JPS63223069A - Titanium dioxide coated iron pigment and production thereof - Google Patents
Titanium dioxide coated iron pigment and production thereofInfo
- Publication number
- JPS63223069A JPS63223069A JP5619387A JP5619387A JPS63223069A JP S63223069 A JPS63223069 A JP S63223069A JP 5619387 A JP5619387 A JP 5619387A JP 5619387 A JP5619387 A JP 5619387A JP S63223069 A JPS63223069 A JP S63223069A
- Authority
- JP
- Japan
- Prior art keywords
- titanium dioxide
- iron oxide
- rutile
- pigment
- titanium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 33
- 239000000049 pigment Substances 0.000 title claims abstract description 16
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title 2
- 229910052742 iron Inorganic materials 0.000 title 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000002245 particle Substances 0.000 claims abstract description 12
- 239000013078 crystal Substances 0.000 claims abstract description 10
- 150000003609 titanium compounds Chemical class 0.000 claims abstract description 10
- 230000007062 hydrolysis Effects 0.000 claims abstract description 7
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 7
- 239000001034 iron oxide pigment Substances 0.000 claims abstract description 5
- 239000011247 coating layer Substances 0.000 claims abstract description 4
- 239000010419 fine particle Substances 0.000 claims abstract description 3
- 150000003751 zinc Chemical class 0.000 claims abstract description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract 2
- 238000010304 firing Methods 0.000 claims description 5
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 239000000725 suspension Substances 0.000 claims description 4
- 230000009466 transformation Effects 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 150000001462 antimony Chemical class 0.000 claims description 2
- 239000007900 aqueous suspension Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229910003002 lithium salt Inorganic materials 0.000 claims description 2
- 159000000002 lithium salts Chemical class 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 7
- 230000007704 transition Effects 0.000 abstract description 6
- 239000011248 coating agent Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 2
- 238000001354 calcination Methods 0.000 abstract 2
- 239000006185 dispersion Substances 0.000 abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000002845 discoloration Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 239000003973 paint Substances 0.000 description 5
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 2
- 230000000007 visual effect Effects 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000004640 Melamine resin Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
Abstract
Description
【発明の詳細な説明】
、本ｊす几辺」Ｌｉ
本発明は、フレーク状の雲母状酸化鉄結晶粒子の表面を
ルチル型二酸化チタンで被覆してなる顔料に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a pigment formed by coating the surface of flaky mica-like iron oxide crystal particles with rutile-type titanium dioxide.
本出願人の特公昭５１−７１７６号には、フレーク状の
雲母状酸化鉄（Ｍ Ｉ Ｏ）の結晶粒子の表面を高屈折
率かつ透明性の全屈酸化物、特に二酸化チタンで被覆し
てなる顔料が記載されている。Japanese Patent Publication No. 51-7176 filed by the present applicant discloses a method in which the surface of flaky mica-like iron oxide (MIO) crystal particles is coated with a highly refractive index and transparent total oxide, especially titanium dioxide. The following pigments are described.
この顔料は被覆層による光の干渉現象によってもとのＭ
ＩＯには見られない美しい色調を有する。This pigment is restored to its original M color by the light interference phenomenon caused by the coating layer.
It has a beautiful color tone that is not seen in IO.
しかしながらこの先行技術に開示された条件では、二酸
化チタン被ｉＭＩｏ顔料の被覆二酸化チタンがアナター
ゼ型であるため、耐光性、耐候性が劣り、長期問屋外に
曝露された場合変色する欠点があった。However, under the conditions disclosed in this prior art, since the titanium dioxide coated in the titanium dioxide-coated iMIo pigment is anatase type, it has poor light resistance and weather resistance, and has the disadvantage of discoloration when exposed outdoors for a long period of time.
