JP2003104718A - Plate-like compound powder and its producing method - Google Patents

Plate-like compound powder and its producing method

Info

Publication number
JP2003104718A
JP2003104718A JP2001301984A JP2001301984A JP2003104718A JP 2003104718 A JP2003104718 A JP 2003104718A JP 2001301984 A JP2001301984 A JP 2001301984A JP 2001301984 A JP2001301984 A JP 2001301984A JP 2003104718 A JP2003104718 A JP 2003104718A
Authority
JP
Japan
Prior art keywords
plate
powder
thickness
synthetic
compound powder
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP2001301984A
Other languages
Japanese (ja)
Other versions
JP5116199B2 (en
Inventor
Masato Kuratani
昌人 倉谷
Shunichi Ota
俊一 太田
Takeyoshi Hayashi
剛芳 林
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Topy Industries Ltd
Original Assignee
Topy Industries Ltd
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Filing date
Publication date
Application filed by Topy Industries Ltd filed Critical Topy Industries Ltd
Priority to JP2001301984A priority Critical patent/JP5116199B2/en
Publication of JP2003104718A publication Critical patent/JP2003104718A/en
Application granted granted Critical
Publication of JP5116199B2 publication Critical patent/JP5116199B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Abstract

PROBLEM TO BE SOLVED: To provide a plate-like compound powder in which a plate-like particle is very smooth, with low brightness and with high safety and its producing method. SOLUTION: The plate-like compound powder contains a plate-like compound of which the ratio of end surface thickness to central thickness of a layer surface is 0.9-1.0 by 60% or more.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明は板状化合物粉体及び
その製造方法、特に板状粒子の平滑性、低光沢性及び粉
体の安全性の改良に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a plate-shaped compound powder and a method for producing the same, and more particularly to improvement of smoothness, low gloss of plate-shaped particles and safety of powder.

【0002】[0002]

【従来の技術】板状化合物粉体は、粉体の滑りのよさ等
に優れ、化粧品等に用いられている。従来、板状化合物
粉体は、結晶成長法で製造、または板状化合物結晶塊を
通常の破砕機で細片化し、ハンマーミル、ロールミル及
びボールミル等を用いて更に微粉化、分級して製造して
いた。
2. Description of the Related Art Plate-like compound powders are used in cosmetics and the like because of their excellent sliding property. Conventionally, the plate-like compound powder is produced by a crystal growth method, or the plate-like compound crystal lumps are fragmented by an ordinary crusher, further finely pulverized using a hammer mill, a roll mill, a ball mill, etc., and produced by classifying. Was there.

【0003】また、結晶物質として合成フッ素雲母を用
いてこのような従来の製造方法で得られた板状合成フッ
素雲母粉体は、溶出しやすいフッ素を含有しており、粉
体が水と接触するとフッ素が溶出するので、化粧品等の
ように人体に近いところで使用される場合には安全性の
面から好ましいものではなかった。
Further, the plate-like synthetic fluoromica powder obtained by such a conventional production method using synthetic fluoromica as a crystalline substance contains fluorine which is easily eluted, and the powder comes into contact with water. Then, since fluorine is eluted, it is not preferable from the viewpoint of safety when used near cosmetics such as cosmetics.

【0004】そこで、従来は板状合成フッ素雲母粉体の
水中でのフッ素溶出量を抑えるために、従来の製造方法
で得られた板状合成フッ素雲母粉体を焼成することで過
剰なフッ素を飛ばしてフッ素の溶出量を抑えていた。
Therefore, conventionally, in order to suppress the elution amount of fluorine in the plate-like synthetic fluoromica powder in water, the plate-like synthetic fluoromica powder obtained by the conventional manufacturing method is fired to remove excess fluorine. The amount of elution of fluorine was suppressed by skipping.

【0005】[0005]

【発明が解決しようとする課題】しかし、このような従
来の製造方法で得られる板状化合物の形状は、図2に示
すように端面側に向かい段差を有し、端面側には不揃い
な凸凹が生じている。そして、このように段差や凹凸が
あると、層面の平滑性が損なわれてしまい、粉体の滑り
のよさ等の特性に影響してしまうという問題があった。
また、現状の製造法では平滑性のある粒子含有量を増や
し、滑り性を改良すると、光沢値も同時に高くなるた
め、低光沢で滑りの良い粉体を得ることは困難である。
However, the shape of the plate-like compound obtained by such a conventional manufacturing method has a step toward the end face side as shown in FIG. 2, and the unevenness is uneven on the end face side. Is occurring. If there is such a step or unevenness, there is a problem that the smoothness of the layer surface is impaired and the characteristics such as the smoothness of the powder are affected.
Further, in the present production method, when the content of particles having smoothness is increased and the slipperiness is improved, the gloss value is also increased at the same time, so it is difficult to obtain a powder having low gloss and good slipperiness.

【0006】また、従来の製造方法で得られた板状合成
フッ素雲母粉体を焼成処理した後も、過酷溶出試験法に
よるフッ素溶出量として、13〜20ppmのフッ素が
粉体から溶出する。そこで、化粧品等の人体に近いとこ
ろで使用されることを考慮すれば、フッ素の溶出量が極
力少ない板状合成フッ素雲母が求められていた。本発明
は前記従来技術の問題に鑑みなされたものであり、その
目的は板状粒子の平滑性が高く、低光沢で、且つ粉体の
安全性が高い板状結晶化合物粉体及びその製造方法を提
供することにある。
Further, even after the plate-like synthetic fluoromica powder obtained by the conventional manufacturing method is subjected to the firing treatment, 13-20 ppm of fluorine is eluted from the powder as a fluorine elution amount by the severe elution test method. Therefore, in consideration of being used in the vicinity of the human body such as cosmetics, there has been a demand for a plate-like synthetic fluoromica that has the least amount of fluorine elution. The present invention has been made in view of the above-mentioned problems of the prior art, and an object thereof is a plate-like crystalline compound powder having high smoothness of plate-like particles, low gloss, and high safety of powder, and a production method thereof. To provide.

【0007】[0007]

【課題を解決するための手段】前記目的を達成するため
に本発明者らは鋭意検討した結果、高圧系ホモジナイザ
ーを用いて差圧100kg/cm以上で粉砕すること
で、平滑性が高く低光沢な板状化合物が得られることを
見出した。また、結晶物質として合成フッ素雲母を用い
た場合には、さらに500〜1200℃で熱処理を行う
ことでフッ素溶出量が10ppm未満の板状合成フッ素
雲母が得られることを見出し本発明を完成するに至っ
た。すなわち、本発明にかかる板状化合物粉体は、端面
の厚み/層面中央部の厚みが0.9〜1.0である板状
化合物を60%以上含むことを特徴とする。
Means for Solving the Problems As a result of intensive studies made by the present inventors in order to achieve the above-mentioned object, it was found that by pulverizing with a high pressure homogenizer at a differential pressure of 100 kg / cm 2 or more, the smoothness is high and low. It was found that a bright plate-like compound can be obtained. Further, in the case of using synthetic fluoromica as a crystalline substance, it was found that a plate-shaped synthetic fluoromica having a fluorine elution amount of less than 10 ppm can be obtained by further performing heat treatment at 500 to 1200 ° C. I arrived. That is, the plate-like compound powder according to the present invention is characterized by containing 60% or more of a plate-like compound having an end face thickness / layer face center portion thickness of 0.9 to 1.0.

