JP3020408B2 - High concentration titanium dioxide aqueous dispersion - Google Patents
High concentration titanium dioxide aqueous dispersionInfo
- Publication number
- JP3020408B2 JP3020408B2 JP6071365A JP7136594A JP3020408B2 JP 3020408 B2 JP3020408 B2 JP 3020408B2 JP 6071365 A JP6071365 A JP 6071365A JP 7136594 A JP7136594 A JP 7136594A JP 3020408 B2 JP3020408 B2 JP 3020408B2
- Authority
- JP
- Japan
- Prior art keywords
- titanium dioxide
- aqueous dispersion
- ultrafine
- aqueous
- weight
- 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
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- Cosmetics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Paints Or Removers (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、超微粒子二酸化チタン
の高濃度水性分散体およびその用途に関する。The present invention relates to a high-concentration aqueous dispersion of ultrafine titanium dioxide and its use.
【０００２】[0002]
【従来の技術】超微粒子二酸化チタンは、透明性の高い
紫外線遮蔽剤として、塗料、化粧品、化学繊維に利用さ
れている。しかし、一般に、超微粒子二酸化チタンは、
一次粒子径が、０．１μｍ以下と非常に小さいため、凝
集した粗大粒子となっているものが多く、本来の紫外線
遮蔽能、可視部透明性が十分に発揮されていないことが
多い。このような問題を改善するために、例えば特開平
２−２１２３１５公報には、水、針状二酸化チタン粒
子、及びポリカルボン酸又はその塩である分散剤からな
る二酸化チタン水性分散体が提案されている。しかしな
がら、前記水性分散体は、実質的な二酸化チタン含有率
を重量基準で５０％以上にしようとすると、高粘度にな
り、取扱いが非常に困難となるため、二酸化チタン含有
量を５０％未満にせざるを得ない。2. Description of the Related Art Ultrafine titanium dioxide is used as a highly transparent ultraviolet shielding agent in paints, cosmetics, and chemical fibers. However, in general, ultrafine titanium dioxide is
Since the primary particle diameter is as small as 0.1 μm or less, many of the particles are aggregated and coarse particles, and the original ultraviolet shielding ability and visible part transparency are often not sufficiently exhibited. In order to improve such a problem, for example, JP-A-2-212315 proposes an aqueous titanium dioxide dispersion comprising water, acicular titanium dioxide particles, and a dispersant which is a polycarboxylic acid or a salt thereof. I have. However, if the aqueous dispersion is intended to have a substantial titanium dioxide content of 50% or more on a weight basis, it becomes highly viscous and very difficult to handle, so that the titanium dioxide content is reduced to less than 50%. I have no choice.
【０００３】[0003]
【発明が解決しようとする課題】一般に、原材料に含ま
れる有効成分の含有率が低いほど、最終製品への添加量
が制限されると共に、有効成分当たりの輸送コストが大
きくなる。従って、二酸化チタン水性分散体において
も、有効成分である二酸化チタンの含有率はできるだけ
高いほうが望ましい。本願発明は、超微粒子二酸化チタ
ン粒子が高度に分散され、かつ高濃度で含まれる二酸化
チタン水性分散体を提供することにある。In general, the lower the content of the active ingredient in the raw material, the more the amount added to the final product is limited, and the higher the transport cost per active ingredient. Therefore, it is desirable that the content of titanium dioxide, which is an active ingredient, be as high as possible in the titanium dioxide aqueous dispersion. An object of the present invention is to provide an aqueous titanium dioxide dispersion in which ultrafine titanium dioxide particles are highly dispersed and contained at a high concentration.
