CN105251476A - Preparation method of CeO2-Cr2O3-Nb2O5 compound oxide catalyst - Google Patents

Preparation method of CeO2-Cr2O3-Nb2O5 compound oxide catalyst Download PDF

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CN105251476A
CN105251476A CN201510651148.6A CN201510651148A CN105251476A CN 105251476 A CN105251476 A CN 105251476A CN 201510651148 A CN201510651148 A CN 201510651148A CN 105251476 A CN105251476 A CN 105251476A
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composite oxide
oxide catalysts
nitrate
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CN105251476B (en
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周仁贤
杨鹏
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The invention provides a preparation method of a CeO2-Cr2O3-Nb2O5 compound oxide catalyst. Chromium nitrate, cerous nitrate and acidic Nb2O5 oxide or niobium oxalate ammonia serve as raw materials, the CeO2-Cr2O3-Nb2O5 compound oxide catalyst is prepared through a precipitation-deposition or co-precipitation method, the molecular ratio of Ce to Cr in the catalyst is 4:1, and the mass ratio of (Cr2O3 + CeO2) to Nb2O5 is 4:1-1:9. The catalyst is simple in preparation technology and low in cost and has good catalytic degradation activity and stability on dichloromethane (DCM), ethylene dichloride (DCE), trichloroethylene (TCE), chlorobenzene and other chlorine-containing organic compounds, CO2 and HCl are high in selectivity, and no polychlorocarbon or other by-products are generated.

