JP2001048505A - Production of particulate cobalt phosphate pigment - Google Patents
Production of particulate cobalt phosphate pigmentInfo
- Publication number
- JP2001048505A JP2001048505A JP2000005925A JP2000005925A JP2001048505A JP 2001048505 A JP2001048505 A JP 2001048505A JP 2000005925 A JP2000005925 A JP 2000005925A JP 2000005925 A JP2000005925 A JP 2000005925A JP 2001048505 A JP2001048505 A JP 2001048505A
- Authority
- JP
- Japan
- Prior art keywords
- cobalt
- phosphate
- pigment
- cobalt phosphate
- aqueous solution
- 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.)
- Pending
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、顔料が従来より使
用されている各種分野、例えば、絵具、塗料、合成樹脂
等の着色剤として利用可能であり、又、本発明により更
に透明性が付与されたことから、透明性、透過性、意匠
性が要求される分野、例えば、硝子の着色やメタリック
塗料の着色剤として使用可能な微粒子リン酸コバルト顔
料及びその製造方法に関する。The present invention can be used in various fields in which pigments have been conventionally used, for example, as a colorant for paints, paints, synthetic resins, etc., and the present invention further imparts transparency. Therefore, the present invention relates to a field in which transparency, transparency, and design are required, for example, a fine particle cobalt phosphate pigment which can be used as a coloring agent for coloring glass or a metallic paint, and a method for producing the same.
【０００２】[0002]
【従来の技術】リン酸コバルト系の顔料は濃い紫色の顔
料で、耐光性、耐熱性が良好であり、主として絵具用と
して使用されてきた。又、従来から、リン酸コバルト系
顔料は、コバルト塩水溶液とリン酸塩水溶液とを混合撹
拌してリン酸コバルトの沈澱を生成させ、得られた青紫
色の沈殿スラリーを熟成させた後、濾過、水洗、乾燥
し、８００℃前後の高温で焼成することで製造されてい
る。しかしながら、この従来の方法で得られるリン酸コ
バルト顔料は、３〜５μｍの１次粒子が凝集して１０〜
数１０μｍの凝集粒子（凝集体）を形成し、更に凝集体
が三次元的に連結して広がっており、その結果、展色を
して評価した時に透過性を大きく低下させる原因となっ
ていた。又、反射色はこの顔料の屈折率が小さいことも
あり、概ね良好であるが、透過色の場合は上記理由によ
り全く光を透過しない状態であった。2. Description of the Related Art Cobalt phosphate pigments are dark purple pigments having good light fastness and heat resistance, and have been used mainly for paints. Conventionally, a cobalt phosphate pigment has been prepared by mixing and stirring an aqueous solution of a cobalt salt and an aqueous solution of a phosphate to form a precipitate of cobalt phosphate, aging the resulting blue-violet precipitation slurry, and then filtering. It is manufactured by washing with water, drying and firing at a high temperature of about 800 ° C. However, the cobalt phosphate pigment obtained by this conventional method has an agglomerated primary particles of 3 to 5 μm,
Agglomerated particles (aggregates) of several tens of μm are formed, and the aggregates are connected and spread three-dimensionally. As a result, when the coloration is evaluated, the permeability is greatly reduced. . The reflection color is generally good because the refractive index of the pigment is small, but the transmission color is in a state where light is not transmitted at all for the above-mentioned reason.
【０００３】こうした問題点を有するにも拘わらず、従
来のリン酸コバルト顔料は比較的分散レベルが緩い絵具
用としては充分に使用可能であったが、特に透過性を要
求される場合には使用不可能であった。また、粉砕によ
り顔料粒子を微細化し、透明性を上げることも検討され
たが、凝集体が堅牢で、耐衝撃性が悪いこともあり、粉
砕時に色相が変化し、色が薄くなるという問題があり、
根本的に問題を解決することが望まれていた。また、リ
ン酸コバルト顔料は、リン酸コバルトの沈殿そのものが
本質的に酸化物系や硫化物系の沈殿と異なって溶解積が
大きいことから、反応中に溶解析出を繰り返し、粒子が
大きくなり易い特徴を持っており、微粒子化が難しい顔
料であった。[0003] Despite these problems, the conventional cobalt phosphate pigments can be used sufficiently for paints having a relatively low dispersion level, but they can be used particularly when transparency is required. It was impossible. In addition, it has been considered to refine pigment particles by pulverization to increase transparency, but there is a problem that the aggregates are strong and the impact resistance is poor, so that the hue changes during pulverization and the color becomes lighter. Yes,
It was desired to solve the problem fundamentally. In addition, cobalt phosphate pigments have a large dissolution product, which is different from oxide-based or sulfide-based precipitates. It was a pigment that had characteristics and was difficult to make fine.
