CN103827036B - There is the spherical magnesium hydroxide particle of high-specific surface area and spherical magnesium oxide particle and their manufacture method - Google Patents
There is the spherical magnesium hydroxide particle of high-specific surface area and spherical magnesium oxide particle and their manufacture method Download PDFInfo
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Abstract
The invention provides the spherical magnesium hydroxide particle and magnesium oxide particle and their manufacture method with high-specific surface area.A kind of magnesium hydroxide particle and magnesium oxide particle, it is spherical for lepidiod primary particle gathering, utilizes 50% particle diameter (D of the volume-cumulative of laser diffraction and scattering formula particle size distribution
50) be 1.0 ~ 5.0 μm, specific surface area is 10m
2/ more than g.
Description
Technical field
The present invention relates to the spherical magnesium hydroxide particle and spherical magnesium oxide particle and their manufacture method with high-specific surface area.
Background technology
Magnesium hydroxide particle and magnesium oxide particle are used to various field.As the purposes of magnesium hydroxide particle, the coating agent of InkJet paper, fire retardant, heat-storing material, catalyzer and electronic material etc. can be listed; As the purposes of magnesium oxide particle, optical material, the coating agent of InkJet paper, catalyzer and electronic material etc. can be listed.
When magnesium hydroxide particle being used for the coating agent of InkJet paper, fire retardant, heat-storing material, catalyzer and electronic material purposes, there is following expectation.In coating agent, require the positive charge that there is the high OH base of the affinity of a large amount of OH bases had with dye ink and be easily adsorbed in the pigment inks with a large amount of negative charge, and there is the magnesium hydroxide particle that dyestuff easily infiltrates intergranular aggregate structure.In addition, in fire retardant, heat-storing material and catalyzer, the magnesium hydroxide particle require that there is excellent dispersion, showing the aggregate structure of hyperergy.And then, in electronic material, that require excellent dispersion, little magnesium hydroxide particle.
Magnesium oxide particle is used for optical material, InkJet paper coating agent, the purposes such as catalyzer and electronic material time, have following expectation.In optical material, require the magnesium oxide particle with excellent dispersion, the easily aggregate structure of diffusion light.In addition, in the catalyst, the magnesium oxide particle of the aggregate structure of excellent dispersion, display hyperergy is required.And then, in electronic material, that require excellent dispersion, little magnesium oxide particle.
Describe a kind of spherical magnesium hydroxide particle in patent documentation 1, it is by making sulfate ion ((SO
4)
2-)/magnesium ion ((Mg)
2+) ion concentration be 0.3 ~ 2.0 scope obtain, and there is loose page (leaflet) the shape sheet bonding of more than 2 different directions and/or the structure of intersection.But, the method recorded in patent documentation 1 cannot stably form spherical magnesium hydroxide, mix the magnesium hydroxide having tabular and column, the dispersiveness of such magnesium hydroxide particle to resin etc. is insufficient, has low, the reactive low such problem of specific surface area when middle uses such as catalyzer.
Prior art document
Patent documentation
Patent documentation 1: Japanese Unexamined Patent Publication 2003-261796 publication
Summary of the invention
the problem that invention will solve
The object of the present invention is to provide the spherical magnesium hydroxide particle and magnesium oxide particle with high-specific surface area, and their manufacture method.
The discoveries such as the present inventor, be selected from by Zn to comprising, Zr, the muriate be selected from by divalent and 3 valency metallic elements is added in the dispersion liquid of the compound of more than a kind in the group of the compound composition of Hf and Ti, and divalent and 3 valency metallic elements nitrate composition group in the compound of more than a kind (wherein, Zn, Zr, except the compound of Hf and Ti), and then add organic acid and obtain reaction solution, this reaction solution is made the surface portion hydration of magnesium oxide particle with in constant temperature humidifier etc. and the magnesium oxide particle obtained mixes, carry out hydration reaction under high shear, excellent dispersion can be obtained thus, reactive high, there is the spherical magnesium hydroxide particle of high-specific surface area.In addition, the discoveries such as the present inventor, by by magnesium hydroxide particle of the present invention in air atmosphere, calcine at 500 DEG C ~ 1400 DEG C, the spherical magnesium oxide particle with high-specific surface area can be obtained.
That is, the present invention relates to magnesium hydroxide particle, it is spherical for lepidiod primary particle gathering, utilizes 50% particle diameter (D of the volume-cumulative of laser diffraction and scattering formula particle size distribution
50) be 1.0 ~ 5.0 μm, specific surface area is 10m
2/ more than g.
