JP2006248854A - Scaly or platy mica particle treated with phosphate and cosmetic using the particle - Google Patents
Scaly or platy mica particle treated with phosphate and cosmetic using the particle Download PDFInfo
- Publication number
- JP2006248854A JP2006248854A JP2005069068A JP2005069068A JP2006248854A JP 2006248854 A JP2006248854 A JP 2006248854A JP 2005069068 A JP2005069068 A JP 2005069068A JP 2005069068 A JP2005069068 A JP 2005069068A JP 2006248854 A JP2006248854 A JP 2006248854A
- Authority
- JP
- Japan
- Prior art keywords
- mica
- plate
- phosphoric acid
- particles
- group mineral
- 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
Links
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- 239000002245 particle Substances 0.000 title claims abstract description 152
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- 229910019142 PO4 Inorganic materials 0.000 title abstract description 7
- 239000010452 phosphate Substances 0.000 title abstract description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title abstract description 5
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- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- HCWCAKKEBCNQJP-UHFFFAOYSA-N magnesium orthosilicate Chemical compound [Mg+2].[Mg+2].[O-][Si]([O-])([O-])[O-] HCWCAKKEBCNQJP-UHFFFAOYSA-N 0.000 description 1
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- IIGMITQLXAGZTL-UHFFFAOYSA-N octyl octadecanoate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCCCCCCCC IIGMITQLXAGZTL-UHFFFAOYSA-N 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 239000004006 olive oil Substances 0.000 description 1
- 235000008390 olive oil Nutrition 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
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- 125000001820 oxy group Chemical group [*:1]O[*:2] 0.000 description 1
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- 239000003002 pH adjusting agent Substances 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
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- 239000002304 perfume Substances 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 229940066842 petrolatum Drugs 0.000 description 1
- 150000003014 phosphoric acid esters Chemical class 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
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- 239000008159 sesame oil Substances 0.000 description 1
- 239000002453 shampoo Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
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- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 210000004243 sweat Anatomy 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- DZKXJUASMGQEMA-UHFFFAOYSA-N tetradecyl tetradecanoate Chemical compound CCCCCCCCCCCCCCOC(=O)CCCCCCCCCCCCC DZKXJUASMGQEMA-UHFFFAOYSA-N 0.000 description 1
- QPQANCNBWQXGTQ-UHFFFAOYSA-N trihydroxy(trimethylsilylperoxy)silane Chemical compound C[Si](C)(C)OO[Si](O)(O)O QPQANCNBWQXGTQ-UHFFFAOYSA-N 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
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- 239000010937 tungsten Substances 0.000 description 1
- 229960002703 undecylenic acid Drugs 0.000 description 1
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Landscapes
- Cosmetics (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
本発明は、雲母族鉱物からなる鱗片状または板状雲母族鉱物粒子に関し、より詳しくは、化粧料、塗料、インキ、トナー、グリース、ゴム、プラスチックス、セラミックスなどの配合成分として有用な鱗片状または板状雲母族鉱物粒子に関する。 The present invention relates to scaly or plate-like mica group mineral particles composed of a mica group mineral, and more specifically, scaly useful as a blending component for cosmetics, paints, inks, toners, greases, rubbers, plastics, ceramics and the like. Or it relates to plate-like mica group mineral particles.
雲母族鉱物の粒子は、通常、鱗片状または板状の形状を有し、従来、化粧料、医薬部外品および医薬品などに用いられている。その中でも、白色度が高く、すべり性に優れたマイカ、セリサイトなどからなる雲母族鉱物粒子が、化粧料の体質顔料などに広く用いられている。また、このような雲母族鉱物粒子を酸化チタンによって表面被覆した表面被覆雲母族鉱物粒子も広く用いられている。例えば、合成マイカの鱗片状または板状粒子に酸化チタンを表面被覆した表面被覆雲母族鉱物粒子は、酸化チタンの高い屈折率から、その表面被覆層厚みにより多様な干渉色を生じ、パールマイカなどと呼ばれ広く用いられている。さらに、近年では、この酸化チタンに代えて酸化鉄や酸化クロムなどを被覆したものや、酸化チタンにさらに酸化鉄や酸化クロムなどを被覆した表面被覆雲母族鉱物粒子などが用いられている。また、さらに染料、顔料が複合された表面被覆雲母族鉱物粒子などが開発されそれらを総称してパール顔料もしくはパール光沢顔料といわれて化粧料などに多く用いられている。このパール顔料としては、チタン雲母、ベンガラ被覆雲母、ベンガラ被覆チタン雲母、黒酸化鉄被覆チタン雲母、カルミン被覆チタン雲母、コンジョウ被覆チタン雲母、カルミン・コンジョウ被覆チタン雲母、酸化クロム被覆チタン雲母、ベンガラ・黒酸化鉄被覆チタン雲母、黒酸化鉄カルミン被覆チタン雲母、黒酸化鉄コンジョウ被覆チタン雲母、チタン雲母＋黄色４号、チタン雲母＋赤色２０２号、チタン雲母＋青色１号、チタン雲母＋青色１号＋黄色４号などがあげられる。 Mica group mineral particles usually have a scaly or plate-like shape, and are conventionally used in cosmetics, quasi drugs, pharmaceuticals, and the like. Among them, mica group mineral particles composed of mica, sericite and the like having high whiteness and excellent slip properties are widely used as extender pigments for cosmetics. In addition, surface-coated mica group mineral particles obtained by coating such mica group mineral particles with titanium oxide are also widely used. For example, surface-coated mica group mineral particles with titanium oxide surface-coated on synthetic mica scale-like or plate-like particles produce various interference colors depending on the thickness of the surface coating layer due to the high refractive index of titanium oxide. It is called and widely used. Further, in recent years, in place of this titanium oxide, those coated with iron oxide, chromium oxide or the like, or surface-coated mica group mineral particles obtained by coating titanium oxide with iron oxide, chromium oxide or the like have been used. In addition, surface-coated mica group mineral particles combined with dyes and pigments have been developed and are generally called pearl pigments or pearl luster pigments and are widely used in cosmetics. The pearl pigments include titanium mica, bengara-coated mica, bengara-coated titanium mica, black iron oxide-coated titanium mica, carmine-coated titanium mica, conjugate-coated titanium mica, carmine-conjoux-coated titanium mica, chromium oxide-coated titanium mica, bengara Black iron oxide coated titanium mica, black iron oxide carmine coated titanium mica, black iron oxide conger coated titanium mica, titanium mica + yellow 4, titanium mica + red 202, titanium mica + blue 1, titanium mica + blue 1 + Yellow No. 4 etc.
しかし、マイカやセリサイトの雲母族鉱物粒子には、通常、天然産出のものが多く用いられることから、不純物成分を含有し、白色度の低いくすんだ状態となったり、臭いを有していたりすることが知られている。このことに対し、特許文献１には、雲母を酸およびアルカリまたは塩基性塩で処理して夾雑物を除去すること、および、その処理により白色色調を有する粉末が得られることが記載されている。
このような雲母族鉱物粒子は、通常、化粧料などに用いられる場合には、油などに分散され用いられたりしている。あるいは、粉末状態とされる場合であっても、使用時には、皮脂や汗などで湿り気を帯びた状態で用いられる。したがって、通常、雲母族鉱物粒子が化粧料などに用いられる場合には、湿潤な状態で用いられている。
However, the mica and sericite mica group mineral particles are usually naturally produced, so they contain impurities and become dull with low whiteness or have an odor. It is known to do. On the other hand, Patent Document 1 describes that mica is treated with an acid and an alkali or a basic salt to remove impurities, and a powder having a white color tone is obtained by the treatment. .
Such mica group mineral particles are usually dispersed in oil or the like when used in cosmetics or the like. Or even if it is a case where it is set as a powder state, it is used in the state dampened with sebum, sweat, etc. at the time of use. Therefore, normally, when the mica group mineral particles are used in cosmetics, they are used in a wet state.
