CN109647420A - Calcium analysis cobalt acid lanthanum perofskite type oxide and its preparation method and application for heat catalytic oxidation toluene - Google Patents

Calcium analysis cobalt acid lanthanum perofskite type oxide and its preparation method and application for heat catalytic oxidation toluene Download PDF

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CN109647420A
CN109647420A CN201811607632.9A CN201811607632A CN109647420A CN 109647420 A CN109647420 A CN 109647420A CN 201811607632 A CN201811607632 A CN 201811607632A CN 109647420 A CN109647420 A CN 109647420A
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toluene
catalytic oxidation
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calcium
cobalt acid
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CN109647420B (en
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梁晓亮
陈汉林
韦高玲
刘鹏
何宏平
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Guangzhou Institute of Geochemistry of CAS
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Abstract

The invention discloses a kind of calcium analysis cobalt acid lanthanum perofskite type oxides for heat catalytic oxidation toluene, preparation method is as follows: using lanthanum salt, cobalt salt, calcium salt as raw material, citric acid is as complexing agent, ethyl alcohol water mixed liquid is as solvent, sol-gel method obtains calcium analysis perovskite presoma, then through calcining, tabletting, broken, screening obtains the perovskite type catalyst for heat catalytic oxidation toluene；Calcium analysis cobalt acid lanthanum perovskite type catalyst prepared by the present invention for heat catalytic oxidation toluene is graininess, can effective catalysis oxidation high concentration toluene, for removing high concentration (> 1000mL/m3) toluene, toluene removal rate can reach 100%；Have many advantages, such as that low in cost, catalytic activity is high, water-resistance is strong, thermal stability is good, without secondary pollution, the purified treatment suitable for industrial waste gas middle and high concentration toluene waste gas.

Description

Calcium analysis cobalt acid lanthanum perofskite type oxide and its system for heat catalytic oxidation toluene Preparation Method and application
Technical field:
The present invention relates to a kind of for the calcium analysis cobalt acid lanthanum perofskite type oxide of heat catalytic oxidation toluene and its preparation Methods and applications.
Background technique:
Now with the rapid industrial development in our country, atmosphere polluting problem is got worse, and industrial waste gas processing technique is more next More receive significant attention.Toluene (C6H5CH3) be organic chemical industry's production field important source material, largely be used as solvent and higher octane It is worth gasoline additive.Toluene is a kind of typical volatile organic matter (VOCs), has acute toxicity, genotoxicity, mutagenesis Deng harm, direct emission can bring serious harm to human health and environment.
Heat catalytic oxidation method is the effective ways of current industrial processing high concentration toluene, has catalytic temperature low, activity The advantages that height, environmental pollution is small.Catalyst is the core of heat catalytic oxidation technology.Traditional catalyst include noble metal catalyst and Metal oxide catalyst.The initial catalytic activity of noble metal catalyst is good, but there are expensive, easily poisoning, high temperature is easy The disadvantages of sintering.Catalyst of transition metal oxide is although cheap, but often catalytic activity is bad.Therefore develop efficiently, Cheap catalyst has become one of the emphasis of heat catalytic oxidation toluene research.Perofskite type oxide belongs to combined oxidation Object, due to composition multiplicity, stable structure, it is inexpensive and environmentally friendly the advantages that, in terms of pollutant control increasingly by Concern.
Summary of the invention:
The object of the present invention is to provide a kind of catalytic activity height, thermal stability is good, water-resistance is strong, low-cost for heat The calcium analysis cobalt acid lanthanum perofskite type oxide of catalysis oxidation toluene optimizes its structure using sol-gal process synthesis is improved, into One step improves its catalytic activity, improves its catalytic performance and water-resistance, is adapted to the thermocatalytic of middle and high concentration industrial toluene exhaust gas Oxidation processes.
