JP2012201511A5 - - Google Patents
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- JP2012201511A5 JP2012201511A5 JP2011064481A JP2011064481A JP2012201511A5 JP 2012201511 A5 JP2012201511 A5 JP 2012201511A5 JP 2011064481 A JP2011064481 A JP 2011064481A JP 2011064481 A JP2011064481 A JP 2011064481A JP 2012201511 A5 JP2012201511 A5 JP 2012201511A5
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すなわち、本発明は、鱗片状の一次粒子が凝集した球形状であり、細孔分布における、モード容積が１．４ｍｌ/ｇ以上であり、モード径が０．４μｍ以上である、水酸化マグネシウム粒子に関する。
本発明は、レーザ回折散乱式粒度分布測定による体積累積の５０％粒子径（Ｄ５０）が０．５〜２０μmである、前記に記載の水酸化マグネシウム粒子に関する。
本発明は、吸油量が３０ｍｌ/１００ｇ以上である、前記に記載の水酸化マグネシウム粒子に関する。
本発明は、さらに、Ｚｎ、Ｚｒ、Ｈｆ、及びＴｉよりなる群から選択される１以上の金属元素を、酸化物換算で０．０１〜４．０質量％含み、さらに、２価及び３価の金属元素からなる群より選択される１以上の金属元素（ただし、Ｚｎ、Ｚｒ、Ｈｆ、及びＴｉは除く）を、金属元素換算で０．０１〜５．０質量％含む、前記に記載の水酸化マグネシウム粒子に関する。
本発明は、鱗片状の一次粒子が凝集した球形状であり、細孔分布における、モード容積が１．４ｍｌ/ｇ以上であり、モード径が０．４μｍ以上である、酸化マグネシウム粒子に関する。
本発明は、レーザ回折散乱式粒度分布測定による体積累積の５０％粒子径（Ｄ５０）が０．５〜２０μｍである、前記に記載の酸化マグネシウム粒子に関する。
本発明は、吸油量が３０ｍｌ/１００ｇ以上である、前記に記載の酸化マグネシウム粒子に関する。
本発明は、さらに、Ｚｎ、Ｚｒ、Ｈｆ、及びＴｉからなる群より選択される１以上の金属元素を、酸化物換算で０．０１〜４．０質量％含み、さらに、２価及び３価の金属元素からなる群より選択される１以上の更なる金属元素（ただし、Ｚｎ、Ｚｒ、Ｈｆ、及びＴｉは除く）を、金属元素換算で０．０１〜５．０質量％含む、前記に記載の酸化マグネシウム粒子に関する。
本発明は、水酸化マグネシウム粒子の製造方法であって、
（ａ）Ｚｎ、Ｚｒ、Ｈｆ、及びＴｉの化合物からなる群より選択される１以上の化合物を含む分散液に、２価及び３価の金属元素の塩化物、並びに２価及び３価の金属元素の硝酸塩からなる群より選択される１以上の化合物（ただし、Ｚｎ、Ｚｒ、Ｈｆ、及びＴｉの化合物は除く）を添加し、さらに、有機酸を添加して反応液を得る工程、
（ｂ）工程（ａ）の反応液及び平均粒子径が０．１〜３０μｍである酸化マグネシウム粒子を混合して、混合液を得る工程、
（ここで、
Ｚｎ、Ｚｒ、Ｈｆ、及びＴｉの化合物からなる群より選択される１以上の化合物は、酸化マグネシウム粒子に対して、酸化物換算で、０．１〜５．０質量％であり、
２価及び３価の金属元素の塩化物、並びに２価及び３価の金属元素の硝酸塩からなる群より選択される１以上の化合物は、酸化マグネシウム粒子に対して、金属元素換算で、０．１〜５．０質量％であり、
有機酸は、酸化マグネシウム粒子１００ｇに対して、０．０１〜３．０ｍｏｌである）
（ｃ）工程（ｂ）の混合液を、５０〜１００℃の温度で、周速が７〜２０ｍ／ｓである撹拌機を用いて混合する工程、
（ｄ）３０〜１００℃の温度で、長時間撹拌して水酸化マグネシウムスラリーを得る工程、
及び
（ｅ）工程（ｄ）の水酸化マグネシウムスラリーをろ過、水洗、乾燥させて、水酸化マグネシウム粒子を得る工程
を含む、水酸化マグネシウム粒子の製造方法に関する。
本発明は、工程（ｂ）の混合液における、酸化マグネシウムの濃度が２０〜２００ｇ／Ｌである、前記に記載の水酸化マグネシウム粒子の製造方法に関する。
本発明は、酸化マグネシウム粒子の製造方法であって、前記に記載の水酸化マグネシウム粒子又は前記に記載の方法により得られた水酸化マグネシウム粒子を、大気雰囲気中で、５００〜１４００℃で焼成する工程を含む、酸化マグネシウム粒子の製造方法に関する。
That is, the present invention has a spherical shape in which scaly primary particles are aggregated, and has a mode volume of 1.4 ml / g or more and a mode diameter of 0.4 μm or more in the pore distribution. Concerning particles.
