KR20080089515A - 할로겐으로부터 가벼운 기체를 분리하는 방법 - Google Patents

할로겐으로부터 가벼운 기체를 분리하는 방법 Download PDF

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KR20080089515A
KR20080089515A KR1020087021011A KR20087021011A KR20080089515A KR 20080089515 A KR20080089515 A KR 20080089515A KR 1020087021011 A KR1020087021011 A KR 1020087021011A KR 20087021011 A KR20087021011 A KR 20087021011A KR 20080089515 A KR20080089515 A KR 20080089515A
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halogen
bromine
vapor
cubr
light
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사가 비. 가드워
피터 케이. 스토이메노브
필립 그로소
에릭 더블유. 맥팔랜드
애슐리 더블유. 브리드
마이클 제이. 웨이스
마이클 디. 위스타
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지알티, 인코포레이티드
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Abstract

하나 또는 그 이상의 물리적인 분리방식과, 화학적인 스크러버와의 접촉을 통해 브롬 또는 염소로부터 하나 또는 그 이상의 가벼운 기체를 분리하여 추가적인 할로겐을 회수하는 방법이 제공된다. 본 발명의 일 태양에 따르면, 이 방법은, (a) 하나 또는 그 이상의 가벼운 기체를 포함하는 할로겐 공급물을 증류컬럼 또는 플래쉬 기화기(flash vaporizer)에 공급하는 단계; (b) 상기 증류컬럼 또는 플래쉬 기화기를 작동시켜 상기 할로겐 공급물을 (i) 다량 (major amount)의 할로겐과 소량(minor amount) 이하의 가벼운 기체를 포함하는 제1액체와, (ii) 다량의 가벼운 기체와 소량 이하의 할로겐을 포함하는 제1증기로 분리하는 단계; 및 (c) 상기 증기를 화학적 스크러버에 공급하여 상기 증기로부터 할로겐을 회수하는 단계를 포함한다.
할로겐, 가벼운 기체, 증류컬럼, 화학적 스크러버, 할로겐 제거제

Description

할로겐으로부터 가벼운 기체를 분리하는 방법{SEPARATION OF LIGHT GASES FROM HALOGENS}
본 발명은 일반적으로 할로겐으로부터 불활성 기체 및 그 외 화합물을 분리하는 방법에 관한 것이다.
산화(oxidation)용 매체로서 공기와 산소 중 어느 기체를 선택할 것인가에 대해 수많은 산업 공정에서 연구가 이루어져 왔다. 반응 화학에 악영향을 미치지 않고 공기가 산화용으로 이용될 수 있는 공정의 경우에는, 투여자본 및 가동비용이 저렴하다는 점에서 공기가 순수한 산소공급에 비해 바람직하다. 산소 이용에 따른 고비용은 질소로부터 산소를 분리하는 비용 때문인데, 통상적으로 이러한 분리공정은 막이나 증류를 이용하여 이루어진다. 공기보다 순수한 산소를 이용하는 것이 바람직한 경우의 일예는 합성개스(syngas) 제조공정인데, 이 공정은 Fisher Tropsch 합성법을 이용하여 천연개스로부터 액체 탄화수소를 제조하는 과정의 첫 번째 공정이다. 반응 화학에 영향을 주는 것 외에도 syngas 생산에 공기를 이용하려면 전환되지 않은 천연개스로부터 질소가 분리되어야 한다. 천연개스로부터 질소를 분리하는 과정은 비용집약적이고, 통상적으로 막이나 압력 순환식 흡착(PSA: pressure swing adsorption) 공정을 이용하여 이루어진다.
불활성 기체 스트림에서 미량원소인 브롬을 포착(capturing)하는 종래의 방법은 알칼리 스크러버(alkaline scrubber)로서 예를 들어 수성 수산화나트륨 용액을 이용하는 것이다. 종래의 스크러빙 방법을 이용하여 포착된 브롬을 회수하는 것은 용이하지 않다. 그외의 종래 방법으로는 아황산나트륨(sodium sulfite), 나트륨이아황산염(sodium bisulfite), 또는 수산화칼슘 수용액 등을 이용하는 방법 등이 있는데, 이러한 방법들은 모두 포착된 브롬을 회수하기가 어렵다는 단점을 가지고 있다.
