JP2009007215A - Spherical magnesium oxide particles and method for producing the same - Google Patents
Spherical magnesium oxide particles and method for producing the same Download PDFInfo
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本発明は、一次粒子が球状である酸化マグネシウムとその製造方法に関する。 The present invention relates to magnesium oxide whose primary particles are spherical and a method for producing the same.
酸化マグネシウム粒子は耐熱性、熱伝導性、電気絶縁性にすぐれており、断熱材、耐熱部品、放熱用フィラーとして有用である。なかでも、酸化マグネシウム粒子を樹脂成形物からなる電子部品等における放熱性フィラーとして用いる際には、成形物を形成する樹脂に高充填し得ることが必要であり、従って、一次粒子としての分散性にすぐれるように、一次粒子が球状である酸化マグネシウム粒子が強く求められている。 Magnesium oxide particles have excellent heat resistance, thermal conductivity, and electrical insulation, and are useful as heat insulating materials, heat resistant components, and heat radiation fillers. In particular, when using magnesium oxide particles as a heat-dissipating filler in electronic parts made of resin moldings, it is necessary that the resin forming the moldings can be highly filled, and thus dispersibility as primary particles. Therefore, there is a strong demand for magnesium oxide particles whose primary particles are spherical.
従来、二次粒子が球状である酸化マグネシウム粒子を製造する方法は、既に、幾つか知られている。例えば、水中で塩化マグネシウムのような水溶性マグネシウム塩１当量とアンモニア１．０〜３．５当量を４０℃程度の温度で反応させ、その際、水酸化マグネシウムの晶析負荷と晶析した水酸化マグネシウムの濃度を制御しつつ、水酸化マグネシウムの一次粒子の集合体を晶析させ、次いで、得られた水酸化マグネシウムを１２００〜２０００℃で焼成して、見掛け上、球状の高耐水性酸化マグネシウム粒子を得ることができることが知られている（特許文献１参照）。 Conventionally, several methods for producing magnesium oxide particles whose secondary particles are spherical are already known. For example, 1 equivalent of a water-soluble magnesium salt such as magnesium chloride and 1.0 to 3.5 equivalents of ammonia are reacted in water at a temperature of about 40 ° C. At that time, the crystallization load of magnesium hydroxide and the crystallized water The aggregate of primary particles of magnesium hydroxide is crystallized while controlling the concentration of magnesium oxide, and then the obtained magnesium hydroxide is calcined at 1200 to 2000 ° C. to give an apparently spherical high water resistance oxidation. It is known that magnesium particles can be obtained (see Patent Document 1).
また、水中で塩化マグネシウムのような水溶性マグネシウム塩１当量とアルカリ性物質０．９５当量以下を４０℃以下で反応させ、得られた反応生成物をその反応母液と共に５０〜１２０℃の温度に更に加熱し、得られた水酸化マグネシウムを噴霧乾燥して、平均二次粒子径約５〜５００μｍに造粒した後、得られた造粒物を１１００〜１６００℃で焼成し、次いで、得られた焼成物を上記平均二次粒子径を破壊しないように粉砕して、上記平均二次粒子径を有し、ほぼ球状である高耐水和性高流動性の酸化マグネシウム粒子を得ることができることも知られている（特許文献２参照）。 Also, 1 equivalent of a water-soluble magnesium salt such as magnesium chloride and 0.95 equivalent or less of an alkaline substance are reacted at 40 ° C. or less in water, and the resulting reaction product is further brought to a temperature of 50 to 120 ° C. together with the reaction mother liquor. After heating and spray-drying the obtained magnesium hydroxide to granulate to an average secondary particle size of about 5 to 500 μm, the resulting granulated product was fired at 1100 to 1600 ° C. and then obtained. It is also known that the baked product can be pulverized so as not to destroy the average secondary particle diameter to obtain highly hydration-resistant and high-fluidity magnesium oxide particles having the average secondary particle diameter and substantially spherical. (See Patent Document 2).
同様に、水中で塩化マグネシウムのような水溶性マグネシウム塩１当量とアルカリ性物質０．９５当量以下を４０℃以下で反応させ、得られた反応生成物をその反応母液と共に更に加熱して、平均二次粒子径２μｍ以下、ＢＥＴ比表面積１〜２０ｍ2／ｇの水酸化マグネシウム粒子を製造し、次いで、この水酸化マグネシウム粒子を約１１００〜１６００℃で焼成した後、得られた焼成物を平均二次粒子径２０μｍ以下に粉砕分級することによって、ほぼ球状の高耐水和性高流動性の酸化マグネシウムを得ることができることが知られている（例えば、特許文献３参照）。 Similarly, 1 equivalent of a water-soluble magnesium salt such as magnesium chloride and 0.95 equivalent or less of an alkaline substance are reacted at 40 ° C. or less in water, and the resulting reaction product is further heated together with the reaction mother liquor to obtain an average of 2 Magnesium hydroxide particles having a secondary particle diameter of 2 μm or less and a BET specific surface area of 1 to 20 m 2 / g are produced. The magnesium hydroxide particles are then fired at about 1100 to 1600 ° C. It is known that an approximately spherical high hydration resistance and high fluidity magnesium oxide can be obtained by pulverizing and classifying to the next particle diameter of 20 μm or less (see, for example, Patent Document 3).
しかし、これまで、一次粒子が球状である酸化マグネシウム粒子を製造する方法は知られていない。
本発明は、酸化マグネシウム粒子の製造における上述した事情に鑑みてなされたものであって、一次粒子が球状である酸化マグネシウム粒子を容易に製造する方法を提供することを目的とし、更に、そのようにして得られる一次粒子が球状である酸化マグネシウム粒子を提供することを目的とする。 The present invention has been made in view of the above-described circumstances in the production of magnesium oxide particles, and an object thereof is to provide a method for easily producing magnesium oxide particles in which the primary particles are spherical. An object of the present invention is to provide magnesium oxide particles in which the primary particles obtained are spherical.