The present invention is achieved by the following technical programs:
A kind of calcium analysis cobalt acid lanthanum perofskite type oxide for heat catalytic oxidation toluene, preparation method are as follows: with As raw material, citric acid is obtained as complexing agent, ethyl alcohol water mixed liquid as solvent, sol-gel method for lanthanum salt, cobalt salt, calcium salt Calcium analysis perovskite presoma, then through calcining, tabletting is crushed, and screening obtains the Ca-Ti ore type for heat catalytic oxidation toluene Catalyst；Specifically includes the following steps:
1) lanthanum salt, cobalt salt, calcium salt and citric acid are added in ethyl alcohol water mixed liquid, 2-3h is stirred at room temperature and obtains colloidal sol, wherein Lanthanum salt, cobalt salt, calcium salt molar ratio be 1-x:1:x, wherein 0 < x≤0.4；The metal cations such as lanthanum ion, cobalt ions, calcium ion Summation and citric acid molar ratio be 1:1.0-1.5；
2) colloidal sol that step 1) obtains continuously stirs dry 20- in 5-6h, then 85-95 DEG C of vacuum oven at 80-85 DEG C For 24 hours, xerogel is obtained, is calcium analysis perovskite presoma；
3) 3-5 hours are calcined at 400-450 DEG C of xerogel that step 2) obtains, then calcination 4-6 is small at 680-720 DEG C When, tabletting is crushed, and classifying screen selects the cobalt acid lanthanum particle of 35~60 mesh, and it is subsequently placed in Muffle furnace at 400 DEG C and is calcined 3 hours, Obtain the calcium analysis cobalt acid lanthanum perovskite oxide for heat catalytic oxidation toluene.
Preferably, the lanthanum salt is La (NO3)3·6H2O, the cobalt salt are Co (NO3)2·6H2O, the calcium salt For Ca (NO3)2·4H2O。
Preferably, the x value is 0.01-0.15, and optimal x value is 0.1.
Preferably, the ethyl alcohol in the ethyl alcohol water mixed liquid and water volume ratio are 1:1-2.
The present invention also protects the calcium analysis cobalt acid lanthanum perofskite type oxide for heat catalytic oxidation toluene being catalyzed Aoxidize the application in terms of toluene.
Beneficial effects of the present invention are as follows: the calcium analysis cobalt acid lanthanum calcium titanium prepared by the present invention for heat catalytic oxidation toluene Mine type catalyst La1-xCaxCoO3(0 < x≤0.4) is graininess, has excellent catalytic activity to toluene, wherein La0.9Ca0.1CoO3Nano particle is 1000ppm in toluene concentration and air speed is 30000cm3g-1h-1Under conditions of, toluene is complete The temperature of oxidation is 215 DEG C, and reaction product only has CO2And H2O has no the generation of other secondary pollution by-products, in addition, the catalysis It is catalyzed toluene 24 hours under conditions of 250 DEG C of agent, does not there is the phenomenon that inactivation, illustrate that the catalyst thermal stability is good, in addition, Under conditions of 5000ppm steam, activity is not reduced, and illustrates that the catalyst has excellent water repelling property.The catalyst has It is low in cost, the advantages that catalytic activity is high, water-resistance is strong, thermal stability is good, without secondary pollution, highly concentrated suitable for industrial waste gas Spend the purified treatment of toluene waste gas.
Detailed description of the invention:
Fig. 1 is that X of the embodiment 1-5 preparation for the calcium analysis cobalt acid lanthanum perofskite type oxide of heat catalytic oxidation toluene is penetrated Ray diffraction diagram；
Fig. 2 is urging for the calcium analysis cobalt acid lanthanum perofskite type oxide that embodiment 1-5 preparation is used for heat catalytic oxidation toluene Change activity rating figure；
Fig. 3 is the calcium analysis cobalt acid lanthanum perofskite type oxide conduct for heat catalytic oxidation toluene prepared by embodiment 2 The water-resistance and estimation of stability figure of catalyst；
Wherein, example 1 is the abbreviation of embodiment 1, and example 2 is the abbreviation of embodiment 2, the abbreviation that example 3 is embodiment 3, Example 4 is the abbreviation of embodiment 4, and example 5 is the abbreviation of embodiment 5.
