KR100407166B1 - Oxidation catalysts and method for controlling co, voc, and halogenated organic - Google Patents

Oxidation catalysts and method for controlling co, voc, and halogenated organic Download PDF

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KR100407166B1
KR100407166B1 KR10-2000-0033081A KR20000033081A KR100407166B1 KR 100407166 B1 KR100407166 B1 KR 100407166B1 KR 20000033081 A KR20000033081 A KR 20000033081A KR 100407166 B1 KR100407166 B1 KR 100407166B1
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organic compounds
carbon monoxide
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honeycomb
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Abstract

담체로 고체분말상의 B2O3, Bi2Ti2O7, Bi2O3, Cr3C2등의 혼합물을 사용하여 여기에 활성 금속을 담지시켜 저온에서, 그리고 빠른 공간속도하에서 일산화탄소와 휘발성 유기화합물, 그리고 할로겐화 유기화합물을 산화시키기 위해 사용되는 배출가스정화 촉매 및 제조법As a carrier, a mixture of B 2 O 3 , Bi 2 Ti 2 O 7 , Bi 2 O 3 , Cr 3 C 2, etc., on a solid powder was used to support the active metal, thereby reducing carbon monoxide and volatility at low temperatures and at high space velocity. Exhaust gas purification catalyst and preparation method for oxidizing organic compounds and halogenated organic compounds

Description

일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매 및 제조방법{OXIDATION CATALYSTS AND METHOD FOR CONTROLLING CO, VOC, AND HALOGENATED ORGANIC}OXIDATION CATALYSTS AND METHOD FOR CONTROLLING CO, VOC, AND HALOGENATED ORGANIC} Removal of Carbon Monoxide, Volatile Organic Compounds and Halogenated Organic Compounds

본 발명은 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거에 사용되는 산화촉매 및 제조방법에 관한 것이다. 이 기술에 사용되는 종래의 촉매들로는 다음과 같다. 할로겐화 탄화수소를 산화시키기 위하여, 미국특허 3,972,979와 4,053,557에 크롬산화물과 보헤마이트에 백금을 담지시켜서 할로겐화 탄화수소를 산화시켰으며, 미국특허 4,059675, 4,059,676, 4059683에서는 산화제 존재하에 루테늄, 루테늄-백급, 백금을 각각 촉매로 사용하였다. 탄화수소와 일산화탄소를 산화시키기 위해서는 미국특허 4,983,366에 Al203, Si02, 제올라이트등의 담체에 바륨, 망간, 구리, 크롬, 니켈과 백금, 팔라듐, 백금-로듐등을 촉매로 사용하였다. 할로겐화유기화합물을 함유한 유기화합물을 산화시키기 위하여 PCT/US90/02386에서는 타이타니아 담체에 V2O5, SnO2를 함유하며 귀금속중 1개를 포함하는 촉매가 소개 되었다. 그리고 미국특허 5,283,041에서는 ZrO2, 망간산화물에 세륨 또는 코발트가바나듐산화물과 함께 담지되어 있는 촉매를 사용하였다.The present invention relates to an oxidation catalyst and a method for producing carbon monoxide, volatile organic compounds and halogenated organic compounds. Conventional catalysts used in this technique are as follows. In order to oxidize halogenated hydrocarbons, US Pat. Were used as catalysts, respectively. Al 2 0 3, Si0 2, barium on a support of zeolite, manganese, copper, chromium, nickel, platinum, palladium and platinum in the US Patent 4,983,366 in order to oxidize hydrocarbons and carbon monoxide-rhodium, etc. was used as a catalyst. In order to oxidize organic compounds containing halogenated organic compounds, PCT / US90 / 02386 introduced a catalyst containing V 2 O 5 , SnO 2 in a titania carrier and containing one of the precious metals. In US Pat. No. 5,283,041, a catalyst supported with ZrO 2 , manganese oxide with cerium or cobalt vanadium oxide was used.

