CN109647430A - A kind of three-way catalyst and the preparation method and application thereof - Google Patents
A kind of three-way catalyst and the preparation method and application thereof Download PDFInfo
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- CN109647430A CN109647430A CN201910120436.7A CN201910120436A CN109647430A CN 109647430 A CN109647430 A CN 109647430A CN 201910120436 A CN201910120436 A CN 201910120436A CN 109647430 A CN109647430 A CN 109647430A
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/889—Manganese, technetium or rhenium
- B01J23/8892—Manganese
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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
- B01J37/0201—Impregnation
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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
- B01J37/082—Decomposition and pyrolysis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/78—Treatment of water, waste water, or sewage by oxidation with ozone
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/20—Nature of the water, waste water, sewage or sludge to be treated from animal husbandry
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
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Abstract
The present invention relates to catalyst technical fields more particularly to a kind of three-way catalyst and the preparation method and application thereof.The invention discloses a kind of preparation methods of three-way catalyst, comprising the following steps: step 1: by containing manganese compound the aqueous solution of aqueous solution, iron containing compounds and the aqueous solution of cerium-containing compound mix, obtain precursor solution；Step 2: by modified γ-Al2O3Bead is immersed in precursor solution, is then dried and is roasted respectively, obtains three-way catalyst.The preparation method uses impregnation-calcination method, easy to operate, and is attached to γ-Al with capable of making three kinds of manganese, iron and cerium metal oxide stabilities2O3Bead surface, and the catalytic activity being prepared is high, solves existing three-way catalyst preparation method complexity, and the problem that the catalytic effect being prepared is lower.
Description
Technical field
The present invention relates to catalyst technical fields more particularly to a kind of three-way catalyst and the preparation method and application thereof.
Background technique
Three-way catalyst is generally made of catalyst carrier and active constituent, and three-way catalyst is widely used in automobile at present
The processing of tail gas and exhaust system, but preparation method is complicated, and the catalytic efficiency for the three-way catalyst being prepared is lower.
Summary of the invention
The present invention provides a kind of preparation methods of three-way catalyst, and it is multiple to solve existing three-way catalyst preparation method
It is miscellaneous, and the problem that the catalytic effect that is prepared is lower.
Its specific technical solution is as follows:
The present invention provides a kind of preparation methods of three-way catalyst, comprising the following steps:
Step 1: the aqueous solution of the aqueous solution of aqueous solution, iron containing compounds containing manganese compound and cerium-containing compound is carried out
Mixing, obtains precursor solution；
Step 2: by the γ-Al of activation2O3Bead is immersed in the precursor solution, is then dried and is roasted respectively
It burns, obtains three-way catalyst.
In the present invention, the γ-Al of activation2O3Bead the preparation method comprises the following steps: by γ-Al2O3After bead is cleaned with deionized water
It is dried；Wherein, γ-Al2O3The partial size of bead is 2-3mm, and dry temperature is 65 DEG C.
In the present invention, the configuration method of precursor solution are as follows: weighed respectively by weight percentage containing manganese compound, iron content
It is dissolved in water after closing object and cerium-containing compound, is settled to 100mL after stirring.
Preferably, the manganese compound that contains is one of manganese nitrate, manganese sulfate and manganese chloride or a variety of, more preferably nitre
Sour manganese；
The iron containing compounds are one of ferric nitrate, ferrous sulfate and iron chloride or a variety of, more preferably ferric nitrate；
The cerium-containing compound is cerous nitrate and/or cerium chloride, more preferably cerous nitrate.
Preferably, in the aqueous solution containing manganese compound containing manganese compound, the iron containing compounds aqueous solution in
Iron containing compounds and the cerium-containing compound aqueous solution cerium-containing compound mass ratio be 0.4~1.6:0.3~1.3:
0.8~2.5, more preferably 1:1:1.5.In the present invention, the aqueous solution of aqueous solution, the iron containing compounds containing manganese compound and
The mass concentration of solute is respectively 0.4~1.6%, 0.3~1.3%, 0.8~2.5% in the aqueous solution of the cerium-containing compound,
Preferably 1%, 1%, 1.5%.