Specific embodiment:
It is to further explanation of the invention, rather than limiting the invention below.
Embodiment 1:
1) 30mL ethyl alcohol is measured, is added in 30mL ultrapure water, stirs evenly, 4.331g (0.01mol) La is then added (NO3)3·6H2O, 2.911g (0.01mol) Co (NO3)2·6H2O and 4.62g citric acid is stirred at room temperature 3h and obtains colloidal sol.
2) gained colloidal sol continuously stirs 6h, then 90 DEG C of vacuum ovens dryings are for 24 hours, done under the conditions of 80 DEG C of oil baths Gel.
3) gained xerogel is placed in Muffle furnace at 400 DEG C to be calcined at 4 hours, then 700 DEG C and be calcined 5 hours, and tabletting is broken Broken, classifying screen chooses the cobalt acid lanthanum of 35~60 mesh, is placed in Muffle furnace at 400 DEG C and is calcined 3 hours, obtains sample 1.
Identification and analysis is carried out to composite sample 1, XRD (spread out by the abbreviation of XRD, that is, X-ray diffraction, X-ray Penetrate) map (as shown in Figure 1) and standard card (PDF) unanimously, this illustrates the cobalt acid lanthanum perovskite for having synthesized pure phase.Take 0.1g should Composite sample 1 is used as catalyst, gas flow rate 100mL/min, and corresponding air speed is 30000mL/ (gh), toluene concentration For 1000mL/m3, in normal pressure, under conditions of temperature is 225 DEG C, toluene removal rate is 8.7%.Activity evaluation such as Fig. 2 institute Show.
Embodiment 2
1) 30mL ethyl alcohol is measured, is added in 30mL ultrapure water, stirs evenly, 3.897g (0.009mol) La is then added (NO3)3·6H2O, 0.236g Ca (NO3)2·4H2O (0.001mol), 2.911g (0.01mol) Co (NO3)2·6H2O (nitric acid Lanthanum, cobalt nitrate, calcium nitrate molar ratio be 0.9:1:0.1) and 4.62g citric acid, 3h is stirred at room temperature and obtains colloidal sol.
2) gained colloidal sol continuously stirs 6h, then 90 DEG C of vacuum ovens dryings are for 24 hours, done under the conditions of 80 DEG C of oil baths Gel.
3) gained xerogel is placed in Muffle furnace at 400 DEG C to be calcined at 4 hours, then 700 DEG C and be calcined 5 hours, and tabletting is broken Broken, classifying screen chooses the cobalt acid lanthanum of 35~60 mesh, is placed in Muffle furnace at 400 DEG C and is calcined 3 hours, obtains object sample 2.
Identification and analysis is carried out to sample 2, XRD spectra is similar to the XRD spectra of cobalt acid lanthanum, and diffraction maximum is inclined to high angle It moves, shows that calcium enters in cobalt acid lanthanum perovskite structure, as shown in Figure 1.Take the 0.1g composite sample 2 as catalyst, gas Body flow velocity is 100mL/min, and corresponding air speed is 30000mL/ (gh), toluene concentration 1000mL/m3, in normal pressure, temperature Under conditions of 225 DEG C, toluene removal rate is 100%.Activity evaluation is as shown in Figure 2.As catalyst water-resistance and Estimation of stability figure such as Fig. 3.It is catalyzed toluene 24 hours under conditions of 250 DEG C of the catalyst, does not have the phenomenon that inactivation, illustrate this Catalyst thermal stability is good, in addition, activity does not reduce under conditions of 5000ppm steam, it is excellent to illustrate that the catalyst has Water repelling property.
Embodiment 3
1) 30mL ethyl alcohol is measured, is added in 30mL ultrapure water, stirs evenly, 3.464g (0.008mol) La is then added (NO3)3·6H2O, 0.472g Ca (NO3)2·4H2O (0.002mol), 2.911g (0.01mol) Co (NO3)2·6H2O (nitric acid Lanthanum, cobalt nitrate, calcium nitrate molar ratio be 0.8:1:0.2) and 4.62g citric acid, 3h is stirred at room temperature and obtains colloidal sol.