그러나 이들 촉매들은 휘발성유기화합물 및 일산화타소를 분해하는 속도가 공간속도 30,000h-1∼50,000h-1정도로 알려져 있다. 그리고 할로겐화 탄화수소 및 휘발성 유기화합물의 70% 이상 분해온도 또는 산화온도가 300℃에서 400℃ 사이인 것으로 미국특허 3,972,979와 5,578,283등에 알려져 있다.However, these catalysts have a speed to decompose the volatile organic compounds and known monoxide Hua Tuo small enough space velocity of 30,000h -1 ~50,000h -1. In addition, US Pat.

본 발명에서는 종래의 기술에 나타난 단점들인 낮은 공간속도와 높은 분해온도를 개선하고자 하였다. 따라서 본 발명에서는 빠른 공간속도에서 촉매의 휘발성유기화합물 또는 일산화탄소의 산화 처리속도를 높이고, 낮은 온도에서 촉매의 전환율을 높여 저온에서 일산화탄소와 휘발성 유기화합물, 그리고 할로겐화 유기화합물의 산화 성능을 극대화 시키는 촉매 및 방법을 제공하는데 있다.In the present invention, it is intended to improve low space velocity and high decomposition temperature which are disadvantages of the prior art. Therefore, the present invention increases the oxidation treatment rate of the volatile organic compounds or carbon monoxide of the catalyst at a high space speed, and the catalyst to maximize the oxidation performance of carbon monoxide and volatile organic compounds, and halogenated organic compounds at low temperatures by increasing the conversion rate of the catalyst at low temperatures and To provide a method.

본 발명에 사용된 담체로 고체 분말상의 B2O3, Bi2Ti2O7, Bi2O3, Cr3C2등을 사용하게 되는데 1개 이상의 화합물이 선택되어 사용된다. 그 사용량은 2개가 선택되었을 때 무게비가 99:1에서 1:99인 상태로 미세하게 분할된 유지물로 포함하는 것을 특징으로 하며, 3가지 무기화합물이 선택되면 먼저 선택된 2개의 무기화합물에 대하여 3번째 것은 1∼10 중량%로 첨가하는 것을 특징으로 한다. 일산화탄소와 휘발성유기화합물, 할로겐화 유기화합물을 산화시키기 위해 본 발명에 사용된 금속원소들로는 Ag, Au, Ni, Co, Cs, Cu, V, Ti 그룹(A)중에서 1개이상, 그리고 Pt, Ru, Ir 의 귀금속 그룹(B) 중에서 1개이상 선택된 원소를 함유하는 방법이며, 이들 금속 원소들은 금속 또는 금속산화물 상태로 존재한다. 이들 금속 원소들은 담체에 대하여 (A)그룹중 1개 이상의원소 + (B)그룹중 1개 이상의 원소의 합이 0.1～25 중량%를 사용함으로써 충분한 발명효과가 발휘된다. 0.1중량% 보다 적은양을 사용하면 충분한 발명효과를 얻기 힘들고, 25중량% 보다 많은 양을 사용하면 금속들이 응집되어 발명의 효과가 떨어진다. (A)그룹 원소와 (B)그룹원소와의 사용비는 1 : 10 ∼ 10 : 1 인 것을 특징으로 한다.As the carrier used in the present invention, solid powdery B 2 O 3 , Bi 2 Ti 2 O 7 , Bi 2 O 3 , Cr 3 C 2, etc. may be used, and at least one compound may be selected and used. The amount of use is characterized in that it comprises a finely divided oil with a weight ratio of 99: 1 to 1:99 when two selected, and if three inorganic compounds are selected, 3 for the first two inorganic compounds selected The second one is characterized by the addition of 1 to 10% by weight. The metal elements used in the present invention to oxidize carbon monoxide, volatile organic compounds, and halogenated organic compounds include at least one of Ag, Au, Ni, Co, Cs, Cu, V, and Ti groups (A), and Pt, Ru, It is a method containing at least one element selected from the noble metal group (B) of Ir, and these metal elements exist in a metal or metal oxide state. These metal elements exhibit sufficient invention effect by using 0.1-25 weight% of the sum of 1 or more elements of (A) group + 1 or more elements of (B) group with respect to a support | carrier. If the amount is less than 0.1% by weight, sufficient invention effect is hardly obtained. If the amount is more than 25% by weight, the metals are aggregated and the effect of the invention is reduced. The use ratio of (A) group element and (B) group element is 1: 10-10: 1, It is characterized by the above-mentioned.

