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反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)用(yong)(yong)(yong)(yong)連(lian)(lian)(lian)(lian)(lian)(lian)續(xu)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)法(fa)制備 聚(ju)醚多元醇,其特征(zheng)在于將環氧(yang)(yang)單(dan)(dan)體(ti)(ti)70-90.起(qi)始(shi)劑(ji)(ji)10-30.催化劑(ji)(ji)30-200×10↑［-6］和(he)(he)質(zhi)子酸0-100×10↑［-6］利用(yong)(yong)(yong)(yong)如(ru)下步(bu)(bu)驟(zou)制 備,其中的含(han)量均為重量百(bai)分(fen)比: 步(bu)(bu)驟(zou)1:按(an)配方(fang)稱取質(zhi)子酸.起(qi)始(shi)劑(ji)(ji).催化劑(ji)(ji)在容器中混(hun)和(he)(he)均勻,并轉入(ru)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)內,高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)密封(feng);所述含(han)量均為重量百(bai) 分(fen)比; 步(bu)(bu)驟(zou)2:連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)瓶(ping)(ping)與(yu)(yu)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan),先打(da)(da)開(kai)(kai)(kai)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)瓶(ping)(ping)閥(fa)(fa)(fa)(fa),調氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)瓶(ping)(ping)減壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)表壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)為0.5-1MPA;接(jie)(jie)(jie)(jie)(jie)(jie)著打(da)(da)開(kai)(kai)(kai)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)瓶(ping)(ping)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)閥(fa)(fa)(fa)(fa),再打(da)(da)開(kai)(kai)(kai)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)連(lian)(lian)(lian)(lian)(lian)(lian) 接(jie)(jie)(jie)(jie)(jie)(jie)進(jin)料(liao)(liao)(liao)(liao)(liao)閥(fa)(fa)(fa)(fa),用(yong)(yong)(yong)(yong)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)置(zhi)換(huan)3-5次(ci)排(pai)除(chu)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)內空(kong)氣(qi)(qi)(qi)(qi)后(hou)(hou),關(guan)(guan)閉(bi)(bi)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)進(jin)料(liao)(liao)(liao)(liao)(liao)閥(fa)(fa)(fa)(fa),關(guan)(guan)閉(bi)(bi)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)瓶(ping)(ping)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)閥(fa)(fa)(fa)(fa);設定(ding)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)溫度(du)(du)為 130-140℃,高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)開(kai)(kai)(kai)始(shi)升(sheng)(sheng)溫,當溫度(du)(du)到80-100℃打(da)(da)開(kai)(kai)(kai)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)抽(chou)(chou)氣(qi)(qi)(qi)(qi)閥(fa)(fa)(fa)(fa)與(yu)(yu)抽(chou)(chou)真(zhen)空(kong)裝(zhuang)(zhuang)置(zhi)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie),開(kai)(kai)(kai)始(shi)脫除(chu)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)體(ti)(ti)系內的水(shui)(shui)分(fen)0.5-1小時后(hou)(hou),關(guan)(guan)閉(bi)(bi) 抽(chou)(chou)氣(qi)(qi)(qi)(qi)閥(fa)(fa)(fa)(fa),斷開(kai)(kai)(kai)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)抽(chou)(chou)氣(qi)(qi)(qi)(qi)閥(fa)(fa)(fa)(fa)與(yu)(yu)抽(chou)(chou)真(zhen)空(kong)裝(zhuang)(zhuang)置(zhi)的連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie); 步(bu)(bu)驟(zou)3:打(da)(da)開(kai)(kai)(kai)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)瓶(ping)(ping)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)閥(fa)(fa)(fa)(fa),再打(da)(da)開(kai)(kai)(kai)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)進(jin)料(liao)(liao)(liao)(liao)(liao)閥(fa)(fa)(fa)(fa),再次(ci)用(yong)(yong)(yong)(yong)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)置(zhi)換(huan)3-5次(ci)以(yi) 排(pai)除(chu)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)內水(shui)(shui)分(fen),關(guan)(guan)閉(bi)(bi)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)進(jin)料(liao)(liao)(liao)(liao)(liao)閥(fa)(fa)(fa)(fa),關(guan)(guan)閉(bi)(bi)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)瓶(ping)(ping)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)閥(fa)(fa)(fa)(fa); 步(bu)(bu)驟(zou)4:打(da)(da)開(kai)(kai)(kai)抽(chou)(chou)氣(qi)(qi)(qi)(qi)閥(fa)(fa)(fa)(fa)與(yu)(yu)抽(chou)(chou)真(zhen)空(kong)裝(zhuang)(zhuang)置(zhi)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie),抽(chou)(chou)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)使(shi)其真(zhen)空(kong)度(du)(du)為 0.090-0.095MPA后(hou)(hou),關(guan)(guan)閉(bi)(bi)抽(chou)(chou)氣(qi)(qi)(qi)(qi)閥(fa)(fa)(fa)(fa); 