四百九十章 侧链再变更(1 / 1)

吴总签好字后,报告到了方总的手上,方总看了看说:“这与你先前会上说的不一样,会议记录上说是60%以上,现在只有56%,差了四个百分点,这字我不签。”

王近之发火了:“我们用的是回收水解物,不是新制的。”

“回收水解物合不合格,如合格是什么指标影响收率,不合格谁允许你投入生产?”方总从文件柜里翻出管理文件,指着里面的一段文字说道:“自个看,白纸黑字写在这上面,你得改一改思维。”

文件被打回来了,一次次地修改文字细节与质量标准。这种细活王者极不喜欢干,一甩手交给了陈骨良,自个去指挥左氧侧链的合成去了。两个月的时间已到,左氧侧链合成还没有取得突破性进展,再拖下去,会被领导打屁股的。

研究所提供的侧链合成路线是乙酸乙酯与乙酸甲酯在氢钠的催化下在甲苯溶剂里反应,生成甲酰基乙酸乙酯钠盐,然后与N,N-二甲基氯化铵反应,生成侧链N,N-二甲氨基丙烯酸乙酯。

“中间的甲酰基乙酸乙酯盐很不稳定,无法中控跟踪转化率,后一步的无水要求太高,多批成品跟踪的结果,都有大量的杂质峰,反应结束后主峰含量不超过65%,课题组已试过无数的反应条件进行优化了,主峰含量并无明显提高,一减压蒸馏后,收率只有40%多一些,没有原工艺的高。”李彪奇边说边拿出一叠图谱:“我们巳经做了近二百批次的反应了,分析结果全都在这里。”

转让的资料里说摩尔收率达到64%,很显然地是把主峰含量当作摩尔收率了,高校与研究所出来的资料常有这样的情况发生,因为试剂价格贵,每次投料只投几克,导致后面的蒸馏根本无法操作,做总结时就以主峰含量替代收率,在他们的理解中,只要是产品,总能蒸馏完全分离出来的。这样的情况在技术转让时不是第一次,更不会是最后一次,原因很简单,没产业化概念而引起的。

王近之沉思了一下说:“你们加大量投一个制备甲酰基乙酸乙酯盐反应,反应毕,分成四等份,我与你们一起进行第二步反应。”

四小时后,第一步反应结束,王近之来到实验室吩咐其中一份按原收率最高的条件往下反应,另一份直接投入到二甲氨盐酸盐水溶液中搅拌。

“这不符合反应原理啊,资料报道要求无水。”听了王近之的吩咐,李彪奇当即提出疑问。

王近之挥了挥手说:“按我说的试一批吧,最坏的结果就是浪费几十克反应液,色谱出来后,对以后的实验也有指导作用。”

反应液投下去了,经水洗后再减压蒸去甲苯,得到的蒸余液呈浅红色,流动性很好,而不是高粘度的棕红色,王近之心中有种极强烈的感觉,实验成功了,当然,分析结果出来前,不能夸口,在送样品时,王近之特地向赵定岳吩咐把这样品排在第一个,一有结果,立即手机通知。

分析结果果如所料,扣除氢化油后,产品纯度达到99.2%,已经合格,只是色泽偏深些。把剩下的两份反应液按同样的方法处理,也得到相同的结果,再经蒸馏,就得到浅黄色液体。第三天,小试就进入工艺验证阶段,第五天,三批小试验证批完成,再往下制备到左氧环合酯、左氧氟羧酸、左氧成品,每一步质量指标都与老工艺相同。

“化工合成是一门实践性的科学,尽信书不如无书。”王近之对李彪奇等同事进行小试复盘时,侃侃而谈。很多学院派的人以为这么做是违背常识,可化工合成的突破往往都是对常识的突破。

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