工(gong)藝流(liu)程(cheng)簡述： ①蒸(zheng)(zheng)餾(liu)(liu) 向 500L 反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)釜內投(tou)(tou)入(ru)(ru)(ru)(ru)乙(yi)醇(chun)(chun)鈉(na)乙(yi)醇(chun)(chun)溶液蒸(zheng)(zheng)餾(liu)(liu) 1 小(xiao)(xiao)(xiao)(xiao)時(shi)，蒸(zheng)(zheng)出的乙(yi)醇(chun)(chun)水(shui)(shui)冷(leng)(leng)(leng)(leng)、深冷(leng)(leng)(leng)(leng)二級冷(leng)(leng)(leng)(leng)凝(ning)回(hui)(hui)(hui)收(shou)(shou)，回(hui)(hui)(hui)收(shou)(shou)的乙(yi)醇(chun)(chun)作為 副(fu)產品出售(shou)，未(wei)(wei)冷(leng)(leng)(leng)(leng)凝(ning)的乙(yi)醇(chun)(chun)活(huo)性炭吸(xi)(xi)(xi)(xi)附后(hou)(hou) 15 米(mi)(mi)排(pai)(pai)氣(qi)(qi)筒(tong)(tong)排(pai)(pai)空。蒸(zheng)(zheng)餾(liu)(liu)完畢，加入(ru)(ru)(ru)(ru)適量乙(yi)酸(suan)(suan)(suan)乙(yi)酯(zhi)，攪拌反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)半小(xiao)(xiao)(xiao)(xiao)時(shi)（處(chu)(chu)理(li)(li)游離堿）。 ②酯(zhi)化(hua)(hua)(hua)(hua)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying) 投(tou)(tou)入(ru)(ru)(ru)(ru)碳(tan)酸(suan)(suan)(suan)二乙(yi)酯(zhi)、間苯(ben)(ben)(ben)(ben)(ben)氧基(ji)苯(ben)(ben)(ben)(ben)(ben)乙(yi)腈，保溫反(fan)(fan)應(ying)(ying)(ying)(ying)(ying) 1 小(xiao)(xiao)(xiao)(xiao)時(shi)。酯(zhi)化(hua)(hua)(hua)(hua)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)收(shou)(shou)率以間苯(ben)(ben)(ben)(ben)(ben)甲(jia)(jia)(jia)(jia)氧基(ji)苯(ben)(ben)(ben)(ben)(ben)乙(yi)腈計(ji) 98%。 ③甲(jia)(jia)(jia)(jia)基(ji)化(hua)(hua)(hua)(hua)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying) 酯(zhi)化(hua)(hua)(hua)(hua)完畢，滴(di)加碳(tan)酸(suan)(suan)(suan)二甲(jia)(jia)(jia)(jia)酯(zhi)，約(yue) 1 小(xiao)(xiao)(xiao)(xiao)時(shi)滴(di)完，繼(ji)續反(fan)(fan)應(ying)(ying)(ying)(ying)(ying) 4 小(xiao)(xiao)(xiao)(xiao)時(shi)。甲(jia)(jia)(jia)(jia)基(ji)化(hua)(hua)(hua)(hua)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)收(shou)(shou)率以酯(zhi)化(hua)(hua)(hua)(hua)物(wu)計(ji) 65%。 ④酸(suan)(suan)(suan)化(hua)(hua)(hua)(hua) 1 甲(jia)(jia)(jia)(jia)基(ji)化(hua)(hua)(hua)(hua)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)結(jie)束后(hou)(hou)，冷(leng)(leng)(leng)(leng)卻 2 小(xiao)(xiao)(xiao)(xiao)時(shi)，投(tou)(tou)入(ru)(ru)(ru)(ru)水(shui)(shui)、15%鹽酸(suan)(suan)(suan)酸(suan)(suan)(suan)洗(xi)，產生的二氧化(hua)(hua)(hua)(hua)碳(tan)直接排(pai)(pai)空。 ⑤靜(jing)置(zhi)分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng) 1 酸(suan)(suan)(suan)化(hua)(hua)(hua)(hua)結(jie)束后(hou)(hou)，開(kai)啟攪拌 10 分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)鐘(zhong)(zhong)，靜(jing)置(zhi)分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng) 30 分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)鐘(zhong)(zhong)，油(you)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)入(ru)(ru)(ru)(ru)專用(yong)桶，水(shui)(shui)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)用(yong)甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu)。 ⑥萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu) 水(shui)(shui)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)加甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu) 30 分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)鐘(zhong)(zhong)，甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)與油(you)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)合(he)并(bing)(bing)，水(shui)(shui)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)重(zhong)復萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu)一次，甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)仍與油(you)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)合(he)并(bing)(bing)，水(shui)(shui)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)排(pai)(pai)入(ru)(ru)(ru)(ru)污(wu)水(shui)(shui)處(chu)(chu)理(li)(li)系統。 ⑦蒸(zheng)(zheng)餾(liu)(liu) 1 將甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)油(you)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)抽回(hui)(hui)(hui)釜中蒸(zheng)(zheng)餾(liu)(liu) 3 小(xiao)(xiao)(xiao)(xiao)時(shi)，收(shou)(shou)集正沸得甲(jia)(jia)(jia)(jia)化(hua)(hua)(hua)(hua)物(wu)，蒸(zheng)(zheng)出的甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)經(jing)水(shui)(shui)冷(leng)(leng)(leng)(leng)、 深冷(leng)(leng)(leng)(leng)二級冷(leng)(leng)(leng)(leng)凝(ning)回(hui)(hui)(hui)收(shou)(shou)， 回(hui)(hui)(hui)收(shou)(shou)的甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)去(qu)萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu)工(gong)段，未(wei)(wei)冷(leng)(leng)(leng)(leng)凝(ning)的甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)廢(fei)氣(qi)(qi) 活(huo)性炭吸(xi)(xi)(xi)(xi)附后(hou)(hou) 15 米(mi)(mi)排(pai)(pai)氣(qi)(qi)筒(tong)(tong)排(pai)(pai)空。蒸(zheng)(zheng)餾(liu)(liu)殘(can)渣(zha)委托(tuo)焚燒(shao)。 ⑧水(shui)(shui)解反(fan)(fan)應(ying)(ying)(ying)(ying)(ying) 碳(tan)用(yong)稀酸(suan)(suan)(suan)噴淋吸(xi)(xi)(xi)(xi)收(shou)(shou)，尾氣(qi)(qi) 15 米(mi)(mi)高排(pai)(pai)氣(qi)(qi)筒(tong)(tong)排(pai)(pai)空。 ⑨酸(suan)(suan)(suan)化(hua)(hua)(hua)(hua) 2 將水(shui)(shui)解液冷(leng)(leng)(leng)(leng)卻 2 小(xiao)(xiao)(xiao)(xiao)時(shi)，加水(shui)(shui)移(yi)至(zhi) 1000L 處(chu)(chu)理(li)(li)釜中，攪拌滴(di)加 15%鹽酸(suan)(suan)(suan)酸(suan)(suan)(suan)化(hua)(hua)(hua)(hua)，約(yue) 1 小(xiao)(xiao)(xiao)(xiao)時(shi)滴(di)完。酸(suan)(suan)(suan)化(hua)(hua)(hua)(hua) 2 反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)收(shou)(shou)率以菲諾(nuo)洛(luo)芬(fen)(fen)鈉(na)計(ji) 100%。 ⑩靜(jing)置(zhi)分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng) 2 攪拌 10 分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)鐘(zhong)(zhong)，靜(jing)置(zhi)分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng) 30 分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)鐘(zhong)(zhong)，將有機(ji)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)入(ru)(ru)(ru)(ru)專用(yong)桶中，水(shui)(shui)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)用(yong)甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu)。 ?萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu) 水(shui)(shui)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)用(yong)甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu) 30 分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)鐘(zhong)(zhong)，甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)并(bing)(bing)入(ru)(ru)(ru)(ru)有機(ji)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)，排(pai)(pai)出水(shui)(shui)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)重(zhong)復萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu)，甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)仍并(bing)(bing)入(ru)(ru)(ru)(ru)有機(ji)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)，排(pai)(pai)出水(shui)(shui)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)再次萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu)，甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)再并(bing)(bing)入(ru)(ru)(ru)(ru)有機(ji)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)，水(shui)(shui)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)去(qu)污(wu)水(shui)(shui)處(chu)(chu)理(li)(li)系統。 ?堿化(hua)(hua)(hua)(hua)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying) 萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu)結(jie)束后(hou)(hou)，將甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)與有機(ji)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)合(he)并(bing)(bing)抽回(hui)(hui)(hui)釜中，投(tou)(tou)入(ru)(ru)(ru)(ru) 5%液堿和水(shui)(shui)堿化(hua)(hua)(hua)(hua)1 小(xiao)(xiao)(xiao)(xiao)時(shi)，得菲諾(nuo)洛(luo)芬(fen)(fen)鈉(na)鹽溶液。堿化(hua)(hua)(hua)(hua)反(fan)(fan)應(ying)(ying)(ying)(ying)(ying)收(shou)(shou)率以 菲諾(nuo)洛(luo)芬(fen)(fen)酸(suan)(suan)(suan)計(ji) 100%。 ?靜(jing)置(zhi)分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng) 3 將鈉(na)鹽溶液靜(jing)置(zhi)分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng) 30 分(fen)(fen)(fen)(fen)(fen)(fen)(fen)(fen)鐘(zhong)(zhong)，排(pai)(pai)出有機(ji)層(ceng)(ceng)(ceng)(ceng)(ceng)(ceng)蒸(zheng)(zheng)餾(liu)(liu)回(hui)(hui)(hui)收(shou)(shou)處(chu)(chu)理(li)(li) 1 小(xiao)(xiao)(xiao)(xiao)時(shi)，甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)經(jing)水(shui)(shui)冷(leng)(leng)(leng)(leng)、深冷(leng)(leng)(leng)(leng)二級冷(leng)(leng)(leng)(leng)凝(ning)回(hui)(hui)(hui)收(shou)(shou)后(hou)(hou)去(qu)萃(cui)(cui)(cui)(cui)取(qu)(qu)(qu)工(gong)段，未(wei)(wei)冷(leng)(leng)(leng)(leng)凝(ning)的甲(jia)(jia)(jia)(jia)苯(ben)(ben)(ben)(ben)(ben)廢(fei)氣(qi)(qi)活(huo)性炭吸(xi)(xi)(xi)(xi)附后(hou)(hou) 15 米(mi)(mi)排(pai)(pai)氣(qi)(qi)筒(tong)(tong)排(pai)(pai)空。蒸(zheng)(zheng)餾(liu)(liu)殘(can)渣(zha)

