CN105413314B - The preparation method of the high active material of particulate filter - Google Patents

The preparation method of the high active material of particulate filter Download PDF

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Publication number
CN105413314B
CN105413314B CN201510749158.3A CN201510749158A CN105413314B CN 105413314 B CN105413314 B CN 105413314B CN 201510749158 A CN201510749158 A CN 201510749158A CN 105413314 B CN105413314 B CN 105413314B
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carrier
hours
particulate filter
ball milling
sintering
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CN105413314A (en
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崔龙
张克金
张斌
于力娜
杨帅
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FAW Group Corp
FAW Jiefang Automotive Co Ltd
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FAW Group Corp
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • B01D39/2068—Other inorganic materials, e.g. ceramics
    • B01D39/2093—Ceramic foam
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D39/00—Filtering material for liquid or gaseous fluids
    • B01D39/14—Other self-supporting filtering material ; Other filtering material
    • B01D39/20—Other self-supporting filtering material ; Other filtering material of inorganic material, e.g. asbestos paper, metallic filtering material of non-woven wires
    • 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
    • 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
    • B01J23/83—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 rare earths or actinides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
    • B01D2239/04—Additives and treatments of the filtering material
    • B01D2239/0407—Additives and treatments of the filtering material comprising particulate additives, e.g. adsorbents

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Ceramic Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Catalysts (AREA)
  • Filtering Materials (AREA)

Abstract

The present invention relates to a kind of preparation method of the high active material of particulate filter, it is characterised in that comprise the following steps that：The basic material of ceramic carrier material is carried out into proportioning according to the material of carrier, made by base paste；1% ~ 5% vaseline is added in base paste, 5% ~ 10% polyethylene glycol is subsequently adding, is subsequently adding basalt chopped fiber 1% ~ 3%, is uniformly mixed；Ball mill ball milling is put into, base paste is made;Raw material drying after ball milling, sintering, makes highly active particulate filter carrier material mixture after grinding；Which is a kind of catalyst coat material with oxidisability, possesses passive regeneration function using the particulate filter of the material, while the frequency of initiative regeneration can be reduced, reduces the consumption of fuel oil.