담체로 사용되는 B2O3, Bi2Ti2O7, Bi2O3, Cr3C2등의 혼합물을 볼밀 등을 사용하여 수성 슬러리로 만들고 일체 구조를 갖는 허니콤에 워시코팅하고, 그후 120℃에서 6시간 이상 건조한후 Ag, Au, Ni, Co, Cs, Cu, V, Ti 그룹(A)중에서 1개 이상, 그리고 Pt, Ru, Ir 의 귀금속 그룹(B) 중에서 1개이상 선택된 원소를 함유하는 방법이며, 이들을 함유하는 혼합수용액을 담체가 워시코팅된 허니콤에 담지시켜 120℃ 이상에서 6시간 이상 건조시킨후 400∼650℃에서 1∼4 시간 동안 소성시킨다. 허니콤에 워시코팅되는 내화성 무기화합물은 허니콤 용적에 대하여 30 ∼ 250g/L(허니콤 용적)의 농도로 존재하는 것을 특징으로 한다.A mixture of B 2 O 3 , Bi 2 Ti 2 O 7 , Bi 2 O 3 , Cr 3 C 2, and the like, which is used as a carrier, is made into an aqueous slurry using a ball mill or the like and wash-coated with a honeycomb having an integral structure. At least one selected from Ag, Au, Ni, Co, Cs, Cu, V, and Ti groups (A) after drying at 120 ° C. for at least 6 hours, and at least one element selected from the precious metal groups (B) of Pt, Ru, Ir It is a method containing, and the mixed aqueous solution containing them is supported on a wash-coated honeycomb carrier and dried at 120 ° C or more for 6 hours or more and then calcined at 400 to 650 ° C for 1 to 4 hours. The refractory inorganic compound wash-coated to the honeycomb is characterized by being present at a concentration of 30 to 250 g / L (honeycomb volume) based on the honeycomb volume.

이러한 본 발명의 촉매는 일산화탄소와 휘발성유기화합물, 할로겐화 유기화합물을 산화시키기 위해 사용할수 있다.다음의 실시예에 의하여 본 발명을 더 상세히 설명하는데 본 발명은 이들 실시예에만 한정되는 것은 아니다.The catalyst of the present invention can be used to oxidize carbon monoxide, volatile organic compounds, and halogenated organic compounds. The present invention will be described in more detail by the following examples, but the present invention is not limited to these examples.

실시예1 에서 실시예 8 까지, 그리고 비교예 1에서 비교예 2까지 일산화탄소3,000 ppm, 톨루엔(Toluene) 1,000ppm, 산소 8%, 수분(H2O) 3%, 메틸브롬 500ppm을 반응가스로 흘려주면서 200℃ ∼ 300℃ 까지 저온으로 온도를 조절하였다. 촉매는 고정층 연속 흐름 반응기내에 충전되어 있으며, 공간속도는 100,000/hr 가 되도록 촉매량과 반응물 유속을 결정하였다. 비교예1은 TiO2를 담체로하는 일반적인 촉매들을 비교하였고, 비교예2는 SiO2를 담체로 사용하는 일반적인 촉매와 비교하였다.실험자료들은 200시간동안 연속으로 실험하여 얻은 값을 나타낸 것이다.From Example 1 to Example 8, and from Comparative Example 1 to Comparative Example 2, 3,000 ppm of carbon monoxide, 1,000 ppm of toluene, 8% of oxygen, 3% of water (H 2 O), and 500 ppm of methyl bromine were flowed into the reaction gas. The temperature was adjusted to low temperature to 200 ℃ to 300 ℃ while giving. The catalyst was charged in a fixed bed continuous flow reactor, and the amount of catalyst and reactant flow rate were determined so that the space velocity was 100,000 / hr. Comparative Example 1 compared general catalysts using TiO 2 as a support, and Comparative Example 2 compared general catalysts using SiO 2 as a support. Experimental data show values obtained by continuous experiments for 200 hours.

