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CN110255590A - A kind of method that rapid precipitation prepares magnesium hydroxide two-dimensional nano piece - Google Patents

A kind of method that rapid precipitation prepares magnesium hydroxide two-dimensional nano piece Download PDF

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Publication number
CN110255590A
CN110255590A CN201910711666.0A CN201910711666A CN110255590A CN 110255590 A CN110255590 A CN 110255590A CN 201910711666 A CN201910711666 A CN 201910711666A CN 110255590 A CN110255590 A CN 110255590A
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CN
China
Prior art keywords
magnesium hydroxide
dimensional nano
rapid precipitation
nahco
nano piece
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN201910711666.0A
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Chinese (zh)
Inventor
赖伟鸿
李用成
宫毅涛
刚勇
李亚书
李东祥
王绍才
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Liaoning Xingkong New Energy Development Co Ltd
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Liaoning Xingkong New Energy Development Co Ltd
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Priority to CN201910711666.0A priority Critical patent/CN110255590A/en
Publication of CN110255590A publication Critical patent/CN110255590A/en
Withdrawn legal-status Critical Current

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    • 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
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/14Magnesium hydroxide
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/03Particle morphology depicted by an image obtained by SEM
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/60Particles characterised by their size
    • C01P2004/62Submicrometer sized, i.e. from 0.1-1 micrometer

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

Abstract

The present invention provides a kind of method that rapid precipitation prepares magnesium hydroxide two-dimensional nano piece, this method has a variety of outstanding features such as efficient, quick, succinct in preparing material, the huge challenge for overcoming regulation two-dimension nano materials caused by the quick crystallization of precipitation reaction, prepares two-dimension nano materials Mg (OH)2, it is that precipitating reagent rapid precipitation goes out target material using sodium bicarbonate.NaHCO3With low dissociation coefficient, OH can be slowly releasedIon, the speed of growth and diffusion velocity of balancing material, so that being grown according to two-dimensional directional of can orienting during the growth process of material.The present invention provides a kind of Mg (OH) with excellent properties2The pattern of nanometer sheet mutually regulates and controls method with object.This method is at low cost, reaction rate is fast, reacts mildly easily-controllable, energy conservation and environmental protection, product purity height and the advantages such as novel in shape.