【0008】さらに前記粉体において、以下に記載の光
沢値測定方法による光沢値が3.5以下であることを特
徴とする。 <光沢値の測定方法>白のボール紙上に、約5〜6cm
の長さに切った両面テープを貼り付ける。両面テープの
上に、約5〜6cmに切ったセロテープを、粘着面を上
にして両面テープとセロテープの間に空気が入らないよ
うに貼り付ける。セロテープの上に余剰の粉体を乗せて
から、化粧品用ハケで、同一方向に10回馴らす。セロ
テープ上及びハケに付いた余分な粉体を払い落としてか
ら、さらに10回同じ方向にハケで馴らす。馴らした方
向に入射→反射が起こるようにして、光沢計(日本電色
工業(株)製「VG−2PD」)で測定する。入射−反
射角は、60度−60度とする。なお、光沢計のゼロ点
及びスパンの調整は、一連の測定毎に一回、測定前に必
ず行う。スパンの調整は、光沢値89の反射板を使用す
る。
Further, the above-mentioned powder is characterized by having a gloss value of 3.5 or less by a gloss value measuring method described below. <Measurement method of gloss value> About 5-6 cm on white cardboard
Stick the double-sided tape cut to the length of. On the double-sided tape, a piece of cellophane tape cut into about 5 to 6 cm is attached with the adhesive surface facing up so that air does not enter between the double-sided tape and the piece of cellophane tape. Place excess powder on top of cellophane tape and apply it 10 times in the same direction with a cosmetic brush. Brush off excess powder on the cellophane tape and on the brush, and apply it 10 times in the same direction with a brush. It is measured with a gloss meter (“VG-2PD” manufactured by Nippon Denshoku Industries Co., Ltd.) so that incident light → reflection occurs in a familiar direction. The incident-reflection angle is 60 ° -60 °. The zero point and span of the gloss meter must be adjusted once for each series of measurements and before the measurement. For the adjustment of the span, a reflector having a gloss value of 89 is used.

【0009】また、本発明にかかる板状合成フッ素雲母
粉体は、過酷溶出試験法による水中でのフッ素溶出量が
10ppm未満であることを特徴とする。また、前記板
状化合物粉体を化粧料に配合するすることが好適であ
る。
Further, the plate-like synthetic fluoromica powder according to the present invention is characterized in that the elution amount of fluorine in water by the severe elution test method is less than 10 ppm. In addition, it is preferable to mix the plate-like compound powder with a cosmetic.

【0010】また、本発明の板状化合物粉体の製造方法
は、高圧系ホモジナイザーを用いて原料の板状化合物粉
体を、差圧100kg/cm以上で粉砕する粉砕工程
を含むことを特徴とする。
Further, the method for producing a plate-like compound powder of the present invention is characterized by including a pulverizing step of pulverizing the plate-like compound powder as a raw material with a high pressure homogenizer at a differential pressure of 100 kg / cm 2 or more. And

【0011】また、本発明の板状合成フッ素雲母粉体の
製造方法は、高圧系ホモジナイザーを用いて原料の板状
合成フッ素雲母粉体を、差圧100kg/cm以上で
粉砕する粉砕工程と、前記粉砕工程の後に500〜12
00℃で熱処理する熱処理工程を含むことを特徴とす
る。
Further, the method for producing a plate-like synthetic fluoromica powder of the present invention comprises a pulverizing step of using a high-pressure homogenizer to pulverize the raw plate-like synthetic fluoromica powder at a differential pressure of 100 kg / cm 2 or more. , 500 to 12 after the crushing step
It is characterized by including a heat treatment step of heat treatment at 00 ° C.

【0012】[0012]

【発明の実施の形態】本発明の板状化合物は、アスペク
ト比10以上の形状の板状化合物を原料として製造され
る。板状化合物を構成する物質としては、アパタイト、
コランダム、クリストバライト等の天然に産出する鉱物
の他、マイカ、タルク、パイロフィライト等の天然もし
くは合成の層状ケイ酸塩、または水酸化アルミニウム、
酸化アルミニウム、ガラスフレーク等の人工物質などが
使用できる。
BEST MODE FOR CARRYING OUT THE INVENTION The plate-like compound of the present invention is produced using a plate-like compound having an aspect ratio of 10 or more as a raw material. As a substance that constitutes the plate-like compound, apatite,
In addition to naturally occurring minerals such as corundum and cristobalite, natural or synthetic layered silicates such as mica, talc and pyrophyllite, or aluminum hydroxide,
Artificial substances such as aluminum oxide and glass flakes can be used.

【0013】前記板状化合物を高圧系ホモジナイザーを
用いて差圧100kg/cm以上、好ましくは300
kg/cm以上の圧力降下をかけることで粒子は加速
され、そのときにかかるせん断力、加速した粒子を壁面
もしくは液体同士でぶつけることによる衝撃力で原料の
板状化合物を粉砕する。そのとき原料の板状化合物は、
急激な圧力降下、せん断力、衝撃力によって面方向での
割れにより微粒子化する。それと共に、急激な圧力降
下、せん断力によって粒子表面の凹凸を剥がすことで、
図2に示すような通常の板状結晶に見られる層面の段差
や端面の不揃いな凹凸は取り除かれ、図1に示すような
略平板状になると考えられる。
The plate-like compound is subjected to a differential pressure of 100 kg / cm 2 or more, preferably 300 using a high-pressure homogenizer.
The particles are accelerated by applying a pressure drop of not less than kg / cm 2 , and the plate-like compound of the raw material is crushed by the shearing force applied at that time and the impact force caused by the accelerated particles colliding with the wall surface or liquids. At that time, the plate-shaped compound of the raw material is
Sudden pressure drop, shearing force, and impact force cause cracks in the surface direction to form fine particles. At the same time, by removing the irregularities on the particle surface by a sudden pressure drop and shearing force,
It is considered that the steps of the layer surfaces and the unevenness of the end faces, which are seen in a normal plate crystal as shown in FIG. 2, are removed, and the plate has a substantially flat plate shape as shown in FIG.

【0014】ここで板状化合物の粉砕に用いられる高圧
系ホモジナイザーは、増圧ポンプと、チャンバーまたは
ユニットと呼ばれる微細なオリフィス管によって構成さ
れる。微細なオリフィス管の管径は、処理前後の物質の
特性を考慮して適宜決定される。高圧系ホモジナイザー
は、キャビテーション、衝撃力、剪断力を粉砕の要素と
するものであり、これらの相互作用により粉砕処理後の
粒子が得られる。以下、これらの各要素について説明す
る。
The high-pressure homogenizer used for pulverizing the plate-like compound is composed of a booster pump and a fine orifice tube called a chamber or unit. The diameter of the fine orifice tube is appropriately determined in consideration of the characteristics of the substance before and after the treatment. The high-pressure homogenizer uses cavitation, impact force, and shearing force as elements for pulverization, and the interaction between these produces particles after pulverization. Each of these elements will be described below.

