CN109603899A - A kind of molecular sieve carried manganese oxide catalyst and preparation method thereof for heat catalytic oxidation toluene - Google Patents
A kind of molecular sieve carried manganese oxide catalyst and preparation method thereof for heat catalytic oxidation toluene Download PDFInfo
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- CN109603899A CN109603899A CN201811440916.3A CN201811440916A CN109603899A CN 109603899 A CN109603899 A CN 109603899A CN 201811440916 A CN201811440916 A CN 201811440916A CN 109603899 A CN109603899 A CN 109603899A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J29/00—Catalysts comprising molecular sieves
- B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
- B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
- B01J29/08—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y
- B01J29/16—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof of the faujasite type, e.g. type X or Y containing arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- 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
- B01D53/864—Removing carbon monoxide or hydrocarbons
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Abstract
The present invention discloses a kind of molecular sieve carried manganese oxide catalyst and preparation method thereof for being used to prepare heat catalytic oxidation toluene, using potassium permanganate and manganese nitrate as the metallic element source of catalyst, it is load with molecular sieve, under the conditions of existing for the template, utilize the redox reaction of potassium permanganate and manganese nitrate, manganese oxide is deposited in molecular sieve surface, after by washing, drying, calcination, the molecular sieve carried manganese oxide catalyst for heat catalytic oxidation toluene is prepared；The template is polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer.At 255 DEG C, the advantages that air speed 45000mL/ (gh) has reached 90% or more to the conversion ratio of toluene (>=200ppm), and catalytic activity is high, preparation method is simple, low in cost, it can be used for the fields such as industry and environmental improvement.
Description
Technical field
The present invention is related to the preparation of molecular sieve carried manganese oxide catalyst a kind of and answers for industry and environmental catalysis field
Use method.
Background technique
With the development of economy, have become public one of concern the most the problems such as environmental pollution.In industry
VOCs mostlys come from exhaust gas discharge, solvent volatilization, the burning of combustible etc., very big to the destruction of environment, while to people
Body also has very big harm.Toluene is as a kind of common VOC, due to its in the industry commonly used, so toluene
Volatilization is particularly important with control.Therefore, developing a kind of pair of toluene has the catalyst of preferable adsorption capacity and catalytic performance tool
It is of great significance.
Molecular sieve has well as a kind of common adsorbent and catalyst carrier in the absorption and catalysis to toluene
Application prospect.Meanwhile high activity and its preferable economy that transition metal element is shown in toluene catalytically, so for example
The transition metal elements such as manganese have extensive research and application in the catalysis of toluene.In current research, molecular sieve carried manganese is urged
For agent mainly using infusion process, the efficiency of this method is lower, and load capacity is not answered excessive, will lead to the hole of molecular sieve when excessive
Road blocking, lower load capacity can not improve the active site of enough toluene catalyticallies again, therefore there are certain limitations.And mistake
The research of metallic catalyst is crossed, has already appeared the research of binary and multicomponent alloy at present, but synthesis condition is comparatively harsh, and
Product can not be to toluene into efficient absorption.
The deposition-precipitation method that Chinese patent CN106179325A is used has synthesized tripolite loading Mn catalyst, at 350 DEG C
When 90% is reached to the catalytic efficiency of toluene (>=1000ppm).
Chinese patent CN105170152A obtains titanium pillared montmorillonite presoma using titanium ion is pillared, obtains by calcination
Titanium ion pillared montmorillonite, being can achieve at 375 DEG C to toluene (>=1000ppm) catalytic efficiency is 90%.
Chinese patent CN104190435A uses manganese-cobalt alloy of two one-step hydrothermals preparation, to 1000ppm at 225 DEG C
Toluene conversion be 50%, 90% conversion ratio is more than 300 DEG C.
Hongpeng etc. reacts hydrogen ion in consumption solution with hydrogen peroxide using potassium permanganate, and the precipitation method are prepared for iron-manganese
Bianry alloy, two kinds of Elemental redistributions are uniform, and at 215 DEG C, toluene (1000ppm) conversion ratio has just reached 90%.
