AU2020103244A4 - Preparation of CuO-LaCoO3 mesoporous supported catalyst - Google Patents
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Abstract
The invention discloses a preparation method of a mesoporous supported catalyst CuO
LaCoO3. Immersing the mesoporous LaCoO3 in copper nitrate solution, and calcinating the
mesoporous LaCoO3 impregnated with Cu ions in muffle furnace at 400-600°C for 4-6 hours,
so as to obtain the final CuO-LaCoO3. The raw materials required are simple and easy to
obtain, and the preparation price is lower than that of precious metal catalysts. Components in
the obtained CuO-LaCoO3 catalyst are uniformly dispersed and interact with each other, which
shows good low-temperature catalytic activity and thermal stability against CO in exhaust gas,
which can be applied in the field of automobile exhaust gas catalysis. The loading of CuO
provides more active oxygen for the original catalyst, thus improving the low-temperature
catalytic activity of the catalyst.
Description
Preparation of CuO-LaCoO3 mesoporous supported catalyst
[01] The invention belongs to the technical field of catalyst, in particular to a preparation method of mesoporous supported catalyst CuO-LaCO3.
[02] Compared with the traditional noble metal (Pt, Ru, Pd) catalysts, the rare earth calcium titanate catalyst ABO3 is a multifunctional catalyst with low cost, stable structure, good catalytic activity and high temperature thermodynamic stability, which is widely used in photocatalysis, thermocatalysis and other catalytic fields. The catalytic mechanism of CO in automobile exhaust is as follows: B ions adsorb gaseous oxygen, adsorbed CO and CO2 on lattice oxygen. The catalytic oxidation reaction is carried out by CO adsorbed and gaseous adsorbed oxygen, and finally CO is oxidized to CO2.
[03] In the field of automobile exhaust redox catalysis, La-Co-O perovskite has relatively good effect and has been more studied. However, due to its poor low temperature ignition characteristics, low specific surface area, and complex components, it is difficult to prepare in batches. Therefore, it limits the advantages of perovskite materials and their practical applications.
[04] The purpose of the present invention is to provide a preparation method of a mesoporous supported catalyst CuO-LaCoO3, which has the advantages of large specific surface area, uniform loading and high activity in low temperature catalytic oxidation of carbon monoxide.
[05] In order to achieve the above purpose, the technical scheme is as follows:
[06] The preparation method of a mesoporous supported catalyst CuO-LaCoO3 has comprises the following steps:
[07] Immersing the mesoporous LaCoO3 in copper nitrate solution, and calcinating the mesoporous LaCoO3 impregnated with Cu ions in muffle furnace at 400 600°C for 4-6 hours, so as to obtain the final CuO-LaCO3.
[08] According to the above technical solution, the preparation process of mesoporous LaCoO3 is as follows:
[09] 1) Taking P123 as the template, n-butanol as the organic additive, tetraethyl silicate as the silicon source, and solvothermal method to prepare the template KIT-6;
[010] 2) Weighing the equivalent amounts of lanthanum nitrate and cobalt nitrate which are dissolved in the ethanol aqueous solution, adding citric acid monohydrate as the chelating agent, and stirring them for reaction to obtain the precursor;
[011] 3) Adding the template obtained in step 1, heating and stirring it until it is viscous;
[012] 4) Transferring the template to the oven for drying to obtain a dry gel, and roast it in the electric furnace to remove citric acid to obtain the black fluffy solid;
[013] 5) The black fluffy solid is heated and calcined in the muffle furnace to obtain the LaCoO3 black powder containing the template;
[014] 6) Washing the template-containing LaCoO3 black powder with sodium hydroxide solution, so as to obtain mesoporous LaCoO3.
[015] According to the above technical solution, the preparation process of the template KIT-6 is as follows:
[016] Completely dissolving P123 and n-butanol in hydrochloric acid, then adding tetraethyl silicate to continue stirring and mixing evenly;
[017] Transferring the solution to the reaction kettle for hydrothermal reaction at 100-130 °C for 24;
[018] Cooling it to room temperature, taking out the lining. Performing filtering, washing and drying respectively to obtain the white powder;
[019] Calcining the obtained powder in a muffle furnace at 550 °C for 5-7h to obtain the KIT-6 template.