【0015】キャビテーション キャビテーションは、流体の速い流れと共に高圧下とな
った状態からの開放により液体に圧力降下が起きて、発
生する気泡である。液体は、圧力が下がれば気化しやす
くなり、1atm、100℃で沸騰する水も0.03a
tmになると沸点は15℃になる。急激な圧力降下を起
こした液体は、蒸気となり水中で気泡を形成し、気泡
は、圧力が元に戻れば、破壊する。このとき、数千度以
上、1000気圧以上の衝撃力を発生する。高圧系ホモ
ジナイザーは、液体を微細なオリフィス管内に高速で、
しかも高圧な状態で流す機構である。そのため、オリフ
ィス管内(液体の高速流動)、オリフィス管出口(液体
の圧力降下)でキャビテーションが起こり、液体中に混
在する物質に大きな衝撃力を与えることができ、粉砕ま
たは剥離、混合、分散の力が働く。
[0015]Cavitation Cavitation is not under high pressure with the rapid flow of fluid.
The pressure drops in the liquid due to the release from the
It is a growing bubble. Liquids tend to vaporize if the pressure drops
It will become 0.03a even if water boils at 1 atm and 100 ° C.
At tm, the boiling point is 15 ° C. Cause a sudden pressure drop
The rubbed liquid becomes vapor and forms bubbles in the water.
Destroys when the pressure returns. At this time, several thousand degrees or more
In addition, an impact force of 1000 atm or more is generated. High pressure system homo
The Genizer is designed to move liquid into a fine orifice tube at high speed.
Moreover, it is a mechanism for flowing under high pressure. Therefore, Orif
Inside the gas pipe (high-speed liquid flow), orifice pipe outlet (liquid
Cavitation occurs due to the pressure drop) and mixes in the liquid.
It can give a great impact to existing substances and
Also, the force of peeling, mixing, and dispersion works.

【0016】衝撃力 チャンバーまたはユニットと呼ばれる部分の微細なオリ
フィス管の形状は、処理する液により変更可能である。
液体同士を衝突させる場合には、管を2方向に分岐させ
た後、1経路に収束させる。衝突する液体同士には衝撃
が加わり、混在する物質に粉砕または剥離、混合、分散
の力が働く。また、オリフィス管経路に角度をつけるこ
とで液体を壁面に衝突させ、衝撃力を加える方法によっ
ても上記のような効果を得ることができる。
[0016]Impact force A fine orientation of a part called a chamber or unit
The shape of the fiss tube can be changed depending on the liquid to be treated.
When colliding liquids with each other, divide the pipe into two directions.
After that, it converges on one path. Impact between colliding liquids
Addition, crushing or exfoliating, mixing, dispersing to mixed substances
The power of works. Also, make an angle to the orifice pipe path.
With the method of colliding the liquid with the wall surface and applying an impact force,
However, the above effects can be obtained.

【0017】せん断力 微細なオリフィス管を液体が高速移動することで、液体
中に混在する物質も高速移動する。流れには部分的速度
差が生じるため、混在物質に剪断力が加わる。また、混
在物質同士の擦れ合いによってもずり応力と共に剪断力
が働き、液体中に混在する物質を粉砕または剥離、混
合、分散する。
[0017]Shear force The liquid moves at high speed through a fine orifice pipe,
The substances mixed in the material also move at high speed. Partial velocity in the flow
Due to the difference, a shear force is applied to the mixed material. In addition,
Shear force as well as shear stress due to rubbing between existing substances
Works, crushing or peeling off substances mixed in the liquid, mixing
If so, disperse.

【0018】高圧系ホモジナイザーの上記した作用によ
り得られた板状化合物粉体は低光沢でありながら、その
平滑性から粉体の滑りが向上する。また、粒子表面の活
性が低減していると予想され、凝集もおこりにくく、発
生したとしても容易に凝集を解くことができる。さら
に、従来の製法に比較して、本発明の製法で得られた粉
体は、粒度分布の分散が非常に小さいので、分級後に高
い収率を示し、工業的に効果が大きい。以上の特性から
この板状化合物粉体は化粧品の原料、樹脂への充填剤、
パール光沢顔料等広い用途に好適である。
The plate-like compound powder obtained by the above-described action of the high-pressure homogenizer has low gloss, but its smoothness improves the sliding of the powder. In addition, it is expected that the activity of the particle surface is reduced, aggregation is unlikely to occur, and even if it occurs, the aggregation can be easily released. Further, the powder obtained by the production method of the present invention has a very small dispersion of the particle size distribution as compared with the conventional production method, and therefore exhibits a high yield after classification and is industrially effective. From the above characteristics, the plate-like compound powder is a raw material for cosmetics, a filler for resin,
Suitable for a wide range of applications such as pearlescent pigments.

【0019】また、原料の板状化合物として板状合成フ
ッ素雲母を用い、高圧系ホモジナイザーを用いて差圧1
00kg/cm以上、好ましくは500kg/cm
以上の圧力降下をかけることで、高圧系ホモジナイザー
による処理過程で合成フッ素雲母の表面近くにある溶出
しやすいフッ素の相当量が水中に溶かし出される。これ
は、キャビテーションによる加熱効果と衝撃力、加速さ
れた粒子にかかるせん断力、加速した粒子を壁面もしく
は液体同士でぶつけることによる衝撃力等によると考え
られる。そして、処理後のスラリーを分級して乾燥し、
500〜1200℃で熱処理することで、後述の過酷溶
出試験法による水中でのフッ素溶出量を10ppm未満
に抑えた板状合成フッ素雲母粉体が得られる。
A plate-like synthetic fluoromica is used as a plate-like compound as a raw material, and a differential pressure of 1 is obtained by using a high-pressure homogenizer.
00kg / cm 2 or more, preferably 500 kg / cm 2
By applying the above-mentioned pressure drop, a considerable amount of fluorine, which is easily eluted near the surface of the synthetic fluoromica during the treatment process by the high-pressure homogenizer, is dissolved in water. It is considered that this is due to the heating effect and impact force due to cavitation, the shearing force applied to the accelerated particles, the impact force caused by the accelerated particles hitting the wall surface or the liquids, and the like. Then, the treated slurry is classified and dried,
By heat treatment at 500 to 1200 ° C., a plate-like synthetic fluoromica powder having an elution amount of fluorine in water suppressed to less than 10 ppm by a later-described severe elution test method can be obtained.

【0020】このような板状合成フッ素雲母粉体の製造
方法によれば、従来の焼成工程でフッ素溶出量を大幅に
抑えることが可能となり、工業的に効果が大きい。ま
た、このようにして得られた板状合成フッ素雲母粉体
は、その低いフッ素溶出量から化粧品のファンデーショ
ン、口紅、クリーム等の用途に好適である。
According to such a method for producing a plate-like synthetic fluoromica powder, it is possible to significantly suppress the amount of fluorine elution in the conventional firing step, which is industrially effective. Further, the plate-like synthetic fluoromica powder thus obtained is suitable for applications such as foundations for cosmetics, lipsticks, creams, etc. due to its low fluorine elution amount.