표1은 촉매처리된 허니콤의 구성성분을 나타내었고, 표2에 일산화탄소, 톨루엔, 클로로에틸렌의 산화전환율을 나타내었다.Table 1 shows the constituents of the catalyzed honeycomb, and Table 2 shows the oxidation conversion rates of carbon monoxide, toluene and chloroethylene.

실시예 1)Example 1

Cr3C2200g을 혼합하여 볼밀로 20시간동안 습식분쇄하여 수성슬러리를 조제하여, 단면적 1평방인치당 200개의 가스유통셀을 갖는 15㎝×15㎝×10㎝ 크기의 하니콤을 상기 슬러리에 침지하고 취출하여 셀내의 과잉 슬러리를 압축공기로 불어내고, 그후 120℃에서 12시간 건조하고, 이것을 Co를 2g 함유하는 코발트나이트레이트와 Pt를 2g 함유하는 클로로플라티닉엑시드 혼합 수용액에 침지하여 함침시키고 120℃에서 12시간동안 건조후 600℃에서 2시간동안 소성시켜 촉매처리된 허니콤을 제조하는데 사용된 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매 및 제조방법200 g of Cr 3 C 2 was mixed and wet pulverized with a ball mill for 20 hours to prepare an aqueous slurry, and a 15 cm × 15 cm × 10 cm sized honeycomb having 200 gas flow cells per square inch of cross section was immersed in the slurry. Then, the excess slurry in the cell was blown out with compressed air, and then dried at 120 ° C. for 12 hours. The mixture was immersed in an aqueous mixed solution of cobalt nitrate containing 2 g of Co and 2 g of Pt and impregnated with 120 Oxidation catalyst and method for removing carbon monoxide, volatile organic compounds, and halogenated organic compounds used to prepare a catalyst-treated honeycomb by drying at 600 ° C. for 12 hours and then baking at 600 ° C. for 2 hours.

실시예 2)Example 2)

표1의 (A) 성분이 B2O3100g, (B)성분이 Cr3C2100g (C) 성분이 Co 2g인 것을제외하고는 실시예 1과 동일한 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매 및 제조방법The same carbon monoxide, volatile organic compounds and halogenated organic compounds as in Example 1, except that (A) component of Table 1 B 2 O 3 100g, (B) component of Cr 3 C 2 100g (C) component of Co 2g Removal oxidation catalyst and preparation method

실시예 3)Example 3

표1의 (A) 성분이 Bi2O3100g, (C) 성분이 Ni 1g, (D) 성분이 Cs 1g (E)성분이 Ir 2g인 것을 제외하고는 실시예 2와 동일한 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매 및 제조방법The same carbon monoxide and volatile organic as Example 2, except that (A) component of Table 1 is 100 g of Bi 2 O 3 , (C) is Ni 1g, (D) is Cs 1g and (E) is Ir 2g. Oxidation catalyst and method for the removal of compounds and halogenated organic compounds

실시예 4)Example 4

표1의 (A) 성분이 Bi2Ti2O7100g (C) 성분이 Ti 1g, (D) 성분이 V 1g인 것을 제외하고는 실시예 2와 동일한 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매 및 제조방법The same carbon monoxide, volatile organic compounds and halogenated organic compounds as in Example 2 were removed, except that 100 g of Bi 2 Ti 2 O 7 in component (A) and 1 g of Ti in component (C) were used. Oxidation Catalyst and Manufacturing Method