Preferably, the dipping successively includes: oscillation dipping and static dipping.
It is described oscillation dipping time be 12~for 24 hours, more preferably 12h, it is described oscillation dipping vibration temperature be 25 DEG C
~30 DEG C, more preferably 30 DEG C, hunting speed are 180rpm~200rpm, more preferably 180rpm；
The time of the static dipping is 12~for 24 hours, the vibration temperature of more preferably 12h, the oscillation dipping are 25 DEG C
~30 DEG C, more preferably 30 DEG C.
Preferably, the temperature of the drying is 65 DEG C~70 DEG C, more preferably 65 DEG C, time of the drying is 12~
For 24 hours, more preferably 12h.
Preferably, the temperature of the roasting is 400~700 DEG C, more preferably 400 DEG C, time of the roasting is 3~
6h, more preferably 4h.
The present invention also provides three-way catalysts made from above-mentioned preparation method.The three-way catalyst is with γ-Al2O3Bead
As carrier, manganese, iron and cerium are supported on γ-Al in the form of oxide2O3Bead surface.
Rare earth element containing special 4f track due to making it have good catalytic property, and ceria to ozone
It is that one kind has cubic fluorite oxide, hole is more, the ability of storage oxygen and oxygen release with higher, in addition to this, by
There are two kinds of valence states of trivalent and tetravalence in cerium, is easy to happen redox reaction in the reaction, makes the oxygen in lattice in conversion process
It is detached from and forms oxygen vacancies, promote the generation of HO.Manganese and iron are transition metal, cheap compared with noble metal, therefore, the ternary
Its preparation cost is lower while catalyst is high-efficient.
γ-Al2O3Bead is a kind of porous material, and advantage has large specific surface area, activity height, adsorption capacity strong, pressure-resistant
Property is good.Compared with homogeneous catalysis ozonisation, heterogeneous catalysis ozonation technique is in addition to can more efficiently decompose O3Generate HO
Outside, metal oxide catalyst exists in solid form, and property is stablized, and metal ion hardly dissolves out, have high catalytic efficiency,
Easily separated, high recycling rate.The present invention is metal oxide supported in γ-Al by three kinds2O3Bead carrier surface increases load
The active site in body surface face, metal oxide and γ-Al2O3Bead synergistic effect, increases the catalysis ozone ability of catalyst.
The present invention also provides a kind of methods for handling milk cattle cultivating waste water, comprising the following steps:
The milk cattle cultivating wastewater pH is adjusted to alkalinity, above-mentioned three-way catalyst is then sequentially added and ozone carries out instead
It answers.
Pollutant in milk cattle cultivating waste water is mainly organic matter, suspended matter, nitrogen, phosphorus, deposit and pathogenic bacteria etc., and companion
Foul smelling, pollutant concentration are up to the decades of times of common sanitary sewage.In waste collection, storage, transport and land use phase
Between all there may be pollution, if processing it is mishandling water body, atmosphere, soil and human health will be caused greatly threaten with
Harm, brings huge negative effect to the sustainable development of aquaculture itself.
Currently, the technology of processing milk cattle cultivating waste water mainly has returning to the field technology, ecological reestablishment and biochemical processing.
Since milk cattle cultivating waste water is high concentrated organic wastewater, domestic and international advanced experience and latest notion should be combined by handling it,
Adaptation to local conditions, because of water suiting measures to different conditions.Although biological treatment is low in cost, it is able to satisfy the processing of most of animal farm wastewater, for
The practical milk cattle cultivating waste water of different regions, wherein the organic matter contained has multiple phenyl ring, property is stablized, traditional processing work
Skill effect is poor, and aerobic tank is discharged COD and coloration is still higher, is unable to qualified discharge.