【0021】[0021]

【実施例】以下、実施例により本発明を詳細に説明する
が、本発明はこれら実施例に限定されるものではない。実施例1 初期平均粒子径48.47μmの合成フッ素金雲母の1
0%懸濁液をみずほ工業株式会社製マイクロフルイダイ
ザーM−210EH型を用いて粉砕した。粉砕条件は差
圧1500kg/cm、流量分速1.0リットル、Z
チャンバー(加速した粒子を壁面にぶつけて粉砕するチ
ャンバー)で処理した。その結果、粒径14.87μm
(σ2.36μm)に粉砕された。粉砕後、分級して得
られた平均粒子径12μmの粒子を走査型電子顕微鏡で
観察した。その写真を図3((A)面方向、(B)端面
方向)に、また、端面の厚み/層面中央部の厚みの平均
と、端面の厚み/層面中央部の厚みが0.9〜1.0の
粒子の含有量、及び粉体の光沢値を表1に示す。なお、
端面の厚み/層面中央部の厚みの平均と端面の厚み/層
面中央部の厚みが0.9〜1.0の粒子の含有量は、走
査型電子顕微鏡により得られた粒子の写真をn数50で
観察し、算出したものである。また、粉体の光沢値は以
下の方法で測定した。
The present invention will be described in detail below with reference to examples.
However, the present invention is not limited to these examples.Example 1 1 of synthetic fluorophlogopite with an initial average particle size of 48.47 μm
0% suspension made by Mizuho Kogyo Co., Ltd.
It was crushed using a Z-M-210EH type. Grinding conditions are different
Pressure 1500kg / cmTwo, Flow rate 1.0 liter per minute, Z
Chamber (a chamber that crushes accelerated particles against the wall to crush them)
Process). As a result, the particle size is 14.87 μm
It was pulverized to (σ 2.36 μm). After grinding, classify and obtain
Scanning electron microscope was used to
I observed. The photograph is shown in Fig. 3 ((A) plane direction, (B) end face)
Direction), and the average of the thickness of the end face / the thickness of the center of the layer face
And the thickness of the end face / the thickness of the central part of the layer face is 0.9 to 1.0
Table 1 shows the content of the particles and the gloss value of the powder. In addition,
End face thickness / layer Average of center face thickness and end face thickness / layer
The content of particles having a thickness of 0.9 to 1.0 in the center of the surface is
Photograph of particles obtained by a scanning electron microscope with n number of 50
Observed and calculated. In addition, the gloss value of the powder is
It was measured by the following method.

【0022】<光沢値の測定方法>白のボール紙上に、
約5〜6cmの長さに切った両面テープを貼り付ける。
両面テープの上に、約5〜6cmに切ったセロテープ
を、粘着面を上にして貼り付ける。この時両面テープと
セロテープの間に空気が入らないように注意する。ま
た、セロテープの粘着面を荒らさないように注意して行
う。セロテープの上に余剰の粉体を乗せてから、化粧品
用ハケで、同一方向に10回馴らす。セロテープ上及び
ハケに付いた余分な粉体を払い落としてから、さらに1
0回同じ方向にハケで馴らす。馴らした方向に入射→反
射が起こるようにして、光沢計(日本電色工業(株)製
「VG−2PD」)で測定する。入射−反射角は、60
度−60度とする。なお、光沢計のゼロ点及びスパンの
調整は、一連の測定毎に一回、測定前に必ず行う。スパ
ンの調整は、光沢値89の反射板を使用する。
<Measurement method of gloss value> On a white cardboard,
Stick double-sided tape cut to a length of about 5-6 cm.
On the double-sided tape, a cellophane tape cut into about 5 to 6 cm is attached with the adhesive side up. At this time, be careful not to let air enter between the double-sided tape and the cellophane tape. Also, be careful not to damage the adhesive surface of the cellophane tape. Place excess powder on top of cellophane tape and apply it 10 times in the same direction with a cosmetic brush. After removing the excess powder on the tape and brush, 1 more
Break in 0 times in the same direction. It is measured with a gloss meter (“VG-2PD” manufactured by Nippon Denshoku Industries Co., Ltd.) so that incident light → reflection occurs in a familiar direction. The incident-reflection angle is 60
The degree is -60 degrees. The zero point and span of the gloss meter must be adjusted once for each series of measurements and before the measurement. For the adjustment of the span, a reflector having a gloss value of 89 is used.

【0023】実施例2 実施例1と同様の合成フッ素金雲母20%懸濁液を実施
例1と同じ条件で粉砕、分級を行った。その結果、粒径1
2.78μm(σ2.16μm)に粉砕され、その後の
分級により平均粒子径10μmの粒子を得た。実施例1
と同様の方法で得た端面の厚み/層面中央部の厚みの平
均と、端面の厚み/層面中央部の厚みが0.9〜1.0
の粒子の含有量、及び粉体の光沢値を表1に示す。
[0023]Example 2 A 20% suspension of synthetic fluorophlogopite as in Example 1 was carried out.
Crushing and classification were carried out under the same conditions as in Example 1. As a result, particle size 1
Crushed to 2.78 μm (σ2.16 μm)
Particles having an average particle diameter of 10 μm were obtained by classification. Example 1
Thickness of end face / thickness of center of layer face obtained by the same method as
Evenly, the thickness of the end face / the thickness of the central part of the layer face is 0.9 to 1.0
The content of the particles and the gloss value of the powder are shown in Table 1.

【0024】実施例3 実施例1と同様の合成フッ素金雲母10%懸濁液を、差
圧を2100kg/cmに変え、それ以外は同じ条件
で粉砕、分級を行った。その結果、粒径11.55μm
(σ2.03μm)に粉砕され、その後の分級により平
均粒子径10μmの粒子を得た。実施例1と同様の方法
で得た端面の厚み/層面中央部の厚みの平均と、端面の
厚み/層面中央部の厚みが0.9〜1.0の粒子の含有
量、及び粉体の光沢値を表1に示す。
[0024]Example 3 A synthetic fluorophlogopite 10% suspension similar to that of Example 1 was
Pressure is 2100kg / cmTwoThe same conditions other than that
Was pulverized and classified. As a result, the particle size is 11.55 μm
(Σ 2.03 μm) and then flattened by subsequent classification
Particles having a uniform particle diameter of 10 μm were obtained. The same method as in Example 1
The average of the thickness of the end face / the thickness of the central part of the layer face obtained in
Containing particles having a thickness / thickness at the center of the layer surface of 0.9 to 1.0
The amount and the gloss value of the powder are shown in Table 1.

【0025】実施例4 初期平均粒子径32.15μmの天然タルク10%懸濁
液を実施例1と同じ条件で粉砕、分級を行った。その結
果、粒径12.16μm(σ1.76μm)に粉砕さ
れ、その後の分級により平均粒子径13μmの粒子を得
た。実施例1と同様の方法で得た端面の厚み/層面中央
部の厚みの平均と、端面の厚み/層面中央部の厚みが
0.9〜1.0の粒子の含有量、及び粉体の光沢値を表
1に示す。
[0025]Example 4 10% suspension of natural talc with an initial average particle size of 32.15 μm
The liquid was pulverized and classified under the same conditions as in Example 1. That conclusion
Fruit, crushed to a particle size of 12.16 μm (σ 1.76 μm)
Then, by classification, particles having an average particle diameter of 13 μm are obtained.
It was End face thickness / layer face center obtained by the same method as in Example 1
The average of the thickness of the part and the thickness of the end face / the thickness of the central part of the layer surface are
The particle content of 0.9 to 1.0 and the gloss value of the powder are displayed.
Shown in 1.