【０００４】[0004]
【課題を解決するための手段】本発明者らは、超微粒子
二酸化チタン粒子が高度によく分散し、かつ高濃度で含
まれる二酸化チタン水性分散体を得るべく種々検討し
た。その結果、縮合リン酸塩を分散剤として使用するこ
とで、実質的に超微粒子二酸化チタンを５０％以上含有
する水性分散体が得られ、このものは、超微粒子二酸化
チタンの優れた可視光透明性や紫外線遮蔽性能を、用途
適用系で十分発揮し得るとともに、当該配合調製作業の
効率化、工程簡略化、安全性などを一層好ましいものと
することの知見を得、本発明を完成したものである。Means for Solving the Problems The present inventors have made various studies to obtain an aqueous dispersion of titanium dioxide in which ultrafine titanium dioxide particles are highly dispersed and contained at a high concentration. As a result, by using the condensed phosphate as a dispersant, an aqueous dispersion substantially containing 50% or more of ultrafine titanium dioxide can be obtained. The present invention has been completed, with the knowledge that the properties and ultraviolet shielding performance can be sufficiently exhibited in the application system, and that the efficiency of the compounding preparation work, the process simplification, the safety, etc. are made more preferable. It is.
【０００５】すなわち、本発明は、 １．分散媒としての水、超微粒子二酸化チタンおよび縮
合リン酸塩を含んでなる高濃度二酸化チタン水性分散
体。 ２．超微粒子二酸化チタンを、５０〜７０重量％含有し
てなる前記１の高濃度二酸化チタン水性分散体。 ３．縮合リン酸塩が、超微粒子二酸化チタンの重量基準
で０．５〜５％である前記１の高濃度二酸化チタン水性
分散体。 ４．超微粒子二酸化チタンが、平均粒子径１０〜１００
ｎｍである前記１の高濃度二酸化チタン水性分散体。 ５．超微粒子二酸化チタンがアルミニウム、珪素、ジル
コニウム、チタン、亜鉛およびスズの少なくとも１種の
酸化物または含水酸化物で被覆されている前記１の高濃
度二酸化チタン水性分散体。 ６．縮合リン酸塩が、ヘキサメタリン酸ナトリウム、テ
トラポリリン酸ナトリウム、トリポリリン酸ナトリウム
およびピロリン酸ナトリウムの少なくとも１種である前
記１の高濃度二酸化チタン水性分散体。 ７．前記１〜６いずれか記載の高濃度二酸化チタン水性
分散体を使用した紫外線遮蔽性化粧料。 ８．前記１〜６いずれか記載の高濃度二酸化チタン水性
分散体を使用した紫外線遮蔽性医薬品。 ９．前記１〜６いずれか記載の高濃度二酸化チタン水性
分散体を使用した紫外線遮蔽性塗料。That is, the present invention provides: A high-concentration aqueous titanium dioxide dispersion comprising water as a dispersion medium, ultrafine titanium dioxide and a condensed phosphate. 2. The high-concentration titanium dioxide aqueous dispersion according to 1 above, which contains 50 to 70% by weight of ultrafine titanium dioxide. 3. The high-concentration titanium dioxide aqueous dispersion according to 1 above, wherein the condensed phosphate is 0.5 to 5% by weight based on the weight of the ultrafine titanium dioxide. 4. Ultrafine titanium dioxide has an average particle size of 10 to 100
The high-concentration titanium dioxide aqueous dispersion according to 1 above, which has a nm. 5. The high-concentration titanium dioxide aqueous dispersion according to 1, wherein the ultrafine titanium dioxide is coated with at least one oxide or hydrated oxide of aluminum, silicon, zirconium, titanium, zinc and tin. 6. The high-concentration titanium dioxide aqueous dispersion according to 1, wherein the condensed phosphate is at least one of sodium hexametaphosphate, sodium tetrapolyphosphate, sodium tripolyphosphate and sodium pyrophosphate. 7. 7. An ultraviolet shielding cosmetic using the high-concentration titanium dioxide aqueous dispersion according to any one of the above 1 to 6. 8. 7. An ultraviolet ray shielding drug using the high-concentration titanium dioxide aqueous dispersion according to any one of 1 to 6 above. 9. 7. An ultraviolet shielding paint using the high-concentration titanium dioxide aqueous dispersion according to any one of 1 to 6 above.
