JPH0158226B2 - - Google Patents
Info
- Publication number
- JPH0158226B2 JPH0158226B2 JP58118688A JP11868883A JPH0158226B2 JP H0158226 B2 JPH0158226 B2 JP H0158226B2 JP 58118688 A JP58118688 A JP 58118688A JP 11868883 A JP11868883 A JP 11868883A JP H0158226 B2 JPH0158226 B2 JP H0158226B2
- Authority
- JP
- Japan
- Prior art keywords
- mica flakes
- titanyl sulfate
- titanium oxide
- coated
- coating layer
- 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
Links
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 45
- 239000010445 mica Substances 0.000 claims description 41
- 229910052618 mica group Inorganic materials 0.000 claims description 41
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 33
- 229910000349 titanium oxysulfate Inorganic materials 0.000 claims description 26
- 239000011247 coating layer Substances 0.000 claims description 11
- 239000000049 pigment Substances 0.000 claims description 11
- 239000000243 solution Substances 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000012452 mother liquor Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 230000003301 hydrolyzing effect Effects 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims 1
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 229910052719 titanium Inorganic materials 0.000 claims 1
- 239000010936 titanium Substances 0.000 claims 1
- 239000010410 layer Substances 0.000 description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 14
- 229910010413 TiO 2 Inorganic materials 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- 239000004408 titanium dioxide Substances 0.000 description 6
- 239000006227 byproduct Substances 0.000 description 5
- 238000010304 firing Methods 0.000 description 4
- 239000002932 luster Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 229910001209 Low-carbon steel Inorganic materials 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Description
本発明は二酸化チタンで被覆した雲母フレーク
よりなる真珠光沢顔料の製造法に関する。
このような真珠光沢顔料は、例えば米国特許第
3087828号に記載されているように、雲母フレー
クを硫酸チタニルの希薄水溶液中に懸濁し、次い
で急速に加熱することにより硫酸チタニルを加水
分解し、含水酸化チタン層を連続的に雲母フレー
ク上に析出させる方法により、または雲母フレー
クを熱水中に懸濁させ、これに硫酸チタニル溶液
を加えて加水分解することにより連続的に雲母フ
レーク上に含水酸化チタン層を析出させる方法に
よつて製造させる。さらに安定化のため、700な
いし1000℃の温度で力焼し、含水酸化チタン層を
酸化チタン層に転換できることも知られている。
これら真珠顔料は、一般に強い真珠光沢感、強
い光輝感および強い干渉色が要求させる。このよ
うな真珠光沢感、光輝感、干渉色は、雲母フレー
ク表面に析出被覆させた酸化チタン層に起因する
ものである。従つてこの酸化チタン層の性質によ
り、真珠光沢感、光輝感、干渉色は大きく左右さ
れ、より強い真珠光沢感、光輝感、干渉色を得る
ためには、非常に均一で、ち密な酸化チタン層を
得る必要がある。
本発明者らは、このような均一で、ち密な酸化
チタン層を形成させる方法について研究した結
果、酸化チタン層を多層に形成すればよいことを
発見した。具体的には、雲母フレーク上に含水酸
化チタン層を被覆する場合、硫酸チタニルの加水
分解をくり返すことによつて効果的に含水酸化チ
タン層を多層に形成することが可能であることが
わかつた。
酸化チタン被覆層を一度に形成する場合に比べ
て、硫酸チタニルの加水分解をくり返して行な
い、多層に形成すれば、酸化チタン層中の酸化チ
タン粒子はより高密度に配列し、これが真珠光沢
顔料のより強い真珠光沢感、光輝感、干渉色を示
す原因でああると考えられる。
本発明はこのように酸化チタン被覆層を多層に
形成するため、公知の雲母フレークを懸濁させた
硫酸チタニル水溶液を加水分解し、雲母フレーク
上に含水酸化チタンの被覆層を形成させ、これを
力焼することによりなる真珠光沢顔料の製造法に
おいて、被覆すべき酸化チタンの総量の一部に相
当する硫酸チタニルを含む水溶液中に雲母フレー
クの全量を懸濁して前記加水分解を行つた後、処
理した雲母フレークを反応母液から分離し、分離
した雲母フレークを他の一部に相当する新たな硫
酸チタニル水溶液に再懸濁して前記加水分解を行
ない、前回形成した被覆層の上に新たな被覆層を
形成させ、この操作を所定の被覆量に達するまで
くり返すことを特徴とするものである。
最初所定量の雲母フレークを水に懸濁させ、か
きまぜながら所定量の硫酸チタニル水溶液を添加
し、90℃ないし100℃で少なくとも１時間にわた
つて加熱すると、硫酸チタニルが加水分解されて
生じた含水酸化チタンが雲母フレーク上に析出す
る。この時懸濁液中には硫酸が副生するが、この
硫酸を含む母液をロ過等の公知の操作で含水酸化
チタンで被覆された雲母フレークケーキより除去
する。
次に上記雲母フレークケーキを水に再懸濁さ
せ、所定量の新たな硫酸チタニル溶液を添加し、
前回と同じ操作によつて最初被覆された含水酸化
チタン層の上に新たな含水酸化チタン被覆層を形
成させる。この時生じた副生硫酸は最初と同じ方
法で除去される。このような操作は所望量の酸化
チタンが雲母フレーク上に被覆されるまでくり返
される。
硫酸チタニルと雲母フレーク、または部分的に
被覆された雲母フレークの添加順序は任意であ
り、前記と逆の順序、すなわち先に硫酸チタニル
を加え、後から雲母フレークを加えたり、または
同時に加えてもよい。
用いられる硫酸チタニルの濃度は50ないし250
