KR20140063575A - 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
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Abstract
Spherical magnesium hydroxide particles having a high specific surface area, spherical magnesium oxide particles, and a process for producing the same.
Wherein the primary particle of the scaly carved particle is spherical in aggregate and has a 50% particle diameter (D 50 ) of 1.0 to 5.0 μm and a specific surface area of 10 m 2 / g or more in terms of volumetric accumulation by laser diffraction scattering particle size distribution measurement, And magnesium oxide particles.
Description
The present invention relates to spherical magnesium hydroxide particles having a high specific surface area (specific surface area), spherical magnesium oxide particles and a process for producing them.
Magnesium hydroxide particles and magnesium oxide particles are used in various fields. Examples of applications of the magnesium hydroxide particles include a coating agent for inkjet paper, a flame retardant, a thermal storage material (heat storage material), a catalyst, and an electronic material. Examples of applications of the magnesium oxide particles include optical materials, And electronic materials.
When the magnesium hydroxide particles are used for coatings, flame retardants, heat storage materials, catalysts and electronic materials for inkjet paper, the following are required. In the case of the coating agent, it is preferable that the dye ink has a hydroxyl group having a OH group having high affinity with many OH groups and a positive charge likely to be adsorbed in a pigment ink having a large negative charge, Magnesium particles are required. In addition, magnesium hydroxide particles having an aggregate structure that exhibits excellent dispersibility and high reactivity in a flame retardant, a heat storage material, and a catalyst are required. Further, in the case of electronic materials, small magnesium hydroxide particles having excellent dispersibility are required.
When magnesium oxide particles are used for optical materials, coating agents for inkjet paper, catalysts and electronic materials, the following are required. In optical materials, there is a demand for magnesium oxide particles having an excellent dispersibility and having an aggregate structure that easily diffuses light. In addition, magnesium oxide particles having an aggregate structure exhibiting excellent dispersibility and high reactivity are required in the catalyst. Further, in the case of electronic materials, small magnesium oxide particles having excellent dispersibility are required.
Patent Document 1 discloses leaflet pieces of two or more different directions obtained by setting the ion concentration ratio of the sulfate ion [(SO 4 ) 2- ] / magnesium ion [(Mg) 2+ ] Spherical magnesium hydroxide particles having this bonded and / or crossed structure are disclosed. However, in the method described in Patent Document 1, spherical magnesium hydroxide is not stably formed, and slaked and columnar magnesium hydroxide are mixed together. Such magnesium hydroxide particles are dispersed in resin and the like And when it is used in a catalyst or the like, the specific surface area is low and the reactivity is low.
It is an object of the present invention to provide spherical magnesium hydroxide particles, spherical magnesium oxide particles having high specific surface area, and a process for producing them.
The inventors of the present invention have found that when a dispersion containing at least one compound selected from the group consisting of Zn, Zr, Hf and Ti is added to a dispersion containing a chloride of a divalent and trivalent metal element and a nitrate of a divalent and trivalent metal element A reaction liquid obtained by adding at least one compound (except for the compound of Zn, Zr, Hf and Ti) and further adding an organic acid and a reaction liquid obtained by partially hydrating the surface of the magnesium oxide particles with a constant- Magnesium hydroxide particles are mixed and subjected to hydration under high shear, whereby spherical magnesium hydroxide particles having excellent dispersibility, high reactivity and high specific surface area can be obtained. Further, the inventors of the present invention have found that spherical magnesium oxide particles having a high specific surface area can be obtained by firing the magnesium hydroxide particles of the present invention at 500 ° C to 1400 ° C in an atmospheric environment.
That is, the present invention is a spherical primary particle having an aggregate of scales and having a 50% particle diameter (D 50 ) of volume accumulation measured by a laser diffraction scattering type particle size distribution measurement of 1.0 To 5.0 m and a specific surface area of 10 m < 2 > / g or more.
The present invention further provides a method for producing a metal alloy comprising 0.01 to 4.0% by mass of a metal element selected from the group consisting of Zn, Zr, Hf and Ti in terms of oxide and further metal elements selected from the group consisting of divalent and trivalent metals, Zn, Zr, Hf and Ti are excluded) in an amount of 0.01 to 5.0% by mass in terms of metal element.
The present invention relates to a spherical primary particle having aggregated spherical primary particles and having a 50% particle diameter (D 50 ) of 1.0 to 5.0 μm and a specific surface area of 10 m 2 / g Magnesium oxide particles.
The present invention further provides a method for producing a metal element comprising 0.01 to 4.0% by mass of a metal element selected from the group consisting of Zn, Zr, Hf and Ti in terms of oxides and further comprising a metal element selected from the group consisting of divalent and trivalent metals, Zn, Zr, Hf and Ti are excluded) in an amount of 0.01 to 5.0% by mass in terms of metal element.