【０００４】[0004]
【発明が解決しようとする課題】上記事情に鑑み、本発
明者らは、リン酸コバルト顔料をより広範囲な用途、例
えば、該顔料が本来有している透明性を利用する分野や
透過性を重視する分野等に使用可能とすべくリン酸コバ
ルト顔料の製造方法を種々検討し、コバルト塩、リン酸
塩及びアルカリを特定な組み合わせで、沈澱媒体に同時
添加してリン酸コバルトの沈澱を生成させることによっ
て、より透明で微粒子のリン酸コバルト顔料が得られる
ことを見出し、この知見に基づいて本発明を完成した。SUMMARY OF THE INVENTION In view of the above circumstances, the present inventors have developed cobalt phosphate pigments for a wider range of applications, for example, in the field of utilizing the transparency inherent in the pigments and the transparency. Investigate various methods for producing cobalt phosphate pigments so that they can be used in fields where importance is placed, and add cobalt salts, phosphates and alkalis in a specific combination to the precipitation medium at the same time to form a precipitate of cobalt phosphate. By doing so, it was found that a cobalt phosphate pigment with more transparency and fine particles was obtained, and the present invention was completed based on this finding.
【０００５】[0005]
【課題を解決するための手段】上記の目的は以下の本発
明により達成される。即ち、本発明は、（イ）コバルト
塩とリン酸塩の混合水溶液と（ロ）アルカリ水溶液と
を、又は、（ハ）コバルト塩水溶液と（ニ）リン酸塩と
アルカリとの混合水溶液とを、同時に沈澱媒体に滴下し
てリン酸コバルトの沈殿を生成せしめ、熟成後、当該沈
殿物を濾過、水洗し、焼成することを特徴とする微粒子
リン酸コバルト顔料の製造方法である。The above objects are achieved by the present invention described below. That is, the present invention provides (a) a mixed aqueous solution of a cobalt salt and a phosphate and (b) an aqueous alkali solution, or (c) an aqueous solution of a cobalt salt and (d) a mixed aqueous solution of a phosphate and an alkali. A method for producing a fine particle cobalt phosphate pigment, comprising simultaneously dropping a precipitate into a precipitation medium to form a precipitate of cobalt phosphate, aging, filtering, washing and calcining the precipitate.
【０００６】[0006]
【発明の実施の形態】次に発明の実施の形態を挙げて本
発明を更に詳細に説明する。本発明でリン酸コバルト顔
料を製造するために使用するコバルト塩、リン酸塩及び
中和用アルカリは、該顔料の製造に従来から用いられて
いるものがいずれも使用可能であり、特に限定されな
い。コバルト塩としては、例えば、コバルトの硫酸塩、
塩化物、硝酸塩がいづれも使用可能である。又、リン酸
塩としては、例えば、リン酸水素二ナトリウム、リン酸
二水素ナトリウム、リン酸、ピロリン酸、トリポリリン
酸等が使用可能である。上記のナトリウム塩と同様にカ
リウム塩も使用可能である。又、中和用のアルカリとし
ては、通常使用される、例えば、水酸化ナトリウム、ソ
ーダ灰、重曹等が使用可能である。BEST MODE FOR CARRYING OUT THE INVENTION Next, the present invention will be described in more detail with reference to embodiments of the present invention. The cobalt salt, phosphate and neutralizing alkali used for producing the cobalt phosphate pigment in the present invention may be any of those conventionally used for producing the pigment, and are not particularly limited. . As the cobalt salt, for example, cobalt sulfate,
Both chloride and nitrate can be used. As the phosphate, for example, disodium hydrogen phosphate, sodium dihydrogen phosphate, phosphoric acid, pyrophosphoric acid, tripolyphosphoric acid and the like can be used. Potassium salts can be used as well as the sodium salts described above. As the alkali for neutralization, commonly used, for example, sodium hydroxide, soda ash, baking soda and the like can be used.