ｇ／（TiO2基準）の濃度であればよい。また
硫酸チタニル溶液中の硫酸濃度は、Ｘ＝H2SO4
濃度／TiO2濃度と規定すれば、Ｘ＝1.5ないし5.0
の範囲となるような濃度であればよい。
雲母フレークの懸濁液中における濃度は50ない
し250ｇ／に変えることができる。また用いら
れる雲母フレークの大きさは３ないし100μの大
きさである。
本発明を実施するに当り特に留意すべき点は、
被覆１回当り硫酸チタニルより副生する系内の硫
酸濃度が10ないし20ｇ／にとどまるように硫酸
チタニルの添加量を選択することである。これか
ら一回当り被覆されるTiO2の量を求めることが
でき、最終的に被覆さるべきTiO2の総量が決ま
れば被覆回数も決まる。
一度に多量の硫酸が副生するような量の硫酸チ
タニルを使用すると、酸化チタン被覆層を複数回
に分けて多層に形成させる意義が失われ、品質の
すぐれた真珠光沢顔料を得ることができなくな
る。
従つて一度に酸化チタンの全量を被覆させる従
来法に比較し、本発明の効果は雲母フレークに対
し被覆すべき酸化チタンの総量が比較的多い時に
特に顕著となる。その理由は本発明においては一
回の被覆で副生される硫酸の濃度が従来法におけ
るよりもかなり低く、そのため雲母フレーク上へ
の酸化チタン粒子の付着が容易であるためである
と考えられる。
このように酸化チタン被覆層を１回で形成させ
るのではなく、何回にも分けて硫酸チタニルの加
水分解を行ない、雲母フレーク上に多層に含水酸
化チタンの被覆層を形成させて行くと、同じ被覆
量を１回の操作で達成させる従来法に比し、より
強い真珠光沢感、光輝感、隠ペイ力を有し、耐光
性もすぐれた真珠光沢顔料が得られることが判つ
た。さらに含水酸化チタンで多層被覆された雲母
フレークを500ないし1000℃で30分ないし５時間
力焼すれば、より均一な酸化チタン層で被覆され
た雲母フレーク顔料を得ることができる。
以下の実施例により本発明をさらに詳しく説明
する。
実施例 １
片の大きさが５ないし20μであるような雲母フ
レーク140ｇを水に添加し、容量を２とした。
これへかきまぜながら220ｇ／（TiO2基準）の
硫酸チタニル溶液（Ｘ＝1.6）100ml（TiO2基準
22ｇ）を加え、急速に加熱沸騰させ、３時間この
状態を維持する。
生成物をロ過洗浄し、290ｇ（水分約45％）の
ウエツトケーキが得られた（以上を操作とす
る。）
このウエツトケーキを水に再懸濁させ、操作
と同じ条件で処理する。（以上を操作とする。）
操作で得られたウエツトケーキを再び水に懸
濁させ、操作と操作と同じ条件で処理する。
（以上を操作とする。）
操作で得られたウエツトケーキを乾燥し、さ
らに800℃で１時間力焼した。力焼後の二酸化チ
タン被覆雲母フレークのTiO2被覆量は30.5％で
あつた。
比較例
対照として硫酸チタニルの全量を一度に添加
し、加水分解する方法を実施した。
実施例１と同じ雲母フレーク140ｇを水に添加
し、容積を２とした。これにかきまぜながら実
施例１と同じ硫酸チタニル溶液300mlを一度に加
え、急速に加熱沸沸騰させ、３時間この状態を維
持した。実施例１と同様に生成物をロ過洗剰し、
乾燥し、800℃で１時間力焼した。力焼後の二酸
化チタン被覆雲母フレークのTiO2被覆量は30.0
％であつた。
実施例１および比較例によつて得られた顔料を
使つて以下の組成を有する透明ラツカーを調整
し、白黒カード紙の上に塗布し、評価した。
ラツカーの組成
硝化綿（片山化学製、固形分72％） 100ｇ
酢酸エチル 105ｇ
トルエン 105ｇ
イソプロピルアルコール 75ｇ
二酸化チタン被覆雲母フレーク 22ｇ
評 価
その１ 黒板上の光沢を変角光度計（スガ試験機
(株)製、UGV―40）で測定した結果を第１表に示
す。
The present invention relates to a method for producing pearlescent pigments consisting of mica flakes coated with titanium dioxide. Such pearlescent pigments are described, for example, in U.S. Pat.
3087828, mica flakes are suspended in a dilute aqueous solution of titanyl sulfate and then rapidly heated to hydrolyze the titanyl sulfate, depositing a layer of hydrated titanium oxide on the mica flakes in a continuous manner. Alternatively, mica flakes are suspended in hot water, and a titanyl sulfate solution is added thereto for hydrolysis, thereby continuously depositing a hydrous titanium oxide layer on mica flakes. It is also known that for further stabilization, the hydrous titanium oxide layer can be converted into a titanium oxide layer by calcining at a temperature of 700 to 1000°C. These pearlescent pigments are generally required to have a strong pearlescent feel, a strong glitter feeling, and a strong interference color. Such pearlescent feel, brightness, and interference color are caused by the titanium oxide layer deposited and coated on the surface of the mica flakes. Therefore, the properties of this titanium oxide layer greatly affect the pearl luster, glitter, and interference colors.In order to obtain stronger pearl luster, glitter, and interference colors, it is necessary to use very uniform and dense titanium oxide. You need to get layers. As a result of research into a method for forming such a uniform and dense titanium oxide layer, the present inventors discovered that it is sufficient to form a multilayer titanium oxide layer. Specifically, when coating a hydrous titanium oxide layer on mica flakes, it was found that it is possible to effectively form a multilayer hydrous titanium oxide layer by repeating the hydrolysis of titanyl sulfate. Ta. Compared to forming a titanium oxide coating layer