The present invention relates to a process for producing magnesium hydroxide particles,
(a) at least one compound selected from the group consisting of Zn, Zr, Hf and Ti is added to a dispersion containing a chloride of a divalent and trivalent metal element and a nitrate of a divalent and trivalent metal element A step of adding at least one compound (except for the compound of Zn, Zr, Hf and Ti) and further adding an organic acid to obtain a reaction solution,
(b) a 50% particle diameter (D 50 ) of 0.1 to 10 탆 and a specific surface area of 1.0 to 20.0 m 2 / g in the volume of the reaction solution obtained by the reaction solution and the laser diffraction scattering type particle size distribution measurement of step (a) A step of mixing a partially hydrated magnesium oxide having an Ig-loss of 2.0 to 25.0% to obtain a mixed solution,
(Wherein at least one compound selected from the group consisting of Zn, Zr, Hf and Ti compounds is 0.1 to 5.0 mass% in terms of oxide relative to a part of hydrated magnesium oxide,
The at least one compound selected from the group consisting of chloride of divalent and trivalent metal elements and nitrate of divalent and trivalent metal elements is 0.1 to 5.0 mass% in terms of metal element with respect to a part of hydrated magnesium oxide,
The organic acid is 0.01 to 3.0 mol based on 100 g of the partially hydrous magnesium oxide)
(c) mixing the mixture of step (b) with a stirrer at a temperature of 50 to 100 ° C at a peripheral speed of 7 to 20 m / s,
(d) stirring at a temperature of 30 to 100 DEG C to obtain a magnesium hydroxide slurry, and
(e) a step of obtaining magnesium hydroxide particles by filtering, washing and drying the magnesium hydroxide slurry of the step (d)
To a process for producing magnesium hydroxide particles.
The present invention is characterized in that a part of hydrated magnesium oxide in step (b) has a 50% particle diameter (D 50 ) of 0.1 to 10 μm and a specific surface area of 1.0 to 15.0 m 2 / g magnesium oxide particles at a temperature of 40 to 95 DEG C and a humidity of 60 to 95% for 0.5 to 24 hours.
The present invention relates to the method described above, wherein the concentration of the partially hydrated magnesium oxide in the mixed liquid of the step (b) is 20 to 200 g / L.
The present invention relates to a process for producing magnesium oxide particles, which comprises a step of calcining magnesium hydroxide particles described above or magnesium hydroxide particles obtained by the above-described method at 500 to 1400 占 폚 in an atmospheric environment ≪ / RTI >
According to the present invention, there are provided spherical magnesium hydroxide particles, spherical magnesium oxide particles and a process for their production having high specific surface area. The magnesium hydroxide particles and the magnesium oxide particles of the present invention have a high specific surface area and a high dispersibility and are useful in various fields. Further, according to the production method of the present invention, magnesium hydroxide particles and magnesium oxide particles can be easily produced.
1 is an electron micrograph of the magnesium hydroxide particles of the present invention.
The magnesium hydroxide particles of the present invention are spherical particles in which primary particles in the form of scales are agglomerated and have a 50% particle diameter (D 50 ) of volume accumulation measured by laser diffraction scattering particle size distribution measurement of 1.0 to 5.0 탆 and a specific surface area 10 m 2 / g or more. In the present invention, the shape of the primary particle is scaly, the thickness (short axis) of the scales is, for example, 0.01 to 0.1 mu m, and the ratio of the maximum scales to the thickness (aspect ratio) For example, 10 to 1000. The spherical particles in which the primary particles are aggregated have uniform pores on the particle surface and have higher specific surface area than the hexagonal plate-like magnesium hydroxide particles obtained by the conventional production method, so that the adsorption of liquid and gas molecules is high, Since the shape is spherical, it is highly dispersible to resin and the like. In addition, when such primary particles are agglomerated spherical particles as a coating agent for paper, the scale-like magnesium hydroxide constituting the spherical particles is not excessively concentrated, so that the adsorption of the ink is good.
The magnesium hydroxide particles of the present invention have a D 50 of 1.0 to 5.0 μm and a specific surface area of 10 m 2 / g or more. In such a range, the viscosity is not excessively increased at the time of blending with a resin or the like, and the aggregation of the particles can be suppressed, so that the dispersibility is good. Further, when magnesium hydroxide particles having such a particle diameter are used as a coating agent for paper, the particles do not protrude from the ink receiving layer, and the ink fixability and water absorption are good. In addition, since the particle diameter is not excessively large, it is useful for optical materials and electronic materials. The D 50 of the magnesium hydroxide particles of the present invention is preferably 2.0 to 5.0 탆, more preferably 3.0 to 5.0 탆, and the specific surface area is preferably 10 to 120 m 2 / g, more preferably 20 to 100 m 2 / g. In the present invention, the specific surface area is determined by the BET method.
The magnesium hydroxide powder of the present invention has a ratio (D 90 / D 10 ) of cumulative 10% particle diameter (D 10 ) to cumulative 90% particle diameter (D 90 ) based on volume measurement by laser diffraction scattering particle size distribution measurement , Preferably 3 or less, more preferably 1 to 3. With this D 90 / D 10 , since the magnesium hydroxide powder has a narrow particle size distribution and less aggregation of particles, more excellent dispersibility can be obtained.
