WO2018193684A1 - Method for producing inorganic flakes and inorganic flakes - Google Patents
Method for producing inorganic flakes and inorganic flakes Download PDFInfo
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- WO2018193684A1 WO2018193684A1 PCT/JP2018/003031 JP2018003031W WO2018193684A1 WO 2018193684 A1 WO2018193684 A1 WO 2018193684A1 JP 2018003031 W JP2018003031 W JP 2018003031W WO 2018193684 A1 WO2018193684 A1 WO 2018193684A1
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/005—Manufacture of flakes
Definitions
- the present invention relates to a method for producing inorganic flakes and inorganic flakes.
- Patent Document 1 discloses that the glitter of effect pigments generated from synthetic flake substrates such as glass flakes is reduced by reducing the amount of substrate particles having a particle size of less than 9 microns and substrate particles having a particle size of more than 85 microns. Techniques to improve are described. Patent Document 1 describes that the required particle size and particle size distribution are obtained by classifying flakes through a screen. “Glass flake” is a registered trademark of Nippon Sheet Glass Co., Ltd.
- Patent Document 2 describes an effect pigment containing an artificial base material such as a glass plate or a synthetic mica plate and having a predetermined volume average cumulative sieving distribution curve.
- the predetermined volume average cumulative sieving distribution curve is realized by performing classification operation on the artificial base material.
- Patent Document 3 describes an effect pigment based on a flaky substrate such as synthetic mica flakes.
- the flaky substrate has a circular coefficient of 1.2-2.
- the flaky substrate is coated with a high refractive index layer having a refractive index of 1.8 or more.
- Patent Document 4 describes a method for producing edgeless glass particles by passing preheated crushed glass particles through a cooling zone having a predetermined width and then passing through the cooling air.
- Patent Document 5 describes a crushed glass particle rounding device including a heating device that is heated to a predetermined temperature equal to or higher than the glass softening temperature of the crushed glass particles.
- Patent Document 6 describes silica in which corners generated when the raw stone is crushed are rounded by heat treatment.
- Patent Document 7 discloses a flaky glass having an edge portion with a corner that wears the edge portion of the flaky glass while simultaneously pulverizing the flaky glass by using an apparatus such as a jet mill. A manufacturing method is described.
- Patent Documents 1 and 2 effect pigments having a predetermined particle size distribution are manufactured by classification.
- Patent Documents 1 to 3 do not describe or suggest that the raw material is heated to the softening temperature or higher before classification.
- the crushed glass particles are heated to the softening temperature or higher, but the crushed glass particles such as cullet are the objects of processing, and the flaky glass particles are the objects of processing. Do not mean.
- silica generated when the raw stone is pulverized is a target of processing
- flaky silica is not a target of processing.
- Patent Documents 7 and 8 are intended to treat flaky glass, there is no description or suggestion that the flaky glass is heated to the softening temperature or higher.
- Patent Documents 1 to 8 do not describe or suggest an appropriate classification operation for a powder obtained by heating a powder containing flaky particles made of an inorganic material to a temperature higher than the softening temperature of the inorganic material.
- the present invention provides a new method for producing inorganic flakes having a narrow particle size distribution by appropriately classifying powder obtained by heating a powder containing flaky particles made of an inorganic substance to a temperature higher than the softening temperature of the inorganic substance.
- the present invention provides an inorganic flake having a narrow particle size distribution, containing a large number of flaky particles having rounded ends.
- the present invention Heating the first powder containing the first flaky particles made of an inorganic material so that the surface temperature of the first flaky particles is higher than the softening temperature of the inorganic material, And preparing a second powder containing spherical particles having a particle size smaller than the particle size of the second flaky particles, The second powder together with running water is passed through a sieve having an opening larger than the particle diameter of the spherical particles to remove the spherical particles, A method for producing inorganic flakes is provided.
- FIG. 1 is a graph showing a volume-based particle size distribution of raw material powders of Examples and Comparative Examples.
- FIG. 2 is a graph showing the volume-based particle size distribution of the intermediate powders of Examples and Comparative Examples.
- FIG. 3 is a graph showing the volume-based particle size distribution of the inorganic flakes according to the example.
- FIG. 4 is a graph showing the volume-based particle size distribution of the final powder according to the comparative example.
- FIG. 5 is a scanning electron microscope (SEM) photograph of the intermediate powder.
- FIG. 6 is an SEM photograph of the intermediate powder.
- FIG. 7 is an SEM photograph of inorganic flakes according to the example.
- FIG. 8 is an SEM photograph of inorganic flakes according to the example.
- FIG. 9 is an SEM photograph of powder according to a comparative example.
- FIG. 10 is an SEM photograph of the raw material powder.
- the present inventor manufactures inorganic flakes having a narrow particle size distribution and containing a large number of flake-like particles having rounded ends from a raw material which is a powder containing flake-like particles made of an inorganic substance.
- the method was examined day and night. As a result, when the present inventors heated the powder as the raw material so that the temperature of the surface of the flaky particles is higher than the softening temperature of the inorganic substance, the relatively small particles contained in the powder as the raw material It has been newly found that particles having a diameter become spherical particles.
- spherical particles mean particles having a ratio of the maximum diameter Dx to the minimum diameter Di (Dx / Di) of 1.5 or less when observed with an SEM.
- the surface of the first flaky particles becomes higher than the softening temperature of the inorganic substance, and the end portions of the first flaky particles are softened.
- the second flaky particles have rounded ends.
- the whole of the particles having a relatively small particle diameter contained in the first powder is easily softened by heating the first powder.
- the whole softened particles are likely to become spherical particles due to surface tension.
- the second powder contains spherical particles in addition to the second flaky particles. Due to the interaction between the spherical particles or the interaction between the spherical particles and the second flaky particles, it is considered that the spherical particles are hardly removed even if the second powder is simply sieved.
- inorganic flakes contain 50% or more of flaky particles having rounded ends on a number basis. Thereby, inorganic flakes have a good tactile sensation.
- the particle diameter corresponding to the cumulative distribution of 10% in the volume-based particle diameter distribution of the first powder, the median diameter, and the particle diameter corresponding to the cumulative distribution of 90% are d1 (10), d1 (50), and d1 ( 90).
- the particle diameter corresponding to 10% of the cumulative distribution in the volume-based particle size distribution of the inorganic flakes, the median diameter, and the particle diameter corresponding to the cumulative distribution of 90% are d2 (10), d2 (50), and d2 ( 90).
- the volume-based particle size distribution of the first powder and inorganic flakes can be measured by, for example, a laser diffraction particle size distribution measuring device. For example, the following relationship is satisfied in the first powder and the inorganic flakes.
- the inorganic flakes produced by the method of the present invention have a narrow particle size distribution compared to the first powder.
- the volume-based particle size distribution of the inorganic flakes is, for example, 1.1 ⁇ d2 (90) / d2 (10) ⁇ 20 and 0.1 ⁇ ⁇ d2 (90) ⁇ d2 (10) ⁇ / d2 (50) ⁇ .
- the relationship of 7 is further satisfied.
- the thickness of the inorganic flake is, for example, 0.2 ⁇ m to 1000 ⁇ m.
- the heating condition of the first powder in the step (i) is such that the end is softened while the overall shape of the first flaky particles having a relatively large particle diameter is maintained. It has been established.
- the heating condition of the first powder in the step (i) is included in the first powder so that the second powder includes spherical particles having a predetermined particle diameter (for example, 100 ⁇ m or less). It is determined so that the whole particles having a relatively small particle size can be softened.
- the conditions for heating the first powder in the step (i) are determined so that the surface temperature of the first flaky particles is 50 ° C. to 250 ° C. higher than the softening temperature of the inorganic substance. .
- the heating of the first powder in the step (i) is performed, for example, by passing the first powder through a flame formed by a burner.
- the flame is formed in the horizontal direction, and the first powder is dropped so as to pass through the flame.
- the first powder is preheated to a predetermined temperature lower than the softening temperature of the inorganic substance.
- the first powder is preheated to a temperature that is 20 ° C. to 100 ° C. lower than the softening temperature of the inorganic substance.
- the first powder can be preheated by bringing the first powder into contact with air heated by a flame formed by a burner.
- the heated first powder is rapidly cooled by cooling air after the first powder is heated.
- the rapid cooling of the first powder is performed, for example, by sending cooling air (outside air) by a blower into a space in which the first powder that has passed through the flame moves.
- the inorganic substance forming the first flaky particles is not limited to a specific inorganic substance as long as it is an inorganic substance that softens at a predetermined temperature, but is, for example, glass or mineral.
- the mineral forming the first flaky particles is, for example, mica or talc.