Description

The preparation method of the high active material of particulate filter
Technical field
The present invention relates to a kind of preparation method of the high active material of particulate filter, high active material diesel engine particles mistake Filter and material manufacture and method, and catalyst coat.
Background technology
Compared with gasoline engine, engine fuel economy is good, oil consumption is low, due to its compression ratio height, waste gas discharge total amount and pollution Thing total emission volumn is above gasoline engine, especially soot particulate（PM）Content, is 40 to 100 times of gasoline engine, therefore for bavin The purification of oil machine soot particulate shows important especially.The exhaust emissions of motor vehicle have become one of city environmental pollution it is main Pollution sources.Also progressively added sternly for the Abgasgesetz of motor vehicle.
In the tail gas that the motor vehicles that power is provided by Diesel engine are discharged, not only including carbon monoxide（CO）With nitrogen oxygen Compound（NOx）, but also including the various ingredients produced in the case of fully from fuel.Affiliated component not only includes hydrocarbon Compound（HC）, also soot or it is referred to as the particulate pollutant of " soot ".Carbon monoxide（CO）, hydrocarbon gas （HC）And not sufficiently combusted organic matter can be attached to above carbon soot particles, so-called volatile organic matter is formed（VOF）.
By SCR（SCR）Technology can be by the nitrogen oxides in diesel motor exhaust（NOx）Conversion Into harmless nitrogen and water.And volatile organic constituents and carbon soot particles can be removed by the catalytic converter of oxidisability Go.
The researcher both domestic and external particulate matter all in waste gas is devoted to for a long time（PM）Control emission work, generally Think diesel particulate filter（DPF）It is the effective means for removing particulate matter, but routine DPF needs to regenerate meeting back pressure Require, one of which method is to coat oxidation catalyst to reduce particle burning temperature on DPF, and your gold custom catalystses are Metal catalyst, this process costs are higher, and need coating procedure, and the present invention adopts oxidized form molecular sieve catalyst conduct Dpf regeneration catalyst, while, the spy that can jointly process, jointly sinter close with carrier material using molecular sieve physicochemical property Point, is fabricated directly into the diesel engine particles grabber with catalysis oxidation function, compared with conventional DPF, has both reduced cost, and Coating processes are reduced, experiment proves that the DPF of present invention making can meet 5 discharge standard of state.
High active material will be favorably improved the performance of catalyst converter, hydrocarbon, and carbon monoxide and volatility are organic Thing, the oxidation of organic carbon soot particles have facilitation.It is often the compound of multiple material to receive in the catalyst material for using Catalyst.Activity of the high activity by material, such as γ types aluminum oxide, anatase titanium dioxide is all with highly active catalyst Material.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the high active material of particulate filter, which is a kind of with oxygen The catalyst coat material of the property changed, possesses passive regeneration function using the particulate filter of the material, while can reduce actively The frequency of regeneration, reduces the consumption of fuel oil.
The technical scheme is that what is be achieved in that：The preparation method of the high active material of particulate filter, its feature It is to comprise the following steps that：1）The basic material of ceramic carrier material is carried out into proportioning according to the material of carrier, magnesia is received Rice gamma-alumina, aoxidizes silicon mol ratio according to 1:1:2.5 carry out dispensing, and the material of carrier is set according to cordierite formula Meter, magnesia in cordierite, nanometer gamma-alumina, silica molar ratio are 1:1:2.5, add sepiolite, sepiolite 1% ~ 20%wt that content is carrier gross mass is added, sepiolite can mutually form good homogeneous phase with cordierite in sintering process Tissue, the ratio for adding deionized water mixing and stirring, deionized water and inorganic powder quality are 1:1~3:2, add oxidation Active catalyst material, addition for carrier gross mass 1% ~ 20%, made by base paste；
