CN105008281B - There is the bar-shaped magnesium hydroxide particle of high-specific surface area and bar-shaped magnesium oxide particle and their manufacture method - Google Patents

There is the bar-shaped magnesium hydroxide particle of high-specific surface area and bar-shaped magnesium oxide particle and their manufacture method Download PDF

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CN105008281B
CN105008281B CN201480008719.8A CN201480008719A CN105008281B CN 105008281 B CN105008281 B CN 105008281B CN 201480008719 A CN201480008719 A CN 201480008719A CN 105008281 B CN105008281 B CN 105008281B
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particle
metallic element
magnesium oxide
magnesium hydroxide
magnesium
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CN105008281A (en
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黑田明
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Tateho Chemical Industries Co Ltd
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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
    • C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
    • 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
    • C01F5/14—Magnesium hydroxide
    • C01F5/16—Magnesium hydroxide by treating magnesia, e.g. calcined dolomite, with water or solutions of salts not containing magnesium
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles
    • 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
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • 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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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The present invention provides has the magnesium hydroxide particle of high-specific surface area and magnesium oxide particle and their manufacture method.A kind of magnesium hydroxide particle and magnesium oxide particle, it is bar-shaped for lepidiod agglomerated primary particles, utilizes 50% particle diameter (D of the volume-cumulative of laser diffraction and scattering formula particle size distribution50) it is 1.0～10.0 μm, specific surface area is 10m2/ more than g.

Description

There is the bar-shaped magnesium hydroxide particle of high-specific surface area and bar-shaped magnesium oxide Grain and their manufacture method
Technical field
The bar-shaped magnesium hydroxide particle that the present invention relates to there is high-specific surface area and bar-shaped magnesium oxide particle and it Manufacture method.
Background technology
Magnesium hydroxide particle and magnesium oxide particle are used for various field.As the purposes of magnesium hydroxide particle, The smears of InkJet paper, fire retardant, heat-storing material, catalyst and electronic material etc. can be listed, as magnesium oxide particle Purposes, can list optical material, the smears of InkJet paper, catalyst and electronic material etc..
Magnesium hydroxide particle is used for the smears of InkJet paper, fire retardant, heat-storing material, catalyst and electronic material use Following expectation is had time on the way.In smears, it is desirable to magnesium hydroxide particle has the affine of a large amount of OH bases of being had with dye ink An OH base that property is high and be easily adsorbed at the positive charge of the pigment inks with a large amount of negative charge and there is dyestuff easily infiltrate into The aggregate structure of intergranular.It addition, in fire retardant, heat-storing material and catalyst, it is desirable to the dispersibility of magnesium hydroxide particle is excellent Different, have display high response aggregate structure.And then, in electronic material, it is desirable to excellent dispersion, little hydroxide Magnesium granules.
When magnesium oxide particle is used for the purposes of optical material, the smears of InkJet paper, catalyst and electronic material etc. There is following expectation.In optical material, it is desirable to the excellent dispersion of magnesium oxide particle, there is the aggregation knot of easily diffusion light Structure.It addition, in the catalyst, it is desirable to the excellent dispersion of magnesium oxide particle, there is the aggregate structure of display high response.Enter And, in electronic material, it is desirable to excellent dispersion, little magnesium oxide particle.
Having recorded a kind of spherical magnesium hydroxide particle in patent documentation 1, it is by making sulfate ion ((SO4)2-〕/ Magnesium ion ((Mg)2+) ion concentration be set to the scope of 0.3～2.0 and obtain, have the lobule of more than 2 different directions (leaflet) structure that shape sheet combines and/or intersects.But, the method described in patent documentation 1 cannot be stably formed Spherical magnesium hydroxide, can be contaminated with the magnesium hydroxide of tabular and column, the dispersion to resin etc. of such magnesium hydroxide particle Property is insufficient, there is specific surface area low etc problem low, reactive when for catalyst etc..
Prior art literature
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 2003-261796 publication
Summary of the invention
The problem that invention is to be solved
It is an object of the invention to provide have the magnesium hydroxide particle of high-specific surface area and magnesium oxide particle and they Manufacture method.
For solving the scheme of problem
The inventors discovered that, the change of more than a kind in the group comprising the compound composition selecting free Zn, Zr, Hf and Ti In the dispersion liquid of compound, add the chloride of the metallic element selecting free divalent and trivalent and the nitre of the metallic element of divalent and trivalent The compound (wherein, in addition to the compound of Zn, Zr, Hf and Ti) of more than a kind in the group of hydrochlorate composition, and then add organic Acid and obtain reactant liquor, by this reactant liquor with make the surface portion of needle-like magnesium oxide particle be hydrated with constant temperature and humidity machine etc. Needle-like magnesium oxide particle mixes, and makes them carry out hydration reaction under high shear, thus can get excellent dispersion and reactivity The magnesium hydroxide particle high, there is high-specific surface area.It addition, the present inventor etc. find, by by the magnesium hydroxide of the present invention Granule in air atmosphere, calcine at 500 DEG C～1400 DEG C, can obtain the magnesium oxide particle with high-specific surface area.
That is, the present invention relates to a kind of magnesium hydroxide particle, it is bar-shaped for lepidiod agglomerated primary particles, utilizes 50% particle diameter (D of the volume-cumulative that laser diffraction and scattering formula particle size distribution obtains50) it is 1.0～10.0 μm, specific surface area For 10m2/ more than g.
The present invention relates to aforesaid magnesium hydroxide particle, it also comprises and is scaled 0.1～5.0 mass % with metallic element , select the metallic element of more than a kind in the group that free Zn, Zr, Hf and Ti form；Comprise with metallic element be scaled 0.1～ 5.0 mass %, more than a kind selected in the group that free divalent and trivalent metallic element form further metallic element is (wherein, In addition to Zn, Zr, Hf and Ti).
The present invention relates to a kind of magnesium oxide particle, it is bar-shaped for lepidiod agglomerated primary particles, utilizes laser 50% particle diameter (D of the volume-cumulative that diffraction scattering formula particle size distribution obtains50) it is 1.0～10.0 μm, specific surface area is 10m2/ more than g.
The present invention relates to aforesaid magnesium oxide particle, its also comprise with metallic element be scaled 0.1～5.0 mass %, Select the metallic element of in the group that free Zn, Zr, Hf and Ti form more than a kind；Comprise and be scaled 0.1～5.0 with metallic element The further metallic element of more than a kind in quality %, group that the metal that selects free divalent and trivalent forms (wherein, except Zn, Beyond Zr, Hf and Ti).
The present invention relates to the manufacture method of a kind of magnesium hydroxide particle, it includes following operation:
A () is to the dispersion of the compound of more than a kind comprised in the group that the compound selecting free Zn, Zr, Hf and Ti forms In liquid, add the nitrate composition of the chloride of the metallic element selecting free divalent and trivalent and the metallic element of divalent and trivalent The compound (wherein, in addition to the compound of Zn, Zr, Hf and Ti) of more than a kind in group, and be further added with machine acid and obtain Obtain the operation of reactant liquor；
B () is by 50% particle diameter (D of the volume-cumulative that utilizes laser diffraction and scattering formula particle size distribution to obtain50) it is 0.1 ～10 μm, specific surface area are 1.0～20.0m2/ g, calcination loss (Ig-loss) are the partially hydrated needle-like oxygen of 2.0～25.0% Change the reactant liquor mixing of magnesium and operation (a) and obtain the operation of mixed liquor,
(herein,
Select the compound of in the group that the compound of free Zn, Zr, Hf and Ti forms more than a kind relative to partially hydrated pin Shape magnesium oxide is scaled 0.1～5.0 mass % with metallic element,
The nitrate selecting the chloride of the metallic element of free divalent and trivalent and the metallic element of divalent and trivalent forms The compound of more than a kind in group is scaled 0.1～5.0 mass % relative to partially hydrated needle-like magnesium oxide with metallic element,
Organic acid is 0.01～3.0mol relative to partially hydrated needle-like magnesium oxide 100g)；
(c) by the mixed liquor of operation (b) at a temperature of 50～100 DEG C, use peripheral speed be 7～20m/s stirring Machine carries out the operation mixed；
D () is stirred at a temperature of 30～100 DEG C and obtains the operation of magnesium hydroxide slurry；And
E the magnesium hydroxide slurry of operation (d) is filtered by (), washing so that it is is dried and obtains the operation of magnesium hydroxide particle.
The present invention relates to aforesaid method, wherein, the partially hydrated needle-like magnesium oxide of operation (b) is by needle-like being aoxidized Magnesium granules is placed 0.5～24 hour in the constant temperature and humidity machine of temperature 40～95 DEG C, humidity 60～95% and is obtained, described pin 50% particle diameter (the D utilizing volume-cumulative that laser diffraction and scattering formula particle size distribution obtains of shape magnesium oxide particle50) it is 0.1 ～10 μm, specific surface area is 1.0～15.0m2/g。
The present invention relates to aforesaid method, wherein, the concentration of the partially hydrated needle-like magnesium oxide in the mixed liquor of operation (b) It is 20～200g/L.
The present invention relates to the manufacture method of a kind of magnesium oxide particle, it includes aforesaid magnesium hydroxide particle or passes through The operation that aforesaid method and the magnesium hydroxide particle that obtains carry out calcining in air atmosphere, at 500～1400 DEG C.
The effect of invention
According to the present invention, it is possible to provide have the bar-shaped hydrogen-oxygen of the lepidiod agglomerated primary particles of high-specific surface area Change magnesium granules and magnesium oxide particle and their manufacture method.Magnesium hydroxide particle and the magnesium oxide particle of the present invention have High-specific surface area and dispersibility, useful in various fields.It addition, manufacturing method according to the invention, can be easily Manufacture and there is high-specific surface area and the magnesium hydroxide particle of dispersibility and magnesium oxide particle.
Accompanying drawing explanation
Fig. 1 is the electron micrograph of the magnesium hydroxide particle of the present invention.One example of lepidiod primary granule is used White circular is irised out.
Detailed description of the invention
The magnesium hydroxide particle of the present invention is the bar-shaped of lepidiod agglomerated primary particles, utilizes laser diffraction and scattering 50% particle diameter (D of the volume-cumulative that formula particle size distribution obtains50) it is 1.0～10.0 μm, specific surface area is 10m2/ more than g.
The primary granule of the present invention be shaped as flakey.Figure 1 illustrates a lepidiod example.The flakey of the present invention The thickness of primary granule be 0.01～0.1 μm, the scope of preferably 0.01～0.05 μm, a diameter of the 0.2 of the circumscribed circle in face ～5 μm, the scope of preferably 0.5～2.5 μm.
Refer to it should be noted that bar-shaped in this specification, length in terms of the granule of lepidiod agglomerated primary particles Footpath ratio (particle length L/ grain section diameter D) is 1.5～20, is preferably the granule of the scope of 2～10.Herein, bar-shaped In the case of, specifically, L be 1～10 μm, D be the scope of 0.1～5 μm.It addition, needle-like refers to, draw ratio (particle length L/ Grain section diameter D) it is 21～1000, is preferably the granule of the scope of 50～500.Herein, in the case of needle-like, L is concrete It it is 0.1～10 μm, the D scope that is specially 0.001～0.5 μm.Referring to it addition, spherical, lepidiod agglomerated primary particles forms Ball shape and granule that draw ratio (particle length L/ grain section diameter D) is the scope of 1.0～1.2.Herein, spherical In the case of, L is specially 1～20 μm, D is specially the scope of 1～20 μm.
There is uniform pore at particle surface in the bar-shaped granule of such agglomerated primary particles, and by existing Manufacture method and the magnesium hydroxide particle (seeing Japanese Unexamined Patent Publication 2006-306659 publication) of hexagonal tabular that obtains compare, Owing to specific surface area is high, thus the adsorptivity of liquids and gases molecule is high.It addition, use such agglomerated primary particles When bar-shaped granule is as the smears of paper using, will not be the closeest owing to constituting the lepidiod magnesium hydroxide of bar-shaped granule Collection, therefore the adsorptivity of ink is good.
The magnesium hydroxide particle of the present invention is the bar-shaped of lepidiod agglomerated primary particles, utilizes laser diffraction and scattering 50% particle diameter (D of the volume-cumulative that formula particle size distribution obtains50) it is 1.0～10.0 μm, specific surface area is 10m2/ more than g. If such scope, then when the compoundings such as resin, viscosity will not be too high, and the gathering of granule is suppressed thus dispersibility Well.It addition, use when there is the magnesium hydroxide particle of such particle diameter as the smears of paper using, the fixation performance of ink and absorption Property is good.And then, particle diameter will not be excessive, thus useful as optical material and electronic material.The magnesium hydroxide particle of the present invention The 50% particle diameter (D utilizing volume-cumulative that laser diffraction and scattering formula particle size distribution obtains50) it is preferably 2.0～9.0 μm, More preferably 3.0～8.0 μm, specific surface area is preferably 10～200m2/ g, more preferably 20～150m2/g.The present invention compares table Area utilizes BET method to obtain.
The magnesium hydroxide particle of the present invention utilize volume reference that laser diffraction and scattering formula particle size distribution obtains Accumulate 90% particle diameter (D90) and accumulation 10% particle diameter (D10) ratio D90/D10It is preferably less than 10, the scope of more preferably 1～8. D is compared if such90/D10, then the narrow particle size distribution of magnesium hydroxide particle, granule gathering few, therefore available more excellent Dispersibility.
The magnesium hydroxide particle of the present invention can also comprise the metallic element of the compound used in its manufacturing process.This Invention magnesium hydroxide particle can comprise with metallic element be scaled 0.1～5.0 mass %, select free Zn, Zr, Hf and Ti The metallic element of more than a kind in the group of composition；And then comprise and be scaled 0.1～5.0 mass %, choosing freely with metallic element Divalent and trivalent metallic element composition group in more than a kind further metallic element (wherein, except Zn, Zr, Hf and Ti with Outward).If the content of these metallic elements, then, when using magnesium hydroxide particle as smears, there is sufficient whiteness, ultraviolet Line absorption and refractive index etc..Select in the group that free Zn, Zr, Hf and Ti form more than a kind metallic element, i.e. Zn, Zr, The content of Hf, Ti or their mixture is preferably 0.2～4.0 mass %, more preferably 0.3～3.0 with metallic element conversion Quality %.
In the present invention, as the further gold of more than a kind in the group selecting the metallic element of free divalent and trivalent to form Belong to element (wherein, in addition to Zn, Zr, Hf and Ti) be not particularly limited, can list Ag, Al, B, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, In, Mn, Mo, Ni, Pb, Sr, Tl and V, preferably Al and Fe.The metallic element selecting free divalent and trivalent forms Group in the content of further metallic element (in addition to Zn, Zr, Hf and Ti) of more than a kind be scaled with metallic element 0.1～5.0 mass %, preferably 0.2～4.0 mass %, more preferably 0.3～3.0 mass %.
The magnesium oxide particle of the present invention is the bar-shaped of lepidiod agglomerated primary particles, utilizes laser diffraction and scattering formula 50% particle diameter (D of the volume-cumulative that particle size distribution obtains50) it is 1.0～10.0 μm, specific surface area is 10m2/ more than g.This Invention primary granule be shaped as flakey, identical with a lepidiod example of Fig. 1.The lepidiod primary granule of the present invention Thickness be 0.01～0.1 μm, the scope of preferably 0.01～0.05 μm, a diameter of 0.2～5 μm of the circumscribed circle in face, preferably It it is the scope of 0.5～2.5 μm.Such magnesium oxide particle excellent dispersion to resin etc..Specifically, there is such grain When the magnesium oxide particle of footpath and specific surface area is used as the smears of paper using, fixation performance and the absorbability of ink are good.It addition, to resin Will not be too high Deng viscosity when coordinating, the gathering of granule is suppressed thus favorable dispersibility.And then, owing to particle diameter will not be excessive, Thus it is useful as optical material and electronic material.The magnesium oxide particle of the present invention utilize laser diffraction and scattering formula particle size distribution Measure 50% particle diameter (D of the volume-cumulative obtained50) it is preferably 2.0～9.0 μm, more preferably 3.0～8.0 μm, specific surface area It is preferably 10～200m2/ g, more preferably 20～150m2/g。
The magnesium oxide particle of the present invention utilize the tired of volume reference that laser diffraction and scattering formula particle size distribution obtains Long-pending 90% particle diameter (D90) and accumulation 10% particle diameter (D10) ratio D90/D10It is preferably less than 10, the scope of more preferably 1～8.If D is compared for such90/D10, then the narrow particle size distribution of magnesium oxide particle, granule gathering few, therefore available more excellent dispersion Property.
The magnesium oxide particle of the present invention can also comprise the metallic element of the compound used in its manufacturing process.This Bright magnesium oxide particle can comprise with metallic element be scaled 0.1～5.0 mass %, select free Zn, Zr, Hf and Ti form Group in the metallic element of more than a kind；And then comprise with metallic element be scaled 0.1～5.0 mass %, select free divalent And trivalent metallic element composition group in more than a kind further metallic element (wherein, except Zn, Zr, Hf and Ti with Outward).If the content of these metallic elements, then, when using magnesium oxide particle as smears, there is sufficient whiteness, ultraviolet Absorbability and refractive index etc..Select in the group that free Zn, Zr, Hf and Ti form more than a kind metallic element, i.e. Zn, Zr, Hf, The content of Ti or their mixture is to be preferably 0.2～4.0 mass %, more preferably 0.3～3.0 with metallic element conversion Quality %.
Further metallic element (its as more than a kind in the group selecting the metallic element of free divalent and trivalent to form In, in addition to Zn, Zr, Hf and Ti) be not particularly limited, can list Ag, Al, B, Ba, Bi, Cd, Co, Cr, Cu, Fe, Ga, In, Mn, Mo, Ni, Pb, Sr, Tl and V, preferably Al and Fe.Select a kind in the group that the metallic element of free divalent and trivalent forms The content of above further metallic element (wherein, in addition to Zn, Zr, Hf and Ti) is preferably 0.2 with metallic element conversion ～4.0 mass %, more preferably 0.3～3.0 mass %.
The manufacture method of the magnesium hydroxide particle of the present invention includes following operation:
A () is to the dispersion of the compound of more than a kind comprised in the group that the compound selecting free Zn, Zr, Hf and Ti forms In liquid, add the nitrate composition of the chloride of the metallic element selecting free divalent and trivalent and the metallic element of divalent and trivalent The compound (wherein, in addition to the compound of Zn, Zr, Hf and Ti) of more than a kind in group, and be further added with machine acid and obtain Obtain the operation of reactant liquor；
B () is by 50% particle diameter (D of the volume-cumulative that utilizes laser diffraction and scattering formula particle size distribution to obtain50) it is 0.1 ～10 μm, specific surface area are 1.0～20.0m2/ g, Ig-loss are 2.0～the partially hydrated needle-like magnesium oxide of 25.0% and operation A the reactant liquor of () mixes and obtains the operation of mixed liquor,
(herein,
Select the compound of in the group that the compound of free Zn, Zr, Hf and Ti forms more than a kind relative to partially hydrated pin Shape magnesium oxide is scaled 0.1～5.0 mass % with metallic element,
The nitrate selecting the chloride of the metallic element of free divalent and trivalent and the metallic element of divalent and trivalent forms The compound of more than a kind in group is scaled 0.1～5.0 mass % relative to partially hydrated needle-like magnesium oxide with metallic element,
Organic acid is 0.01～3.0mol relative to partially hydrated needle-like magnesium oxide 100g)；
(c) by the mixed liquor of operation (b) at a temperature of 50～100 DEG C, use peripheral speed be 7～20m/s stirring Machine carries out the operation mixed；
D () is stirred at a temperature of 30～100 DEG C and obtains the operation of magnesium hydroxide slurry；And
E the magnesium hydroxide slurry of operation (d) is filtered by (), washing so that it is is dried and obtains the operation of magnesium hydroxide particle.
Operation (a) is for obtaining the operation of the reactant liquor of the hydration reaction for part magnesium hydroxide.
The compound selecting in the group that the compound of free Zn, Zr, Hf and Ti forms more than a kind is to make the present invention Magnesium hydroxide particle and magnesium oxide particle and add.Thus, whiteness, ultraviolet-absorbing and refractive index etc. improve, and can obtain The magnesium hydroxide of the present invention and magnesium oxide particle to the smears being suitable to optical material, InkJet paper.
As the compound of Zn, Zr, Hf and Ti, as long as the compound with these metallic elements limits the most especially Fixed, oxide, hydroxide, hydride, halogenide (fluoride, chloride, bromide and iodide), phosphoric acid can be listed Salt, carbonate and nitrate etc., preferably zinc oxide, zinc hydroxide, zinc chloride, zinc nitrate, zirconium oxide, zirconium hydroxide, chlorination Zirconium, zirconium nitrate, hafnium oxide, hafnium hydroxide, hafnium chloride, hafnium nitrate, titanium oxide, titanium hydroxide, titanium chloride and Titanium Nitrate.
The purity of the compound of Zn, Zr, Hf and Ti is preferably more than 99.0%, and more preferably more than 99.5%.The present invention Moderate purity refers to, measure Zn, Zr, Hf and Ti compound in impurity element (Ag, Al, B, Ba, Bi, Ca, Cd, Cl, Co, Cr, Cu, Fe, Ga, Hf, In, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Si, Sr, Ti, Tl, V, Zn and Zr) content and from 100 The value deducting their total content in quality % and obtain.
It should be noted that as object constitute Zn, Zr, Hf and Ti compound itself element be equivalent to aforementioned Zn, Zr, Hf and Ti compound in impurity element time, this element is not included in impurity element.Such as, in operation (a) When the compound of Zn, Zr, Hf and Ti of using is ZnO, constitute the Zn chemical combination not included in aforesaid Zn, Zr, Hf and Ti of ZnO In impurity element in thing.As the method for the content measuring these impurity elements, use ICP emission spectrographic analysis dress can be enumerated The assay method put.
The D of the compound of Zn, Zr, Hf and Ti50It is preferably 0.1～100 μm, more preferably 0.5～50 μm.
Dispersion liquid as the compound of more than a kind in the group comprising the compound composition selecting free Zn, Zr, Hf and Ti In solvent, ion exchange water can be enumerated.The dispersion liquid used in operation (a) such as can be by adding in ion exchange water Select the compound of more than a kind in the group that the compound of free Zn, Zr, Hf and Ti forms and obtain.
The divalent used in operation (a) and the nitric acid of the metallic element of the chloride of the metallic element of trivalent and divalent and trivalent Salt is the dissolubility of the magnesium hydroxide particle in order to control the present invention and speed of separating out and adds.As divalent and the metal of trivalent The nitrate of the metallic element of the chloride of element and divalent and trivalent, preferably aluminum chloride, iron chloride, aluminum nitrate and nitric acid Ferrum.The purity of the nitrate of the metallic element of the chloride of the metallic element of divalent and trivalent and divalent and trivalent is preferably 99.0% Above, more preferably more than 99.5%.It addition, the chloride of the metallic element of divalent and trivalent and divalent and the metallic element of trivalent The D of nitrate50It is preferably 0.1～100 μm, more preferably 0.5～50 μm.
In the present invention, organic acid is in order to suppress raw material, the dissolubility of the most partially hydrated needle-like magnesium oxide and to add.Make For organic acid, aliphatic organic acid or the aromatic organic acid with carboxyl, preferably formic acid, acetic acid, propanoic acid, fourth can be listed Acid and benzoic acid.
Operation (b) is for by the reactant liquor for hydration reaction obtained in operation (a) and partially hydrated needle-like magnesium oxide The operation of grain mixing.The partially hydrated needle-like magnesium oxide particle used in operation (b) is for utilizing laser diffraction and scattering formula granularity to divide Cloth measures 50% particle diameter (D of the volume-cumulative obtained50) be 0.1～10 μm, specific surface area be 1.0～20.0m2/g、Ig-loss Be 2.0～25.0%, the part on surface is by the needle-like magnesium oxide of hydration, needle-like magnesium oxide that i.e. part is hydrated. By using such partially hydrated needle-like magnesium oxide, the lepidiod agglomerated primary particles that can obtain there is high-specific surface area and The bar-shaped magnesium hydroxide particle become.
In operation (b), the partially hydrated needle-like magnesium oxide particle of use utilizes laser diffraction and scattering formula particle size distribution 50% particle diameter (D of the volume-cumulative obtained50) less than 0.1 μm time, hydration rate becomes too fast, forms thick aggregated particle. It addition, D50During more than 10 μm, hydration reaction is the most fully carried out, and can remain the granule including magnesium oxide.D50Be preferably 0.1～ 5.0μm。
The specific surface area of the partially hydrated needle-like magnesium oxide particle used in operation (b) is more than 20.0m2During/g, hydration speed Degree becomes too fast, forms thick aggregated particle.It addition, specific surface area is less than 1.0m2During/g, hydration reaction is the most fully carried out, The granule including magnesium oxide can be remained.Specific surface area is preferably 2.0～18.0m2/ g, more preferably 3.0～15.0m2/g。
Water in the adhesive water of the partially hydrated needle-like magnesium oxide particle used in expression operation (b) and hydrate structure The Ig-loss (calcination loss) of the total divided is 2.0～25.0% (mass conversion).That is, the portion during Ig-loss represents the present invention Divide the degree of the hydration of hydration needle-like magnesium oxide particle.When Ig-loss is less than 2.0%, hydration rate easily becomes uneven, shape Become the unbodied thick aggregated particle that specific surface area is low.When Ig-loss is more than 25.0%, hydration reaction is suppressed, can be residual Stay the needle-like magnesium oxide not being hydrated, form thick aggregated particle, not as preferably.In order to make hydration reaction enter fully Going and then obtain the rod-like magnesium hydroxide with high-specific surface area, Ig-loss is preferably 2.0～20.0%, more preferably 3.0 ～18.0%.In the present invention, Ig-loss is by surveying after being calcined 3600 seconds at 1000 DEG C by partially hydrated needle-like magnesium oxide particle Determine and obtain.
The partially hydrated needle-like magnesium oxide used in such operation (b) can be by utilizing laser diffraction and scattering formula grain 50% particle diameter (D of the volume-cumulative that degree measure of spread obtains50) be 0.1～10 μm, specific surface area be 1.0～15.0m2The pin of/g Shape magnesium oxide particle temperature 40～95 DEG C and humidity 60～95% constant temperature and humidity machine in place 0.5～24 hour operation and Obtain.Ig-loss usually as the needle-like magnesium oxide of raw material is 0.1～1.0%, by increasing putting in constant temperature and humidity machine Put temperature and time, it is possible to make Ig-loss increase.
As the D of the needle-like magnesium oxide of the raw material of the partially hydrated needle-like magnesium oxide of use in operation (b)50It is preferably 0.1 ～5.0 μm.
It addition, as the specific surface of the needle-like magnesium oxide of the raw material of the partially hydrated needle-like magnesium oxide of preparation in operation (b) Long-pending preferably 2.0～15.0m2/ g, more preferably 3.0～15.0m2/g。
Preparation method as the needle-like magnesium oxide of the raw material of the partially hydrated needle-like magnesium oxide used in operation (b) does not has It is particularly limited to, such as, magnesium sulfate and sodium carbonate can be made to react and the magnesium carbonate purification of needle-like for preparing at 1200 DEG C Under calcine and obtain.
The amount of each composition that the partially hydrated needle-like magnesium oxide used in operation (b) and dispersion liquid are comprised is as follows.
Select the amount of compound of in the group that the compound of free Zn, Zr, Hf and Ti forms more than a kind relative to part water Close needle-like magnesium oxide particle, be scaled 0.1～5.0 mass % with metallic element.Select the compound group of free Zn, Zr, Hf and Ti When the amount of the compound in the group become is less than 0.1 mass %, when as smears, whiteness, ultraviolet-absorbing and refractive index Etc. insufficient, grain shape also will not become the rod-shpaed particle of lepidiod agglomerated primary particles, and becomes hexagonal tabular Granule.During it addition, select the amount of the compound in the group of the compound composition of free Zn, Zr, Hf and Ti to be more than 5.0 mass %, The rod-shpaed particle of the such lepidiod agglomerated primary particles of the present invention will not be become, and become the granule of hexagon prism shape. Select the amount of compound of in the group that the compound of free Zn, Zr, Hf and Ti forms more than a kind relative to partially hydrated needle-like oxygen Change magnesium granules and be preferably 0.2～4.0 mass %, more preferably 0.3～3.0 mass %.
The nitrate selecting the chloride of the metallic element of free divalent and trivalent and the metallic element of divalent and trivalent forms The amount of the compound of more than a kind in group relative to partially hydrated needle-like magnesium oxide particle, with metallic element be scaled 0.1～ 5.0 mass %.Addition less than 0.1 mass % time, the speed of separating out of crystal is slack-off, become monodispersed hexagonal column Grain, when addition is more than 5.0 mass %, the speed of separating out of crystal becomes too fast, can form thick aggregated particle.Choosing free 2 In the group of the nitrate composition of the metallic element of the chloride of the metallic element of valency and trivalent and divalent and trivalent more than a kind The amount of compound, relative to partially hydrated needle-like magnesium oxide particle, is preferably 0.2～4.0 mass % with metallic element conversion, more It is preferably 0.3～3.0 mass %.
The addition of organic acid is 0.01～3.0mol relative to partially hydrated needle-like magnesium oxide particle 100g.Organic acid When addition is less than 0.01mol relative to partially hydrated needle-like magnesium oxide particle 100g, the speed of separating out of crystal is slack-off, becomes single Scattered hexagonal plate or the granule of hexagonal column, during more than 3.0mol, the speed of separating out of crystal becomes too fast, can be formed thick Aggregated particle.The addition of organic acid is preferably 0.01～2.0mol relative to partially hydrated needle-like magnesium oxide 100g.
In operation (b), the concentration of the partially hydrated needle-like magnesium oxide in mixed liquor is preferably 20～200g/L, more preferably 50～180g/L, and then preferably 50～150g/L.That is, partially hydrated needle-like magnesium oxide is anti-relative to obtain in operation (a) It is preferred that the amount answering liquid adjusts to 20～200g/L, more preferably 50～180g/L, and then preferably 50～150g/L.If this The concentration of the partially hydrated needle-like magnesium oxide in the reactant liquor of sample, then hydration reaction is sufficiently carried out.
Operation (c) at a temperature of 50～100 DEG C, use peripheral speed be 7～20m/s blender carry out mixing Operation.The rotating speed of stirring is adjusted for dispersed when controlling reaction.
In the present invention, when peripheral speed is less than 7m/s, it is impossible to access the bar-shaped of lepidiod agglomerated primary particles Magnesium hydroxide.During it addition, peripheral speed is more than 20m/s, magnesium hydroxide particle exceedingly disperses when nucleus growth, becomes single point The hexagonal plate dissipated or the magnesium hydroxide particle of hexagonal column, it is impossible to access the such magnesium hydroxide particle of the present invention.As this The device for stirring of sample, being not particularly limited as long as meeting above-mentioned peripheral speed, can enumerate HOMODISPER (PRIMIX Corporation, T.K.HOMODISPER) etc..Peripheral speed is preferably 8～18m/s, more preferably 9～15m/s.Operation (c) In reaction temperature be preferably 55～95 DEG C, more preferably 60～95 DEG C.In operation (c), incorporation time can be anti-according to hydration The degree answered and change, such as can be set to 10～360 minutes, preferably 20～200 minutes.
Operation (d) obtains the operation of magnesium hydroxide slurry for being stirred at a temperature of 30～100 DEG C.Thus, may be used Magnesium hydroxide is made to promote the hydration reaction of unreacted partially hydrated needle-like magnesium oxide in operation (c).Temperature is preferably 50～95 DEG C, more preferably 70～90 DEG C.As long as mixing speed can be sufficiently stirred for the degree of magnesium hydroxide slurry, just It is not particularly limited, for example, it is possible to the blender of 3 blades and be set to 100～500rpm.As long as mixing time is fully entered Row hydration reaction and the time of available desired magnesium hydroxide slurry, be not particularly limited, such as can be set to 0.5～ 6 hours.
Operation (e) is by the magnesium hydroxide slurry filtration of operation (d), washing so that it is is dried and obtains magnesium hydroxide particle Operation.Thus, the magnesium hydroxide particle of the available present invention.
The magnesium oxide particle of the present invention is by including that the method for following operation obtains: by the magnesium hydroxide of the present invention Granule or the magnesium hydroxide particle that obtained by the manufacture method of the operation (a)～operation (e) that include the present invention are at air Calcine in atmosphere, at 500～1400 DEG C.
The calcining of magnesium hydroxide particle can be calcined by using electric furnace etc..Herein, calcining can be by including The method for calcinating of following operation and reach: be warming up to the operation of calcining heat and in calcining heat with the programming rate of regulation The operation of the lower time keeping regulation.Programming rate is preferably 1～20 DEG C/min, more preferably 3～10 DEG C/min.Calcining temperature Degree is 500～1400 DEG C, preferably 600～1300 DEG C.The time, the i.e. calcination time that keep at calcination temperatures are preferably 0.1 ～5 hours, more preferably 0.1～3 hour.Herein, when calcining heat is less than 500 DEG C, heat is inadequate, can remaining hydrogen magnesium oxide. On the other hand, when calcining heat is more than 1400 DEG C, magnesium oxide generation grain grows, and will not form bar-shaped magnesium oxide.
Consequently, it is possible to the bar-shaped magnesium hydroxide particle of available excellent dispersion and magnesium oxide particle.Pass through the present invention Manufacture method obtain magnesium hydroxide particle and magnesium oxide particle primary granule be preferably shaped to flakey, with Fig. 1's A lepidiod example is identical.The thickness of the lepidiod primary granule of the present invention is 0.01～0.1 μm, preferably 0.01～0.05 The scope of μm, a diameter of 0.2～5 μm of the circumscribed circle in face, the scope of preferably 0.5～2.5 μm.It is further preferred that by this The manufacture method of invention, the bar-shaped magnesium hydroxide particle of the lepidiod agglomerated primary particles of the available present invention and oxygen Change magnesium granules.
Embodiment
Hereinafter, by embodiment and comparative example, the present invention is described in further detail, but the invention is not restricted to these and implement Example.
[analysis method]
(1) laser diffraction and scattering formula particle size distribution
Use laser diffraction and scattering formula particle size distribution device (trade name: MT3300, NIKKISO CO., LTD. system), Measure the accumulation 10% particle diameter (D of volume reference10), the accumulation 50% particle diameter (D of volume reference50) and the accumulation of volume reference 90% particle diameter (D90)。
(2) the quality determination method of element
For become in granule measure object element (Ag, Al, B, Ba, Bi, Ca, Cd, Co, Cr, Cu, Fe, Ga, Hf, In, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, Si, Sr, Ti, Tl, V, Zn and Zr), use ICP emission spectrographic analysis device (business The name of an article: SPS-5100, Seiko Instruments Inc. system), by sample dissolution after acid, quality measurement.
For Cl, use spectrophotometer (trade name: UV-2550, Shimadzu Seisakusho Ltd.), by sample dissolution after acid, Quality measurement.
(3) BET specific surface area algoscopy
Use specific area measuring device (trade name: Macsorb1210, Mountech Co., Ltd. system), pass through gas Determination of adsorption method specific surface area.
(4) Ig-loss algoscopy
Use electric furnace (Wan Xiang electrical equipment Co., Ltd. system), with 1000 DEG C, under conditions of 3600 seconds, measure Ig-loss.
(embodiment 1)
By 50% particle diameter (D50) be 1.12 μm, specific surface area be 10.64m2The magnesium oxide of/g is in temperature 80 DEG C, humidity 90% Constant temperature and humidity machine in place 3 hours, make surface carry out partially hydrated, obtaining specific surface area is 13.46m2/ g, Ig-loss are The partially hydrated needle-like magnesium oxide of 9.08%, wherein, described magnesium oxide is anti-by Adlerika and sodium carbonate will be made to occur The needle-like magnesium carbonate answered and prepare carries out calcining at calcining heat 1200 DEG C and makes.
It is scaled 0.5 mass % with metallic element to the partially hydrated needle-like magnesium oxide comprised relative to using in reaction In the ion exchange water solution of zinc oxide and ion exchange water 1 liter, add the chlorination being scaled 0.5 mass % with metallic element Aluminum 6 hydrate and be the propanoic acid of 0.02mol relative to partially hydrated needle-like magnesium oxide 100g, thus makes reactant liquor.Will The temperature of the reactant liquor prepared is warming up to 60 DEG C, puts into and makes surface carry out partially hydrated magnesium oxide 100g, obtains mixed liquor. After putting into magnesium oxide, making the temperature of reactant liquor rise to 95 DEG C, (PRIMIX Corporation manufactures to use blender T.K.HOMODISPER) and regulating circumferential speed is 9.1m/s, reaction is made to carry out 1 hour.
Then, at 90 DEG C, with can be sufficiently stirred for the degree of slurry rotating speed stir 4 hours, thus make hydroxide Magnesium slurry.Prepared magnesium hydroxide slurry is filtered, washes so that it is be dried, thus obtain the rod-like magnesium hydroxide of the present invention Grain.
(embodiment 2)
Use aluminum sulfate to replace aluminum chloride, in addition, carry out similarly to Example 1.
(embodiment 3)
By needle-like magnesium oxide temperature 60 C, humidity 90% constant temperature and humidity machine in place 12 hours, make surface carry out portion Divide hydration, specific surface area is set to 10.18m2/ g, Ig-loss are set to 21.42%, in addition, enter similarly to Example 1 OK.
(embodiment 4)
The magnesium hydroxide prepared in embodiment 1 is carried out in air atmosphere the calcining of 600 DEG C × 1 hour, is aoxidized Magnesium granules.
(embodiment 5)
The magnesium hydroxide prepared in embodiment 1 is carried out in air atmosphere the calcining of 800 DEG C × 1 hour, is aoxidized Magnesium granules.
(embodiment 6)
The magnesium hydroxide prepared in embodiment 1 is carried out in air atmosphere the calcining of 1000 DEG C × 1 hour, is aoxidized Magnesium granules.
(embodiment 7)
Propanoic acid is changed to acetic acid, in addition, carries out similarly to Example 1.
(embodiment 9)
Propanoic acid is changed to butanoic acid, in addition, carries out similarly to Example 1.
(comparative example 1)
Use 50% particle diameter be 1.19 μm, specific surface area be 10.82m2/ g, be not the magnesium oxide of needle-like, in addition, Carry out similarly to Example 1.It should be noted that the Ig-loss as the magnesium oxide of raw material is 0.78%.
(comparative example 2)
The surface making magnesium oxide does not carry out partially hydrated and uses, and in addition, carries out similarly to Example 1.
(comparative example 3)
By needle-like magnesium oxide temperature 80 DEG C, humidity 90% constant temperature and humidity machine in place 12 hours, specific surface area is set For 8.09m2/ g, Ig-loss are set to 26.78%, in addition, carry out similarly to Example 1.
(comparative example 4)
By needle-like magnesium oxide temperature 60 C, humidity 90% constant temperature and humidity machine in place 3 hours, specific surface area is set to 12.41m2/ g, Ig-loss are set to 11.5%, calcining heat is set to 1500 DEG C, in addition, carry out similarly to Example 4.
Mensuration relevant with magnesium oxide particle for the magnesium hydroxide particle obtained by above embodiment and comparative example is measured Result is shown in Table 1.
