JP4523684B2 - Method for producing organic compound-treated titanium dioxide pigment - Google Patents
Method for producing organic compound-treated titanium dioxide pigment Download PDFInfo
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Description
【０００１】
【本発明の属する技術分野】
本発明は二酸化チタン顔料に優れた分散性を付与するため、有機化合物を工業的、経済的有利に二酸化チタン顔料に処理する技術に関する。
【０００２】
【従来の技術】
二酸化チタン顔料は白色度に優れ、隠ペイ性、着色力が高いので、白色顔料として塗料、インキ、プラスチックスなどの分野で広く使用されているが、近年製造工程の省力化や、製品の高外観化のため、分散性の優れた二酸化チタン顔料が求められている。二酸化チタン顔料に優れた分散性を付与する手段として二酸化チタン粒子表面を有機化合物の分散剤、または分散助剤で処理する技術が一般的に知られている。
【０００３】
有機化合物を処理した二酸化チタン顔料を製造する方法として、湿式で処理する方法、乾式で混合、処理する方法など各種が知られているが、湿式法では有機化合物が二酸化チタンに強く吸着、または固着する必要があり、使用できる有機化合物種が大きく限定される。
【０００４】
乾式法では上記のような問題が少なく、二酸化チタン顔料の仕上粉砕として乾式粉砕する際に有機化合物を粉砕機に添加すれば連続的に製造でき、さらに気流式粉砕機を用いれば、粉砕効率が優れているばかりでなく、混合性が良好なので二酸化チタン顔料を仕上粉砕すると同時にその粒子表面に有機化合物を均一に処理することができる。
【０００５】
乾式法で処理する場合、有機化合物が固体であれば二酸化チタンと均一に混合するには予め粉砕、整粒しておく必要があるので、水やアルコールなどの溶媒で溶解しておくことが一般的に行われている。また、有機化合物が液体であっても、二酸化チタンに処理する有機化合物の処理量は、二酸化チタン顔料に対して通常約１％以下と比較的微量であるので、高濃度の原液で添加すると添加速度の調整や、二酸化チタン顔料への歩留まり量の調節が困難であるので、溶媒で希釈しておくことも一般的である。
【０００６】
上記の添加方法では溶媒を最終的に除去する必要があるが、気流式粉砕機では粉砕機内部の温度を上げて有機化合物溶液を粉砕機内で気化、または霧化させているので、この熱によって溶媒を蒸発させ、除去することが可能となる。しかし、この方法では有機化合物溶液が粉砕機内に添加されると同時に急激に膨張するため、添加口近辺の材質を著しく磨耗させ、粉砕機の耐久性を損ねるばかりでなく、磨耗物が混入し製品を汚染する。また、粉砕機内で乱流が発生するので、製品を粉砕機からサイクロンなどの集塵機を用いて回収する際に、排気系から飛散する二酸化チタン顔料の量が多く収率が下がってしまう。収率の低下を防止するために粉砕媒気体の供給量を減らすこともできるが、粉砕効率が低下する。液体の有機化合物を原液で添加する場合でも、二酸化チタンに処理するには気流式粉砕機内部を加温して気化、または霧化させるので同様の問題が生じる。
【０００７】
【発明が解決しようとする問題点】
本発明では以上に述べた従来技術の問題点を克服し、分散性に優れた二酸化チタン顔料を工業的、経済的に有利に製造する方法を提供するためになされたものである。
【０００８】
本発明者らは鋭意研究を重ねた結果、液体の有機化合物、液体または固体の有機化合物を溶解または希釈した溶液、及びにそれらの分散液を予め気化、または霧化させた状態で加熱した粉砕媒気体と混合し、気流式粉砕機に供給すれば、粉砕機を磨耗させることなく、また十分な量の粉砕媒気体を供給しても収率を下げることなく、分散性が優れた有機化合物処理の二酸化チタン顔料を製造できるとの知見に基づき本発明を完成した。
【０００９】
すなわち、気流式粉砕機に二酸化チタン粗顔料と加熱した粉砕媒気体とを供給して二酸化チタン粗顔料を粉砕する方法において、予め該粉砕媒気体に液状の有機化合物を添加混合して混合気体とした後、該粉砕機に供給して二酸化チタン粗顔料を粉砕しながら該顔料粒子表面を該有機化合物で被覆処理することを特徴とする二酸化チタン顔料の製造方法である。
【発明実施の形態】
【００１０】