2）1% ~ 5% vaseline is added in base paste, 5% ~ 10% polyethylene glycol is subsequently adding, polyethylene glycol can be with Make the aqueous solution addition, polyethylene glycol with water be ratio be 1:10~1:20, basalt chopped fiber 1% ~ 3% is subsequently adding, It is uniformly mixed；
3）Ball mill ball milling is put into, base paste is made, during ball milling, pellet mass ratio 2:1,20 ~ 60HZ of drum's speed of rotation, 16 ~ 28 hours time, the raw material particle size after ball milling are less than 2 μm；Raw material drying after ball milling, sintering, it is little that ventilation stands 24 ~ 36 When, or 105 DEG C, 6 ~ 8 hours of baking oven；Sintering temperature is 1100 DEG C ~ 1700 DEG C, 1050 DEG C ~ 1150 DEG C of more excellent sintering temperature, 2 ~ 16 hours time, after grinding, make highly active particulate filter carrier material mixture；
4）High-activity particle filter-carrier material blends are put into into tug mill equipment, 10% ~ 30% deionization is added Water, pore-forming material, mixing and stirring, and mud 2 ~ 6 hours；The mud become reconciled, is transported to pugging equipment, refines 2 ~ 6 hours；Turn Ceramic honey comb extrusion equipment is transported to, by suitable mould, extrusion makes the carrier blank of different meshes, as needed, cutting Into the carrier blank section of different volumes；60 ~ the 330mm of diameter of extrusion die, 100 ~ 900 mesh of mesh number；
5）By carrier blank section, standing is needed at room temperature 12 ~ 36 hours, or 110 DEG C of blast heatings 2 ~ 6 hours, it After be put in high temperature sintering furnace and calcine, 600 DEG C ~ 1500 DEG C of temperature, is subsequently cooled to room temperature, obtains honeycomb 10 ~ 16 hours time Shape structure carrier；
6）By alveolate texture carrier two ends asymmetric alternately plug-hole, then 300 ~ 600 DEG C of sintering again, obtain possessing passive The particulate filter carrier of regeneration function.
The positive effect of the present invention is that its material is prepared simply, and production efficiency is significantly lifted, and is adapted to industrialized batch Production, and cost is lower.Using oxidizing catalytic agent material is contained in particulate filter prepared by the material, the monoblock type contains The carrier for having catalyst is better than coating the particulate filter of catalyst coat as the processor effect of passive regeneration, can be effective Ground solves the problems, such as the coating shedding that catalyst is caused by tail gas erosion process, and it is sudden and violent that the carrier surface for coming off has new catalysis material Expose and work on, extend the life-span of processor, it is ensured that catalytic conversion efficiency.
Description of the drawings
Fig. 1 is sepiolite.
Fig. 2 is basalt chopped fiber.
Fig. 3 is the high active material of Mn/La/Ce catalysis.
Fig. 4 is the high active material of Co/Ce catalysis.
Particulate filters of the Fig. 5 for high active material.
Specific embodiment
The present invention will be further described with reference to the accompanying drawings and examples：As shown in Figure 1-2, the height of particulate filter The preparation method of active material, it is characterised in that comprise the following steps that：1）By the basic material of ceramic carrier material according to carrier Material carry out proportioning, by magnesia, nanometer gamma-alumina, oxidation silicon mol ratio is according to 1:1:2.5 carry out dispensing, the material of carrier Matter is designed according to cordierite formula, magnesia in cordierite, nanometer gamma-alumina, and silica molar ratio is 1: 1:2.5, add sepiolite, sepiolite adds content for 1% ~ 20%wt of carrier gross mass, and in sintering process, sepiolite can be with Cordierite mutually forms good homogeneous phase constitution, adds deionized water mixing and stirring, deionized water and inorganic powder quality Ratio be 1:1~3:2, add oxidation activity catalyst material, addition for carrier gross mass 1% ~ 20%, made by basis Slurry；
2）1% ~ 5% vaseline is added in base paste, 5% ~ 10% polyethylene glycol is subsequently adding, polyethylene glycol can be with Make the aqueous solution addition, polyethylene glycol with water be ratio be 1:10~1:20, basalt chopped fiber 1% ~ 3% is subsequently adding, It is uniformly mixed；
3）Ball mill ball milling is put into, base paste is made, during ball milling, pellet mass ratio 2:1,20 ~ 60HZ of drum's speed of rotation, 16 ~ 28 hours time, the raw material particle size after ball milling are less than 2 μm；Raw material drying after ball milling, sintering, it is little that ventilation stands 24 ~ 36 When, or 105 DEG C, 6 ~ 8 hours of baking oven；Sintering temperature is 1100 DEG C ~ 1700 DEG C, 1050 DEG C ~ 1150 DEG C of more excellent sintering temperature, 2 ~ 16 hours time, after grinding, make highly active particulate filter carrier material mixture；
