1. Ordinary copper bronze does not always give satisfactory results in the Ullmann reaction. More
uniform results are obtained if the copper bronze is prepared as suggested by Kleiderer and Adams.1
The copper bronze is treated with 2 l. of a 2% solution of iodine in acetone for 5–10 minutes. The
product is then collected on a Büchner funnel, removed, washed by stirring into a slurry with 1 l. of a
1:1 solution of concentrated hydrochloric acid in acetone, and again filtered. The copper iodide
dissolves, and the copper bronze remaining is separated by filtration and washed with acetone. It is then
dried in a vacuum desiccator. It should be used immediately.
1. 請參考U.S.EPA, Sulfur Cleanup, Test Methods for Evaluating Solid Waste, Method 3660A, 1992.
2. 稀硝酸活化才是正確的方式.
3. Sillica jel 管柱也有去硫的功能!!
4. 要當心銅粉造成分析物的分解.
铜的活化,两种方法:
1.用还原性的气体如氢气,一氧化碳,氨气热还原一下,类似于合成氨的还原性铁粉。适用于铜粉。
2.用稀硝酸活化,但这种适合于铜片或铜丝铜网
制备方法如下
[ Last edited by 梅若鸣 on 2008-10-9 at 08:42 ]
1. Ordinary copper bronze does not always give satisfactory results in the Ullmann reaction. More
uniform results are obtained if the copper bronze is prepared as suggested by Kleiderer and Adams.1
The copper bronze is treated with 2 l. of a 2% solution of iodine in acetone for 5–10 minutes. The
product is then collected on a Büchner funnel, removed, washed by stirring into a slurry with 1 l. of a
1:1 solution of concentrated hydrochloric acid in acetone, and again filtered. The copper iodide
dissolves, and the copper bronze remaining is separated by filtration and washed with acetone. It is then
dried in a vacuum desiccator. It should be used immediately.
Cu粉的活化:
5g的铜粉置于100ml干燥的蛋形瓶中,搅拌下加入50ml含有5%碘的丙酮溶液,室温剧烈搅拌30min,随后砂芯过滤,固体再放入干燥的蛋形瓶中,加入丙酮-浓盐酸(1:1)混合溶剂30ml,剧烈搅拌5 min,随后砂芯过滤。如此反复二次,然后用水,丙酮和无水乙醚洗涤,抽干,置于干燥器中保存,
偶最近也是这样做的!
问一下上面那段英文 The copper bronze is treated with 2 l. of a 2% solution of iodine in acetone for 5–10 minutes是中的2 l. 是什么意思啊?
请教楼上,我按英文的那种方法用碘的丙酮溶液操作,为什么搅拌一会后会出现乳白色混浊,是什么东西啊?应该怎么操作?