本発明では、液状の有機化合物を加熱した粉砕媒気体と接触させ、気化、または霧化し、粉砕媒気体との混合気体として気流式粉砕機に供給し、二酸化チタンを粉砕しながらその粒子表面に有機化合物を処理する。このようにして液状の有機化合物を予め気化、または霧化した状態で粉砕機に供給すると、前記の粉砕機の磨耗や、粉砕機内で乱流の発生による収率の低下といった問題が生じ難い。液状の有機化合物はスプレーなどで微細化して供給してもよいが、粉砕媒気体が粉砕機供給用の配管内で高い流速を与えられているなら、液状の有機化合物を該配管内に添加するだけで十分に気化または霧化される。
【００１１】
本発明で用いる液状の有機化合物には特に制限は無く、液体のものの原液、液体または固体のものを溶解または希釈した溶液、及びこれらの分散液などいずれの形態でも良い。溶解、または希釈に用いる溶媒は水、またはアルコールなどの有機溶剤のいずれでもよいが、有機化合物が水に容易に溶解するものであれば、作業性や安全性の点で水が望ましい。また、分散液に用いる分散媒も特に制限は無いが、同様の理由で水が望ましい。疎水性を有する有機化合物はアルコールなどの水との相溶性を有する有機溶媒を少量加えて水溶液とすることもでき、少量の分散剤を用いるなどして水分散液として用いることもできる。有機化合物溶液、または分散液の濃度は添加作業が効率よく行える粘度になるように適宜調節する。
【００１２】
有機化合物種としてはトリメチロールエタン、トリメチロールプロパン、ペンタエリスリトールなどの多価アルコールや、トリエタノールアミンなどのアルカノールアミン、またはその誘導体、またはそれらの混合物や、シロキサン、シランカップリング剤などの有機シリコン系化合物、ステアリン酸などの高級脂肪酸など一般的に酸化チタン顔料に適用されるものであれば特に制限は無い。また、2種以上の有機化合物を混合液として用いることもできる。
【００１３】
本発明で用いる気流式粉砕機に特に制限はないが、ジェットミルのような旋回型が粉砕効率が良く、二酸化チタンと有機化合物との混合性も良いので特に好ましい。また、粉砕媒気体は経済性の点で乾燥空気や乾燥スチームが好ましい。本発明では有機化合物が粉砕機への添加前に十分に気化、または霧化していることが必要なので、粉砕媒気体を有機化合物の融点、または溶媒、または分散媒の沸点より少なくとも高い温度に加熱しなければならない。粉砕媒気体の加熱温度は用いる有機化合物種や、溶媒種、分散媒種によって異なるが、例えば有機化合物水溶液や水分散液の場合、１２０〜３００℃が好ましく、さらに好ましくは１２０〜２００℃である。
【００１４】
本発明で有機化合物を処理される二酸化チタンは、ルチル型結晶構造を有するものであっても、アナタ−ゼ型の結晶構造を有するものであっても、それらの混合物のいずれでもよい。また、硫酸法と呼ばれる硫酸チタンを液相で加水分解、焼成する方法で得られたものや、塩素法と呼ばれる四塩化チタンを気相酸化する方法で得られたものや、それらの混合物であっても良い。さらには、有機化合物を処理する前にアルミニウム、ケイ素、チタニウム、ジルコニウムなどの無機物の酸化物、または含水酸化物で被覆されていても良い。
【００１５】
【実施例】
次に実施例によって本発明をさらに説明するが、これらは本発明を限定するものではない。
実施例１
図1及び図２に示す旋回型気流式粉砕機を用い、粉砕媒気体としての高圧乾燥スチーム（ａ）を約３００℃に加熱して粉砕機の粉砕媒気体供給用配管（４）に供給し、該粉砕媒気体供給用配管（４）に設けた有機化合物溶液供給口（Ａ）よりトリメチロールエタン水溶液を添加し、二酸化チタン・ＣＲ―６０（石原産業（株）製塩素法小粒子径アルミナ処理品）を粉砕しながら、トリメチロールエタンをその粒子表面に処理して試料を調製した。
【００１６】
実施例２
二酸化チタンとしてＣＲ―５０（石原産業（株）製塩素法中粒子径アルミナ処理品）を用いた以外、実施例１と同様の方法で試料を調製した。
【００１７】
実施例３
二酸化チタンとしてＣＲ―５８（石原産業（株）製塩素法大粒子径アルミナ処理品）を用いた以外、実施例１と同様の方法で試料を調製した。
【００１８】
実施例４
二酸化チタンとしてＣＲ―９３（石原産業（株）製塩素法大粒子径アルミナ／シリカ処理品）を用いた以外、実施例１と同様の方法で試料を調製した。
【００１９】
比較例１
粉砕機上部プレート（１）に設けた有機化合物溶液供給口（Ｂ）よりトリメチロールエタン水溶液を添加した以外、実施例１と同様の方法で試料を調製した。
【００２０】
比較例２
二酸化チタンとしてＣＲ―５０を用いた以外、比較例１と同様の方法で試料を調製した。
【００２１】
比較例３
二酸化チタンとしてＣＲ―５８を用いた以外、比較例１と同様の方法で試料を調製した。
【００２２】
比較例４
二酸化チタンとしてＣＲ―９３を用いた以外、比較例１と同様の方法で試料を調製した。
【００２３】
評価１