4）High-activity particle filter-carrier material blends are put into into tug mill equipment, 10% ~ 30% deionization is added Water, pore-forming material, mixing and stirring, and mud 2 ~ 6 hours；The mud become reconciled, is transported to pugging equipment, refines 2 ~ 6 hours；Turn Ceramic honey comb extrusion equipment is transported to, by suitable mould, extrusion makes the carrier blank of different meshes, as needed, cutting Into the carrier blank section of different volumes；60 ~ the 330mm of diameter of extrusion die, 100 ~ 900 mesh of mesh number；
5）By carrier blank section, standing is needed at room temperature 12 ~ 36 hours, or 110 DEG C of blast heatings 2 ~ 6 hours, it After be put in high temperature sintering furnace and calcine, 600 DEG C ~ 1500 DEG C of temperature, is subsequently cooled to room temperature, obtains honeycomb 10 ~ 16 hours time Shape structure carrier；
6）By alveolate texture carrier two ends asymmetric alternately plug-hole, then 300 ~ 600 DEG C of sintering again, obtain possessing passive The particulate filter carrier of regeneration function.
Embodiment 1
In 5L deionized waters, magnesia, aluminum oxide, silica, sepiolite, basalt chopped fiber are sequentially added, It is stirred until homogeneous, above-mentioned inorganic powder quality is followed successively by 8mol, 8mol, 20mol, 1.5kg, 0.1kg, is subsequently added pore-forming material Graphite 0.05kg, powdered rice hulls 0.05kg, the Mn/La/Ce catalysis material 1.0kg with oxidative function；
Vaseline 0.1kg, polyethylene glycol 0.1kg are added, ball milling in ball mill is put into, rotating speed is 20Hz, material ball ratio 1:2, Ball milling 20h；
Product is taken out, 105 DEG C are dehydrated to formation slurry；
Slurry is sintered, 550 DEG C of temperature, the insulation of 4 hours time, along with the furnace cooling；
Grinding product, particle diameter are less than 2 μm.Obtain possessing the particulate filter carrier material mixture of passive regeneration function such as Fig. 3.
Mixture material tests the hole of its sample using the mercury injection apparatus of the AutoPore VI9510 models of Merck ＆ Co., Inc of the U.S. Gap rate 75 ~ 80%.
Embodiment 2
In 8L deionized waters, magnesia, aluminum oxide, silica, sepiolite are sequentially added, basalt chopped fiber, It is stirred until homogeneous, above-mentioned inorganic powder quality is followed successively by 10mol, 10mol, 25mol, 1.5kg, is subsequently added pore-forming material graphite 0.01kg, powdered rice hulls 0.1kg, the Co/Ce combined oxidation catalysis material 1.0kg with oxidative function；
Vaseline 0.1kg, polyethylene glycol 0.1kg are added, ball milling in ball mill is put into, rotating speed is 30Hz, material ball ratio 1:2, Ball milling 18h；
Product is taken out, 110 DEG C are dehydrated to forming extrudable mud；
Above-mentioned mud extrusion is constituted into honeycomb, streaming support greenware is made, is stood, ageing is dehydrated；1000℃ Sintering, after cooling, two ends form wall-flow type structure by asymmetric alternately plug-hole.
1h is sintered at 600 DEG C, particulate filter carrier such as Fig. 4 that room temperature obtains high active material is cooled to the furnace.
Mixture material tests the hole of its sample using the mercury injection apparatus of the AutoPore VI9510 models of Merck ＆ Co., Inc of the U.S. Gap rate 70 ~ 75%.
Embodiment 3
In 6L deionized waters, magnesia, aluminum oxide, silica, sepiolite, basalt chopped fiber are sequentially added, It is stirred until homogeneous, above-mentioned inorganic powder quality is followed successively by 12mol, 12mol, 30mol, 2kg, 0.15kg, is subsequently added pore-forming material Work stone ink 0.05kg, powdered rice hulls 0.1kg, the La/Co/Sr composite catalyzing material 1.5kg with oxidative function；
Vaseline 0.2kg, polyethylene glycol 0.1kg are added, ball milling in ball mill is put into, rotating speed is 20Hz, material ball ratio 1:2, Ball milling 20h；
Product is taken out, 100 DEG C are dehydrated to forming extrudable mud；
Above-mentioned mud extrusion is constituted into honeycomb, streaming support greenware is made, is stood, ageing is dehydrated；1000℃ Sintering, after cooling, two ends form wall-flow type structure by asymmetric alternately plug-hole.
1h is sintered at 600 DEG C, particulate filter carrier such as Fig. 5 that room temperature obtains high active material is cooled to the furnace.
Particulate filter carrier tests its sample using the mercury injection apparatus of the AutoPore VI9510 models of Merck ＆ Co., Inc of the U.S. Porosity 50 ~ 60%, aperture be less than 18 microns.

