CN108002449A - A kind of MnCo2O4The preparation method of spinelle type composite oxides - Google Patents

A kind of MnCo2O4The preparation method of spinelle type composite oxides Download PDF

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Publication number
CN108002449A
CN108002449A CN201711284428.3A CN201711284428A CN108002449A CN 108002449 A CN108002449 A CN 108002449A CN 201711284428 A CN201711284428 A CN 201711284428A CN 108002449 A CN108002449 A CN 108002449A
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mnco
composite oxides
type composite
spinelle type
preparation
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刘焕荣
代晓东
石会龙
陈艳红
韩东敏
崔红霞
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Shengli College China University of Petroleum
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Shengli College China University of Petroleum
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/40—Cobaltates
    • 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
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/2073—Manganese
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20746—Cobalt
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM

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

Abstract

The present invention relates to a kind of MnCo2O4The preparation method of spinelle type composite oxides.Comprise the following steps that：The first step：Dissolving metal salts are weighed in deionized water；Second step：Complexing agent glucose sugar is weighed, is dissolved in deionized water；3rd step：The first step is dissolved to obtain metal salt solution and is poured slowly into the enveloping agent solution that second step dissolves, is mixed；4th step：3rd step solution is placed in aging in vacuum drying chamber, obtains vitreosol；5th step：Colloidal sol obtained by 4th step is placed in vacuum drying chamber drying；6th step：Muffle kiln roasting is placed on again, is down to room temperature naturally, and product is made.Beneficial effect is：The present invention is preferable as complexing agent, its promotion effect using relatively inexpensive biochemical reagents glucose；In addition, raw material can obtain the mixing of molecular level in the synthesis process, and dry glue is easily formed, synthesized MnCo2O4Spinelle type composite oxides catalyst has higher catalytic activity.