The magnesium hydroxide particles of the present invention may further contain a metal element of a compound used in the production process. The magnesium hydroxide particles of the present invention contain 0.01 to 4.0% by mass of at least one metal element selected from the group consisting of Zn, Zr, Hf and Ti in terms of oxide, and further contain at least one element selected from the group consisting of divalent and trivalent metal elements (Excluding Zn, Zr, Hf and Ti) in an amount of 0.01 to 5.0% by mass in terms of the metal element. The content of these metal elements is sufficient for whiteness, ultraviolet absorptivity and refractive index when magnesium hydroxide particles are used as a coating agent. The content of at least one metal element selected from the group consisting of Zn, Zr, Hf and Ti, that is, Zn, Zr, Hf, Ti or a mixture thereof is preferably 0.05 to 4.0% by mass, 0.05 to 3.0% by mass, and more preferably 0.05 to 2.5% by mass.
In the present invention, at least one additional metal element (except for Zn, Zr, Hf and Ti) selected from the group consisting of divalent and trivalent metal elements is not particularly limited, and Ag, Al, B, Ba, Bi, Cd, Co, Cr, Cu, Fe, Ga, In, Mn, Mo, Ni, Pb, Sr, Tl and V are preferable. The content of at least one additional metal element (excluding Zn, Zr, Hf and Ti) selected from the group consisting of divalent and trivalent metal elements is preferably 0.05 to 5.0 mass% in terms of the metal element, More preferably from 0.1 to 5.0% by mass, and still more preferably from 0.3 to 4.0% by mass.
The magnesium oxide particles of the present invention are spherical particles in which primary particles of aggregate form aggregated and have a 50% particle diameter (D 50 ) of volume accumulation by laser diffraction scattering particle size distribution measurement of 1.0 to 5.0 μm and a specific surface area 10 m 2 / g or more. Such magnesium oxide particles are excellent in dispersibility into a resin or the like. Specifically, the magnesium oxide particles having such a particle diameter and specific surface area are preferably used as a coating agent for paper when the particles do not protrude from the ink-receiving layer and have good fixability and water absorbability of the ink, The viscosity does not become too high, and the aggregation of the particles is suppressed, so that the dispersibility is good. Further, since the particle diameter is not too large, it is useful for optical materials and electronic materials. The D 50 of the magnesium oxide particles of the present invention is preferably 2.0 to 5.0 탆, more preferably 3.0 to 5.0 탆, and the specific surface area is preferably 10 to 120 m 2 / g, more preferably 20 to 100 m 2 / g.
The magnesium oxide powder of the present invention has a ratio (D 90 / D 10 ) of cumulative 10% particle diameter (D 10 ) to cumulative 90% particle diameter (D 90 ) based on volume measurement by laser diffraction scattering particle size distribution measurement , Preferably 3 or less, and more preferably 1 to 3. With such a ratio (D 90 / D 10 ), since the particle size distribution of the magnesium oxide powder is narrow and the aggregation of the particles is small, further excellent dispersibility can be obtained.
The magnesium oxide particles of the present invention may further contain a metal element of a compound used in the production process. The magnesium oxide particles of the present invention contain 0.01 to 4.0% by mass of at least one metal element selected from the group consisting of Zn, Zr, Hf and Ti in terms of oxide, and further contain at least one element selected from the group consisting of divalent and trivalent metal elements (Excluding Zn, Zr, Hf and Ti) in an amount of 0.01 to 5.0% by mass in terms of the metal element. With such a content of the metallic element, when the magnesium oxide particles are used as a coating agent, whiteness, ultraviolet ray absorptivity and refractive index are sufficient. The content of at least one metal element selected from the group consisting of Zn, Zr, Hf and Ti, that is, Zn, Zr, Hf, Ti or a mixture thereof is preferably 0.05 to 4.0% by mass, more preferably 0.2 To 4.0% by mass, and more preferably 0.4% by mass to 4.0% by mass.
(Excluding Zn, Zr, Hf and Ti) selected from the group consisting of divalent and trivalent metal elements is not specifically limited and may be any one of Ag, Al, B, Ba, Bi, Cd, Co, Cr, Cu, Fe, Ga, In, Mn, Mo, Ni, Pb, Sr, Tl and V, and Al and Fe are preferable. The content of at least one additional metal element (excluding Zn, Zr, Hf and Ti) selected from the group consisting of divalent and trivalent metal elements is preferably 0.1 to 5.0 mass% in terms of metal element, More preferably from 0.3 to 4.0% by mass, and still more preferably from 0.4 to 4.0% by mass.