実施例１〜４、及び比較例１〜4で得られた試料に固定された有機化合物の量を、高周波燃焼式有機物分析器（ＨＯＲＩＢＡ（株）製）を用いて炭素（Ｃ）の含有量として測定した。
【００２４】
評価２
実施例１〜４、及び比較例１〜4で得られた試料の収率を下式で求めた。
収率（％）＝（試料の総回収量÷粉砕前二酸化チタンの総供給量）×１００
【００２５】
評価３
実施例１〜４に示した方法を約１年間実施したが、粉砕機の上部プレート（１）には磨耗は認められなかった。しかし、比較例１〜４に示す方法で同様にしたところ、粉砕機の上部プレート（１）の、特に有機化合物溶液供給口（Ｂ）近辺が著しく磨耗していた。これらの実施例１〜４及び比較例１〜４に示した方法を実施した場合の粉砕機の上部プレート（１）の摩耗度について、摩耗が認められなかったものを○、著しく摩耗していたものを×と評価した。
【００２６】
評価１〜３の結果を表１に示す。
【００２７】
【表１】
【発明の効果】
本発明の製造方法では、液状の有機化合物を加熱した粉砕媒気体と接触させ、これと混合することで、予め気化、または霧化した状態で有機化合物溶液、または分散液が気流式粉砕機に供給されるので、粉砕機内で乱流の発生を抑制することができるため、粉砕機の材質を磨耗させること無く、工業的、経済的に有利に分散性の優れた有機化合物処理二酸化チタン顔料を提供することができる。
【図面の簡単な説明】
【図１】図１は本発明に用いる旋回式気流粉砕機の側面図を示す。
【図２】図２は本発明に用いる旋回式気流粉砕機の上部の平面図を示す。
【符号の説明】
（１）上部プレート
（２）下部プレート
（３）粉砕媒気体供給リング
（４）粉砕媒気体供給用配管
（５）粉砕媒気体供給口
（６）二酸化チタン供給用配管
（７）集塵機
（８）排気ダクト
（Ａ）実施例１〜４で用いた有機化合物溶液供給口
（Ｂ）比較例１〜４で用いた有機化合物溶液供給口
（ａ）粉砕媒気体（乾燥スチーム）
（ｂ）二酸化チタン（粉砕前）
（ｃ）有機化合物処理二酸化チタン顔料（製品）
（ｄ）排気ガス[0001]
[Technical field to which the present invention pertains]
The present invention relates to a technique for treating an organic compound into a titanium dioxide pigment industrially and economically in order to impart excellent dispersibility to the titanium dioxide pigment.
[0002]
[Prior art]
Titanium dioxide pigments have excellent whiteness, high concealment properties, and high coloring power, so they are widely used as white pigments in the fields of paints, inks, plastics, etc. A titanium dioxide pigment having excellent dispersibility is required for appearance. As a means for imparting excellent dispersibility to a titanium dioxide pigment, a technique of treating the surface of titanium dioxide particles with an organic compound dispersant or a dispersion aid is generally known.
[0003]
Various methods are known for producing a titanium dioxide pigment treated with an organic compound, such as a wet treatment method, a dry mixing method, and a treatment method. In the wet method, the organic compound strongly adsorbs or adheres to titanium dioxide. Therefore, the types of organic compounds that can be used are greatly limited.
