CN113083324B - Formaldehyde oxidation catalyst used at room temperature and preparation method thereof - Google Patents
Formaldehyde oxidation catalyst used at room temperature and preparation method thereof Download PDFInfo
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Abstract
The invention provides a method for formaldehyde oxidation at room temperaturePt/NiO @ NiMnO of x (2.5<x<3) A catalyst and a preparation method thereof. The catalyst has a core-shell structure as a carrier, niO nanoparticles as a core and NiMnO as a shell layer x Amorphous complex oxide of which 2.5<x<3; the active component is Pt, and the load of the Pt is 0.1 to 1.0 wt.%. The preparation method comprises the steps of preparation of a carrier with a core-shell structure, loading of an active component, reduction activation of a catalyst and the like. The catalyst of the invention has high formaldehyde oxidation activity and good stability, and can completely convert 300ppm of formaldehyde into CO at room temperature 2 And H 2 O, and the conversion rate remained stable for 60 hours continuously. The catalyst has the advantages of low Pt loading capacity, low price, simple preparation and good formaldehyde purification effect, and is suitable for industrial production and application.
Description
Technical Field
The invention relates to the field of environmental catalysis and the field of indoor air purification, and the formaldehyde in air is catalytically oxidized under room temperature. The catalyst can be used for catalytically oxidizing 300ppm of formaldehyde gas into carbon dioxide and water at room temperature, the conversion rate of formaldehyde can reach 100%, and the conversion rate is kept stable after continuous reaction for 60 hours.
Background
Formaldehyde is an important chemical raw material and widely exists in building materials, decoration materials and textiles. The formaldehyde in these materials is slowly released and ubiquitous in the indoor environment, becoming a major indoor air pollutant. The long-term exposure in even a low-concentration formaldehyde environment can cause great harm to human bodies, and respiratory diseases and even carcinogenesis can be caused. The condition that the indoor formaldehyde exceeds the standard in China is still very serious, so that the method for effectively eliminating the formaldehyde in the indoor air has great application value.
At present, the widely applied indoor formaldehyde purification technology is physical or chemical adsorption and photocatalysis. Adsorption technology has limited energy absorption capacity of the adsorption material, so the adsorption material needs to be replaced regularly, the application cost is high, and secondary pollution can be generated. The light source required by the photocatalytic technology is generally high-energy ultraviolet light, the energy consumption is high, byproducts are easily generated to cause secondary pollution, and in addition, the photocatalyst is also easily inactivated. The room temperature formaldehyde oxidation catalysis technology is an ideal indoor formaldehyde purification method due to the advantages of high purification efficiency, no secondary pollution, no need of additional energy input and the like, and the key point is the formaldehyde oxidation catalyst with high activity and high stability.
The catalyst for formaldehyde oxidation at room temperature is generally a catalyst taking noble metal as an active component, for example, patent CN 106040230a loads Pt on boehmite and applies the Pt to formaldehyde catalytic oxidation reaction, and the catalyst is found to have good adsorption performance on formaldehyde, and can oxidize part of formaldehyde at room temperature. When the Pt content is 2 to 2.5 wt.%, the conversion rate of formaldehyde at normal temperature is 72 percent, and the conversion rate is 60 percent o C can be completely converted. The patent CN 106492792A uses the titanium dioxide nanobelt after acid treatment as a carrier and Pt as an active component to prepare the supported formaldehyde oxidation catalyst. Wherein the loading amount of Pt is 0.5 wt%, the particle size is 2-4nm, and metallic Pt and ionic Pt coexist. The catalyst has the full formaldehyde conversion temperature of 41.9% under the environment with room temperature and relative humidity RH = 0-80%, the Pt load is improved to 1.5 wt%, and the room temperature conversion rate of formaldehyde reaches 100%. The type and nature of the support also has a significant effect on the catalyst activity. Such as Colussi et al (Catalysis Today 253 (2015) 163-171) with CeO 2 ，TiO 2 ，Al 2 O 3 And ZrO 2 Equal load of 1 wt% Pt for formaldehyde oxidation reaction, pt/Al 2 O 3 Highest activity, 25 o The formaldehyde conversion at C was 62%. Patent CN 106964348A compares P25, al 2 O 3 And the effect of AlOOH as a support on the activity of the Pt-based catalyst, 1 wt% Pt/AlOOH formaldehyde activity is higher than Pt/P25 and Pt/Al under the same conditions 2 O 3 。
The Pt-based catalyst has good catalytic performance for formaldehyde oxidation reaction based on the above, but there is less research on the stability of the catalyst. In addition, most of the catalysts have high Pt content, and the application of the Pt-based catalyst in indoor formaldehyde purification is limited due to high price and small storage capacity. Therefore, the development of a Pt-based catalyst with low load, high activity and stability has great practical significance by selecting a proper carrier.