In the method for producing magnesium hydroxide particles of the present invention,
(a) at least one compound selected from the group consisting of Zn, Zr, Hf and Ti is added to a dispersion containing a chloride of a divalent and trivalent metal element and a nitrate of a divalent and trivalent metal element A step of adding at least one compound (except for the compound of Zn, Zr, Hf and Ti) and further adding an organic acid to obtain a reaction solution,
(b) a reaction solution of the step (b) and a 50% particle diameter (D 50 ) of volume accumulation measured by laser diffraction scattering type particle size distribution of 0.1 to 10 탆 and a specific surface area of 1.0 to 20.0 m 2 / g, and a part of hydrated magnesium oxide having an Ig-loss of 2.0 to 25.0% are mixed to obtain a mixed solution,
(Wherein at least one compound selected from the group consisting of Zn, Zr, Hf and Ti compounds is 0.1 to 5.0 mass% in terms of oxide relative to a part of hydrated magnesium oxide,
The at least one compound selected from the group consisting of chloride of divalent and trivalent metal elements and nitrate of divalent and trivalent metal elements is 0.1 to 5.0 mass% in terms of metal element with respect to a part of hydrated magnesium oxide,
The organic acid is 0.01 to 3.0 mol based on 100 g of the partially hydrous magnesium oxide)
(c) mixing the mixture of step (b) at a temperature of from 50 to 100 캜 using a stirrer having a peripheral speed of from 7 to 20 m / s,
(d) stirring at a temperature of 30 to 100 DEG C to obtain a magnesium hydroxide slurry, and
(e) a step of obtaining magnesium hydroxide particles by filtering, washing and drying the magnesium hydroxide slurry of the step (d)
.
Step (a) is a step of obtaining a reaction liquid for hydration reaction of magnesium oxide. At least one compound selected from the group consisting of Zn, Zr, Hf and Ti is added to prepare the composite hydroxide and composite oxide which are the magnesium hydroxide particles and the magnesium oxide particles of the present invention. This improves the whiteness degree, ultraviolet ray absorptivity, refractive index and the like, and makes it possible to obtain magnesium hydroxide and magnesium oxide particles of the present invention suitable for optical materials and coating agents for inkjet paper.
As the compound of Zn, Zr, Hf and Ti, there is no particular limitation as long as it is a compound having these metal elements, and oxides, hydroxides, hydrides, halides (fluorides, chlorides, bromides and iodides), phosphates, Zirconium, zirconium, zirconium, hafnium oxide, hafnium hydroxide, hafnium chloride, hafnium nitrate, titanium oxide, titanium hydroxide, titanium chloride and the like, and at least one selected from the group consisting of zinc oxide, zinc hydroxide, zinc chloride, zinc nitrate, zirconium oxide, zirconium hydroxide, Titanium nitrate is preferred. The compound of Zn, Zr, Hf and Ti preferably has a purity of 99.0% or more, more preferably 99.5% or more. In the present invention, the purity of the impurity element (Ag, Al, B, Ba, Bi, Cd, Cl, Co, Cr, Cu, Fe, Ga, In, K, Li, The content of Mg, Mn, Mo, Na, Ni, P, Pb, S, Si, Sr, Tl, V, Zn, Ti and Zr is measured and the total content thereof is subtracted from 100 mass%. When the element constituting the target compound of Zn, Zr, Hf and Ti corresponds to the impurity element in the compound of Zn, Zr, Hf and Ti, the element is not included in the impurity element. For example, when the compound of Zn, Zr, Hf and Ti used in the step (a) is ZnO, Zn constituting ZnO is not included in the impurity element in the compound of Zn, Zr, Hf and Ti described above. As a method for measuring the content of these impurity elements, a measurement method using an ICP emission spectrometer can be mentioned. The compound of Zn, Zr, Hf and Ti preferably has a D 50 of 0.1 to 100 탆, more preferably 0.5 to 50 탆.
As a solution in a dispersion containing at least one compound selected from the group consisting of Zn, Zr, Hf and Ti, ion-exchange water can be mentioned. The dispersion used in the step (a) can be obtained, for example, by adding at least one compound selected from the group consisting of Zn, Zr, Hf and Ti compounds to ion-exchanged water.
Chlorides of divalent and trivalent metal elements and nitrates of divalent and trivalent metal elements are added to control the solubility and precipitation rate of the magnesium hydroxide particles of the present invention. As the nitrate of divalent and trivalent metal elements and the nitrate of divalent and trivalent metal elements, aluminum chloride, iron chloride, aluminum nitrate and iron nitrate are preferred. The chloride of divalent and trivalent metal elements and the nitrate of divalent and trivalent metal elements preferably have a purity of 99.0% or more, more preferably 99.5% or more. The chloride of the divalent and trivalent metal elements and the nitrate of the divalent and trivalent metal elements preferably have a D 50 of 0.1 to 100 탆, more preferably 0.5 to 50 탆.
In the present invention, the organic acid is added to suppress the solubility of the magnesium oxide particles as the raw material. As the organic acid, an aliphatic or aromatic organic acid having a carboxyl group can be mentioned, and formic acid, acetic acid, propionic acid, butyric acid and benzoic acid are preferable.