The present invention relates to the magnesium hydroxide particles as described above, wherein the 50% particle diameter (D 50 ) of volume accumulation by laser diffraction scattering type particle size distribution measurement is 0.5 to 20 μm.
The present invention relates to the magnesium hydroxide particles described above, wherein the oil absorption is 30 ml / 100 g or more.
The present invention further includes 0.01 to 4.0% by mass of one or more metal elements selected from the group consisting of Zn, Zr, Hf, and Ti in terms of oxides, and further includes divalent and trivalent elements. Including one to one or more metal elements selected from the group consisting of metal elements (excluding Zn, Zr, Hf, and Ti) in terms of metal elements of 0.01 to 5.0% by mass It relates to magnesium hydroxide particles.
The present invention relates to magnesium oxide particles having a spherical shape in which scaly primary particles are aggregated, having a mode volume of 1.4 ml / g or more and a mode diameter of 0.4 μm or more in a pore distribution.
The present invention relates to the magnesium oxide particles described above, wherein the 50% particle diameter (D 50 ) of cumulative volume by laser diffraction scattering particle size distribution measurement is 0.5 to 20 μm.
The present invention relates to the magnesium oxide particles described above having an oil absorption of 30 ml / 100 g or more.
The present invention further includes one or more metal elements selected from the group consisting of Zn, Zr, Hf, and Ti in an amount of 0.01 to 4.0% by mass in terms of oxides. One to one or more further metal elements selected from the group consisting of metal elements (excluding Zn, Zr, Hf, and Ti) are contained in an amount of 0.01 to 5.0% by mass in terms of metal elements, It relates to the described magnesium oxide particles.
The present invention is a method for producing magnesium hydroxide particles,
(A) In a dispersion containing one or more compounds selected from the group consisting of Zn, Zr, Hf, and Ti, divalent and trivalent metal element chlorides, and divalent and trivalent metals Adding one or more compounds selected from the group consisting of elemental nitrates (excluding Zn, Zr, Hf, and Ti compounds), and further adding an organic acid to obtain a reaction solution;
(B) a step of mixing the reaction solution of step (a) and magnesium oxide particles having an average particle size of 0.1 to 30 μm to obtain a mixed solution;
(here,
One or more compounds selected from the group consisting of compounds of Zn, Zr, Hf, and Ti are 0.1 to 5.0% by mass in terms of oxides with respect to the magnesium oxide particles,
One or more compounds selected from the group consisting of chlorides of divalent and trivalent metal elements, and nitrates of divalent and trivalent metal elements are in the form of 0. 1 to 5.0 mass%,
(The organic acid is 0.01 to 3.0 mol with respect to 100 g of magnesium oxide particles)
(C) A step of mixing the mixed liquid of step (b) at a temperature of 50 to 100 ° C. using a stirrer having a peripheral speed of 7 to 20 m / s,
(D) a step of stirring for a long time at a temperature of 30 to 100 ° C. to obtain a magnesium hydroxide slurry;
And (e) relates to a method for producing magnesium hydroxide particles, comprising the step of filtering, washing and drying the magnesium hydroxide slurry in step (d) to obtain magnesium hydroxide particles.