一般にルチル型二酸化チタンはアナターゼ型二酸化チタ
ンに比し、転移温度が高くおよび／または転移時間が長
いため、通常の条件でＭＩＯに沈着した含水二酸化チタ
ンをルチル型に転移せしめようとすると、ＭＩＯと二酸
化チタンの熱反応により干渉色が損われる。In general, rutile-type titanium dioxide has a higher transition temperature and/or a longer transition time than anatase-type titanium dioxide, so when attempting to transform hydrated titanium dioxide deposited on MIO to rutile type under normal conditions, MIO and The thermal reaction of titanium dioxide destroys the interference color.
そこで本発明者らは、干渉効果の損われないような条件
下においてルチル型へ転移させる方法について研究し、
被覆二酸化チタンの実質上大部分をルチル型へ転移させ
ることにより、公知の二酸化チタン被覆ＭＩＯ顔料の欠
点を改良することに成功した。Therefore, the present inventors researched a method of transitioning to rutile type under conditions that would not impair the interference effect, and
By converting substantially the majority of the coated titanium dioxide into the rutile form, we have succeeded in overcoming the deficiencies of known titanium dioxide coated MIO pigments.
木発皿勿盟盟
一面において本発明は、フレーク状の雲母状酸化鉄結晶
粒子の表面をルチル型二酸化チタンで被覆してなること
を特徴とする顔料を提供する。In one aspect, the present invention provides a pigment characterized in that the surface of flaky mica-like iron oxide crystal particles is coated with rutile-type titanium dioxide.
他の面において本発明は、フレーク状の雲母状酸化鉄結
晶粒子の水性懸濁液へチタン化合物溶液を添加し、該チ
タン化合物の加水分解によって生成した含水二酸化チタ
ンの微粒子を沈着せしめ、口遇、洗浄、乾燥および焼成
して二酸化チタン被覆酸化鉄顔料を製造する方法におい
て、前記懸濁液へ焼成前の任意の工程において亜鉛塩、
スズ塩、アンチモン塩、リチウム塩より選ばれたルチル
型転移促進剤を添加し、焼成時に二酸化チタンの被覆層
の実施上大部分をルチル型に転移せしめることを特徴と
する二酸化チタン被覆酸化鉄顔料の製造方法を提供する
。In another aspect, the present invention includes adding a titanium compound solution to an aqueous suspension of flaky mica-like iron oxide crystal particles, depositing fine particles of hydrated titanium dioxide produced by hydrolysis of the titanium compound, and , washing, drying and firing to produce a titanium dioxide-coated iron oxide pigment, in which a zinc salt,
A titanium dioxide-coated iron oxide pigment characterized by adding a rutile-type transformation accelerator selected from tin salts, antimony salts, and lithium salts to transform most of the titanium dioxide coating layer into the rutile type upon firing. Provides a manufacturing method.
鉦且支公実上五僅
本発明の二酸化チタン被覆ＭＩＯ顔料の製法は、ルチル
型転移促進剤を使用することを除いて、先に引用した特
公昭５１−７１７６号に記載の方法と基本的に同じでよ
い。The method for producing the titanium dioxide-coated MIO pigment of the present invention is basically the same as the method described in the above-cited Japanese Patent Publication No. 7176/1983, except that a rutile-type transition accelerator is used. It can be the same as .
ＭＩＯとしては、天然品および合成ＭＩＯのいずれも使
用することができ、径は一般に２〜２００μ、好ましく
は５〜１００μ、厚み０．３〜５μ。As MIO, both natural products and synthetic MIO can be used, and the diameter is generally 2 to 200 microns, preferably 5 to 100 microns, and the thickness is 0.3 to 5 microns.
好ましくは０．５〜３μのフレーク状の結晶粒子を用い
ることができる。Preferably, flaky crystal particles of 0.5 to 3 μm can be used.
ＭＩＯ粒子の被覆は、ＭＩＯを水に懸濁してスラリーと
し、これへチタン化合物の溶液をかきまぜながら添加し
、スラリーを常温からゆっくり８０℃〜沸点まで加熱昇
温し、または塩基により徐々に中和し、チタン化合物を
加水分解することによって行われる。To coat MIO particles, MIO is suspended in water to form a slurry, a titanium compound solution is added to this while stirring, and the slurry is slowly heated from room temperature to 80°C to boiling point, or gradually neutralized with a base. This is done by hydrolyzing a titanium compound.