Description

A kind of MnCo2O4The preparation method of spinelle type composite oxides
Technical field
The present invention relates to a kind of preparation method of exhaust gas from diesel vehicle processing catalyst, more particularly to a kind of MnCo2O4Spinelle The preparation method of type composite oxides.
Background technology
With the continuous improvement of living standard, the quantity of automobile is also rapidly increasing, thing followed automobile exhaust pollution Problem is increasingly aggravating.Diesel vehicle because with fuel economy is good, ignition point is higher, be not easy because cas fortuit be ignited or Occur explosion, using it is safer stable the characteristics of and as " favorite " of nowadays numerous fans.But exhaust gas from diesel vehicle In the soot particulate that contains（PM）Up to 50 times of gasoline engine, are one of main sources of haze, to human health damage pole Greatly.Stringent motor vehicle exhaust emission regulation, European diesel have been formulated in the problem of for exhaust gas from diesel vehicle exhaust emission, countries in the world Tail gas Abgasgesetz provides that diesel vehicle is upgraded to Europe VI from Europe V, and PM must reduce by 50%.The state V that China will implement discharges For standard compared with V standards of state I, PM reduction amounts require higher, reach 82%.Under these circumstances, fuel qualities, diesel engine are lifted Emission controls by improving combustion and existing diesel engine after treatment device have been unable to meet new diesel emission standard requirement, develop high activity Exhaust gas from diesel vehicle processing catalyst become and solve one of fastest means of current problem.Therefore, reduce and eliminate diesel oil Carbon soot particles in tail gas are the vital tasks of diesel car tail gas refining.
Research shows, under lean-burn condition, while purifies and removes the catalytic reaction of NOx and carbon soot particles in diesel engine vent gas In, simple oxide, composite oxides all have certain catalytic action.The stability of alkali metal is poor, loose contact conditions Lower alkaline-earth metal it is active low, be not used alone generally；Noble metal catalyst is expensive, tight to engine air-fuel ratio requirement Lattice, the SOx in tail gas are also possible to generate a large amount of sulfate with catalyst reaction, bring environmental pollution；Single transition metal and its The activity difference of oxide catalyst is larger, volatile.Spinel type composite metal oxide is with stable structure and relatively Preferable catalytic activity, can remove carbon soot particles and NOx in exhaust gas from diesel vehicle at the same time, and the specific structure of spinelle has Beneficial to the doping vario-property of catalyst, therefore, spinelle type composite oxides are as removing urging for soot and NOx in exhaust gas from diesel vehicle Agent will be development trend from now on.In order to overcome conventional sol-gel processes to prepare spinel oxide gelling temperature height, time The shortcomings that long, by adding glucose, change reaction condition, promote its plastic, MnCo is prepared with this2O4Spinel-type composite oxygen Compound catalyst, realizes the purpose for reducing soot combustion temperature.
The content of the invention
The purpose of the present invention is aiming at drawbacks described above existing in the prior art, there is provided a kind of MnCo2O4Spinel-type is compound The preparation method of oxide, it is higher can to solve soot combustion temperature, it is impossible to be able to oxidizing fire completely and be discharged into air, pollute The practical problem of environment.
A kind of MnCo that the present invention mentions2O4The preparation method of spinelle type composite oxides, comprises the following steps that：
The first step：In molar ratio 2:1 weighs metal salt Co (NO3)3·6H2O and Mn (AC)2·4H2O is dissolved in deionized water In, it is spare；
Second step：Complexing agent glucose sugar is weighed, metal ion presses 0.4~1.0 molar ratio with glucose, is dissolved in deionization It is spare in water；
3rd step：The first step is dissolved to obtain metal salt solution and is poured slowly into the enveloping agent solution that second step dissolves, is mixed Close stirring 30min；
4th step：3rd step solution is placed in aging 12h in 60 DEG C of vacuum drying chambers, obtains vitreosol；
5th step：By colloidal sol obtained by the 4th step be placed in 120 DEG C of vacuum drying chambers it is dry the powdered xerogel of gray fluffy；
6th step：Xerogel is placed on Muffle kiln roasting, roasting condition is；In atmosphere with 5 DEG C/min speed by room temperature liter For height to 600 DEG C, constant temperature 4h, is down to room temperature naturally, and MnCo is made2O4Spinel complex oxide.
Above-mentioned metal salt Co (NO3)3·6H2O and Mn (AC)2·4H2O is technical grade product, content 99%.
