CN103586022B - The Catalysts and its preparation method of high efficiency synchronous catalytic oxidation of low-concentration gaseous formaldehyde, carbon monoxide and hydrogen under room temperature condition - Google Patents
The Catalysts and its preparation method of high efficiency synchronous catalytic oxidation of low-concentration gaseous formaldehyde, carbon monoxide and hydrogen under room temperature condition Download PDFInfo
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- CN103586022B CN103586022B CN201310612996.7A CN201310612996A CN103586022B CN 103586022 B CN103586022 B CN 103586022B CN 201310612996 A CN201310612996 A CN 201310612996A CN 103586022 B CN103586022 B CN 103586022B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The invention provides under a kind of room temperature condition can the Catalysts and its preparation method of high efficiency synchronous catalytic oxidation of low-concentration gaseous formaldehyde, carbon monoxide and hydrogen.Catalyst in the present invention take titanium dioxide as carrier, and the two noble metal platinum of load and gold are as active component, and noble-metal-supported amount is 0.89 ~ 1.92wt%.The mode that described noble metal component platinum and gold adopt substep to introduce loads to titanium dioxide surface successively, first adopts infusion process Supported Pt Nanoparticles component, then adopts deposition-precipitation method gold-supported component.This catalyst can the efficient oxidation formaldehyde, carbon monoxide and hydrogen be water and carbon dioxide at ambient temperature, 54, and 000 ~ 200,000h
-1space velocity range in, the oxygenation efficiency of formaldehyde, carbon monoxide and hydrogen all can reach more than 95%, and oxidation product is carbon dioxide and water.The carrier of this catalyst is easy to get simultaneously, and the load capacity of noble metal is few, and preparation method is simple, can be widely used in closed in space and the process of Indoor environment purification of air.
Description
Technical field
The present invention relates to a kind of two noble metal catalyst and preparation method thereof, belong to technical field of air purification.
Background technology
Along with the fast development of science and technology, the position of the technical equipments such as spaceship, Space-Work station, submarine, deep water workboat, underground fortification, extraordinary chemical workshop, extraordinary laboratory in human civilization life is more and more important.Particularly the development of space flight and submarine technology is the symbol of national comprehensive strength, is the embodiment of whole National Technical level.Be the operation that manned spacecraft or submarine all need people, so the operating efficiency that the air quality in these closed in space drastically influence personnel in cabin is even healthy, and then threaten the safety of spacecraft and submarine.Therefore, the air quality improving closed in space and other confined spaces has become a urgent task.
In closed in space and other confined spaces, derive from the air quality that multiple light concentration gas pollutant that material outgassing, instrument and equipment release and human metabolism produce has a strong impact on cabin and other confined spaces.Wherein formaldehyde, carbon monoxide and hydrogen are typical micro-molecular gas pollutants, are difficult to effectively remove according to traditional treatment method such as absorption and absorption, and catalytic oxidation technologies then shows huge advantage in this pollutant of purification.In recent years, catalytic oxidation treatment gas phase low concentration formaldehyde has obtained new breakthrough and progress, and the open report such as patent CN200410102837.3 and CN200710121423.9 demonstrates the feasibility of platinum catalyst catalyze oxidation of formaldehyde under room temperature condition; Load type gold catalyst then achieves under cryogenic to the complete oxidation of carbon monoxide; And the oxidation for hydrogen, palladium-platinum bimetallic catalyst catalytic activity at room temperature is also gratifying.So independent catalyze oxidation of formaldehyde, carbon monoxide and hydrogen can carry out efficiently and stably on different catalyst under room temperature condition.But when these pollutants coexist in closed in space and other confined spaces, the catalyst of these patent literatures then faces can not synchronous high-efficiency purification, or catalyst poisoning and the catalytic activity that causes descends rapidly degradation problem.Such as, when correlative study result shows that carbon monoxide and formaldehyde coexist, the strong adsorption effect of carbon monoxide on platinum inhibits the Adsorption and decomposition of formaldehyde in platinum active sites, finally causes the decline of formaldehyde conversion.And the lower formaldehyde that causes of the oxidation activity of load type gold catalyst PARA FORMALDEHYDE PRILLS(91,95) is accumulated at catalyst surface, inhibit the oxidation of carbon monoxide in golden active sites, catalytic oxidation while mist can not be realized.Obviously, developing the catalyst of simultaneously catalyze oxidation of formaldehyde, carbon monoxide and hydrogen to be that catalytic oxidation technologies is applied in closed in space and the key of other confined space multiple pollutant gas treatment.