[020] According to the above scheme, the ratio of anhydrous ethanol to deionized water in the aqueous solution of ethylene glycol in step 2) is 3: 1.
[021] According to the above scheme, the temperature rise rate is 2°C/min, the calcination temperature is 700 °C and the calcination time is 4-8h in step 5).
[022] According to the above scheme, the concentration of the sodium hydroxide solution in step 6) is 2 mol/L, and the washing and heating temperature is 40-80°C and the time is 6-12 hours.
[023] The invention has the following beneficial effects:
[024] The raw materials required are simple and easy to obtain, and the preparation price is lower than that of precious metal catalysts.
[025] Components in the obtained CuO-LaCoO3catalyst are uniformly dispersed and interact with each other, which shows good low-temperature catalytic activity and thermal stability against CO in exhaust gas, which can be applied in the field of automobile exhaust gas catalysis.
[026] The loading of CuO provides more active oxygen for the original catalyst, thus improving the low-temperature catalytic activity of the catalyst.
[027] Fig. 1 is the XRD pattern of a series of mesoporous LACO3 catalysts.
[028] Fig. 2 is the XRD pattern of mesoporous supported CuO-LaCoO3 catalyst.
[029] Fig. 3 is the CO conversion efficiency of a series of catalysts.
[030] Fig. 4 is the TEM diagram of the template KIT-6 obtained in Example 1.
[031] Fig. 5 is the TEM diagram of a series of mesoporous LACO3 catalysts.
[032] Fig. 6 is the TEM diagram of CuO-LaCoO3 catalyst loaded with CuO in Example 2.
[033] The following examples further illustrate the technical scheme of the present invention, but they are not taken as limiting the scope of protection of the present invention.
[034] Example 1
[035] The preparation of mesoporous LaCoO3 catalyst with large specific surface area comprises the following steps:
[036] Preparation of template KIT-6: taking P123 as the template, n-butanol as the organic additive, tetraethyl silicate as the silicon source, and solvothermal preparation as the method; The specific process is as follows: dissolving 6g of P123 and 6g of n-butanol in 217g of deionized water and 11.4g of 37% hydrochloric acid, which are stirred at 38°C for 1 hour until completely dissolved, then adding 12.9g of tetraethyl silicate and continue to stir for 24 hours; Transferring the obtained solution to the reaction kettle, and hydrothermally reacted at 100°C for 24h; Cooling the reaction kettle to room temperature, taking out the inner lining, and performing filtering, washing, and drying to obtain the white powder; The obtained powder is calcined in a muffle furnace at 550°C for 5 hours to obtain KIT-6 template. The TEM image of the prepared template KIT-6 is shown in Figure 4, which clearly shows a very ordered mesoporous structure.
[037] Respectively taking 8mmol lanthanum nitrate and cobalt nitrate into 80ml aqueous solution, taking 8mmol of monohydrate citric acid as the chelating agent which is added to the precursor, and stirring them overnight at room temperature;
[038] Adding l6mmol of the prepared template slowly while stirring, heating and stirring until the template is viscous;
[039] Transferring the wet gel to the oven for drying to obtain a dry gel, and roasting it in the electric furnace for 2 hours to remove citric acid, so as to obtain a black fluffy body;
[040] Calcining Black fluffy solid in the muffle furnace at 700°C for 6h at the heating rate of 2°C/min, so as to obtain LaCoO3 black powder containing template;
[041] Taking the sodium hydroxide solution with the concentration of 2mol/L to wash away SiO2 by stirring them at 40°C for 12 hours to obtain mesoporous perovskite LaCoO3, which is denoted as LaCoO3-CoHi.
