CN115710434A - White pearlescent pigment and preparation method and application thereof - Google Patents
White pearlescent pigment and preparation method and application thereof Download PDFInfo
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- CN115710434A CN115710434A CN202211428251.0A CN202211428251A CN115710434A CN 115710434 A CN115710434 A CN 115710434A CN 202211428251 A CN202211428251 A CN 202211428251A CN 115710434 A CN115710434 A CN 115710434A
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- 239000000049 pigment Substances 0.000 title claims abstract description 75
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 63
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 59
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 55
- 239000004332 silver Substances 0.000 claims abstract description 55
- 229910052709 silver Inorganic materials 0.000 claims abstract description 55
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 48
- 239000010703 silicon Substances 0.000 claims abstract description 48
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 33
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 30
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 16
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims description 116
- 239000006185 dispersion Substances 0.000 claims description 39
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 239000007787 solid Substances 0.000 claims description 28
- 239000010445 mica Substances 0.000 claims description 16
- 229910052618 mica group Inorganic materials 0.000 claims description 16
- 239000000463 material Substances 0.000 claims description 14
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 13
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 13
- ZXAUZSQITFJWPS-UHFFFAOYSA-J zirconium(4+);disulfate Chemical compound [Zr+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O ZXAUZSQITFJWPS-UHFFFAOYSA-J 0.000 claims description 13
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 12
- 239000004115 Sodium Silicate Substances 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 12
- 239000008103 glucose Substances 0.000 claims description 12
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 10
- 230000003213 activating effect Effects 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 230000004913 activation Effects 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 7
- 239000012190 activator Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- RJDOZRNNYVAULJ-UHFFFAOYSA-L [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[F-].[F-].[Mg++].[Mg++].[Mg++].[Al+3].[Si+4].[Si+4].[Si+4].[K+] RJDOZRNNYVAULJ-UHFFFAOYSA-L 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 239000002537 cosmetic Substances 0.000 claims description 4
- IPCAPQRVQMIMAN-UHFFFAOYSA-L zirconyl chloride Chemical compound Cl[Zr](Cl)=O IPCAPQRVQMIMAN-UHFFFAOYSA-L 0.000 claims description 4
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 239000011521 glass Substances 0.000 claims description 3
- 239000002304 perfume Substances 0.000 claims description 3
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 3
- 239000001119 stannous chloride Substances 0.000 claims description 3
- 235000011150 stannous chloride Nutrition 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract description 28
- 238000000576 coating method Methods 0.000 abstract description 16
- 239000004408 titanium dioxide Substances 0.000 abstract description 14
- 239000011248 coating agent Substances 0.000 abstract description 13
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- 230000006750 UV protection Effects 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 102
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
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- 238000005054 agglomeration Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 3
- XFVGXQSSXWIWIO-UHFFFAOYSA-N chloro hypochlorite;titanium Chemical compound [Ti].ClOCl XFVGXQSSXWIWIO-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
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- 206010028980 Neoplasm Diseases 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical group [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a white pearlescent pigment and a preparation method and application thereof, and relates to the technical field of pigments. The white pearlescent layer comprises a substrate and a white pearlescent layer coated on the surface of the substrate, wherein the white pearlescent layer comprises at least two of a zirconium-containing pearlescent layer, a silicon-containing pearlescent layer and a silver-containing pearlescent layer. By utilizing the different refractive indexes of the zirconium dioxide, the silicon dioxide and the silver and selecting at least two of the zirconium dioxide, the silicon dioxide and the silver as the raw materials of the white pearlescent layer, the white pearlescent pigment with good glossiness and good light reflection effect can be prepared without adding titanium dioxide, and simultaneously, the pearlescent pigment has better ultraviolet resistance, and the glossiness of the pearlescent pigment can be further improved by adding the silver. The white pearlescent pigment obtained by coating at least two of the zirconium-containing pearlescent layer, the silicon-containing pearlescent layer and the silver-containing pearlescent layer on the surface of the substrate is safe and has good glossiness, and can be safely and permanently applied to daily chemical products.
Description
Technical Field
The invention relates to the technical field of pigments, in particular to a white pearlescent pigment and a preparation method and application thereof.
Background
The pearlescent pigment is widely applied to industries such as cosmetics, plastics, printing ink, artificial leather, wallpaper, enamel, ceramics, architectural coatings and the like. The preparation of pearlescent pigments, especially white pearlescent pigments, currently relies primarily on the use of titanium dioxide, the thickness of which can affect the pearlescent effect.
