CN106391131B - The preparation method of auto-exhaust catalyst - Google Patents

The preparation method of auto-exhaust catalyst Download PDF

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CN106391131B
CN106391131B CN201610740023.5A CN201610740023A CN106391131B CN 106391131 B CN106391131 B CN 106391131B CN 201610740023 A CN201610740023 A CN 201610740023A CN 106391131 B CN106391131 B CN 106391131B
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powder
preparation
auto
suspension
catalyst
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CN106391131A (en
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谷鹏
卢利平
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Henan Polytechnic Institute
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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
    • B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
    • B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
    • B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
    • 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
    • B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
    • B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
    • B01D53/9445—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC]
    • B01D53/945—Simultaneously removing carbon monoxide, hydrocarbons or nitrogen oxides making use of three-way catalysts [TWC] or four-way-catalysts [FWC] characterised by a specific catalyst
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/10—Noble metals or compounds thereof
    • B01D2255/102—Platinum group metals
    • B01D2255/1023—Palladium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/70—Non-metallic catalysts, additives or dopants
    • B01D2255/705—Ligands for metal-organic catalysts

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Catalysts (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)

Abstract

The invention discloses a kind of preparation methods of auto-exhaust catalyst, include the following steps: zirconium oxide, cerium oxide, nickel powder and lanthanum powder, manganese oxide mixing and ball milling by mass fraction, then alumina powder is added and continues ball milling, after ball milling, gained composite powder is blended with nano-titania particle dispersion liquid, after being heated to water whole evaporation, with activated carbon fibre, chitosan/Cu2O suspension mixes in proportion, obtains suspension；Gained suspension is added drop-wise in NaOH solution, resulting brick-red gelled pill is placed in the solution by preparations such as palladium chlorides, is taken out, solidification separates gained gel ball, and washing to neutrality is dry.Gained catalyst of the invention has very strong absorption and degradation capability, is added to nickel, lanthanum and manganese and the activity of catalyst is improved；Pass through chitosan/Cu2The addition of O suspension, nano-titanium dioxide etc. considerably increases the purifying property of gained catalyst, and regenerates conveniently, reduces costs.