本発明によれば、水酸化マグネシウム１００モル部に対して酢酸基換算で３〜２０モル部の酢酸塩を含有する水酸化マグネシウム組成物を調製し、これを１０００〜１８００℃の範囲の温度で焼成することからなり、上記酢酸塩が酢酸アルカリ金属塩、酢酸アルカリ土類金属及び酢酸アンモニウムから選ばれる少なくとも１種である、一次粒子が球状である酸化マグネシウム粒子の製造方法が提供される。 According to the present invention, a magnesium hydroxide composition containing 3 to 20 parts by mole of acetate in terms of acetate groups with respect to 100 parts by weight of magnesium hydroxide is prepared, and this is at a temperature in the range of 1000 to 1800 ° C. There is provided a method for producing magnesium oxide particles, the primary particles of which are at least one selected from alkali metal acetates, alkaline earth metal acetates, and ammonium acetate.
更に、本発明によれば、上述した方法によって得られる一次粒子が球状である酸化マグネシウム粒子が提供される。 Furthermore, according to this invention, the magnesium oxide particle whose primary particle obtained by the method mentioned above is spherical is provided.
本発明の方法によれば、一次粒子が球状である酸化マグネシウムを容易に得ることができる。このような酸化マグネシウムは、ハンドリング性がよく、例えば、放熱性フィラー、ＰＤＰ保護膜用原料、ＰＤＰ蛍光体用原料、ＰＤＰ酸化マグネシウム層用原料、誘電体用原料等として好適に用いることができる。 According to the method of the present invention, magnesium oxide whose primary particles are spherical can be easily obtained. Such magnesium oxide has good handling properties, and can be suitably used as, for example, a heat-dissipating filler, a PDP protective film material, a PDP phosphor material, a PDP magnesium oxide layer material, and a dielectric material.
本発明による一次粒子が球状である酸化マグネシウム粒子の製造方法は、水酸化マグネシウム１００モル部に対して酢酸基換算で３〜２０モル部の酢酸塩を含有する水酸化マグネシウム組成物を調製し、これを１０００〜１８００℃の範囲の温度で焼成することからなる。 The method for producing magnesium oxide particles in which the primary particles are spherical according to the present invention is prepared by preparing a magnesium hydroxide composition containing 3 to 20 mol parts of acetate in terms of acetate groups with respect to 100 mol parts of magnesium hydroxide, This consists of firing at a temperature in the range of 1000-1800 ° C.
本発明において用いる水酸化マグネシウムは、天然鉱物を粉砕して得られる天然品、水中にて水溶性マグネシウム塩をアルカリ性物質で中和することによって得られる合成品等、その由来において何ら限定されるものではないが、好ましくは、後者の合成品が用いられる。合成品を製造する場合において、上記水溶性マグネシウム塩としては、例えば、塩化マグネシウム、硫酸マグネシウム、硝酸マグネシウム、酢酸マグネシウム等が用いられる。また、上記アルカリ性物質としては、例えば、水酸化ナトリウム、水酸化カリウム、アンモニア等が用いられる。本発明においては、このようなアルカリ性物質は、通常、水溶性マグネシウム塩１当量について、０．８〜１．２当量の範囲で用いられる。 Magnesium hydroxide used in the present invention is a natural product obtained by pulverizing a natural mineral, a synthetic product obtained by neutralizing a water-soluble magnesium salt with an alkaline substance in water, etc. However, the latter synthetic product is preferably used. In the case of producing a synthetic product, examples of the water-soluble magnesium salt include magnesium chloride, magnesium sulfate, magnesium nitrate, and magnesium acetate. Moreover, as said alkaline substance, sodium hydroxide, potassium hydroxide, ammonia etc. are used, for example. In the present invention, such an alkaline substance is usually used in the range of 0.8 to 1.2 equivalents per 1 equivalent of the water-soluble magnesium salt.
本発明においては、水中にて水溶性マグネシウム塩をアルカリ性物質と反応させて、水酸化マグネシウムを製造する場合、好ましくは、水溶性マグネシウム塩１当量をアルカリ性物質０．８〜１．２当量、好ましくは、１．０〜１．２当量と反応させて、水酸化マグネシウムの沈殿を含むスラリーを得、このスラリーを加圧下に温度１２０〜２００℃の範囲で加熱する水熱処理を行い、次いで、得られた反応混合物を、通常、常温まで冷却し、濾過、水洗して、副生塩を除去し、乾燥、粉砕して、通常、平均一次粒子径０．１〜２μｍ、比表面積１〜３０ｍ2／ｇ、好ましくは、平均一次粒子径０．１〜０．２μｍ、比表面積２２〜３０ｍ2／ｇの範囲の六角板状の形状を有する水酸化マグネシウムを得、これに所定の割合で酢酸塩を含有させて、水酸化マグネシウム組成物とし、これを焼成することによって、通常、平均一次粒子径１〜３μｍの範囲の球状の酸化マグネシウム粒子を得ることができる。 In the present invention, when water-soluble magnesium salt is reacted with an alkaline substance in water to produce magnesium hydroxide, preferably 1 equivalent of water-soluble magnesium salt is 0.8 to 1.2 equivalent of alkaline substance, preferably Is reacted with 1.0 to 1.2 equivalents to obtain a slurry containing magnesium hydroxide precipitate, which is hydrothermally treated under pressure at a temperature in the range of 120 to 200 ° C., and then obtained. The resulting reaction mixture is usually cooled to room temperature, filtered and washed with water to remove by-product salts, dried and pulverized, and usually has an average primary particle size of 0.1 to 2 μm and a specific surface area of 1 to 30 m 2. / G, preferably, magnesium hydroxide having a hexagonal plate shape with an average primary particle diameter of 0.1 to 0.2 μm and a specific surface area of 22 to 30 m 2 / g is obtained. Contain In this way, spherical magnesium oxide particles having an average primary particle diameter in the range of 1 to 3 μm can be usually obtained by preparing a magnesium hydroxide composition and firing the composition.