【0026】実施例5 初期平均粒子径36.05μmの合成フッ素金雲母の1
0%懸濁液を株式会社ジーナス社製ジェットミルジーナ
スPYPRE03−15型を用いて粉砕した。粉砕条件
は差圧2200kg/cm、流量分速0.30リット
ル、ジーナスPYユニット(液相ジェット流を発生さ
せ、ジェット流同士を衝突させて微粒化を行うユニッ
ト)で処理した。その結果、粒径14.87μm(σ1.
80μm)に粉砕され、その後の分級により平均粒子径
13μmの粒子を得た。実施例1と同様の方法で得た端
面の厚み/層面中央部の厚みの平均と、端面の厚み/層
面中央部の厚みが0.9〜1.0の粒子の含有量、及び
粉体の光沢値を表1に示す。
[0026]Example 5 1 of synthetic fluorophlogopite with an initial average particle size of 36.05 μm
Jet Mill Gena made by Genus Corporation with 0% suspension
It was pulverized using a PYPRE03-15 type. Grinding conditions
Is a differential pressure of 2200 kg / cmTwo, Flow rate per minute 0.30 lit
Le Genus PY unit
The jet streams to collide with each other for atomization.
Process). As a result, the particle size is 14.87 μm (σ1.
80 μm) and then classified to obtain an average particle size
13 μm particles were obtained. Edge obtained by the same method as in Example 1
Surface thickness / layer Average of center surface thickness and end face thickness / layer
Content of particles having a thickness of 0.9 to 1.0 in the center of the plane, and
The gloss value of the powder is shown in Table 1.

【0027】実施例6 実施例5と同様の合成フッ素金雲母20%懸濁液を粉砕
条件のみ350kg/cmとし、他条件は実施例5と
同じにして粉砕、分級を行った。その結果、粒径27.1
8μm(σ1.55μm)に粉砕され、その後の分級に
より平均粒子径25μmの粒子を得た。処理後の粒子を
走査型電子顕微鏡で観察した。その代表的な写真を図4
((A)面方向、(B)端面方向)に、また実施例1と
同様の方法で得た端面の厚み/層面中央部の厚みの平均
と、端面の厚み/層面中央部の厚みが0.9〜1.0の
粒子の含有量、及び粉体の光沢値を表1に示す。
[0027]Example 6 A 20% suspension of synthetic fluorophlogopite similar to that in Example 5 was ground.
Condition only 350kg / cmTwoAnd other conditions are as in Example 5.
Grinding and classification were performed in the same manner. As a result, the particle size is 27.1.
It is crushed to 8 μm (σ1.55 μm) and then classified.
Thus, particles having an average particle diameter of 25 μm were obtained. The treated particles
It was observed with a scanning electron microscope. Figure 4 shows a representative photograph
((A) surface direction, (B) end surface direction) and Example 1
Average of end face thickness / layer center thickness obtained by the same method
And the thickness of the end face / the thickness of the central part of the layer face is 0.9 to 1.0
Table 1 shows the content of the particles and the gloss value of the powder.

【0028】比較例1 実施例1と同様の合成フッ素金雲母10%懸濁液1リッ
トルをボールミルを用いて6時間かけて粉砕した。その
結果、粒径11.98μm(σ4.36μm)に粉砕さ
れ、その後の分級により平均粒子径11μmの粒子を得
た。処理後粒子を走査型電子顕微鏡で観察した。その写
真を図5((A)面方向、(B)端面方向)に、また実
施例1と同様の方法で得た端面の厚み/層面中央部の厚
みの平均と、端面の厚み/層面中央部の厚みが0.9〜
1.0の粒子の含有量、及び粉体の光沢値を表1に示
す。
[0028]Comparative Example 1 A synthetic fluorine phlogopite 10% suspension 1 liter similar to that of Example 1
The tor was crushed using a ball mill for 6 hours. That
As a result, it was crushed to a particle size of 11.98 μm (σ 4.36 μm).
And then classify to obtain particles with an average particle size of 11 μm.
It was The treated particles were observed with a scanning electron microscope. That copy
The true is shown in Fig. 5 ((A) surface direction, (B) end surface direction) and again
Thickness of end face / thickness of central part of layer face obtained by the same method as in Example 1
Average and the thickness of the end face / thickness of the center of the layer face is 0.9 to
The particle content of 1.0 and the gloss value of the powder are shown in Table 1.
You

【0029】比較例2 実施例4と同様の天然タルク10%懸濁液1リットルを
ボールミルを用いて6時間かけて粉砕した。その結果、
粒径10.12μm(σ3.92μm)に粉砕され、そ
の後の分級により平均粒子径11μmの粒子を得た。実
施例1と同様の方法で得た端面の厚み/層面中央部の厚
みの平均と、端面の厚み/層面中央部の厚みが0.9〜
1.0の粒子の含有量、及び粉体の光沢値を表1に示
す。。
[0029]Comparative example 2 1 liter of 10% natural talc suspension as in Example 4
It pulverized for 6 hours using a ball mill. as a result,
Particle size 10.12 μm (σ3.92 μm)
Particles having an average particle diameter of 11 μm were obtained by the subsequent classification. Fruit
Thickness of end face / thickness of central part of layer face obtained by the same method as in Example 1
Average and the thickness of the end face / thickness of the center of the layer face is 0.9 to
The particle content of 1.0 and the gloss value of the powder are shown in Table 1.
You .

【0030】比較例3 合成された板状アルミニウム粉体を比較例1と同じ条件
で粉砕した。その結果、粒径23μm(σ3.36μ
m)に粉砕され、その後の分級により平均粒子径25μ
mの粒子を得た。実施例1と同様の方法で得た端面の厚
み/層面中央部の厚みの平均と、端面の厚み/層面中央
部の厚みが0.9〜1.0の粒子の含有量、及び粉体の
光沢値を表1に示す。
[0030]Comparative Example 3 The synthesized plate-like aluminum powder was treated under the same conditions as in Comparative Example 1.
Crushed with. As a result, the particle size is 23 μm (σ3.36 μ
m) and then classified to have an average particle size of 25μ
m particles were obtained. Thickness of end face obtained by the same method as in Example 1
Average / thickness of center of layer surface and thickness of end face / center of layer surface
Content of particles having a thickness of 0.9 to 1.0, and
The gloss values are shown in Table 1.