Summary of the invention
The present invention is directed to problems of the prior art, provide a kind of can the catalyst of high efficiency synchronous catalyze oxidation of formaldehyde, carbon monoxide and hydrogen.This catalyst uses commercial titanium dioxide to be carrier, and adopt infusion process and deposition-precipitation method carried noble metal platinum and gold as active component successively, preparation method is easy.Under room temperature condition, prepare gained catalyst 54,000 ~ 200,000h
-1space velocity range in, the oxygenation efficiency of formaldehyde, carbon monoxide and hydrogen all can reach more than 95%.Oxidation product is carbon dioxide and water.
In the present invention, the noble metal component platinum of catalyst and the total load amount of gold are 0.89 ~ 1.92wt%, wherein the load capacity of single metal component is 0.09 ~ 1.83wt%, and noble metal component platinum and gold element diverse ways are in turn carried on catalyst carrier titanium dioxide.The preparation method of this catalyst mainly comprises the following steps:
The first step, is scattered in deionized water by catalyst carrier titanium dioxide powder, forms uniform suspension, stirs under the rotating speed of 110rpm, adds presoma platinum salting liquid simultaneously, floods after 2 ~ 6 hours at 70 DEG C of rotary evaporation removing excessive moistures.Gained slurry 80 DEG C of vacuum drying 8 ~ 12 hours, then roasting 4 ~ 8 hours under the condition of 400 DEG C in air atmosphere.
Described presoma platinum salt is Pt (NO
3)
2, H
2ptCl
66H
2o and Pt (NO
2)
2(NH
3)
2in any one.
Second step, by above-mentioned steps gained sample dispersion in deionized water, form uniform suspension, stir under the rotating speed of 110rpm, regulate simultaneously and the pH value of suspension is stabilized between 9 ~ 10, add presoma gold salting liquid and stablize 2 ~ 6 hours at 60 DEG C of temperature, gained precipitation is through repeatedly suction filtration, deionized water are washed extremely without after chlorion, 80 DEG C of vacuum drying 8 ~ 12 hours, finally roasting 4 ~ 8 hours under the condition of 200 DEG C in air atmosphere, obtained required catalyst.
Described presoma gold salt is HAuCl
44H
2o and NaAuCl
42H
2any one in O.
The invention has the advantages that:
(1) preparation method is simple, and easily realize, the medicine adopted, reagent, equipment etc. are all common to be easy to get.
(2) catalyst can simultaneously by formaldehyde, carbon monoxide and hydrogen complete oxidation at ambient temperature.
(3) catalyst can keep the conversion ratio of formaldehyde, carbon monoxide and hydrogen all more than 95% in wider space velocity range, and oxidation product is only carbon dioxide and water.
(4) catalyst efficiency is high, simple equipments, is applicable to closed in space and the use of other limited-space environment.
Detailed description of the invention
In order to clearly the present invention is described, enumerate following examples, but it is without any restrictions to scope of the present invention.Below in conjunction with embodiment to low concentration formaldehyde, carbon monoxide and hydrogen under room temperature condition of the present invention simultaneously catalyst for catalytic oxidation and preparation method thereof be described in detail.
embodiment 1
Get 2 grams of TiO
2powder dispersion, in 50ml deionized water, adds 11.0mlPt (NO
3)
2solution impregnation 2 hours, 80 DEG C of vacuum drying 10 hours after 70 DEG C of rotary evaporations removing excessive moistures, then 400 DEG C of roastings 6 hours in air atmosphere.1 gram of gained sample is scattered in 50ml deionized water again, regulate by NaOH solution and the pH value maintaining suspension between 9 ~ 10, add 0.2mlNaAuCl
42 hours are stablized at 60 DEG C after solution, gained precipitation through repeatedly suction filtration, washing to without after chlorion, 80 DEG C of vacuum drying 10 hours, finally 200 DEG C of roastings 4 hours in air atmosphere, namely obtain embodiment 1 catalyst material, wherein the load capacity of platinum and gold is respectively 1.55wt% and 0.11wt%.