【０００６】本発明において使用する超微粒子二酸化チ
タンは、種々の方法によって製造し得るが、例えば四塩
化チタン水溶液をアルカリで中和加水分解し、得られた
含水二酸化チタンを焼成するか、あるいは含水二酸化チ
タンを水酸化ナトリウムで加熱処理し、得られた反応生
成物を酸で加熱熟成して得ることができる。このもの
は、さらに必要に応じて焼成して粒子径や粒子形状の調
整、さらに耐候性の向上をはかってもよい。また硫酸チ
タン水溶液や四塩化チタン水溶液を加熱加水分解して得
られた含水二酸化チタンを酸で解膠処理したものや、こ
のものをさらに焼成したものであってもよい。さらに超
微粒子二酸化チタンは、親和性や耐光性の向上をはかる
べく、例えばアルミニウム、珪素、ジルコニウム、チタ
ン、亜鉛およびスズの少なくとも１種の酸化物または含
水酸化物で被覆してもよい。The ultrafine titanium dioxide used in the present invention can be produced by various methods. For example, an aqueous titanium tetrachloride solution is neutralized and hydrolyzed with an alkali, and the obtained hydrous titanium dioxide is calcined or hydrous titanium dioxide is obtained. The titanium dioxide can be heat-treated with sodium hydroxide, and the resulting reaction product can be obtained by heat aging with an acid. This may be further baked, if necessary, to adjust the particle diameter and particle shape, and to further improve the weather resistance. Further, a hydrous titanium dioxide solution obtained by heating and hydrolyzing a titanium sulfate aqueous solution or a titanium tetrachloride aqueous solution may be peptized with an acid, or may be further calcined. Further, the ultrafine titanium dioxide may be coated with at least one oxide or hydrated oxide of, for example, aluminum, silicon, zirconium, titanium, zinc and tin in order to improve affinity and light resistance.
【０００７】二酸化チタン水性分散体における超微粒子
二酸化チタンの含有率は、種々の用途適用系での配合調
製時の添加量の自由度、輸送コスト等の面より、できる
だけ高いほうが望ましい。本発明の二酸化チタン水性分
散体は、縮合リン酸塩の存在下で分散することにより、
実質的に超微粒子二酸化チタンを５０重量％以上含有さ
せることができる。しかしながら、７０重量％を超える
ようなあまりに高濃度にしようとすると、粘度が高くな
ったり、流動性を失ったりして、取扱が困難になり易
い。The content of the ultrafine titanium dioxide in the aqueous titanium dioxide dispersion is preferably as high as possible from the viewpoints of the degree of freedom of the amount added at the time of blending and preparation in various applications and the transportation cost. The aqueous titanium dioxide dispersion of the present invention is dispersed in the presence of a condensed phosphate,
Substantially 50% by weight or more of ultrafine titanium dioxide can be contained. However, if the concentration is excessively high, such as exceeding 70% by weight, the viscosity tends to be high, the fluidity is lost, and the handling tends to be difficult.
【０００８】本発明において使用する縮合リン酸塩は、
種々のものを使用しうるが、例えばピロリン酸、トリポ
リリン酸、テトラポリリン酸、ヘキサメタリン酸等の縮
合リン酸のアルカリ金属塩である。縮合リン酸塩は、二
酸化チタンの重量基準で０．５〜５％、好ましくは１〜
１．２％配合することによって、分散性、粘度、安定性
等の点で良好な水性分散体が得られる。概ね、二酸化チ
タンの比表面積が大きいほど、また、表面被覆剤の量が
多いほど、縮合リン酸塩の最適配合量は多くなる。ま
た、超微粒子二酸化チタンの製法、表面被覆剤の種類に
よっても縮合リン酸塩の最適配合量は異なってくる。縮
合リン酸塩は、１種のものに限定する必要はなく、２種
以上のものを組み合わせて使用してもよい。The condensed phosphate used in the present invention is:
Various types can be used, and examples thereof include alkali metal salts of condensed phosphoric acid such as pyrophosphoric acid, tripolyphosphoric acid, tetrapolyphosphoric acid, and hexametaphosphoric acid. The condensed phosphate is 0.5 to 5% by weight of titanium dioxide, preferably 1 to 5%.