【０００７】本発明の特徴は、上記の原料を用いてリン
酸コバルトの沈澱を生成させる際に、（イ）コバルト塩
とリン酸塩の混合水溶液と（ロ）中和用のアルカリ水溶
液とを、又は、（ハ）コバルト塩水溶液と（ニ）リン酸
塩とアルカリの混合水溶液とを、沈澱媒体に同時に滴下
することである。沈澱媒体としては、通常、水が使用さ
れる。このようにして原料成分を沈澱媒体に同時に滴下
することによって、微細なリン酸コバルトの沈澱を生成
させることができる。[0007] A feature of the present invention is that, when a precipitate of cobalt phosphate is formed using the above raw materials, (a) a mixed aqueous solution of a cobalt salt and a phosphate and (b) an alkaline aqueous solution for neutralization are used. Or (c) simultaneously dropping an aqueous solution of a cobalt salt and (d) a mixed aqueous solution of a phosphate and an alkali onto a precipitation medium. Water is usually used as the precipitation medium. By simultaneously dropping the raw material components onto the precipitation medium in this manner, a fine precipitate of cobalt phosphate can be generated.
【０００８】その際、コバルト塩及びリン酸塩を所定の
化学量論量より過剰にすることにより、更に微細な沈殿
を生成させることができる。この場合のコバルト塩及び
リン酸塩の過剰量は、コバルト塩の場合８モル％以内が
適当であり、リン酸塩の場合は１０モル％以内が良好
で、それより多いと過剰量に対する効果が少なく無駄で
ある。どちらも過剰使用による効果があるが、コバルト
塩を過剰に使用する方が効果が大きい傾向にある。これ
らの塩の過剰分は、コバルト塩水溶液や上記の混合水溶
液に上記の過剰量となるように含ませることもできる
が、沈澱媒体に添加することもできる。後者の方が効果
的である。[0008] At this time, a finer precipitate can be formed by making the cobalt salt and the phosphate in excess of a predetermined stoichiometric amount. In this case, the excess amount of the cobalt salt and the phosphate is suitably within 8 mol% in the case of the cobalt salt, and is preferably within 10 mol% in the case of the phosphate. Less wasteful. Both have the effect of overuse, but the overuse of the cobalt salt tends to be more effective. The excess of these salts can be included in the aqueous cobalt salt solution or the above-mentioned mixed aqueous solution in the above-mentioned excess amount, but can also be added to the precipitation medium. The latter is more effective.
【０００９】沈澱温度は、特に限定されないが、通常、
室温〜７０℃の範囲である。又、沈殿ｐＨは３．５〜１
０．０の範囲が好ましく、ｐＨが低過ぎると生成した沈
殿が溶解し易くなり、また溶解析出も加速され粗大粒子
になり易くなる。又、ｐＨが高過ぎるとコバルトの水酸
化物の沈殿の生成が支配的となり、リン酸コバルト沈澱
の生成が難くなる。その結果、焼成により水酸化コバル
トが酸化コバルトへと変化し、得られるリン酸コバルト
顔料のくすみや黒化の原因となるので好ましくない。[0009] The precipitation temperature is not particularly limited.
The range is from room temperature to 70 ° C. The precipitation pH is 3.5 to 1
The range of 0.0 is preferable. If the pH is too low, the formed precipitate is easily dissolved, and the dissolution and precipitation are accelerated to become coarse particles. On the other hand, if the pH is too high, the formation of cobalt hydroxide precipitates becomes dominant, and the formation of cobalt phosphate precipitates becomes difficult. As a result, the cobalt hydroxide is changed to cobalt oxide by firing, which causes dullness and blackening of the obtained cobalt phosphate pigment, which is not preferable.