The present invention relates to the method for producing magnesium hydroxide particles as described above, wherein the concentration of magnesium oxide in the mixed liquid in step (b) is 20 to 200 g / L.
The present invention is a method for producing magnesium oxide particles, wherein the magnesium hydroxide particles described above or the magnesium hydroxide particles obtained by the method described above are fired at 500 to 1400 ° C. in an air atmosphere. The present invention relates to a method for producing magnesium oxide particles, including a step.
本発明の水酸化マグネシウム粒子は、鱗片状の一次粒子が凝集した球形状であり、細孔分布のモード容積が１．４ｍｌ/ｇ以上であり、モード径が０．４μｍ以上である。本発明において、一次粒子の形状は鱗片状であり、鱗片の厚み（短軸）が、例えば０．０１〜０．１μｍであり、厚みに対する鱗片の最大長さの比率（アスペクト比）が、例えば１０〜１０００である。このような一次粒子が凝集した球形状の粒子は、均一な細孔が粒子表面に存在し、従来の製造方法により得られる六角板状の水酸化マグネシウム粒子に比べて、液体及び気体分子の吸着性が高く、形状が球状であることから樹脂等に対する分散性が高い。また、このようなモード径を有する水酸化マグネシウム粒子を用紙のコーティング剤として使用した場合、インクの定着性及び吸収性が良好である。さらに、このようなモード容積を有する水酸化マグネシウム粒子は、球状を構成している鱗片状の水酸化マグネシウムが密集しすぎないため、インクの吸着性が良好である。本発明の水酸化マグネシウム粒子の細孔分布のモード容積は、好ましくは１．４〜１０ｍｌ/ｇであり、モード径は、好ましくは０．４〜３．０μｍであり、より好ましくは０．５〜２．０μｍである。 The magnesium hydroxide particle of the present invention has a spherical shape in which scaly primary particles are aggregated, has a mode volume of pore distribution of 1.4 ml / g or more, and a mode diameter of 0.4 μm or more. In the present invention, the shape of the primary particles is scaly, the thickness of the scale (short axis) is, for example, 0.01 to 0.1 μm, and the ratio of the maximum length of the scale to the thickness (aspect ratio) is, for example, 10 to 1000. Spherical particles in which primary particles are agglomerated have uniform pores on the particle surface and adsorb liquid and gas molecules compared to hexagonal plate-like magnesium hydroxide particles obtained by conventional manufacturing methods. High dispersibility with respect to resins and the like due to its spherical shape. In addition, when the magnesium hydroxide particles having such a mode diameter are used as a paper coating agent, the ink fixing property and absorption property are good. Furthermore, the magnesium hydroxide particles having such a mode volume have good ink adsorbability because the scale-like magnesium hydroxide constituting the sphere is not too dense. The mode volume of pore distribution of the magnesium hydroxide particles of the present invention is preferably 1.4 to 10 ml / g , and the mode diameter is preferably 0.4 to 3.0 μm, more preferably 0.00. 5 to 2.0 μm.
本発明の酸化マグネシウム粒子は、鱗片状の一次粒子が凝集した球形状であり、細孔分布のモード容積が１．４ｍｌ/ｇ以上であり、モード径が０．４μｍ以上である。このような酸化マグネシウム粒子は、樹脂等への分散性が優れている。具体的には、このようなモード径を有する酸化マグネシウム粒子は、用紙のコーティング剤として使用した場合、インクの定着性及び吸収性が良好であり、またこのようなモード容積を有する酸化マグネシウム粒子は、球状を構成している鱗片状の酸化マグネシウムが密集しすぎず、インクの吸着性が良好である。細孔分布のモード容積は、好ましくは１．４〜１０ｍｌ/ｇであり、モード径は、好ましくは０．４〜３．０μｍであり、より好ましくは０．５〜２．０μｍである。 The magnesium oxide particles of the present invention have a spherical shape in which scaly primary particles are aggregated, the mode volume of pore distribution is 1.4 ml / g or more, and the mode diameter is 0.4 μm or more. Such magnesium oxide particles have excellent dispersibility in a resin or the like. Specifically, when the magnesium oxide particles having such a mode diameter are used as a paper coating agent, the fixability and absorbability of the ink are good, and the magnesium oxide particles having such a mode volume are In addition, the scale-like magnesium oxide constituting the sphere is not too dense, and the ink adsorbability is good. The mode volume of the pore distribution is preferably 1.4 to 10 ml / g , and the mode diameter is preferably 0.4 to 3.0 μm, more preferably 0.5 to 2.0 μm.
