CN106824192A - A kind of carbon-smoke combustion CuO catalyst of high activity and its preparation method and application - Google Patents

A kind of carbon-smoke combustion CuO catalyst of high activity and its preparation method and application Download PDF

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Publication number
CN106824192A
CN106824192A CN201611229138.4A CN201611229138A CN106824192A CN 106824192 A CN106824192 A CN 106824192A CN 201611229138 A CN201611229138 A CN 201611229138A CN 106824192 A CN106824192 A CN 106824192A
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carbon
smoke combustion
preparation
alkaline solution
cuo catalyst
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赵晗
周晓霞
王敏
潘琳钰
陈航榕
施剑林
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Shanghai Institute of Ceramics of CAS
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Shanghai Institute of Ceramics of CAS
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/72Copper
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/50Catalysts, in general, characterised by their form or physical properties characterised by their shape or configuration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23GCREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G7/00Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
    • F23G7/06Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
    • F23G7/07Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases in which combustion takes place in the presence of catalytic material
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23GCREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G2209/00Specific waste
    • F23G2209/14Gaseous waste or fumes

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Nanotechnology (AREA)
  • Organic Chemistry (AREA)
  • Environmental & Geological Engineering (AREA)
  • Composite Materials (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Catalysts (AREA)

Abstract

A kind of carbon-smoke combustion CuO catalyst the present invention relates to high activity and its preparation method and application, the carbon-smoke combustion CuO catalyst is Nanoparticulate pattern, and particle diameter distribution is 20~100 nm.Carbon-smoke combustion CuO catalyst prepared by the present invention is free of any noble metal, and well-crystallized.The method is with low cost, and yield efficiently, without professional equipment, is worth with great industrialization production.