Description

The preparation method of auto-exhaust catalyst
Technical field
The present invention relates to car tail gas purificant fields, and in particular to a kind of preparation method of auto-exhaust catalyst.
Background technique
With the increase of car ownership, CO, HC, NOX that automobile is discharged into atmosphere are more and more.Currently, many states Family takes stringent control emission measure to motor vehicle exhaust emission.Therefore the processing of vehicle exhaust has become important Project.It in the prior art, is to be realized by installing catalytic cleaner additional to the control of motor vehicle exhaust emission, and catalytic cleaner Key be catalyst.Catalyst generallys use three-decker and is made of active component, washcoat and carrier.From rare earth calcium Titanium ore oxide (PTO) is for since its position A, B can replace and having generated Lacking oxygen, while such is urged since tail gas catalyzed Agent has biggish price advantage to noble metal catalyst, so that such catalyst becomes the hot spot of research.But it is existing single The PTO catalytic performance of component is bad, stability is poor, is not able to satisfy increasingly serious motor vehicle exhaust emission pollution.
Summary of the invention
To solve the above problems, the present invention provides a kind of preparation method of auto-exhaust catalyst, gained is tail gas catalyzed Agent performance is stablized, good tail gas purification effect.
To achieve the above object, the technical scheme adopted by the invention is as follows:
The preparation method of auto-exhaust catalyst, includes the following steps:
S1, mass fraction is pressed by zirconium oxide, cerium oxide, nickel powder and lanthanum powder, manganese oxide mixing and ball milling, aluminium oxide is then added Powder continues ball milling, obtains composite powder；
S2, it 1-10 parts of nano-titanium dioxides is weighed is scattered in pure water by supersonic oscillations equipment and form inorganic nano Particle dispersion；
S3, dispersion liquid is blended as liquid feeding pump injection high-speed mixer composite powder with obtained by, it is complete is heated to water Portion's evaporation, obtains powder；
S4, gained powder and 1-10 parts of activated carbon fibre are put into homogenization machine stirring 27-37min, it is poly- with 30-50 parts of shells Sugar/Cu25-30min is mixed in O suspension, obtains mixing suspension；
S5, above-mentioned suspension is drawn with 10mL syringe and is added drop-wise to 50mL, 2.0molL dropwise-1NaOH solution in, Generate brick-red gelled pill；
S6, resulting brick-red gelled pill is placed in and is prepared by palladium chloride, ammonium hydroxide, EDTA, hydrazine hydrate and deionized water Solution in, impregnate 2min after, take out, solidification for 24 hours, obtain gel ball；
S7, gained gel ball is separated, is washed with distilled water, until it is neutral, it is then dried in vacuo for 24 hours, must urge at 60 DEG C Agent.
Preferably, the time of the mixing and ball milling is 33-47h, drum's speed of rotation 180-220r/min, ratio of grinding media to material 5-7: 1。
Preferably, the time of the ball milling is 17-33h, drum's speed of rotation 160-200r/min, ratio of grinding media to material 5-7: 1.
Preferably, the chitosan/Cu2O suspension is as obtained by following steps preparation:
By Cu2O nanoparticle is proportionally added into the chitosan-acetic acid solution that mass fraction is 2%, ultrasonic wave dispersion 10min obtains finely dispersed suspension.
Preferably, Cu2The mass ratio for the chitosan-acetic acid solution that O and mass fraction are 2% is 3: 1-5: 1.
Preferably, homogenization machine revolving speed is 13-17r/min in the step S4.
Preferably, zirconium oxide accounts for 3-8wt% in the composite powder, and cerium oxide accounts for 13-21wt%, and nickel accounts for 2-4wt%, lanthanum 1-3wt%, manganese oxide 2-3% are accounted for, surplus is aluminium oxide.
The invention has the following advantages:
Gained catalyst has very strong absorption and degradation capability, is added to nickel, lanthanum and manganese and the active of catalyst is obtained To improvement；Pass through chitosan/Cu2The addition of O suspension, nano-titanium dioxide etc. considerably increases the purification of gained catalyst Performance, and regenerate conveniently, it reduces costs.
Specific embodiment
In order to which objects and advantages of the present invention are more clearly understood, the present invention is carried out with reference to embodiments further It is described in detail.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to limit this hair It is bright.
Chitosan/Cu used in following embodiment in following embodiment2O suspension prepares institute by following steps : by Cu2O nanoparticle is proportionally added into the chitosan-acetic acid solution that mass fraction is 2%, and ultrasonic wave disperses 10min, Obtain finely dispersed suspension, wherein Cu2The mass ratio for the chitosan-acetic acid solution that O and mass fraction are 2% is 3: 1-5: 1. The time of mixing and ball milling is 33-47h, drum's speed of rotation 180-220r/min, ratio of grinding media to material 5-7: 1；The time of ball milling is 17- 33h, drum's speed of rotation 160-200r/min, ratio of grinding media to material 5-7: 1.
Embodiment 1