embodiment 2
Get 2 grams of TiO
2powder dispersion, in 50ml deionized water, adds 4.0mlH
2ptCl
6solution impregnation 6 hours, 80 DEG C of vacuum drying 8 hours after 70 DEG C of rotary evaporations removing excessive moistures, then 400 DEG C of roastings 4 hours in air atmosphere.1 gram of gained sample is scattered in 50ml deionized water again and forms suspension, regulate by NaOH solution and the pH value maintaining suspension between 9 ~ 10, add 0.4mlHAuCl
46 hours are stablized at 60 DEG C after solution, gained precipitation is through repeatedly suction filtration, deionized water are washed extremely without after chlorion, 80 DEG C of vacuum drying 8 hours, last 200 DEG C of roastings 8 hours in air atmosphere, namely obtain embodiment 2 catalyst material, wherein the load capacity of platinum and gold is respectively 0.74wt% and 0.15wt%.
embodiment 3
Get 2 grams of TiO
2powder dispersion, in 50ml deionized water, forms uniform suspension, adds 2.5mlPt (NO in suspension
2)
2(NH
3)
2solution impregnation 4 hours, 80 DEG C of vacuum drying 12 hours after 70 DEG C of rotary evaporations removing excessive moistures, then 400 DEG C of roastings 8 hours in air atmosphere.1 gram of gained sample is scattered in 50ml deionized water again, regulate by NaOH solution and the pH value maintaining suspension between 9 ~ 10, add 1.0mlNaAuCl
44 hours are stablized at 60 DEG C after solution, gained precipitation through repeatedly suction filtration, washing to without after chlorion, in 80 DEG C of vacuum 12 hours, finally 200 DEG C of roastings 6 hours in air atmosphere, namely obtain embodiment 3 catalyst material, wherein the load capacity of platinum and gold is respectively 0.44wt% and 0.53wt%.
embodiment 4
Get 2 grams of TiO
2powder dispersion, in 50ml deionized water, adds 5.0mlH
2ptCl
6solution impregnation 2 hours, 80 DEG C of vacuum drying 8 hours after 70 DEG C of rotary evaporations removing excessive moistures, then 400 DEG C of roastings 6 hours in air atmosphere.1 gram of gained sample is scattered in 50ml deionized water again, regulate by NaOH solution and the pH value maintaining suspension between 9 ~ 10, add 2.0mlNaAuCl
44 hours are stablized at 60 DEG C after solution, gained precipitation through repeatedly suction filtration, washing to without after chlorion, 80 DEG C of vacuum drying 8 hours, finally 200 DEG C of roastings 8 hours in air atmosphere, namely obtain embodiment 4 catalyst material, wherein the load capacity of platinum and gold is respectively 0.89wt% and 0.81wt%.
embodiment 5
Get 2 grams of TiO
2powder dispersion, in 50ml deionized water, adds 0.5mlPt (NO
3)
2solution impregnation 4 hours, 80 DEG C of vacuum drying 10 hours after 70 DEG C of rotary evaporations removing excessive moistures, then 400 DEG C of roastings 8 hours in air atmosphere.1 gram of gained sample is scattered in 50ml deionized water again, regulate by NaOH solution and the pH value maintaining suspension between 9 ~ 10, add 4.0mlHAuCl
46 hours are stablized at 60 DEG C after solution, gained precipitation through repeatedly suction filtration, washing to without after chlorion, 80 DEG C of vacuum drying 10 hours, finally 200 DEG C of roastings 4 hours in air atmosphere, namely obtain embodiment 5 catalysis material, wherein the load capacity of platinum and gold is respectively 0.12wt% and 1.78wt%.