Description

A kind of method that rapid precipitation prepares magnesium hydroxide two-dimensional nano piece
Technical field
The present invention relates to technical field of nanometer material preparation, and in particular to a kind of rapid precipitation prepares two wiener of magnesium hydroxide The method of rice piece.
Background technique
Magnesium hydroxide (Mg (OH)2) belong to metal hydroxides, because of its special crystal structure and its Derived Oxides Keep this substance fire-retardant in energy storage, the numerous areas such as electrode-clad, and catalysis have extensive potential application.Rapid, high volume system Standby this electrode material preparation and ionic conductor material synthesis field have extensive use.Especially its special two-dimensional structure has The electronic and ionic conduction orientation of orientation, powerful stress ability to bear and short axial ion transmission path, it is considered to be ten Divide important nano material branch.Existing preparation two dimension Mg (OH)2The method of nano material mainly utilizes lye, sodium oxalate, ammonia Water is prepared in water heating kettle.The preparation method needs at high temperature under high pressure, and time-consuming, and at high cost, safety is poor, low output.Cause This, two-dimentional Mg (OH) can simply, quickly be prepared by inventing one kind2The method of nano material will be in following industrialization, Yi Ji great Amount application produces particularly important.The precipitation method have efficiently in preparing material, quickly, a variety of outstanding features such as succinct.But it is same When, the quick crystallization of precipitation reaction makes preparation, regulates and controls along specific dimension nano material: such as two-dimension nano materials have very Big challenge.
Summary of the invention
For the prior art is insufficient or Improvement requirement, the present invention provides a kind of rapid precipitation and prepares magnesium hydroxide two-dimensional nano The method of piece, this method have a variety of outstanding features such as efficient, quick, succinct in preparing material, overcome precipitation reaction The huge challenge of regulation two-dimension nano materials, prepares two-dimension nano materials Mg (OH) caused by quick crystallization2, utilize carbonic acid Hydrogen sodium is that precipitating reagent rapid precipitation goes out target material.NaHCO3With low dissociation coefficient, OH can be slowly released-Ion is put down Weigh the speed of growth and diffusion velocity of material, so that growing according to two-dimensional directional of can orienting during the growth process of material.This Invention provides a kind of Mg (OH) with excellent properties2The pattern of nanometer sheet mutually regulates and controls method with object.
To achieve the above object, the invention is realized by the following technical scheme:
The present invention provides a kind of method that rapid precipitation prepares magnesium hydroxide two-dimensional nano piece, which is characterized in that with Mg (NO3)2 And NaHCO3It for raw material, is synthesized using liquid-phase precipitation method, magnesium hydroxide two-dimensional nano tablet raw material is by following weight parts Group is grouped as:
Concentration is the Mg (NO of 0.19-0.58%3)2·6H250-60 parts of O
Concentration is the NaHCO of 0.42-0.59%340-50 parts of solution
Step 1, by above-mentioned Mg (NO3)2·6H2O and NaHCO3It is dissolved in the water, 10-20 is stirred persistently with 200-500r/min Minute;
Step 2 is centrifuged 5-10 minutes by mixed material supercentrifuge obtained by step 1 with 3500-5000r/min;
Step 3 cleans gained shallow white depositions 1-3 times with 96 % ethanol solutions;
Step 4, by step 3 resulting material 60-80 DEG C dry 5-12 hours to get magnesium hydroxide two-dimensional nano piece.
Solution reaction environment temperature is 60-70 DEG C in the step 1
Compared with prior art, the beneficial effects of the present invention are: the present invention carries out material preparation using the liquid phase room temperature precipitation method, with Conventional hydrothermal method compares, and this method is easy to operate, and prepared product morphology is novel, quality is stablized.
Detailed description of the invention
Fig. 1 is Mg (OH) in embodiment 12Nanometer sheet X-ray diffraction (XRD) figure.
Fig. 2 is Mg (OH) in embodiment 12Nanometer sheet scanning electron microscope (SEM) test chart.
Specific embodiment
Preparation method of the invention is described further below with reference to embodiment:
Embodiment 1:
The present invention provides a kind of method that rapid precipitation prepares magnesium hydroxide two-dimensional nano piece.This method is with Mg (NO3)2With NaHCO3It for raw material, is synthesized using liquid-phase precipitation method, is realized by following technical side:
At 65 DEG C, the Mg (NO for being 0.19% by 520g concentration3)2·6H2The NaHCO that O and 480g concentration is 0.42%3It is dissolved in In water, persistently stirred with 300r/min 10 minutes;By gained mixed material supercentrifuge with 5000r/min, it is centrifuged 5 points Clock;The shallow white depositions of gained are cleaned 3 times with the ethyl alcohol of 96 %;Resulting material is dried 12 hours at 60 DEG C to get hydrogen-oxygen Change magnesium two-dimensional nano piece.
XRD result such as Fig. 1 product structure is magnesium hydroxide, and pattern is as shown in Fig. 2, be nanoscale laminated structure, nanometer The width of piece is 500nm or so.
Embodiment 2:
The present invention provides a kind of method that rapid precipitation prepares magnesium hydroxide two-dimensional nano piece.This method is with Mg (NO3)2With NaHCO3It for raw material, is synthesized using liquid-phase precipitation method, is realized by following technical side:
At 65 DEG C, the Mg (NO for being 0.38% by 540g concentration3)2·6H2The NaHCO that O and 460g concentration is 0.50%3It is dissolved in In water, persistently stirred with 300r/min 10 minutes;By gained mixed material supercentrifuge with 5000r/min, it is centrifuged 5 points Clock;The shallow white depositions of gained are cleaned 3 times with the ethyl alcohol of 96 %;Resulting material is dried 12 hours at 60 DEG C to get hydrogen-oxygen Change magnesium two-dimensional nano piece.
Embodiment 3:
The present invention provides a kind of method that rapid precipitation prepares magnesium hydroxide two-dimensional nano piece.This method is with Mg (NO3)2With NaHCO3It for raw material, is synthesized using liquid-phase precipitation method, is realized by following technical side:
At 65 DEG C, the Mg (NO for being 0.58% by 580g concentration3)2·6H2The NaHCO that O and 420g concentration is 0.59%3It is dissolved in In water, persistently stirred with 300r/min 10 minutes;By gained mixed material supercentrifuge with 5000r/min, it is centrifuged 5 points Clock;The shallow white depositions of gained are cleaned 3 times with the ethyl alcohol of 96 %;Resulting material is dried 12 hours at 60 DEG C to get hydrogen-oxygen Change magnesium two-dimensional nano piece.

