JPH07102973B2 - Ultrafine titanium oxide powder and cosmetics containing the same - Google Patents
Ultrafine titanium oxide powder and cosmetics containing the sameInfo
- Publication number
- JPH07102973B2 JPH07102973B2 JP23149387A JP23149387A JPH07102973B2 JP H07102973 B2 JPH07102973 B2 JP H07102973B2 JP 23149387 A JP23149387 A JP 23149387A JP 23149387 A JP23149387 A JP 23149387A JP H07102973 B2 JPH07102973 B2 JP H07102973B2
- Authority
- JP
- Japan
- Prior art keywords
- titanium oxide
- ultrafine
- black
- powder
- oxide powder
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims description 102
- 239000000843 powder Substances 0.000 title claims description 51
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 title claims description 42
- 239000002537 cosmetic Substances 0.000 title claims description 16
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 claims description 31
- 239000004408 titanium dioxide Substances 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000011882 ultra-fine particle Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 description 18
- 239000000049 pigment Substances 0.000 description 15
- 238000006722 reduction reaction Methods 0.000 description 14
- 239000007789 gas Substances 0.000 description 13
- 238000004040 coloring Methods 0.000 description 9
- KELHQGOVULCJSG-UHFFFAOYSA-N n,n-dimethyl-1-(5-methylfuran-2-yl)ethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=C(C)O1 KELHQGOVULCJSG-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 6
- 239000006229 carbon black Substances 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 239000010419 fine particle Substances 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000004020 conductor Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229940056319 ferrosoferric oxide Drugs 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- DSEKYWAQQVUQTP-XEWMWGOFSA-N (2r,4r,4as,6as,6as,6br,8ar,12ar,14as,14bs)-2-hydroxy-4,4a,6a,6b,8a,11,11,14a-octamethyl-2,4,5,6,6a,7,8,9,10,12,12a,13,14,14b-tetradecahydro-1h-picen-3-one Chemical compound C([C@H]1[C@]2(C)CC[C@@]34C)C(C)(C)CC[C@]1(C)CC[C@]2(C)[C@H]4CC[C@@]1(C)[C@H]3C[C@@H](O)C(=O)[C@@H]1C DSEKYWAQQVUQTP-XEWMWGOFSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 210000004709 eyebrow Anatomy 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007794 irritation Effects 0.000 description 1
- 229940057995 liquid paraffin Drugs 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 150000003956 methylamines Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q1/00—Make-up preparations; Body powders; Preparations for removing make-up
- A61Q1/02—Preparations containing skin colorants, e.g. pigments
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/29—Titanium; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/41—Particular ingredients further characterized by their size
- A61K2800/413—Nanosized, i.e. having sizes below 100 nm
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Nanotechnology (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- Animal Behavior & Ethology (AREA)
- Biotechnology (AREA)
- Birds (AREA)
- Molecular Biology (AREA)
- Pharmacology & Pharmacy (AREA)
- Crystallography & Structural Chemistry (AREA)
- Medical Informatics (AREA)
- Inorganic Chemistry (AREA)
- Medicinal Chemistry (AREA)
- Epidemiology (AREA)
- General Engineering & Computer Science (AREA)
- Biophysics (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Conductive Materials (AREA)
- Cosmetics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Description
【発明の詳細な説明】 発明の技術分野 本発明は、超微粒子酸化チタン粉末およびこれを配合し
てなる化粧料に関し、さらに詳しくは、主に黒色顔料と
しての用途、化粧料としての用途あるいは導電材などの
用途が期待される黒色系色彩を有する超微粒子酸化チタ
ン粉末およびこれを配合してなる化粧料に関する。TECHNICAL FIELD OF THE INVENTION The present invention relates to ultrafine titanium oxide powder and a cosmetic composition containing the same, and more specifically, it is mainly used as a black pigment, as a cosmetic composition, or as a conductive material. TECHNICAL FIELD The present invention relates to an ultrafine particle titanium oxide powder having a black color, which is expected to be used as a material, and a cosmetic material containing the same.