(Hydrolysis driving redox reaction to synthesize Mn-Fe binary oxides as
highly active catalysts for the removal of toluene[J].Chemical Engineering
Journal,2017,330.).The oxidation with bivalent manganese and ferrous iron in the solution simultaneously using potassium permanganate such as Limin Guo
Reduction reaction is also prepared for the alloy of two kinds of element good mixings, at 197 DEG C, reaches to the conversion ratio of 500ppm toluene
90%.(Enhanced Toluene Combustion over Highly Homogeneous Iron Manganese
Oxide Nanocatalysts[J].2018,1(3):1066-1075.)。
The catalytic efficiency of loaded catalyst is too low, and the preparation method of alloy-type catalyst is relatively complicated, and higher cost.
Therefore, the catalytic efficiency for improving loaded catalyst is a kind of practicable method.
Summary of the invention
The first purpose of the invention is to provide it is a kind of prepare at a low price, efficient for toluene heat catalytic oxidation catalyst and its
Preparation method.
A kind of molecular sieve carried manganese oxide catalyst being used to prepare heat catalytic oxidation toluene is load with molecular sieve,
Under the conditions of template is existing, using the redox reaction of potassium permanganate and manganese nitrate, manganese oxide is deposited in molecular sieve table
Face, after by washing, drying, calcination, obtain the molecular sieve carried manganese oxide catalyst for heat catalytic oxidation toluene.
The template is polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (abbreviation P123),
It disperses molecular sieve in deionized water, P123 is added, at a certain temperature stirring stirring, then manganese nitrate is dissolved in suspension
In, whole system is placed under certain temperature, then certain density permanganic acid solution is added dropwise until excess.
It is preferred that the whipping temp of the suspension is 90 DEG C, mixing time 1h.
It is preferred that the molecular sieve is NaX type molecular sieve.
The concentration of the molecular sieve in deionized water is 0.02g/ml~1g/ml, and the mass ratio of P123 and molecular sieve is
100:1~10:1, the concentration of liquor potassic permanganate are 0.01mol/L~0.1mol/L.
It is preferred that the drying temperature is 100 DEG C, drying time 2h or more, the calcination temperature is 300 DEG C, calcination time
For 2h or more.
The reaction temperature of the whole system is ice bath, room temperature or boiling water bath.
Second object of the present invention is to provide molecular sieve carried manganese oxide catalyst in terms of heat catalytic oxidation toluene
Application.
Prepared by the method molecular sieve carried manganese oxide catalyst particle, mesoporous manganese oxide are supported on the table of molecular sieve
Face.It can efficiently catalyzing and oxidizing toluene (200ppm), at 255 DEG C, air speed 45000mL/ (gh), to toluene (>=200ppm)
Conversion ratio reached 90% or more, the advantages that catalytic activity is high, preparation method is simple, low in cost, can be used for industry and
The fields such as environmental improvement.
Detailed description of the invention
Fig. 1 is the surface sweeping electron microscopic picture of the molecular sieve carried manganese oxide catalyst of embodiment 1-3 preparation, and wherein a, b, c divide
Catalyst prepared by embodiment 1-3 is not represented.
Fig. 2 is the surface sweeping electron microscopic picture of the standby molecular sieve carried manganese oxide catalyst of embodiment 4-6, and wherein a, b, c distinguish
Represent catalyst prepared by embodiment 4-6.
Fig. 3 is embodiment 1-3 at different temperatures to the transformation efficiency of toluene, air speed
45000mL/(g·h)
Fig. 4 is embodiment 2,4-6 at different temperatures to the transformation efficiency of toluene, air speed 45000mL/ (gh)
Specific embodiment
Embodiment 1:
2g molecular sieve is dispersed with stirring in 100ml deionized water, P123 is added, wherein the quality of P123 and molecular sieve
Than placing the beaker in water-bath, heating stirring 1h for 100:1~10:1, after its cooling, tetra- water manganese nitrate of 0.2g is added,
The potassium permanganate of 0.01mol/L~0.1mol/L is added dropwise again to excess, entire reaction carries out (25 DEG C) at room temperature.Reaction terminates
Afterwards, it filters, washing is dry in baking oven.Afterwards using Muffle furnace calcination, product is obtained.Its to air speed 45000mL/ (gh),
The catalytic efficiency of 200ppm toluene reaches 90% at 278 DEG C.
