JPS6330313A - Composite powder and its production - Google Patents

Composite powder and its production

Info

Publication number
JPS6330313A
JPS6330313A JP61174578A JP17457886A JPS6330313A JP S6330313 A JPS6330313 A JP S6330313A JP 61174578 A JP61174578 A JP 61174578A JP 17457886 A JP17457886 A JP 17457886A JP S6330313 A JPS6330313 A JP S6330313A
Authority
JP
Japan
Prior art keywords
powder
water
composite powder
clay mineral
inorg
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
JP61174578A
Other languages
Japanese (ja)
Other versions
JPH0696447B2 (en
Inventor
Kazuo Higashikubo
東久保 和雄
Michihiro Yamaguchi
山口 道広
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shiseido Co Ltd
Original Assignee
Shiseido Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shiseido Co Ltd filed Critical Shiseido Co Ltd
Priority to JP61174578A priority Critical patent/JPH0696447B2/en
Priority to PCT/JP1987/000540 priority patent/WO1988000572A1/en
Priority to EP87904938A priority patent/EP0277244B1/en
Priority to DE3750576T priority patent/DE3750576T2/en
Publication of JPS6330313A publication Critical patent/JPS6330313A/en
Priority to US07/538,595 priority patent/US5165915A/en
Publication of JPH0696447B2 publication Critical patent/JPH0696447B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q1/00Make-up preparations; Body powders; Preparations for removing make-up
    • A61Q1/12Face or body powders for grooming, adorning or absorbing
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241Containing particulates characterized by their shape and/or structure
    • A61K8/025Explicitly spheroidal or spherical shape
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0241Containing particulates characterized by their shape and/or structure
    • A61K8/0279Porous; Hollow
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/26Aluminium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/29Titanium; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/84Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions otherwise than those involving only carbon-carbon unsaturated bonds
    • A61K8/88Polyamides
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/0081Composite particulate pigments or fillers, i.e. containing at least two solid phases, except those consisting of coated particles of one compound
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09CTREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40Compounds of aluminium
    • C09C1/42Clays

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Chemical & Material Sciences (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Inorganic Chemistry (AREA)
  • Organic Chemistry (AREA)
  • Dispersion Chemistry (AREA)
  • Composite Materials (AREA)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Powder Metallurgy (AREA)
  • General Preparation And Processing Of Foods (AREA)
  • Formation And Processing Of Food Products (AREA)
  • Medicinal Preparation (AREA)
  • Cosmetics (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

PURPOSE:To obtain the title composite powder without damaging the function of the object powder such as org., inorg., and metal powder, without reacting with the coexistent components in various systems, and providing a stable product by the mixing with all sorts of bases by uniformly dispersing metal powder in water-swollen clay mineral powder. CONSTITUTION:The aq. dispersion of one or >=2 kinds among org., inorg., or metal powder and a water-swollen clay mineral is spray-dried to obtain composite powder wherein one or >=2 kinds among, org., inorg., or metal powder are contained in the powder consisting of the water-swollen clay mineral. The water-swollen clay mineral is phyllosilicate belonging to a smectite group, and montmorillonite, beidellite, etc., can be exemplified. The powder of polyamide resin, polyester resin, etc., can be exemplified as the org. powder, titanium dioxide, talc, calcium carbonate, etc., can be exemplified as the inorg. powder, and the powder of aluminum, gold, silver, iron, copper, etc., can be exemplified as the metal powder.

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は有機、無機又は金属粉体の1種もしくは2種以
上を内部に均一に分散させた水膨潤性粘土鉱物よりなる
複合粉体及びその製造方法に関する。更に詳しくは、有
機、無機又は金属粉体の1種もしくは2種以上と水膨潤
性粘土鉱物とを水性溶媒中に分散させ、しかる後に該分
散液を噴霧乾燥することによって得られる有機、無機又
は金属粉体が内部に一次粒子に近い状態で均一に分散し
ている水膨潤性粘土鉱物粉体及びその製造法に関する。
Detailed Description of the Invention [Industrial Application Field] The present invention relates to a composite powder made of a water-swellable clay mineral in which one or more types of organic, inorganic or metal powder are uniformly dispersed; It relates to its manufacturing method. More specifically, organic, inorganic or The present invention relates to a water-swellable clay mineral powder in which metal powder is uniformly dispersed in a state similar to that of primary particles, and a method for producing the same.

〔従来の技術〕[Conventional technology]

一般に、粉体類は表面活性を有するため、医薬品、食品
、化粧品、塗料等の系中において共存成分を劣化させる
ことが多い。
In general, since powders have surface activity, they often degrade coexisting components in systems such as pharmaceuticals, foods, cosmetics, and paints.