- the particles having a relatively small particle size contained in the first powder tend to be spherical particles.
- the second powder contains, for example, 1% to 49% of spherical particles based on the number. Moreover, the particle diameter of the spherical particles contained in the second powder is, for example, 100 ⁇ m or less.
- the sieve used in the step (ii) has an opening larger than the particle diameter of the spherical particles.
- the sieve desirably has an opening smaller than the particle size of most of the second flaky particles contained in the second powder.
- the opening of the sieve is, for example, 2 ⁇ m to 1000 ⁇ m.
- the inorganic flakes according to the present invention can be obtained by collecting the powder that has not passed through the sieve.
- the water adhering to the inorganic flakes is removed by a natural drying process or a drying process in a drying furnace.
- the inorganic flakes may be given a predetermined coating.
- the inorganic flakes according to the present invention exhibit a good tactile sensation because most of the second flaky particles have round ends.
- the inorganic flakes according to the present invention have, for example, a static friction coefficient of 0.9 or less and a dynamic friction coefficient of 0.7 or less on a friction surface formed by attaching inorganic flakes to the adhesive surface of a fixed adhesive tape. Or one.
- Raw material powder (manufactured by Nippon Sheet Glass Co., Ltd., product name: glass flake MTD160FY) was prepared.
- the average thickness of the flaky particles contained in the raw material powder is 0.4 ⁇ m
- the true density of the raw material powder is 2.7 g / cm 3
- the bulk density of the raw material powder is 0.03 g / cm 3 . there were.
- the softening temperature Ts of the glass forming the raw material powder was 870 ° C. to 880 ° C.
- the glass transition temperature Tg of the glass forming the raw material powder was about 700 ° C.
- the volume-based particle size distribution of the raw material powder was measured using a laser diffraction particle size distribution measuring device (manufactured by Nikkiso Co., Ltd., product name: Microtrack MT3500). The results are shown in FIG. An SEM photograph of the raw material powder is shown in FIG. As shown in FIG. 10, the raw material powder had sharp edges.
- the intermediate powder contained flaky particles and spherical particles.
- the intermediate powder contained about 20% spherical particles on a number basis.
- the particle size distribution of the intermediate powder includes a particle size distribution having a single peak at a relatively large particle size and a particle size having a single peak at a relatively small particle size. It had a distribution that overlapped with the distribution. It is considered that the particle size distribution of the intermediate powder reflects a state in which flaky particles having a relatively large particle size and spherical particles having a relatively small particle size are mixed.
- most of the flaky particles of the intermediate powder had rounded ends. Of the flaky particles of the intermediate powder, about 90% or more of the flaky particles on the number basis had rounded ends.
- the intermediate powder was stirred in water for 30 minutes at room temperature. Thereafter, the intermediate powder was passed through a sieve having an opening of 106 ⁇ m while flowing tap water. During this period, the sieve was moved back and forth several times in the horizontal direction. The flow rate of tap water was 10 cm 3 / sec.
- the powder remaining on the sieve was dried at 100 ° C. for 30 minutes in a drying furnace to obtain inorganic flakes according to the example.
- the volume-based particle size distribution of the inorganic flakes according to the example was measured using a laser diffraction particle size distribution measuring device (manufactured by Nikkiso Co., Ltd., product name: Microtrack MT3500). The results are shown in FIG. As shown in FIG. 3 and Table 1, it was suggested that the inorganic flakes according to the examples have a narrow particle size distribution. SEM photographs of the inorganic flakes are shown in FIGS. As shown in FIG. 7, the inorganic flakes contained almost no spherical particles, suggesting that the spherical particles in the intermediate powder were almost removed. As shown in FIG. 8, many of the particles of inorganic flakes had rounded ends.
- the inorganic flakes according to the examples have smaller values of D90 / D10 and smaller values of (D90-D10) / D50 and narrower particles compared to the powders of the comparative examples. It had a diameter distribution. It is possible to produce inorganic flakes having a narrow particle size distribution by changing particles having a relatively small particle size in the raw material powder into spherical particles by heat treatment and selecting an appropriate classification operation for removing the spherical particles. It was suggested.
- Flakes (D10: 64 ⁇ m, D50: 149 ⁇ m, D90: 262 ⁇ m) according to a comparative example made of flaky particles not subjected to heat treatment and having rounded (angular) ends were prepared.
- the static friction coefficient and the dynamic friction coefficient of the adhesive surface of the double-sided tape to which the flakes according to the comparative example adhered were measured in the same manner except that the flakes according to the comparative example were used instead of the inorganic flakes according to the examples. The results are shown in Table 2.
- the adhesive surface of the double-sided tape to which the inorganic flakes according to the examples adhered had a lower static friction coefficient and a lower dynamic friction coefficient than the adhesive surface of the double-sided tape to which the flakes according to the comparative example adhered. For this reason, it was suggested that the inorganic flakes according to the examples can impart a good tactile sensation.
Abstract
The method according to the present invention involves heating a first powder and producing a second powder. The first powder comprises first flake-like particles made from an inorganic substance. The first powder is heated such that the temperature of the surface of the first flake-like particles is higher than the softening temperature of the inorganic substance. The second powder comprises second flake-like particles and spherical particles. The spherical particles have a particle size that is smaller than the particle size of the second flake-like particles. The second powder is sieved together with running water with a sieve having a mesh size that is greater than the particle size of the spherical particles to remove the spherical particles so as to produce the inorganic flakes.
Description
本発明は、無機物フレークを製造する方法及び無機物フレークに関する。
The present invention relates to a method for producing inorganic flakes and inorganic flakes.
従来、効果顔料として使用される、ガラス又は鉱物等の無機物でできたフレークが知られている。
Conventionally, flakes made of an inorganic material such as glass or mineral, which are used as effect pigments, are known.
例えば、特許文献１には、ガラスフレークなどの合成小片基質から生成される効果顔料が示すきらめきを、９ミクロン未満の粒度の基質粒子及び８５ミクロンを超える粒度の基質粒子の量を少なくすることで向上させる技術が記載されている。特許文献１には、スクリーンを通してフレークを分級することにより、必要な粒度及び粒度分布を得ることが記載されている。なお、「ガラスフレーク」は、日本板硝子株式会社の登録商標である。
For example, Patent Document 1 discloses that the glitter of effect pigments generated from synthetic flake substrates such as glass flakes is reduced by reducing the amount of substrate particles having a particle size of less than 9 microns and substrate particles having a particle size of more than 85 microns. Techniques to improve are described. Patent Document 1 describes that the required particle size and particle size distribution are obtained by classifying flakes through a screen. “Glass flake” is a registered trademark of Nippon Sheet Glass Co., Ltd.
特許文献２には、ガラス微小板又は合成マイカの微小板などの人工基材を含む効果顔料であって、所定の体積平均累積篩下分布曲線を有する効果顔料が記載されている。所定の体積平均累積篩下分布曲線は、人工基材について分級の操作を行うことによって実現されている。
Patent Document 2 describes an effect pigment containing an artificial base material such as a glass plate or a synthetic mica plate and having a predetermined volume average cumulative sieving distribution curve. The predetermined volume average cumulative sieving distribution curve is realized by performing classification operation on the artificial base material.
特許文献３には、合成雲母フレーク等のフレーク状基材に基づく効果顔料が記載されている。フレーク状基材は１．２～２の円形係数を有する。フレーク状基材は、１．８以上の屈折率を有する高屈折率層によってコーティングされている。
Patent Document 3 describes an effect pigment based on a flaky substrate such as synthetic mica flakes. The flaky substrate has a circular coefficient of 1.2-2. The flaky substrate is coated with a high refractive index layer having a refractive index of 1.8 or more.
また、ガラス粒子等の無機物でできた粒子のエッジ部分を丸くする技術も知られている。例えば、特許文献４には、予熱した破砕ガラス粒子を所定の幅の火炎帯を通過させた後に冷却用空気中を通過させることにより、無エッジガラス粒子を製造する方法が記載されている。
Also known is a technique for rounding the edge portion of particles made of inorganic materials such as glass particles. For example, Patent Document 4 describes a method for producing edgeless glass particles by passing preheated crushed glass particles through a cooling zone having a predetermined width and then passing through the cooling air.
特許文献５には、破砕ガラス粒子のガラス軟化温度以上の所定の温度に昇温される加熱装置を備えた破砕ガラス粒子の丸め装置が記載されている。
Patent Document 5 describes a crushed glass particle rounding device including a heating device that is heated to a predetermined temperature equal to or higher than the glass softening temperature of the crushed glass particles.
