CN104607181B - A kind of preparation method of diesel oxidation catalyst - Google Patents
A kind of preparation method of diesel oxidation catalyst Download PDFInfo
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- CN104607181B CN104607181B CN201510019689.7A CN201510019689A CN104607181B CN 104607181 B CN104607181 B CN 104607181B CN 201510019689 A CN201510019689 A CN 201510019689A CN 104607181 B CN104607181 B CN 104607181B
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Abstract
The invention discloses a kind of diesel oxidation catalyst (DOC) preparation method, comprise the following steps:(1) citric acid and ethylene glycol are added into stirring and dissolving in deionized water, platinum nitrate aqueous solution is added into above-mentioned solution and mixed liquor is sufficiently stirred for obtaining;(2) alumina powder is added in above-mentioned mixed liquor and be well mixed, and stirring is evaporated at a certain temperature;(3) by it is above-mentioned be evaporated product dry and roasting obtain diesel oxidation catalyst (DOC).Diesel oxidation catalyst (DOC) noble metal dosage prepared by the present invention is few, initiation temperature is low.
Description
Technical field
The present invention relates to the technical field of purifying vehicle exhaust, and in particular to it is net that one kind can be applied to diesel engine vent gas catalysis
The preparation method of the catalyst in field such as change.
Background technology
With developing rapidly for automobile industry, China's diesel vehicle recoverable amount continues to increase.In exhaust emissions of diesel engine thing
Particulate matter (PM) has become one of city primary pollution source.Granular material discharged into air to prevent, effective way is to adopt
With grain catcher (DPF) come trap particulate matter.For light-duty diesel vehicle, diesel oxidation catalyst DOC+ is generally used at present
DPF technology path reduces the discharge of particulate matter.The effect of diesel oxidation catalyst (DOC) is:On the one hand oxidation is eliminated
The carbon monoxide and hydrocarbon of tail gas;On the other hand the fuel combustion of spray produces high-temperature gas after making in blast pipe, promotes
The oxidation of the particulate matter trapped on DPF is eliminated, and reaches the purpose of regeneration.Therefore, exploitation initiation temperature is low, excellent in te pins of durability
DOC catalyst is to solve the problems, such as one of key technology of dpf regeneration.
Chinese patent CN103052446A reports a kind of oxidation catalyst (DOC), with than relatively low initiation temperature, its
Heat resistance and excellent in te pins of durability.But the noble metal dosage of the oxidation catalyst is preferably 1.5~3.5g/L, large usage quantity, and newly
The initiation temperature of fresh state catalyst is still more than 180 DEG C, and the initiation temperature of the catalyst after aging is still more than 190 DEG C.
The content of the invention
It is an object of the invention to provide a kind of diesel oxidation catalyst (DOC) preparation method, to overcome existing skill
Catalyst noble metal large usage quantity (> 30g/ft in art3), the problem of initiation temperature is higher, compared with prior art, the present invention
Preparation method is simple, reduces 15-20% noble metal dosage, and the catalyst of preparation has lower initiation temperature, easily realized
Process control, is conducive to industrialized production.
In order to solve the above technical problems, the concrete technical scheme that the present invention is used is as follows:
A kind of preparation method of diesel oxidation catalyst, comprises the following steps:
Step one, citric acid and ethylene glycol are added in deionized water in stirring and dissolving at 45~55 DEG C, then added
Platinum nitrate aqueous solution obtains mixed solution after being stirred 1~2 hour at 50~60 DEG C, wherein mole of the citric acid and ethylene glycol
Than for 1:1~1:4, the total moles ratio of platinum nitrate and citric acid and ethylene glycol is 1:9~1:15;
Step 2, added into step one gained mixed solution alumina powder of the particle diameter for 100~200 mesh in 400~
Be stirred at room temperature under 600 revs/min of mixing speed 0.5~1 hour, then heat to 70~90 DEG C stirring 6~8 hours after must steam
Dry product, wherein Alpha-alumina and gama-alumina mass ratio are 1 in the alumina powder:3;
Step 3, will be evaporated in step 2 product 100~130 DEG C dry 3~5 hours, then in 500~550 DEG C
Diesel oxidation catalyst (DOC) is obtained after being calcined 2~3h under 0.3~0.5MPa nitrogen atmosphere.
