JP2002255544A - Highly pure, highly oriented magnesium hydroxide powder and method for producing the same - Google Patents

Highly pure, highly oriented magnesium hydroxide powder and method for producing the same

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Publication number
JP2002255544A
JP2002255544A JP2001048415A JP2001048415A JP2002255544A JP 2002255544 A JP2002255544 A JP 2002255544A JP 2001048415 A JP2001048415 A JP 2001048415A JP 2001048415 A JP2001048415 A JP 2001048415A JP 2002255544 A JP2002255544 A JP 2002255544A
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JP
Japan
Prior art keywords
mass
less
terms
compound
magnesium hydroxide
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Application number
JP2001048415A
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Japanese (ja)
Other versions
JP3965279B2 (en
Inventor
Hiroshi Arita
洋 在田
Toyotaka Uchida
豊隆 内田
Yojiro Ichimura
洋二郎 市村
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Ube Material Industries Ltd
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Ube Material Industries Ltd
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Publication of JP3965279B2 publication Critical patent/JP3965279B2/en
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Abstract

PROBLEM TO BE SOLVED: To obtain a highly pure and highly oriented magnesium hydroxide powder industrially producible, and preferably usable as a magnesium oxide raw material for an electronic material (especially for a thin film electronic material). SOLUTION: The highly pure and highly oriented magnesium hydroxide powder comprises (by mass) <=0.01% of a calcium compound in terms of calcium atom, <=0.02% of a silicon compound in terms of silicon atom, <=0.015% of an iron compound in terms of iron atom, <=0.015% of an aluminum compound in terms of aluminum atom, and <=0.005% of a zirconium compound in terms of zirconium atom, wherein the content of magnesium hydroxide is >=99.5%, and the main part of the particles forms a plate-like primary particle.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、不純物(特に、カ
ルシウム化合物、珪素化合物、鉄化合物、アルミニウム
化合物、そしてジルコニウム化合物)の含有量の少ない
高純度高配向性水酸化マグネシウム粉末、及びその製造
方法に関する。また、本発明は、高純度酸化マグネシウ
ム粉末にも関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a high-purity and high-orientation magnesium hydroxide powder having a low content of impurities (particularly calcium compounds, silicon compounds, iron compounds, aluminum compounds and zirconium compounds), and a method for producing the same. About. The present invention also relates to a high-purity magnesium oxide powder.

【0002】[0002]

【従来の技術】水酸化マグネシウム粉末は、例えば、合
成樹脂用の充填材として利用されている。また、最近で
は、水酸化マグネシウム粉末を電子材料用の酸化マグネ
シウム原料として利用することが検討されている。例え
ば、近年開発が進められている酸化マグネシウムを有効
成分として含む誘電体セラミック組成物(特開2000
−103668号公報参照)の酸化マグネシウム原料と
して水酸化マグネシウム粉末を利用することが検討され
ている。
2. Description of the Related Art Magnesium hydroxide powder is used, for example, as a filler for synthetic resins. Recently, it has been studied to use magnesium hydroxide powder as a raw material of magnesium oxide for electronic materials. For example, a dielectric ceramic composition containing magnesium oxide as an active ingredient, which is being developed in recent years, is disclosed in
Utilization of a magnesium hydroxide powder as a raw material of magnesium oxide has been studied.

【0003】誘電体セラミック組成物などの電子材料用
の酸化マグネシウム原料として使用する水酸化マグネシ
ウム粉末は不純物含有量が少ない、すなわち高純度であ
ること、及び分散性が高いことが望まれる。特に、薄膜
状電子材料(例;積層セラミックコンデンサの誘電体セ
ラミック組成物層)用の酸化マグネシウム原料として使
用する水酸化マグネシウム粉末では、より高度な分散性
が要求される。
It is desired that magnesium hydroxide powder used as a raw material of magnesium oxide for electronic materials such as a dielectric ceramic composition has a small impurity content, that is, high purity and high dispersibility. Particularly, magnesium hydroxide powder used as a magnesium oxide raw material for a thin film electronic material (eg, a dielectric ceramic composition layer of a multilayer ceramic capacitor) requires higher dispersibility.

【0004】本出願人は、気相合成法により製造された
酸化マグネシウム粉末を水和させて得た一次粒子の微細
な水酸化マグネシウム粉末が高純度、高分散性を示すこ
とを見出し、この知見に基づいて特許出願している(特
願2000−117433号)。上記の水酸化マグネシ
ウム粉末は、電子材料(特に薄膜状電子材料)用の酸化
マグネシウム原料として好適に使用できる。しかしなが
ら、製造原料である酸化マグネシウム粉末は、その製造
に特別な装置を必要とし工業的な生産コストが高いた
め、上記の水酸化マグネシウム粉末はコスト的に高価で
ある。
[0004] The present applicant has found that magnesium hydroxide powder having fine primary particles obtained by hydrating magnesium oxide powder produced by a gas phase synthesis method exhibits high purity and high dispersibility. (Japanese Patent Application No. 2000-117433). The above magnesium hydroxide powder can be suitably used as a magnesium oxide raw material for electronic materials (particularly, thin film electronic materials). However, magnesium oxide powder, which is a raw material for production, requires special equipment for its production and has a high industrial production cost. Therefore, the above magnesium hydroxide powder is expensive in terms of cost.

【0005】従来より、一次粒子が均一によく発達した
水酸化マグネシウム粉末もまた、高い分散性を示すこと
が知られている。このような水酸化マグネシウム粉末を
得る方法として、酸化マグネシウム焼成物を各種イオン
性物質の存在下で水和させる方法が知られている。
[0005] Conventionally, it has been known that magnesium hydroxide powder in which primary particles are uniformly and well developed also exhibits high dispersibility. As a method of obtaining such a magnesium hydroxide powder, a method of hydrating a calcined product of magnesium oxide in the presence of various ionic substances is known.

【0006】特開昭56−109820号公報には、1
400℃以上の温度で焼成された酸化マグネシウム焼成
物を、好ましくは250μm以下、さらに好ましくは1
00μm以下に粉砕し、酸化マグネシウム原料中の酸化
カルシウムの当量数を超える量に相当する酸基の量の酸
あるいはそのマグネシウム塩存在下で水和させることに
より、水酸化マグネシウム粉末を製造する方法が開示さ
れている。上記公報に開示された方法によれば、一次粒
子が均一によく発達し、平均粒子径が1μm以下であっ
て、粒度分布の比較的狭い、水酸化マグネシウム粉末を
得ることができるとされている。このような水酸化マグ
ネシウム粉末は、一次粒子同士が二次凝集を起こさず、
分散性に優れているとされている。
JP-A-56-109820 discloses that 1
The calcined magnesium oxide calcined at a temperature of 400 ° C. or more is preferably 250 μm or less, more preferably 1 μm or less.
A method for producing a magnesium hydroxide powder by pulverizing to less than 00 μm and hydrating in the presence of an acid having an amount of an acid group corresponding to an amount exceeding the equivalent number of calcium oxide in the magnesium oxide raw material or its magnesium salt. It has been disclosed. According to the method disclosed in the above publication, primary particles are uniformly and well developed, an average particle diameter is 1 μm or less, and a magnesium hydroxide powder having a relatively narrow particle size distribution can be obtained. . Such magnesium hydroxide powder, primary particles do not cause secondary aggregation,
It is said to have excellent dispersibility.

