CN104511289A - Preparation methods and application of alpha-manganese oxide loaded cobalt strontium catalyst - Google Patents
Preparation methods and application of alpha-manganese oxide loaded cobalt strontium catalyst Download PDFInfo
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- CN104511289A CN104511289A CN201410713793.1A CN201410713793A CN104511289A CN 104511289 A CN104511289 A CN 104511289A CN 201410713793 A CN201410713793 A CN 201410713793A CN 104511289 A CN104511289 A CN 104511289A
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Abstract
The invention discloses a preparation method and application of an alpha-manganese oxide loaded cobalt strontium catalyst. The catalyst is prepared as follows: under the regulation of an acetic acid buffer solution, an alpha-manganese oxide loaded cobalt strontium catalyst sample Co / SR-alpha-MnO2 with high specific surface area (100-130 m<2> / g) and high thermal stability (> 650 DEG C) can be prepared by reflux reaction of manganese sulfate, potassium permanganate, cobalt nitrate, strontium sulfate and a dispersion agent. The catalyst has high elimination efficiency to high space velocity (60,000 h<-1>-100,000 <-1>) and low concentration benzene and toluene. The catalyst can completely transform the benzene into non-poisonous materials CO2 and H2O at 230 DEG C, the benzene elimination rate can be kept greater than 90% at 230 DEG C within 100 hours, the toluene can be completely transformed into the non-poisonous materials CO2 and H2O at 200 DEG C, and the toluene elimination rate can be kept greater than 90% at 200 DEG C within 100 hours. The catalyst has the advantage of cheap raw materials, simple catalyst preparation technology, strong practicability, low benzene series complete elimination temperature, high efficiency, no secondary pollution and the like.
Description
Technical field
The present invention relates to a kind of manganese oxide for catalytic combustion elimination benzene homologues (α-MnO
2) Supported Co strontium Co/Sr-α-MnO
2the preparation of catalyst, and for efficient cryogenic catalytic combustion elimination benzene homologues.
Background technology
Benzene homologues is one of main component of VOCs.It generally includes eight kinds of compounds such as benzene, toluene, ethylbenzene, ortho-xylene, and wherein benzene homologues is classified as priority pollutants by the air toxic list that Environmental Protection Agency (USEPA) formulates.Benzene homologues in air can enter human body by respiratory tract, alimentary canal and skin, causes human body to present all discomforts, thus induces an illness and then carcinogenic, and it causes larger impact to environmental and human health impacts.The treatment technology of benzene homologues mainly burns, the mode of burning disposal has directly burning and catalytic combustion two kinds, the product that direct burning generates easily causes secondary pollution, and catalytic combustion makes benzene homologues under lower initiation temperature, carry out flameless combustion by catalyst to be decomposed into carbon dioxide and steam.Due to the species that Benzene and Toluene is for the most difficult catalytic combustion elimination in benzene homologues, so the present invention represents benzene homologues with Benzene and Toluene, with this type of benzene homologues of prepared catalyst catalytic combustion process.The domestic and international research of the catalytic combustion elimination to benzene homologues is less at present, and the reaction temperature of complete catalytic removal benzene homologues is higher.Such as: " The effect of mass transfer on the catalytic combustion of benzene and methane overpalladium catalysts supported on porous materials " (Catal.Today that the research of Gon SeoO seminar of Korea S is delivered, 83 (2003) 131 – 139) in paper, be 60,000h in air speed
-1, when the concentration of benzene is 10,000ppm, (air speed is lower than of the present invention 100,000h
-1, benzene concentration is higher than 1000ppm of the present invention), use FAU zeolite, MCM-41 and KIT-1 Pt-supported catalyst carry out catalyst combustion reaction to benzene, and the temperature of its complete catalytic combustion elimination benzene is mostly more than 300 DEG C.
Manganese oxide (the MnO that this project system is standby
2) carrier, belong to α-MnO
2, because there being loose structure, there is the manganese ion of mixed valence, the Acidity of Aikalinity on surface is gentle and have excellent ion-exchange performance, becomes another new study hotspot after zeolite type tetrahedron molecular sieve.Its crystal structure is by the octahedron [MnO of common seamed edge
6] chain formation, again by octahedra [MnO between chain and chain
6] summit oxygen atom with common corner angle be connected, form one-dimentional structure.As a kind of novel functional material, have been reported support type α-MnO
2in Catalytic Thermal Decomposition aminodiphenylamine and liquid phase oxidation alcohols etc., all there is ideal catalytic activity, thus there is prospects for commercial application extensively.
This project implementation obtains: project of national nature science fund project (numbering: 21277008; 20777005); Education Commission of Beijing development in science and technology plan general project (KM2013100050010); Beijing institution of higher education directly under the jurisdiction of a municipal government Construction of Creativity Team promotes the subsidy of planning item (KM2013100050010), is also the research contents of these projects.
Summary of the invention
The object of this invention is to provide the cheap manganese sulfate of a kind of use is raw material, uses cushioning liquid and dispersant control method to prepare the alpha-oxidation manganese (α-MnO of high-ratio surface sum high thermal stability
2) Supported Co strontium CATALYST Co/Sr-α-MnO
2, and use it for low-temperature catalytic burning elimination benzene homologues.
The invention provides a kind of preparation method for catalytic combustion elimination benzene homologues catalyst.
(1) preparation method of above-mentioned catalyst provided by the present invention, comprises the steps:
KAc solution and HAc solution are mixed into cushioning liquid in KAc/HAc mol ratio=0.1 ~ 10.0 ratio, regulate pH between 3.74 ~ 5.74, subsequently by the SrSO of 0.01g ~ 0.05g
4with 0.29g ~ 3.24g Co (NO
3)
26H
2o is dissolved in above 40ml hac buffer.By the PVAC polyvinylalcohol (molecular formula (C of 0.0g ~ 2.0g
2h
4o)
n, molecular weight 20000) and to be dissolved in 20ml ~ 60ml concentration be 1.0mol/L ~ 2.0mol/L MnSO
4in solution, the cushioning liquid above containing slaine is joined in this solution, mixes.Be 0.1mol/L ~ 0.4mol/L KMnO by 120ml ~ 170ml concentration subsequently
4solution instills in above-mentioned mixed solution, wherein KMnO
4/ MnSO
4(mol ratio)=0.5 ~ 1.0, stir 2 ~ 4 hours, sealing ageing 12 hours, 80 ~ 120 DEG C of backflows 20 ~ 26 hours, revolve steaming 3 ~ 4 hours until powdered, with deionized water rinsing to neutral, 100 DEG C ~ 140 DEG C dryings 10 ~ 12 hours, then grind into powder, obtains black presoma.Get above-mentioned presoma to mix than for 8g:200ml ratio with straight alcohol.This mixture is stirred 24 hours, revolves steaming and solution was evaporated in 3 ~ 4 hours.The product obtained in pure oxygen atmosphere with the speed of 1 DEG C/min, be raised to the roasting 1 ~ 4 hour of 300 DEG C ~ 500 DEG C degree, finally obtain Co/Sr-α-MnO
2product.
(2) the present invention also provides a kind of described catalyst to eliminate the application in benzene homologues at low-temperature catalytic burning.
The catalytic combustion elimination reaction of benzene (or toluene) is carried out in fixed bed quartz tube reactor.Crystal reaction tube, external diameter is 10mm, catalyst filling amount 100mg.Pass into the gaseous mixture of benzene homologues and air, wherein Benzene series Concentrations is 500ppm ~ 1000ppm, and air-flow air speed is 60,000h
-1~ 100,000h
-1.Gas-chromatography TCD detection reaction tail gas CO
2with CO, FID detect the content of benzene and other organic species.Effect of the present invention is: under the concentration and air speed of above benzene homologues, and prepared catalyst of the present invention has higher low-temperature catalytic burning elimination activity, 200 DEG C ~ 310 DEG C time, completely Benzene and Toluene can be changed into non-poisonous material CO
2and H
2o, at this temperature, keeps Benzene and Toluene elimination factor >90% in 100 hours.Kaolinite Preparation of Catalyst uses raw material sulphuric acid manganese low price, and catalyst preparation process is simple, other metal of not load or noble metal.The present invention does not need additional any fuel, directly utilizes O in air
2for oxidant, have that raw material are economical and practical, use procedure energy consumption is low, easy and simple to handle, reaction condition is gentle, secondary pollution and can the advantage such as continuous operation can be reduced.
Accompanying drawing explanation
Co/Sr-α-MnO prepared by Fig. 1 embodiment 1,2,3 and 4
2xRD figure
Fig. 2 is Co/Sr-α-MnO prepared by the embodiment of the present invention 1,2,3 and 4
2benzene catalytic combustion activity figure
Fig. 3 is Co/Sr-α-MnO prepared by the embodiment of the present invention 1,2,3 and 4
2toluene catalytic combustion activity figure
Fig. 4 is Co/Sr-α-MnO prepared by the embodiment of the present invention 4
2-IV catalyst is to benzene catalytic combustion stability
Fig. 5 is Co/Sr-α-MnO prepared by the embodiment of the present invention 4
2-IV catalyst toluene catalytic combustion stability
Detailed description of the invention
Embodiment 1
(1) preparation method of above-mentioned catalyst provided by the present invention, comprises the steps:
Be that KAc and the 0.1mol/L HAc of 0.1mol/L is mixed into cushioning liquid in KAc/HAc mol ratio=0.1 ratio by concentration, regulate pH=3.74, subsequently by the SrSO of 0.01g
4with 0.29g Co (NO
3)
26H
2o is dissolved in above 40ml hac buffer.Cushioning liquid above containing slaine is joined 24ml 1.0mol/L MnSO
4in solution, mix.Be 0.1mol/L KMnO by 120ml concentration subsequently
4solution instills in above-mentioned mixed solution, wherein KMnO
4/ MnSO
4(mol ratio)=0.5, stirs 2 hours, sealing ageing 12 hours, 80 DEG C of backflows 20 hours, revolve steaming 3 hours until powdered, with deionized water rinsing to neutral, 100 DEG C of dryings 10 hours, then grind into powder, obtains black presoma.Get above-mentioned presoma to mix than for 8g:200ml ratio with straight alcohol.This mixture is stirred 24 hours, revolves steaming and solution was evaporated in 3 hours.The product obtained in pure oxygen atmosphere with the speed of 1 DEG C/min, be raised to the roasting 1 hour of 300 DEG C of degree, finally obtain Co/Sr-α-MnO
2-I product.
(2) catalyst activity evaluation.Benzene concentration is 500ppm, and air-flow air speed is 60,000h
-1.Gas-chromatography TCD detection reaction tail gas CO
2with CO, FID detect the content of benzene and other organic species.The temperature of the complete catalytic combustion elimination benzene of catalyst obtained by the embodiment of the present invention 1 (benzene 100% transforms) is 290 DEG C, when 220 DEG C, the conversion ratio of benzene reaches 50%, when temperature is in the scope of 150 DEG C ~ 290 DEG C, benzene conversion ratio straight line raises until reach 100%, in the catalytic combustion elimination reaction of benzene, benzene changes into CO completely
2and H
2o; When reaction temperature is 170 DEG C, the conversion ratio of toluene reaches 50%, and when 200 DEG C, the conversion ratio of toluene reaches 100%, and product only has CO
2and H
2o.
Embodiment 2
(1) preparation method of above-mentioned catalyst provided by the present invention, comprises the steps:
Be that KAc and the 0.1mol/L HAc of 0.1mol/L is mixed into cushioning liquid in KAc/HAc mol ratio=1.0 ratio by concentration, regulate about pH=4.74, subsequently by the SrSO of 0.02g
4with 1.00g Co (NO
3)
26H
2o is dissolved in above 40ml hac buffer.By the PVAC polyvinylalcohol (molecular formula (C of 0.5g
2h
4o)
n, molecular weight 20000) and to be dissolved in 30ml concentration be 1.3mol/LMnSO
4in solution, the cushioning liquid above containing slaine is joined 40ml 1.0mol/L MnSO
4in solution, mix.Be 0.2mol/L KMnO by 140ml concentration subsequently
4solution instills in above-mentioned mixed solution, wherein KMnO
4/ MnSO
4(mol ratio)=0.7, stirs 2 hours, sealing ageing 12 hours, 90 DEG C of backflows 23 hours, revolve steaming 3 hours until powdered, with deionized water rinsing to neutral, 110 DEG C of dryings 10 hours, then grind into powder, obtains black presoma.Get above-mentioned presoma to mix than for 8g:200ml ratio with straight alcohol.This mixture is stirred 24 hours, revolves steaming and solution was evaporated in 3 hours.The product obtained in pure oxygen atmosphere with the speed of 1 DEG C/min, be raised to the roasting 2 hours of 400 DEG C of degree, finally obtain Co/Sr-α-MnO
2-II product.
(2) catalyst activity evaluation.Benzene series Concentrations is 500ppm, and air-flow air speed is 60,000h
-1.Gas-chromatography TCD detection reaction tail gas CO
2with CO, FID detect the content of benzene and other organic species.The temperature of the complete catalytic combustion elimination benzene of catalyst obtained by the embodiment of the present invention 2 (benzene 100% transforms) is 310 DEG C, when 240 DEG C, the conversion ratio of benzene reaches 50%, when temperature is in the scope of 150 DEG C ~ 300 DEG C, benzene conversion ratio straight line raises until reach 100%, in the catalytic combustion elimination reaction of benzene, benzene changes into CO completely
2and H
2o; When reaction temperature is 200 DEG C, the conversion ratio of toluene reaches 50%, and when 250 DEG C, the conversion ratio of toluene reaches 100%, and product only has CO
2and H
2o.
Embodiment 3
(1) preparation method of above-mentioned catalyst provided by the present invention, comprises the steps:
Be that KAc and the 0.1mol/L HAc of 0.1mol/L is mixed into cushioning liquid in KAc/HAc mol ratio=5.0 ratio by concentration, regulate pH about 5.44, subsequently by the SrSO of 0.03g
4with 2.50g Co (NO
3)
26H
2o is dissolved in above 40ml hac buffer.By the PVAC polyvinylalcohol (molecular formula (C of 1.8g
2h
4o)
n, molecular weight 20000) and to be dissolved in 40ml concentration be 1.5mol/L MnSO
4in solution, the cushioning liquid above containing slaine is joined in this solution, mixes.Be 0.3mol/L KMnO by 160ml concentration subsequently
4solution instills in above-mentioned mixed solution, wherein KMnO
4/ MnSO
4(mol ratio)=0.8, stirs 3 hours, sealing ageing 12 hours, 110 DEG C of backflows 26 hours, revolve steaming 4 hours until powdered, with deionized water rinsing to neutral, 140 DEG C of dryings 12 hours, then grind into powder, obtains black presoma.Get above-mentioned presoma to mix than for 8g:200ml ratio with straight alcohol.This mixture is stirred 24 hours, revolves steaming and solution was evaporated in 4 hours.The product obtained in pure oxygen atmosphere with the speed of 1 DEG C/min, be raised to the roasting 4 hours of 450 DEG C of degree, finally obtain Co/Sr-α-MnO
2-III product.
(2) catalyst activity evaluation.Benzene series Concentrations is 1000ppm, and air-flow air speed is 100,000h
-1.Gas-chromatography TCD detection reaction tail gas CO
2with CO, FID detect the content of benzene and other organic species.The temperature of the complete catalytic combustion elimination benzene of catalyst obtained by the embodiment of the present invention 3 (benzene 100% transforms) is 300 DEG C, when 260 DEG C, the conversion ratio of benzene reaches 50%, when temperature is in the scope of 150 DEG C ~ 300 DEG C, benzene conversion ratio straight line raises until reach 100%, in the catalytic combustion elimination reaction of benzene, benzene changes into CO completely
2and H
2o; When reaction temperature is 215 DEG C, the conversion ratio of toluene reaches 50%, and when 250 DEG C, the conversion ratio of toluene reaches 100%, and product only has CO
2and H
2o.
Embodiment 4
(1) preparation method of above-mentioned catalyst provided by the present invention, comprises the steps:
Be that KAc and the 0.1mol/L HAc of 0.1mol/L is mixed into cushioning liquid in KAc/HAc mol ratio=10.0 ratio by concentration, regulate pH about 5.74, subsequently by the SrSO of 0.05g
4with 3.24g Co (NO
3)
26H
2o is dissolved in above 40ml hac buffer.By the PVAC polyvinylalcohol (molecular formula (C of 2.0g
2h
4o)
n, molecular weight 20000) and to be dissolved in 34ml concentration be 2.0mol/L MnSO
4in solution, the cushioning liquid above containing slaine is joined in this solution, mixes.Be 0.4mol/L KMnO by 170ml concentration subsequently
4solution instills in above-mentioned mixed solution, wherein KMnO
4/ MnSO
4(mol ratio)=1.0, stir 4 hours, sealing ageing 12 hours, 120 DEG C of backflows 26 hours, revolve steaming 4 hours until powdered, with deionized water rinsing to neutral, 140 DEG C of dryings 12 hours, then grind into powder, obtains black presoma.Get above-mentioned presoma to mix than for 8g:200ml ratio with straight alcohol.This mixture is stirred 24 hours, revolves steaming and solution was evaporated in 4 hours.The product obtained in pure oxygen atmosphere with the speed of 1 DEG C/min, be raised to the roasting 4 hours of 500 DEG C of degree, finally obtain Co/Sr-α-MnO
2-IV product.
(2) catalyst activity evaluation.Benzene series Concentrations is 1000ppm, and air-flow air speed is 100,000h
-1.Gas-chromatography TCD detection reaction tail gas CO
2with CO, FID detect the content of benzene and other organic species.The temperature of the complete catalytic combustion elimination benzene of catalyst obtained by the embodiment of the present invention 4 (benzene 100% transforms) is 230 DEG C, when 200 DEG C, the conversion ratio of benzene reaches 50%, when temperature is in the scope of 150 DEG C ~ 230 DEG C, benzene conversion ratio straight line raises until reach 100%, in the catalytic combustion elimination reaction of benzene, benzene changes into CO completely
2and H
2o; When reaction temperature is 170 DEG C, the conversion ratio of toluene reaches 50%, and when 200 DEG C, the conversion ratio of toluene reaches 100%, and product only has CO
2and H
2o.
Claims (4)
1. a preparation method for alpha-oxidation manganese Supported Co strontium catalyst, is characterized in that:
KAc solution and HAc solution are mixed into cushioning liquid in KAc/HAc mol ratio=0.1 ~ 10.0 ratio, regulate pH between 3.74 ~ 5.74, subsequently by the SrSO of 0.01g ~ 0.05g
4with 0.29g ~ 3.24gCo (NO
3)
26H
2o is dissolved in above 40ml hac buffer; The PVAC polyvinylalcohol of 0.0g ~ 2.0g being dissolved in 20ml ~ 60ml concentration is 1.0mol/L ~ 2.0mol/L MnSO
4in solution, the cushioning liquid above containing slaine is joined in this solution, mixes; Be 0.1mol/L ~ 0.4mol/L KMnO by 120ml ~ 170ml concentration subsequently
4solution instills in above-mentioned mixed solution, wherein KMnO
4/ MnSO
4mol ratio=0.5 ~ 1.0, stir 2 ~ 4 hours, sealing ageing 12 hours, 80 ~ 120 DEG C of backflows 20 ~ 26 hours, revolve steaming 3 ~ 4 hours until powdered, with deionized water rinsing to neutral, 100 DEG C ~ 140 DEG C dryings 10 ~ 12 hours, then grind into powder, obtains black presoma; Get above-mentioned presoma to mix than for 8g:200ml ratio with straight alcohol; This mixture is stirred 24 hours, revolves steaming and solution was evaporated in 3 ~ 4 hours; The product obtained in pure oxygen atmosphere with the speed of 1 DEG C/min, be raised to the roasting 1 ~ 4 hour of 300 DEG C ~ 500 DEG C degree, finally obtain Co/Sr-α-MnO
2product.
2. preparation method according to claim 1, is characterized in that: the molecular formula of PVAC polyvinylalcohol is (C
2h
4o)
n, molecular weight 20000.
3. the application in benzene homologues eliminated by the catalyst prepared of preparation method according to claim 1, it is characterized in that: be placed on by above-mentioned catalyst in continuous-flow fixed bed device and pass into benzene or toluene and air Mixture and react; Reaction pressure is normal pressure ~ 2MPa, and reaction velocity is 60,000h
-1~ 100,000h
-1, in air and benzene or toluene gaseous mixture, the concentration of benzene or toluene is 500ppm ~ 1000ppm, reaction temperature 25 ~ 300 DEG C.
4. apply according to claim 3, it is characterized in that: in above-mentioned reaction mixture gas, air is the Standard Gases of configuration, its N
2: O
2volume ratio is 79:21.
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Cited By (3)
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|---|---|---|---|---|
| CN104941631A (en) * | 2015-07-22 | 2015-09-30 | 重庆工商大学 | Preparation method of nano-alpha-MnO2 catalyst, nano-alpha-MnO2 catalyst and application of nano-alpha-MnO2 catalyst |
| CN111686754A (en) * | 2020-07-07 | 2020-09-22 | 四川大学 | Non-noble metal catalyst for catalytic combustion of volatile organic compounds and preparation method thereof |
| CN114471622A (en) * | 2021-12-23 | 2022-05-13 | 常州大学 | Ozone decomposition catalyst and preparation method thereof |
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| CN114471622B (en) * | 2021-12-23 | 2023-09-05 | 常州大学 | Ozone decomposition catalyst and preparation method thereof |
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