The invention still further relates to aforementioned described magnesium hydroxide particle, its comprise with oxide compound be scaled 0.01 ~ 4.0 quality %, the metallic element be selected from the group that is made up of Zn, Zr, Hf and Ti, comprise with metallic element be scaled 0.01 ~ 5.0 quality %, the further metallic element (wherein, except Zn, Zr, Hf and Ti) be selected from the group that is made up of divalent and 3 valency metals.
The present invention relates to magnesium oxide particle, it is spherical for lepidiod primary particle gathering, utilizes 50% particle diameter (D of the volume-cumulative of laser diffraction and scattering formula particle size distribution
50) be 1.0 ~ 5.0 μm, specific surface area is 10m
2/ more than g.
The invention still further relates to aforementioned described magnesium oxide particle, its comprise with oxide compound be scaled 0.01 ~ 4.0 quality %, the metallic element be selected from the group that is made up of Zn, Zr, Hf and Ti, comprise with metallic element be scaled 0.01 ~ 5.0 quality %, the further metallic element (wherein, except Zn, Zr, Hf and Ti) be selected from the group that is made up of divalent and 3 valency metals.
The present invention relates to the manufacture method of magnesium hydroxide particle, it comprises following operation:
A () adds the compound of more than a kind in the group being selected from and being made up of divalent and the muriate of 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements (wherein in the dispersion liquid of the compound of more than a kind comprised in the group that is selected from and is made up of the compound of Zn, Zr, Hf and Ti, except the compound of Zn, Zr, Hf and Ti), and further add organic acid and obtain the operation of reaction solution;
B () is by the reaction solution of operation (a) and the 50% particle diameter (D of volume-cumulative utilizing laser diffraction and scattering formula particle size distribution
50) be 0.1 ~ 10 μm, specific surface area is 1.0 ~ 20.0m
2/ g, Ig-loss are the partially hydrated magnesium oxide mixing of 2.0 ~ 25.0%, obtain the operation of mixed solution
(herein,
The Compound Phase being selected from more than a kind in the group be made up of the compound of Zn, Zr, Hf and Ti, for partially hydrated magnesium oxide, is scaled 0.1 ~ 5.0 quality % with oxide compound,
Be selected from the Compound Phase of more than a kind in the group be made up of divalent and the muriate of 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements for partially hydrated magnesium oxide, be scaled 0.1 ~ 5.0 quality % with metallic element,
Organic acid is 0.01 ~ 3.0mol relative to partially hydrated magnesium oxide 100g);
(c) by the mixed solution of operation (b) at the temperature of 50 ~ 100 DEG C, be the operation that the stirrer of 7 ~ 20m/s carries out mixing by circumferential speed;
D () carries out stirring and obtains the operation of magnesium hydroxide slurry at the temperature of 30 ~ 100 DEG C; And
E the magnesium hydroxide slurry of operation (d) filters by (), wash, make it dry and obtain the operation of magnesium hydroxide particle.
The present invention relates to aforementioned described method, wherein, the partially hydrated magnesium oxide of operation (b) obtains by being placed 0.5 ~ 24 hour in the constant temperature high humidity machine of temperature 40 ~ 95 DEG C, humidity 60 ~ 95% by magnesium oxide particle, the 50% particle diameter (D utilizing the volume-cumulative of laser diffraction and scattering formula particle size distribution of described magnesium oxide particle
50) be 0.1 ~ 10 μm, specific surface area is 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 operation that the present invention relates to the manufacture method of magnesium oxide particle, it to be comprised aforementioned described magnesium hydroxide particle or the magnesium hydroxide particle that obtained by aforementioned described method in air atmosphere, carry out calcining at 500 ~ 1400 DEG C.
According to the present invention, the spherical magnesium hydroxide particle and 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, are useful in various field.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 the spherical of lepidiod primary particle gathering, utilizes 50% particle diameter (D of the volume-cumulative of laser diffraction and scattering formula particle size distribution
50) be 1.0 ~ 5.0 μm, specific surface area is 10m
2/ more than g.In the present invention, the shape of primary particle is flakey, and the thickness (minor axis) of scale is such as 0.01 ~ 0.1 μm, and the maximum length of scale is such as 10 ~ 1000 relative to the ratio (length-to-diameter ratio) of thickness.Uniform pore is there is in the spherical particle that such primary particle is assembled at particle surface, compared with the magnesium hydroxide particle of the hexagonal tabular obtained by existing manufacture method, because specific surface area is higher, the adsorptivity of liquids and gases molecule is high, because shape is spherical and high to the dispersiveness of resin etc.In addition, when being used as the coating agent of paper using by the spherical particle of this primary particle gathering, because structure glomerate flakey magnesium hydroxide can not be too intensive, therefore the adsorptivity of ink is good.