캘리포니아주 산타바바라시 소재의 GRT사가 개발한 기술에 의하면, 반응기에서 탄화수소와 할로겐을 혼합함으로써 메탄이나 천연개스로부터 고급 탄화수소를 합성하여 알킬할라이드 및 하이드로젠할라이드, HX를 생성할 수 있다. 알킬할라이드와 HX는 금속 산화물 또는 그와 유사한 물질과 접촉하여 고급 탄화수소와 금속 할라이드가 생성된다. 이 금속 할라이드는 산화되어 금속 산화물과 할로겐으로 되는데, 이들 모두 리사이클된다. 공기가 산화용으로 이용될 때, 생성되는 할로겐은 질소와 이산화탄소와 같은 불활성 기체를 포함하는데, 이들은 회수되지 않는 경우에는 할로겐화 섹션과 커플링 섹션을 통과하게 되고, 그 섹션에서 고급 탄화수소가 생성된다. GRT사에 의해 개발된 또 다른 기술에 의하면, 촉매의 존재하에 알킬할라이드와 할로겐을 반응시킴으로써 탄화수소가 생성되고, HX가 부산물로서 생성된다. 할로겐을 전체 공정의 그 다음 공정에서 이용하도록 재생하기 위해서, 촉매의 존재하에서 공기 또는 산소를 이용하여 HX를 산화시킨다. 전술한 두 가지 방식의 기술에서는 할로겐을 다음 공정 사이클에서 이용하기 전에 질소, 이산화탄소 및 기 타 가벼운 기체 (예: 미반응의 가벼운 탄화수소 등)로부터 재생된 할로겐과 물을 분리하는 것이 바람직하다. 사이클 또는 연속 공정의 경우에는, 특히 질소와 같은 기체는 분리되지 않으면 급속하게 축적된다. 따라서, 할로겐으로부터 불활성 기체 및 기타 화합물들을 효율적이고 경제적으로 분리하는 방법이 필요한 것은 명백하다.
본 발명에 따르면, 하나 또는 그 이상의 물리적인 분리방식과, 화학적인 스크러버와의 접촉을 통해 브롬 또는 염소로부터 하나 또는 그 이상의 가벼운 기체를 분리하여 추가적인 할로겐을 회수하는 방법이 제공된다. 본 발명의 일 태양에 따르면, 상기 방법은, (a) 하나 또는 그 이상의 가벼운 기체를 포함하는 할로겐 공급물을 증류컬럼 또는 플래쉬 기화기(flash vaporizer)에 공급하는 단계; (b) 상기 증류컬럼 또는 플래쉬 기화기를 작동시켜 상기 할로겐 공급물을 (i) 다량 (major amount)의 할로겐과 소량(minor amount) 이하의 가벼운 기체를 포함하는 제1액체와, (ii) 다량의 가벼운 기체와 소량 이하의 할로겐을 포함하는 제1증기로 분리하는 단계; 및 (c) 상기 증기를 화학적 스크러버에 공급하여 상기 증기로부터 할로겐을 회수하는 단계를 포함한다.
본 발명의 제2 태양에 따르면, 두 가지 또는 그 이상의 분리공정이 이용되는데, 이들 각각의 분리공정에 의해 연속적으로 점진적인 농화에 이르게 되는데, 액상 중의 할로겐과 기상 중의 가벼운 기체의 농화가 이루어지게 된다. 예를 들어, (가벼운 기체가 농화된) 증류컬럼으로부터의 증기가 제2 증류컬럼에 공급되고, 제2증류컬럼에서 다시 새로운 증기와 새로운 액체로 더 분리되고, 이들 새로운 기체에서는 가벼운 기체가 더 농화되고, 새로운 액체에서는 할로겐이 더 농화된다.
본 발명에서 이용되는 화학적 스크러버는 하나 또는 그 이상의 할로겐 제거제(scavenger)를포함하는데, 이것은 할로겐을 화학적으로 흡착(sorbing)할 수 있는 물질인데, 예를 들어 이러한 흡착은 할로겐과의 산화환원 반응을 통해 이루어진다. 이러한 물질의 바람직한 예는 브롬화구리(I)(CuBr)가 있는데, 이 물질은 브롬화구리(II)(CuBr2)로 전환됨으로써 브롬을 흡착할 수 있다.
본 발명의 특징 및 장점은 발명의 상세한 설명과 도면을 참조하여 보다 잘 이해될 것이다.