【００１０】生成したリン酸コバルトの沈澱は、沈澱媒
体中で、通常沈澱時の温度で、３０分〜２時間程度熟成
させ、未反応分を反応させると同時に粒子径を整えさせ
る。熟成後、沈澱を常法に従って濾過し、洗浄により水
可溶性成分を除去し、１００〜１３０℃程度の温度で乾
燥させることによりリン酸コバルト顔料の前駆体が得ら
れる。次いで該顔料の前駆体は焼成に付されるが、この
際の焼成温度は４５０〜７００℃が好ましく、より好ま
しくは４５０〜６００℃前後であり、高過ぎると微粒の
粒子同士が焼結し、透過性が著しく損なわれる。また、
低過ぎると充分な発色が得られない。The resulting precipitate of cobalt phosphate is aged in a precipitation medium at the temperature at the time of precipitation, usually for about 30 minutes to 2 hours, so that unreacted components are reacted and the particle size is adjusted. After aging, the precipitate is filtered by a conventional method, water-soluble components are removed by washing, and the precipitate is dried at a temperature of about 100 to 130 ° C. to obtain a precursor of a cobalt phosphate pigment. Next, the precursor of the pigment is subjected to calcination, the calcination temperature at this time is preferably 450 ~ 700 ℃, more preferably about 450 ~ 600 ℃, if too high, fine particles are sintered, The permeability is significantly impaired. Also,
If it is too low, sufficient color development cannot be obtained.
【００１１】以上の様にして得られた微粒子リン酸コバ
ルト顔料は従来よりソフトテキスチャーで分散し易く、
このままでも充分に要求に応えれられるが、更に性能を
向上させるには、易分散化されたことを利用して、上記
の該顔料前駆体を一度粉砕してから焼成するとよい。こ
れにより透過性は更に向上する。好ましい焼成温度は４
５０〜６００℃であり、更に好ましくは４７０〜５５０
℃である。又、焼成品（上記の該顔料前駆体を粉砕、焼
成したものも含む）を粉砕して再焼成すると、顔料前駆
体を粉砕する場合と同様に顔料は更に微粒子化され、透
過性が一段と向上する。焼成温度は上記と同様である。The fine particle cobalt phosphate pigment obtained as described above is easier to disperse with a soft texture than before,
Although it is possible to sufficiently meet the requirements as it is, to further improve the performance, the pigment precursor may be pulverized once and then fired, utilizing the fact that it is easily dispersed. Thereby, the transmittance is further improved. Preferred firing temperature is 4
50 to 600 ° C, more preferably 470 to 550.
° C. Further, when the calcined product (including the pigment precursor obtained by pulverizing and calcining the pigment precursor) is pulverized and recalcined, the pigment is further finely divided as in the case of pulverizing the pigment precursor, and the permeability is further improved. I do. The firing temperature is the same as above.
【００１２】[0012]
【実施例】次に実施例及び比較例を挙げて本発明を更に
具体的に説明する。尚、文中の部及び％は特に断りのな
い限り重量基準である。Next, the present invention will be described more specifically with reference to examples and comparative examples. The parts and percentages in the text are based on weight unless otherwise specified.
【００１３】実施例１ リン酸二水素ナトリウム４６．８部と中和用アルカリと
してのソーダ灰３３．２５部を水２５０部に溶解させ、
リン酸塩とアルカリの混合水溶液を調製した。一方、硫
酸コバルト１２６．５部を水２５０部に溶解させてコバ
ルト塩水溶液を調製した。次に、これらの水溶液の同時
添加を行うため、反応用ビーカーに沈殿水として５００
部の水を入れ、室温でｐＨ６にて、上記のリン酸塩とア
ルカリの混合水溶液とコバルト塩水溶液を同時に滴下
し、ｐＨ６を維持しつつ２０分間かけて滴下を終了し
た。Example 1 46.8 parts of sodium dihydrogen phosphate and 33.25 parts of soda ash as a neutralizing alkali were dissolved in 250 parts of water.
A mixed aqueous solution of phosphate and alkali was prepared. On the other hand, 126.5 parts of cobalt sulfate was dissolved in 250 parts of water to prepare a cobalt salt aqueous solution. Next, in order to perform simultaneous addition of these aqueous solutions, 500 mL of precipitation water was added to a reaction beaker.
Then, at pH 6 at room temperature, the above mixed aqueous solution of phosphate and alkali and aqueous solution of cobalt salt were simultaneously dropped, and the dropping was completed over 20 minutes while maintaining pH 6.