The step (b) is a step of mixing the reaction liquid for hydration reaction and the partially hydrated magnesium oxide particles obtained in the step (a). In some hydrated magnesium oxide particles used in step (b), the activity of the magnesium oxide particles is adjusted. The partially hydrated magnesium oxide particles used in the step (b) have a 50% particle diameter (D 50 ) of 0.1 to 10 μm and a specific surface area of 1.0 to 20.0 m 2 / g and an Ig-loss of 2.0 to 25.0%, which is a partly hydrated magnesium oxide, that is, partially hydrated magnesium oxide. By using such a partially hydrous magnesium oxide, magnesium hydroxide particles having a high specific surface area can be obtained.
When the D 50 of the partially hydrated magnesium oxide particles used in the step (b) is smaller than 0.1 탆, the hydration rate becomes excessively fast, resulting in coarse and coarse aggregated particles. If the D 50 is larger than 10 탆, the hydration reaction does not proceed sufficiently and particles containing magnesium oxide remain. D 50 is preferably 0.1 ~ 5.0㎛. When the specific surface area of some hydrated magnesium oxide particles used in the step (b) exceeds 20.0 m 2 / g, the hydration rate becomes too fast, resulting in coarse and coarse aggregated particles. If the specific surface area is less than 1.0 m 2 / g, the hydration reaction does not progress sufficiently and particles containing magnesium oxide remain. The specific surface area is preferably 2.0 to 18.0 m 2 / g, more preferably 3.0 to 15.0 m 2 / g.
The Ig-loss (loss on ignition loss) indicating the sum of the water content of the hydrated magnesium particles and the water content in the hydrate structure used in the step (b) is 2.0 to 25.0%. That is, Ig-loss represents the degree of hydration in some hydrated magnesium oxide particles in the present invention. If the Ig-loss exceeds 25.0%, the hydration reaction is inhibited and magnesium oxide, which can not be hydrated, remains, which is undesirable. In order to sufficiently accelerate the hydration reaction and obtain magnesium hydroxide having a high specific surface area, the Ig-loss is preferably 2.0 to 20.0%, more preferably 3.0 to 18.0%. In the present invention, Ig-loss is determined by measuring a part of the hydrated magnesium oxide particles after calcination at 1,273 K for 3600 seconds.
Part of the hydrated magnesium oxide prepared in this step (b) has a 50% particle diameter (D 50 ) of 0.1 to 10 μm in volume accumulation by laser diffraction scattering particle size distribution measurement and a specific surface area of 1.0 to 15.0 m 2 / g magnesium oxide particles at a temperature of 40 to 95 캜 and a humidity of 60 to 95% for 0.5 to 24 hours. Generally, the Ig-loss of the magnesium oxide as a raw material is 0.1 to 1.0%, and Ig-loss can be increased by increasing the holding time in a high-temperature and high-humidity environment. The D 50 of the magnesium oxide used as the raw material of the partially hydrated magnesium oxide prepared in the step (b) is preferably 0.1 to 5.0 탆. The specific surface area of the magnesium oxide to be a raw material of the partially hydrated magnesium oxide prepared in the step (b) is preferably 2.0 to 15.0 m 2 / g, more preferably 3.0 to 15.0 m 2 / g.
The amount of each component contained in the partially hydrous magnesium oxide and the dispersion used in the step (b) is as follows.
The amount of at least one compound selected from the group consisting of Zn, Zr, Hf and Ti is 0.1 to 5.0 mass% in terms of oxide with respect to a part of hydrated magnesium oxide particles. When the amount of the compound selected from the group consisting of Zn, Zr, Hf and Ti is less than 0.1% by mass, the whiteness, ultraviolet ray absorptivity and refractive index are not sufficient when used as a coating agent, The primary particle does not become spherical particles that are aggregated and becomes a hexagonal particle. If the amount of the compound selected from the group consisting of Zn, Zr, Hf, and Ti is greater than 5.0 mass%, the scaly primary particles as in the present invention do not become aggregated spherical particles, Columnar). The amount of at least one compound selected from the group consisting of Zn, Zr, Hf, and Ti is preferably 0.4 to 4.0 mass% with respect to some hydrated magnesium oxide particles.
The amount of at least one compound selected from the group consisting of chloride of divalent and trivalent metal elements and nitrate of divalent and trivalent metal elements is 0.1 to 5.0 mass% in terms of metal element with respect to some hydrated magnesium oxide particles. If the amount of the additive is less than 0.1% by mass, the rate of precipitation of crystals is slowed to form hexagonal pillar-shaped particles. If the amount of the additive is more than 5.0% by mass, the precipitation rate of the crystals becomes too fast and coarse and coarse aggregated particles are obtained. The amount of at least one compound selected from the group consisting of chloride of divalent and trivalent metal elements and nitrate of divalent and trivalent metal elements is more preferably 0.4 to 4.0 mass% in terms of metal element with respect to some hydrated magnesium oxide particles Do.
