CN106179325A - A kind of tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene and preparation method thereof - Google Patents
A kind of tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene and preparation method thereof Download PDFInfo
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- CN106179325A CN106179325A CN201610508494.3A CN201610508494A CN106179325A CN 106179325 A CN106179325 A CN 106179325A CN 201610508494 A CN201610508494 A CN 201610508494A CN 106179325 A CN106179325 A CN 106179325A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/32—Manganese, technetium or rhenium
- B01J23/34—Manganese
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
- B01J37/031—Precipitation
- B01J37/035—Precipitation on carriers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/06—Washing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
- B01D2257/7027—Aromatic hydrocarbons
Abstract
The invention discloses a kind of tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene and preparation method thereof.The present invention originates using manganese salt as metallic element, carbamide is as precipitant, the kieselguhr that pickling purifies is as carrier, use deposition-precipitation method synthesis tripolite loading Mn oxide type presoma, the most scrubbed, it is dried, tabletting, broken, screening, roasting prepares the tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene.It can effectively be catalyzed the toluene (>=1000ppm) of oxidation of high density, and time more than 350 DEG C, clearance reaches more than 90%；Have that catalysis activity is high, initiation temperature is low, non-secondary pollution and the advantage such as with low cost, it is adaptable to the purified treatment of industrial waste gas middle and high concentration toluene.
Description
Technical field:
The invention belongs to toluene oxidation processing technology field, be specifically related to a kind of kieselguhr for heat catalytic oxidation toluene
Supported Manganese oxide type catalyst and preparation method thereof.
Background technology:
In areas such as China Pearl River Deltas, the industry such as automobile making and maintenance, Furniture manufacture, building coating use, shoemaking
Volatile organic matter (VOCs) discharge capacity is the most surprising.It is limited to technical method or production cost, VOCs the most directly discharge.Greatly
Quantity research shows, VOCs is photochemical ozone (O3) predecessor, be also PM2.5 (or " gray haze ") composition Secondary Organic gas molten
The important predecessor of glue, and photochemical ozone (O3) it is our the most prominent air quality of facing of current and future with PM2.5
Problem.Additionally, some high toxic VOCs is attached to PM2.5 fine grained, dramatically increase the Atmospheric particulates prestige to health
The side of body.Therefore, the effectively reduction of discharging of VOCs is the important step of control atmosphere pollution.Practice have shown that, in numerous VOCs processing methods
In, the advantage of heat catalytic oxidation method seems especially prominent.Be applicable to concentration for the treatment of change greatly, the organic exhaust gas of complicated component, have
There is removal efficiency high, the advantages such as energy resource consumption is few, non-secondary pollution.
But, catalyst is the key point of heat catalytic oxidation method application.Common catalyst have noble metal catalyst (as
Pt, Ru, Au, Rh etc.) and catalyst of transition metal oxide (such as the transition metal oxides such as V, Cr, Mn, Fe, Co, Ni or compound
Oxide).The initiation temperature of noble metal catalyst is low, activity with temperature rise quickly, but expensive, deposit at high temperature because of
Distillation and run off, easily inactivate and the problem such as sintering.Catalyst of transition metal oxide have cheap, stability is strong, right
Sulfur, the advantages such as resistivity is strong of chlorine (murder by poisoning catalyst elements common in industrial waste gas).Therefore, develop inexpensive and efficient
Catalyst of transition metal oxide more has using value.
Kieselguhr is a kind of by the mineral resources formed after remains (diatom shell) accumulation and sediment of diatom biology, in China
Changbaishan area, northeast rich reserves, quality is good, has the advantages such as wide material sources, production cost be low.Diatom shell mainly one-tenth
Credit is amorphous Si O2, there is the natural macroporous/mesoporous type pore structure based on macropore and excellent physical and chemical performance be (high
Thermostability, acid resistance, low bulk density and strong adsorptivity etc.), therefore, diatom opal has been widely used as adsorbent, carrier
And filtering agent etc..Therefore select diatomite support carrying transition metal oxide to prepare the catalyst of VOCs catalysis oxidation, can rise
To increase catalyst and the contact area of VOCs, prevent the benefits such as nanoparticle agglomerates.