Disclosure of Invention
Aiming at the defects of high Pt loading, high price and limited application of the existing Pt-based catalyst for realizing the full conversion of formaldehyde, the invention aims to develop a catalyst which can completely convert indoor harmful gas formaldehyde into CO under the room temperature condition 2 And H 2 O, or a salt thereof. The catalyst has the characteristics of low platinum loading capacity, high formaldehyde oxidation activity, high stability, relatively low price and the like. The formaldehyde eliminating agent is suitable for effectively eliminating formaldehyde in closed spaces or semi-closed spaces such as production workshops, building material and decoration material markets, home environments and the like.
The purpose of the invention can be realized by the following technical scheme: a formaldehyde oxidation catalyst used at room temperature comprises a carrier and an active component.
The carrier is of a core-shell structure, niO nano particles are used as a core, and amorphous composite oxide NiMnO is used x Is a shell, wherein 2.5<x<3。
The active component is Pt, and the loading amount of the Pt is 0.1 to 1wt.%.
In the carrier, the particle size of the NiO nano-particles is 2-20 nm.
In the carrier, the molar ratio of Ni/(Ni + Mn) is 0.1 to 0.5.
The carrier is obtained by the following method: the precipitation sequence is controlled by controlling the adding sequence of manganese and nickel precursors, after a precipitator is added, a coprecipitate with the center of nickel salt precipitation and the shell of manganese-nickel composite precipitation is formed, and then NiO @ NiMnO with a core-shell structure is obtained by washing, drying and roasting x （2.5<x<3) Carrier
The Mn precursor comprises manganese nitrate, manganese sulfate, manganous chloride and manganese acetate.
The Ni precursor comprises nickel nitrate, nickel sulfate, nickel chloride and nickel acetate.
The precipitator is one or more of sodium carbonate, sodium hydroxide, ammonia water or oxalic acid, and the addition molar amount of the precipitator is 2 times or more of the total molar amount of the metal ions.
The roasting temperature of the carrier is 350-450 ℃.
A method for preparing a formaldehyde oxidation catalyst, the method comprising the steps of:
soaking the carrier in Pt precursor water solution, and finally drying, roasting and reducing by hydrogen to obtain Pt/NiO @ NiMnO x （2.5<x<3) A catalyst.
The precursor of Pt is selected from H 2 PtCl 6 、Pt(NO 3 ) 2 、PtCl 4 、Pt(NH 3 ) 4 Cl 2 And Pt (NH) 3 ) 4 (NO 3 ) 2 One kind of (1).
H 2 The reduction temperature is between 200 and 300 ℃, and the reduction time is 0.5 to 2 hours. Compared with the prior art, the invention has the following advantages.