The preparation method of auto-exhaust catalyst, includes the following steps:
S1, mass fraction is pressed by zirconium oxide, cerium oxide, nickel powder and lanthanum powder, manganese oxide mixing and ball milling, aluminium oxide is then added Powder continues ball milling, obtains composite powder；Zirconium oxide accounts for 3wt% in the composite powder, and cerium oxide accounts for 21wt%, and nickel accounts for 2wt%, Lanthanum accounts for 1wt%, manganese oxide 2%, and surplus is aluminium oxide；
S2, it weighs 1 part of nano-titanium dioxide and is scattered in pure water by supersonic oscillations equipment and form inorganic nano-particle Sub- dispersion liquid；
S3, dispersion liquid is blended as liquid feeding pump injection high-speed mixer composite powder with obtained by, it is complete is heated to water Portion's evaporation, obtains powder；
S4, gained powder and 1 part of activated carbon fibre are put into homogenization machine stirring 27-37min, homogenization machine revolving speed is 13- 17r/min, with 30 parts of chitosan/Cu25-30min is mixed in O suspension, obtains mixing suspension；
S5, above-mentioned suspension is drawn with 10mL syringe and is added drop-wise to 50mL, 2.0molL dropwise-1NaOH solution in, Generate brick-red gelled pill；
S6, resulting brick-red gelled pill is placed in and is prepared by palladium chloride, ammonium hydroxide, EDTA, hydrazine hydrate and deionized water Solution in, impregnate 2min after, take out, solidification for 24 hours, obtain gel ball；
S7, gained gel ball is separated, is washed with distilled water, until it is neutral, it is then dried in vacuo for 24 hours, must urge at 60 DEG C Agent.
Embodiment 2
The preparation method of auto-exhaust catalyst, includes the following steps:
S1, mass fraction is pressed by zirconium oxide, cerium oxide, nickel powder and lanthanum powder, manganese oxide mixing and ball milling, aluminium oxide is then added Powder continues ball milling, obtains composite powder；Zirconium oxide accounts for 8wt% in the composite powder, and cerium oxide accounts for 13wt%, and nickel accounts for 2wt%, Lanthanum accounts for 1wt%, manganese oxide 2%, and surplus is aluminium oxide；
S2, it 10 parts of nano-titanium dioxides is weighed is scattered in pure water by supersonic oscillations equipment and form inorganic nano-particle Sub- dispersion liquid；
S3, dispersion liquid is blended as liquid feeding pump injection high-speed mixer composite powder with obtained by, it is complete is heated to water Portion's evaporation, obtains powder；
S4, gained powder and 10 parts of activated carbon fibre are put into homogenization machine stirring 27-37min, homogenization machine revolving speed is 13- 17r/min, with 50 parts of chitosan/Cu25-30min is mixed in O suspension, obtains mixing suspension；
S5, above-mentioned suspension is drawn with 10mL syringe and is added drop-wise to 50mL, 2.0molL dropwise-1NaOH solution in, Generate brick-red gelled pill；
S6, resulting brick-red gelled pill is placed in and is prepared by palladium chloride, ammonium hydroxide, EDTA, hydrazine hydrate and deionized water Solution in, impregnate 2min after, take out, solidification for 24 hours, obtain gel ball；
S7, gained gel ball is separated, is washed with distilled water, until it is neutral, it is then dried in vacuo for 24 hours, must urge at 60 DEG C Agent.
Embodiment 3
The preparation method of auto-exhaust catalyst, includes the following steps:
S1, mass fraction is pressed by zirconium oxide, cerium oxide, nickel powder and lanthanum powder, manganese oxide mixing and ball milling, aluminium oxide is then added Powder continues ball milling, obtains composite powder；Zirconium oxide accounts for 5.5wt% in the composite powder, and cerium oxide accounts for 17wt%, and nickel accounts for 3wt%, lanthanum account for 2wt%, manganese oxide 2.5%, and surplus is aluminium oxide；
S2, it 5.5 parts of nano-titanium dioxides is weighed is scattered in pure water by supersonic oscillations equipment and form inorganic nano Particle dispersion；
S3, dispersion liquid is blended as liquid feeding pump injection high-speed mixer composite powder with obtained by, it is complete is heated to water Portion's evaporation, obtains powder；
S4, gained powder and 5.5 parts of activated carbon fibre are put into homogenization machine stirring 27-37min, homogenization machine revolving speed is 13-17r/min, with 40 parts of chitosan/Cu25-30min is mixed in O suspension, obtains mixing suspension；
S5, above-mentioned suspension is drawn with 10mL syringe and is added drop-wise to 50mL, 2.0molL dropwise-1NaOH solution in, Generate brick-red gelled pill；
S6, resulting brick-red gelled pill is placed in and is prepared by palladium chloride, ammonium hydroxide, EDTA, hydrazine hydrate and deionized water Solution in, impregnate 2min after, take out, solidification for 24 hours, obtain gel ball；
S7, gained gel ball is separated, is washed with distilled water, until it is neutral, it is then dried in vacuo for 24 hours, must urge at 60 DEG C Agent.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art For member, without departing from the principle of the present invention, it can also make several improvements and retouch, these improvements and modifications are also answered It is considered as protection scope of the present invention.