【００１４】次いで撹拌しながら、熟成を行い１時間後
に終了し、デカンテーションによる水洗に共した。この
際に沈殿スラリーの状態は青紫色からピンク色へと変化
し、ｐＨは６．０〜４．５まで低下した。熟成の終了し
た沈殿スラリーは、上澄み水の伝導度が３００μｓ／ｃ
ｍになるまで洗い、濾過した後、沈澱を１２０℃で１２
時間乾燥させ、顔料前駆体を得た。得られたピンク色の
顔料前駆体を５００℃で３０分〜１時間焼成し、目的と
する紫色の微粒子リン酸コバルト顔料を得た。Next, the mixture was aged while stirring, and after one hour, the operation was completed, followed by washing with water by decantation. At this time, the state of the precipitation slurry changed from blue-violet to pink, and the pH dropped to 6.0 to 4.5. The matured precipitate slurry has a supernatant water conductivity of 300 μs / c.
m, and after filtration, the precipitate was
After drying for a time, a pigment precursor was obtained. The obtained pink pigment precursor was calcined at 500 ° C. for 30 minutes to 1 hour to obtain the desired purple fine particle cobalt phosphate pigment.
【００１５】実施例２ 同時添加する際の滴下塩の組み合わせを、コバルト塩と
リン酸塩の混合水溶液とソーダ灰の水溶液とした以外は
実施例１と同様にして目的とする紫色の微粒子リン酸コ
バルト顔料を得た。Example 2 The objective purple fine particle phosphoric acid was prepared in the same manner as in Example 1 except that the combination of the dripped salts used for simultaneous addition was a mixed aqueous solution of a cobalt salt and a phosphate and an aqueous solution of soda ash. A cobalt pigment was obtained.
【００１６】実施例３ 焼成温度を７００℃とする以外は実施例１と同様にして
目的とする紫色のリン酸コバルト顔料を得た。Example 3 A target purple cobalt phosphate pigment was obtained in the same manner as in Example 1 except that the sintering temperature was 700 ° C.
【００１７】実施例４ コバルト塩の量を化学量論量より４モル％過剰とし、過
剰分を同時添加前に、予め沈殿水中に溶解しておく以外
は実施例１と同様にして目的とする紫色の微粒子リン酸
コバルト顔料を得た。Example 4 The objective was the same as in Example 1 except that the amount of the cobalt salt was 4 mol% excess from the stoichiometric amount, and the excess was dissolved in the precipitation water before the simultaneous addition. A purple particulate cobalt phosphate pigment was obtained.
【００１８】実施例５ リン塩の量を化学量論量より５モル％過剰とし、過剰分
を同時添加前に、予め沈殿水中に溶解しておく以外は実
施例１と同様にして目的とする紫色の微粒子リン酸コバ
ルト顔料を得た。Example 5 The objective was the same as in Example 1 except that the amount of the phosphate was 5 mol% excess from the stoichiometric amount, and the excess was dissolved in the precipitation water before the simultaneous addition. A purple particulate cobalt phosphate pigment was obtained.
【００１９】実施例６ 実施例１により得られたリン酸コバルト顔料前駆体を３
０部とり、分散剤としてクエン酸等のアニオン系分散剤
を顔料に対し０．３重量％添加し、水１００部に硝子ビ
ーズ３００部を加え、ペイントシェイカーにて２時間湿
式粉砕を行い、濾過後１２０℃にて１２時間乾燥し、得
られたものを５００℃で３０分〜１時間焼成し、目的と
する紫色の微粒子リン酸コバルト顔料を得た。Example 6 The cobalt phosphate pigment precursor obtained in Example 1
0 part, anionic dispersant such as citric acid as a dispersant is added in an amount of 0.3% by weight based on the pigment, 300 parts of glass beads are added to 100 parts of water, and wet grinding is performed for 2 hours by a paint shaker, followed by filtration. Thereafter, the resultant was dried at 120 ° C. for 12 hours, and the obtained product was baked at 500 ° C. for 30 minutes to 1 hour to obtain a desired purple fine particle cobalt phosphate pigment.
【００２０】実施例７実施例１で得られた微粒子リン酸
コバルト顔料を実施例６と同様にして湿式粉砕し、濾
過、乾燥、焼成し、目的とする紫色の微粒子リン酸コバ
ルト顔料を得た。Example 7 The fine particle cobalt phosphate pigment obtained in Example 1 was wet-pulverized, filtered, dried and calcined in the same manner as in Example 6 to obtain the desired purple fine particle cobalt phosphate pigment. .