【0031】[0031]

【表1】 端面厚み(A) 中央部厚み(B) A/B 含有量 光沢値 (平均値、μm)(平均値、μm) (%) 実施例1 0.09 0.10 0.90 60 3.0 実施例2 0.25 0.27 0.93 70 2.9 実施例3 0.41 0.44 0.93 80 3.3 実施例4 0.55 0.58 0.94 65 3.2 実施例5 0.21 0.22 0.95 70 3.1 実施例6 0.48 0.50 0.96 60 3.4 比較例1 0.38 0.98 0.38 55 4.0 比較例2 0.46 0.94 0.49 40 3.7比較例3 0.25 0.40 0.62 58 5.2 [Table 1]           Edge thickness (A) Central thickness (B) A / B content Gloss value(Average value, μm) (Average value, μm) (%) Example 1 0.09 0.10 0.90 60 3.0 Example 2 0.25 0.27 0.93 70 2.9 Example 3 0.41 0.44 0.93 80 3.3 Example 4 0.55 0.58 0.94 65 3.2 Example 5 0.21 0.22 0.95 70 3.1 Example 6 0.48 0.50 0.96 60 3.4 Comparative Example 1 0.38 0.98 0.38 55 4.0 Comparative Example 2 0.46 0.94 0.49 40 3.7Comparative Example 3 0.25 0.40 0.62 58 5.2

【0032】表1に示した結果より明らかなように、実
施例1〜6はその平滑性において比較例1〜2と比較し
て40〜50%高く、端面の厚み/層面中央部の厚みが
0.9〜1.0である板状化合物を60%以上含む。ま
た、同時にその光沢値が3.5以下と低光沢になってい
る。また、図3及び図4に示した実施例1と実施例6の
走査型電子顕微鏡写真においても、図5に示した比較例
1の走査型電子顕微鏡写真に見られるような端面の凹凸
はほとんど見られない。
As is clear from the results shown in Table 1, the smoothness of Examples 1 to 6 is 40 to 50% higher than that of Comparative Examples 1 to 2, and the thickness of the end face / the thickness of the central portion of the layer face is It contains 60% or more of a plate-like compound of 0.9 to 1.0. At the same time, the gloss value is 3.5 or less, which is low gloss. Also, in the scanning electron micrographs of Example 1 and Example 6 shown in FIGS. 3 and 4, there is almost no unevenness on the end face as seen in the scanning electron micrograph of Comparative Example 1 shown in FIG. can not see.

【0033】さらに、分級前の実施例1〜6のσ(分
散)の値を比較例1〜3のそれと比較すると、実施例1
〜6のσの値は小さく、粒径のばらつきが少ないことが
わかる。すなわち、本発明の製法により得られる板状結
晶化合物粉体では、一定の粒度範囲における収率が向上
していることがわかる。
Further, comparing the value of σ (dispersion) of Examples 1 to 6 before classification with that of Comparative Examples 1 to 3, Example 1
It can be seen that the value of σ of ˜6 is small and the variation in particle size is small. That is, it is understood that the plate-like crystal compound powder obtained by the production method of the present invention has an improved yield in a certain particle size range.

【0034】実施例7 実施例1と同様の合成フッ素金雲母を、実施例1と同じ
条件で粉砕、分級した。得られた合成フッ素金雲母をフ
ィルタープレスによって回収した後、乾燥機中に入れ3
00℃で乾燥させた。乾燥した合成フッ素金雲母を解砕
し、1000℃で1時間熱処理を施して試料を得た。フ
ッ素溶出量の評価は「化粧品種別許可基準」記載の「合
成金雲母 過酷溶出試験法」に基づいて、下記方法によ
って、フッ素溶出量試験を行った。その結果を表2に示
す。
[0034]Example 7 The same synthetic fluorophlogopite as in Example 1 was used as in Example 1.
It was crushed and classified under the conditions. The synthetic fluorophlogopite obtained is
After collecting with a filter press, put it in the dryer 3
It was dried at 00 ° C. Crush dried synthetic phlogopite
Then, heat treatment was performed at 1000 ° C. for 1 hour to obtain a sample. F
The elution amount of fluorine can be evaluated according to the
The method below is based on the "Narushin Mica Severe Dissolution Test Method".
Then, a fluorine elution amount test was conducted. The results are shown in Table 2.
You

【0035】<過酷溶出試験法>製品5gと蒸留水10
0mlをフラスコに入れ、1時間加熱還流を行った。冷
却後、濾紙及びメンブランフィルターで濾過した。濾液
全量をフッ素試験法に従って蒸留を行い、試験溶液を作
成した。その後のフッ素分析は、ランタン・アリザリン
コンプレキソンを用いた吸光光度法により行った。尚、許
容フッ素溶出量の規格値は、20ppm以下である。
<Severe dissolution test method> 5 g of product and 10 distilled water
0 ml was placed in the flask and heated under reflux for 1 hour. After cooling, it was filtered with a filter paper and a membrane filter. The whole amount of the filtrate was distilled according to the fluorine test method to prepare a test solution. Subsequent fluorine analysis was performed by absorptiometry using lanthanum-alizarin complexone. In addition, the standard value of the allowable fluorine elution amount is 20 ppm or less.

【0036】実施例8 実施例2と同様の合成フッ素金雲母を、実施例2と同じ
条件で粉砕、分級した。得られた合成フッ素金雲母をフ
ィルタープレスによって回収した後、乾燥機中に入れ3
00℃で乾燥させた。乾燥した合成フッ素金雲母を解砕
し、1000℃で1時間熱処理を施して試料を得た。フ
ッ素溶出量の評価は実施例7と同様に行った。結果を表
2に示す。
[0036]Example 8 The same synthetic fluorophlogopite as in Example 2 was used as in Example 2.
It was crushed and classified under the conditions. The synthetic fluorophlogopite obtained is
After collecting with a filter press, put it in the dryer 3
It was dried at 00 ° C. Crush dried synthetic phlogopite
Then, heat treatment was performed at 1000 ° C. for 1 hour to obtain a sample. F
The elution amount of fluorine was evaluated in the same manner as in Example 7. Table of results
2 shows.

【0037】実施例9 実施例3と同様の合成フッ素金雲母を、実施例3と同じ
条件で粉砕、分級した。得られた合成フッ素金雲母をフ
ィルタープレスによって回収した後、乾燥機中に入れ3
00℃で乾燥させた。乾燥した合成フッ素金雲母を解砕
し、1000℃で1時間熱処理を施して試料を得た。フ
ッ素溶出量の評価は実施例7と同様に行った。結果を表
2に示す。
[0037]Example 9 The same synthetic fluorophlogopite as in Example 3 was used as in Example 3.
It was crushed and classified under the conditions. The synthetic fluorophlogopite obtained is
After collecting with a filter press, put it in the dryer 3
It was dried at 00 ° C. Crush dried synthetic phlogopite
Then, heat treatment was performed at 1000 ° C. for 1 hour to obtain a sample. F
The elution amount of fluorine was evaluated in the same manner as in Example 7. Table of results
2 shows.

【0038】比較例4 実施例1と同様の合成フッ素金雲母10%懸濁液1リッ
トルをボールミルを用いて6時間かけて粉砕した。その
結果、粒径は11.98μm(σ4.36μm)に粉砕
され、その後の分級により平均粒子径10μmの粒子を
得た。同フッ素金雲母をフィルタープレスによって回収
した後、乾燥機中に入れ300℃で乾燥させた。乾燥し
た合成フッ素金雲母を解砕し、1000℃で1時間熱処
理を施して試料を得た。フッ素溶出量の評価は実施例7
と同様に行った。結果を表2に示す。
[0038]Comparative Example 4 A synthetic fluorine phlogopite 10% suspension 1 liter similar to that of Example 1
The tor was crushed using a ball mill for 6 hours. That
As a result, the particle size was pulverized to 11.98 μm (σ 4.36 μm)
And then classify particles with an average particle size of 10 μm
Obtained. The fluorophlogopite is collected by a filter press
After that, it was placed in a dryer and dried at 300 ° C. Dried
Synthetic Fluor phlogopite was crushed and heat-treated at 1000 ° C for 1 hour.
A sample was obtained by applying processing. Example 7 was used to evaluate the amount of fluorine elution.
I went the same way. The results are shown in Table 2.