실시예 5)Example 5

표1의 (A) 성분이 Bi2O3100g (B) 성분이 B2O3100g, (C)성분이 Ag 1g (D) 성분이 Co 1g, (E) 성분이 Pt 1g, (F) 성분이 Ir 1g인 것을 제외하고는 실시예 1과 동일한 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물제거 산화촉매 및 제조방법Table 1 (A) is 100 g of Bi 2 O 3 (B) is 100 g of B 2 O 3 , (C) is Ag 1g (D) is Co 1g, (E) is Pt 1g, (F) Oxidation catalyst and preparation method for removing carbon monoxide, volatile organic compounds and halogenated organic compounds same as those of Example 1 except that the component is Ir 1g

실시예 6)Example 6

표1의 (A) 성분이 Bi2Ti2O320g, (B) 성분이 Cr3C2180g, (C) 성분이 Ni 1g, (D) 성분이 Au 1g, (E) 성분이 Pt 1g, (F) 성분이 Ru 1g인 것을 제외하고는 실시예 1과 동일한 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매및 제조방법(A) component of Table 1 20 g of Bi 2 Ti 2 O 3 , (B) component of Cr 3 C 2 180 g, (C) component of Ni 1g, (D) component of Au 1g, (E) component of Pt 1g , (F) The same oxidation catalyst as in Example 1 except that the component Ru is 1g, volatile organic compounds and halogenated organic compounds.

실시예 7)Example 7

표1의 (A) 성분이 Bi2O320g, (B) 성분이 Bi2Ti2O7180g, (C) 성분이 Cs 1g, (D) 성분이 Cu 1g, (E) 성분이 Ru 1g, (F) 성분이 Ir 1g인 것을 제외하고는 실시예 1과 동일한 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매 및 제조방법20 g of Bi 2 O 3 in component (A), 180 g of Bi 2 Ti 2 O 7 in component (B), 1 g of Cs in component (C), 1 g of Cu in component (D), and 1 g of Ru in component (E) , Oxidation catalyst and preparation method of the same carbon monoxide, volatile organic compounds and halogenated organic compounds as in Example 1, except that component (F) is Ir 1g

실시예 8)Example 8

표1의 (A) 성분이 Bi2Ti2O7200g인 것을 제외하고는 실시예 1과 동일한 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매 및 제조방법Oxidation catalyst and preparation method of carbon monoxide, volatile organic compounds and halogenated organic compounds same as those of Example 1 except that component (A) of Table 1 is 200 g of Bi 2 Ti 2 O 7

비교예 1)Comparative Example 1)

표1의 (A) 성분이 TiO2200g, (E) 성분이 Pt 4g인 것을 제외하고는 실시예 1과 동일한 일반적인 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매.The same oxidation catalyst as the general carbon monoxide, volatile organic compounds and halogenated organic compounds as in Example 1, except that component (A) of Table 1 is 200 g of TiO 2 and component (4) of Pt.

비교예 2)Comparative example 2)

표1의 (A) 성분이 SiO2200g, (C) 성분이 Co 2g으로 (E) 성분이 Pt 4g인것을 제외하고는 실시예 1과 동일한 일반적인 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매The same oxidation catalyst as in Example 1 is removed except that (A) is 200 g of SiO 2 , (C) is Co 2g, and (E) is 4t of Pt.

이상에서 상세히 설명한 바와 같이, 본 발명 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물질을 제거함에 있어서, 저온과 빠른 공간속도에서 휘발성유기화합물과 할로겐화 유기화합물의 산화 성능이 높고, 또한 일산화탄소의 산화 성능도 매우 높은 효과를 제공한다.As described in detail above, in the removal of the carbon monoxide, volatile organic compounds and halogenated organic compounds of the present invention, the oxidation performance of volatile organic compounds and halogenated organic compounds is high at low temperature and high space velocity, and the oxidation performance of carbon monoxide is also very high. Provides a high effect.