発明の技術的背景ならびにその問題点 従来、黒色顔料としてカーボンブラック粉末あるいは四
三酸化鉄粉末が広く用いられている。このうちカーボン
ブラックは、黒色度および着色力ともに優れているが、
疎水性であるため水に濡れにくく、また一般に粒径が極
端に小さ過ぎるため、混合して用いる場合配合に応じ流
動性が敏感に変動しすぎ、このため使用時に困難が伴う
という問題点があった。またカーボンブラックには、3,
4−ベンツピレンなどの発癌性物質が混入する可能性が
指摘されており、人体への悪影響が懸念されている。TECHNICAL BACKGROUND OF THE INVENTION AND PROBLEMS THEREOF Carbon black powder or ferrosoferric oxide powder has been widely used as a black pigment. Among them, carbon black is excellent in both blackness and coloring power,
Since it is hydrophobic, it is difficult to get wet with water, and in general, the particle size is extremely small, so when used as a mixture, the fluidity changes too sensitively depending on the formulation, which causes difficulties during use. It was In addition, carbon black has 3,
It has been pointed out that carcinogenic substances such as 4-benzpyrene may be mixed in, and it is feared that the human body will be adversely affected.
一方、四三酸化鉄は、その磁性のため凝集しやすく、顔
料として用いた場合に、色むらが生じやすいという問題
点があった。そしてまた、四三酸化鉄は、大気中で約15
0℃程度の温度に加熱されると、酸化されてγ−Fe2O3に
変化するため、熱安定性に乏しいという点で問題点があ
った。On the other hand, ferrosoferric oxide has a problem that it tends to aggregate due to its magnetism and that when used as a pigment, color unevenness easily occurs. And, ferrosoferric oxide is about 15 in the atmosphere.
When heated to a temperature of about 0 ° C., it is oxidized and changed to γ-Fe 2 O 3 , which has a problem in that it has poor thermal stability.
このように、従来公知の黒色顔料には、何らかの問題点
があり、より品質の優れた黒色顔料が望まれ、このよう
な情況のもとで、本発明者らによって水素ガスを用いて
二酸化チタンを還元して黒色系色彩を有する低次酸化チ
タンを得る方法がすでに提案されている。しかし、この
方法では、1,100℃以上の高温に加熱しないと還元反応
は進行せず、しかもこの際粒子が焼結して粗大化し、微
細で分散性の良い粉末を得ることはできないという問題
点があることが、本発明者らによって見出された。As described above, conventionally known black pigments have some problems, and black pigments of higher quality are desired. Under such circumstances, the present inventors have used hydrogen gas to produce titanium dioxide. A method for reducing low-order titanium oxide having a black color has already been proposed. However, in this method, the reduction reaction does not proceed unless it is heated to a high temperature of 1,100 ° C. or higher, and at this time, the particles are sintered and coarsened, and it is not possible to obtain a fine powder having good dispersibility. It has been found by the inventors.
そこで、上記のような技術的課題を解決するため、本発
明者等は鋭意研究したところ、超微粒子（一般に粒径が
0.1μｍ以下の粒子を超微粒子と呼んでいる）状の二酸
化チタン粉末をメチルアミンガス雰囲気下で、700〜1,1
00℃の温度で加熱還元することによって、黒色度、着色
度、分散性、耐熱性、および人体に対する安全性に優れ
ている黒色系色彩を有する一酸化チタンTiOが得られる
ことを見出し、さらに詳細に検討し、本発明を完成する
に至った。Therefore, in order to solve the above technical problems, the present inventors have conducted diligent research and found that ultrafine particles (generally,
Particles of 0.1 μm or less are called ultrafine particles) -like titanium dioxide powder in a methylamine gas atmosphere at 700 to 1,1
It was found that titanium monoxide TiO having a black color, which is excellent in blackness, coloring degree, dispersibility, heat resistance, and safety for human body, can be obtained by heating and reducing at a temperature of 00 ° C, and further details And completed the present invention.
