CN110560063A - High-temperature stable supported cobaltosic oxide catalyst with core-shell structure and preparation method and application thereof - Google Patents

High-temperature stable supported cobaltosic oxide catalyst with core-shell structure and preparation method and application thereof Download PDF

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CN110560063A
CN110560063A CN201910852464.8A CN201910852464A CN110560063A CN 110560063 A CN110560063 A CN 110560063A CN 201910852464 A CN201910852464 A CN 201910852464A CN 110560063 A CN110560063 A CN 110560063A
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catalyst
shell structure
core
carrier
temperature stable
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蔡婷
袁静
刘喆
赵昆峰
金彩虹
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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Shanghai National Engineering Research Center for Nanotechnology Co Ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/74—Iron group metals
    • B01J23/75—Cobalt
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
    • F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
    • F23G7/07—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material

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  • Environmental & Geological Engineering (AREA)
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  • General Engineering & Computer Science (AREA)
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Abstract

The invention discloses a preparation method of a high-temperature stable supported cobaltosic oxide catalyst with a core-shell structure, and a product and application thereof, wherein the catalyst is Al2O3，TiO2Or SiO2Loaded Co3O4the loading amount is 1% -5%, and the catalyst is commercial Al2O3,TiO2Or SiO2as a carrier, with Co (NO)36H2O is used as a cobalt source, urea is used as a precipitator, and the supported core-shell structure Co is obtained by a precipitation and heat treatment method3O4a catalyst. The preparation method mainly comprises two parts: the first part firstly synthesizes precursor materials, and the second part carries out heat treatment on the precursors to obtain Co with different carrier loads and a core-shell structure3O4A catalyst. The process is simple, and the prepared Co with the core-shell structure3O4Having a high degree of dispersionAnd has good catalytic performance on VOCs and CVOCs.