all at once, by repeatedly hydrolyzing titanyl sulfate to form multiple layers, the titanium oxide particles in the titanium oxide layer are arranged more densely, and this creates a pearlescent pigment. This is thought to be the cause of the stronger pearl luster, glitter, and interference color. In order to form a multilayer titanium oxide coating layer in this way, the present invention hydrolyzes a known titanyl sulfate aqueous solution in which mica flakes are suspended to form a hydrous titanium oxide coating layer on the mica flakes. In a method for producing a pearlescent pigment by force firing, the entire amount of mica flakes is suspended in an aqueous solution containing titanyl sulfate corresponding to a part of the total amount of titanium oxide to be coated, and then the hydrolysis is carried out, The treated mica flakes are separated from the reaction mother liquor, and the separated mica flakes are resuspended in a new titanyl sulfate aqueous solution corresponding to the other part to perform the hydrolysis, and a new coating is formed on the previously formed coating layer. It is characterized by forming a layer and repeating this operation until a predetermined amount of coverage is reached. First, a predetermined amount of mica flakes is suspended in water, a predetermined amount of titanyl sulfate aqueous solution is added while stirring, and heated at 90°C to 100°C for at least 1 hour. Titanium oxide is deposited on the mica flakes. At this time, sulfuric acid is produced as a by-product in the suspension, and the mother liquor containing this sulfuric acid is removed from the mica flake cake coated with hydrous titanium oxide by a known operation such as filtration. The mica flake cake is then resuspended in water, a predetermined amount of fresh titanyl sulfate solution is added,
A new hydrous titanium oxide coating layer is formed on the initially coated hydrous titanium oxide layer by the same operation as the previous time. The by-product sulfuric acid produced at this time is removed in the same manner as the initial method. These operations are repeated until the desired amount of titanium oxide is coated on the mica flakes. The order of addition of titanyl sulfate and mica flakes or partially coated mica flakes is arbitrary and may be added in the reverse order, i.e. titanyl sulfate is added first followed by mica flakes, or they may be added simultaneously. good. The concentration of titanyl sulfate used is between 50 and 250
It is sufficient if the concentration is g/(TiO 2 standard). Also, the sulfuric acid concentration in the titanyl sulfate solution is X=H 2 SO 4
If defined as concentration/TiO 2 concentration, then X = 1.5 to 5.0
The concentration may be within the range of . The concentration of mica flakes in the suspension can vary from 50 to 250 g/ml. The size of the mica flakes used is 3 to 100 μm. Points to be noted in particular when implementing the present invention are:
The amount of titanyl sulfate to be added is selected so that the concentration of sulfuric acid in the system as a by-product from titanyl sulfate per coating remains at 10 to 20 g/l. From this, the amount of TiO 2 to be coated per time can be determined, and once the total amount of TiO 2 to be coated is finally determined, the number of times of coating can also be determined. If titanyl sulfate is used in such an amount that a large amount of sulfuric acid is produced as a by-product at one time, the significance of forming