【0007】上記の方法で得られる水酸化マグネシウム
粉末の不純物量は、上記公報の実施例によれば、酸化カ
ルシウム(CaO)含有量が0.02質量%(カルシウ
ム原子換算量で0.014質量%に相当)、酸化珪素
(Si2O)含有量が0.22質量%(珪素原子換算量
で0.10質量%に相当)、酸化鉄(Fe23)含有量
が0.04質量%(鉄原子換算量で0.028質量%に
相当)、酸化アルミニウム(Al23)含有量が0.0
4質量%(アルミニウム原子換算量で0.021質量%
に相当)である(実施例1を参照)。
According to the examples in the above publication, the content of calcium oxide (CaO) in the magnesium hydroxide powder obtained by the above method is 0.02% by mass (0.014% by mass in terms of calcium atoms). %), A silicon oxide (Si 2 O) content of 0.22 mass% (corresponding to 0.10 mass% in terms of silicon atoms), and an iron oxide (Fe 2 O 3 ) content of 0.04 mass. % (Corresponding to 0.028 mass% in terms of iron atoms), and the content of aluminum oxide (Al 2 O 3 ) is 0.0
4% by mass (0.021% by mass in terms of aluminum atom)
(See Example 1).

【0008】また、本出願人は、1150〜1350℃
の温度で焼成して得られた酸化マグネシウム焼成物を粉
砕して、(200)方向の結晶子径が800〜1500
オングストローム、BET比表面積が0.7〜2m2
g、平均粒子径が2〜5μmの酸化マグネシウム粉末を
得て、これをマグネシウム塩存在下で水和させることに
より、生成する水酸化マグネシウム粉末の優れた特性を
損なうことなく、酸化マグネシウム焼成物の水和反応に
要する時間を短縮できることを見出し、この知見に基づ
いて特許出願した(特開平1−131022号公報参
照)。この公報に開示された方法によれば、一次粒子が
均一によく発達し、二次凝集体を形成していない高分散
性水酸化マグネシウム粉末を工業的規模で経済的に効率
よく製造することができる。
[0008] Further, the applicant of the present invention has a temperature of 1150-1350 ° C.
The calcined product of magnesium oxide obtained by calcining at a temperature of is pulverized and the crystallite diameter in the (200) direction is 800 to 1500.
Angstrom, BET specific surface area 0.7-2 m 2 /
g, a magnesium oxide powder having an average particle diameter of 2 to 5 μm is obtained, and hydrated in the presence of a magnesium salt, without impairing the excellent properties of the magnesium hydroxide powder to be produced. They found that the time required for the hydration reaction could be shortened, and applied for a patent based on this finding (see Japanese Patent Application Laid-Open No. 1-131022). According to the method disclosed in this publication, primary particles are uniformly and well developed, and a highly dispersible magnesium hydroxide powder that does not form secondary aggregates can be economically and efficiently produced on an industrial scale. it can.

【0009】[0009]

【発明が解決しようとする課題】一次粒子が発達した水
酸化マグネシウム粉末は、工業的に比較的安価に製造す
ることができる。しかしながら、本発明者の研究によれ
ば、上記の水酸化マグネシウム粉末には、製造原料の酸
化マグネシウム焼成物に含まれている不純物(カルシウ
ム化合物、珪素化合物、鉄化合物、アルミニウム化合
物)や、酸化マグネシウム焼成物を粉砕する際に粉砕装
置から侵入する鉄、アルミニウム、又はジルコニウムか
ら生じる不純物(鉄化合物、アルミニウム化合物、ジル
コニウム化合物)が混入する傾向にあり、この不純物が
電子材料用の酸化マグネシウム原料として用いる場合に
は問題となるおそれがあることが判明した。
SUMMARY OF THE INVENTION Magnesium hydroxide powder having developed primary particles can be produced industrially at relatively low cost. However, according to the study of the present inventor, the magnesium hydroxide powder contains impurities (calcium compound, silicon compound, iron compound, aluminum compound) contained in the baked product of magnesium oxide and magnesium oxide. There is a tendency that impurities (iron compounds, aluminum compounds, zirconium compounds) generated from iron, aluminum, or zirconium entering from a pulverizer when pulverizing the fired product tend to be mixed, and these impurities are used as a raw material of magnesium oxide for electronic materials. It turned out that in some cases this could be a problem.

【0010】また、上記の水酸化マグネシウム粉末を薄
膜状電子材料用の酸化マグネシウム原料として使用する
場合には、該電子材料中に水酸化マグネシウムの一次粒
子が均一に分散するように、水酸化マグネシウム粉末の
粒子のほとんど(主要部)が板状の一次粒子であるこ
と、すなわち配向性が高いことも要求される。しかしな
がら、本発明者の研究によれば、上記の水酸化マグネシ
ウム粉末は、薄膜状電子材料用の酸化マグネシウム原料
として使用するには配向性がやや低い傾向にあることも
判明した。
When the above-mentioned magnesium hydroxide powder is used as a raw material of magnesium oxide for a thin-film electronic material, magnesium hydroxide is so dispersed that the primary particles of magnesium hydroxide are uniformly dispersed in the electronic material. It is also required that most (main part) of the powder particles be plate-like primary particles, that is, have high orientation. However, according to the study of the present inventor, it has also been found that the above-mentioned magnesium hydroxide powder tends to have a slightly lower orientation when used as a magnesium oxide raw material for a thin-film electronic material.

【0011】従って、本発明の目的は、工業的に安価に
製造でき、かつ電子材料(特に薄膜状電子材料)用の酸
化マグネシウム原料として好適に使用できる高純度高配
向性水酸化マグネシウム粉末を提供することにある。本
発明はまた、特に電子材料の添加剤として有利に使用で
きる高純度酸化マグネシウム粉末を提供することもその
目的とする。本発明はさらに、高純度高配向性水酸化マ
グネシウム粉末を工業的に効率よく製造する方法を提供
することもその目的とする。
Accordingly, an object of the present invention is to provide a high-purity and highly-oriented magnesium hydroxide powder which can be industrially manufactured at low cost and can be suitably used as a raw material of magnesium oxide for electronic materials (especially thin-film electronic materials). Is to do. Another object of the present invention is to provide a high-purity magnesium oxide powder which can be advantageously used particularly as an additive for electronic materials. Another object of the present invention is to provide a method for industrially and efficiently producing a high-purity and high-orientation magnesium hydroxide powder.

【0012】[0012]

【課題を解決するための手段】本発明者は、上記目的を
達成すべく鋭意研究を重ねた結果、特定の無機化合物の
含有量が調整された酸化マグネシウム焼成物を、水溶性
マグネシウム塩の存在下、特定の条件下にて水和させる
ことにより、上記の不純物(カルシウム化合物、珪素化
合物、鉄化合物、アルミニウム化合物、そしてジルコニ
ウム化合物)の含有量の少ない高純度高配向性水酸化マ
グネシウム粉末を得ることができることを見出した。
Means for Solving the Problems As a result of intensive studies to achieve the above object, the present inventor has found that a magnesium oxide calcined product in which the content of a specific inorganic compound has been adjusted is reduced to the presence of a water-soluble magnesium salt. By hydrating under specific conditions, a high-purity high-orientation magnesium hydroxide powder having a low content of the above impurities (calcium compound, silicon compound, iron compound, aluminum compound, and zirconium compound) is obtained. I found that I can do it.