Description

A kind of carbon-smoke combustion CuO catalyst of high activity and its preparation method and application
Technical field
The invention belongs to catalysis material technical field, and in particular to the one kind for purifying soot in exhaust gas from diesel vehicle is high living Carbon-smoke combustion CuO catalyst of property and preparation method thereof.
Background technology
Diesel vehicle is widely used due to the advantage such as its economy, thermal effect are high and voyage is long in real life. However, the particulate matter (PM, predominantly carbon black granules) of diesel emission and nitrogen oxides serious harm environment and the mankind, because This, efficient post processing purification technique is imperative.Generally, a particulate filter (DPF) is used to collect exhaust gas from diesel vehicle In carbon black granules, the carbon black granules of collection can an at a relatively high temperature (>600 DEG C) by O2Oxidation.However, diesel engine Delivery temperature it is general at 150 to 400 DEG C, its relatively low temperature makes it difficult for the carbon black granules in tail gas to be burnt, and makes for a long time DPF is caused to inactivate after.Therefore, a kind of efficient catalyst is developed, complete oxidation is at a lower temperature to make carbon black granules One extremely urgent work.
The catalyst of carbon soot particles oxidation is commonly used in, such as:CeO2Based compound, perovskite oxide, noble metal base Catalyst etc., or be unfavorable for contact of the avtive spot with carbon particle in default of loose structure and then cause catalyst activity It is too low, or because the preparation cost of loose structure is excessively high, or because the high cost and easy Poisoning of noble metal, so that It is unfavorable for the sizable application of carbon soot particles oxidation catalyst.
The content of the invention
In view of the shortcomings of the prior art, present invention aim at a kind of low-load amount noble metal type carbon-smoke combustion catalysis of offer Agent and its preparation method and application.
On the one hand, the invention provides a kind of carbon-smoke combustion CuO catalyst of high activity, the carbon-smoke combustion CuO catalysis Agent is Nanoparticulate pattern, and particle diameter distribution is 20~100nm.
The carbon-smoke combustion CuO catalyst of high activity of the present invention is transition metal oxide type catalyst, with crystallization Structure, is presented high-dispersion nano graininess pattern, can with carbon particle high-efficient contact, and in terms of the combustion degradation of solid pollutant There is potential application foreground.
It is preferred that the specific surface area of the carbon-smoke combustion CuO catalyst is 10-20m2/ g, pore size is 10-160nm, Pore volume is 0.05-0.10cm3/g。
On the other hand, present invention also offers a kind of preparation method of carbon-smoke combustion CuO catalyst, it is characterised in that will Certain hour is stirred after Cu salting liquids A and alkaline solution B mixing, then 1 is calcined at 400~600 DEG C after washing being centrifuged, dries ~5 hours, obtain the carbon-smoke combustion CuO catalyst.
The present invention prepares the carbon-smoke combustion CuO catalyst using the precipitation method, and methods described is easy to operate and amplify production, Raw material is cheap and easy to get, without professional equipment, with great commercial application prospect.
It is preferred that nitrate of the Cu salt for Cu, acetate, at least one in sulfate, chloride, the Cu salt The molar concentration of solution A is 0.01~0.50mol/L.
It is preferred that solute is bicarbonate or/and carbonate, preferably bicarbonate, the alkali in the alkaline solution B Property solution B concentration be 0.5~5.0mol/L.
It is preferred that the volume ratio of the Cu salting liquids A and alkaline solution B is (0.1~10):1.
It is preferred that the Cu salting liquids A and alkaline solution B hybrid modes are quickly poured into Cu salting liquids A for alkaline solution B In, Cu salting liquids A instill in alkaline solution B or Cu salting liquids A and alkaline solution B parallel-flow precipitations, preferably alkaline solution B is fast Speed is poured into Cu salting liquids A.It is preferred that the metal salt solution A and alkaline solution B are stirred at 0~100 DEG C 5 minutes~ 24 hours.
It is preferred that the heating rate of the calcining is 0.5~10 DEG C/min, preferably 1 DEG C/min.
Another further aspect, present invention also offers a kind of application of carbon-smoke combustion CuO catalyst in motor-driven vehicle gas disposal.
Carbon-smoke combustion CuO catalyst the invention provides a kind of high activity and preparation method thereof.The material is through precipitation Method is obtained, and generates at room temperature, and without any organic matter, crystallization is good after calcining, and high-dispersion nano graininess pattern is presented, Carbon soot particles can be burnt completely below 390 DEG C.Carbon-smoke combustion CuO catalyst prepared by the present invention is free of any your gold Category, and well-crystallized.The method is with low cost, and yield efficiently, without professional equipment, is worth with great industrialization production.
Brief description of the drawings
Fig. 1 is the transmission electron microscope of the carbon-smoke combustion CuO catalyst of the high activity obtained by the embodiment of the present invention 1 Figure;
Fig. 2 is the high-resolution transmission electron microscopy of the carbon-smoke combustion CuO catalyst of the high activity obtained by the embodiment of the present invention 1 Mirror figure;
Fig. 3 is the X ray diffracting spectrum of the carbon-smoke combustion CuO catalyst of the high activity obtained by the embodiment of the present invention 1;
Fig. 4 is the carbon-smoke combustion CuO catalyst carbon-smoke combustion design sketch of high activity in the embodiment of the present invention 2.
Specific embodiment
The present invention is further illustrated below by way of following implementation methods, it should be appreciated that following implementation methods are merely to illustrate this Invention, is not intended to limit the present invention.
The present invention prepares the carbon-smoke combustion CuO catalyst of high activity with mantoquita and alkaline solution as raw material using the precipitation method. Wherein, the carbon-smoke combustion CuO catalyst is the transition metal oxide type catalyst that high-dispersion nano graininess pattern is presented, Its well-crystallized.The diameter of the carbon-smoke combustion CuO catalyst nano-particles can be 20~100nm.
The present invention obtains the soot combustion catalyst of high activity using the method for very cheap and simple.Following exemplary The preparation method of the carbon-smoke combustion CuO catalyst of the high activity that the ground explanation present invention is provided.
A certain amount of, a certain proportion of raw material is dissolved into a certain amount of solvent (such as water, alcohol water mixed solvent etc.) In obtain Cu salting liquids A (hereinafter referred to as solution A).Raw material can be the nitrate of Cu, acetate, sulfate or chlorination One or more in thing, Cu sources are preferably nitrate.In solution A the concentration of metal ion (copper ion) can for 0.01~ 0.50mol/L, preferably 0.10~0.30mol/L.
