CN103827036A - Spherical magnesium hydroxide particles and magnesium oxide particles having a large specific surface area, as well as method for producing same - Google Patents
Spherical magnesium hydroxide particles and magnesium oxide particles having a large specific surface area, as well as method for producing same Download PDFInfo
- Publication number
- CN103827036A CN103827036A CN201280045052.XA CN201280045052A CN103827036A CN 103827036 A CN103827036 A CN 103827036A CN 201280045052 A CN201280045052 A CN 201280045052A CN 103827036 A CN103827036 A CN 103827036A
- Authority
- CN
- China
- Prior art keywords
- particle
- magnesium oxide
- magnesium hydroxide
- compound
- surface area
- 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.)
- Granted
Links
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/02—Compounds of alkaline earth metals or magnesium
- C09C1/028—Compounds containing only magnesium as metal
-
- D—TEXTILES; PAPER
- D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
- D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
- D21H19/00—Coated paper; Coating material
- D21H19/36—Coatings with pigments
- D21H19/38—Coatings with pigments characterised by the pigments
- D21H19/385—Oxides, hydroxides or carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/50—Solid solutions
- C01P2002/52—Solid solutions containing elements as dopants
-
- 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
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
- C01P2004/34—Spheres hollow
-
- 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
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- 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
-
- 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
- C01P2006/13—Surface area thermal stability thereof at high temperatures
Abstract
Provided are spherical magnesium hydroxide particles and magnesium oxide particles having a large specific surface area, as well as a method for producing the same. The magnesium hydroxide particles and magnesium oxide particles are spherical particles that are obtained when scale-like primary particles aggregate. The particles have a volume-cumulative 50% grain diameter (D50) as determined by laser diffraction scattering-type sizing that is between 1.0 and 5.0 [mu]m and a specific surface area of 10 m2/g or higher.
Description
Technical field
The present invention relates to have spherical magnesium hydroxide particle and spherical magnesium oxide particle and their manufacture method of high-specific surface area.
Background technology
Magnesium hydroxide particle and magnesium oxide particle are used to various fields.As the purposes of magnesium hydroxide particle, can list coating agent, fire retardant, heat-storing material, catalyzer and the electronic material etc. of ink-jet paper using; As the purposes of magnesium oxide particle, can list coating agent, catalyzer and the electronic material etc. of optical material, ink-jet paper using.
Magnesium hydroxide particle during for the coating agent of ink-jet paper using, fire retardant, heat-storing material, catalyzer and electronic material purposes, is had to following expectation.In coating agent, the positive charge that requires to there is the OH base that the affinity of a large amount of OH bases that have with dye ink is high and be easily adsorbed in the pigment inks with a large amount of negative charges, and there is dyestuff and easily infiltrate the magnesium hydroxide particle of intergranular aggregate structure.In addition, in fire retardant, heat-storing material and catalyzer, the magnesium hydroxide particle that require to there is excellent dispersion, shows the aggregate structure of hyperergy.And then, in electronic material, require magnesium hydroxide particle excellent dispersion, little.
Magnesium oxide particle during for purposes such as coating agent, catalyzer and the electronic materials of optical material, ink-jet paper using, is had to following expectation.In optical material, requirement has the magnesium oxide particle of the aggregate structure of excellent dispersion, easy diffusion light.In addition, in catalyzer, require the magnesium oxide particle of the aggregate structure of excellent dispersion, demonstration hyperergy.And then, in electronic material, require magnesium oxide particle excellent dispersion, little.
In patent documentation 1, recorded a kind of spherical magnesium hydroxide particle, it is by making sulfate ion ((SO
4)
2-)/magnesium ion ((Mg)
2+) ion concentration be 0.3～2.0 scope obtains and to there is loose page (leaflet) shape sheet bonding of more than 2 different directions and/or the structure that intersection forms.But, the method of recording in patent documentation 1 cannot stably form spherical magnesium hydroxide, mix and have tabular and magnesium hydroxide column, such magnesium hydroxide particle is insufficient to the dispersiveness of resin etc., has while use in catalyzer etc. that specific surface area is low, the low such problem of reactivity.
Prior art document
Patent documentation
Patent documentation 1: TOHKEMY 2003-261796 communique
Summary of the invention
the problem that invention will solve
The object of the present invention is to provide spherical magnesium hydroxide particle and the magnesium oxide particle with high-specific surface area, and their manufacture method.
The discoveries such as the inventor, select free Zn to comprising, Zr, in the dispersion liquid of a kind of above compound in the group of the compound composition of Hf and Ti, add the muriate that selects free divalent and 3 valency metallic elements, and a kind of above compound in the group of the nitrate of divalent and 3 valency metallic elements composition (wherein, Zn, Zr, except the compound of Hf and Ti), and then add organic acid and obtain reaction solution, by this reaction solution with in constant temperature humidifier etc., the surface magnesium oxide particle partially hydrated and that obtain of magnesium oxide particle is mixed, under high-shear, carry out hydration reaction, can obtain thus excellent dispersion, reactive high, there is the spherical magnesium hydroxide particle of high-specific surface area.In addition, the discoveries such as the inventor, by by magnesium hydroxide particle of the present invention in air atmosphere, calcine at 500 ℃～1400 ℃, can obtain having the spherical magnesium oxide particle of high-specific surface area.
That is, the present invention relates to magnesium hydroxide particle, it assembles for lepidiod primary particle form spherical, utilizes 50% particle diameter (D of the volume accumulation of laser diffraction and scattering formula particle size distribution
50) be 1.0～5.0 μ m, specific surface area is 10m
2more than/g.
The invention still further relates to aforementioned described magnesium hydroxide particle, it comprises with oxide compound and is scaled the metallic element in group 0.01～4.0 quality %, that select free Zn, Zr, Hf and Ti composition, comprise with metallic element and be scaled the further metallic element (wherein, except Zn, Zr, Hf and Ti) in group 0.01～5.0 quality %, that select free divalent and 3 valency metals composition.