チタン化合物としては、硫酸チタニル、四塩化チタンま
たはそれらの混合物を使用することができるが、四塩化
チタンが好ましい。As the titanium compound, titanyl sulfate, titanium tetrachloride or a mixture thereof can be used, but titanium tetrachloride is preferred.
ルチル型転移促進剤は、ＭＩＯの懸濁液へ、チタン化合
物の添加前、同時または添加後に添加することができ、
さらに一旦ＭＩＯを含水二酸化チタンで被Ｎｌ＆洗浄し
、水へ再懸濁し、それへ添加し、加水分解してもよい。The rutile-type transformation promoter can be added to the suspension of MIO before, simultaneously with, or after the addition of the titanium compound,
Furthermore, MIO may be once washed with hydrous titanium dioxide, resuspended in water, and added thereto for hydrolysis.
ルチル型転移促進剤は、亜鉛、スズ、アンチモン、リチ
ウムより選ばれた金属の塩化物、硝酸塩、硫酸塩、それ
らの混合物などの水溶性塩が使用し得る。亜鉛およびス
ズの塩が好ましい。As the rutile type transition accelerator, water-soluble salts such as chlorides, nitrates, sulfates, and mixtures thereof of metals selected from zinc, tin, antimony, and lithium can be used. Zinc and tin salts are preferred.
被覆処理の間は常時攪拌するのが好ましい、被覆処理後
は、口過、洗浄、乾燥後、ケーキを５００〜１０００℃
、好ましくは６００〜８００℃で焼成し、被覆二酸化チ
タンの実質上大部分をルチル型へ転移させることによっ
て、公知の二酸化チタン被覆ＭＩＯ顔料に比較して耐光
性および耐候性にすぐれた顔料が得られる。このように
ルチル型転移促進剤の使用により、干渉効果が損われな
い条件下で被覆二酸化チタンをルチル型へ転移させるこ
とができる。It is preferable to constantly stir during the coating process.After the coating process, after filtration, washing, and drying, the cake is heated to 500-1000℃.
, preferably at 600 to 800° C., to transform substantially most of the coated titanium dioxide into the rutile type, resulting in a pigment with superior light resistance and weather resistance compared to known titanium dioxide coated MIO pigments. It will be done. Thus, the use of a rutile type transformation accelerator allows the coated titanium dioxide to be converted to the rutile type under conditions where interference effects are not impaired.
二酸化チタンの被覆量は、ＭＩＯを基準として、一般に
０．１〜３０重量％の範囲が好ましく、転移促進剤は、
金属酸化物として、二酸化チタンの５０重量％以下でよ
い。The coating amount of titanium dioxide is generally preferably in the range of 0.1 to 30% by weight based on MIO, and the transition accelerator is
The metal oxide may be 50% by weight or less of titanium dioxide.
以下に本発明の実施例を示す。Examples of the present invention are shown below.
実施例Ｉ
Ｍ１０２００ｇを水１．４１に分散し、攪拌下で四塩化
チタン水溶液（Ｔｉ０ｇ ２７．４％、ＨＣ２３２゜３
％を含む）１４６ｇと、５ｎＣｅａ ・５Ｈｚ０１４
ｇの混合液を添加し、その後１分間に１℃の速度でゆ
っ（り加熱昇温し、９８℃で３時間維持して加水分解し
、ＭＩＯの表面に含水二酸化チタンと含水酸化スズとの
混合層を被覆した。次に懸濁液を口遇し、ケーキを洗浄
、乾燥後７００℃で１時間焼成し、被覆ＭＩＯＩＩｉ料
を得た。このもののＸ線回折チャートはルチル型である
ことを示した。Example I 10200 g of M was dispersed in 1.41 g of water, and with stirring, a titanium tetrachloride aqueous solution (0 g of Ti 27.4%, HC232°3
%) 146g and 5nCea・5Hz014
g of the mixed solution was added, and then the temperature was slowly raised at a rate of 1°C per minute, and the temperature was maintained at 98°C for 3 hours to cause hydrolysis, resulting in a mixture of hydrated titanium dioxide and hydrated tin oxide on the surface of MIO. The mixed layer was coated.The suspension was then mixed, and the cake was washed, dried, and baked at 700°C for 1 hour to obtain a coated MIOIIi material.The X-ray diffraction chart of this material showed that it was of rutile type. Indicated.
