CN103252242B - Non-noble metal catalyst used for catalytic combustion of PTA exhaust gas and preparation method thereof - Google Patents
Non-noble metal catalyst used for catalytic combustion of PTA exhaust gas and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a non-noble metal catalyst used for catalytic combustion of a PTA exhaust gas. The catalyst is prepared by mixing CuO, MnO2 and CeO2 oxide composite particles, uniformly dispersing, and loading on honeycomb ceramic, wherein CuO, MnO2 and CeO2 are in such weight parts that a ratio of amount of substance of copper and manganese is 1 : 1 to 1 : 7, and a ratio of a total mass of the CuO and the MnO2 and a mass of the CeO2 is 1 : 3 to 1 : 19. The catalyst uses honeycomb ceramic as base, an oxygen storage material CeO2 as a coating, and non-noble metals Cu and Mn as active components. The catalyst prepared by the invention has characteristics of low raw material cost, simple preparation technology, high catalytic activity and good toxin immunity, and can realize high-efficient catalytic combustion removal for PTA exhaust gas and other industrial exhaust gas.
Description
Technical field
The present invention relates to a kind of base metal integral catalyzer for the tail gas catalyzed burning of PTA and preparation method, belong to catalytic combustion environmental protection technical field.
Background technology
Organic exhaust gas is the common contaminant of petroleum chemical industry discharge, normal containing hydrocarbon compound, oxygen-containing organic compound, nitrogenous, sulphur, halogen and organic phosphorus compound etc. in organic exhaust gas.As do not added process to these waste gas, directly entering air and will cause severe contamination to environment, being detrimental to health.PTA oxidation reaction tail gas is the maximum pernicious gas of quantity that PTA device is discharged, containing organic total mass concentration more than 1000 mg/m
3, mass concentration about 100 mg/m of bromide
3, mass concentration about 5000 mg/m of CO
3, also have CO
2, O
2, N
2deng.
Traditional organic waste-gas purification method comprises absorption method, condensation method and direct combustion method etc., these methods easily produce secondary pollution, energy consumption large, be subject to the shortcomings such as organic exhaust gas concentration and temperature limiting.And catalytic combustion technology advantage that is high with its treatment effeciency, that do not produce secondary pollution and lower energy ezpenditure receives increasing concern, raise in subsidiary's chemical plant P3 device, what PTA vent gas treatment adopted is exactly catalytic combustion technology.
Current industrialization catalyst for catalytic combustion mainly concentrates on noble metal catalyst, and noble metal is used for the history that catalytic combustion has had decades, is that preparation or the research of reaction mechanism of catalyst all achieves more deep research.For catalytic combustion, Pd and Pt is the catalytically-active materials that investigation and application is maximum.The catalyst that current China adopts is import, and there are the companies such as Engelhard, Johnson Matthey in main supplier, all with the noble metals such as Pt, Pd be active component, ceramic honey comb for carrier, very expensive (9.9 ten thousand dollars/m of price
3left and right).The major defect of this kind of catalyst is resource scarcity, expensive, and resistance to Poisoning is poor, and people strive to find substitute always or reduce its consumption as far as possible.(the petrochemical industry such as Zhu Lianli, 2010,39 (4): 449-453) the two noble metal catalyst of a series of Pt-Pd that adopted infusion process to prepare, and add the metal promoters such as Fe, W, V, Ag modification is carried out to catalyst, investigate auxiliary agent, the PH of maceration extract, impregnation sequence to the impact of methyl acetate activity in catalyst oxidation PTA tail gas and Celfume to the intoxication of catalyst.Result shows, the oxidation reaction of auxiliary agent to methyl acetate all has facilitation; The PH of maceration extract should be less than 4, and first after dipping Pt-Pd, two noble metal catalyst activity of impregnating metal auxiliary agent are higher; Add A10 and A11 auxiliary agent in the two noble metal catalyst of Pt-Pd after, its anti-bromomethane poisoning ability obviously promotes.But this catalyst still with precious metals pd-Pt for main active component, metal promoter is trace doped, fails significantly to reduce its cost.