the titanium oxide coating layer in multiple layers will be lost, making it impossible to obtain a pearlescent pigment of excellent quality. It disappears. Therefore, compared to the conventional method in which the entire amount of titanium oxide is coated at one time, the effects of the present invention are particularly noticeable when the total amount of titanium oxide to be coated on mica flakes is relatively large. The reason for this is thought to be that in the present invention, the concentration of sulfuric acid produced as a by-product in one coating is considerably lower than in the conventional method, and therefore titanium oxide particles can easily adhere to the mica flakes. In this way, instead of forming a titanium oxide coating layer in one go, the titanyl sulfate is hydrolyzed in several steps to form a multilayer hydrous titanium oxide coating layer on the mica flakes. It has been found that a pearlescent pigment with stronger pearl luster, glitter, hiding power, and excellent light resistance can be obtained compared to the conventional method in which the same amount of coverage is achieved in one operation. Furthermore, by calcining the mica flakes coated with multiple layers of hydrous titanium oxide at 500 to 1000°C for 30 minutes to 5 hours, it is possible to obtain mica flake pigments coated with a more uniform layer of titanium oxide. The invention will be explained in more detail by the following examples. Example 1 140 g of mica flakes with a flake size of 5 to 20 microns were added to water to a volume of 2.
While stirring, add 100 ml of 220 g/(based on TiO 2 ) titanyl sulfate solution (X = 1.6) (based on TiO 2
Add 22g), rapidly bring to a boil, and maintain this state for 3 hours. The product was filtered and washed to obtain 290 g (approximately 45% moisture) of a wet cake (the above is the procedure). This wet cake is resuspended in water and treated under the same conditions as the procedure. (The above is considered an operation.) The wet cake obtained in the operation is resuspended in water and treated under the same conditions as the operation.
(The above is considered as the operation.) The wet cake obtained in the operation was dried and further calcined at 800°C for 1 hour. The TiO 2 coverage of the titanium dioxide-coated mica flakes after power firing was 30.5%. Comparative Example As a control, a method was carried out in which the entire amount of titanyl sulfate was added at once and hydrolyzed. 140 g of the same mica flakes as in Example 1 were added to the water to give a volume of 2. While stirring, 300 ml of the same titanyl sulfate solution as in Example 1 was added at once to the solution, rapidly heated to boiling point, and maintained at this state for 3 hours. Filter wash the product as in Example 1,
It was dried and calcined at 800°C for 1 hour. TiO 2 coverage of titanium dioxide coated mica flakes after force firing is 30.0
It was %. A transparent lacquer having the following composition was prepared using the pigments obtained in Example 1 and Comparative Example, coated on black and white card paper, and evaluated. Composition of Lutzker Nitrified cotton (manufactured by Katayama Chemical, solid content 72%) 100g Ethyl acetate 105g Toluene 105g Isopropyl alcohol 75g Titanium dioxide coated mica flakes 22g Evaluation 1 Measure the gloss on the blackboard using a variable angle photometer (Suga Test Instruments)
Table 1 shows the results measured with UGV-40 (manufactured by Co., Ltd.).
