)(fu)溫(wen)度(du)為 130-140℃,高(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)反應(ying)釜(fu)(fu)開(kai)(kai)(kai)始(shi)升溫(wen),當溫(wen)度(du)到80-100℃打開(kai)(kai)(kai)高(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)反應(ying)釜(fu)(fu)抽氣(qi)(qi)閥(fa)與(yu)(yu)(yu)抽真(zhen)空(kong)(kong)裝置連(lian)(lian)(lian)(lian)接(jie)(jie),開(kai)(kai)(kai)始(shi)脫除反應(ying)體系內的水分0.5-1小時后(hou),關(guan)閉 抽氣(qi)(qi)閥(fa),斷開(kai)(kai)(kai)高(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)反應(ying)釜(fu)(fu)抽氣(qi)(qi)閥(fa)與(yu)(yu)(yu)抽真(zhen)空(kong)(kong)裝置的連(lian)(lian)(lian)(lian)接(jie)(jie);
步驟3:打(da)(da)開加料(liao)罐(guan)與(yu)氮(dan)(dan)氣瓶連接閥,再(zai)打(da)(da)開加料(liao)罐(guan)與(yu)高壓(ya)反應釜連接進(jin)料(liao)閥,再(zai)次用氮(dan)(dan)氣置換3-5次以(yi) 排除(chu)高壓(ya)反應釜內水分,關(guan)閉加料(liao)罐(guan)與(yu)高壓(ya)反應釜連接進(jin)料(liao)閥,關(guan)閉加料(liao)罐(guan)與(yu)氮(dan)(dan)氣瓶連接閥;
步驟4:打開(kai)抽氣(qi)閥與抽真空裝置連接,抽高壓反應釜使其真空度為 0.090-0.095MPA后,關(guan)閉抽氣(qi)閥;
步驟5:將加料罐與(yu)(yu)抽真空(kong)裝(zhuang)置(zhi)連接(jie),抽加料罐內(nei)真空(kong)度為(wei)0.098-0.1MPA后,斷開加料罐與(yu)(yu)抽真空(kong) 裝(zhuang)置(zhi)的連接(jie),關閉抽真空(kong)裝(zhuang)置(zhi),利用(yong)加料罐內(nei)真空(kong)度吸入環(huan)氧單體;
步(bu)驟6:高壓(ya)(ya)(ya)(ya)反(fan)應(ying)(ying)(ying)釜升(sheng)溫(wen)到130-140℃恒溫(wen)后,打開加料罐與(yu)氮氣瓶(ping)連(lian)接(jie)(jie)閥(fa),再打開加 料罐與(yu)高壓(ya)(ya)(ya)(ya)反(fan)應(ying)(ying)(ying)釜連(lian)接(jie)(jie)的(de)進料閥(fa),用氮氣壓(ya)(ya)(ya)(ya)入環氧單體,當(dang)高壓(ya)(ya)(ya)(ya)反(fan)應(ying)(ying)(ying)釜壓(ya)(ya)(ya)(ya)力為0.2-0.25MPA時,關閉高壓(ya)(ya)(ya)(ya)反(fan)應(ying)(ying)(ying)釜與(yu)加料罐連(lian)接(jie)(jie)的(de)進料閥(fa),關閉氮氣瓶(ping)閥(fa); 當(dang)高壓(ya)(ya)(ya)(ya)反(fan)應(ying)(ying)(ying)釜溫(wen)度上升(sheng)并伴有壓(ya)(ya)(ya)(ya)力下降時,反(fan)應(ying)(ying)(ying)誘導期完(wan)成,打開氮氣瓶(ping)閥(fa),調減壓(ya)(ya)(ya)(ya)表壓(ya)(ya)(ya)(ya)為0.5-1MPA;
步驟7:打開高(gao)(gao)壓(ya)(ya)反(fan)(fan)應(ying)釜(fu)與(yu)(yu)加(jia)(jia)(jia)料(liao)(liao)罐連接的(de)(de)進料(liao)(liao)閥(fa), 把(ba)剩余的(de)(de)環氧(yang)單(dan)體(ti)(ti)用氮氣持續(xu)(xu)加(jia)(jia)(jia)入高(gao)(gao)壓(ya)(ya)反(fan)(fan)應(ying)釜(fu),加(jia)(jia)(jia)料(liao)(liao)過(guo)程中調節高(gao)(gao)壓(ya)(ya)反(fan)(fan)應(ying)釜(fu)與(yu)(yu)加(jia)(jia)(jia)料(liao)(liao)罐連接的(de)(de)進料(liao)(liao)閥(fa)使高(gao)(gao)壓(ya)(ya)反(fan)(fan)應(ying)釜(fu)內壓(ya)(ya)力(li)(li)在0.4MPA以下(xia),連續(xu)(xu)用氮氣壓(ya)(ya)入環氧(yang)單(dan) 體(ti)(ti),1-5小(xiao)時后(hou),當(dang)高(gao)(gao)壓(ya)(ya)反(fan)(fan)應(ying)釜(fu)內的(de)(de)壓(ya)(ya)力(li)(li)出(chu)現(xian)(xian)持續(xu)(xu)上升至外部氮氣的(de)(de)壓(ya)(ya)力(li)(li)時,關閉高(gao)(gao)壓(ya)(ya)反(fan)(fan)應(ying)釜(fu)與(yu)(yu)加(jia)(jia)(jia)料(liao)(liao)罐連接的(de)(de)進料(liao)(liao)閥(fa),30分(fen)鐘(zhong)后(hou)高(gao)(gao)壓(ya)(ya)反(fan)(fan)應(ying)釜(fu)壓(ya)(ya)力(li)(li)不再下(xia)降時,加(jia)(jia)(jia) 料(liao)(liao)完成,關閉氮氣瓶閥(fa).繼續(xu)(xu)反(fan)(fan)應(ying)1H后(hou)降溫出(chu)料(liao)(liao),即得聚(ju)(ju)醚(mi)多元(yuan)醇(chun).具有(you)設備簡單(dan),能實現(xian)(xian)連續(xu)(xu)加(jia)(jia)(jia)料(liao)(liao),且所合成聚(ju)(ju)醚(mi)具有(you)平均官能度高(gao)(gao),分(fen)子(zi)量分(fen)布窄(zhai),聚(ju)(ju)合反(fan)(fan)應(ying)平穩可(ke)控的(de)(de)優點.
