CN104445296B - A kind of synthetic method of spherical MgO nano particle - Google Patents

A kind of synthetic method of spherical MgO nano particle Download PDF

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Publication number
CN104445296B
CN104445296B CN201410684834.9A CN201410684834A CN104445296B CN 104445296 B CN104445296 B CN 104445296B CN 201410684834 A CN201410684834 A CN 201410684834A CN 104445296 B CN104445296 B CN 104445296B
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nano particle
active agent
mgo nano
tensio
synthetic method
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CN104445296A (en
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彭玲玲
刘碧桃
韩涛
曹仕秀
黄敏
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Chongqing University of Arts and Sciences
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Chongqing University of Arts and Sciences
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/02—Magnesia
    • C01F5/06—Magnesia by thermal decomposition of magnesium compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

A synthetic method for spherical MgO nano particle, belongs to the technology of preparing of nano-metal-oxide, according to each element chemistry metering ratio, takes corresponding magnesium acetate Mg (CH 3cOO) 2with ethanamide C 2h 5nO; Take tensio-active agent and the polyoxyethylene glycol of above medicine total mass 0.1% ~ 3% more respectively.By the magnesium acetate Mg (CH taken 3cOO) 2and Acetamide? C 2h 5nO, tensio-active agent and polyoxyethylene glycol fully mix in ethanol or ethylene glycol part, the mass ratio of reactant and part is 1:5-8, is then positioned in magnetic stirring apparatus and carries out constant temperature stirring, and whipping temp is 40 DEG C, churning time is 8-10h, till reactant fully mixes with part.Above-mentioned product is positioned over 60 DEG C of oven dry in loft drier, obtains precursor powder; Calcined in retort furnace by precursor powder, calcining temperature is 250-350 DEG C, and combustion time is 2 ~ 5 hours, obtains target product.