In the present invention, pH value is 9~10；Milk cattle cultivating waste water is the water outlet of certain milk cattle cultivating waste water aerobic pond, is practical useless
The mixed system of water, appearance are in brownish red, and COD is 400~500mg/L, include a variety of bio-refractories such as phenyl ring, polyatomic phenol
Substance.
The present invention for the first time applies three-way catalyst in processing milk cattle cultivating waste water, and in the present invention, three-way catalyst is logical
Cross manganese, iron, cerium oxide load, play concerted catalysis effect, wherein ceria is that a kind of have cubic fluorite oxygen
Compound, hole is more, the ability of storage oxygen and oxygen release with higher, in addition to this, since Ce has two kinds of valences of trivalent and tetravalence
State is easy to happen redox reaction in the reaction, is detached from the oxygen in lattice in conversion process and forms oxygen vacancies, promotes
The generation of HO, three kinds of oxides can generate surface hydroxyl in water, to generate hydroxyl radical free radical with ozone reaction, cause
Free chain reaction, so that the degradation capability to the organic matter of bio-refractory is improved, the increase of hydroxyl radical free radical in system
There is the outputted aerobic water effect to degradation milk cattle cultivating waste water to significantly improve.
Preferably, the mass ratio of the volume of the milk cattle cultivating waste water and the three-way catalyst is 4L/20g~4L/
80g, more preferably 4L/20g.
Preferably, the dosage of the ozone is 11.25mgL-1·min-1~18.75mgL-1·min-1, more preferably
For 11.25mgL-1·min-1。
Preferably, the time of the reaction is 20min~60min, more preferably 20min.
As can be seen from the above technical solutions, the invention has the following advantages that
The present invention provides a kind of preparation method of three-way catalyst, which uses impregnation-calcination method, operation letter
It is single, and it is attached to γ-Al while three kinds of manganese, iron and cerium metal oxide stabilities can be made2O3Bead surface, and three be prepared
First catalyst activity is high, and compared with unit and binary catalyst, load effect is strengthened, and is mainly manifested in abundant and increases
The active point for having added original carrier surface plays concerted catalysis effect, this three by the load of the oxide of manganese, iron and cerium
First catalyst is heterogeneous catalysis, is easily separated with reaction solution, reusable, and the catalyst is without precious metal, cost
It is lower, steadily in the long term, so that the proportion of goods damageds are low, can be avoided and cause secondary pollution to environment.The three-way catalyst is applied and is being located
It manages in milk cow waste water, the coloration and COD of milk cattle cultivating waste water can be substantially reduced.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention without any creative labor, may be used also for those of ordinary skill in the art
To obtain other attached drawings according to these attached drawings.
Fig. 1 is effect picture of the different catalysts that provide of the embodiment of the present invention 2 to wastewater COD removal rate；
Fig. 2 is effect picture of the different catalysts that provide of the embodiment of the present invention 2 to waste water clearance rate；
Fig. 3 is the effect after the three-way catalyst that the embodiment of the present invention 1 provides is reused 10 times to wastewater COD removal rate
Figure.
Specific embodiment
It in order to make the invention's purpose, features and advantages of the invention more obvious and easy to understand, below will be to of the invention real
The technical solution applied in example is clearly and completely described, it is clear that the embodiments described below are only present invention a part
Embodiment, and not all embodiment.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creation
Property labour under the premise of all other embodiment obtained, shall fall within the protection scope of the present invention.
Embodiment 1
The present embodiment is the preparation of three-way catalyst.
Specific step is as follows:
(1) carrier is chosen: choosing the γ-Al of partial size 2-3mm2O3Bead is as catalyst carrier, γ-Al2O3Bead is chosen
In Jiangsu Sanji Industry Co., Ltd..
(2) support-activated: by γ-Al2O3Bead is cleaned with deionized water, after be put in baking oven, under conditions of 65 DEG C do
It is dry.