embodiment 6
Get 2 grams of TiO
2powder dispersion, in 50ml deionized water, adds 14.0mlPt (NO
3)
2solution impregnation 2 hours, 80 DEG C of vacuum drying 10 hours after 70 DEG C of rotary evaporations removing excessive moistures, then 400 DEG C of roastings 6 hours in air atmosphere.1 gram of gained sample is scattered in 50ml deionized water again, regulate by NaOH solution and the pH value maintaining suspension between 9 ~ 10, add 0.1mlNaAuCl
42 hours are stablized at 60 DEG C after solution, gained precipitation through repeatedly suction filtration, washing to without after chlorion, 80 DEG C of vacuum drying 10 hours, finally 200 DEG C of roastings 4 hours in air atmosphere, namely obtain embodiment 1 catalyst material, wherein the load capacity of platinum and gold is respectively 1.83wt% and 0.09wt%.
comparative example 1
Get 1 gram of TiO
2powder dispersion, in 50ml deionized water, adds 2.0mlH
2ptCl
6and 0.4mlHAuCl
4solution impregnation 2 hours, 80 DEG C of vacuum drying 12 hours after 70 DEG C of rotary evaporations removing excessive moistures, finally 400 DEG C of roastings 4 hours in air atmosphere, namely obtain comparative example 1 catalysis material, wherein the load capacity of platinum and gold is respectively 0.76wt% and 0.13wt%.
comparative example 2
Get 1 gram of TiO
2powder dispersion in 50ml deionized water, regulate by NaOH solution and the pH value maintaining suspension between 9 ~ 10, add 2.0mlH
2ptCl
6solution and 0.4mlHAuCl
42 hours are stablized at 60 DEG C after solution, gained precipitation through repeatedly suction filtration, washing to without after chlorion, 80 DEG C of vacuum drying 12 hours, finally in air atmosphere in 200 DEG C of roastings 4 hours, namely obtain comparative example 2 catalysis material, wherein the load capacity of platinum and gold is respectively 0.72wt% and 0.14wt%.
comparative example 3
Get 1 gram of TiO
2powder dispersion, in 50ml deionized water, adds 2.5mlH
2ptCl
6solution impregnation 2 hours, 80 DEG C of vacuum drying 12 hours after 70 DEG C of rotary evaporations removing excessive moistures, finally 400 DEG C of roastings 4 hours in air atmosphere, namely obtain comparative example 3 catalysis material, wherein the load capacity of platinum is 0.88wt%.
comparative example 4
Get 1 gram of TiO
2powder dispersion in 50ml deionized water, regulate by NaOH solution and the pH value maintaining suspension between 9 ~ 10, add 2.0mlHAuCl
44H
2stablize 2 hours at 60 DEG C after O liquid, gained precipitation is through repeatedly suction filtration, washing to without after chlorion, and 80 DEG C of vacuum drying 12 hours, finally 200 DEG C of roastings 4 hours in air atmosphere, namely obtain comparative example 4 catalysis material, wherein golden load capacity was 0.93wt%.
comparative example 5
Get 1 gram of Al
2o
3powder dispersion in 50ml deionized water, regulate by NaOH solution and the pH value maintaining suspension between 9 ~ 10, add 2.0mlHAuCl
4stablize 2 hours at 60 DEG C after solution, gained precipitation is through repeatedly suction filtration, washing to without after chlorion, and 80 DEG C of vacuum drying 12 hours, finally 200 DEG C of roastings 4 hours in air atmosphere, namely obtain comparative example 5 catalysis material, wherein golden load capacity was 0.89wt%.
comparative example 6
Get 1 gram of Al
2o
3powder dispersion, in 50ml deionized water, adds 2.5mlH
2ptCl
6solution and 4.5mlPd (NO
3)
2solution impregnation 2 hours, 80 DEG C of vacuum drying 12 hours after 70 DEG C of rotary evaporations removing excessive moistures, finally 400 DEG C of roastings 4 hours in air atmosphere, namely obtain comparative example 6 catalysis material, wherein the load capacity of platinum and palladium is respectively 0.87wt% and 0.91wt%.