実施例２
Ｍ１０２００ｇを水１．１！に分散し、攪拌下で四塩化
チタン水溶液（Ｔｉ０ｚ ２７．４％、Ｈ（ｊ！３２゜
３％を含む）１４６ｇを添加し、その１′に１分間に１
℃の速度でゆっくり加熱昇温し、９５℃で３時間保って
加水分解し、ＭＩＯの表面に含水二酸化チタン層を被覆
した。懸濁液を一旦口過し、ケーキを洗浄後水１βに再
懸濁し、これにＺｔ＋Ｃ１２ｚ １５ｇを少量の水に溶
解して添加後、アンモニア水でゆっくり中和してＩ）
Ｈ６，５とし、３０分間攪拌を続けた後、粒子を口過、
洗浄、乾燥後、７３０℃で１時間焼成して被ｉＭＩｏ顔
料を得た。このもののＸ線回折チャートはルチル型であ
ることを示した。Example 2 M10200g water 1.1! 146 g of titanium tetrachloride aqueous solution (Ti0z 27.4%, H (containing J!32°3%)) was added under stirring, and the titanium tetrachloride aqueous solution (containing 3% of J!
The temperature was slowly increased at a rate of 95° C., and the mixture was kept at 95° C. for 3 hours for hydrolysis, thereby coating the surface of MIO with a hydrous titanium dioxide layer. Once the suspension was passed through the mouth, the cake was washed and resuspended in water 1β. After adding 15 g of Zt+C12z dissolved in a small amount of water, the mixture was slowly neutralized with aqueous ammonia (I)
After adjusting the temperature to H6.5 and continuing stirring for 30 minutes, the particles were passed through the mouth.
After washing and drying, it was fired at 730° C. for 1 hour to obtain an iMIo pigment. The X-ray diffraction chart of this product showed that it was of rutile type.
比較例
ＭＩ０２００ｇを水１．４１に分散し、攪拌下で硫酸チ
タニル溶液（Ｔｉ０２２００ ｇ／ ｌ、 Ｈ２ＳＯ４
３，４０ｇ／ｌを含む）２００献を添加し、その後１分
間に１℃の速度で加熱昇温し、９８℃で３時間維持して
加水分解し、ＭＩＯ表面に含水二酸化チタン層を被覆し
た。被覆顔料を口過、洗浄、乾燥後７００℃で１時間焼
成し、被ｉＭ Ｉ Ｏ顔料を得た。このもののＸ線回折
チャートはアナターゼ型であることを示した。Comparative Example 200 g of MI0 was dispersed in 1.41 g of water and mixed with a titanyl sulfate solution (2200 g/l of Ti0, H2SO4) under stirring.
After that, the temperature was increased at a rate of 1°C per minute, and the temperature was maintained at 98°C for 3 hours for hydrolysis, thereby coating the MIO surface with a hydrated titanium dioxide layer. . The coated pigment was passed through the mouth, washed, dried, and then fired at 700° C. for 1 hour to obtain an iM IO pigment. The X-ray diffraction chart of this product showed that it was anatase type.