ところで、従来、粉末を油や水などの液体で湿らせた湿潤な状態とした場合には、乾燥した粉末の状態に比べて、その色合いが変化することが知られている。例えば、粉末の状態では優れた白色度を有するものが湿潤状態では、白色度が低下してくすみを生じてしまったりしている。そのため、前述のように鱗片状または板状の雲母族鉱物粒子が化粧料などに用いられる場合などにおいてもこの雲母族鉱物粒子の白色度が低下してくすみが生じるおそれを有している。このような湿潤状態で白色度が低下することについては、その抑制方法が従来検討されておらず、先述の特許文献１においても、粉末状態での白色度について記載されているのみで湿潤状態で白色度が低下することについては、何等検討されていない。したがって、この湿潤状態で白色度が低下することに対する対策も従来確立されていない。
すなわち、前述の化粧料などに用いられる鱗片状または板状の雲母族鉱物粒子のごとく、湿潤状態における白色度が要望される分野において、従来の鱗片状または板状雲母族鉱物粒子は、その要望を満足させることが困難であるという問題を有している。
By the way, conventionally, when the powder is wetted with a liquid such as oil or water, it is known that the color changes as compared with the dry powder. For example, in a powder state, what has an excellent whiteness is wet, and in a wet state, the whiteness is lowered and a haze is generated. Therefore, even when the scaly or plate-like mica group mineral particles are used for cosmetics as described above, the whiteness of the mica group mineral particles may be reduced, resulting in a dullness. Regarding the decrease in whiteness in such a wet state, the suppression method has not been studied in the past, and in the above-mentioned Patent Document 1, the whiteness in the powder state is only described in the wet state. No consideration has been given to the decrease in whiteness. Therefore, a countermeasure against the decrease in whiteness in the wet state has not been established.
That is, in the field where whiteness in a wet state is desired, such as the scale-like or plate-like mica group mineral particles used in the above-described cosmetics, the conventional scale-like or plate-like mica group mineral particles are desired. It is difficult to satisfy the above.
本発明は、上記問題点を鑑み、湿潤状態における白色度の低下を抑制し得る鱗片状または板状の雲母族鉱物粒子の提供を課題としている。 In view of the above problems, an object of the present invention is to provide scale-like or plate-like mica group mineral particles that can suppress a decrease in whiteness in a wet state.
本発明者らは、鱗片状または板状雲母族鉱物粒子の湿潤状態における白色度の低下を抑制すべく鋭意検討を行った結果、鱗片状または板状雲母族鉱物粒子には、製造時に水洗工程を経ているものでも、その表面にチタン、鉄、マグネシウム、イオウ、ナトリウム、カルシウム、リン、ストロンチウム、ジルコニウム、マンガンなどの不純物成分が存在していることを見出し、このうち、表面被覆雲母族鉱物粒子に酸化チタンとして安定な状態で存在するチタンなどと異なり、水や酸などに可溶な不純物として鱗片状または板状雲母族鉱物粒子に存在するチタンが湿潤状態における白色度の低下に影響していること、ならびに、鱗片状または板状の雲母族鉱物粒子の表面をリン酸洗浄することで、他の酸で洗浄した場合に比べて不純物として存在するチタンをより多く除去でき、湿潤状態における白色度の低下も抑制されることを見出し、本発明の完成に到ったのである。
すなわち、本発明は、前記課題を解決すべく、鱗片状または板状の雲母族鉱物粒子の表面がリン酸洗浄されてなることを特徴とする鱗片状または板状のリン酸処理雲母粒子を提供する。
As a result of intensive studies to suppress the decrease in whiteness in the wet state of the scaly or plate-like mica group mineral particles, the scaly or plate-like mica group mineral particles are subjected to a water washing step during production. It has been found that impurity components such as titanium, iron, magnesium, sulfur, sodium, calcium, phosphorus, strontium, zirconium, and manganese are present on the surface, and among these, surface-coated mica mineral particles Unlike titanium, which exists in a stable state as titanium oxide, titanium present in scale-like or plate-like mica group mineral particles as a soluble impurity in water or acid affects the decrease in whiteness in a wet state. In addition, the surface of the scale-like or plate-like mica group mineral particles is washed with phosphoric acid, so that it exists as an impurity compared with the case of washing with other acids. Titanium can remove more of a decrease in whiteness in a wet state is also found to be suppressed, it was led to completion of the present invention.
That is, the present invention provides scale-like or plate-like phosphoric acid-treated mica particles, wherein the surface of scale-like or plate-like mica group mineral particles is washed with phosphoric acid in order to solve the above problems. To do.
本発明によれば、鱗片状または板状の雲母族鉱物粒子の表面がリン酸洗浄されていることから、その表面に不純物として付着しているチタンを他の酸で洗浄した場合に比べてより多く除去でき、洗浄後の粒子を湿潤状態における白色度の低下が抑制されたものとし得る。 According to the present invention, since the surface of the scale-like or plate-like mica group mineral particles is washed with phosphoric acid, it is more than when the titanium adhering to the surface as an impurity is washed with other acids. A large amount can be removed, and it can be assumed that the decrease in whiteness of the washed particles is suppressed in a wet state.
以下に、本発明の好ましい実施の形態について、化粧料などに用いられる鱗片状または板状のリン酸処理雲母粒子を例に説明する。
本実施形態の鱗片状または板状のリン酸処理雲母粒子は、鱗片状または板状の雲母族鉱物粒子の表面がリン酸洗浄されて製造される。
前記リン酸洗浄される鱗片状または板状の雲母族鉱物としては、天然産出あるいは、人工的に合成された雲母族鉱物の粒子（雲母族鉱物粒子）やこの雲母族鉱物の表面に有機物または無機物の表面被覆が施された表面被覆雲母族鉱物粒子を用いることができる。
Hereinafter, preferred embodiments of the present invention will be described by taking, as an example, scaly or plate-like phosphoric acid-treated mica particles used in cosmetics and the like.
The scale-like or plate-like phosphoric acid-treated mica particles of the present embodiment are produced by washing the surface of the scale-like or plate-like mica group mineral particles with phosphoric acid.
Examples of the scale-like or plate-like mica group mineral to be washed with phosphoric acid include naturally produced or artificially synthesized mica group mineral particles (mica group mineral particles) and organic or inorganic substances on the surface of the mica group mineral. Surface-coated mica group mineral particles having a surface coating of can be used.
前記雲母族鉱物粒子としては、例えば、セリサイト、マイカ（白雲母、金雲母、紅雲母、黒雲母、リチア雲母、合成雲母）などの鱗片状または板状粒子を用いることができる。
前記表面被覆雲母族鉱物粒子としては、酸化チタン被覆雲母（チタン雲母）、酸化チタン被覆セリサイト、酸化チタン被覆タルク、ベンガラ被覆雲母、ベンガラ被覆チタン雲母、黒酸化鉄被覆チタン雲母、カルミン被覆チタン雲母、コンジョウ被覆チタン雲母、カルミン・コンジョウ被覆チタン雲母、酸化クロム被覆チタン雲母、ベンガラ・黒酸化鉄被覆チタン雲母、黒酸化鉄カルミン被覆チタン雲母、黒酸化鉄コンジョウ被覆チタン雲母、チタン雲母＋黄色４号、チタン雲母＋赤色２０２号、チタン雲母＋青色１号、チタン雲母＋青色１号＋黄色４号などといったパール顔料などの各種の鱗片状または板状粒子があげられる。
As the mica group mineral particles, for example, scaly or plate-like particles such as sericite and mica (muscovite, phlogopite, saucite, biotite, lithia mica, synthetic mica) can be used.
Examples of the surface-coated mica group mineral particles include titanium oxide-coated mica (titanium mica), titanium oxide-coated sericite, titanium oxide-coated talc, Bengala-coated mica, Bengala-coated titanium mica, black iron oxide-coated titanium mica, and carmine-coated titanium mica. , Tungsten mica coated with conger, Titanium mica coated with carmine and conger, Titanium mica coated with chromium oxide, Titanium mica coated with black iron oxide, Titanium mica coated with black iron oxide Carmine coated titanium mica, Titanium mica coated with black iron oxide conger, Titanium mica + Yellow No. 4 And various kinds of scale-like or plate-like particles such as pearl pigments such as titanium mica + red No. 202, titanium mica + blue No. 1, titanium mica + blue No. 1 + yellow No. 4 and the like.