特に、本発明によれば、上述したように、水中にて水溶性マグネシウム塩をアルカリ性物質と反応させて、水酸化マグネシウムを製造する場合に、水溶性マグネシウム塩１当量をアルカリ性物質１当量以上と反応させることによって、平均一次粒子径０．２μｍ以下、比表面積２２ｍ2／ｇ以上の水酸化マグネシウム粒子を得ることができる。 In particular, according to the present invention, as described above, when magnesium hydroxide is produced by reacting a water-soluble magnesium salt with an alkaline substance in water, 1 equivalent of the water-soluble magnesium salt is 1 equivalent or more of the alkaline substance. By reacting, magnesium hydroxide particles having an average primary particle diameter of 0.2 μm or less and a specific surface area of 22 m 2 / g or more can be obtained.
本発明の方法によれば、上記酢酸塩は、酢酸アルカリ金属、酢酸アルカリ土類金属及び酢酸アンモニウムから選ばれる少なくとも１種であり、酢酸アルカリ金属として、例えば、酢酸ナトリウム、酢酸カリウム等を挙げることができ、酢酸アルカリ土類金属として、例えば、酢酸カルシウム、酢酸マグネシウム等を挙げることができる。これらの酢酸塩のなかでは、酢酸アルカリ金属又は酢酸アルカリ土類金属が好ましく用いられる。 According to the method of the present invention, the acetate is at least one selected from alkali metal acetate, alkaline earth metal acetate and ammonium acetate, and examples of the alkali metal acetate include sodium acetate and potassium acetate. Examples of the alkaline earth metal acetate include calcium acetate and magnesium acetate. Among these acetates, alkali metal acetate or alkaline earth metal acetate is preferably used.
更に、本発明によれば、上記酢酸塩は、水酸化マグネシウム１００モル部に対して酢酸基換算で３〜２０モル部の範囲で加えられて、均一な組成物が調製され、この組成物が焼成に供される。ここに、酢酸基とは、ＣＨ3ＣＯＯ- で表される有機基である。焼成に供する組成物の含有する酢酸塩の割合が水酸化マグネシウム１００モル部に対して酢酸基換算で３モル部よりも少ないときは、そのような組成物を焼成しても、一次粒子が球状である酸化マグネシウムを得ることができない。他方、組成物中の酢酸塩の割合が水酸化マグネシウム１００モル部に対して酢酸基換算で２０モル部を越えても、そのような組成物の焼成によって得られる酸化マグネシウムの球状性は、酢酸塩の割合が水酸化マグネシウム１００モル部に対して酢酸基換算で２０モル部までの場合と変わらないので、特に、酢酸塩を水酸化マグネシウム１００モル部に対して酢酸基換算で２０モル部を越える量にて含有させる必要もなく、また、酢酸塩の種類によっては、例えば、酢酸塩がアルカリ金属塩やアルカリ土類金属塩であれば、得られる酸化マグネシウムにおいて、それらマグネシウム以外の金属成分の含有率が大きくなるので、用途によっては、好ましくない場合もある。 Furthermore, according to the present invention, the above-mentioned acetate is added in a range of 3 to 20 parts by mole in terms of acetate based on 100 parts by weight of magnesium hydroxide to prepare a uniform composition. Used for firing. Here, the acetic acid group is an organic group represented by CH 3 COO 2 — . When the proportion of acetate contained in the composition to be fired is less than 3 parts by mole in terms of acetate groups with respect to 100 parts by weight of magnesium hydroxide, the primary particles are spherical even if the composition is fired. It is not possible to obtain magnesium oxide. On the other hand, even when the proportion of acetate in the composition exceeds 20 mol parts in terms of acetate groups with respect to 100 mol parts of magnesium hydroxide, the spherical nature of magnesium oxide obtained by firing such a composition is Since the ratio of the salt is not different from the case of up to 20 mol parts in terms of acetate groups with respect to 100 mol parts of magnesium hydroxide, in particular, 20 mol parts of acetate in terms of acetate groups with respect to 100 mol parts of magnesium hydroxide. It is not necessary to contain in an excess amount, and depending on the type of acetate, for example, if the acetate is an alkali metal salt or an alkaline earth metal salt, the obtained magnesium oxide contains metal components other than those magnesium. Since the content rate is increased, it may not be preferable depending on the application.
本発明によれば、このように、水酸化マグネシウム１００モル部に対して酢酸基換算で３〜２０モル部の酢酸塩を含有する水酸化マグネシウムと酢酸塩との均一な組成物を調製し、これを１０００〜１８００℃の範囲の温度で焼成することによって、一次粒子が球状である酸化マグネシウムを得ることができる。具体的には、好ましくは、水酸化マグネシウムと酢酸塩の均一な組成物を調製し、この組成物を１０００〜１８００℃の範囲の温度で焼成する。 According to the present invention, in this way, a uniform composition of magnesium hydroxide and acetate containing 3 to 20 mole parts of acetate in terms of acetate groups with respect to 100 mole parts of magnesium hydroxide is prepared, By baking this at a temperature in the range of 1000 to 1800 ° C., magnesium oxide whose primary particles are spherical can be obtained. Specifically, preferably, a uniform composition of magnesium hydroxide and acetate is prepared, and the composition is fired at a temperature in the range of 1000 to 1800 ° C.