発明の目的 本発明は、上記のような問題点を解決しようとするもの
であって、微細で分散性が良く、顔料、化粧料、導電材
などの用途が期待される黒色系色彩を有する超微粒子お
よびこれを配合してなる化粧料を提供することにある。An object of the present invention is to solve the above-mentioned problems, and it is fine and has a good dispersibility, and has a superb color having a black color which is expected to be used for pigments, cosmetics, conductive materials and the like. It is an object to provide fine particles and a cosmetic containing the fine particles.
発明の概要 本発明に係る黒色系色彩を有する超微粒子酸化チタン粉
末は、超微粒子二酸化チタン粉末を、メチルアミンガス
雰囲気下で、700〜1,100℃の温度で加熱還元して得られ
ることを特徴とし、また本発明に係る化粧料は、上記黒
色系色彩を有する超微粒子酸化チタン粉末を配合してな
ることを特徴としている。SUMMARY OF THE INVENTION Ultrafine titanium oxide powder having a black color according to the present invention is characterized in that it is obtained by heating and reducing ultrafine titanium dioxide powder at a temperature of 700 to 1,100 ° C. under a methylamine gas atmosphere. The cosmetic according to the present invention is characterized by being blended with the ultrafine titanium oxide powder having the above black color.
発明の具体的説明 以下、本発明に係る黒色系色彩を有する超微粒子酸化チ
タン粉末およびこれを配合してなる化粧料について、具
体的に説明する。DETAILED DESCRIPTION OF THE INVENTION The ultrafine titanium oxide powder having a black color according to the present invention and the cosmetic containing the same will be specifically described below.
本発明に係る超微粒子酸化チタン粉末は、黒色度、着色
度、分散性、耐熱性および人体に対する安全性等に優れ
ているため、黒色顔料、化粧料、導電材、触媒、焼結体
用原料粉末等の用途に使用することができる。The ultrafine titanium oxide powder according to the present invention is excellent in blackness, coloring degree, dispersibility, heat resistance, safety for human body, etc., and is therefore a black pigment, a cosmetic material, a conductive material, a catalyst, a raw material for a sintered body. It can be used for powders and the like.
本発明に係る超微粒子酸化チタン粉末を製造するには、
まず、超微粒子状の二酸化チタン粉末を準備する。この
超微粒子状の二酸化チタンの粒径は0.01〜0.04μｍであ
ることが好ましい。本発明にあっては、二酸化チタンは
アナターゼ型、ルチル型あるいはブルッカイト型のいず
れを用いてもよく、その種類は問わないが、アナターゼ
型二酸化チタンを用いた場合には、濃黒色の超微粒子酸
化チタン粉末が得られるため、黒色顔料を製造するため
の原料としては、このアナターゼ型二酸化チタンが特に
好ましい。なお、ルチル型、ブルッカイト型二酸化チタ
ンを用いた場合には、若干青味を帯びた黒色の超微粒子
酸化チタン粉末が得られる。To produce the ultrafine titanium oxide powder according to the present invention,
First, a titanium dioxide powder in the form of ultrafine particles is prepared. The particle size of the ultrafine titanium dioxide is preferably 0.01 to 0.04 μm. In the present invention, titanium dioxide may be of anatase type, rutile type or brookite type, and its type is not limited, but when anatase type titanium dioxide is used, dark black ultrafine particles are oxidized. This anatase-type titanium dioxide is particularly preferable as a raw material for producing the black pigment because titanium powder is obtained. When rutile type or brookite type titanium dioxide is used, a slightly bluish black ultrafine particle titanium oxide powder is obtained.
また、粒径0.01〜0.04μｍの超微粒子二酸化チタン粉末
を用いることによって、還元反応を促進することがで
き、より加熱処理温度を下げることができるという効果
が認められる。すなわち、本発明にあっては、加熱処理
温度を700℃程度にまで下げることが可能であり、この
ため粒子同志が焼結しにくくなり、還元反応により得ら
れる黒色酸化チタンの粒径を小さくすることができ、0.