Summary of the invention:
First purpose of the present invention is to provide and a kind of is catalyzed that activity is high, low and with low cost the urging for heat of initiation temperature
Change tripolite loading Mn oxide type catalyst of oxidation toluene and preparation method thereof.
The preparation method of the tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene of the present invention, it is special
Levying and be, comprise the following steps: originate as metallic element using manganese salt, carbamide is made as precipitant, the kieselguhr that pickling purifies
For carrier, use deposition-precipitation synthesis tripolite loading Mn oxide type presoma, the most scrubbed, it is dried, tabletting, broken
Broken, screening, roasting prepares the tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene.
Described originate using manganese salt as metallic element, carbamide as precipitant, the kieselguhr that pickling purifies as carrier,
Using deposition-precipitation synthesis tripolite loading Mn oxide type presoma is kieselguhr manganese salt, carbamide and pickling purified
It is added to the water and is prepared as suspension, Mn in manganese salt2+With the amount that the consumption of carbamide presses material ratio for 1:10, the diatom that pickling purifies
Soil and water consumption ratio for 1g:50mL, solid-liquid separation after reaction, take solid and obtain the oxidation of tripolite loading manganese after drying through water washing
Thing type presoma, described water and amount of urea are 500:5.5～22 in mass ratio.
Described suspension, it is to react 10 hours in 90 DEG C, and period stirs.
Preferably, in described suspension, the substance withdrawl syndrome of carbamide is 0.18-0.73mol/L.
Preferably, described manganese salt is Mn (NO3)2。
The kieselguhr that described pickling purifies is prepared by the following method: kieselguhr joins 2mol/L HCl molten
In liquid, pickling is several times, then with pure water to supernatant without Cl-Residual, takes solid and obtains the diatom that pickling purifies after drying
Soil.
Preferably, described is dried, and its temperature is 80 DEG C, and drying time is more than 12 hours.
Described tabletting, broken, screening, roasting be by dried tripolite loading Mn oxide type presoma in
Maintain 15s under 10MPa, prepare flake block, screen the graininess sample that particle diameter is 0.25-0.5mm after crushing, in Muffle furnace
In roasting 2h at 400 DEG C, obtain the tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene.
A kind of tripolite loading manganese for heat catalytic oxidation toluene prepared according to above-mentioned preparation method aoxidizes
Thing type catalyst.
The tripolite loading Mn oxide type that second object of the present invention is to provide for heat catalytic oxidation toluene is catalyzed
Agent application in terms of catalysis oxidation toluene.
The tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene utilizing the present invention to prepare is granule
Shape, Mn oxide successfully loads in kieselguhr surface and hole, and manganese load capacity is 2.9-14.1%.It can effectively be catalyzed oxidation
The toluene (>=1000ppm) of high concentration, time more than 350 DEG C, clearance reaches more than 90%；There is catalysis activity height, ignition
Temperature is low, non-secondary pollution and the advantage such as with low cost, it is adaptable to the purified treatment of industrial waste gas middle and high concentration toluene.
Accompanying drawing illustrates:
Fig. 1 is the tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene prepared by embodiment 1-3
Transmission electron microscope picture, wherein a, b, c represent the tripolite loading manganese oxygen for heat catalytic oxidation toluene prepared by embodiment 1-3 respectively
Compound type catalyst, a2 is the enlarged drawing in a1 white box portion, and b2 is the enlarged drawing in b1 white box portion, and c2 is c1 white box
The enlarged drawing in portion.