特許文献６には、原石を粉砕する際に生じた角（かど）を加熱処理で丸くしたシリカが記載されている。
Patent Document 6 describes silica in which corners generated when the raw stone is crushed are rounded by heat treatment.
特許文献７には、ジェットミル等の装置を用いてフレーク状ガラスに衝撃を与えてフレーク状ガラスを粉砕すると同時にフレーク状ガラスのエッジ部を摩耗させる、エッジ部の角の取れたフレーク状ガラスの製造方法が記載されている。
Patent Document 7 discloses a flaky glass having an edge portion with a corner that wears the edge portion of the flaky glass while simultaneously pulverizing the flaky glass by using an apparatus such as a jet mill. A manufacturing method is described.
特許文献８には、フレーク状ガラスを、ガラスを腐食可能な液体で処理することを含む、エッジ部の角の取れたフレーク状ガラスの製造方法が記載されている。
Patent Document 8 describes a method for producing flaky glass having a corner with a corner that includes treating flaky glass with a liquid that can corrode the glass.
特許文献１及び２の記載によれば、分級を行って所定の粒度分布を有する効果顔料が製造されている。しかし、特許文献１～３には、分級の前に原料を軟化温度以上に加熱することは記載も示唆もされていない。特許文献４及び５の技術によれば、破砕ガラス粒子が軟化温度以上に加熱されてはいるが、カレット等の破砕ガラス粒子が処理の対象であり、フレーク状のガラス粒子が処理の対象であるわけではない。特許文献６に記載の技術によれば、原石を粉砕する際に生じたシリカが処理の対象であり、フレーク状のシリカが処理の対象であるわけではない。特許文献７及び８に記載の技術は、フレーク状ガラスを処理対象とはしているが、フレーク状ガラスを軟化温度以上に加熱することは記載も示唆もされていない。
According to the description in Patent Documents 1 and 2, effect pigments having a predetermined particle size distribution are manufactured by classification. However, Patent Documents 1 to 3 do not describe or suggest that the raw material is heated to the softening temperature or higher before classification. According to the techniques of Patent Documents 4 and 5, the crushed glass particles are heated to the softening temperature or higher, but the crushed glass particles such as cullet are the objects of processing, and the flaky glass particles are the objects of processing. Do not mean. According to the technique described in Patent Document 6, silica generated when the raw stone is pulverized is a target of processing, and flaky silica is not a target of processing. Although the techniques described in Patent Documents 7 and 8 are intended to treat flaky glass, there is no description or suggestion that the flaky glass is heated to the softening temperature or higher.
上記の通り、特許文献１～８には、無機物できたフレーク状粒子を含む粉体を無機物の軟化温度以上に加熱して得られた粉体にとって適切な分級操作について記載も示唆もされていない。そこで、本発明は、無機物でできたフレーク状粒子を含む粉体を無機物の軟化温度以上に加熱して得られた粉体を適切に分級して粒子径分布の狭い無機物フレークを製造できる新たな方法を提供する。また、本発明は、丸みを持った端部を有するフレーク状粒子を多く含み、狭い粒子径分布を有する無機物フレークを提供する。
As described above, Patent Documents 1 to 8 do not describe or suggest an appropriate classification operation for a powder obtained by heating a powder containing flaky particles made of an inorganic material to a temperature higher than the softening temperature of the inorganic material. . Accordingly, the present invention provides a new method for producing inorganic flakes having a narrow particle size distribution by appropriately classifying powder obtained by heating a powder containing flaky particles made of an inorganic substance to a temperature higher than the softening temperature of the inorganic substance. Provide a method. In addition, the present invention provides an inorganic flake having a narrow particle size distribution, containing a large number of flaky particles having rounded ends.
本発明は、
無機物でできた第一フレーク状粒子を含有する第一粉体を前記第一フレーク状粒子の表面の温度が前記無機物の軟化温度よりも高い温度になるように加熱して、第二フレーク状粒子及び前記第二フレーク状粒子の粒子径よりも小さい粒子径を有する球状粒子を含有する第二粉体を作製し、
流水とともに前記第二粉体を前記球状粒子の粒子径よりも大きい目開きを有する篩にかけて前記球状粒子を除去して、
無機物フレークを製造する方法を提供する。 The present invention
Heating the first powder containing the first flaky particles made of an inorganic material so that the surface temperature of the first flaky particles is higher than the softening temperature of the inorganic material, And preparing a second powder containing spherical particles having a particle size smaller than the particle size of the second flaky particles,
The second powder together with running water is passed through a sieve having an opening larger than the particle diameter of the spherical particles to remove the spherical particles,
A method for producing inorganic flakes is provided.
無機物でできた第一フレーク状粒子を含有する第一粉体を前記第一フレーク状粒子の表面の温度が前記無機物の軟化温度よりも高い温度になるように加熱して、第二フレーク状粒子及び前記第二フレーク状粒子の粒子径よりも小さい粒子径を有する球状粒子を含有する第二粉体を作製し、
流水とともに前記第二粉体を前記球状粒子の粒子径よりも大きい目開きを有する篩にかけて前記球状粒子を除去して、
無機物フレークを製造する方法を提供する。 The present invention
Heating the first powder containing the first flaky particles made of an inorganic material so that the surface temperature of the first flaky particles is higher than the softening temperature of the inorganic material, And preparing a second powder containing spherical particles having a particle size smaller than the particle size of the second flaky particles,
The second powder together with running water is passed through a sieve having an opening larger than the particle diameter of the spherical particles to remove the spherical particles,
A method for producing inorganic flakes is provided.
また、本発明は、
無機物フレークであって、
丸みを持った端部を有するフレーク状粒子を個数基準で５０％以上含有し、
当該無機物フレークの体積基準の粒子径分布における累積分布１０％に相当する粒子径、メジアン径、及び累積分布９０％に相当する粒子径をそれぞれｄ２（１０）、ｄ２（５０）、及びｄ２（９０）と表したときに、
１０μｍ≦ｄ２（５０）≦１０００μｍ、
１．１≦ｄ２（９０）／ｄ２（１０）≦２０、及び
０．１≦｛ｄ２（９０）－ｄ２（１０）｝／ｄ２（５０）≦７の関係を満たす、
無機物フレークを提供する。 The present invention also provides:
Inorganic flakes,
Containing 50% or more of flaky particles having rounded ends on a number basis;
In the volume-based particle size distribution of the inorganic flakes, the particle size corresponding to 10% cumulative distribution, the median size, and the particle size corresponding to 90% cumulative distribution are d2 (10), d2 (50), and d2 (90 )
10 μm ≦ d2 (50) ≦ 1000 μm,
1.1 ≦ d2 (90) / d2 (10) ≦ 20 and 0.1 ≦ {d2 (90) −d2 (10)} / d2 (50) ≦ 7 are satisfied.
Provide inorganic flakes.
無機物フレークであって、
丸みを持った端部を有するフレーク状粒子を個数基準で５０％以上含有し、
当該無機物フレークの体積基準の粒子径分布における累積分布１０％に相当する粒子径、メジアン径、及び累積分布９０％に相当する粒子径をそれぞれｄ２（１０）、ｄ２（５０）、及びｄ２（９０）と表したときに、
１０μｍ≦ｄ２（５０）≦１０００μｍ、
１．１≦ｄ２（９０）／ｄ２（１０）≦２０、及び
０．１≦｛ｄ２（９０）－ｄ２（１０）｝／ｄ２（５０）≦７の関係を満たす、
無機物フレークを提供する。 The present invention also provides:
Inorganic flakes,
Containing 50% or more of flaky particles having rounded ends on a number basis;
In the volume-based particle size distribution of the inorganic flakes, the particle size corresponding to 10% cumulative distribution, the median size, and the particle size corresponding to 90% cumulative distribution are d2 (10), d2 (50), and d2 (90 )
10 μm ≦ d2 (50) ≦ 1000 μm,
1.1 ≦ d2 (90) / d2 (10) ≦ 20 and 0.1 ≦ {d2 (90) −d2 (10)} / d2 (50) ≦ 7 are satisfied.
Provide inorganic flakes.
上記の方法によれば、丸みを持った端部を有するフレーク状粒子を多く含み、狭い粒子径分布を有する無機物フレークを製造できる。
According to the above method, it is possible to produce inorganic flakes having a narrow particle size distribution including many flaky particles having rounded ends.
以下、本発明の実施形態について説明する。なお、以下の説明は、本発明の一例に関するものであり、本発明はこれらによって限定されるものではない。
Hereinafter, embodiments of the present invention will be described. The following description relates to an example of the present invention, and the present invention is not limited to these.