However, with the improvement of living standard and the increasing progress of science and technology, the research on titanium dioxide is also deepened gradually. Through long-term research, people find that the use of titanium dioxide or the relation between titanium dioxide and cancer, along with the gradual deepening of research, more and more industries start to limit the use and the use amount of titanium dioxide, and the most prominent is in the field of daily chemical products. More and more laws and regulations are beginning to limit the use or content of titanium dioxide in daily chemical products, but the demand for pearlescent pigments in daily chemical products is not reduced, so that the proposal of a new formulation and preparation method of pearlescent pigments is a technical problem to be solved urgently by those skilled in the art.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a white pearlescent pigment, a preparation method and application thereof, which is a novel white pearlescent pigment without titanium dioxide and has good pearlescent degree.
The invention is realized by the following steps:
in a first aspect, the present invention provides a white pearlescent pigment, which comprises a substrate and a white pearlescent layer coated on the surface of the substrate, wherein the white pearlescent layer comprises at least two of a zirconium-containing pearlescent layer, a silicon-containing pearlescent layer and a silver-containing pearlescent layer.
In an alternative embodiment, the white pearlescent layer is a multilayer structure formed alternately, the multilayer structure is at least 3 layers, and the multilayer structure comprises at least two of a zirconium-containing pearlescent layer, a silicon-containing pearlescent layer, and a silver-containing pearlescent layer.
Preferably, the multilayer structure is at least 4 layers.
In an alternative embodiment, the substrate comprises at least one of mica, glass, alumina, and silica.
The mica includes natural mica or synthetic mica.
The particle size of the base material is 5-45 μm, and the average particle size is 25-30 μm.
In a second aspect, the present invention provides a method for preparing a white pearlescent pigment according to any one of the preceding embodiments, which comprises placing a substrate or a solid containing the substrate in a solution to react at least twice, and the solution of each reaction is different from the solution of the previous reaction, and the solution of each reaction comprises any one of a zirconium-containing solution, a silicon-containing solution or a silver-containing solution.
In an alternative embodiment, the method comprises the steps of placing a substrate in water for activation treatment to obtain a first dispersion, adding a zirconium-containing solution into the first dispersion for a first reaction, adding a silicon-containing solution for a second reaction, adding a zirconium-containing solution for a third reaction, collecting a solid containing the substrate after the third reaction, placing the solid containing the substrate in water again to obtain a second dispersion, and adding a silver-containing solution into the second dispersion for a fourth reaction.
In an alternative embodiment, the zirconium-containing solution added in the first reaction and the third reaction is any one of zirconium sulfate and zirconyl chloride; preferably, the zirconium dioxide content of the zirconium-containing solution is 4 to 6g/L.
Preferably, the ratio of the mass of the substrate to the volume of water in the first dispersion is between 0.8 and 1.2g:18 to 22ml.
Preferably, in the first reaction, the volume ratio of the water in the first dispersion to the zirconium-containing solution is 1.8 to 2.2:0.28 to 0.32.
Preferably, in the third reaction, the volume ratio of the water in the first dispersion to the zirconium-containing solution is 1.8 to 2.2:0.30 to 0.35.
Preferably, the temperature of the first reaction and the third reaction is 75-80 ℃, and the pH of the reaction liquid is 2-3.
Preferably, the reaction time after the zirconium-containing solution is added in the first reaction and the third reaction is 20 to 40min.
Preferably, the preparation of the solid containing the substrate comprises filtering the reaction solution after the third reaction, and sequentially washing, drying and calcining the solid.
Preferably, the drying temperature is 100-120 ℃, and the drying time is 10-15 h.
Preferably, the calcining temperature is 750-800 ℃, and the calcining time is 20-40 min.
In an alternative embodiment, the silicon-containing solution comprises any one of sodium silicate, sodium metasilicate.
Preferably, the silicon content of the silicon-containing solution is 10 to 30%.
Preferably, the volume ratio of water to the silicon-containing solution in the first dispersion is 1.8-2.2: 0.4 to 0.6.
Preferably, the reaction temperature of the second reaction is 75-80 ℃, the pH of the reaction solution is 7.5-8.5, and the reaction time after the silicon-containing solution is added is 20-40 min.
In an alternative embodiment, the silver-containing solution is a silver ammonia solution, and preferably, the silver content in the silver ammonia solution is 0.5-2%.
Preferably, the volume ratio of the water in the second dispersion liquid to the silver-ammonia solution is 1.8-2.2: 0.01 to 0.1.
Preferably, the ratio of the mass of the solid containing the substrate to the volume of water in the second dispersion is 0.8 to 1.2g:18 to 22ml.