【0039】比較例5 実施例1と同様の合成フッ素金雲母10%懸濁液1リッ
トルをボールミルを用いて6時間かけて粉砕、した。そ
の結果、粒径11.98μm(σ4.36μm)に粉砕
され、その後の分級により平均粒子径13μmの粒子を
得た。同フッ素金雲母をフィルタープレスによって回収
した後、乾燥機中に入れ300℃で乾燥させた。乾燥し
た合成フッ素金雲母を解砕し、1000℃で24時間熱
処理を施したところ、合成フッ素金雲母は焼結してい
た。同焼結体をハンマーで粗砕した後にサンプルミルを
用いて粉砕して試料を得た。同試料はガラス化してお
り、合成フッ素金雲母特有の光沢感はなくなっていた。
フッ素溶出量の評価は実施例7と同様に行った。結果を
表2に示す。
[0039]Comparative Example 5 A synthetic fluorine phlogopite 10% suspension 1 liter similar to that of Example 1
The tor was crushed using a ball mill for 6 hours. So
As a result, crushed to a particle size of 11.98 μm (σ 4.36 μm)
Then, by classification, particles with an average particle size of 13 μm
Obtained. The fluorophlogopite is collected by a filter press
After that, it was placed in a dryer and dried at 300 ° C. Dried
Crush synthetic synthetic phlogopite and heat at 1000 ℃ for 24 hours
After the treatment, the synthetic fluorophlogopite was not sintered.
It was After roughly crushing the sintered body with a hammer,
It was crushed and used to obtain a sample. The sample was vitrified
As a result, the glossiness peculiar to synthetic fluorine phlogopite has disappeared.
Evaluation of the fluorine elution amount was performed in the same manner as in Example 7. The result
It shows in Table 2.

【0040】比較例6 実施例1と同様の合成フッ素金雲母1kgをサンプルミ
ルを用いて粉砕した。その結果、粒径13.12μm
(σ4.75μm)に粉砕され、その後の分級により平
均粒子径11μmの粒子を得た。同フッ素金雲母を電気
炉に入れ1000℃で4時間かけて焼成した。フッ素溶
出量の評価は実施例7と同様に行った。結果を表2に示
す。
[0040]Comparative Example 6 1 kg of synthetic fluorophlogopite as in Example 1 was sampled.
It was crushed using a mill. As a result, the particle size is 13.12 μm
(Σ 4.75 μm) and then flattened by subsequent classification
Particles having a uniform particle diameter of 11 μm were obtained. Electric Fluoro phlogopite
It was placed in a furnace and baked at 1000 ° C. for 4 hours. Fluorine dissolution
The evaluation of the output amount was performed in the same manner as in Example 7. The results are shown in Table 2.
You

【0041】[0041]

【表2】 [Table 2]

【0042】表2に示した結果より明らかなように、各
実施例、比較例について処理前後の粒子径は同程度の条
件であったにもかかわらず実施例7〜9のフッ素溶出量
はいずれも10ppm未満であり、比較例4と比較する
とフッ素溶出量を大幅に抑えていることがわかる。ま
た、比較例6と比較してもフッ素溶出量を約半分にまで
抑えていることがわかる。また、比較例5のようにフッ
素溶出量を低くするために長時間焼成すると、構造が分
解してしまい合成フッ素金雲母ではなくなってしまう。
As is clear from the results shown in Table 2, the fluorine elution amount of each of Examples 7 to 9 was invariable although the particle diameters before and after the treatment were the same in each of the Examples and Comparative Examples. Is also less than 10 ppm, which shows that the amount of fluorine elution is significantly suppressed as compared with Comparative Example 4. Further, it can be seen that the fluorine elution amount is suppressed to about half even when compared with Comparative Example 6. Further, when firing is carried out for a long time in order to reduce the elution amount of fluorine as in Comparative Example 5, the structure is decomposed and synthetic fluorophlogopite is no longer used.

【0043】次に、実施例1または比較例1の合成フッ
素金雲母を用いて下記処方のパウダリーファンデーショ
ンを常法により製造した。パネル10名により、ファン
デーション塗布の際の使用感(塗布のしやすさ)及び塗
布後の仕上がり(マット感)について、以下の評価基準
により評価した。評価基準 ○:実施例1の合成フッ素金雲母を用いた場合(実施例
10)のほうが比較例1の合成フッ素金雲母を用いた場
合(比較例7)に比して塗布のしやすさ及びマット感に
優れると回答したパネルが8名以上。 ×:実施例1の合成フッ素金雲母を用いた場合(実施例
10)のほうが比較例1の合成フッ素金雲母を用いた場
合(比較例7)に比して塗布のしやすさ及びマット感に
優れると回答したパネルが8名未満。 評価結果を表3に示す。
Next, the synthetic foot of Example 1 or Comparative Example 1 was used.
The powdery foundation of the following prescription using elemental mica
Were prepared by conventional methods. Fan by panel 10 people
A feeling of use (easiness of application) and application
Regarding the finish (matte feeling) after cloth, the following evaluation criteria
It was evaluated by.Evaluation criteria ◯: When the synthetic fluorophlogopite of Example 1 was used (Example
10) is the case where the synthetic fluorophlogopite of Comparative Example 1 is used.
Ease of application and matt feeling compared to the case of Comparative Example 7
More than 8 panelists answered that they were excellent. X: When the synthetic fluorophlogopite of Example 1 was used (Example
10) is the case where the synthetic fluorophlogopite of Comparative Example 1 is used.
Ease of application and matt feeling compared to the case of Comparative Example 7
Less than 8 panelists answered excellent. The evaluation results are shown in Table 3.

【0044】[0044]

【表3】 処方 実施例10 比較例7 タルク 20 20 合成フッ素金雲母(実施例1) 35 − 合成フッ素金雲母(比較例1) − 35 カオリン 5 5 二酸化チタン 10 10 雲母チタン 3 3 ステアリン酸亜鉛 1 1 ベンガラ 1 1 黄酸化鉄 3 3 黒酸化鉄 0.2 0.2 ナイロンパウダー 10 10 スクワラン 6 6 酢酸ラノリン 1 1ミリスチン 酸オクチルト゛テ゛シル 2 2シ゛イソオクタン 酸ネオヘ゜ンチルク゛リコール 2 2 モノオレイン酸ソルビタン 0.5 0.5 防腐剤 適量 適量 酸化防止剤 適量 適量香料 適量 適量 塗布のしやすさ及びマット感の上記比較評価:○ [Table 3]Prescription Example 10 Comparative Example 7 Talc 20 20 Synthetic Fluoro phlogopite (Example 1) 35 − Synthetic Fluor phlogopite (Comparative Example 1) -35 Kaolin 5 5 Titanium dioxide 10 10 Mica titanium 3 3 Zinc stearate 11 Bengal 1 1 Yellow iron oxide 33 Black iron oxide 0.2 0.2 Nylon powder 10 10 Squalane 6 6 Lanolin acetate 11 myristin Acid Octyl Tedecyl 222 Diisooctane Acid neopentyl glycol 2 2 Sorbitan monooleate 0.5 0.5 Preservative Suitable amount Suitable amount Antioxidant Proper amount Proper amountPerfume Suitable amount Suitable amount The above comparative evaluation of ease of application and matt feeling: ○

【0045】表3の結果より明らかなように、実施例1
の合成フッ素金雲母を用いた場合には、その平滑性、低
光沢性により塗布感及びファンデーションのマットな仕
上がり感に優れている。
As is clear from the results shown in Table 3, Example 1
When the synthetic fluorine phlogopite is used, the smoothness and low gloss are excellent in application feeling and matte finish of foundation.

【0046】[0046]

【発明の効果】以上説明したように本発明にかかる板状
結晶化合物粉体及びその製造方法によれば、板状粒子の
平滑性が高く、低光沢な板状化合物粉体が得られ、また
粉体の安全性が高い板状合成フッ素雲母粉体が得られ
る。
As described above, according to the plate crystal compound powder and the method for producing the same according to the present invention, a plate compound powder having high smoothness of plate particles and low gloss, and A plate-like synthetic fluoromica powder having high powder safety can be obtained.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明の板状結晶化合物粉体の説明図である。FIG. 1 is an explanatory view of a plate crystal compound powder of the present invention.

【図2】従来の板状結晶化合物粉体の説明図である。FIG. 2 is an explanatory view of a conventional plate crystal compound powder.

【図3】本発明の製造方法により得られた板状結晶化合
物粉体の走査型電子顕微鏡写真である。
FIG. 3 is a scanning electron micrograph of plate crystal compound powder obtained by the production method of the present invention.

【図4】本発明の製造方法により得られた板状結晶化合
物粉体の走査型電子顕微鏡写真である。
FIG. 4 is a scanning electron micrograph of a plate-like crystalline compound powder obtained by the production method of the present invention.

【図5】本発明外の製造方法により得られた板状結晶化
合物粉体の走査型電子顕微鏡写真である。
FIG. 5 is a scanning electron micrograph of a plate-shaped crystal compound powder obtained by a production method other than the present invention.

───────────────────────────────────────────────────── フロントページの続き (72)発明者 林 剛芳 東京都千代田区四番町5番地9 トピー工 業株式会社内 Fターム(参考) 4C083 AB212 AB232 AB242 AB431 AB432 AB442 AC022 AC242 AC352 AC392 AC442 AD072 AD512 BB26 CC01 CC12 DD17 EE06 EE07 EE10 FF01 4G073 BD21 CM22 FD24 FD25 GA34 UB31    ─────────────────────────────────────────────────── ─── Continued front page    (72) Inventor Takeyoshi Hayashi             9 Topy work, 5-4 Yonbancho, Chiyoda-ku, Tokyo             Business F-term (reference) 4C083 AB212 AB232 AB242 AB431                       AB432 AB442 AC022 AC242                       AC352 AC392 AC442 AD072                       AD512 BB26 CC01 CC12                       DD17 EE06 EE07 EE10 FF01                 4G073 BD21 CM22 FD24 FD25 GA34                       UB31

Claims (6)

【特許請求の範囲】[Claims] 【請求項1】 端面の厚み/層面中央部の厚みが0.9
〜1.0である板状化合物を60%以上含むことを特徴
とする板状化合物粉体。
1. The thickness of the end surface / the thickness of the central portion of the layer surface is 0.9.
A plate-like compound powder containing 60% or more of a plate-like compound having an amount of 1.0.
【請求項2】 請求項1記載の粉体において、以下に記
載の光沢値測定方法による光沢値が3.5以下であるこ
とを特徴とする板状化合物粉体。 <光沢値の測定方法>白のボール紙上に、約5〜6cm
の長さに切った両面テープを貼り付ける。両面テープの
上に、約5〜6cmに切ったセロテープ(登録商標)
を、粘着面を上にして両面テープとセロテープの間に空
気が入らないように貼り付ける。セロテープの上に余剰
の粉体を乗せてから、化粧品用ハケで、同一方向に10
回馴らす。セロテープ上及びハケに付いた余分な粉体を
払い落としてから、さらに10回同じ方向にハケで馴ら
す。馴らした方向に入射→反射が起こるようにして、光
沢計(日本電色工業(株)製「VG−2PD」)で測定
する。入射−反射角は、60度−60度とする。なお、
光沢計のゼロ点及びスパンの調整は、一連の測定毎に一
回、測定前に必ず行う。スパンの調整は、光沢値89の
反射板を使用する。
2. The plate-like compound powder according to claim 1, which has a gloss value of 3.5 or less according to the gloss value measuring method described below. <Measurement method of gloss value> About 5-6 cm on white cardboard
Stick the double-sided tape cut to the length of. Cellotape (registered trademark) cut into about 5-6 cm on double-sided tape
, With the adhesive side facing up, between the double-sided tape and cellophane tape so that air does not enter. Put excess powder on top of cellophane tape, then use a brush for cosmetics in the same direction 10
Acclimate. Brush off excess powder on the cellophane tape and on the brush, and apply it 10 times in the same direction with a brush. It is measured with a gloss meter (“VG-2PD” manufactured by Nippon Denshoku Industries Co., Ltd.) so that incident light → reflection occurs in a familiar direction. The incident-reflection angle is 60 ° -60 °. In addition,
Make sure to adjust the zero point and span of the gloss meter once for each series of measurements and before measurement. For the adjustment of the span, a reflector having a gloss value of 89 is used.
【請求項3】 過酷溶出試験法による水中でのフッ素溶
出量が10ppm未満であることを特徴とする請求項1
又は2記載の板状合成フッ素雲母粉体。
3. The fluorine elution amount in water according to the severe elution test method is less than 10 ppm.
Or the plate-like synthetic fluoromica powder according to 2.
【請求項4】 請求項1〜3のいずれかに記載の板状化
合物粉体を含有することを特徴とする化粧料。
4. A cosmetic containing the plate-like compound powder according to claim 1.
【請求項5】 高圧系ホモジナイザーを用いて原料の板
状化合物粉体を、差圧100kg/cm以上で粉砕す
る粉砕工程を含むことを特徴とする板状化合物粉体の製
造方法。
5. A method for producing a plate-shaped compound powder, comprising a pulverization step of pulverizing a raw material plate-shaped compound powder using a high-pressure homogenizer at a differential pressure of 100 kg / cm 2 or more.
【請求項6】 高圧系ホモジナイザーを用いて原料の板
状合成フッ素雲母粉体を、差圧100kg/cm以上
で粉砕する粉砕工程と、前記粉砕工程の後に500〜1
200℃で熱処理する熱処理工程を含むことを特徴とす
る板状合成フッ素雲母粉体の製造方法。
6. A pulverization step of pulverizing a raw material plate-like synthetic fluoromica powder using a high-pressure homogenizer at a differential pressure of 100 kg / cm 2 or more, and 500 to 1 after the pulverization step.
A method for producing a plate-like synthetic fluoromica powder, comprising a heat treatment step of heat treatment at 200 ° C.
JP2001301984A 2001-09-28 2001-09-28 Plate-like compound powder and method for producing the same Expired - Lifetime JP5116199B2 (en)

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Publication number Priority date Publication date Assignee Title
JP2015038037A (en) * 2014-11-18 2015-02-26 株式会社巴川製紙所 Method of producing clay dispersion and method of producing clay film

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