01〜0.05μｍ程度の一酸化チタンの黒色粉末が得られ
る。Further, by using the ultrafine titanium dioxide powder having a particle size of 0.01 to 0.04 μm, it is recognized that the reduction reaction can be promoted and the heat treatment temperature can be further lowered. That is, in the present invention, it is possible to reduce the heat treatment temperature to about 700 ° C., which makes it difficult for the particles to sinter each other, and to reduce the particle size of black titanium oxide obtained by the reduction reaction. You can, 0.
A black powder of titanium monoxide of about 01 to 0.05 μm is obtained.
次に、準備した前記超微粒子二酸化チタン粉末を、メチ
ルアミンガス雰囲気下で700〜1,100℃の温度で加熱還元
する。Next, the prepared ultrafine titanium dioxide powder is heated and reduced at a temperature of 700 to 1,100 ° C. in a methylamine gas atmosphere.
メチルアミンガスを用いることにより、二酸化チタン中
の酸素原子がメチルアミンの構成元素である水素原子の
みならず炭素原子の作用で脱離した還元反応が促進さ
れ、二酸化チタンの一酸化チタンへの還元反応は、上記
水素ガスまたはアンモニアガスを用いる場合よりも、極
めて速やかに効率よく進行する。したがって、本発明で
は、メチルアミンガスを用いることにより還元反応時間
を大幅に短縮することができる。たとえば、アンモニア
ガスを用いた場合、通常、還元反応時間として４〜５時
間要していたが、メチルアミンガスを用いることによっ
て、還元反応時間を１〜２時間程度に短縮することがで
きる。The use of methylamine gas promotes the reduction reaction in which the oxygen atoms in titanium dioxide are eliminated by the action of not only the hydrogen atoms, which are the constituent elements of methylamine, but also the carbon atoms, and the reduction of titanium dioxide to titanium monoxide. The reaction proceeds extremely rapidly and efficiently as compared with the case of using the above hydrogen gas or ammonia gas. Therefore, in the present invention, the reduction reaction time can be significantly shortened by using methylamine gas. For example, when ammonia gas is used, the reduction reaction time usually takes 4 to 5 hours, but by using methylamine gas, the reduction reaction time can be shortened to about 1 to 2 hours.
またメチルアミンガスを用いる本発明では、二酸化チタ
ンの一酸化チタンへの還元率が極めて高いため、得られ
る一酸化チタン粉末は、黒色度がより高くなり、また導
電性も増大して品質の向上を図ることができる。また、
原料の二酸化チタン粉末の微細さを維持することができ
るため、粒径が0.01〜0.05μｍである超微粒子状の一酸
化チタン黒色粉末を得ることができる。Further, in the present invention using methylamine gas, since the reduction rate of titanium dioxide to titanium monoxide is extremely high, the obtained titanium monoxide powder has higher blackness and also has increased conductivity and improved quality. Can be achieved. Also,
Since the fineness of the raw material titanium dioxide powder can be maintained, it is possible to obtain ultrafine particulate titanium monoxide black powder having a particle size of 0.01 to 0.05 μm.
加熱温度が700℃未満であると、得られる酸化チタン
は、その色調が灰色系となるため、黒色顔料として好ま
しくない。700℃未満の温度で加熱した場合には、還元
反応が十分進まないため、得られる酸化チタンの色調が
灰色系となるのであろうと推察される。また、1,100℃
を越えた温度で加熱すると高温すぎるため、焼結が進行
しすぎて粒子が粗大化し、細かい分散性の良い粉末は得
られないため、好ましくない。本発明にあっては、700
〜1,100℃の温度範囲内の温度で加熱処理した場合に、
良好な黒色系色彩を有する超微粒子酸化チタン粉末が得
られる。When the heating temperature is lower than 700 ° C., the obtained titanium oxide has a grayish tone, which is not preferable as a black pigment. When heated at a temperature lower than 700 ° C., the reduction reaction does not proceed sufficiently, and it is presumed that the obtained titanium oxide has a grayish color tone. In addition, 1,100 ℃
If the heating temperature is higher than the above, the temperature is too high, the sintering proceeds too much, the particles become coarse, and a fine powder having good dispersibility cannot be obtained, which is not preferable. In the present invention, 700
When heat-treated at a temperature within the temperature range of ~ 1,100 ° C,
Ultrafine titanium oxide powder having a good black color is obtained.