【0013】本発明は、カルシウム化合物、珪素化合
物、鉄化合物、アルミニウム化合物、そしてジルコニウ
ム化合物の含有量が、それぞれカルシウム原子換算量で
0.01質量%以下、珪素原子換算量で0.02質量%
以下、鉄原子換算量で0.015質量%以下、アルミニ
ウム原子換算量で0.015質量%以下、及びジルコニ
ウム原子換算量で0.005質量%以下であり、水酸化
マグネシウム含有量が99.5質量%以上であって、粒
子の主要部が板状の一次粒子をなすことを特徴とする高
純度高配向性水酸化マグネシウム粉末にある。
According to the present invention, the content of a calcium compound, a silicon compound, an iron compound, an aluminum compound, and a zirconium compound is 0.01% by mass or less in terms of calcium atom, and 0.02% by mass in terms of silicon atom.
Hereinafter, the content is 0.015% by mass or less in terms of iron atoms, 0.015% by mass or less in terms of aluminum atoms, and 0.005% by mass or less in terms of zirconium atoms, and the content of magnesium hydroxide is 99.5. % By mass or more, and the main part of the particles is plate-like primary particles, and is a high-purity and high-orientation magnesium hydroxide powder.

【0014】本発明の高純度高分散性水酸化マグネシウ
ム粉末の好ましい態様を、下記に示す。
Preferred embodiments of the high-purity and high-dispersion magnesium hydroxide powder of the present invention are shown below.

【0015】(1)カルシウム化合物、珪素化合物、鉄
化合物、アルミニウム化合物、そしてジルコニウム化合
物の含有量が、それぞれカルシウム原子換算量で0.0
07質量%以下、珪素原子換算量で0.015質量%以
下、鉄原子換算量で0.01質量%以下、アルミニウム
原子換算量で0.01質量%以下、及びジルコニウム原
子換算量で0.001質量%以下である。
(1) The contents of calcium compound, silicon compound, iron compound, aluminum compound and zirconium compound are each 0.00 in terms of calcium atom.
07% by mass or less, 0.015% by mass or less in terms of silicon atoms, 0.01% by mass or less in terms of iron atoms, 0.01% by mass or less in terms of aluminum atoms, and 0.001 in terms of zirconium atoms. % By mass or less.

【0016】(2)水酸化マグネシウム含有量が99.
7質量%以上、より好ましくは99.8質量%以上であ
る。
(2) The content of magnesium hydroxide is 99.
It is at least 7% by mass, more preferably at least 99.8% by mass.

【0017】(3)ナトリウム化合物の含有量がナトリ
ウム原子換算量で0.003質量%以下、より好ましく
0.002質量%以下であり、かつカリウム化合物の含
有量がカリウム原子換算量で0.002質量%以下、よ
り好ましく0.001質量%以下である。
(3) The content of the sodium compound is 0.003% by mass or less, preferably 0.002% by mass or less, in terms of sodium atom, and the content of the potassium compound is 0.002% by mass in terms of potassium atom. % By mass, more preferably 0.001% by mass or less.

【0018】(4)フッ化物、塩化物及び臭化物の含有
量がそれぞれフッ素、塩素及び臭素の原子換算量で0.
005質量%以下、より好ましくは0.003質量%以
下である。
(4) The content of fluoride, chloride and bromide is 0.1 in terms of atom of fluorine, chlorine and bromine respectively.
005 mass% or less, more preferably 0.003 mass% or less.

【0019】(5)ホウ素化合物の含有量がホウ素原子
換算量で0.01質量%以下、より好ましくは0.00
5質量%以下であり、硫黄化合物の含有量が硫黄原子換
算量で0.005質量%以下、より好ましくは0.00
2質量%である。
(5) The content of the boron compound is 0.01% by mass or less, more preferably 0.00% by mass in terms of boron atom.
5% by mass or less, and the content of the sulfur compound is 0.005% by mass or less, more preferably 0.005% by mass, in terms of sulfur atom.
2% by mass.

【0020】(6)クロム化合物の含有量がクロム原子
換算量で0.001質量%以下であり、ニッケル化合物
の含有量がニッケル原子換算量で0.005質量%以下
であり、マンガン化合物の含有量がマンガン原子換算量
で0.002質量%以下であり、銅化合物の含有量が銅
原子換算量で0.001質量%以下であり、亜鉛化合物
の含有量が亜鉛原子換算量で0.001質量%以下であ
り、鉛化合物の含有量が鉛原子換算量で0.001質量
%以下であり、砒素化合物の含有量が砒素原子換算量で
0.0001質量%以下である。
(6) The content of the chromium compound is 0.001% by mass or less in terms of chromium atoms, the content of the nickel compound is 0.005% by mass or less in terms of nickel atoms, and the content of the manganese compound is The amount is 0.002% by mass or less in terms of manganese atom, the content of the copper compound is 0.001% by mass or less in terms of copper atom, and the content of the zinc compound is 0.001% or less in terms of zinc atom. % By mass, the content of lead compound is 0.001% by mass or less in terms of lead atom, and the content of arsenic compound is 0.0001% by mass or less in terms of arsenic atom.

【0021】(7)配向度が30%以上、より好ましく
は60%以上である。この配向度は、水酸化マグネシウ
ム粉末としての配向性を示す指標である。すなわち、配
向度が高いほど水酸化マグネシウム粉末中の板状一次粒
子の割合が高いことを示す。
(7) The degree of orientation is 30% or more, more preferably 60% or more. This degree of orientation is an index indicating the orientation as the magnesium hydroxide powder. That is, the higher the degree of orientation, the higher the ratio of the plate-like primary particles in the magnesium hydroxide powder.

【0022】上記の配向度は、水酸化マグネシウム粉末
を一軸成形機によりペレット状に成形し、この平坦面
(プレス面)のX線回折パターンから、水酸化マグネシ
ウムの(001)(101)(102)(110)(1
11)(103)の各面に相当するX線回折ピークの積
分強度を求め、下記式(1)により算出した値である。
なお、下記式(1)は、特公昭56−35004号に記
載されている配向性フェライト焼結体の配向度の計算式
に準じた式である。
The degree of orientation is determined by molding the magnesium hydroxide powder into pellets using a uniaxial molding machine, and examining the (001) (101) (102) of magnesium hydroxide from the X-ray diffraction pattern of the flat surface (pressed surface). ) (110) (1)
11) The value obtained by calculating the integrated intensity of the X-ray diffraction peak corresponding to each surface of (103) and calculating by the following equation (1).
The following formula (1) is a formula based on the formula for calculating the degree of orientation of the oriented ferrite sintered body described in Japanese Patent Publication No. 56-35004.

【0023】式(1): 配向度(%)={S(I001)/S(ΣIhkl)−R(I
001)/R(ΣIhkl)}/{1−R(I001)/R(Σ
hkl)}×100 ここで、S、Rはそれぞれ測定対象の試料及び標準試薬
の因子であることを示し、(I001)は面指数(00
1)面のX線回折ピークの積分強度を示し、(Σ
hkl)は面指数(001)(101)(102)(1
10)(111)(103)の各面のX線回折ピークの
積分強度の和を示す。
Equation (1): Degree of orientation (%) = {S (I 001 ) / S (ΣI hkl ) -R (I
001 ) / R ({I hkl )} / {1-R (I 001 ) / R (Σ
I hkl )} × 100 where S and R indicate factors of a sample to be measured and a standard reagent, respectively, and (I 001 ) is a plane index (00)
1) indicates the integrated intensity of the X-ray diffraction peak of the plane,
I hkl ) is the plane index (001) (101) (102) (1
10) shows the sum of the integrated intensities of the X-ray diffraction peaks of each surface of (111) and (103).