도1은 본 발명의 일태양에 따라 브롬으로부터 가벼운 기체를 분리하는 공정의 개략도이고;
도2는 도1에 도시된 공정의 개략도로서, 브롬 형성(브롬 재생)과 물 흡착을 위한 추가 부재가 구비되어 있으며;
도3은 본 발명의 또 다른 실시예에 따라 3개의 플래쉬 기화기를 차례로 작동시켜 브롬으로부터 가벼운 기체를 분리하는 공정의 개략도이고;
도4는 본 발명의 일태양에 따라 천연개스를 고급 탄화수소로 전환하기 위한 연속공정에 대한 개략도로서, 이 공정에서 생성된 브롬을 가벼운 기체로부터 분리하는 부공정을 포함하며;
도5는 본 발명의 일 실시예에서 이용되는 할로겐 제거제에서 할로겐 브레이크쓰루(breakthrough)를 측정하는 실험적인 방법을 나타내는 도면이고;
도6은 본 발명의 일실시예에서, 브롬/질소 스트림에 노출되었던 CuBr 튜브의 사진을 나타낸다.
본 발명의 신규의 공정에 있어서, 하나 또는 그 이상의 가벼운 기체를 포함하는 할로겐 공급물을 액체와 증기로 물리적으로 분리함으로써 브롬 또는 염소로부터 하나 또는 그 이상의 가벼운 기체를 분리하며, 상기 액체는 다량의 할로겐과 소량 이하의 가벼운 기체를 포함하며, 상기 증기는 다량의 가벼운 기체와 소량 이하의 할로겐을 포함한다. 상기 증기를 할로겐 제거제를 포함하는 화학적 스크러버를 통해 통과시킴으로써 추가적인 할로겐을 분리해낸다. 본 명세서에서 "가벼운 기체"란 이들과 혼합되어 있는 할로겐보다 비점이 낮은 기체를 의미한다. 대기압에서 브롬과 염소의 비점은 각각 약 59℃ 및 -34℃이다. 이러한 정의에 포함되는 기체로는 질소, 이산화탄소 및 가벼운 탄화수소로서 C1-C4 탄화수소가 있는데, 염소가 할로겐인 경우에는, 염소의 비점이 C4 탄화수소의 비점보다 낮기 때문에 C4 탄화수소(부탄 및 부텐)는 가벼운 기체로 간주되지 않는다. 다량(major amount) 및 소량(minor amount)이라는 용어는 상대적인 용어이다; 다량의 제1성분과 소량의 제2성분을 포함하는 액체(또는 증기)란 제2성분보다 제1성분을 더 많이 포함한다는 의미이다. 일반적으로 본 발명의 대부분의 실시예에서, 주어진 액체(또는 증기)상 은 하나의 성분(할로겐 또는 가벼운 기체)을 우세하게 포함하며, 그 나머지 성분은 매우 적은 양으로 포함한다.
본 발명의 일 실시예가 도1에 도시되어 있는데, 도1은 브롬으로부터 가벼운 기체(본 실시예에 있어서는 질소 및 이산화탄소)를 분리하기 위한 시스템(10)을 도시하고 있다. 질소와 이산화탄소를 포함하는 브롬 공급물(12)이 상부(16)와 (바닥부(18)을 가진 증류컬럼(14)에 공급된다. 열교환기(20 및 22)가 각각 부분적인 컨덴서 및 토탈 리플럭스로서 작용하여 브롬이 농화된 "바닥"부의 액체(소량 이하의 가벼운 기체도 포함하며, 일반적으로는 브롬 중의 두 기체의 용해도 한계 이하로 포함함)가 상기 증류컬럼으로부터 인출되도록 하며, 열교환기(24)에 의해 추가적인 온도 저하가 이루어진다.
컬럼의 상부에서, 리플럭스 드럼으로부터의 액체의 토탈 리플럭스는 열교환기(22)에 의해 용이하게 이루어지게 되어 가벼운 기체가 농화된 증기(소량 이하의 브롬도 포함함)가 생성되는데, 이것은 다시 화학적 스크러버(26)으로 이송되고, 여기서 상기 소량의 브롬이 제거되어 가벼운 기체(질소 및 이산화탄소)를 생성한다. 후술하는 바와 같이, 가열에 의해 상기 스크러버로부터 브롬이 회수될 수 있다.
본 발명의 다른 실시예(도시되지 않음)에서는, 2개 또는 그 이상의 증류컬럼이 직렬로 연결되고, 각각의 컬럼의 헤드(증기)는 다음 컬럼으로의 공급물로서 연결되어, 계속적으로 칵 컬럼의 바닥부 스트림에는 브롬이 농화되고 증기에는 가벼운 기체가 농화된다.