The D of magnesium hydroxide particle of the present invention
50be 1.0 ~ 5.0 μm, specific surface area is 10m
2/ more than g.If be such scope, then compounding in resin etc. time viscosity can not become too high, the gathering of particle can be suppressed in addition, therefore favorable dispersity.In addition, when the magnesium hydroxide particle that will have such particle diameter uses as the coating agent of paper using, particle can not be given prominence to from black receiving layer, and fixation performance and the absorptivity of ink are good.And then particle diameter can not be excessive, be therefore useful for optical material and electronic material.The D of magnesium hydroxide particle of the present invention
50be preferably 2.0 ~ 5.0 μm, be more preferably 3.0 ~ 5.0 μm; Specific surface area is preferably 10 ~ 120m
2/ g, is more preferably 20 ~ 100m
2/ g.In the present invention, specific surface area is obtained by BET method.
The accumulation 10% particle diameter (D utilizing the volume reference of 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 less than 3, be more preferably the scope of 1 ~ 3.If be such ratio D
90/ D
10, then the narrow particle size distribution of magnesium hydroxide powder, 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 used in its manufacturing process.Magnesium hydroxide particle of the present invention comprise with oxide compound be scaled 0.01 ~ 4.0 quality %, the metallic element of more than a kind be selected from the group that is made up of Zn, Zr, Hf and Ti, comprise with metallic element be scaled 0.01 ~ 5.0 quality %, the further metallic element (wherein, except Zn, Zr, Hf and Ti) of more than a kind be selected from the group that is made up of divalent and 3 valency metallic elements.If be the content of these metallic elements, then when being used as coating agent by magnesium hydroxide particle, whiteness, ultraviolet-absorbing and specific refractory power etc. are abundant.The content of metallic element, i.e. Zn, Zr, Hf, Ti or their mixture of being selected from more than a kind in the group be made up of Zn, Zr, Hf and Ti converts with oxide compound, be preferably 0.05 ~ 4.0 quality %, be more preferably 0.05 ~ 3.0 quality %, more preferably 0.05 ~ 2.5 quality %.
In the present invention, as the further metallic element of more than a kind be selected from the group that is made up of divalent and 3 valency metallic elements (wherein, except Zn, Zr, Hf and Ti), be not particularly limited, Ag, Al, B, Ba, Bi, Cd, Co, Cr, Cu, Fe, Ga, In, Mn, Mo, Ni, Pb, Sr, Tl and V can be listed, preferred Al and Fe.Be selected from the further metallic element of more than a kind in the group be made up of divalent and 3 valency metallic elements (wherein, except Zn, Zr, Hf and Ti) content convert with metallic element, be preferably 0.05 ~ 5.0 quality %, be more preferably 0.1 ~ 5.0 quality %, more preferably 0.3 ~ 4.0 quality %.
Magnesium oxide particle of the present invention is the spherical of lepidiod primary particle gathering, utilizes 50% particle diameter (D of the volume-cumulative of laser diffraction and scattering formula particle size distribution
50) be 1.0 ~ 5.0 μm, specific surface area is 10m
2/ more than g.Such magnesium oxide particle is to the excellent dispersion of resin etc.Specifically, there is the magnesium oxide particle of such particle diameter and specific surface area when the coating agent as paper using uses, particle can not be given prominence to from black receiving layer, the fixation performance of ink and absorptivity is good or compounding in resin etc. time viscosity can not become too high, particle aggregation can be suppressed, therefore favorable dispersity.And particle diameter can not be excessive, be therefore useful for optical material and electronic material.The D of magnesium oxide particle of the present invention
50be preferably 2.0 ~ 5.0 μm, be more preferably 3.0 ~ 5.0 μm; Specific surface area is preferably 10 ~ 120m
2/ g, is more preferably 20 ~ 100m
2/ g.
The accumulation 10% particle diameter (D utilizing the volume reference of 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 less than 3, be more preferably the scope of 1 ~ 3.If such ratio D
90/ D
10, then the narrow particle size distribution of magnesium oxide powder, the gathering of particle is few, therefore, it is possible to obtain more excellent dispersiveness.
Magnesium oxide particle of the present invention can also be included in the metallic element of the compound used in its manufacturing process.Magnesium oxide particle of the present invention comprise with oxide compound be scaled 0.01 ~ 4.0 quality %, the metallic element of more than a kind be selected from the group that is made up of Zn, Zr, Hf and Ti, comprise with metallic element be scaled 0.01 ~ 5.0 quality %, the further metallic element (wherein, except Zn, Zr, Hf and Ti) of more than a kind be selected from the group that is made up of divalent and 3 valency metallic elements.If be the content of such metallic element, then when being used as coating agent by magnesium oxide particle, whiteness, ultraviolet-absorbing and specific refractory power etc. are abundant.The content of metallic element, i.e. Zn, Zr, Hf, Ti or their mixture of being selected from more than a kind in the group be made up of Zn, Zr, Hf and Ti converts with oxide compound, be preferably 0.05 ~ 4.0 quality %, be more preferably 0.2 ~ 4.0 quality %, more preferably 0.4 ~ 4.0 quality %.