【００２１】比較例１ リン酸二水素ナトリウム４６．８部と中和用アルカリと
してのソーダ灰３３．２５部を水２５０部に溶解し、リ
ン塩とアルカリの混合水溶液を調製した。一方、硫酸コ
バルト１２６．５部を水２５０部に溶解させてコバルト
塩水溶液を調製した。室温にて、上記のコバルト塩水溶
液にリン酸塩とアルカリの混合水溶液を投入し、良く撹
拌しながら１時間熟成を行った。この際生成した沈殿
は、初期の状態は青紫色のゲル状の沈殿であったが、時
間と共に徐々にピンク色に変化した。生成した沈殿その
ものは非常に凝集した状態であった。このものをデカン
テーションで水洗し、伝導度が３００μｓ／ｃｍまで洗
い、濾過し、１２０℃で１２時間乾燥させて顔料前駆体
を得た。次いで、このものを５００℃で３０分〜１時間
焼成し、紫色のリン酸コバルト顔料を得た。Comparative Example 1 46.8 parts of sodium dihydrogen phosphate and 33.25 parts of soda ash as a neutralizing alkali were dissolved in 250 parts of water to prepare a mixed aqueous solution of a phosphate and an alkali. On the other hand, 126.5 parts of cobalt sulfate was dissolved in 250 parts of water to prepare a cobalt salt aqueous solution. At room temperature, a mixed aqueous solution of a phosphate and an alkali was added to the above aqueous solution of the cobalt salt, and the mixture was aged for 1 hour with good stirring. The precipitate formed at this time was initially a blue-purple gel-like precipitate, but gradually changed to pink with time. The formed precipitate itself was in a very aggregated state. This was washed with water by decantation, washed to a conductivity of 300 μs / cm, filtered, and dried at 120 ° C. for 12 hours to obtain a pigment precursor. Next, this was fired at 500 ° C. for 30 minutes to 1 hour to obtain a purple cobalt phosphate pigment.
【００２２】以上のようにして得られたリン酸コバルト
顔料の透明性と透過性を評価するため、ペイントシェイ
カーにてメラミン・アルキッド樹脂１００部と各顔料の
それぞれ３０部（顔料３０ＰＨＲ）とを９０分間分散さ
せた。得られた分散物を黒帯付アート紙に３ミルアプリ
ケーターにて展色し、黒帯部分を光源のある側の上部か
ら観察して透明性を評価した。更に透過性を評価するた
めに、同様にしてＰＥＴフィルムに展色し、透過具合の
評価を行った。これらの評価結果を表１に示す。表１か
ら、本発明の方法で得られた微粒子リン酸コバルト顔料
は、従来の方法で製造した比較例の顔料に比べていづれ
も透明性、透過性、分散性が向上していることがわか
る。To evaluate the transparency and permeability of the cobalt phosphate pigment obtained as described above, 100 parts of melamine alkyd resin and 30 parts of each pigment (30 PHR pigment) were mixed with a paint shaker. Dispersed for minutes. The obtained dispersion was colored on art paper with black belt using a 3 mil applicator, and the black belt was observed from above the light source side to evaluate the transparency. In order to further evaluate the transmittance, the film was similarly colored on a PET film and the degree of transmission was evaluated. Table 1 shows the results of these evaluations. From Table 1, it can be seen that the fine particle cobalt phosphate pigment obtained by the method of the present invention has improved transparency, permeability, and dispersibility even when compared with the pigment of Comparative Example manufactured by the conventional method. .