【0024】本発明はまた、上記の高純度配向性水酸化
マグネシウム粉末を350℃以上の温度で焼成して得ら
れる高純度酸化マグネシウム粉末にもある。
The present invention also provides a high-purity magnesium oxide powder obtained by firing the above-mentioned high-purity oriented magnesium hydroxide powder at a temperature of 350 ° C. or more.

【0025】本発明はさらに、カルシウム化合物、珪素
化合物、鉄化合物、アルミニウム化合物、そしてジルコ
ニウム化合物の含有量が、それぞれカルシウム原子換算
量で2質量%以下、珪素原子換算量で2質量%以下、鉄
原子換算量で0.15質量%以下、アルミニウム原子換
算量で0.15質量%以下、及びジルコニウム原子換算
量で0.05質量%以下であって、酸化マグネシウム含
有量が95質量%以上である酸化マグネシウム焼成物
を、水溶性マグネシウム塩の存在下、100〜250℃
の温度、1〜30気圧の水蒸気圧に調整されたオートク
レーブ中にて水和させることを特徴とする高純度高配向
性水酸化マグネシウム粉末の製造方法にもある。
The present invention further provides that the content of calcium compound, silicon compound, iron compound, aluminum compound and zirconium compound is 2% by mass or less in terms of calcium atom, 2% by mass or less in terms of silicon atom, respectively. It is 0.15% by mass or less in terms of atom, 0.15% by mass or less in terms of aluminum atom, and 0.05% by mass or less in terms of zirconium atom, and the magnesium oxide content is 95% by mass or more. The calcined product of magnesium oxide is heated at 100 to 250 ° C. in the presence of a water-soluble magnesium salt.
Hydration in an autoclave adjusted to a temperature of 1 to 30 atm and a steam pressure of 1 to 30 atm.

【0026】[0026]

【発明の実施の形態】本発明の高純度高配向性水酸化マ
グネシウム粉末は、特定の無機化合物の含有量が調整さ
れた酸化マグネシウム焼成物を、水溶性マグネシウム塩
の存在下、100〜250℃の温度、1〜30気圧の水
蒸気圧に調整されたオートクレーブ中にて水和させるこ
とにより製造することができる。
BEST MODE FOR CARRYING OUT THE INVENTION The high-purity and high-orientation magnesium hydroxide powder of the present invention is prepared by heating a calcined magnesium oxide having a specific inorganic compound content adjusted to 100 to 250 ° C. in the presence of a water-soluble magnesium salt. At a steam pressure of 1 to 30 atm.

【0027】本発明の高純度高配向性水酸化マグネシウ
ム粉末の製造に使用する酸化マグネシウム焼成物は、カ
ルシウム化合物、珪素化合物、鉄化合物、アルミニウム
化合物、そしてジルコニウム化合物の含有量が、それぞ
れカルシウム原子換算量で2質量%以下、珪素原子換算
量で2質量%以下、鉄原子換算量で0.15質量%以
下、アルミニウム原子換算量で0.15質量%以下、及
びジルコニウム原子換算量で0.05質量%以下であっ
て、酸化マグネシウム含有量が95質量%以上であるこ
とが必要である。カルシウム化合物、珪素化合物、鉄化
合物、アルミニウム化合物、そしてジルコニウム化合物
の含有量が上記数値を超えると、目的とする高純度高配
向性水酸化マグネシウム粉末を得るのが困難になる。
The calcined product of magnesium oxide used for producing the high-purity highly-oriented magnesium hydroxide powder of the present invention has a calcium compound, a silicon compound, an iron compound, an aluminum compound, and a zirconium compound, each having a calcium atom equivalent. 2% by mass or less, 2% by mass or less in terms of silicon atoms, 0.15% by mass or less in terms of iron atoms, 0.15% by mass or less in terms of aluminum atoms, and 0.05 in terms of zirconium atoms. Mass% or less, and the magnesium oxide content needs to be 95 mass% or more. When the contents of the calcium compound, the silicon compound, the iron compound, the aluminum compound, and the zirconium compound exceed the above-mentioned values, it becomes difficult to obtain the desired high-purity and high-orientation magnesium hydroxide powder.

【0028】上記酸化マグネシウム焼成物のカルシウム
化合物含有量は、カルシウム原子換算量で1質量%以下
であることが好ましく、0.5質量%以下であることが
より好ましい。上記酸化マグネシウム焼成物の珪素化合
物含有量は珪素原子換算量で1質量%以下であることが
好ましく、0.5質量%以下であることがより好まし
い。また、上記酸化マグネシウム焼成物のカルシウム化
合物及び珪素化合物の含有量はそれぞれ、カルシウム原
子換算量と珪素原子換算量との重量比(珪素原子量/カ
ルシウム原子量)が1以下となる量であることが好まし
く、0.5以下であることがより好ましい。上記重量比
が1よりも大きくなると、水和反応時に難溶性のカルシ
ウム珪酸塩が生成する傾向があり、これが水酸化マグネ
シウム粉末に混入して不純物含有量が高くなることがあ
る。
The calcium compound content of the calcined magnesium oxide product is preferably 1% by mass or less, more preferably 0.5% by mass or less in terms of calcium atoms. The silicon compound content of the magnesium oxide fired product is preferably 1% by mass or less, more preferably 0.5% by mass or less in terms of silicon atoms. In addition, the content of the calcium compound and the silicon compound in the calcined product of magnesium oxide is preferably such that the weight ratio of the converted amount of calcium atom to the converted amount of silicon atom (silicon atomic weight / calcium atomic weight) is 1 or less. , 0.5 or less. When the weight ratio is larger than 1, a poorly soluble calcium silicate tends to be generated during the hydration reaction, and this may be mixed into the magnesium hydroxide powder to increase the impurity content.

【0029】上記酸化マグネシウム焼成物の鉄化合物含
有量は鉄原子換算量で0.1質量%以下であることが好
ましく、0.05質量%以下であることがより好まし
い。上記酸化マグネシウム焼成物のアルミニウム化合物
含有量はアルミニウム原子換算量で0.1質量%以下で
あることが好ましく、0.05質量%以下であることが
より好ましい。上記酸化マグネシウム焼成物のジルコニ
ウム化合物含有量はジルコニウム原子換算量で0.01
質量%以下であることが好ましく、0.005質量%以
下であることがより好ましい。上記酸化マグネシウム焼
成物の酸化マグネシウム含有量は98質量%以上である
ことが好ましく、99質量%以上であることがより好ま
しい。
The iron compound content of the calcined product of magnesium oxide is preferably not more than 0.1% by mass, more preferably not more than 0.05% by mass in terms of iron atom. The aluminum compound content of the calcined magnesium oxide product is preferably 0.1% by mass or less, more preferably 0.05% by mass or less in terms of aluminum atoms. The zirconium compound content of the magnesium oxide fired product is 0.01 in terms of zirconium atoms.
It is preferably at most 0.005% by mass, more preferably at most 0.005% by mass. The magnesium oxide content of the fired magnesium oxide product is preferably 98% by mass or more, and more preferably 99% by mass or more.