Claims (7)

1. the preparation method of auto-exhaust catalyst, which comprises the steps of:
S1, by mass fraction by zirconium oxide, cerium oxide, nickel powder and lanthanum powder, manganese oxide mixing and ball milling, be then added alumina powder after Continuous ball milling, obtains composite powder；
S2, it 1-10 parts of nano-titanium dioxides is weighed is scattered in pure water by supersonic oscillations equipment and form inorganic nano-particle Dispersion liquid；
S3, dispersion liquid is blended as liquid feeding pump injection high-speed mixer composite powder with obtained by, is heated to water and all steams Hair, obtains powder；
S4, gained powder be put into homogenization machine with 1-10 part of activated carbon fibre stir 27-37min, with 30-50 parts of chitosans/ Cu25-30min is mixed in O suspension, obtains mixing suspension；
S5, above-mentioned suspension is drawn with 10mL syringe and is added drop-wise to 50mL, 2.0molL dropwise-1NaOH solution in, generate Brick-red gelled pill；
S6, resulting brick-red gelled pill is placed in by the molten of palladium chloride, ammonium hydroxide, EDTA, hydrazine hydrate and deionized water preparation In liquid, after impregnating 2min, take out, solidification for 24 hours, obtains gel ball；
S7, gained gel ball is separated, is washed with distilled water, until it is neutral, it is then dried in vacuo at 60 DEG C for 24 hours, obtains catalyst.
2. the preparation method of auto-exhaust catalyst as described in claim 1, which is characterized in that the time of the mixing and ball milling For 33-47h, drum's speed of rotation 180-220r/min, ratio of grinding media to material 5-7: 1.
3. the preparation method of auto-exhaust catalyst as described in claim 1, which is characterized in that the time of the ball milling is 17-33h, drum's speed of rotation 160-200r/min, ratio of grinding media to material 5-7: 1.
4. the preparation method of auto-exhaust catalyst as described in claim 1, which is characterized in that the chitosan/Cu2O is suspended Liquid is as obtained by following steps preparation:
By Cu2O nanoparticle is proportionally added into the chitosan-acetic acid solution that mass fraction is 2%, and ultrasonic wave disperses 10min, Obtain finely dispersed suspension.
5. the preparation method of auto-exhaust catalyst as claimed in claim 4, which is characterized in that Cu2O and mass fraction are 2% Chitosan-acetic acid solution mass ratio be 3: 1-5: 1.
6. the preparation method of auto-exhaust catalyst as described in claim 1, which is characterized in that homogenization machine in the step S4 Revolving speed is 13-17r/min.
7. the preparation method of auto-exhaust catalyst as described in claim 1, which is characterized in that aoxidized in the composite powder Zirconium accounts for 3-8wt%, and cerium oxide accounts for 13-21wt%, and nickel accounts for 2-4wt%, and lanthanum accounts for 1-3wt%, manganese oxide 2-3%, and surplus is oxidation Aluminium.
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CN109113837A (en) * 2018-08-31 2019-01-01 长春工程学院 A kind of catalysis treatment method of vehicle exhaust

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102974347A (en) * 2012-12-03 2013-03-20 南京大学 Method for preparing copper-based nano-catalyst with different valence states
CN104722281A (en) * 2015-03-30 2015-06-24 上海师范大学 Nano titanium dioxide/chitosan three-dimensional porous composite material and preparation method thereof
CN105688905A (en) * 2016-04-27 2016-06-22 柳州申通汽车科技有限公司 Preparation technology of automobile exhaust catalyst

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102974347A (en) * 2012-12-03 2013-03-20 南京大学 Method for preparing copper-based nano-catalyst with different valence states
CN104722281A (en) * 2015-03-30 2015-06-24 上海师范大学 Nano titanium dioxide/chitosan three-dimensional porous composite material and preparation method thereof
CN105688905A (en) * 2016-04-27 2016-06-22 柳州申通汽车科技有限公司 Preparation technology of automobile exhaust catalyst

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