Preferably, the reaction temperature of the fourth reaction is 40 to 60 ℃, and the pH of the reaction solution is 6.8 to 7.2.
Preferably, the reaction is carried out for 8-12 min after the silver ammonia solution is added, and then the glucose solution is added into the reaction solution.
Preferably, the concentration of glucose in the glucose solution is between 0.8 and 1.2%.
In an alternative embodiment, the activating comprises adding an activating agent to the water to activate the substrate, the activating agent comprising any one of tin tetrachloride, stannous chloride.
Preferably, the tin tetrachloride has a tin content of 8 to 12%.
Preferably, the volume ratio of the activator to the water in the first dispersion is from 0.04 to 0.06:1.8 to 2.2.
Preferably, the reaction temperature for activation is 60 to 70 ℃ and the pH of the reaction solution is 1 to 2.
In a third aspect, the present invention provides a use of the white pearlescent pigment according to any one of the preceding embodiments or the white pearlescent pigment prepared by the preparation method according to any one of the preceding embodiments in the field of daily use chemical products.
Preferably, the daily use chemical product comprises a cosmetic or perfume.
The invention has the following beneficial effects:
the invention provides a white pearlescent pigment and a preparation method and application thereof, wherein when a zirconium-containing pearlescent layer is coated on the surface of a substrate, zirconium dioxide is used as a main pearlescent element to reflect light; when the silicon-containing pearlescent layer is coated on the surface of the substrate, silicon dioxide is used as a main pearlescent element to reflect light, at least two of zirconium dioxide, zirconium dioxide and silver are selected as raw materials of the white pearlescent layer by utilizing different refractive indexes of the zirconium dioxide, the zirconium dioxide and the silver, so that white pearlescent pigment with good glossiness and good light reflection effect can be prepared without adding titanium dioxide, and the glossiness of the pearlescent pigment can be further improved by adding the silver. The white pearlescent pigment obtained by coating at least two of the zirconium-containing pearlescent layer, the silicon-containing pearlescent layer and the silver-containing pearlescent layer on the surface of the substrate is safe and has good glossiness, and can be safely and permanently applied to daily chemical products.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a scanning electron microscope photograph of a cross-section of a white pearlescent pigment provided in example 1 of the present invention;
FIG. 2 is a scanning electron microscope photograph of the surface of a white pearlescent pigment provided in example 1 of the present invention;
FIG. 3 is a picture of a white pearlescent pigment provided in example 1 of the present invention after spraying;
FIG. 4 is a photograph of a plastic article coated with a white pearlescent pigment according to example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In a first aspect, the invention provides a white pearlescent pigment, which comprises a substrate and a white pearlescent layer coated on the surface of the substrate, wherein the white pearlescent layer comprises at least two of a zirconium-containing pearlescent layer, a silicon-containing pearlescent layer and a silver-containing pearlescent layer.
For example, the white pearlescent layer may be a zirconium-containing pearlescent layer and a silicon-containing pearlescent layer, or a zirconium-containing pearlescent layer and a silver-containing pearlescent layer, or a silver-containing pearlescent layer and a silicon-containing pearlescent layer, or a structure having a zirconium-containing pearlescent layer, a silicon-containing pearlescent layer and a silver-containing pearlescent layer. It should be noted that, when two or three of the zirconium-containing pearlescent layer, the silicon-containing pearlescent layer and the silver-containing pearlescent layer are selected in the embodiment, each pearlescent layer may be one or more layers, for example, when the white pearlescent layer is a zirconium-containing pearlescent layer and a silicon-containing pearlescent layer, the zirconium-containing pearlescent layer may have one layer or more layers, and the silicon-containing pearlescent layer may also have one layer or more layers.
When the zirconium-containing pearlescent layer is coated on the surface of the substrate, zirconium dioxide is used as a main pearlescent element to reflect light; when the silicon-containing pearlescent layer is coated on the surface of the substrate, silicon dioxide is used as a main pearlescent element to reflect light, at least two of the silicon dioxide, the zirconium dioxide and the silver are selected as raw materials of the white pearlescent layer by utilizing different refractive indexes of the zirconium dioxide, the zirconium dioxide and the silver, so that the white pearlescent pigment with good glossiness and good light reflection effect can be prepared without adding titanium dioxide, and the glossiness of the pearlescent pigment can be further improved by adding the silver. The white pearlescent pigment obtained by coating at least two of the zirconium-containing pearlescent layer, the silicon-containing pearlescent layer and the silver-containing pearlescent layer on the surface of the substrate is safe and has good glossiness, and can be safely and permanently applied to daily chemical products.