증류를 위해, 전형적인 압력 범위는 0.1 - 50바, 보다 바람직하기로는 5-20 바로 설정되고, 온도는 증류시스템의 압력에 따라 설정되는데, 브롬의 통상적인 비점이 약 59℃라는 점에 주의해야 한다. 스테이지의 수는 2-200, 바람직하기로는 5-30이다.
도2는 도1에 도시된 실시에의 변형예로서, 할로겐 공급물(예, Br2)이 할로겐재생유닛(28)으로부터 공급된다. 이 실시예에서는, 할로겐 재생유닛(28)으로부터 공급되는 할로겐 공급물이 물을 포함하는데, 이 물은 물흡착유닛(건조제 포함함)에서 제거된다. 또 다른 방식으로서, 상기 공급물은 먼저 증류되어 브롬-물 공비혼합물(azeotrope)가 형성될 때까지 물로부터 브롬을 제거하고, 나머지 물은 건조제가 들어 있는 물흡착컬럼에서 제거된다.
본 발명의 또 다른 실시예에 있어서, 하나 또는 그 이상의 증기-액체 플래쉬 분리유닛(플래쉬 기화기)을 이용하여 할로겐 공급물과 가벼운 기체를 분리한 다음 화학적 스크러버를 이용하여 추가적인 분리공정을 수행한다. 도3은 이러한 시스템(50)을 도시한 것인데, 질소와 이산화탄소를 포함하는 브롬 공급물이 제1플래쉬 기화기(52)에 공급된다. 기화기의 내용물이 플래쉬되어 브롬이 농화된 (예: 브롬회수율 97%) 제1액체와 단지 소량의 브롬을 포함하는 가벼운기체-농화된 제1증기(질소, 이산화탄소)를 생성한다. 제1증기는 제2플래쉬기화기에 공급되고, 그 내용물이 플래쉬되어 브롬이 농화된 제2액체(추가로 1.5%의 브롬이 회수됨)와 가벼운 기체가 농화된 제2증기를 생성하며, 이것은 다시 제2열교환기(58)를 통과한 다음 제3플레쉬기화기(60)에 공급된다. 제3플래쉬기화기의 내용물은 플래쉬되어, 추가 적으로 0.5% 브롬(액체)과 가벼운 기체가 매우 농화된 증기를 생성한다. 제3증기 스트림내에 있는 미량의 브롬이 브롬 스크러버(62)에서 제거된다.
필요한 경우에는, 추가적인 플래쉬 기화기가 이용될 수 있다. 그러나, 실제적인 문제로서 증가된 설비 비용과 가동비용이 정당화될 수 있는 한계를 넘지 않게 이를 조절해야 하는 포인트(추가적으로 회수되는 브롬의 양의 관점에서)가 있다. 증류컬럼과 플래쉬 기화기를 모두 이용하는 혼합시스템도 이용될 수 있다.
일반적으로, 브롬으로부터 가벼운 기체를 분리하는 경우에, 할로겐과 할로겐에 포함된 가벼운 기체 간의 비점의 차이에 주의하여, 각각의 플래쉬 기화기는 -60 내지 40℃, 바람직하기로는 -20 내지 10℃, 0.1-50바, 바람직하기로는 5-20바의 압력에서 가동된다. 1-3개의 플래쉬 기화기를 사용하는 것이 바람직하다. 압력은 각 기화기에서 다르게 조절될 수 있지만, 비용을 절감하기 위해서는 비용이 많이 드는 컴프레션(compression)을 피할 수 있는 시스템 압력에서 작동시키는 것이 바람직하다. 플래쉬 기화기의 작동 온도는 압력에 따라 조절된다. 예를 들어, 고압 가동은 비교적 고온에서도 양호한 브롬분리를 가능하게 한다. 그러나, 저압 가동에서는 플래쉬유닛의 냉각을 위해 냉매가 필요할 수 있다. 일련의 증기-액체 플래쉬는 하나 또는 그 이상의 플래쉬를 포함할 수 있다.