水酸化マグネシウムを焼成して酸化マグネシウムを得る場合には、先ず、４８０℃程度の温度にて水酸化マグネシウムが脱水分解すると共に、一次粒子の六角板状の形状が崩壊して、微細で不定形の酸化マグネシウムの核が生成し、次に、１０００℃以上の温度でこの核同士が焼結して、酸化マグネシウムが形状性をもつ粒子に成長し、通常は立方体状の粒子に成長する。 In the case of obtaining magnesium oxide by baking magnesium hydroxide, first, magnesium hydroxide is dehydrated and decomposed at a temperature of about 480 ° C., and the hexagonal plate shape of the primary particles collapses, resulting in a fine and irregular shape. Then, the nuclei of magnesium oxide are formed, and then the nuclei are sintered at a temperature of 1000 ° C. or more, so that the magnesium oxide grows into particles having a shape, and usually grows into cubic particles.
ここに、本発明によれば、所定の割合にて酢酸塩を含有する水酸化マグネシウム組成物を焼成する。そこで、本発明によれば、上記酸化マグネシウムが形状性をもつ粒子に成長するに際して、酢酸塩又は酢酸基が酸化マグネシウムの粒子成長を形状的に制御して、粒子の球状化が進むものと推測される。焼成温度が１０００℃より低い場合は、水酸化マグネシウムが脱水分解し、粒子成長する移行段階であり、酸化マグネシウム粒子が未だ、成長していない。一方、焼成温度が１８００℃より高い場合には、それより低い温度において球状の一次粒子が生成していても、その一次粒子は、１８００℃より高い温度において、酸化マグネシウムの本来の結晶系である立方晶の性質を強く有することとなって、その形状が立方体に近づくために、一次粒子の球状性が損なわれる。 Here, according to the present invention, the magnesium hydroxide composition containing acetate at a predetermined ratio is fired. Therefore, according to the present invention, when the magnesium oxide grows into particles having a shape, it is assumed that the acetate or acetate group controls the particle growth of the magnesium oxide in shape, and the spheroidization of the particles proceeds. Is done. When the firing temperature is lower than 1000 ° C., it is a transitional stage in which magnesium hydroxide is dehydrated and decomposed to grow particles, and magnesium oxide particles have not yet grown. On the other hand, when the firing temperature is higher than 1800 ° C., even if spherical primary particles are generated at a lower temperature, the primary particles are the original crystal system of magnesium oxide at a temperature higher than 1800 ° C. Since it has the property of a cubic crystal and its shape approaches that of a cube, the spherical nature of the primary particles is impaired.
酢酸塩として酢酸アンモニウムを用いる場合も、酢酸アンモニウムが分解して生じた酢酸基が上述したように、酸化マグネシウムの粒子成長に際して、粒子成長を形状的に制御して、粒子の球状化が進むものと推測される。 Even when ammonium acetate is used as the acetate salt, the acetate group generated by decomposition of ammonium acetate, as described above, controls the particle growth in the form of magnesium oxide particles, and the particles become more spherical. It is guessed.
前述したように、水中にて水溶性マグネシウム塩をアルカリ性物質と反応させて、水酸化マグネシウムを製造する場合であれば、水中にて水溶性マグネシウム塩をアルカリ性物質で中和して、水酸化マグネシウムのスラリーを得、このスラリーを濾過、水洗、乾燥、粉砕して、水酸化マグネシウムの粉末を得た後、この水酸化マグネシウムを水中に再度、懸濁させて、水酸化マグネシウムの水性スラリーを得、このスラリーに水酸化マグネシウムに対して所定量の酢酸塩を溶解させ、攪拌、混合した後、スラリーを蒸発乾固して、水酸化マグネシウムと酢酸塩との均一な組成物を得、これを焼成に供すればよい。 As described above, in the case of producing magnesium hydroxide by reacting a water-soluble magnesium salt with an alkaline substance in water, the water-soluble magnesium salt is neutralized with an alkaline substance in water, The slurry was filtered, washed with water, dried, and pulverized to obtain a magnesium hydroxide powder. The magnesium hydroxide was suspended again in water to obtain an aqueous magnesium hydroxide slurry. In this slurry, a predetermined amount of acetate is dissolved in magnesium hydroxide, stirred and mixed, and then the slurry is evaporated to dryness to obtain a uniform composition of magnesium hydroxide and acetate. What is necessary is just to use for baking.
また、場合によっては、上述した方法において、水酸化マグネシウムのスラリーを得、このスラリーに過剰量の酢酸塩を溶解させた後、この酢酸塩が水酸化マグネシウムに対して所定の割合で残存するように濾過、水洗し、乾燥して、水酸化マグネシウムと酢酸塩の均一な組成物を調製し、これを焼成に供してもよい。 In some cases, in the above-described method, a magnesium hydroxide slurry is obtained, and after an excessive amount of acetate is dissolved in the slurry, the acetate remains at a predetermined ratio with respect to magnesium hydroxide. The mixture may be filtered, washed with water, and dried to prepare a uniform composition of magnesium hydroxide and acetate, which may be subjected to calcination.
本発明によれば、水溶性マグネシウム塩として、特に酢酸マグネシウムを用いて、これをアルカリ性物質と反応させて、副生酢酸塩と共に水酸化マグネシウムを得、このような副生塩を利用して、水酸化マグネシウムと酢酸塩の均一な組成物を調製し、これを焼成することによっても、一次粒子が球状である酸化マグネシウム粒子を得ることができる。 According to the present invention, magnesium acetate is used as a water-soluble magnesium salt, and this is reacted with an alkaline substance to obtain magnesium hydroxide together with a by-product acetate salt. By using such a by-product salt, Magnesium oxide particles whose primary particles are spherical can also be obtained by preparing a uniform composition of magnesium hydroxide and acetate and firing it.