The present invention relates to magnesium oxide particle, it assembles for lepidiod primary particle form spherical, utilizes 50% particle diameter (D of the volume accumulation of laser diffraction and scattering formula particle size distribution
50) be 1.0～5.0 μ m, specific surface area is 10m
2more than/g.
The invention still further relates to aforementioned described magnesium oxide particle, it comprises with oxide compound and is scaled the metallic element in group 0.01～4.0 quality %, that select free Zn, Zr, Hf and Ti composition, comprise with metallic element and be scaled the further metallic element (wherein, except Zn, Zr, Hf and Ti) in group 0.01～5.0 quality %, that select free divalent and 3 valency metals composition.
The present invention relates to the manufacture method of magnesium hydroxide particle, it comprises following operation:
(a) to adding the more than a kind compound that selects in the group that the muriate of free divalent and 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements forms in the dispersion liquid of the more than a kind compound in the group that comprises the compound composition that selects free Zn, Zr, Hf and Ti (wherein, except the compound of Zn, Zr, Hf and Ti), and further add organic acid and obtain the operation of reaction solution;
(b) by the reaction solution of operation (a) and utilize 50% particle diameter (D of the volume accumulation of laser diffraction and scattering formula particle size distribution
50) be that 0.1～10 μ m, specific surface area are 1.0～20.0m
2/ g, Ig-loss are 2.0～25.0% partially hydrated magnesium oxide mixing, obtain the operation of mixed solution
(herein,
Select a kind of above Compound Phase in the group of compound composition of free Zn, Zr, Hf and Ti for partially hydrated magnesium oxide, be scaled 0.1～5.0 quality % with oxide compound,
Select a kind of above Compound Phase in the group of the muriate of free divalent and 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements composition for partially hydrated magnesium oxide, be scaled 0.1～5.0 quality % with metallic element,
Organic acid is 0.01～3.0mol with respect to partially hydrated magnesium oxide 100g);
(c) operation of the mixed solution of operation (b) being mixed at the temperature of 50～100 ℃, with the stirrer that circumferential speed is 7～20m/s;
(d) at the temperature of 30～100 ℃, stir and obtain the operation of magnesium hydroxide slurry; And
(e) magnesium hydroxide slurry of operation (d) is filtered, washes, makes its operation dry and acquisition magnesium hydroxide particle.
The present invention relates to aforementioned described method, wherein, the partially hydrated magnesium oxide of operation (b) is by magnesium oxide particle is placed and obtained for 0.5～24 hour in the constant temperature high humidity machine of 40～95 ℃ of temperature, humidity 60～95%, 50% particle diameter (D of the volume accumulation that utilizes laser diffraction and scattering formula particle size distribution of described magnesium oxide particle
50) be that 0.1～10 μ m, specific surface area are 1.0～15.0m
2/ g.
The present invention relates to aforementioned described method, wherein, the partially hydrated magnesian concentration in the mixed solution of operation (b) is 20～200g/L.
The present invention relates to the manufacture method of magnesium oxide particle, it comprises the operation that the magnesium hydroxide particle obtaining by aforementioned described magnesium hydroxide particle or by aforementioned described method is calcined in air atmosphere, at 500～1400 ℃.
According to the present invention, spherical magnesium hydroxide particle and the magnesium oxide particle with high-specific surface area can be provided, and their manufacture method.Magnesium hydroxide particle of the present invention and magnesium oxide particle have high-specific surface area, have polymolecularity, in various fields, are useful.In addition, manufacturing method according to the invention, can easily manufacture magnesium hydroxide particle and magnesium oxide particle.
Accompanying drawing explanation
Fig. 1 is the electron micrograph of magnesium hydroxide particle of the present invention.
Embodiment
Magnesium hydroxide particle of the present invention is that lepidiod primary particle is assembled form spherical, utilizes 50% particle diameter (D of the volume accumulation of laser diffraction and scattering formula particle size distribution
50) be 1.0～5.0 μ m, specific surface area is 10m
2more than/g.In the present invention, primary particle be shaped as flakey, the thickness (minor axis) of scale is for example 0.01～0.1 μ m, the maximum length of scale is for example 10～1000 with respect to the ratio (length-to-diameter ratio) of thickness.Such primary particle is assembled the spherical particle forming and is had uniform pore at particle surface, compared with the magnesium hydroxide particle tabular with the hexagonal obtaining by existing manufacture method, because specific surface area is high compared with adsorptivity high and liquids and gases molecule, spherical and high to the dispersiveness of resin etc. owing to being shaped as.In addition, when this primary particle is assembled the spherical particle that forms and used as the coating agent of paper using, because the glomerate flakey magnesium hydroxide of structure can be too not intensive, therefore the adsorptivity of China ink is good.
The D of magnesium hydroxide particle of the present invention
50be 1.0～5.0 μ m, specific surface area is 10m
2more than/g.Such scope if, can not become too high in compounding viscosity in resin etc. time, can suppress in addition the gathering of particle, therefore favorable dispersity.In addition, while use in the coating agent using the magnesium hydroxide particle with such particle diameter as paper using, particle can be outstanding from black receiving layer, and fixation performance and the absorptivity of China ink are good.And then particle diameter can be not excessive, for optical material and electronic material, be therefore useful.The D of magnesium hydroxide particle of the present invention
50be preferably 2.0～5.0 μ m, more preferably 3.0～5.0 μ m; Specific surface area is preferably 10～120m
2/ g, more preferably 20～100m
2/ g.In the present invention, specific surface area is obtained by BET method.
The accumulation 10% particle diameter (D of the volume reference of utilizing laser diffraction and scattering formula particle size distribution of magnesium hydroxide powder of the present invention
10) and accumulation 90% particle diameter (D
90) ratio D
90/ D
10be preferably below 3, more preferably 1～3 scope.Such ratio D if
90/ D
10, the size-grade distribution of magnesium hydroxide powder is narrow, and the gathering of particle is few, therefore can obtain more excellent dispersiveness.
