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可呼啦啦鐵蟲 (初入文壇)
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[求助]
不同直徑介孔碳小球
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急需 !有哪位大神在做,能請教一下么 趙東元院士課題組的 單分散高氮介孔碳納米小球 不同直徑的我這邊重復(fù)的 沒有做出小球來是怎么回事,是跟著如下這篇文獻(xiàn)做的 Monodisperse Ultrahigh Nitrogen-Containing Mesoporous Carbon Nanospheres from Melamine-Formaldehyde Resin DingYi Guo ,ZhaoDongYuan The mesoporous MF polymer nanospheres were synthesized through a facile aqueous emulsion polymerization self-assembly process. Typically, 0.6 g of Pluronic F127 was dissolved in 10 mL of deionized water. Then 0.6 g of TMB was added and vigorously stirred for 6 h (denoted as solutionA). 3.0 mmol of melamine, 3.0 mmol of formaldehyde aqueous solution (37 wt%), and 0.05 mL of 0.1 m NaOH aqueous solution were added to 40 mL of deionized water and stirred at 100 °C for 0.5 h for the formation of soluble prepolymerized MF resin solution (denoted as solution B).Subsequently, the solution A was added into the above solution B and stirred for another 2 h to allow the formation of the stabilized TMB/F127 emulsion droplets. Afterward, appropriate amount of HCl aqueous solution, with a mole ratio of HCl to melamine in the range of 0.27–0.53, was added and continuously stirred over 6 h. Finally, the solution turned to bright milky white. The obtained mesoporous MF polymer nanospheres were collected by centrifugation and then washed with deionized water and absolute ethanol at least three times, respectively. After drying in an oven at 60 °C overnight, the white power was preheated at 350 °C for 3 h and finally calcined at 800 °C for 2 h in nitrogen atmosphere with a heating rate of 1 °C min−1to obtain the resultant ultrahigh nitrogen-containing mesoporous carbon nanospheres (N-MCSs). The products were denoted as MF-x and N-MCSs-x (where x represents the particle size in nanometers), respectively. 問題1:HCl是濃鹽酸嗎 里邊沒有表明所用濃度 問題2:當(dāng)A溶液:F127溶液 +TMB 加入B溶液:三聚氰胺+甲醛(37%)+NaOH(0.1M) 是需要多少溫度進(jìn)行反應(yīng)呢 我看其他文獻(xiàn)一般是F127溶液加入后用的66或是70攝氏度 問題3:轉(zhuǎn)速沒有具體表明 ,只說是劇烈攪拌,我這邊看文獻(xiàn)有的說是500rpm 不知道有沒有問題 問題4:有說表面活性劑是要針管慢慢注射的,我是直接一次性加入攪拌的 |
鐵蟲 (初入文壇)
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