上記のような加熱は、１〜２時間程度であることが好ま
しく、比較的短時間のうちに還元反応が進行する。The heating as described above is preferably for about 1 to 2 hours, and the reduction reaction proceeds in a relatively short time.
本発明に係る化粧料は、上記のようにして製造された黒
色系色彩を有する超微粒子酸化チタン粉末を配合してな
る化粧料であり、この超微粒子酸化チタン粉末は、黒色
度が高く、また粒径が0.01〜0.05μｍであるので分散性
が良く、しかも後述する実施例１におけるパッチ・テス
トの試験結果からもわかるように、人体に対する安全性
にも優れているため、化粧料の黒色顔料として好適であ
る。The cosmetic according to the present invention is a cosmetic prepared by blending the ultrafine particle titanium oxide powder having a black color produced as described above, and the ultrafine particle titanium oxide powder has a high degree of blackness, and Since the particle size is 0.01 to 0.05 μm, the dispersibility is good, and as it can be seen from the test results of the patch test in Example 1 which will be described later, it is also excellent in safety for the human body. Is suitable as
このような黒色系色彩を有する超微粒子酸化チタン粉末
が配合された化粧料としては、従来黒色顔料が配合され
る化粧料が挙げられ、具体的には、アイライナー、マス
カラ、アイシャドー、まゆずみなどが挙げられる。Examples of cosmetics in which the ultrafine titanium oxide powder having such a black color is blended include cosmetics in which a black pigment has been conventionally blended, and specifically, eyeliner, mascara, eye shadow, and eyebrows. And so on.
本発明に係る超微粒子酸化チタン粉末は、超微粒子二酸
化チタン粉末を、メチルアミンガス雰囲気下で、700〜
1,100℃の温度で加熱還元して製造されているので、粉
末の粗大化を防止することが可能となり、粒径が0.01〜
0.05μｍ程度の微細な黒色の一酸化チタン粉末が得られ
る。Ultrafine titanium oxide powder according to the present invention, ultrafine titanium dioxide powder, under a methylamine gas atmosphere, 700 ~.
Since it is manufactured by heating and reducing at a temperature of 1,100 ° C, it is possible to prevent coarsening of the powder, and the particle size is 0.01 ~
A fine black titanium oxide powder of about 0.05 μm is obtained.
このように、本発明に係る超微粒子酸化チタン粉末は、
その粒径が微細であるため従来のミクロン単位の黒色粉
末では得られない諸々の特性を有し、たとえば黒色顔料
として用いた場合、その着色力が大きく、また分散性が
非常によい、等の特性を有している。Thus, the ultrafine titanium oxide powder according to the present invention,
Because of its fine particle size, it has various characteristics that cannot be obtained with conventional black powder of the micron unit. For example, when it is used as a black pigment, its coloring power is large and its dispersibility is very good. It has characteristics.
またこの一酸化チタン粉末は、着色力、分散性に優れて
いるだけでなく、後述する実施例１におけるパッチ・テ
ストの試験結果からもわかるように、人体に対する安全
性にも優れているため、化粧料としての用途にもより好
適なものとして使用できる。Further, this titanium monoxide powder is not only excellent in coloring power and dispersibility, but also excellent in safety for human body, as can be seen from the test results of the patch test in Example 1 described later. It can be used as a more suitable material for cosmetics.
さらに、導電材料として用いた場合、テープ等へのコー
ティング性に著しい向上が見られ、さらにまた微細粒子
は、一般に反応活性が高いため触媒としての用途も期待
できる。Further, when used as a conductive material, the coating property on a tape or the like is remarkably improved, and since fine particles generally have high reaction activity, they can be expected to be used as a catalyst.