By adding 1.2%, an aqueous dispersion excellent in dispersibility, viscosity, stability and the like can be obtained. Generally, the larger the specific surface area of titanium dioxide and the larger the amount of the surface coating agent, the larger the optimal amount of the condensed phosphate. The optimum amount of the condensed phosphate varies depending on the production method of the ultrafine titanium dioxide and the type of the surface coating agent. The condensed phosphate need not be limited to one kind, and two or more kinds may be used in combination.
【０００９】本発明の二酸化チタン水性分散体には、必
要に応じて防腐剤、例えばアルキルパラベン等を添加す
ることができる。A preservative, for example, an alkyl paraben can be added to the aqueous titanium dioxide dispersion of the present invention, if necessary.
【００１０】次に、本発明の二酸化チタン水性分散体の
製造方法の製造方法について述べる。本発明の二酸化チ
タン水性分散体は、縮合リン酸塩、水性媒液及び超微粒
子二酸化チタンを、種々の方法によって分散させること
によって得られるが、例えば羽根型攪拌機、ディスパ
−、ホモミキサ−等を用いて予備混合したのち、サンド
ミル、ペブルミル、ディスクミル等の粉砕機を用いて、
超微粒子二酸化チタンを分散せしめることによって調製
することができる。前記において、予備混合法として
は、先ず水性媒液に分散剤を溶解し、次いで超微粒子二
酸化チタンを投入、混合する方法、あるいは、予め分散
剤粉末と超微粒子二酸化チタン粉末を乾式混合し、これ
を水性媒液に投入、混合するする方法を適宜選択でき
る。また、超微粒子二酸化チタンは、その製造工程途中
の仕上げ乾燥前のケ−キを使用してもよい。この場合、
乾燥による強い凝集を避けることができ、分散体製造時
の粉砕工程を簡略化できる。前記の超微粒子二酸化チタ
ンの分散に際しては、粉砕機の種類、粉砕メディアの選
定、最適粉砕条件の設定が、高度な分散体を調製する上
で重要である。例えば縦型、横型のサンドミルで直径
０．５ｍｍのジルコニアビ−ズを用いて粉砕するのが望
ましい。Next, a method for producing the aqueous titanium dioxide dispersion of the present invention will be described. The aqueous titanium dioxide dispersion of the present invention can be obtained by dispersing a condensed phosphate, an aqueous medium and ultrafine titanium dioxide by various methods, for example, using a blade-type stirrer, a disperser, a homomixer, or the like. After pre-mixing, using a crusher such as a sand mill, pebble mill, and disc mill,
It can be prepared by dispersing ultrafine titanium dioxide. In the above, as a premixing method, a method in which a dispersant is first dissolved in an aqueous medium and then ultrafine titanium dioxide is charged and mixed, or a method in which a dispersant powder and an ultrafine titanium dioxide powder are dry-mixed in advance, Can be appropriately selected by adding and mixing into the aqueous medium. The ultrafine titanium dioxide may be a cake before finishing and drying in the course of the production process. in this case,
Strong agglomeration due to drying can be avoided, and the pulverization step during dispersion production can be simplified. In dispersing the ultrafine titanium dioxide, the type of crusher, the selection of crushing media, and the setting of optimum crushing conditions are important for preparing a high-dispersion dispersion. For example, it is desirable to grind with a vertical or horizontal sand mill using zirconia beads having a diameter of 0.5 mm.
【００１１】このようにして得られた高濃度超微粒子二
酸化チタン水性分散体は、超微粒子二酸化チタンを高い
濃度で含有するため、従来の超微粒子二酸化チタン水性
分散体に比べて、輸送コストを大幅に節減できる上に、
塗料、化粧料といった用途適用系での添加量範囲を拡大
し易い。[0011] The high-concentration ultrafine titanium dioxide aqueous dispersion thus obtained contains a high concentration of ultrafine titanium dioxide, so that the transportation cost is significantly higher than that of the conventional ultrafine titanium dioxide aqueous dispersion. In addition to saving money
It is easy to expand the range of the amount added in the application system such as paints and cosmetics.