Claims (1)

1. the preparation method of the high active material of particulate filter, it is characterised in that comprise the following steps that：1）By ceramic monolith material The basic material of material carries out proportioning according to the material of carrier, by magnesia, nanometer gamma-alumina, aoxidizes silicon mol ratio according to 1:1: 2 .5 carry out dispensing, and the material of carrier is designed according to cordierite formula, magnesia in cordierite, the oxidation of nanometer γ Aluminium, silica molar ratio are 1:1:2 .5, add sepiolite, sepiolite to add 1% ~ 20%wt that content is carrier gross mass, In sintering process, sepiolite can mutually form good homogeneous phase constitution with cordierite, add deionized water mixing and stirring, The ratio of deionized water and inorganic powder quality is 1:1~3:2, oxidation activity catalyst material is added, addition is the total matter of carrier The 1% ~ 20% of amount, makes base paste；
2）1% ~ 5% vaseline is added in base paste, 5% ~ 10% polyethylene glycol is subsequently adding, polyethylene glycol can be made The aqueous solution is added, and polyethylene glycol and water are that ratio is 1:10~1:20, it is subsequently adding basalt chopped fiber 1% ~ 3%, stirring mixing Uniformly；
3）Ball mill ball milling is put into, base paste is made, during ball milling, pellet mass ratio 2:1,20 ~ 60Hz of drum's speed of rotation, time 16 ~ 28 hours, the raw material particle size after ball milling was less than 2 μm；Raw material drying after ball milling, sintering, ventilation stand 24 ~ 36 hours, or 105 DEG C, 6 ~ 8 hours of person's baking oven；Sintering temperature is 1100 DEG C ~ 1700 DEG C, 2 ~ 16 hours time, highly active is made after grinding Grain filter-carrier material blends；
4）High-activity particle filter-carrier material blends are put into into tug mill equipment, 10% ~ 30% deionized water is added, into Porous materials, mixing and stirring, and mud 2 ~ 6 hours；The mud become reconciled, is transported to pugging equipment, refines 2 ~ 6 hours；It is transported to honeybee Nest ceramics extrusion equipment, by suitable mould, extrusion is made the carrier blank of different meshes, as needed, cuts into difference The carrier blank section of volume；60 ~ the 330mm of diameter of extrusion die, 100 ~ 900 mesh of mesh number；
5）By carrier blank section, standing is needed at room temperature 12 ~ 36 hours, or 110 DEG C of blast heatings 2 ~ 6 hours, Zhi Houfang Calcine in entering high temperature sintering furnace, 600 DEG C ~ 1500 DEG C of temperature 10 ~ 16 hours time, is subsequently cooled to room temperature, obtains cellular knot Structure carrier；
6）By alveolate texture carrier two ends asymmetric alternately plug-hole, then 300 ~ 600 DEG C of sintering again, obtain possessing passive regeneration The particulate filter carrier of function.
CN201510749158.3A 2015-11-06 2015-11-06 The preparation method of the high active material of particulate filter Active CN105413314B (en)

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CN105413314B true CN105413314B (en) 2017-04-05

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Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
ATE372449T1 (en) * 2001-12-03 2007-09-15 Hitachi Metals Ltd CERAMIC HONEYCOMB FILTER
JP4361449B2 (en) * 2004-09-24 2009-11-11 日本碍子株式会社 Method for producing cordierite honeycomb structure
WO2006137157A1 (en) * 2005-06-24 2006-12-28 Ibiden Co., Ltd. Honeycomb structure body
FR2931366B1 (en) * 2008-05-22 2011-01-21 Saint Gobain Ct Recherches SIC-VITROCERAMIC COMPOSITE FILTER
JP5126681B2 (en) * 2008-11-28 2013-01-23 日立金属株式会社 Ceramic honeycomb filter and manufacturing method thereof

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Effective date of registration: 20180817

Address after: 130011 2259 Dongfeng Street, Xinxin economic and Technological Development Zone, Changchun, Jilin

Co-patentee after: FAW Jiefang Automotive Co., Ltd.

Patentee after: China FAW Group Corporation

Address before: 130011 2259 Dongfeng Street, Xinxin economic and Technological Development Zone, Changchun, Jilin

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