Fig. 2 is the tripolite loading Mn oxide type catalyst prepared of the embodiment 1-3 first for heat catalytic oxidation toluene
Benzene clearance figure, wherein embodiment 1,2,3 represents the kieselguhr for heat catalytic oxidation toluene prepared by embodiment 1-3 respectively and bears
Carry Mn oxide type catalyst.
Fig. 3 is the tripolite loading Mn oxide type catalyst prepared of the embodiment 1-3 CO for heat catalytic oxidation toluene2
Production rate figure, wherein embodiment 1,2,3 represents the tripolite loading for heat catalytic oxidation toluene prepared by embodiment 1-3 respectively
Mn oxide type catalyst.
Detailed description of the invention:
Following example are to further illustrate the present invention rather than limitation of the present invention.
Embodiment 1:
1. weigh 30g Changbai kieselguhr, add to the 2mol/L HCl solution of 500mL, be heated to boiling, backflow
And stir 4 hours, centrifugation, repeat aforementioned acid pickling step three times, finally with pure water to supernatant without Cl-Residual, in
Dry at 80 DEG C overnight (more than 12 hours), obtain the kieselguhr that pickling purifies.
2. weigh the kieselguhr that 10g pickling purifies, 5.5g carbamide, pipette 2.1mL Mn (NO simultaneously3)2Solution (contains
The Mn of 0.00917mol2+), add 500mL H2In O, after stirring 30min under room temperature, at 90 DEG C, constant temperature stirs 10 hours.
3. the solid in step with centrifugal separation 2, obtains tripolite loading Mn oxide type presoma, washes with ultra-pure water is centrifugal
Wash 3 times, at 80 DEG C, dry overnight (more than 12 hours), obtain the tripolite loading Mn oxide type presoma being dried.
4., by dry tripolite loading Mn oxide type presoma, under being not added with any binding agent, maintain under 10MPa
15s, prepares flake block, and after simple crushing, screening particle diameter is the graininess sample of 0.25-0.5mm.
5. by step 4, the 0.25-0.5mm graininess sample of acquisition is in Muffle furnace, under air atmosphere, in 400 DEG C of roastings
Burn 2 hours, obtain composite sample 1.
6. pair composite sample 1 carries out manganese load capacity analysis, and recording element manganese load capacity by atomic absorption method is 2.9%；
Fig. 1 a1 and Fig. 1 a2 is its transmission electron microscope picture, finds that Mn oxide is successfully supported in kieselguhr surface and hole.Taking 0.2g should
Composite sample 1, as catalyst, is 30000mL/ (g h) in air speed, and toluene concentration is 1000ppm, normal pressure, toluene removal rate
And CO2Production rate is 90%, and required minimum response temperature is respectively 312 DEG C and 342 DEG C, and result is as shown in Figures 2 and 3.
Thus, checking composite sample 1 is the tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene to be prepared.
Embodiment 2:
1. weigh 30g Changbai kieselguhr, add to the 2mol/L HCl solution of 500mL, be heated to boiling, backflow
And stir 4 hours, centrifugation, repeat aforementioned acid pickling step three times, finally with pure water to supernatant without Cl-Residual, in
Dry at 80 DEG C overnight (more than 12 hours), obtain the kieselguhr that pickling purifies.
2. weigh the kieselguhr that 10g pickling purifies, 11.0g carbamide, pipette 4.2mL Mn (NO simultaneously3)2Solution (contains
The Mn of 0.0183mol2+), add 500mL H2In O, after stirring 30min under room temperature, at 90 DEG C, constant temperature stirs 10 hours.
3. the solid in step with centrifugal separation 2, obtains tripolite loading Mn oxide type presoma, washes with ultra-pure water is centrifugal
Wash 3 times, at 80 DEG C, dry overnight (more than 12 hours), obtain the tripolite loading Mn oxide type presoma being dried.
4., by dry tripolite loading Mn oxide type presoma, under being not added with any binding agent, maintain under 10MPa
15s, prepares flake block, and after simple crushing, screening particle diameter is the graininess sample of 0.25-0.5mm.