Above-mentioned glucose sugar is technical grade product, content 99%.
The aging drying process of step 4 kind uses vacuum drying chamber, avoids and air contact.
A kind of MnCo that the present invention mentions2O4MnCo made of the preparation method of spinelle type composite oxides2O4Spinelle The application method of type composite oxides, comprises the following steps：
By 10:1 mass ratio weighs MnCo2O4Spinelle type composite oxides and the common 165g of carbon soot particles, after being mixed with spoon Add in reaction tube, both ends are fixed with silica wool, are placed on the miniature fixed-bed reactor in laboratory and are reacted, tail gas Tested and analyzed through chromatography.
The beneficial effects of the invention are as follows：The sol-gel synthesis method of the present invention, using relatively inexpensive biochemical reagents Portugal Grape sugar is used as complexing agent, its promotion effect is preferable；In addition, raw material can obtain the mixing of molecular level in the synthesis process, and Easily form dry glue, synthesized MnCo2O4Spinelle type composite oxides catalyst has higher catalytic activity；
In addition, the present invention adds substantial amounts of glucose in preparation process, on the one hand when roasting, can burn the substantial amounts of heat of releasing, Help to reduce calcination temperature；On the other hand, burn gas CO, CO of formation2Bulk product is expanded, forms duct, increase MnCo2O4The contact area of spinelle type composite oxides and carbon soot particles, reduces the ignition temperature of soot.
Brief description of the drawings
Attached drawing 1 is MnCo prepared by the present invention2O4The scanning electron microscope (SEM) photograph of spinelle type composite oxides；
Attached drawing 2 is MnCo prepared by the present invention2O4The scanning electron microscope (SEM) photograph of spinelle type composite oxides.
Embodiment
The preferred embodiment of the present invention is illustrated below in conjunction with attached drawing, it will be appreciated that described herein preferred real Apply example to be merely to illustrate and explain the present invention, be not intended to limit the present invention.
Embodiment 1：The MnCo that the present invention mentions2O4The preparation method of spinelle type composite oxides, as the molten of catalyst Glue-gel method is as follows：
Four acetate hydrate manganese 4.9g are weighed in beaker first, add ionized water stirring and dissolving, it is stand-by；Claim again in another beaker Cabaltous nitrate hexahydrate 11.64g is taken, adds ionized water stirring and dissolving, it is stand-by；Molar ratio according to glucose and total metal ion claims 6.48g glucose is taken, ionized water stirring and dissolving is added, the aqueous solution of manganese acetate and cobalt nitrate is then slowly added to grape at the same time In the solution of sugar；30min is stirred, aging 12h in 70 DEG C of vacuum drying chamber is placed in, obtains vitreosol；It is then placed in 120 Dry the powdered xerogel of gray fluffy in DEG C vacuum drying chamber；Xerogel is finally placed on Muffle kiln roasting, roasts bar Part is；600 DEG C are increased to by room temperature with 5 DEG C/min speed in atmosphere, constant temperature 4h, is down to room temperature naturally, and MnCo is made2O4Point Spar composite oxides.
It is as follows that evaluation test of the exhaust gas from diesel vehicle discharge to catalytic activity is simulated on miniature fixed-bed reactor：
By 10:1 mass ratio weighs MnCo prepared by the present invention2O4Spinelle type composite oxides and the common 165g of carbon soot particles, Added after being mixed with spoon in reaction tube, both ends are fixed with silica wool, are placed on the miniature fixed-bed reactor in laboratory Reacted, tail gas is tested and analyzed through chromatography.
The MnCo prepared using sol-gel process2O4Catalyst can significantly reduce the ignition temperature of soot, wherein being catalyzed Carbon-smoke combustion reactionT 10 、T 50 、T 90 Respectively 345 DEG C, 407 DEG C, 506 DEG C, compared with noncatalytic combustion, 137 are reduced respectively ℃、178℃、140℃。
The present invention is in order to overcome conventional sol-gel processes to prepare spinel oxide gelling temperature height, the shortcomings that time is long, By adding glucose, change reaction condition, promote its plastic, MnCo is prepared with this2O4Spinelle type composite oxides are catalyzed Agent, realizes the purpose for reducing soot combustion temperature.
Referring to the drawings 1, the MnCo for preparing of the present invention2O4Spinelle type composite oxides, more common solid reaction process raw material It is uniformly mixed, calcination temperature is low, and the catalyst formed has certain microcellular structure, can increase catalyst and be connect with soot Tactile surface area, and then the temperature of carbon-smoke combustion is reduced, achieve the purpose that to reduce soot particulate discharge.
