CN105776255A - Preparation method of spherical magnesium oxide particles with large specific surface area - Google Patents

Preparation method of spherical magnesium oxide particles with large specific surface area Download PDF

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Publication number
CN105776255A
CN105776255A CN201610100599.5A CN201610100599A CN105776255A CN 105776255 A CN105776255 A CN 105776255A CN 201610100599 A CN201610100599 A CN 201610100599A CN 105776255 A CN105776255 A CN 105776255A
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acetamide
preparation
predecessor
magnesium acetate
weigh
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CN201610100599.5A
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CN105776255B (en
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彭玲玲
刘碧桃
曹仕秀
韩涛
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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Priority claimed from CN201410684834.9A external-priority patent/CN104445296B/en
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Nanotechnology (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Composite Materials (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Catalysts (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a preparation method of spherical magnesium oxide particles with the large specific surface area.The preparation method comprises the steps that corresponding magnesium acetate (Mg(CH3COO)2) and acetamide (C2H5NO) are weighed according to the stoichiometric ratio of all elements, and a surfactant and polyethylene glycol which account for 0.1%-3% of the total mass of magnesium acetate and acetamide are weighed; the weighted magnesium acetate (Mg(CH3COO)2), acetamide (C2H5NO), the surfactant and polyethylene glycol are fully mixed in ethyl alcohol or ethylene glycol ligands, the mass ratio of the reactants to the ligands is 1:(5-8), and the materials are put in a magnetic stirrer to be stirred at constant temperature until the reactants and the ligands are fully mixed, wherein the stirring temperature is 40 DEG C, and the stirring time is 8-10 h; a product is put in a drying box to be dried at 60 DEG C, and precursor powder is obtained; the precursor powder is calcined in a muffle furnace, the calcining temperature is 250 DEG C-350 DEG C, the calcining time is 2-5 hours, and then the target product is obtained.

Description

The preparation method of the spherical alumina magnesium granules that a kind of specific surface area is big
The application is for Application No. 201410684834.9, filing date on November 25th, 2014, the divisional application of invention entitled " synthetic method of a kind of spherical MgO nano-particle ".
Technical field
The invention belongs to technical field of inorganic nanometer material, particularly to the preparation method of ball shaped nano oxide material.
Background technology
MgO is a kind of important industrial chemicals, has a wide range of applications in fields such as catalysis, antibacterial, refractory material superconductors, is also used as the filler of paper, cosmetics etc. simultaneously.Bulk effect and skin effect specific to nano material, the composite of the formation such as nano-MgO and high polymer has good in microwave absorbing property, additionally MgO nano-particle has higher surface activity, show many at aspects such as catalysis and absorption and be different from the chemical characteristic of body material so that it is 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.Its surface adsorption property and catalytic performance can be caused tremendous influence by the pattern of nano oxidized magnesium granules, and therefore exploitation operational approach is easy, granule-morphology is good, the method for the MgO nano-particle material of size uniform, favorable dispersibility is significant.The preparation method of MgO nano-particle material mainly has room temperature solid-state reaction method, the sedimentation method and electrochemical reaction method etc. at present.These preparation methoies are respectively arranged with advantage and deficiency, but granule-morphology as simple to operate in solid phase method is bad, sedimentation method pattern well but complex process, electrochemical method high in cost of production.Therefore the preparation method developing new MgO nano-particle still has the biggest captivation.So far, have no that soft template method prepares the report of spherical MgO nano-particle.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that the preparation method of the spherical MgO nano-particle that a kind of specific surface area is big.
Spherical MgO nano-particle that the present invention proposes and preparation method thereof comprises the following steps:
(1) measure ratio according to each element chemistry, weigh corresponding magnesium salt and acetamide C2H5NO；Weigh surfactant and the Polyethylene Glycol of above medicine gross mass 0.1% ~ 3% the most respectively.
(2) by the magnesium salt weighed and Acetamide C2H5NO, surfactant and Polyethylene Glycol are sufficiently mixed in part, reactant is 1:5-8 with the mass ratio of part, is then placed in magnetic stirring apparatus carrying out constant temperature stirring, and whipping temp is 40 DEG C, mixing time is 8-10h, till reactant is sufficiently mixed with part.
(3) above-mentioned product is positioned over 60 DEG C of drying in drying baker, obtains predecessor powder；
(4) being calcined in Muffle furnace by predecessor powder, calcining heat is 250-350 DEG C, and burning time is 2 ~ 5 hours, obtains target product；
In the present invention, described in step (1), magnesium salt is Mg (CH3COO)2；Described surfactant is tetrapropylene benzene sodium sulfonate or Dodecyl trimethyl ammonium chloride.
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 inventive method is with magnesium salt, acetamide as raw material, Polyethylene Glycol is soft template, chelating chemical reaction is there is during temperature constant magnetic stirring, the mixing carrying out raw material in organic solvent can increase the specific surface area of reactant, improves reactant contact surface and reaction rate, therefore improves the ratio of nucleation rate and growth rate, preparing uniform predecessor, predecessor drying, sintering that reaction generates obtain target product.There is advantages that
1, the MgO nano-particle that the present invention prepares is spherical in rule.
2, the spherical MgO nano-particle of present invention synthesis uses soft template synthesis technique, and subsequent calcination process temperature is low, and the time is short, is conducive to improving the uniformity of nano-particle, and production efficiency is high.
3, the MgO specific surface area of present invention synthesis is big, have good absorption property.
Accompanying drawing explanation
Fig. 1 is the XRD figure spectrum of spherical MgO nano-particle；
Fig. 2 is spherical MgO nano-particle pattern photo under scanning electron microscope.
Detailed description of the invention
Embodiment 1
1, dispensing
Measure ratio according to each element chemistry, weigh corresponding magnesium acetate Mg (CH3COO)2With acetamide C2H5NO；Weigh tetrapropylene benzene sodium sulfonate and the polyethylene glycol-800 of above medicine gross mass 1% the most respectively.
2, prepared by predecessor
Magnesium acetate Mg (the CH that will weigh3COO)2With acetamide C2H5NO, tetrapropylene benzene sodium sulfonate and polyethylene glycol-800 are sufficiently mixed in dehydrated alcohol, reactant is 1:5 with the mass ratio of part, is then placed in magnetic stirring apparatus carrying out constant temperature stirring, and whipping temp is 40 DEG C, mixing time is 10h, till reactant is sufficiently mixed with part.
3, it is dried
Above-mentioned product is positioned over 60 DEG C of drying in drying baker, obtains predecessor；
4, calcining
Being calcined in Muffle furnace by predecessor, calcining heat is 280 DEG C, and burning time is 4 hours, obtains target product.
Embodiment 2
1, dispensing
Measure ratio according to each element chemistry, weigh corresponding magnesium acetate Mg (CH3COO)2With acetamide C2H5NO；Weigh tetrapropylene benzene sodium sulfonate and the cetomacrogol 1000 of above medicine gross mass 2% the most respectively.
2, prepared by predecessor
Magnesium acetate Mg (the CH that will weigh3COO)2With acetamide C2H5NO, tetrapropylene benzene sodium sulfonate and polyethylene glycol-800 are sufficiently mixed in dehydrated alcohol, reactant is 1:7 with the mass ratio of part, is then placed in magnetic stirring apparatus carrying out constant temperature stirring, and whipping temp is 40 DEG C, mixing time is 8h, till reactant is sufficiently mixed with part.
3, it is dried
Above-mentioned product is positioned over 60 DEG C of drying in drying baker, obtains predecessor；
4, calcining
Being calcined in Muffle furnace by predecessor, calcining heat is 300 DEG C, and burning time is 4 hours, obtains target product.
Embodiment 3
1, dispensing
Measure ratio according to each element chemistry, weigh corresponding magnesium acetate Mg (CH3COO)2With acetamide C2H5NO；Weigh cetyl trimethylammonium bromide and the cetomacrogol 1000 of above medicine gross mass 3% the most respectively.
2, prepared by predecessor
Magnesium acetate Mg (the CH that will weigh3COO)2With acetamide C2H5NO, cetyl trimethylammonium bromide and cetomacrogol 1000 are sufficiently mixed in dehydrated alcohol, reactant is 1:8 with the mass ratio of part, is then placed in magnetic stirring apparatus carrying out constant temperature stirring, and whipping temp is 40 DEG C, mixing time is 8h, till reactant is sufficiently mixed with part.
3, it is dried
Above-mentioned product is positioned over 60 DEG C of drying in drying baker, obtains predecessor；
4, calcining
Being calcined in Muffle furnace by predecessor, calcining heat is 280 DEG C, and burning time is 4 hours, obtains target product.