In an alternative embodiment, in order to improve the glossiness of the pearlescent pigment, the white pearlescent layers are of a multilayer structure formed alternately, and the difference of the refractive indexes of the raw materials in each pearlescent layer can be fully utilized to generate a better pearlescent effect. The multilayer structure is at least 3 layers, and the multilayer structure comprises at least two of a zirconium-containing pearlescent layer, a silicon-containing pearlescent layer and a silver-containing pearlescent layer.
Preferably, the multilayer structure is at least 4 layers.
Preferably, in order to obtain the white pearlescent pigment with better glossiness and light reflection effect, the white pearlescent layer has a 4-layer structure and comprises a zirconium-containing pearlescent layer, a silicon-containing pearlescent layer, a zirconium-containing pearlescent layer and a silver-containing pearlescent layer which are coated outwards in sequence along the surface of the substrate.
Because the refractive indexes of the zirconium dioxide, the silicon dioxide and the silver are different, the refractive index of the zirconium dioxide is the highest, and the refractive index of the silicon dioxide is the lowest, and a process from high to low to high in refractive index is generated when the surface of the base material is coated with the white pearlescent layer, so that the reflectivity of light on the surface of the pearlescent pigment is improved, and the pearlescent effect is shown. In addition, the refractive index is changed in the coating process from the zirconium-containing pearlescent layer to the silver-containing pearlescent layer, so that the silver-containing pearlescent layer can directly improve the glossiness of the white pearlescent pigment, and the light reflectivity of the white pearlescent pigment can be improved through the difference of the refractive indexes of two adjacent pearlescent layers.
In an alternative embodiment, the substrate comprises at least one of mica, glass, alumina, and silica.
The mica includes natural mica or synthetic mica.
The particle size of the base material is 5-45 μm, and the average particle size is 25-30 μm.
In a second aspect, the present invention provides a method for preparing a white pearlescent pigment according to any one of the preceding embodiments, which comprises placing a substrate or a solid containing the substrate in a solution to react at least twice, and the solution of each reaction is different from the solution of the previous reaction, and the solution of each reaction comprises any one of a zirconium-containing solution, a silicon-containing solution or a silver-containing solution.
In an alternative embodiment, in order to obtain a white pearlescent pigment with good glossiness and light reflection capability, the preparation method comprises the following steps:
s01, placing the base material in water for activation treatment to obtain a first dispersion liquid;
in an alternative embodiment, the activating comprises adding an activating agent to the water to activate the substrate, the activating agent comprising any one of tin tetrachloride, stannous chloride.
Preferably, the tin tetrachloride has a tin content of 8 to 12%.
Preferably, in order to disperse the substrate more uniformly so that each surface of the substrate is more easily activated by the activator, the ratio of the mass of the substrate to the volume of water in the first dispersion is 0.8 to 1.2g:18 to 22ml.
Preferably, the volume ratio of the activator to the water in the first dispersion is from 0.04 to 0.06:1.8 to 2.2.
Preferably, the reaction temperature for activation is 60 to 70 ℃ and the pH of the reaction solution is 1 to 2. Wherein the temperature and pH are required to be maintained within the above-mentioned ranges throughout the reaction until the end of the reaction. The temperature and pH of the activation reaction are controlled to improve the activation capability of the substrate, and a better material basis is provided for the preparation of the white pearlescent layer.
Preferably, the activator is added in a slow dropwise manner, so that the reaction between the substrate and the activator is not uniform, and the partial surface of the substrate is not activated sufficiently.
S02, adding a zirconium-containing solution into the first dispersion liquid to carry out a first reaction;
in an alternative embodiment, the zirconium-containing solution is any one of zirconium sulfate and zirconyl chloride; preferably, the zirconium-containing solution has a zirconium dioxide content of 4 to 6g/L.
Preferably, the volume ratio of water to zirconium-containing solution in the first dispersion is 1.8-2.2: 0.28 to 0.32.
Preferably, the reaction temperature of the first reaction is 75 to 80 ℃, the pH of the reaction solution is 2 to 3, and the reaction time after the zirconium-containing solution is added is 20 to 40min. Wherein the temperature and pH are required to be maintained within the above-mentioned ranges throughout the reaction until the end of the reaction. The zirconium dioxide is easier to coat on the surface of the base material by controlling the temperature and the pH value of the first reaction, so that the zirconium-containing pearlescent layer is obtained.
Preferably, the zirconium-containing solution is added in a slow dropwise manner, so that the phenomenon that the uniformity of the pearlescent layer on the surface of the substrate is affected due to the uneven reaction between the substrate and the zirconium-containing solution is avoided.