Magnesium hydroxide particle of the present invention can also be included in the metallic element of the compound using in its manufacturing process.Magnesium hydroxide particle of the present invention comprises with oxide compound and is scaled a kind of above metallic element in group 0.01～4.0 quality %, that select free Zn, Zr, Hf and Ti composition, comprise with metallic element and be scaled a kind of above further metallic element (wherein, except Zn, Zr, Hf and Ti) in group 0.01～5.0 quality %, that select free divalent and 3 valency metallic elements composition.The content of these metallic elements if, using magnesium hydroxide particle when coating agent uses, whiteness, ultraviolet-absorbing and specific refractory power etc. are abundant.Select a kind of above metallic element in the group of free Zn, Zr, Hf and Ti composition, the content of Zn, Zr, Hf, Ti or their mixture converts with oxide compound, be preferably 0.05～4.0 quality %, more preferably 0.05～3.0 quality %, more preferably 0.05～2.5 quality %.
In the present invention, as a kind in the group of selecting free divalent and 3 valency metallic elements to form above further metallic element (wherein, except 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 of above further metallic element in the group of free divalent and 3 valency metallic elements composition (wherein, except Zn, Zr, Hf and Ti) content convert with metallic element, be preferably 0.05～5.0 quality %, more preferably 0.1～5.0 quality %, more preferably 0.3～4.0 quality %.
Magnesium oxide particle of the present invention is that lepidiod primary particle is assembled form spherical, utilizes 50% particle diameter (D of the volume accumulation of laser diffraction and scattering formula particle size distribution
50) be 1.0～5.0 μ m, specific surface area is 10m
2more than/g.The excellent dispersion of such magnesium oxide particle to resin etc.Particularly, when the magnesium oxide particle with such particle diameter and specific surface area uses in the coating agent as paper using, particle can be not outstanding from black receiving layer, the fixation performance of China ink and absorptivity are good or can not become too high in compounding viscosity in resin etc. time, can suppress particle aggregation, therefore favorable dispersity.And particle diameter can be not excessive, for optical material and electronic material, be therefore useful.The D of magnesium oxide particle of the present invention
50be preferably 2.0～5.0 μ m, more preferably 3.0～5.0 μ m; Specific surface area is preferably 10～120m
2/ g, more preferably 20～100m
2/ g.
The accumulation 10% particle diameter (D of the volume reference of utilizing laser diffraction and scattering formula particle size distribution of magnesium oxide powder of the present invention
10) and accumulation 90% particle diameter (D
90) ratio D
90/ D
10be preferably below 3, more preferably 1～3 scope.Ratio D if so
90/ D
10, the size-grade distribution of magnesium oxide powder is narrow, and the gathering of particle is few, therefore can obtain more excellent dispersiveness.
Magnesium oxide particle of the present invention can also be included in the metallic element of the compound using in its manufacturing process.Magnesium oxide particle of the present invention comprises with oxide compound and is scaled a kind of above metallic element in group 0.01～4.0 quality %, that select free Zn, Zr, Hf and Ti composition, comprise with metallic element and be scaled a kind of above further metallic element (wherein, except Zn, Zr, Hf and Ti) in group 0.01～5.0 quality %, that select free divalent and 3 valency metallic elements composition.The content of such metallic element if, using magnesium oxide particle when coating agent uses, whiteness, ultraviolet-absorbing and specific refractory power etc. are abundant.Select a kind of above metallic element in the group of free Zn, Zr, Hf and Ti composition, the content of Zn, Zr, Hf, Ti or their mixture converts with oxide compound, be preferably 0.05～4.0 quality %, more preferably 0.2～4.0 quality %, more preferably 0.4～4.0 quality %.
As a kind in the group of selecting free divalent and 3 valency metallic elements to form above further metallic element (wherein, except 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 of above further metallic element in the group of free divalent and 3 valency metallic elements composition (wherein, except Zn, Zr, Hf and Ti) content convert with metallic element, be preferably 0.1～5.0 quality %, more preferably 0.3～4.0 quality %, more preferably 0.4～4.0 quality %.
The manufacture method of magnesium hydroxide particle of the present invention comprises following operation:
(a) to adding the more than a kind compound that selects in the group that the muriate of free divalent and 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements forms in the dispersion liquid of the more than a kind compound in the group that comprises the compound composition that selects free Zn, Zr, Hf and Ti (wherein, except the compound of Zn, Zr, Hf and Ti), and further add organic acid and obtain reaction solution operation,
(b) by the reaction solution of operation (a) and utilize 50% particle diameter (D of the volume accumulation of laser diffraction and scattering formula particle size distribution
50) be that 0.1～10 μ m, specific surface area are 1.0～20.0m
2/ g, Ig-loss are 2.0～25.0% partially hydrated magnesium oxide mixing, obtain the operation of mixed solution
(herein,
Select a kind of above Compound Phase in the group of compound composition of free Zn, Zr, Hf and Ti for partially hydrated magnesium oxide, be scaled 0.1～5.0 quality % with oxide compound,
Select a kind of above Compound Phase in the group of the muriate of free divalent and 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements composition for partially hydrated magnesium oxide, be scaled 0.1～5.0 quality % with metallic element,
Organic acid is 0.01～3.0mol with respect to partially hydrated magnesium oxide 100g);
(c) operation of the mixed solution of operation (b) being mixed at the temperature of 50～100 ℃, with the stirrer that circumferential speed is 7～20m/s;
(d) at the temperature of 30～100 ℃, stir and obtain the operation of magnesium hydroxide slurry; And
(e) magnesium hydroxide slurry of operation (d) is filtered, washes, makes its operation dry and acquisition magnesium hydroxide particle.
Operation (a) is for obtaining the operation for the reaction solution of magnesian hydration reaction.Select a kind of above compound in the group of compound composition of free Zn, Zr, Hf and Ti to add in order to make as complex hydroxide and the composite oxides of magnesium hydroxide particle of the present invention and magnesium oxide particle.Thus, the raisings such as whiteness, ultraviolet-absorbing and specific refractory power, can obtain magnesium hydroxide of the present invention and the magnesium oxide particle of the coating agent that is suitable for optical material, ink-jet paper using.