Claims (2)

1. a kind of method that rapid precipitation prepares magnesium hydroxide two-dimensional nano piece, which is characterized in that with Mg (NO3)2And NaHCO3For Raw material is synthesized using liquid-phase precipitation method, and magnesium hydroxide two-dimensional nano tablet raw material is made of following components in parts by weight:
Concentration is the Mg (NO of 0.19-0.58%3)2·6H250-60 parts of O
Concentration is the NaHCO of 0.42-0.59%340-50 parts of solution
Step 1, by above-mentioned Mg (NO3)2·6H2O and NaHCO3It is dissolved in the water, 10-20 points is persistently stirred with 200-500r/min Clock;
Step 2 is centrifuged 5-10 minutes by mixed material supercentrifuge obtained by step 1 with 3500-5000r/min;
Step 3 cleans gained shallow white depositions 1-3 times with 96 % ethanol solutions;
Step 4, by step 3 resulting material 60-80 DEG C dry 5-12 hours to get magnesium hydroxide two-dimensional nano piece.
2. the method that a kind of rapid precipitation according to claim 1 prepares magnesium hydroxide two-dimensional nano piece, which is characterized in that Solution reaction environment temperature is 60-70 DEG C in the step 1.
CN201910711666.0A 2019-08-02 2019-08-02 A kind of method that rapid precipitation prepares magnesium hydroxide two-dimensional nano piece Withdrawn CN110255590A (en)

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Application Number Priority Date Filing Date Title
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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB648315A (en) * 1942-07-15 1951-01-03 Permanente Metals Corp Process of producing magnesium oxide and products resulting therefrom
WO2008041833A1 (en) * 2006-10-03 2008-04-10 Servicios Industriales Peñoles, S.A. De C.V. Method for producing stable, monodispersed, nanometric magnesium hydroxide and resulting product
CN101607722A (en) * 2008-05-27 2009-12-23 浙江理工大学 A kind of synthetic method of magnesium hydrate hexagonal nano-flake
WO2014046471A1 (en) * 2012-09-18 2014-03-27 Hanwha Chemical Corporation. Method for preparing metal catalyst for preparing carbon nanotubes and method for preparing carbon nanotubes using the same
CN105217696A (en) * 2015-09-17 2016-01-06 南昌大学 A kind of preparation method of nickel acid magnesium nanometer sheet of three-dimensional super-structure
EP3072933A1 (en) * 2015-03-23 2016-09-28 Universität Graz Stabilized alkaline composite nanoparticles, method for producing the same and use thereof
CN109354076A (en) * 2018-12-14 2019-02-19 辽宁星空钠电电池有限公司 A kind of rapid precipitation preparation dimensional Co CO3Method
US20190193061A1 (en) * 2017-12-22 2019-06-27 Universidad De Chile Method for preparing laminar zinc hydroxide organic-inorganic nanocomposites for use in the removal and degradation of dyes from textile effluents

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB648315A (en) * 1942-07-15 1951-01-03 Permanente Metals Corp Process of producing magnesium oxide and products resulting therefrom
WO2008041833A1 (en) * 2006-10-03 2008-04-10 Servicios Industriales Peñoles, S.A. De C.V. Method for producing stable, monodispersed, nanometric magnesium hydroxide and resulting product
CN101607722A (en) * 2008-05-27 2009-12-23 浙江理工大学 A kind of synthetic method of magnesium hydrate hexagonal nano-flake
WO2014046471A1 (en) * 2012-09-18 2014-03-27 Hanwha Chemical Corporation. Method for preparing metal catalyst for preparing carbon nanotubes and method for preparing carbon nanotubes using the same
EP3072933A1 (en) * 2015-03-23 2016-09-28 Universität Graz Stabilized alkaline composite nanoparticles, method for producing the same and use thereof
CN105217696A (en) * 2015-09-17 2016-01-06 南昌大学 A kind of preparation method of nickel acid magnesium nanometer sheet of three-dimensional super-structure
US20190193061A1 (en) * 2017-12-22 2019-06-27 Universidad De Chile Method for preparing laminar zinc hydroxide organic-inorganic nanocomposites for use in the removal and degradation of dyes from textile effluents
CN109354076A (en) * 2018-12-14 2019-02-19 辽宁星空钠电电池有限公司 A kind of rapid precipitation preparation dimensional Co CO3Method

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Application publication date: 20190920