また、このような雲母族鉱物粒子、表面被覆雲母族鉱物粒子としては、例えば、平均粒径が１〜３００μｍの鱗片状または板状の鉱物粒子を用いることができる。なお、本明細書中における、前記平均粒径とは、レーザ回折法により求められる累積粒度分布を示す曲線の５０ｖｏｌ％の値を意味し、例えば、日本レーザー株式会社から「ロドス」の商品名にて市販のレーザ回折式粒度分布測定装置などにより測定することができる。 In addition, as such mica group mineral particles and surface-coated mica group mineral particles, for example, scale-like or plate-like mineral particles having an average particle diameter of 1 to 300 μm can be used. In addition, the said average particle diameter in this specification means the value of 50 vol% of the curve which shows the cumulative particle size distribution calculated | required by the laser diffraction method, for example, the brand name of "Rodos" from Japan Laser Corporation. It can be measured by a commercially available laser diffraction type particle size distribution measuring device.
また、このような雲母族鉱物粒子、表面被覆雲母族鉱物粒子は、化粧料に使用した際にキシミ感を生じさせることなくソフトな感触を持たせるためには、その平板平面における長径の平均値が１〜１０００μｍ程度、短径の平均値が上記長径の平均値の１／２倍以上で、かつ厚みが、上記長径の平均値の１／１０００倍以上、１／２倍未満程度であるのが好ましい。
なお長径の平均値は、上記の範囲内でもとくに３〜５００μｍ程度であるのが好ましい。また短径の比率の上限は、言うまでもなく長径の１倍である。さらに厚みは、上記の範囲内でもとくに、長径の平均値の１／１００〜１／５倍程度であるのが好ましい。平板平面における長径の平均値が上記の範囲未満では、全体としてのサイズが小さすぎて、たとえ全体形状として鱗片状、板状を維持していても化粧料に使用すると、肌に対するすべり感が不十分になるおそれがある。また逆にこの範囲を超えた場合には、大きくなりすぎた粒子が割れたり折れたりして却ってそのサイズが小さくなりやすく、しかも割れたり折れたりしたものは、長径に対する短径および厚みの比率が前記の範囲を外れて、もはや鱗片状、板状とは言いがたいものとなってしまうおそれを有するために、かかる粒子を使用して製造された化粧料に使用すると、やはり肌に対するすべり感が不十分になるおそれがある。
Moreover, in order to give such a mica group mineral particle and surface-coated mica group mineral particle a soft feel without causing a squeaky feeling when used in cosmetics, the average value of the major axis in the flat plate plane Is about 1 to 1000 μm, the average value of the minor axis is ½ times or more of the average value of the major axis, and the thickness is about 1/1000 times or more and less than ½ times the average value of the major axis. Is preferred.
In addition, it is preferable that the average value of a major axis is about 3-500 micrometers especially also in said range. Needless to say, the upper limit of the ratio of the minor axis is one time the major axis. Further, the thickness is preferably about 1/100 to 1/5 times the average value of the major axis, even in the above range. If the average value of the major axis on the flat plate surface is less than the above range, the overall size is too small, and even if the overall shape is maintained as a scale or plate, there is no slipperiness to the skin when used in cosmetics. May be sufficient. On the other hand, if this range is exceeded, particles that have become too large will break or break, and the size will tend to be small, and those that are cracked or broken will have a ratio of the short diameter and thickness to the long diameter. Since there is a possibility that it would be difficult to say scale-like or plate-like outside the above range, when used in a cosmetic produced using such particles, there is still a feeling of slipping on the skin. May be insufficient.
また、これら雲母族鉱物粒子、表面被覆雲母族鉱物粒子を洗浄するリン酸としては、一般に市販されている７５〜８９質量％の濃度のものを水などで適宜希釈したリン酸水溶液として用いることができる。 Moreover, as phosphoric acid for washing these mica group mineral particles and surface-coated mica group mineral particles, a commercially available phosphoric acid aqueous solution having a concentration of 75 to 89% by mass appropriately diluted with water or the like is used. it can.
前記雲母族鉱物粒子、表面被覆雲母族鉱物粒子をリン酸洗浄する方法としては、特に、限定されるものではなく、雲母族鉱物粒子、表面被覆雲母族鉱物粒子にリン酸水溶液をシャワーリングする方法や、漬け洗いする方法など、一般の粒状物の洗浄処理方法を採用することができるが、雲母族鉱物粒子、表面被覆雲母族鉱物粒子を全体的に均一かつ十分に洗浄処理し得る点から、漬け洗い方法を行うことが好ましい。 The method for washing the mica group mineral particles and surface-coated mica group mineral particles with phosphoric acid is not particularly limited, and the mica group mineral particles and the surface-coated mica group mineral particles are showered with a phosphoric acid aqueous solution. In addition, it is possible to employ a general granular cleaning method such as a pickling method, but from the point that the mica group mineral particles and the surface-coated mica group mineral particles can be uniformly and sufficiently cleaned as a whole, It is preferable to perform the pickling method.
前記漬け洗い方法としては、例えば、容器内で、雲母族鉱物粒子、表面被覆雲母族鉱物粒子とリン酸水溶液とを混合攪拌する方法を採用することができる。なお、このとき、リン酸水溶液に、雲母族鉱物粒子、表面被覆雲母族鉱物粒子を混合する方法や、水に一旦雲母族鉱物粒子、表面被覆雲母族鉱物粒子を分散させた後にリン酸を添加する方法などを採用することができる。
この漬け洗い方法における、リン酸水溶液の濃度としては、例えば、３〜５０質量％のものを用いることができる。また、漬け洗い方法における、雲母族鉱物粒子や表面被覆雲母族鉱物粒子とリン酸水溶液との比率は、良好なる分散性を得られる点において重量で、１：１〜１：１０（鉱物粒子：リン酸水溶液）程度とされることが好ましく、１：１〜１：５（鉱物粒子：リン酸水溶液）の比率とされることがより好ましい。また、この漬け洗い時には、雲母族鉱物粒子、表面被覆雲母族鉱物粒子を全体的に均一かつ十分に洗浄処理し得る点から、攪拌が実施されることが好ましく、この攪拌としては、一般的に用いられる攪拌翼を用いて例えば０．５〜５時間の攪拌を行えばよい。また、この攪拌後の雲母族鉱物粒子、表面被覆雲母族鉱物粒子は、そのままリン酸水溶液中にて０．１〜４８時間程度静置されることが好ましい。なお、要すれば、静置時間を４８時間以上とすることも可能である。
As the pickling method, for example, a method of mixing and stirring the mica group mineral particles, the surface-coated mica group mineral particles, and the phosphoric acid aqueous solution in a container can be employed. At this time, a method of mixing mica group mineral particles and surface-coated mica group mineral particles with phosphoric acid aqueous solution, or adding phosphoric acid after dispersing mica group mineral particles and surface-coated mica group mineral particles in water once The method to do can be adopted.
The concentration of the phosphoric acid aqueous solution in this pickling method can be, for example, 3 to 50% by mass. In the pickling method, the ratio of the mica group mineral particles or surface-coated mica group mineral particles to the phosphoric acid aqueous solution is 1: 1 to 1:10 by weight in terms of obtaining good dispersibility (mineral particles: Phosphoric acid aqueous solution) is preferable, and a ratio of 1: 1 to 1: 5 (mineral particles: phosphoric acid aqueous solution) is more preferable. Further, at the time of this pickling, stirring is preferably carried out from the point that the mica group mineral particles and the surface-coated mica group mineral particles can be uniformly and sufficiently cleaned as a whole. What is necessary is just to perform stirring for 0.5 to 5 hours, for example using the stirring blade used. Further, it is preferable that the agitated mica group mineral particles and the surface-coated mica group mineral particles are allowed to stand in the phosphoric acid aqueous solution for about 0.1 to 48 hours. If necessary, the standing time can be 48 hours or longer.