【００２３】表 １ （顔料３０ＰＨＲ）Table 1 (Pigment 30PHR)
【００２４】[0024]
【発明の効果】以上の本発明によれば、透明性及び透過
性に優れた微粒子リン酸コバルト顔料が提供される。こ
れらの特性を活かして、本発明で得られる顔料は、一般
の顔料と同様に各種用途の着色剤や硝子の着色やメタリ
ック塗料の着色剤として使用可能である。According to the present invention described above, a fine particle cobalt phosphate pigment excellent in transparency and permeability is provided. Taking advantage of these properties, the pigment obtained in the present invention can be used as a coloring agent for various uses, a coloring agent for glass, and a coloring agent for metallic paints, like general pigments.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 寺田 裕美 東京都中央区日本橋馬喰町１−７−６ 大 日精化工業株式会社内 Ｆターム(参考） 4J037 AA08 CA14 CA22 EE26 EE29 EE33 EE43 EE46 FF02 FF08 FF13 FF22 ────────────────────────────────────────────────── ─── Continuing from the front page (72) Inventor Hiromi Terada 1-7-6, Nihonbashi Bakurocho, Chuo-ku, Tokyo Dai-Nissei Chemical Industry Co., Ltd. F-term (reference) 4J037 AA08 CA14 CA22 EE26 EE29 EE33 EE43 EE46 FF02 FF22 FF13 FF22
Claims (8)
溶液と（ロ）アルカリ水溶液とを、又は、（ハ）コバル
ト塩水溶液と（ニ）リン酸塩とアルカリとの混合水溶液
とを、同時に沈澱媒体に滴下してリン酸コバルトの沈殿
を生成せしめ、熟成後、当該沈殿物を濾過、水洗し、焼
成することを特徴とする微粒子リン酸コバルト顔料の製
造方法。1. An aqueous solution of a mixture of (a) a cobalt salt and a phosphate and (b) an aqueous solution of an alkali, or (c) an aqueous solution of a cobalt salt and (d) an aqueous solution of a mixture of a phosphate and an alkali. A process for producing a cobalt phosphate precipitate by dropping the precipitate at the same time into a precipitation medium to produce a precipitate of cobalt phosphate, aging, filtering, washing and calcining the precipitate.
ル％以内で過剰である請求項１に記載の微粒子リン酸コ
バルト顔料の製造方法。2. The method for producing a fine particle cobalt phosphate pigment according to claim 1, wherein the amount of cobalt used is excessive within 8 mol% of the stoichiometric amount.
％以内で過剰である請求項１に記載の微粒子リン酸コバ
ルト顔料の製造方法。3. The method for producing a fine particle cobalt phosphate pigment according to claim 1, wherein the amount of phosphorus used is excessive within 10 mol% of the stoichiometric amount.
０．０の範囲にある請求項１に記載の微粒子リン酸コバ
ルト顔料の製造方法。4. The precipitation pH at the time of simultaneous dropping is 3.5 to 1
2. The method for producing a particulate cobalt phosphate pigment according to claim 1, which is in the range of 0.0.
ある請求項１記載の微粒子リン酸コバルト顔料の製造方
法。5. The method for producing a particulate cobalt phosphate pigment according to claim 1, wherein the firing temperature is in the range of 450 ° C. to 600 ° C.
を粉砕し、４５０℃〜６００℃の範囲で焼成することを
特徴とする微粒子リン酸コバルト顔料の製造方法。6. A method for producing a fine particle cobalt phosphate pigment, comprising crushing the precipitate of cobalt phosphate according to claim 1 and calcining the precipitate at a temperature of 450 ° C. to 600 ° C.
微粒子リン酸コバルト顔料を粉砕し、４７０℃〜５５０
℃の範囲で焼成することを特徴とする微粒子リン酸コバ
ルト顔料の製造方法。7. A finely divided cobalt phosphate pigment obtained by the method according to claim 1 is pulverized, and is 470 ° C. to 550 ° C.
A method for producing a particulate cobalt phosphate pigment, characterized by firing at a temperature in the range of ° C.
法で得られる微粒子リン酸コバルト顔料。8. A fine particle cobalt phosphate pigment obtained by the method according to claim 1. Description:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000005925A JP2001048505A (en) | 1999-06-04 | 2000-01-07 | Production of particulate cobalt phosphate pigment |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP11-158548 | 1999-06-04 | ||
| JP15854899 | 1999-06-04 | ||
| JP2000005925A JP2001048505A (en) | 1999-06-04 | 2000-01-07 | Production of particulate cobalt phosphate pigment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2001048505A true JP2001048505A (en) | 2001-02-20 |
Family
ID=26485632
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2000005925A Pending JP2001048505A (en) | 1999-06-04 | 2000-01-07 | Production of particulate cobalt phosphate pigment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2001048505A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015502325A (en) * | 2011-12-21 | 2015-01-22 | ケミスケ ファブリック ブデンヘイム ケージー | Metal phosphate and its manufacturing process |
-
2000
- 2000-01-07 JP JP2000005925A patent/JP2001048505A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015502325A (en) * | 2011-12-21 | 2015-01-22 | ケミスケ ファブリック ブデンヘイム ケージー | Metal phosphate and its manufacturing process |
| US9653732B2 (en) | 2011-12-21 | 2017-05-16 | Chemische Fabrik Budenheim Kg | Metal phosphates and process for the preparation thereof |
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