Get the catalyst material of certain mass comparative example 1 ~ comparative example 6 and embodiment 2 respectively, compressing tablet, the catalysis material 0.25g of screening 40 ~ 60 order particle diameters, be positioned over the evaluation experimental carrying out catalytic performance in fixed-bed micro-reactor, experiment condition is as follows: formaldehyde is produced by Bubbling method, and carbon monoxide and hydrogen are supplied by steel cylinder gas, and carrier gas is synthesis of air (oxygen 20%, nitrogen 80%), control concentration of formaldehyde is 133.9mg/m
3, carbonomonoxide concentration is 1000mg/m
3, density of hydrogen is 80mg/m
3, reaction velocity is 90,000h for (GHSV)
-1, reaction temperature is 25 DEG C.
Table 1 different catalysts room temperature is catalyze oxidation of formaldehyde, carbon monoxide and hydrogen expression activitiy simultaneously
Result is as shown in table 1, and catalyst of the present invention at ambient temperature PARA FORMALDEHYDE PRILLS(91,95), carbon monoxide and hydrogen all has very high catalytic activity, and the conversion ratio of formaldehyde, carbon monoxide and hydrogen and carbon dioxide selectivity are all higher than other catalyst.
Get the catalyst material of the certain mass platinum embodiment 1 ~ embodiment 6 different with golden constituent content respectively, compressing tablet, the catalysis material 0.25g of screening 40 ~ 60 order particle diameters, be positioned over the evaluation experimental carrying out catalytic performance in fixed-bed micro-reactor, experiment condition is as follows: formaldehyde is produced by Bubbling method, and carbon monoxide is supplied by steel cylinder gas, and carrier gas is synthesis of air (oxygen 20%, nitrogen 80%), control concentration of formaldehyde is 133.9mg/m
3, carbonomonoxide concentration is 1000mg/m
3, density of hydrogen is 80mg/m
3, reaction velocity is 90,000h for (GHSV)
-1, reaction temperature is 25 DEG C.
The different platinum of table 2 and golden constituent content catalyst room temperature catalyze oxidation of formaldehyde, carbon monoxide and hydrogen expression activitiy simultaneously
Result is as shown in table 2, catalyst of the present invention is (embodiment 2, embodiment 3, embodiment 5) when noble metal platinum load capacity is less than 0.74wt%, under room temperature condition, catalyst still has very high conversion ratio to carbon monoxide, but the activity decrease of catalysis formaldehyde and hydrogen, the selective of carbon dioxide also declines simultaneously.When noble metal platinum load capacity is greater than 1.83wt% (embodiment 6), the conversion ratio of catalyst to carbon monoxide is lower; When noble metal platinum load capacity is greater than (embodiment 1, embodiment 4) when 0.74wt% is less than 1.83wt%, the conversion ratio of catalyst PARA FORMALDEHYDE PRILLS(91,95), carbon monoxide and hydrogen and carbon dioxide selectivity all can reach more than 95%.Therefore for catalyst provided by the invention, the load capacity of preferred platinum is greater than 0.74wt% and is less than or equal to 1.83wt%.
Get the catalyst material of the embodiment 2 of certain mass, compressing tablet, the catalysis material 0.25g of screening 40 ~ 60 order particle diameters, be positioned over the evaluation experimental carrying out catalytic performance in fixed-bed micro-reactor, experiment condition is as follows: formaldehyde is produced by Bubbling method, and carbon monoxide is supplied by steel cylinder gas, and carrier gas is synthesis of air (oxygen 20%, nitrogen 80%), control concentration of formaldehyde is 133.9mg/m
3, carbonomonoxide concentration is 1000mg/m
3, density of hydrogen is 80mg/m
3, reaction temperature is 25 DEG C.
Embodiment 2 room temperature catalyze oxidation of formaldehyde, carbon monoxide and hydrogen expression activitiy simultaneously under the different air speed of table 3
Result is as shown in table 3, catalyst of the present invention 54,000 ~ 120,000h
-1space velocity range in, the conversion ratio of PARA FORMALDEHYDE PRILLS(91,95), carbon monoxide and hydrogen and carbon dioxide selectivity all can reach more than 95%, stable in catalytic performance.