Claims (13)
（ａ）Ｚｎ、Ｚｒ、Ｈｆ、及びＴｉの化合物からなる群より選択される１以上の化合物を含む分散液に、２価及び３価の金属元素の塩化物、並びに２価及び３価の金属元素の硝酸塩からなる群より選択される１以上の化合物（ただし、Ｚｎ、Ｚｒ，Ｈｆ、及びＴｉの化合物は除く）を添加し、さらに、有機酸を添加して反応液を得る工程、
（ｂ）工程（ａ）の反応液及び平均粒子径が０．１〜３０μｍである酸化マグネシウム粒子を混合して、混合液を得る工程
（ここで、
Ｚｎ、Ｚｒ、Ｈｆ、及びＴｉの化合物からなる群より選択される１以上の化合物は、酸化マグネシウムに対して、酸化物換算で０．１〜５．０質量％であり、
２価及び３価の金属元素の塩化物、並びに２価及び３価の金属元素硝酸塩からなる群より選択される１以上の化合物は、酸化マグネシウムに対して、金属元素換算で０．１〜５．０質量％であり、
有機酸は、酸化マグネシウム１００ｇに対し、０．０１〜３．０ｍｏｌである）、
（ｃ）工程（ｂ）の混合液を５０〜１００℃の温度で、周速が７〜２０ｍ／ｓである撹拌機を用いて混合する工程、
（ｄ）３０〜１００℃の温度で、長時間撹拌して水酸化マグネシウムスラリーを得る工程、
及び
（ｅ）工程（ｄ）の水酸化マグネシウムスラリーをろ過、水洗、乾燥させて、水酸化マグネシウム粒子を得る工程
を含む、水酸化マグネシウム粒子の製造方法。 A method for producing magnesium hydroxide particles, comprising:
(A) In a dispersion containing one or more compounds selected from the group consisting of Zn, Zr, Hf, and Ti, divalent and trivalent metal element chlorides, and divalent and trivalent metals Adding one or more compounds selected from the group consisting of elemental nitrates (excluding Zn, Zr, Hf, and Ti compounds), and further adding an organic acid to obtain a reaction solution;
(B) A step of mixing the reaction solution of step (a) and magnesium oxide particles having an average particle size of 0.1 to 30 μm to obtain a mixed solution (here,
One or more compounds selected from the group consisting of compounds of Zn, Zr, Hf, and Ti are 0.1 to 5.0% by mass in terms of oxides with respect to magnesium oxide,
One or more compounds selected from the group consisting of divalent and trivalent metal element chlorides and divalent and trivalent metal element nitrates are 0.1 to 5 in terms of metal elements with respect to magnesium oxide. 0.0 mass%,
The organic acid is 0.01 to 3.0 mol with respect to 100 g of magnesium oxide)
(C) A step of mixing the mixed liquid in step (b) at a temperature of 50 to 100 ° C. using a stirrer having a peripheral speed of 7 to 20 m / s,
(D) a step of stirring for a long time at a temperature of 30 to 100 ° C. to obtain a magnesium hydroxide slurry;
And (e) A method for producing magnesium hydroxide particles, comprising the step of filtering, washing with water and drying the magnesium hydroxide slurry in step (d) to obtain magnesium hydroxide particles.