[042] The XRD pattern of the obtained mesoporous LaCoO3-CoHi perovskite is shown in Fig. 1, and the target product is generated. Transmission electron microscopy (tem) images are shown in Fig. 5C and Fig.5D. It can be seen that perovskite LaCoO3 CoHi only partially replicates the mesoporous structure of template KIT-6, and some places are still disordered and non-mesoporous. The reason may be as follows: the precursor has high solubility in water, calcination can produce LaCoO3 well. However, the water and ability are too strong, which makes it difficult for the precursors to aggregate and migrate on the surface of the mesoporous silica template, so that the final product has a low degree of order.
[043] Example 2
[044] To prepare mesoporous LaCoO3 catalyst with large specific surface area, it comprises the following steps:
[045] Dissolving 8mmol of lanthanum nitrate and cobalt nitrate in 80ml of ethanol solution (the volume ratio of absolute ethanol to deionized water is 3:1), adding 8mmol of citric acid monohydrate to the precursor as the chelating agent, and stirring them at room temperature for one night;
[046] Adding l6mmol of the prepared template slowly while stirring, heating and stirring until the template is viscous;
[047] Transferring the wet gel to the oven for drying to obtain the dry gel, and roasting it in the electric furnace for 2 hours to remove citric acid to obtain a black fluffy solid;
[048] Calcining the black fluffy solid at 700°C for 6 hours in muffle furnace at a heating rate of 2°C/min to obtain LaCoO3 black powder containing template;
[049] With 2mol/L sodium hydroxide solution, stirring the powder at 40°C for 12h to wash awaySiO 2 , so as to obtain mesoporous perovskite LaCoO3,which is named as LaCoO3-C3Hi.
[050] The XRD pattern of the obtained mesoporous LaCoO3-C3Hi perovskite is shown in Fig. 1, and the target product is generated. The transmission electron microscope images are shown in Fig. 5A and Fig. 5B. it can be seen that the perovskite product LaCoO3-C3Hi well replicates the mesoporous structure of template KIT-6, with uniform pore size and order. The selected area electron diffraction pattern (SAED) in Figure 5A also shows the polycrystalline features of the resulting LaCoO3 sample. The results show that the mesoporous LaCoO3prepared by this solvent ratio has high yield and good structure, which is beneficial to the uniform dispersion and loading of CuO.
[051] Example 3
[052] To prepare a mesoporous LaCoO3 catalyst with a large specific surface area, it includes the following steps:
[053] Taking 8mmol of lanthanum nitrate and cobalt nitrate into 80ml of absolute ethanol, putting 8mmol of citric acid monohydrate as the chelating agent, which is added to the precursor, and stirring them at room temperature overnight;
[054] Slowly adding l6mmol of prepared template under stirring, heating and stirring it until it is viscous; Transferring the wet gel to the oven for drying to obtain the dry gel, and roasting it in the electric furnace for 2 hours to remove citric acid to obtain a black fluffy body;
[055] Calcining the black fluffy solid in the muffle furnace at the heating rate of 2°C/min at 700°C for 6 hours to obtain the black LaCoO3 powder containing the template;
[056] Use a sodium hydroxide solution with a concentration of 2mol/L and stir at °C for 12 hours to wash away theSiO 2 toobtain the mesoporous perovskite LaCoO3, denoted as LaCoO3-CiHo.The XRD pattern of the obtained mesoporous LaCoO3-CiH perovskite is shown in Fig. 1. The characteristic diffraction line intensity is low, that is, the amount of LaCoO3finally produced is small and the effect is not good. Analyzing the reason, it may be that the solubility of the precursor in ethanol is lower than that in water, and part of the precursor is not dissolved, resulting in a low production rate of the final product.
[057] With 2mol/L sodium hydroxide solution, stirring the powder at 40°C for 12h to wash away SiO2, so as to obtain mesoporous perovskite LaCoO3, which is named as LaCoO3-CiHo.
[058] The XRD pattern of mesoporous LaCoO3-CiHo perovskite is shown in Fig. 1, and the intensity of characteristic diffraction line is low, that is, the amount of LaCoO3 finally produced is small, and the effect is not good. The reason may be that the solubility of precursors in ethanol is lower than that in water, and some precursors are not dissolved. Therefore, the final product generation rate is low.