Precipitating reagent is dissolved into a certain amount of solvent (such as water, alcohol water mixed solvent etc.) and obtains alkaline solution B.Alkalescence Precipitating reagent used by solution B can be bicarbonate, the alkaline matter such as carbonate (such as ammonium carbonate or/and sodium carbonate), preferably Bicarbonate (such as ammonium hydrogen carbonate, sodium acid carbonate etc.).The concentration of precipitating reagent can be 0.5~5.0mol/ in gained alkaline solution B L, preferably 0.5~1.0mol/L.
Under stirring condition, solution A, alkaline solution B are mixed, certain hour is stirred under uniform temperature, obtain containing precipitation The mixed liquor of material (carbonate or/and bicarbonate of Cu).Wherein solution A, alkaline solution B hybrid modes can be that alkalescence is molten Liquid B is quickly poured into solution A, and (alkali formula) carbonate deposition, when quickly mixing, large-scale homogeneous nucleation are formd during being somebody's turn to do Almost occur simultaneously, it is then synchronous to grow up, finally give the product of fine grain.Or in solution A instillation alkaline solution B, should During form (alkali formula) carbonate deposition, adopt when mixing in this way, precipitation is quick to be formed, and is similarly served to favor and is obtained particulate Footpath product.(alkali formula) carbonate deposition can be formd, using this during being somebody's turn to do with solution A, alkaline solution B parallel-flow precipitations When mode mixes, precipitation is quick to be formed, and is similarly served to favor and is obtained fine grain product.Wherein hybrid mode is preferably alkaline from the above Solution B is quickly poured into solution A, beneficial to the sediment for obtaining single dispersing, uniform particle diameter.When by the way of being quickly poured into, its Speed is added to be generally more than 50mL/min, more preferably above preferably greater than 600ml/ minutes, 1200mL/min.Using the side being added dropwise During formula, it can be 1-50mL/min that it adds speed.Solution A, alkaline solution B mixing can be carried out at 0~100 DEG C, preferably be existed Carried out at 25 DEG C of room temperature.Room temperature reaction need not be heated or cooled, beneficial to energy-conservation.Solution A, alkaline solution B incorporation times are 5 minutes By 24 hours, preferably 10 minutes to 1 hour, reaction was quick, saving of work and time.The volume ratio of the solution A and alkaline solution B can It is (0.1~10):1.
By deposit through centrifugation washing, dry after by centrifugation washing and dried process after, calcine under certain condition Oxide is obtained, by the oxide catalyst that calcining can be stablized.Calcination atmosphere can be static or moving air, preferably Still air.The temperature of calcining can be 400~600 DEG C, preferably 500 DEG C.Calcination time can be 1~5 hour, and preferably 2 is small When.Calcining heat is warming up to the speed of 0.5~10 DEG C/min (preferably 1 DEG C/min) during calcining, after insulation a period of time, Furnace cooling.
The specific surface area that the present invention can obtain the catalyst of preparation of the present invention by BET methods or/instrument is 10-20m2/g。
The present invention is 10-160nm by the catalyst pore size that BJH methods or/instrument can obtain preparation of the present invention.
The pore volume that the present invention can obtain the catalyst of preparation of the present invention by BJH methods or/instrument is 0.05-0.10%.
The preparation method of cheap and simple of the present invention obtains being urged with the base metal base high activity of carbon particle high-efficient contact Agent, the carbon-smoke combustion CuO catalyst of prepared high activity, has in fields such as motor vehicle (especially diesel vehicle) vent gas treatments Potential application foreground.
Embodiment is enumerated further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this hair Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific Technological parameter etc. is also only that an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
The copper nitrate solution of 7.5mmol is dissolved in 30 milliliters of water and obtains solution A, by 0.03mol NaHCO3It is dissolved into 30 milliliters Solution B is obtained in water.Under stirring condition, B (adds speed 1800mL/min) in being quickly poured into A, reacts 30 minutes at room temperature.Through After crossing centrifugation washing and dried process, end-product, the ratio of the end-product are obtained in 500 DEG C of calcining 2h in static atmosphere of air Surface area is 9m2/ g, pore size is 10-156nm, and pore volume is 0.07cm3/g。
Fig. 1 is the transmission electron microscope of the carbon-smoke combustion CuO catalyst of the high activity obtained by the embodiment of the present invention (TEM) figure.Visible products therefrom is presented the Nanoparticulate pattern of high dispersive in figure, and diameter is about 40~80nm.This shape Looks feature is close with carbon particle particle size, is conducive to contact of the carbon particle with catalyst granules, and then promote catalytic performance Improve;
Fig. 2 is the high-resolution transmission electron microscopy of the carbon-smoke combustion CuO catalyst of the high activity obtained by the embodiment of the present invention Mirror (HRTEM) figure.The lattice fringe of CuO can be clearly visible in figure, it is shown that good crystallinity;
Fig. 3 is the X ray diffracting spectrum of the carbon-smoke combustion CuO catalyst of the high activity obtained by the embodiment of the present invention.Can in figure See, reconfirm that products therefrom crystallization is good.
Effect example
To verify the catalytic eliminating effect of the carbon-smoke combustion CuO catalyst to carbon soot particles in exhaust gas from diesel vehicle of high activity of the invention Really, special simulation exhaust gas from diesel vehicle condition, designs and carries out following experiment in laboratory conditions.
Embodiment 2
Load in fixed bed reactors by the method for embodiment 1 prepare 0.1g high activity carbon-smoke combustion CuO catalyst, The carbon soot particles of 0.01g, the mixture of 1g quartz sand particles composition, are passed through following gaseous mixture at room temperature:The concentration of NO is 500ppm, O2Concentration be 10 (V) %, N2It is Balance Air, total flow is 0.2L/min.As a comparison, will in another test The carbon-smoke combustion CuO catalyst removal of the high activity of 0.1g, other conditions are constant.Catalysis in 200-700 DEG C of temperature range of test As a result agent is listed in Fig. 4 to the changing effect of carbon soot particles, and the catalyst for being prepared using embodiment as can be seen from Figure 4 can be by soot Particle burns completely below 390 DEG C.Typically, soot conversion ratio reach 90% corresponding temperature can as terminate ignition temperature Tf, in this example, Tf=390 DEG C, less than 400 DEG C, i.e., the catalyst may be such that carbon soot particles burn in the range of normal exhaust temperature Completely.
It is visible in sum, the catalyst that the present invention is provided, presentation high-dispersion nano graininess pattern, well-crystallized, and With catalysis activity well for carbon-smoke combustion.Precipitation method simple economy provided by the present invention, raw material is cheap, with compared with Versatility high.This catalyst has potential application foreground in terms of the combustion degradation of solid pollutant.
Finally be necessary described herein be:Above example is served only for making further in detail technical scheme Ground explanation, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art's the above of the invention Some the nonessential modifications and adaptations made belong to protection scope of the present invention.