Description

A kind of CeO 2-Cr 2o 3-Nb 2o 5the preparation method of composite oxide catalysts
Technical field
The present invention relates to a kind of preparation method of high performance chloride organic exhaust gas combustion catalyst, particularly relate to CeO 2-Cr 2o 3-Nb 2o 5the preparation method of composite oxide catalysts.
Background technology
Chloride volatile organic matter (CVOCs) is that a class has the compound of high risks to environment and human health, common are carrene (DCM), chloroform (CF), dichloroethanes (DCE), trichloro-ethylene (TCE), carbon tetrachloride (CT), chlorobenzene (PhCl) etc., because they have good chemical stability, be widely used usually used as the semi-finished product in organic solvent and chemical process.Catalytic combustion technology is the important of CVOCs pollutant purification process and very one of effective means, therefore, develops efficient, stable chloride organic exhaust gas combustion catalyst and has great importance for the extensive use of catalytic combustion technology.Although the catalyzing oxidizing degrading of noble metal catalyst to all kinds of VOCs has higher catalytic activity, chlorinated hydrocarbon or the VOCs catalytic removal containing chlorohydrocarbon are reacted, in course of reaction, be vulnerable to chlorinated compound decompose the Cl produced 2with HCl poisoning effect; Oxychlorination compound is easily generated and inactivation in high-temperature region; On the other hand, noble metal catalyst to Deacon reaction and chlorination activity also very high, easily produce many chloro organic cpds in catalytic degradation process, the process especially for chlorinated aromatic hydrocarbons often produces the larger many chlorine aromatic hydrocarbons of toxicity and dioxin compounds.In general, the catalytic activity of non-noble metal oxide (VB, II B) is lower than noble metal, but at anti-hetero atom as slightly strong in Cl, Br, S poisoning capability.But, CeO 2and composite oxides have good oxygen ability of storing and Lattice Oxygen mobility, good oxidation susceptibility is shown in the reaction of catalytic removal CVOCs, its catalytic activity and selective even higher than noble metal catalyst, therefore, causes the extensive concern of people.
Summary of the invention
The object of this invention is to provide a kind of high performance chloride organic exhaust gas combustion catalyst, specifically refer to CeO 2-Cr 2o 3-Nb 2o 5the preparation method of composite oxide catalysts.
The present invention is achieved through the following technical solutions:
A kind of CeO 2-Cr 2o 3-Nb 2o 5the preparation method of composite oxide catalysts, with chromic nitrate, cerous nitrate, Nb 2o 3oxide or niobium oxalate ammonia are primary raw material, adopt precipitation-deposition or coprecipitation to prepare CeO 2-Cr 2o 3-Nb 2o 5composite oxide catalysts, in catalyst, the mol ratio of Ce/Cr is 4:1, (Cr 2o 3+ CeO 2)/Nb 2o 5mass ratio be 4:1 ~ 1:9, concrete preparation process is as follows:
By described CeO 2+ Cr 2o 3/ Nb 2o 5mass ratio, setting concentration cerous nitrate [Ce (NO 3) 36H 2o] and chromic nitrate [Cr (NO 3) 39H 2o] add the predecessor of the Nb of set amount in mixed solution, drip (the NH of setting concentration after stirring under vigorous stirring 4) 2cO 3precipitating reagent, drop to solution ph and reach 9.0 rear room temperatures placement ageing 12 hours, then filtration, deionized water and ethanol washing are repeatedly neutral to filtrate, drying 2 hours at 110 DEG C, and at 500 DEG C, roasting processes for 2 hours, obtains CeO 2-Cr 2o 3-Nb 2o 5composite oxide catalysts.
As improving further, (Cr of the present invention 2o 3+ CeO 2)/Nb 2o 5optimum quality ratio be 3:4 ~ 1:4.
As improving further, cerous nitrate of the present invention [Ce (NO 3) 36H 2o] and chromic nitrate [Cr (NO 3) 39H 2o] predecessor that adds Nb in mixed solution is Nb 2o 5powder or niobium oxalate ammonia [(NH 4) 3nbO (C 2o 4) 34H 2o].
As improving further, cerous nitrate of the present invention [Ce (NO 3) 36H 2o] and chromic nitrate [Cr (NO 3) 39H 2o] concentration (C of mixed solution ce+Cr), or cerous nitrate [Ce (NO 3) 36H 2o], chromic nitrate [Cr (NO 3) 39H 2o] and niobium oxalate ammonia [(NH 4) 3nbO (C 2o 4) 34H 2o] concentration (C of mixed solution ce+Cr+Nb) be 0.25mol/L.
As improving further, (NH of the present invention 4) 2cO 3the concentration of precipitating reagent is 0.5mol/L.
The beneficial effect that the present invention has is as follows:
Adopt cheap cerous nitrate, chromic nitrate and niobium oxalate ammonia or niobium oxide to be raw material, adopt precipitation-deposition or coprecipitation to obtain CeO 2-Cr 2o 3-Nb 2o 5composite oxide catalysts, preparation technology is simple, and catalyst cost is low, has good catalytic degradation activity and stability, is a kind of high performance chloride organic exhaust gas combustion catalyst, has great importance to the extensive use of catalytic combustion technology.
Detailed description of the invention
Below by specific embodiment, technical scheme of the present invention is further described:
Embodiment 1
By 3.6gCr (NO 3) 39H 2o and 15.6gCe (NO 3) 36H 2o is dissolved in 180mL water, adds 13.8gNb after stirring 2o 5powder.Drip (NH under vigorous stirring 4) 2cO 3precipitating reagent, drop to solution ph and reach 9.0 rear room temperatures placement ageing 12 hours, then filtration, deionized water and ethanol washing are repeatedly neutral to filtrate, drying 2 hours at 110 DEG C, and at 500 DEG C, roasting processes for 2 hours, obtains CeO 2-Cr 2o 3-Nb 2o 5composite oxide catalysts.In this catalyst, the mol ratio of Ce/Cr is 4:1, (Cr 2o 3+ CeO 2)/Nb 2o 5mass ratio 1:2.
Embodiment 2
With the operation that embodiment 1 is identical, difference is: by 1.1gCr (NO 3) 39H 2o, 4.7gCe (NO 3) 36H 2o and 15.6g niobium oxalate ammonia is dissolved in 180mL water jointly, drips (NH under vigorous stirring after stirring 4) 2cO 3precipitating reagent.In this catalyst, the mol ratio of Ce/Cr is 4:1, (Cr 2o 3+ CeO 2)/Nb 2o 5mass ratio 1:2.
Embodiment 3
With the operation that embodiment 1 is identical, difference is: by 0.6gCr (NO 3) 39H 2o, 2.8gCe (NO 3) 36H 2o and 18.4g niobium oxalate ammonia is dissolved in 180mL water jointly, drips (NH under vigorous stirring after stirring 4) 2cO 3precipitating reagent.In this catalyst, the mol ratio of Ce/Cr is 4:1, (Cr 2o 3+ CeO 2)/Nb 2o 5mass ratio 1:4.
Embodiment 4
With the operation that embodiment 1 is identical, difference is: by 3.6gCr (NO 3) 39H 2o and 15.6gCe (NO 3) 36H 2o is dissolved in 180mL water, drips (NH under vigorous stirring after stirring 4) 2cO 3precipitating reagent.In this catalyst, the mol ratio of Ce/Cr is 4:1, not containing Nb 2o 5.
Embodiment 5
With the operation that embodiment 1 is identical, difference is: by 2.3gCr (NO 3) 39H 2o, 9.9gCe (NO 3) 36H 2o and 8.2g niobium oxalate ammonia is dissolved in 180mL water jointly, drips (NH under vigorous stirring after stirring 4) 2cO 3precipitating reagent.In this catalyst, the mol ratio of Ce/Cr is 4:1, (Cr 2o 3+ CeO 2)/Nb 2o 5mass ratio 2:1.
In 1 ~ 4 example, the catalytic degradation activity of catalyst to chlorinated organics is as shown in the table:
Note: 0.3mL, particle diameter are 40-60 object catalyst, and air speed is 15000h -1.
What more than enumerate is only some embodiments of the present invention; obviously, the invention is not restricted to above embodiment, many distortion can also be had; all distortion that those of ordinary skill in the art can directly derive from content disclosed by the invention or associate, all should think protection scope of the present invention.