As the further metallic element of more than a kind be selected from the group that is made up of divalent and 3 valency metallic elements (wherein, except Zn, Zr, Hf and Ti), be not particularly limited, Ag, Al, B, Ba, Bi, Cd, Co, Cr, Cu, Fe, Ga, In, Mn, Mo, Ni, Pb, Sr, Tl and V can be listed, preferred Al and Fe.Be selected from the further metallic element of more than a kind in the group be made up of divalent and 3 valency metallic elements (wherein, except Zn, Zr, Hf and Ti) content convert with metallic element, be preferably 0.1 ~ 5.0 quality %, be 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 () adds the compound of more than a kind in the group being selected from and being made up of divalent and the muriate of 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements (wherein in the dispersion liquid of the compound of more than a kind comprised in the group that is selected from and is made up of the compound of Zn, Zr, Hf and Ti, except the compound of Zn, Zr, Hf and Ti), and further add organic acid and obtain reaction solution operation,
B () is by the reaction solution of operation (a) and the 50% particle diameter (D of volume-cumulative utilizing laser diffraction and scattering formula particle size distribution
50) be 0.1 ~ 10 μm, specific surface area is 1.0 ~ 20.0m
2/ g, Ig-loss are the partially hydrated magnesium oxide mixing of 2.0 ~ 25.0%, obtain the operation of mixed solution
(herein,
The Compound Phase being selected from more than a kind in the group be made up of the compound of Zn, Zr, Hf and Ti, for partially hydrated magnesium oxide, is scaled 0.1 ~ 5.0 quality % with oxide compound,
Be selected from the Compound Phase of more than a kind in the group be made up of divalent and the muriate of 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements for partially hydrated magnesium oxide, be scaled 0.1 ~ 5.0 quality % with metallic element,
Organic acid is 0.01 ~ 3.0mol relative to partially hydrated magnesium oxide 100g);
(c) by the mixed solution of operation (b) at the temperature of 50 ~ 100 DEG C, be the operation that the stirrer of 7 ~ 20m/s carries out mixing by circumferential speed;
D () carries out stirring and obtains the operation of magnesium hydroxide slurry at the temperature of 30 ~ 100 DEG C; And
E the magnesium hydroxide slurry of operation (d) filters by (), wash, make it dry and obtain the operation of magnesium hydroxide particle.
Operation (a) is for obtaining the operation of the reaction solution for magnesian hydration reaction.The compound being selected from more than a kind in the group be made up of the compound of Zn, Zr, Hf and Ti adds as the complex hydroxide of magnesium hydroxide particle of the present invention and magnesium oxide particle and composite oxides to make.Thus, the raisings such as whiteness, ultraviolet-absorbing and specific refractory power, can obtain being suitable for optical material, the magnesium hydroxide of the present invention of coating agent of InkJet paper and magnesium oxide particle.
As the compound of Zn, Zr, Hf and Ti, as long as the compound with these metallic elements is just not particularly limited, oxide compound, oxyhydroxide, hydride, halogenide (fluorochemical, muriate, bromide and iodide), phosphoric acid salt, carbonate and nitrate etc. can be listed, 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%, is more preferably more than 99.5%.In the present invention, purity refers to the content of 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 measuring Zn, Zr, Hf and Ti, deducts their total content and the value that obtains from 100 quality %.It should be noted that, when the element formed as the compound itself of Zn, Zr, Hf and Ti of object is equivalent to the impurity element in the compound of aforementioned Zn, Zr, Hf and Ti, this element is not included in impurity element.Such as, when the compound of Zn, Zr, Hf and Ti of using in operation (a) is for ZnO, form in the Zn of the ZnO impurity element not included in the compound of aforementioned Zn, Zr, Hf and Ti.As the measuring method of the content of these impurity elements, the measuring method using ICP emmission spectrometric analysis device can be listed.The D of the compound of Zn, Zr, Hf and Ti
50be preferably 0.1 ~ 100 μm, be more preferably 0.5 ~ 50 μm.
As the solvent in the dispersion liquid of the compound of more than a kind comprised in the group that is selected from and is made up of the compound of Zn, Zr, Hf and Ti, ion exchanged water can be listed.Dispersion liquid used in operation (a) such as can obtain by adding the compound of more than a kind be selected from the group be made up of the compound of Zn, Zr, Hf and Ti in ion exchanged water.
