CN105170152B - A kind of iron ion exchange titanium ion pillared montmorillonite catalyst and preparation method thereof for heat catalytic oxidation toluene - Google Patents

A kind of iron ion exchange titanium ion pillared montmorillonite catalyst and preparation method thereof for heat catalytic oxidation toluene Download PDF

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CN105170152B
CN105170152B CN201510560923.7A CN201510560923A CN105170152B CN 105170152 B CN105170152 B CN 105170152B CN 201510560923 A CN201510560923 A CN 201510560923A CN 105170152 B CN105170152 B CN 105170152B
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titanium
montmorillonite
pillared
ion
iron
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CN105170152A (en
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戚飞鸿
梁晓亮
刘鹏
何宏平
杨士建
林枭举
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Guangzhou Institute of Geochemistry of CAS
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Guangzhou Institute of Geochemistry of CAS
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Abstract

The iron ion exchange titanium ion pillared montmorillonite catalyst and preparation method thereof that the invention discloses a kind of for heat catalytic oxidation toluene.The present invention is using na-montmorillonite, molysite, titanium salt as raw material, na-montmorillonite obtains titanium pillared montmorillonite presoma by the way that titanium ion is pillared, titanium pillared montmorillonite is obtained after calcining, then titanium pillared montmorillonite is exchanged with iron ion, it synthesizes iron ion and exchanges titanium ion pillared montmorillonite presoma, it is washed, it is dry, sieving, calcining, which is prepared, exchanges titanium ion pillared montmorillonite catalyst for the iron ion of heat catalytic oxidation toluene.It can effective catalysis oxidation high concentration toluene, for removed under the conditions of 375 DEG C high concentration (>1000mL/m3) first it is stupid, toluene removal rate reaches 90% or more；Have many advantages, such as that catalytic activity is high, low in cost, thermal stability is good, without secondary pollution, the purified treatment suitable for industrial waste gas middle and high concentration toluene.

Description

A kind of iron ion exchange titanium ion pillared montmorillonite for heat catalytic oxidation toluene is urged Agent and preparation method thereof
Technical field：
The invention belongs to toluene oxidation processing technology fields, and in particular to a kind of iron ion for heat catalytic oxidation toluene Exchange titanium ion pillared montmorillonite catalyst and preparation method thereof.
Background technique：
With the rapid industrial development in our country, atmosphere polluting problem is got worse, industrial waste gas processing technique increasingly by To extensive concern.Toluene (C6H5CH3) be organic chemical industry's production field important source material, largely be used as solvent and high-octane rating vapour Oil additive.Toluene is a kind of typical volatile organic matter (VOCs), has the danger such as acute toxicity, genotoxicity, mutagenesis Evil, 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.Metal oxide catalyst is although cheap, but often catalytic activity is bad.Therefore it develops efficiently, inexpensively Catalyst have become one of the emphasis of heat catalytic oxidation toluene research.Natural smectite is inexpensive and right since source is wide Advantages of environment protection, in terms of pollutant control more and more attention has been paid to.Natural smectite can be pillared by ion exchange Other ions are introduced interlayer, change its interlayer environment, make its structure and properties that corresponding change occur by the physical chemistry methods such as modified, It is adapted to the improvement of pollutant.
Summary of the invention：
That the first purpose of the invention is to provide a kind of catalytic activity is high, thermal stability is good, low-cost urges for heat Change the iron ion exchange titanium ion pillared montmorillonite catalyst and preparation method thereof of oxidation toluene.
The preparation side of iron ion exchange titanium ion pillared montmorillonite catalyst for heat catalytic oxidation toluene of the invention Method, which is characterized in that include the following steps：Using na-montmorillonite, molysite, titanium salt as raw material, na-montmorillonite by titanium from Son is pillared to obtain titanium pillared montmorillonite presoma, and titanium pillared montmorillonite is obtained after calcining, then pillared with iron ion exchange titanium Montmorillonite, synthesis iron ion exchanges titanium ion pillared montmorillonite presoma, washed, dry, sieving, and calcining, which is prepared, to be used for The iron ion of heat catalytic oxidation toluene exchanges titanium ion pillared montmorillonite catalyst.