(3) three-way catalyst catalyst preparation: is prepared by impregnation-calcination method, comprising the following steps:
1) presoma maceration extract configure: take concentration be respectively the aqueous solution of 1% manganese nitrate, 1% ferric nitrate aqueous solution and
The aqueous solution of 1.5% cerous nitrate, is dissolved in distilled water, is sufficiently stirred, and forms presoma maceration extract after being settled to 100mL；
2) it impregnates: by 20g γ-Al2O3Bead immerses in presoma maceration extract, impregnates respectively through oscillation dipping and static state,
Middle oscillation dipping is 12h, oscillating condition are as follows: vibration temperature is 30 DEG C, hunting speed 180rpm；Static state dipping 12h, static item
Part are as follows: placed under conditions of 30 DEG C.Make Metal Supported in γ-Al2O3Bead surface；
3) dry: to filter off maceration extract, take out catalyst and put it into dry 12h in the baking oven that temperature is 65 DEG C；
4) it roasts: after the catalyst after drying is placed in crucible, being put in the Muffle kiln roasting 4h that temperature is 400 DEG C, roasting
Three-way catalyst is obtained after burning.
The present embodiment three-way catalyst γ-Al2O3Bead surface is at rufous and is mixed with black, illustrates metal oxide
It has been supported on bead surface.
Comparative example 1
This comparative example is the preparation of binary catalyst, this comparative example difference from Example 1 is only that presoma impregnates
The raw material of liquid is manganese nitrate and cerous nitrate.
Embodiment 2
The present embodiment uses the three-way catalyst of embodiment 1, the binary catalyst of comparative example 1, γ-Al2O3Bead is located respectively
Milk cattle cultivating waste water is managed, to be only passed through ozone as blank control.
PH to 9 is adjusted, takes the level-one outputted aerobic water of four groups of 4L milk cattle cultivating waste water, it is public which is taken at the magnificent milk in Guangzhou
It takes charge of in (Green Dragon base), 20g three-way catalyst, binary catalyst, γ-Al is added in three groups of water2O3Bead, then four groups of difference
It is passed through ozone, ozone dosage 11.25mgL-1·min-1, reaction time 20min.
Embodiment 3
The present embodiment is separately sampled when 2 reaction time of embodiment is 0min, 5min, 10min, 15min, 20min, uses
Ultraviolet spectrophotometer method measures waste water COD, calculates the COD removal rate of waste water, using the coloration of extension rate method measurement waste water.
Measurement result is as shown in Figure 1 and Figure 2.
As seen from Figure 1, when handling practical milk cattle cultivating waste water, contain due to being complex system, and wherein
More bio-refractory organic matter, the effect relative to unitary system have significant difference.But with the experiment of independent ozone and independent load
The experiment of body catalytic ozonation is compared, and the catalyst of carried metal shows significant COD removal rate, and loads three-way catalyst
COD removal rate is better than binary catalyst, removal rate 45%.As shown in figure 3, right after reusing the three-way catalyst 10 times
COD removal rate is being 42%, is still able to maintain good catalytic efficiency.
As seen from Figure 2, ozone has remarkable effect to the color removal of waste water, and four groups reflect higher coloration and go
Except rate.By being measured with extension rate method to each water sample coloration, independent ozone, independent carrier catalysis ozone oxidation, two
The chroma removal rate of first catalyst ozone oxidation and catalytic ozone oxidation respectively reached 75%, 80%,
97.5%, 97.5%.It is positively correlated as it can be seen that being formed with COD removal rate, the catalyst of carried metal is compared to independent ozone and individually
Carrier catalysis ozonisation, shows better effect.
In conclusion practical milk cow wastewater degradation COD and color of the three-way catalyst for catalytic ozonation mixed system
Degree shows good removal effect.