[0004]
The dry method has few problems as described above, and can be continuously produced by adding an organic compound to the pulverizer when dry pulverizing the titanium dioxide pigment as a final pulverizer, and if an airflow pulverizer is used, the pulverization efficiency is improved. Not only is it excellent, but since the mixing property is good, the titanium dioxide pigment can be finished and pulverized and simultaneously the organic compound can be uniformly treated on the particle surface.
[0005]
When processing by the dry method, if the organic compound is a solid, it must be pulverized and sized in advance for uniform mixing with titanium dioxide, so it is generally dissolved in a solvent such as water or alcohol. Has been done. Even if the organic compound is liquid, the treatment amount of the organic compound to be treated with titanium dioxide is usually a relatively small amount of about 1% or less with respect to the titanium dioxide pigment. Since it is difficult to adjust the speed and the yield amount of the titanium dioxide pigment, it is generally diluted with a solvent.
[0006]
In the above addition method, it is necessary to finally remove the solvent. However, in the airflow type pulverizer, the temperature inside the pulverizer is raised to vaporize or atomize the organic compound solution in the pulverizer. The solvent can be evaporated and removed. However, in this method, the organic compound solution is rapidly expanded at the same time as it is added to the pulverizer, so that the material near the addition port is significantly worn, not only deteriorating the durability of the pulverizer, but also wear products mixed in the product. Contaminate. Further, since turbulent flow is generated in the pulverizer, when the product is recovered from the pulverizer using a dust collector such as a cyclone, the amount of titanium dioxide pigment scattered from the exhaust system is large and the yield is lowered. Although the supply amount of the grinding medium gas can be reduced in order to prevent the yield from being lowered, the grinding efficiency is lowered. Even when a liquid organic compound is added as a stock solution, the same problem arises because the inside of the airflow type pulverizer is heated and vaporized or atomized to treat titanium dioxide.
[0007]
[Problems to be solved by the invention]
The present invention has been made in order to overcome the problems of the prior art described above and to provide a method for producing a titanium dioxide pigment excellent in dispersibility in an industrially and economically advantageous manner.
[0008]
As a result of intensive research, the inventors of the present invention have pulverized a liquid organic compound, a solution in which a liquid or solid organic compound is dissolved or diluted, and a dispersion thereof heated in a vaporized or atomized state in advance. Organic compound with excellent dispersibility without mixing the grinding machine and reducing the yield even if a sufficient amount of grinding medium gas is supplied if it is mixed with the medium gas and supplied to the airflow type grinding machine The present invention has been completed based on the knowledge that a treated titanium dioxide pigment can be produced.
[0009]
That is, in a method of pulverizing titanium dioxide crude pigment by supplying titanium dioxide crude pigment and heated grinding medium gas to an airflow type pulverizer, a liquid organic compound is added to and mixed with the grinding medium gas in advance. Then, the pigment particle surface is coated with the organic compound while being supplied to the pulverizer and pulverizing the titanium dioxide crude pigment, thereby producing a titanium dioxide pigment.
DETAILED DESCRIPTION OF THE INVENTION
[0010]
In the present invention, a liquid organic compound is brought into contact with a heated pulverizing medium gas, vaporized or atomized, and supplied to an airflow type pulverizer as a mixed gas with the pulverizing medium gas. Treat organic compounds. When the liquid organic compound is supplied to the pulverizer in a vaporized or atomized state in this way, problems such as wear of the pulverizer and a decrease in yield due to generation of turbulent flow in the pulverizer hardly occur. The liquid organic compound may be finely supplied by spraying or the like, but if the pulverizing medium gas is given a high flow rate in the pulverizer supply pipe, the liquid organic compound is added to the pipe. Just fully vaporized or atomized.
[0011]
The liquid organic compound used in the present invention is not particularly limited, and may be any form such as a liquid stock solution, a solution obtained by dissolving or diluting a liquid or solid, and a dispersion thereof. The solvent used for dissolution or dilution may be either water or an organic solvent such as alcohol, but water is desirable from the viewpoint of workability and safety as long as the organic compound can be easily dissolved in water. The dispersion medium used for the dispersion is not particularly limited, but water is desirable for the same reason. The hydrophobic organic compound can be made into an aqueous solution by adding a small amount of an organic solvent having compatibility with water such as alcohol, and can also be used as an aqueous dispersion by using a small amount of a dispersant. The concentration of the organic compound solution or the dispersion is appropriately adjusted so that the viscosity can be efficiently added.