Claims (10)

1. the carbon-smoke combustion CuO catalyst of a kind of high activity, it is characterised in that the carbon-smoke combustion CuO catalyst is nanometer Granular pattern, particle diameter distribution is 20~100 nm.
2. carbon-smoke combustion CuO catalyst according to claim 1, it is characterised in that the carbon-smoke combustion CuO catalyst Specific surface area is 10~20 m2/ g, pore size is 10~160 nm, and pore volume is 0.05~0.10 cm3/g。
3. a kind of preparation method of carbon-smoke combustion CuO catalyst as claimed in claim 1 or 2, it is characterised in that by Cu salting liquids Certain hour is stirred after A and alkaline solution B mixing, then is calcined 1~5 hour at 400~600 DEG C after washing being centrifuged, dries, Obtain the carbon-smoke combustion CuO catalyst.
4. preparation method according to claim 3, it is characterised in that the Cu salt is the nitrate of Cu, acetate, sulfuric acid At least one in salt, chloride, the molar concentration of the Cu salting liquids A is 0.01~0.50mol/L.
5. the preparation method according to claim 3 or 4, it is characterised in that solute is bicarbonate in the alkaline solution B Or/and carbonate, preferably bicarbonate, the concentration of the alkaline solution B is 0.5~5.0 mol/L.
6. the preparation method according to any one of claim 3-5, it is characterised in that the Cu salting liquids A and alkalescence are molten Liquid B is stirred 5 minutes~24 hours at 0~100 DEG C.
7. the preparation method according to any one of claim 3-6, it is characterised in that the Cu salting liquids A and alkalescence are molten The volume ratio of liquid B is(0.1~10):1.
8. the preparation method according to any one of claim 3-7, it is characterised in that the heating rate of the calcining is 0.5~10 DEG C/min, preferably 1 DEG C/min.
9. the preparation method according to any one of claim 3-8, it is characterised in that the Cu salting liquids A and alkalescence are molten During liquid B hybrid modes are quickly poured into Cu salting liquids A for alkaline solution B, Cu salting liquids A instilled in alkaline solution B or Cu salting liquids A and alkaline solution B parallel-flow precipitations, preferably alkaline solution B are quickly poured into Cu salting liquids A.
10. application of a kind of carbon-smoke combustion CuO catalyst as claimed in claim 1 or 2 in motor-driven vehicle gas disposal.
CN201611229138.4A 2016-12-27 2016-12-27 A kind of carbon-smoke combustion CuO catalyst of high activity and its preparation method and application Pending CN106824192A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110496623A (en) * 2019-07-05 2019-11-26 重庆大学 A kind of catalyst CuO/K of catalyzed conversion carbon soot particles2Ti4O9And preparation method thereof
CN112439414A (en) * 2020-11-11 2021-03-05 南京东焱氢能源科技有限公司 Preparation method of high-activity palladium hydroxide carbon based on microreactor

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CN101024182A (en) * 2007-01-11 2007-08-29 清华大学 Catalyst for eliminating carbon smoke from copper and cerium and preparing method

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齐智国: ""去除柴油车碳烟颗粒物低温催化剂的研究"", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110496623A (en) * 2019-07-05 2019-11-26 重庆大学 A kind of catalyst CuO/K of catalyzed conversion carbon soot particles2Ti4O9And preparation method thereof
CN112439414A (en) * 2020-11-11 2021-03-05 南京东焱氢能源科技有限公司 Preparation method of high-activity palladium hydroxide carbon based on microreactor

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Application publication date: 20170613