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北京石油化工学院2026年研究生招生接收调剂公告
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kadizhijia

金虫 (小有名气)

[求助] 介孔二氧化硅合成出现大量微米级块状物质

我是合成介孔二氧化硅的新手,体系:0.1gCTAB超声溶解于48mL水中,加入0.35mL2M氢氧化钠,80度机械搅拌30分钟。滴加0.5mLTEOS。80度机械搅拌2h.离心后用水洗和醇洗。还未进行煅烧,拿去测SEM之后出现了很多微米级块状物体,样品均一性也不好,请问哪位可以给些指导呀?谢谢

介孔二氧化硅合成出现大量微米级块状物质
1_m001.jpg


介孔二氧化硅合成出现大量微米级块状物质-1
1_m008.jpg
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阳光西骑士

木虫 (正式写手)

Synthesis of FITC–APTES

A solution of FITC (8.6 mg) in anhydrous ethanol (2 mL) was mixed with APTES (0.197 mL) and then the mixture was stirred at room temperature for 24 h. The prepared FITC–APTES stock solution was kept at 4 °C.
Synthesis of amino-modified MSNs (denoted as MSNs-NH2)

The synthesis of MSNs-NH2 was similar to that of magnetic MSNs-NH2.18 Typically, 0.3 g CTAB and 0.1 g PVP30 were added to a solution containing 90 mL of deionized water and 60 mL of methanol. The solution was adjusted to pH 10.2 by an ammonia solution, and then 600 μL TEOS and 50 μL APTES were added. After stirring for 2.5 h at room temperature, the resultant particles were separated and washed with ethanol and water. The extraction of organic templates for the as-synthesized particles was performed by dispersing these particles into 50 mL of a mixed solution of ethanol and NH4NO3 (0.3 g) at 60 °C for 1 h. The synthesis of FITC-labeled MSNs-NH2 is similar to that of the unlabeled ones, except that FITC-APTES (50 μL) and APTES were added together during the condensation process.
3楼2016-12-15 22:39:55
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kadizhijia

金虫 (小有名气)

有注意到合成过程不出现泡沫,TEOS滴加速度大概20s0.1mL,请问操作上还有什么其他需要注意的吗?谢谢
2楼2016-12-15 14:07:07
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阳光西骑士

木虫 (正式写手)

引用回帖:
3楼: Originally posted by 阳光西骑士 at 2016-12-15 22:39:55
Synthesis of FITC–APTES

A solution of FITC (8.6 mg) in anhydrous ethanol (2 mL) was mixed with APTES (0.197 mL) and then the mixture was stirred at room temperature for 24 h. The prepared FITC–A ...

TEM如图 虽然产率不高 但是可以做出来
介孔二氧化硅合成出现大量微米级块状物质-2
c5ra01281c-f1_hi-res.gif

4楼2016-12-15 22:42:20
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kadizhijia

金虫 (小有名气)

引用回帖:
4楼: Originally posted by 阳光西骑士 at 2016-12-15 22:42:20
TEM如图 虽然产率不高 但是可以做出来

c5ra01281c-f1_hi-res.gif
...

谢谢您的回复,请问 这个合成出的结果是MSN 吗?看您发的内容好像是MSN-NH2。请问您用这个方法合成过吗?另外,我查阅了大量的文献大部分都是采用的我所述的方法,请问你当初为什么没有采用我所述的方法呢?
5楼2016-12-16 09:26:07
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