Description

A kind of synthetic method of spherical MgO nano particle
Technical field
The invention belongs to technical field of inorganic nanometer material, particularly ball shaped nano oxide material, be specifically related to the synthetic method of spherical MgO nano particle.
Background technology
MgO is a kind of important industrial chemicals, has a wide range of applications in fields such as catalysis, antibacterial, refractory materials superconducting materials, simultaneously can also as the weighting agent of paper, makeup etc.Volume effect and surface effects specific to nano material, the matrix material that nano-MgO and superpolymer etc. are formed has good in microwave absorbing property, MgO nano particle has higher surfactivity in addition, in catalysis and absorption etc., show many chemical propertys being different from body material, make it at these fields potential application foreground widely.China's magnesium resource is abundant, with low cost simultaneously, makes MgO nano-particle material have significant practical value.The pattern of nano oxidized magnesium granules can cause tremendous influence to its surface adsorption property and catalytic performance, and therefore development and operation method is easy, granule-morphology good, the method for the MgO nano-particle material of size uniform, favorable dispersity is significant.The preparation method of current MgO nano-particle material mainly contains room temperature solid-state reaction method, the precipitator method and electrochemical reaction method etc.These preparation methods respectively have advantages and disadvantages, but granule-morphology as simple to operate in solid phase method is bad, precipitator method pattern well but complex process, electrochemical method high in cost of production.Therefore the preparation method developing new MgO nano particle still has very large magnetism.So far, the report that soft template method prepares spherical MgO nano particle is had no.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of synthetic method of spherical MgO nano particle is provided.This method with magnesium salts, ethanamide for raw material, polyoxyethylene glycol is soft template, chelating chemical reaction is there is in temperature constant magnetic stirring process, the mixing carrying out raw material in organic solvent can increase the specific surface area of reactant, improve reactant contact surface and speed of reaction, therefore improve the ratio of nucleation rate and growth rate, prepare uniform precursor, the precursor drying that reaction generates, sintering obtain target product.
Spherical MgO nano particle that the present invention proposes and preparation method thereof comprises the following steps:
(1) according to each element chemistry metering ratio, corresponding magnesium salts and ethanamide C is taken 2h 5nO; Take tensio-active agent and the polyoxyethylene glycol of above medicine total mass 0.1% ~ 3% more respectively.
(2) by the magnesium salts that takes and Acetamide C 2h 5nO, tensio-active agent and polyoxyethylene glycol fully mix in part, the mass ratio of reactant and part is 1:5-8, is then positioned in magnetic stirring apparatus and carries out constant temperature stirring, and whipping temp is 40 DEG C, churning time is 8-10h, till reactant fully mixes with part.
(3) above-mentioned product is positioned over 60 DEG C of oven dry in loft drier, obtains precursor powder;
(4) calcined in retort furnace by precursor powder, calcining temperature is 250-350 DEG C, and combustion time is 2 ~ 5 hours, obtains target product;
In the present invention, described in step (1), magnesium salts is Mg (CH 3cOO) 2; Described tensio-active agent is tetrapropylene benzene sodium sulfonate or Trimethyllaurylammonium bromide.
In the present invention, described in step (2), described in part step (2), part is dehydrated alcohol or ethylene glycol.
Compared with prior art, the present invention has following beneficial effect:
1, the MgO nano particle that the present invention prepares is the spherical of rule.
2, the spherical MgO nano particle of the present invention's synthesis adopts soft template synthesis technique, and subsequent calcination process temperature is low, and the time is short, and be conducive to the homogeneity improving nano particle, production efficiency is high.
3, the MgO specific surface area of the present invention's synthesis large, there is good absorption property.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of spherical MgO nano particle;
Fig. 2 is the pattern photo of spherical MgO nano particle under scanning electron microscope.
Embodiment
Embodiment 1
1, prepare burden
According to each element chemistry metering ratio, take corresponding magnesium acetate Mg (CH 3cOO) 2with ethanamide C 2h 5nO; Take tetrapropylene benzene sodium sulfonate and the polyethylene glycol-800 of above medicine total mass 1% more respectively.
2, precursor preparation
By the magnesium acetate Mg (CH taken 3cOO) 2with ethanamide C 2h 5nO, tetrapropylene benzene sodium sulfonate and polyethylene glycol-800 fully mix in dehydrated alcohol, the mass ratio of reactant and part is 1:5, is then positioned in magnetic stirring apparatus and carries out constant temperature stirring, and whipping temp is 40 DEG C, churning time is 10h, till reactant fully mixes with part.
3, dry
Above-mentioned product is positioned over 60 DEG C of oven dry in loft drier, obtains precursor;
4, calcine
Calcined in retort furnace by precursor, calcining temperature is 280 DEG C, and combustion time is 4 hours, obtains target product;
Embodiment 2
1, prepare burden
According to each element chemistry metering ratio, take corresponding magnesium acetate Mg (CH 3cOO) 2with ethanamide C 2h 5nO; Take tetrapropylene benzene sodium sulfonate and the cetomacrogol 1000 of above medicine total mass 2% more respectively.
2, precursor preparation
By the magnesium acetate Mg (CH taken 3cOO) 2with ethanamide C 2h 5nO, tetrapropylene benzene sodium sulfonate and polyethylene glycol-800 fully mix in dehydrated alcohol, the mass ratio of reactant and part is 1:7, is then positioned in magnetic stirring apparatus and carries out constant temperature stirring, and whipping temp is 40 DEG C, churning time is 8h, till reactant fully mixes with part.
3, dry
Above-mentioned product is positioned over 60 DEG C of oven dry in loft drier, obtains precursor;
4, calcine
Calcined in retort furnace by precursor, calcining temperature is 300 DEG C, and combustion time is 4 hours, obtains target product;
Embodiment 3
1, prepare burden
According to each element chemistry metering ratio, take corresponding magnesium acetate Mg (CH 3cOO) 2with ethanamide C 2h 5nO; Take cetyl trimethylammonium bromide and the cetomacrogol 1000 of above medicine total mass 3% more respectively.
2, precursor preparation
By the magnesium acetate Mg (CH taken 3cOO) 2with ethanamide C 2h 5nO, cetyl trimethylammonium bromide and cetomacrogol 1000 fully mix in dehydrated alcohol, the mass ratio of reactant and part is 1:8, is then positioned in magnetic stirring apparatus and carries out constant temperature stirring, and whipping temp is 40 DEG C, churning time is 8h, till reactant fully mixes with part.
3, dry
Above-mentioned product is positioned over 60 DEG C of oven dry in loft drier, obtains precursor;
4, calcine
Calcined in retort furnace by precursor, calcining temperature is 280 DEG C, and combustion time is 4 hours, obtains target product.

