Page 120 - 《精细化工》2023年第4期
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g806g ㏳ࡃጒ FINE CHEMICALS す 40 ࢤ
ᐼ͚喟N(t)̭ͧั⤳У̸⮱Ꭰ㣹㥪喑͗喠 MnO 2 ⮱䉕䛼ܳܳݘͧ 1.84%Ƞ4.68%হ 13.07%喑
N(t 0 )ͧ叾ᯄ⣜ධ̸⾧⮪㏱⮱Ꭰ㣹㥪喑͗ȡ ѻλᄦᏁ⮱ MnO 2 ⤳䃧䉕䛼ܳ 5%Ƞ10%হ 20%喑
㶕ᬻ䘕ܳ MnO 2 ᱗㘪➏ధ↶⼜λ UP 㶕䲏ȡ
2 㐀̻䃕䃧
UPM-3 ⮱ XRD ఫ喍ఫ 2e喎ܧ⣝ښⰥ NaYF 4
2.1 ᒏ䆹̻ࡃ႓㐀ᲱܳᲽ 喍JCPDS No.16-0334喎㵺ᄱም喑ѳ⇎ᰶᮣᔮ MnO 2
⮱➦ᒮ㵺ᄱም喑䃮 MnO 2 ͧᬍჇᒏ㐀Ჱ喑̻ XU
᱙ౕࣺ᪴ⰥᓛΠ⋟Ҁ㈨͚ᄦ UCNPs ̭ₒฺव
ぶ [25] 3+ 3+
PDAȠPEI হ MnO 2 ȡDA ౕ KMnO 4 ⮱⅔ࡃ҉⩕̸㜗 䛴⩕䔅࣌∂ݣิ⮱ NaYF 4 ńYb /Er @NaYF 4
@MnO 2 @Au ͚⮱ᬍჇᒏ MnO 2 ㆨѩȡⰥ℁̸喑ᒀ
㖇व⩌ PDA喑PDA ౕ͑ϟᕔ㶕䲏≨ᕔݯ Lgepal
CO-520 ⮱ႅ̸ౕ࠲㸦ౕ⇦䚥ԛ亝⮱ UCNPs 㶕䲏 [24] ȡ ̺⌨ߍ KMnO 4 ᬣ喍ఫ 2d喎喑Ҁ㈨͚⏣㼐⮱ O 2 ᄦ DA
⮱⅔ࡃ㖇वҬϔ➖ UP ͚ PDA ࠲㸦ᅯ⮱㶕䲏ⰥᄦᎠ
PEI 䕇䓴ፚ๘ⷞࣺᏁᝃ䓵ٸᅁߍࣺᏁᣒౕ PDA
⏾ [24] ȡᩜࡃ PEI ᣒፓᲒ⮱Ѻ䭨᩵Ꮑज㘪ౕ̭Ⴧ⼸
䨫̷Ꭳ᭫㦄倅ㆿၽ⮱㶕䲏ₐ⩢Ѻթ喑⩞λ KMnO 4
Ꮣ̷䭨ⶺ DA ⮱㖇वࣺᏁ喑ᄩ㜡 PDA ࠲㺳ᅯᒵ㪱ȡ
⮱䔅࣌ϔ➖ MnO 2 ⮱㶕䲏ڤᰶ䉌⩢ᕔ喑PEI ⮱ᣒᰶ
ߖλ PDA ࠲㸦ᅯᄦ MnO 2 ⮱㐀व [15] ȡᵤ৮⮱ TEM Ռߖ FTIR 㶕ᒮγϔ➖⮱ࡃ႓㐀Ჱ喑㐀ຯఫ 3
–1
ȡᰟ㏬ a ͚喑1561 হ 1446 cm ͧ UCNPs 㶕䲏
হ XRD ఫຯఫ 2 ȡ ⇦䚥͚㓔䚥ᵦ⮱ࣺᄦ⼝হᄦ⼝ѥ㑖ᡜߕ॥ᩣምȡUP
–1
ౕ 3423 cm ัͧ PDA হ PEI ͚ N—H 䩛হ OÿH
–1
䩛ѥ㑖ᡜߕፓ⮱䛺ऍ喑1622 হ 1519 cm ัܳݘͧ
㟠⣜⮱ѥ㑖ᡜߕ॥ᩣምহ䚝㘧⮱ NÿH 䩛⮱ѥ㑖ᡜ