このようなことを防止する目的で、粉体表面に他の粉体
をボールミルなどを利用して被覆することにより複合粉
体化することが行われている。しかし、これらの複合粉
体にあっても、表面を被覆する粉体が、やはり劣化の原
因になることが多い。
In order to prevent this, the surface of the powder is coated with another powder using a ball mill or the like to form a composite powder. However, even with these composite powders, the powder that coats the surface often causes deterioration.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

本発明者らは、このような事情に鑑み、これらの欠点を
改良すべく鋭意研究を重ねた結果、水膨潤性粘土鉱物よ
りなる粉体中に、有機、無機又は金属粉体の1種もしく
は2種以上を含有する複合粉体、すなわち目的の粉体と
水膨潤性粘土鉱物とを水性溶媒中に分散させ、しかる後
に該分散液を噴霧乾燥することにより得られる複合粉体
が、目的粉体の機能を損なうことなく、目的粉体の表面
活性を封じ込め、もって様々な系中でも安定な粉体に成
りえることを見いだして、本発明をなすに至った。
In view of the above circumstances, the present inventors have conducted extensive research to improve these drawbacks, and have found that one or more of organic, inorganic, or metal powders are added to the water-swellable clay mineral powder. A composite powder containing two or more types, that is, a composite powder obtained by dispersing a target powder and a water-swellable clay mineral in an aqueous solvent, and then spray-drying the dispersion, is a target powder. The present invention was achieved by discovering that the surface activity of the target powder can be contained without impairing the body's functions, thereby making the powder stable in various systems.

〔問題点を解決するための手段〕[Means for solving problems]

すなわち本発明は、水膨潤性粘土鉱物よりなる粉体中に
、有機、無機又は金属粉体の1種もしくは2種以上を含
有することを特徴とする複合粉体である。
That is, the present invention is a composite powder characterized by containing one or more types of organic, inorganic, or metal powder in the powder made of water-swellable clay mineral.

また本発明は、有機、無機又は金属粉体の1種もしくは
2種以上と水膨潤性粘土鉱物の水性分散液とを噴霧乾燥
することを特徴とする、上記複合粉体の製造法を提供す
る。
The present invention also provides a method for producing the composite powder described above, which comprises spray-drying one or more organic, inorganic, or metal powders and an aqueous dispersion of water-swellable clay minerals. .

水膨潤性粘土鉱物からなる粉体中に他の成分を担持させ
る技術は知られている。しかしながら、担持される他の
成分としては、色素等が知られているのみであり、これ
らはいずれも分子として粘土鉱物層間に入っており、本
発明に係る有機、無機又は金属粉体の1種もしくは2種
以上のように固体としてではない。
Techniques for supporting other components in powder made of water-swellable clay minerals are known. However, the only other components known to be supported are pigments, etc., and these are all intercalated between clay mineral layers as molecules, and are one type of organic, inorganic, or metal powder according to the present invention. Or not as a solid, such as two or more types.

また従来技術にあっては、水膨潤性粘土鉱物と色素等と
からなる複合粉体を水性溶媒中から粉体として取り出す
場合には、濾過や遠心分離等の操作を経て沈澱物を乾燥
した後強い機械力を用いて粉砕するという工程をとるた
め、作業に手間取る。
Furthermore, in the conventional technology, when a composite powder consisting of a water-swellable clay mineral and a pigment is extracted from an aqueous solvent as a powder, the precipitate is dried through operations such as filtration or centrifugation, and then The process of crushing using strong mechanical force is time-consuming.

また得られる粉体の粒子形は鋭角な角を多く持つ不定形
になり易く、とくに使用感触を重視する化粧品などへの
多量配合が難しいという欠点を有していた。
In addition, the particle shape of the resulting powder tends to be amorphous with many sharp corners, and it has the disadvantage that it is difficult to incorporate it in large quantities into cosmetics, etc., where the feel of the product is especially important.

以下、本発明の構成について更に詳細に説明する。Hereinafter, the configuration of the present invention will be explained in more detail.

本発明に用いる水膨潤性粘土鉱物は、3層構造を有する
コロイド性含水ケイ酸アルミニウムの1種で、一般に下
記一般式 %式% で表せ、具体的にはモンモリロナイト、サボナイト及び
ヘクトライト等の天然または合成のスメクタイト群(市
販品ではバング−ビルト社製のビーガム、国峰鉱化製の
クニピア、ラボルテ社製のラポナイト等がある)及びナ
トリウムシリシックマイカやナトリウム又はリチウムテ
ニオライトの名で知られる合成雲母(市販品ではトピー
エ業製のグイモナイト等)等である。
The water-swellable clay mineral used in the present invention is a type of colloidal hydrated aluminum silicate having a three-layer structure, and is generally expressed by the following general formula %. Or synthetic smectites (commercially available products include Veegum manufactured by Bang-Bilt, Kunipia manufactured by Kunimine Minerals, Laponite manufactured by Laborte, etc.) and synthetic compounds known as sodium silicic mica or sodium or lithium teniolite. Mica (commercially available products include Guimonite manufactured by Topie Industries), etc.