The amount of the organic acid to be added is 0.01 to 3.0 mol per 100 g of the partially hydrous magnesium oxide particles. When the amount of the organic acid to be added is less than 0.01 mol per 100 g of magnesium hydroxide particles, the precipitation rate of crystals is slowed to form monodispersed hexagonal pillar-shaped particles. When the addition amount of organic acid is more than 3.0 mol, the precipitation rate of crystals becomes too fast, . The amount of the organic acid to be added is preferably 0.01 to 2.0 mol based on 100 g of the partially hydrous magnesium oxide.
In step (b), the concentration of partially hydrated magnesium oxide in the mixed solution is preferably 20 to 200 g / L, more preferably 50 to 180 g / L, and still more preferably 50 to 150 g / L. That is, the amount of partially hydrated magnesium oxide in the reaction solution obtained in the step (a) is adjusted to preferably 20 to 200 g / L, more preferably 50 to 180 g / L, and still more preferably 50 to 150 g / L do. If the hydrated magnesium oxide concentration in this reaction solution is partially hydrated, the hydration reaction proceeds sufficiently.
In the step (b), the temperature of the reaction liquid is preferably 50 to 100 캜, more preferably 50 to 95 캜, and still more preferably 70 to 90 캜. At this temperature, the hydration reaction proceeds sufficiently.
The step (c) is a step of mixing at a temperature of 50 to 100 캜 using a stirrer having a main velocity of 7 to 20 m / s. The number of revolutions of the stirring is adjusted to control the dispersion state at the time of the reaction. If the peripheral velocity is less than 7 m / s, spherical magnesium hydroxide with agglomerated primary particles in scaly pieces can not be obtained. On the other hand, if the main flux is larger than 20 m / s, the magnesium hydroxide particles are sufficiently dispersed at the time of nucleation to form monodispersed magnesium hydroxide particles of hexagonal columnar phase, and spherical magnesium hydroxide particles as in the present invention can not be obtained. As an apparatus for such agitation, homodisperse (Primix Co., T.K. homodisperser) and the like can be mentioned. The peripheral velocity is preferably 8 to 18 m / s, and more preferably 9 to 15 m / s. The reaction temperature in the step (c) is preferably 55 to 95 占 폚, more preferably 60 to 95 占 폚. In the step (c), the mixing time can be changed according to the degree of the hydration reaction, and can be, for example, 10 to 360 minutes, preferably 20 to 200 minutes.
Step (d) is a step of obtaining magnesium hydroxide slurry by stirring at a temperature of 30 to 100 캜. As a result, the hydration reaction of the partially hydrated magnesium oxide in the unreacted portion in the step (c) can be promoted to form magnesium hydroxide. The temperature is preferably 50 to 95 占 폚, more preferably 70 to 90 占 폚. The stirring speed is not particularly limited and may be, for example, 100 to 500 rpm by means of a stirrer of three springs, so long as the magnesium hydroxide slurry can be sufficiently stirred. The agitation time is not particularly limited as long as hydration reaction proceeds sufficiently and a desired magnesium hydroxide slurry can be obtained. For example, the agitation time can be 0.5 to 6 hours.
Step (e) is a step of obtaining magnesium hydroxide particles by filtering, washing with water and drying the magnesium hydroxide slurry in step (d). As a result, the magnesium hydroxide particles of the present invention can be obtained.
The magnesium oxide particles of the present invention are obtained by firing the magnesium hydroxide particles of the present invention or the magnesium hydroxide particles obtained by the manufacturing method including the steps (a) to (e) of the present invention at 500 to 1400 ° C ≪ / RTI > Preferably, a step of firing at 600 to 1300 占 폚. For example, the magnesium hydroxide particles of the present invention or the magnesium hydroxide particles obtained by the production method including the steps (a) to (e) of the present invention are heated at a temperature raising rate of 1 to 20 ° C / Is heated to 500 to 1400 ° C, preferably 600 to 1300 ° C at a temperature of 3 to 10 ° C / minute, and then heated at 500 to 1400 ° C, preferably 600 to 1300 ° C, for 0.1 to 5 hours, Magnesium oxide particles can be obtained. If the calcination temperature is less than 500 캜, the amount of heat is insufficient and magnesium hydroxide remains. On the other hand, when the firing temperature exceeds 1400 deg. C, magnesium oxide grows into particles, and the primary particles in the form of scales do not aggregate into spherical magnesium oxide.
In this way, spherical magnesium hydroxide particles and magnesium oxide particles having excellent dispersibility can be obtained. In the method for producing magnesium hydroxide and magnesium oxide according to the present invention, the specific surface area can be controlled simply by adjusting the hydrate of magnesium oxide as a raw material with a constant temperature and high humidity, magnesium hydroxide and magnesium oxide can be easily produced have.