Because Precious Metals Resources reduces and expensive day by day, non-precious metal catalyst is as in widespread attention in the application of the oxide of Cu, Mn, Co etc. in catalytic combustion.But single metal oxide catalyst activity is often not ideal enough, need to be improved to improve its catalytic activity.O composite metallic oxide catalyst, as Cu-Mn, Cu-Co etc., such catalyst under certain conditions, can reach the catalytic effect of noble metal catalyst, be the focus of catalytic combustion area research, and many high performance composite oxide catalysts are are researched and developed.Liu Fengfen etc. (Nanjing University of Technology's journal, 2010,32 (6): 31-35) adopted coprecipitation to prepare Ce-Mn composite oxides and one pack system Ce, Mn oxide catalyst, investigates their catalytic activitys to methylene bromide burning.And characterize with the crystal phase structure of XRD, TPR means to catalyst.Result shows, Ce-Mn composite oxides are significantly better than one pack system Ce, Mn oxide catalyst to the catalytic combustion properties of methylene bromide, and methylene bromide conversion ratio is greater than 95%.But catalyst prepared by this technology is pellet type catalyst, is only applicable to laboratory scale exploratory development, and is not suitable for the exhaust-gas treatment in practical application in industry.
Summary of the invention
The object of the invention is to there is the problems such as cost is high, mithridatism is poor for the current noble metal catalyst for industrial waste gas process, a kind of base metal integral catalyzer for the tail gas catalyzed burning of PTA and preparation method are proposed, it is low that prepared catalyst has cost of material, preparation technology is simple, the advantages such as catalytic activity is high, and mithridatism is good.
The tail gas catalyzed burning non-precious metal catalyst of PTA, at least comprises CuO, MnO
2and CeO
2oxide compound particle mixes dispersed, and is carried on ceramic honey comb; CuO, MnO
2and CeO
2weight portion make copper be 1:1 ~ 1:7, CuO and MnO with the ratio of the amount of substance of manganese
2gross mass and CeO
2mass ratio is 1:3 ~ 1:19.
Employing ceramic honey comb is carrier, CuO, MnO
2and CeO
2oxide compound particle mixes and to be dispersed in water and to apply or be carried on ceramic honey comb, forms the monolith honeycomb catalysts with coating material.
CuO, MnO
2first be carried on CeO
2, obtained CuO-MnO
2/ CeO
2, then uniform load is in ceramic honey comb; CuMn/CeO
2cuO-MnO can be expressed as
2/ CeO
2.
A preparation method for the tail gas catalyzed burning non-precious metal catalyst of PTA, concrete steps are as follows:
(1) CeO
2the preparation of coating material:
Coating material CeO
2prepared by the employing precipitation method, at Ce (NO
3)
3the aqueous solution of precipitating reagent is dripped while stirring in solution, dropping to pH value is 8 ~ 10, continue stirring 0.5 ~ 3h, aging 12 ~ 48 h, then suction filtration, spends deionized water and becomes neutral to filtrate PH, then dry 8 ~ 20 h at 100 ~ 120 DEG C, at 400 ~ 700 DEG C, roasting 2 ~ 5 h, obtains coating material CeO
2;
(2) preparation of coating liquid
By the mixed solution of loading requirement preparation copper, manganese salt; By CuO and MnO
2listed as parts by weight ratio add form mixed solution, by quantitative CeO
2join in mixed solution, stir 2 ~ 10h; Then baking oven is gone in 100 ~ 120 DEG C of drying 10 ~ 20h, finally at 500 ~ 700 DEG C of roasting 2 ~ 5h, obtained CuO, MnO
2and CeO
2the catalyst of weight portion; The catalyst fines of metering is put into ball grinder, adds suitable quantity of water ball milling 2 ~ 5h and make coating liquid;
Precipitating reagent of the present invention is one or more the mixed uses in sodium carbonate, ammonium carbonate, carbonic hydroammonium, ammoniacal liquor.