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011064481A JP5773695B2 (en) | 2011-03-23 | 2011-03-23 | Spherical magnesium hydroxide particles, spherical magnesium oxide particles, and methods for producing them |
| CN201280014702.4A CN103443028B (en) | 2011-03-23 | 2012-01-16 | Spherical magnesium hydroxide particle and spherical magnesium oxide particle and their manufacture method |
| KR1020137023864A KR101859071B1 (en) | 2011-03-23 | 2012-01-16 | Spherical magnesium hydroxide particle, spherical magnesium oxide particle, and method for producing same |
| PCT/JP2012/050706 WO2012127889A1 (en) | 2011-03-23 | 2012-01-16 | Spherical magnesium hydroxide particle, spherical magnesium oxide particle, and method for producing same |
| TW101104168A TWI519483B (en) | 2011-03-23 | 2012-02-09 | Globular magnesium hydroxide particles, globular mangesium oxide particles and method for manufacturing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011064481A JP5773695B2 (en) | 2011-03-23 | 2011-03-23 | Spherical magnesium hydroxide particles, spherical magnesium oxide particles, and methods for producing them |
Publications (3)
| Publication Number | Publication Date |
|---|---|
| JP2012201511A JP2012201511A (en) | 2012-10-22 |
| JP2012201511A5 true JP2012201511A5 (en) | 2014-10-30 |
| JP5773695B2 JP5773695B2 (en) | 2015-09-02 |
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| JP2011064481A Active JP5773695B2 (en) | 2011-03-23 | 2011-03-23 | Spherical magnesium hydroxide particles, spherical magnesium oxide particles, and methods for producing them |
Country Status (5)
| Country | Link |
|---|---|
| JP (1) | JP5773695B2 (en) |
| KR (1) | KR101859071B1 (en) |
| CN (1) | CN103443028B (en) |
| TW (1) | TWI519483B (en) |
| WO (1) | WO2012127889A1 (en) |
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| JP5992846B2 (en) * | 2013-02-13 | 2016-09-14 | タテホ化学工業株式会社 | Rod-shaped magnesium hydroxide particles having a high specific surface area, rod-shaped magnesium oxide particles, and methods for producing them |
| JP6817235B2 (en) * | 2017-02-17 | 2021-01-20 | タテホ化学工業株式会社 | Spherical magnesium oxide and its manufacturing method |
| JP6901726B2 (en) * | 2017-08-31 | 2021-07-14 | タテホ化学工業株式会社 | Chemical heat storage material and its manufacturing method |
| CN113874323A (en) * | 2019-03-29 | 2021-12-31 | 达泰豪化学工业株式会社 | Spherical magnesium oxide, method for producing same, thermally conductive filler, and resin composition |
| CN112752732B (en) * | 2019-03-29 | 2023-03-17 | 达泰豪化学工业株式会社 | Spherical magnesium oxide, method for producing same, thermally conductive filler, and resin composition |
| JP7478631B2 (en) * | 2020-09-15 | 2024-05-07 | デンカ株式会社 | Magnesium oxide powder, filler composition, resin composition, and heat dissipation part |
| TW202330412A (en) * | 2021-10-15 | 2023-08-01 | 日商達泰豪化學工業股份有限公司 | Spherical magnesium oxide, method for producing the same, resin filler and resin composition |
| 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 |
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| 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 |
| JPS61168522A (en) * | 1985-01-19 | 1986-07-30 | Asahi Glass Co Ltd | Magnesium hydroxide and production thereof |
| EP0189098B1 (en) * | 1985-01-19 | 1992-05-06 | Asahi Glass Company Ltd. | Magnesium hydroxide, process for its production and resin composition containing it |
| 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 |
| CN101679058B (en) * | 2007-03-30 | 2012-11-14 | 宇部材料工业株式会社 | Magnesium hydroxide powder and method for producing the same |
| JP5016993B2 (en) * | 2007-06-27 | 2012-09-05 | タテホ化学工業株式会社 | Magnesium oxide particle aggregate and method for producing the same |
-
2011
- 2011-03-23 JP JP2011064481A patent/JP5773695B2/en active Active
-
2012
- 2012-01-16 KR KR1020137023864A patent/KR101859071B1/en active IP Right Grant
- 2012-01-16 WO PCT/JP2012/050706 patent/WO2012127889A1/en active Application Filing
- 2012-01-16 CN CN201280014702.4A patent/CN103443028B/en active Active
- 2012-02-09 TW TW101104168A patent/TWI519483B/en active
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