即ち、水中にて酢酸マグネシウムをアルカリ性物質と反応させて、水酸化マグネシウムと共に、上記アルカリ性物質に対応する酢酸塩を生成させ、例えば、アルカリ性物質として、水酸化ナトリウムを用いた場合には、酢酸ナトリウムを生成させ、かくして、得られた水酸化マグネシウムにおいて、副生した酢酸塩が水酸化マグネシウムに対して前記所定の割合にて残存するように、得られた水酸化マグネシウムを水洗、濾過し、これを乾燥して、水酸化マグネシウムと酢酸塩との均一な組成物を得、これを焼成に供する。酢酸マグネシウムとアルカリ性物質との反応によって得られた水酸化マグネシウムに残存する酢酸塩の量は、例えば、得られた水酸化マグネシウムを水洗したときの水洗水の導電率を調べることによって知ることができる。 That is, magnesium acetate is reacted with an alkaline substance in water to form an acetate corresponding to the alkaline substance together with magnesium hydroxide. For example, when sodium hydroxide is used as the alkaline substance, sodium acetate In this way, the obtained magnesium hydroxide was washed with water and filtered so that the by-produced acetate remained at the predetermined ratio with respect to the magnesium hydroxide. Is dried to obtain a uniform composition of magnesium hydroxide and acetate, which is subjected to calcination. The amount of acetate remaining in magnesium hydroxide obtained by the reaction between magnesium acetate and an alkaline substance can be known, for example, by examining the conductivity of the washing water when the obtained magnesium hydroxide is washed with water. .
更に、本発明によれば、任意の方法で得た水酸化マグネシウムの水性スラリー、例えば、前述したように、水溶性マグネシウム塩とアルカリ性物質を水中で反応させ、水酸化マグネシウムを生成させて、水酸化マグネシウムの水性スラリーを得、これに酢酸を加えて、水酸化マグネシウムと反応させて、酢酸塩を生成させ、これを利用して、酢酸塩と水酸化マグネシウムとの組成物を調製してもよく、また、酢酸と、これと反応して酢酸塩を生成する化合物を加えて、酢酸塩を生成させ、これを利用して、酢酸塩と水酸化マグネシウムとの組成物を調製してもよい。 Furthermore, according to the present invention, an aqueous slurry of magnesium hydroxide obtained by an arbitrary method, for example, as described above, a water-soluble magnesium salt and an alkaline substance are reacted in water to produce magnesium hydroxide, An aqueous slurry of magnesium oxide is obtained, and acetic acid is added thereto to react with magnesium hydroxide to produce an acetate salt. This can be used to prepare a composition of acetate and magnesium hydroxide. Well, acetic acid and a compound that reacts with it to form an acetate salt are added to form an acetate salt, which can be used to prepare a composition of acetate and magnesium hydroxide. .
以下に比較例と共に実施例を挙げて本発明を説明するが、本発明はこれら実施例によって何ら限定されるものではない。以下の実施例及び比較例において、得られた酸化マグネシウム粒子の比表面積はＢＥＴ法によって測定した。 Hereinafter, the present invention will be described by way of examples together with comparative examples, but the present invention is not limited to these examples. In the following examples and comparative examples, the specific surface area of the obtained magnesium oxide particles was measured by the BET method.
また、得られた酸化マグネシウム粒子の平均一次粒子径と形状性は走査型電子顕微鏡写真から評価した。即ち、適切な倍率の走査型電子顕微鏡写真の短辺と長辺のそれぞれの中間点から写真の中心点を通る２本の直線と２本の対角線を描き、これら４本の直線の少なくともいずれかの線上にある粒子を対象粒子として合計１００個の粒子を選択した。この際、複数の写真を合計して評価してもよいとした。平均一次粒子径の測定については、選択した１００個の粒子の写真の長辺方向の長さを測定し、その平均を平均一次粒子径とした。 Moreover, the average primary particle diameter and shape of the obtained magnesium oxide particles were evaluated from scanning electron micrographs. That is, draw two straight lines and two diagonals from the middle point of the short side and long side of the scanning electron micrograph of an appropriate magnification through the center point of the photo, and at least one of these four straight lines A total of 100 particles were selected with the particles on the line as the target particles. At this time, a plurality of photographs may be totaled and evaluated. About the measurement of an average primary particle diameter, the length of the long side direction of the photograph of 100 selected particles was measured, and the average was made into the average primary particle diameter.
形状性については、選択した１００個の粒子について、その形状性を観察した。本発明では、この形状性における球状粒子とは、粒子の短軸と長軸の比（短軸／長軸比）が０．８以上、１．０以下であると共に、輪郭線が凸である曲線（１つの直線を含んでもよい）から形成されている酸化マグネシウム粒子をいうものとする。一次粒子が球状な酸化マグネシウムとは、形状性を観察した１００個の粒子のうち、８０％以上が球状粒子であるものとする。 Regarding the shape, the shape of the selected 100 particles was observed. In the present invention, the spherical particles in this formability have a ratio of the minor axis to the major axis (minor axis / major axis ratio) of 0.8 or more and 1.0 or less, and the contour is convex. Magnesium oxide particles formed from a curve (which may include one straight line) shall be used. Magnesium oxide with spherical primary particles means that 80% or more of 100 particles whose shape properties are observed are spherical particles.
実施例１
（酢酸ナトリウムを用いる酸化マグネシウム粒子Ａの製造）
純水０．３Ｌを張った沈殿反応器に４モル／Ｌ濃度の塩化マグネシウム水溶液１Ｌと１４．３モル／Ｌ濃度の水酸化ナトリウム水溶液０．５５９Ｌを同時に注入して、水酸化マグネシウムの沈殿を含むスラリーを得た。水熱処理として、このスラリーを２時間をかけて１６０℃まで加熱し、その時点で加熱を止めて、室温まで放冷した。このようにして得られた反応混合物を濾過、水洗、乾燥した後、粉砕して、水酸化マグネシウム粉末を得た。この水酸化マグネシウムの平均一次粒子径は０．２μｍ、比表面積は２３ｍ2／ｇであった。
Example 1
(Production of magnesium oxide particles A using sodium acetate)
1 L of 4 mol / L magnesium chloride aqueous solution and 0.559 L of 14.3 mol / L sodium hydroxide aqueous solution were simultaneously injected into a precipitation reactor filled with 0.3 L of pure water to precipitate magnesium hydroxide. A slurry containing was obtained. As a hydrothermal treatment, this slurry was heated to 160 ° C. over 2 hours, at which point the heating was stopped and the mixture was allowed to cool to room temperature. The reaction mixture thus obtained was filtered, washed with water, dried and then pulverized to obtain a magnesium hydroxide powder. This magnesium hydroxide had an average primary particle size of 0.2 μm and a specific surface area of 23 m 2 / g.