1. In the preparation process of the catalyst carrier, the selection of the type of the precipitator, the roasting temperature and the auxiliary agent can greatly influence the crystal phase of manganese species and the structure of the carrier. Different crystalline phases, e.g. amorphous manganese oxide, mn 2 O 3 、Mn 3 O 4 And the like, has obvious influence on the formaldehyde oxidation activity. Through a large number of experiments, the invention preferably selects amorphous NiMnO x （2.5<x<3) The crystal phase with optimal activity is adopted; the NiO nano-particles are preferably selected as the core, so that on one hand, the redox performance of the manganese oxide and the adsorption performance of formaldehyde can be enhanced, on the other hand, the interaction between the carrier and the active component Pt can be promoted, the chemical state of Pt can be adjusted, and further, the formaldehyde oxidation performance of the catalyst can be improved.
2. The carrier is prepared by a distributed precipitation method, and the precipitator is one or more of sodium carbonate, sodium hydroxide, ammonia water or oxalic acid. Firstly adding a nickel precursor and a precipitator into deionized water to form a nickel salt precipitate, and then simultaneously adding the nickel precursor, the manganese precursor and the precipitator to form a manganese-nickel composite precipitate at the periphery of the nickel salt precipitate. Washing, drying and roasting the obtained precipitate to obtain NiO @ NiMnO x （2.5<x<3) A carrier with a core-shell structure. Pt is loaded on a carrier by an impregnation method, for example, the carrier is impregnated in a Pt precursor water solution, and finally Pt/NiO @ NiMnO is obtained by drying, roasting and hydrogen reduction activation x （2.5<x<3) A catalyst.
Drawings
FIG. 1 shows the stability of the catalyst obtained in examples 13 to 15 at 25 ℃ in the formaldehyde oxidation reaction.
Detailed Description
The formaldehyde oxidation catalyst and the preparation method thereof according to the present invention are further illustrated by the following specific examples, and it should be noted that the following examples are only for describing the contents of the present invention, and the scope of the present invention is not limited to these examples. It is within the scope of the present invention to make simple modifications or substitutions to the methods, procedures or conditions for preparing the catalyst of the present invention without departing from the spirit or essential attributes thereof; the basic operations used in the examples are conventional and well known to those skilled in the art, unless otherwise specified. The evaluation of the formaldehyde oxidation activity of the catalyst is carried out in a fixed bed reactor, the concentration of formaldehyde is 300ppm, the balance is air, and the mass space velocity is 40000 mL/g.h.
Example 1
Adding 0.016 mol of Mn (NO) 3 ) 2 Dissolving the manganese oxalate into 200 mL deionized water, and adding 0.032 mol of oxalic acid as a precipitator to obtain manganese oxalate precipitate. Filtering, washing and drying the precipitate, and roasting at 350 ℃ for 2 hours to obtain amorphous MnO x （1.5<x<2) A catalyst.
Example 2
Adding 0.016 mol of Mn (NO) 3 ) 2 Dissolving the manganese oxalate into 200 mL deionized water, and adding 0.032 mol of oxalic acid as a precipitator to obtain manganese oxalate precipitate. Filtering, washing and drying the precipitate, and roasting at 400 ℃ for 2 hours to obtain MnO 2 A catalyst.
Example 3
0.016 mol of Mn (NO) 3 ) 2 Dissolving the manganese oxalate into 200 mL deionized water, and adding 0.032 mol of oxalic acid as a precipitator to obtain manganese oxalate precipitate. Filtering, washing and drying the precipitate, and roasting at 450 ℃ for 2 hours to obtain Mn 2 O 3 A catalyst.
Example 4
0.016 mol of Ni (NO) 3 ) 2 Dissolving in 200 mL deionized water, and adding 0.032 mol of oxalic acid as a precipitating agent to obtain nickel oxalate precipitate. And filtering, washing and drying the precipitate, and roasting at 400 ℃ for 2 hours to obtain the NiO catalyst.
Example 5
Preparation of MnO in example 1 x （1.5<x<2) Oxide, then 0.004 mol Ni (NO) by the isovolumetric impregnation method 3 ) 2 Drying and roasting at 400 ℃ for 2 hours to obtain 0.2NiO/MnO x （1.5<x<2) Catalyst, wherein the molar ratio Ni/(Ni + Mn) is 0.2.