Description

High-temperature stable supported cobaltosic oxide catalyst with core-shell structure and preparation method and application thereof
Technical Field
The invention belongs to the technical field of catalytic environmental protection, and particularly relates to a preparation method of a high-temperature stable supported cobaltosic oxide catalyst with a core-shell structure, and a product and application thereof.
Background
Co3O4is one of the transition metal oxides having the highest catalytic combustion activity for VOCs. Because the high activity performance of the catalyst is similar to that of noble metals, the catalyst has wide application prospect. But when present alone, tend to agglomerate, resulting in a substantial reduction in activity. The dispersion degree and the stability of the catalyst can be improved by loading the catalyst on a carrier, so that the catalyst is not easy to agglomerate. However, in supported cobalt-based catalysts, the active cobalt species are prone to strong interactions with the support, resulting in reduced activity. In response to this problem, various methods have been proposed to increase the activity of the supported catalyst. The method comprises the following steps of modifying a carrier, doping an active component, carrying out post-treatment (acid, alkali and the like) on a catalyst, and the like so as to improve the catalytic oxidation activity of the catalyst. However, it is difficult to substantially increase the activity of the supported cobalt-based catalyst in any of these ways.
The invention provides high-temperature stable load type core-shell structure Co3O4The preparation method of the catalyst mainly comprises the steps of improving the thermal stability of the supported cobalt-based catalyst through high-temperature roasting, and then highly dispersing active components in the supported cobalt-based catalyst on the surface of a carrier through reduction and in-situ reoxidation. By controlling oxidation, high-stability core-shell structure Co is obtained3O4A catalyst. The catalyst shows higher catalytic oxidation activity and stability to VOCs and CVOCs. The method provides reference for the preparation of the existing supported cobalt-based catalyst.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method of a supported cobaltosic oxide catalyst with a core-shell structure, which is stable at high temperature.
yet another object of the present invention is to: provides a high-temperature stable supported type core-shell structure cobaltosic oxide catalyst product prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The object of the present invention is achieved bythe scheme is realized as follows: a process for preparing the high-temp stable load-type cobaltosic oxide catalyst with core-shell structure from Al2O3、TiO2or SiO2as a carrier, with Co (NO)36H2o is used as a cobalt source, urea is used as a precipitator, and the supported core-shell structure Co is obtained by a precipitation and heat treatment method3O4The catalyst is prepared by a method of combining precipitation and heat treatment, and at least comprises two partial steps of synthesis of a precursor and heat treatment, wherein:
A first part: synthesis of a precursor:
(1) preparing 1mol/L urea aqueous solution;
(2) Weighing carrier Al2O3、TiO2Or SiO2dispersing in water to enable the mass ratio of the carrier to the water to be 1/50, and stirring for 15-30 min to obtain a suspension;
(3) With Co3O4measured as Co3O4Weighing cobalt nitrate with the mass ratio of 1-5% to the carrier, and dissolving the cobalt nitrate in the suspension of the carrier in the step (2);
(4) Transferring the suspension into an oil bath kettle at 80 ℃, dropwise adding the urea solution obtained in the step (1) until the pH is about =9, and continuously stirring for 2 hours;
(5) Taking out, and aging overnight;
(6) Performing suction filtration, washing with deionized water for 3-5 times, and then washing with ethanol for 2-3 times;
(7) drying in a 50 ℃ oven overnight to obtain a precursor;
A second part: and (3) heat treatment:
(1) roasting the obtained precursor in air at 500-800 ℃ for 4-6 h;
(2) reducing the roasted catalyst in 5-10% hydrogen-argon mixed gas at 300-800 ℃ for 3-5 h;
(3) passivating the reduced catalyst for 12 hours at room temperature in air;
(4) Taken out and then put in a reaction atmosphere (0.1 percent (V)PropaneV or VVinyl chloridev) + air) at 300-500 ℃ for 4-6 h to obtainthe high-temperature stable supported cobaltosic oxide catalyst with the core-shell structure.
The invention obtains a high-stability cobalt-based catalyst by carrying out post-treatment on the supported cobalt-based catalyst on the existing research, compared with the Co existing independently3O4it shows high catalytic oxidation activity to both VOCs and CVOCs.
The invention also provides a high-temperature stable load type core-shell structure Co3O4Catalyst, prepared according to the process described above, with Al2O3，TiO2Or SiO2Loaded Co3O4the catalyst has a loading of 1-5%.
the invention also provides a high-temperature stable load type core-shell structure Co3O4the application of the catalyst VOCs or CVOCs in the catalytic combustion process.
VOCs pollutant gas is simulated by propane standard gas, and the activity evaluation of the catalyst for catalytic combustion is carried out in a fixed bed microreactor (a quartz tube with an inner diameter of 3 mm). The catalyst amount is 100mg, and the temperature is automatically controlled by a K-type thermocouple. The methane/propane standard mixed gas is mixed with air and fed into the reactor to make combustion. The total flow is controlled by a mass flow meter, the concentration of propane is 100ppm, air is used as carrier gas, the concentration of oxygen is 10 percent, the reaction temperature is 50-550 ℃, and the reaction is carried out under the normal pressure environment.