Embodiment 2：A kind of MnCo that the present invention mentions2O4The preparation method of spinelle type composite oxides, including following step Suddenly：
Four acetate hydrate manganese 7.35g are weighed in beaker first, add ionized water stirring and dissolving, it is stand-by；Again in another beaker Cabaltous nitrate hexahydrate 17.46g is weighed, adds ionized water stirring and dissolving, it is stand-by；According to the molar ratio of glucose and total metal ion 9.72g glucose is weighed, ionized water stirring and dissolving is added, the aqueous solution of manganese acetate and cobalt nitrate is then slowly added to Portugal at the same time In the solution of grape sugar；45min is stirred, aging 8h in 100 DEG C of vacuum drying chamber is placed in, obtains vitreosol；It is then placed in Dry the powdered xerogel of gray fluffy in 140 DEG C of vacuum drying chambers；Xerogel is finally placed on Muffle kiln roasting, is roasted Condition is；600 DEG C are increased to by room temperature with 10 DEG C/min speed in atmosphere, constant temperature 5h, is down to room temperature naturally, and MnCo is made2O4 Spinel complex oxide.
Evaluation test of the exhaust gas from diesel vehicle discharge to catalytic activity is simulated on miniature fixed-bed reactor.
By 10:1 mass ratio weighs MnCo prepared by the present invention2O4Spinelle type composite oxides are total to carbon soot particles 160g, adds in reaction tube after being mixed with spoon, and both ends are fixed with silica wool, is placed into the miniature fixed bed reaction dress in laboratory Put and reacted, tail gas is tested and analyzed through chromatography.
The MnCo prepared using the present invention2O4Catalyst can significantly reduce the ignition temperature of soot, wherein catalysis soot combustion Burn reactionT 10 、T 50 、T 90 Respectively 338 DEG C, 412 DEG C, 506 DEG C, compared with noncatalytic combustion, respectively reduce by 145 DEG C, 173 ℃、140℃。
Embodiment 3：A kind of MnCo that the present invention mentions2O4The preparation method of spinelle type composite oxides, including following step Suddenly：
Four acetate hydrate manganese 4.9g are weighed in beaker first, add ionized water stirring and dissolving, it is stand-by；Claim again in another beaker Cabaltous nitrate hexahydrate 11.64g is taken, adds ionized water stirring and dissolving, it is stand-by；Molar ratio according to glucose and total metal ion claims 8.64g glucose is taken, ionized water stirring and dissolving is added, the aqueous solution of manganese acetate and cobalt nitrate is then slowly added to grape at the same time In the solution of sugar；35min is stirred, aging 10h in 80 DEG C of vacuum drying chamber is placed in, obtains vitreosol；It is then placed in 160 Dry the powdered xerogel of gray fluffy in DEG C vacuum drying chamber；Xerogel is finally placed on Muffle kiln roasting, roasts bar Part is；600 DEG C are increased to by room temperature with 10 DEG C/min speed in atmosphere, constant temperature 6h, is down to room temperature naturally, and MnCo is made2O4Point Spar composite oxides.
Evaluation test of the exhaust gas from diesel vehicle discharge to catalytic activity is simulated on miniature fixed-bed reactor.
By 10:1 mass ratio weighs MnCo prepared by the present invention2O4Spinelle type composite oxides are total to carbon soot particles 150g, adds in reaction tube after being mixed with spoon, and both ends are fixed with silica wool, is placed into the miniature fixed bed reaction dress in laboratory Put and reacted, tail gas is tested and analyzed through chromatography.
The MnCo prepared using the present invention2O4Catalyst can significantly reduce the ignition temperature of soot, wherein catalysis soot combustion Burn reactionT 10 、T 50 、T 90 Respectively 328 DEG C, 402 DEG C, 496 DEG C, compared with noncatalytic combustion, respectively reduce by 164 DEG C, 183 ℃、150℃。
Referring to the drawings 2, sol-gel process make use of to prepare MnCo2O4Spinelle type composite oxides catalyst, more commonly Solid reaction process raw material be uniformly mixed, calcination temperature is low, and formed catalyst there is certain microcellular structure, Ke Yizeng The surface area that big catalyst is contacted with soot, and then the temperature of carbon-smoke combustion is reduced, reach the mesh for reducing soot particulate discharge 's.
The above, is only the part preferred embodiment of the present invention, and any those skilled in the art may profit Equivalent technical solution is changed or is revised as with the technical solution of above-mentioned elaboration.Therefore, the technology according to the present invention Any simple modification or substitute equivalents that scheme is carried out, belong to the greatest extent the scope of protection of present invention.