【００１２】本発明の二酸化チタン水性分散体は、超微
粒子二酸化チタンを高濃度に含有しかつ優れた分散安定
性を有するものであり、透明性の高い紫外線遮蔽剤とし
て塗料、繊維、化粧品などに、広くかつ有効に利用可能
な材料である。本発明の高濃度超微粒子二酸化チタン水
性分散体を日焼け止め化粧料として利用する場合には、
例えば油性成分、保湿剤、界面活性剤、顔料、香料、防
腐剤、水、アルコ−ル類、増粘剤等と配合し、ロ−ショ
ン状、クリ−ム状、ペ−スト状、スティック状、乳液状
など、各種の形態で用いることができる。The aqueous titanium dioxide dispersion of the present invention contains ultra-fine titanium dioxide in a high concentration and has excellent dispersion stability, and is used as a highly transparent ultraviolet shielding agent for paints, fibers, cosmetics, and the like. Is a widely and effectively usable material. When using the high-concentration ultrafine titanium dioxide aqueous dispersion of the present invention as a sunscreen cosmetic,
For example, blended with oily components, humectants, surfactants, pigments, fragrances, preservatives, water, alcohols, thickeners, etc. to give lotions, creams, pastes, sticks , Milky liquid and the like can be used in various forms.
【００１３】紫外線防止用塗料として利用するには、例
えばポリビニルアルコ−ル樹脂、塩ビ−酢ビ樹脂、アク
リル樹脂、エポキシ樹脂、ウレタン樹脂、アルキッド樹
脂、ポリエステル樹脂、エチレン酢酸ビニル共重合体、
アクリル−スチレン共重合体、繊維素樹脂、フェノ−ル
樹脂、アミノ樹脂などに配合され、水性溶媒中で分散さ
れる。For use as an ultraviolet ray preventing paint, for example, polyvinyl alcohol resin, vinyl chloride-vinyl acetate resin, acrylic resin, epoxy resin, urethane resin, alkyd resin, polyester resin, ethylene vinyl acetate copolymer,
It is mixed with an acryl-styrene copolymer, a cellulose resin, a phenol resin, an amino resin and the like, and dispersed in an aqueous solvent.
【００１４】[0014]
実施例１ 四塩化チタン水溶液（ＴｉＯ2 ２００ｇ／ｌ）を室温に
保持しながら、水酸化ナトリウム水溶液で中和してコロ
イド状の非晶質水酸化チタンを析出させ、その後熟成し
てルチル型の微小チタニアゾルを得た。このゾルを濾
過、洗浄した後６００℃で３時間焼成し、流体エネルギ
−ミルで粉砕して平均粒子径４０ｎｍの超微粒子二酸化
チタン粉末を得た。この超微粒子二酸化チタン粉末60重
量部とピロリン酸ナトリウム０．４重量部を乳鉢で混合
した後、精製水３９．６重量部に投入し、ディスパ−で
混合した。次に、これを直径０．５ｍｍのジルコンビ−
ズを粉砕メディアとして用い、サンドミルで粉砕したと
ころ、ｐＨ８．２の水性分散体（Ａ）を得た。Example 1 While maintaining an aqueous solution of titanium tetrachloride (TiO 2 200 g / l) at room temperature, neutralization was performed with an aqueous solution of sodium hydroxide to precipitate colloidal amorphous titanium hydroxide. A fine titania sol was obtained. This sol was filtered, washed, calcined at 600 ° C. for 3 hours, and pulverized by a fluid energy mill to obtain ultrafine titanium dioxide powder having an average particle diameter of 40 nm. 60 parts by weight of this ultrafine titanium dioxide powder and 0.4 parts by weight of sodium pyrophosphate were mixed in a mortar, then added to 39.6 parts by weight of purified water, and mixed by a disper. Next, this was mixed with a 0.5 mm diameter zircon
The resulting mixture was pulverized with a sand mill using a pulverizing medium as a pulverizing medium, whereby an aqueous dispersion (A) having a pH of 8.2 was obtained.