The evaluation of the activity of the catalyst used for the catalytic combustion of vinyl chloride is carried out in a fixed bed microreactor (a quartz tube with an inner diameter of 3 mm), the dosage of the catalyst is 200mg, and the temperature is automatically controlled by a K-type thermocouple. The chloroethylene standard gas is mixed with air and enters a reactor for combustion. The total flow is controlled by a mass flow meter, the concentration of chloroethylene is 0.05 vol%, air is used as carrier gas, the concentration of oxygen is 10%, the reaction temperature is 140-500 ℃, and the reaction is carried out under the normal pressure environment. The relationship between the conversion of vinyl chloride and the reaction temperature is shown in Table 1, wherein T50%、T90%The reaction temperatures required for 50% and 90% conversion, respectively. The reaction tail gas is subjected to chromatographic on-line tracking, and the main reaction products are HCl, carbon dioxide, water and a very small amount of trichloroethylene.
Compared with the existing catalyst, the catalyst and the preparation method thereof provided by the invention have the characteristics that: (1) the thermal stability of the existing supported cobalt-based catalyst is improved; (2) a method for increasing the activity of a supported cobalt-based catalyst is provided.
Drawings
FIG. 1 is a TEM image of example 2;
FIG. 2 is a TEM image of example 4.
Detailed Description
example 1
as a comparative example, it was prepared by the following procedure
(1) Preparing 1mol/L urea aqueous solution;
(2) 3.00g of Al are weighed2O3Dispersing the carrier in 150ml of water, and stirring for 15 min;
(3) weighing 0.55g of cobalt nitrate to dissolve in the suspension of the carrier in the step (2);
(4) the suspension is transferred to 80oc, dropwise adding the urea solution obtained in the step (1) into an oil bath kettle until the pH is about =9, and continuously stirring for 2 hours;
(5) Taking out, and aging overnight; performing suction filtration, washing with deionized water for 3-5 times, and then washing with ethanol for 2-3 times; oven drying at 50 deg.C overnight;
(6) roasting the obtained precursor in the air at 800 ℃ for 4h, and recording the roasted precursor as 5 CoAl; the catalytic combustion activity of propane and that of vinyl chloride are shown in Table 1 and Table 2, respectively.
Example 2
A high-temperature stable supported type core-shell structure cobaltosic oxide catalyst, which is prepared from Al2O3As a carrier, with Co (NO)36H2o is used as a cobalt source, urea is used as a precipitator, and the supported core-shell structure Co is obtained by a precipitation and heat treatment method3O4The catalyst is prepared by a method of combining precipitation and heat treatment, and at least comprises two partial steps of synthesis of a precursor and heat treatment, wherein:
a preparation method of a high-temperature stable supported cobaltosic oxide catalyst with a core-shell structure comprises the following steps:
(1) preparing 1mol/L urea aqueous solution;
(2) 3.00g of Al are weighed2O3Dispersing the carrier in 150ml of water, and stirring for 15 min;
(3) Weighing 0.55g of cobalt nitrate to dissolve in the suspension of the carrier in the step (2);
(4) Transferring the suspension into an oil bath kettle at the temperature of 80 ℃, dropwise adding the urea solution obtained in the step (1) until the pH is about =9, and continuously stirring for 2 hours;
(5) Taking out, and aging overnight; performing suction filtration, washing with deionized water for 3-5 times, and then washing with ethanol for 2-3 times; drying in a 50 ℃ oven overnight to obtain a precursor;
(6) roasting the obtained precursor in the air at 800 ℃ for 4h;
(7) Reducing the calcined catalyst in 10% hydrogen-argon mixed gas at 500 ℃ for 5h;
(8) Passivating the reduced catalyst for 12 hours at room temperature in air;
(9) Taking out and reacting in 0.1% V atmospherePropane/Vair (a)the catalyst of the present invention was obtained by calcining at 500 ℃ for 4 hours under the conditions shown in TEM image of FIG. 1, and designated as 5 CoAl-P. The propane catalytic combustion activity is shown in Table 1.
Example 3
a high-temperature stable supported type core-shell structure cobaltosic oxide catalyst is prepared by the following steps:
(1) Preparing 1mol/L urea aqueous solution;
(2) 3.00g of Al are weighed2O3dispersing the carrier in 150ml of water, and stirring for 15 min;
(3) weighing 0.55g of cobalt nitrate to dissolve in the suspension of the carrier in the step (2);
(4) The suspension is transferred to 80oC, dropwise adding the urea solution obtained in the step (1) into an oil bath kettle until the pH is about =9, and continuously stirring for 2 hours;
(5) Taking out, and aging overnight; performing suction filtration, washing with deionized water for 3-5 times, and then washing with ethanol for 2-3 times; oven drying at 50 deg.C overnight;
(6) Roasting the obtained precursor in the air at 800 ℃ for 4h;
(7) reducing the calcined catalyst in 10% hydrogen-argon mixed gas at 500 ℃ for 5h;
(8) Passivating the reduced catalyst for 12 hours at room temperature in air;
(9) Taken out and then is at 0.1 percent Vvinyl chloride/Vair (a)Roasting at 500 deg.c for 4 hr to obtain the catalyst named 5 CoAl-VC; the catalytic combustion activity of vinyl chloride is shown in Table 2.
Example 4
A high-temperature stable supported type core-shell structure cobaltosic oxide catalyst, which is prepared from TiO2Is used as a carrier and is prepared by the following steps:
(1) Preparing 1mol/L urea aqueous solution;
(2) 3.00g of TiO were weighed2dispersing the carrier in 150ml of water, and stirring for 15 min;
(3) Weighing 0.55g of cobalt nitrate to dissolve in the suspension of the carrier in the step (2);