本発明者は、無機物でできたフレーク状粒子を含有する粉体である原料から、丸みを持った端部を有するフレーク状粒子を多く含み、かつ、狭い粒子径分布を有する無機物フレークを製造する方法について日夜検討を行った。その結果、本発明者は、原料である粉体をフレーク状粒子の表面の温度が無機物の軟化温度よりも高い温度になるように加熱すると、原料である粉体に含有される比較的小さい粒子径の粒子が球状粒子になることを新たに見出した。狭い粒子径分布を有する無機物フレークを製造する観点から、このような球状粒子を除去するために球状粒子を含有する粉体を球状粒子の粒子径よりも大きい目開きを有する篩にかけることが考えられる。しかし、発明者は、球状粒子を含有する粉体を単にそのような篩にかけても球状粒子を適切に除去できないことを新たに見出した。そこで、本発明者は、球状粒子を適切に除去できる分級操作についてさらに検討を重ね、本発明に係る無機物フレークの製造方法を案出した。なお、本明細書において、「球状粒子」とは、ＳＥＭで観察したときに最小径Ｄｉに対する最大径Ｄｘの比（Ｄｘ／Ｄｉ）が１．５以下である粒子を意味する。
The present inventor manufactures inorganic flakes having a narrow particle size distribution and containing a large number of flake-like particles having rounded ends from a raw material which is a powder containing flake-like particles made of an inorganic substance. The method was examined day and night. As a result, when the present inventors heated the powder as the raw material so that the temperature of the surface of the flaky particles is higher than the softening temperature of the inorganic substance, the relatively small particles contained in the powder as the raw material It has been newly found that particles having a diameter become spherical particles. From the viewpoint of producing inorganic flakes having a narrow particle size distribution, in order to remove such spherical particles, it is considered to apply a powder containing spherical particles to a sieve having an opening larger than the particle size of the spherical particles. It is done. However, the inventor has newly found that the spherical particles cannot be removed properly by simply passing the powder containing the spherical particles through such a sieve. Accordingly, the present inventors have further studied the classification operation capable of appropriately removing the spherical particles, and have devised a method for producing inorganic flakes according to the present invention. In the present specification, “spherical particles” mean particles having a ratio of the maximum diameter Dx to the minimum diameter Di (Dx / Di) of 1.5 or less when observed with an SEM.
本発明に係る無機物フレークは、典型的には、以下の工程（ｉ）及び（ii）を含む方法によって製造される。
（ｉ）無機物でできた第一フレーク状粒子を含有する第一粉体を第一フレーク状粒子の表面の温度が無機物の軟化温度よりも高い温度になるように加熱して、第二粉体を作製する。ここで、第二粉体は、第二フレーク状粒子及び第二フレーク状粒子の粒子径よりも小さい粒子径を有する球状粒子を含有する。
（ii）流水とともに第二粉体を球状粒子の粒子径よりも大きい目開きを有する篩にかけて球状粒子を除去する。 The inorganic flakes according to the present invention are typically produced by a method including the following steps (i) and (ii).
(I) The first powder containing the first flaky particles made of an inorganic material is heated so that the surface temperature of the first flaky particles is higher than the softening temperature of the inorganic material, and the second powder Is made. Here, the second powder contains spherical particles having a particle size smaller than the particle size of the second flaky particles and the second flaky particles.
(Ii) The spherical particles are removed by passing the second powder together with running water through a sieve having an opening larger than the particle diameter of the spherical particles.
（ｉ）無機物でできた第一フレーク状粒子を含有する第一粉体を第一フレーク状粒子の表面の温度が無機物の軟化温度よりも高い温度になるように加熱して、第二粉体を作製する。ここで、第二粉体は、第二フレーク状粒子及び第二フレーク状粒子の粒子径よりも小さい粒子径を有する球状粒子を含有する。
（ii）流水とともに第二粉体を球状粒子の粒子径よりも大きい目開きを有する篩にかけて球状粒子を除去する。 The inorganic flakes according to the present invention are typically produced by a method including the following steps (i) and (ii).
(I) The first powder containing the first flaky particles made of an inorganic material is heated so that the surface temperature of the first flaky particles is higher than the softening temperature of the inorganic material, and the second powder Is made. Here, the second powder contains spherical particles having a particle size smaller than the particle size of the second flaky particles and the second flaky particles.
(Ii) The spherical particles are removed by passing the second powder together with running water through a sieve having an opening larger than the particle diameter of the spherical particles.
第一粉体を上記のように加熱することにより、第一フレーク状粒子の表面が無機物の軟化温度よりも高い温度になり、第一フレーク状粒子の端部が軟化する。これにより、第二フレーク状粒子が丸みを持った端部を有する。また、第一粉体の加熱により、第一粉体に含まれる比較的小さい粒子径を有する粒子の全体が軟化しやすい。全体が軟化した粒子は表面張力により球状粒子になりやすい。このため、第二粉体は、第二フレーク状粒子に加えて、球状粒子を含有する。球状粒子同士の相互作用又は球状粒子と第二フレーク状粒子との相互作用により、第二粉体を単に篩にかけても球状粒子が除去されにくいと考えられる。しかし、流水が篩を通過する状態で第二粉体を篩にかけると流水とともに球状粒子の多くが篩を通過して球状粒子が除去される。その結果、丸みを持った端部を有するフレーク状粒子を多く含み、かつ、狭い粒子径分布を有する無機物フレークを製造できる。
By heating the first powder as described above, the surface of the first flaky particles becomes higher than the softening temperature of the inorganic substance, and the end portions of the first flaky particles are softened. Thereby, the second flaky particles have rounded ends. Moreover, the whole of the particles having a relatively small particle diameter contained in the first powder is easily softened by heating the first powder. The whole softened particles are likely to become spherical particles due to surface tension. For this reason, the second powder contains spherical particles in addition to the second flaky particles. Due to the interaction between the spherical particles or the interaction between the spherical particles and the second flaky particles, it is considered that the spherical particles are hardly removed even if the second powder is simply sieved. However, when the second powder is passed through the sieve while the flowing water passes through the sieve, most of the spherical particles pass through the sieve together with the flowing water, and the spherical particles are removed. As a result, it is possible to produce inorganic flakes containing a large number of flaky particles having rounded ends and having a narrow particle size distribution.
例えば、無機物フレークは、丸みを持った端部を有するフレーク状粒子を個数基準で５０％以上含有する。これにより、無機物フレークが良好な触感を有する。
For example, inorganic flakes contain 50% or more of flaky particles having rounded ends on a number basis. Thereby, inorganic flakes have a good tactile sensation.
第一粉体の体積基準の粒子径分布における累積分布１０％に相当する粒子径、メジアン径、及び累積分布９０％に相当する粒子径をそれぞれｄ１（１０）、ｄ１（５０）、及びｄ１（９０）と表す。また、無機物フレークの体積基準の粒子径分布における累積分布１０％に相当する粒子径、メジアン径、及び累積分布９０％に相当する粒子径をそれぞれｄ２（１０）、ｄ２（５０）、及びｄ２（９０）と表す。第一粉体及び無機物フレークの体積基準の粒子径分布は、例えば、レーザー回折式粒度分布測定装置によって測定できる。第一粉体及び無機物フレークにおいて、例えば以下の関係が満たされている。
１０μｍ≦ｄ１（５０）≦１０００μｍ
１０μｍ≦ｄ２（５０）≦１０００μｍ
ｄ２（９０）／ｄ２（１０）＜ｄ１（９０）／ｄ１（１０）
｛ｄ２（９０）－ｄ２（１０）｝／ｄ２（５０）＜｛ｄ２（９０）－ｄ２（１０）｝／ｄ２（５０） The particle diameter corresponding to the cumulative distribution of 10% in the volume-based particle diameter distribution of the first powder, the median diameter, and the particle diameter corresponding to the cumulative distribution of 90% are d1 (10), d1 (50), and d1 ( 90). In addition, the particle diameter corresponding to 10% of the cumulative distribution in the volume-based particle size distribution of the inorganic flakes, the median diameter, and the particle diameter corresponding to the cumulative distribution of 90% are d2 (10), d2 (50), and d2 ( 90). The volume-based particle size distribution of the first powder and inorganic flakes can be measured by, for example, a laser diffraction particle size distribution measuring device. For example, the following relationship is satisfied in the first powder and the inorganic flakes.