本発明の実施にあたっては、これらの水膨潤性粘土鉱物
のうちから1種また2種以上が任意に選択される。
In carrying out the present invention, one or more water-swellable clay minerals are arbitrarily selected from among these water-swellable clay minerals.

本発明の水膨潤性粘土鉱物よりなる粉体中に含有される
粉体としては、任意の有機、無機又は金属粉体を用いる
ことができる。
Any organic, inorganic or metal powder can be used as the powder contained in the water-swellable clay mineral powder of the present invention.

代表例をあげれば、ポリアミド樹脂、ポリエチレン樹脂
、アクリル樹脂、ポリエステル樹脂、フッ素樹脂及びセ
ルロース系樹脂等の有機粉体、二酸化チタン、タルク、
カオリン、ハイドロキシアパタイト、亜鉛華、硫酸バリ
ウム、炭酸マグネシウム、炭酸カルシウム、シリカ、第
2リン酸カルシウム、酸化鉄、酸化クロム、水酸化クロ
ム、群青、紺青等の無機粉体、並びにアルミニウム粉、
金粉、銀粉、鉄粉、銅粉、亜鉛粉などの金属粉体である
Typical examples include organic powders such as polyamide resin, polyethylene resin, acrylic resin, polyester resin, fluorine resin, and cellulose resin, titanium dioxide, talc,
Inorganic powders such as kaolin, hydroxyapatite, zinc white, barium sulfate, magnesium carbonate, calcium carbonate, silica, dicalcium phosphate, iron oxide, chromium oxide, chromium hydroxide, ultramarine blue, deep blue, and aluminum powder,
Metal powders such as gold powder, silver powder, iron powder, copper powder, and zinc powder.

ただし、上記有機、無機又は金属粉体の粒子径は水膨潤
性粘土鉱物とこれらの粉体とによって構成される複合粉
体の粒子径が2〜30μm程度であることから、平均粒
子径が0.5μm以下、とくに好ましくは0.1μm以
下であることが好ましい。
However, the particle size of the above-mentioned organic, inorganic or metal powder is such that the particle size of the composite powder composed of water-swellable clay minerals and these powders is about 2 to 30 μm, so the average particle size is 0. It is preferably .5 μm or less, particularly preferably 0.1 μm or less.

これより大きいと水膨潤性粘土鉱物の粉体中に含有され
るべき上記粉末が複合粉体表面上に顔を出すことが多く
なり、好ましくない。
If it is larger than this, the powder that should be contained in the water-swellable clay mineral powder often appears on the surface of the composite powder, which is not preferable.

水膨潤性粘土鉱物と有機、無機又は金属粉体の1種又は
2種以上とからなる複合粉体中に占める有機、無機又は
金属粉体の1種又は2種以上の含有量は、複合粉体全量
中の0.1〜100重量%である。
The content of one or more types of organic, inorganic, or metal powder in a composite powder consisting of a water-swellable clay mineral and one or more types of organic, inorganic, or metal powder is The amount is 0.1 to 100% by weight based on the total body weight.

また水膨潤性粘土鉱物と有機、無機又は金属粉体の1種
又は2種以上とからなる複合粉体の粒子径は、平均で2
〜30μmである。
In addition, the average particle size of the composite powder consisting of water-swellable clay mineral and one or more types of organic, inorganic, or metal powder is 2.
~30 μm.

複合粉体の形状は任意であるが、とくに化粧品等の使用
感触を大事にする製品中に配合する場合は、できるだけ
球状に近い方が好ましい。球状の複合粉体を得るために
は、本願に係る次の製造方法が最も好ましい。
Although the shape of the composite powder is arbitrary, it is preferable that it be as close to a spherical shape as possible, especially when it is incorporated into products such as cosmetics where the feeling of use is important. In order to obtain a spherical composite powder, the following manufacturing method according to the present application is most preferable.

次に本発明の複合粉体の製造法について述べる。Next, a method for producing the composite powder of the present invention will be described.

まず、含有されるべき有機、無機又は金属粉体の1種又
は2種以上を水性溶媒中に分散させる。
First, one or more organic, inorganic, or metal powders to be contained are dispersed in an aqueous solvent.