[table 1]
[table 2]
By the result of table 1 it is clear that the magnesium hydroxide particle of the present invention and magnesium oxide particle are lepidiod primary It is bar-shaped that grain is assembled, 50% particle diameter (D50) it is 1.0～10.0 μm, specific surface area is 10m2/ more than g.It addition, confirm D90/D10It is less than 10, excellent dispersion.On the other hand, by the result of table 2 it is clear that comparative example 1 is spherical hydrogen-oxygen Change magnesium granules.It addition, the specific surface area of the magnesium hydroxide particle of comparative example 2 is 8.26m2/g.It addition, the hydroxide of comparative example 3 It is amorphous that the aggregation that magnesium granules is variously-shaped is mixed, and specific surface area is 7.45m2/g.It addition, the oxygen of comparative example 4 Change the growth of magnesium granules generation grain, thus lose shape when lepidiod magnesium hydroxide becomes magnesium oxide and become amorphous, than Surface area is 6.87m2/g。
Industrial applicability
The magnesium hydroxide of the present invention and the manufacture method of magnesium oxide only by by the magnesium oxide of raw material at constant temperature and humidity machine etc. In carry out hydration regulation, it becomes possible to control specific surface area simply, therefore can be easily manufactured magnesium hydroxide and magnesium oxide.
The magnesium hydroxide particle of the present invention and magnesium oxide particle are bar-shaped, and 50% particle diameter is little and uniform, favorable dispersibility, tool Having high-specific surface area, therefore the serviceability in various fields is high.It addition, the manufacture method of the present invention can be easily Manufacturing magnesium hydroxide as described above and magnesium oxide particle, therefore convenience is high.The magnesium hydroxide particle of the present invention can enumerate spray The ink smears of paper using, fire retardant, heat-storing material, catalyst and electronic material etc., as the purposes of magnesium oxide particle, can be used for The purposes of optical material, the smears of InkJet paper, catalyst and electronic material etc..

Claims (8)

1. a magnesium hydroxide particle, it is lepidiod agglomerated primary particles, particle length L and grain section diameter The ratio of D be 1.5～2.0 bar-shaped, utilize 50% particle diameter of the volume-cumulative that laser diffraction and scattering formula particle size distribution obtains D50Being 1.0～10.0 μm, specific surface area is 10m2/ more than g.
Magnesium hydroxide particle the most according to claim 1, it also comprises and is scaled 0.1～5.0 mass % with metallic element , select the metallic element of more than a kind in the group that free Zn, Zr, Hf and Ti form；Comprise with metallic element be scaled 0.1～ Entering of in 5.0 mass %, group that choosing freely divalent in addition to Zn, Zr, Hf and Ti and trivalent metallic element form more than a kind The metallic element of one step.
3. a magnesium oxide particle, it is lepidiod agglomerated primary particles, particle length L and grain section diameter D Ratio be 1.5～2.0 bar-shaped, utilize 50% particle diameter D of the volume-cumulative that laser diffraction and scattering formula particle size distribution obtains50 Being 1.0～10.0 μm, specific surface area is 10m2/ more than g.
Magnesium oxide particle the most according to claim 3, its also comprise with metallic element be scaled 0.1～5.0 mass %, Select the metallic element of in the group that free Zn, Zr, Hf and Ti form more than a kind；Comprise and be scaled 0.1～5.0 with metallic element In the group that quality %, choosing freely divalent in addition to Zn, Zr, Hf and Ti and trivalent metal forms more than a kind further Metallic element.
5. a manufacture method for magnesium hydroxide particle, it includes following operation:
(a) to comprise select free Zn, Zr, Hf and Ti compound composition group in more than a kind compound dispersion liquid in, Add chloride in addition to the compound of Zn, Zr, Hf and Ti, that select the metallic element of free divalent and trivalent and divalent and trivalent Metallic element nitrate composition group in the compound of more than a kind, and the machine that is further added with is sour and obtain reactant liquor Operation；
B () is by 50% particle diameter D of the volume-cumulative that utilizes laser diffraction and scattering formula particle size distribution to obtain50Be 0.1～10 μm, Specific surface area is 1.0～20.0m2/ g, calcination loss are 2.0～the partially hydrated needle-like magnesium oxide of 25.0% and operation (a) Reactant liquor mixes and obtains the operation of mixed liquor,
Herein,
Select the compound of in the group that the compound of free Zn, Zr, Hf and Ti forms more than a kind relative to partially hydrated needle-like oxygen Change magnesium and be scaled 0.1～5.0 mass % with metallic element,
Select in the group that the nitrate of the chloride of the metallic element of free divalent and trivalent and the metallic element of divalent and trivalent forms The compound of more than a kind be scaled 0.1～5.0 mass % relative to partially hydrated needle-like magnesium oxide with metallic element,
Organic acid is 0.01～3.0mol relative to partially hydrated needle-like magnesium oxide 100g；
(c) by the mixed liquor of operation (b) at a temperature of 50～100 DEG C, use peripheral speed be 7～20m/s blender enter The operation of row mixing；
D () is stirred at a temperature of 30～100 DEG C and obtains the operation of magnesium hydroxide slurry；And
E the magnesium hydroxide slurry of operation (d) is filtered by (), washing so that it is is dried and obtains the operation of magnesium hydroxide particle.
Method the most according to claim 5, wherein, the partially hydrated needle-like magnesium oxide of operation (b) is by by needle-like oxygen Change magnesium granules to place 0.5～24 hour in the constant temperature and humidity machine of temperature 40～95 DEG C, humidity 60～95% and obtain, described The 50% particle diameter D utilizing volume-cumulative that laser diffraction and scattering formula particle size distribution obtains of needle-like magnesium oxide particle50It is 0.1 ～10 μm, specific surface area is 1.0～15.0m2/g。
7. according to the method described in claim 5 or 6, wherein, partially hydrated needle-like magnesium oxide in the mixed liquor of operation (b) Concentration is 20～200g/L.
8. a manufacture method for magnesium oxide particle, it includes the magnesium hydroxide particle described in claim 1 or 2 or passes through Method according to any one of claim 5～7 and the magnesium hydroxide particle that obtains are in air atmosphere, at 500～1400 DEG C Carry out the operation calcined.
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