• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Transparent, colored pigments based on platelet-shaped, transparent substrates, such as mica, talc or glass, are coated with colored metal oxides or metal hydroxides, wherein the metal oxide or hydroxide layer contains 0.1-5% by weight of an alkaline earth metal compound. These new, transparent, colored pigments are prepared by a process in which a platelet-shaped, transparent substrate, such as mica, talc or glass, is coated, in the presence of a base, with a colored metal oxide or hydroxide, and 0.1 to 5% by weight of an alkaline earth metal oxide or hydroxide is incorporated in the layer. The pigments have improved dispersibility, gloss, color power and stability to heat and weathering and also filling and adhesion properties. The pigments can be used for all the customary purposes, especially in cosmetics.
    公开号:SU1466651A3
    申请号:SU823506790
    申请日:1982-10-25
    公开日:1989-03-15
    发明作者:Ватанабе Такайи；Ногуши Тамио
    申请人:Мерк Патент Гмбх (Фирма)；
    IPC主号:
    专利说明:

    one ,
    This invention relates to the preparation of a clear colored pigment based on a flaky transparent substrate, on which oxides or hydroxides of coloring metals are deposited.
    The purpose of the invention is to increase the heat resistance of a pigment and improve its dispersibility.
    According to the method of obtaining a transparent colored pigment, in which a chewy, transparent substrate in an aqueous suspension in the presence of an alkaline agent, oxide or hydroxide of the coloring metal is removed from its salt and after that the precipitate is separated, washed, dried and calcined, osacterized
    metal oxides or metal hydroxides are given in the presence of a magnesium salt, taken in an amount of 0.9-4.1 wt. in the calculation of the precipitated oxide, and as the alkaline agent use urea.
    B quality scaly transparent
    I substrates are mica, e.g. muscovite, sericite or phlogopite, talcum scale. These substrates
     typically used in video, particles of a size of the order of 1-100 µm, preferably of a size of the order of 5-50 µm.
    As non-ferrous metal oxides or metal hydroxides, for example, FeO (OH), Fe (OH), Fe (OH) h, Co (OH), Cr (OH) g,

    but
    Q5
    but
    SP
    s
    at
    , CoO or, R may colorless metal oxides, for example, ZrO or TiO, if necessary, may precipitate out.
    All of these metal oxides or metal hydroxides can be p-layers, either individually or together, and mixtures of oxides of these metals can be composed. However, it is decisive that the pigment contains 0.9-4.1 wt.% Of magnesium oxide. With a content of less than 0.9% by weight of magnesia, good results are not obtained. With a content of more than 4.1% by weight, the properties are not improved.
    To obtain the pigment according to the invention, a scaly, transparent substrate is suspended in an aqueous solution which contains at least one metal salt and a magnesium salt. Suitable metal salts for the formation of non-ferrous oxides or hydroxides are, for example, FeSO, FeCl, Fe (NH4) a (S04) 7, Fe (NO3) a, Fe5 (804) 3, FeClj, FeNH4 (S04 2, Fe (N05) 3, CoCl,, CoSo, CoCNOj), CrClj, CrNH4 (S04) i. As metal salts which are suitable for further deposition, if necessary, the precipitations are colorless with metal oxides, for example, AliCSO), A1NH4: (S04) 4, AlNaCSO), AIKCSO). ZnCli, ZnS04, TiOSO, TiCl4. Suitable magnesium salts are, for example, MgS04, MgCNO,), MgCl, MgBr, MgJ. In particular, MgS04, MgCl are mainly used.
    All these metal solts and magnesium salts can be used in combination with each other, and especially when coating with color oxides or hydroxides, the ratios of different metal salts and the weight ratio of coating to substrate according to the desired color can be freely chosen.
    Prepare a 5-25% slurry substrate suspension in a solution of metal salts, which contains about 9 x
     X
     metal salts
    1 m covered surface subX
    on
    stratum. When the base is added, the salts are hydrolyzed and the metals, including magnesium, are deposited on the substrate in the form of hydroxides. Urea is used as a base, which is converted by hydrolysis to
    4666514
    ammonia. Urea is particularly preferred, since particularly small sizes of hydrated metal oxide particles deposited on the substrate can be achieved here, and thus the transparency of the products is especially good. In addition, thanks to urea, Q is achieved in particular, homogeneous precipitation of metal oxide hydrates on the substrate. Urea is added in an amount of about 3-30 equivalents of urea, calculated as metal oxides, and the suspension is boiled for 0.5-5 hours.