As the compound of Zn, Zr, Hf and Ti, as long as the compound with these metallic elements is just not particularly limited, can list oxide compound, oxyhydroxide, hydride, halogenide (fluorochemical, muriate, bromide and iodide), phosphoric acid salt, carbonate and nitrate etc., preferential oxidation zinc, zinc hydroxide, zinc chloride, zinc nitrate, zirconium white, zirconium hydroxide, zirconium chloride, zirconium nitrate, hafnia, 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%, more preferably more than 99.5%.In the present invention, purity refers to the content of measuring the impurity element (Ag, Al, B, Ba, Bi, Cd, Cl, Co, Cr, Cu, Fe, Ga, In, K, Li, Mg, Mn, Mo, Na, Ni, P, Pb, S, Si, Sr, Tl, V, Zn, Ti and Zr) in the compound of Zn, Zr, Hf and Ti, deducts their total content and the value that obtains from 100 quality %.It should be noted that, form while being equivalent to the impurity element in the compound of aforementioned Zn, Zr, Hf and Ti as the element of the compound of Zn, Zr, Hf and the Ti of object itself, this element is not included in impurity element.For example, the compound of Zn, Zr, Hf and the Ti using in operation (a) is during for ZnO, in the impurity element of the Zn that forms ZnO not included in the compound of aforementioned Zn, Zr, Hf and Ti.As the measuring method of the content of these impurity elements, can list the measuring method that uses ICP emmission spectrometric analysis device.The D of the compound of Zn, Zr, Hf and Ti
50be preferably 0.1～100 μ m, more preferably 0.5～50 μ m.
As the solvent in the dispersion liquid of a kind of above compound in the group that comprises the compound composition that selects free Zn, Zr, Hf and Ti, can list ion exchanged water.In operation (a), dispersion liquid used for example can obtain by the more than a kind compound adding in ion exchanged water in the group of the compound composition that selects free Zn, Zr, Hf and Ti.
The nitrate of the muriate of divalent and 3 valency metallic elements and divalent and 3 valency metallic elements adds for solubleness and the speed of separating out of controlling magnesium hydroxide particle of the present invention.As the muriate of divalent and 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements, preferably aluminum chloride, iron(ic) chloride, aluminum nitrate and iron nitrate.The purity of the nitrate of the muriate of divalent and 3 valency metallic elements and divalent and 3 valency metallic elements is preferably more than 99.0%, more preferably more than 99.5%.In addition, the D of the nitrate of the muriate of divalent and 3 valency metallic elements and divalent and 3 valency metallic elements
50be preferably 0.1～100 μ m, more preferably 0.5～50 μ m.
In the present invention, organic acid adds in order to control as the solubleness of the magnesium oxide particle of raw material.As organic acid, can list aliphatics or the aromatic organic acid with carboxyl, preferable formic acid, acetic acid, propionic acid, butyric acid and phenylformic acid.
Operation (b) is the operation that the reaction solution for hydration reaction obtaining in operation (a) is mixed with partially hydrated magnesium oxide particle.In operation (b), partially hydrated magnesium oxide particle used is that the activity degree of magnesium oxide particle has been carried out to the partially hydrated magnesium oxide particle regulating.In operation (b), partially hydrated magnesium oxide particle used is the 50% particle diameter (D that utilizes the volume accumulation of laser diffraction and scattering formula particle size distribution
50) be that 0.1～10 μ m, specific surface area are 1.0～20.0m
2/ g, Ig-loss are the magnesium oxide that a part 2.0～25.0%, surface has been carried out hydration, and part is carried out the magnesium oxide that hydration forms.By using so partially hydrated magnesium oxide, can obtain the magnesium hydroxide particle with high-specific surface area.
The D of partially hydrated magnesium oxide particle used in operation (b)
50while being less than 0.1 μ m, it is too fast that hydration rate becomes, and can become thick aggregated particles.In addition, D
50while being greater than 10 μ m, hydration reaction cannot fully be carried out and residually be comprised magnesian particle.D
50be preferably 0.1～5.0 μ m.In operation (b), the specific surface area of partially hydrated magnesium oxide particle used exceedes 20.0m
2when/g, it is too fast that hydration rate becomes, and can become thick aggregated particles.In addition, specific surface area is lower than 1.0m
2when/g, hydration reaction cannot fully be carried out and residually be comprised magnesian particle.Specific surface area is preferably 2.0～18.0m
2/ g, more preferably 3.0～15.0m
2/ g.
The Ig-loss(calcination loss of the total amount of the moisture in expression operation (b) in adhesive water and the hydrate structure of partially hydrated magnesium oxide particle used) be 2.0～25.0%., Ig-loss represents the hydration levels in the partially hydrated magnesium oxide particle in the present invention.When Ig-loss exceedes 25.0%, hydration reaction is suppressed, and has unhydrated magnesium oxide residual, is not preferred.For hydration reaction is fully carried out, and then obtain having the magnesium hydroxide of high-specific surface area, Ig-loss is preferably 2.0～20.0%, and more preferably 3.0～18.0%.In the present invention, Ig-loss measures and obtains by partially hydrated magnesium oxide particle being calcined under 1273K after 3600 seconds.
The partially hydrated magnesium oxide of preparing in this operation (b) can obtain by the operation that magnesium oxide particle is placed 0.5～24 hour in the constant temperature high humidity machine of 40～95 ℃ of temperature, humidity 60～95%, 50% particle diameter (D of the volume accumulation that utilizes laser diffraction and scattering formula particle size distribution of described magnesium oxide particle
50) be 0.1～10 μ m, specific surface area is 1.0～15.0m
2/ g.Conventionally, be 0.1～1.0% as the magnesian Ig-loss of raw material, by being increased in the time of placing in constant temperature high humidity machine, can make Ig-loss increase.Become the magnesian D of the partially hydrated magnesian raw material of preparing in operation (b)
50be preferably 0.1～5.0 μ m.In addition, the magnesian specific surface area that becomes the partially hydrated magnesian raw material of preparing in operation (b) is preferably 2.0～15.0m
2/ g, more preferably 3.0～15.0m
2/ g.
The amount of the each composition comprising in partially hydrated magnesium oxide used and dispersion liquid in operation (b) is as described below.