Claims (3)
1. the preparation method of the catalyst of high efficiency synchronous catalytic oxidation of low-concentration gaseous formaldehyde, carbon monoxide and hydrogen under room temperature condition, is characterized in that:
The first step, is scattered in deionized water by catalyst carrier titanium dioxide powder, forms uniform suspension, stirs under the rotating speed of 110rpm, adds presoma platinum salting liquid simultaneously, floods after 2 ~ 6 hours at 70 DEG C of rotary evaporation removing moisture; Gained slurry 80 DEG C of vacuum drying 8 ~ 12 hours, then roasting 4 ~ 8 hours under the condition of 400 DEG C in air atmosphere;
Second step, by above-mentioned first step gained sample dispersion in deionized water, form uniform suspension, stir under the rotating speed of 110rpm, regulate simultaneously and the pH value of suspension is stabilized between 9 ~ 10, adding presoma gold solution and stablize 2 ~ 6 hours at 60 DEG C of temperature, gained precipitation is through repeatedly suction filtration, deionized water are washed extremely without after chlorion, 80 DEG C of vacuum drying 8 ~ 12 hours, finally roasting 4 ~ 8 hours under the condition of 200 DEG C in air atmosphere, obtained required catalyst; This catalyst is with TiO
2for carrier, with precious metals pt and Au for active component, the total load amount of Pt and Au is 0.89 ~ 1.92wt%, wherein the load capacity 0.09 ~ 1.83wt% of single metal.
2. preparation method according to claim 1, is characterized in that: the presoma of precious metals pt is Pt (NO
3)
2, H
2ptCl
66H
2o and Pt (NO
2)
2(NH
3)
2in any one; The presoma of noble metal Au is HAuCl
44H
2o and NaAuCl
42H
2any one of O.
3. preparation method according to claim 1, is characterized in that: the load capacity 0.74 ~ 1.83wt% preparing single metal Pt in the catalyst obtained.
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| EP3150553A1 (en) * | 2015-09-30 | 2017-04-05 | Casale SA | Method for purification of a co2 stream |
| CN105749974A (en) * | 2016-02-06 | 2016-07-13 | 慈溪市梦园果蔬专业合作社 | Formaldehyde degradation catalyst and preparation method thereof |
| CN106268299B (en) * | 2016-08-22 | 2019-03-29 | 湖北格林森绿色环保材料股份有限公司 | A kind of microporous medium catalysis oxidation prepares the method and material for air purification of material for air purification |
| CN109395573A (en) * | 2018-11-29 | 2019-03-01 | 河北迪酷环保科技有限公司 | A kind of nanogold compound biological enzyme removes aldehyde eliminating smell agent |
| CN110628274A (en) * | 2019-10-12 | 2019-12-31 | 谢海峰 | For removing H2CO and HCHO paint and preparation method thereof |
| CN110721680A (en) * | 2019-10-23 | 2020-01-24 | 中国科学院生态环境研究中心 | Catalyst for simultaneously catalyzing and oxidizing formaldehyde and CO, and preparation method and application thereof |
| CN112427035A (en) * | 2020-11-24 | 2021-03-02 | 吉林大学 | High-dispersion supported ruthenium hydroxide catalyst, preparation method and application thereof in selective oxidation of alcohol |
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| EP1676625A1 (en) * | 2004-12-28 | 2006-07-05 | Mitsubishi Denki Kabushiki Kaisha | Method and catalyst for the oxidative decomposition of formaldehyde gas |
| CN101559377A (en) * | 2009-05-21 | 2009-10-21 | 浙江师范大学 | Supported catalyst for eliminating formaldehyde, preparation method and application thereof |
| CN102247837A (en) * | 2010-05-18 | 2011-11-23 | 上海牛翼新能源科技有限公司 | Titanium oxide supported catalyst for eliminating formaldehyde in microenvironment air |
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| EP1676625A1 (en) * | 2004-12-28 | 2006-07-05 | Mitsubishi Denki Kabushiki Kaisha | Method and catalyst for the oxidative decomposition of formaldehyde gas |
| CN101559377A (en) * | 2009-05-21 | 2009-10-21 | 浙江师范大学 | Supported catalyst for eliminating formaldehyde, preparation method and application thereof |
| CN102247837A (en) * | 2010-05-18 | 2011-11-23 | 上海牛翼新能源科技有限公司 | Titanium oxide supported catalyst for eliminating formaldehyde in microenvironment air |
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