以上のように、本発明に係る超微粒子の黒色酸化チタン
は、前記のような用途が考えられるが、次に（イ）カー
ボンブラック、（ロ）四三酸化鉄ならびに（ハ）流速２
／分のアンモニアガス雰囲気下で、粒径0.02μｍのア
ナターゼ型二酸化チタン粉末を800℃の温度条件で３時
間加熱処理して得られた黒色酸化チタンと、本発明に係
る超微粒子の黒色酸化チタンとの特性の比較を表１に示
す。As described above, the ultrafine black titanium oxide according to the present invention may be used as described above. Next, (a) carbon black, (b) triiron tetraoxide and (c) a flow rate of 2
Black titanium oxide obtained by heat-treating anatase type titanium dioxide powder having a particle size of 0.02 μm at a temperature condition of 800 ° C. for 3 hours in an ammonia gas atmosphere of 1 / min, and ultrafine black titanium oxide particles according to the present invention. Table 1 shows a comparison of the characteristics with and.
表１より本発明に係る超微粒子の黒色酸化チタンは、そ
の色調（Ｌ値）が８〜10で十分な黒さを持ち、またその
微細さにおいても優れていることがわかる。 From Table 1, it is understood that the ultrafine black titanium oxide according to the present invention has a sufficient blackness with a color tone (L value) of 8 to 10, and is also excellent in fineness.
発明の効果 本発明に係る超微粒子酸化チタン粉末は、超微粒子二酸
化チタン粉末を、メチルアミンガス雰囲気下で、700〜
1,100℃の温度で加熱還元して製造されているので、粉
末の粗大化を防止することが可能となり、粒径が0.01〜
0.05μｍ程度の微細な黒色の一酸化チタン粉末が得られ
る。Effects of the Invention Ultrafine titanium oxide powder according to the present invention, ultrafine titanium dioxide powder, in a methylamine gas atmosphere, 700 ~
Since it is manufactured by heating and reducing at a temperature of 1,100 ° C, it is possible to prevent coarsening of the powder, and the particle size is 0.01 ~
A fine black titanium oxide powder of about 0.05 μm is obtained.
このように、本発明に係る超微粒子酸化チタン粉末は、
その粒径が微細であるため従来のミクロン単位の黒色粉
末では得られない諸々の特性を有し、たとえば黒色顔料
として用いた場合、その着色力が大きく、また分散性が
非常によい、等の特性を有している。Thus, the ultrafine titanium oxide powder according to the present invention,
Because of its fine particle size, it has various characteristics that cannot be obtained with conventional black powder of the micron unit. For example, when it is used as a black pigment, its coloring power is large and its dispersibility is very good. It has characteristics.
以下、本発明を実施例により説明するが、本発明はこれ
ら実施例に限定されるものではない。Hereinafter, the present invention will be described with reference to examples, but the present invention is not limited to these examples.
実施例１ ［超微粒子酸化チタン粉末の製造］ 原料として粒径0.01μｍのアナターゼ型二酸化チタン粉
末を用いた。メチルアミンガスを流速２／分で流しな
がら、このメチルアミンガス雰囲気下で、前記二酸化チ
タン粉末を800℃の温度条件で２時間加熱還元処理し、
次いで400℃以下に冷却して生成物を取り出した。Example 1 [Production of Ultrafine Titanium Oxide Powder] Anatase type titanium dioxide powder having a particle size of 0.01 μm was used as a raw material. While flowing methylamine gas at a flow rate of 2 / min, the titanium dioxide powder was heat-reduced for 2 hours at a temperature of 800 ° C. under the methylamine gas atmosphere,
Then, the product was taken out by cooling to 400 ° C or lower.
得られた生成物は、超微粒子状の黒色酸化チタンであ
り、前記二酸化チタンの一酸化チタンへの還元率は98％
であった。また、その粒径は0.01〜0.02μｍ、色調Ｌ値
は10、比表面積は50m2/gであった。The obtained product is ultrafine black titanium oxide, and the reduction rate of titanium dioxide to titanium monoxide is 98%.
Met. The particle size was 0.01 to 0.02 μm, the color tone L value was 10, and the specific surface area was 50 m 2 / g.