The nitrate of the muriate of divalent and 3 valency metallic elements and divalent and 3 valency metallic elements adds in order to the solubleness and speed of separating out controlling magnesium hydroxide particle of the present invention.As divalent and the muriate of 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements, preferred 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%, is more preferably more than 99.5%.In addition, the D of the muriate of divalent and 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements
50be preferably 0.1 ~ 100 μm, be more preferably 0.5 ~ 50 μm.
In the present invention, organic acid adds in order to the solubleness controlled as the magnesium oxide particle of raw material.As organic acid, the aliphatics or aromatic organic acid with carboxyl can be listed, preferable formic acid, acetic acid, propionic acid, butyric acid and phenylformic acid.
Operation (b) is the operation mixed with partially hydrated magnesium oxide particle for the reaction solution of hydration reaction will obtained in operation (a).Partially hydrated magnesium oxide particle used in operation (b) is the partially hydrated magnesium oxide particle regulated the activity degree of magnesium oxide particle.Partially hydrated magnesium oxide particle used in operation (b) is 50% particle diameter (D of the volume-cumulative utilizing laser diffraction and scattering formula particle size distribution
50) be 0.1 ~ 10 μm, specific surface area is 1.0 ~ 20.0m
2/ g, Ig-loss be 2.0 ~ 25.0%, the magnesium oxide that with a portion of hydration on surface, namely part carries out the magnesium oxide of hydration.By using so partially hydrated magnesium oxide, the magnesium hydroxide particle with high-specific surface area can be obtained.
The D of partially hydrated magnesium oxide particle used in operation (b)
50when being less than 0.1 μm, hydration rate becomes too fast, can become thick aggregated particles.In addition, D
50when being greater than 10 μm, hydration reaction fully cannot be carried out and residual comprise magnesian particle.D
50be preferably 0.1 ~ 5.0 μm.The specific surface area of partially hydrated magnesium oxide particle used in operation (b) is more than 20.0m
2during/g, hydration rate becomes too fast, can become thick aggregated particles.In addition, specific surface area is lower than 1.0m
2during/g, hydration reaction fully cannot be carried out and residual comprise magnesian particle.Specific surface area is preferably 2.0 ~ 18.0m
2/ g, is more preferably 3.0 ~ 15.0m
2/ g.
Represent the Ig-loss(calcination loss of the total amount of the moisture in the adhesive water of partially hydrated magnesium oxide particle used in operation (b) and hydrate structure) be 2.0 ~ 25.0%.That is, the hydration levels during Ig-loss represents in the present invention partially hydrated magnesium oxide particle.When Ig-loss is more than 25.0%, hydration reaction is suppressed, and having unhydrated magnesium oxide to remain, is not preferred.In order to make hydration reaction fully carry out, and then obtain the magnesium hydroxide with high-specific surface area, Ig-loss is preferably 2.0 ~ 20.0%, is more preferably 3.0 ~ 18.0%.In the present invention, Ig-loss carries out measuring after passing through that partially hydrated magnesium oxide particle is calcined 3600 seconds under 1273K and obtains.
The partially hydrated magnesium oxide prepared in this operation (b) can by placing the operation of 0.5 ~ 24 hour by magnesium oxide particle and obtaining, the 50% particle diameter (D utilizing the volume-cumulative of laser diffraction and scattering formula particle size distribution of described magnesium oxide particle in the constant temperature high humidity machine of temperature 40 ~ 95 DEG C, humidity 60 ~ 95%
50) be 0.1 ~ 10 μm, specific surface area is 1.0 ~ 15.0m
2/ g.Usually, the magnesian Ig-loss as raw material is 0.1 ~ 1.0%, by being increased in the time of placing in constant temperature high humidity machine, Ig-loss can be made to increase.Become the magnesian D of the partially hydrated magnesian raw material prepared in operation (b)
50be preferably 0.1 ~ 5.0 μm.In addition, the magnesian specific surface area becoming the partially hydrated magnesian raw material prepared in operation (b) is preferably 2.0 ~ 15.0m
2/ g, is more preferably 3.0 ~ 15.0m
2/ g.
The amount of each composition comprised in partially hydrated magnesium oxide used in operation (b) and dispersion liquid is as described below.
The amount being selected from the compound of more than a kind in the group be made up of the compound of Zn, Zr, Hf and Ti, relative to partially hydrated magnesium oxide particle, is scaled 0.1 ~ 5.0 quality % with oxide compound.When the amount being selected from the compound in the group be made up of the compound of Zn, Zr, Hf and Ti is less than 0.1 quality %, when using as coating agent, whiteness, ultraviolet-absorbing and specific refractory power etc. are insufficient, particle shape also can not become the spherical particle that lepidiod primary particle is assembled, but becomes the particle of hexagonal tabular.In addition, when the amount being selected from the compound in the group be made up of the compound of Zn, Zr, Hf and Ti is greater than 5.0 quality %, the spherical particle that the so lepidiod primary particle of the present invention is assembled can not be become, but become the particle of hexa-prism.Be selected from the amount of the compound of more than a kind in the group be made up of the compound of Zn, Zr, Hf and Ti relative to partially hydrated magnesium oxide particle, be preferably 0.4 ~ 4.0 quality %.