S03, adding a silicon-containing solution for a second reaction;
in an alternative embodiment, the silicon-containing solution comprises any one of sodium silicate, sodium metasilicate.
Preferably, the silicon content of the silicon-containing solution is 10 to 30%.
Preferably, the volume ratio of water in the first dispersion to the silicon-containing solution is 1.8 to 2.2:0.4 to 0.6.
Preferably, the reaction temperature of the second reaction is 75-80 ℃, the pH of the reaction solution is 7.5-8.5, and the reaction time after the silicon-containing solution is added is 20-40 min. Wherein the temperature and pH are required to be maintained within the above-mentioned ranges throughout the reaction until the end of the reaction. And controlling the temperature and pH of the second reaction to enable the silicon dioxide to be coated on the surface of the substrate more easily, thereby obtaining the silicon-containing pearl layer.
Preferably, the silicon-containing solution is added in a slow dropwise manner, so that the phenomenon that the uniformity of the pearlescent layer on the surface of the substrate is influenced due to the uneven reaction between the substrate and the silicon-containing solution is avoided.
S04, adding a zirconium-containing solution for a third reaction, and collecting a solid containing the base material after the third reaction;
in an alternative embodiment, the zirconium-containing solution is any one of zirconium sulfate and zirconyl chloride; preferably, the zirconium-containing solution has a zirconium dioxide content of 4 to 6g/L.
Preferably, in the third reaction, the volume ratio of the water in the first dispersion to the zirconium-containing solution is 1.8 to 2.2:0.30 to 0.35.
Preferably, the reaction temperature of the third reaction is 75-80 ℃, the pH of the reaction solution is 2-3, and the reaction time after the zirconium-containing solution is added is 20-40 min. Wherein the temperature and pH are required to be maintained within the above-mentioned ranges throughout the reaction until the end of the reaction. The zirconium dioxide is easier to coat on the surface of the base material by controlling the temperature and the pH value of the third reaction, so that the zirconium-containing pearlescent layer is obtained.
Preferably, the zirconium-containing solution is added in a slow dropwise manner, so that the phenomenon that the uniformity of the pearlescent layer on the surface of the substrate is affected due to the uneven reaction between the substrate and the zirconium-containing solution is avoided.
Preferably, the preparation of the solid containing the substrate comprises filtering the reaction solution after the third reaction, and sequentially washing, drying and calcining the solid.
Preferably, the drying temperature is 100-120 ℃, and the drying time is 10-15 h.
Preferably, the calcining temperature is 750-800 ℃, and the calcining time is 20-40 min.
S05, putting the solid containing the base material into water again to obtain a second dispersion liquid, and adding a silver-containing solution into the second dispersion liquid to carry out fourth reaction;
in an alternative embodiment, the silver-containing solution is a silver ammonia solution, and preferably, the silver content in the silver ammonia solution is 0.5-2%.
Preferably, the volume ratio of the water in the second dispersion liquid to the silver-ammonia solution is 1.8-2.2: 0.01 to 0.1.
Preferably, in order to disperse the substrate-containing solid more uniformly so that each surface of the substrate-containing solid is coated with the silver-containing pearl layer relatively easily, the ratio of the mass of the substrate-containing solid to the volume of water in the second dispersion is 0.8 to 1.2g:18 to 22ml.
Preferably, the reaction temperature of the fourth reaction is 40 to 60 ℃, and the pH of the reaction solution is 6.8 to 7.2. Wherein the temperature and pH are required to be maintained within the above-mentioned ranges throughout the reaction until the end of the reaction. The silver is easier to generate in situ on the surface of the substrate by controlling the temperature and the pH of the fourth reaction, so that the silver-containing pearlescent layer is obtained.
Preferably, the reaction is carried out for 8-12 min after the silver ammonia solution is added, and then the glucose solution is added into the reaction solution.
Preferably, the concentration of glucose in the glucose solution is between 0.8 and 1.2%. The addition of the glucose solution was based on the end of the silver mirror reaction.
Preferably, the glucose solution is added in a slow dropwise manner, so that the phenomenon that the reaction of the silver mirror on the solid surface containing the substrate is uneven, and the uniformity of the pearlescent layer is influenced is avoided.
Preferably, after the fourth reaction is finished, the reaction liquid is filtered, and the solid is washed and dried to obtain the white pearlescent pigment.
Preferably, in order to avoid the generation of impurities and obtain white pearlescent pigments with better quality, the water added in the invention is soft water or deionized water.