(4) transferring the suspension into an oil bath kettle at the temperature of 80 ℃, dropwise adding the urea solution obtained in the step (1) until the pH is about =9, and continuously stirring for 2 hours;
(5) Taking out, and aging overnight; performing suction filtration, washing with deionized water for 3-5 times, and then washing with ethanol for 2-3 times; oven drying at 50 deg.C overnight;
(6) roasting the obtained precursor in air at 500 ℃ for 4h;
(7) reducing the calcined catalyst in 5 percent hydrogen-argon mixed gas for 3 hours at the temperature of 500 ℃;
(8) Passivating the reduced catalyst for 12 hours at room temperature in air;
(9) Taken out and then is at 0.1 percent Vpropane/VAir (a)Roasting at 500 deg.c for 4 hr to obtain the catalyst, named 5 CoTi-P; the propane catalytic combustion activity is shown in Table 1.
Example 5
a high-temperature stable supported type core-shell structure cobaltosic oxide catalyst is prepared by the following steps:
(1) Preparing 1mol/L urea aqueous solution;
(2) 3.00g of TiO were weighed2Dispersing the carrier in 150ml of water, and stirring for 15 min;
(3) Weighing 0.55g of cobalt nitrate to dissolve in the suspension of the carrier in the step (2);
(4) Transferring the suspension into an oil bath kettle at the temperature of 80 ℃, dropwise adding the urea solution obtained in the step (1) until the pH is about =9, and continuously stirring for 2 hours;
(5) taking out, and aging overnight; performing suction filtration, washing with deionized water for 3-5 times, and then washing with ethanol for 2-3 times; oven drying at 50 deg.C overnight;
(6) Roasting the obtained precursor in air at 500 ℃ for 4h;
(7) Reducing the calcined catalyst in 5 percent hydrogen-argon mixed gas for 3 hours at the temperature of 300 ℃;
(8) Passivating the reduced catalyst for 12 hours at room temperature in air;
(9) Taken out and then is at 0.1 percent Vvinyl chloride/VAir (a)The catalyst was obtained by calcination at 300 ℃ for 4h under the conditions described, and the catalytic combustion activity of vinyl chloride is shown in Table 2, and is designated 5 CoTi-VC.
Example 6
A high-temperature stable load type core-shell structure cobaltosic oxide catalyst, which is prepared from SiO2Is used as a carrier and is prepared by the following steps:
(1) Preparing 1mol/L urea aqueous solution;
(2) 3.00g of SiO are weighed2Dispersing the carrier in 150ml of water, and stirring for 15 min;
(3) weighing 0.11g of cobalt nitrate to dissolve in the suspension of the carrier in the step (2);
(4) transferring the suspension into an oil bath kettle at the temperature of 80 ℃, dropwise adding the urea solution obtained in the step (1) until the pH is about =9, and continuously stirring for 2 hours;
(5) Taking out, and aging overnight; performing suction filtration, washing with deionized water for 3-5 times, and then washing with ethanol for 2-3 times; oven drying at 50 deg.C overnight;
(6) Roasting the obtained precursor in air at 500 ℃ for 4h;
(7) Reducing the calcined catalyst in 5 percent hydrogen-argon mixed gas for 3 hours at the temperature of 500 ℃;
(8) Passivating the reduced catalyst for 12 hours at room temperature in air;
(9) Taken out and then is at 0.1 percent VPropane/VAir (a)the catalyst of the present invention was obtained by calcining at 300 ℃ for 6 hours under the conditions described in Table 1, and its propane catalytic combustion activity was noted as 1 CoSi-P.
catalyst Activity test
(1) propane Activity test
The catalysts of examples 1, 2, 4 and 6 were used for propane catalytic combustion and for the activity evaluation of the catalyst used for catalytic combustion, in a fixed-bed microreactor (quartz tube 3mm in internal diameter) using propane standard gas to simulate VOCs pollutant gases. The catalyst amount is 100mg, and the temperature is automatically controlled by a K-type thermocouple. The methane/propane standard mixed gas is mixed with air and fed into the reactor to make combustion. The total flow is controlled by a mass flow meter, the concentration of propane is 100ppm, air is used as carrier gas, the concentration of oxygen is 10 percent, the reaction temperature is 50-550 ℃, and the reaction is carried out under the normal pressure environment. The results of the activity test are shown in Table 1.
(2) Vinyl chloride Activity test
The catalysts of examples 1, 3 and 5 were used for the catalytic combustion of vinyl chloride, and the evaluation of the activity of the catalyst used for the catalytic combustion of vinyl chloride was carried out in a fixed-bed microreactor (quartz tube 3mm in internal diameter), the amount of the catalyst used was 200mg, and the temperature was automatically controlled using a K-type thermocouple. The chloroethylene standard gas is mixed with air and enters a reactor for combustion. The total flow is controlled by a mass flow meter, the concentration of chloroethylene is 0.05 vol%, air is used as carrier gas, the concentration of oxygen is 10%, the reaction temperature is 140-500 ℃, and the reaction is carried out under the normal pressure environment. The relationship between the conversion of vinyl chloride and the reaction temperature is shown in Table 1, wherein T50%、T90%When the conversion rate reaches 50% and 90%, respectivelyThe required reaction temperature. The reaction tail gas is subjected to chromatographic on-line tracking, and the main reaction products are HCl, carbon dioxide, water and a very small amount of trichloroethylene. The results of the activity test are shown in table 2:
As can be seen from the results of tables 1 and 2, the alumina-supported core-shell structure cobaltosic oxide has higher catalytic oxidation activity than the alumina-supported cobaltosic oxide. Therefore, the preparation method of the supported cobalt-based catalyst with the core-shell structure can greatly improve the activity of the supported cobalt-based catalyst. Provides reference for the preparation of high activity supported cobalt-based catalysts.