Claims (5)

  1. A kind of 1. MnCo2O4The preparation method of spinelle type composite oxides, it is characterized in that comprising the following steps that：
    The first step：In molar ratio 2:1 weighs metal salt Co (NO3)3·6H2O and Mn (AC)2·4H2O is dissolved in deionized water, It is spare；
    Second step：Complexing agent glucose sugar is weighed, metal ion presses 0.4~1.0 molar ratio with glucose, is dissolved in deionization It is spare in water；
    3rd step：The first step is dissolved to obtain metal salt solution and is poured slowly into the enveloping agent solution that second step dissolves, is mixed Close stirring 30min；
    4th step：3rd step solution is placed in aging 12h in 60 DEG C of vacuum drying chambers, obtains vitreosol；
    5th step：By colloidal sol obtained by the 4th step be placed in 120 DEG C of vacuum drying chambers it is dry the powdered xerogel of gray fluffy；
    6th step：Xerogel is placed on Muffle kiln roasting, roasting condition is；In atmosphere with 5 DEG C/min speed by room temperature liter For height to 600 DEG C, constant temperature 4h, is down to room temperature naturally, and MnCo is made2O4Spinel complex oxide.
  2. 2. MnCo according to claim 12O4The preparation method of spinelle type composite oxides, it is characterized in that：The metal Salt Co (NO3)3·6H2O and Mn (AC)2·4H2O is technical grade product, content 99%.
  3. 3. MnCo according to claim 12O4The preparation method of spinelle type composite oxides, it is characterized in that：The glucose Sugar is technical grade product, content 99%.
  4. 4. MnCo according to claim 12O4The preparation method of spinelle type composite oxides, it is characterized in that：Step 4 kind Aging drying process use vacuum drying chamber, avoid and air contact.
  5. A kind of 5. MnCo any one of using claim 1-42O4The preparation method of spinelle type composite oxides is made MnCo2O4The application method of spinelle type composite oxides, it is characterized in that：Comprise the following steps：
    By 10:1 mass ratio weighs MnCo2O4Spinelle type composite oxides and the common 165g of carbon soot particles, add after being mixed with spoon Enter in reaction tube, both ends are fixed with silica wool, are placed on the miniature fixed-bed reactor in laboratory and are reacted, tail gas warp Chromatography tests and analyzes.
CN201711284428.3A 2017-12-07 2017-12-07 A kind of MnCo2O4The preparation method of spinelle type composite oxides Pending CN108002449A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110844944A (en) * 2019-11-29 2020-02-28 昆明理工大学 Preparation method of Ce-Mn-Co-O oxygen carrier and application of Ce-Mn-Co-O oxygen carrier in chemical looping reforming hydrogen production of blast furnace gas
CN111282578A (en) * 2020-04-09 2020-06-16 国电科学技术研究院有限公司 Metal-doped manganese-based low-temperature denitration catalyst and preparation method thereof
CN111584893A (en) * 2020-05-28 2020-08-25 蔚蓝(广东)新能源科技有限公司 Air electrode catalyst of aluminum-air battery, air electrode and preparation method of air electrode catalyst
CN113548873A (en) * 2021-08-13 2021-10-26 新乡学院 Preparation method of manganese cobalt oxide ceramic material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
刘焕荣: ""MnCo2O4尖晶石型复合氧化物的制备及其应用研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110844944A (en) * 2019-11-29 2020-02-28 昆明理工大学 Preparation method of Ce-Mn-Co-O oxygen carrier and application of Ce-Mn-Co-O oxygen carrier in chemical looping reforming hydrogen production of blast furnace gas
CN111282578A (en) * 2020-04-09 2020-06-16 国电科学技术研究院有限公司 Metal-doped manganese-based low-temperature denitration catalyst and preparation method thereof
CN111282578B (en) * 2020-04-09 2023-01-31 国电科学技术研究院有限公司 Metal-doped manganese-based low-temperature denitration catalyst and preparation method thereof
CN111584893A (en) * 2020-05-28 2020-08-25 蔚蓝(广东)新能源科技有限公司 Air electrode catalyst of aluminum-air battery, air electrode and preparation method of air electrode catalyst
CN113548873A (en) * 2021-08-13 2021-10-26 新乡学院 Preparation method of manganese cobalt oxide ceramic material
CN113548873B (en) * 2021-08-13 2022-07-29 新乡学院 Preparation method of manganese cobalt oxide ceramic material

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Application publication date: 20180508