【0030】上記酸化マグネシウム焼成物はさらに、沸
点1150℃以下の無機化合物の含有量がそれぞれ、ナ
トリウム原子換算量で0.02質量%以下、カリウム原
子換算量で0.01質量%以下、フッ素、塩素及び臭素
の原子換算量で0.03質量%以下、ホウ素原子換算量
で0.1質量%以下、そして硫黄原子換算量で0.02
質量%以下であることが好ましく、ナトリウム原子換算
量で0.01質量%以下、カリウム原子換算量で0.0
05質量%以下、フッ素、塩素及び臭素の原子換算量で
0.01質量%以下、ホウ素原子換算量で0.05質量
%以下、そして硫黄原子換算量で0.01質量%以下で
あることがより好ましい。
The fired product of magnesium oxide further contains an inorganic compound having a boiling point of 1150 ° C. or lower in an amount of 0.02% by mass or less in terms of sodium atom, 0.01% by mass or less in terms of potassium atom, and fluorine, 0.03% by mass or less in terms of chlorine and bromine, 0.1% by mass or less in terms of boron, and 0.02% in terms of sulfur.
% By mass, preferably 0.01% by mass or less in terms of sodium atom, and 0.0% by mass in terms of potassium atom.
Not more than 0.05% by mass, not more than 0.01% by mass in terms of atoms of fluorine, chlorine and bromine, not more than 0.05% by mass in terms of boron atoms, and not more than 0.01% by mass in terms of sulfur atoms. More preferred.

【0031】上記酸化マグネシウム焼成物の大きさに特
に制限はないが、通常は粒径が20mm以下、好ましく
は5mm以下、より好ましくは0.3〜5mmの範囲、
特に好ましくは1〜3mmの範囲の粒状物である。この
酸化マグネシウム焼成物は、水酸化マグネシウムを11
50〜2000℃の温度で焼成して製造された酸化マグ
ネシウムクリンカを粗砕することによって製造されるこ
とが好ましい。上記酸化マグネシウムクリンカの代わり
に電融マグネシアを用いてもよい。上記の粗砕には、公
知の粗砕装置を使用することができ、例えば、ジョーク
ラッシャを使用することができる。
The size of the magnesium oxide fired product is not particularly limited, but is usually 20 mm or less, preferably 5 mm or less, more preferably 0.3 to 5 mm.
Particularly preferred is a granular material in the range of 1 to 3 mm. This magnesium oxide calcined product contains 11% magnesium hydroxide.
It is preferably manufactured by crushing magnesium oxide clinker manufactured by firing at a temperature of 50 to 2000 ° C. Electrofused magnesia may be used instead of the magnesium oxide clinker. For the crushing, a known crushing device can be used, for example, a jaw crusher can be used.

【0032】高純度高分散性水酸化マグネシウム粉末
は、上記酸化マグネシウム焼成物を水溶性マグネシウム
塩の存在下、100〜250℃の温度、1〜30気圧の
水蒸気圧に調整されたオートクレーブ中にて水和させる
ことによって製造することができる。
The high-purity and high-dispersion magnesium hydroxide powder is prepared by heating the calcined magnesium oxide in the presence of a water-soluble magnesium salt in an autoclave adjusted to a temperature of 100 to 250 ° C. and a steam pressure of 1 to 30 atm. It can be produced by hydration.

【0033】上記水和反応において、製造原料である酸
化マグネシウム焼成物濃度は、水和反応溶液に対して2
0〜300g/リットルの範囲にあることが好ましい。
In the above-mentioned hydration reaction, the concentration of the calcined magnesium oxide as a raw material for production is 2 to the hydration reaction solution.
It is preferably in the range of 0 to 300 g / liter.

【0034】上記水溶性マグネシウム塩は、酢酸マグネ
シウム、ギ酸マグネシウム及びクエン酸マグネシウムな
どの有機マグネシウム塩を挙げることができるが、酢酸
マグネシウムであることが特に好ましい。水和反応液中
の上記マグネシウム塩の濃度は、0.02〜0.5モル
/リットルの範囲内にあることが好ましく、特に0.1
〜0.4モル/リットルの範囲内であることが好まし
い。上記水溶性マグネシウム塩の代わりに、マグネシウ
ムとともに上記マグネシウム塩を形成する酸、例えば、
酢酸、ギ酸及びクエン酸などの有機酸を用いてもよい。
Examples of the water-soluble magnesium salt include organic magnesium salts such as magnesium acetate, magnesium formate and magnesium citrate, and magnesium acetate is particularly preferred. The concentration of the magnesium salt in the hydration reaction solution is preferably in the range of 0.02 to 0.5 mol / L, and particularly preferably 0.1 to 0.5 mol / L.
It is preferably in the range of 0.40.4 mol / liter. Instead of the water-soluble magnesium salt, an acid that forms the magnesium salt with magnesium, for example,
Organic acids such as acetic acid, formic acid and citric acid may be used.

【0035】上記の水和反応を100〜250℃の温
度、1〜30気圧の水蒸気圧(好ましくは120〜20
0℃の温度、2〜15気圧の水蒸気圧)に調整されたオ
ートクレーブ中にて行うことによりに、30〜360分
で目的とする水酸化マグネシウムを得ることができる。
上記の条件下にて生成する水酸化マグネシウムの一次粒
子は板状であり、二次凝集を起こしにくく、配向性及び
分散性が高い。
The above hydration reaction is carried out at a temperature of 100 to 250 ° C. and a steam pressure of 1 to 30 atm (preferably 120 to 20 atm).
By performing the reaction in an autoclave adjusted to a temperature of 0 ° C. and a steam pressure of 2 to 15 atm), the desired magnesium hydroxide can be obtained in 30 to 360 minutes.
The primary particles of magnesium hydroxide produced under the above conditions are plate-like, hardly cause secondary aggregation, and have high orientation and dispersibility.

【0036】こうして得られた水酸化マグネシウムを、
公知の手法に従って水洗、ろ過、乾燥することにより、
高純度高配向性水酸化マグネシウム粉末を製造すること
ができる。
The thus obtained magnesium hydroxide is
By washing, filtering, and drying according to a known method,
High purity and high orientation magnesium hydroxide powder can be produced.

【0037】本発明の高純度酸化マグネシウム粉末は、
上記のようにして製造される高純度高配向性水酸化マグ
ネシウム粉末を350℃以上、好ましくは500℃以上
の温度で焼成することにより製造することができる。特
に、本発明の高純度高配向性水酸化マグネシウム粉末を
350〜1100℃の温度で焼成することにより、水酸
化マグネシウム一次粒子の形状を維持した板状結晶の酸
化マグネシウム粉末を製造することができる。
The high-purity magnesium oxide powder of the present invention comprises:
The high-purity and high-orientation magnesium hydroxide powder produced as described above can be produced by firing at a temperature of 350 ° C. or more, preferably 500 ° C. or more. In particular, by firing the high-purity and highly-oriented magnesium hydroxide powder of the present invention at a temperature of 350 to 1100 ° C., a plate-like crystal magnesium oxide powder that maintains the shape of magnesium hydroxide primary particles can be produced. .