Claims (3)

1. A preparation method of a high-temperature stable supported cobaltosic oxide catalyst with a core-shell structure is characterized in that Al is used2O3、TiO2or SiO2As a carrier, with Co (NO)36H2O is used as a cobalt source, urea is used as a precipitator, and the supported core-shell structure Co is obtained by a precipitation and heat treatment method3O4The catalyst is prepared by a method of combining precipitation and heat treatment, and at least comprises two partial steps of synthesis of a precursor and heat treatment, wherein:
A first part: synthesis of a precursor:
(1) preparing 1mol/L urea aqueous solution;
(2) weighing carrier Al2O3、TiO2or SiO2dispersing in water to enable the mass ratio of the carrier to the water to be 1/50, and stirring for 15-30 min to obtain a suspension;
(3) with Co3O4measured as Co3O4weighing cobalt nitrate with the mass ratio of 1-5% to the carrier, and dissolving the cobalt nitrate in the suspension of the carrier in the step (2);
(4) Transferring the suspension into an oil bath kettle at 80 ℃, dropwise adding the urea solution obtained in the step (1) until the pH is =9, and continuously stirring for 2 hours;
(5) Taking out, and aging overnight;
(6) performing suction filtration, washing with deionized water for 3-5 times, and then washing with ethanol for 2-3 times;
(7) drying in a 50 ℃ oven overnight to obtain a precursor;
A second part: and (3) heat treatment:
(1) roasting the obtained precursor in air at 500-800 ℃ for 4-6 h;
(2) Reducing the roasted catalyst in 5-10% hydrogen-argon mixed gas at 300-800 ℃ for 3-5 h;
(3) Passivating the reduced catalyst for 12 hours at room temperature in air;
(4) taken out and then put in a reaction atmosphere (0.1 percent (V)propanev or VVinyl chloridev) + air) at 300-500 ℃ for 4-6 h to obtain the high-temperature stable supported cobaltosic oxide catalyst with the core-shell structure.
2. high-temperature stable load type core-shell structure Co3O4Catalyst, characterized in that it is obtained by a process according to claim 1, made of Al2O3，TiO2Or SiO2Loaded Co3O4the catalyst has a loading of 1-5%.
3. the high-temperature stable supported core-shell structure Co according to claim 23O4the application of the catalyst VOCs or CVOCs in the catalytic combustion process.
CN201910852464.8A 2019-09-09 2019-09-09 High-temperature stable supported cobaltosic oxide catalyst with core-shell structure and preparation method and application thereof Pending CN110560063A (en)

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CN111841542A (en) * 2020-07-10 2020-10-30 中国地质大学（武汉） CoTiO with yolk-eggshell structure3@Co3O4Preparation method and application of nano composite material
CN113070071A (en) * 2021-03-25 2021-07-06 华中师范大学 Propane low-temperature catalytic combustion catalyst with high thermal stability and preparation method and application thereof
CN113171774A (en) * 2021-04-26 2021-07-27 复旦大学 Alkali metal poisoning resistant VOCs catalytic combustion catalyst and preparation method thereof
CN113457681A (en) * 2021-07-08 2021-10-01 上海纳米技术及应用国家工程研究中心有限公司 MOFs-derived Co-based catalyst for catalytic combustion of non-methane total hydrocarbons and preparation method and application thereof
CN114588932A (en) * 2022-03-16 2022-06-07 浙江师范大学 Based on Co3O4Preparation method and application of supported catalyst
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Application publication date: 20191213