It is described using na-montmorillonite, molysite, titanium salt as raw material, na-montmorillonite obtains titanium column by the way that titanium ion is pillared Support montmorillonite presoma, titanium pillared montmorillonite is obtained after calcining, then with iron ion exchange titanium pillared montmorillonite, synthesis iron from Preferably at 60 DEG C, titanium ion solution is added in montmorillonite suspension exchange titanium ion pillared montmorillonite presoma, covers de- Stone suspension Tu Shui ratio is 1g:100ml, the pillared amount of titanium are 5mmol/g montmorillonite, are separated by solid-liquid separation after reaction, after taking solid dry Titanium pillared montmorillonite presoma is obtained, titanium pillared montmorillonite presoma obtains titanium pillared montmorillonite after calcining, then uses iron ion Titanium pillared montmorillonite is exchanged, iron concentration 0.05M obtains iron ion exchange titanium ion pillared montmorillonite presoma.
It is preferred that the molysite is Fe (NO3)3·9H2O, the titanium salt are TiCl4。
It is preferred that the pillared temperature of the titanium ion is 60 DEG C, the pillared time is that for 24 hours, iron ion swap time is 6h.
The drying is dry in 80 DEG C of blowing-type drying boxes.
The sieving, calcining are the particles that the sample after drying is filtered out to 35~60 mesh, in Muffle furnace at 500 DEG C It roasting oxidation 3 hours, obtains exchanging titanium ion pillared montmorillonite catalyst for the iron ion of heat catalytic oxidation toluene.
It is a kind of that the pillared illiteracy of titanium ion is exchanged according to the iron ion for heat catalytic oxidation toluene that the above method is prepared De- stone catalyst.
A second object of the present invention is to provide pillared cover of iron ion exchange titanium ion for heat catalytic oxidation toluene to take off Application of the stone catalyst in terms of catalysis oxidation toluene.
The prepared by the method iron ion for heat catalytic oxidation toluene exchanges titanium ion pillared montmorillonite catalyst For graininess.It can effective catalysis oxidation high concentration toluene, for remove high concentration (>1000mL/m3) toluene, toluene goes Except rate can reach 90% or more；Have many advantages, such as that low in cost, catalytic activity is high, thermal stability is good, without secondary pollution, is suitable for The purified treatment of industrial waste gas middle and high concentration toluene.
Detailed description of the invention：
Fig. 1 is the iron for heat catalytic oxidation toluene of composite sample 1 prepared by embodiment 1 and embodiment 2-5 preparation The X-ray diffractogram of ion exchange titanium ion pillared montmorillonite catalyst, wherein 1,2,3,4,5 respectively represent composite sample 1 Titanium ion pillared montmorillonite catalyst is exchanged with the iron ion for heat catalytic oxidation toluene of embodiment 2-5 preparation.
Fig. 2 is the iron for heat catalytic oxidation toluene of composite sample 1 prepared by embodiment 1 and embodiment 2-5 preparation The catalytically active assessment figure of ion exchange titanium ion pillared montmorillonite catalyst, wherein example 1,2,3,4,5 respectively represents compound Object sample 1 and the iron ion for heat catalytic oxidation toluene of embodiment 2-5 preparation exchange titanium ion pillared montmorillonite catalyst.
Specific embodiment：
The following examples are further illustrations of the invention, rather than limiting the invention.
Embodiment 1：
1. measuring 15mL HCl, it is dissolved in 60mL ultrapure water, stirs evenly, 22.5mL TiCl is then added4Solution, with Ultrapure water constant volume is to 250mL, and ageing is for 24 hours.[H at this time+]=0.6M, [Ti4+]=0.82M is the pillared liquid of titanium ion
2. weighing 10g na-montmorillonite, it is dissolved in 1000mL ultrapure water, stirring at normal temperature is montmorillonite suspension for 24 hours.
3. measuring the pillared liquid of 61mL titanium ion, it is slowly added in montmorillonite suspension, under 60 DEG C of water bath conditions, continuously stirs It mixes for 24 hours, centrifugation takes solids, cleans, and is placed in 80 DEG C of blowing-type drying boxes dry 12h, obtains titanium pillared montmorillonite forerunner Body.
4. classifying screen chooses the titanium pillared montmorillonite presoma of 35~60 mesh, it is small that calcination 3 at 500 DEG C is placed in Muffle furnace When, obtain composite sample 1.