In alternative embodiments, the pH adjustment contemplated in the present invention may be performed using conventional pH adjusters, such as hydrochloric acid, dilute sulfuric acid, sodium hydroxide, and the like, as long as the pH is adjusted to the desired range without affecting the formation of the white pearlescent layer.
It should be noted that in some embodiments of the present invention, the term "water in the first dispersion" or "water in the second dispersion" appears, which shall mean water added to the first dispersion or the second dispersion in an initial state for dispersing the substrate or the solid containing the substrate, and does not include water contained in a solution subsequently added to the first dispersion or the second dispersion.
In a third aspect, the present invention provides a use of the white pearlescent pigment according to any one of the preceding embodiments or the white pearlescent pigment prepared by the preparation method according to any one of the preceding embodiments in the field of daily use chemical products.
Preferably, the daily chemical product comprises a cosmetic or perfume.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a white pearlescent pigment, which consists of mica and a white pearlescent layer on the surface of the mica, wherein the white pearlescent layer is a zirconium-containing pearlescent layer, a silicon-containing pearlescent layer, a zirconium-containing pearlescent layer and a silver-containing pearlescent layer in sequence along the surface of the mica, and the preparation method comprises the following steps:
s01, setting the reactor to be in a stirring state, weighing 100g of synthetic mica, adding 2L of soft water into the reactor, heating the mixture to 65 ℃, and reacting the mixture with a reaction solution prepared from 1:1, regulating the pH value to 1.5, slowly dropwise adding 50ml of 10% stannic chloride solution, and adopting 30% sodium hydroxide to keep the pH value of the reaction solution unchanged during the dropwise adding process.
Wherein the mica has a particle diameter of 5 to 45 μm and an average particle diameter of 25 to 30 μm.
S02, heating the solution to 78 ℃, adjusting the pH value to 2.5, slowly adding 300ml of zirconium sulfate solution, keeping the pH value of the reaction solution unchanged by using 30% sodium hydroxide, and continuously stirring for 30min after the zirconium sulfate is added.
S03, controlling the temperature of the solution to be 78 ℃, adjusting the pH value to be 8.0, slowly adding 500ml of sodium silicate solution with the silicon content of 20%, keeping the pH value of the reaction solution unchanged by using 10% hydrochloric acid, and continuously stirring for 30min after the sodium silicate is completely added.
And S04, controlling the temperature of the solution to be 78 ℃, adjusting the pH value to be 2.5, slowly adding 320ml of zirconium sulfate solution, keeping the pH value of the reaction solution unchanged by using 30% sodium hydroxide, and continuously stirring for 30min after the zirconium sulfate is added, wherein the content of zirconium dioxide in the zirconium sulfate solution is 5 g/L.
And after the reaction is finished, filtering the reaction solution, and sequentially washing, drying and calcining the solid. The drying temperature is 110 ℃, and the drying time is 12h. The calcination temperature was 780 ℃ and the calcination time was 30min to obtain a solid containing the substrate.
S05, adjusting the reactor to a stirring state, weighing 100g of solid containing the base material, dispersing the solid in 2L of soft water, raising the temperature to 50 ℃, adjusting the pH value to 7.0, adding 50ml of silver-ammonia solution, wherein the silver content is 1%, stirring for 10min, slowly dropwise adding 1% glucose solution into the reaction solution until the silver mirror reaction is finished, filtering the reaction solution, and washing and drying the solid to obtain the white pearlescent pigment.
The results shown in fig. 1 and 2 were obtained by observing the white pearlescent pigment of example 1 through scanning electron microscope imaging, and it can be seen from the SEM photographs of fig. 1 and 2 that the titanium dioxide particles on the entire surface of the example of the present invention have a uniform average size and a good glossiness. The pearlescent pigment obtained in example 1 was sprayed and the spraying effect was observed, and the results shown in fig. 3 and 4 were obtained, and it can be seen from fig. 3 and 4 that the pearlescent pigment provided in example 1 has excellent glossiness and fine and uniform color.
Example 2
This example provides a white pearlescent pigment, which is prepared in the same manner as in example 1 except that 800ml of a sodium silicate solution having a silicon content of 20% is slowly added during the preparation of the silicon-containing pearlescent layer.
Comparative example 1
This comparative example provides a white pearlescent pigment, which was prepared in the same manner as in example 1 except that the zirconium sulfate solution added in the steps of S02 and S04 was replaced with a titanium-containing solution, as follows:
s02, heating the solution to 78 ℃, adjusting the pH value to 2.5, slowly adding 30ml of titanium oxychloride solution, keeping the pH value of the reaction solution unchanged by using 30% sodium hydroxide, and continuously stirring for 30min after the titanium oxychloride is added.