(3) coating of ceramic honey comb matrix
Ceramic honey comb is immersed 20 ~ 60min in coating liquid, take out and dry up slurries residual in duct, then go to baking oven in 100 ~ 120 DEG C of drying 1 ~ 3 h, 500 ~ 700 DEG C of roasting 2 ~ 5h, weigh, and repetitive coatings process to coated weight is 140 ~ 200g/L, obtained CuMn/CeO
2/ honeycomb ceramic integral formula catalyst.
Ce (NO of the present invention
3)
3concentration is 0.25 ~ 1 mol/L, and precipitant concentration is 0.25 ~ 0.5 mol/L.
Copper of the present invention, manganese salt are the one in nitrate, sulfate, acetate.
In copper manganese mixed salt solution of the present invention, the ratio of the amount of substance of copper manganese is 1:1 ~ 1:7.
In coating liquid of the present invention, solid content is 20 ~ 40 %.
Catalyst activity evaluation is carried out in continuous-flow fixed-bed quartz reactor.With main component methyl acetate in PTA tail gas for process gas, concentration is 2 ~ 20 g/m
3; In mithridatism experiment, take bromoethane as process gas, concentration is 500 ~ 2000 mg/ m
3, unstripped gas overall flow rate is 12 ~ 120 L/h.
Beneficial effect
(1) the base metal integral catalyzer preparation technology of the present invention's proposition is simple, and raw material sources are extensive, cheap.
(2) the base metal integral catalyzer catalytic activity prepared of the present invention is high, and mithridatism good (conversion ratio of methyl acetate is greater than 99%, and the conversion ratio of bromoethane is greater than 96%), the catalytic combustion that can be widely used in the industrial waste gases such as PTA tail gas removes.
Detailed description of the invention
Embodiment 1
Measure the cerous nitrate solution of 2 L 0.25mol/L, the sodium carbonate liquor of 0.25mol/L is dripped while stirring in solution, dropping to pH value is 8, continue to stir 0.5h, aging 12h, then suction filtration, spend deionized water and become neutral to filtrate PH, then dry 8h at 100 DEG C, roasting 5h at 500 DEG C, obtained coating CeO
2.Measure the copper nitrate solution of 30mL 0.5mol/L, the manganese nitrate solution of 150mL0.5mol/L and 420mL deionized water, make mixed solution.By 96.615gCeO
2join in maceration extract, stir dipping 2 h.Then go to baking oven in 100 DEG C of dry 10h, finally at 500 DEG C of roasting 5 h, obtained load capacity is the CuMn/CeO of 5%
2catalyst.Take 100g catalyst fines and put into ball grinder, add 400g water for ball milling 2 h and make coating liquid, in coating liquid, solid content is 20%.Described solution is the aqueous solution, also can be suspension.
If adopt manganese nitrate 180mL ~ 210 mL, concentration is that 0.5mol/L also can.
By ceramic honey comb (150 × 150 × 150 mm, hole density 400 holes/inch
2) immerse 20 min in coating liquid, take out and dry up slurries residual in duct, then go to baking oven in 100 DEG C of dry 1h, at 500 DEG C of roasting 5h, weigh, repetitive coatings process to coated weight is 140g/L, obtained 5%CuMn/CeO
2/ honeycomb ceramic integral formula catalyst.
Catalyst activity evaluation is carried out in continuous-flow fixed-bed quartz reactor.The quartzy cotton parcel of integral catalyzer is placed in the middle part of reactor, and in unstripped gas, methyl acetate concentration is about 2 g/m
3, feed gas flow rates is 12 L/h.Reaction temperature is 420 DEG C time, and the conversion ratio of methyl acetate is 99.34%.