본 발명의 중요한 점은 대부분 가벼운 기체로 이루어진 매우 희석된 기체 스트림으로부터 브롬 또는 염소를 화학적으로 스크러빙하는 방법을 제공한다는 것이다. 이 방법은 할로겐을 흡착할 수 있는 할로겐 제거제를 이용한다. 바람직하기로는, 상기 제거제는 희석된 기체 스트림으로부터 브롬 증기를 흡착한 다음 그것을 다시 유리(free) 브롬으로서 정량적으로 방출할 수 있다. 브롬의 흡착은 실온 또는 상승된 온도에서 일어날 수 있다.
일반적으로, 브롬과 반응하여 가열에 의해 브롬을 다시 방출할 수 있는 물질이라면 어떠한 물질이라도 브롬 제거제로서 이용될 수 있다. 할로겐 제거제로서 사용되기에 적합한 물질의 비제한적인 예로는 CuBr, CuCl, FeBr2, FeCl2, AuCL, AuBr, InBr, InCl, FeO, Cu2O, Hg2Br2, Cu, Ag, Au, Hg, Pt, Pd, Ru, Rh, Fe, Os 및 Ir을 들 수 있는데, 이들은 단독으로 또는 조합되어 사용된다. 현재, CuBr이 바람직하다. 표면적이 큰 브롬화구리(담체상에 지지된 형태)가 사용되는 경우에는, 브롬화구리의 총량이 훨씬 적어도 훨씬 높은 활성을 얻게 된다. 침전방법에 의해 제조된 CuBr이 스톡(stock) CuBr보다 좋은 것으로 나타났다.
브롬화구리(I)는 브롬과 반응하여 하기 식에 따라 브롬화구리(II)를 형성한다:
2CuBr + Br2 → 2CuBr2 .
이 반응은 빠르며 완전하고 바람직하게도 실온에서 일어난다. 반응은 표면에서 일어나는 것으로 보인다. 벌크 CuBr을 이용하는 경우에는, 브레이크쓰루가 일어날 때까지 약 1%의 고체가 사용된다. (CuBr과 CuBr2의 밀도는 매우 유사하고, 표면이 그다지 리프래쉬되지 않는다: 4.6 대 4.0 g/cm3). CuBr과 Br2 증기와의 반응이 기체와 고체의 반응이기 때문에 반응속도는 고체-기체 계면(interface)에 의 해 제한되고, 따라서 표면적이 클수록 반응성이 높아진다. 실제로, 커다란 크리스탈 형태의 CuBr이 가장 효과가 떨어지는 흡착제이다. 브레이크쓰루가 일어날 때 (Br2가 더이상 고체에 의해 머무르게 되지 않을 때), 사용된 CuBr의 양은 총 고체 용량의 약 0.2%인데, 이는 고체의 표면만이 반응에 참여한다는 것을 의미한다. 낮은 반응 온도는 이온의 이동 가능성과 잔류하는 벌크 CuBr의 이용성을 떨어뜨린다.
저온에서 Br2를 흡착하는 CuBr의 능력은, 브롬 분리 공정에서 나오는 불활성 기체 스트림(미량의 브롬 포함)의 온도가 저온 또는 주위온도라는 점에서 바람직하다; 그러므로, 주위온도 또는 그 근처의 온도에서 스크러버를 가동하면 추가 에너지를 필요로 하지 않는다.
스크러빙된 브롬은 약 250℃ 이상으로, 일반적으로 250℃ 내지 275℃로의 가열에 의해 고체(본 실시예에서는 브롬화구리(II))를 재생함으로써 회수된다. 재생반응은 다음과 같은 반응식에 따라 일어난다:
2CuBr2 (heat) → CuBr + Br2
브롬화구리가 제거제로 사용되는 경우에, 재생은 열에 의해 활성화되므로 산소를 필요로 하지 않는다.
할로겐 제거제는 벌크 파우더 또는 담체상에 입혀진 형태로 이용될 수 있다. 이러한 물질의 예로는 실리카, 알루미나, 지르코니아, 티타니아, WO3, CaO, MgO, Cr2O3, 및 여러가지 탄화물, 질화물 및 이와 유사한 물질들이 있다. 이들이 갖추 어야 할 일차적인 요건은 담체의 표면적이 5-1500M2/g이어야 한다는 것이다. 본 실시예에서는 Davicat SiZr4700 또는 Davicat Si1151A (Davidson Corporation), 고표면적 (약 300 m2/g)을 가진 실리카 (Si4700B는 약 3wt.% ZrO2를 함유함) 상에 지지된 Cu(I)Br 또는 Cu(I)Br을 이용하였다. 그외의 담체들도 브롬화구리에 대한 스크러빙 반응을 수행하는데 마찬가지로 효과적이어야 한다.