碳用稀酸(suan)噴淋吸(xi)收(shou)，尾(wei)氣(qi)(qi)(qi) 15 米高(gao)排(pai)(pai)(pai)氣(qi)(qi)(qi)筒(tong)(tong)排(pai)(pai)(pai)空(kong)。 ?萃(cui)取(qu)(qu) 將(jiang)鈉(na)鹽(yan)溶(rong)液(ye)用甲(jia)苯(ben)(ben)萃(cui)取(qu)(qu) 30 分鐘(zhong)(zhong)， 重復(fu)三次，分別排(pai)(pai)(pai)出的(de)(de)有機(ji)層(ceng)合并蒸(zheng)(zheng)餾(liu)回(hui)收(shou)處理(li) 1 小(xiao)(xiao)(xiao)時，蒸(zheng)(zheng)出的(de)(de)甲(jia)苯(ben)(ben)水冷(leng)(leng)(leng)、深冷(leng)(leng)(leng)二級冷(leng)(leng)(leng)凝(ning)(ning)回(hui)收(shou)后去萃(cui)取(qu)(qu)工段，未冷(leng)(leng)(leng)凝(ning)(ning)的(de)(de)甲(jia)苯(ben)(ben)廢(fei)(fei)活性(xing)炭(tan)吸(xi)附(fu)后 15 米排(pai)(pai)(pai)氣(qi)(qi)(qi)筒(tong)(tong)排(pai)(pai)(pai)空(kong)。蒸(zheng)(zheng)餾(liu)殘渣(zha)委托焚燒(shao)。 ?脫(tuo)(tuo)色(se)過濾 將(jiang)鈉(na)鹽(yan)溶(rong)液(ye)抽入(ru)(ru)(ru)(ru) 1000L 反(fan)應(ying)(ying)(ying)釜(fu)內(nei)(nei)，攪拌(ban)升溫 30 分鐘(zhong)(zhong)后，加入(ru)(ru)(ru)(ru)活性(xing)炭(tan)，保溫脫(tuo)(tuo)色(se) 1 小(xiao)(xiao)(xiao)時。將(jiang)脫(tuo)(tuo)色(se)液(ye)通過過濾器壓濾，濾液(ye)進(jin)入(ru)(ru)(ru)(ru) 1000L 成鹽(yan)釜(fu)內(nei)(nei)，活性(xing)炭(tan)渣(zha)委托焚燒(shao)。 ?成鹽(yan)反(fan)應(ying)(ying)(ying)在成鹽(yan)釜(fu)中(zhong)(zhong)(zhong)，投(tou)入(ru)(ru)(ru)(ru)純化水、乙(yi)(yi)醇(chun)，攪拌(ban)升溫 30 分鐘(zhong)(zhong)，加入(ru)(ru)(ru)(ru) EDTA 攪拌(ban) 5分鐘(zhong)(zhong)，滴加經(jing)脫(tuo)(tuo)色(se)處理(li)的(de)(de) 15%氯(lv)化鈣(gai)(gai)水溶(rong)液(ye)，約 1 小(xiao)(xiao)(xiao)時滴完，繼續反(fan)應(ying)(ying)(ying) 1 小(xiao)(xiao)(xiao)時。成鹽(yan)反(fan)應(ying)(ying)(ying)收(shou)率以(yi)菲諾(nuo)洛(luo)(luo)芬鈉(na)計 100%。 ?冷(leng)(leng)(leng)卻結(jie)晶、離(li)心(xin)分離(li) 將(jiang)反(fan)應(ying)(ying)(ying)液(ye)冷(leng)(leng)(leng)卻結(jie)晶 3 小(xiao)(xiao)(xiao)時。將(jiang)成鹽(yan)釜(fu)內(nei)(nei)物料放入(ru)(ru)(ru)(ru)離(li)心(xin)機(ji)離(li)心(xin) 1 小(xiao)(xiao)(xiao)時， 得菲諾(nuo)洛(luo)(luo)芬鈣(gai)(gai)濕品(pin)(pin)。離(li)心(xin)母液(ye)蒸(zheng)(zheng)餾(liu)回(hui)收(shou)處理(li) 1 小(xiao)(xiao)(xiao)時，回(hui)收(shou)的(de)(de)乙(yi)(yi)醇(chun)去成鹽(yan)工段，未冷(leng)(leng)(leng)凝(ning)(ning)的(de)(de)乙(yi)(yi)醇(chun)廢(fei)(fei)氣(qi)(qi)(qi)活性(xing)炭(tan)吸(xi)附(fu)后 15 米排(pai)(pai)(pai)氣(qi)(qi)(qi)筒(tong)(tong)排(pai)(pai)(pai)空(kong)。釜(fu)中(zhong)(zhong)(zhong)的(de)(de)廢(fei)(fei)水去污水處理(li)系統?干燥(zao) 將(jiang)菲諾(nuo)洛(luo)(luo)芬鈣(gai)(gai)濕品(pin)(pin)放入(ru)(ru)(ru)(ru)真空(kong)干燥(zao)箱內(nei)(nei)干燥(zao) 24 小(xiao)(xiao)(xiao)時， 得菲諾(nuo)洛(luo)(luo)芬鈣(gai)(gai)成品(pin)(pin)。烘干過程中(zhong)(zhong)(zhong)排(pai)(pai)(pai)出乙(yi)(yi)醇(chun)廢(fei)(fei)氣(qi)(qi)(qi)活性(xing)炭(tan)吸(xi)附(fu)后 15 米排(pai)(pai)(pai)氣(qi)(qi)(qi)筒(tong)(tong)排(pai)(pai)(pai)空(kong)。本工藝中(zhong)(zhong)(zhong)甲(jia)苯(ben)(ben)、乙(yi)(yi)醇(chun)為溶(rong)劑，EDTA 為絡合劑。