[059] Example 4:
[060] The preparation method of a mesoporous supported catalyst CuO-LaCoO3, which includes the following steps:
[061] Mesoporous LaCoO3 with large specific surface area obtained in Example 1; According to the ratio of ncu: nla = 1: 10, dissolving copper nitrate was in 1.5ml of deionized water, and a certain concentration of copper nitrate solution is prepared and impregnated on a certain amount of mesoporous LaCoO3 by equal volume impregnation method.
[062] The above LaCoO3 impregnated with Cu ions is calcined in the muffle furnace at 500°C for 4 ~ 6 hours, and finally 10% CuO-LaCoO3 can be obtained.
[063] The XRD patterns of mesoporous LaCoO3 obtained in example 3 and CuO LaCoO3 obtained in example 4 are shown in Fig. 2. There are only characteristic diffraction peaks of LaCoO3 and CuO, but no other heterogeneous characteristic peaks, indicating that the sample prepared in example 3 is a single-phase LaCoO3 perovskite, and CuO is formed on the surface of LaCoO3 in example 4, instead of Cu entering the perovskite skeleton.
[064] Example 5:
[065] The preparation method of a mesoporous supported catalyst CuO-LaCoO3, which includes the following steps:
[066] Preparation of template KIT-6: P123 is used as a template, n-butanol is used as an organic additive, and tetraethyl silicate is used as a silicon source, and prepared by solvothermal method;
[067] Dissolving 8mmol of lanthanum nitrate and cobalt nitrate dissolved in 80ml of ethanol aqueous solution (the volume ratio of absolute ethanol to deionized water is 3:1), and weighing 8mmol of monohydrate citric acid as the chelating agent, which is added to the precursor at room temperature, and stirring it overnight;
[068] Slowly adding l6mmol of the prepared template under stirring, heating and stirring until it is viscous;
[069] Transferring the wet gel to the oven to dry to obtain a dry gel, and roasting it in the electric furnace for 2 hours to remove citric acid to obtain a black fluffy solid;
[070] Calcining the black fluffy solid in the muffle furnace at the heating rate of 2°C/min at 700°C for 6 hours to obtain the LaCoO3 black powder containing the template;
[071] Mesoporous LaCoO3 with large specific surface area is obtained by washingSiO 2 with 2mol/L sodium hydroxide solution at 40°C for 12h;
[072] According to the ratio of nCu:nLa=1:20, dissolving copper nitrate and in 1.5ml of deionized water, preparing a certain concentration of copper nitrate solution and impregnating a certain amount of mesoporous LaCoO3 by an equal volume immersion method;
[073] The above-mentioned LaCoO3 impregnated with Cu ions is calcined in the muffle furnace at 500°C for 4-6 hours, and finally 5% CuO-LaCoO3 can be obtained.
[074] Example 6:
[075] The preparation method of mesoporous supported catalyst CuO-LaCoO3, which comprises the following steps:
[076] Template KIT-6 is prepared by solvothermal method with P123 as template agent, n-butanol as organic additive and tetraethyl silicate as silicon source.
[077] Taking 8mmol of lanthanum nitrate and cobalt nitrate into 80ml of ethanol water solution (the volume ratio of absolute ethanol to deionized water is 3:1), and weighing 8mmol of citric acid monohydrate as the chelating agent, which is added to the precursor, and stirring them at room temperature for one night;
[078] Slowly adding l6mmol of the prepared template while stirring, heating and stirring it until it is viscous;
[079] Transferring the wet gel to an oven for drying to obtain the dry gel, and roasting it in the electric furnace for 2 hours to remove citric acid to obtain a black fluffy solid;
[080] Calcining the black fluffy solid in the muffle furnace at the heating rate of 2°C/min at 700°C for 6 hours to obtain the LaCoO3 black powder containing the template;
[081] Mesoporous LaCoO3 with large specific surface area is obtained by washingSiO 2 with 2mol/L sodium hydroxide solution at 40°C for 12h;
[082] According to the ratio of nCu:nLa=1:20, dissolving copper nitrate and in 1.5ml of deionized water, preparing a certain concentration of copper nitrate solution and impregnating a certain amount of mesoporous LaCoO3 by an equal volume immersion method;
[083] The above LaCoO3 impregnated with Cu ions is calcined in a muffle furnace at 500°C for 4 ~ 6 hours, and finally 20% CuO-LaCoO3 can be obtained.