5. by step 4, the 0.25-0.5mm graininess sample of acquisition is in Muffle furnace, under air atmosphere, in 400 DEG C of roastings
Burn 2 hours, obtain composite sample 2.
6. pair composite sample 2 carries out manganese load capacity analysis, and recording element manganese load capacity by atomic absorption method is 7.6%；
Fig. 1 b1 and Fig. 1 b2 is its transmission electron microscope picture, finds that Mn oxide is successfully supported in kieselguhr surface and hole.Taking 0.2g should
Composite sample 2, as catalyst, is 30000mL/ (g h) in air speed, and toluene concentration is 1000ppm, normal pressure, toluene removal rate
And CO2Production rate is 90%, and required minimum response temperature is respectively 272 DEG C and 294 DEG C, and result is as shown in Figures 2 and 3.
Thus, checking composite sample 2 is the tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene to be prepared.
Embodiment 3:
1. weigh 30g Changbai kieselguhr, add to the 2mol/L HCl solution of 500mL, be heated to boiling, backflow
And stir 4 hours, centrifugation, repeat aforementioned acid pickling step three times, finally with pure water to supernatant without Cl-Residual, in
Dry at 80 DEG C overnight (more than 12 hours), obtain the kieselguhr that pickling purifies.
2. weigh the kieselguhr that 10g pickling purifies, 22.0g carbamide, pipette 8.4mL Mn (NO simultaneously3)2Solution (contains
The Mn of 0.0367mol2+), add 500mL H2In O, after stirring 30min under room temperature, at 90 DEG C, constant temperature stirs 10 hours.
3. the solid in step with centrifugal separation 2, obtains tripolite loading Mn oxide type presoma, washes with ultra-pure water is centrifugal
Wash 3 times, at 80 DEG C, dry overnight (more than 12 hours), obtain the tripolite loading Mn oxide type presoma being dried.
4., by dry tripolite loading Mn oxide type presoma, under being not added with any binding agent, maintain under 10MPa
15s, prepares flake block, and after simple crushing, screening particle diameter is the graininess sample of 0.25-0.5mm.
5. by step 4, the 0.25-0.5mm graininess sample of acquisition is in Muffle furnace, under air atmosphere, in 400 DEG C of roastings
Burn 2 hours, obtain composite sample 3.
6. pair composite sample 3 carries out manganese load capacity analysis, and recording element manganese load capacity by atomic absorption method is 14.1%；
Fig. 1 c1 and Fig. 1 c2 is its transmission electron microscope picture, finds that Mn oxide is successfully supported in kieselguhr surface and hole.Taking 0.2g should
Composite sample 3, as catalyst, is 30000mL/ (g h) in air speed, and toluene concentration is 1000ppm, normal pressure, toluene removal rate
And CO2Production rate is 90%, and required minimum response temperature is respectively 266 DEG C and 274 DEG C, and result is as shown in Figures 2 and 3.
Thus, checking composite sample 3 is the tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene to be prepared.
Claims (10)
1. being used for a preparation method for the tripolite loading Mn oxide type catalyst of heat catalytic oxidation toluene, its feature exists
In, comprising the following steps: originate using manganese salt as metallic element, carbamide is as precipitant, and the kieselguhr that pickling purifies is as load
Body, uses deposition-precipitation synthesis tripolite loading Mn oxide type presoma, the most scrubbed, is dried, tabletting, broken, sieve
Choosing, roasting prepares the tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene.
Preparation method the most according to claim 1, it is characterised in that described originates using manganese salt as metallic element, urine
Element is as precipitant, and the kieselguhr that pickling purifies, as carrier, uses deposition-precipitation synthesis tripolite loading Mn oxide type
Presoma is to be added to the water the kieselguhr that manganese salt, carbamide and pickling purify to be prepared as suspension, Mn in manganese salt2+With carbamide
Consumption presses the amount of material ratio for 1:10, and the kieselguhr that pickling purifies and water consumption ratio for 1g:50mL, solid-liquid separation after reaction, takes
Solid obtains tripolite loading Mn oxide type presoma after drying through water washing, and described water and amount of urea are in mass ratio
500:5.5～22.