Embodiment 2:
2g molecular sieve is dispersed with stirring in 100ml deionized water, P123 is added, wherein the quality of P123 and molecular sieve
Than placing the beaker in water-bath, heating stirring 1h for 100:1~10:1, after its cooling, tetra- water manganese nitrate of 0.2g is added,
The potassium permanganate of 0.01mol/L~0.1mol/L is added dropwise again to excess, entirely reacts on progress (0 DEG C) under ice-water bath.Reaction knot
Shu Hou is filtered, and washing is dry in baking oven.Afterwards using Muffle furnace calcination, product is obtained.It is to air speed 45000mL/ (g
H), the catalytic efficiency of 200ppm toluene reaches 90% at 263 DEG C.
Embodiment 3:
2g molecular sieve is dispersed with stirring in 100ml deionized water, P123 is added, wherein the quality of P123 and molecular sieve
Than placing the beaker in water-bath, heating stirring 1h for 100:1~10:1, after its cooling, tetra- water manganese nitrate of 0.2g is added,
The potassium permanganate of 0.01mol/L~0.1mol/L is added dropwise again to excess, entirely reacts on progress (100 DEG C) under boiling water bath.Reaction
After, it filters, washing is dry in baking oven.Afterwards using Muffle furnace calcination, product is obtained.It is to air speed 45000mL/
(gh), the catalytic efficiency of 200ppm toluene reaches 90% at 270 DEG C.
Embodiment 4:
2g molecular sieve is dispersed with stirring in 100ml deionized water, P123 is added, wherein the quality of P123 and molecular sieve
Than placing the beaker in water-bath, heating stirring 1h for 100:1~10:1, after its cooling, tetra- water manganese nitrate of 0.1g is added,
The potassium permanganate of 0.01mol/L~0.1mol/L is added dropwise again to excess, entirely reacts on progress (100 DEG C) under boiling water bath.Reaction
After, it filters, washing is dry in baking oven.Afterwards using Muffle furnace calcination, product is obtained.It is to air speed 45000mL/
(gh), the catalytic efficiency of 200ppm toluene reaches 90% at 285 DEG C.
Embodiment 5:
2g molecular sieve is dispersed with stirring in 100ml deionized water, P123 is added, wherein the quality of P123 and molecular sieve
Than placing the beaker in water-bath, heating stirring 1h for 100:1~10:1, after its cooling, tetra- water manganese nitrate of 0.3g is added,
The potassium permanganate of 0.01mol/L~0.1mol/L is added dropwise again to excess, entirely reacts on progress (100 DEG C) under boiling water bath.Reaction
After, it filters, washing is dry in baking oven.Afterwards using Muffle furnace calcination, product is obtained.It is to air speed 45000mL/
(gh), the catalytic efficiency of 200ppm toluene reaches 90% at 255 DEG C.
Embodiment 6:
2g molecular sieve is dispersed with stirring in 100ml deionized water, P123 is added, wherein the quality of P123 and molecular sieve
Than placing the beaker in water-bath, heating stirring 1h for 100:1~10:1, after its cooling, tetra- water manganese nitrate of 0.5g is added,
The potassium permanganate of 0.01mol/L~0.1mol/L is added dropwise again to excess, entirely reacts on progress (100 DEG C) under boiling water bath.Reaction
After, it filters, washing is dry in baking oven.Afterwards using Muffle furnace calcination, product is obtained.It is to air speed 45000mL/
(gh), the catalytic efficiency of 200ppm toluene reaches 90% at 279 DEG C.