ここで分散性を高めるために各種界面活性剤やヘキサメ
タリン酸ソーダなどの分散剤を加えてもよい。次いで、
これに水膨潤性粘土鉱物を分散してゲルを調製する。ゲ
ル中で上記の有機、無機又は金属粉体の1種又は2種以
上が均一に分散していることが大事である。最後に、こ
うして得られた分散液を噴霧乾燥するとノズルより吹き
出した水滴から水が瞬時に蒸発し、本発明の複合粉末が
得られる。得られた複合粉末は球状となる。
Here, various surfactants and dispersants such as sodium hexametaphosphate may be added to improve dispersibility. Then,
Water-swellable clay minerals are dispersed in this to prepare a gel. It is important that one or more of the above organic, inorganic or metal powders are uniformly dispersed in the gel. Finally, when the dispersion thus obtained is spray-dried, water instantly evaporates from the water droplets blown out from the nozzle, yielding the composite powder of the present invention. The obtained composite powder becomes spherical.

上記のゲル中における水膨潤性粘土鉱物の濃度は10重
量%以下が好ましい。これを超える濃度ではゲル粘度が
高くなり過ぎ、噴霧乾燥時のuniノズルへの液の送り
が難しく、またノズルの目づまり等が生じ易くなる。
The concentration of the water-swellable clay mineral in the above gel is preferably 10% by weight or less. If the concentration exceeds this, the gel viscosity will become too high, making it difficult to feed the liquid to the uni nozzle during spray drying, and clogging of the nozzle will likely occur.

ゲル中における有機、無機又は金属粉体の1種又は2種
以上の含有量は、乾燥後の複合粉体全量中に占める重量
が、上述の範囲になるように定めればよい。
The content of one or more organic, inorganic, or metal powders in the gel may be determined so that the weight of the total amount of the composite powder after drying falls within the above-mentioned range.

噴霧乾燥に際しては、ディスクタイプや加圧ノズル式、
2流体ノズル式などの一般的噴霧乾燥法が通用できる。
For spray drying, disc type, pressure nozzle type,
A general spray drying method such as a two-fluid nozzle method can be used.

噴霧時の入口空気温度は有機、無機又は金属粉体の1種
又は2種以上の安定性にもよるが、水膨潤性粘土鉱物が
300℃位までは熱的に十分安定であることから、約1
00〜300℃の広い温度範囲が設定できる。
The inlet air temperature during spraying depends on the stability of one or more of the organic, inorganic, or metal powders, but since water-swellable clay minerals are sufficiently thermally stable up to about 300°C, Approximately 1
A wide temperature range of 00 to 300°C can be set.

また、排気温度はノズルからの噴霧流量などによって異
なるが、概ね100℃前後で良い。
Further, the exhaust temperature may vary depending on the spray flow rate from the nozzle, etc., but may be approximately 100°C.

こうして得られる球状粘土鉱物の粒子径は2〜30μm
であり、球状を呈している。また粒子表面は、調製した
ゲルの外観が透明であって、かつゲルの粘度が高い(例
えばボラナイトの場合)程、均一でなめらかとなる。
The particle size of the spherical clay mineral thus obtained is 2 to 30 μm.
and has a spherical shape. Furthermore, the more transparent the appearance of the prepared gel and the higher the viscosity of the gel (for example, in the case of boranite), the more uniform and smooth the particle surface becomes.

このようにして得られる本発明の複合複体は、噴霧乾燥
の条件により若干具なるが、その粒子径は平均で2〜3
0μm程度となる。
The composite material of the present invention obtained in this way has a particle size of 2 to 3 on average, although the particle size varies slightly depending on the spray drying conditions.
It is approximately 0 μm.

〔発明の効果〕〔Effect of the invention〕

本発明に従えば、有機、無機又は金属粉体の1種又は2
種以上を系中の他の共存成分との反応も無くあらゆる基
剤に配合して安定な製品を提供し得る。また、形状を球
状に揃えれば揃えれる程、とくに充填効率がよく充填剤
として好適である。
According to the invention, one or two of organic, inorganic or metal powders
A stable product can be provided by blending more than one species into any base without reacting with other coexisting components in the system. Furthermore, the more spherical the shape is, the better the filling efficiency is and the more suitable it is as a filler.

また塗料などに用いた時は作業性や分散性がよく、化粧
品に用いた時には使用性がよいなどの特徴を併せ持って
いる。
It also has the characteristics of good workability and dispersibility when used in paints, etc., and good usability when used in cosmetics.

〔実施例〕〔Example〕

つぎに実施例をあげて更に詳細に説明するが、本発明は
これによって限定されるものではない。
Next, the present invention will be described in more detail with reference to Examples, but the present invention is not limited thereto.