The above, the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although referring to before
Stating embodiment, invention is explained in detail, those skilled in the art should understand that: it still can be to preceding
Technical solution documented by each embodiment is stated to modify or equivalent replacement of some of the technical features；And these
It modifies or replaces, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (10)
1. a kind of preparation method of three-way catalyst, which comprises the following steps:
Step 1: by containing manganese compound the aqueous solution of aqueous solution, iron containing compounds and the aqueous solution of cerium-containing compound mix
It closes, obtains precursor solution；
Step 2: by modified γ-Al2O3Bead is immersed in the precursor solution, is then dried and is roasted respectively, obtains
To three-way catalyst.
2. preparation method according to claim 1, which is characterized in that it is described containing manganese compound be manganese nitrate, manganese sulfate and
One of manganese chloride is a variety of；
The iron containing compounds are one of ferric nitrate, ferrous sulfate and iron chloride or a variety of；
The cerium-containing compound is cerous nitrate and/or cerium chloride.
3. preparation method according to claim 2, which is characterized in that contain manganese in the aqueous solution containing manganese compound
Close the cerium-containing compound of the aqueous solution of the iron containing compounds and the cerium-containing compound in the aqueous solution of object, the iron containing compounds
Mass ratio be 0.4~1.6:0.3~1.3:0.8~2.5.
4. preparation method according to claim 1, which is characterized in that the dipping successively includes: oscillation dipping and static state
Dipping；
The time of the oscillation dipping is 12h~for 24 hours, and the vibration temperature of the oscillation dipping is 25 DEG C~30 DEG C, hunting speed
For 180rpm~200rpm；
The time of the static dipping is 12h~for 24 hours, and the vibration temperature of the oscillation dipping is 25 DEG C~30 DEG C.
5. preparation method according to claim 1, which is characterized in that the temperature of the roasting is 400 DEG C~700 DEG C, institute
The time for stating roasting is 3h~6h.
6. three-way catalyst made from preparation method described in claim 1 to 5 any one.
7. a kind of method for handling milk cattle cultivating waste water, which comprises the following steps:
The milk cattle cultivating wastewater pH is adjusted to alkalinity, then sequentially add three-way catalyst and ozone described in claim 6 into
Row reaction.
8. the method according to the description of claim 7 is characterized in that the volume of the milk cattle cultivating waste water and the three-element catalytic
The mass ratio of agent is 4L/20g~4L/80g.
9. the method according to the description of claim 7 is characterized in that the dosage of the ozone is 11.25mgL-1·min-1
~18.75mgL-1·min-1。
10. the method according to the description of claim 7 is characterized in that the time of the reaction is 20min~60min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111889108A (en) * | 2020-07-15 | 2020-11-06 | 格丰环保科技有限公司 | Catalyst material for oxidative decomposition of organic matters in wastewater and preparation method thereof |
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| CN103240111A (en) * | 2013-05-03 | 2013-08-14 | 东南大学 | Structured catalyst for treating printing and dyeing wastewater and preparation method thereof |
| CN105363465A (en) * | 2015-07-07 | 2016-03-02 | 博天环境集团股份有限公司 | Preparation method of ozone oxidation catalyst loaded with polymetallic oxide |
| CN106268783A (en) * | 2016-07-19 | 2017-01-04 | 中国矿业大学 | Mn Ce/Al2o3the preparation of catalyst and the method for catalytic ozonation organic wastewater with difficult degradation thereby |
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2019
- 2019-02-18 CN CN201910120436.7A patent/CN109647430A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103240111A (en) * | 2013-05-03 | 2013-08-14 | 东南大学 | Structured catalyst for treating printing and dyeing wastewater and preparation method thereof |
| CN105363465A (en) * | 2015-07-07 | 2016-03-02 | 博天环境集团股份有限公司 | Preparation method of ozone oxidation catalyst loaded with polymetallic oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111889108A (en) * | 2020-07-15 | 2020-11-06 | 格丰环保科技有限公司 | Catalyst material for oxidative decomposition of organic matters in wastewater and preparation method thereof |
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