【表】
第１表に示すように、実施例１の方が比較例よ
りも光沢がすぐれている。
その２ 白黒カード上の白板および黒板上のそれ
ぞれのＹ値を色差計（スガ試験機(株)製、SM―３
型）で測定し、Ｙ値（黒板上）／Ｙ値（白板上）
の比を測定した。結果を第２表に示す。[Table] As shown in Table 1, Example 1 has better gloss than Comparative Example. Part 2 Measure the Y values on the white board and blackboard on the black and white card using a color difference meter (manufactured by Suga Test Instruments Co., Ltd., SM-3).
Y value (on the blackboard) / Y value (on the white board)
The ratio of The results are shown in Table 2.
【表】
第２表に示すように、実施例１の方が比較例よ
りもそれぞれのＹ値の比が高く、隠ペイ力が高い
ことを示している。
耐 光 性
耐光性を評価するため、下記組成の常乾アクリ
ルウレタン塗料を調製し、灰色下塗り処理された
軟鋼板に塗布し、屋外に曝露した。
常乾アクリルウレタン塗料の組成
アクリデイツク Ａ―801（固形分50％） 90部
バーノツク DN―950（固形分75％） 27部
溶 剤 15部
二酸化チタン被覆雲母フレーク ２部
第３表は曝露前と、曝露10ケ月後の色差を示
す。[Table] As shown in Table 2, the ratio of each Y value is higher in Example 1 than in the comparative example, indicating that the concealment power is higher. Light Resistance In order to evaluate light resistance, an air-dry acrylic urethane paint with the following composition was prepared, applied to a gray undercoated mild steel plate, and exposed outdoors. Composition of air-dry acrylic urethane paint Acrylic A-801 (solid content 50%) 90 parts Burnock DN-950 (solid content 75%) 27 parts Solvent 15 parts Titanium dioxide coated mica flakes 2 parts Table 3 shows before exposure and Shows the color difference after 10 months of exposure.
【表】
第３表に示すように、実施例１のものは比較例
に比べて変色（△Ｅ）が少なかつた。
実施例 ２
実施例１と同じ雲母フレークを実施例１と同じ
方法で処理した。ただし、１回当りの硫酸チタニ
ル溶液の添加量を100mlから60mlへ減少する代り
に、被覆回路を５回に増加した。
生成物の酸化チタン被覆量は30.5％であつた。
評 価
その１ 第４表に実施例１と同じ方法で測定した
Ｙ値の比を示す。[Table] As shown in Table 3, Example 1 had less discoloration (ΔE) than Comparative Example. Example 2 The same mica flakes as in Example 1 were treated in the same manner as in Example 1. However, instead of reducing the amount of titanyl sulfate solution added per time from 100 ml to 60 ml, the number of coating cycles was increased to 5 times. The titanium oxide coverage of the product was 30.5%. Evaluation 1 Table 4 shows the ratio of Y values measured in the same manner as in Example 1.
【表】
第４表に示すように、実施例２の方がそれぞれ
のＹ値の比が高く、隠ペイ力が高いことを示して
いる。
その２ 力焼前の二酸化チタン被覆雲母の比表面
積を窒素吸着法によつて測定した。使用した測定
器は柴田理化学機械(株)製のSA―1000型である。
第５表に測定結果を示す。[Table] As shown in Table 4, Example 2 has a higher ratio of each Y value, indicating that the concealment power is higher. Part 2: The specific surface area of titanium dioxide-coated mica before calcining was measured by a nitrogen adsorption method. The measuring instrument used was model SA-1000 manufactured by Shibata Rikagaku Kikai Co., Ltd.
Table 5 shows the measurement results.
【表】
第５表に示すように、力焼前の比表面積を比較
すると、実施例２のものは比較例のものよりも小
さい。これは雲母フレーク表面を被覆している含
水酸化チタンの粒子が密に付着していることを示
している。[Table] As shown in Table 5, when comparing the specific surface areas before force firing, those of Example 2 are smaller than those of Comparative Examples. This indicates that the hydrous titanium oxide particles coating the mica flake surface are densely adhered.