実施例1 水1.000−にヘキサメタリン酸ソーダ0.5gを溶
解し、さらに0.1μm以下で平均粒径0.03μmの
微粒子二酸化チタン(微粒子二酸化チタンP−25;デ
グサ社製)10gをディスパーを用いて分散させる。分
散液に水膨潤性粘土鉱物(ラポナイトXLG、ラポルテ
社製)30gを分散させてゲル化させる。得られたゲル
をディスク式噴霧乾燥実験器により噴霧乾燥(ディスク
回転数 20. OOOrpm、入口空気温度約180
℃、排気温度約110℃)して、2〜15μmの球状複
合粉体32gを得た。
Example 1 0.5 g of sodium hexametaphosphate was dissolved in 1.000 μm of water, and 10 g of fine particle titanium dioxide (fine particle titanium dioxide P-25; manufactured by Degussa) with an average particle size of 0.1 μm or less and 0.03 μm was added to the dispersion solution. Disperse using. 30 g of a water-swellable clay mineral (Laponite XLG, manufactured by Laporte) is dispersed in the dispersion and gelatinized. The obtained gel was spray-dried using a disk-type spray-drying experiment device (disc rotation speed 20.OOOrpm, inlet air temperature approximately 180°C).
℃, exhaust temperature about 110℃) to obtain 32 g of spherical composite powder with a diameter of 2 to 15 μm.

この複合粉体の走査型電子顕微鏡写真を図1に示す。真
球状を呈していることがわかる。
A scanning electron micrograph of this composite powder is shown in FIG. It can be seen that it has a true spherical shape.

また、この真球状の複合粉末をエネルギー分散型X線分
析装置を用いて分析すると、どの部位からもチタンの存
在が確認でき、この球状複合粉体中に微粒子二酸化チタ
ンが均一に分散されていることがわかった。
Furthermore, when this spherical composite powder is analyzed using an energy dispersive X-ray analyzer, the presence of titanium can be confirmed from any part, indicating that fine particles of titanium dioxide are uniformly dispersed in this spherical composite powder. I understand.

試験例1 実施例1で得た球状複合粉体10重量%をヒマシ油に分
散し、三本ローラーで十分に練合後、石英板上にアプリ
ケーターを用いて5μmの厚さで塗布し、紫外線吸収量
を測定した。
Test Example 1 10% by weight of the spherical composite powder obtained in Example 1 was dispersed in castor oil, thoroughly kneaded with three rollers, applied to a thickness of 5 μm on a quartz plate using an applicator, and exposed to ultraviolet light. The amount of absorption was measured.

比較試験例1 本発明の複合粉体化を施していない微粒子二酸化チタン
(微粒子二酸化チタンP−25iデグサ社)2.5%(
微粒子二酸化チタン量で試験例1と同じ)をヒマシ油に
分散し、実施例2と同様にして紫外線吸収量を測定した
Comparative Test Example 1 Fine particle titanium dioxide (fine particle titanium dioxide P-25i Degussa) 2.5% (
The amount of fine particle titanium dioxide (same as in Test Example 1) was dispersed in castor oil, and the amount of ultraviolet absorption was measured in the same manner as in Example 2.

試験例1および比較試験例1の粉体の紫外線吸収量した
本発明の球状複合粉体は、微粒子二酸化チタン単独の場
合と同様の紫外線防御能を持つことが判る。
It can be seen that the spherical composite powder of the present invention, which has the ultraviolet absorption amount of the powders of Test Example 1 and Comparative Test Example 1, has the same ultraviolet protection ability as fine particle titanium dioxide alone.

試験例2 試験例1で得た球状複合粉体50重量%をヒマシ油に分
散して、ヒマシ油の変臭度合を測定した。
Test Example 2 50% by weight of the spherical composite powder obtained in Test Example 1 was dispersed in castor oil, and the degree of odor change of the castor oil was measured.

比較試験例2 本発明の複合粉体化を施していない微粒子二酸化チタン
(微粒子二酸化チタンP−25.デグサ社)12.5%
(微粒子二酸化チタン量で試験例2と同じ)をヒマシ油
に分散し、の変臭度合を測定した。
Comparative Test Example 2 Fine-particle titanium dioxide (fine-particle titanium dioxide P-25. Degussa) 12.5% without the composite powder of the present invention
(The amount of fine particle titanium dioxide is the same as Test Example 2) was dispersed in castor oil, and the degree of odor change was measured.

試験例2および比較試験例2のヒマシ油分散液を50℃
恒温槽中に保存し、2週間後の変臭の度合を感情評価し
た。
The castor oil dispersions of Test Example 2 and Comparative Test Example 2 were heated at 50°C.
It was stored in a constant temperature bath, and the degree of odor was evaluated emotionally after two weeks.