Embodiment 2
Measure the cerous nitrate solution of 1 L0.5mol/L, the sal volatile of 0.5mol/L is dripped while stirring in solution, dropping to pH value is 10, continue to stir 3h, aging 48h, then suction filtration, spend deionized water and become neutral to filtrate PH, then dry 20h at 120 DEG C, roasting 2h at 700 DEG C, obtained coating CeO
2.Measure the copper-bath of 500mL 0.5mol/L, the manganese sulfate solution of 500mL0.5mol/L and 1L deionized water, make mixed solution.By 89.25gCeO
2join in maceration extract, stir dipping 12h.Then go to baking oven in 120 DEG C of dry 20h, finally at 700 DEG C of roasting 2 h, obtained load capacity is the CuMn/CeO of 25%
2catalyst.Take 200g catalyst fines and put into ball grinder, add 300g water for ball milling 2 h and make coating liquid, in coating liquid, solid content is 40%.
By ceramic honey comb (150 × 150 × 150 mm, hole density 400 holes/inch
2) immerse 60 min in coating liquid, take out and dry up slurries residual in duct, then go to baking oven in 120 DEG C of dry 3h, at 700 DEG C of roasting 2h, weigh, repetitive coatings process to coated weight is 200g/L, obtained 25%CuMn/CeO
2/ honeycomb ceramic integral formula catalyst.
Catalyst activity evaluation is carried out in continuous-flow fixed-bed quartz reactor, and the quartzy cotton parcel of integral catalyzer is placed in the middle part of reactor, and in unstripped gas, methyl acetate concentration is about 20 g/m
3, feed gas flow rates is 120 L/h.Reaction temperature is 420 DEG C time, and the conversion ratio of methyl acetate is 99.09%.
Embodiment 3
Measure the cerous nitrate solution of 1L0.5mol/L, the ammonium bicarbonate soln of 0.5mol/L is dripped while stirring in solution, dropping to pH value is 9, continue to stir 2h, aging 24h, then suction filtration, spend deionized water and become neutral to filtrate PH, then dry 12h at 110 DEG C, roasting 3h at 600 DEG C, obtained coating CeO
2.Measure the Schweinfurt green solution of 100mL 0.5mol/L, the manganese acetate solution of 700mL0.5mol/L and 1.2L deionized water, make mixed solution.By 127.217gCeO
2join in maceration extract, stir dipping 10h.Then go to baking oven in 110 DEG C of dry 12h, finally at 600 DEG C of roasting 3 h, obtained load capacity is the CuMn/CeO of 15%
2catalyst.Take 150g catalyst fines and put into ball grinder, add 350g water for ball milling 2 h and make coating liquid, in coating liquid, solid content is 30%.The manganese acetate solution of the 0.5mol/L of 300 ~ 600mL also can.
By ceramic honey comb (150 × 150 × 150 mm, hole density 400 holes/inch
2) immerse 30 min in coating liquid, take out and dry up slurries residual in duct, then go to baking oven in 110 DEG C of dry 2h, at 600 DEG C of roasting 3h, weigh, repetitive coatings process to coated weight is 180g/L, obtained 15%CuMn/CeO
2/ honeycomb ceramic integral formula catalyst.
Catalyst activity evaluation is carried out in continuous-flow fixed-bed quartz reactor, and the quartzy cotton parcel of integral catalyzer is placed in the middle part of reactor, and in unstripped gas, methyl acetate concentration is about 10 g/m
3, feed gas flow rates is 60 L/h.Reaction temperature is 420 DEG C time, and the conversion ratio of methyl acetate is 99.21%.