The amount being selected from the compound of more than a kind in the group be made up of divalent and the muriate of 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements, relative to partially hydrated magnesium oxide particle, is 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.The amount being selected from the compound of more than a kind in the group be made up of divalent and the muriate of 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements, relative to partially hydrated magnesium oxide particle, converts with metallic element and is more preferably 0.4 ~ 4.0 quality %.
Organic acid addition is 0.01 ~ 3.0mol relative to partially hydrated magnesium oxide particle 100g.When organic acid addition is less than 0.01mol relative to partially hydrated magnesium oxide particle 100g, the speed of separating out of crystal is slack-off, becomes monodispersed hexa-prism particle; When being greater than 3.0mol, the speed of separating out of crystal becomes too fast, becomes thick aggregated particles.Organic acid addition, relative 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, is more preferably 50 ~ 180g/L, more preferably 50 ~ 150g/L.That is, it is preferred for the amount of the reaction solution of middle relative to operation (a) for partially hydrated magnesium oxide acquisition being adjusted to 20 ~ 200g/L, is more preferably 50 ~ 180g/L, more preferably 50 ~ 150g/L.If be the partially hydrated magnesium oxide concentration in such reaction solution, then hydration reaction is carried out fully.
In operation (b), the temperature of reaction solution is preferably 50 ~ 100 DEG C, is more preferably 50 ~ 95 DEG C, more preferably 70 ~ 90 DEG C.If be such temperature, then hydration reaction is carried out fully.
Operation (c) is the operation that the stirrer of 7 ~ 20m/s carries out mixing for using circumferential speed at the temperature of 50 ~ 100 DEG C.In order to control dispersion state when reacting, can the revolution stirred be regulated.When circumferential speed is less than 7m/s, the spherical magnesium hydroxide that lepidiod primary particle is assembled cannot be obtained.In addition, when circumferential speed is greater than 20m/s, magnesium hydroxide particle fully disperses when karyogenesis, forms monodispersed hexa-prism magnesium hydroxide particle, cannot obtain the spherical magnesium hydroxide particle that the present invention is such.As the device for this stirring, can HOMODISPER(PRIMIXCorporation, T.K.HOMODISPER be listed) etc.Circumferential speed is preferably 8 ~ 18m/s, is more preferably 9 ~ 15m/s.Temperature of reaction in operation (c) is preferably 55 ~ 95 DEG C, is more preferably 60 ~ 95 DEG C.In operation (c), mixing time can change according to the degree of hydration reaction, such as, can be set to 10 ~ 360 minutes, is preferably set to 20 ~ 200 minutes.
Operation (d) for carrying out stirring and obtaining the operation of magnesium hydroxide slurry at the temperature of 30 ~ 100 DEG C.Thus, promote unreacted partially hydrated magnesian hydration reaction in operation (c), can magnesium hydroxide be made.Temperature is preferably 50 ~ 95 DEG C, is more preferably 70 ~ 90 DEG C.As long as stirring velocity fully can stir the degree of magnesium hydroxide slurry, to be not particularly limited, such as, can be set to 100 ~ 500rpm with the stirrer of 3 blades.As long as the time of the magnesium hydroxide slurry that churning time hydration reaction is fully carried out, can obtain expectation is just not particularly limited, such as, can be set to 0.5 ~ 6 hour.
Operation (e) obtains the operation of magnesium hydroxide particle for filtering the magnesium hydroxide slurry of operation (d), washing, make its drying.Thus, magnesium hydroxide particle of the present invention can be obtained.
Magnesium oxide particle of the present invention is obtained by the method comprising following operation: by magnesium hydroxide particle of the present invention or the magnesium hydroxide particle that obtained by the manufacture method comprising operation (a) of the present invention ~ operation (e) in air atmosphere, calcine at 500 ~ 1400 DEG C.Obtain preferably by being included in the method for carrying out the operation of calcining at 600 ~ 1300 DEG C.Such as, magnesium hydroxide particle of the present invention or the magnesium hydroxide particle that obtained by the manufacture method comprising operation (a) of the present invention ~ operation (e) are warming up to 500 ~ 1400 DEG C with heat-up rate 1 ~ 20 DEG C/min (preferably 3 ~ 10 DEG C/min), are preferably 600 ~ 1300 DEG C in air atmosphere, after intensification, calcining 0.1 ~ 5 hour at 500 ~ 1400 DEG C, preferably 600 ~ 1300 DEG C, can obtain magnesium oxide particle of the present invention thus.When calcining temperature is lower than 500 DEG C, shortage of heat and have magnesium hydroxide remain.On the other hand, when calcining temperature is more than 1400 DEG C, magnesium oxide generation grain growing, can not form the spherical magnesium oxide that lepidiod primary particle is assembled.