2) gained colloidal sol continuously stirs 6h, then 90 DEG C of vacuum ovens dryings are for 24 hours under the conditions of 80 DEG C of oil baths.It is done Gel.
3) gained xerogel is placed in Muffle furnace at 400 DEG C to be calcined at 4 hours, then 700 DEG C and be calcined 5 hours, and tabletting is broken Broken, classifying screen chooses the cobalt acid lanthanum of 35~60 mesh, is placed in Muffle furnace at 400 DEG C and is calcined 3 hours, obtains sample 3.
Identification and analysis is carried out to sample 3, XRD spectra is similar to the XRD spectra of cobalt acid lanthanum, and diffraction maximum is inclined to high angle It moves, shows that calcium enters in cobalt acid lanthanum perovskite structure, as shown in Figure 1.As shown in Figure 1.Take 0.1g 1 conduct of composite sample Catalyst, gas flow rate 100mL/min, corresponding air speed be 30000mL/ (gh), toluene concentration 1000mL/m3, Normal pressure, under conditions of temperature is 225 DEG C, toluene removal rate is 41%.Activity evaluation is as shown in Figure 2.250 DEG C of the catalyst Under conditions of be catalyzed toluene 24 hours, do not have the phenomenon that inactivation, illustrate that the catalyst thermal stability is good, in addition, in 5000ppm Under conditions of steam, activity is not reduced, and illustrates that the catalyst has excellent water repelling property.
Embodiment 4
1) 30mL ethyl alcohol is measured, is added in 30mL ultrapure water, stirs evenly, 3.031g (0.007mol) La is then added (NO3)3·6H2O, 0.708g (0.003mol) Ca (NO3)2·4H2O, 2.911g (0.01mol) Co (NO3)2·6H2O (nitric acid Lanthanum, cobalt nitrate, calcium nitrate molar ratio be 0.7:1:0.3) and 4.62g citric acid, 3h is stirred at room temperature and obtains colloidal sol.
2) gained colloidal sol continuously stirs 6h, then 90 DEG C of vacuum ovens dryings are for 24 hours under the conditions of 80 DEG C of oil baths.It is done Gel.
3) gained xerogel is placed in Muffle furnace at 400 DEG C to be calcined at 4 hours, then 700 DEG C and be calcined 5 hours, and tabletting is broken Broken, classifying screen chooses the cobalt acid lanthanum of 35~60 mesh, is placed in Muffle furnace at 400 DEG C and is calcined 3 hours, obtains sample 4.
Identification and analysis is carried out to sample 4, XRD spectra is similar to the XRD spectra of cobalt acid lanthanum, and diffraction maximum is inclined to high angle It moves, shows that calcium enters in cobalt acid lanthanum perovskite structure, as shown in Figure 1.As shown in Figure 1.Take 0.1g 1 conduct of composite sample Catalyst, gas flow rate 100mL/min, corresponding air speed are 30000mL/ (gh), toluene concentration 1000mL/m3, Normal pressure, under conditions of temperature is 225 DEG C, toluene removal rate is 29%.Activity evaluation is as shown in Figure 2.250 DEG C of the catalyst Under conditions of be catalyzed toluene 24 hours, do not have the phenomenon that inactivation, illustrate that the catalyst thermal stability is good, in addition, in 5000ppm Under conditions of steam, activity is not reduced, and illustrates that the catalyst has excellent water repelling property.
Embodiment 5
1) 30mL ethyl alcohol is measured, is added in 30mL ultrapure water, stirs evenly, 2.598g (0.006mol) La is then added (NO3)3·6H2O, 0.944g Ca (NO3)2·4H2O (0.004mol), 2.911g (0.01mol) Co (NO3)2·6H2O (nitric acid Lanthanum, cobalt nitrate, calcium nitrate molar ratio be 0.6:1:0.4) and 4.62g citric acid, 3h is stirred at room temperature and obtains colloidal sol.