Example 6
NiO oxide was prepared in the same manner as in example 2, followed by impregnation of 0.004 mol of Mn (NO) by an isovolumetric impregnation method 3 ) 2 Drying and roasting at 400 ℃ for 2 hours to obtain 0.2MnO x /NiO（1.5<x<2) Catalyst, wherein the Mn/(Ni + Mn) molar ratio is 0.2.
Example 7
0.001 mol of Ni (NO) 3 ) 2 Dissolving in 200 mL deionized water, adding 0.002 mol oxalic acid as a precipitator to obtain nickel oxalate precipitate. Then 0.018 mol of Mn (NO) 3 ) 2 And 0.001 mol of Ni (NO) 3 ) 2 Dissolving the solution in the above liquid, adding 0.038 mol oxalic acid as precipitant to form composite precipitate of manganese oxalate and nickel oxalate around the nickel oxalate precipitate. Filtering, washing, drying and roasting at 400 ℃ for 2 hours to obtain 0.1Nio @ NiMnO with a core-shell structure x （2.5<x<3) A catalyst.
Example 8
0.002 mol of Ni (NO) 3 ) 2 Dissolving in 200 mL deionized water, adding 0.004 mol oxalic acid as a precipitating agent to obtain nickel oxalate precipitate. Then 0.016 mol of Mn (NO) 3 ) 2 And 0.002 mol of Ni (NO) 3 ) 2 Dissolving the solution in the above liquid, adding 0.036 mol oxalic acid as precipitant to form composite precipitate of manganese oxalate and nickel oxalate around the nickel oxalate precipitate. The obtained precipitate is filtered, washed, dried and cooled to 400 DEG CRoasting for 2 hours to obtain 0.2NiO @ NiMnO of core-shell structure x （2.5<x<3) A catalyst.
Example 9
The catalysts obtained in examples 1 to 8 were subjected to a formaldehyde oxidation activity test. Evaluation of the catalytic oxidation activity of formaldehyde of each catalyst was carried out in a fixed bed reactor (quartz tube, inner diameter 6 mm) under normal pressure. The mass of the catalyst is 0.30 g, the concentration of formaldehyde is 300ppm 2 The bubbling flow rate and the air flow rate are respectively 30 and 170 mL/min, and the mass space velocity is WHSV = 40000 mL g -1 ·h -1 . The temperature of the catalyst bed layer is increased from 25 ℃ to 200 ℃, and the temperature rising rate is 2 ℃/min. And (4) detecting the concentration of the formaldehyde at the inlet and the outlet on line by using a GC2060 gas chromatograph (Porapak-Q chromatographic column). The conversion of formaldehyde was calculated using the following formula: conversion = (C) in -C out ）/C in X 100%. Wherein C is in And C out The concentrations (ppm) of the formaldehyde at the inlet and outlet, respectively. The formaldehyde oxidation activity of the catalyst obtained in each of the examples is shown in Table 1. As can be seen from Table 1, pure manganese oxide has poor activity, and amorphous MnO is contained in manganese oxides of different crystal forms x （1.5<x<2) The total conversion temperature is the lowest and is 138 ℃. The activity of the pure nickel oxide catalyst is worse, and the full conversion temperature of 300ppm formaldehyde reaches 188 ℃. NiO is simply supported in MnO x （1.5<x<2) The formaldehyde oxidation activity of the catalyst is not improved. The existence of a core-shell structure greatly improves the activity of the nickel-manganese composite catalyst, wherein 0.2NiO @ NiMnO x （2.5<x<3) The activity is highest, and the full conversion temperature of 300ppm formaldehyde is 97 ℃. Generally speaking, for a catalyst containing no noble metal, the conversion rate of formaldehyde at room temperature is very low, and the elimination of formaldehyde at room temperature in daily life is difficult to meet. In order to further improve the formaldehyde purification efficiency at room temperature, the subsequent examples were carried out with Pt loading, and the formaldehyde purification effect was tested.