Claims (10)
1. a kind of molecular sieve carried manganese oxide catalyst for being used to prepare heat catalytic oxidation toluene, which is characterized in that with permanganic acid
Potassium and metallic element source of the manganese nitrate as catalyst are to load with molecular sieve, under the conditions of existing for the template, utilize height
Manganese oxide is deposited in molecular sieve surface by the redox reaction of potassium manganate and manganese nitrate, after by washing, drying, calcination, system
It is standby to obtain the molecular sieve carried manganese oxide catalyst for heat catalytic oxidation toluene；The template is poly- for polyethylene oxide-
Propylene oxide-polyethylene oxide triblock copolymer.
2. a kind of preparation method for the molecular sieve carried manganese oxide catalyst for being used to prepare heat catalytic oxidation toluene, feature exist
In it is water-soluble to be that polyethylene oxide-polypropylene oxide-polyethylene oxide three block copolymer is dispersed in for molecular sieve and template
In liquid, manganese nitrate is added in solution after stirring, then liquor potassic permanganate is added dropwise into mixed liquor, until potassium permanganate mistake
Amount；Using the redox reaction of potassium permanganate and manganese nitrate, manganese oxide is deposited in molecular sieve surface, after by washing, doing
The molecular sieve carried manganese oxide catalyst for heat catalytic oxidation toluene is prepared in dry, calcination.
3. preparation method according to claim 2, which is characterized in that the molecular sieve is MCM-41 type molecular sieve, NAX type
One or more of molecular sieve, NAY molecular sieve.
4. preparation method according to claim 2, which is characterized in that molecular sieve and polyethylene oxide-polypropylene oxide-are poly-
The mass ratio of ethylene oxide triblock copolymer is 100:1~10:1, and the concentration of molecular sieve is 0.02g/ml~1g/ in suspension
ml。
5. preparation method according to claim 2, which is characterized in that the concentration of the liquor potassic permanganate is 0.01mol/
L~1mol/L, the amount that the substance of manganese nitrate is added is 0.01mol~0.1mol.
6. the preparation method according to claim 4, which is characterized in that molecular sieve and polyethylene oxide-polypropylene oxide-are poly-
The mixed suspension of ethylene oxide triblock copolymer stirs 1h~2h at 60 DEG C~100 DEG C.
7. preparation method according to claim 2, which is characterized in that when liquor potassic permanganate is added dropwise, entire reaction exists
It is completed under ice-water bath or room temperature or boiling water bath.
8. preparation method according to claim 2, which is characterized in that the drying temperature is 100 DEG C, drying time 2h.
9. preparation method according to claim 2, which is characterized in that the calcination temperature is 300 DEG C~500 DEG C, calcination
Time is 3h~5h.
10. a kind of molecular sieve carried manganese oxide type catalyst as described in claim 1 is being used to prepare heat catalytic oxidation toluene
Application.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111841621A (en) * | 2020-07-07 | 2020-10-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of molecular sieve supported manganese oxide catalyst, product and application thereof |
| CN113941350A (en) * | 2021-10-25 | 2022-01-18 | 湖南大学 | Bone carbon supported catalyst and preparation method and application thereof |
| 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 |
| CN115253665A (en) * | 2022-07-04 | 2022-11-01 | 江苏理工学院 | Method for catalyzing and degrading VOCs and NOx by K modified OMS-2 in cooperation with low-temperature plasma |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111841621A (en) * | 2020-07-07 | 2020-10-30 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of molecular sieve supported manganese oxide catalyst, product and application thereof |
| CN113941350A (en) * | 2021-10-25 | 2022-01-18 | 湖南大学 | Bone carbon supported catalyst and preparation method and application thereof |
| CN113941350B (en) * | 2021-10-25 | 2023-04-28 | 湖南大学 | Bone carbon supported catalyst and preparation method and application thereof |
| 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 |
| CN115253665A (en) * | 2022-07-04 | 2022-11-01 | 江苏理工学院 | Method for catalyzing and degrading VOCs and NOx by K modified OMS-2 in cooperation with low-temperature plasma |
| CN115253665B (en) * | 2022-07-04 | 2023-05-30 | 江苏理工学院 | Method for degrading VOCs and NOx by K modified OMS-2 in cooperation with low-temperature plasma catalysis |
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