被覆ＭＩＯ１Ｉｉ料 ２０．Ｏｆｆｉ
量部ツルペッツｔｏｏ ８．０
〃トルエン ２４．０ 〃
酢酸エチル ８，０〃酢酸ブチ
ル ８．０〃１％シリコーン
０．４〃１）大日本インキ化学工業
ｎｉ アクリル樹脂２）同社製メラミン樹脂
実施例および比較例にて得た被覆ＭＩＯ顔料を上記配合
でディスパーにて１８０Ｏｒｐｍで５分間分散し、カラ
ーベース塗料に調製した。Coated MIO1Ii material 20. Offi
Quantity Tsurupets too 8.0
〃Toluene 24.0 〃
Ethyl acetate 8.0 Butyl acetate 8.0 1% silicone
0.4〃1) Dainippon Ink & Chemicals Co., Ltd. acrylic resin 2) Melamine resin manufactured by the same company The coated MIO pigments obtained in Examples and Comparative Examples were dispersed in a disper at 180 Orpm for 5 minutes with the above formulation to prepare a color base paint. did.
Ｌユを二１且
トルエン １６．８ 〃酢酸
エチル １２．６ 〃酢酸ブ
チル ８．４〃ツルペツツ１０
０ ４．２ 〃カラーベース塗料
と同様な操作によって上記配合のクリヤー塗料を調製し
た。21 toluene 16.8 ethyl acetate 12.6 butyl acetate 8.4 10
0 4.2 A clear paint having the above formulation was prepared in the same manner as the color base paint.
拭政塗装板
ボンデ処理軟鋼板に、カーボンブラックエナメルを塗装
焼付後、＃５００サンドペーパーにて研磨し、水洗乾燥
し、その上に前記カラーベース塗料を乾燥膜厚２５μに
なるように吹付塗装し、１０分間セット後、前記クリヤ
ー塗料を乾燥膜厚６０μになるように吹付塗装し、３０
分間セントした後、１４０℃×２５分間焼付けて試験片
とした。Carbon black enamel was painted on a bonded mild steel plate, polished with #500 sandpaper, washed with water, dried, and sprayed with the color base paint to a dry film thickness of 25 μm. After setting for 10 minutes, spray coat the clear paint to a dry film thickness of 60 μm.
After centrifuging for a minute, the test pieces were baked at 140°C for 25 minutes.
且久比式験
各試験片について、カーボンアーク、サンシャイン、ウ
エザオメーター（スガ試験機）により、１２０分中１ｚ
分降雨、ブラックパネル温度６３℃の条件で曝露試験を
行った。結果を下表に示す。For each test piece, carbon arc, sunshine, and weather-o-meter (Suga Test Instruments) were used to test each specimen for 1z in 120 minutes.
An exposure test was conducted under the conditions of minute rainfall and a black panel temperature of 63°C. The results are shown in the table below.
表
注：変色の目視判定の基準は下記のとおりランク
変色程度
Ｉ： 変色が認められず。Table note: The criteria for visual judgment of discoloration are as follows:
Discoloration degree I: No discoloration observed.
２： 僅かに変色が認められる。2: Slight discoloration is observed.
３： 変色が認められる。3: Discoloration is observed.
５人の判定者の評価ランクを合計して変色目視評価とし
た。The evaluation ranks of the five judges were summed to form a visual evaluation of discoloration.
図面は実施例および比較例によって得られたＸ線回折チ
ャートである。The drawings are X-ray diffraction charts obtained in Examples and Comparative Examples.
Claims (2)
ル型二酸化チタンで被覆してなることを特徴とする顔料
。(1) A pigment characterized in that the surface of flaky mica-like iron oxide crystal particles is coated with rutile-type titanium dioxide.
へチタン化合物溶液を添加し、該チタン化合物の加水分
解によって生成した含水二酸化チタンの微粒子を沈着せ
しめ、ロ過、洗浄、乾燥および焼成して二酸化チタン被
覆酸化鉄顔料を製造する方法において、前記懸濁液へ焼
成前の任意の工程において亜鉛塩、スズ塩、アンチモン
塩、リチウム塩より選ばれたルチル型転移促進剤を添加
し、焼成時に二酸化チタンの被覆層の実質上大部分をル
チル型に転移せしめることを特徴とする二酸化チタン被
覆酸化鉄顔料の製造方法。(2) A titanium compound solution is added to an aqueous suspension of flaky mica-like iron oxide crystal particles to deposit fine particles of hydrated titanium dioxide produced by hydrolysis of the titanium compound, followed by filtration, washing, drying and In the method of manufacturing a titanium dioxide-coated iron oxide pigment by firing, a rutile type transformation accelerator selected from zinc salt, tin salt, antimony salt, and lithium salt is added to the suspension in an arbitrary step before firing. A method for producing a titanium dioxide-coated iron oxide pigment, characterized in that substantially most of the titanium dioxide coating layer is transformed into a rutile type during firing.
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62056193A JP2668072B2 (en) | 1987-03-11 | 1987-03-11 | Titanium dioxide A method for transferring a coated titanium dioxide layer to a rutile type without losing the interference color of iron oxide pigments |
| DE8888302147T DE3868089D1 (en) | 1987-03-11 | 1988-03-11 | Mica-like iron oxide pigments coated with titanium oxide and process for their production. |
| EP88302147A EP0282329B1 (en) | 1987-03-11 | 1988-03-11 | Titanium dioxide coated micaceous iron oxide pigments and method for producing the same |
| US07/488,463 US5002608A (en) | 1987-03-11 | 1990-02-26 | Titanium dioxide coated micaceous iron oxide pigments and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62056193A JP2668072B2 (en) | 1987-03-11 | 1987-03-11 | Titanium dioxide A method for transferring a coated titanium dioxide layer to a rutile type without losing the interference color of iron oxide pigments |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63223069A true JPS63223069A (en) | 1988-09-16 |
| JP2668072B2 JP2668072B2 (en) | 1997-10-27 |
Family
ID=13020273
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62056193A Expired - Fee Related JP2668072B2 (en) | 1987-03-11 | 1987-03-11 | Titanium dioxide A method for transferring a coated titanium dioxide layer to a rutile type without losing the interference color of iron oxide pigments |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2668072B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010509164A (en) * | 2006-11-08 | 2010-03-25 | ロックウッド イタリア スパ | Iron oxide containing precipitated crystalline titanium dioxide and its manufacturing process |
| CN101980989A (en) * | 2008-03-31 | 2011-02-23 | 意大利乐科伍德公司 | Granulate having photocatalytic activity and methods for manufacturing the same |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4855217A (en) * | 1971-11-12 | 1973-08-03 | ||
| JPS5434010A (en) * | 1977-07-20 | 1979-03-13 | Seiko Instr & Electronics Ltd | Electronic clock |
| JPS59170151A (en) * | 1983-03-16 | 1984-09-26 | Sanyo Shikiso Kk | Manufacture of mica-based pearlescent pigment |
-
1987
- 1987-03-11 JP JP62056193A patent/JP2668072B2/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS4855217A (en) * | 1971-11-12 | 1973-08-03 | ||
| JPS5434010A (en) * | 1977-07-20 | 1979-03-13 | Seiko Instr & Electronics Ltd | Electronic clock |
| JPS59170151A (en) * | 1983-03-16 | 1984-09-26 | Sanyo Shikiso Kk | Manufacture of mica-based pearlescent pigment |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010509164A (en) * | 2006-11-08 | 2010-03-25 | ロックウッド イタリア スパ | Iron oxide containing precipitated crystalline titanium dioxide and its manufacturing process |
| CN101980989A (en) * | 2008-03-31 | 2011-02-23 | 意大利乐科伍德公司 | Granulate having photocatalytic activity and methods for manufacturing the same |
| JP2011518656A (en) * | 2008-03-31 | 2011-06-30 | ロックウッド イタリア スパ | Granules having photocatalytic activity and method for producing the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2668072B2 (en) | 1997-10-27 |
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Free format text: JAPANESE INTERMEDIATE CODE: R250 |
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