Claims (1)

1. the preparation method of the spherical alumina magnesium granules that a specific surface area is big, it is characterised in that specifically comprise the following steps that
(1), dispensing
Measure ratio according to each element chemistry, weigh corresponding magnesium acetate Mg (CH3COO)2With acetamide C2H5NO；Weigh tetrapropylene benzene sodium sulfonate and the cetomacrogol 1000 of above medicine gross mass 2% the most respectively；
(2), prepared by predecessor
Magnesium acetate Mg (the CH that will weigh3COO)2With acetamide C2H5NO, tetrapropylene benzene sodium sulfonate and polyethylene glycol-800 are sufficiently mixed in dehydrated alcohol part, reactant is about 1:7 with the mass ratio of dehydrated alcohol part, it is then placed in magnetic stirring apparatus carrying out constant temperature stirring, whipping temp is about 40 DEG C, mixing time is about 8h, till reactant is sufficiently mixed with part；
(3), it is dried
Above-mentioned product is positioned over 60 DEG C of drying in drying baker, obtains predecessor；
(4), calcining
Being calcined in Muffle furnace by predecessor, calcining heat is 300 DEG C, and burning time is 4 hours, obtains target product.
CN201610100599.5A 2014-11-25 2014-11-25 A kind of preparation method of the big spherical alumina magnesium granules of specific surface area Active CN105776255B (en)

Priority Applications (1)

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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

Applications Claiming Priority (2)

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CN201410684834.9A CN104445296B (en) 2014-11-25 2014-11-25 A kind of synthetic method of spherical MgO nano particle
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

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109627547A (en) * 2018-11-30 2019-04-16 全球能源互联网研究院有限公司 Bitter earth nano ball and its preparation, using the high voltage direct current cable material of bitter earth nano ball and its preparation

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101353176A (en) * 2007-07-26 2009-01-28 郑州大学 Novel method for preparing nano-magnesia

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101353176A (en) * 2007-07-26 2009-01-28 郑州大学 Novel method for preparing nano-magnesia

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
LINGLING PENG ET AL.: ""Multiplesite structure and photoluminescence properties of Eu3+ doped MgO nanocrystals"", 《APPLIED PHYSICS A》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109627547A (en) * 2018-11-30 2019-04-16 全球能源互联网研究院有限公司 Bitter earth nano ball and its preparation, using the high voltage direct current cable material of bitter earth nano ball and its preparation

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