The mass ratio of above-mentioned platinum nitrate and aluminum oxide is 0.006:1~0.012:1.
It ensure that noble metal platinum is golden in roasting process in preparation method step 3 of the present invention under specific nitrogen pressure
Belong to the stability of valence state, the consumption of noble metal is reduced to a certain extent.
According to another aspect of the present invention, the present invention adds the lemon of specific proportioning when platinum Supported alumina is prepared
Lemon acid and ethylene glycol, efficiently control the dispersiveness and valence distribution of noble metal platinum, can reduce the consumption of noble metal, and have
Excellent catalytic performance.
The present invention has the advantages that compared with prior art:
1. noble metal dosage used in the preparation method of diesel oxidation catalyst of the present invention is few;
2. the diesel oxidation catalyst that preparation method of the present invention is prepared has lower initiation temperature;
3. preparation is simple by the present invention, easy implementation process control, be conducive to industrialized production.
Embodiment
To make the object, technical solutions and advantages of the present invention of greater clarity, with reference to embodiment, to this
Invention is further described.It should be understood that these descriptions are merely illustrative, and it is not intended to limit the scope of the present invention.
Comparative example
2.45g platinum nitrate aqueous solutions (concentration of platinum is 15%) are added in 100.0g deionized waters and are sufficiently stirred for, so
100.0g alumina powders are added in above-mentioned mixed liquor afterwards and are well mixed, 80 DEG C are heated with stirring to until being evaporated.Finally, will be upper
State be evaporated product 100 DEG C dry 3h and 500 DEG C roasting 2h produce diesel oxidation catalyst (DOC).
Embodiment 1:
1.63g citric acids and 0.52g ethylene glycol are added in 100.0g deionized waters in stirring and dissolving at 45~55 DEG C,
2.45g platinum nitrate aqueous solutions (concentration of platinum is 15%) are added into above-mentioned solution must mix after being stirred 1 hour at 50~60 DEG C
Close solution.Then by 100.0g particle diameters for 100~200 mesh alumina powder (Alpha-alumina and γ wherein in alumina powder-
Quality of alumina ratio is 1:3) it is added in above-mentioned mixed liquor, in being stirred at room temperature 0.5 under 400~600 revs/min of mixing speed
~1 hour, it is then heated to after 70 DEG C of stirrings 7 hours until be evaporated.Finally, by the above-mentioned product that is evaporated in 100 DEG C of dry 3h, so
2h is calcined under 500 DEG C, 0.3-0.5MPa nitrogen atmospheres afterwards and produces diesel oxidation catalyst (DOC).
Embodiment 2:
1.77g citric acids and 1.14g ethylene glycol are added in 100.0g deionized waters in stirring and dissolving at 45~55 DEG C,
3.26g platinum nitrate aqueous solutions (concentration of platinum is 15%) are added into above-mentioned solution must mix after being stirred 1 hour at 50~60 DEG C
Close solution.Then by 100.0g particle diameters for 100~200 mesh alumina powder (Alpha-alumina and γ wherein in alumina powder-
Quality of alumina ratio is 1:3) it is added in above-mentioned mixed liquor, in being stirred at room temperature 0.5 under 400~600 revs/min of mixing speed
~1 hour, it is then heated to after 80 DEG C of stirrings 8 hours until be evaporated.Finally, by the above-mentioned product that is evaporated in 110 DEG C of dry 4h, so
3h is calcined under 550 DEG C, 0.3-0.5MPa nitrogen atmospheres afterwards and produces diesel oxidation catalyst (DOC).