Operation like this, 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 by means of only carrying out hydration adjustment and control ratio surface-area simply in constant temperature high humidity machine etc. as the magnesium oxide of raw material, therefore, it is possible to 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 evenly, favorable dispersity, has high-specific surface area, and therefore in various field, availability is high.In addition, manufacture method of the present invention can easily prepare 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 the coating agent of InkJet paper, fire retardant, heat-storing material, catalyzer and electronic material etc., as the purposes of magnesium oxide particle, may be used for optical material, the coating agent of InkJet paper, the purposes such as catalyzer and electronic material.
Embodiment
Below, further describe the present invention in detail by embodiment and comparative example, but the present invention does not limit by these embodiments.
［ 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, NIKKISOCO., 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) of the determination object become in particle, use ICP emmission spectrometric analysis device (trade(brand)name: SPS-5100, SeikoInstrumentsInc. manufacture), by sample dissolution quality measurement after acid.
(3) BET specific surface area assay method
Use specific area measuring device (trade(brand)name: Macsorb1210, MountechCo., 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, 3600 seconds condition mensuration Ig-loss.
(embodiment 1)
By median size (D
50) be 1.08 μm, specific surface area is 10.94m
2the magnesium oxide of/g is placed 3 hours in the constant temperature high humidity machine of temperature 80 DEG C, humidity 90%, and surface is carried out partially hydrated, obtaining specific surface area is 13.11m
2/ g, Ig-loss are the partially hydrated magnesium oxide of 9.08%.
Relative to the partially hydrated magnesium oxide used in reaction, to in the ion-exchange aqueous solution of the zinc oxide and ion exchanged water 1 liter that comprise 0.5 quality %, add the aluminum chloride hexahydrate being scaled 0.5 quality % with metallic element, and be the propionic acid of 0.02mol relative to partially hydrated magnesium oxide 100g, make reaction solution thus.Make the temperature to 60 DEG C of the reaction solution of making, drop into 100g surface is carried out partially hydrated magnesium oxide, obtain mixed solution.Drop into after magnesium oxide, make the temperature of reaction solution rise to 95 DEG C, use stirrer (PRIMIXCorporation manufactures T.K.homodisper) and regulating circumferential speed is 9m/s, make reaction carry out 1 hour.
Thereafter, at 90 DEG C, stir 4 hours with the speed of rotation that fully can stir the degree of slurry, make magnesium hydroxide slurry thus.The magnesium hydroxide slurry of making is filtered, washes, make it dry and obtain magnesium hydroxide particle of the present invention.
(embodiment 2)
Be 2.58 μm by median size, specific surface area is 3.59m
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, makes specific surface area be 4.23m
2/ g, Ig-loss are 4.72%, in addition, carry out similarly to Example 1.
(embodiment 3)
Be 0.68 μm by median size, specific surface area is 12.68m
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, makes specific surface area be 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 set to 3.0 quality %, in addition, carries out similarly to Example 1.
(embodiment 5)
The addition of zinc oxide is set to 0.1 quality %, in addition, carries out similarly to Example 1.
(embodiment 6)
Propionic acid is become the acetic acid of 0.02mol, in addition, carry out similarly to Example 1.
(embodiment 7)
Propionic acid is become the butyric acid of 0.02mol, in addition, carry out similarly to Example 1.
(embodiment 8)
The magnesium hydroxide made in embodiment 1 is calcined 800 DEG C × 1 hour in air atmosphere, obtains magnesium oxide particle.
(comparative example 1)
Use median size is 5.88 μm, specific surface area is 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, the magnesian Ig-loss as raw material is 0.44%.
(comparative example 2)
Be 0.76 μm by median size, specific surface area is 19.68m
2the magnesian surface 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, makes specific surface area be 20.78m
2/ g, Ig-loss are 2.58%, in addition, carry out similarly to Example 1.
(comparative example 3)
Be 1.86 μm by median size, specific surface area is 1.59m
2the magnesium oxide of/g is placed 30 hours in the constant temperature high humidity machine of temperature 80 DEG C, humidity 90%, makes specific surface area be 3.8m
2/ g, Ig-loss are 25.3%, in addition, carry out similarly to Example 1.
(comparative example 4)
The magnesium hydroxide made in embodiment 1 is calcined 1500 DEG C × 1 hour in air atmosphere, obtains magnesium oxide particle.