この雲母族鉱物粒子、表面被覆雲母族鉱物粒子を漬け洗いして得られたリン酸処理雲母粒子は、遠心脱水などの一般的な脱水手段により、リン酸水溶液を除去し、更に水洗、脱水が実施され、最終的に、２ｇのリン酸処理雲母粒子を５０ｍＬの蒸留水に分散させ、１０分間攪拌の後１０分間静置したものをろ過したろ液のｐＨが４．５〜９．０となるよう水洗されることが好ましい。 The phosphoric acid-treated mica particles obtained by dipping and washing the mica group mineral particles and the surface-coated mica group mineral particles are removed by removing the phosphoric acid aqueous solution by a general dehydration means such as centrifugal dehydration, and further washed with water and dehydrated. Finally, 2 g of phosphoric acid-treated mica particles are dispersed in 50 mL of distilled water, and after stirring for 10 minutes and standing for 10 minutes, the filtrate has a pH of 4.5 to 9.0. It is preferable to wash with water.
次いで、このように雲母族鉱物粒子、表面被覆雲母族鉱物粒子をリン酸水溶液で漬け洗い、水洗、乾燥され製造された鱗片状または板状のリン酸処理雲母粒子が配合された化粧料について説明する。
前述のごとく鱗片状または板状の雲母族鉱物粒子の表面がリン酸洗浄されて製造された鱗片状または板状のリン酸処理雲母粒子は、湿潤時の白色度低下を抑制できるとともに、他の酸で洗浄された鱗片状または板状雲母族鉱物粒子に比べて、肌触りがソフトで、また、雲母族鉱物の臭いも他の酸で洗浄された場合よりも低減することができることから化粧料に好適なものとなる。
この化粧料としては、たとえば粉白粉、固形白粉、ファンデーション、口紅、アイシャドーなどの他、チーク、ネイルカラーなどのメイクアップ化粧料、シャンプー、リンス、コンディショナー、ヘアートリートメントなどの頭髪化粧料、ボディパウダーなどのデオドラント化粧料、乳液、ローション、クリーム、クレンジング、パック、サンスクリーン剤、化粧下地料などの基礎化粧料があげられる。
また、これらの化粧料には、前記鱗片状または板状のリン酸処理雲母粒子が、例えば、０．１〜１００質量％配合される。
Next, description will be made on cosmetics containing scale-like or plate-like phosphoric acid-treated mica particles produced by immersing mica group mineral particles and surface-coated mica group mineral particles with a phosphoric acid aqueous solution, washing with water and drying. To do.
As described above, the scale-like or plate-like phosphoric acid-treated mica particles produced by washing the surface of the scale-like or plate-like mica group mineral particles with phosphoric acid can suppress a decrease in whiteness when wet. Compared to scaly or plate-like mica group mineral particles washed with acid, the skin feels softer, and the odor of mica group mineral can be reduced than when washed with other acids. This is preferable.
Examples of the cosmetics include powdered white powder, solid white powder, foundation, lipstick, and eye shadow, makeup cosmetics such as teak and nail color, hair cosmetics such as shampoo, rinse, conditioner, and hair treatment, and body powder. Basic cosmetics such as deodorant cosmetics such as, emulsions, lotions, creams, cleansings, packs, sunscreens, and makeup bases.
Moreover, 0.1-100 mass% of the scale-like or plate-like phosphoric acid-treated mica particles are blended in these cosmetics, for example.
上記化粧料に配合する鱗片状または板状のリン酸処理雲母粒子は、事前に表面処理されていてもよい。表面処理の例としては、たとえばフッ素化合物処理、シリコーン処理、金属石鹸処理、アシル化リジン処理、油剤処理、シラン処理、アミノ酸処理、ワックス処理、金属酸化物処理などがあげられるが、化粧料で従来用いられている処理であればいずれも採用できる。もちろん、鱗片状または板状のリン酸処理雲母粒子は、表面処理せずに化粧料に使用してもよい。 The scale-like or plate-like phosphoric acid-treated mica particles to be blended in the cosmetic material may be surface-treated in advance. Examples of surface treatments include, for example, fluorine compound treatment, silicone treatment, metal soap treatment, acylated lysine treatment, oil agent treatment, silane treatment, amino acid treatment, wax treatment, and metal oxide treatment. Any processing that is used can be adopted. Of course, the scale-like or plate-like phosphoric acid-treated mica particles may be used in cosmetics without being surface-treated.
前記化粧料には、鱗片状または板状のリン酸処理雲母粒子以外に、化粧料に通常に使用される油剤、粉体（顔料、色素）、樹脂、界面活性剤、粘剤、防腐剤、香料、紫外線吸収剤（有機系、無機系を含む）、保湿剤、生理活性成分、塩類、溶媒、酸化防止剤、キレート剤、中和剤、ｐＨ調整剤などの種々の成分を配合することができる。油剤の例としては、たとえばセチルアルコール、イソステアリルアルコール、ラウリルアルコール、ヘキサデシルアルコール、オクチルドデカノールなどの高級アルコール類、イソステアリン酸、ウンデシレン酸、オレイン酸などの脂肪酸類、グリセリン、ソルビトール、エチレングリコール、プロピレングリコール、ポリエチレングリコールなどの多価アルコール類、ミリスチン酸ミリスチル、ラウリン酸ヘキシル、オレイン酸デシル、ミリスチン酸イソプロピル、ジメチルオクタン酸ヘキシルデシル、モノステアリン酸グリセリン、フタル酸ジエチル、モノステアリン酸エチレングリコール、オキシステアリン酸オクチルなどのエステル類、流動パラフィン、イソパラフィン、ワセリン、スクワランなどの炭化水素類、ラノリン、還元ラノリン、カルナバロウなどのロウ、ミンク油、カカオ脂、ヤシ油、パーム核油、ツバキ油、ゴマ油、ヒマシ油、オリーブ油などの油脂類があげられる。 In addition to the scale-like or plate-like phosphoric acid-treated mica particles, the cosmetics include oils, powders (pigments, pigments), resins, surfactants, stickers, preservatives that are commonly used in cosmetics, Various ingredients such as fragrances, ultraviolet absorbers (including organic and inorganic), humectants, physiologically active ingredients, salts, solvents, antioxidants, chelating agents, neutralizing agents, pH adjusting agents, etc. it can. Examples of oils include higher alcohols such as cetyl alcohol, isostearyl alcohol, lauryl alcohol, hexadecyl alcohol, octyldodecanol, fatty acids such as isostearic acid, undecylenic acid, oleic acid, glycerin, sorbitol, ethylene glycol, Polyhydric alcohols such as propylene glycol and polyethylene glycol, myristyl myristate, hexyl laurate, decyl oleate, isopropyl myristate, hexyl decyl dimethyloctanoate, glyceryl monostearate, diethyl phthalate, ethylene glycol monostearate, oxy Esters such as octyl stearate, hydrocarbons such as liquid paraffin, isoparaffin, petrolatum, squalane, lanolin, reduced Phosphorus, waxes such as carnauba wax, mink oil, cacao butter, coconut oil, palm kernel oil, camellia oil, sesame oil, castor oil, oils and fats such as olive oil and the like.
また、別の形態の油剤の例としては、例えばジメチルポリシロキサン、メチルハイドロジェンポリシロキサン、メチルフェニルポリシロキサン、ポリエーテル変性オルガノポリシロキサン、アルキル変性オルガノポリシロキサン、糖変性シリコーン、グリセリル変性シリコーン、アモジメチコーン、アミノ変性オルガノポリシロキサン、シリコーンゲル、アクリルシリコーン、トリメチルシロキシケイ酸、シリコーンＲＴＶゴムなどのシリコーン化合物があげられる。 Examples of other forms of oil include dimethylpolysiloxane, methylhydrogenpolysiloxane, methylphenylpolysiloxane, polyether-modified organopolysiloxane, alkyl-modified organopolysiloxane, sugar-modified silicone, glyceryl-modified silicone, and amodimethicone. And silicone compounds such as amino-modified organopolysiloxane, silicone gel, acrylic silicone, trimethylsiloxysilicic acid, and silicone RTV rubber.