Embodiment 3:
1.96g citric acids and 1.89g ethylene glycol are added in 100.0g deionized waters in stirring and dissolving at 45~55 DEG C,
4.08g platinum nitrate aqueous solutions (concentration of platinum is 15%) are added into above-mentioned solution must mix after being stirred 1 hour at 50~60 DEG C
Close solution.Then by 100.0g particle diameters for 100~200 mesh alumina powder (Alpha-alumina and γ wherein in alumina powder-
Quality of alumina ratio is 1:3) it is added in above-mentioned mixed liquor, in being stirred at room temperature 0.5 under 400~600 revs/min of mixing speed
~1 hour, it is then heated to after 90 DEG C of stirrings 6 hours until be evaporated.Finally, by the above-mentioned product that is evaporated in 120 DEG C of dry 5h,
500 DEG C, roasting 2h produces diesel oxidation catalyst (DOC) under 0.3-0.5MPa nitrogen atmospheres.
Embodiment 4:
2.17g citric acids and 2.80g ethylene glycol are added in 100.0g deionized waters in stirring and dissolving at 45~55 DEG C,
4.89g platinum nitrate aqueous solutions (concentration of platinum is 15%) are added into above-mentioned solution must mix after being stirred 1 hour at 50~60 DEG C
Close solution.Then by 100.0g particle diameters for 100~200 mesh alumina powder (Alpha-alumina and γ wherein in alumina powder-
Quality of alumina ratio is 1:3) it is added in above-mentioned mixed liquor, in being stirred at room temperature 0.5 under 400~600 revs/min of mixing speed
~1 hour, it is then heated to after 80 DEG C of stirrings 7 hours until be evaporated.Finally, by the above-mentioned product that is evaporated in 130 DEG C of dry 4h,
550 DEG C, roasting 3h produces diesel oxidation catalyst (DOC) under 0.3-0.5MPa nitrogen atmospheres.
Catalyst obtained by comparative example and embodiment 1-4 is tested, experimental result is as shown in table 1.
Table 1 utilizes the catalytic performance of catalyst made from the inventive method
Data as shown in Table 1 it will be apparent that, durable processing still has good at 750 DEG C after 100 hours
The expulsion rate of low temperature light-off performance and coating is greatly lowered, and can improve tolerance of the catalyst in adverse circumstances.
Although embodiments of the present invention are described in detail, it should be understood that, without departing from the present invention's
In the case of spirit and scope, embodiments of the present invention can be made with various changes, replace and change.
Claims (2)
1. a kind of preparation method of diesel oxidation catalyst, it is characterised in that comprise the following steps:
Step one, citric acid and ethylene glycol are added in deionized water in stirring and dissolving at 45~55 DEG C, then add nitric acid
The platinum aqueous solution obtains mixed solution after being stirred 1~2 hour at 50~60 DEG C, wherein the mol ratio of the citric acid and ethylene glycol is
1:1~1:4, the total moles ratio of platinum nitrate and citric acid and ethylene glycol is 1:9~1:15;
Step 2, alumina powder of the particle diameter for 100~200 mesh is added into step one gained mixed solution in 400~600
Rev/min mixing speed under be stirred at room temperature 0.5~1 hour, then heat to 70~90 DEG C stirring 6~8 hours after must be evaporated
Product, wherein Alpha-alumina and gama-alumina mass ratio are 1 in the alumina powder:3;
Step 3, will be evaporated product and dries 3~5 hours at 100~130 DEG C in step 2, then in 500~550 DEG C 0.3~
Diesel oxidation catalyst (DOC) is obtained after being calcined 2~3h under 0.5MPa nitrogen atmosphere.
2. a kind of preparation method of diesel oxidation catalyst as claimed in claim 1, it is characterised in that:Platinum nitrate and oxidation
The mass ratio of aluminium is 0.006:1~0.012:1.
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CN103052446B (en) * | 2010-08-20 | 2014-12-17 | 三井金属矿业株式会社 | Oxidation catalyst suitable for combustion of light oil component |
CN102916201A (en) * | 2012-10-11 | 2013-02-06 | 常州大学 | Palladium-carbon nanocatalyst and preparation method thereof |
WO2014178635A1 (en) * | 2013-05-02 | 2014-11-06 | 희성촉매 주식회사 | Catalyst for preventing diesel engine from discharging white smoke |
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