Embodiment 4
Measure the cerous nitrate solution of 2L0.25mol/L, the sal volatile of 0.5mol/L is dripped while stirring in solution, dropping to pH value is 10, continue to stir 1h, aging 24h, then suction filtration, spend deionized water and become neutral to filtrate PH, then dry 12h at 110 DEG C, roasting 3h at 600 DEG C, obtained coating CeO
2.Measure the copper nitrate solution of 100mL 0.5mol/L, the manganese nitrate solution of 500mL0.5mol/L and 1.4L deionized water, make mixed solution.By 152.55gCeO
2join in maceration extract, stir dipping 10h.Then go to baking oven in 110 DEG C of dry 12h, finally at 600 DEG C of roasting 3 h, obtained load capacity is the CuMn/CeO of 10%
2catalyst.Take 150g catalyst fines and put into ball grinder, add 450g water for ball milling 2 h and make coating liquid, in coating liquid, solid content is 25%.
By ceramic honey comb (150 × 150 × 150 mm, hole density 400 holes/inch
2) immerse 30 min in coating liquid, take out and dry up slurries residual in duct, then go to baking oven in 110 DEG C of dry 2h, at 600 DEG C of roasting 3h, weigh, repetitive coatings process to coated weight is 180g/L, obtained 10%CuMn/CeO
2/ honeycomb ceramic integral formula catalyst.
Catalyst activity evaluation is carried out in continuous-flow fixed-bed quartz reactor, and the quartzy cotton parcel of integral catalyzer is placed in the middle part of reactor, and in unstripped gas, bromoethane concentration is about 500mg/m
3, feed gas flow rates is 60 L/h.Reaction temperature is 420 DEG C time, and the conversion ratio of bromoethane is 97.20%.
Embodiment 5
Measure the cerous nitrate solution of 2L0.25mol/L, the ammonia spirit of 0.5mol/L is dripped while stirring in solution, dropping to pH value is 10, continue to stir 1h, aging 24h, then suction filtration, spend deionized water and become neutral to filtrate PH, then dry 12h at 110 DEG C, roasting 3h at 600 DEG C, obtained coating CeO
2.Measure the copper nitrate solution of 100mL 0.5mol/L, the manganese nitrate solution of 500mL0.5mol/L and 1.4L deionized water, make mixed solution.By 152.55gCeO
2join in maceration extract, stir dipping 10h.Then go to baking oven in 110 DEG C of dry 12h, finally at 600 DEG C of roasting 3 h, obtained load capacity is the CuMn/CeO of 10%
2catalyst.Take 150g catalyst fines and put into ball grinder, add 450g water for ball milling 2 h and make coating liquid, in coating liquid, solid content is 25%.
By ceramic honey comb (150 × 150 × 150 mm, hole density 400 holes/inch
2) immerse 30 min in coating liquid, take out and dry up slurries residual in duct, then go to baking oven in 110 DEG C of dry 2h, at 600 DEG C of roasting 3h, weigh, repetitive coatings process to coated weight is 180g/L, obtained 10%CuMn/CeO
2/ honeycomb ceramic integral formula catalyst.
Catalyst activity evaluation is carried out in continuous-flow fixed-bed quartz reactor, and the quartzy cotton parcel of integral catalyzer is placed in the middle part of reactor, and in unstripped gas, bromoethane concentration is about 2000 mg/m
3, feed gas flow rates is 120 L/h.Reaction temperature is 420 DEG C time, and the conversion ratio of bromoethane is 96.46%.