할로겐 제거제 또는 할로겐 제거제-담체는 팩킹된 컬럼 반응기 구조 또는 쉘 앤드 튜브 반응기(shell and tube reactor)와 같은 다른 구조의 반응기에 사용될 수 있다. 스크러버의 활성 성분들을 재생 온도까지 도달시키는데 필요한 열을 전달하기 위해 표준 열전달매체가 이용될 수 있다. 이러한 공정은 2개의 반응기를 포함할 수 있는데, 하나의 반응기는 스크러빙을 담당하게 되고, 다른 하나의 반응기는 재생을 담당하게 된다.
고체 스크러빙제는 불활성 기체 플로우로부터 모든 브롬량을 완전하게 유지할 수 있다 (스크러버로부터의 브롬 손실은 1ppb 미만인 것으로 추정된다). 담체에 지지된 브롬화구리(I)는 복수회의 소비-재생 사이클 후에도 재현성 있는 결과를 보여준다.
담체(예: 실리카)가 사용되는 경우에는, 불균일한 표면이 더 작은 결정성으로 인해 더 큰 표면적을 가능하게 하는 핵형성부위(nucleation site)를 생성한다. 지지된 물질이 단지 15 중량%의 CuBr을 포함하는 경우에도, CuBr의 큰 표면적으로 인해 브롬 증기를 체류시키기에 매우 적합한 물질로 작용할 수 있다.
할로겐 제거제로서 브롬화구리(I)의 효과를 알아보기 위해서, 상업적으로 입수가능한 CuBr, 담체 지지된 CuBr, 및 침전에 의해 형성된 CuBr을 이용하여 일련의 실험을 실시하였다. 원래의 제거제(CuBr)는 CuBr2를 가열함으로써 재생시켰다. 그 결과가 표1에 나타나 있다.
표1: Br2 제거 결과
제거제/ 담체 Br 2 증기에 노출된 시간
10 분 20분 40분 80분
CuBr (commercial) 100% 70-75% 비실험 비실험
CuBr/Si4700B 비실험 100% ~100%* 비실험
CuBr/Si1151A 실험예정 실험예정 실험예정 실험예정
CuBr, 침전형** 100% 100% 100% 100%
주: %는 제거제에 의해 체류되는 브롬의 총량이다.
재생은 275℃에서 10-15분 이내에 종결된다.
CuBr/4700B에대해 활성의 저하 없이 복수회의 사이클로 테스트하였다.
* : 미량의 AgBr이 형성되었으나 그 양은 <10-4g이다.
**: 재생 후, 그 효과가 상업적으로 입수가능한 물질의 효과 수준으로 저하된다.
도6은 실온에서 30분동안 브롬/질소 스트림에 노출된, 침전된 CuBr 튜브에 대한 사진이다. 어두운 물질은 CuBr2이다. 가열시, 색채가 다시 CuBr의 연한 녹색으로 돌아가면서 브롬을 방출한다.
실험 프로토콜: 30sccm/min N2와 1.5sccm N2를 혼합하여 0℃로 냉각된 Br2 버블러에 통과시켰다. 고체 흡착제베드가 지름이 1cm인 실런더형 유리튜브에 포함되었다. 질소 중 희석된 브롬에 대한 노출시간은 실온에서 40분이었다. 스크러버에 의해 처리된 기체를 1M NaOH를 함유하는 트랩을 통해 버블링시켰다.
담체 지지된 CuBr 물질의 제조: 담체를 약 20중량% CuBr2 수용액에 분산시킨 다음 용액의 색체가 거의 무색으로 될 때까지 SO2로 버블링시켰다. 그 현택액을 여과하여 115℃에서 밤새 건조시켰다.
재생: 체류된 브롬의 재생은 275℃에서 20분동안 고체 스크러빙제를 넣고 반응기를 가열함으로써 실시하였다. 방출된 브롬을 모아서 1M NaOH 트랩용액 중에 방출된 브롬을 포획함으써 정량하였다. 포획된 브롬의 거의 완전한 회수가 가능하다.