Select the amount of a kind of above compound in the group of compound composition of free Zn, Zr, Hf and Ti with respect to partially hydrated magnesium oxide particle, be scaled 0.1～5.0 quality % with oxide compound.While selecting the amount of the compound in the group of compound composition of free Zn, Zr, Hf and Ti to be less than 0.1 quality %, in situation about using as coating agent, whiteness, ultraviolet-absorbing and specific refractory power etc. are insufficient, particle shape can not become lepidiod primary particle yet and assemble the spherical particle forming, but becomes the tabular particle of hexagonal.In addition, while selecting the amount of the compound in the group of compound composition of free Zn, Zr, Hf and Ti to be greater than 5.0 quality %, can not become the so lepidiod primary particle of the present invention and assemble the spherical particle forming, but become the particle of hexa-prism.Select the amount of a kind of above compound in the group of compound composition of free Zn, Zr, Hf and Ti with respect to partially hydrated magnesium oxide particle, be preferably 0.4～4.0 quality %.
Select the amount of a kind of above compound in the group of the muriate of free divalent and 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements composition with respect to partially hydrated magnesium oxide particle, be scaled 0.1～5.0 quality % with metallic element.When addition is less than 0.1 quality %, the speed of separating out of crystal is slack-off, becomes monodispersed hexa-prism particle; When addition is greater than 5.0 quality %, the speed of separating out of crystal becomes too fast, becomes thick aggregated particles.Select the amount of a kind of above compound in the group of the muriate of free divalent and 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements composition with respect to partially hydrated magnesium oxide particle, with metallic element more preferably 0.4～4.0 quality % that converts.
Organic acid addition is 0.01～3.0mol with respect to partially hydrated magnesium oxide particle 100g.When organic acid addition is less than 0.01mol with respect to partially hydrated magnesium oxide particle 100g, the speed of separating out of crystal is slack-off, becomes monodispersed hexa-prism particle; While being greater than 3.0mol, the speed of separating out of crystal becomes too fast, becomes thick aggregated particles.Organic acid addition, with respect to partially hydrated magnesium oxide 100g, is preferably 0.01～2.0mol.
In operation (b), the partially hydrated magnesian concentration in mixed solution is preferably 20～200g/L, more preferably 50～180g/L, more preferably 50～150g/L., partially hydrated magnesium oxide is adjusted to 20～200g/L for preferred with respect to the amount of the reaction solution of the middle acquisition of operation (a), more preferably 50～180g/L, more preferably 50～150g/L.Partially hydrated magnesium oxide concentration in such reaction solution if, hydration reaction is carried out fully.
In operation (b), the temperature of reaction solution is preferably 50～100 ℃, and more preferably 50～95 ℃, more preferably 70～90 ℃.Such temperature if, hydration reaction is carried out fully.
Operation (c) is the operation that the stirrer of 7～20m/s mixes for use circumferential speed at the temperature of 50～100 ℃.Dispersion state while reaction in order to control, can regulate the revolution stirring.When circumferential speed is less than 7m/s, cannot obtains lepidiod primary particle and assemble the spherical magnesium hydroxide forming.In addition, when circumferential speed is greater than 20m/s, magnesium hydroxide particle fully disperses in the time of karyogenesis, forms monodispersed hexa-prism magnesium hydroxide particle, cannot obtain the so spherical magnesium hydroxide particle of the present invention.As the device for this stirring, can list HOMODISPER(PRIMIX Corporation, T.K.HOMODISPER) etc.Circumferential speed is preferably 8～18m/s, more preferably 9～15m/s.Temperature of reaction in operation (c) is preferably 55～95 ℃, more preferably 60～95 ℃.In operation (c), mixing time can change according to the degree of hydration reaction, for example, can be made as 10～360 minutes, is preferably made as 20～200 minutes.
Operation (d) is for stirring the operation that obtains magnesium hydroxide slurry at the temperature at 30～100 ℃.Thus, promote unreacted partially hydrated magnesian hydration reaction in operation (c), can make magnesium hydroxide.Temperature is preferably 50～95 ℃, more preferably 70～90 ℃.Stirring velocity, as long as can fully stirring the degree of magnesium hydroxide slurry, is not particularly limited, for example, can and be made as 100～500rpm with the stirrer of 3 blades.The time that the magnesium hydroxide slurry of expectation is fully carried out, can be obtained to churning time as long as hydration reaction is just not particularly limited, for example, can be made as 0.5～6 hour.
Operation (e) is for filtering the magnesium hydroxide slurry of operation (d), wash, make its dry operation that obtains magnesium hydroxide particle.Thus, can obtain magnesium hydroxide particle of the present invention.
Magnesium oxide particle of the present invention is that the method by comprising following operation obtains: by magnesium hydroxide particle of the present invention or by comprising that magnesium hydroxide particle that the manufacture method of operation of the present invention (a)～operation (e) obtains calcines in air atmosphere, at 500～1400 ℃.Preferably obtain by the method that is included in the operation of calcining at 600～1300 ℃.For example, by magnesium hydroxide particle of the present invention or by comprising that the magnesium hydroxide particle that the manufacture method of operation of the present invention (a)～operation (e) obtains is warming up to 500～1400 ℃, is preferably 600～1300 ℃ with 1～20 ℃/min of heat-up rate (preferably 3～10 ℃/min) in air atmosphere, after intensification 500～1400 ℃, preferably calcine 0.1～5 hour at 600～1300 ℃, can obtain thus magnesium oxide particle of the present invention.Calcining temperature is during lower than 500 ℃, shortage of heat and have magnesium hydroxide residual.On the other hand, when calcining temperature exceedes 1400 ℃, magnesium oxide generation grain growing, can not form lepidiod primary particle and assemble the spherical magnesium oxide forming.
So operate, can obtain spherical magnesium hydroxide particle and the magnesium oxide particle of excellent dispersion.Magnesium hydroxide of the present invention and magnesian manufacture method can be only control ratio surface-area by carrying out hydration adjusting in constant temperature high humidity machine etc. as the magnesium oxide of raw material and simply, therefore can easily manufacture magnesium hydroxide and magnesium oxide.