步(bu)(bu)驟(zou)5:將加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)抽(chou)(chou)真(zhen)空(kong)裝(zhuang)(zhuang)置(zhi)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie),抽(chou)(chou)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)內真(zhen)空(kong)度(du)(du)為0.098-0.1MPA后(hou)(hou),斷開(kai)(kai)(kai)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)抽(chou)(chou)真(zhen)空(kong) 裝(zhuang)(zhuang)置(zhi)的連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie),關(guan)(guan)閉(bi)(bi)抽(chou)(chou)真(zhen)空(kong)裝(zhuang)(zhuang)置(zhi),利用(yong)(yong)(yong)(yong)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)內真(zhen)空(kong)度(du)(du)吸入(ru)環氧(yang)(yang)單(dan)(dan)體(ti)(ti); 步(bu)(bu)驟(zou)6:高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)升(sheng)(sheng)溫到130-140℃恒(heng)溫后(hou)(hou),打(da)(da)開(kai)(kai)(kai)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)瓶(ping)(ping)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)閥(fa)(fa)(fa)(fa),再打(da)(da)開(kai)(kai)(kai)加(jia)(jia)(jia) 料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)與(yu)(yu)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)的進(jin)料(liao)(liao)(liao)(liao)(liao)閥(fa)(fa)(fa)(fa),用(yong)(yong)(yong)(yong)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)入(ru)環氧(yang)(yang)單(dan)(dan)體(ti)(ti),當高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)力為0.2-0.25MPA時,關(guan)(guan)閉(bi)(bi)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)與(yu)(yu)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)的進(jin)料(liao)(liao)(liao)(liao)(liao)閥(fa)(fa)(fa)(fa),關(guan)(guan)閉(bi)(bi)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)瓶(ping)(ping)閥(fa)(fa)(fa)(fa); 當高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)溫度(du)(du)上升(sheng)(sheng)并伴有壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)力下降時,反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)誘導期(qi)完(wan)成(cheng),打(da)(da)開(kai)(kai)(kai)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)瓶(ping)(ping)閥(fa)(fa)(fa)(fa),調減壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)表壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)為0.5-1MPA; 步(bu)(bu)驟(zou)7:打(da)(da)開(kai)(kai)(kai)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)與(yu)(yu)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)的進(jin)料(liao)(liao)(liao)(liao)(liao)閥(fa)(fa)(fa)(fa), 把(ba)剩余(yu)的環氧(yang)(yang)單(dan)(dan)體(ti)(ti)用(yong)(yong)(yong)(yong)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)持(chi)續(xu)加(jia)(jia)(jia)入(ru)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu),加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)過程中調節高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)與(yu)(yu)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)的進(jin)料(liao)(liao)(liao)(liao)(liao)閥(fa)(fa)(fa)(fa)使(shi)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)內壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)力在0.4MPA以(yi)下,連(lian)(lian)(lian)(lian)(lian)(lian)續(xu)用(yong)(yong)(yong)(yong)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)入(ru)環氧(yang)(yang)單(dan)(dan) 體(ti)(ti),1-5小時后(hou)(hou),當高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)內的壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)力出(chu)現持(chi)續(xu)上升(sheng)(sheng)至外部氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)的壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)力時,關(guan)(guan)閉(bi)(bi)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)與(yu)(yu)加(jia)(jia)(jia)料(liao)(liao)(liao)(liao)(liao)罐(guan)(guan)(guan)(guan)連(lian)(lian)(lian)(lian)(lian)(lian)接(jie)(jie)(jie)(jie)(jie)(jie)的進(jin)料(liao)(liao)(liao)(liao)(liao)閥(fa)(fa)(fa)(fa),30分(fen)鐘后(hou)(hou)高(gao)(gao)(gao)(gao)(gao)(gao)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜(fu)(fu)(fu)壓(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)(ya)力不再下降時,加(jia)(jia)(jia) 料(liao)(liao)(liao)(liao)(liao)完(wan)成(cheng),關(guan)(guan)閉(bi)(bi)氮(dan)(dan)(dan)(dan)(dan)(dan)氣(qi)(qi)(qi)(qi)瓶(ping)(ping)閥(fa)(fa)(fa)(fa).繼續(xu)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)1H后(hou)(hou)降溫出(chu)料(liao)(liao)(liao)(liao)(liao),即得(de)聚(ju)醚多元醇. 所合成(cheng)聚(ju)醚具有平均官能度(du)(du)高(gao)(gao)(gao)(gao)(gao)(gao),分(fen)子量分(fen)布窄,聚(ju)合反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)平穩可控的優點.