WO2018193684A1 - Procédé de production de flocons inorganiques et flocons inorganiques - Google Patents

Procédé de production de flocons inorganiques et flocons inorganiques Download PDF

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Publication number
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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WO
WIPO (PCT)
Prior art keywords
particle size
powder
inorganic
particles
flakes
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PCT/JP2018/003031
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English (en)
Japanese (ja)
Inventor
中村　浩一郎
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日本板硝子株式会社
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Publication date
Application filed by 日本板硝子株式会社 filed Critical 日本板硝子株式会社
Priority to JP2019513232A priority Critical patent/JP6839757B2/ja
Publication of WO2018193684A1 publication Critical patent/WO2018193684A1/fr

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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.

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  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)

Abstract

La présente invention concerne un procédé consistant à chauffer une première poudre et à produire une seconde poudre. La première poudre comprend de premières particules de type flocons constituées d'une substance inorganique. La première poudre est chauffée de sorte que la température de la surface des premières particules de type flocons est supérieure à la température de ramollissement de la substance inorganique. La seconde poudre comprend de secondes particules de type flocons et des particules sphériques. Les particules sphériques présentent une taille de particule qui est inférieure à la taille de particule des secondes particules de type flocons. La seconde poudre est tamisée conjointement avec de l'eau courante avec un tamis présentant une taille de maille supérieure à la taille de particule des particules sphériques pour retirer les particules sphériques afin de produire les flocons inorganiques.
PCT/JP2018/003031 2017-04-21 2018-01-30 Procédé de production de flocons inorganiques et flocons inorganiques WO2018193684A1 (fr)

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JP2019513232A JP6839757B2 (ja) 2017-04-21 2018-01-30 無機物フレークを製造する方法及び無機物フレーク

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JP2017-084529 2017-04-21
JP2017084529 2017-04-21

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000119028A (ja) * 1998-10-13 2000-04-25 Union Corp 無エッジガラス粒子及びその製造方法
WO2007114442A1 (fr) * 2006-04-05 2007-10-11 Nippon Sheet Glass Company, Limited Particule friable et pigment eclaircissant, et preparation cosmetique, composition de revetement, composition de resine et composition d'encre, chacune contenant ces elements
WO2010067825A1 (fr) * 2008-12-10 2010-06-17 日本板硝子株式会社 Procédé de fabrication d'un verre en copeaux dont les angles ont été arrondis
JP2013530921A (ja) * 2010-07-07 2013-08-01 グラスフレイク・リミテッド ガラスフレークおよびそれらの製造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000119028A (ja) * 1998-10-13 2000-04-25 Union Corp 無エッジガラス粒子及びその製造方法
WO2007114442A1 (fr) * 2006-04-05 2007-10-11 Nippon Sheet Glass Company, Limited Particule friable et pigment eclaircissant, et preparation cosmetique, composition de revetement, composition de resine et composition d'encre, chacune contenant ces elements
WO2010067825A1 (fr) * 2008-12-10 2010-06-17 日本板硝子株式会社 Procédé de fabrication d'un verre en copeaux dont les angles ont été arrondis
JP2013530921A (ja) * 2010-07-07 2013-08-01 グラスフレイク・リミテッド ガラスフレークおよびそれらの製造方法

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