Magnesium hydroxide particle of the present invention and magnesium oxide particle are spherical, and median size is little and even, and favorable dispersity has high-specific surface area, and therefore in various fields, availability is high.In addition, manufacture method of the present invention can easily be prepared magnesium hydroxide as described above and magnesium oxide particle, and therefore convenience is high.The purposes of magnesium hydroxide particle of the present invention can list coating agent, fire retardant, heat-storing material, catalyzer and the electronic material etc. of ink-jet paper using, as the purposes of magnesium oxide particle, can be for purposes such as coating agent, catalyzer and the electronic materials of optical material, ink-jet paper using.
Embodiment
Below, further describe the present invention in detail by embodiment and comparative example, but the present invention is not limited by these embodiment.
［ analytical procedure ］
(1) laser diffraction and scattering formula particle size distribution
Use laser diffraction and scattering formula particle size distribution device (trade(brand)name: MT3300, NIKKISO CO., LTD. manufactures), measure the accumulation 10% particle diameter (D of volume reference
10), the accumulation 50% particle diameter (D of volume reference
50) and the accumulation 90% particle diameter (D of volume reference
90).
(2) the quality determination method of element
For the element (Al, Fe, Zn, Zr, Hf, Ti) that becomes the determination object in particle, use ICP emmission spectrometric analysis device (trade(brand)name: SPS-5100, Seiko Instruments Inc. manufacture), by sample dissolution quality measurement after acid.
(3) BET specific area measuring method
Use specific area measuring device (trade(brand)name: Macsorb1210, Mountech Co., Ltd. manufactures), by gas adsorption method measurement the specific area.
(4) Ig-loss assay method
Use electric furnace (manufactures of Wan Xiang electrical equipment Co., Ltd.), according to 1273K, the condition mensuration Ig-loss of 3600 seconds.
(embodiment 1)
By median size (D
50) be that 1.08 μ m, specific surface area are 10.94m
2the magnesium oxide of/g is placed 3 hours in the constant temperature high humidity machine of 80 ℃ of temperature, humidity 90%, surface is carried out partially hydrated, and obtaining specific surface area is 13.11m
2/ g, Ig-loss are 9.08% partially hydrated magnesium oxide.
With respect to the partially hydrated magnesium oxide using in reaction, in the ion-exchange aqueous solution of 1 liter of the zinc oxide that comprises 0.5 quality % and ion exchanged water, add the aluminum chloride hexahydrate that is scaled 0.5 quality % with metallic element, and the propionic acid that is 0.02mol with respect to partially hydrated magnesium oxide 100g, make thus reaction solution.Make the temperature of the reaction solution of making be warming up to 60 ℃, drop into 100g and make surface carry out partially hydrated magnesium oxide, obtain mixed solution.Drop into after magnesium oxide, make the temperature rise to 95 ℃ of reaction solution, using stirrer (PRIMIX Corporation manufactures T.K.homodisper) regulating circumferential speed is 9m/s, and reaction is carried out 1 hour.
Thereafter, at 90 ℃, with can fully stir slurry degree speed of rotation stir 4 hours, make thus magnesium hydroxide slurry.Filter, wash, make it to be dried the magnesium hydroxide slurry of making and obtain magnesium hydroxide particle of the present invention.
(embodiment 2)
Be that 2.58 μ m, specific surface area are 3.59m by median size
2the magnesium oxide of/g is placed 1 hour in the constant temperature high humidity machine of temperature 60 C, humidity 90%, surface is carried out partially hydrated, and making specific surface area is 4.23m
2/ g, Ig-loss are 4.72%, in addition, carry out similarly to Example 1.
(embodiment 3)
Be that 0.68 μ m, specific surface area are 12.68m by median size
2the magnesium oxide of/g is placed 24 hours in the constant temperature high humidity machine of temperature 60 C, humidity 90%, surface is carried out partially hydrated, and making specific surface area is 16.72m
2/ g, Ig-loss are 16.97%, in addition, carry out similarly to Example 1.
(embodiment 4)
The addition of zinc oxide is made as to 3.0 quality %, in addition, carries out similarly to Example 1.
(embodiment 5)
The addition of zinc oxide is made as to 0.1 quality %, in addition, carries out similarly to Example 1.
(embodiment 6)
Propionic acid is become to the acetic acid of 0.02mol, in addition, carry out similarly to Example 1.
(embodiment 7)
Propionic acid is become to the butyric acid of 0.02mol, in addition, carry out similarly to Example 1.
(embodiment 8)
The magnesium hydroxide of making in embodiment 1 is calcined 800 ℃ × 1 hour in air atmosphere, obtained magnesium oxide particle.
(comparative example 1)
Using median size is that 5.88 μ m, specific surface area are 1.34m
2the magnesium oxide of/g and not make its surface carry out partially hydrated, in addition, carries out similarly to Example 1.It should be noted that, be 0.44% as the magnesian Ig-loss of raw material.
(comparative example 2)
Be that 0.76 μ m, specific surface area are 19.68m by median size
2place 1 hour in the constant temperature high humidity machine of temperature 60 C, humidity 90% on the magnesian surface of/g, surface is carried out partially hydrated, and making specific surface area is 20.78m
2/ g, Ig-loss are 2.58%, in addition, carry out similarly to Example 1.
(comparative example 3)
Be that 1.86 μ m, specific surface area are 1.59m by median size
2the magnesium oxide of/g is placed 30 hours in the constant temperature high humidity machine of 80 ℃ of temperature, humidity 90%, and making specific surface area is 3.8m
2/ g, Ig-loss are 25.3%, in addition, carry out similarly to Example 1.
(comparative example 4)
The magnesium hydroxide of making in embodiment 1 is calcined 1500 ℃ × 1 hour in air atmosphere, obtained magnesium oxide particle.
Measurement result about the magnesium hydroxide particle obtaining by above embodiment and magnesium oxide particle is shown in table 1, is shown in about the measurement result of the magnesium hydroxide particle obtaining by comparative example and magnesium oxide particle
Table 2.