2) gained colloidal sol continuously stirs 6h, then 90 DEG C of vacuum ovens dryings are for 24 hours under the conditions of 80 DEG C of oil baths.It is done Gel.
3) gained xerogel is placed in Muffle furnace at 400 DEG C to be calcined at 4 hours, then 700 DEG C and be calcined 5 hours, and tabletting is broken Broken, classifying screen chooses the cobalt acid lanthanum of 35~60 mesh, is placed in Muffle furnace at 400 DEG C and is calcined 3 hours, obtains sample 5.
Identification and analysis is carried out to sample 5, XRD spectra is similar to the XRD spectra of cobalt acid lanthanum, and diffraction maximum is inclined to high angle It moves, shows that calcium enters in cobalt acid lanthanum perovskite structure, as shown in Figure 1.As shown in Figure 1.Take 0.1g 1 conduct of composite sample Catalyst, gas flow rate 100mL/min, corresponding air speed are 30000mL/ (gh), toluene concentration 1000mL/m3, Normal pressure, under conditions of temperature is 225 DEG C, toluene removal rate is 25%.Activity evaluation is as shown in Figure 2.250 DEG C of the catalyst Under conditions of be catalyzed toluene 24 hours, do not have the phenomenon that inactivation, illustrate that the catalyst thermal stability is good, in addition, in 5000ppm Under conditions of steam, activity is not reduced, and illustrates that the catalyst has excellent water repelling property.

Claims (6)

1. a kind of calcium analysis cobalt acid lanthanum perofskite type oxide for heat catalytic oxidation toluene, which is characterized in that its preparation side Method the following steps are included:
1) lanthanum salt, cobalt salt, calcium salt and citric acid are added in ethyl alcohol water mixed liquid, 2-3h is stirred at room temperature and obtains colloidal sol, wherein lanthanum Salt, cobalt salt, calcium salt molar ratio be 1-x:1:x, 0 < x≤0.4；The summation of metal cation and the molar ratio of citric acid are 1: 1.0-1.5；
2) colloidal sol that step 1) obtains continuously stirs dry 20-24h in 5-6h, then 85-95 DEG C of vacuum oven at 80-85 DEG C, Obtain xerogel；
3) it is calcined 3-5 hours at 400-450 DEG C of xerogel that step 2) obtains, is then calcined 4-6 hours at 680-720 DEG C, presses Piece is crushed, and classifying screen selects the cobalt acid lanthanum particle of 35~60 mesh, is subsequently placed in Muffle furnace at 400 DEG C and is calcined 3 hours, obtains Calcium analysis cobalt acid lanthanum perovskite oxide for heat catalytic oxidation toluene.
2. being used for the calcium analysis cobalt acid lanthanum perofskite type oxide of heat catalytic oxidation toluene, feature according to claim 1 It is, the lanthanum salt is La (NO3)3·9H2O, the cobalt salt are Co (NO3)2·6H2O, the calcium salt are Ca (NO3)2·4H2O。
3. the calcium analysis cobalt acid lanthanum perofskite type oxide according to claim 1 or claim 2 for heat catalytic oxidation toluene, special Sign is that the x value is 0.01-0.15.
4. being used for the calcium analysis cobalt acid lanthanum perofskite type oxide of heat catalytic oxidation toluene, feature according to claim 3 It is, x value is 0.1.
5. the calcium analysis cobalt acid lanthanum perofskite type oxide according to claim 1 or claim 2 for heat catalytic oxidation toluene, special Sign is that the ethyl alcohol in the ethyl alcohol water mixed liquid and water volume ratio are 1:1-2.
6. the calcium analysis cobalt acid lanthanum perofskite type oxide described in claim 1 for heat catalytic oxidation toluene is in catalysis oxidation first Application in terms of benzene.
CN201811607632.9A 2018-12-27 2018-12-27 Calcium-doped lanthanum perovskite cobaltite type oxide for thermal catalytic oxidation of toluene and preparation method and application thereof Expired - Fee Related CN109647420B (en)

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