さらにフッ素系油剤の例としては、たとえばパーフルオロデカリンなどのフルオロカーボン類、パーフルオロポリエーテル、フッ化ピッチ、パーフルオロアルキル鎖を有するフルオロアルコールなどのアルコール類、パーフルオロアルキルリン酸エステルトリエタノールアミン塩などのリン酸エステル類、フルオロアルキル鎖を有するカルボン酸類、フルオロアルキル変性シリコーン、フッ素・ポリエーテル共変性シリコーン、フッ素化シリコーン樹脂などがあげられる。 Furthermore, examples of fluorine-based oils include, for example, fluorocarbons such as perfluorodecalin, alcohols such as perfluoropolyether, fluorinated pitch and fluoroalcohol having a perfluoroalkyl chain, and perfluoroalkyl phosphate triethanolamine salts. And phosphoric acid esters such as carboxylic acids having a fluoroalkyl chain, fluoroalkyl-modified silicones, fluorine / polyether co-modified silicones, and fluorinated silicone resins.
粉体類の例としては、セリサイト（無処理のもの）、マイカ（白雲母、金雲母、紅雲母、黒雲母、リチア雲母、合成雲母）、タルク、カオリン、バーミキュライト、スメクタイト、酸化チタン被覆雲母（チタン雲母）、酸化チタン被覆セリサイト、酸化チタン被覆タルクなどのパール顔料や、あるいは魚鱗箔、窒化ホウ素などの他、ナイロンビーズ、シリコーンビーズ、ＰＴＦＥパウダー、シリコーンエラストマーなどの樹脂粉体や、黄酸化鉄、赤色酸化鉄、黒酸化鉄、酸化クロム、酸化コバルト、カーボンブラツク、群青、紺青、酸化亜鉛、酸化チタン、酸化ジルコニウム、酸化珪素、酸化アルミニウム、酸化セリウム、硫酸バリウム、炭酸カルシウム、炭酸マグネシウム、珪酸アルミニウム、珪酸マグネシウム、炭化珪素、有機色素、レーキ、微粒子酸化チタン、微粒子酸化亜鉛、微粒子酸化鉄、板状硫酸バリウムなどがあげられる。 Examples of powders include sericite (unprocessed), mica (muscovite, phlogopite, saucite, biotite, lithia mica, synthetic mica), talc, kaolin, vermiculite, smectite, titanium oxide-coated mica. (Titanium mica), pearl pigments such as titanium oxide-coated sericite, titanium oxide-coated talc, fish scale foil, boron nitride, and other resin powders such as nylon beads, silicone beads, PTFE powder, silicone elastomer, and yellow Iron oxide, red iron oxide, black iron oxide, chromium oxide, cobalt oxide, carbon black, ultramarine, bitumen, zinc oxide, titanium oxide, zirconium oxide, silicon oxide, aluminum oxide, cerium oxide, barium sulfate, calcium carbonate, magnesium carbonate , Aluminum silicate, magnesium silicate, silicon carbide, organic dye, Yellow, particulate titanium oxide, particulate zinc oxide, particulate iron oxide, etc. plate-like barium sulfate.
これらの粉体類は、フッ素化合物処理、シリコーン処理、金属石鹸処理、アシル化リジン処理、油剤処理、シラン処理、アミノ酸処理、ワックス処理、金属酸化物処理、シランカップリング剤処理、有機チタネート処理、脂肪酸処理などの表面処理を施した状態で使用してもよい。界面活性剤としては、アニオン型界面活性剤、カチオン型界面活性剤、ノニオン型界面活性剤、ベタイン型界面活性剤のいずれを用いることもできる。 These powders are fluorine compound treatment, silicone treatment, metal soap treatment, acylated lysine treatment, oil agent treatment, silane treatment, amino acid treatment, wax treatment, metal oxide treatment, silane coupling agent treatment, organic titanate treatment, You may use it in the state which gave surface treatments, such as a fatty-acid treatment. As the surfactant, any of an anionic surfactant, a cationic surfactant, a nonionic surfactant, and a betaine surfactant can be used.
生理活性成分の例としては、たとえば抗炎症剤、血行促進剤、ビタミン類、チロシナーゼ活性阻害剤、尿素などがあげられる。溶媒の例としては、たとえば精製水、メタノール、エタノール、イソプロピルアルコール、エーテル、ＬＰＧ、揮発性シリコーン、軽質流動イソパラフィン、代替フロンなどがあげられる。なお精製水の代わりにミネラルウォーターを使用することもできる。 Examples of the physiologically active component include anti-inflammatory agents, blood circulation promoters, vitamins, tyrosinase activity inhibitors, urea and the like. Examples of the solvent include purified water, methanol, ethanol, isopropyl alcohol, ether, LPG, volatile silicone, light liquid isoparaffin, and alternative chlorofluorocarbon. Mineral water can also be used instead of purified water.
なお、このような化粧料として、粉白粉、固形白粉、ファンデーションにおいては、配合される前記鱗片状または板状のリン酸処理雲母粒子の平均粒径は、１〜５０μｍであることが、感触面において好ましく、アイシャドー、チーク、口紅、ネイルカラーにおいては、それらの化粧が施された部位にきらめきを与え美観を向上させ得る点において、配合される鱗片状または板状のリン酸処理雲母粒子の平均粒径は、５０〜１００μｍであることが好ましい。
なお、本実施形態においては、鱗片状または板状のリン酸処理雲母粒子を化粧料に用いる場合を例に説明したが、本発明においては、鱗片状または板状のリン酸処理雲母粒子の用途を化粧料に限定するものではない。
また、本実施形態においては、鱗片状または板状の粒子状態の雲母鉱物粒子とリン酸水溶液とを混合する場合を例に、鱗片状または板状のリン酸処理雲母粒子の製造方法を説明したが、例えば、数ｍｍ〜数十ｃｍの大きさの、雲母族鉱物の粗大塊（粗大片）をリン酸水溶液中にて細かく砕いて鱗片状または板状のリン酸処理雲母粒子を製造する場合も本発明の意図する範囲である。
As such cosmetics, in powdered white powder, solid white powder, and foundation, the average particle diameter of the scale-like or plate-like phosphoric acid-treated mica particles to be blended is 1 to 50 μm. In the eye shadow, teak, lipstick, and nail color, the scale-like or plate-like phosphate-treated mica particles to be blended are used in that they can give a glittering site and improve the aesthetic appearance. The average particle size is preferably 50 to 100 μm.
In the present embodiment, the case where the scaly or plate-like phosphoric acid-treated mica particles are used in the cosmetic has been described as an example. However, in the present invention, the application of the scaly or plate-like phosphoric acid-treated mica particles is used. Is not limited to cosmetics.
Further, in the present embodiment, the method for producing scale-like or plate-like phosphoric acid-treated mica particles has been described by taking as an example the case of mixing scale-like or plate-like mica mineral particles and phosphoric acid aqueous solution. However, for example, when scaly or plate-like phosphoric acid-treated mica particles are produced by finely crushing a coarse mass (coarse piece) of a mica group mineral having a size of several mm to several tens of cm in a phosphoric acid aqueous solution Is also within the intended scope of the present invention.
