KR101905862B1 - 위치 선택적 다공성 분리막의 제조방법 및 상기 제조된 다공성 분리막을 이용한 가스분리방법 - Google Patents
위치 선택적 다공성 분리막의 제조방법 및 상기 제조된 다공성 분리막을 이용한 가스분리방법 Download PDFInfo
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- KR101905862B1 KR101905862B1 KR1020170037504A KR20170037504A KR101905862B1 KR 101905862 B1 KR101905862 B1 KR 101905862B1 KR 1020170037504 A KR1020170037504 A KR 1020170037504A KR 20170037504 A KR20170037504 A KR 20170037504A KR 101905862 B1 KR101905862 B1 KR 101905862B1
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- JBFYUZGYRGXSFL-UHFFFAOYSA-N imidazolide Chemical compound C1=C[N-]C=N1 JBFYUZGYRGXSFL-UHFFFAOYSA-N 0.000 claims description 4
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- LDZYRENCLPUXAX-UHFFFAOYSA-N 2-methyl-1h-benzimidazole Chemical compound C1=CC=C2NC(C)=NC2=C1 LDZYRENCLPUXAX-UHFFFAOYSA-N 0.000 claims description 2
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Images
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- B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
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Abstract
Description
도 2는 본 발명의 일 실시예에 따른 (a1)-(a2) α-Al2O3 디스크와 (b1)-(b2) γ-/α-Al2O3 디스크의 SEM 이미지이다.
도 3은 본 발명의 일 실시예에 따른 α-Al2O3 디스크(하단) 및 γ-/α-Al2O3 디스크(상단)의 XRD 패턴을 도시한 도면이다.
도 4는 본 발명의 일 실시예에 따른 멤브레인의 단면 SEM 이미지로서, (a1)-(a2) ZIF-8_α 및 (b1)-(b2) ZIF-8_γα의 SEM 이미지이다.
도 5는 본 발명의 일 실시예에 따른 (a1)-(a4)에 대한 저배율(제1열)의 4개의 지지체 위치(제1열의 저배율 SEM 이미지에 표시) (제2 내지 제5열) 단면 SEM 이미지로서 (a1)-(a4) ZIF-8_α 및 (b1)-(b4) ZIF-8_γα의 SEM 이미지이다.
도 6은 본 발명의 일 실시예에 따른 ZIF-8(아래)과 ZnO (위)의 시뮬레이션된 XRD 패턴을 참조로 한 멤브레인 ZIF-8_α 및 ZIF-8_γα의 XRD 패턴을 도시한 도면이다.
도 7은 본 발명의 일 실시예에 의한 BJH 분석을 통한 지지체(α-Al2O3 및 γ-/Al-Al2O3 디스크)와 지지된 막(ZIF-8_α 및 ZIF-8_γα)의 기공 크기 분포 및 77 K에서의 N2 흡착 등온선; (b) 및 (e) BJH 흡착 브랜치(adsorption branch) 및 (c) 및 (f) BJH 탈착 브랜치(desorption branch)를 도시한 도면이다.
도 8은 본 발명의 일 실시예에 의한 (a1)-(b1) 온전한 멤브레인 및 (a2)-(b2) 의도적으로 손상된 멤브레인 ZIF-8_α와 ZIF-8_γα의 200 ℃까지의 온도에서의 H2/CO2 분리성능의 함수 및 (a3)-(b3) 손상되지 않은 멤브레인 ZIF-8_α 및 ZIF-8_γα 최대 300 ℃에서의 분리성능을 도시한 도면이다.
도 9는 본 발명의 일 실시예에 따른 멤브레인 ZIF-8_α(위) 및 ZIF-8_γα(아래)에서 물방울의 접촉각을 도시한 도면이다.
도 10은 본 발명의 일 실시예에 따른 멤브레인 (a1)-(a2) ZIF-8_α 및 (b1)-(b2) ZIF-8_γα의 200 및 250 ℃에서 최대 72시간의 H2/CO2 분리성능을 확인하여 열안정성을 조사한 도면이다.
도 11은 본 발명의 일 실시예에 따른 200 및 250 ℃에서의 장기 안정성 시험 전후의 멤브레인 (a1)-(a2) ZIF-8_α 및 (b1)-(b2) ZIF-8_γα의 XRD 패턴을 도시한 도면이다.
도 12는 본 발명의 일 실시예에 따른 열안정성 시험 전후의 (c)-(d) XRD 패턴과 함께 300 ℃에서 72시간까지 측정한 멤브레인 (a) ZIF-8_α와 (b) ZIF-8_γα의 H2/CO2 분리성능을 확인한 도면이다.
도 13은 본 발명의 일 실시예에 따른 70 ℃에서 24시간 건조한 ZIF-8 입자의 XRD 패턴과 CO2 환경 및 300 ℃에서 7일간 열처리한 ZIF-8 입자의 XRD 패턴을 도시한 도면이다.
도 14는 본 발명의 일 실시예에 따른 다른 유형의 ZIF 막과 ZIF-8_α(α로 표시) 및 ZIF-8_γα(γ로 표시)의 H2/CO2 SFs vs 막투과성(H2)을 비교한 그래프이다.