TABLE 1 catalysts obtained in examples 1 to 8 have catalytic Formaldehyde oxidation activity
Example 10
MnO preparation by the method of example 1 x （1.5<x<2) A carrier;
2g of MnO was taken x （1.5<x<2) The carrier was impregnated with 2 mL at a concentration of 0.001g Pt H/mL 2 PtCl 6 Drying the mixture in an aqueous solution, roasting the dried mixture for 2 hours at 400 ℃ in an air atmosphere, and finally reducing the dried mixture for 1 hour in hydrogen at 300 ℃ to obtain Pt/MnO x （1.5<x<2) A catalyst wherein the Pt loading is 0.1 wt%.
Example 11
Prepared by the method of example 7 to obtain 0.1NiO @ NiMnO x （2.5<x<3) A carrier;
2g of 0.1NiO @ NiMnO was taken x （2.5<x<3) The carrier was impregnated with 2 mL at a concentration of 0.001g Pt H/mL 2 PtCl 6 Drying in water solution, roasting in air atmosphere at 400 ℃ for 2 hours, and finally reducing in hydrogen at 300 ℃ for 1 hour to obtain Pt/0.1NiO @ NiMnO x （2.5<x<3) A catalyst wherein the Pt loading is 0.1 wt%.
Example 12
Prepared by the method of example 8 to obtain 0.2NiO @ NiMnO x （2.5<x<3) A carrier;
taking 2g of 0.2NiO @ NiMnO x （2.5<x<3) The carrier was impregnated with 2 mL at a concentration of 0.001g Pt H/mL 2 PtCl 6 Drying in water solution, roasting in air atmosphere at 400 ℃ for 2 hours, and finally reducing in hydrogen at 300 ℃ for 1 hour to obtain Pt/0.2NiO @ NiMnO x （2.5<x<3) A catalyst wherein the Pt loading is 0.1 wt%.
Example 13
The catalyst was prepared analogously to example 12, with the difference that H was used 2 PtCl 6 The concentration of the aqueous solution was 0.002g Pt and/mL. The prepared Pt/0.2NiO @ NiMnO x （2.5<x<3) The catalyst Pt loading was 0.2 wt%.
Example 14
Preparation method of catalystThe process is similar to example 13, except that sodium carbonate is used as the precipitant in the preparation of the support, and the amount of sodium carbonate added is 0.040 mol. The prepared Pt/0.2NiO @ NiMnO x （2.5<x<3) The catalyst Pt loading was 0.2 wt%.
Example 15
The catalyst was prepared in a similar manner to example 13, except that the precursor of Pt was Pt (NO) 3 ) 2 Pt (NO) used 3 ) 2 The concentration of the aqueous solution was 0.002g Pt and/mL. The prepared Pt/0.2NiO @ NiMnO x （2.5<x<3) The catalyst Pt loading was 0.2 wt%.
Example 16
The preparation method of the catalyst is similar to that of example 14, except that the calcination temperature of the carrier is 450 ℃ and the calcination time is 2 hours. The prepared Pt/0.2NiO @ NiMnO x （2.5<x<3) The catalyst Pt loading was 0.2 wt%.
Example 17
The formaldehyde oxidation activity of the catalysts obtained in examples 10 to 16 was measured by the method of example 9, and the formaldehyde oxidation activity of each of the catalysts obtained is shown in table 2. The stability test was performed on catalysts (examples 13 to 15) having a formaldehyde conversion of 100% at room temperature. The test conditions were similar to the activity test except that the catalyst bed temperature was always controlled at 25 ℃ and the conversion of formaldehyde was measured every 1 hour. The formaldehyde oxidation stability of the catalysts obtained in examples 13 to 15 is shown in FIG. 1.