次に実施例を挙げて本発明をさらに詳しく説明するが、本発明はこれらに限定されるものではない。
（実施例１）
イオン交換水１５リットルに、三信鉱工株式会社製セリサイト（商品名「ＦＳＥ」：平均粒径約８μｍ、平板平面の長径の平均値約８μｍ、短径の平均値約５μｍ、厚さ平均値約０．１μｍ）５ｋｇを添加して１０分間攪拌した後、食物添加用７５質量％リン酸１．５ｋｇを添加し、さらに１０分間攪拌し、２４時間の静置し、漬け洗いを実施した。
ついで、この漬け洗いされたセリサイトを吸引ろ過してリン酸水溶液を除去し、引き続きろ別されたセリサイトの上から水を供給しつつ吸引ろ過を継続させ、ろ過された洗浄水のｐＨが５．０になるまで実施した。
このように水洗されたセリサイトは、１２０℃×１２時間の乾燥を実施した後に、ピンミルにて凝集塊をほぐし、２００メッシュで篩い分けし篩い残分を除去し鱗片状または板状のリン酸処理雲母粒子を製造した。なお、このときの得られた鱗片状または板状のリン酸処理雲母粒子の平均粒径は、約９．４μｍと初期よりも増大していたが、これは、平均粒径よりも小さな微粒子分が洗浄時に流失してしまったためであると見られる。
EXAMPLES Next, although an Example is given and this invention is demonstrated in more detail, this invention is not limited to these.
Example 1
In 15 liters of ion-exchanged water, sericite manufactured by Sanshin Mining Co., Ltd. After adding 5 kg (about 0.1 μm) and stirring for 10 minutes, 1.5 kg of 75% by mass phosphoric acid for food addition was added, and further stirred for 10 minutes, allowed to stand for 24 hours, and pickled.
Subsequently, the soaked sericite is filtered by suction to remove the phosphoric acid aqueous solution. Subsequently, the suction filtration is continued while supplying water from above the filtered sericite. It was carried out until it reached 5.0.
After the sericite washed with water is dried at 120 ° C. for 12 hours, the aggregate is loosened with a pin mill, sieved with 200 mesh to remove the sieve residue, and scaly or plate-like phosphate Treated mica particles were produced. The average particle size of the scaly or plate-like phosphoric acid-treated mica particles obtained at this time was about 9.4 μm, which was larger than the initial particle size. Seems to have been washed away during washing.
（実施例２）
実施例１のセリサイトに代えてマイカ（株式会社山口雲母工業所製「Ｙ−２４００」：平均粒径約１８μｍ）を用いたこと以外は、実施例１と同様に鱗片状または板状のリン酸処理雲母粒子を製造した。なお、このときの得られた鱗片状または板状のリン酸処理雲母粒子の平均粒径は、約１８μｍで実施例１の場合と異なり初期の平均粒子径を維持している。これは、このマイカ「Ｙ−２４００」が、元々微粒子分がカットされ製造されたものであることに起因していると見られる。
(Example 2)
Except for using mica (“Y-2400” manufactured by Yamaguchi Mica Industry Co., Ltd .: average particle size of about 18 μm) instead of the sericite of Example 1, scaly or plate-like phosphorus Acid-treated mica particles were produced. In addition, unlike the case of Example 1, the average particle diameter of the scaly or plate-like phosphoric acid-treated mica particles obtained at this time is about 18 μm, and the initial average particle diameter is maintained. This seems to be due to the fact that this mica “Y-2400” was originally produced by cutting the fine particles.
（実施例３）
実施例１のセリサイトに代えてパールマイカ（日本光研工業株式会社製「ＰＥＡＲＬ−ＧＬＡＺＥ ＭＶ−１００Ｒ」：平均粒径約１７μｍ）を用いたこと以外は、実施例１と同様に鱗片状または板状のリン酸処理雲母粒子を製造した。なお、このときの得られた鱗片状または板状のリン酸処理雲母粒子の平均粒径は、約１８μｍであった。
(Example 3)
Instead of the sericite of Example 1, pearl mica (“PEARL-GLIZE MV-100R” manufactured by Nippon Koken Kogyo Co., Ltd .: average particle size of about 17 μm) was used in the same manner as in Example 1 except that it was scaly or Plate-like phosphoric acid-treated mica particles were produced. The average particle size of the scaly or plate-like phosphoric acid-treated mica particles obtained at this time was about 18 μm.
（比較例１）
実施例１のリン酸水溶液（イオン交換水１５リットル＋７５質量％リン酸１．５ｋｇ）に代えて２Ｎ塩酸を用いたこと以外は、実施例１と同様に鱗片状または板状の雲母族鉱物粒子を製造した。なお、このときの得られた鱗片状または板状の雲母族鉱物粒子の平均粒径は、約９．４μｍであった。
(Comparative Example 1)
Scale-like or plate-like mica group mineral particles as in Example 1 except that 2N hydrochloric acid was used in place of the phosphoric acid aqueous solution of Example 1 (15 liters of ion-exchanged water +75 kg of 75% by mass phosphoric acid). Manufactured. The average particle size of the scaly or plate-like mica group mineral particles obtained at this time was about 9.4 μm.
（比較例２）
実施例１のリン酸水溶液に代えて１Ｎ硝酸を用いたこと以外は、実施例１と同様に鱗片状または板状の雲母族鉱物粒子を製造した。
(Comparative Example 2)
Scale-like or plate-like mica group mineral particles were produced in the same manner as in Example 1 except that 1N nitric acid was used instead of the phosphoric acid aqueous solution of Example 1.
（比較例３）
実施例１のリン酸水溶液に代えて２Ｎ硫酸を用いたこと以外は、実施例１と同様に鱗片状または板状の雲母族鉱物粒子を製造した。
(Comparative Example 3)
Scale-like or plate-like mica group mineral particles were produced in the same manner as in Example 1 except that 2N sulfuric acid was used instead of the phosphoric acid aqueous solution of Example 1.
（評価）
（不純物除去効果）
実施例１で漬け洗いに用いたリン酸水溶液と略同等の濃度である７．５質量％の溶液、２Ｎ塩酸水溶液、１Ｎ硝酸水溶液、２Ｎ硫酸水溶液ならびにイオン交換水、それぞれ３０ｍｌを用いて、実施例１、２に用いたセリサイト、マイカ５．０ｇとを三角フラスコ内にて混合し、スターラーを用いて６０分間攪拌を行った。攪拌後、Ｎｏ．１ろ紙を用いてろ別し、ろ過されたろ液を５倍希釈し、下記ＩＣＰにて元素分析を行った。結果を表１、表２に示す。また、実施例３に用いたパールマイカと、７．５質量％のリン酸水溶液、イオン交換水とにより上記と同様にろ液のＩＣＰ元素分析を行った。結果を表３に示す。
（ＩＣＰ測定条件）
使用機器：エスアイアイ・ナノテクノロジー株式会社製「ＳＰＳ−４０００」
測光高さ：１０．０ｍｍ〜Ｎａ，Ｋ５．０ｍｍ
積分条件：３回−１秒（積算１回）
プラズマ流量（１６．０Ｌ／ｍｉｎ）、キャリア流量（１．０Ｌ／ｍｉｎ）、補助流量（０．５Ｌ／ｍｉｎ）
(Evaluation)
(Impurity removal effect)
Using 7.5 ml of a 2% hydrochloric acid aqueous solution, a 1N nitric acid aqueous solution, a 2N sulfuric acid aqueous solution, and ion-exchanged water, each having a concentration substantially equal to that of the phosphoric acid aqueous solution used for the pickling in Example 1, was carried out. The sericite and mica 5.0g used in Examples 1 and 2 were mixed in an Erlenmeyer flask and stirred for 60 minutes using a stirrer. After stirring, no. The filtrate was filtered using 1 filter paper, the filtrate filtered was diluted 5-fold, and elemental analysis was performed by the following ICP. The results are shown in Tables 1 and 2. The filtrate was subjected to ICP elemental analysis in the same manner as described above using pearl mica used in Example 3, 7.5% by mass phosphoric acid aqueous solution, and ion-exchanged water. The results are shown in Table 3.
(ICP measurement conditions)
Equipment used: “SPS-4000” manufactured by SII Nano Technology Co., Ltd.
