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zcyjdd

铜虫 (初入文坛)

[求助] CTAB法合成介孔二氧化硅碰到的问题,急 已有5人参与

各位虫友,我们最近利用CTAB+TOES+氨水+APTES合成氨基修饰的介孔二氧化硅颗粒。但是合成的颗粒在TEM下,大部分好像是实心的,见下图。
我用的方法如下:
(1)(CTAB, 1.00 g) was first dissolved in 50ml of pure water by heating.
(2)After cooling to room temperature, aqueous ammonia (13ml) and ethanol (75 ml) were added.
(3)The mixture was stirred for 15 min and TEOS (1.94 ml) added rapidly while stirring was continued.
(4)TEOS (30 ml) and APTES (30 ml) were introduced 30 min later. The mixture was allowed to stir for 2h to give rise to white precipitates.
(5)The solid product was filtered, washed with deionized water and methanol, and dried in air.
(6)To remove the surfactant template (CTAB), the white powder was refluxed for 16h in a solution of 1.00ml of HCl (37%) and 80.00ml of methanol followed by extensively washing with deionized water and methanol.
        
        从TEM上看,大部分都是实心颗粒,只有少一部分是介孔颗粒。如何从实验上进行调整呢?
        另外,我们还从公司买了一部分没有修饰氨基的介孔二氧化硅颗粒,如何进行氨基修饰呢?是否有较为成熟的实验方法?谢谢大家!由于之前从来没有做过化学合成的实验,所以希望大家在实验细节上给一些建议,甚至包括回流的条件。非常感谢!!!
CTAB法合成介孔二氧化硅碰到的问题,急
sample-1414.jpg


CTAB法合成介孔二氧化硅碰到的问题,急-1
sample-1405.jpg


CTAB法合成介孔二氧化硅碰到的问题,急-2
sample-1410.jpg
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xinyuanhappy

至尊木虫 (知名作家)

引用回帖:
19楼: Originally posted by qiujichuan at 2014-06-09 08:37:26
用乙醇超声洗几遍就可以?...

3-4遍吧!
20楼2014-06-09 08:38:43
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gaoxin7620

木虫 (著名写手)

跳虫

【答案】应助回帖

感谢参与,应助指数 +1
TEOS (30 ml) and APTES (30 ml) were introduced 30 min later,这个量也太吓人了吧,第三步不是已经加过TEOS了吗,第四步到底是什么意思
Behappy!
2楼2014-02-28 17:48:04
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zcyjdd

铜虫 (初入文坛)

更正一下,TEOS (30 微升) and APTES (微升) were introduced 30 min later
3楼2014-02-28 17:49:15
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zcyjdd

铜虫 (初入文坛)

引用回帖:
2楼: Originally posted by gaoxin7620 at 2014-02-28 17:48:04
TEOS (30 ml) and APTES (30 ml) were introduced 30 min later,这个量也太吓人了吧,第三步不是已经加过TEOS了吗,第四步到底是什么意思

更正一下,TEOS (30 微升) and APTES (微升) were introduced 30 min later
4楼2014-02-28 17:53:15
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