As can be seen from table 2, the room temperature formaldehyde oxidation activity of the catalysts obtained in the examples was greatly improved after Pt loading. The introduction of NiO is also beneficial to the oxidation of formaldehyde, and particularly, pt is loaded on NiO @ NiMnO x （2.5<x<3) The structure of the carrier shows the best formaldehyde catalytic activity, and when the Pt loading is 0.2 wt percent, the Pt/0.2NiO @ NiMnO x （2.5<x<3) The catalyst can completely oxidize 300ppm formaldehyde at room temperature. The catalyst with the same components and structure prepared by the precipitator type and the Pt precursor type in the preparation process of the replaced carrier has similar formaldehyde oxidation activity, thereby being beneficial to the industrial production and the preparation of the catalystApplication is carried out. From the stability test results in FIG. 1, it can be seen that the Pt loading was 0.2 wt.% Pt/0.2NiO @ NiMnO x （2.5<x<3) The catalyst continuously reacts for 60 hours, the conversion rate of formaldehyde at room temperature is maintained at 100%, and the catalyst has stable formaldehyde oxidation performance and practical application value.
TABLE 2 catalysts obtained in examples 10 to 16 have formaldehyde catalytic oxidation activity
Claims (10)
1. A formaldehyde oxidation catalyst used at room temperature, which comprises a carrier and an active component, and is characterized in that: the carrier is of a core-shell structure, niO nano particles are used as cores, and amorphous composite oxide NiMnO is used x Is a shell, wherein 2.5<x<3; the active component is Pt, and the loading amount of the Pt is 0.1 to 1wt.%.
2. The formaldehyde oxidation catalyst as recited in claim 1, wherein the NiO nanoparticles in the carrier have a particle size of 2 to 20nm.
3. The formaldehyde oxidation catalyst according to claim 1, wherein the molar ratio of Ni/(Ni + Mn) in the carrier is from 0.1 to 0.5.
4. The formaldehyde oxidation catalyst according to claim 1, wherein the carrier is obtained by the following method: the precipitation sequence is controlled by controlling the adding sequence of manganese and nickel precursors, the nickel precursor and a precipitator are firstly added into deionized water to form a nickel salt precipitate, then the nickel precursor, the manganese precursor and the precipitator are simultaneously added, a manganese-nickel composite precipitate is formed at the periphery of the nickel salt precipitate to form a coprecipitate with a nickel salt precipitate at the center and a manganese-nickel composite precipitate at the shell layer, and NiO @ NiMnO with a core-shell structure is obtained by washing, drying and roasting x （2.5<x<3) And (3) a carrier.
5. The formaldehyde oxidation catalyst as set forth in claim 4 wherein the Mn precursor includes manganese nitrate, manganese sulfate, manganous chloride and manganese acetate.
6. The formaldehyde oxidation catalyst according to claim 4, wherein the Ni precursor comprises nickel nitrate, nickel sulfate, nickel chloride and nickel acetate.
7. The formaldehyde oxidation catalyst according to claim 4, wherein the precipitant is one or more selected from the group consisting of sodium carbonate, sodium hydroxide, ammonia water and oxalic acid, and the precipitant is added in a molar amount of 2 times or more of the total molar amount of the metal ions.
8. The formaldehyde oxidation catalyst according to claim 4, wherein the calcination temperature of the carrier is from 350 ℃ to 450 ℃.
9. A method for preparing the formaldehyde oxidation catalyst as set forth in any one of claims 1 to 8, characterized in that the method comprises the steps of: soaking the carrier in Pt precursor water solution, and finally drying, roasting and reducing by hydrogen to obtain Pt/NiO @ NiMnO x （2.5<x<3) A catalyst.
10. The method for preparing the formaldehyde oxidation catalyst according to claim 9, wherein the precursor of Pt is selected from H 2 PtCl 6 、Pt(NO 3 ) 2 、PtCl 4 、Pt(NH 3 ) 4 Cl 2 And Pt (NH) 3 ) 4 (NO 3 ) 2 One kind of (1).
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