Photometric height: 10.0 mm to Na, K 5.0 mm
Integration condition: 3 times-1 second (1 time of integration)
Plasma flow rate (16.0 L / min), carrier flow rate (1.0 L / min), auxiliary flow rate (0.5 L / min)
この、表１乃至３からもわかるように、鱗片状または板状の雲母族鉱物粒子の表面がリン酸洗浄されることにより、他の酸で洗浄した場合に比べてチタンをより多く除去できることがわかる。
As can be seen from Tables 1 to 3, the surface of the scaly or plate-like mica group mineral particles is washed with phosphoric acid, so that more titanium can be removed than when washed with other acids. Recognize.
（湿潤時白色度）
実施例１、２、比較例１乃至３について、１２０℃で約２時間乾燥された粉末状態での白色度と、鱗片状または板状の雲母族鉱物粒子を約２倍の重量の水中に入れて攪拌した後、沈殿させた状態（湿潤状態）とで、白色度をＪＩＳ Ｋ ７１０５の規定に準拠し、色差計（日本電色工業社製、「ＮＤ−１００１ＤＰ」）にて、試料面積３０ｍｍφ、試料容器３０ｍｍφ×１３ｍｍ、標準版の三刺激値（Ｘ＝８１．２、Ｙ＝８２．６、Ｚ＝９２．５）の条件下にて測定した。評価結果を、表４に示す。
(Whiteness when wet)
For Examples 1 and 2 and Comparative Examples 1 to 3, whiteness in a powder state dried at 120 ° C. for about 2 hours and scale-like or plate-like mica group mineral particles were put in water about twice as heavy as water. After stirring, the whiteness of the precipitated state (wet state) conforms to the provisions of JIS K 7105, and the sample area is 30 mmφ with a color difference meter (“ND-1001DP” manufactured by Nippon Denshoku Industries Co., Ltd.). The sample container was measured under the conditions of 30 mmφ × 13 mm and the standard version of tristimulus values (X = 81.2, Y = 82.6, Z = 92.5). The evaluation results are shown in Table 4.
（触感試験）
実施例１乃至３、比較例１乃至３で得られた粒子を、顔に塗り伸ばした際の感触を、被験者１０人に下記の３段階で評価してもらった。結果を表５に示す。
良好：ソフト感があり、感触が良い
不良：ソフト感がなく、感触が悪い
普通：良好、不良のどちらでもなく中間
なお、比較例１乃至３の鱗片状または板状の雲母族鉱物粒子においては、わずかにイオウ臭が感じられたが実施例１の鱗片状または板状のリン酸処理雲母粒子は、無臭であった。このことから、リン酸洗浄されることで、他の酸で洗浄される場合に比べてセリサイトのイオウ臭が低減できていることも確認できた。
(Tactile test)
The feeling when the particles obtained in Examples 1 to 3 and Comparative Examples 1 to 3 were spread on the face was evaluated by the 10 subjects in the following three stages. The results are shown in Table 5.
Good: soft feeling, good feel Bad: no soft feeling, bad feel Normal: neither good nor bad
In the scale-like or plate-like mica group mineral particles of Comparative Examples 1 to 3, a slight sulfur odor was felt, but the scale-like or plate-like phosphoric acid-treated mica particles of Example 1 were odorless. It was. From this, it was confirmed that the sulfur odor of sericite could be reduced by washing with phosphoric acid as compared with the case of washing with other acids.
（化粧料製造例）
（化粧料１）
実施例１の鱗片状または板状のリン酸処理雲母粒子を用いて以下の配合１によりファンデーションを製造した。
（配合１）
成分 質量％
酸化鉄 ４．５
鱗片状または板状のリン酸処理雲母粒子 ３３
板状硫酸バリウム ３４
酸化チタン ８
タルク １０
パーフルオロポリエーテル ７
フッ素変成シリコーン ３
防腐剤および香料 ０．５
上記ファンデーションは、感触に優れており、肌に塗り伸ばす際にソフト感が得られた。
(Example of cosmetic production)
(Cosmetics 1)
Using the scale-like or plate-like phosphoric acid-treated mica particles of Example 1, a foundation was produced by the following formulation 1.
(Formulation 1)
Ingredient Mass%
Iron oxide 4.5
Scale-like or plate-like phosphoric acid-treated mica particles 33
Plate-like barium sulfate 34
Titanium oxide 8
Talc 10
Perfluoropolyether 7
Fluorine-modified silicone 3
Preservatives and fragrances 0.5
The foundation was excellent in touch, and a soft feeling was obtained when applied to the skin.
（化粧料２）
前記化粧料１の実施例１（鱗片状または板状のリン酸処理雲母粒子）に代えて比較例１の鱗片状または板状の雲母族鉱物粒子ものを用いたこと以外は、化粧料１と同様にファンデーションを製造した。このファンデーションは、肌に塗り伸ばす際に化粧料１のファンデーションに比べソフト感が得られなかった。
(Cosmetics 2)
Cosmetic 1 except that Example 1 (scale-like or plate-like phosphoric acid-treated mica particles) of the cosmetic 1 was used instead of the scale-like or plate-like mica group mineral particles of Comparative Example 1. Similarly, a foundation was produced. When this foundation was applied to the skin, a soft feeling was not obtained as compared with the foundation of Cosmetic 1.
（化粧料３）実施例１の鱗片状または板状のリン酸処理雲母粒子（下記配合２中「鱗片状または板状のリン酸処理雲母粒子１」）と実施例２の鱗片状または板状のリン酸処理雲母粒子（下記配合２中「鱗片状または板状のリン酸処理雲母粒子２」）とを用いて以下の配合２によりファンデーションを製造した。なお、鱗片状または板状のリン酸処理雲母粒子を含めて全ての無機粉体は、該無機粉体１００重量部に対して、パーフルオロアルキルリン酸エステル塩３重量部を用いて処理したものである。
（配合２）
成分 質量％
酸化鉄 ４．５
鱗片状または板状のリン酸処理雲母粒子１ ２０
鱗片状または板状のリン酸処理雲母粒子２ １０
板状硫酸バリウム ３２
酸化チタン ８
微粒子酸化チタン ２
タルク １０
シリコーンエラストマー ３
有機系紫外線吸収剤 ３
パーフルオロポリエーテル ５．５
グリセリン ０．５
白色ワセリン １
防腐剤および香料 ０．５
上記ファンデーションは、紫外線防止効果に優れるとともに、感触に優れており、肌に塗り伸ばす際にソフト感が得られた。
(Cosmetics 3) Scale-like or plate-like phosphoric acid-treated mica particles of Example 1 (“Scalate-like or plate-like phosphoric acid-treated mica particles 1” in Formula 2 below) and Scale-like or plate-like of Example 2 The following foundation 2 was used to prepare a foundation using the above-mentioned phosphoric acid-treated mica particles (“scale-like or plate-like phosphoric acid-treated mica particles 2” in the following composition 2). All inorganic powders including scale-like or plate-like phosphoric acid-treated mica particles were treated with 3 parts by weight of perfluoroalkyl phosphate ester salt with respect to 100 parts by weight of the inorganic powder. It is.
(Formulation 2)
Ingredient Mass%
Iron oxide 4.5
Scale-like or plate-like phosphoric acid-treated mica particles 120
Scale-like or plate-like phosphoric acid-treated mica particles 2 10
Plate-like barium sulfate 32
Titanium oxide 8
Fine particle titanium oxide 2
Talc 10
Silicone elastomer 3
Organic UV absorber 3
Perfluoropolyether 5.5
Glycerin 0.5
White petrolatum 1
Preservatives and fragrances 0.5
The above foundation was excellent in the effect of preventing ultraviolet rays and excellent in touch, and a soft feeling was obtained when applied to the skin.
