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mutangyushui

银虫 (初入文坛)

[求助] 合成过程有点不懂 已有4人参与

MWHAc-UIO-66.  Typically, ZrCl4 (150 mg, 0.644 mmol) was dissolved in acetic acid (5 ml, 87.36 mmol)/DMF(40 ml, 516 mmol) to give a clear solution and continuously stirred for half an hour. Then, BDC (120 mg, 0.723 mmol) was dissolved into the solution. Finally, this mixed solution with a molar ratio of DMF:HAc:BDC:ZrCl4 of 800:135:1.12:1 was placed into a microwave oven and irradiated at 100 °C for 2 hours. The product was centrifuged at 6000 rpm for 5 min, washed three times with ethanol and dried at 60 °C overnight. The yield (based on ZrCl4) was close to 90%.
MWBA-UIO-66.  MWBA-UIO-66 was prepared according to the above process, in which ZrCl4 was dissolved in a mixture of benzoic acid/DMF with 30 equivalents of benzoic acid. The after treatment used was the same as the above procedure. The yield (based on ZrCl4) was close to 85%.


MWBA-UIO-66 was prepared according to the above process, in which ZrCl4 was dissolved in a mixture of benzoic acid/DMF with 30 equivalents of benzoic acid.
这句话的意思是苯甲酸的含量是DMF的30倍吗?那就是1200mL  这么多吗?
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urotensin

木虫 (正式写手)

【答案】应助回帖

感谢参与,应助指数 +1
是摩尔比,如上面所写acetic acid (5 ml, 87.36 mmol)/DMF(40 ml, 516 mmol) ,这样DMF是HOAc的5.9-6倍,如果DMF是benzoic acid的30 equiv的话,就是1克benzoic acid(8.2mmol), 20mL左右的DMF(0.25mol)
2楼2015-05-07 12:29:54
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mutangyushui

银虫 (初入文坛)

引用回帖:
2楼: Originally posted by urotensin at 2015-05-07 12:29:54
是摩尔比,如上面所写acetic acid (5 ml, 87.36 mmol)/DMF(40 ml, 516 mmol) ,这样DMF是HOAc的5.9-6倍,如果DMF是benzoic acid的30 equiv的话,就是1克benzoic acid(8.2mmol), 20mL左右的DMF(0.25mol)

我还是没懂 是DMF是苯甲酸的30倍还是苯甲酸是DMF的30倍
3楼2015-05-07 14:18:24
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peterflyer

木虫之王 (文学泰斗)

peterflyer


【答案】应助回帖

感谢参与,应助指数 +1
引用回帖:
3楼: Originally posted by mutangyushui at 2015-05-07 14:18:24
我还是没懂 是DMF是苯甲酸的30倍还是苯甲酸是DMF的30倍...

感觉苯甲酸的摩尔数是DMF摩尔数的30倍。
4楼2015-05-07 17:31:36
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urotensin

木虫 (正式写手)

【答案】应助回帖

引用回帖:
3楼: Originally posted by mutangyushui at 2015-05-07 14:18:24
我还是没懂 是DMF是苯甲酸的30倍还是苯甲酸是DMF的30倍...

常识上看应该是DMF过量吧,不然怎么溶解
5楼2015-05-08 14:22:24
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cx陈旋cx

新虫 (初入文坛)

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调节剂苯甲酸30当量是相对于氯化锆而言的,和溶剂DMF 无关吧
6楼2016-11-28 14:18:41
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chshch472

银虫 (小有名气)

【答案】应助回帖

与上段文字作对比:溶剂中AC/DMF的摩尔比为1/6,不太可能在后边忽然变化到1/30或者30;另外前边的数据直接给出了所有分子与ZrCl4的比例关系。
考虑后边实验的产额也低于前者,30倍也低于前一实验135倍的Ac用量,猜测这个30倍是相对于ZrCl4的倍数。
从这句话的结构来讲,确实存在较大的争议,更像是你说的这样。这文稿是英美国家的人写的么?
刚搜索了一下,是不是这篇《Microwave-assisted synthesis of UIO-66 and itsadsorption performance towards dyes》,作者是中国人,你直接发邮件给作者确定下吧。Yafeng Li@mail.ccut.edu.cn.
7楼2016-11-29 11:29:47
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