結果を表1に示す。本発明の球状複合粉体は、ヒマシ油
の劣化による変臭の発生を著しく抑制していることが判
る。これは、ヒマシ油の劣化・変臭をもたらす微粒子二
酸化チタンの表面活性点のほとんどが、本発明による複
合粉体化により複合粉体の内部に包みこまれ、分散媒で
あるヒマシ油と非接触になったためである。
The results are shown in Table 1. It can be seen that the spherical composite powder of the present invention significantly suppresses the occurrence of odor caused by deterioration of castor oil. This is because most of the surface active sites of particulate titanium dioxide, which cause deterioration and odor in castor oil, are wrapped inside the composite powder by the composite powder according to the present invention, and do not come into contact with the castor oil, which is the dispersion medium. This is because it has become.

表1 50℃ 2週間後の変臭度合 実施例3  はとんど変臭が感じられない比較例2  
著しい酌味臭を感じた (以下金白) 実施例2 実施例1で得た球状複合粉体を200メツシユのふるい
で分割し、粒径2〜10μmの球状複合粉体を得た。
Table 1 Degree of odor after 2 weeks at 50°C Example 3 Comparative example 2 where almost no odor is felt
A significant sour odor was felt (hereinafter referred to as "Kinpaku"). Example 2 The spherical composite powder obtained in Example 1 was divided through a 200-mesh sieve to obtain spherical composite powder with a particle size of 2 to 10 μm.

比較例1 ラポナイ)XLG30部及び微粒子二酸化チタン(P−
25iデグサ社!!り 10部を十分に混合し、両者の
混合粉体を得た。
Comparative Example 1 30 parts of XLG (Laponai) and particulate titanium dioxide (P-
25i Degussa! ! 10 parts of the mixture were thoroughly mixed to obtain a mixed powder of both.

実施例2および比較例1で得た粉体の動摩擦係数を測定
し、表2の結果を得た。
The dynamic friction coefficients of the powders obtained in Example 2 and Comparative Example 1 were measured, and the results shown in Table 2 were obtained.

動摩擦係数の測定は、粉体摩擦試験機(粉体工学会誌v
o1.21.11h9.565頁、1984)を用い、
水平に設置した鉄板上に両面粘着テープを貼り付け、そ
の上に試料をのせた後、アルミニウム製のアタッチメン
トに荷重(5〜70g/cal)をかけて、アタッチメ
ントを左右に毎秒10酊の速度で移動させた時のズリ応
力をストレインゲージにより測定し、荷重とズリ応力の
関係から動摩擦係数を求めた。
The dynamic friction coefficient is measured using a powder friction tester (Journal of Powder Engineering Society v
o1.21.11h9.565 page, 1984),
After pasting double-sided adhesive tape on a horizontally installed iron plate and placing the sample on it, a load (5 to 70 g/cal) was applied to the aluminum attachment, and the attachment was moved from side to side at a speed of 10 seconds per second. The shear stress during movement was measured using a strain gauge, and the dynamic friction coefficient was determined from the relationship between the load and the shear stress.

表2 動摩擦係数 実施例2    0.32 比較例1    0.60 表2から判る様に、本発明の球状複合粉体は、比較例1
の単純な混合粉末に較べ、動摩擦係数の小さいすべりの
良い優れた球状複合粉体であることが判る。
Table 2 Coefficient of dynamic friction Example 2 0.32 Comparative example 1 0.60 As can be seen from Table 2, the spherical composite powder of the present invention
It can be seen that this is an excellent spherical composite powder with a small dynamic friction coefficient and good sliding properties compared to a simple mixed powder.

実施例3 水1 、000−にヘキサメタリン酸ソーダ0.25g
を溶解させ、さらに0.1μm以下でかつ平均粒径0.
04μmの微粒子亜鉛華8gをよく分散させる。
Example 3 0.25 g of sodium hexametaphosphate in 1,000- of water
is dissolved, and furthermore, the particle size is 0.1 μm or less and the average particle size is 0.
8 g of fine zinc white particles of 0.04 μm are well dispersed.

この分散液にスメクタイトSY(日本化薬社!!りを1
2g分散させゲルを調製する。このゲルを実施例1と同
様に噴霧乾燥することによりて微粒子亜鉛華40重量%
を含有する球状複合粉体15gが得られた。
Add 1 smectite SY (Nippon Kayaku Co., Ltd.) to this dispersion.
Disperse 2g to prepare a gel. By spray-drying this gel in the same manner as in Example 1, 40% by weight of fine zinc white particles were obtained.
15 g of spherical composite powder containing .