[084] The CO catalytic conversion efficiency of the catalysts obtained in Examples 3, 4, 5 and 6 is shown in Figure 3. It can be seen that the catalytic conversion efficiency of CO increases with the increase of temperature, and the order from low to high is as follows: LaCoO3<20% Cu / LaCoO3<5%Cu/LaCoO3 <10%Cu/LaCoO3. The oxidation of CO by CuO itself is not high, but it is worth noting that the catalytic efficiency of CO is improved when a layer of CuO is loaded on the surface of LaCoO3, which indicates that the loading of CuO may change the surface properties of LaCoO3, thus improving the ability of the catalyst to oxidize CO.
[085] Although the invention has been described with reference to specific examples, it will be appreciated by those skilled in the art that the invention may be embodied in many other forms, in keeping with the broad principles and the spirit of the invention described herein.
[086] The present invention and the described embodiments specifically include the best method known to the applicant of performing the invention. The present invention and the described preferred embodiments specifically include at least one feature that is industrially applicable
Claims (6)
1. The preparation method of a mesoporous supported catalyst CuO-LaCoO3, is characterized in that it comprises the following steps: immersing the mesoporous LaCoO3 in copper nitrate solution, and calcinating the mesoporous LaCoO3 impregnated with Cu ions in muffle furnace at 400-600°C for 4-6 hours, so as to obtain the final CuO-LaCoO3.
2. The preparation method of a mesoporous supported catalyst CuO-LaCoO3 according to claim 1, it is characterized in that the preparation process of mesoporous LaCoO3 is as follows:
1) Taking P123 as the template, n-butanol as the organic additive, tetraethyl silicate as the silicon source, and solvothermal method to prepare the template KIT-6;
2) Weighing the equivalent amounts of lanthanum nitrate and cobalt nitrate which are dissolved in the ethanol aqueous solution, adding citric acid monohydrate as the chelating agent, and stirring them for reaction to obtain the precursor;
3) Adding the template obtained in step 1, heating and stirring it until it is viscous;
4) Transferring the template to the oven for drying to obtain a dry gel, and roast it in the electric furnace to remove citric acid to obtain the black fluffy solid;
5) The black fluffy solid is heated and calcined in the muffle furnace to obtain the LaCoO3 black powder containing the template;
6) Washing the template-containing LaCoO3 black powder with sodium hydroxide solution, so as to obtain mesoporous LaCoO3.
3. The preparation method of a mesoporous supported catalyst CuO-LaCoO3 according to claim 2, it is characterized in that the preparation process of the template KIT-6 is as follows:
Completely dissolving P123 and n-butanol in hydrochloric acid, then adding tetraethyl silicate to continue stirring and mixing evenly; Transferring the solution to the reaction kettle for hydrothermal reaction at 100-130 °C for 24; Cooling it to room temperature, taking out the lining. Performing filtering, washing and drying respectively to obtain the white powder; Calcining the obtained powder in a muffle furnace at 550 °C for 5-7h to obtain the KIT-6 template.
4. The preparation method of a mesoporous supported catalyst CuO-LaCoO3 according to claim 1, it is characterized in that the ratio of anhydrous ethanol to deionized water in the aqueous solution of ethylene glycol in step 2) is 3: 1.
5. The preparation method of a mesoporous supported catalyst CuO-LaCoO3 according to claim 1, it is characterized in that the temperature rise rate is 2°C/min, the calcination temperature is 700 °C and the calcination time is 4-8h in step 5).
6. The preparation method of a mesoporous supported catalyst CuO-LaCoO3 according to claim 1, It is characterized in that the concentration of the sodium hydroxide solution in step 6) is 2 mol/L, and the washing and heating temperature is -80°C and the time is 6-12 hours.
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