Claims (5)

내화성 화합물로 고체분말상의 B2O3, Bi2O3, Bi2Ti2O3, Cr3C2중 1개 이상의 화합물을 선택하고, 여기에 (A)그룹 금속으로 Ag, Au, Ni, Co, Cs, V, Cu, Ti중에서 1개이상, 그리고 (B)그룹금속으로 Pt, Ru, Ir중에서 1개이상 선택된 원소를 함유하는 방법이며, (A)그룹금속중 1개 이상의 원소 + (B)그룹금속중 1개 이상의 원소의 합이 담체로 사용되는 내화성 화합물에 대하여 0.1∼25중량％로 사용하는 것을 특징으로 하는 일산화탄소, 휘발성유기화합물, 및 할로겐화유기화합물 제거 산화촉매As the refractory compound, at least one compound of solid powder B 2 O 3 , Bi 2 O 3 , Bi 2 Ti 2 O 3 , Cr 3 C 2 is selected, and as the (A) group metal, Ag, Au, Ni, At least one of Co, Cs, V, Cu, Ti, and (B) a group metal containing at least one element selected from Pt, Ru, Ir, (A) at least one element of the group metal + ( B) Carbon monoxide, volatile organic compounds, and halogenated organic compounds removal oxidation catalyst, characterized in that the sum of at least one element in the group metal is used at 0.1 to 25% by weight relative to the refractory compound used as a carrier. 제 1항에 있어서 B2O3, Bi2O3, Bi2Ti2O3, Cr3C2의 사용량은 2개가 선택되었을 때 무게비가 99:1에서 1:99인 상태로 미세하게 분할된 유지물로 포함하는 것을 특징으로 하며, 3가지 무기산화물이 선택되면 먼저 선택된 2개의 무기산화물에 대하여 3번째 것은 1∼10 중량%로 첨가하는 것을 특징으로 하는 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매According to claim 1, wherein the amount of B 2 O 3 , Bi 2 O 3 , Bi 2 Ti 2 O 3 , Cr 3 C 2 is finely divided in a weight ratio of 99: 1 to 1:99 when two are selected. When the three inorganic oxides are selected, the third one is added in an amount of 1 to 10% by weight based on the first two inorganic oxides, and the carbon monoxide, the volatile organic compounds and the halogenated organic compounds are removed. Oxidation catalyst 삭제delete 제 1항에 있어서 (A)그룹 금속원소와 (B)그룹 금속원소와의 사용비는 무게비가 1:10 ∼ 10:1 인 것을 특징으로 하는 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매2. The catalyst for removing carbon monoxide, volatile organic compounds and halogenated organic compounds according to claim 1, wherein the use ratio of the metal group (A) and the metal group (B) is 1:10 to 10: 1 by weight. 제 1항에 있어서 내화성 화합물 혼합물은 수성 슬러리로 만들고 일체 구조를 갖는 허니콤에 워시코팅하고, 그후 120℃에서 6시간 이상 건조한후 선택된 하나 이상의 금속 혼합수용액을 내화성 화합물이 워시코팅된 허니콤에 담지시켜 120℃ 이상에서 6시간 이상 건조시킨후 400∼650℃에서 1∼4 시간 동안 소성시키며, 허니콤에 워시코팅되는 내화성 화합물은 허니콤 용적에 대하여 30 ∼ 250g/L(허니콤 용적)의 농도로 존재하는 것을 특징으로 하는 일산화탄소, 휘발성유기화합물 및 할로겐화유기화합물 제거 산화촉매 제조방법The refractory compound mixture according to claim 1, wherein the refractory compound mixture is made of an aqueous slurry and washcoated in a honeycomb having a monolithic structure, and then dried at 120 ° C. for at least 6 hours. After drying at 120 ° C or more for 6 hours or more and baking at 400 to 650 ° C for 1 to 4 hours, the refractory compound wash-coated with honeycomb has a concentration of 30 to 250 g / L (honeycomb volume) based on the honeycomb volume. Carbon monoxide, volatile organic compounds and halogenated organic compounds removal oxidation catalyst manufacturing method characterized in that present
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