Measurement result about the magnesium hydroxide particle obtained by above embodiment and magnesium oxide particle is shown in table 1, and the measurement result about the magnesium hydroxide particle obtained by comparative example and magnesium oxide particle is shown in
Table 2.
[table 1]
[table 2]
Claims (6)
1. a magnesium hydroxide particle, it is spherical for lepidiod primary particle gathering, utilizes 50% particle diameter D of the volume-cumulative of laser diffraction and scattering formula particle size distribution
50be 1.0 ~ 5.0 μm, specific surface area is 10m
2/ more than g, its also comprise with oxide compound be scaled 0.01 ~ 4.0 quality %, the metallic element be selected from the group that is made up of Zn, Zr, Hf and Ti, comprise with metallic element be scaled 0.01 ~ 5.0 quality %, the further metallic element be selected from the group that is made up of the divalent except Zn, Zr, Hf and Ti and 3 valency metals.
2. a magnesium oxide particle, it is spherical for lepidiod primary particle gathering, utilizes 50% particle diameter D of the volume-cumulative of laser diffraction and scattering formula particle size distribution
50be 1.0 ~ 5.0 μm, specific surface area is 10m
2/ more than g, its also comprise with oxide compound be scaled 0.01 ~ 4.0 quality %, the metallic element be selected from the group that is made up of Zn, Zr, Hf and Ti, comprise with metallic element be scaled 0.01 ~ 5.0 quality %, the further metallic element be selected from the group that is made up of the divalent except Zn, Zr, Hf and Ti and 3 valency metals.
3. a manufacture method for magnesium hydroxide particle, it comprises following operation:
A () adds the compound of more than a kind be selected from group except the compound of Zn, Zr, Hf and Ti, that be made up of divalent and the muriate of 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements in the dispersion liquid of the compound of more than a kind comprised in the group that is selected from and is made up of the compound of Zn, Zr, Hf and Ti, and further interpolation organic acid and obtain the operation of reaction solution;
B () is by the reaction solution of operation (a) and the 50% particle diameter D of volume-cumulative utilizing laser diffraction and scattering formula particle size distribution
50be 0.1 ~ 10 μm, specific surface area is 1.0 ~ 20.0m
2/ g, Ig-loss are the partially hydrated magnesium oxide mixing of 2.0 ~ 25.0%, obtain the operation of mixed solution,
Herein,
The Compound Phase being selected from more than a kind in the group be made up of the compound of Zn, Zr, Hf and Ti, for partially hydrated magnesium oxide, is scaled 0.1 ~ 5.0 quality % with oxide compound,
Be selected from the Compound Phase of more than a kind in the group be made up of divalent and the muriate of 3 valency metallic elements and the nitrate of divalent and 3 valency metallic elements for partially hydrated magnesium oxide, be scaled 0.1 ~ 5.0 quality % with metallic element,
Organic acid is 0.01 ~ 3.0mol relative to partially hydrated magnesium oxide 100g;
(c) by the mixed solution of operation (b) at the temperature of 50 ~ 100 DEG C, be the operation that the stirrer of 7 ~ 20m/s carries out mixing by circumferential speed;
D () carries out stirring and obtains the operation of magnesium hydroxide slurry at the temperature of 30 ~ 100 DEG C; And
E the magnesium hydroxide slurry of operation (d) filters by (), wash, make it dry and obtain the operation of magnesium hydroxide particle.
4. method according to claim 3, wherein, the partially hydrated magnesium oxide of operation (b) obtains by being placed 0.5 ~ 24 hour in the constant temperature high humidity machine of temperature 40 ~ 95 DEG C, humidity 60 ~ 95% by magnesium oxide particle, the 50% particle diameter D utilizing the volume-cumulative of laser diffraction and scattering formula particle size distribution of described magnesium oxide particle
50be 0.1 ~ 10 μm, specific surface area is 1.0 ~ 15.0m
2/ g.
5. the method according to claim 3 or 4, wherein, the partially hydrated magnesian concentration in the mixed solution of operation (b) is 20 ~ 200g/L.
6. a manufacture method for magnesium oxide particle, it to be comprised magnesium hydroxide particle according to claim 1 or the magnesium hydroxide particle that obtained by method according to any one of claim 3 ~ 5 in air atmosphere, the operation of carrying out calcining at 500 ~ 1400 DEG C.
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| JP2011-203776 | 2011-09-16 | ||
| 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 |
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| JP6726146B2 (en) * | 2017-09-19 | 2020-07-22 | 宇部マテリアルズ株式会社 | Red tide control agent and red tide control method using the same |
| 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 |
| CN115926492B (en) * | 2022-11-07 | 2024-05-28 | 广东金戈新材料股份有限公司 | Preparation method and application method of mineralizer capable of reducing oil absorption value of magnesium oxide |
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| 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 |
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