[table 1]
[table 2]
Claims (8)
1. a magnesium hydroxide particle, it assembles for lepidiod primary particle form spherical, utilizes 50% particle diameter D of the volume accumulation of laser diffraction and scattering formula particle size distribution
50be 1.0～5.0 μ m, specific surface area is 10m
2more than/g.
2. magnesium hydroxide particle according to claim 1, it also comprises with oxide compound and is scaled the metallic element in group 0.01～4.0 quality %, that select free Zn, Zr, Hf and Ti composition, comprise with metallic element be scaled 0.01～5.0 quality %, in the choosing group that freely divalent except Zn, Zr, Hf and Ti and 3 valency metals form further metallic element.
3. a magnesium oxide particle, it assembles for lepidiod primary particle form spherical, utilizes 50% particle diameter D of the volume accumulation of laser diffraction and scattering formula particle size distribution
50be 1.0～5.0 μ m, specific surface area is 10m
2more than/g.
4. magnesium oxide particle according to claim 3, it also comprises with oxide compound and is scaled the metallic element in group 0.01～4.0 quality %, that select free Zn, Zr, Hf and Ti composition, comprises with metallic element and is scaled further metallic element 0.01～5.0 quality %, in the choosing group that freely divalent except Zn, Zr, Hf and Ti and 3 valency metals form.
5. a manufacture method for magnesium hydroxide particle, it comprises following operation:
(a) be selected from the more than a kind compound in group except the compound of Zn, Zr, Hf and Ti, that formed by the muriate of divalent and 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements to interpolation in the dispersion liquid of the more than a kind compound in the group that comprises the compound composition that selects free Zn, Zr, Hf and Ti, and further add organic acid and obtain the operation of reaction solution;
(b) by the reaction solution of operation (a) and utilize 50% particle diameter D of the volume accumulation of laser diffraction and scattering formula particle size distribution
50be that 0.1～10 μ m, specific surface area are 1.0～20.0m
2/ g, Ig-loss are 2.0～25.0% partially hydrated magnesium oxide mixing, obtain the operation of mixed solution,
Herein,
Select a kind of above Compound Phase in the group of compound composition of free Zn, Zr, Hf and Ti for partially hydrated magnesium oxide, be scaled 0.1～5.0 quality % with oxide compound,
Select a kind of above Compound Phase in the group of the muriate of free divalent and 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements composition for partially hydrated magnesium oxide, be scaled 0.1～5.0 quality % with metallic element,
Organic acid is 0.01～3.0mol with respect to partially hydrated magnesium oxide 100g;
(c) operation of the mixed solution of operation (b) being mixed at the temperature of 50～100 ℃, with the stirrer that circumferential speed is 7～20m/s;
(d) at the temperature of 30～100 ℃, stir and obtain the operation of magnesium hydroxide slurry; And
(e) magnesium hydroxide slurry of operation (d) is filtered, washes, makes its operation dry and acquisition magnesium hydroxide particle.
6. method according to claim 5, wherein, the partially hydrated magnesium oxide of operation (b) is by magnesium oxide particle is placed and obtained for 0.5～24 hour in the constant temperature high humidity machine of 40～95 ℃ of temperature, humidity 60～95%, 50% particle diameter D of the volume accumulation that utilizes laser diffraction and scattering formula particle size distribution of described magnesium oxide particle
50be that 0.1～10 μ m, specific surface area are 1.0～15.0m
2/ g.
7. according to the method described in claim 5 or 6, wherein, the partially hydrated magnesian concentration in the mixed solution of operation (b) is 20～200g/L.
8. a manufacture method for magnesium oxide particle, it comprises the operation that the magnesium hydroxide particle that the magnesium hydroxide particle described in claim 1 or 2 or the method by described in any one in claim 5～7 are obtained is calcined in air atmosphere, at 500～1400 ℃.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011-203776 | 2011-09-16 | ||
| JP2011203776A JP5864178B2 (en) | 2011-09-16 | 2011-09-16 | Spherical magnesium hydroxide particles having a high specific surface area, spherical magnesium oxide particles, and methods for producing them |
| PCT/JP2012/073169 WO2013039055A1 (en) | 2011-09-16 | 2012-09-11 | Spherical magnesium hydroxide particles and magnesium oxide particles having a large specific surface area, as well as method for producing same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103827036A true CN103827036A (en) | 2014-05-28 |
| CN103827036B CN103827036B (en) | 2015-11-25 |
Family
ID=47883285
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201280045052.XA Active CN103827036B (en) | 2011-09-16 | 2012-09-11 | There is the spherical magnesium hydroxide particle of high-specific surface area and spherical magnesium oxide particle and their manufacture method |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP5864178B2 (en) |
| KR (1) | KR101878846B1 (en) |
| CN (1) | CN103827036B (en) |
| TW (1) | TWI546257B (en) |
| WO (1) | WO2013039055A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109293246A (en) * | 2018-10-29 | 2019-02-01 | 刘凡领 | A kind of preparation method of high insulated heat seal glass |
| CN109516538A (en) * | 2017-09-19 | 2019-03-26 | 宇部材料工业株式会社 | Red tide expellent and the red tide expelling method for using it |
| CN111717926A (en) * | 2020-07-31 | 2020-09-29 | 河北镁神科技股份有限公司 | Preparation method of magnesium oxide for plastic master batch and magnesium oxide prepared by preparation method |
| CN115926492A (en) * | 2022-11-07 | 2023-04-07 | 广东金戈新材料股份有限公司 | Preparation method and use method of mineralizer capable of reducing oil absorption value of magnesium oxide |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101878963B1 (en) * | 2016-05-13 | 2018-07-16 | 코노시마카가쿠코우교우 가부시키가이샤 | Magnesium oxide powder and manufacturing method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04224873A (en) * | 1990-12-26 | 1992-08-14 | Risho Kogyo Co Ltd | Filler for sealing resin and preparation thereof |
