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JP7680899B2 - Aluminum hydroxide powder and its manufacturing method - Google Patents
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JP7680899B2 - Aluminum hydroxide powder and its manufacturing method - Google Patents

Aluminum hydroxide powder and its manufacturing method Download PDF

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JP7680899B2
JP7680899B2 JP2021112854A JP2021112854A JP7680899B2 JP 7680899 B2 JP7680899 B2 JP 7680899B2 JP 2021112854 A JP2021112854 A JP 2021112854A JP 2021112854 A JP2021112854 A JP 2021112854A JP 7680899 B2 JP7680899 B2 JP 7680899B2
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智孝 北
巧介 前田
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Sumitomo Chemical Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
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    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
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    • C01F7/02Aluminium oxide; Aluminium hydroxide; Aluminates
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Description

本開示は水酸化アルミニウム粉末およびその製造方法に関する。 This disclosure relates to aluminum hydroxide powder and a method for producing the same.

水酸化アルミニウム粉末は、樹脂成形体(封止材、サーマルインターフェース材料(Thermal Interface Material:TIM)、人工大理石等)への充填材として需要が高まっている。
例えば特許文献1には、原料水酸化アルミニウムを、圧縮能力が5~500kgf/cmであるスクリュー型捏和機で粉砕することを特徴とする、充填材用途の水酸化アルミニウムの製造方法が開示されている。
Demand for aluminum hydroxide powder is increasing as a filler for resin molded products (sealants, thermal interface materials (TIM), artificial marble, etc.).
For example, Patent Document 1 discloses a method for producing aluminum hydroxide for use as a filler, which is characterized in that raw aluminum hydroxide is pulverized in a screw-type kneader having a compression capacity of 5 to 500 kgf/ cm2 .

特開2001-322813号公報JP 2001-322813 A

しかしながら、特許文献1に開示されるような従来技術では、水酸化アルミニウム粉末を樹脂に添加した際に増粘しやすいおそれがあることがわかった。 However, it has been found that conventional techniques such as those disclosed in Patent Document 1 may lead to increased viscosity when aluminum hydroxide powder is added to the resin.

本発明はこのような状況に鑑みてなされたものであり、その目的の1つは、樹脂に添加した際に粘度上昇を十分に抑制できる水酸化アルミニウム粉末およびその製造方法を提供することである。 The present invention was made in consideration of these circumstances, and one of its objectives is to provide an aluminum hydroxide powder that can sufficiently suppress viscosity increase when added to a resin, and a method for producing the same.

本発明の態様1は、
10MPaで成型したときの密度が1.59~2.00g/cmであり、
XRDパターンにおける(110)面の回折強度に対する(002)面の回折強度の比が、2.0~7.5である、水酸化アルミニウム粉末である。
Aspect 1 of the present invention is
The density when molded at 10 MPa is 1.59 to 2.00 g/ cm3 ,
The aluminum hydroxide powder has an XRD pattern in which the ratio of the diffraction intensity of the (002) plane to the diffraction intensity of the (110) plane is 2.0 to 7.5.

本発明の態様2は、
90質量%粒子径(D90)が100μm未満である、態様1に記載の水酸化アルミニウム粉末である。
Aspect 2 of the present invention is
The aluminum hydroxide powder according to aspect 1, wherein the 90% by mass particle size (D90) is less than 100 μm.

本発明の態様3は、
質量基準粒度分布において1~200μmの粒径範囲に1つ又は2つのピークを有し、
ピークが1つの場合は、該ピークの頻度が4.0質量%以上であり、
ピークが2つの場合は、一方のピークの頻度が4.0質量%以上であり、他方のピークの頻度が0質量%超4.0質量%以下である、態様1または2に記載の水酸化アルミニウム粉末である。
Aspect 3 of the present invention is
The mass standard particle size distribution has one or two peaks in the particle size range of 1 to 200 μm,
When there is one peak, the frequency of the peak is 4.0% by mass or more,
In the case where there are two peaks, the frequency of one peak is 4.0 mass% or more, and the frequency of the other peak is more than 0 mass% and 4.0 mass% or less, in the aluminum hydroxide powder according to aspect 1 or 2.

本発明の態様4は、
50質量%粒子径(D50)が10~200μmであり、且つ半径0.05~1μmの細孔の累積容積が0.01~1mL/gである水酸化アルミニウム粉末を、49.0~294.0MPaの圧力で粉砕した後、92m/秒以下の衝突速度で解砕することを含む、水酸化アルミニウム粉末の製造方法である。
Aspect 4 of the present invention is
The method for producing aluminum hydroxide powder comprises crushing aluminum hydroxide powder having a 50% mass particle size (D50) of 10 to 200 μm and a cumulative volume of pores with a radius of 0.05 to 1 μm of 0.01 to 1 mL/g under a pressure of 49.0 to 294.0 MPa, and then disintegrating the powder at a collision speed of 92 m/sec or less.

本発明の実施形態によれば、樹脂に添加した際に粘度上昇を十分に抑制できる水酸化アルミニウム粉末およびその製造方法を提供することが可能である。 According to an embodiment of the present invention, it is possible to provide an aluminum hydroxide powder that can sufficiently suppress an increase in viscosity when added to a resin, and a method for producing the same.

本発明者らは、樹脂に添加した際の粘度(以下「樹脂粘度」とも称する)の上昇を十分に抑制できる水酸化アルミニウム粉末を実現するべく、様々な角度から検討した。その結果、10MPaで成型したときの密度(以下「成型密度」とも称する)およびXRDパターンにおける(110)面の回折強度に対する(002)面の回折強度の比(以下「(002)/(110)回折強度比」とも称する)を所定範囲に制御することにより、樹脂粘度の上昇を十分に抑制できることを見出した。
成型密度および(002)/(110)回折強度比を所定範囲に制御するために、原料水酸化アルミニウム粉末の粒径および細孔容積を所定範囲に制御するとともに、従来技術よりも大きな圧力(500~3000kgf/cm、すなわち49.0~294.0MPa)で粉砕し、さらに92m/秒以下という比較的弱い衝突速度で解砕することが重要であることを見出した。
The present inventors have conducted research from various angles in order to realize an aluminum hydroxide powder that can sufficiently suppress an increase in viscosity (hereinafter also referred to as "resin viscosity") when added to a resin. As a result, they have found that an increase in resin viscosity can be sufficiently suppressed by controlling, within a predetermined range, the density when molded at 10 MPa (hereinafter also referred to as "molded density") and the ratio of the diffraction intensity of the (002) plane to the diffraction intensity of the (110) plane in the XRD pattern (hereinafter also referred to as "(002)/(110) diffraction intensity ratio").
It has been found that in order to control the molding density and the (002)/(110) diffraction intensity ratio within a predetermined range, it is important to control the particle size and pore volume of the raw aluminum hydroxide powder within a predetermined range, to crush the powder at a pressure greater than that of the conventional technology (500 to 3000 kgf/ cm2 , i.e., 49.0 to 294.0 MPa), and to disintegrate the powder at a relatively low impact speed of 92 m/sec or less.

以下に、本発明の実施形態が規定する各要件の詳細を示す。 The following provides details of each requirement stipulated by the embodiment of the present invention.

<1.水酸化アルミニウム粉末>
本発明の実施形態に係る水酸化アルミニウム粉末は、10MPaで成型したときの密度が1.59~2.00g/cmであり、XRDパターンにおける(110)面の回折強度に対する(002)面の回折強度の比が、2.0~7.5である。これにより、樹脂粘度の上昇を十分に抑制できる。
<1. Aluminum hydroxide powder>
The aluminum hydroxide powder according to the embodiment of the present invention has a density of 1.59 to 2.00 g/ cm3 when molded at 10 MPa, and a ratio of the diffraction intensity of the (002) plane to the diffraction intensity of the (110) plane in the XRD pattern of 2.0 to 7.5. This makes it possible to sufficiently suppress an increase in the resin viscosity.

成型密度が1.59g/cm未満であると、樹脂粘度が上昇する。成型密度の上限については特に制限されないが、例えば2.00g/cm超とするためにはより詳細な製造条件の設定が必要となり、生産性を考慮すると2.00g/cm以下にしておくことが好ましい。 If the molding density is less than 1.59 g/ cm3 , the resin viscosity increases. There is no particular upper limit to the molding density, but to make it exceed 2.00 g/ cm3 , for example, more detailed manufacturing conditions must be set, and it is preferable to keep it at 2.00 g/cm3 or less in consideration of productivity.

なお、成型密度は以下のようにして求めるものとする。
水酸化アルミニウム粉末3.00gを内径20.0mmの円筒一軸成形用金型に入れ、万能材料試験機(例えばエー・アンド・デイ(A&D)社製、TENSILON RTG-1310)を用い、当該水酸化アルミニウム粉末を圧縮速度1mm/分で10MPaの圧力になるまで圧縮充填し、重量/体積の比を成形密度とする。
The molding density is determined as follows.
3.00 g of aluminum hydroxide powder is placed in a cylindrical uniaxial molding die having an inner diameter of 20.0 mm, and the aluminum hydroxide powder is compressed and packed at a compression speed of 1 mm/min to a pressure of 10 MPa using a universal material testing machine (e.g., TENSILON RTG-1310 manufactured by A&D Corporation), and the weight/volume ratio is defined as the molding density.

(002)/(110)回折強度比が7.5超であると、水酸化アルミニウム粉末が、例えば、通常球状に近い形状であり得るところ板状のように歪形状となり、樹脂粘度が上昇する。好ましくは、(002)/(110)回折強度比が6.0以下である。(002)/(110)回折強度比の下限は特に制限されないが、(002)/(110)回折強度比を2.0未満とするためにはより詳細な製造条件の設定が必要となり、生産性を考慮すると2.0以上にしておくことが好ましい。 If the (002)/(110) diffraction intensity ratio exceeds 7.5, the aluminum hydroxide powder, which may normally have a shape close to a sphere, will become distorted, for example, into a plate-like shape, and the resin viscosity will increase. Preferably, the (002)/(110) diffraction intensity ratio is 6.0 or less. There is no particular lower limit to the (002)/(110) diffraction intensity ratio, but in order to make the (002)/(110) diffraction intensity ratio less than 2.0, more detailed manufacturing conditions must be set, and it is preferable to set it to 2.0 or more in consideration of productivity.

なお、(002)/(110)回折強度比は以下のようにして求めるものとする。
水酸化アルミニウム粉末を測定用ガラスセルに圧密して充填した後、粉末X線回折測定装置(例えばリガク社製、RINT-2000)を用いて、ステップ幅0.02deg、スキャンスピード0.04deg/sec、加速電圧40kV、加速電流30mAにてXRDパターンを測定する。X線源としてはCu-Kαを用いる。得られたXRDパターンにおいて、2θ=18.3°の位置に現れるピークを(002)面のピークとし、2θ=20.3°の位置に現れるピークを(110)面のピークとして、(110)面のピークの回折強度(ピーク高さ)に対する(002)面のピークの回折強度(ピーク高さ)の比を、(002)/(110)回折強度比とする。
The (002)/(110) diffraction intensity ratio is determined as follows.
The aluminum hydroxide powder is compacted and packed into a glass cell for measurement, and then an XRD pattern is measured using a powder X-ray diffraction measuring device (e.g., Rigaku Corporation, RINT-2000) with a step width of 0.02 deg, a scan speed of 0.04 deg/sec, an acceleration voltage of 40 kV, and an acceleration current of 30 mA. Cu-Kα is used as the X-ray source. In the obtained XRD pattern, the peak appearing at 2θ=18.3° is taken as the peak of the (002) plane, and the peak appearing at 2θ=20.3° is taken as the peak of the (110) plane, and the ratio of the diffraction intensity (peak height) of the peak of the (002) plane to the diffraction intensity (peak height) of the peak of the (110) plane is taken as the (002)/(110) diffraction intensity ratio.

本発明の実施形態に係る水酸化アルミニウム粉末は、90質量%粒子径(すなわち、質量基準粒度分布における、微粒側からの累積頻度が90質量%となる粒子径であって、D90とも称する)が100μm未満であることが好ましい。これにより、水酸化アルミニウム粉末を樹脂成形体に充填したときの外観不良を十分に抑制することができ、また樹脂成形体の強度を十分に確保しやすくなる。好ましくは、D90が90μm以下であり、より好ましくは65μm以下であり、さらに好ましくは45μm以下である。
本発明の実施形態に係る水酸化アルミニウム粉末は、D90が20μm以上であることが好ましい。これにより、水酸化アルミニウム粉末を液中に分散させる際の分散不良を抑制することができる。
The aluminum hydroxide powder according to the embodiment of the present invention preferably has a 90% by mass particle size (i.e., the particle size at which the cumulative frequency from the fine particle side in the mass-based particle size distribution is 90% by mass, also referred to as D90) of less than 100 μm. This makes it possible to sufficiently suppress poor appearance when the aluminum hydroxide powder is filled into a resin molded body, and also makes it easier to ensure sufficient strength of the resin molded body. Preferably, D90 is 90 μm or less, more preferably 65 μm or less, and even more preferably 45 μm or less.
The aluminum hydroxide powder according to the embodiment of the present invention preferably has a D90 of 20 μm or more, which can suppress poor dispersion when dispersing the aluminum hydroxide powder in a liquid.

本発明の実施形態に係る水酸化アルミニウム粉末は、質量基準粒度分布において1~200μmの粒径範囲に1つ又は2つのピークを有することが好ましい。これにより、水酸化アルミニウム粉末を樹脂成形体に充填したときの外観不良を抑制することができ、また水酸化アルミニウム粉末を液中に分散させる際の分散不良を抑制することもできる。ピークが1つの場合は、該ピークの頻度が4.0質量%以上であり得る。ピークが2つの場合は、一方のピークの頻度が4.0質量%以上であり得、他方のピークの頻度が0質量%超4.0質量%以下であり得る。この場合、好ましくは、質量基準粒度分布において1~200μmの粒径範囲にピークを1つのみ有することである。これにより、上記樹脂成形体の外観不良および分散不良を、さらに抑制することができる。 The aluminum hydroxide powder according to the embodiment of the present invention preferably has one or two peaks in the particle size range of 1 to 200 μm in the mass-based particle size distribution. This can suppress poor appearance when the aluminum hydroxide powder is filled into a resin molded body, and can also suppress poor dispersion when the aluminum hydroxide powder is dispersed in a liquid. When there is one peak, the frequency of the peak may be 4.0 mass% or more. When there are two peaks, the frequency of one peak may be 4.0 mass% or more, and the frequency of the other peak may be more than 0 mass% and 4.0 mass% or less. In this case, it is preferable that there is only one peak in the particle size range of 1 to 200 μm in the mass-based particle size distribution. This can further suppress poor appearance and poor dispersion of the resin molded body.

本発明の実施形態に係る水酸化アルミニウム粉末は、質量基準粒度分布において、1μm未満および200μm超の粒径範囲の一方または両方のそれぞれに1つ以上のピークを有し得、前記ピークの頻度は0質量%超0.5質量%以下であってもよく、または、1μm未満および200μm超の粒径範囲にピークを有さなくてもよい。 The aluminum hydroxide powder according to the embodiment of the present invention may have one or more peaks in the mass-based particle size distribution in one or both of the particle size ranges of less than 1 μm and more than 200 μm, and the frequency of the peaks may be greater than 0 mass% and less than 0.5 mass%, or may have no peaks in the particle size ranges of less than 1 μm and more than 200 μm.

本発明の実施形態に係る水酸化アルミニウム粉末は、50質量%粒子径(すなわち、質量基準粒度分布における、微粒側からの累積頻度が50質量%となる粒子径であって、D50とも称する)が30μm以下であることが好ましい。これにより、水酸化アルミニウム粉末を樹脂成形体に充填したときの外観不良を抑制することができ、また樹脂成形体の強度を確保しやすくなる。
本発明の実施形態に係る水酸化アルミニウム粉末は、D50が7μm以上であることが好ましい。これにより、水酸化アルミニウム粉末を液中に分散させる際の分散不良を抑制することができる。
The aluminum hydroxide powder according to the embodiment of the present invention preferably has a 50% by mass particle size (i.e., the particle size at which the cumulative frequency from the fine particle side in the mass-based particle size distribution is 50% by mass, also referred to as D50) of 30 μm or less, which can suppress poor appearance when the aluminum hydroxide powder is filled into a resin molded body, and also makes it easier to ensure the strength of the resin molded body.
The aluminum hydroxide powder according to the embodiment of the present invention preferably has a D50 of 7 μm or more, which can suppress poor dispersion when dispersing the aluminum hydroxide powder in a liquid.

なお、質量基準粒度分布(D50およびD90含む)は、以下のようにして求める。
水酸化アルミニウム粉末を0.2質量%ヘキサメタリン酸ナトリウム水溶液中に加え、出力25Wの超音波を120秒間照射して水酸化アルミニウム粉末を水溶液中に分散させたものに対して、レーザー散乱式粒子径分布測定装置を用いて質量基準粒度分布(D50およびD90含む)を求める。該粒度分布は、粒子径0.02μm~2000μmの範囲を対数スケールで132分割し、各区間の粒子径を有する水酸化アルミニウムの質量を測定して求めるものとする。なお、レーザー散乱式粒子径分布測定装置としては、機器間差および本実施例等との整合性を考慮すると、マイクロトラックMT-3300EXII(日機装社製)又はそれと同等の装置を使用することが好ましい。また、粒度分布測定時において、水酸化アルミニウム粉末の濃度を上記測定装置の測定可能濃度に適宜調整した上で測定するのがよい。
The mass-based particle size distribution (including D50 and D90) is determined as follows.
Aluminum hydroxide powder is added to a 0.2% by mass aqueous solution of sodium hexametaphosphate, and ultrasonic waves of 25 W are applied for 120 seconds to disperse the aluminum hydroxide powder in the aqueous solution. The mass-based particle size distribution (including D50 and D90) of the aluminum hydroxide powder is determined using a laser scattering particle size distribution measuring device. The particle size distribution is determined by dividing the particle size range of 0.02 μm to 2000 μm into 132 parts on a logarithmic scale and measuring the mass of aluminum hydroxide having a particle size in each section. In addition, as the laser scattering particle size distribution measuring device, it is preferable to use a Microtrac MT-3300EXII (manufactured by Nikkiso Co., Ltd.) or a device equivalent thereto, taking into consideration the difference between devices and the consistency with the present embodiment and the like. In addition, when measuring the particle size distribution, it is preferable to appropriately adjust the concentration of the aluminum hydroxide powder to a measurable concentration of the measuring device before measurement.

本発明の実施形態に係る水酸化アルミニウム粉末は、BET比表面積を2.0m/g以下とすることが好ましい。これにより、水酸化アルミニウム粉末を液中に分散させる際の分散不良を抑制することができる。なお、BET比表面積は、JIS-Z-8830:2013に規定された方法に従って、全自動比表面積測定装置(例えば、Mountech社製、Macsorb HM-1201)を用いて窒素吸着法により求めるものとする。 The aluminum hydroxide powder according to the embodiment of the present invention preferably has a BET specific surface area of 2.0 m 2 /g or less. This makes it possible to suppress poor dispersion when dispersing the aluminum hydroxide powder in a liquid. The BET specific surface area is determined by a nitrogen adsorption method using a fully automatic specific surface area measuring device (e.g., Macsorb HM-1201 manufactured by Mountech) in accordance with the method specified in JIS-Z-8830:2013.

本発明の実施形態に係る水酸化アルミニウム粉末は、不純物としてNaOを含み得る。NaOの含有量は、例えば0.13質量%以下とすることが好ましい。これにより、樹脂成形体に充填したときの樹脂の劣化および絶縁性の低下を抑制することができる。ここで、NaO含有量は、水酸化アルミニウム粉末を無機酸の水溶液に溶解させて水溶液を調製した後、ICP発光分光分析装置を用いて求めるものとする。具体的には、ナトリウムの波長(589.592nm)の強度を測定し、NaOに換算して、NaOの質量を算出し、溶解させた水酸化アルミニウム粉末の質量に対する該NaOの質量の比を、NaO含有量(質量%)とする。また、本発明の実施形態に係る水酸化アルミニウム粉末は、Al(OH)およびNaOの他、不可避不純物を含んでもよい。不可避不純物として、原料、資材、製造設備等の状況によって持ち込まれる元素等の混入が許容される。 The aluminum hydroxide powder according to the embodiment of the present invention may contain Na 2 O as an impurity. The content of Na 2 O is preferably, for example, 0.13 mass% or less. This can suppress deterioration of the resin and decrease in insulation when filled into a resin molded body. Here, the Na 2 O content is determined by dissolving the aluminum hydroxide powder in an aqueous solution of an inorganic acid to prepare an aqueous solution, and then using an ICP emission spectrometer. Specifically, the intensity of the wavelength of sodium (589.592 nm) is measured, converted into Na 2 O, the mass of Na 2 O is calculated, and the ratio of the mass of the Na 2 O to the mass of the dissolved aluminum hydroxide powder is the Na 2 O content (mass%). In addition to Al(OH) 3 and Na 2 O, the aluminum hydroxide powder according to the embodiment of the present invention may contain inevitable impurities. As inevitable impurities, the inclusion of elements brought in due to the conditions of raw materials, materials, manufacturing equipment, etc. is permitted.

本発明の実施形態に係る水酸化アルミニウム粉末は、樹脂に添加した際に粘度上昇を十分に抑制でき、樹脂成形体(封止材、サーマルインターフェース材料(Thermal Interface Material:TIM)、人工大理石等)への充填材として好適である。適用可能な樹脂としては、例えば、不飽和ポリエステル樹脂、エポキシ樹脂、フェノール樹脂、ポリウレタン樹脂等の熱硬化性樹脂や、ポリエチレン、ポリプロピレン、エチレンとプロピレンとの共重合体、エチレン及び/又はプロピレンと例えばブテン-1、ペンテン-1、ヘキセン-1、ヘプテン-1、オクテン-1、ノネン-1、4-メチルペンテン-1、デセン-1等の他のα-オレフィンとの共重合体で代表されるポリオレフィン、スチレン(共)重合体、メタクリル酸メチル(共)重合体、ポリアミド、ポリカーボネート、エチレン-酢酸ビニル共重合体、ポリアセタール、アクリロニトリル-ブタジエン-スチレン共重合体、ポリフェニレンオキサイド、ポリエーテルサルホン、ポリアリレート、ポリエーテルエーテルケトン、ポリメチルペンテン等の熱可塑性樹脂等が挙げられる。本発明の実施形態に係る水酸化アルミニウム粉末は上記樹脂に限らず、他の合成樹脂、天然樹脂又は紙等の充填材として使用することも可能である。 The aluminum hydroxide powder according to the embodiment of the present invention can sufficiently suppress the increase in viscosity when added to a resin, and is suitable as a filler for resin molded bodies (sealing materials, thermal interface materials (TIM), artificial marble, etc.). Applicable resins include, for example, thermosetting resins such as unsaturated polyester resins, epoxy resins, phenolic resins, and polyurethane resins, and thermoplastic resins such as polyethylene, polypropylene, copolymers of ethylene and propylene, copolymers of ethylene and/or propylene with other α-olefins such as butene-1, pentene-1, hexene-1, heptene-1, octene-1, nonene-1, 4-methylpentene-1, and decene-1, tyrenic (co)polymers, methyl methacrylate (co)polymers, polyamides, polycarbonates, ethylene-vinyl acetate copolymers, polyacetals, acrylonitrile-butadiene-styrene copolymers, polyphenylene oxides, polyethersulfones, polyarylates, polyetheretherketones, and polymethylpentenes. The aluminum hydroxide powder according to the embodiment of the present invention is not limited to the above resins, but can also be used as a filler for other synthetic resins, natural resins, paper, etc.

<2.水酸化アルミニウム粉末の製造方法>
本発明の実施形態に係る水酸化アルミニウム粉末の製造方法は、(a)50質量%粒子径(D50)が10~200μmであり、且つ半径0.05~1μmの細孔の累積容積が0.01~1mL/gである水酸化アルミニウム粉末を用意する工程と、(b)49.0~294.0MPaの圧力で粉砕する工程と、(c)92m/秒以下の衝突速度で解砕する工程と、を含む。以下、各工程について詳述する。
2. Method for producing aluminum hydroxide powder
The method for producing an aluminum hydroxide powder according to an embodiment of the present invention includes the steps of (a) preparing an aluminum hydroxide powder having a 50% by mass particle size (D50) of 10 to 200 μm and a cumulative volume of pores with a radius of 0.05 to 1 μm of 0.01 to 1 mL/g, (b) pulverizing the powder at a pressure of 49.0 to 294.0 MPa, and (c) disintegrating the powder at a collision speed of 92 m/sec or less. Each step will be described in detail below.

[(a)水酸化アルミニウム粉末を用意する工程]
まず、原料となる水酸化アルミニウム粉末(以下、「原料水酸化アルミニウム粉末」とも称する)を用意する。原料水酸化アルミニウム粉末は、50質量%粒子径(D50)が10~200μmであり、且つ半径0.05~1μmの細孔の累積容積(以下「細孔累積容積」とも称する)が0.01~1mL/gである必要がある。これにより、所望の成型密度が得やすくなる。好ましくは、細孔累積容積が0.02~1mL/gである。これにより、所望のD90を得やすくなり、また、所望の質量基準粒度分布である水酸化アルミニウム粉末を得やすくなる。
[(a) Step of preparing aluminum hydroxide powder]
First, aluminum hydroxide powder (hereinafter also referred to as "raw aluminum hydroxide powder") is prepared as a raw material. The raw aluminum hydroxide powder must have a 50% mass particle size (D50) of 10 to 200 μm and a cumulative volume of pores with a radius of 0.05 to 1 μm (hereinafter also referred to as "accumulated pore volume") of 0.01 to 1 mL/g. This makes it easier to obtain a desired molding density. Preferably, the cumulative pore volume is 0.02 to 1 mL/g. This makes it easier to obtain a desired D90 and also makes it easier to obtain aluminum hydroxide powder with a desired mass-based particle size distribution.

D50が10μm未満もしくは200μm超、および/または細孔累積容積が0.01mL/g未満もしくは1mL/g超であると、所望の成型密度が得にくくなる。 If D50 is less than 10 μm or more than 200 μm, and/or the cumulative pore volume is less than 0.01 mL/g or more than 1 mL/g, it will be difficult to obtain the desired molding density.

なお、細孔累積容積は以下のように求める。
水酸化アルミニウム粉末を120℃で4時間乾燥を行い、吸着水分を除去する。その後、精密天秤にて0.5~0.6g程度秤量し、直径15mm、高さ24mmの測定セルに充填する。この測定セルを自動ポロシメータ(例えば、Micromeritics社製、オートポアIII9420)にセットし、低圧側(1~10000psi)、高圧側(10000~60000psi)に分けて測定する。これらの測定データを合算し、細孔半径0.002μm以上100μm以下の領域における細孔容積分布を求め、細孔半径0.05μm以上1.0μm以下の領域における累積容積を算出する。
The cumulative pore volume is determined as follows.
The aluminum hydroxide powder is dried at 120°C for 4 hours to remove adsorbed moisture. Then, about 0.5 to 0.6 g is weighed out using a precision balance and filled into a measurement cell with a diameter of 15 mm and a height of 24 mm. This measurement cell is set in an automatic porosimeter (e.g., Autopore III9420, manufactured by Micromeritics), and measurements are performed separately on the low pressure side (1 to 10,000 psi) and the high pressure side (10,000 to 60,000 psi). These measurement data are added together to determine the pore volume distribution in the region of pore radius of 0.002 μm to 100 μm, and the cumulative volume in the region of pore radius of 0.05 μm to 1.0 μm is calculated.

原料水酸化アルミニウム粉末の結晶構造は例えばギブサイト型、バイヤライト型等であり、好ましくはギブサイト型である。 The crystal structure of the raw aluminum hydroxide powder may be, for example, gibbsite type or bayerite type, and is preferably gibbsite type.

原料水酸化アルミニウム粉末は、過飽和状態にあるアルミン酸ナトリウム溶液に種晶を添加し、攪拌しながら加水分解し、水酸化アルミニウムを析出させ、得られた水酸化アルミニウムをろ過洗浄し、乾燥する方法によって製造することができる。ここで、析出条件を適宜調整すること(及び/又は析出したものを一部溶解させること、及び/又は析出したものを粉砕または解砕すること)等により、上記粒子径および細孔累積容積を有する原料水酸化アルミニウム粉末が得られる。なお、上記粒子径および細孔累積容積を満たすものであれば、市販の水酸化アルミニウム粉末を用いてもよい。 The raw aluminum hydroxide powder can be produced by adding seed crystals to a supersaturated sodium aluminate solution, hydrolyzing with stirring to precipitate aluminum hydroxide, and filtering, washing, and drying the resulting aluminum hydroxide. Here, the raw aluminum hydroxide powder having the above particle size and cumulative pore volume can be obtained by appropriately adjusting the precipitation conditions (and/or partially dissolving the precipitate, and/or crushing or crushing the precipitate). Note that commercially available aluminum hydroxide powders may be used as long as they satisfy the above particle size and cumulative pore volume.

[(b)49.0~294.0MPaの圧力で粉砕する工程]
次に、上記原料水酸化アルミニウム粉末を49.0~294.0MPaの圧力で粉砕する。ここで「粉砕」とは、ある大きさの固体粒子(例えば一次粒子)に何らかのエネルギーを加えて、元の大きさよりも小さくする操作を意味する。
[(b) Crushing at a pressure of 49.0 to 294.0 MPa]
Next, the raw aluminum hydroxide powder is pulverized at a pressure of 49.0 to 294.0 MPa. Here, "pulverization" refers to an operation of applying some energy to solid particles of a certain size (e.g., primary particles) to make them smaller than their original size.

粉砕時の圧力が49.0MPa未満だと、所望の成型密度が得られない。好ましくは49.0MPa超であり、より好ましくは68.6MPa以上である。粉砕時の圧力の上限は特に制限されないが、生産性を考慮すると294.0MPa以下にしておくことが好ましい。 If the pressure during grinding is less than 49.0 MPa, the desired molding density cannot be obtained. It is preferably more than 49.0 MPa, and more preferably 68.6 MPa or more. There is no particular upper limit to the pressure during grinding, but considering productivity, it is preferable to keep it at 294.0 MPa or less.

上記圧力で粉砕する粉砕機としては、例えば、コニーダー、オンレーター、セルフクリーニング型捏和機、ギヤコンパウンダー、一軸式スクリュー型捏和機、二軸式スクリュー型捏和機等が挙げられる。当該装置は1種単独で用いてもよく、又は2種以上を組合せて用いてもよい。また、粉砕機は回分式、連続式のいずれの形式も適用できるが、単位重量当りの粉砕エネルギーを低減する観点からは連続式が好ましい。連続式粉砕機を使用するとき、粉砕機内の原料水酸化アルミニウムが必ずしも全体的に粉砕されている必要はなく、例えば原料水酸化アルミニウムの移送方向(軸方向)に順次粉砕度が高くなるようにすればよい。スクリュー型捏和機の場合、圧縮能力は例えばスクリューの形状、長さや回転数、ローター(原料をスクリューに移送する作用をする。)の回転数等により調節することができる。 Examples of mills that mill at the above pressure include co-kneaders, onlators, self-cleaning kneaders, gear compounders, single-shaft screw kneaders, and twin-shaft screw kneaders. These devices may be used alone or in combination of two or more. Either batch or continuous mills can be used, but continuous mills are preferred from the viewpoint of reducing the milling energy per unit weight. When using a continuous mill, it is not necessary for the raw aluminum hydroxide in the mill to be milled entirely, and it is sufficient to make the degree of milling gradually increase in the direction of transport (axial direction) of the raw aluminum hydroxide. In the case of a screw kneader, the compression capacity can be adjusted by, for example, the shape, length, and rotation speed of the screw, and the rotation speed of the rotor (which acts to transport the raw material to the screw).

粉砕機内には、固相として原料水酸化アルミニウム粉末が存在し、その他に、通常、気相として空気等、液相として水等が存在する。粉砕時における粉砕機内のそれらの状態が粉砕により得られる水酸化アルミニウム粉末の物性に影響を及ぼすことがあるので、粉砕は、固相、液相及び気相の充填形態が(i)固相及び気相が連続し液相が実質的に存在しないドライ(Dry)状態、(ii)固相及び気相が連続で液相が不連続なペンデュラー(Pendular)状態又は(iii)固相、気相及び液相が連続なファニキュラーI(Funicular I)状態で行われることが好ましい。このような充填形態は外観上、サラサラないしパサパサした混合系を構成している。 In the grinding mill, raw aluminum hydroxide powder is present as the solid phase, and in addition, air, etc. is usually present as the gas phase, and water, etc. is present as the liquid phase. Since the state of the inside of the grinding mill during grinding can affect the physical properties of the aluminum hydroxide powder obtained by grinding, grinding is preferably performed in a state where the solid, liquid, and gas phases are packed in (i) a dry state in which the solid and gas phases are continuous and the liquid phase is substantially absent, (ii) a pendular state in which the solid and gas phases are continuous and the liquid phase is discontinuous, or (iii) a funicular I state in which the solid, gas, and liquid phases are continuous. Such a packing form constitutes a mixture system that is smooth or dry in appearance.