次に、このようにして得られた水酸化マグネシウム２１３ｇを純水中に再懸濁して、水酸化マグネシウムの水性スラリーとし、これに酢酸ナトリウム１０．５ｇ加え、１時間攪拌した後、この水性スラリーを蒸発乾固して、酢酸ナトリウムと水酸化マグネシウムとの均一な組成物を得た。これを１１００℃で１時間焼成して、本発明による酸化マグネシウム粒子Ａを得た。 Next, 213 g of the magnesium hydroxide thus obtained was resuspended in pure water to obtain an aqueous slurry of magnesium hydroxide, 10.5 g of sodium acetate was added thereto, and the mixture was stirred for 1 hour. Was evaporated to dryness to obtain a uniform composition of sodium acetate and magnesium hydroxide. This was fired at 1100 ° C. for 1 hour to obtain magnesium oxide particles A according to the present invention.
用いた酢酸塩の酢酸基換算の量と得られた酸化マグネシウム粒子における球状粒子の割合と平均一次粒子径を表１に示す（以下、同じ）。 The amount of acetate used in terms of acetate group, the ratio of spherical particles in the obtained magnesium oxide particles and the average primary particle size are shown in Table 1 (hereinafter the same).
実施例２
（酢酸ナトリウムを用いる酸化マグネシウム粒子Ｂの製造）
実施例１と同様にして得られた酢酸ナトリウムと水酸化マグネシウムとの均一な組成物を１２００℃で１時間焼成して、本発明による酸化マグネシウム粒子Ｂを得た。
Example 2
(Production of magnesium oxide particles B using sodium acetate)
A uniform composition of sodium acetate and magnesium hydroxide obtained in the same manner as in Example 1 was calcined at 1200 ° C. for 1 hour to obtain magnesium oxide particles B according to the present invention.
実施例３
（酢酸ナトリウムを用いる酸化マグネシウム粒子Ｃの製造）
実施例１と同様にして得られた酢酸ナトリウムと水酸化マグネシウムとの均一な組成物を１４００℃で１時間焼成して、本発明による酸化マグネシウム粒子Ｃを得た。
Example 3
(Production of magnesium oxide particles C using sodium acetate)
A uniform composition of sodium acetate and magnesium hydroxide obtained in the same manner as in Example 1 was calcined at 1400 ° C. for 1 hour to obtain magnesium oxide particles C according to the present invention.
実施例４
（酢酸ナトリウムを用いる酸化マグネシウム粒子Ｄの製造）
実施例１と同様にして得られた水酸化マグネシウム２１３ｇを純水中に再懸濁して、水酸化マグネシウムの水性スラリーとし、この水性スラリー中に酢酸ナトリウム２１ｇを加え、１時間攪拌した後、この水性スラリーを蒸発乾固して、酢酸ナトリウムと水酸化マグネシウムとの均一な組成物を得た。これを１２００℃で１時間焼成して、本発明による酸化マグネシウム粒子Ｄを得た。
Example 4
(Production of magnesium oxide particles D using sodium acetate)
213 g of magnesium hydroxide obtained in the same manner as in Example 1 was resuspended in pure water to form an aqueous slurry of magnesium hydroxide, 21 g of sodium acetate was added to this aqueous slurry, and the mixture was stirred for 1 hour. The aqueous slurry was evaporated to dryness to obtain a uniform composition of sodium acetate and magnesium hydroxide. This was calcined at 1200 ° C. for 1 hour to obtain magnesium oxide particles D according to the present invention.
実施例５
（酢酸ナトリウムを用いる酸化マグネシウム粒子Ｅの製造）
実施例１と同様にして得られた水酸化マグネシウム２１３ｇを純水中に再懸濁して、水酸化マグネシウムの水性スラリーとし、この水性スラリー中に酢酸ナトリウム４２ｇ加え、１時間攪拌した後、これを蒸発乾固して、酢酸ナトリウムと水酸化マグネシウムとの均一な組成物を得た。これを１２００℃で１時間焼成して、本発明による酸化マグネシウム粒子Ｅを得た。
Example 5
(Production of magnesium oxide particles E using sodium acetate)
213 g of magnesium hydroxide obtained in the same manner as in Example 1 was resuspended in pure water to form an aqueous slurry of magnesium hydroxide, 42 g of sodium acetate was added to this aqueous slurry, and the mixture was stirred for 1 hour. Evaporation to dryness gave a homogeneous composition of sodium acetate and magnesium hydroxide. This was calcined at 1200 ° C. for 1 hour to obtain magnesium oxide particles E according to the present invention.