[0012]
Organic compound types include polyhydric alcohols such as trimethylolethane, trimethylolpropane, and pentaerythritol, alkanolamines such as triethanolamine, or derivatives thereof, and organic silicon such as siloxane and silane coupling agents. There is no particular limitation as long as it is generally applied to titanium oxide pigments, such as higher fatty acids such as system compounds and stearic acid. Two or more organic compounds can also be used as a mixed solution.
[0013]
Although there is no particular limitation on the air current pulverizer used in the present invention, good pivot type grinding efficiency as Jettomi Le particularly preferred because good also miscibility with titanium dioxide and an organic compound. The grinding medium gas is preferably dry air or dry steam from the viewpoint of economy. In the present invention, the organic compound needs to be sufficiently vaporized or atomized before being added to the pulverizer, so that the pulverizing medium gas is heated to a temperature at least higher than the melting point of the organic compound or the boiling point of the solvent or dispersion medium. Must. The heating temperature of the grinding medium gas varies depending on the organic compound species, the solvent species, and the dispersion medium species to be used. For example, in the case of an organic compound aqueous solution or an aqueous dispersion, 120 to 300 ° C is preferable, and 120 to 200 ° C is more preferable. .
[0014]
Titanium dioxide to be treated with an organic compound in the present invention may have a rutile crystal structure, an anatase crystal structure, or a mixture thereof. In addition, it is obtained by hydrolyzing and baking titanium sulfate called the sulfuric acid method in a liquid phase, obtained by a vapor phase oxidation method of titanium tetrachloride called the chlorine method, and a mixture thereof. May be. Furthermore, before processing an organic compound, you may coat | cover with inorganic oxides, such as aluminum, silicon, titanium, a zirconium, or a hydrous oxide.
[0015]
【Example】
The following examples further illustrate the present invention but are not intended to limit the invention.
Example 1
Using the swirl type airflow pulverizer shown in FIGS. 1 and 2, the high-pressure dry steam (a) as the pulverizing medium gas is heated to about 300 ° C. and supplied to the pulverizing medium gas supply pipe (4). The trimethylolethane aqueous solution was added from the organic compound solution supply port (A) provided in the grinding medium gas supply pipe (4), and titanium dioxide, CR-60 (Ishihara Sangyo Co., Ltd. chlorine method small particle size alumina) A sample was prepared by treating the particle surface with trimethylolethane while pulverizing the treated product.
[0016]
Example 2
A sample was prepared in the same manner as in Example 1 except that CR-50 (Ishihara Sangyo Co., Ltd., chlorine-treated medium particle size alumina treated product) was used as titanium dioxide.
[0017]
Example 3
A sample was prepared in the same manner as in Example 1 except that CR-58 (chlorine method large particle diameter alumina treated product manufactured by Ishihara Sangyo Co., Ltd.) was used as titanium dioxide.
[0018]
Example 4
A sample was prepared in the same manner as in Example 1 except that CR-93 (Ishihara Sangyo Co., Ltd. chlorine method large particle size alumina / silica treated product) was used as titanium dioxide.
[0019]
Comparative Example 1
A sample was prepared in the same manner as in Example 1 except that an aqueous trimethylolethane solution was added from the organic compound solution supply port (B) provided in the pulverizer upper plate (1).
[0020]
Comparative Example 2
A sample was prepared in the same manner as in Comparative Example 1 except that CR-50 was used as titanium dioxide.
[0021]
Comparative Example 3
A sample was prepared in the same manner as in Comparative Example 1 except that CR-58 was used as titanium dioxide.
[0022]
Comparative Example 4
A sample was prepared in the same manner as in Comparative Example 1 except that CR-93 was used as titanium dioxide.
[0023]
The amount of the organic compound fixed to the samples obtained in Examples 1 to 4 and Comparative Examples 1 to 4 was measured using a high-frequency combustion type organic substance analyzer (manufactured by HORIBA Ltd.). As measured.
[0024]
The yield of the sample obtained in Examples 1-4 and Comparative Examples 1-4 was calculated | required with the following Formula.