Claims (3)

1. a synthetic method for spherical MgO nano particle, is characterized in that: adopt soft template method to prepare presoma, the spherical MgO nano particle of low-temperature burning precursor power median size <20nm, its crystalline structure is simple cubic structure;
Described soft template method prepares presoma specifically:
(1) with magnesium salts and ethanamide C 2h 5nO is raw material, and polyoxyethylene glycol is soft template, according to each element chemistry metering ratio, takes corresponding magnesium salts and ethanamide; Take tensio-active agent and the polyoxyethylene glycol of above medicine total mass 0.1% ~ 3% more respectively; (2) magnesium salts taken and ethanamide, tensio-active agent and polyoxyethylene glycol are fully mixed in part, the mass ratio of reactant and part is 1:5 ~ 8, then be positioned in magnetic stirring apparatus and carry out constant temperature stirring, whipping temp is 40 DEG C, churning time is 8-10h, till reactant fully mixes with part; Its reaction equation is as follows: CH 3cONH 2+ Mg 2+→ (CH 3cO) 2mg+NH 2 +; (3) above-mentioned product is positioned over 60 DEG C of oven dry in loft drier, obtains precursor powder;
Calcined in retort furnace by precursor powder, calcining temperature is 250-350 DEG C, and combustion time is 2 ~ 5 hours, obtains target product; Product checking: XRD surveys crystalline structure, and SEM/TEM surveys pattern and granularity.
2. the synthetic method of a kind of spherical MgO nano particle as claimed in claim 1, is characterized in that described in step (1), magnesium salts is Mg (CH 3cOO) 2, described tensio-active agent is tetrapropylene benzene sodium sulfonate or Trimethyllaurylammonium bromide.
3. the synthetic method of a kind of spherical MgO nano particle as claimed in claim 1, is characterized in that described in step (2), part is dehydrated alcohol or ethylene glycol.
CN201410684834.9A 2014-11-25 2014-11-25 A kind of synthetic method of spherical MgO nano particle Active CN104445296B (en)

Priority Applications (2)

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CN201610100599.5A CN105776255B (en) 2014-11-25 2014-11-25 A kind of preparation method of the big spherical alumina magnesium granules of specific surface area
CN201410684834.9A CN104445296B (en) 2014-11-25 2014-11-25 A kind of synthetic method of spherical MgO nano particle

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CN201610100600.4A Division CN105731504A (en) 2014-11-25 2014-11-25 Method for preparing good-adsorbability nanometer particles

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1974881A (en) * 2006-11-10 2007-06-06 北京工业大学 Prepn process of cubic monocrystalline magnesia particle with tetragonal and hexagonal burrow-shaped mesopores
CN101015862A (en) * 2007-03-02 2007-08-15 江南大学 Process for preparing gold nano particle by using aqueous phase soft mould plate method
CN101323460A (en) * 2008-07-11 2008-12-17 北京工业大学 Method for preparing high specific surface area three-dimensional mesoporous active aluminum oxide by hard template

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Publication number Priority date Publication date Assignee Title
JP3733599B2 (en) * 1993-08-11 2006-01-11 住友化学株式会社 Metal oxide powder and method for producing the same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1974881A (en) * 2006-11-10 2007-06-06 北京工业大学 Prepn process of cubic monocrystalline magnesia particle with tetragonal and hexagonal burrow-shaped mesopores
CN101015862A (en) * 2007-03-02 2007-08-15 江南大学 Process for preparing gold nano particle by using aqueous phase soft mould plate method
CN101323460A (en) * 2008-07-11 2008-12-17 北京工业大学 Method for preparing high specific surface area three-dimensional mesoporous active aluminum oxide by hard template

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
低温燃烧合成纳米MgO;董澄宇等;《光谱学与光谱分析》;20121031;第32卷(第10期);第333-334页 *

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