24小时热门版块排行榜    

Znn3bq.jpeg
查看: 2150  |  回复: 1

dxyan

木虫 (正式写手)

[求助] MIL-101的合成及纯化

采用不用HF合成MIL-101(Cr),参考文献:Chem. Mater. 2012, 24, 166。但是做了很久比表面上不去。2200左右。其中DMF洗部分也洗了3次,每次12小时,70度,但是比表面积也就2400。DMF洗涤后也用甲醇,丙酮各洗过3,4次。但是BET依旧不行,吸附仪活化也达到足够的时间。合成完后釜壁面有灰色的一层,在各种溶剂洗的过程中离心完后离心管底部有层灰色的,但是大部分是绿色。谁能帮忙分析一下会是什么原因。原料或者釜的原因吗?加HF酸的方法也试过了,水洗醇洗后,加入氟化铵,然后再水洗,醇洗。但是比表面都2000以下。氟化铵交换2次,BET才达到2200。求各位帮忙分析一下,谢谢!
Cr(NO3)3·9H2O (1.0 g, 2.5 mmol), terephthalic acid (0.42 g, 2.5 mmol), and deionized water (10 mL) were
blended and briefly sonicated resulting in a dark blue-colored suspension. The suspension was placed in a
Teflon-lined autoclave bomb and kept in an oven at 218 °C for 18 h. After the bomb cooled down to room
temperature, the resultant fine green MIL-101 crystals were separated from water using a centrifuge and
washed with water, methanol and acetone. The suspension in acetone was centrifuged and separated, the
solids were placed in N, N-dimethylformamide (10 mL) and the suspension was sonicated for 10 min and
then kept at 70 °C overnight. The resulting solids were separated by centrifugation, repeatedly washed with
methanol and acetone, dried at 75 °C overnight,
回复此楼
已阅   回复此楼   关注TA 给TA发消息 送TA红花 TA的回帖

MephisroWW

铁虫 (初入文坛)

同问,请问楼主解决了嘛
2楼2024-11-13 21:55:13
已阅   回复此楼   关注TA 给TA发消息 送TA红花 TA的回帖
相关版块跳转 我要订阅楼主 dxyan 的主题更新
最具人气热帖推荐 [查看全部] 作者 回/看 最后发表
[考研] 0831生医工第一轮调剂失败求助 +6 小熊睿睿_s 2026-04-11 9/450 2026-04-11 06:45 by JSWSK2012
[考研] 272分材料子求调剂 +28 Loy0361 2026-04-10 36/1800 2026-04-11 00:45 by success5733
[考研] 本人女孩 +5 吼吼, 2026-04-10 6/300 2026-04-11 00:09 by 任文亮
[考研] 本科南方医科大学 一志愿985 药学学硕284分 求调剂 +4 弱水听文 2026-04-09 4/200 2026-04-10 22:01 by doctff
[考研] 本9 一志愿西工大085601 324求调剂 +5 wysyjs25 2026-04-10 5/250 2026-04-10 16:57 by luoyongfeng
[考研] 机械专硕270求调剂,接受跨专业 +10 老师看看我吧aba 2026-04-09 11/550 2026-04-10 10:41 by cal0306
[考研] 269求调剂 +10 啊啊我我 2026-04-07 10/500 2026-04-10 10:38 by 高维春
[考研] 求调剂 +11 翩翩一书生 2026-04-09 13/650 2026-04-10 10:27 by liuhuiying09
[考研] 080100力学316求调剂 +7 L_Hairui 2026-04-07 7/350 2026-04-10 09:45 by vgtyfty
[考研] 308求调剂 +21 倘若起风了呢 2026-04-05 21/1050 2026-04-10 08:13 by Sammy2
[考研] 085404,285分求调剂 +12 薇薇考研 2026-04-07 14/700 2026-04-09 23:10 by parmtree
[考研] 求机械专硕297第二批调剂 +5 拾柒12。 2026-04-08 5/250 2026-04-09 16:43 by 允当适度
[考研] 电子信息346 +4 zuoshaodian 2026-04-08 4/200 2026-04-08 11:54 by zzucheup
[考研] 307求调剂 +14 超级伊昂大王 2026-04-06 14/700 2026-04-08 07:03 by 无际的草原
[考研] 生物调剂 +5 橙子橙子橙子啊 2026-04-05 9/450 2026-04-07 15:31 by 上岸快快
[考研] 305分求调剂 +3 哈_哈_哈_哈_哈 2026-04-04 5/250 2026-04-07 14:49 by 哈_哈_哈_哈_哈
[考研] 考研调剂 +7 15615482637 2026-04-04 7/350 2026-04-06 22:56 by chenzhimin
[考研] 材料调剂 +5 小刘同学吖吖 2026-04-06 5/250 2026-04-06 18:34 by sherry_1901
[考研] (调剂)一志愿报考哈尔滨工业大学0857资源与环境专业378分考生 +7 狠狠加油 2026-04-05 8/400 2026-04-06 16:52 by momo皓
[考研] 346分的生物与医药08600求调剂 +6 常雨阳上岸 2026-04-05 7/350 2026-04-06 12:36 by lys0704
信息提示
请填处理意见