    Thus, for example, magnesium hydroxide, iron (II) hydroxide, iron (III) hydroxide, cobalt hydroxide, chromium hydroxide 20 "aluminum hydroxide, zinc hydroxide, titanium hydroxide, titanium hydroxide or iron hydroxide precipitates. After the precipitation is complete, the products are separated, washed and dried 25 at 100-120 ° C. Next, calcining is carried out, for example, which is carried out at 400-900 ° C for about 0.5-5 hours and at which the hydroxides or hydrates of the hydroxides are converted into oxides.
    Since the metal oxides named, with the exception of aluminum, zinc and titanium, are colored by choosing the type of metal oxides or by choosing the ratio of mixtures of different metal oxides, different colors can be obtained, for example, red, yellow, blue, green and black. , as well as neutral colors, Q and so many shades.
    To obtain a yellow, transparent pigment, a 5-25% aqueous suspension of flaky substrate 45 is prepared, which contains in the form of a solution 10-150 hours, mostly about 30-90, iron salt, 1-50 hours, mostly 2-30, salts magnesium and Yu-400 hours, mainly 30-270, urea and 5Q, in each case converted to 100 hours of substrate, the suspension is boiled for 0.5-5 hours, after which a yellow pigment can be obtained by separating, proming and drying
    55 at a temperature of about lOS-IIO C.
    By treatment at 300-1200 ° C, preferably 400-900 ° C, a red, transparent pigment can be obtained from this pigment.
    thirty
    ZB
    51466651
    To obtain a black, transparent pigment, a 5–25% scaly substrate is prepared, which keeps dissolved 50–300 hours, preferably 150–250, iron salts, 3–90 hours, mainly magnesium salts, 25–1500 hours, mainly 75-1000, urea and 2.5-90 hours, mainly 8-75, potassium nitrate in each case recalculated for 100 hours of the substrate. After boiling for 0.5-5 hours, separating, washing and drying at 100-100 ° C, a black, transparent pigment is obtained.
    To obtain a green, transparent pigment, a 5-25% aqueous suspension of a scaly substrate is prepared, which contains
    wa 11 li g ho
    out of 18
    ten
    20-200 hours, preimz (T 40%, 150-150, cobalt salts, 20-200 hours, mainly AO-150, aluminum salts, 7-60 hours, mainly 10-30, magnesium salts and 100-80 hours, mainly 200-450 urea, in each case recalculated to 100 parts of the substrate. After boiling for 0.5-5 hours, separation, washing and placing of the
    what is
    15 right ave
    of
    20 sou 90 90 10 to
    a temperature of about 120 ° C and calcining at a temperature of about 500-700 ° C, a green transparent pigment is obtained.
    By calcining at 800-1200 ° C, a blue, transparent pigment is obtained from this pigment.
    The resulting pigments are excellent in terms of dispersibility, luminance, color, transparency and heat resistance, and can be used for many uses, especially in cosmetics. Example. A solution consisting of 55 g of ammonium iron (III) ammonium sulfate, magnesium oxide sulphate and 80 g of urea per 900 ml of water, in which 90 g of mica suspended in particles of 1-10 microns is heated to 95-98 C for 1 hour. After that, the product is separated, washed with water and dried at 105-110 C. A yellow colored iron oxide hydroxide pigment is obtained, which has good clarity and dispersibility.
    EXAMPLE 2 A solution consisting of 7.5 g of ammonium iron (III) sulfate, 1.5 g of magnesium sulfate and 20 g of urea per 100 ml of water, in which 10 suspensions are suspended for 1 called product sluts, industrial30
    g of talc, heated to 95-98 s. Obra fi 8 cha pr
    by t pr
    of
    35 sou 90 90 10 - up to
    40 mga nor topr
    1 cr
    of
    50 sul 30 that ra
    55 fi soo 11 more than one
    45

    They are watered with water and dried at 105-110 C. The pigment formed, as applied to talcum powder, ferric oxide hydroxide g is yellow in color and has good dispersibility.
    PRI me R 3. A solution consisting of 80 g of ammonium iron sulfate (til), 18 g of magnesium sulfate and 162 g of urea per 90 ml of water, which contains suspended 90 g of mica particles 1-10 microns in size, is heated in those of
    ten
    1 hour to 95-98 C. The product is separated, washed with water and dried
    15 at 105-110 ° C. The resulting pigment is yellow-ocher in color and has horoschto transparency and dispersibility.
    PRI me R 4. A solution consisting of 64 g of iron (III) chloride, 13 g
    20 mg of magnesium sulfate and 128 g of urea per 90 ml of water, in which 90 g of mica with a particle size of 1–10 µm are dispersed, are heated for 2 hours to 95–98 ° C. After this solution from,
    thirty
     filtered, washed and dried for 8 hours at 105-110 0. A yellow ocher pigment is obtained with good transparency and dispersibility.