5. pair composite sample 1 carries out identification and analysis, XRD (abbreviation of XRD, that is, X-ray diffraction, X-ray Diffraction) map is compared with na-montmorillonite, and 001 peak disappears, this illustrates that Ti ion has entered the lamellar structure of montmorillonite, by forging After burning, lamellar structure is destroyed, and occurs being partially stripped phenomenon, as shown in Figure 1.Take 0.1g 1 conduct of composite sample Catalyst, gas flow rate 100mL/min, corresponding air speed are 60000mL/ (gh), toluene concentration 1000mL/m3, Normal pressure, under conditions of temperature is 375 DEG C, toluene removal rate is 20%.Activity evaluation is as shown in Figure 2.
Embodiment 2
1. measuring 15mL HCl, it is dissolved in 60mL ultrapure water, stirs evenly, 22.5mL TiCl is then added4Solution, with Ultrapure water constant volume is to 250mL, and ageing is for 24 hours.[H at this time+]=0.6M, [Ti4+]=0.82M is the pillared liquid of titanium ion
2. weighing 10g na-montmorillonite, it is dissolved in 1000mL ultrapure water, stirring at normal temperature is montmorillonite suspension for 24 hours.
3. measuring the pillared liquid of 61mL titanium ion, it is slowly added in montmorillonite suspension, under 60 DEG C of water bath conditions, continuously stirs It mixes for 24 hours, centrifugation takes solids, cleans, and is placed in 80 DEG C of blowing-type drying boxes dry 12h, obtains titanium pillared montmorillonite forerunner Body.
4. classifying screen chooses the titanium pillared montmorillonite presoma of 35~60 mesh, it is placed in Muffle furnace and is calcined 2h at 350 DEG C, obtain To titanium pillared montmorillonite.
5. weighing the iron nitrate solution that 200mL0.05M is added in 2g titanium pillared montmorillonite, 6h is stirred at room temperature, takes solids, clearly It washes, is placed in 80 DEG C of blowing-type drying boxes dry 12h, obtain iron ion exchange titanium ion pillared montmorillonite presoma.
6. the iron ion that classifying screen chooses 35~60 mesh exchanges titanium ion pillared montmorillonite presoma, it is placed in Muffle furnace It is calcined 3 hours at 500 DEG C, obtains composite sample 2.
7. pair composite sample 2 carries out identification and analysis, XRD spectra is similar to the XRD spectra of titanium pillared montmorillonite, such as schemes Shown in 1.Take the 0.1g composite sample 2 as catalyst, gas flow rate 100mL/min, corresponding air speed is 60000mL/ (gh), toluene concentration 1000mL/m3, in normal pressure, under conditions of temperature is 375 DEG C, toluene removal rate is 97%.Activity is commented Valence result is as shown in Figure 2.Verifying composite sample 2 is that the iron ion to be prepared for heat catalytic oxidation toluene is handed over as a result, Change titanium ion pillared montmorillonite catalyst.
Embodiment 3
1. measuring 15mL HCl, it is dissolved in 60mL ultrapure water, stirs evenly, 22.5mL TiCl is then added4Solution, with Ultrapure water constant volume is to 250mL, and ageing is for 24 hours.[H at this time+]=0.6M, [Ti4+]=0.82M is the pillared liquid of titanium ion.
2. weighing 10g na-montmorillonite, it is dissolved in 1000mL ultrapure water, stirring at normal temperature is montmorillonite suspension for 24 hours.
3. measuring the pillared liquid of 61mL titanium ion, it is slowly added in montmorillonite suspension, under 60 DEG C of water bath conditions, continuously stirs It mixes for 24 hours, centrifugation takes solids, cleans, and is placed in 80 DEG C of blowing-type drying boxes dry 12h, obtains titanium pillared montmorillonite forerunner Body.
4. classifying screen chooses the titanium pillared montmorillonite presoma of 35~60 mesh, it is placed in Muffle furnace and is calcined 2h at 350 DEG C, obtain To titanium pillared montmorillonite.