지지체 | Pore size (nm) | Porosity (%) |
α-Al2O3 disc | 151.1 | 40.3 |
γ-/α-Al2O3 disc | 154.7 | 40.7 |
α-Al2O3 디스크의 위치 | 멤브레인 ZIF-8_α | 멤브레인 ZIF-8_γα |
중량비 (Zn (wt%)/Al (wt%)) |
중량비 (Zn (wt%)/Al (wt%)) |
|
상단(top) | 7.7 ± 4.5 | 8.5 ± 1.3 (γ-Al2O3 층) |
8.5 ± 1.1 | ||
중간(middle) | 0 | 0 |
하단(bottom) | 0 | 0 |
샘플 | 멤브레인 합성 전후에 측정된 샘플 중량으로부터 얻은 ZIF-8 상의 예상 중량(mg) | 미세기공 표면적을 비교하여 얻은 ZIF-8 상의 예상 중량(mg) |
ZIF-8_α | 11 ± 0.1 | 8.0 |
ZIF-8_γα | 12 ± 0.1 | 8.4 |
BET 표면적(m2/g) | 외부 표면적(m2/g) | 미세기공 면적(m2/g) | |
α-Al2O3 디스크 | 3.88 ± 0.008 | 3.84 | 0.036 |
γ-/α-Al2O3 디스크 | 4.30 ± 0.008 | 2.92 | 0.96 |
ZIF-8_α | 10.06 ± 0.04 | 2.13 | 7.92 |
ZIF-8_γα | 10.56 ± 0.04 | 2.39 | 8.17 |
ZIF-8 분말1 ) | 1643.3 ± 9.8 | 65.6 | 1577.7 |
Claims (12)
- 다음 단계를 포함하는 다공성 분리막의 제조방법:
(a) 다공성 지지체 위에, 상기 다공성 지지체보다 작은 기공을 가진 입자를 코팅하여 계층구조 다공성 지지체를 합성하는 단계; 및
(b) 상호확산법(counter diffusion)을 수행하여 상기 계층구조 다공성 지지체의 계면 바로 아래로부터 내부에 ZIFs(Zeoliteic Imidazolate Frameworks)가 매립되어 형성된 분리막을 합성하는 단계.
- 제1항에 있어서, 상기 (b) 단계는 상기 (a) 단계에서 합성된 계층구조 다공성 지지체를 아연염 용액에 침지시켜 Zn2+를 흡착시킨 다음, 이미다졸 또는 이미다졸 유도체 용액에 침지시켜 Zn2+ 이미다졸의 결정을 다공성 지지체 내부에 형성시키는 것을 특징으로 하는 다공성 분리막의 제조방법.
- 제1항에 있어서, 상기 계층구조 다공성 지지체는 다공성 지지체 한 면에 상기 다공성 지지체보다 작은 기공이 형성된 것을 특징으로 하는 다공성 분리막의 제조방법.
- 제3항에 있어서, 상기 다공성 지지체의 기공 크기는 50~1000 nm이고, 상기 다공성 지지체보다 작은 기공을 가진 입자의 기공 크기는 2~50 nm인 것을 특징으로 하는 다공성 분리막의 제조방법.
- 제1항에 있어서, 상기 (a) 단계의 다공성 지지체보다 작은 기공을 가진 입자는 α-알루미나, γ-알루미나, 실리카, 글래스, 멀라이트(mullite), 지르코니아(zirconia), 티타니아(titania), 이트리아(yttria), 세리아(ceria), 바나디아(vanadia), 실리콘, 스테인레스 스틸, 칼슘 산화물, 인 산화물 및 그 혼합물로 구성된 군에서 선택되는 1종 이상인 것을 특징으로 하는 다공성 분리막의 제조방법.
- 제2항에 있어서, 상기 아연염은 질산아연, 아세트산아연, 염화아연, 황산아연, 브롬화아연 및 요오드화아연으로 구성된 군에서 선택되는 하나 이상인 것을 특징으로 하는 다공성 분리막의 제조방법.
- 제2항에 있어서, 상기 이미다졸 또는 이미다졸 유도체는 벤지미다졸(benzimidazole), 2-메틸이미다졸(2-methylimidazole), 4-메틸이미다졸(4-methylimidazole), 2-메틸벤지미다졸(2-methylbenzimidazole), 2-니트로이미다졸(2-nitroimidazole), 5-니트로벤지미다졸(5-nitrobenzimidazole), 및 5-클로로벤지미다졸(5-chlorobenzimidazole)로 구성된 군에서 선택되는 하나 이상인 것을 특징으로 하는 다공성 분리막의 제조방법.
- 제2항에 있어서, 상기 아연염 용액 또는 이미다졸 또는 이미다졸 유도체 용액은 메탄올, 에탄올, 프로판올, iso-프로판올, tert-부탄올, n-부탄올, 메톡시에탄올, 에톡시에탄올, 디메틸아세트아마이드, 디메틸포름아마이드, n-메틸-2-피롤리돈(NMP), 포름산, 니트로메탄, 아세트산 및 증류수로 구성된 군에서 선택되는 하나 이상의 용매에 용해시킨 것을 특징으로 하는 다공성 분리막의 제조방법.
- 제1항에 있어서, 상기 다공성 분리막의 두께는 0.1~500 μm인 것을 특징으로 하는 다공성 분리막의 제조방법.
- 제1항 내지 제9항 중 어느 한 항의 방법에 의해 제조된, 50~1000 nm 크기의 기공을 형성하는 세라믹 지지체 한 면에 세라믹 입자가 코팅되어 2~50 nm 크기의 기공이 형성된 계층구조 다공성 지지체의 계면 바로 아래로부터 내부에 ZIFs가 매립되어 형성되고 0.1~500 μm의 두께를 가진 것을 특징으로 하는 다공성 분리막.
- 제10항의 다공성 분리막을 이용하여 H2와 CO2의 혼합가스 또는 합성가스(syngas)로부터 수소를 분리하는 방법.
- 제11항에 있어서, 100~500 ℃의 온도에서 수행하는 것을 특징으로 하는 수소를 분리하는 방법.
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