    PRI me R 5. The pigment obtained in example 4, is calcined for t hours, at. A red, transparent pigment is obtained. .
    Example 6. A solution consisting of 128 g of iron (III) chloride, 26 g
    35 magnesium sulphate and 256 g of urea per 900 ml of water, in which 90 g of mica with a particle size of 1-10 microns are dispersed, is heated for 2 hours. - up to 95-98 ° C. After filtration, drying with water and drying for 8 hours at 105-110 ° C, a yellow-brown pigment with good transparency and dispersibility is obtained.
    PRI me R 7. The pigment obtained in Example 6 is calcined for 1 hour at 700 ° C. A violet red transparent pigment is obtained.
    PRI me R 8. A solution consisting of 178 g of iron (II) sulfate, 40 g
    50 mg of magnesium sulphate 32 g of potassium nitrate and 300 g of urea per 900 ml of water, in which 80 g of mica with a particle size of 1-10 μm are dispersed, are heated to 95-98 ° C for 4 hours. After.
    55 filtering, washing with water and drying for 10 hours at 105-110 ° C produce a black pigment with good transparency and dispersibility.
    45
    EXAMPLE 9 A solution consisting of 3.0 g of aluminum chloride, g of cobalt chloride, 1.0 g of magnesium sulphate and 20 g of urea per 60 ml of water, which contains particles of SjO g dispersion with particle size 1 -10 µm, warmed for 2 hours. The product is filtered, washed with water and dried for 2 hours at 105-1. After calcining the resulting whitish product at 600 ° C. for 1 hour, a transparent pigment is obtained.
    Example 10. The whitish pigment obtained in Example 9 is calcined for 1 hour at. A blue, transparent pigment is obtained.
    PRI me R 11. PacTBops consisting of 20 g of iron (III) chloride in 300 ml of water, which contains dispersed 30 g of mica with a particle size of 1-10 microns, is heated to 78-82 ° C for 1 hour and after that, they are mixed for 85 hours with 85 ml of 10% sodium alkali. To a solution that has a pH value of 2.3, a 6% solution of calcium chloride is added over 5 minutes and then an amount of 10% sodium alkali is needed to achieve a neutral pH. The product is separated, washed with water and dried for 2 hours at 105-110 ° C. After calcining for 1 hour, a red, transparent pigment is obtained.
    Example 12. A solution consisting of 3.0 g of chromium (III) sulfate, 1.0 g of magnesium sulfate and 10.0 g of urea per 150 ml of water, which contains dispersed 10 g of mica with a particle size of 1- 10 µm, heated for 0.5 h to 95-98 0. The product is filtered, washed with a Veda and dried, for 5 h at 98-105 C. After calcining the light green product for 1 h at 800 ° C, get blue - green, transparent pigment.
    EXAMPLE 13 A solution consisting of 2.0 g of zinc chloride, 2.0 g of iron (III) chloride, 1.0 g of magnesium sulfate and 20 g of urea per 100 ml of water, which contains 5 dispersed, 0 g of mica with a particle size of 1-10 microns, is heated for 1 h to 95-98 C. The product is filtered, washed with water and dried for 10 h at 98-105 ° C. After cal
    Curing the product for 1 hour gives a yellow ocher color, a transparent pigment.
    PRI me R 14. Suspensions of 5 g of mica with a particle size of 1-10 microns in 50 ml of water are heated for 0.5 h to 95-98 C and then mixed with a solution consisting of 20 g of titanium sulphate, 4 g of magnesium sulphate and 40 g of urea in 100 ml of water and stirred for 1 hour. After calcining the whitish product thus obtained at 800 ° C for 1 hour,
    transparent pigment with blue-green terferentsionny color.
    in
    EXAMPLE 15 A solution consisting of 55 g of ammonium iron sulfate (111) 9 g of magnesium chloride and 80 g of urea per 900 ml of water, in which 90 g of mica is suspended, the size of particles 1-15 microns, is heated for 3 h before C. After that, the product is separated, washed with water and dried at 105-G | 0 ° C. A yellow-colored iron oxide hydroxide pigment is obtained, which has good transparency and dispersibility.
    PRI me R 16. A solution consisting of 45 g of ammonium iron (III) sulfate 5 12 magnesium bromide and 70 g of urea per 800 ml of water, in which 90 g of mica substrate suspended with a particle size of 1-15 µm, The mixture is heated to 95-98 ° C for 3 hours. The resulting product is separated, splashed with water and dried at 105 °. The resulting pigment has a yellow iron hydroxide color and has good dispersibility and transparency.