Claims (1)
液を加水分解し、雲母フレーク上に含水酸化チタ
ンの被覆層を形成させ、これを力焼することより
なる真珠光沢顔料の製造法において、被覆すべき
酸化チタンの総量の一部に相当する硫酸チタニル
を含む水溶液中に雲母フレークの全量を懸濁して
前記加水分解を行なつた後、処理した雲母フレー
クを反応母液から分離し、分離した雲母フレーク
を他の一部に相当する新たな硫酸チタニル水溶液
に再懸濁して前記加水分解を行なつて前回形成し
た被覆層の上に新たな被覆層を形成させ、この操
作を所定の被覆量に達するまでくり返すことを特
徴とする真珠光沢顔料の製造法。1 In a method for producing a pearlescent pigment, which comprises hydrolyzing an aqueous titanyl sulfate solution in which mica flakes are suspended to form a coating layer of hydrous titanium oxide on the mica flakes, and calcining this, the oxidation to be coated is After carrying out the hydrolysis by suspending the entire amount of mica flakes in an aqueous solution containing titanyl sulfate corresponding to a part of the total amount of titanium, the treated mica flakes are separated from the reaction mother liquor, and the separated mica flakes are The sample is resuspended in a new aqueous titanyl sulfate solution corresponding to a portion of the total amount of titanyl sulfate and subjected to the hydrolysis to form a new coating layer on the previously formed coating layer, and this operation is repeated until a predetermined coating amount is reached. A method for producing a pearlescent pigment characterized by its return.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11868883A JPS6011560A (en) | 1983-06-29 | 1983-06-29 | Production of pigment having iridescent luster |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11868883A JPS6011560A (en) | 1983-06-29 | 1983-06-29 | Production of pigment having iridescent luster |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6011560A JPS6011560A (en) | 1985-01-21 |
| JPH0158226B2 true JPH0158226B2 (en) | 1989-12-11 |
Family
ID=14742720
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP11868883A Granted JPS6011560A (en) | 1983-06-29 | 1983-06-29 | Production of pigment having iridescent luster |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6011560A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1281690C (en) * | 2001-08-10 | 2006-10-25 | 日本光研工业株式会社 | Titanium oxide compsn. having high brilliant color, compsn. comprising coating and cosmetic compsn. and method for their prepn. |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3087828A (en) * | 1961-06-28 | 1963-04-30 | Du Pont | Nacreous pigment compositions |
| JPS4949174A (en) * | 1972-09-19 | 1974-05-13 | ||
| JPS4949173A (en) * | 1972-09-18 | 1974-05-13 | ||
| JPS50744A (en) * | 1972-11-10 | 1975-01-07 | ||
| JPS504021A (en) * | 1973-05-17 | 1975-01-16 | ||
| JPS516172A (en) * | 1974-07-08 | 1976-01-19 | Asahi Chemical Ind | Haigasuno shorihoho |
| JPS5152432A (en) * | 1974-11-01 | 1976-05-10 | Fujikura Kasei Kk | Sementoseihinno keshohoho |
| JPS5434010A (en) * | 1977-07-20 | 1979-03-13 | Seiko Instr & Electronics Ltd | Electronic clock |
-
1983
- 1983-06-29 JP JP11868883A patent/JPS6011560A/en active Granted
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3087828A (en) * | 1961-06-28 | 1963-04-30 | Du Pont | Nacreous pigment compositions |
| JPS4949173A (en) * | 1972-09-18 | 1974-05-13 | ||
| JPS4949174A (en) * | 1972-09-19 | 1974-05-13 | ||
| JPS50744A (en) * | 1972-11-10 | 1975-01-07 | ||
| JPS504021A (en) * | 1973-05-17 | 1975-01-16 | ||
| JPS516172A (en) * | 1974-07-08 | 1976-01-19 | Asahi Chemical Ind | Haigasuno shorihoho |
| JPS5152432A (en) * | 1974-11-01 | 1976-05-10 | Fujikura Kasei Kk | Sementoseihinno keshohoho |
| JPS5434010A (en) * | 1977-07-20 | 1979-03-13 | Seiko Instr & Electronics Ltd | Electronic clock |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6011560A (en) | 1985-01-21 |
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