実施例６
（酢酸ナトリウムを用いる酸化マグネシウム粒子Ｆの製造）
純水０．３Ｌを張った沈殿反応器に４モル／Ｌ濃度の塩化マグネシウム水溶液１Ｌと１４．３モル／Ｌ濃度の水酸化ナトリウム水溶液０．５０３Ｌを同時に注入して、水酸化マグネシウムの沈殿を含むスラリーを得た。このスラリーを加熱し、１７０℃で１時間水熱処理した。この後、得られた反応混合物を濾過、水洗、乾燥した後、粉砕して、水酸化マグネシウム粉末を得た。この水酸化マグネシウムの平均一次粒子径は０．８μｍ、比表面積は７ｍ2／ｇであった。
Example 6
(Production of magnesium oxide particles F using sodium acetate)
1 L of 4 mol / L magnesium chloride aqueous solution and 0.503 L of 14.3 mol / L sodium hydroxide aqueous solution were simultaneously injected into a precipitation reactor filled with 0.3 L of pure water to precipitate magnesium hydroxide. A slurry containing was obtained. This slurry was heated and hydrothermally treated at 170 ° C. for 1 hour. Thereafter, the obtained reaction mixture was filtered, washed with water, dried and then pulverized to obtain a magnesium hydroxide powder. This magnesium hydroxide had an average primary particle size of 0.8 μm and a specific surface area of 7 m 2 / g.
次に、このようにして得られた水酸化マグネシウム２０３ｇを純水中に再懸濁して、水酸化マグネシウムの水性スラリーとし、この水性スラリー中に酢酸ナトリウム１０ｇ加え、１時間攪拌した後、これを蒸発乾固して、酢酸ナトリウムと水酸化マグネシウムとの均一な組成物を得た。この酢酸ナトリウムを含む水酸化マグネシウムを１２００℃で１時間焼成して、本発明による酸化マグネシウム粒子Ｆを得た。 Next, 203 g of the magnesium hydroxide thus obtained was resuspended in pure water to form an aqueous slurry of magnesium hydroxide, 10 g of sodium acetate was added to the aqueous slurry, and the mixture was stirred for 1 hour. Evaporation to dryness gave a homogeneous composition of sodium acetate and magnesium hydroxide. The magnesium hydroxide containing sodium acetate was fired at 1200 ° C. for 1 hour to obtain magnesium oxide particles F according to the present invention.
実施例７
（酢酸アンモニウムを用いる酸化マグネシウム粒子Ｇの製造）
実施例１と同様にして得られた水酸化マグネシウム２１３ｇを純水中に再懸濁して、水酸化マグネシウムの水性スラリーとし、この水性スラリーに酢酸アンモニウム２１ｇを加え、１時間攪拌した後、これを蒸発乾固して、酢酸アンモニウムと水酸化マグネシウムとの均一な混合物を得た。これを１２００℃で１時間焼成して、本発明による酸化マグネシウム粒子Ｆを得た。
Example 7
(Production of magnesium oxide particles G using ammonium acetate)
213 g of magnesium hydroxide obtained in the same manner as in Example 1 was resuspended in pure water to form an aqueous slurry of magnesium hydroxide, 21 g of ammonium acetate was added to the aqueous slurry, and the mixture was stirred for 1 hour. Evaporation to dryness gave a homogeneous mixture of ammonium acetate and magnesium hydroxide. This was fired at 1200 ° C. for 1 hour to obtain magnesium oxide particles F according to the present invention.
実施例８
（酢酸マグネシウムを用いる酸化マグネシウム粒子Ｈの製造）
純水０．３Ｌを張った沈殿反応器に２．３モル／Ｌ濃度の酢酸マグネシウム水溶液１．２Ｌと１８．１モル／Ｌ濃度の水酸化ナトリウム水溶液０．２９９Ｌを同時に注入して、水酸化マグネシウムの沈殿を含むスラリーを得た。このスラリーを濾過、水洗、乾燥した後、粉砕して、水酸化マグネシウムの粉末を得た。この水酸化マグネシウムの平均一次粒子径は０．１μｍ、比表面積は２８ｍ2／ｇであった。
Example 8
(Production of magnesium oxide particles H using magnesium acetate)
To a precipitation reactor filled with 0.3 L of pure water, 1.2 L of a magnesium acetate aqueous solution having a concentration of 2.3 mol / L and 0.299 L of a sodium hydroxide aqueous solution having a concentration of 18.1 mol / L were simultaneously injected. A slurry containing magnesium precipitate was obtained. The slurry was filtered, washed with water, dried and then pulverized to obtain a magnesium hydroxide powder. This magnesium hydroxide had an average primary particle size of 0.1 μm and a specific surface area of 28 m 2 / g.
次に、この水酸化マグネシウム１４６ｇを純水中に再懸濁して、水酸化マグネシウムの水性スラリーとし、これに酢酸マグネシウム２８．２ｇを加え、１時間攪拌した後、この水性スラリーを蒸発乾固して、酢酸マグネシウムと水酸化マグネシウムとの均一な組成物を得た。これを１２００℃で１時間焼成して、本発明による酸化マグネシウム粒子Ｈを得た。 Next, 146 g of this magnesium hydroxide is resuspended in pure water to make an aqueous slurry of magnesium hydroxide, to which 28.2 g of magnesium acetate is added and stirred for 1 hour, and then this aqueous slurry is evaporated to dryness. Thus, a uniform composition of magnesium acetate and magnesium hydroxide was obtained. This was calcined at 1200 ° C. for 1 hour to obtain magnesium oxide particles H according to the present invention.