【００１５】実施例２ 実施例１の超微粒子二酸化チタン粉末を水中に分散させ
てサンドミルで湿式粉砕して超微粒子二酸化チタンスラ
リ−（ＴｉＯ2 ２００ｇ／ｌ）とした。このスラリ−を
７０℃に加熱した後よく攪拌しながらアルミン酸ナトリ
ウムをＡｌ2 Ｏ3 としてＴｉＯ2 重量基準で２％添加
し、引き続き熟成してアルミニウムの水和酸化物を該二
酸化チタン粒子上に沈殿、被覆させた。その固形分を濾
過、洗浄し、洗浄ケ−キを乾燥した後ハンマ−タイプミ
ルで粉砕して超微粒子二酸化チタン粉末を得た。この超
微粒子二酸化チタン粉末６０重量部とヘキサメタリン酸
ナトリウム０．６重量部を乳鉢で混合した後、精製水３
９．４重量部に投入し、ディスパ−で混合した。次に、
これを直径０．５ｍｍのジルコンビ−ズを粉砕メディア
として用い、サンドミルで粉砕したところ、ｐＨ８．６
の水性分散体（Ｂ）を得た。Example 2 The ultrafine titanium dioxide powder of Example 1 was dispersed in water and wet-pulverized with a sand mill to obtain ultrafine titanium dioxide slurry (TiO 2 200 g / l). After heating this slurry to 70 ° C., 2% by weight of sodium aluminate as Al 2 O 3 was added as TiO 2 while stirring well, and then aging was performed to hydrate the aluminum hydrated oxide on the titanium dioxide particles. Precipitated and coated. The solid content was filtered and washed, and the washed cake was dried and pulverized with a hammer type mill to obtain ultrafine titanium dioxide powder. After mixing 60 parts by weight of this ultrafine titanium dioxide powder and 0.6 parts by weight of sodium hexametaphosphate in a mortar, purified water 3
The mixture was added to 9.4 parts by weight and mixed with a disper. next,
This was pulverized with a sand mill using zircon beads having a diameter of 0.5 mm as a pulverizing medium.
Thus, an aqueous dispersion (B) was obtained.
【００１６】比較例 実施例２の超微粒子二酸化チタンスラリ−（ＴｉＯ2 ２
００ｇ／ｌ）を７０℃に加熱した後よく攪拌しながらケ
イ酸ナトリウムをＳｉＯ2 としてＴｉＯ2 重量基準で４
％添加し、引き続き熟成してケイ素の水和酸化物を該二
酸化チタン粒子上に沈殿、被覆させた。さらに、このス
ラリ−をよく攪拌しながら、アルミン酸ナトリウムをAl
2O3 としてＴｉＯ2 重量基準で２％添加し、引き続き熟
成してアルミニウムの水和酸化物を該二酸化チタン粒子
上に沈殿、被覆させた。その固形分を濾過、洗浄し、洗
浄ケ−キを乾燥した後ハンマ−タイプミルで粉砕して超
微粒子二酸化チタン粉末を得た。この超微粒子二酸化チ
タン粉末４０重量部とカルボキシビニルポリマ−４重量
部を乳鉢で混合した後、精製水５６重量部に投入し、デ
ィスパ−で混合した。次に、これを直径０．５ｍｍのジ
ルコンビ−ズを粉砕メディアとして用い、サンドミルで
粉砕したところ、ｐＨ６．０の水性分散体（Ｃ）を得
た。Comparative Example The ultrafine titanium dioxide slurry of Example 2 (TiO 2 2
00g / l) 4 with TiO 2 by weight relative to the good stirring sodium silicate was heated to 70 ° C. as SiO 2
%, Followed by aging to precipitate and coat the hydrated oxide of silicon on the titanium dioxide particles. Further, while stirring the slurry well, the sodium aluminate was changed to Al.
2 % by weight of TiO 2 was added as 2 O 3 , followed by aging to precipitate and coat a hydrated oxide of aluminum on the titanium dioxide particles. The solid content was filtered and washed, and the washed cake was dried and pulverized with a hammer type mill to obtain ultrafine titanium dioxide powder. After mixing 40 parts by weight of the ultrafine titanium dioxide powder and 4 parts by weight of carboxyvinyl polymer in a mortar, the mixture was added to 56 parts by weight of purified water and mixed by a disper. Next, this was pulverized with a sand mill using zircon beads having a diameter of 0.5 mm as a pulverization medium, to obtain an aqueous dispersion (C) having a pH of 6.0.
【００１７】試験例１ 超微粒子二酸化チタン水性分散体の粘度を、円錐平板型
回転粘度計を用いて測定した。Test Example 1 The viscosity of the ultrafine titanium dioxide aqueous dispersion was measured using a conical flat plate type rotational viscometer.
【００１８】試験例２ 超微粒子二酸化チタン水性分散体を下記の処方で配合し
て日焼け止めクリ−ム（Ｏ／Ｗエマルジョン）を得た。 （１）ステアリン酸 ３．５重量部 （２）サラシミツロウ ５．０重量部 （３）セタノ−ル ５．０重量部 （４）スクワラン ２０．０重量部 （５）モノステアリン酸グリセリン ３．５重量部 （６）ポリオキシエチレンソルビタンモノステアレ−ト ２．５重量部 （７）超微粒子二酸化チタン水性分散体 ＴｉＯ2 として６．０重量部 （８）メチルパラベン ０．１重量部 （９）グリセリン １７．０重量部 （１０）トリエタノ−ルアミン １．５重量部 （１１）精製水 残部 （１２）香料 ０．３重量部 成分（１）〜（７）を８０℃で加熱混合したものを、成
分（８）〜（11）を８０℃で加熱混合したものに加え、
ホモミキサ−でよく混合し、強く攪拌する。４５℃付近
で（１２）を添加し日焼け止めクリ−ムを調製した。Test Example 2 An ultrafine titanium dioxide aqueous dispersion was blended according to the following formulation to obtain a sunscreen (O / W emulsion). (1) 3.5 parts by weight of stearic acid (2) 5.0 parts by weight of beeswax (3) 5.0 parts by weight of setanol (4) 20.0 parts by weight of squalane (5) Glycerin monostearate 3.5 (6) Polyoxyethylene sorbitan monostearate 2.5 parts by weight (7) Ultrafine titanium dioxide aqueous dispersion 6.0 parts by weight as TiO 2 (8) Methyl paraben 0.1 parts by weight (9) Glycerin 17.0 parts by weight (10) 1.5 parts by weight of triethanolamine (11) Remaining purified water (12) 0.3 parts by weight of fragrance Components obtained by heating and mixing components (1) to (7) at 80 ° C. (8) to (11) were added to the mixture obtained by heating and mixing at 80 ° C.,
Mix well with a homomixer and stir vigorously. At around 45 ° C., (12) was added to prepare a sunscreen cream.
【００１９】評価方法 上記クリ−ムを石英ガラス板上に１２μｍとなるように
塗布し、分光光度計にて７５０〜３００ｎｍの透過率を
測定した。以上の試験・評価結果を表１に示した。Evaluation method The above cream was applied on a quartz glass plate so as to have a thickness of 12 μm, and the transmittance at 750 to 300 nm was measured with a spectrophotometer. Table 1 shows the above test and evaluation results.
【００２０】[0020]
【表１】 [Table 1]
【００２１】[0021]
【発明の効果】本発明の超微粒子二酸化チタン水性分散
体は、超微粒子二酸化チタン濃度を５０重量％以上の高
濃度においても粘度を低く抑えることができるものであ
り、紫外線遮蔽剤として塗料、化粧料といった用途適
用系へ添加する際の添加量の制限が緩和される、二酸
化チタンあたりの輸送コストが安くなり、経済的に有利
であるなど、優れた効果を発現する。The aqueous dispersion of ultrafine titanium dioxide of the present invention can reduce the viscosity even at a high concentration of ultrafine titanium dioxide of 50% by weight or more. In addition, the present invention has excellent effects, such as less restrictions on the amount of addition to the application system such as feedstock, lower transport costs per titanium dioxide, and is economically advantageous.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 昭60−175530（ＪＰ，Ａ) 特開 昭60−1268（ＪＰ，Ａ) 特開 平８−59241（ＪＰ，Ａ) 特開 平２−212315（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C01G 23/047 C09D 5/32 ＣＡ（ＳＴＮ)──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-60-175530 (JP, A) JP-A-60-1268 (JP, A) JP-A-8-59241 (JP, A) JP-A-2- 212315 (JP, A) (58) Field surveyed (Int. Cl. 7 , DB name) C01G 23/047 C09D 5/32 CA (STN)
Claims (4)
ン酸塩を粉砕機を用いて分散させて得られる 、分散媒と
しての水、平均粒子径１０〜１００ｎｍである超微粒子
二酸化チタンを５０〜７０重量％および縮合リン酸塩を
含んでなる高濃度二酸化チタン水性分散体。(1) water, ultrafine titanium dioxide and condensation resin;
The emissions salt dispersed using a pulverizer obtained high concentration comprising water as a dispersion medium, 50 to 70 wt% ultrafine titanium dioxide, which is the average particle diameter of 10~100nm and polyphosphate Aqueous dispersion of titanium dioxide.