10 μm ≦ d1 (50) ≦ 1000 μm
10 μm ≦ d2 (50) ≦ 1000 μm
d2 (90) / d2 (10) <d1 (90) / d1 (10)
{D2 (90) -d2 (10)} / d2 (50) <{d2 (90) -d2 (10)} / d2 (50)
１０μｍ≦ｄ１（５０）≦１０００μｍ
１０μｍ≦ｄ２（５０）≦１０００μｍ
ｄ２（９０）／ｄ２（１０）＜ｄ１（９０）／ｄ１（１０）
｛ｄ２（９０）－ｄ２（１０）｝／ｄ２（５０）＜｛ｄ２（９０）－ｄ２（１０）｝／ｄ２（５０） The particle diameter corresponding to the cumulative distribution of 10% in the volume-based particle diameter distribution of the first powder, the median diameter, and the particle diameter corresponding to the cumulative distribution of 90% are d1 (10), d1 (50), and d1 ( 90). In addition, the particle diameter corresponding to 10% of the cumulative distribution in the volume-based particle size distribution of the inorganic flakes, the median diameter, and the particle diameter corresponding to the cumulative distribution of 90% are d2 (10), d2 (50), and d2 ( 90). The volume-based particle size distribution of the first powder and inorganic flakes can be measured by, for example, a laser diffraction particle size distribution measuring device. For example, the following relationship is satisfied in the first powder and the inorganic flakes.
10 μm ≦ d1 (50) ≦ 1000 μm
10 μm ≦ d2 (50) ≦ 1000 μm
d2 (90) / d2 (10) <d1 (90) / d1 (10)
{D2 (90) -d2 (10)} / d2 (50) <{d2 (90) -d2 (10)} / d2 (50)
上記の通り、本発明の方法により製造された無機物フレークは、第一粉体に比べて、狭い粒子径分布を有する。無機物フレークの体積基準の粒子径分布は、例えば、１．１≦ｄ２（９０）／ｄ２（１０）≦２０及び０．１≦｛ｄ２（９０）－ｄ２（１０）｝／ｄ２（５０）≦７の関係をさらに満たしている。
As described above, the inorganic flakes produced by the method of the present invention have a narrow particle size distribution compared to the first powder. The volume-based particle size distribution of the inorganic flakes is, for example, 1.1 ≦ d2 (90) / d2 (10) ≦ 20 and 0.1 ≦ {d2 (90) −d2 (10)} / d2 (50) ≦. The relationship of 7 is further satisfied.
無機物フレークの厚みは、例えば、０．２μｍ～１０００μｍである。
The thickness of the inorganic flake is, for example, 0.2 μm to 1000 μm.
上記（ｉ）の工程における第一粉体の加熱の条件は、典型的には、比較的大きな粒子径を有する第一フレーク状粒子の全体的な形状が維持されつつ端部が軟化するように定められている。加えて、上記（ｉ）の工程における第一粉体の加熱の条件は、第二粉体に所定の粒子径（例えば、１００μｍ以下）の球状粒子が含まれるように、第一粉体に含まれる比較的小さい粒子径を有する粒子の全体を軟化させることができるように定められている。例えば、上記（ｉ）の工程における第一粉体の加熱の条件は、第一フレーク状粒子の表面の温度が無機物の軟化温度よりも５０℃～２５０℃高い温度になるように定められている。
Typically, the heating condition of the first powder in the step (i) is such that the end is softened while the overall shape of the first flaky particles having a relatively large particle diameter is maintained. It has been established. In addition, the heating condition of the first powder in the step (i) is included in the first powder so that the second powder includes spherical particles having a predetermined particle diameter (for example, 100 μm or less). It is determined so that the whole particles having a relatively small particle size can be softened. For example, the conditions for heating the first powder in the step (i) are determined so that the surface temperature of the first flaky particles is 50 ° C. to 250 ° C. higher than the softening temperature of the inorganic substance. .
上記（ｉ）の工程における第一粉体の加熱は、例えば、バーナーによって形成された火炎に第一粉体を通過させることにより行われる。例えば、火炎が水平方向に形成されており、火炎を通過するように第一粉体を落下させる。この場合、望ましくは、火炎に第一粉体を通過させる前に、第一粉体を無機物の軟化温度よりも低い所定の温度になるように予熱する。例えば、第一粉体は無機物の軟化温度よりも２０℃～１００℃低い温度になるように予熱される。例えば、バーナーによって形成された火炎によって加熱された空気に第一粉体を接触させることにより第一粉体を予熱できる。上記（ｉ）の工程において、望ましくは、第一粉体の加熱後に、加熱された第一粉体が冷却空気によって急冷される。これにより、第二粉体に含まれる粒子の形状が適切な形状に定まりやすい。第一粉体の急冷は、例えば、火炎を通過した第一粉体が移動する空間にブロアによって冷却空気（外気）を送り込むことによって行われる。
The heating of the first powder in the step (i) is performed, for example, by passing the first powder through a flame formed by a burner. For example, the flame is formed in the horizontal direction, and the first powder is dropped so as to pass through the flame. In this case, preferably, before passing the first powder through the flame, the first powder is preheated to a predetermined temperature lower than the softening temperature of the inorganic substance. For example, the first powder is preheated to a temperature that is 20 ° C. to 100 ° C. lower than the softening temperature of the inorganic substance. For example, the first powder can be preheated by bringing the first powder into contact with air heated by a flame formed by a burner. In the step (i), desirably, the heated first powder is rapidly cooled by cooling air after the first powder is heated. Thereby, the shape of the particles contained in the second powder is easily determined to an appropriate shape. The rapid cooling of the first powder is performed, for example, by sending cooling air (outside air) by a blower into a space in which the first powder that has passed through the flame moves.
第一粉体において、第一フレーク状粒子をなす無機物は、所定の温度で軟化する無機物である限り特定の無機物に制限されないが、例えば、ガラス又は鉱物である。第一フレーク状粒子をなす鉱物は、例えば、マイカ又はタルクである。この場合、上記（ｉ）の工程において、第一粉体に含有されている比較的小さい粒子径を有する粒子が球状粒子になりやすい。
In the first powder, the inorganic substance forming the first flaky particles is not limited to a specific inorganic substance as long as it is an inorganic substance that softens at a predetermined temperature, but is, for example, glass or mineral. The mineral forming the first flaky particles is, for example, mica or talc. In this case, in the step (i), the particles having a relatively small particle size contained in the first powder tend to be spherical particles.
第二粉体は、例えば、球状粒子を個数基準で１％～４９％含有している。また、第二粉体に含有される球状粒子の粒子径は、例えば１００μｍ以下である。第二粉体から球状粒子を除去することにより、狭い粒子径分布を有する無機物フレークが得られる。
The second powder contains, for example, 1% to 49% of spherical particles based on the number. Moreover, the particle diameter of the spherical particles contained in the second powder is, for example, 100 μm or less. By removing the spherical particles from the second powder, inorganic flakes having a narrow particle size distribution can be obtained.
上記（ii）の工程において使用する篩は、球状粒子の粒子径よりも大きい目開きを有する。この篩は、望ましくは第二粉体に含有される第二フレーク状粒子の大部分の粒子径よりも小さい目開きを有する。篩の目開きは、例えば２μｍ～１０００μｍである。
The sieve used in the step (ii) has an opening larger than the particle diameter of the spherical particles. The sieve desirably has an opening smaller than the particle size of most of the second flaky particles contained in the second powder. The opening of the sieve is, for example, 2 μm to 1000 μm.
上記（ii）の工程において、流水とともに球状粒子が篩を通過すると考えられる。このため、第二粉体から多くの球状粒子を除去するために、第二粉体の全体が満遍なく流水に接触することが望ましい。そこで、上記（ii）の工程において、流水の流れ方向と垂直な方向に篩を動かすことが望ましい。
In the process (ii) above, it is considered that spherical particles pass through the sieve together with running water. For this reason, in order to remove many spherical particles from the second powder, it is desirable that the entire second powder is uniformly in contact with running water. Therefore, in the step (ii), it is desirable to move the sieve in a direction perpendicular to the flowing direction of the flowing water.
上記（ii）の工程における流水の流量は、球状粒子を除去できるとともに、第二フレーク状粒子を砕かないように定められている。例えば、上記（ii）の工程における流水の流量は、１ｃｍ3／秒～１０００ｃｍ3／秒である。
The flow rate of the flowing water in the step (ii) is determined so that the spherical particles can be removed and the second flaky particles are not crushed. For example, the flow rate of flowing water in the step (ii) is 1 cm 3 / sec to 1000 cm 3 / sec.