【0038】[0038]

【実施例】以下、本発明を実施例に基づいて具体的に説
明するが、これらは本発明を限定するものではない。な
お、実施例に記載の各元素の含有量及び物性は次のよう
にして測定した値である。
EXAMPLES Hereinafter, the present invention will be described specifically with reference to Examples, but these do not limit the present invention. The contents and physical properties of each element described in the examples are values measured as follows.

【0039】酸化マグネシウム含有量及び水酸化マグネ
シウム含有量は、試料を塩酸に溶解して、マグネシウム
イオンをEDTA溶液で滴定し、このマグネシウムイオ
ン量から算出した。なお、試料は105℃に調整した乾
燥機にて恒量になるまで乾燥したものを用いた。
The content of magnesium oxide and the content of magnesium hydroxide were calculated by dissolving a sample in hydrochloric acid, titrating magnesium ions with an EDTA solution, and calculating the amounts of magnesium ions. The sample used was dried by a dryer adjusted to 105 ° C. until a constant weight was obtained.

【0040】ハロゲン元素含有量(F、Cl、Br)
は、液体イオンクロマト法により測定した。
Halogen content (F, Cl, Br)
Was measured by a liquid ion chromatography method.

【0041】ハロゲン以外の各元素含有量(Ca、S
i、Fe、Al、Zr、Na、K、B、S、Cr、N
i、Mn、Cu、Zn、Pb、As)は、JIS K
0050に準じ、試料を塩酸に溶解し、誘導結合高周波
プラズマ発光分析装置及び原子吸光分光光度測定装置を
用いて測定した。
The content of each element other than halogen (Ca, S
i, Fe, Al, Zr, Na, K, B, S, Cr, N
i, Mn, Cu, Zn, Pb, As) are JIS K
According to 0050, the sample was dissolved in hydrochloric acid, and measured using an inductively coupled high-frequency plasma emission spectrometer and an atomic absorption spectrophotometer.

【0042】一次粒子の形状は、電子顕微鏡にて観察し
た。
The shape of the primary particles was observed with an electron microscope.

【0043】配向度(%)は、一軸成形機を用いて水酸
化マグネシウムの円柱状ペレットを作成し、このペレッ
トの平坦面に平行な面のX線回折パターンを得て、前記
の計算式(1)により算出した。水酸化マグネシウムの
円柱状ペレットは、重さ0.9±0.1g、直径24m
m、高さ3mmの大きさとした。X線回折装置には
(株)リガク製X線回折装置RINT2100/PCを
使用した。なお、X線回折パターンは回折角2θが5〜
70度の範囲で測定した。
The degree of orientation (%) can be determined by preparing a cylindrical pellet of magnesium hydroxide using a uniaxial molding machine, obtaining an X-ray diffraction pattern of a plane parallel to the flat surface of the pellet, and calculating the above formula ( It was calculated according to 1). Magnesium hydroxide cylindrical pellets weigh 0.9 ± 0.1 g, 24 m in diameter
m and a height of 3 mm. An X-ray diffractometer RINT2100 / PC manufactured by Rigaku Corporation was used as the X-ray diffractometer. The X-ray diffraction pattern has a diffraction angle 2θ of 5 to 5.
It was measured in the range of 70 degrees.

【0044】比表面積は、BET法により測定した。The specific surface area was measured by the BET method.

【0045】平均粒子径は、レーザ回折法により測定し
た。
The average particle diameter was measured by a laser diffraction method.

【0046】[実施例1]1350℃で焼成したマグネ
シアクリンカをジョークラッシャにより破砕し、篩で分
級して粒子径が1〜3mmの酸化マグネシウム粒状物を
得た。得られた酸化マグネシウム粒状物の酸化マグネシ
ウム含有量及び不純物の原子換算量を表1に示す。この
酸化マグネシウム粒状物1.0kgを0.25モル/リ
ットルの酢酸マグネシウム水溶液10リットル中に投入
し、充分な攪拌下に全容20リットルのオートクレーブ
中にて170℃(水蒸気圧は8気圧)、3時間反応させ
た後、45μmの篩で分級した。篩通過率は99%であ
った。上記の篩下生成物を水洗、ろ過、乾燥して得た粉
末は、水和率が100%であった。この粉末の粉体物
性、水酸化マグネシウム含有量及び不純物の原子換算量
の測定結果を表2に示す。
Example 1 Magnesia clinker fired at 1350 ° C. was crushed by a jaw crusher and classified by a sieve to obtain magnesium oxide granules having a particle diameter of 1 to 3 mm. Table 1 shows the magnesium oxide content and the atomic conversion of impurities of the obtained magnesium oxide granules. 1.0 kg of the magnesium oxide granules is put into 10 liters of a 0.25 mol / l aqueous solution of magnesium acetate, and 170 ° C. (steam pressure is 8 atm) in a 20 liter autoclave under sufficient stirring. After reacting for an hour, the mixture was classified with a 45 μm sieve. The sieve passing rate was 99%. The powder obtained by washing, filtering and drying the above-mentioned undersize product had a hydration ratio of 100%. Table 2 shows the measurement results of the powder physical properties, the content of magnesium hydroxide, and the atomic conversion of impurities.

【0047】[比較例1]実施例1で使用したものと同
じマグネシアクリンカを、ボールミル(鉄製ボールを使
用するもの)にて粉砕し、平均粒子径が3.5μmの酸
化マグネシウム粉末を得た。得られた酸化マグネシウム
粉末の酸化マグネシウム含有量及び不純物の原子換算量
を表1に示す。この酸化マグネシウム粉末1.0kgを
90℃に加熱保持された0.028モル/リットルの酢
酸マグネシウム水溶液10リットル中に投入し、充分な
撹拌下に3時間反応させた後、45μmの篩で分級し
た。篩通過率は96%であった。篩下生成物を実施例1
と同じ後処理をして得た粉末は、水和率が99%であっ
た。この粉末の粉体物性、水酸化マグネシウム含有量及
び不純物の原子換算量の測定結果を表2に示す。
Comparative Example 1 The same magnesia clinker used in Example 1 was pulverized with a ball mill (using an iron ball) to obtain a magnesium oxide powder having an average particle diameter of 3.5 μm. Table 1 shows the magnesium oxide content of the obtained magnesium oxide powder and the atomic conversion amount of impurities. 1.0 kg of this magnesium oxide powder was put into 10 liters of a 0.028 mol / l aqueous solution of magnesium acetate heated and maintained at 90 ° C., reacted for 3 hours with sufficient stirring, and then classified with a 45 μm sieve. . The sieve passing rate was 96%. Example 1
The powder obtained by performing the same post-treatment as described above had a hydration ratio of 99%. Table 2 shows the measurement results of the powder physical properties, the content of magnesium hydroxide, and the atomic conversion of impurities.

【0048】[0048]

【表1】 表1 ──────────────────────────────────── 実施例1の酸化マグネ 比較例1の酸化マグネ シウム粒状物原料 シウム粉末原料 ──────────────────────────────────── MgO(%) 99.3 99.3 ──────────────────────────────────── 不純物の原子換算量(%) Ca 0.350 0.350 Si 0.030 0.030 Fe 0.015 0.060 Al 0.014 0.014 Zr 0.0005以下 0.0005以下 Na 0.001 0.001 K 0.0005 0.0005 F 0.0001以下 0.0001以下 Cl 0.005 0.005 Br 0.0001以下 0.0001以下 B 0.004 0.004 S 0.004 0.004 Cr 0.001 0.001 Ni 0.004 0.004 Mn 0.001 0.001 Cu 0.0001以下 0.0001以下 Zn 0.0003 0.0003 Pb 0.0001 0.0001 As 0.00001 0.00001 ────────────────────────────────────Table 1 Table 1 酸化 Magnetooxide of Example 1 Comparative Example 1 Magnesium oxide granular material raw material Sium powder raw material Mg MgO (% ) 99.3 99.3 原子 Atomic conversion amount of impurities (% ) Ca 0.350 0.350 Si 0.030 0.030 Fe 0.015 0.060 Al 0.014 0.014 Zr 0.0005 or less 0.0005 or less Na 0.001 0.001 K 0.00005 0 0.0005 F 0.0001 or less 0.0001 or less Cl 0.005 0.005 Br 0.0001 or less 0.0001 or less B 0.00 0.004 S 0.004 0.004 Cr 0.001 0.001 Ni 0.004 0.004 Mn 0.001 0.001 Cu 0.0001 or less 0.0001 or less Zn 0.0003 0.0003 Pb 0.01 0001 0.0001 As 0.00001 0.00001 ────────────────────────────────────

【0049】[比較例2]市販の高純度試薬の粉体物
性、水酸化マグネシウム含有量及び不純物の原子換算量
の測定結果を表2に示す。
Comparative Example 2 Table 2 shows the measurement results of the powder properties, the content of magnesium hydroxide, and the amount of impurities in terms of atoms of a commercially available high-purity reagent.

【0050】[0050]

【表2】 表2 ──────────────────────────────────── 実施例1 比較例1 比較例2 ──────────────────────────────────── 一次粒子の形状 板状 六角板状 不定形 ──────────────────────────────────── 配向度 64 26 0 ──────────────────────────────────── 比表面積(m2/g) 10 14 25 ──────────────────────────────────── 平均粒子径(μm) 1.7 0.5 24 ──────────────────────────────────── Mg(OH)2(%) 99.9 99.7 99.1 ──────────────────────────────────── 不純物の原子換算量(%) Ca 0.0050 0.0650 0.0160 Si 0.0100 0.0150 0.0510 Fe 0.0090 0.0400 0.0160 Al 0.0090 0.0120 0.0200 Zr 0.0005以下 0.0005以下 0.0005以下 Na 0.0008 0.0010 0.0030 K 0.0001 0.0005 0.0006 F 0.0001以下 0.0001以下 0.0002 Cl 0.0020 0.0030 0.0040 Br 0.0001以下 0.0001以下 0.0002 B 0.0020 0.0020 0.1000 S 0.0010 0.0020 0.1400 Cr 0.0006 0.0008 0.0002以下 Ni 0.0030 0.0030 0.0007 Mn 0.0009 0.0010 0.0040 Cu 0.0001以下 0.0001以下 0.0001以下 Zn 0.0002 0.0002 0.0010 Pb 0.0001以下 0.0001以下 0.0001以下 As 0.00001以下 0.00001以下 0.0001 ────────────────────────────────────Table 2 Table 1 Example 1 Comparative Example 1 Comparative Example 2 形状 Primary particle shape Plate shape Hexagon plate shape Indefinite shape ──配 向 Orientation 64 26 0 ─────────── ───────────────────────── Specific surface area (m 2 / g) 10 14 25 ────────────── ────────────────────── Average particle size (μm) 1.7 0.5 24 ─────────────────── ───────────────── Mg (OH) 2 (%) 99.9 99.7 99.1 ────────────────────── ─────────原子 Atomic conversion amount of impurities (%) Ca 0.0050 0.0650 0.0160 Si 0.0100 0.0150 0.0510 Fe 0.0090 0.0400 0.0160 Al 0.0090 0.0120 0.0200 Zr 0.0005 or less 0.0005 or less 0.0005 or less Na 0.0008 0.0010 0.0030 K 0.0001 0.0005 0.0006 F 0.0001 or less 0.0001 or less 0.0002 Cl 0.0020 0.0030 0.0040 Br 0.0001 or less 0.0001 or less 0.0002 B 0.0020 0.0020 0.1000 S 0.0010 0.0020 0.1400 Cr 0.0006 0.0008 0.0002 or less Ni 0.0030 0.0030 0.0007 Mn 0.0009 0.0010 0.0040 Cu 0.0001 or less 0.0001 or less 0.0001 or less Zn 0.0002 0.0002 0.0010 Pb 0.0001 or less 0.0001 or less 0.0001 As 0.00001 or less 0.00001 or less 0.0001 ────────────────────────────────────

【0051】[実施例2]実施例1で製造した水酸化マ
グネシウム粉末50gを、1リットルの純水に分散させ
た水酸化マグネシウム分散液を調製した。この分散液を
平滑な石英片に塗布し、1000℃に加熱して固形物を
得た。得られた固形物をX線回折法により同定したとこ
ろ、酸化マグネシウムであることが確認された。さら
に、この固形物を電子顕微鏡(SEM)で観察した結
果、板状結晶が配向していることがわかった。固形物の
酸化マグネシウム含有量及び不純物の原子換算量の測定
結果を表3に示す。
Example 2 A magnesium hydroxide dispersion was prepared by dispersing 50 g of the magnesium hydroxide powder produced in Example 1 in 1 liter of pure water. The dispersion was applied to a smooth piece of quartz and heated to 1000 ° C. to obtain a solid. When the obtained solid was identified by an X-ray diffraction method, it was confirmed to be magnesium oxide. Furthermore, as a result of observing this solid with an electron microscope (SEM), it was found that the plate-like crystals were oriented. Table 3 shows the measurement results of the magnesium oxide content of the solid and the atomic conversion of impurities.

【0052】[0052]

【表3】 表3 ──────────────────────────────────── 実施例2 ──────────────────────────────────── MgO(%) 99.9 ──────────────────────────────────── 不純物の原子換算量(%) Ca 0.0070 Si 0.0150 Fe 0.0130 Al 0.0130 Zr 0.0005以下 Na 0.0010 K 0.0001 F 0.0001以下 Cl 0.0030 Br 0.0001以下 B 0.0030 S 0.0015 Cr 0.0009 Ni 0.0040 Mn 0.0013 Cu 0.0001以下 Zn 0.0003 Pb 0.0001以下 As 0.00001以下 ────────────────────────────────────[Table 3] Table 3 {Example 2} ─────────────────────────────── MgO (%) 99.9 ────────────原子 Atomic conversion amount of impurities (%) Ca 0.0070 Si 0.0150 Fe 0.0130 Al 0.0130 Zr 0 0.0005 or less Na 0.0010 K 0.0001 F 0.0001 or less Cl 0.0030 Br 0.0001 or less B 0.0030 S 0.0015 Cr 0.0009 Ni 0.0040 Mn 0.0013 Cu 0.0001 or less Zn 0.0003 Pb 0.0001 or less As 0.00001 or less ──────────────── ───────────────────

【0053】[0053]