5. weighing the iron nitrate solution that 200mL0.05M is added in 2g titanium pillared montmorillonite, 6h is stirred at room temperature, is centrifuged, by lower layer The iron nitrate solution of 200mL0.05M is added in sediment again, and centrifugation takes solids, cleans, and is placed in 80 DEG C of baking ovens dry 12h obtains iron ion exchange titanium ion pillared montmorillonite presoma.
6. the iron ion that classifying screen chooses 35~60 mesh exchanges titanium ion pillared montmorillonite presoma, it is placed in Muffle furnace It is calcined 3 hours at 500 DEG C, obtains composite sample 3.
7. pair composite sample 3 carries out identification and analysis, XRD spectra is similar to the XRD spectra of titanium pillared montmorillonite, such as schemes Shown in 1.Take the 0.1g composite sample 3 as catalyst, gas flow rate 100mL/min, corresponding air speed is 60000mL/ (gh), toluene concentration 1000mL/m3, in normal pressure, under conditions of temperature is 375 DEG C, toluene removal rate is 100%.Activity Evaluation result is as shown in Figure 2.Verifying composite sample 3 is the iron ion to be prepared for heat catalytic oxidation toluene as a result, Exchange titanium ion pillared montmorillonite catalyst.
Embodiment 4
1. measuring 15mL HCl, it is dissolved in 60mL ultrapure water, stirs evenly, 22.5mL TiCl is then added4Solution, with Ultrapure water constant volume is to 250mL, and ageing is for 24 hours.[H at this time+]=0.6M, [Ti4+]=0.82M is the pillared liquid of titanium ion.
2. weighing 10g na-montmorillonite, it is dissolved in 1000mL ultrapure water, stirring at normal temperature is montmorillonite suspension for 24 hours.
3. measuring the pillared liquid of 61mL titanium ion, it is slowly added in montmorillonite suspension, under 60 DEG C of water bath conditions, continuously stirs It mixes for 24 hours, centrifugation takes solids, cleans, and is placed in 80 DEG C of baking ovens dry 12h, obtains titanium pillared montmorillonite presoma.
4. classifying screen chooses the titanium pillared montmorillonite presoma of 35~60 mesh, it is placed in Muffle furnace and is calcined 2h at 350 DEG C, obtain To titanium pillared montmorillonite.
5. the iron nitrate solution that 200mL0.05M is added in 2g titanium pillared montmorillonite is weighed, in 60 DEG C of stirred in water bath 6h, from The heart takes solids, cleaning, is placed in 80 DEG C of baking ovens dry 12h, obtains iron ion exchange titanium ion pillared montmorillonite presoma.
6. the iron ion that classifying screen chooses 35~60 mesh exchanges titanium ion pillared montmorillonite presoma, it is placed in Muffle furnace It is calcined 3 hours at 500 DEG C, obtains composite sample 4.
7. pair composite sample 4 carries out identification and analysis, XRD spectra is similar to the XRD spectra of titanium pillared montmorillonite, such as schemes Shown in 1.Take the 0.1g composite sample 4 as catalyst, gas flow rate 100mL/min, corresponding air speed is 60000mL/ (gh), toluene concentration 1000mL/m3, in normal pressure, under conditions of temperature is 375 DEG C, toluene removal rate is 98%.Activity is commented Valence result is as shown in Figure 2.Verifying composite sample 4 is that the iron ion to be prepared for heat catalytic oxidation toluene is handed over as a result, Change titanium ion pillared montmorillonite catalyst.
Embodiment 5
1. measuring 15mL HCl, it is dissolved in 60mL ultrapure water, stirs evenly, 22.5mL TiCl is then added4Solution, with Ultrapure water constant volume is to 250mL, and ageing is for 24 hours.[H at this time+]=0.6M, [Ti4+]=0.82M is the pillared liquid of titanium ion.
2. weighing 10g na-montmorillonite, it is dissolved in 1000mL ultrapure water, stirring at normal temperature is montmorillonite suspension for 24 hours.
3. measuring the pillared liquid of 61mL titanium ion, it is slowly added in montmorillonite suspension, under 60 DEG C of water bath conditions, continuously stirs It mixes for 24 hours, centrifugation takes solids, cleans, and is placed in 80 DEG C of baking ovens dry 12h, obtains titanium pillared montmorillonite presoma.