The magnesium hydroxide particles and the magnesium oxide particles of the present invention are spherical, have a small average particle diameter, are uniform, have a good dispersibility, and have a high specific surface area, and thus are highly useful in various fields. Further, since the magnesium hydroxide and magnesium oxide particles as described above can be easily prepared, the production method of the present invention is highly convenient. The magnesium hydroxide particles of the present invention can be used as a coating agent for inkjet paper, a flame retardant agent, a heat storage material, a catalyst, and an electronic material. Examples of applications of the magnesium oxide particles include optical materials, coating agents for inkjet paper, .
[Example]
Hereinafter, the present invention will be described in more detail by way of examples and comparative examples, but the present invention is not limited to these examples.
[Analysis method]
(1) Laser diffraction scattering type particle size distribution measurement
A cumulative 10% particle diameter (D 10 ) on a volume basis, a cumulative 50% particle diameter (D 50 ) on a volume basis, and a volume-based cumulative particle size distribution (D 50 ) on a volume basis were measured using a laser diffraction scattering type particle size distribution analyzer (trade name: MT3300, The cumulative 90% particle diameter (D 90 ) was measured.
(2) Mass measurement of element
(Al, Fe, Zn, Zr, Hf, and Ti) to be measured in the particles were measured using an ICP emission spectrometer (trade name: SPS-5100, manufactured by Seiko Instruments Inc.) Respectively.
(3) BET specific surface area measurement method
The specific surface area was measured by a gas absorption method using a specific surface area measuring apparatus (trade name: Macsorb 1210, manufactured by Moonec Co., Ltd.).
(4) Ig-loss measurement method
The Ig-loss was measured by using an electric furnace (manufactured by Maruso Electric Co., Ltd.) under the condition of 12700 K at 3600 seconds.
[Example 1]
The mean particle size (D 50) and a specific surface area of the 1.08㎛ with 10.94m 2 / g of 3 hours the magnesium, in the temperature 80 ℃, constant temperature and humidity of a humidity of 90% oxidized, some hydrated by the surface a specific surface area of 13.11m 2 / g and an Ig loss of 9.08%.
To an ion-exchanged water solution containing 0.5 mass% of zinc oxide and 1 liter of ion-exchanged water with respect to a part of the hydrated magnesium oxide used in the reaction was added 0.5 mass% aluminum chloride hexahydrate in terms of metal element and 100 mass% 0.02 mol of propionic acid was added to the reaction solution to prepare a reaction solution. The temperature of the reaction solution thus prepared was raised to 60 캜, and 100 g of magnesium hydroxide whose surface was partially hydrated was added to obtain a mixed solution. After the addition of magnesium oxide, the temperature of the reaction solution was raised to 95 캜, and the reaction solution was adjusted to have a peripheral speed of 9 m / s with a stirrer (T.K. homodisperser manufactured by Primimix) and reacted for 1 hour.
Thereafter, the slurry was stirred at 90 DEG C for 4 hours at a rotational speed sufficient to sufficiently stir the slurry, thereby preparing a magnesium hydroxide slurry. The prepared magnesium hydroxide slurry was filtered, washed with water and dried to obtain magnesium hydroxide particles of the present invention.
[Example 2]
A mean particle size of 2.58㎛ and a specific surface area of 3.59m 2 / g of the magnesium oxide, the temperature 60 ℃, the humidity in the constant temperature and humidity with one hours of 90%, some hydrated by the surface of a specific surface area of 4.23m 2 / g, The procedure of Example 1 was repeated except that the Ig-loss was 4.72%.
[Example 3]
A mean particle size of 0.68㎛ and a specific surface area of 12.68m 2 / g of the magnesium oxide, the temperature 60 ℃, with 24 hours in a constant temperature and humidity of 90% humidity, some hydrated by the surface of a specific surface area of 16.72m 2 / g, The procedure of Example 1 was repeated except that the Ig-loss was changed to 16.97%.
[Example 4]
The procedure of Example 1 was repeated except that the addition amount of zinc oxide was changed to 3.0 mass%.
[Example 5]
The procedure of Example 1 was repeated except that the addition amount of zinc oxide was changed to 0.1 mass%.
[Example 6]
Propionic acid was replaced by 0.02 mol of acetic acid.
[Example 7]
Propionic acid was replaced by 0.02 mol of butyric acid.
[Example 8]
Magnesium hydroxide produced in Example 1 was fired at 800 deg. C for 1 hour in an air atmosphere to obtain magnesium oxide particles.
[Comparative Example 1]
The procedure of Example 1 was repeated except that the surface of magnesium oxide having an average particle diameter of 5.88 mu m and a specific surface area of 1.34 m < 2 > / g was used without partial hydration. The Ig-loss of the magnesium oxide as the raw material was 0.44%.
[Comparative Example 2]
A mean particle size of 0.76㎛ and a specific surface area with 19.68m 2 / g of 1 hour and the surface of the magnesium in the temperature 60 ℃, a humidity of 90% humidity and a constant temperature oxidation, the surface part by a specific surface area of hydrated 20.78m 2 / g , And the Ig-loss was 2.58%.
