JP2001234090A - Color flake pigment and method for producing the same - Google Patents
Color flake pigment and method for producing the sameInfo
- Publication number
- JP2001234090A JP2001234090A JP2000044142A JP2000044142A JP2001234090A JP 2001234090 A JP2001234090 A JP 2001234090A JP 2000044142 A JP2000044142 A JP 2000044142A JP 2000044142 A JP2000044142 A JP 2000044142A JP 2001234090 A JP2001234090 A JP 2001234090A
- Authority
- JP
- Japan
- Prior art keywords
- pigment
- hydrotalcite
- particles
- flake
- double hydroxide
- 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.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、粉体における滑り
感と塗布層における視覚効果や被覆保護効果が有用性を
もち、加えて人体無害性が要求されるメイクアップ化粧
品等の分野で着色料となるフレーク顔料とその製造法に
関するものである。BACKGROUND OF THE INVENTION The present invention relates to a coloring agent in the field of makeup cosmetics and the like in which the slipperiness of a powder, the visual effect and the protective effect of a coating layer are useful, and in addition, harmlessness to the human body is required. And a method for producing the flake pigment.
【０００２】[0002]
【従来の技術】従来、感触や仕上がりを重視するメイク
アップ化粧品分野でのタルク、雲母、セリサイト、カオ
リンなど天然物の利用を初め、塗膜における光学的効果
や被覆保護効果を目的として、薄片状炭酸カルシウム、
薄片状硫酸バリウム、薄片状酸化亜鉛、酸化チタン被覆
雲母、水酸化アルミニウム被覆雲母などの無機フレーク
顔料が次々と開発されてきた。これらの新素材の出現は
塗装の多様化をもたらし、美的役割や保護的役割によっ
てメイクアップ化粧品の機能化の一端を担うものとなっ
ている。2. Description of the Related Art Conventionally, the use of natural products such as talc, mica, sericite, kaolin, etc. in the field of makeup cosmetics, which emphasizes the feel and finish, has been studied for the purpose of optical effect and coating protection effect on coating films. Calcium carbonate,
Inorganic flake pigments such as flaky barium sulfate, flaky zinc oxide, titanium oxide-coated mica, and aluminum hydroxide-coated mica have been developed one after another. The emergence of these new materials has led to the diversification of coatings and has played a part in the functionalization of makeup cosmetics through aesthetic and protective roles.
【０００３】[0003]
【発明が解決しようとする課題】前記無機フレーク顔料
は本質的に無彩色顔料であり、着色の目的には別途着色
料の添加を必要とする。本発明では、塗装の多様化や化
粧料の機能化のための新素材とするために、鮮明で濃色
な有彩色フレーク顔料を開発する。The above-mentioned inorganic flake pigment is essentially an achromatic pigment, and requires a separate addition of a coloring agent for coloring. In the present invention, a chromatic flake pigment having a clear and dark color is developed in order to use it as a new material for diversifying coatings and functionalizing cosmetics.
【０００４】[0004]
【課題を解決するための手段】本発明者らは、ハイドロ
タルサイト型層状複水酸化物の結晶構造の層間にアニオ
ンとして色素アニオンを導入した着色組成物（ハイドロ
タルサイト型着色組成物と称する）が、平面６角網状層
構造においてケイ酸塩粘土鉱物の層構造と整合性を有す
るために、タルク，雲母，セリサイト，カオリン等の無
機フレーク状粒子表面において結晶核生成することを見
出した。この現象を利用してフレーク状粒子の表面をハ
イドロタルサイト型着色組成物で被覆することを着想
し、本発明に至った。Means for Solving the Problems The present inventors have proposed a coloring composition in which a dye anion is introduced as an anion between layers having a crystal structure of a hydrotalcite-type layered double hydroxide (referred to as a hydrotalcite-type coloring composition). ) Has been found to form crystal nuclei on the surface of inorganic flake-like particles such as talc, mica, sericite, kaolin, etc. in order to have consistency with the layer structure of the silicate clay mineral in the planar hexagonal mesh layer structure. . The present invention was conceived to cover the surface of the flake-like particles with a hydrotalcite-type coloring composition by utilizing this phenomenon, and reached the present invention.
【０００５】即ち、本発明が提供するのは、無機フレー
ク状粒子上にハイドロタルサイト型着色組成物の被覆層
を有することを特徴とする着色フレーク顔料であり、ま
た、その製造法として、無機フレーク状粒子を含有する
水性懸濁液中で可溶性アニオン色素と複数の可溶性金属
塩と中和用塩基とを反応させて、該フレーク状粒子表面
上にハイドロタルサイト型着色組成物を析出生成させる
ことを特徴とする方法である。That is, the present invention provides a colored flake pigment characterized in that a coating layer of a hydrotalcite-type coloring composition is provided on inorganic flake-like particles. A soluble anionic dye, a plurality of soluble metal salts, and a neutralizing base are reacted in an aqueous suspension containing flake-like particles to precipitate and form a hydrotalcite-type coloring composition on the surface of the flake-like particles. A method characterized by the following.
【０００６】[0006]
【発明の実施の形態】ハイドロタルサイト型着色組成物
とは、マグネシウム、カルシウム、亜鉛等の二価金属イ
オン（Ｍ）とアルミニウムのような三価金属イオン
（Ｍ'）から形成されるハイドロタルサイト型層状複水
酸化物［Ｍ1-xＭ'x(ＯＨ)2］(Ａn-)x/n・ｍＨ2Ｏ （0.2
≦ｘ≦0.33）において、層間アニオン（Ａn-）として色
素アニオンを導入して得られる層状の結晶構造をもった
着色組成物であり、これを生成させるには大別して３種
の方法がある。第１は、Ａn-がＣl-であるＣl形ハイド
ロタルサイトをアニオン色素水溶液に接してアニオン交
換させるイオン交換法である。第２は、ＣＯ3形ハイド
ロタルサイトを約500℃で焼成し、脱水・脱炭酸させて
一旦無定形酸化物としたのち、水溶液中で色素アニオン
と反応させ、アニオン交換された形でハイドロタルサイ
ト構造を再生させる再構築法である。第３は、前記組成
式に従う複数の金属塩溶液と色素溶液および中和当量の
塩基溶液を適宜の方法で混合して、色素アニオン形ハイ
ドロタルサイトを析出させる直接生成法である。それぞ
れの方法によって到達される色素含有量を前記組成式に
よる理論量と比較し百分率として表わすと、赤色２０１
号の場合、第１の方法では75％まで、第２の方法では45
％までであるのに対し、第３の方法では95％以上で色素
アニオンを含有するハイドロタルサイト型着色組成物が
得られる（久保、辻：色材協会誌，69［10］，667-677
頁（1996年））。本発明のためにはいずれの方法も採用
しうるが、濃色の着色フレーク顔料を得る目的には、こ
の直接生成法が最も適している。BEST MODE FOR CARRYING OUT THE INVENTION A hydrotalcite-type coloring composition refers to a hydrotalcite formed from a divalent metal ion (M) such as magnesium, calcium, and zinc and a trivalent metal ion (M ') such as aluminum. Site type layered double hydroxide [M 1-x M ′ x (OH) 2 ] (A n− ) x / n · mH 2 O (0.2
≦ x ≦ 0.33), a colored composition having a layered crystal structure obtained by introducing a dye anion as an interlayer anion (A n− ). There are roughly three methods for producing this. . First, A n-it is Cl - ion exchange method in which anion exchange against the Cl form hydrotalcite anionic dye solution is. Second, CO 3 type hydrotalcite is calcined at about 500 ° C., dehydrated and decarboxylated to form an amorphous oxide, and then reacted with a dye anion in an aqueous solution to form an anion-exchanged hydrotalcite. This is a reconstruction method that reproduces the site structure. The third is a direct production method in which a plurality of metal salt solutions according to the above composition formula, a dye solution and a neutralization equivalent base solution are mixed by an appropriate method to precipitate a dye anion-type hydrotalcite. When the dye content achieved by each method is compared with the theoretical amount according to the above composition formula and expressed as a percentage, red 201
In the case of No. 1, up to 75% in the first method and 45% in the second method
%, Whereas in the third method, a hydrotalcite-type coloring composition containing 95% or more of a pigment anion can be obtained (Kubo, Tsuji: Journal of the Society of Color Materials, 69 [10], 667-677).
P. (1996)). Either method can be employed for the present invention, but for the purpose of obtaining a dark colored flake pigment, this direct production method is most suitable.
【０００７】本発明の製法で使用される金属塩として
は、人体無害性の観点から、二価金属に対してはマグネ
シウム、カルシウム、亜鉛等の塩化物、硫酸塩、硝酸塩
等が、三価金属に対してはアルミニウムの塩化物、硫酸
塩、硝酸塩等およびアルミン酸ナトリウムが用いられ
る。中和に用いる塩基物質としては、水酸化ナトリウム
やアンモニアや尿素等を用いうるが、炭酸ナトリウムは
ＣＯ3形ハイドロタルサイトを優先して生成させるため
不可である。アニオン色素としては、食用黄色４号(Tar
trazine)，黄色５号(Sunset Yellow FCF)，青色１号(Br
illiant Blue FCF)，赤色３号(Erythrosine)，赤色１０
４号(Floxine B)，赤色２０１号(Lithol Rubin B)等
の、食品衛生法または薬事法で規定された食品，医薬
品，医薬部外品および化粧品用タール色素の中から選ば
れる可溶性アニオン色素が用いられる。[0007] From the viewpoint of harmlessness to the human body, chlorides, sulfates, nitrates and the like of magnesium, calcium, zinc and the like are used as the metal salts used in the production method of the present invention. For these, aluminum chloride, sulfate, nitrate and the like and sodium aluminate are used. As the basic substance used for neutralization, sodium hydroxide, ammonia, urea, or the like can be used, but sodium carbonate is not possible because CO 3 -type hydrotalcite is preferentially generated. Edible Yellow No. 4 (Tar
trazine), Yellow No. 5 (Sunset Yellow FCF), Blue No. 1 (Br
illiant Blue FCF), Red No. 3 (Erythrosine), Red 10
No. 4 (Floxine B), Red No. 201 (Lithol Rubin B), etc., soluble anionic dyes selected from tar dyes for foods, pharmaceuticals, quasi-drugs and cosmetics prescribed by the Food Sanitation Law or the Pharmaceutical Affairs Law Used.
【０００８】製造工程においては、前記の原料物質をそ
れぞれ水に溶解し（赤色２０１号のように溶解度の低い
ものは懸濁させ）、アニオン色素の種類に応じて２種な
いし４種、あるいは５種（尿素を添加する場合）の別個
の溶液としたのち、最終的にはこれらを無機フレーク状
粒子を分散させた懸濁液と合して一つに混合する。反応
槽中にはフレーク粒子懸濁液および色素溶液と予め混合
できる原料溶液とを入れ、よく撹拌しつつこの中にその
他の原料溶液を滴下混合する。予め混合できる原料溶液
の組合せは、各原料の反応性などを考慮して決められ
る。青色１号のように耐酸および耐塩基性を欠く色素に
対しては、反応槽中で色素溶液のｐＨを終始中性域に保
つために、金属塩溶液と中和塩基溶液を同時滴下する。
赤色２０１号のように耐塩基性の大な色素においては、
アルミン酸ナトリウム溶液あるいは中和塩基溶液と予め
混合しておくことができる。滴下混合終了後８０℃以上
に加温熟成することにより、徐々にハイドロタルサイト
型着色組成物がフレーク粒子表面に生成する。生成速度
は原料物質および混合方法によって異なり、半日から数
日に及ぶ。In the production process, the above-mentioned raw materials are each dissolved in water (a substance having a low solubility such as Red No. 201 is suspended), and two to four or five or five kinds are selected depending on the kind of the anionic dye. After separate solutions of the seeds (if urea is added), they are finally combined with the suspension in which the inorganic flake-like particles are dispersed and mixed together. A flake particle suspension and a raw material solution that can be mixed in advance with the dye solution are put into the reaction tank, and the other raw material solutions are dropped and mixed therein with good stirring. The combination of the raw material solutions that can be mixed in advance is determined in consideration of the reactivity of each raw material and the like. For a dye lacking acid resistance and base resistance, such as Blue No. 1, a metal salt solution and a neutralizing base solution are simultaneously dropped in the reaction vessel in order to keep the pH of the dye solution in a neutral range throughout.
In a dye having a large basic resistance such as Red No. 201,
It can be previously mixed with a sodium aluminate solution or a neutralization base solution. After completion of the dropping and mixing, the mixture is heated and aged at 80 ° C. or higher, whereby a hydrotalcite-type coloring composition is gradually formed on the surface of the flake particles. The rate of formation depends on the raw materials and mixing method and ranges from half a day to several days.
【０００９】前述の方法で無機フレーク状粒子表面をハ
イドロタルサイト型着色組成物で被覆することができる
が、被覆物の性状には用いる原料と中和方法によって顕
著な差異が生ずる。金属塩化物を原料として用い水酸化
ナトリウムで中和する方法では、図１（実施例１）に示
すような微粒子集合体による被覆となり、粒子表面の平
滑性が失われる。同じ原料で水酸化ナトリウムの６分の
１を尿素に替えると、図２（実施例７）に示すような均
一で平滑な被覆が得られる。Although the surface of the inorganic flake particles can be coated with the hydrotalcite-type coloring composition by the above-mentioned method, the properties of the coating vary significantly depending on the raw materials used and the neutralization method. In the method of using metal chloride as a raw material and neutralizing with sodium hydroxide, coating with fine particle aggregates as shown in FIG. 1 (Example 1) is performed, and the smoothness of the particle surface is lost. If one sixth of sodium hydroxide is replaced with urea using the same raw material, a uniform and smooth coating as shown in FIG. 2 (Example 7) can be obtained.
【００１０】[0010]
【作用】ハイドロタルサイト型着色組成物が前記粘土鉱
物のフレーク状粒子表面に析出して被覆するという作用
については、次のような説明を与えることができる。ハ
イドロタルサイト型構造はブルーサイト(Ｍｇ(ＯＨ)2)
型の平面６角網状層を基本とするが、この層と前記粘土
鉱物のケイ酸塩平面６角網状層とは酸素イオンの配置に
おいて整合する。このため、原料混合溶液からハイドロ
タルサイト型構造が析出する際に、粘土鉱物表面が核生
成の場となりうる。核生成速度が速く結晶核がフレーク
粒子表面上の各所に多数生成すれば、被覆は微粒子集合
体となって表面平滑性を失う。中和塩基の一部として尿
素を添加することは核生成速度を遅らせる効果をもち、
ランダムな核生成が抑制されて平滑な表面被覆が形成さ
れると推定される。The effect that the hydrotalcite-type coloring composition is deposited on the surface of the flake-like particles of the clay mineral and coated thereon can be explained as follows. Hydrotalcite type structure is brucite (Mg (OH) 2 )
It is based on a planar hexagonal reticulated layer of a mold, which layer and the silicate planar hexagonal reticulated layer of the clay mineral are matched in the arrangement of oxygen ions. For this reason, when the hydrotalcite-type structure is precipitated from the raw material mixed solution, the clay mineral surface can be a nucleation site. If the nucleation rate is high and a large number of crystal nuclei are formed at various places on the surface of the flake particle, the coating becomes a fine particle aggregate and loses surface smoothness. The addition of urea as part of the neutralizing base has the effect of slowing the nucleation rate,
It is presumed that random nucleation is suppressed and a smooth surface coating is formed.
【００１１】[0011]
【実施例】次に、本発明の具体的態様を示すために、比
較例とともに代表的な実施例を挙げるが、本発明の技術
的範囲を限定するものではない。EXAMPLES Next, in order to show specific embodiments of the present invention, representative examples will be given together with comparative examples, but the technical scope of the present invention is not limited thereto.
【００１２】実施例１ 黄色５号（純度91.6％）12.4g、0.5N-NaOH 620mLおよび
水砕雲母粉（平均粒径24.1μm）50.0gを1.5Lの三角フラ
スコ中にとり、煮沸して脱炭酸した水を用いて全量 1,0
00mLの均一な分散液とする。別にMgCl2・6H2O 20.3gとA
lCl3・6H2O 12.1gとを水に溶解して300mLとした溶液を
作り、上記の分散液中に撹拌しつつ室温で１時間かけて
滴下混合する。水を加えて全量を1,500mLとしたのち室
温でさらに１時間撹拌を続け、次いで100℃に加温して2
4時間還流しつつ撹拌する。この熟成によって雲母粒子
表面にハイドロタルサイト型着色組成物が生成し、鮮明
な橙色となる。熟成終了後室温にまで冷却し、生成物を
濾過して濾液が殆ど無色になるまで水で繰り返し洗浄を
行ったのち、50℃で乾燥する。この方法により収量67.7
gで橙色フレーク顔料を得た。（生成物の走査型電子顕
微鏡写真を図１に示す。） Example 1 12.4 g of Yellow No. 5 (purity: 91.6%), 620 mL of 0.5N-NaOH and 50.0 g of granulated mica powder (average particle size: 24.1 μm) were placed in a 1.5 L Erlenmeyer flask, boiled and decarbonated. 1,0 using water
Make a uniform dispersion of 00 mL. Separately MgCl 2 · 6H 2 O 20.3g and A
A solution prepared by dissolving 12.1 g of lCl 3 .6H 2 O in water to make 300 mL is mixed dropwise with the above dispersion at room temperature for 1 hour with stirring. After adding water to make the total volume 1,500 mL, stirring was continued at room temperature for another hour, and then the mixture was heated to 100 ° C.
Stir at reflux for 4 hours. Due to this aging, a hydrotalcite-type coloring composition is formed on the surface of the mica particles, and becomes a clear orange color. After completion of aging, the mixture is cooled to room temperature, the product is filtered, washed repeatedly with water until the filtrate becomes almost colorless, and then dried at 50 ° C. This method yields 67.7
g gave an orange flake pigment. (A scanning electron micrograph of the product is shown in FIG. 1.)
【００１３】実施例２ 青色１号（純度91.6％）21.6gと水砕セリサイト粉（平
均粒径20.0μm）50.0gを1.5Lの三角フラスコ中にとり、
煮沸して脱炭酸した水に溶解して全量 300mLの均一な分
散液とする。別にMgCl2・6H2O 20.3gを水に溶解して300
mLとした溶液とAlCl3・6H2O 12.1gを水に溶解して300mL
とした溶液を作り、0.5N-NaOH溶液 600mLとともに、３
溶液同時的に上記の分散液中に撹拌しつつ室温で１時間
かけて滴下混合する。水を加えて全量を1,500mLとした
のち室温でさらに１時間撹拌を続け、次いで100℃に加
温して24時間還流しつつ撹拌する。この熟成によってセ
リサイト粒子表面にハイドロタルサイト型着色組成物が
生成し、青色が鮮明化する。以下、実施例１と同様に行
って、青色フレーク顔料68.6gを得た。 Example 2 21.6 g of Blue No. 1 (purity: 91.6%) and 50.0 g of granulated sericite powder (average particle size: 20.0 μm) were placed in a 1.5 L Erlenmeyer flask.
Dissolve in boiling and decarbonated water to make a uniform dispersion of 300 mL in total volume. Separately MgCl 2 · 6H 2 O 20.3g was dissolved in water 300
mL and solution with the AlCl 3 · 6H 2 O 12.1g was dissolved in water 300mL
Solution with 600 mL of 0.5N-NaOH solution and 3
The solution is simultaneously added dropwise to the above dispersion at room temperature for 1 hour while stirring. After adding water to make the total amount 1,500 mL, stirring is further continued at room temperature for 1 hour, and then the mixture is heated to 100 ° C. and stirred under reflux for 24 hours. By this aging, a hydrotalcite-type coloring composition is formed on the surface of the sericite particles, and the blue color is sharpened. Hereinafter, in the same manner as in Example 1, 68.6 g of a blue flake pigment was obtained.
【００１４】実施例３ 赤色201号（純度92.5％）11.6g、0.5N-NaOH 620mLおよ
び水砕タルク粉（平均粒径17.8μm）50.0gを1.5Lの三角
フラスコ中にとり、煮沸して脱炭酸した水を用いて全量
1,000mLの均一な分散液とする。別にMgSO4・7H2O 24.7
gとAl2(SO4)3・18H2O 16.7gとを水に溶解して300mLとし
た溶液を作り、上記の分散液中に撹拌しつつ室温で１時
間かけて滴下混合する。水を加えて全量を1,500mLとし
たのち室温でさらに１時間撹拌を続け、次いで100℃に
加温して還流しつつ24時間撹拌する。この熟成によって
タルク粒子表面にハイドロタルサイト型着色組成物が生
成し、赤色が鮮明化する。以下、実施例１と同様に行っ
て、赤色フレーク顔料68.2gを得た。 Example 3 11.6 g of Red No. 201 (purity: 92.5%), 620 mL of 0.5N-NaOH and 50.0 g of granulated talc powder (average particle size: 17.8 μm) were placed in a 1.5 L Erlenmeyer flask, boiled and decarbonated. Total amount using water
Make a 1,000 mL homogeneous dispersion. Separately MgSO 4 · 7H 2 O 24.7
g and 16.7 g of Al 2 (SO 4 ) 3 .18H 2 O are dissolved in water to make a 300 mL solution, and the mixture is added dropwise to the above dispersion at room temperature for 1 hour with stirring. After adding water to make the total amount 1,500 mL, stirring is further continued for 1 hour at room temperature, and then the mixture is heated to 100 ° C. and stirred for 24 hours while refluxing. By this aging, a hydrotalcite-type coloring composition is formed on the surface of the talc particles, and the red color is sharpened. Thereafter, the same procedure as in Example 1 was carried out to obtain 68.2 g of a red flake pigment.
【００１５】実施例４ 黄色５号（純度91.6％）12.4g、0.5N-NaOH 145mL、アル
ミン酸ナトリウム溶液（浅田化学工業K.K.製＃2019, Al
2O3 20％, Na2O 19％, 比重 1.50）12.8gおよび水砕セ
リサイト粉（平均粒径20.0μm）50.0gを1.5Lの三角フラ
スコ中にとり、煮沸して脱炭酸した水を用いて全量 1,0
00mLの均一な分散液とする。別にMgSO4・7H2O 24.7gを
水に溶解して300mLとした溶液を作り、上記の分散液中
に撹拌しつつ室温で１時間かけて滴下混合する。水を加
えて全量を1,500mLとしたのち室温でさらに１時間撹拌
を続け、次いで100℃に加温して還流しつつ24時間撹拌
する。以下、実施例１と同様に行って、橙色フレーク顔
料66.7gを得た。 Example 4 12.4 g of Yellow No. 5 (purity: 91.6%), 145 mL of 0.5 N NaOH, sodium aluminate solution (# 2019, Al, manufactured by Asada Chemical Industry KK)
2 O 3 20%, Na 2 O 19%, taking the specific gravity 1.50) 12.8 g and granulated sericite powder (average particle diameter 20.0 .mu.m) 50.0 g in an Erlenmeyer flask of 1.5 L, using boiled decarboxylated water 1,0
Make a uniform dispersion of 00 mL. Separately MgSO 4 · 7H 2 O 24.7g create a solution was 300mL dissolved in water and mixed dropwise over 1 hour at room temperature with stirring to the dispersion in the. After adding water to make the total amount 1,500 mL, stirring is further continued for 1 hour at room temperature, and then the mixture is heated to 100 ° C. and stirred for 24 hours while refluxing. Thereafter, the same procedure as in Example 1 was carried out to obtain 66.7 g of an orange flake pigment.
【００１６】実施例５ 黄色５号（純度91.6％）12.4gと水砕セリサイト粉（平
均粒径20.0μm）50.0gを1.5Lの三角フラスコ中にとり、
煮沸して脱炭酸した水に溶解して全量 300mLの均一な分
散液とする。別にZnSO4・7H2O 28.8gとAl2(SO4)3・18H2
O 16.7gを水に溶解して300mLとした溶液を作り、0.5N-N
aOH溶液 600mLとともに、２溶液同時的に上記の分散液
中に撹拌しつつ室温で１時間かけて滴下混合する。水を
加えて全量を1,500mLとしたのち室温でさらに１時間撹
拌を続け、次いで100℃に加温して24時間還流しつつ撹
拌する。以下、実施例１と同様に行って、橙色フレーク
顔料71.2gを得た。 Example 5 12.4 g of Yellow No. 5 (purity: 91.6%) and 50.0 g of granulated sericite powder (average particle size: 20.0 μm) were placed in a 1.5 L Erlenmeyer flask.
Dissolve in boiling and decarbonated water to make a uniform dispersion of 300 mL in total volume. Separately ZnSO 4 · 7H 2 O 28.8g and Al 2 (SO 4) 3 · 18H 2
Dissolve 16.7g of O in water to make a solution of 300mL, 0.5NN
With 600 mL of the aOH solution, the two solutions are simultaneously added dropwise to the above dispersion at room temperature for 1 hour with stirring. After adding water to make the total amount 1,500 mL, stirring is further continued at room temperature for 1 hour, and then the mixture is heated to 100 ° C. and stirred under reflux for 24 hours. Hereinafter, in the same manner as in Example 1, 71.2 g of an orange flake pigment was obtained.
【００１７】実施例６ 赤色201号（純度92.5％）11.6g、0.5N-NaOH 145mL、ア
ルミン酸ナトリウム溶液（浅田化学工業K.K.製＃2019,
Al2O3 20％, Na2O 19％, 比重 1.50）12.8gおよびカオ
リナイト（平均粒径18.2μm）50.0gを1.5Lの三角フラス
コ中にとり、煮沸して脱炭酸した水を用いて全量 1,000
mLの均一な分散液とする。別にMgSO4・7H2O 24.7gを水
に溶解して300mLとした溶液を作り、上記の分散液中に
撹拌しつつ室温で１時間かけて滴下混合する。水を加え
て全量を1,500mLとしたのち室温でさらに１時間撹拌を
続け、次いで100℃に加温して還流しつつ24時間撹拌す
る。以下、実施例１と同様に行って、赤色フレーク顔料
66.1gを得た。 Example 6 11.6 g of Red No. 201 (purity: 92.5%), 145 mL of 0.5N NaOH, sodium aluminate solution (manufactured by Asada Chemical Industry KK # 2019,
12.8 g of Al 2 O 3 20%, Na 2 O 19%, specific gravity 1.50) and 50.0 g of kaolinite (average particle size 18.2 μm) were placed in a 1.5-L Erlenmeyer flask, and all the water was added using boiling and decarbonated water. 1,000
Make a homogeneous dispersion of mL. Separately MgSO 4 · 7H 2 O 24.7g create a solution was 300mL dissolved in water and mixed dropwise over 1 hour at room temperature with stirring to the dispersion in the. After adding water to make the total amount 1,500 mL, stirring is further continued for 1 hour at room temperature, and then the mixture is heated to 100 ° C. and stirred for 24 hours while refluxing. Hereinafter, a red flake pigment was prepared in the same manner as in Example 1.
66.1 g were obtained.
【００１８】実施例７ 黄色５号（純度91.6％）12.4g、0.5N-NaOH 500mL、水砕
雲母粉（平均粒径24.1μm）50.0g、MgCl2・6H2O 20.3
g、AlCl3・6H2O 12.1gおよび尿素 41.9gを1.5Lの三角フ
ラスコ中にとり、全量 1,500mLの均一な水分散液とす
る。次いで100℃に加温して24時間還流しつつ撹拌す
る。尿素の分解とともに中和反応が進行し、雲母粒子表
面にハイドロタルサイト型着色組成物が生成して、鮮明
な橙色となる。熟成終了後室温にまで冷却し、生成物を
濾過して濾液が無色になるまで水で繰り返し洗浄を行っ
たのち、50℃で乾燥する。この方法により収量67.3gで
橙色フレーク顔料を得た。（生成物の走査型電子顕微鏡
写真を図２に示す。） Example 7 12.4 g of Yellow No. 5 (purity: 91.6%), 500 mL of 0.5N-NaOH, 50.0 g of granulated mica powder (average particle size: 24.1 μm), MgCl 2 .6H 2 O 20.3
g, take AlCl 3 · 6H 2 O 12.1g and urea 41.9g in Erlenmeyer flask 1.5 L, a uniform aqueous dispersion of the total amount 1,500 mL. Then, the mixture is heated to 100 ° C. and stirred under reflux for 24 hours. The neutralization reaction proceeds with the decomposition of urea, and a hydrotalcite-type coloring composition is formed on the surface of the mica particles, and the color becomes vivid orange. After completion of ripening, the mixture is cooled to room temperature, the product is filtered, washed repeatedly with water until the filtrate becomes colorless, and then dried at 50 ° C. By this method, orange flake pigment was obtained in a yield of 67.3 g. (A scanning electron micrograph of the product is shown in FIG. 2.)
【００１９】実施例８ 赤色201号（純度92.5％）11.6g、0.5N-NaOH 300mL、水
砕雲母粉（平均粒径24.1μm）50.0g、MgCl2・6H2O 20.3
g、AlCl3・6H2O 12.1gおよび尿素 41.9gを1.5Lの三角フ
ラスコ中にとり、全量 1,500mLの均一な水分散液とす
る。次いで100℃に加温して24時間還流しつつ撹拌す
る。尿素の分解とともに中和反応が進行し、雲母粒子表
面にハイドロタルサイト型着色組成物が生成して、赤色
が鮮明化する。以下、実施例１と同様に行って、赤色フ
レーク顔料64.3gを得た。 Example 8 11.6 g of Red No. 201 (purity: 92.5%), 300 mL of 0.5N-NaOH, 50.0 g of granulated mica powder (average particle size: 24.1 μm), MgCl 2 .6H 2 O 20.3
g, take AlCl 3 · 6H 2 O 12.1g and urea 41.9g in Erlenmeyer flask 1.5 L, a uniform aqueous dispersion of the total amount 1,500 mL. Then, the mixture is heated to 100 ° C. and stirred under reflux for 24 hours. The neutralization reaction proceeds along with the decomposition of urea, and a hydrotalcite-type coloring composition is formed on the surface of the mica particles, and the red color is sharpened. Thereafter, the same procedure as in Example 1 was carried out to obtain 64.3 g of a red flake pigment.
【００２０】[0020]
【発明の効果】無機フレーク状粒子上にハイドロタルサ
イト型着色組成物を被覆させた着色フレーク顔料を実現
させ、新規な着色料となる可能性をもたらす。According to the present invention, a colored flake pigment in which a hydrotalcite-type coloring composition is coated on inorganic flake-like particles is realized, and the possibility of becoming a new coloring agent is brought about.
【図１】実施例１による生成物の走査型電子顕微鏡写真
である。FIG. 1 is a scanning electron micrograph of a product according to Example 1.
【図２】実施例７による生成物の走査型電子顕微鏡写真
である。FIG. 2 is a scanning electron micrograph of a product according to Example 7.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） // Ａ６１Ｋ 7/02 Ａ６１Ｋ 7/02 Ｎ Ｆターム(参考） 4C083 AB441 AB442 BB25 CC11 EE06 EE07 FF01 4J037 AA26 AA27 CA11 CA12 CA15 CB28 DD10 EE02 EE16 EE17 EE43 FF09 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI theme coat ゛ (reference) // A61K 7/02 A61K 7/02 NF term (reference) 4C083 AB441 AB442 BB25 CC11 EE06 EE07 FF01 4J037 AA26 AA27 CA11 CA12 CA15 CB28 DD10 EE02 EE16 EE17 EE43 FF09
Claims (7)
たハイドロタルサイト型層状複水酸化物を無機フレーク
状粒子表面に被覆層として有することを特徴とする着色
フレーク顔料。1. A colored flake pigment comprising a hydrotalcite-type layered double hydroxide having a dye anion introduced between layers having a crystal structure as a coating layer on the surface of inorganic flake-like particles.
セリサイト、カオリンから選ばれた粘土鉱物であること
を特徴とする請求項１に記載の顔料。2. The method according to claim 1, wherein the inorganic flake particles are talc, mica,
The pigment according to claim 1, wherein the pigment is a clay mineral selected from sericite and kaolin.
がマグネシウム、カルシウム、亜鉛の二価金属から選ば
れる少なくとも１種とアルミニウムとの複水酸化物であ
ることを特徴とする請求項１に記載の顔料。3. The method according to claim 1, wherein the hydrotalcite-type layered double hydroxide is a double hydroxide of aluminum and at least one selected from divalent metals of magnesium, calcium and zinc. The pigment as described.
法で規定された食品、医薬品、医薬部外品および化粧品
用タール色素の中から選ばれる可溶性アニオン色素に由
来するアニオンであることを特徴とする請求項１に記載
の顔料。4. The dye anion is an anion derived from a soluble anion dye selected from food, pharmaceutical, quasi-drug and cosmetic tar dyes specified by the Food Sanitation Law or the Pharmaceutical Affairs Law. The pigment according to claim 1, wherein
ハイドロタルサイト型層状複水酸化物を被覆層として無
機フレーク状粒子の表面上に有する着色フレーク顔料の
製造法であって、無機フレーク状粒子を含有する水性懸
濁液中で可溶性アニオン色素と該層状複水酸化物の原料
となる複数の可溶性金属塩と中和用塩基とを反応させ、
該無機フレーク状粒子表面上に該ハイドロタルサイト型
層状複水酸化物を析出生成させることを特徴とする着色
フレーク顔料の製造法。5. A method for producing a colored flake pigment comprising a coating layer of a hydrotalcite-type layered double hydroxide having a dye anion introduced between layers having a crystal structure on the surface of inorganic flake-like particles. Reacting a soluble anion dye and a plurality of soluble metal salts and a neutralizing base as raw materials of the layered double hydroxide in an aqueous suspension containing particles,
A method for producing a colored flake pigment, comprising depositing and forming the hydrotalcite-type layered double hydroxide on the surface of the inorganic flake-like particles.
ミン酸ナトリウムであることを特徴とする請求項５に記
載の製造法。6. The method according to claim 5, wherein at least a part of the soluble metal salt is sodium aluminate.
あることを特徴とする請求項５に記載の製造法。7. The method according to claim 5, wherein at least a part of the neutralizing base is urea.
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|---|---|---|---|
| JP2000044142A JP2001234090A (en) | 2000-02-22 | 2000-02-22 | Color flake pigment and method for producing the same |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000044142A JP2001234090A (en) | 2000-02-22 | 2000-02-22 | Color flake pigment and method for producing the same |
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|---|---|
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Family
ID=18566953
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|---|---|---|---|
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| Country | Link |
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