実施例９
（酢酸ナトリウムを用いる酸化マグネシウム粒子Ｉの製造）
純水０．３Ｌを張った沈殿反応器に２．３モル／Ｌ濃度の酢酸マグネシウム水溶液１．２Ｌと１８．１モル／Ｌ濃度の水酸化ナトリウム水溶液０．２９９Ｌを同時に注入して、水酸化マグネシウムの沈殿と共に、副生塩である酢酸ナトリウムを溶解含有するスラリーを得、このスラリーを上記酢酸ナトリウムが残存するように洗浄した。即ち、水酸化マグネシウムと酢酸ナトリウムを含むスラリーを濾過、水洗した後、再度、水に懸濁させ、得られたスラリーの導電率を測定する操作を繰り返して、スラリーの導電率が７．５ｍＳ／ｃｍまで低下したときに水洗を止めて、スラリーを濾過し、乾燥して、酢酸ナトリウムと水酸化マグネシウムとの均一な組成物を得た。この組成物中の酢酸ナトリウムの割合は、酢酸基に換算して、水酸化マグネシウム１００モル部に対して、７．９モル部であった。
Example 9
(Production of magnesium oxide particles I using sodium acetate)
To a precipitation reactor filled with 0.3 L of pure water, 1.2 L of a magnesium acetate aqueous solution having a concentration of 2.3 mol / L and 0.299 L of a sodium hydroxide aqueous solution having a concentration of 18.1 mol / L were simultaneously injected. A slurry containing dissolved sodium acetate as a by-product salt was obtained together with precipitation of magnesium, and this slurry was washed so that the sodium acetate remained. That is, after the slurry containing magnesium hydroxide and sodium acetate was filtered and washed with water, the operation of measuring the conductivity of the obtained slurry was repeated again by suspending in water, and the conductivity of the slurry was 7.5 mS / When it was reduced to cm, the washing was stopped and the slurry was filtered and dried to obtain a uniform composition of sodium acetate and magnesium hydroxide. The ratio of sodium acetate in this composition was 7.9 mol parts with respect to 100 mol parts of magnesium hydroxide in terms of acetate groups.
この水酸化マグネシウムと酢酸ナトリウムの組成物の平均一次粒子径は０．１μｍ、比表面積は２８ｍ2／ｇであった。この組成物を１４５０℃で３時間焼成して、本発明による酸化マグネシウム粒子Ｉを得た。 The composition of magnesium hydroxide and sodium acetate had an average primary particle size of 0.1 μm and a specific surface area of 28 m 2 / g. This composition was calcined at 1450 ° C. for 3 hours to obtain magnesium oxide particles I according to the present invention.
比較例１
（酸化マグネシウム粒子Ｊの製造）
実施例１と同様にして得られた水酸化マグネシウムに酢酸ナトリウムを加えることなく、１２００℃で１時間焼成して、酸化マグネシウム粒子Ｊを得た。
Comparative Example 1
(Manufacture of magnesium oxide particles J)
Magnesium oxide particles J were obtained by calcination at 1200 ° C. for 1 hour without adding sodium acetate to the magnesium hydroxide obtained in the same manner as in Example 1.
比較例２
（酸化マグネシウム粒子Ｋの製造）
実施例６と同様にして得られた水酸化マグネシウムに酢酸ナトリウムを加えることなく、１２００℃で１時間焼成して、酸化マグネシウム粒子Ｋを得た。
Comparative Example 2
(Manufacture of magnesium oxide particles K)
Magnesium oxide particles K were obtained by calcination at 1200 ° C. for 1 hour without adding sodium acetate to magnesium hydroxide obtained in the same manner as in Example 6.
比較例３
（酸化マグネシウム粒子Ｌの製造）
実施例６と同様にして得られた水酸化マグネシウムに酢酸ナトリウムを加えることなく、１４５０℃で３時間焼成して、酸化マグネシウム粒子Ｌを得た。
Comparative Example 3
(Manufacture of magnesium oxide particles L)
Magnesium oxide particles L were obtained by calcination at 1450 ° C. for 3 hours without adding sodium acetate to the magnesium hydroxide obtained in the same manner as in Example 6.
比較例４
（酸化マグネシウム粒子Ｍの製造）
実施例１と同様にして得られた水酸化マグネシウム２１３ｇを水に再懸濁させて、水酸化マグネシウムの水性スラリーを得、この水性スラリーに酢酸ナトリウム６．３ｇを加え、１時間攪拌した。この水性スラリーを蒸発乾固して、酢酸ナトリウムと水酸化マグネシウムとの均一な組成物を得た。これを１２００℃で１時間焼成して、酸化マグネシウム粒子Ｍを得た。
Comparative Example 4
(Manufacture of magnesium oxide particles M)
213 g of magnesium hydroxide obtained in the same manner as in Example 1 was resuspended in water to obtain an aqueous slurry of magnesium hydroxide. To this aqueous slurry was added 6.3 g of sodium acetate, and the mixture was stirred for 1 hour. This aqueous slurry was evaporated to dryness to obtain a uniform composition of sodium acetate and magnesium hydroxide. This was fired at 1200 ° C. for 1 hour to obtain magnesium oxide particles M.
比較例５
（酸化マグネシウム粒子Ｎの製造）
実施例１と同様にして得られた酢酸ナトリウムを含む水酸化マグネシウムを９００℃で１時間焼成して、本発明による酸化マグネシウム粒子Ｎを得た。
Comparative Example 5
(Manufacture of magnesium oxide particles N)
Magnesium hydroxide containing sodium acetate obtained in the same manner as in Example 1 was calcined at 900 ° C. for 1 hour to obtain magnesium oxide particles N according to the present invention.
表１に結果を示すように、本発明によれば、一次粒子が球状である酸化マグネシウム粒子を容易に得ることができる。しかし、水酸化マグネシウムに酢酸塩を含有させることなく、これを焼成しても、また、水酸化マグネシウムに酢酸塩を含有させた場合であっても、水酸化マグネシウムに対する酢酸塩の割合が少ないときは、一次粒子が球状である酸化マグネシウムを得ることができなかった。 As shown in Table 1, according to the present invention, magnesium oxide particles whose primary particles are spherical can be easily obtained. However, even if the magnesium hydroxide is baked without containing the acetate or the magnesium hydroxide contains the acetate, the ratio of the acetate to the magnesium hydroxide is small. Could not obtain magnesium oxide having primary spherical particles.
Claims (4)
Magnesium oxide particles in which the primary particles obtained by the method according to claim 1 are spherical.
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| KR20110036475A (en) * | 2009-10-01 | 2011-04-07 | 장학정 | Method of manufacturing a magnesium oxide nanoparticle and magnesium oxide nanoparticle using the same |
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