Claims (5)

1. a CeO 2-Cr 2o 3-Nb 2o 5the preparation method of composite oxide catalysts, is characterized in that, with chromic nitrate, cerous nitrate, Nb 2o 3oxide or niobium oxalate ammonia are primary raw material, adopt precipitation-deposition or coprecipitation to prepare CeO 2-Cr 2o 3-Nb 2o 5composite oxide catalysts, in catalyst, the mol ratio of Ce/Cr is 4:1, (Cr 2o 3+ CeO 2)/Nb 2o 5mass ratio be 4:1 ~ 1:9, concrete preparation process is as follows:
By described CeO 2+ Cr 2o 3/ Nb 2o 5mass ratio, setting concentration cerous nitrate [Ce (NO 3) 36H 2o] and chromic nitrate [Cr (NO 3) 39H 2o] add the predecessor of the Nb of set amount in mixed solution, drip (the NH of setting concentration after stirring under vigorous stirring 4) 2cO 3precipitating reagent, drop to solution ph and reach 9.0 rear room temperatures placement ageing 12 hours, then filtration, deionized water and ethanol washing are repeatedly neutral to filtrate, drying 2 hours at 110 DEG C, and at 500 DEG C, roasting processes for 2 hours, obtains CeO 2-Cr 2o 3-Nb 2o 5composite oxide catalysts.
2. CeO according to claim 1 2-Cr 2o 3-Nb 2o 5the preparation method of composite oxide catalysts, is characterized in that, described (Cr 2o 3+ CeO 2)/Nb 2o 5optimum quality ratio be 3:4 ~ 1:4.
3. CeO according to claim 1 and 2 2-Cr 2o 3-Nb 2o 5the preparation method of composite oxide catalysts, is characterized in that, described cerous nitrate [Ce (NO 3) 36H 2o] and chromic nitrate [Cr (NO 3) 39H 2o] predecessor that adds Nb in mixed solution is Nb 2o 5powder or niobium oxalate ammonia [(NH 4) 3nbO (C 2o 4) 34H 2o].
4. CeO according to claim 1 and 2 2-Cr 2o 3-Nb 2o 5the preparation method of composite oxide catalysts, is characterized in that, described cerous nitrate [Ce (NO 3) 36H 2o] and chromic nitrate [Cr (NO 3) 39H 2o] concentration (C of mixed solution ce+Cr), or cerous nitrate [Ce (NO 3) 36H 2o], chromic nitrate [Cr (NO 3) 39H 2o] and niobium oxalate ammonia [(NH 4) 3nbO (C 2o 4) 34H 2o] concentration (C of mixed solution ce+Cr+Nb) be 0.25mol/L.
5. CeO according to claim 1 and 2 2-Cr 2o 3-Nb 2o 5the preparation method of composite oxide catalysts, is characterized in that, described (NH 4) 2cO 3the concentration of precipitating reagent is 0.5mol/L.
CN201510651148.6A 2015-10-10 2015-10-10 A kind of CeO2‑Cr2O3‑Nb2O5The preparation method of composite oxide catalysts Expired - Fee Related CN105251476B (en)

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CN112371106A (en) * 2020-11-30 2021-02-19 绍兴文理学院 Synthesis method and application of Ce-Nb-O composite metal oxide catalyst
CN112958071A (en) * 2021-03-08 2021-06-15 上海睿筑环境科技有限公司 High-stability catalyst for low-temperature catalytic combustion of chlorine-containing volatile organic compounds and preparation method thereof
CN113244938A (en) * 2021-05-21 2021-08-13 华东理工大学 P-Nb/Co for low-temperature vinyl chloride catalytic combustion3O4Catalyst, preparation method and application thereof

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