Claims (1)
1. a preparation method for the tail gas catalyzed burning non-precious metal catalyst of PTA, is characterized in that at least comprising CuO, MnO
2and CeO
2oxide compound particle mixes dispersed, and is carried on ceramic honey comb; CuO, MnO
2and CeO
2weight portion make copper be 1:1 ~ 1:7, CuO and MnO with the ratio of the amount of substance of manganese
2gross mass and CeO
2mass ratio is 1:3 ~ 1:19; , CuO, MnO
2and CeO
2oxide compound particle mixes and to be dispersed in water and to apply or be carried on ceramic honey comb, forms the integral catalyzer with coating material; CuO, MnO
2first be carried on CeO
2, obtained CuO-MnO
2/ CeO
2, then uniform load is in ceramic honey comb; CuMn/CeO
2be expressed as CuO-MnO
2/ CeO
2;
Concrete steps are as follows:
(1) CeO
2the preparation of coating material:
Coating material CeO
2prepared by the employing precipitation method, at Ce (NO
3)
3the aqueous solution of precipitating reagent is dripped while stirring in solution, dropping to pH value is 8 ~ 10, continue stirring 0.5 ~ 3h, aging 12 ~ 48 h, then suction filtration, spends deionized water and becomes neutral to filtrate pH, then dry 8 ~ 20 h at 100 ~ 120 DEG C, at 400 ~ 700 DEG C, roasting 2 ~ 5 h, obtains coating material CeO
2; Cerous nitrate concentration is 0.25 ~ 0.5 mol/L;
(2) preparation of coating liquid
By the mixed solution of loading requirement preparation copper, manganese salt; By CuO and MnO
2listed as parts by weight ratio add form mixed solution, by quantitative CeO
2join in mixed solution, stir 2 ~ 10h; Then baking oven is gone in 100 ~ 120 DEG C of drying 10 ~ 20h, finally at 500 ~ 700 DEG C of roasting 2 ~ 5h, obtained CuO, MnO
2and CeO
2the catalyst of weight portion; The catalyst fines of metering is put into ball grinder, adds suitable quantity of water ball milling 2 ~ 5h and make coating liquid; In described coating liquid, solid content is 20 ~ 40 %;
(3) coating of ceramic honey comb matrix
Ceramic honey comb is immersed 20 ~ 60min in coating liquid, take out and dry up coating liquid residual in duct, then go to baking oven in 100 ~ 120 DEG C of drying 1 ~ 3 h, 500 ~ 700 DEG C of roasting 2 ~ 5h, weigh, and repetitive coatings process to coated weight is 140 ~ 200g/L, obtained CuMn/CeO
2/ honeycomb ceramic integral formula catalyst;
Precipitating reagent is one or more the mixed uses in sodium carbonate, ammonium carbonate, carbonic hydroammonium, ammoniacal liquor; Precipitant concentration is 0.25 ~ 0.5 mol/L.
2. preparation method according to claim 1, is characterized in that, described copper, manganese salt are the one in nitrate, sulfate, acetate.
3. preparation method according to claim 1, is characterized in that: in described copper manganese mixed salt solution, the ratio of the amount of substance of copper manganese is 1:1 ~ 1:7.
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| CN105618043B (en) * | 2015-12-28 | 2020-04-10 | 成都信息工程大学 | Catalyst, preparation method and application |
| CN111054374A (en) * | 2018-10-16 | 2020-04-24 | 中国石油化工股份有限公司 | Catalytic combustion catalyst for PTA oxidized tail gas and application thereof |
| CN111375423B (en) * | 2018-12-31 | 2023-09-01 | 中国石油化工股份有限公司 | High-temperature catalytic combustion catalyst and preparation method thereof |
| CN112547084A (en) * | 2019-09-26 | 2021-03-26 | 中国石油化工股份有限公司 | Supported catalyst and preparation method and application thereof |
| CN110833833A (en) * | 2019-11-14 | 2020-02-25 | 西安凯立新材料股份有限公司 | Non-noble metal composite oxide honeycomb catalyst for catalytic combustion of low-carbon hydrocarbons |
| CN114570435A (en) * | 2020-11-30 | 2022-06-03 | 中大汇智源创(北京)科技有限公司 | Honeycomb catalyst and preparation method and application thereof |
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| US10792647B2 (en) * | 2009-04-21 | 2020-10-06 | Johnson Matthey Public Limited Company | Base metal catalysts for the oxidation of carbon monoxide and volatile organic compounds |
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