CN101618350A - Mesoporous alumina carrier capable of reducing content of carbon monoxide in cigarette smoke, preparation method and application thereof - Google Patents

Mesoporous alumina carrier capable of reducing content of carbon monoxide in cigarette smoke, preparation method and application thereof Download PDF

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Publication number
CN101618350A
CN101618350A CN200910305600A CN200910305600A CN101618350A CN 101618350 A CN101618350 A CN 101618350A CN 200910305600 A CN200910305600 A CN 200910305600A CN 200910305600 A CN200910305600 A CN 200910305600A CN 101618350 A CN101618350 A CN 101618350A
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carrier
meso
cigarette
catalyst
carbon monoxide
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银董红
刘建福
秦亮生
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China Tobacco Hunan Industrial Co Ltd
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China Tobacco Hunan Industrial Co Ltd
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Abstract

The invention relates to a catalyzer carrier capable of reducing the content of carbon monoxide in cigarette smoke at normal temperature, a preparation method and an application thereof, belonging to the field of reducing harm and coke from cigarettes. A guidance agent with a different structure is used for synthesizing mesoporous alumina with higher specific surface and more surface alkalescence positions as the catalyzer carrier. The surface alkalescence of mesoporous metallic alumina is from 0.01-0.08 mmol/g, and the surface isoelectric point (IEP value) pH is from 8 to 10. By adding a catalyzer prepared by the carrier to a cigarette filter stick, the content of the carbon monoxide in the cigarette smoke can be selectively reduced.

Description

A kind of mesoporous alumina carrier and preparation and application that can be used for reducing the cigarette smoke carbon monoxide content
Technical field
The invention belongs to cigarette lowering harm and decreasing coking field, specifically, relate to a kind of catalyst carrier and preparation method and application that can be used for to reduce at normal temperatures the cigarette smoke carbon monoxide content.
Background technology
In recent years, people have carried out big quantity research aspect the CO burst size in reducing cigarette smoke, adoptable method mainly comprise to the cigarette tipping paper punching and increase mode such as cigarette paper natural permeable degree dilute flue gas concentration, add expanded cut tobacco or reconstituted tobacoo with reduce the pipe tobacco consumption, add combustion adjuvant make the pipe tobacco burning more complete, use composite filter tip to hold back CO and use catalyst that CO is converted into CO by absorption 2Deng.Early 1980s, the river, city of Japan is taken charge of clearly and has been invented a kind of porous material (as active carbon) filter tip [U.S.Patent 4414988] of Protoporphyrins compound solution of ferrous ion that contained the dipping chelating, can effectively remove CO, benzo [a] pyrene and derivative thereof etc. in the flue gas.Catalyst is added in the filter tip forming paper, also it can be loaded on the porous carriers such as active carbon, molecular sieve, make composite filter tip [U.S.Patent, 4022223] then.It is CO that a kind of CO catalytic oxidation under low temperature has been invented by Britain Gallaher company 2Additives of filter tip [U.S.Patent, 4450245], crystallite (polycrystalline particle) form that this catalyst is made up of Cr, Sn, noble metal, transition metal and VI, VII, VIII family metal, be dispersed in to heavens and make in the whole pore system of carrier (molecular sieve, diatomite etc.), in addition, carrier itself also can play catalytic action sometimes, and like this, this class catalyst often plays bifunctional effect.BP in 1980 has been reported catalyst [the UK Patent of load 6wt%Cu and 0.5wt%Pd isoreactivity component on the 13X molecular sieve, 2042364A], be used for the CO oxidation of cigarette smoke, the CO conversion ratio can reach 76% when reaction temperature is 150 ℃, and the rising of reaction temperature or reduction all make catalyst activity reduction.1997, a United States Patent (USP) report [U.S.Patent, 5671758] was with V 2O 5, Mo 2O 3Or Rh 2This class simple oxide such as O adds in the filter tip on active carbon or other filtering material as catalyst cupport again, all can make the CO in the flue gas be oxidized to CO 2Loaded with nano metal oxide catalyst [CN1805694] on the high surface area carrier particle such as is reined at by KB section, makes an addition in pipe tobacco or the cigarette paper, it is said to reduce carbon monoxide content in the main flume.Zhu Jianhuas etc. have been invented a kind of mesoporous silicon based functional material [CN1460641] that contains rare earth metal or transition metal atoms, can reduce nitroso compound total content minimizing 30~47% in the cigarette smoke.Meng Zhaoyu etc. have invented a kind of mesoporous silicon based molecular sieve (as MCM-41, SBA-15 etc.) adsorbent of cigarette filter tip usefulness surface modification and preparation method thereof [CN101077223], add this adsorbent to make in the cigarette filter composite tip stick and can obviously reduce harmful substance contents such as the tar in the flue gas, low molecule aldehyde ketone, nitrosamine, condensed-nuclei aromatics, can improve the organoleptic quality of cigarette simultaneously.