정량실험: 스크러빙제에 의해 체류되지 않은 브롬의 양, 또는 소모된 스크러빙제로부터 제생된 브롬의 양은 NaOH 트랩 중의 흡착에 의해 정량적으로 측정하였는데, 이 트랩을 pH가 5 이하로 떨어질 때까지 질산으로 산성화시킨 다음 과량의 0.5M 질산은 용액을 이용하여 (더 이상 침전이 생기지 않을 때 까지 질산은 용액을 부가함) AgBr을 침전시켰다. AgBr 침전물을 여과하여 건조시키는데 사용되는 필터(glass fritted filter)로부터, 그 중량이 더 이상 변화되지 않을 때까지 건조시 켜, 증가된 질량을 측정하여 존재하는 브롬의 양을 계산하였다.
브롬 브레이크쓰루는 Br과 BrO-와 Ag+의 침전반응을 이용하여 측정된다. NaOh 트랩을 산성이 될 때까지 HON3로 산성화하고; 더 이상 침전이 형성되지 않을때 까지 AgNO3를 부가하고; 그 현탁액을 40분동안 에이징하여 건조되고 미리 질량을 측정해 놓은 깔떼기(glass-fritted funnel)를 이용하여 여과하고 일정한 질량으로 될 때까지 건조시켜, 얻은 질량차이가 AgBr이다.
AgNO3 + Br- → AgBr↓ + NO3 -
AgNO3 + BrO- → AgBrO↓ + NO3 -
AgBrO → AgBr + O2
AgBr에 대한 용해도 상수, Ksp는 5x10-13mol2l-2이다. 질산은 용액은 0.5M이고, 3ml(또는 그 이상의 양)의 질산은 용액을 약 20-25ml의 산성화된 NaOH 트랩에 부가한다. 최종 Ag+ 농도는 약 0.06M이다. Br-의 검출가능한 최저농도는 약 8x10-12M인데, 이는 약 0.6ppb에 해당한다. 비이상적인 경우를 가정하더라도 (고이온 강도, 1이 아닌 이온활성), 감도는 여전히 ppb 범위에 있다.
실시예:
약 25부피%의 브롬을 함유하는, 유속 40sccm(standard cubic cm per minute) 의 질소로 된 불활성 기체 스트림을 본 실시예에 기재된 방법에 따K라 처리하였다. 이 스트림을 25℃로 냉각시켰는데, 공업적으로는 공냉 열교환기를 이용하여 냉각시킬 수 있다. 25바의 압력 상태의 상기 스트림을 5℃에서 작동되는 단일 증기 액체 플래쉬 유닛에서 플래쉬시킨다. 상기 플래쉬로부터 유출되는 액체는 원래 공급물 중의 브롬의 98% 이상을 함유하며 브롬 스트림 중에 용해딘 약간의 불활성 기체도 함유한다. 상기 불활성 기체와 미량의 브롬을 함유하는 증기 스트림을 실온에서 담체 지지된 브롬화구리(I)로 된 베드에 통과시킨다. 불활성 기체 스트림으로부터 브롬 포획을 종결시키고 40분동안 스크러빙베드에서 브롬 포획을 실시한다. 브롬화구리(II)와 브롬화구리(I)을 포함하는 스크러빙 베드를 275℃로 가열하여 15분 내에 거의 완전한 브롬 회수를 관찰하였다.
본 발명은 화학약품 제조용 원료 또는 중간체로서 할로겐을 이용하는 수많은 공업 공정에 이용되는데, 할로겐 회수 또는 정제가 불활성 개체 또는 가벼운 기체의 제거에 의해 개선됨에 따라 투자비용 및 가동비용을 크게 줄일 수 있다. 이러한 공정의 예로는 미국특허 6,486,368, 6,472,572, 6,465,696, 6,462,243 및 6,403,840호에 기재된 알콜, 에테르, 올레핀, 알콕실레이트 제조공정과, 동일자 출원된 미국특허출원 (발명의 명칭: 탄화수소 원료를 고급 탄화수소 및 올레핀으로 전환하기 위한 연속공정 (Attorney Docket No. 56987/G506)에 기재된 고급 탄화수소 제조공정이 있으며, 이들의 내용 전체가 원용에 의해 본 명세서에 포함된다. 예를 들어, 천연개스로부터 가솔린급 탄화수소를 제조하기 위한 공정에서, 공기가 재생을 위해 이용되는 경우에 질소와 이산화탄소가 브롬화 및 복분해(metathesis) 섹션으로 이송된다. 전환되지 않은 메탄을 재순환시키기 위해서는 메탄으로부터 질소를 분리해야 하는데, 이 공정은 비용 집약적이다. 또한, 재생공정에서 발생된 이산화탄소도 압력순환식흡착법이나 아민계 시스템을 이용하여 전환되지 않은 메탄으로부터 분리해야 하는데, 이 고정 또한 비용 집약적이다. 브롬으로부터 가벼운 기체를 분리하는 것은 반응기의 크기를 줄여줄 뿐만 아니라 생성물 및 전환되지 않은 반응물로부터 가벼운 기체를 분리하는 공정을 단순화시킨다. 본 명세서에 기재된 분리방법들은 브롬과 같은 할로겐으로부터 가벼운 기체(질소 및 이산화탄소를 포함함)를 분리하는 방법으로서 경제적인 방법을 제공한다.