粉砕は、粉砕時においてドライ状態、ペンデュラー状態又はファニキュラーI状態が達成されるように、原料水酸化アルミニウム粉末の含液率を粉砕前に調節してから行うことが好ましい。含液率の調節は、例えば、原料水酸化アルミニウム粉末を乾燥したり又は水、アルコール等の液体を添加したりして行えばよい。好ましい含液率は、原料水酸化アルミニウムの粒度分布等によって異なり一義的ではないが、例えば、30重量%以下、より好ましくは10重量%以下であり、また1重量%以上、より好ましくは5重量%以上である。含液率が高くなり過ぎると、原料水酸化アルミニウムを効率的に粉砕することは困難となる。 It is preferable to adjust the liquid content of the raw aluminum hydroxide powder before grinding so that a dry state, a pendular state, or a funicular I state is achieved during grinding. The liquid content can be adjusted, for example, by drying the raw aluminum hydroxide powder or adding a liquid such as water or alcohol. The preferred liquid content varies depending on the particle size distribution of the raw aluminum hydroxide and is not unambiguous, but is, for example, 30% by weight or less, more preferably 10% by weight or less, and 1% by weight or more, more preferably 5% by weight or more. If the liquid content is too high, it becomes difficult to grind the raw aluminum hydroxide efficiently.

粉砕時に水等の液体を添加したり、水等を含む原料水酸化アルミニウム粉末を粉砕したとき、粉砕後の水酸化アルミニウム粉末には、通常、乾燥が施される。乾燥は例えば、公知の乾燥機を使う方法、又は粉砕を連続式粉砕機で行うときにはこの粉砕機の一部を加熱する方法等によって行うことができる。 When liquid such as water is added during grinding, or when raw aluminum hydroxide powder containing water is ground, the aluminum hydroxide powder after grinding is usually dried. Drying can be performed, for example, by using a known dryer, or by heating part of a continuous grinder when grinding is performed with the grinder.

[(c)92m/秒以下の衝突速度で解砕する工程]
上記工程(b)後、92m/秒以下の衝突速度で解砕する。ここで「解砕」とは、細かい粒子が集まって一塊になっているもの(例えば二次粒子)を、ほぐして細かくする(例えば一次粒子にする)操作を意味する。
[(c) Crushing at a collision speed of 92 m/s or less]
After the step (b), the mixture is crushed at a collision speed of 92 m/s or less. Here, "crushing" refers to a process of breaking down agglomerates of fine particles (e.g., secondary particles) into smaller particles (e.g., primary particles).

解砕時の衝突速度が92m/秒超であると、所望の(002)/(110)回折強度比が得られない。例えば衝撃式の粉砕機等を用いることで、上記衝突速度で解砕することができる。 If the impact speed during crushing exceeds 92 m/sec, the desired (002)/(110) diffraction intensity ratio cannot be obtained. For example, by using an impact crusher, it is possible to crush at the above impact speed.

本発明の実施形態に係る水酸化アルミニウム粉末の製造方法は、本発明の目的が達成される範囲内で、他の工程(例えば表面処理工程等)を含んでいてもよい。 The method for producing aluminum hydroxide powder according to an embodiment of the present invention may include other steps (e.g., a surface treatment step, etc.) within the scope of achieving the object of the present invention.

以下、実施例を挙げて本発明の実施形態をより具体的に説明する。本発明の実施形態は以下の実施例によって制限を受けるものではなく、前述および後述する趣旨に合致し得る範囲で、適宜変更を加えて実施することも可能であり、それらはいずれも本発明の実施形態の技術的範囲に包含される。 The following provides a more detailed explanation of the embodiments of the present invention, using examples. The embodiments of the present invention are not limited to the following examples, and may be modified as appropriate within the scope of the intent described above and below, and all such modifications are within the technical scope of the embodiments of the present invention.

原料水酸化アルミニウム粉末(D50:81μm、細孔累積容積:0.09mL/g)を水分率5wt%に調整し、粉砕機(一軸スクリュー型捏和機)に連続的に投入して粉砕した。粉砕機の圧力は、投入速度を調節して196.0MPaとした。なお、粉砕機の圧力については、別途同じ原料水酸化アルミニウム粉末を冷間等方圧プレスにて圧縮粉砕してプレス圧とD90の関係を調査しておき、粉砕後の水酸化アルミニウム粉末のD90から粉砕機の圧力を簡易的に求めている。
得られた粉砕物を、120℃で乾燥し、衝撃粉砕機(自由粉砕機、奈良機械製)に投入して解砕し、実施例1の水酸化アルミニウム粉末を得た。衝撃粉砕機の衝突速度は、46m/秒とした。
また上記実施例1の製造方法から、以下の表1のように各条件を変更して、実施例2~4および比較例1~2の水酸化アルミニウム粉末を得た。さらに市販の水酸化アルミニウム粉末を比較例3(住友化学製、CW-308)、比較例4(住友化学製、C-305)、比較例5(住友化学製、CM-3080)とした。
The raw aluminum hydroxide powder (D50: 81 μm, pore cumulative volume: 0.09 mL/g) was adjusted to a moisture content of 5 wt % and continuously fed into a grinder (single-screw type kneader) for grinding. The grinder pressure was set to 196.0 MPa by adjusting the feeding speed. Regarding the grinder pressure, the same raw aluminum hydroxide powder was separately compressed and ground using a cold isostatic press to investigate the relationship between the pressing pressure and D90, and the grinder pressure was simply calculated from the D90 of the ground aluminum hydroxide powder.
The obtained pulverized product was dried at 120° C. and then charged into an impact pulverizer (Jiyuu pulverizer, manufactured by Nara Kikai) and pulverized to obtain the aluminum hydroxide powder of Example 1. The impact speed of the impact pulverizer was set to 46 m/sec.
Moreover, the various conditions were changed from the production method of Example 1 as shown in Table 1 below to obtain aluminum hydroxide powders of Examples 2 to 4 and Comparative Examples 1 and 2. Furthermore, commercially available aluminum hydroxide powders were set as Comparative Example 3 (manufactured by Sumitomo Chemical, CW-308), Comparative Example 4 (manufactured by Sumitomo Chemical, C-305), and Comparative Example 5 (manufactured by Sumitomo Chemical, CM-3080).

Figure 0007680899000001
Figure 0007680899000001

実施例1~4および比較例1~5の水酸化アルミニウム粉末に対し、以下の方法により、成型密度、(002)/(110)回折強度比、質量基準粒度分布(D50及びD90含む)、BET比表面積およびNaO含有量を求めた。 For the aluminum hydroxide powders of Examples 1 to 4 and Comparative Examples 1 to 5, the compact density, (002)/(110) diffraction intensity ratio, mass-based particle size distribution (including D50 and D90), BET specific surface area and Na 2 O content were determined by the following methods.

[成型密度]
水酸化アルミニウム粉末3.00gを内径20.0mmの円筒一軸成形用金型に入れ、万能材料試験機(エー・アンド・デイ(A&D)社製、TENSILON RTG-1310)を用い、当該水酸化アルミニウム粉末を圧縮速度1mm/分で10MPaの圧力になるまで圧縮充填し、重量/体積の比を成形密度とした。
[Molding density]
3.00 g of aluminum hydroxide powder was placed in a cylindrical uniaxial molding die having an inner diameter of 20.0 mm, and the aluminum hydroxide powder was compressed and packed at a compression speed of 1 mm/min to a pressure of 10 MPa using a universal material testing machine (TENSILON RTG-1310, manufactured by A&D Corporation), and the weight/volume ratio was defined as the molding density.

[(002)/(110)回折強度比]
水酸化アルミニウム粉末を測定用ガラスセルに圧密して充填した後、粉末X線回折測定装置(リガク社製、RINT-2000)を用いて、ステップ幅0.02deg、スキャンスピード0.04deg/sec、加速電圧40kV、加速電流30mAにてXRDパターンを測定した。X線源としてはCu-Kαを用いた。得られたXRDパターンにおいて、2θ=18.3°の位置に現れるピークを(002)面のピークとし、2θ=20.3°の位置に現れるピークを(110)面のピークとして、(110)面のピークの回折強度(ピーク高さ)に対する(002)面のピークの回折強度(ピーク高さ)の比を、(002)/(110)回折強度比とした。
[(002)/(110) diffraction intensity ratio]
The aluminum hydroxide powder was compacted and packed into a glass cell for measurement, and then the XRD pattern was measured using a powder X-ray diffraction measuring device (Rigaku Corporation, RINT-2000) with a step width of 0.02 deg, a scan speed of 0.04 deg/sec, an acceleration voltage of 40 kV, and an acceleration current of 30 mA. Cu-Kα was used as the X-ray source. In the obtained XRD pattern, the peak appearing at 2θ=18.3° was taken as the peak of the (002) plane, and the peak appearing at 2θ=20.3° was taken as the peak of the (110) plane, and the ratio of the diffraction intensity (peak height) of the peak of the (002) plane to the diffraction intensity (peak height) of the peak of the (110) plane was taken as the (002)/(110) diffraction intensity ratio.

[質量基準粒度分布(D50及びD90含む)]
水酸化アルミニウム粉末を0.2質量%ヘキサメタリン酸ナトリウム水溶液中に加え、出力25Wの超音波を120秒間照射して水酸化アルミニウム粉末を水溶液中に分散させたものに対して、レーザー散乱式粒子径分布測定装置を用いて質量基準粒度分布(D50およびD90含む)を求めた。該粒度分布は、粒子径0.02μm~2000μmの範囲を対数スケールで132分割し、各区間の粒子径を有する水酸化アルミニウムの質量を測定して求めた。レーザー散乱式粒子径分布測定装置としては、マイクロトラックMT-3300EXII(日機装社製)を使用した。また、粒度分布測定時において、水酸化アルミニウム粉末の濃度を上記測定装置の測定可能濃度に適宜調整した上で測定した。
[Mass-based particle size distribution (including D50 and D90)]
Aluminum hydroxide powder was added to a 0.2% by mass aqueous solution of sodium hexametaphosphate, and ultrasonic waves of 25 W were applied for 120 seconds to disperse the aluminum hydroxide powder in the aqueous solution. The mass-based particle size distribution (including D50 and D90) of the dispersion was determined using a laser scattering particle size distribution analyzer. The particle size distribution was determined by dividing the particle size range of 0.02 μm to 2000 μm into 132 ranges on a logarithmic scale and measuring the mass of aluminum hydroxide having a particle size in each range. As the laser scattering particle size distribution analyzer, a Microtrac MT-3300EXII (manufactured by Nikkiso Co., Ltd.) was used. In addition, when measuring the particle size distribution, the concentration of the aluminum hydroxide powder was appropriately adjusted to a concentration measurable by the above-mentioned measuring device before measurement.

[BET比表面積]
JIS-Z-8830:2013に規定された方法に従って、全自動比表面積測定装置(Mountech社製、Macsorb HM-1201)を用いて窒素吸着法によりBET比表面積を求めた。
[BET specific surface area]
According to the method specified in JIS-Z-8830:2013, the BET specific surface area was determined by the nitrogen adsorption method using a fully automatic specific surface area measuring device (Macsorb HM-1201, manufactured by Mountech).

[NaO含有量]
水酸化アルミニウム粉末を無機酸の水溶液に溶解させて水溶液を調製した後、ICP発光分光分析装置を用いてNaO含有量を求めた。具体的には、ナトリウムの波長(589.592nm)の強度を測定し、NaOに換算して、NaOの質量を算出し、溶解させた水酸化アルミニウム粉末の質量に対する該NaOの質量の比を、NaO含有量(質量%)とした。
[Na 2 O content]
After preparing an aqueous solution by dissolving aluminum hydroxide powder in an aqueous solution of an inorganic acid, the Na 2 O content was determined using an ICP atomic emission spectrometer. Specifically, the intensity of the wavelength of sodium (589.592 nm) was measured and converted into Na 2 O to calculate the mass of Na 2 O, and the ratio of the mass of the Na 2 O to the mass of the dissolved aluminum hydroxide powder was defined as the Na 2 O content (mass%).