And S04, controlling the temperature of the solution to be 78 ℃, adjusting the pH value to be 2.5, slowly adding 32ml of titanium oxychloride solution, keeping the pH value of the reaction solution unchanged by using 30% sodium hydroxide, and continuing to stir for 30min after the zirconium sulfate is added.
Comparative example 2
This comparative example provides a white pearlescent pigment, which was prepared similarly to example 1 except that in coating zirconium dioxide, sodium silicate solution was used instead of sodium hydroxide for neutralization while coating a mixed coating layer of zirconium dioxide and silicon oxide. Finally, the obtained pigment has serious agglomeration and poor glossiness. The hydrolysis coating of zirconium sulfate and sodium silicate has far different pH values, and the zirconium sulfate and sodium silicate are directly dissociated in the system and cannot be coated on the mica sheet.
Comparative example 3
This comparative example provides a white pearlescent pigment, which is prepared similarly to example 1 except that only a zirconium dioxide layer is coated on the mica sheet. The final product has poor glossiness and low covering power.
Comparative example 4
This comparative example provides a white pearlescent pigment, which was prepared similarly to example 1 except that a zirconium dioxide layer and a metallic silver layer were coated on the mica sheet. The final product has serious agglomeration, poor glossiness and low covering power.
Test example 1
The white pearlescent pigments of examples 1 to 2 and comparative examples 1 to 4 were coated by a conventional method of coating a card or a spray board. Adding the pearlescent pigment into resin or paint, stirring uniformly, coating or spraying a plate, and testing the color and the smoothness by using an X-Rite MA68 color difference instrument. The test results are shown in table 1:
TABLE 1 luster and smoothness of pearlescent pigments
As can be seen from Table 1, compared with comparative examples 1 to 4, under certain coating conditions, dissociation occurs with the increase of the coating amount, and the agglomeration phenomenon causes the reduction of the brightness and the hiding power of the product. The white pearlescent pigment obtained in the embodiment under the specific coating amount and the structural design is excellent in brightness and hiding power, and can obtain the effects of glossiness and hiding power which are similar to those of the titanium dioxide coated pearlescent pigment which is commercially available at present. The pearlescent pigment prepared by the embodiment of the invention does not contain titanium dioxide, and is safer when being used as a coating or an additive.
The embodiment of the invention provides a white pearlescent pigment and a preparation method and application thereof, and the white pearlescent pigment at least has the following advantages:
when the zirconium-containing pearlescent layer is coated on the surface of the substrate, zirconium dioxide is used as a main pearlescent element to reflect light; when the silicon-containing pearlescent layer is coated on the surface of the substrate, silicon dioxide is used as a main pearlescent element to reflect light, at least two of the silicon dioxide, the zirconium dioxide and the silver are selected as raw materials of the white pearlescent layer by utilizing different refractive indexes of the zirconium dioxide, the zirconium dioxide and the silver, so that the white pearlescent pigment with good glossiness and good light reflection effect can be prepared without adding titanium dioxide, and the glossiness of the pearlescent pigment can be further improved by adding the silver. The white pearlescent pigment obtained by coating at least two of the zirconium-containing pearlescent layer, the silicon-containing pearlescent layer and the silver-containing pearlescent layer on the surface of the substrate is safe and has good glossiness, and can be safely and permanently applied to daily chemical products.
Because the refractive indexes of the zirconium dioxide, the silicon dioxide and the silver are different, the refractive index of the zirconium dioxide is the highest, and the refractive index of the silicon dioxide is the lowest, and a process from high to low to high in refractive index appears when the white pearlescent layer is coated on the surface of the base material, so that the reflectivity of light on the surface of the pearlescent pigment is improved, and the pearlescent effect is shown. In addition, the refractive index is changed in the coating process from the zirconium-containing pearlescent layer to the silver-containing pearlescent layer, so that the silver-containing pearlescent layer can directly improve the glossiness of the white pearlescent pigment, and the light reflectivity of the white pearlescent pigment can be improved through the difference of the refractive indexes of two adjacent pearlescent layers.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The white pearlescent pigment is characterized by comprising a substrate and a white pearlescent layer coated on the surface of the substrate, wherein the white pearlescent layer comprises at least two of a zirconium-containing pearlescent layer, a silicon-containing pearlescent layer and a silver-containing pearlescent layer.