    Example 17. A solution consisting of 60 g of ammonium ferric (III) ammonium sulfate, 10 g of magnesium nitrate and 80 g of urea per 700 ml of water in which 90 are suspended. G of mica, 1-15 µm in size, is heated for 3 hours to 95-98 ° C. The product is separated, washed with water and dried at 10555
    110 C. The yellow pigment formed has a good transparency and dispersibility. .
    The data for examples on the content of magnesium oxide in the resulting pigments are as follows:
    Below are examples for comparison, proving the achievement of the objectives of the invention.
    Comparative Example 1. A solution consisting of 128 g of iron (III) chloride and 256 urea per 900 ml of water, which contains dispersed 90 g of mica with a particle size of 1-10 µm, is heated for 2 hours to 95-98 ° C. After filtering washing with water, drying for 8 hours at 105-110 ° C, and calcining for 1 hour. A violet red pigment is obtained. The dispersibility of this product is compared with the product of Example 7 by the following 11 {method. Into a 300-milliliter beaker are introduced 45 g of a conventional varnish base (VS medium ink) and 5.0 of the corresponding pigment is added with stirring at a speed of 500 rpm. In each case, after 5, 10, 30, and 60 minutes, the samples are removed and applied to the coated paper, which has a white and black base. Based on the samples thus obtained, it is possible to assess the dispersibility of the corresponding pigment. While the pigment in Example 7 is very well dispersible after 5 minutes, the compared pigment is not sufficiently dispersible even after 60 minutes.
    Comparative Example 2. A solution consisting of 178 g of iron (I) sulfate, 32 g of potassium nitrate and 300 g of urea per 900 ml of water, which contains dispersed 80 g of mica, with a particle size of 1-10 microns, is heated for 4 h to 95-98 s, then the product is filtered, washed with water and dried in a te0
    five
    0
    0 5 0 5 0
    g
    10 hours at 98-105 ° С. The heat resistance and stability against oxidation of these samples are determined by measuring the TgA and DTA values on a Shinku-Rikoh Kabushiki Kaisch instrument, model AgNE, TVD-1500. TdA and DTA change at 155 ° C, and the color tone of the pigment changes from black to reddish brown, with the transformation of FejO c. In comparison with this, the pigment obtained in Example 8, which contains magnesium, does not detect any change to 260 ° C.
    Comparative example 3. The pigments of example 8 and ntf are prepared for comparative example 2. The dispersibility of these products is compared by the following method: In a 300 ml beaker, 45 g of a conventional varnish base (VS medium ink) and 5.0 g are added. the corresponding pigment is added with stirring at a speed of 500 rpm. Each time after 4.8, 15 and 60 minutes, the samples are removed and applied to the coated paper, which has a white and black base. On the basis of the samples thus obtained, it is possible to estimate the dispersibility of the corresponding pigment. While the pigment in Example 8 is very well dispersed after 8 minutes, the compared pigment is still dispersible even after 60 minutes.
    Comparative example 4. The pigments of example 7 and comparative example 1 are obtained. The heat resistance and oxidation stability of these samples are compared by the methods of DTA and TPA. It was shown that the pigment according to example 7 does not undergo changes up to 250 s. In contrast, the pigment for comparison gives the change on the analytical curve already at.
    Dp proofs of the best dispersibility of the proposed pigments are done as follows. The pigments according to example 7 and comparative example 1 are made, they are applied a lacquer base and applied to the paper. . After that, discernable within a certain area of macroscale (agglomerates) are calculated. The results were obtained, and are shown in the table.
    eleven
    U6665112
    In the cosmetic thus obtained, the proposed pigment has better transparency and better filling and adhesion properties than the used pigments of iron oxide.
    From the obtained digital values, it can be seen that the proposed pigments are dispersed much better.
    An example of application. The composition of the compact powder for use, wt.%: The pigment according to example 5.30 Talc52,5
    Kaolin3
    Calcium stearate 5 Grain starch 3 RTzopropyl Laurate 5 Isopropyl myristate ti Perfume0,5
    权利要求:
    Claims (1)
    [1]
    Invention Formula
    five
    five
    The method of obtaining a transparent colored pigment based on a scaly-frequent transparent substrate - mica or talc, including the deposition of oxide or hydroxy-dye staining of metals on the substrate particles by treating them with an alkaline agent, separating the precipitate formed, washing it 0 and heat treating it so that, in order to increase the heat resistance of the pigment and improve its dispersibility, precipitation is carried out in the presence of a magnesium salt, - taken in an amount of 0.9–4.1 wt.% oxide, and as an alkaline agent, urethane is used.
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    PL238729A2|1983-06-20|
    KR870001881B1|1987-10-20|
    AU561659B2|1987-05-14|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    JP56170148A|JPH0160511B2|1981-10-26|1981-10-26|
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