上記（ii）の工程においてより多くの球状粒子を除去する観点から、望ましくは、第二粉体を篩にかける前に液中に添加して所定期間攪拌する。第二粉体を添加する液体は、第二粉体を変質させず、第二粉体を分散可能な液体である限り特に制限されないが、例えば、水である。また、攪拌時間は、特定の時間に制限されず、例えば０．１分間～６０分間である。
From the viewpoint of removing more spherical particles in the step (ii), preferably, the second powder is added to the liquid before being sieved and stirred for a predetermined period. The liquid to which the second powder is added is not particularly limited as long as it is a liquid that does not alter the second powder and can disperse the second powder, and is, for example, water. Further, the stirring time is not limited to a specific time and is, for example, 0.1 minute to 60 minutes.
上記（ii）の工程において、篩を通過しなかった粉体を回収することにより、本発明に係る無機物フレークが得られる。この場合、無機物フレークに付着した水分は、自然乾燥処理又は乾燥炉における乾燥処理によって除去される。なお、無機物フレークには、所定のコーティングが施されてもよい。
In the step (ii), the inorganic flakes according to the present invention can be obtained by collecting the powder that has not passed through the sieve. In this case, the water adhering to the inorganic flakes is removed by a natural drying process or a drying process in a drying furnace. The inorganic flakes may be given a predetermined coating.
本発明に係る無機物フレークは、第二フレーク状粒子の多くが丸みを持った端部を有することにより、良好な触感を発揮する。本発明に係る無機物フレークは、例えば、固定された粘着テープの粘着面に無機物フレークを付着させて形成された摩擦面に、０．９以下の静摩擦係数及び０．７以下の動摩擦係数の少なくともいずれか１つを付与する。
The inorganic flakes according to the present invention exhibit a good tactile sensation because most of the second flaky particles have round ends. The inorganic flakes according to the present invention have, for example, a static friction coefficient of 0.9 or less and a dynamic friction coefficient of 0.7 or less on a friction surface formed by attaching inorganic flakes to the adhesive surface of a fixed adhesive tape. Or one.
実施例により、本発明をより詳細に説明する。なお、本発明は以下の実施例に限定されない。
The present invention will be described in more detail by way of examples. The present invention is not limited to the following examples.
＜実施例＞
原料粉体（日本板硝子社製、製品名：ガラスフレークＭＴＤ１６０ＦＹ）を準備した。原料粉体に含まれるフレーク状粒子の平均厚みは０．４μｍであり、原料粉体の真密度は２．７ｇ／ｃｍ3であり、原料粉体のかさ密度は、０．０３ｇ／ｃｍ3であった。また、原料粉体をなすガラスの軟化温度Ｔｓは８７０℃～８８０℃であり、原料粉体をなすガラスのガラス転移温度Ｔｇは約７００℃であった。レーザー回折式粒度分布測定装置（日機装社製、製品名：マイクロトラックＭＴ３５００）を用いて原料粉体の体積基準の粒子径分布を測定した。結果を図１及び表１に示す。原料粉体のＳＥＭ写真を図１０に示す。図１０に示す通り、原料粉体は鋭い端部を有していた。 <Example>
Raw material powder (manufactured by Nippon Sheet Glass Co., Ltd., product name: glass flake MTD160FY) was prepared. The average thickness of the flaky particles contained in the raw material powder is 0.4 μm, the true density of the raw material powder is 2.7 g / cm 3 , and the bulk density of the raw material powder is 0.03 g / cm 3 . there were. The softening temperature Ts of the glass forming the raw material powder was 870 ° C. to 880 ° C., and the glass transition temperature Tg of the glass forming the raw material powder was about 700 ° C. The volume-based particle size distribution of the raw material powder was measured using a laser diffraction particle size distribution measuring device (manufactured by Nikkiso Co., Ltd., product name: Microtrack MT3500). The results are shown in FIG. An SEM photograph of the raw material powder is shown in FIG. As shown in FIG. 10, the raw material powder had sharp edges.
原料粉体（日本板硝子社製、製品名：ガラスフレークＭＴＤ１６０ＦＹ）を準備した。原料粉体に含まれるフレーク状粒子の平均厚みは０．４μｍであり、原料粉体の真密度は２．７ｇ／ｃｍ3であり、原料粉体のかさ密度は、０．０３ｇ／ｃｍ3であった。また、原料粉体をなすガラスの軟化温度Ｔｓは８７０℃～８８０℃であり、原料粉体をなすガラスのガラス転移温度Ｔｇは約７００℃であった。レーザー回折式粒度分布測定装置（日機装社製、製品名：マイクロトラックＭＴ３５００）を用いて原料粉体の体積基準の粒子径分布を測定した。結果を図１及び表１に示す。原料粉体のＳＥＭ写真を図１０に示す。図１０に示す通り、原料粉体は鋭い端部を有していた。 <Example>
Raw material powder (manufactured by Nippon Sheet Glass Co., Ltd., product name: glass flake MTD160FY) was prepared. The average thickness of the flaky particles contained in the raw material powder is 0.4 μm, the true density of the raw material powder is 2.7 g / cm 3 , and the bulk density of the raw material powder is 0.03 g / cm 3 . there were. The softening temperature Ts of the glass forming the raw material powder was 870 ° C. to 880 ° C., and the glass transition temperature Tg of the glass forming the raw material powder was about 700 ° C. The volume-based particle size distribution of the raw material powder was measured using a laser diffraction particle size distribution measuring device (manufactured by Nikkiso Co., Ltd., product name: Microtrack MT3500). The results are shown in FIG. An SEM photograph of the raw material powder is shown in FIG. As shown in FIG. 10, the raw material powder had sharp edges.
７７５℃～８５５℃（代表温度：８２０℃）に予熱した原料粉体を、バーナーによって形成された火炎を通過させることによって加熱処理し、その後ブロアから吹き出された冷却空気に接触させることによって急冷処理を行った。火炎を通過する際の原料粉体の粒子の表面温度は、９２５℃～１１２５℃（代表温度：１０２０℃）であり、原料粉体をなすガラスの軟化温度Ｔｓよりも高かった。このようにして、中間粉体を得た。レーザー回折式粒度分布測定装置（日機装社製、製品名：マイクロトラックＭＴ３５００）を用いて中間粉体の体積基準の粒子径分布を測定した。結果を図２及び表１に示す。また、中間粉体のＳＥＭ写真を図５及び６に示す。図５に示す通り、中間粉体は、フレーク状粒子及び球状粒子を含有していた。中間粉体は、個数基準で約２０％の球状粒子を含有していた。図２のヒストグラムに示す通り、中間粉体の粒子径分布は、相対的に大きい粒子径で単一のピークを有する粒子径分布と、相対的に小さい粒子径で単一のピークを有する粒子径分布とを重ね合せたような分布を有していた。中間粉体の粒子径分布は、相対的に大きい粒子径を有するフレーク状粒子と、相対的に小さい粒子径を有する球状粒子とが混在している状態を反映していたと考えられる。図６に示す通り、中間粉体のフレーク状粒子の多くは丸みを持った端部を有していた。中間粉体のフレーク状粒子のうち、個数基準で約９０％以上のフレーク状粒子が丸みを持った端部を有していた。
The raw material powder preheated to 775 ° C. to 855 ° C. (typical temperature: 820 ° C.) is heated by passing through a flame formed by a burner, and then rapidly cooled by contacting with the cooling air blown out from the blower Went. The surface temperature of the raw material powder particles when passing through the flame was 925 ° C. to 1125 ° C. (typical temperature: 1020 ° C.), which was higher than the softening temperature Ts of the glass forming the raw material powder. In this way, an intermediate powder was obtained. The volume-based particle size distribution of the intermediate powder was measured using a laser diffraction particle size distribution measuring device (manufactured by Nikkiso Co., Ltd., product name: Microtrack MT3500). The results are shown in FIG. Further, SEM photographs of the intermediate powder are shown in FIGS. As shown in FIG. 5, the intermediate powder contained flaky particles and spherical particles. The intermediate powder contained about 20% spherical particles on a number basis. As shown in the histogram of FIG. 2, the particle size distribution of the intermediate powder includes a particle size distribution having a single peak at a relatively large particle size and a particle size having a single peak at a relatively small particle size. It had a distribution that overlapped with the distribution. It is considered that the particle size distribution of the intermediate powder reflects a state in which flaky particles having a relatively large particle size and spherical particles having a relatively small particle size are mixed. As shown in FIG. 6, most of the flaky particles of the intermediate powder had rounded ends. Of the flaky particles of the intermediate powder, about 90% or more of the flaky particles on the number basis had rounded ends.