【発明の効果】本発明の高純度高配向水酸化マグネシウ
ム粉末は、電子材料、特に薄膜状の電子材料用の酸化マ
グネシウム原料として好適に使用することができる。ま
た、本発明の高純度酸化マグネシウム粉末は、電子材料
の添加剤として好適に使用することができる。さらに、
本発明の高純度高配向水酸化マグネシウム粉末の製造方
法によれば、不純物含有量が少なく、配向性が高い水酸
化マグネシウム粉末を、工業的な規模で経済的に効率よ
く製造することができる。
The high-purity and highly-oriented magnesium hydroxide powder of the present invention can be suitably used as a raw material of magnesium oxide for electronic materials, especially thin-film electronic materials. Further, the high-purity magnesium oxide powder of the present invention can be suitably used as an additive for electronic materials. further,
According to the method for producing a highly pure and highly oriented magnesium hydroxide powder of the present invention, a magnesium hydroxide powder having a low impurity content and a high orientation can be produced economically and efficiently on an industrial scale.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 市村 洋二郎 山口県宇部市大字小串1985番地 宇部マテ リアルズ株式会社内 Fターム(参考) 4G076 AA10 AB02 BA09 BB08 BD02 BD10 CA02 CA05 CA15 CA26 CA28 CA36 DA03  ────────────────────────────────────────────────── ─── Continuing on the front page (72) Inventor Yojiro Ichimura 1985 Kogushi, Obe, Ube City, Yamaguchi Prefecture F-term in Ube Mate Reals Co., Ltd. 4G076 AA10 AB02 BA09 BB08 BD02 BD10 CA02 CA05 CA15 CA26 CA28 CA36 DA03

Claims (8)

【特許請求の範囲】[Claims] 【請求項1】 カルシウム化合物、珪素化合物、鉄化合
物、アルミニウム化合物、そしてジルコニウム化合物の
含有量が、それぞれカルシウム原子換算量で0.01質
量%以下、珪素原子換算量で0.02質量%以下、鉄原
子換算量で0.015質量%以下、アルミニウム原子換
算量で0.015質量%以下、及びジルコニウム原子換
算量で0.005質量%以下であり、水酸化マグネシウ
ム含有量が99.5質量%以上であって、粒子の主要部
が板状の一次粒子をなすことを特徴とする高純度高配向
性水酸化マグネシウム粉末。
1. The content of each of a calcium compound, a silicon compound, an iron compound, an aluminum compound, and a zirconium compound is 0.01% by mass or less in terms of calcium atom, and 0.02% by mass or less in terms of silicon atom. The content is 0.015% by mass or less in terms of iron atoms, 0.015% by mass or less in terms of aluminum atoms, and 0.005% by mass or less in terms of zirconium atoms, and the magnesium hydroxide content is 99.5% by mass. The high purity and high orientation magnesium hydroxide powder as described above, wherein the main parts of the particles form plate-like primary particles.
【請求項2】 ナトリウム化合物の含有量がナトリウム
原子換算量で0.003質量%以下であり、かつカリウ
ム化合物の含有量がカリウム原子換算量で0.002質
量%以下であることを特徴とする請求項1に記載の高純
度高配向性水酸化マグネシウム粉末。
2. The method according to claim 1, wherein the content of the sodium compound is 0.003% by mass or less in terms of sodium atom, and the content of the potassium compound is 0.002% by mass or less in terms of potassium atom. The high-purity and high-orientation magnesium hydroxide powder according to claim 1.
【請求項3】 フッ化物、塩化物及び臭化物の含有量が
それぞれフッ素、塩素及び臭素の原子換算量で0.00
5質量%以下であることを特徴とする請求項1もしくは
2に記載の高純度高配向性水酸化マグネシウム粉末。
3. The contents of fluoride, chloride and bromide are 0.00, respectively, in terms of the atomic amount of fluorine, chlorine and bromine.
The high-purity and high-orientation magnesium hydroxide powder according to claim 1 or 2, which is 5% by mass or less.
【請求項4】 ホウ素化合物の含有量がホウ素原子換算
量で0.01質量%以下であり、硫黄化合物の含有量が
硫黄原子換算量で0.005質量%以下であることを特
徴とする請求項1乃至3のうちのいずれかの項に記載の
高純度高配向性水酸化マグネシウム粉末。
4. The method according to claim 1, wherein the content of the boron compound is 0.01% by mass or less in terms of boron atoms, and the content of the sulfur compound is 0.005% by mass or less in terms of sulfur atoms. Item 4. The high-purity and high-orientation magnesium hydroxide powder according to any one of Items 1 to 3.
【請求項5】 配向度が30%以上であることを特徴と
する請求項1乃至4のうちのいずれかの項に記載の高純
度高配向性水酸化マグネシウム粉末。
5. The high-purity and high-orientation magnesium hydroxide powder according to claim 1, wherein the degree of orientation is 30% or more.
【請求項6】 請求項1乃至5のうちのいずれかの項に
記載の高純度高配向性水酸化マグネシウム粉末を350
℃以上の温度で焼成して得られる高純度酸化マグネシウ
ム粉末。
6. The high-purity and high-orientation magnesium hydroxide powder according to any one of claims 1 to 5,
High-purity magnesium oxide powder obtained by firing at a temperature of at least ℃.
【請求項7】 カルシウム化合物、珪素化合物、鉄化合
物、アルミニウム化合物、そしてジルコニウム化合物の
含有量が、それぞれカルシウム原子換算量で2質量%以
下、珪素原子換算量で2質量%以下、鉄原子換算量で
0.15質量%以下、アルミニウム原子換算量で0.1
5質量%以下、及びジルコニウム原子換算量で0.05
質量%以下であって、酸化マグネシウム含有量が95質
量%以上である酸化マグネシウム焼成物を、水溶性マグ
ネシウム塩の存在下、100〜250℃の温度、1〜3
0気圧の水蒸気圧に調整されたオートクレーブ中にて水
和させることを特徴とする請求項1に記載の高純度高配
向性水酸化マグネシウム粉末の製造方法。
7. The content of each of a calcium compound, a silicon compound, an iron compound, an aluminum compound, and a zirconium compound is 2% by mass or less in terms of calcium atoms, 2% by mass or less in terms of silicon atoms, and iron in terms of atoms. 0.15% by mass or less in terms of aluminum atom
5% by mass or less, and 0.05 in terms of zirconium atom
Mass% or less, and a magnesium oxide content of 95 mass% or more, in the presence of a water-soluble magnesium salt, at a temperature of 100 to 250 ° C.,
The method for producing a highly pure and highly oriented magnesium hydroxide powder according to claim 1, wherein the hydration is performed in an autoclave adjusted to a water vapor pressure of 0 atm.
【請求項8】 前記酸化マグネシウム焼成物が、沸点1
150℃以下の無機化合物の含有量がそれぞれ、ナトリ
ウム原子換算量で0.02質量%以下、カリウム原子換
算量で0.01質量%以下、フッ素、塩素及び臭素の原
子換算量で0.03質量%以下、ホウ素原子換算量で
0.1質量%以下、そして硫黄原子換算量で0.02質
量%以下であることを特徴とする請求項7に記載の高純
度高配向性水酸化マグネシウム粉末の製造方法。
8. The fired magnesium oxide product having a boiling point of 1
The content of the inorganic compound at 150 ° C. or less is 0.02% by mass or less in terms of sodium atom, 0.01% by mass or less in terms of potassium atom, and 0.03% by mass in terms of atom amount of fluorine, chlorine and bromine. % Or less, 0.1% by mass or less in terms of boron atoms, and 0.02% by mass or less in terms of sulfur atoms. Production method.
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