ߕ॥ᩣም喑䃮ᬻ UCNPs ̻ PDA হ PEI ⮱ߌฺव [26] ȡ
䚝㘧⮱ C==OȠNÿH 䩛হ PEI ⮱ CÿH 䩛ぶ॥ᩣፓ
–1
⮱Ⱕο䛺ऍᄩ㜡 UPM ౕ 1300~1640 cm ܧ⣝ც॥
–1
ᩣፓ喑580 cm ัͧ MnÿO 䩛⮱ѥ㑖ᡜߕ॥ᩣም喑
㶕ᬻ MnO 2 ⮱ߌฺवȡ
ఫ 3 UCNPs喍a喎ȠUP喍b喎হ UPM-3喍c喎⮱ FTIR 䅞ఫ
Fig. 3 FTIR spectra of UCNPs (a), UP (b) and UPM-3 (c)
ఫ 2 UPM-1喍a喎ȠUPM-2喍b喎ȠUPM-3喍c喎ȠUP喍d喎
হ UCNPs喍d ڲఫ喎⮱ TEM ఫВࣷ UPM-3 ⮱ Ռߖ XPS ܳᲽ UPM-3 ⮱ٰ㉍Ჱহ㶕䲏ࡃ႓
XRD 䅞ఫ喍e喎 ⟣ᔮ喑㐀ຯఫ 4 ȡఫ 4a ᭫喑UPM ⮱ XPS
Fig. 2 TEM images of UPM-1 (a), UPM-2 (b), UPM-3 (c), 䅞क़ᰶ GdȠCȠNȠO হ Mn ぶٰ㉍⮱Ԏतም喑̻
UP (d) and UCNPs (insert in d); XRD image of
UPM-3(e) Ⱋᴴٶ᩼ݯक़⮱ٰ㉍ᄦᏁȡఫ 4b ͚喑Mn 2p ⮱
㏳䅞ౕ653.2হ641.9 eVัԎतምܳݘᄦᏁλMn喍Ė喎
⩞ఫ 2a~c जВⰸܧ喑UPM ڤᰶᵥภ㐀Ჱ喑ౕ ⮱ Mn 2p 1/2 হ Mn 2p 3/2 Ԏत喑䄡ᬻᵤ৮ UPM-3 ͚क़
⌞㞟৾䧰ಸ UCNPs ⮱㶕䲏ᰶᒵ㪱⮱≲㞟 PDA/PEI ᰶ MnO 2 ȡఫ 4c ͚喑N 1s 䅞࠲क़ 399.7 eV ั⮱ PEI
࠲㸦ᅯ喑䮼Ɑ KMnO 4 ⩕䛼⮱๔喑PDA/PEI ࠲㺳ᅯ ͚㘧ധ喍ÿNH 2 喎N ̻ॎણ N Вࣷ 401.1 eV ั⮱ⴠ
⮱ࣇᏓअࡃ̺ᬻ᭫喑ѳ⪒᭫⌞㞟Ƞ䷄ㆿ⟣হ̺㻱݆ ࡃ N喑ⴠࡃ N ज㘪Გ⎽λ PDA ౕ KMnO 4 ҉⩕
❴⟣ MnO 2 ⮱䛼็́ᅧᄥᬻ᭫๔喑㶕ᬻ UPM ̸⮱⅔ࡃ [27] ȡఫ 4d ͚喑149.1 হ 143.1 eV ั⮱ምᄦ
͚ MnO 2 ⮱Ⱕᄦक़䛼䮼 KMnO 4 ⩕䛼⮱ߍ㔹็ȡ Ꮑλ Gd喍ĕ喎⮱ Gd 4d 3/2 হ Gd 4d 5/2 Ԏत [28] ȡ̷䔝
ICP ≸䄂㐀㶕ᬻ喑UPM-1ȠUPM-2 হ UPM-3 ͚ 㐀䔈̭ₒ䃮ٶ᩼ݯڤᰶ䶱⮱ࡃ႓㏱ȡ