さらに以下の方法で樹脂粘度を求めた。
水酸化アルミニウム粉末5.59質量部とビスフェノールA型エポキシ樹脂混合物(AQ010-8140、常温硬化樹脂 53型主剤)1.86質量部を遊星式撹拌機(シンキー社製、あわとり練太郎ARV-310)を用いて1000rpmで3分間混合し、コンパウンドを得た。動的粘弾性測定装置(Rheosol-G3000)に直径30mmパラレルプレートを装着し、ここへ上記コンパウンドをセットした。パラレルプレートのギャップを0.50mm、温度100℃の条件にて10分間静置した後に、せん断速度40s-1における樹脂粘度を測定した。
結果を以下の表2にまとめる。なお、表2において、「第2のピーク」の欄の「-」は、第2のピークが存在しなかったことを意味する。
Furthermore, the resin viscosity was determined by the following method.
5.59 parts by mass of aluminum hydroxide powder and 1.86 parts by mass of bisphenol A type epoxy resin mixture (AQ010-8140, room temperature curing resin 53 type base agent) were mixed at 1000 rpm for 3 minutes using a planetary mixer (Thinky Corporation, Awatori Rentaro ARV-310) to obtain a compound. A 30 mm diameter parallel plate was attached to a dynamic viscoelasticity measuring device (Rheosol-G3000), and the compound was set on it. After leaving it for 10 minutes under the conditions of a parallel plate gap of 0.50 mm and a temperature of 100°C, the resin viscosity at a shear rate of 40 s -1 was measured.
The results are summarized in the following Table 2. In Table 2, "-" in the "second peak" column means that the second peak was not present.

Figure 0007680899000002
Figure 0007680899000002

表2の結果より、次のように考察できる。表2の実施例1~4は、いずれも本発明の実施形態で規定する要件の全てを満足する例であり、樹脂粘度が10Pa・s以下であって樹脂粘度の上昇を十分に抑制できた。そのうち、実施例1~3は、D90が100μm未満であるため、樹脂成形体に充填したときの外観不良を十分に抑制することができ、また樹脂成形体の強度を十分に確保しやすい点で、好ましい例であった。実施例4は、原料水酸化アルミニウム粉末の細孔累積容積が0.02mL/g未満であったため、D90が100μm以上となった。
一方、比較例1~5は、本発明の実施形態で規定する要件を満たしていない例であり、樹脂粘度が10Pa・s超であって樹脂粘度の上昇を十分に抑制できなかった。
From the results in Table 2, the following can be considered. All of Examples 1 to 4 in Table 2 are examples that satisfy all of the requirements stipulated in the embodiments of the present invention, and the resin viscosity was 10 Pa·s or less, so that an increase in the resin viscosity could be sufficiently suppressed. Of these, Examples 1 to 3 were preferable examples in that they had a D90 of less than 100 μm, so that poor appearance when filled into a resin molded body could be sufficiently suppressed and the strength of the resin molded body could be easily ensured. In Example 4, the cumulative pore volume of the raw aluminum hydroxide powder was less than 0.02 mL/g, so that D90 was 100 μm or more.
On the other hand, Comparative Examples 1 to 5 are examples that do not satisfy the requirements defined in the embodiment of the present invention, and the resin viscosity exceeded 10 Pa·s, so that the increase in the resin viscosity could not be sufficiently suppressed.

比較例1は、解砕時の衝突速度が92m/秒超であったため、(002)/(110)回折強度比が7.5超となり、樹脂粘度が10Pa・s超となった。 In Comparative Example 1, the impact speed during disintegration was greater than 92 m/s, so the (002)/(110) diffraction intensity ratio was greater than 7.5 and the resin viscosity was greater than 10 Pa·s.

比較例2は、粉砕時の圧力が49.0MPa未満であったため、成型密度が1.59g/cm未満となり、樹脂粘度が10Pa・s超となった。 In Comparative Example 2, the pressure during crushing was less than 49.0 MPa, so the molding density was less than 1.59 g/cm 3 and the resin viscosity exceeded 10 Pa·s.

比較例3および4は、成型密度が1.59g/cm未満であったため、樹脂粘度が10Pa・s超となった。 In Comparative Examples 3 and 4, the molded density was less than 1.59 g/cm 3 , and therefore the resin viscosity exceeded 10 Pa·s.

比較例5は、(002)/(110)回折強度比が7.5超であったため、樹脂粘度が10Pa・s超となった。 In Comparative Example 5, the (002)/(110) diffraction intensity ratio was greater than 7.5, and the resin viscosity was greater than 10 Pa·s.

Claims (4)

10MPaで成型したときの密度が1.59~2.00g/cmであり、
XRDパターンにおける(110)面の回折強度に対する(002)面の回折強度の比が、2.0~7.5であ
50質量%粒子径(D50)が33μm以下であり、
BET比表面積が2.0m /g以下であり、
質量基準粒度分布において1~200μmの粒径範囲に1つ又は2つのピークを有し、
前記質量基準粒度分布において、1μm未満に、ピークを有さないか、頻度が0質量%超0.5質量%以下である1つ以上のピークを有する、水酸化アルミニウム粉末。
The density when molded at 10 MPa is 1.59 to 2.00 g/ cm3 ,
the ratio of the diffraction intensity of the (002) plane to the diffraction intensity of the (110) plane in the XRD pattern is 2.0 to 7.5;
The 50% by mass particle size (D50) is 33 μm or less,
The BET specific surface area is 2.0 m 2 /g or less;
The mass standard particle size distribution has one or two peaks in the particle size range of 1 to 200 μm,
The aluminum hydroxide powder has no peak or one or more peaks having a frequency of more than 0 mass% and not more than 0.5 mass% below 1 μm in the mass-based particle size distribution .
90質量%粒子径(D90)が100μm未満である、請求項1に記載の水酸化アルミニウム粉末。 The aluminum hydroxide powder according to claim 1, having a 90% by mass particle size (D90) of less than 100 μm. 前記質量基準粒度分布において1~200μmの粒径範囲に1つのピークを有する場合は、該ピークの頻度が4.0質量%以上であり、
前記質量基準粒度分布において1~200μmの粒径範囲に2つのピークを有する場合は、一方のピークの頻度が4.0質量%以上であり、他方のピークの頻度が0質量%超4.0質量%以下である、請求項1または2に記載の水酸化アルミニウム粉末。
When the mass-based particle size distribution has one peak in the particle size range of 1 to 200 μm , the frequency of the peak is 4.0 mass% or more,
3. The aluminum hydroxide powder according to claim 1, wherein, when the mass-based particle size distribution has two peaks in the particle size range of 1 to 200 μm , the frequency of one peak is 4.0 mass% or more, and the frequency of the other peak is more than 0 mass% and 4.0 mass% or less.
50質量%粒子径(D50)が10~200μmであり、且つ半径0.05~1μmの細孔の累積容積が0.01~1mL/gである水酸化アルミニウム粉末を、49.0~294.0MPaの圧力で粉砕した後、92m/秒以下の衝突速度で解砕することを含む、水酸化アルミニウム粉末の製造方法。 A method for producing aluminum hydroxide powder, comprising crushing aluminum hydroxide powder having a 50% by mass particle size (D50) of 10 to 200 μm and a cumulative volume of pores with a radius of 0.05 to 1 μm of 0.01 to 1 mL/g at a pressure of 49.0 to 294.0 MPa, and then disintegrating the powder at a collision speed of 92 m/sec or less.
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