室温において中間粉体を水中で３０分間撹拌した。その後、水道水を流しながら中間粉体を１０６μｍの目開きを有する篩にかけた。この期間に、篩を、水平方向に数回往復するように動かした。水道水の流量は、１０ｃｍ3／秒であった。
The intermediate powder was stirred in water for 30 minutes at room temperature. Thereafter, the intermediate powder was passed through a sieve having an opening of 106 μm while flowing tap water. During this period, the sieve was moved back and forth several times in the horizontal direction. The flow rate of tap water was 10 cm 3 / sec.
篩に残留した粉体を乾燥炉において１００℃で３０分間乾燥させ、実施例に係る無機物フレークを得た。レーザー回折式粒度分布測定装置（日機装社製、製品名：マイクロトラックＭＴ３５００）を用いて実施例に係る無機物フレークの体積基準の粒子径分布を測定した。結果を図３及び表１に示す。図３及び表１に示す通り、実施例に係る無機物フレークは狭い粒子径分布を有することが示唆された。無機物フレークのＳＥＭ写真を図７及び図８に示す。図７に示す通り、無機物フレークには、球状粒子はほとんど含まれておらず、中間粉体における球状粒子がほとんど除去されていることが示唆された。図８に示す通り、無機物フレークの粒子の多くは丸みを持った端部を有していた。
The powder remaining on the sieve was dried at 100 ° C. for 30 minutes in a drying furnace to obtain inorganic flakes according to the example. The volume-based particle size distribution of the inorganic flakes according to the example was measured using a laser diffraction particle size distribution measuring device (manufactured by Nikkiso Co., Ltd., product name: Microtrack MT3500). The results are shown in FIG. As shown in FIG. 3 and Table 1, it was suggested that the inorganic flakes according to the examples have a narrow particle size distribution. SEM photographs of the inorganic flakes are shown in FIGS. As shown in FIG. 7, the inorganic flakes contained almost no spherical particles, suggesting that the spherical particles in the intermediate powder were almost removed. As shown in FIG. 8, many of the particles of inorganic flakes had rounded ends.
＜比較例＞
水道水を流さずに乾燥した中間粉体を１０６μｍの目開きを有する篩にかけた。篩に残留した粉体を回収して比較例に係る粉体を得た。レーザー回折式粒度分布測定装置（日機装社製、製品名：マイクロトラックＭＴ３５００）を用いて比較例に係る粉体の体積基準の粒子径分布を測定した。結果を図４及び表１に示す。比較例に係る粉体のＳＥＭ写真を図９に示す。図９に示す通り、比較例に係る粉体には、多くの球状粒子が含まれていた。 <Comparative example>
The intermediate powder dried without running tap water was passed through a sieve having an opening of 106 μm. The powder remaining on the sieve was collected to obtain a powder according to a comparative example. The volume-based particle size distribution of the powder according to the comparative example was measured using a laser diffraction particle size distribution measuring apparatus (manufactured by Nikkiso Co., Ltd., product name: Microtrack MT3500). The results are shown in FIG. An SEM photograph of the powder according to the comparative example is shown in FIG. As shown in FIG. 9, the powder according to the comparative example contained many spherical particles.
水道水を流さずに乾燥した中間粉体を１０６μｍの目開きを有する篩にかけた。篩に残留した粉体を回収して比較例に係る粉体を得た。レーザー回折式粒度分布測定装置（日機装社製、製品名：マイクロトラックＭＴ３５００）を用いて比較例に係る粉体の体積基準の粒子径分布を測定した。結果を図４及び表１に示す。比較例に係る粉体のＳＥＭ写真を図９に示す。図９に示す通り、比較例に係る粉体には、多くの球状粒子が含まれていた。 <Comparative example>
The intermediate powder dried without running tap water was passed through a sieve having an opening of 106 μm. The powder remaining on the sieve was collected to obtain a powder according to a comparative example. The volume-based particle size distribution of the powder according to the comparative example was measured using a laser diffraction particle size distribution measuring apparatus (manufactured by Nikkiso Co., Ltd., product name: Microtrack MT3500). The results are shown in FIG. An SEM photograph of the powder according to the comparative example is shown in FIG. As shown in FIG. 9, the powder according to the comparative example contained many spherical particles.
表１に示す通り、実施例に係る無機物フレークは、比較例に係る粉体と比較すると、より小さいＤ９０／Ｄ１０の値及びより小さい（Ｄ９０－Ｄ１０）／Ｄ５０の値を有し、より狭い粒子径分布を有していた。原料粉体における比較的小さい粒子径を有する粒子を加熱処理により球状粒子に変化させ、球状粒子を除去するための適切な分級操作を選択することによって狭い粒子径分布を有する無機物フレークを製造できることが示唆された。
As shown in Table 1, the inorganic flakes according to the examples have smaller values of D90 / D10 and smaller values of (D90-D10) / D50 and narrower particles compared to the powders of the comparative examples. It had a diameter distribution. It is possible to produce inorganic flakes having a narrow particle size distribution by changing particles having a relatively small particle size in the raw material powder into spherical particles by heat treatment and selecting an appropriate classification operation for removing the spherical particles. It was suggested.
＜摩擦係数の評価＞
摩擦感測定装置（トリニティーラボ社製、製品名：ＴＬ２０１Ｔｓ）の測定ステージに両面テープを貼り、両面テープの粘着面に０.１ｇの実施例に係る無機物フレークを万遍なくまぶした。その後、以下の条件で実施例に係る無機物フレークが付着した両面テープの粘着面の静摩擦係数及び動摩擦係数を測定した。結果を表２に示す。
測定子：指紋タイプ
両面テープの粘着面にかけた荷重：３０ｇ
測定距離：３０ｍｍ
サンプリングピッチ：１ミリ秒
測定回数：３回 <Evaluation of friction coefficient>
A double-sided tape was affixed to the measurement stage of a friction feeling measuring device (manufactured by Trinity Labs, product name: TL201Ts), and 0.1 g of inorganic flakes according to the examples were uniformly applied to the adhesive surface of the double-sided tape. Then, the static friction coefficient and the dynamic friction coefficient of the adhesive surface of the double-sided tape to which the inorganic flakes according to the examples adhered were measured under the following conditions. The results are shown in Table 2.
Measuring point: Fingerprint type Load applied to the adhesive surface of double-sided tape: 30 g
Measuring distance: 30mm
Sampling pitch: 1 millisecond Measurement count: 3 times
摩擦感測定装置（トリニティーラボ社製、製品名：ＴＬ２０１Ｔｓ）の測定ステージに両面テープを貼り、両面テープの粘着面に０.１ｇの実施例に係る無機物フレークを万遍なくまぶした。その後、以下の条件で実施例に係る無機物フレークが付着した両面テープの粘着面の静摩擦係数及び動摩擦係数を測定した。結果を表２に示す。
測定子：指紋タイプ
両面テープの粘着面にかけた荷重：３０ｇ
測定距離：３０ｍｍ
サンプリングピッチ：１ミリ秒
測定回数：３回 <Evaluation of friction coefficient>
A double-sided tape was affixed to the measurement stage of a friction feeling measuring device (manufactured by Trinity Labs, product name: TL201Ts), and 0.1 g of inorganic flakes according to the examples were uniformly applied to the adhesive surface of the double-sided tape. Then, the static friction coefficient and the dynamic friction coefficient of the adhesive surface of the double-sided tape to which the inorganic flakes according to the examples adhered were measured under the following conditions. The results are shown in Table 2.
Measuring point: Fingerprint type Load applied to the adhesive surface of double-sided tape: 30 g
Measuring distance: 30mm
Sampling pitch: 1 millisecond Measurement count: 3 times
加熱処理を行っておらず、丸みを持たない（角張った）端部を有するフレーク状粒子からなる比較例に係るフレーク（Ｄ１０：６４μｍ、Ｄ５０：１４９μｍ、Ｄ９０：２６２μｍ）を準備した。実施例に係る無機物フレークの代わりに、比較例に係るフレークを用いた以外は同様にして、比較例に係るフレークが付着した両面テープの粘着面の静摩擦係数及び動摩擦係数を測定した。結果を表２に示す。表２に示す通り、実施例に係る無機物フレークが付着した両面テープの粘着面は、比較例に係るフレークが付着した両面テープの粘着面と比べて、低い静摩擦係数及び低い動摩擦係数を有した。このため、実施例に係る無機物フレークは、良好な触感を付与できることが示唆された。
Flakes (D10: 64 μm, D50: 149 μm, D90: 262 μm) according to a comparative example made of flaky particles not subjected to heat treatment and having rounded (angular) ends were prepared. The static friction coefficient and the dynamic friction coefficient of the adhesive surface of the double-sided tape to which the flakes according to the comparative example adhered were measured in the same manner except that the flakes according to the comparative example were used instead of the inorganic flakes according to the examples. The results are shown in Table 2. As shown in Table 2, the adhesive surface of the double-sided tape to which the inorganic flakes according to the examples adhered had a lower static friction coefficient and a lower dynamic friction coefficient than the adhesive surface of the double-sided tape to which the flakes according to the comparative example adhered. For this reason, it was suggested that the inorganic flakes according to the examples can impart a good tactile sensation.