Yield (%) = (Total recovered amount of sample ÷ Total supply amount of titanium dioxide before pulverization) × 100
[0025]
Although the methods shown in Examples 1 to 4 were carried out for about 1 year, no abrasion was observed on the upper plate (1) of the grinder. However, when the same method as shown in Comparative Examples 1 to 4 was used, the upper plate (1) of the pulverizer, particularly the vicinity of the organic compound solution supply port (B), was significantly worn. As for the degree of wear of the upper plate (1) of the crusher when the methods shown in Examples 1 to 4 and Comparative Examples 1 to 4 were carried out, the case where no wear was observed was markedly worn. Things were rated as x.
[0026]
The results of
[0027]
[Table 1]
【The invention's effect】
In the production method of the present invention, a liquid organic compound is brought into contact with a heated pulverizing medium gas and mixed therewith, whereby the organic compound solution or the dispersion liquid is preliminarily vaporized or atomized into the airflow pulverizer. Since it is supplied, it is possible to suppress the occurrence of turbulent flow in the pulverizer, so that the organic compound-treated titanium dioxide pigment having excellent dispersibility can be produced industrially and economically without wearing the material of the pulverizer. Can be provided.
[Brief description of the drawings]
FIG. 1 shows a side view of a swirling airflow crusher used in the present invention.
FIG. 2 is a plan view of the upper part of a swirling airflow crusher used in the present invention.
[Explanation of symbols]
(1) Upper plate (2) Lower plate (3) Grinding medium gas supply ring (4) Grinding medium gas supply pipe (5) Grinding medium gas supply port (6) Titanium dioxide supply pipe (7) Dust collector (8) Exhaust duct (A) Organic compound solution supply port used in Examples 1-4 (B) Organic compound solution supply port used in Comparative Examples 1-4 (a) Grinding medium gas (dry steam)
(B) Titanium dioxide (before grinding)
(C) Organic compound-treated titanium dioxide pigment (product)
(D) Exhaust gas
Claims (13)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28312999A JP4523684B2 (en) | 1999-10-04 | 1999-10-04 | Method for producing organic compound-treated titanium dioxide pigment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP28312999A JP4523684B2 (en) | 1999-10-04 | 1999-10-04 | Method for producing organic compound-treated titanium dioxide pigment |
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| Publication Number | Publication Date |
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| JP2001106939A JP2001106939A (en) | 2001-04-17 |
| JP4523684B2 true JP4523684B2 (en) | 2010-08-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| JP28312999A Expired - Lifetime JP4523684B2 (en) | 1999-10-04 | 1999-10-04 | Method for producing organic compound-treated titanium dioxide pigment |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7144838B2 (en) | 2002-03-13 | 2006-12-05 | Ishihara Sangyo Kaisha, Ltd. | Process for production of titanium dioxide pigment and resin composition containing the pigment |
| DE10304849A1 (en) | 2003-02-06 | 2004-08-19 | Institut für Neue Materialien gemeinnützige Gesellschaft mit beschränkter Haftung | Chemomechanical production of functional colloids |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59117559A (en) * | 1982-12-16 | 1984-07-06 | タイオキサイド・グル−プ・ピ−エルシ− | Pigment |
| JPS6064647A (en) * | 1983-09-19 | 1985-04-13 | フロイント産業株式会社 | Coating method and apparatus |
| JPS6251609A (en) * | 1985-08-30 | 1987-03-06 | Miyoshi Kasei:Kk | Production of cosmetic |
| JPH0350120A (en) * | 1989-07-18 | 1991-03-04 | Ishihara Sangyo Kaisha Ltd | Production of titanium dioxide pigment powder |
-
1999
- 1999-10-04 JP JP28312999A patent/JP4523684B2/en not_active Expired - Lifetime
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59117559A (en) * | 1982-12-16 | 1984-07-06 | タイオキサイド・グル−プ・ピ−エルシ− | Pigment |
| JPS6064647A (en) * | 1983-09-19 | 1985-04-13 | フロイント産業株式会社 | Coating method and apparatus |
| JPS6251609A (en) * | 1985-08-30 | 1987-03-06 | Miyoshi Kasei:Kk | Production of cosmetic |
| JPH0350120A (en) * | 1989-07-18 | 1991-03-04 | Ishihara Sangyo Kaisha Ltd | Production of titanium dioxide pigment powder |
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| JP2001106939A (en) | 2001-04-17 |
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