4. classifying screen chooses the titanium pillared montmorillonite presoma of 35~60 mesh, it is placed in Muffle furnace and is calcined 2h at 350 DEG C, obtain To titanium pillared montmorillonite.
5. the iron nitrate solution that 200mL0.05M is added in 2g titanium pillared montmorillonite is weighed, in 60 DEG C of stirred in water bath 6h, from The iron nitrate solution of 200mL0.05M is added in lower sediment thing by the heart again, and in 60 DEG C of stirred in water bath 6h, centrifugation takes solid Object, cleaning are placed in 80 DEG C of baking ovens dry 12h, obtain iron ion exchange titanium ion pillared montmorillonite presoma.
6. the iron ion that classifying screen chooses 35~60 mesh exchanges titanium ion pillared montmorillonite presoma, it is placed in Muffle furnace It is calcined 3 hours at 500 DEG C, obtains composite sample 5.
7. pair composite sample 5 carries out identification and analysis, XRD spectra is similar to the XRD spectra of titanium pillared montmorillonite, such as schemes Shown in 1.Take the 0.1g composite sample 5 as catalyst, gas flow rate 100mL/min, corresponding air speed is 60000mL/ (gh), toluene concentration 1000mL/m3, in normal pressure, under conditions of temperature is 375 DEG C, toluene removal rate is 97%.Activity is commented Valence result is as shown in Figure 2.Verifying composite sample 5 is that the iron ion to be prepared for heat catalytic oxidation toluene is handed over as a result, Change titanium ion pillared montmorillonite catalyst.

Claims (1)

1. the iron ion exchange titanium ion pillared montmorillonite catalyst for heat catalytic oxidation toluene is in heat catalytic oxidation toluene side The application in face,
The iron ion exchange titanium ion pillared montmorillonite catalyst for heat catalytic oxidation toluene is by the following method Preparation：Using na-montmorillonite, molysite, titanium salt as raw material, na-montmorillonite is taken off by the pillared pillared illiteracy of titanium that obtains of titanium ion Stone presoma obtains titanium pillared montmorillonite after calcining, and then exchanges titanium pillared montmorillonite, synthesis iron ion exchange with iron ion Titanium ion pillared montmorillonite presoma, washed, dry, sieving, calcining be prepared the iron for heat catalytic oxidation toluene from Son exchange titanium ion pillared montmorillonite catalyst；It is described using na-montmorillonite, molysite, titanium salt as raw material, na-montmorillonite Titanium pillared montmorillonite presoma is obtained by the way that titanium ion is pillared, titanium pillared montmorillonite is obtained after calcining, is then handed over iron ion Titanium pillared montmorillonite is changed, synthesis iron ion exchange titanium ion pillared montmorillonite presoma is at 60 DEG C, and titanium ion solution is added In montmorillonite suspension, montmorillonite suspension Tu Shui ratio is 1g:100ml, the pillared amount of titanium is 5mmol/g montmorillonite, solid after reaction Liquid separation obtains titanium pillared montmorillonite presoma after taking solid dry, and it is pillared that titanium pillared montmorillonite presoma obtains titanium after calcining Montmorillonite, then exchanges titanium pillared montmorillonite with iron ion, and iron concentration 0.05M obtains iron ion exchange titanium ion column Support montmorillonite presoma；The pillared temperature of the titanium ion is 60 DEG C, and the pillared time is that for 24 hours, iron ion swap time is 6h；
The molysite is Fe (NO3)3·9H2O, the titanium salt are TiCl4；
The drying is dry in 80 DEG C of blowing-type drying boxes；
The sieving, calcining are the particles that the sample after drying is filtered out to 35~60 mesh, are roasted at 500 DEG C in Muffle furnace Oxidation 3 hours obtains exchanging titanium ion pillared montmorillonite catalyst for the iron ion of heat catalytic oxidation toluene.
CN201510560923.7A 2015-09-02 2015-09-02 A kind of iron ion exchange titanium ion pillared montmorillonite catalyst and preparation method thereof for heat catalytic oxidation toluene Expired - Fee Related CN105170152B (en)

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CN108502894B (en) * 2018-04-23 2020-09-25 中国科学院广州地球化学研究所 Rapid ion exchange method, reduced-charge clay mineral and preparation method thereof
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