본 발명은 다양한 구현예 및 실시예에 의해 설명되었으나, 이들로만 제한되는 것은 아니며. 그외 변형예 및 첨부된 특허청구범위의 균등물도 본 발명의 범위에 포함된다.

Claims (12)

  1. 브롬 또는 염소로부터 가벼운 기체를 분리하는 방법으로서, 상기 방법은
    (a) 하나 또는 그 이상의 가벼운 기체를 포함하는 할로겐 공급물을 증류컬럼 또는 플래쉬 기화기에 공급하는 단계;
    (b) 상기 증류컬럼 또는 플래쉬 기화기를 작동시켜 상기 할로겐 공급물을, (i) 다량 (major amount)의 할로겐과 소량(minor amount) 이하의 가벼운 기체를 포함하는 제1액체와, (ii) 다량의 가벼운 기체와 소량 이하의 할로겐을 포함하는 제1증기로 분리하는 단계; 및
    (c) 상기 증기를 화학적 스크러버에 공급하여 상기 증기로부터 할로겐을 회수하는 단계
    를 포함하는 방법.
  2. 제1항에 있어서, 상기 제1액체를 증류컬럼 또는 플래쉬 기화기에 공급하여 상기 제1액체를, (i) 다량의 할로겐과 소량 이하의 가벼운 기체를 포함하는 제2액체와, (ii) 다량의 가벼운 기체와 소량 이하의 할로겐을 포함하는 제2증기로 분리하는 단계, 및
    (c) 상기 제2증기를 화학적 스크러버에 공급하여 상기 증기로부터 할로겐을 회수하는 단계를 더 포함하는 방법.
  3. 제1항에 있어서, 상기 할로겐이 브롬인 방법.
  4. 제1항에 있어서, 상기 할로겐이 염소인 방법.
  5. 제1항에 있어서, 상기 가벼운 기체가 질소를 포함하는 방법.
  6. 제1항에 있어서, 상기 가벼운 기체가 질소 및 추가 기체로서 이산화탄소와 C1-C4 탄화수소로 이루어진 군으로부터 선택된 하나 또는 그 이상의 추가 기체를 포함하는 방법.
  7. 제1항에 있어서, 상기 화학적 스크러버가 담체에 의해 지지된 또는 지지되지 않은 화학적 제거제인 방법.
  8. 제7항에 있어서, 상기 할로겐 제거제가 CuBr, CuCl, FeBr2, FeCl2, AuCL, AuBr, InBr, InCl, FeO, Cu2O, Hg2Br2, Cu, Ag, Au, Hg, Pt, Pd, Ru, Rh, Fe, Os 및 Ir 및 그 혼합물로 이루어진 군으로부터 선택된 물질을 포함하는 방법.
  9. 제1항에 있어서, 상기 할로겐 제거제가 CuBr을 포함하는 방법.
  10. 제1항에 있어서, 상기 할로겐 제거제가 금속 산화물, 금속 탄화물, 금속 질화물, 탄소, 클레이 및 그 혼합물로 이루어진 군으로부터 선택된 물질상에 지지된 것인 방법.
  11. 제1항에 있어서, 상기 할로겐 제거제가 Al2O3, SiO2, ZrO2, TiO2, WO3, CaO, MgO, Cr2O, SiC, Mo4C, TiN, W2N, 탄소, 제올라이트, 베르미쿨라이트 및 그 혼합물로 이루어진 군으로부터 선택된 물질 상에 지지된 것인 방법.
  12. 제1항에 있어서, 상기 화학적 스크러버를 가열하여 그로부터 할로겐을 방출시키는 단계를 더 포함하는 방법.
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AU2007212493B2 (en) 2012-09-27
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