| JPH06171928A (en) * | 1992-12-01 | 1994-06-21 | Kyowa Chem Ind Co Ltd | Production of magnesium oxide high in hydration resistance and high in fluidity |
| JP2000357537A (en) * | 1999-06-16 | 2000-12-26 | Mitsubishi Chemicals Corp | Magnesium oxide for purification of nonaqueous electrolyte and its preparation |
| CN101679058A (en) * | 2007-03-30 | 2010-03-24 | 宇部材料工业株式会社 | Magnesium hydroxide powder and preparation method thereof |
| CN101687659A (en) * | 2007-06-27 | 2010-03-31 | 达泰豪化学工业株式会社 | Magnesium oxide particle aggregate, and method for production thereof |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6136119A (en) * | 1984-07-27 | 1986-02-20 | Asahi Glass Co Ltd | Production of highly water-resistant magnesium oxide |
| JP4412879B2 (en) | 2002-03-11 | 2010-02-10 | メルク株式会社 | Extender pigment and method for producing the same |
| JP2007217201A (en) * | 2006-02-14 | 2007-08-30 | Merck Ltd | Porous magnesia and method for producing the same |
-
2011
- 2011-09-16 JP JP2011203776A patent/JP5864178B2/en active Active
-
2012
- 2012-09-11 KR KR1020147001904A patent/KR101878846B1/en active IP Right Grant
- 2012-09-11 WO PCT/JP2012/073169 patent/WO2013039055A1/en active Application Filing
- 2012-09-11 CN CN201280045052.XA patent/CN103827036B/en active Active
- 2012-09-14 TW TW101133638A patent/TWI546257B/en active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH04224873A (en) * | 1990-12-26 | 1992-08-14 | Risho Kogyo Co Ltd | Filler for sealing resin and preparation thereof |
| JPH06171928A (en) * | 1992-12-01 | 1994-06-21 | Kyowa Chem Ind Co Ltd | Production of magnesium oxide high in hydration resistance and high in fluidity |
| JP2000357537A (en) * | 1999-06-16 | 2000-12-26 | Mitsubishi Chemicals Corp | Magnesium oxide for purification of nonaqueous electrolyte and its preparation |
| CN101679058A (en) * | 2007-03-30 | 2010-03-24 | 宇部材料工业株式会社 | Magnesium hydroxide powder and preparation method thereof |
| CN101687659A (en) * | 2007-06-27 | 2010-03-31 | 达泰豪化学工业株式会社 | Magnesium oxide particle aggregate, and method for production thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109516538A (en) * | 2017-09-19 | 2019-03-26 | 宇部材料工业株式会社 | Red tide expellent and the red tide expelling method for using it |
| CN109293246A (en) * | 2018-10-29 | 2019-02-01 | 刘凡领 | A kind of preparation method of high insulated heat seal glass |
| CN111717926A (en) * | 2020-07-31 | 2020-09-29 | 河北镁神科技股份有限公司 | Preparation method of magnesium oxide for plastic master batch and magnesium oxide prepared by preparation method |
| CN115926492A (en) * | 2022-11-07 | 2023-04-07 | 广东金戈新材料股份有限公司 | Preparation method and use method of mineralizer capable of reducing oil absorption value of magnesium oxide |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2013063878A (en) | 2013-04-11 |
| CN103827036B (en) | 2015-11-25 |
| WO2013039055A1 (en) | 2013-03-21 |
| KR101878846B1 (en) | 2018-07-17 |
| JP5864178B2 (en) | 2016-02-17 |
| TW201323334A (en) | 2013-06-16 |
| TWI546257B (en) | 2016-08-21 |
| KR20140063575A (en) | 2014-05-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103443028B (en) | Spherical magnesium hydroxide particle and spherical magnesium oxide particle and their manufacture method | |
| CN105008281A (en) | Rod-like magnesium hydroxide particle and rod-like magnesium oxide particle each having high specific surface area, and methods respectively for producing said particles | |
| JP6190023B1 (en) | Method for producing zirconium tungstate phosphate | |
| CN103827036B (en) | There is the spherical magnesium hydroxide particle of high-specific surface area and spherical magnesium oxide particle and their manufacture method | |
| CN105377766B (en) | Nickel-manganese is compound oxyhydroxide, its manufacturing method and application thereof | |
| CA2905519C (en) | Complexometric precursor formulation methodology for industrial production of fine and ultrafine powders and nanopowders of layered lithium mixed metal oxides for battery applications | |
| WO2011030786A1 (en) | Ferric phosphate hydrate particle powder and process for production thereof, olivine-type lithium iron phosphate particle powder and process for production thereof, and non-aqueous electrolyte secondary battery | |
| KR102030866B1 (en) | Metal-containing trimanganese tetraoxide composite particles and method for producing same | |
| CN107376827A (en) | A kind of zirconia-coated manganese systems lithium ion sieve and its preparation method and application | |
| WO2011040593A1 (en) | Magnesium oxide powder having excellent dispersion properties and method of manufacturing same | |
| JP4801617B2 (en) | Conductive zinc oxide particles and method for producing the same | |
| CN110194480A (en) | A kind of nano-cerium oxide and preparation method thereof | |
| CN102040381A (en) | Method for preparing superfine zirconia powder | |
| CN105948098A (en) | Spherical lanthanum oxide | |
| TWI596062B (en) | Trimanganese tetroxide and its manufacturing method | |
| CN102030372B (en) | Preparation method of nano spinel zinc manganate | |
| TWI386369B (en) | Magnesium oxide powder | |
| TWI580100B (en) | Nickel lithium metal composite oxide, and a nickel-lithium metal composite oxide obtained by the production method and a positive electrode active material composed of a nickel-lithium metal composite oxide | |
| JP6031177B2 (en) | Spherical magnesium hydroxide particles having a high specific surface area and method for producing the same | |
| JP2007055880A (en) | Method for producing metal oxide particulate powder | |
| JP7280573B2 (en) | Method for producing precursor of lithium adsorbent | |
| WO2019235573A1 (en) | Lithium-manganese-based composite oxide and method for producing same | |
| JP5558287B2 (en) | Aluminum-doped zinc oxide particles and method for producing the same | |
| JP7428456B1 (en) | Surface-treated calcium carbonate and resin composition using the same | |
| KR20150054769A (en) | Loosely aggregated thin film magnesium oxide particles |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |