JPH08259841A - Pearly luster pigment and coating material composition, cosmetic, ink and plastics blended with the same - Google Patents

Pearly luster pigment and coating material composition, cosmetic, ink and plastics blended with the same

Info

Publication number
JPH08259841A
JPH08259841A JP9752095A JP9752095A JPH08259841A JP H08259841 A JPH08259841 A JP H08259841A JP 9752095 A JP9752095 A JP 9752095A JP 9752095 A JP9752095 A JP 9752095A JP H08259841 A JPH08259841 A JP H08259841A
Authority
JP
Japan
Prior art keywords
synthetic mica
luster pigment
pearl luster
synthetic
mica
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
JP9752095A
Other languages
Japanese (ja)
Other versions
JP2889837B2 (en
Inventor
Masaru Yamamoto
勝 山本
Akitsugu Andou
彰嗣 安藤
Tetsushi Kosugi
哲史 小杉
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
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Topy Industries Ltd filed Critical Topy Industries Ltd
Priority to JP9752095A priority Critical patent/JP2889837B2/en
Priority to US08/582,427 priority patent/US5741355A/en
Publication of JPH08259841A publication Critical patent/JPH08259841A/en
Application granted granted Critical
Publication of JP2889837B2 publication Critical patent/JP2889837B2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Abstract

PURPOSE: To obtain a pigment for a coating material, etc., by coating a synthetic mica having a smooth particle surface and an iron content equal to or lower than a specific value with a metal oxide, showing no yellow at a mass tone angle and a shade part, causing no faded color of an interference color. CONSTITUTION: A synthetic mica (e.g. tetrasilicon fluoride mica, etc.) containing Ti, Zn, Na, B, Li, Ca, Ge, Sr, Zr, etc., having <=1.58 average refractive index and <=1.0% iron content is mixed with water while stirring, blended with a solution of titanyl sulfate, rapidly heated to 100 deg.C, reacted at the temperature for 3 hours, filtered, washed with water and dried at 110 deg.C to give powder,, which is baked at 800 deg.C for 1 hour to give the objective pigment for a coating material, etc., by coating a synthetic mica which comprises the synthetic mica coated with a metal oxide (e.g. titanium dioxide, etc.), shows no yellow at a mass tone angle and a shade part, has solved the problem of a faded color of an interference color and is useful as a coating composition, cosmetic, ink, plastics etc.

Description

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

【0001】[0001]

【産業上の利用分野】この発明は、合成マイカを基質と
するパ−ル光沢顔料及び該パ−ル光沢顔料を含有する塗
料、化粧料、インキ並びにプラスチックに関するもので
ある。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a pearl luster pigment using synthetic mica as a substrate, and a paint, cosmetics, ink and plastic containing the pearl luster pigment.

【0002】[0002]

【従来の技術】天然の雲母に酸化鉄、酸化チタン等の金
属酸化物を被覆して、パ−ル感を出すパ−ル光沢顔料
は、従来から公知である。しかして、この種従来のパ−
ル光沢顔料は、マスト−ンアングル,シエイド部分でマ
イカ独特の黄味がでることと、干渉効果が弱く、そのた
め干渉色が色ぼけする欠点があった。一方、合成マイカ
は、極めて透明度の高い製品が得られ、その点ではパ−
ル光沢顔料の優れた基質ということができる。しかしな
がら、従来公知の合成マイカを使用したパ−ル光沢顔料
は、天然雲母を使用した場合と同じように、マスト−ン
アングル,シエイド部分で黄味がでることと、干渉色が
色ぼけする問題があった。
2. Description of the Related Art A pearl luster pigment which gives a pearly feel by coating a natural mica with a metal oxide such as iron oxide or titanium oxide has been known. Then, this kind of conventional par
The luster pigment has a drawback that a mica-specific yellowish color appears in the mast angle and shade portions and that the interference effect is weak, and therefore the interference color is blurred. On the other hand, synthetic mica gives a product with extremely high transparency, and in that respect
It can be said that it is an excellent substrate for luster pigments. However, the pearl luster pigment using the conventionally known synthetic mica has a problem that the mast angle and the shade portion have a yellowish tint and the interference color is blurred as in the case of using natural mica. there were.

【0003】[0003]

【発明が解決しようとする課題】この発明は、このよう
な問題点を解決しようとするものであり、マスト−ンア
ングル,シエイド部分で黄味がでることと、干渉色が色
ぼけする問題を解決した合成マイカを基質とするパ−ル
光沢顔料を提供することを目的とする。
SUMMARY OF THE INVENTION The present invention is intended to solve such a problem, and solves the problems that the mast angle and the shade portion have a yellowish tint and the interference color is blurred. It is an object of the present invention to provide a pearl luster pigment using the synthetic mica as a substrate.

【0004】[0004]

【課題を解決するための手段】本発明者等は、上記問題
点を解決するため鋭意研究の結果、原料及び製造工程
で、合成マイカ中に鉄分が混入しないようにして、鉄分
1.0%以下の合成マイカを合成し、これを基質とした
パ−ル光沢顔料が、マスト−ンアングル,シエイド部分
で黄味がでることと、干渉色が色ぼけする問題が生じな
いという予想外の事実を見いだし、本発明に到達した。
即ち本発明は、合成マイカ上に金属酸化物を被覆したパ
−ル光沢顔料に於いて、前記合成マイカの粒子表面を平
滑とし、合成マイカ中の鉄含有量を1.0%以下とした
ことを特徴とする。
Means for Solving the Problems As a result of intensive research to solve the above-mentioned problems, the inventors of the present invention have confirmed that the raw material and the manufacturing process do not mix iron in the synthetic mica with an iron content of 1.0%. The following synthetic mica was synthesized, and the pearl luster pigment using this as a substrate showed the unexpected fact that there was no problem that the interference color was blurred due to the yellowish appearance at the mast angle and shade part. Found and arrived at the present invention.
That is, in the present invention, in a pearl luster pigment obtained by coating a synthetic mica with a metal oxide, the particle surface of the synthetic mica is made smooth and the iron content in the synthetic mica is 1.0% or less. Is characterized by.

【0005】本発明に使用する合成マイカは、次式
(1)で表される。 X0.5-12-3410(F,OH)2 (1) 式中、Xは、配位数12の位置を占める層間イオンで、
+,Na+,Li+,Rb+,Cs+,Tl+,Ca2+,S
2+,Ba2+を表し、Yは、配位数6の位置を占める八
面体イオンで、Mg2+,Fe2+,Co2+,Ni2+,Mn
2+,Li+,Ti2+,Zn2+,Cu2+,Al3+,T
3+,Cr3+,Fe3+,Mn3+を表し、Zは、配位数4
の位置を占める四面体イオンでSi4+,Al3+,B3+
Fe3+,Mn3+,Be2+,Zn2+,Ge4+を表す。
The synthetic mica used in the present invention is represented by the following formula (1). X 0.5-1 Y 2-3 Z 4 O 10 (F, OH) 2 (1) In the formula, X is an interlayer ion occupying the position of coordination number 12, and
K + , Na + , Li + , Rb + , Cs + , Tl + , Ca 2+ , S
Representing r 2+ and Ba 2+ , Y is an octahedral ion occupying the position of coordination number 6, and is Mg 2+ , Fe 2+ , Co 2+ , Ni 2+ , Mn.
2+ , Li + , Ti2 + , Zn2 + , Cu2 + , Al3 + , T
i 3+ , Cr 3+ , Fe 3+ , Mn 3+ , and Z is a coordination number 4
Of tetrahedral ions occupying the positions of Si 4+ , Al 3+ , B 3+ ,
It represents Fe 3+ , Mn 3+ , Be 2+ , Zn 2+ , Ge 4+ .

【0006】上記合成マイカの中で、Ti、Zn、N
a、B、Li、Ca、Ge、Sr及びZrからなる群か
ら選ばれる少なくとも1種以上を、0.01〜5%含有
する合成マイカを使用するのが好ましい。本発明に使用
する合成マイカ中の鉄含有量は、1.0%以下である必
要があり、特に0.1%以下とするのが好ましい。これ
より含有量が多いと、マスト−ンアングル,シエイド部
分で黄味がでることと、干渉色が色ぼけする問題が生じ
る。特に鉄含有量を、0.1%以下とした場合は、マス
ト−ンアングル,シエイド部分で黄味がでることと、干
渉色が色ぼけする問題は全く生じない。
Among the above synthetic mica, Ti, Zn, N
It is preferable to use a synthetic mica containing 0.01 to 5% of at least one selected from the group consisting of a, B, Li, Ca, Ge, Sr and Zr. The iron content in the synthetic mica used in the present invention needs to be 1.0% or less, and preferably 0.1% or less. If the content is larger than this, problems such as yellowing at the mast angle and shade portions and blurring of the interference color occur. In particular, when the iron content is set to 0.1% or less, there is no problem of yellowing at the mast angle and shade portions and blurring of interference colors.

【0007】従来公知の合成マイカは、文献などの記載
によれば、0.01モル(Fe換算0.13%)以上の
鉄分を含有している。全鉄含有量を1.0%以下とした
本発明の合成マイカは、次のようにして製造することが
できる。合成マイカ原料のSiO2、MgO、Al
23、K2iF6、KF及びタルク、長石等は、該原料中
に含まれる不純物の全鉄含有量が、合計で1.0%以下
となるように選定若しくは精製する。また、原料混合時
に混合機等からのFeの混入を防止するため、混合機等
はセラミックス等のコ−テイングをしたものを使用す
る。更に、混合、粉砕工程で混入した鉄分は、必要なら
粉砕後に脱鉄機を使用したり、無機酸、有機酸、キレ−
ト剤等を用いて除去すると良い。
According to the description in the literature, the conventionally known synthetic mica contains 0.01 mol (0.13% in terms of Fe) of iron. The synthetic mica of the present invention having a total iron content of 1.0% or less can be manufactured as follows. Synthetic mica raw material SiO 2 , MgO, Al
2 O 3 , K 2 iF 6 , KF, talc, feldspar, etc. are selected or purified so that the total iron content of impurities contained in the raw material is 1.0% or less in total. Further, in order to prevent Fe from being mixed in from a mixer or the like when mixing the raw materials, a mixer or the like coated with ceramics or the like is used. Further, the iron content mixed in the mixing and crushing steps may be used in a deironing machine after crushing, if necessary, in an inorganic acid, an organic acid, or a crusher.
It is advisable to remove it by using an agent.

【0008】本発明に使用する合成マイカ粉末は、表面
が平滑である必要がある。合成マイカは、結晶が硬く、
へき開しにくいため、通常の方法では表面平滑な薄片状
とすることができず、ギザギザした断面及び表面を持っ
た不定形粉末となる。表面平滑な合成マイカ粉とするに
は、剥離し易い合成マイカ結晶塊を微粉化すれば良い。
剥離し易い合成マイカ結晶塊を得るには、例えば、合成
マイカを溶融合成する際、合成マイカ融液に、少なくと
も1%以上の合成マイカ微粉末を加えて、凝固・結晶化
させると良い。このような合成マイカ結晶塊は剥離し易
く、ジヨ−クラッシャ−等通常の破砕機で細片化して
も、マイカ表面が荒れて傷付くことを回避できる。
The surface of the synthetic mica powder used in the present invention must be smooth. Synthetic mica has hard crystals,
Since it is difficult to cleave, it cannot be made into a flaky shape having a smooth surface by a usual method, and an irregularly shaped powder having a jagged cross section and a surface is obtained. In order to obtain a synthetic mica powder having a smooth surface, finely pulverizing a synthetic mica crystal mass that is easy to peel off.
In order to obtain a synthetic mica crystal mass that can be easily peeled off, for example, when the synthetic mica is melt-synthesized, at least 1% or more of the synthetic mica fine powder is added to the synthetic mica melt to coagulate and crystallize. Such synthetic mica crystal lumps are easily peeled off, and even if they are made into pieces by an ordinary crushing machine such as a Jaw crusher, it is possible to prevent the mica surface from being roughened and damaged.

【0009】上記合成マイカ細片を、例えば、ハンマ−
ミル、ロ−ルミル、ボ−ルミル等を用いて更に100ミ
クロン程度以下に微粉化する場合、そのままではマイカ
細片に過大な粉砕力がかかり、ギザギザした断面及び表
面を持った不定形粉末となる。そこで、例えば、グリセ
リン、流動パラフイン、エチレングリコ−ル等の高粘度
媒液を加えて処理することによって、マイカ表面を荒ら
すことなく微粉化できる。尚、本発明に於いては、60
0〜1350℃で熱処理してマイカ表面を平滑にしたも
のを使用することもできる。本発明に使用する合成マイ
カの屈折率は、1.58以下が好ましい。このような合
成マイカを使用することによって、パ−ル光沢顔料の光
輝感が向上し、色が鮮やかとなり、余色が濁らなくな
る。これは、被覆する酸化物との屈折率差が大きくなる
ためか、本発明のパ−ル光沢顔料を適用する有機樹脂
(屈折率1.4〜1.6)との屈折率差が小さくなるた
めと考えられるが、その理由は理論的に十分解明されて
いない。
[0009] The above synthetic mica strip can be treated, for example, with a hammer.
When finely pulverized to a size of about 100 microns or less using a mill, roll mill, ball mill, etc., the mica pieces are subjected to excessive crushing force as they are, resulting in an irregularly shaped powder having a jagged cross section and surface. . Therefore, for example, by adding a high-viscosity medium liquid such as glycerin, liquid paraffin, or ethylene glycol, the mica can be pulverized without roughening the surface. In the present invention, 60
It is also possible to use a mica surface that has been smoothed by heat treatment at 0 to 1350 ° C. The refractive index of the synthetic mica used in the present invention is preferably 1.58 or less. By using such synthetic mica, the lustrous feeling of the pearl luster pigment is improved, the color becomes vivid, and the residual color does not become turbid. This is probably because the difference in refractive index with the oxide to be coated is large, and the difference in refractive index with the organic resin (refractive index 1.4 to 1.6) to which the pearl luster pigment of the present invention is applied is small. This is probably because the reason has not been fully understood theoretically.

【0010】本発明に使用する合成マイカは、面方向の
径が3〜100ミクロン、厚みが0.05〜1ミクロン
の鱗片状粒子を使用するのが良い。このような合成マイ
カを使用することによって、パ−ル光沢顔料の光輝感が
向上し、色が鮮やかとなり、余色が濁らなくなる。合成
マイカのアスペクト比は、60以上であるのが良く、こ
れより小さいと、干渉効果が不十分となり、光沢がでに
くくなる。本発明に使用する合成マイカとしては、例え
ば、フッ素金雲母、フッ素四ケイ素雲母、フッ素テニオ
ライト及びこれらの同形置換体のようなフッ素雲母が好
適に使用できるが、特にフッ素金雲母を使用するのが好
ましい。合成マイカの製法自体は、溶融合成、水熱合
成、固相反応などいずれでも良いが、結晶性が良好であ
るという理由で特に溶融合成法が好ましい。
As the synthetic mica used in the present invention, it is preferable to use scaly particles having a diameter in the plane direction of 3 to 100 μm and a thickness of 0.05 to 1 μm. By using such synthetic mica, the lustrous feeling of the pearl luster pigment is improved, the color becomes vivid, and the residual color does not become turbid. The aspect ratio of the synthetic mica is preferably 60 or more, and if it is smaller than this, the interference effect becomes insufficient and the gloss becomes difficult. As the synthetic mica used in the present invention, for example, fluorophlogopite such as fluorophlogopite, fluorotetrasilicon phlogopite, fluoro teniolite, and isomorphs thereof can be preferably used, but especially fluorophlogopite is used. preferable. The synthetic mica itself may be produced by any of melt synthesis, hydrothermal synthesis, solid-state reaction, etc., but the melt synthesis method is particularly preferable because of its good crystallinity.

【0011】合成マイカ粉体に、金属酸化物を被覆する
には、公知の方法で行えば良い。例えば、酸化チタンを
被覆する方法は、希薄なチタン酸水溶液中に合成マイカ
粉体を懸濁させ、70〜100℃に加温し、チタン塩を
加水分解して合成マイカ粉体上に水和酸化チタン粒子を
析出させ、その後700〜1000℃の高温で焼成して
製造することができる。使用する金属酸化物としては、
例えば、チタン、ジルコニウム、鉄、クロムまたはバナ
ジウムの酸化物等が挙げられる。これらは単独若しくは
混合して使用することができる。金属酸化物、好ましく
は、二酸化チタンは、塩化スズのようなルチル化剤でル
チル化するのが好ましい。このようにルチル化すること
によって、パール光沢顔料の耐候性が向上する。本発明
のパ−ル光沢顔料は、従来のパ−ル光沢顔料と同様にし
て、各種塗料に混合して塗料組成物としたり、各種プラ
スチックに練り込んで独特のパ−ル感を発現したプラス
チックとしたり、化粧品等の着色剤としたり、インキの
着色剤とすることができる。
The synthetic mica powder may be coated with a metal oxide by a known method. For example, the method of coating with titanium oxide is to suspend the synthetic mica powder in a dilute aqueous solution of titanic acid, heat it to 70 to 100 ° C., hydrolyze the titanium salt, and hydrate it on the synthetic mica powder. It can be manufactured by precipitating titanium oxide particles and then firing at a high temperature of 700 to 1000 ° C. The metal oxide used is
Examples thereof include oxides of titanium, zirconium, iron, chromium or vanadium. These can be used alone or in combination. The metal oxide, preferably titanium dioxide, is preferably rutiled with a rutile agent such as tin chloride. Such rutile conversion improves the weather resistance of the pearlescent pigment. The pearly luster pigment of the present invention is a plastic which is mixed with various paints to form a paint composition or kneaded with various plastics in the same manner as in the conventional pearly luster pigment to express a unique pearly feeling. Or as a colorant for cosmetics or as a colorant for inks.

【0012】[0012]

【作用】本発明の鉄含有量1.0%以下とした表面平滑
な合成マイカを基材とすることによって、マスト−ンア
ングル,シエイド部分で黄味がでることと、干渉色が色
ぼけする問題が実質的に生じないパ−ル光沢顔料が得ら
れる、しかしながら、その理由は、理論的に十分解明さ
れていない。
The use of the synthetic mica of the present invention having an iron content of 1.0% or less and a smooth surface as a base material causes a yellowish tint at the mast angle and shade portions, and the interference color is blurred. It is possible to obtain a pearl luster pigment that does not substantially occur, however, the reason therefor is not fully understood theoretically.

【0013】[0013]

【実施例】次に、実施例、比較例を挙げて本発明を更に
説明するが、本発明はこれら実施例に限定されない。 実施例1 粒径10〜60μmの合成フッ素金雲母粉体(平均屈折
率1.56、鉄含有量0.04%)20gと水400ミ
リリットルとを、1リットルのガラス製容器中に入れて
撹拌した。次いで、この中に硫酸チタニル溶液(TiO
280g/リットル)200ミリリットルを添加して、
急速に100℃まで加温し、この温度で3時間反応させ
た。反応終了後、濾過、水洗し、110℃の温度で乾燥
した。得られた粉体を800℃で1時間焼成して、本発
明のパ−ル光沢顔料を得た。このパ−ル光沢顔料は、ク
リヤ−ラッカ−中に分散させると、黄金色を呈し、満足
すべき十分な光沢のある光彩を示した。このパ−ル光沢
顔料のマスト−ンアングル,シエイド部分の色合いと干
渉色の色ぼけを測定した。結果を後記表Iに示す。
EXAMPLES Next, the present invention will be further described with reference to Examples and Comparative Examples, but the present invention is not limited to these Examples. Example 1 20 g of synthetic fluorophlogopite powder having an average particle size of 10 to 60 μm (average refractive index 1.56, iron content 0.04%) and 400 ml of water were placed in a 1 liter glass container and stirred. did. Then, in this, a titanyl sulfate solution (TiO 2
2 80 g / liter) 200 ml,
The temperature was rapidly raised to 100 ° C., and the reaction was carried out at this temperature for 3 hours. After the reaction was completed, it was filtered, washed with water, and dried at a temperature of 110 ° C. The obtained powder was calcined at 800 ° C. for 1 hour to obtain a pearl luster pigment of the present invention. This pearl luster pigment, when dispersed in a clear lacquer, exhibited a golden color with a satisfactory and sufficiently lustrous shine. The mast angle and shade of the shade portion of this pearl luster pigment and the blurring of interference color were measured. The results are shown in Table I below.

【0014】(試験方法)マスト−ンアングル,シエイ
ド部分の色合いは、白地のパネルにパ−ル光沢顔料を含
有させた塗料を塗布乾燥し、得られた塗膜面を干渉色の
見えない角度から観察して、黄味の有無を、下記3段階
の基準で評価した。 ◎・・・・・・・・全く黄味は観察されなかった。 ○・・・・・・・・非常に僅かの黄味が観察された。 ×・・・・・・・・かなりの黄味が観察された。 干渉色の色ぼけは、白地又は黒地のパネルに、パ−ル光
沢顔料を含有させた塗料を塗布乾燥し、得られた塗膜面
の干渉色を観察し、干渉色自体の色ぼけを、下記3段階
の基準で評価した。 ◎・・・・・・・・全く色ぼけはなかった。 ○・・・・・・・・非常に僅かの色ぼけが観察された。 ×・・・・・・・・かなりの色ぼけが観察された。
(Test method) The tone of the mast angle and shade portion was determined by applying a paint containing a pearl luster pigment to a white background panel and drying it, and then the resulting coating film surface was examined from the angle at which no interference color was visible. It was observed and the presence or absence of yellowing was evaluated according to the following three-stage criteria. ∘: No yellowish color was observed. O: A very slight yellowish tint was observed. X: A considerable yellowish color was observed. Interference color blurring is a white background or a black background panel, a coating containing a pearl luster pigment is applied and dried, the interference color of the obtained coating film surface is observed, and the interference color itself is blurred. The evaluation was made according to the following three-stage criteria. ◎ ... There was no color blur at all. O: A very slight color blur was observed. × ・ ・ ・ ・ ・ ・ A considerable amount of color blur was observed.

【0015】実施例2 粒径10〜60μmのボロン含有合成フッ素金雲母粉体
(平均屈折率1.52、鉄含有量0.05%)25gと
水400ミリリットルとを、1リットルのガラス製容器
中に入れて撹拌した。次いで、この中に硫酸チタニル溶
液(TiO280g/リットル)200ミリリットルを
添加して、急速に100℃まで加熱し、この温度で3時
間反応させた。反応終了後、濾過、水洗し、110℃の
温度で乾燥した。この乾燥物の全量をガラス製容器中に
移し、水570ミリリットルを加えて撹拌した。これ
に、硫酸ジルコニウム溶液(ZrO2=100g/リッ
トル)30ミリリットルを添加し、更に尿素を徐々に加
えて、pHを2.0にした。この溶液を急速に100℃
まで加熱し、反応を1時間継続した。反応終了後、濾
過、水洗し、110℃で乾燥した後、800℃で1時間
焼成して、本発明のパ−ル光沢顔料を得た。このパ−ル
光沢顔料をクリヤ−ラッカ−中に分散させると、鮮やか
な金色を呈した。実施例1と同様にして、このパ−ル光
沢顔料のマスト−ンアングル,シエイド部分の色合いと
干渉色の色ぼけを測定した。結果を後記表Iに示す。
Example 2 25 g of boron-containing synthetic fluorophlogopite powder having an average particle size of 10 to 60 μm (average refractive index 1.52, iron content 0.05%) and 400 ml of water were placed in a 1-liter glass container. It was put in and stirred. Then, 200 ml of a titanyl sulfate solution (TiO 2 80 g / liter) was added thereto, and the mixture was rapidly heated to 100 ° C. and reacted at this temperature for 3 hours. After the reaction was completed, it was filtered, washed with water, and dried at a temperature of 110 ° C. The whole amount of this dried product was transferred into a glass container, 570 ml of water was added, and the mixture was stirred. To this, 30 ml of a zirconium sulfate solution (ZrO 2 = 100 g / liter) was added, and urea was gradually added to adjust the pH to 2.0. The solution is rapidly heated to 100 ° C.
The reaction was continued for 1 hour. After completion of the reaction, the mixture was filtered, washed with water, dried at 110 ° C., and then calcined at 800 ° C. for 1 hour to obtain a pearl luster pigment of the present invention. When this pearl luster pigment was dispersed in a clear lacquer, a bright golden color was exhibited. In the same manner as in Example 1, the mast angle of this pearl luster pigment, the shade of the shade portion and the blurring of the interference color were measured. The results are shown in Table I below.

【0016】実施例3 実施例1で使用したのと同じ合成フッ素金雲母粉体30
gと水400ミリリットルとを、1リットルのガラス製
容器中に入れて撹拌した。次いで、この中に硫酸ジルコ
ニウム溶液(ZrO2=100g/リットル)200ミ
リリットルを添加し、更に尿素を徐々に加えて、pHを
2.0にした。この溶液を急速に100℃まで加熱し、
反応を3時間継続した。反応終了後、濾過、水洗し、1
10℃で乾燥した後、800℃で1時間焼成して、本発
明のパ−ル光沢顔料を得た。このパ−ル光沢顔料は、ク
リヤ−ラッカ−中に分散させると、黄味を帯びた銀白色
の外観と満足すべき十分な光沢のある光彩を示した。実
施例1と同様にして、このパ−ル光沢顔料のマスト−ン
アングル,シエイド部分の色合いと干渉色の色ぼけを測
定した。結果を後記表Iに示す。
Example 3 The same synthetic fluorophlogopite powder 30 used in Example 1
g and 400 ml of water were placed in a 1 liter glass container and stirred. Next, 200 ml of a zirconium sulfate solution (ZrO 2 = 100 g / liter) was added thereto, and urea was gradually added to adjust the pH to 2.0. The solution is rapidly heated to 100 ° C,
The reaction was continued for 3 hours. After completion of the reaction, filtration, washing with water, 1
After drying at 10 ° C., it was baked at 800 ° C. for 1 hour to obtain a pearlescent pigment of the present invention. The pearl luster pigment, when dispersed in a clear lacquer, exhibited a yellowish silver-white appearance and a satisfactorily lustrous glow. In the same manner as in Example 1, the mast angle of this pearl luster pigment, the shade of the shade portion and the blurring of the interference color were measured. The results are shown in Table I below.

【0017】実施例4 粒径10〜60μmのナトリウム含有合成フッ素金雲母
粉体(平均屈折率1.53、鉄含有量0.10%)25
gと水370ミリリットルとを、1リットルのガラス製
容器中に入れて撹拌した。次いで、この中に硫酸第二ク
ロム溶液(Cr23=100g/リットル)30ミリリ
ットルを添加し、90℃まで加熱した。更に硫酸チタニ
ル溶液(TiO280g/リットル)200ミリリット
ルを添加して100℃まで加熱し、反応を3時間継続し
た。反応終了後、濾過、水洗し、約110℃で乾燥した
後、800℃で1時間焼成して、本発明のパ−ル光沢顔
料を得た。このパ−ル光沢顔料は、鮮明な金色反射色を
示した。実施例1と同様にして、このパ−ル光沢顔料の
マスト−ンアングル,シエイド部分の色合いと干渉色の
色ぼけを測定した。結果を後記表Iに示す。
Example 4 Sodium-containing synthetic fluorophlogopite powder having a particle size of 10 to 60 μm (average refractive index 1.53, iron content 0.10%) 25
g and 370 ml of water were placed in a 1 liter glass container and stirred. Then, 30 ml of a chromic sulfate solution (Cr 2 O 3 = 100 g / liter) was added thereto and heated to 90 ° C. Further, 200 ml of a titanyl sulfate solution (TiO 2 80 g / liter) was added and heated to 100 ° C., and the reaction was continued for 3 hours. After completion of the reaction, the mixture was filtered, washed with water, dried at about 110 ° C., and calcined at 800 ° C. for 1 hour to obtain a pearlescent pigment of the present invention. This pearl luster pigment showed a vivid golden reflection color. In the same manner as in Example 1, the mast angle of this pearl luster pigment, the shade of the shade portion and the blurring of the interference color were measured. The results are shown in Table I below.

【0018】実施例5 実施例1で使用した合成フッ素金雲母粉体30gを使用
し、実施例1と同様にして、二酸化チタン被覆合成マイ
カ45gを調製した。この全量をガラス製容器に移し、
水570ミリリットルを加えて撹拌した。これに、硫酸
第二鉄溶液(Fe23=100g/リットル)30ミリ
リットルを添加し、更に尿素を徐々に加えて、pHを
2.0にした。この溶液を急速に100℃まで加熱し、
反応を1時間継続した。反応終了後、濾過、水洗し、1
10℃で乾燥した後、800℃で1時間焼成して、本発
明のパ−ル光沢顔料を得た。このパ−ル光沢顔料は、ク
リヤ−ラッカ−中に分散させると、濃い金色反射色を有
する干渉性の優れた真珠光沢を示した。実施例1と同様
にして、このパ−ル光沢顔料のマスト−ンアングル,シ
エイド部分の色合いと干渉色の色ぼけを測定した。結果
を後記表Iに示す。
Example 5 45 g of titanium dioxide-coated synthetic mica was prepared in the same manner as in Example 1, except that 30 g of the synthetic fluorophlogopite powder used in Example 1 was used. Transfer all of this to a glass container,
570 ml of water was added and stirred. To this, 30 ml of ferric sulfate solution (Fe 2 O 3 = 100 g / liter) was added, and urea was gradually added to adjust the pH to 2.0. The solution is rapidly heated to 100 ° C,
The reaction was continued for 1 hour. After completion of the reaction, filtration, washing with water, 1
After drying at 10 ° C., it was baked at 800 ° C. for 1 hour to obtain a pearlescent pigment of the present invention. This pearl luster pigment, when dispersed in a clear lacquer, exhibited an excellent interfering pearl luster with a deep golden reflection color. In the same manner as in Example 1, the mast angle of this pearl luster pigment, the shade of the shade portion and the blurring of the interference color were measured. The results are shown in Table I below.

【0019】実施例6 粒径10〜60μmの合成フッ素金雲母粉体(平均屈折
率1.56、鉄含有量1.0%)を使用する以外は、実
施例1と同様にして、二酸化チタン被覆マイカを製造し
た。このものをクリヤ−ラッカ−中に分散させると、黄
金色を呈し、満足すべき十分な光沢のある光彩を示し
た。実施例1と同様にして、このパ−ル光沢顔料のマス
ト−ンアングル,シエイド部分の色合いと干渉色の色ぼ
けを測定した。結果を後記表Iに示す。
Example 6 Titanium dioxide was prepared in the same manner as in Example 1 except that synthetic fluorophlogopite powder having an average particle diameter of 10 to 60 μm (average refractive index 1.56, iron content 1.0%) was used. A coated mica was produced. When this was dispersed in a clear lacquer, it exhibited a golden color and exhibited a satisfactory and sufficiently lustrous glow. In the same manner as in Example 1, the mast angle of this pearl luster pigment, the shade of the shade portion and the blurring of the interference color were measured. The results are shown in Table I below.

【0020】実施例7 Ti1%を含有する合成フッ素金雲母粉体(平均屈折率
1.56、鉄含有量0.04%)20gと水400ミリ
リットルとを、1リットルのガラス製容器中に入れて撹
拌した。次いで、この中に硫酸チタニル溶液(TiO2
80g/リットル)200ミリリットルを添加して、急
速に100℃まで加温し、この温度で3時間反応させ
た。反応終了後、濾過、水洗し、110℃の温度で乾燥
した。得られた粉体を800℃で1時間焼成して、本発
明のパ−ル光沢顔料を得た。このパ−ル光沢顔料は、ク
リヤ−ラッカ−中に分散させると、黄金色を呈し、満足
すべき十分な光沢のある光彩を示した。このパ−ル光沢
顔料のマスト−ンアングル,シエイド部分の色合いと干
渉色の色ぼけを測定した。結果を後記表Iに示す。
Example 7 20 g of synthetic fluorophlogopite powder containing 1% of Ti (average refractive index 1.56, iron content 0.04%) and 400 ml of water were placed in a 1 liter glass container. And stirred. Then, a titanyl sulfate solution (TiO 2
(80 g / liter) 200 ml was added, and the mixture was rapidly heated to 100 ° C. and reacted at this temperature for 3 hours. After the reaction was completed, it was filtered, washed with water, and dried at a temperature of 110 ° C. The obtained powder was calcined at 800 ° C. for 1 hour to obtain a pearl luster pigment of the present invention. This pearl luster pigment, when dispersed in a clear lacquer, exhibited a golden color with a satisfactory and sufficiently lustrous shine. The mast angle and shade of the shade portion of this pearl luster pigment and the blurring of interference color were measured. The results are shown in Table I below.

【0021】実施例8〜16 下記合成フッ素金雲母粉体を使用する以外は実施例1と
同様にして本発明のパ−ル光沢顔料を得た。 実施例8 Zn1%を含有する合成フッ素金雲母(Fe含有量0.06%) 実施例9 Ba1%を含有する合成フッ素金雲母(Fe含有量0.04%) 実施例10 Na1%を含有する合成フッ素金雲母(Fe含有量0.05%) 実施例11 B 1%を含有する合成フッ素金雲母(Fe含有量0.04%) 実施例12 Li1%を含有する合成フッ素金雲母(Fe含有量0.04%) 実施例13 Ca1%を含有する合成フッ素金雲母(Fe含有量0.07%) 実施例14 Ge1%を含有する合成フッ素金雲母(Fe含有量0.04%) 実施例15 Sr1%を含有する合成フッ素金雲母(Fe含有量0.84%) 実施例16 Zr1%を含有する合成フッ素金雲母(Fe含有量0.04%) これらはいずれも、クリヤ−ラッカ−中に分散させる
と、黄金色を呈し、満足すべき十分な光沢のある光彩を
示した。このパ−ル光沢顔料のマスト−ンアングル,シ
エイド部分の色合いと干渉色の色ぼけを測定した。結果
を後記表Iに示す。
Examples 8 to 16 The pearlescent pigments of the present invention were obtained in the same manner as in Example 1 except that the following synthetic fluorophlogopite powder was used. Example 8 Synthetic fluorophlogopite containing 1% Zn (Fe content 0.06%) Example 9 Synthetic fluorophlogopite containing 1% Ba (Fe content 0.04%) Example 10 Containing 1% Na Synthetic Fluoro phlogopite (Fe content 0.05%) Example 11 Synthetic fluorophlogopite containing B 1% (Fe content 0.04%) Example 12 Synthetic fluorophlogopite containing Li 1% (Fe content) Amount 0.04%) Example 13 Synthetic Fluoro phlogopite containing 1% Ca (Fe content 0.07%) Example 14 Synthetic fluorophlogopite containing 1% Ge (Fe content 0.04%) Example 15 Synthetic Fluoro phlogopite containing 1% Sr (Fe content 0.84%) Example 16 Synthetic fluorophlogopite containing 1% Zr (Fe content 0.04%) All of these are in clear lacquer. Disperse in And showed a golden color and a sufficiently glossy glow that was satisfactory. The mast angle and shade of the shade portion of this pearl luster pigment and the blurring of interference color were measured. The results are shown in Table I below.

【0022】実施例17 Zn1%を含有する合成フッ素金雲母粉体(鉄含有量
0.05%)25gと水370ミリリットルとを、1リ
ットルのガラス製容器中に入れて撹拌した。次いで、こ
の中に硫酸第二クロム溶液(Cr23=100g/リッ
トル)30ミリリットルを添加し、90℃まで加熱し
た。更に硫酸チタニル溶液(TiO280g/リット
ル)200ミリリットルを添加して100℃まで加熱
し、反応を3時間継続した。反応終了後、濾過、水洗
し、110℃で乾燥した後、800℃で1時間焼成し
て、本発明のパ−ル光沢顔料を得た。このパ−ル光沢顔
料は、鮮明な金色反射色を示した。実施例1と同様にし
て、このパ−ル光沢顔料のマスト−ンアングル,シエイ
ド部分の色合いと干渉色の色ぼけを測定した。結果を後
記表Iに示す。
Example 17 25 g of synthetic fluorophlogopite powder containing 1% Zn (iron content: 0.05%) and 370 ml of water were placed in a 1-liter glass container and stirred. Then, 30 ml of a chromic sulfate solution (Cr 2 O 3 = 100 g / liter) was added thereto and heated to 90 ° C. Further, 200 ml of a titanyl sulfate solution (TiO 2 80 g / liter) was added and heated to 100 ° C., and the reaction was continued for 3 hours. After completion of the reaction, the mixture was filtered, washed with water, dried at 110 ° C., and then calcined at 800 ° C. for 1 hour to obtain a pearl luster pigment of the present invention. This pearl luster pigment showed a vivid golden reflection color. In the same manner as in Example 1, the mast angle of this pearl luster pigment, the shade of the shade portion and the blurring of the interference color were measured. The results are shown in Table I below.

【0023】実施例18 面方向平均粒子径20ミクロン、平均アスペクト比80
の合成フッ素金雲母粉体(鉄含有量0.04%)20g
と水400ミリリットルとを、1リットルのガラス製容
器中に入れて撹拌した。この中に、塩化スズ溶液(酸化
スズ換算で5重量%溶液)5ミリリットルを加え、70
℃で30分間反応させた。次いで、この中に硫酸チタニ
ル溶液(TiO280g/リットル)200ミリリット
ルを添加して、急速に100℃まで加温し、この温度で
3時間反応させた。反応終了後、濾過、水洗し、110
℃の温度で乾燥した。得られた粉体を800℃で1時間
焼成して、本発明のパ−ル光沢顔料を得た。粉末X線回
折法により、被覆二酸化チタン層の結晶形を同定したと
ころ、アナタ−ゼ型結晶に基づく回折ピ−クは見られ
ず、ルチル型結晶に基づく回折ピ−クが観測された。こ
のパ−ル光沢顔料は、クリヤ−ラッカ−中に分散させる
と、黄金色を呈し、満足すべき十分な光沢のある光彩を
示した。このパ−ル光沢顔料のマスト−ンアングル,シ
エイド部分の色合いと干渉色の色ぼけを測定した。結果
を後記表Iに示す。
Example 18 Average particle size in plane direction 20 μm, average aspect ratio 80
Synthetic Fluor phlogopite powder (iron content 0.04%) 20g
And 400 ml of water were placed in a 1 liter glass container and stirred. To this, 5 ml of tin chloride solution (5 wt% solution in terms of tin oxide) was added,
The reaction was carried out at 30 ° C. for 30 minutes. Then, 200 ml of a titanyl sulfate solution (TiO 2 80 g / l) was added thereto, and the mixture was rapidly heated to 100 ° C. and reacted at this temperature for 3 hours. After completion of the reaction, filtration and washing with water
It was dried at a temperature of ° C. The obtained powder was calcined at 800 ° C. for 1 hour to obtain a pearl luster pigment of the present invention. When the crystal form of the coated titanium dioxide layer was identified by the powder X-ray diffraction method, the diffraction peak based on the anatase type crystal was not seen, but the diffraction peak based on the rutile type crystal was observed. This pearl luster pigment, when dispersed in a clear lacquer, exhibited a golden color with a satisfactory and sufficiently lustrous shine. The mast angle and shade of the shade portion of this pearl luster pigment and the blurring of interference color were measured. The results are shown in Table I below.

【0024】実施例19 面方向平均粒子径20ミクロン、平均アスペクト比80
の合成フッ素金雲母粉体(鉄含有量0.05%)30g
と水400ミリリットルとを、1リットルのガラス製容
器中に入れて撹拌した。次いで、この中に硫酸ジルコニ
ウム溶液(ZrO2=100g/リットル)200ミリ
リットルを添加し、更に尿素を徐々に加えて、pHを
2.0にした。この溶液を急速に100℃まで加熱し、
反応を3時間継続した。反応終了後、濾過、水洗し、1
10℃で乾燥した後、900℃で1時間焼成して、本発
明のパ−ル光沢顔料を得た。このパ−ル光沢顔料は、ク
リヤ−ラッカ−中に分散させると、黄味を帯びた銀白色
の外観と満足すべき十分な光沢のある光彩を示した。実
施例1と同様にして、このパ−ル光沢顔料のマスト−ン
アングル,シエイド部分の色合いと干渉色の色ぼけを測
定した。結果を後記表Iに示す。
Example 19 Average particle size in plane direction: 20 μm, average aspect ratio: 80
Synthetic Fluor phlogopite powder (iron content 0.05%) 30g
And 400 ml of water were placed in a 1 liter glass container and stirred. Next, 200 ml of a zirconium sulfate solution (ZrO 2 = 100 g / liter) was added thereto, and urea was gradually added to adjust the pH to 2.0. The solution is rapidly heated to 100 ° C,
The reaction was continued for 3 hours. After completion of the reaction, filtration, washing with water, 1
After drying at 10 ° C., it was baked at 900 ° C. for 1 hour to obtain a pearlescent pigment of the present invention. The pearl luster pigment, when dispersed in a clear lacquer, exhibited a yellowish silver-white appearance and a satisfactorily lustrous glow. In the same manner as in Example 1, the mast angle of this pearl luster pigment, the shade of the shade portion and the blurring of the interference color were measured. The results are shown in Table I below.

【0025】実施例20 面方向平均粒子径30ミクロン、平均アスペクト比10
0の合成フッ素金雲母粉体(鉄含有量0.05%)25
gと水370ミリリットルとを、1リットルのガラス製
容器中に入れて撹拌した。次いで、この中に硫酸第二ク
ロム溶液(Cr23=100g/リットル)30ミリリ
ットルを添加し、90℃まで加熱した。更に硫酸チタニ
ル溶液(TiO280g/リットル)200ミリリット
ルを添加して100℃まで加熱し、反応を3時間継続し
た。反応終了後、濾過、水洗し、約110℃で乾燥した
後、700℃で1時間焼成して、本発明のパ−ル光沢顔
料を得た。このパ−ル光沢顔料は、鮮明な金色反射色を
示した。実施例1と同様にして、このパ−ル光沢顔料の
マスト−ンアングル,シエイド部分の色合いと干渉色の
色ぼけを測定した。結果を後記表Iに示す。
Example 20 Surface-direction average particle diameter 30 μm, average aspect ratio 10
0 Synthetic Fluor phlogopite powder (iron content 0.05%) 25
g and 370 ml of water were placed in a 1 liter glass container and stirred. Then, 30 ml of a chromic sulfate solution (Cr 2 O 3 = 100 g / liter) was added thereto and heated to 90 ° C. Further, 200 ml of a titanyl sulfate solution (TiO 2 80 g / liter) was added and heated to 100 ° C., and the reaction was continued for 3 hours. After completion of the reaction, the mixture was filtered, washed with water, dried at about 110 ° C., and calcined at 700 ° C. for 1 hour to obtain a pearl luster pigment of the present invention. This pearl luster pigment showed a vivid golden reflection color. In the same manner as in Example 1, the mast angle of this pearl luster pigment, the shade of the shade portion and the blurring of the interference color were measured. The results are shown in Table I below.

【0026】比較例1 天然白雲母粉体(Fe含有量1.2%、平均屈折率1.
60)を使用する以外は、実施例1と同様にして、二酸
化チタン被覆雲母を製造した。このものをクリヤ−ラッ
カ−中に分散させると、金色の真珠光沢を示したが、実
施例1の本発明の顔料と比べて、干渉帯の色巾が狭く、
しかも余色が濁り、発色の鮮明度に欠けるものであっ
た。実施例1と同様にして、このパ−ル光沢顔料のマス
ト−ンアングル,シエイド部分の色合いと干渉色の色ぼ
けを測定した。結果を後記表Iに示す。
Comparative Example 1 Natural muscovite powder (Fe content 1.2%, average refractive index 1.
A titanium dioxide-coated mica was produced in the same manner as in Example 1 except that 60) was used. When this product was dispersed in a clear lacquer, it showed a golden pearl luster, but compared with the pigment of the present invention of Example 1, the color width of the interference band was narrower,
Moreover, the residual color was turbid, and the clarity of color development was lacking. In the same manner as in Example 1, the mast angle of this pearl luster pigment, the shade of the shade portion and the blurring of the interference color were measured. The results are shown in Table I below.

【0027】比較例2 天然白雲母粉体(Fe含有量1.1%、平均屈折率1.
60)を使用する以外は、実施例3と同様にして、二酸
化ジルコニウム被覆雲母を製造した。このものをクリヤ
−ラッカ−中に分散させると、銀白色の真珠光沢を示し
たが、実施例1の本発明の顔料と比べて、干渉帯の色巾
が狭く、しかも余色が濁り、発色の鮮明度に欠けるもの
であった。実施例1と同様にして、このパ−ル顔料のマ
スト−ンアングル,シエイド部分の色合いと干渉色の色
ぼけを測定した。結果を後記表Iに示す。
Comparative Example 2 Natural muscovite powder (Fe content 1.1%, average refractive index 1.
A zirconium dioxide-coated mica was produced in the same manner as in Example 3 except that 60) was used. When this product was dispersed in a clear lacquer, it exhibited a silver-white pearlescent luster, but compared to the pigment of the present invention of Example 1, the interference band had a narrower color range, and the residual color was turbid, resulting in color development. It lacked in clarity. In the same manner as in Example 1, the mast angle and shade of the shade portion of this pearlescent pigment and the blurring of interference color were measured. The results are shown in Table I below.

【0028】[0028]

【表1】 [Table 1]

【0029】実施例21:塗料 実施例1で得た本発明のパ−ル光沢顔料を、熱硬化性ア
クリルメラミン樹脂(大日本インキ製、アクリデイック
47ー712とス−パ−ベッカミンG821ー60の重
量比7:3の混合物)に約10重量%混合し、黒エナメ
ル(日本ペイント社製、ス−パ−ラックF−47)を下
塗した鋼板にスプレーし、ウエットオンウエットで熱硬化
性アクリルメラミン樹脂(大日本インキ製、アクリデイ
ック44ー179とス−パ−ベッカミンL117ー60
の重量比7:3の混合物)トップクリヤ−をスプレ−し
て、140℃で18分間焼付けた。塗膜は、彩度、明
度、干渉性の高い金色虹彩真珠光沢を示した。
Example 21: Coating material The pearl luster pigment of the present invention obtained in Example 1 was converted into a thermosetting acrylic melamine resin (manufactured by Dainippon Ink and manufactured by Acridic 47-712 and Super Beckamine G821-60). 10% by weight in a weight ratio of 7: 3), and sprayed on a steel plate coated with black enamel (Super Paint F-47, manufactured by Nippon Paint Co., Ltd.) and wet-on-wet for thermosetting acrylic. Melamine resin (manufactured by Dainippon Ink Co., Ltd., Acridic 44-179 and Super Beckamine L117-60
(7: 3 weight ratio mixture) was sprayed on top clear and baked at 140 ° C. for 18 minutes. The coating exhibited a golden iris pearl luster with high saturation, brightness and interference.

【0030】実施例22:プラスチック 実施例1で得た本発明のパ−ル光沢顔料4部を、塩化ビ
ニ−ル樹脂約100部、ジオクチルフタレ−ト40部及
びステアリン酸亜鉛3部と混合して、165℃に加熱し
た混練二本ロ−ルで3分間処理し、これを0.5mmの
厚さのシ−トに成型した。半透明の反射光が黄金色の虹
彩真珠光沢の美麗な塩化ビニ−ルシ−トを得た。
Example 22: Plastic 4 parts of the inventive pearl luster pigment obtained in Example 1 are mixed with about 100 parts of vinyl chloride resin, 40 parts of dioctyl phthalate and 3 parts of zinc stearate. Then, it was treated with two kneading rolls heated to 165 ° C. for 3 minutes, and this was molded into a sheet having a thickness of 0.5 mm. A beautiful vinyl chloride sheet with semi-transparent reflected light and a golden iris pearl luster was obtained.

【0031】実施例23:化粧料(口紅) 次の組成から口紅を製造した。 実施例1で得た顔料 15部 赤色226号 1部 香料 0.5部 口紅基材 83.5部 但し、上記口紅基材としては、下記のものを配合して使
用した。 密ろう 15部 セチルアルコ−ル 3部 ラノリン 15部 ひまし油 62部 流動パラフイン 5部 このようにして製造した口紅は、金色の鮮やかな真珠光
沢を示した。
Example 23: Cosmetic (lipstick) A lipstick was produced from the following composition. Pigment obtained in Example 1 15 parts Red No. 226 1 part Perfume 0.5 part Lipstick base material 83.5 parts However, the following lipstick base materials were blended and used. Beeswax 15 parts Cetyl alcohol 3 parts Lanolin 15 parts Castor oil 62 parts Fluid paraffin 5 parts The lipstick thus produced showed a golden bright pearlescent luster.

【0032】実施例24:化粧料(フアンデ−ションク
リ−ム) 実施例3で得た顔料 20部 流動パラフイン 25部 ワセリン 5部 イソプロピルミリステ−ト 5部 ステアリン酸 2部 POE(25)モノステアレ−ト 2部 黄酸化鉄 2部 ベンガラ 1部 タルク 5部 プロピレングリコ−ル 5部 グリセリン 5部 香料 0.5部 精製水 22.5部 上記処方物を、75〜80℃で均一に溶解・混合した
後、30℃まで冷却し、製品とした。この製品は、鮮明
度が高く、展延性に富むため大変化粧し易く、しかも化
粧くずれのしないものであった。
Example 24: Cosmetic (foundation cream) The pigment obtained in Example 3 20 parts Liquid paraffin 25 parts Vaseline 5 parts Isopropyl myristate 5 parts Stearic acid 2 parts POE (25) monostearate 2 parts Yellow iron oxide 2 parts Bengal 1 part Talc 5 parts Propylene glycol 5 parts Glycerin 5 parts Perfume 0.5 parts Purified water 22.5 parts After uniformly dissolving and mixing the above formulation at 75 to 80 ° C The product was cooled to 30 ° C. This product had a high degree of sharpness and was excellent in spreadability, so that it was very easy to apply makeup, and the makeup was not damaged.

【0033】実施例25:インキ グラビアインキメジウム100部に対し、実施例1で得
た顔料15部を加え、十分混合してグラビアパ−ルイン
キを調合した。このインキを用いて印刷した印刷紙は、
流麗な虹彩真珠光沢と高級感に満ちた黄金色の干渉色を
示した。
Example 25: Ink 15 parts of the pigment obtained in Example 1 was added to 100 parts of gravure ink medium and mixed well to prepare a gravure pal ink. Printing paper printed with this ink is
It had a flowing iris pearl luster and a golden interference color full of luxury.

【0034】[0034]

【効果】以上述べたごとく、本発明によれば、原料合成
マイカの鉄含有量を1.0%以下とすることによって、
マスト−ンアングル,シエイド部分でのマイカ独特の色
合いが消失すると共に、干渉効果が強くなって、塗装し
たときに底色が白ぼける等の問題が解消されるので、パ
−ル光沢顔料の光輝感や色の鮮明度が格段に向上し、こ
の種従来のパ−ル光沢顔料には全く見られない顕著な光
輝感を発現するから、塗料、プラスチック、インキ、化
粧品の新しい光輝材として極めて有用である。
[Effect] As described above, according to the present invention, by setting the iron content of the raw material synthetic mica to 1.0% or less,
As the mica's unique color in the mast angle and shade part disappears, the interference effect becomes stronger, and the problem of the underlying color becoming white when applied is solved, so the bright feeling of the pearl luster pigment And the sharpness of color are remarkably improved, and a remarkable brilliance that is not seen at all in conventional pearl luster pigments of this kind is exhibited, so that it is extremely useful as a new brilliant material for paints, plastics, inks and cosmetics. is there.

Claims (12)

【特許請求の範囲】[Claims] 【請求項1】合成マイカ上に金属酸化物を被覆したパ−
ル光沢顔料に於いて、前記合成マイカの粒子表面を平滑
とし、合成マイカ中の鉄含有量を1.0%以下としたこ
とを特徴とするパ−ル光沢顔料。
1. A metal mica coated synthetic oxide mica.
In the luster pigment, the particle surface of the synthetic mica is made smooth, and the iron content in the synthetic mica is 1.0% or less.
【請求項2】前記合成マイカの平均屈折率が、1.58
以下である請求項1に記載のパ−ル光沢顔料。
2. The average refractive index of the synthetic mica is 1.58.
The pearlescent pigment according to claim 1, which is as follows.
【請求項3】前記合成マイカが、Ti、Zn、Na、
B、Li、Ca、Ge、Sr及びZrからなる群から選
ばれる少なくとも1種以上を0.01〜5%含有してな
る請求項1に記載のパ−ル光沢顔料。
3. The synthetic mica is Ti, Zn, Na,
The pearlescent pigment according to claim 1, which comprises 0.01 to 5% of at least one selected from the group consisting of B, Li, Ca, Ge, Sr, and Zr.
【請求項4】前記合成マイカ中の鉄含有量を0.1%以
下とした請求項1または2に記載のパ−ル光沢顔料。
4. The pearl luster pigment according to claim 1, wherein the iron content in the synthetic mica is 0.1% or less.
【請求項5】前記合成マイカは、面方向の径が、3〜1
00ミクロン、厚みが0.05〜1ミクロンの鱗片状粒
子である請求項1〜4のいずれかに記載のパ−ル光沢顔
料。
5. The synthetic mica has a diameter of 3 to 1 in the plane direction.
The pearl luster pigment according to any one of claims 1 to 4, which is a scaly particle having a size of 00 microns and a thickness of 0.05 to 1 micron.
【請求項6】前記合成マイカの平均アスペクト比が、6
0以上である請求項1〜5のいずれかに記載のパ−ル光
沢顔料。
6. The average aspect ratio of the synthetic mica is 6
The pearl luster pigment according to any one of claims 1 to 5, which is 0 or more.
【請求項7】前記金属酸化物をルチル化してなる請求項
1〜6のいずれかに記載のパ−ル光沢顔料。
7. The pearlescent pigment according to claim 1, which is formed by rutileizing the metal oxide.
【請求項8】前記金属酸化物が二酸化チタンであり、該
二酸化チタンを塩化スズでルチル化してなる請求項7に
記載のパ−ル光沢顔料。
8. The pearlescent pigment according to claim 7, wherein the metal oxide is titanium dioxide, and the titanium dioxide is rutile-ized with tin chloride.
【請求項9】合成マイカ上に金属酸化物を被覆したパ−
ル光沢顔料に於いて、前記合成マイカの粒子表面を平滑
とし、合成マイカ中の鉄含有量を1.0%以下としたパ
−ル光沢顔料を配合したことを特徴とする塗料組成物。
9. A perforated sheet of synthetic mica coated with a metal oxide.
A coating composition comprising a pearl luster pigment having a particle surface of the synthetic mica smoothed and having an iron content in the synthetic mica of 1.0% or less.
【請求項10】合成マイカ上に金属酸化物を被覆したパ
−ル光沢顔料に於いて、前記合成マイカの粒子表面を平
滑とし、合成マイカ中の鉄含有量を1.0%以下とした
パ−ル光沢顔料を配合したことを特徴とする化粧料。
10. A pearl luster pigment comprising a synthetic mica coated with a metal oxide, wherein the surface of the particles of the synthetic mica is made smooth, and the iron content in the synthetic mica is 1.0% or less. -A cosmetic material characterized by containing a luster pigment.
【請求項11】合成マイカ上に金属酸化物を被覆したパ
−ル光沢顔料に於いて、前記合成マイカの粒子表面を平
滑とし、合成マイカ中の鉄含有量を1.0%以下とした
パ−ル光沢顔料を配合したことを特徴とするインキ。
11. A pearl luster pigment comprising a synthetic mica coated with a metal oxide, wherein the particle surface of the synthetic mica is made smooth, and the iron content in the synthetic mica is 1.0% or less. -An ink characterized by containing a luster pigment.
【請求項12】合成マイカ上に金属酸化物を被覆したパ
−ル光沢顔料に於いて、前記合成マイカの粒子表面を平
滑とし、合成マイカ中の鉄含有量を1.0%以下とした
パ−ル光沢顔料を配合したことを特徴とするプラスチッ
ク。
12. A pearl luster pigment comprising a synthetic mica coated with a metal oxide, wherein the surface of the particles of the synthetic mica is made smooth, and the iron content in the synthetic mica is 1.0% or less. -A plastic characterized by containing a luster pigment.
JP9752095A 1995-01-27 1995-03-31 Pall gloss pigment and coating composition, cosmetic, ink and plastic containing the pigment Expired - Fee Related JP2889837B2 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
JP9752095A JP2889837B2 (en) 1995-01-27 1995-03-31 Pall gloss pigment and coating composition, cosmetic, ink and plastic containing the pigment
US08/582,427 US5741355A (en) 1995-01-27 1996-01-03 Pearlescent pigment, and paint composition, cosmetic material, ink and plastics blended with the new pearlescent pigment

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP7-30182 1995-01-27
JP3018295 1995-01-27
JP9752095A JP2889837B2 (en) 1995-01-27 1995-03-31 Pall gloss pigment and coating composition, cosmetic, ink and plastic containing the pigment

Publications (2)

Publication Number Publication Date
JPH08259841A true JPH08259841A (en) 1996-10-08
JP2889837B2 JP2889837B2 (en) 1999-05-10

Family

ID=26368490

Family Applications (1)

Application Number Title Priority Date Filing Date
JP9752095A Expired - Fee Related JP2889837B2 (en) 1995-01-27 1995-03-31 Pall gloss pigment and coating composition, cosmetic, ink and plastic containing the pigment

Country Status (1)

Country Link
JP (1) JP2889837B2 (en)

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002155240A (en) * 2000-11-22 2002-05-28 Nippon Paint Co Ltd Bright coating composition, method for forming film and multilayered film
JP2002155243A (en) * 2000-11-22 2002-05-28 Nippon Paint Co Ltd Method for forming bright film and coated material
JP2003011260A (en) * 2001-06-29 2003-01-15 Pilot Ink Co Ltd Metallic luster style heat discolorative laminate
JP2003034005A (en) * 2001-07-24 2003-02-04 Pilot Ink Co Ltd Metal gloss-like reversible temperature-sensitive multicolor color-changeable laminate
JP2003054936A (en) * 2001-08-10 2003-02-26 Topy Ind Ltd Method for producing synthetic sheet silicate
JP2007063127A (en) * 2006-10-23 2007-03-15 Topy Ind Ltd Mica-based composite material and its producing method
JP2007308361A (en) * 2006-04-16 2007-11-29 National Institute Of Advanced Industrial & Technology Clay mineral particle having grown particle and method of manufacturing clay mineral particle
JP2008163046A (en) * 1998-12-23 2008-07-17 Merck Patent Gmbh Use of pigment mixture in cosmetic preparation
JP2009544818A (en) * 2006-07-21 2009-12-17 ビー・エイ・エス・エフ、コーポレーション Synthetic mica-based ferrite-containing pearlescent pigments
JP2011046695A (en) * 2009-07-30 2011-03-10 Fujifilm Corp Cosmetic
CZ304584B6 (en) * 2013-10-15 2014-07-16 Vysoká Škola Báňská-Technická Univerzita Ostrava Process for preparing pearlescent pigment based on graphite/TiO2

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016216751A (en) * 1998-12-23 2016-12-22 メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングMerck Patent Gesellschaft mit beschraenkter Haftung Pigment mixture
JP2017203163A (en) * 1998-12-23 2017-11-16 メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングMerck Patent Gesellschaft mit beschraenkter Haftung Pigment mixture
JP2008163046A (en) * 1998-12-23 2008-07-17 Merck Patent Gmbh Use of pigment mixture in cosmetic preparation
JP2017160462A (en) * 1998-12-23 2017-09-14 メルク パテント ゲゼルシャフト ミット ベシュレンクテル ハフツングMerck Patent Gesellschaft mit beschraenkter Haftung Pigment mixture
JP2002155243A (en) * 2000-11-22 2002-05-28 Nippon Paint Co Ltd Method for forming bright film and coated material
JP2002155240A (en) * 2000-11-22 2002-05-28 Nippon Paint Co Ltd Bright coating composition, method for forming film and multilayered film
JP2003011260A (en) * 2001-06-29 2003-01-15 Pilot Ink Co Ltd Metallic luster style heat discolorative laminate
JP2003034005A (en) * 2001-07-24 2003-02-04 Pilot Ink Co Ltd Metal gloss-like reversible temperature-sensitive multicolor color-changeable laminate
JP2003054936A (en) * 2001-08-10 2003-02-26 Topy Ind Ltd Method for producing synthetic sheet silicate
JP2007308361A (en) * 2006-04-16 2007-11-29 National Institute Of Advanced Industrial & Technology Clay mineral particle having grown particle and method of manufacturing clay mineral particle
JP2009544818A (en) * 2006-07-21 2009-12-17 ビー・エイ・エス・エフ、コーポレーション Synthetic mica-based ferrite-containing pearlescent pigments
JP4624333B2 (en) * 2006-10-23 2011-02-02 トピー工業株式会社 Mica-based composite material and method for producing the same
JP2007063127A (en) * 2006-10-23 2007-03-15 Topy Ind Ltd Mica-based composite material and its producing method
JP2011046695A (en) * 2009-07-30 2011-03-10 Fujifilm Corp Cosmetic
CZ304584B6 (en) * 2013-10-15 2014-07-16 Vysoká Škola Báňská-Technická Univerzita Ostrava Process for preparing pearlescent pigment based on graphite/TiO2

Also Published As

Publication number Publication date
JP2889837B2 (en) 1999-05-10

Similar Documents

Publication Publication Date Title
KR0178855B1 (en) Pearlescent pigment and paint compositions cosmetic material ink ind plastics blended therewith
US6019831A (en) Non-lustrous pigments
JP4647494B2 (en) Black bright pigment and cosmetics, coating composition, resin composition and ink composition containing the same
JP4334204B2 (en) High-luminance and high-saturation iris pigment and method for producing the same
US8211225B2 (en) Magnetic pigments and process of enhancing magnetic properties
US5741355A (en) Pearlescent pigment, and paint composition, cosmetic material, ink and plastics blended with the new pearlescent pigment
EP2075290A2 (en) Improved effect pigment comprising a mixture of at least 2 substrate materials
JP2003055575A (en) Color pigment
JP2889837B2 (en) Pall gloss pigment and coating composition, cosmetic, ink and plastic containing the pigment
JP3934819B2 (en) Silky luster pigment and coating composition, cosmetic, ink and plastic containing the pigment
JP3673844B2 (en) Novel par gloss pigment and coating composition, cosmetic, ink and plastic containing the pigment
JP2922148B2 (en) Novel pearlescent pigments and coating compositions, cosmetics, inks and plastics containing the pigments
CA2511990C (en) Improved effect pigment
US20080118448A1 (en) Colored Metal Pigments, Method for the Production Thereof, Use of the Colored Metal Pigments in Cosmetics, and Cosmetic Containing These
JP2646454B2 (en) Coated pigment
JP5186071B2 (en) Silky luster pigment
JPS63254169A (en) Coating pigment and production thereof
JP4190174B2 (en) High iris color titanium oxide and its manufacturing method
JPH08269357A (en) Pearl-lustered pigment
JPH05230395A (en) Scaly pigment composition, its production and cosmetic blended with the same
JP3884534B2 (en) Cosmetics
JP2931180B2 (en) Method for producing iron-containing ultrafine titanium dioxide
JP2000290526A (en) Pearly lustrous pigment, paint composition, cosmetic, ink and plastic containing said pigment
JPH08199087A (en) Novel pearlescent pigment, and coating composition, cosmetic, ink and plastic containing same
KR100736859B1 (en) Black glazed cosmetice without black absorbent colors

Legal Events

Date Code Title Description
R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

R250 Receipt of annual fees

Free format text: JAPANESE INTERMEDIATE CODE: R250

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20100219

Year of fee payment: 11

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20110219

Year of fee payment: 12

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20110219

Year of fee payment: 12

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20120219

Year of fee payment: 13

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130219

Year of fee payment: 14

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130219

Year of fee payment: 14

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20140219

Year of fee payment: 15

LAPS Cancellation because of no payment of annual fees