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优花

金虫 (正式写手)

[交流] 【求助】 做聚合的朋友帮我看看

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 mba
r. 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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chensthjkl

铁虫 (著名写手)

★ ★ ★ ★ ★
优花(金币+5,VIP+0):十分感谢
Vigreux column就是带刺的分馏柱,a Dean-Stark-type condenser就是分水器。抽真空可用液氮冷凝低沸点化合物。
everythingispossible
2楼2008-09-10 12:14:53
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chensthjkl

铁虫 (著名写手)

everythingispossible
3楼2008-09-10 12:16:10
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yuyang031985

金虫 (正式写手)

我用过水冷凝的方法试过,根本看不到冷凝的东西,可能是量太少的原因。反正水和小分子量的聚合物少,抽进去也无所谓了。
说说你不开心的事让我们开心一下哈!
4楼2008-09-13 17:05:51
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polywind

木虫 (正式写手)

铁杆木虫

用带泠凝系统的旋转蒸发器可以,以酒精为冷凝液,可达-20度。
朝闻道,夕死可矣
5楼2008-09-13 20:56:05
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