さらに、この実施例１において得られた、本発明に係る
超微粒子状の黒色酸化チタンについて、前記表１におけ
る（イ）カーボンブラック、（ロ）四三酸化鉄、（ハ）
アンモニアガスを用いて得られた黒色酸化チタンととも
に、下記の方法で着色力試験、分散性試験を行ない、そ
れぞれＬ値を測定し、分散状態を評価した。Furthermore, regarding the ultrafine particulate black titanium oxide according to the present invention obtained in this Example 1, (a) carbon black, (b) iron tetroxide, (c) in Table 1 above
A coloring strength test and a dispersibility test were performed by the following methods together with the black titanium oxide obtained using ammonia gas, and the L value was measured for each to evaluate the dispersion state.
その結果を表２に示す。The results are shown in Table 2.
［着色力試験方法］ 試料の配合は、黒色顔料３部、白色二酸化チタン47部、
流動パラフィン39部、界面活性剤１部およびセレシン10
部とし、東京電色（株）製カラーアナライザーを用いて
この試料の明度の目安であるＬ値を測定する。[Testing method for tinting strength] The composition of the sample was as follows: 3 parts of black pigment, 47 parts of white titanium dioxide,
Liquid paraffin 39 parts, surfactant 1 part and ceresin 10
The L value, which is a measure of the brightness of this sample, is measured using a color analyzer manufactured by Tokyo Denshoku Co., Ltd.
［分散性試験方法］ 試料の配合は、黒色顔料３部、酢酸ビニル樹脂エマルジ
ョン50部、カルボキシセルロース10重量％水溶液11部、
蒸溜水36部とし、この試料を十分に撹拌した後、１日放
置し、このときの試料の分散状態を目視により観察す
る。分散状態の評価は10段階による評価とし、最も分散
性の良好な試料の分散状態を10とする。[Dispersion test method] The sample composition is 3 parts of a black pigment, 50 parts of a vinyl acetate resin emulsion, 11 parts of a 10% by weight carboxycellulose aqueous solution,
After making 36 parts of distilled water, the sample was sufficiently stirred and allowed to stand for 1 day, and the dispersion state of the sample at this time is visually observed. The dispersion state is evaluated in 10 steps, and the dispersion state of the sample having the best dispersibility is set to 10.
表２より本発明の実施例１の黒色酸化チタンを用いた試
料が、他の黒色顔料を用いた試料と比較して最も大きな
着色力を有し、また最も良好な分散性を有することがわ
かる。 From Table 2, it can be seen that the sample using black titanium oxide of Example 1 of the present invention has the largest coloring power and the best dispersibility as compared with the samples using other black pigments. .
また、本発明に係る実施例１の超微粒子状の黒色酸化チ
タンの人体に対する安全性について、本発明に係る超微
粒子状の黒色酸化チタンを少量の蒸溜水で練り、これを
リントに塗布して30名を対象に、上腕部に24時間閉塞パ
ッチ・テストを行なったところ、陽性率が零であり刺激
性がないことが判明した。Regarding the safety of the ultrafine particulate black titanium oxide of Example 1 according to the present invention to the human body, the ultrafine particulate black titanium oxide according to the present invention was kneaded with a small amount of distilled water and applied to lint. A 24-hour occlusive patch test on the upper arm of 30 subjects revealed that the positive rate was zero and there was no irritation.
これらの試験結果より、本発明に係る超微粒子状の黒色
酸化チタンが、着色力、分散性および人体に対する安全
性に優れ、メイクアップ化粧料としての用途等に好適で
あることがわかる。From these test results, it is understood that the ultrafine particulate black titanium oxide according to the present invention is excellent in coloring power, dispersibility, and safety for human body, and is suitable for use as makeup cosmetics and the like.