Yet, have the mesoporous metal oxide alumina supporter of surface alkalinty and use it for harmful substances such as reducing in the cigarette smoke carbon monoxide and do not appear in the newspapers as yet with preparation.
Summary of the invention
Purpose of the present invention aims to provide the meso-porous alumina that can be used for reducing the employed special carrier Zhao of harmful substance catalyst tool surface alkalinty such as carbon monoxide in the cigarette smoke, and economy and the simple preparation method of preparation process.
The invention provides a kind of meso-porous alumina that has surface alkalinty especially, and be applied to prepare the catalyst carrier that reduces the carbon monoxide burst size in the cigarette mainstream flue gas in the cigarette.
The objective of the invention is to realize in the following manner:
Described carrier is a meso-porous alumina, and described mesoporous alumina carrier surface alkalinty position is: 0.01~0.08mmol[OH -]/g, surperficial isoelectric point is pH=8~10.
The mesoporous alumina carrier specific surface is 100~400m 2/ g, the aperture is 2.0~10nm.
Meso-porous alumina also is doped with rare earth metal or its oxide, as La, and Ce etc.
Meso-porous alumina (Al of the present invention 2O 3) preparation method of carrier is:
The present invention is with shitosan, surfactant P123 (EO 20PO 70EO 20), in the softex kw (CTABr) one or more are as structure directing agent, with aluminum nitrate, aluminium secondary butylate etc. is the aluminium source, has prepared the meso-porous alumina (Al that has than high-ratio surface and more surface alkalinty position by hydrolysis, isolated by filtration, drying, roasting 2O 3) carrier.
At meso-porous alumina (Al 2O 3) also can mix in the preparation process of carrier and add rare earth compound and be prepared.
With the above-mentioned meso-porous alumina (Al for preparing 2O 3) carrier, adopt the homogeneous deposition precipitation method, deposition-precipitation method that nano metal catalytic active component (as one or more catalytic active component in the noble metals such as gold (Au), platinum Pt and palladium Pd) high degree of dispersion has been prepared the mesoporous metal oxide Al catalysts that contains nano metal in carrier surface.
The mesoporous metal oxide Al catalysts that contains of preparation is made an addition in cigarette filter rod or cigarette forming paper and the groove paper surface, be used for reducing cigarette mainstream flue gas carbon monoxide burst size.
Preparation method's concrete steps of the present invention are as follows:
Mesoporous Al 2O 3The preparation of carrier
With shitosan, P123 (EO 20PO 70EO 20) and softex kw (CTABr) in one or more be structure directing agent, with aluminum nitrate, aluminium secondary butylate etc. is the aluminium source, add certain rare earth compound (as La, Ce etc.), prepared the meso-porous alumina (Al that has than high-ratio surface and more surface alkalinty position by steps such as hydrolysis, isolated by filtration, drying and roastings 2O 3) carrier.
The used mesoporous alumina carrier of the present invention is different from traditional mesoporous silicon based carrier, be characterized in that carrier surface has abundant surface alkalinty position, surface isoelectric point height, help precious metal catalyst active components such as nanometer Au, Pt that load height disperses and Pd, and traditional mesoporous silicon based mesoporous carrier surface isoelectric point is low, is difficult to obtain nanometer Au, Pt and the Pd catalyst of high dispersive.In addition, be carrier with the meso-porous alumina of the present invention preparation, tenor is low in the metallic catalyst of preparation, and the decentralization height is higher to removing in the flue gas catalytic activity of CO.Use the prepared catalyst of carrier of the present invention and also have the characteristics that can significantly reduce carbon monoxide content in the cigarette mainstream flue gas under the normal temperature, removal efficiency can reach 10-30%; The present invention prepares simply, and easy to operate, cost is low.
Description of drawings
Accompanying drawing 1: with meso-porous alumina (meso-Al of the present invention 2O 3-a) the 2.0%Au of load (HDP) catalyst TEM photo and goldc grains footpath distribution map.
Accompanying drawing 2: with meso-porous alumina (meso-Al of the present invention 2O 3-b) the 2.0%Au of load (HDP) catalyst TEM photo and goldc grains footpath distribution map.
Accompanying drawing 3: with meso-porous alumina (meso-Al of the present invention 2O 3-c) the 2.0%Au of load (HDP) catalyst TEM photo and goldc grains footpath distribution map.
Accompanying drawing 4: with meso-porous alumina (meso-Al of the present invention 2O 3-d) the 2.0%Au of load (HDP) catalyst TEM photo and goldc grains footpath distribution map.
The specific embodiment
Following examples are intended to illustrate the present invention rather than limitation of the invention further.
Embodiment 1
Carrier meso-Al 2O 3-a's is synthetic: 6.078g touches plate agent P123 (EO 20PO 70EO 20) and 0.060g LaCl 3Be dissolved in together in the 25ml sec-butyl alcohol, stir adding 5.4ml aluminium secondary butylate down.After stirring 1h under the room temperature, with the mixed liquor (1.14mlH of water and sec-butyl alcohol 2O/10mlsec-butanol) slowly be added dropwise to wherein, mixture consists of 0.01La 3+: 1.0Al (Bu sO) 3: 0.10EO 20PO 70EO 20: 3.0H 2O:15.5Bu sOH.Mixture continues down to stir 48 hours at 45 ℃, filters, and drying, in air atmosphere, 500 ℃ of calcining 6h obtain product, are labeled as meso-Al 2O 3-a.Use low temperature N 2The adsorption-desorption method is measured meso-Al 2O 3The specific surface of-b is 325m 2/ g, pore volume are 0.93cm 3/ g, average pore size is 7.5nm; Use CO 2Temperature programmed desorption (CO 2-TPD) method to measure its surface alkalinty be 0.0369mmol[OH -]/g; Carrier surface isoelectric point IEP is pH=8.4.
Get certain amount of H AuCl 4(concentration is 9.71mmol/L) and 1.0g carrier meso-Al 2O 3-a mixes, and slowly is heated to 70-80 ℃.Meanwhile add urea and transfer the pH=7 of solution, under this temperature, keep 4h.Filter, hot water (70-80 ℃) washing is used AgNO for several times 3(0.10mol/L) detect no Cl -, 70 ℃ of following dry 8-10h.Calcine 1.0h down at 350 ℃ then, be cooled to normal temperature, use hydrogen reducing 1.0h down at 300-350 ℃ again, obtain catalyst A u/meso-Al 2O 3-a.Use low temperature N 2The adsorption-desorption method is measured Au/meso-Al 2O 3The specific surface of-a (HDP) is 258m 2/ g, pore volume are 0.49cm 3/ g, average pore size is 4.9nm; The average-size that adopts transmission electron microscope (TEM) to observe carrier surface nanometer Au particle is 4.4nm.(seeing accompanying drawing 1).
With catalyst A u/meso-Al 2O 3-a compressing tablet, sieve, choose 40-60 order particle and be scattered in the diacetate fiber, make the cigarette binary compound filter candle, contain catalyst 40mg in every cigarette filter rod, the composite filter cigarette is become cigarette.Suction on FiltronaCOA200 orthoscopic smoking machine (suction capacity 35ml/min), according to the CO content in YC/T-30-1996 (non-scattering infrared method) the mensuration cigarette smoke, contrast with the cigarette that does not add catalyst, the result shows, compare with the contrast cigarette, the prepared catalyst of the present invention can make CO content decline 15% in the main flume.
Embodiment 2
Carrier meso-Al 2O 3-b's is synthetic: (a) 0.8gNaOH is dissolved in 4mlH 2Among the O, join in the 80ml triethanolamine, 120 ℃ down heating 5min under agitation the 21.8ml aluminium secondary butylate is added dropwise to wherein to remove water wherein, be heated to 150 ℃ and kept 10 minutes, this is a solution one; (b) under 60 ℃, 14.56g softex kw (CTABr) is dissolved in the 240ml water, this is a solution two; (c) keep 60 ℃ of constant temperature, under vigorous stirring, solution one is slowly joined in the solution two ageing 72h.Filter, use the absolute ethanol washing secondary, 30 ℃ of dryings, 500 ℃ of calcining 5h obtain product in the air atmosphere, are labeled as meso-Al 2O 3-b.Use low temperature N 2The adsorption-desorption method is measured meso-Al 2O 3The specific surface of-b is 302m 2/ g, pore volume are 0.78cm 3/ g, average pore size is 7.2nm; Use CO 2Temperature programmed desorption (CO 2-TPD) method to measure its surface alkalinty be 0.0606mmol[OH -]/g; Carrier surface isoelectric point IEP is pH=9.4.
Obtain catalyst A u/meso-Al according to method for preparing catalyst among the embodiment 1 2O 3-b.Use low temperature N 2The adsorption-desorption method is measured Au/meso-Al 2O 3The specific surface of-b (HDP) is 310m 2/ g, pore volume are 0.48cm 3/ g, average pore size is 4.0nm; The average-size that adopts transmission electron microscope (TEM) to observe carrier surface nanometer Au particle is 3.2nm.(seeing accompanying drawing 2)
With catalyst A u/meso-Al 2O 3-b compressing tablet, sieve, choose 40-60 order particle and be scattered in the diacetate fiber, make the cigarette binary compound filter candle, contain catalyst 40mg in every cigarette filter rod, the composite filter cigarette is become cigarette.Press the CO content in the method mensuration cigarette mainstream flue gas in the embodiment 1, contrast with the cigarette that does not add catalyst, the result shows, compares with the contrast cigarette, and the prepared catalyst of the present invention can make CO content decline 26.4% in the main flume.
Embodiment 3
Carrier meso-Al 2O 3-c's is synthetic: with 4.60gAl (NO 3) 39H 2O be dissolved in 20ml go dried up in, then this solution is slowly joined the 50mlCH that contains the 1.50g shitosan 3In the COOH solution (5%V/V), under vigorous stirring, kept one hour.And then this solution slowly is added to 800ml50%V/V) in the ammonia spirit, under vigorous stirring, kept one hour.Filter normal temperature dry 72 hours down then.550 ℃ of calcinings obtained product in 1.5 hours in the air atmosphere, were labeled as meso-Al 2O 3-c.Use low temperature N 2The adsorption-desorption method is measured meso-Al 2O 3The specific surface of-c is 271m 2/ g, pore volume are 0.48cm 3/ g, average pore size is 4.9nm; Use CO 2Temperature programmed desorption (CO 2-TPD) method to measure its surface alkalinty be 0.0503mmol[OH -]/g; Carrier surface isoelectric point IEP is pH=9.2.
Obtain catalyst A u/meso-Al according to method for preparing catalyst among the embodiment 1 2O 3-c.Use low temperature N 2The adsorption-desorption method is measured Au/meso-Al 2O 3The specific surface of-c (HDP) is 292m 2/ g, pore volume are 0.47cm 3/ g, average pore size is 4.5nm; The average-size that adopts transmission electron microscope (TEM) to observe carrier surface nanometer Au particle is 3.6nm, sees accompanying drawing 3..
With catalyst A u/meso-Al 2O 3-c (HDP) compressing tablet, sieve, choose 40-60 order particle and be scattered in the diacetate fiber, make the cigarette binary compound filter candle, contain catalyst 40mg in every cigarette filter rod, the composite filter cigarette is become cigarette.Press the CO content in the method mensuration cigarette mainstream flue gas in the embodiment 1, contrast with the cigarette that does not add catalyst, the result shows, compares with the contrast cigarette, and the prepared catalyst of the present invention can make CO content decline 24.3% in the main flume.
Embodiment 4
Carrier meso-Al 2O 3-d's is synthetic: 3.038g touches plate agent P123 (EO 20PO 70EO 20) and 0.030g LaCl 3Be dissolved in together in the 12.5ml sec-butyl alcohol, be configured to solution 1; Under the vigorous stirring 1.0g shitosan is dissolved in 30ml CH 3In the COOH solution (5%V/V), wiring solution-forming 2.Under the stirring at room, with the mixed liquor (1.14mlH of water and sec-butyl alcohol 2O/10mlsec-butanol) slowly be added dropwise in the mixed solution of solution 1 and solution 2, continue down to stir 48 hours, filter at 45 ℃, drying, in air atmosphere, 500 ℃ of calcining 6h obtain product, are labeled as meso-Al 2O 3-d.Use low temperature N 2The adsorption-desorption method is measured meso-Al 2O 3The specific surface of-d is 290m 2/ g, pore volume are 0.76cm 3/ g, average pore size is 7.0nm; Use CO 2Temperature programmed desorption (CO 2-TPD) method to measure its surface alkalinty be 0.0467mmol[OH -]/g; Carrier surface isoelectric point IEP is pH=8.9.
Obtain catalyst A u/meso-Al according to method for preparing catalyst among the embodiment 1 2O 3-d.Use low temperature N 2The adsorption-desorption method is measured Au/meso-Al 2O 3The specific surface of-a (HDP) is 236m 2/ g, pore volume are 0.54cm 3/ g, average pore size is 5.3nm; The average-size that adopts transmission electron microscope (TEM) to observe carrier surface nanometer Au particle is 4.9nm, (seeing accompanying drawing 4).
With catalyst A u/meso-Al 2O 3-d compressing tablet, sieve, choose 40-60 order particle and be scattered in the diacetate fiber, make the cigarette binary compound filter candle, contain catalyst 40mg in every cigarette filter rod, the composite filter cigarette is become cigarette.Press the CO content in the method mensuration cigarette mainstream flue gas in the embodiment 1, contrast with the cigarette that does not add catalyst, the result shows, compares with the contrast cigarette, and the prepared catalyst of the present invention can make CO content decline 20% in the main flume.
Embodiment 5
Meso-Al with preparation among the embodiment 2 2O 3-b is a carrier, prepares mesoporous Al according to embodiment 1 method 2O 3-b carrier surface load Au and Pt alloy catalyst.Get certain amount of H AuCl 4And H 2PtCl 21 (atomic ratio)) and 1.0g carrier meso-Al (concentration is respectively 9.71mmol/L to solution, Au: Pt=1: 2O 3-b mixes, and slowly is heated to 70-80 ℃.Meanwhile add urea and transfer the pH=7 of solution, under this temperature, keep 4h.Filter, hot water (70-80 ℃) washing is used AgNO for several times 3(0.10mol/L) detect no Cl-, 70 ℃ of following dry 8-10h.Calcine 1.0h down at 350 ℃ then, be cooled to normal temperature, use hydrogen reducing 1.0h down at 300-350 ℃ again, obtain catalyst A u-Pt/meso-Al 2O 3-b (HDP).Use low temperature N 2The specific surface that the adsorption-desorption method is measured catalyst is 293m 2/ g, pore volume are 0.47cm 3/ g, average pore size is 4.5nm, the average-size of carrier surface nanometer Au particle is 3.8nm.With catalyst A u-Pt/meso-Al 2O 3-b compressing tablet, sieve, choose 40-60 order particle and be scattered in the diacetate fiber, make the cigarette binary compound filter candle, contain catalyst 40mg in every cigarette filter rod, the composite filter cigarette is become cigarette.Press the CO content in the method mensuration cigarette mainstream flue gas in the embodiment 1, contrast with the cigarette that does not add catalyst, the result shows, compares with the contrast cigarette, and the Au-Pt nanocatalyst of the meso-porous alumina load that the present invention is prepared can make CO content decline 26% in the main flume.