[Comparative Example 3]
The average particle diameter of 1.86㎛ a specific surface area 1.59m 2 / g of the magnesium oxide, the temperature 80 ℃, with 30 hours in a constant temperature and humidity of the humidity of 90%, a specific surface area of 3.8m 2 / g, the Ig-loss 25.3 %, In the same manner as in Example 1.
[Comparative Example 4]
The magnesium hydroxide produced in Example 1 was calcined at 1,500 DEG C for 1 hour in an air atmosphere to obtain magnesium oxide particles.
The measurement results of the magnesium hydroxide particles and the magnesium oxide particles obtained by the above examples are shown in Table 1, and the measurement results of the magnesium hydroxide particles and the magnesium oxide particles obtained by the comparative examples are shown in Table 2.
Raw material magnesium oxide
Some hydrated magnesium oxide
Some hydrated magnesium oxide
Claims (8)
Further, it is preferable to add 0.01 to 4.0 mass% in terms of oxide of a metal element selected from the group consisting of Zn, Zr, Hf and Ti, and further metal elements selected from the group consisting of divalent and trivalent metals (provided that Zn, Zr, Hf and Ti are excluded) in an amount of 0.01 to 5.0% by mass in terms of metal element.
Further, it is preferable to add 0.01 to 4.0 mass% in terms of oxide of a metal element selected from the group consisting of Zn, Zr, Hf and Ti, and further metal elements selected from the group consisting of divalent and trivalent metals (provided that Zn, Zr, Hf and Ti are excluded) in an amount of 0.01 to 5.0% by mass in terms of metal element.
(a) at least one compound selected from the group consisting of Zn, Zr, Hf and Ti is added to a dispersion containing a chloride of a divalent and trivalent metal element and a nitrate of a divalent and trivalent metal element A step of adding at least one compound (except for the compound of Zn, Zr, Hf and Ti) and further adding an organic acid to obtain a reaction solution,
(b) a 50% particle diameter (D 50 ) of 0.1 to 10 탆 and a specific surface area of 1.0 to 20.0 m 2 / g in the volume of the reaction solution obtained by the reaction solution and the laser diffraction scattering type particle size distribution measurement of step (a) A step of mixing a partially hydrated magnesium oxide having Ig-loss of 2.0 to 25.0% to obtain a mixed solution,
(Wherein at least one compound selected from the group consisting of Zn, Zr, Hf and Ti compounds is 0.1 to 5.0 mass% in terms of oxide relative to a part of hydrated magnesium oxide particles,
The at least one compound selected from the group consisting of chloride of divalent and trivalent metal elements and nitrate of divalent and trivalent metal elements is 0.1 to 5.0 mass% in terms of metal element with respect to a part of hydrated magnesium oxide,
And the organic acid is 0.01 to 3.0 moles with respect to 100 g of a part of hydrated magnesium oxide)
(c) mixing the mixture of step (b) at a temperature of from 50 to 100 캜 using a stirrer having a peripheral speed of from 7 to 20 m / s,
(d) stirring at a temperature of 30 to 100 DEG C to obtain a magnesium hydroxide slurry, and
(e) a step of obtaining magnesium hydroxide particles by filtering, washing and drying the magnesium hydroxide slurry of the step (d)
≪ / RTI >
Wherein the partially hydrous magnesium oxide of step (b) has a volume fraction of 50% particle size (D 50 ) of 0.1 to 10 μm and a specific surface area of 1.0 to 15.0 m 2 / g by volume particle size measurement by laser diffraction scattering type particle size distribution measurement Wherein the magnesium particles are kept at a temperature of 40 to 95 DEG C and a humidity of 60 to 95% for 0.5 to 24 hours.
Wherein the concentration of the partially hydrated magnesium oxide in the mixed solution of step (b) is 20 to 200 g / L.
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| 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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| 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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| KR20100022047A (en) * | 2007-06-27 | 2010-02-26 | 다테호 가가쿠 고교 가부시키가이샤 | Magnesium oxide particle aggregate, and method for production thereof |
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| JP2835473B2 (en) * | 1990-12-26 | 1998-12-14 | 利昌工業株式会社 | Filler for sealing resin and method for producing the same |
| 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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| JP2000357537A (en) * | 1999-06-16 | 2000-12-26 | Mitsubishi Chemicals Corp | Magnesium oxide for purification of nonaqueous electrolyte and its preparation |
| JP2003261796A (en) | 2002-03-11 | 2003-09-19 | Merck Ltd | Extender and method for producing the same |
| JP2007217201A (en) * | 2006-02-14 | 2007-08-30 | Merck Ltd | Porous magnesia and method for producing the same |
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| KR101878963B1 (en) * | 2016-05-13 | 2018-07-16 | 코노시마카가쿠코우교우 가부시키가이샤 | Magnesium oxide powder and manufacturing method thereof |
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| JP2013063878A (en) | 2013-04-11 |
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| TWI546257B (en) | 2016-08-21 |
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