実施例２ ［超微粒子酸化チタン粉末の製造］ 原料として粒径0.02μｍのルチル型二酸化チタン粉末を
用いた。メチルアミンガスを流速３／分で流しなが
ら、このメチルアミンガス雰囲気下で、前記二酸化チタ
ン粉末を950℃の温度条件で１時間加熱還元処理し、次
いで400℃以下に冷却して生成物を取り出した。Example 2 [Production of Ultrafine Titanium Oxide Powder] Rutile titanium dioxide powder having a particle diameter of 0.02 μm was used as a raw material. While flowing methylamine gas at a flow rate of 3 / min, the titanium dioxide powder was subjected to a heat reduction treatment at a temperature condition of 950 ° C. for 1 hour in this methylamine gas atmosphere, and then cooled to 400 ° C. or lower to take out the product. It was
得られた生成物は、超微粒子状の黒色酸化チタンであ
り、前記二酸化チタンの一酸化チタンへの還元率は99％
であった。また、その粒径は0.02〜0.03μｍ、色調Ｌ値
は９、比表面積は45m2/gであった。The resulting product is ultrafine black titanium oxide, and the reduction rate of the titanium dioxide to titanium monoxide is 99%.
Met. The particle size was 0.02 to 0.03 μm, the color tone L value was 9, and the specific surface area was 45 m 2 / g.
実施例３ 実施例１で調製した超微粒子状の黒色酸化チタンを用い
て、次の配合によりアイペンシルを製造した。Example 3 Using the ultrafine particulate black titanium oxide prepared in Example 1, an eye pencil was produced with the following formulation.
実施例４ 実施例２で調製した超微粒子状の黒色酸化チタンを用い
て、次の配合によりアイライナーを製造した。 Example 4 Using the ultrafine particulate black titanium oxide prepared in Example 2, an eyeliner was produced according to the following formulation.
Claims (2)
ンガス雰囲気下で、700〜1,100℃の温度で加熱還元して
得られることを特徴とする黒色系色彩を有する超微粒子
酸化チタン粉末。1. An ultrafine particle titanium oxide powder having a blackish color, which is obtained by heating and reducing ultrafine particle titanium dioxide powder in a methylamine gas atmosphere at a temperature of 700 to 1,100 ° C.
ンガス雰囲気下で、700〜1,100℃の温度で加熱還元して
得られる黒色系色彩を有する超微粒子酸化チタン粉末を
配合してなる化粧料。2. A cosmetic comprising an ultrafine titanium oxide powder having a black color obtained by heating and reducing the ultrafine titanium dioxide powder in a methylamine gas atmosphere at a temperature of 700 to 1,100 ° C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23149387A JPH07102973B2 (en) | 1987-09-16 | 1987-09-16 | Ultrafine titanium oxide powder and cosmetics containing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23149387A JPH07102973B2 (en) | 1987-09-16 | 1987-09-16 | Ultrafine titanium oxide powder and cosmetics containing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6472922A JPS6472922A (en) | 1989-03-17 |
| JPH07102973B2 true JPH07102973B2 (en) | 1995-11-08 |
Family
ID=16924353
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23149387A Expired - Lifetime JPH07102973B2 (en) | 1987-09-16 | 1987-09-16 | Ultrafine titanium oxide powder and cosmetics containing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07102973B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3688205A4 (en) * | 2017-09-26 | 2021-11-03 | Applied Materials, Inc. | PROCESS, MATERIALS AND PROCESS FOR THE REMOVAL OF NATIVE OXIDE AND THE REFORMATION OF DIELECTRIC OXIDES, ALLOWING BETTER BIOCAPTER PERFORMANCE |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009091206A (en) * | 2007-10-10 | 2009-04-30 | Tayca Corp | Fine particle titanium monoxide composition and method for producing the same |
| JP6841088B2 (en) * | 2017-03-01 | 2021-03-10 | 堺化学工業株式会社 | Conductive material and electrode material |
-
1987
- 1987-09-16 JP JP23149387A patent/JPH07102973B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP3688205A4 (en) * | 2017-09-26 | 2021-11-03 | Applied Materials, Inc. | PROCESS, MATERIALS AND PROCESS FOR THE REMOVAL OF NATIVE OXIDE AND THE REFORMATION OF DIELECTRIC OXIDES, ALLOWING BETTER BIOCAPTER PERFORMANCE |
| US11598000B2 (en) | 2017-09-26 | 2023-03-07 | Applied Materials, Inc. | Method, materials and process for native oxide removal and regrowth of dielectric oxides for better biosensor performance |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6472922A (en) | 1989-03-17 |
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