Preparation method the most according to claim 2, it is characterised in that described suspension, it is little in 90 DEG C of reactions 10
Time, period stirring.
Preparation method the most according to claim 2, it is characterised in that the substance withdrawl syndrome of carbamide in described suspension
For 0.18-0.73mol/L.
5. according to the preparation method described in claim 1,2 or 3, it is characterised in that described manganese salt is Mn (NO3)2。
6. according to the preparation method described in claim 1,2 or 3, it is characterised in that the kieselguhr that described pickling purifies is logical
Cross prepared by following methods: kieselguhr is joined pickling in 2mol/L HCl solution several times, then supreme with pure water
Clear liquid is without Cl-Residual, takes solid and obtains the kieselguhr that pickling purifies after drying.
Preparation method the most according to claim 1, it is characterised in that described is dried, and its temperature is 80 DEG C, drying time
It it is more than 12 hours.
8. according to the preparation method described in claim 1,2 or 3, it is characterised in that described tabletting, broken, screening, roasting is
Dried tripolite loading Mn oxide type presoma is maintained 15s under 10MPa, prepares flake block, sieve after crushing
The graininess sample selecting particle diameter to be 0.25-0.5mm, in Muffle furnace, roasting 2h at 400 DEG C, obtains for heat catalytic oxidation toluene
Tripolite loading Mn oxide type catalyst.
9. the tripolite loading for heat catalytic oxidation toluene that a preparation method according to claim 1 prepares
Mn oxide type catalyst.
10. the tripolite loading Mn oxide type catalyst for heat catalytic oxidation toluene described in claim 9 is at catalysis oxygen
Change the application in terms of toluene.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107442130A (en) * | 2017-08-24 | 2017-12-08 | 中国科学院广州地球化学研究所 | A kind of palygorskite load type national standard method and its preparation method and application |
| CN109647420A (en) * | 2018-12-27 | 2019-04-19 | 中国科学院广州地球化学研究所 | Calcium analysis cobalt acid lanthanum perofskite type oxide and its preparation method and application for heat catalytic oxidation toluene |
| CN109745976A (en) * | 2019-03-05 | 2019-05-14 | 中国科学院广州地球化学研究所 | Clay mineral carried metal or metal oxide nanoparticles composite material and preparation method |
| CN109893998A (en) * | 2019-04-04 | 2019-06-18 | 南京理工大学 | It is a kind of for removing the absorption-low temperature thermocatalyst of volatile organic contaminant |
| CN114192187A (en) * | 2021-12-06 | 2022-03-18 | 内蒙古工业大学 | Coal series kaolinite-based catalyst, preparation method thereof and application thereof in toluene catalytic degradation |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107442130A (en) * | 2017-08-24 | 2017-12-08 | 中国科学院广州地球化学研究所 | A kind of palygorskite load type national standard method and its preparation method and application |
| CN109647420A (en) * | 2018-12-27 | 2019-04-19 | 中国科学院广州地球化学研究所 | Calcium analysis cobalt acid lanthanum perofskite type oxide and its preparation method and application for heat catalytic oxidation toluene |
| CN109745976A (en) * | 2019-03-05 | 2019-05-14 | 中国科学院广州地球化学研究所 | Clay mineral carried metal or metal oxide nanoparticles composite material and preparation method |
| CN109893998A (en) * | 2019-04-04 | 2019-06-18 | 南京理工大学 | It is a kind of for removing the absorption-low temperature thermocatalyst of volatile organic contaminant |
| CN114192187A (en) * | 2021-12-06 | 2022-03-18 | 内蒙古工业大学 | Coal series kaolinite-based catalyst, preparation method thereof and application thereof in toluene catalytic degradation |
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