2. The white pearlescent pigment of claim 1, wherein the white pearlescent layer is a multilayer structure formed alternately, the multilayer structure is at least 3 layers, and the multilayer structure comprises at least two of a zirconium-containing pearlescent layer, a silicon-containing pearlescent layer and a silver-containing pearlescent layer;
preferably, the multilayer structure is at least 4 layers.
3. The white pearlescent pigment of claim 1, wherein the substrate comprises at least one of mica, glass, alumina, and silica;
the mica comprises natural mica or synthetic mica;
the particle size of the base material is 5-45 μm, and the average particle size is 25-30 μm.
4. A method for producing a white pearlescent pigment according to any one of claims 1 to 3, which comprises placing a substrate or a solid containing a substrate in a solution to react at least twice, and the solution of each reaction is different from the solution of the previous reaction, and the solution of each reaction comprises any one of a zirconium-containing solution, a silicon-containing solution or a silver-containing solution.
5. The method according to claim 4, comprising the steps of placing the substrate in water to perform an activation treatment to obtain a first dispersion, adding a zirconium-containing solution to the first dispersion to perform a first reaction, adding a silicon-containing solution to perform a second reaction, adding a zirconium-containing solution to perform a third reaction, collecting a solid containing the substrate after the third reaction, placing the solid containing the substrate in water again to obtain a second dispersion, and adding a silver-containing solution to the second dispersion to perform a fourth reaction.
6. The method according to claim 5, wherein the zirconium-containing solution added in the first reaction and the third reaction is any one of zirconium sulfate and zirconyl chloride; preferably, the content of zirconium dioxide in the zirconium-containing solution is 4-6 g/L;
preferably, the ratio of the mass of the base material to the volume of water in the first dispersion is 0.8 to 1.2g:18 to 22ml;
preferably, in the first reaction, the volume ratio of the water in the first dispersion liquid to the zirconium-containing solution is 1.8-2.2: 0.28 to 0.32;
preferably, in the third reaction, the volume ratio of the water in the first dispersion to the zirconium-containing solution is 1.8 to 2.2:0.30 to 0.35;
preferably, the temperature of the first reaction and the third reaction is 75-80 ℃, and the pH of the reaction liquid is 2-3;
preferably, the reaction time after the zirconium-containing solution is added in the first reaction and the third reaction is 20-40 min;
preferably, the preparation of the solid containing the base material comprises filtering the reaction liquid after the third reaction is finished, and sequentially washing, drying and calcining the solid;
preferably, the drying temperature is 100-120 ℃, and the drying time is 10-15 h;
preferably, the calcining temperature is 750-800 ℃, and the calcining time is 20-40 min.
7. The method of claim 5, wherein the silicon-containing solution comprises any one of sodium silicate and sodium metasilicate;
preferably, the silicon dioxide content in the silicon-containing solution is 10-30%;
preferably, the volume ratio of the water in the first dispersion to the silicon-containing solution is 1.8-2.2: 0.4 to 0.6;
preferably, the reaction temperature of the second reaction is 75-80 ℃, the pH of the reaction solution is 7.5-8.5, and the reaction time after the silicon-containing solution is added is 20-40 min.
8. The preparation method according to claim 5, wherein the silver-containing solution is a silver ammonia solution, preferably, the content of silver in the silver ammonia solution is 0.5-2%;
preferably, the volume ratio of the water in the second dispersion liquid to the silver ammonia solution is 1.8-2.2: 0.01 to 0.1;
preferably, the ratio of the mass of the solid containing the substrate to the volume of water in the second dispersion is 0.8 to 1.2g:18 to 22ml;
preferably, the reaction temperature of the fourth reaction is 40-60 ℃, and the pH of the reaction solution is 6.8-7.2;
preferably, after the silver ammonia solution is added, the reaction is carried out for 8 to 12min, and then the glucose solution is added into the reaction solution;
preferably, the concentration of glucose in the glucose solution is 0.8 to 1.2%.
9. The preparation method according to claim 5, wherein the activating comprises adding an activating agent to the water to activate the substrate, wherein the activating agent comprises any one of stannic chloride and stannous chloride;
preferably, the content of tin in the tin tetrachloride is 8 to 12 percent;
preferably, the volume ratio of the activator to the water in the first dispersion is from 0.04 to 0.06:1.8 to 2.2;
preferably, the reaction temperature of the activation is 60 to 70 ℃, and the pH of the reaction solution is 1 to 2.
10. Use of the white pearlescent pigment according to any one of claims 1 to 3 or the white pearlescent pigment prepared by the preparation method according to any one of claims 4 to 9 in the field of daily chemical products;
preferably, the daily chemical product comprises a cosmetic or perfume.
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