Embodiment 6
Meso-Al with preparation among the embodiment 3 2O 3-c is a carrier, obtains catalyst Pt-Au/meso-Al according to method for preparing catalyst among the embodiment 5 2O 3-c (HDP) catalyst (Pt: Au atomic ratio=1: 1).With catalyst Pt-Au/meso-Al 2O 3-c (HDP) compressing tablet, sieve, choose 40-60 order particle and be scattered in the diacetate fiber, make the cigarette binary compound filter candle, contain catalyst 40mg in every cigarette filter rod, the composite filter cigarette is become cigarette.Press the CO content in the method mensuration cigarette mainstream flue gas in the embodiment 1, contrast with the cigarette that does not add catalyst, the result shows, compares with the contrast cigarette, adopts the prepared catalyst of carrier of the present invention can make CO content decline 25.1% in the main flume.
Embodiment 7
Au/meso-Al with preparation among the embodiment 3 2O 3-c catalyst compressing tablet, sieve, choose the forming paper surface that 40-60 order particle is coated cigarette paper, roll into cigarette, contain catalyst 20mg in every cigarette.Press the CO content in the method mensuration cigarette mainstream flue gas in the embodiment 1, contrast with the cigarette that does not add catalyst, the result shows, compares with the contrast cigarette, adopts the prepared catalyst of carrier of the present invention can make CO content decline 20.9% in the main flume.

Claims (6)

1. a mesoporous alumina carrier that can be used for reducing carbon monoxide content in the cigarette smoke is characterized in that, described carrier is a meso-porous alumina; Described mesoporous alumina carrier surface alkalinty position is: 0.01~0.08mmol[OH-]/g, surperficial isoelectric point is pH=8~10.
2. carrier according to claim 1 is characterized in that, the specific surface of described mesoporous alumina carrier is 100~400m2/g, and the aperture is 2.0~10nm.
3. carrier according to claim 1 and 2 is characterized in that, meso-porous alumina also is doped with rare earth metal or its oxide.
4. the method for preparing the described carrier of claim 1, it is characterized in that, may further comprise the steps: one or more in employing shitosan, surfactant P123, the softex kw are as structure directing agent, with aluminum nitrate or sec-butyl alcohol is the aluminium source, makes by hydrolysis, isolated by filtration, drying, roasting.
5. the preparation method of a kind of mesoporous alumina carrier according to claim 4 is characterized in that, also mixing is added with rare earth compound.
6. the application of the described meso-porous alumina of claim 1 is characterized in that, described meso-porous alumina is used for preparing the catalyst of the carbon monoxide burst size that reduces cigarette mainstream flue gas.
CN200910305600A 2009-08-13 2009-08-13 Mesoporous alumina carrier capable of reducing content of carbon monoxide in cigarette smoke, preparation method and application thereof Pending CN101618350A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101999756A (en) * 2010-11-02 2011-04-06 湖南中烟工业有限责任公司 Absorbent for reducing hydrocyanic acid content of main stream smoke of cigarettes and use thereof
CN102793270A (en) * 2012-08-07 2012-11-28 广西中烟工业有限责任公司 Cigarette filter rod capable of reducing content of volatile carbonyl compounds in cigarette smoke and preparation method of cigarette filter rod
WO2015117269A1 (en) * 2014-02-07 2015-08-13 East China University Of Science And Technology Methods, systems and catalysts for oxidizing carbon monoxide to carbon dioxide

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101999756A (en) * 2010-11-02 2011-04-06 湖南中烟工业有限责任公司 Absorbent for reducing hydrocyanic acid content of main stream smoke of cigarettes and use thereof
CN102793270A (en) * 2012-08-07 2012-11-28 广西中烟工业有限责任公司 Cigarette filter rod capable of reducing content of volatile carbonyl compounds in cigarette smoke and preparation method of cigarette filter rod
CN102793270B (en) * 2012-08-07 2013-12-25 广西中烟工业有限责任公司 Cigarette filter rod capable of reducing content of volatile carbonyl compounds in cigarette smoke and preparation method of cigarette filter rod
WO2015117269A1 (en) * 2014-02-07 2015-08-13 East China University Of Science And Technology Methods, systems and catalysts for oxidizing carbon monoxide to carbon dioxide
US10130941B2 (en) 2014-02-07 2018-11-20 East China University Of Science And Technology Methods, systems and catalysts for oxidizing carbon monoxide to carbon dioxide

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