(以下°余白) この複合粉体は走査型電子顕微鏡やEDX測定より真球
状で亜鉛華が極めて均一に粉体中に分散していることが
確かめられた。
(Hereinafter referred to as "margin") It was confirmed by scanning electron microscopy and EDX measurement that this composite powder was perfectly spherical and that the zinc white was extremely uniformly dispersed in the powder.

実施例4 水1 、000−に0.1μm以下で平均粒径0.05
μmのハイドロキシアパタイト5gを分散させる。さら
にビーガム30gを分散させてゲルにした。このゲルを
実施例1と同様に噴霧乾燥することによってハイドロキ
シアパタイトを含有する球状複合粉体32gが得られた
Example 4 Water 1,000-0.1 μm or less and average particle size 0.05
Disperse 5 g of μm hydroxyapatite. Furthermore, 30 g of Veegum was dispersed to form a gel. By spray drying this gel in the same manner as in Example 1, 32 g of spherical composite powder containing hydroxyapatite was obtained.

この複合粉体は走査型電子顕微鏡やEDX測定より真球
状でハイドロキシアパタイトが極めて均一に粉体中に分
散していることが確かめられた。
It was confirmed by scanning electron microscopy and EDX measurement that this composite powder was perfectly spherical and that hydroxyapatite was extremely uniformly dispersed in the powder.

実施例5 水t 、 ooo−に0.1.um以下で平均粒径0.
08μmのポリアミド樹脂Logをよく分散させる。さ
らにクニビア30gを分散させゲル化させる。このゲル
を実施例1と同様に噴霧乾燥してポリアミド樹脂をがす
る球状粘土鉱物32gが得られた。
Example 5 Water t, ooo- to 0.1. um or less and the average particle size is 0.
08 μm polyamide resin Log is well dispersed. Furthermore, 30 g of Kunivia is dispersed and gelatinized. This gel was spray-dried in the same manner as in Example 1 to obtain 32 g of spherical clay mineral from which the polyamide resin was removed.

この複合粉体は走査型電子顕微鏡観察により真球状でポ
リアミド樹脂が極めて均一に粉体中に分散していること
が確かめられた。
It was confirmed by scanning electron microscopy that this composite powder had a true spherical shape and that the polyamide resin was extremely uniformly dispersed in the powder.

実施例6 水1 、000−に0.1.crm以下で平均粒i0.
olbrmのアルミニウム粉Logをよく分散させる。
Example 6 Water 1,000-0.1. Average grain i0. below crm.
Thoroughly disperse olbrm's aluminum powder Log.

さらにラポナイトXLGを30g分散させゲル化させる
Furthermore, 30g of Laponite XLG is dispersed and gelatinized.

このゲルを実施例1と同様に噴霧乾燥してアルミニウム
樹脂を含有する球状複合粉体32gが得られた。
This gel was spray-dried in the same manner as in Example 1 to obtain 32 g of spherical composite powder containing aluminum resin.

この複合粉体は走査型電子顕微鏡観察により真球状でア
ルミニウム粉が極めて均一に粉体中に分散していること
が確かめられた。
It was confirmed by scanning electron microscopy that this composite powder was perfectly spherical and the aluminum powder was extremely uniformly dispersed in the powder.

(以下余白)(Margin below)

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

図1は、実施例1で得られた微粒子二酸化チタンを25
重量%含有する本発明の球状複合粉体の結晶構造を示す
走査型電子顕微鏡写真、図2はヒマシ油中に分散させた
本発明の複合粉体(微粒子二酸化チタン含有)と同じく
ヒマシ油中に分散させた微粒子二酸化チタン単独の紫外
線吸光曲線を示す。
Figure 1 shows that the fine particle titanium dioxide obtained in Example 1 was
A scanning electron micrograph showing the crystal structure of the spherical composite powder of the present invention containing % by weight, Figure 2 shows the composite powder of the present invention (containing fine particle titanium dioxide) dispersed in castor oil. The ultraviolet absorption curve of dispersed fine particle titanium dioxide alone is shown.

Claims (2)

【特許請求の範囲】[Claims] (1)水膨潤性粘土鉱物よりなる粉体中に、有機、無機
又は金属粉体の1種もしくは2種以上を含有することを
特徴とする複合粉体。
(1) A composite powder characterized by containing one or more types of organic, inorganic, or metal powder in the powder made of water-swellable clay mineral.
(2)有機、無機又は金属粉体の1種もしくは2種以上
と水膨潤性粘土鉱物の水性分散液とを噴霧乾燥すること
を特徴とする、水膨潤性粘土鉱物よりなる粉体中に有機
、無機又は金属粉体の1種もしくは2種以上を含有して
なる複合粉体の製造法。
(2) A powder made of a water-swellable clay mineral, characterized by spray-drying one or more of organic, inorganic or metal powders and an aqueous dispersion of a water-swellable clay mineral. , a method for producing a composite powder containing one or more types of inorganic or metal powder.
JP61174578A 1986-07-24 1986-07-24 Composite powder and its manufacturing method Expired - Lifetime JPH0696447B2 (en)

Priority Applications (5)

Application Number Priority Date Filing Date Title
JP61174578A JPH0696447B2 (en) 1986-07-24 1986-07-24 Composite powder and its manufacturing method
PCT/JP1987/000540 WO1988000572A1 (en) 1986-07-24 1987-07-24 Spherical clay mineral powder, process for its production, and composition containing same
EP87904938A EP0277244B1 (en) 1986-07-24 1987-07-24 Spherical clay mineral powder, process for its production, and composition containing same
DE3750576T DE3750576T2 (en) 1986-07-24 1987-07-24 SPHERICAL SMALL POWDER, METHOD FOR THE PRODUCTION AND COMPOSITION THAT CONTAINS THIS.
US07/538,595 US5165915A (en) 1986-07-24 1990-06-14 Spherical clay mineral powder, process for production thereof and composition containing the same

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP61174578A JPH0696447B2 (en) 1986-07-24 1986-07-24 Composite powder and its manufacturing method

Publications (2)

Publication Number Publication Date
JPS6330313A true JPS6330313A (en) 1988-02-09
JPH0696447B2 JPH0696447B2 (en) 1994-11-30

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ID=15981005

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Country Status (1)

Country Link
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991005736A1 (en) * 1989-10-19 1991-05-02 Shiseido Company, Ltd. Hydrophilic polymer-silicate mineral composite and its use
JPH06157264A (en) * 1992-11-12 1994-06-03 Kanebo Ltd Skin cosmetic
JP2007518845A (en) * 2003-12-16 2007-07-12 ソルヴェイ Method for producing composite material, composite material and use thereof
JP2009035536A (en) * 2007-07-06 2009-02-19 Kenji Nakamura Crystalline complex powder and method for producing the same
JP2014148486A (en) * 2013-02-04 2014-08-21 Daito Kasei Kogyo Kk Spherical composite powder, production method of the spherical composite powder, and cosmetic containing the spherical composite powder
JP2015151357A (en) * 2014-02-13 2015-08-24 日本メナード化粧品株式会社 composite powder

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5647477A (en) * 1979-09-17 1981-04-30 Rohm & Haas Thicking composition for aqueous composition
JPS5677208A (en) * 1979-11-29 1981-06-25 Takeda Chem Ind Ltd Stabilized solid agricultural chemical composition
JPS6054914A (en) * 1983-09-05 1985-03-29 Miyoshi Kasei:Kk Production of microspherical silica gel
JPS60200822A (en) * 1984-03-27 1985-10-11 Agency Of Ind Science & Technol Microporous clayey material consisting of smectite type mineral, neutral polymer and silica and its production
JPS616119A (en) * 1984-06-21 1986-01-11 Kunimine Kogyo Kk Highly swellable inorganic granule

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5647477A (en) * 1979-09-17 1981-04-30 Rohm & Haas Thicking composition for aqueous composition
JPS5677208A (en) * 1979-11-29 1981-06-25 Takeda Chem Ind Ltd Stabilized solid agricultural chemical composition
JPS6054914A (en) * 1983-09-05 1985-03-29 Miyoshi Kasei:Kk Production of microspherical silica gel
JPS60200822A (en) * 1984-03-27 1985-10-11 Agency Of Ind Science & Technol Microporous clayey material consisting of smectite type mineral, neutral polymer and silica and its production
JPS616119A (en) * 1984-06-21 1986-01-11 Kunimine Kogyo Kk Highly swellable inorganic granule

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1991005736A1 (en) * 1989-10-19 1991-05-02 Shiseido Company, Ltd. Hydrophilic polymer-silicate mineral composite and its use
JPH06157264A (en) * 1992-11-12 1994-06-03 Kanebo Ltd Skin cosmetic
JP2007518845A (en) * 2003-12-16 2007-07-12 ソルヴェイ Method for producing composite material, composite material and use thereof
JP2009035536A (en) * 2007-07-06 2009-02-19 Kenji Nakamura Crystalline complex powder and method for producing the same
JP2014148486A (en) * 2013-02-04 2014-08-21 Daito Kasei Kogyo Kk Spherical composite powder, production method of the spherical composite powder, and cosmetic containing the spherical composite powder
JP2015151357A (en) * 2014-02-13 2015-08-24 日本メナード化粧品株式会社 composite powder

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