Flakes (D10: 64 μm, D50: 149 μm, D90: 262 μm) according to a comparative example made of flaky particles not subjected to heat treatment and having rounded (angular) ends were prepared. The static friction coefficient and the dynamic friction coefficient of the adhesive surface of the double-sided tape to which the flakes according to the comparative example adhered were measured in the same manner except that the flakes according to the comparative example were used instead of the inorganic flakes according to the examples. The results are shown in Table 2. As shown in Table 2, the adhesive surface of the double-sided tape to which the inorganic flakes according to the examples adhered had a lower static friction coefficient and a lower dynamic friction coefficient than the adhesive surface of the double-sided tape to which the flakes according to the comparative example adhered. For this reason, it was suggested that the inorganic flakes according to the examples can impart a good tactile sensation.
Claims (8)
- 無機物でできた第一フレーク状粒子を含有する第一粉体を前記第一フレーク状粒子の表面の温度が前記無機物の軟化温度よりも高い温度になるように加熱して、第二フレーク状粒子及び前記第二フレーク状粒子の粒子径よりも小さい粒子径を有する球状粒子を含有する第二粉体を作製し、
流水とともに前記第二粉体を前記球状粒子の粒子径よりも大きい目開きを有する篩にかけて前記球状粒子を除去して、
無機物フレークを製造する方法。 Heating the first powder containing the first flaky particles made of an inorganic material so that the surface temperature of the first flaky particles is higher than the softening temperature of the inorganic material, And preparing a second powder containing spherical particles having a particle size smaller than the particle size of the second flaky particles,
The second powder together with running water is passed through a sieve having an opening larger than the particle diameter of the spherical particles to remove the spherical particles,
A method for producing inorganic flakes. - 前記第一粉体の体積基準の粒子径分布における累積分布１０％に相当する粒子径、メジアン径、及び累積分布９０％に相当する粒子径をそれぞれｄ１（１０）、ｄ１（５０）、及びｄ１（９０）と表し、
当該無機物フレークの体積基準の粒子径分布における累積分布１０％に相当する粒子径、メジアン径、及び累積分布９０％に相当する粒子径をそれぞれｄ２（１０）、ｄ２（５０）、及びｄ２（９０）と表したときに、
１０μｍ≦ｄ１（５０）≦１０００μｍ、
１０μｍ≦ｄ２（５０）≦１０００μｍ、
ｄ２（９０）／ｄ２（１０）＜ｄ１（９０）／ｄ１（１０）、及び
｛ｄ２（９０）－ｄ２（１０）｝／ｄ２（５０）＜｛ｄ２（９０）－ｄ２（１０）｝／ｄ２（５０）の関係を満たす、
請求項１に記載の方法。 The particle size corresponding to 10% of the cumulative distribution in the volume-based particle size distribution of the first powder, the median diameter, and the particle size corresponding to 90% of the cumulative distribution are d1 (10), d1 (50), and d1, respectively. (90)
In the volume-based particle size distribution of the inorganic flakes, the particle size corresponding to 10% cumulative distribution, the median size, and the particle size corresponding to 90% cumulative distribution are d2 (10), d2 (50), and d2 (90 )
10 μm ≦ d1 (50) ≦ 1000 μm,
10 μm ≦ d2 (50) ≦ 1000 μm,
d2 (90) / d2 (10) <d1 (90) / d1 (10), and {d2 (90) −d2 (10)} / d2 (50) <{d2 (90) −d2 (10)} / satisfies the relationship of d2 (50).
The method of claim 1. - １．１≦ｄ２（９０）／ｄ２（１０）≦２０及び０．１≦｛ｄ２（９０）－ｄ２（１０）｝／ｄ２（５０）≦７の関係をさらに満たす、請求項２に記載の方法。 3. The relationship according to claim 2, further satisfying a relationship of 1.1 ≦ d2 (90) / d2 (10) ≦ 20 and 0.1 ≦ {d2 (90) −d2 (10)} / d2 (50) ≦ 7. Method.
- 前記第二フレーク状粒子は、丸みを持った端部を有する、請求項１～３のいずれか１項に記載の方法。 The method according to any one of claims 1 to 3, wherein the second flaky particles have rounded ends.
- 前記第二粉体を前記篩にかける前に液中に添加して所定期間攪拌する、請求項１～４のいずれか１項に記載の方法。 The method according to any one of claims 1 to 4, wherein the second powder is added to the liquid and stirred for a predetermined period before passing through the sieve.
- 前記無機物は、ガラス又は鉱物である、請求項１～５のいずれか１項に記載の方法。 The method according to any one of claims 1 to 5, wherein the inorganic substance is glass or mineral.
- 無機物フレークであって、
丸みを持った端部を有するフレーク状粒子を個数基準で５０％以上含有し、
当該無機物フレークの体積基準の粒子径分布における累積分布１０％に相当する粒子径、メジアン径、及び累積分布９０％に相当する粒子径をそれぞれｄ２（１０）、ｄ２（５０）、及びｄ２（９０）と表したときに、
１０μｍ≦ｄ２（５０）≦１０００μｍ、
１．１≦ｄ２（９０）／ｄ２（１０）≦２０、及び
０．１≦｛ｄ２（９０）－ｄ２（１０）｝／ｄ２（５０）≦７の関係を満たす、
無機物フレーク。 Inorganic flakes,
Containing 50% or more of flaky particles having rounded ends on a number basis;
In the volume-based particle size distribution of the inorganic flakes, the particle size corresponding to 10% cumulative distribution, the median size, and the particle size corresponding to 90% cumulative distribution are d2 (10), d2 (50), and d2 (90 )
10 μm ≦ d2 (50) ≦ 1000 μm,
1.1 ≦ d2 (90) / d2 (10) ≦ 20 and 0.1 ≦ {d2 (90) −d2 (10)} / d2 (50) ≦ 7 are satisfied.
Inorganic flakes. - 固定された粘着テープの粘着面に当該無機物フレークを付着させて形成された摩擦面に、０．９以下の静摩擦係数及び０．７以下の動摩擦係数の少なくともいずれか１つを付与する、請求項７に記載の無機物フレーク。 The friction surface formed by adhering the inorganic flakes to the adhesive surface of the fixed adhesive tape is provided with at least one of a static friction coefficient of 0.9 or less and a dynamic friction coefficient of 0.7 or less. 7. The inorganic flake according to 7.
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/JP2018/003031 WO2018193684A1 (en) | 2017-04-21 | 2018-01-30 | Method for producing inorganic flakes and inorganic flakes |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP6839757B2 (en) |
| WO (1) | WO2018193684A1 (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000119028A (en) * | 1998-10-13 | 2000-04-25 | Union Corp | Edgeless glass particle and its production |
| WO2007114442A1 (en) * | 2006-04-05 | 2007-10-11 | Nippon Sheet Glass Company, Limited | Flaky particle and brightening pigment, and cosmetic preparation, coating composition, resin composition, and ink composition each containing these |
| WO2010067825A1 (en) * | 2008-12-10 | 2010-06-17 | 日本板硝子株式会社 | Method for producing glass flakes having rounded corners |
| JP2013530921A (en) * | 2010-07-07 | 2013-08-01 | グラスフレイク・リミテッド | Glass flakes and methods for producing them |
-
2018
- 2018-01-30 WO PCT/JP2018/003031 patent/WO2018193684A1/en active Application Filing
- 2018-01-30 JP JP2019513232A patent/JP6839757B2/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000119028A (en) * | 1998-10-13 | 2000-04-25 | Union Corp | Edgeless glass particle and its production |
| WO2007114442A1 (en) * | 2006-04-05 | 2007-10-11 | Nippon Sheet Glass Company, Limited | Flaky particle and brightening pigment, and cosmetic preparation, coating composition, resin composition, and ink composition each containing these |
| WO2010067825A1 (en) * | 2008-12-10 | 2010-06-17 | 日本板硝子株式会社 | Method for producing glass flakes having rounded corners |
| JP2013530921A (en) * | 2010-07-07 | 2013-08-01 | グラスフレイク・リミテッド | Glass flakes and methods for producing them |
Also Published As
| Publication number | Publication date |
|---|---|
| JP6839757B2 (en) | 2021-03-10 |
| JPWO2018193684A1 (en) | 2019-11-07 |
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