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【求助】 做聚合的朋友帮我看看
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做过聚合的朋友帮我看下下面这段有关聚合的过程,我有几个问题想请教: A typical polymerization was carried out according to the following procedure. Succinic acid (44.9 g, 0.38 mol) and isosorbide (63.4 g, 0.43 mol) were weighed into a 250 mL round-bottom glass flange reactor. The reactor was fitted with a Vigreux column and a Dean- Stark-type condenser to collect the condensation product. During the first part of the synthesis, the setup was continuously flushed with inert gas to limit oxidation and facilitate transport of water vapor. While being stirred, the mixture was heated to 180 °C using a heating mantle. Titanium(IV) n-butoxide (0.02 mol % relative to succinic acid), dissolved in toluene, was added to the melt. Subsequently, the reaction temperature was increased stepwise to maintain distillation of the formed water. The maximum reaction temperature was 250 °C. After 4 h, vacuum processing was started at 230-250 °C, with typical pressures ranging from 1 to 5 mbar. Vacuum was applied for 4 h, after which the polymer was discharged from the reactor and left to cool and solidify. 其中的“Vigreux column 和a Dean-Stark-type condenser”中文是什么意思,因为我想搭装置,要准备这些东西; 另外还想问,他反应完要抽真空,我看真空度要达到1-5mbar,这应该要用油泵抽的吧,可是这反应体系中会有水和一些小分子量的聚合物,抽到油泵中会损害油泵,这中间需要加一些什么东西来过滤或者冷凝呢,请高手们指教 [ Last edited by wizardfox on 2008-9-10 at 15:09 ] |
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