の重量基準で０．５〜５％である請求項１記載の高濃度
二酸化チタン水性分散体。2. The high-concentration aqueous titanium dioxide dispersion according to claim 1, wherein the condensed phosphate is 0.5 to 5% by weight of the ultrafine titanium dioxide.
ム、珪素、ジルコニウム、チタン、亜鉛およびスズの少
なくとも１種の酸化物または含水酸化物で被覆されてい
る請求項１記載の高濃度二酸化チタン水性分散体。3. The high-concentration titanium dioxide aqueous dispersion according to claim 1, wherein the ultrafine titanium dioxide is coated with at least one oxide or hydrated oxide of aluminum, silicon, zirconium, titanium, zinc and tin. .
リウム、テトラポリリン酸ナトリウム、トリポリリン酸
ナトリウムおよびピロリン酸ナトリウムの少なくとも１
種である請求項１記載の高濃度二酸化チタン水性分散
体。4. The condensed phosphate is at least one of sodium hexametaphosphate, sodium tetrapolyphosphate, sodium tripolyphosphate and sodium pyrophosphate.
2. The high concentration aqueous titanium dioxide dispersion of claim 1 which is a seed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6071365A JP3020408B2 (en) | 1994-03-15 | 1994-03-15 | High concentration titanium dioxide aqueous dispersion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6071365A JP3020408B2 (en) | 1994-03-15 | 1994-03-15 | High concentration titanium dioxide aqueous dispersion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07257923A JPH07257923A (en) | 1995-10-09 |
| JP3020408B2 true JP3020408B2 (en) | 2000-03-15 |
Family
ID=13458410
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6071365A Expired - Lifetime JP3020408B2 (en) | 1994-03-15 | 1994-03-15 | High concentration titanium dioxide aqueous dispersion |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3020408B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660092B (en) * | 2008-08-27 | 2011-04-13 | 宝山钢铁股份有限公司 | High-strength high-tenacity Zr-B composite micro-alloyed steel and manufacturing method thereof |
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| JP2001220141A (en) * | 2000-02-03 | 2001-08-14 | Toho Titanium Co Ltd | Titanium oxide dispersion |
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| JP2002338245A (en) * | 2001-05-16 | 2002-11-27 | Tayca Corp | Dispersion with high concentration of particulate titanium oxide |
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| JP5257041B2 (en) * | 2008-12-11 | 2013-08-07 | Ｊｆｅスチール株式会社 | Method for analyzing Ti-based precipitates in steel welds |
| CN105143108A (en) | 2012-12-28 | 2015-12-09 | 精工爱普生株式会社 | Surface coated particles and use of same |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101660092B (en) * | 2008-08-27 | 2011-04-13 | 宝山钢铁股份有限公司 | High-strength high-tenacity Zr-B composite micro-alloyed steel and manufacturing method thereof |
| CN104190313A (en) * | 2014-06-06 | 2014-12-10 | 济南裕兴化工有限责任公司 | A cost-reducing wetting dispersant used for titanium dioxide |
| CN104190313B (en) * | 2014-06-06 | 2015-10-21 | 济南裕兴化工有限责任公司 | A kind of titanium dioxide wetting dispersing agent |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07257923A (en) | 1995-10-09 |
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