（化粧料４）
実施例１の鱗片状または板状のリン酸処理雲母粒子を用いて以下の配合３によりファンデーションを製造した。なお、はじめに成分Ａと成分Ｂとを混合し、次いで成分Ｃを加えてさらに混合し、混合物を粉砕して金型を用いて金皿に打型して製品とした。
また、成分Ａは、各々１００重量部に対して、パーフルオロアルキルリン酸エステル塩３重量部を用いて処理したものである。
（配合３）
成分Ａ 質量％
酸化鉄 ４．５
鱗片状または板状のリン酸処理雲母粒子 １０
板状硫酸バリウム ３４
酸化チタン ８
タルク １０
成分Ｂ 質量％
シリコーンエラストマー ３
成分Ｃ 質量％
パーフルオロポリエーテル ７
フッ素変成シリコーン ３
防腐剤および香料 ０．５
上記ファンデーションは、紫外線防止効果、耐皮脂性（化粧持続性）に優れるとともに、感触に優れており、肌に塗り伸ばす際にソフト感が得られた。
(Cosmetics 4)
Using the scale-like or plate-like phosphoric acid-treated mica particles of Example 1, a foundation was produced by the following formulation 3. First, component A and component B were mixed, then component C was added and further mixed, the mixture was pulverized and cast into a metal dish using a mold to obtain a product.
In addition, Component A is processed using 3 parts by weight of a perfluoroalkyl phosphate ester salt with respect to 100 parts by weight of each.
(Formulation 3)
Component A mass%
Iron oxide 4.5
Scale-like or plate-like phosphoric acid-treated mica particles 10
Plate-like barium sulfate 34
Titanium oxide 8
Talc 10
Component B Mass%
Silicone elastomer 3
Ingredient C
Perfluoropolyether 7
Fluorine-modified silicone 3
Preservatives and fragrances 0.5
The above foundation was excellent in UV prevention effect, sebum resistance (makeup persistence) and excellent in touch, and a soft feeling was obtained when applied to the skin.
（化粧料５）
実施例３の鱗片状または板状のリン酸処理雲母粒子を用いて以下の配合４によりアイシャドーを製造した。なお、はじめに成分Ａを混合し、次いで成分Ｂを加えてさらに混合し中皿に充填しアイシャドーを作成した。
（配合４）
成分Ａ 質量％
タルク 残余
セリサイト ６
合成マイカ １２
球状ＰＭＭＡ粉末 ３
板状硫酸バリウム ８
鱗片状または板状のリン酸処理雲母粒子 ８
酸化鉄 ２
窒化ホウ素 ３
成分Ｂ 質量％
スクワラン １
ジメチルポリシロキサン ２
モノオレイン酸ソルビタン １
防腐剤および香料 ０．５
上記アイシャドーは、感触に優れており、肌に塗り伸ばす際にソフト感が得られた。
(Cosmetics 5)
An eye shadow was produced by the following formulation 4 using the scale-like or plate-like phosphoric acid-treated mica particles of Example 3. Ingredient A was first mixed, then Component B was added and further mixed and filled in an intermediate dish to prepare an eye shadow.
(Formulation 4)
Component A mass%
Talc Residue Sericite 6
Synthetic mica 12
Spherical PMMA powder 3
Plate-like barium sulfate 8
Scale-like or plate-like phosphoric acid-treated mica particles 8
Iron oxide 2
Boron nitride 3
Component B Mass%
Squalane 1
Dimethylpolysiloxane 2
Sorbitan monooleate 1
Preservatives and fragrances 0.5
The eye shadow was excellent in touch, and a soft feeling was obtained when applied to the skin.
（化粧料６）
実施例３の鱗片状または板状のリン酸処理雲母粒子を用いて以下の配合５により口紅を製造した。なお、はじめに成分Ａを８０℃に加熱混合し、次いで成分Ｂを加えて３本ロールでさらに分散させた後、再び加熱して成分Ｃを加えて分散攪拌し、容器に充填し口紅を作成した。
（配合５）
成分Ａ 質量％
ポリエチレンワックス １０
セレンワックス ３
ラノリン ２０
ポリブテン １８
オクチルメトキシシナメート ５
ジメチルポリシロキサン １２
成分Ｂ 質量％
酸化チタン ４．５
赤色２０１号 ０．５
赤色２０２号 １．２
赤色２２３号 ３．５
成分Ｃ 質量％
エステル油 ９．８
球状ポリエチレン粉末 ３．５
鱗片状または板状のリン酸処理雲母粒子 ９
防腐剤および香料 適量
上記口紅は、感触に優れており、唇に塗り伸ばす際にソフト感が得られた。
(Cosmetics 6)
Using the scale-like or plate-like phosphoric acid-treated mica particles of Example 3, a lipstick was produced according to the following formulation 5. First, component A was heated and mixed at 80 ° C., then component B was added and further dispersed with a three roll, then heated again, component C was added, dispersed and stirred, filled into a container, and a lipstick was prepared. .
(Formulation 5)
Component A mass%
Polyethylene wax 10
Selenium wax 3
Lanolin 20
Polybutene 18
Octyl methoxycinnamate 5
Dimethylpolysiloxane 12
Component B Mass%
Titanium oxide 4.5
Red No. 201 0.5
Red No. 202 1.2
Red 223 3.5
Ingredient C
Ester oil 9.8
Spherical polyethylene powder 3.5
Scale-like or plate-like phosphoric acid-treated mica particles 9
Preservative and perfume Appropriate amount The above lipstick was excellent in touch, and a soft feeling was obtained when applied to the lips.
Claims (5)
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| Application Number | Priority Date | Filing Date | Title |
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| JP2005069068A JP4590286B2 (en) | 2005-03-11 | 2005-03-11 | Scale-like or plate-like phosphoric acid-treated mica particles and cosmetics using the particles |
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| JP2005069068A JP4590286B2 (en) | 2005-03-11 | 2005-03-11 | Scale-like or plate-like phosphoric acid-treated mica particles and cosmetics using the particles |
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| JP4590286B2 JP4590286B2 (en) | 2010-12-01 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006327961A (en) * | 2005-05-24 | 2006-12-07 | Sekisui Plastics Co Ltd | Cosmetic |
| JP2008094773A (en) * | 2006-10-13 | 2008-04-24 | Mitsubishi Pencil Co Ltd | Cosmetic pencil lead and method for producing the same |
| JP2009234989A (en) * | 2008-03-27 | 2009-10-15 | Kose Corp | Oil-based cosmetic |
| JP2012193111A (en) * | 2011-03-14 | 2012-10-11 | Naris Cosmetics Co Ltd | Method for producing powder cosmetic, and powder cosmetic |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2001251A1 (en) * | 1969-01-17 | 1970-08-27 | Rikkihappo Oy | Process for the production of phosphorus-potash fertilizers from phosphoric acid and minerals of the mica group |
| JPS571486B2 (en) * | 1978-02-09 | 1982-01-11 | ||
| JP2001213964A (en) * | 2000-02-04 | 2001-08-07 | Shin Etsu Chem Co Ltd | Novel silicone compound, powder having surface treated therewith, and cosmetic containing the compound |
-
2005
- 2005-03-11 JP JP2005069068A patent/JP4590286B2/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2001251A1 (en) * | 1969-01-17 | 1970-08-27 | Rikkihappo Oy | Process for the production of phosphorus-potash fertilizers from phosphoric acid and minerals of the mica group |
| JPS571486B2 (en) * | 1978-02-09 | 1982-01-11 | ||
| JP2001213964A (en) * | 2000-02-04 | 2001-08-07 | Shin Etsu Chem Co Ltd | Novel silicone compound, powder having surface treated therewith, and cosmetic containing the compound |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006327961A (en) * | 2005-05-24 | 2006-12-07 | Sekisui Plastics Co Ltd | Cosmetic |
| JP4492961B2 (en) * | 2005-05-24 | 2010-06-30 | 積水化成品工業株式会社 | Cosmetics |
| JP2008094773A (en) * | 2006-10-13 | 2008-04-24 | Mitsubishi Pencil Co Ltd | Cosmetic pencil lead and method for producing the same |
| JP2009234989A (en) * | 2008-03-27 | 2009-10-15 | Kose Corp | Oil-based cosmetic |
| JP2012193111A (en) * | 2011-03-14 | 2012-10-11 | Naris Cosmetics Co Ltd | Method for producing powder cosmetic, and powder cosmetic |
Also Published As
| Publication number | Publication date |
|---|---|
| JP4590286B2 (en) | 2010-12-01 |
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