CN111040476A - Preparation method of zirconium-aluminum coated rutile titanium dioxide - Google Patents

Preparation method of zirconium-aluminum coated rutile titanium dioxide Download PDF

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CN111040476A
CN111040476A CN201911316679.4A CN201911316679A CN111040476A CN 111040476 A CN111040476 A CN 111040476A CN 201911316679 A CN201911316679 A CN 201911316679A CN 111040476 A CN111040476 A CN 111040476A
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titanium dioxide
dioxide slurry
aluminum
slurry
zirconium
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顾勇
王唯诚
杜茂平
周华
徐新春
钱蕾
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NANJING TITANIUM DIOXIDE CHEMICAL CO Ltd
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NANJING TITANIUM DIOXIDE CHEMICAL CO Ltd
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Abstract

The invention provides a preparation method of zirconium-aluminum coated rutile titanium dioxide, which comprises the following steps: preparing titanium dioxide slurry with aluminum hydroxide of a boehmite structure deposited on the surface; the second step is that: cooling the titanium dioxide slurry to 60-65 ℃, then adding an acidic aluminum-containing compound to adjust the pH of the titanium dioxide slurry to 6.5-7.5 to obtain aluminum hydroxide with an amorphous structure to be deposited on the surfaces of titanium dioxide particles, and the third step: and (3) carrying out filter pressing on the titanium dioxide slurry to form a filter cake, drying the filter cake, then crushing, and synchronously adding an organic auxiliary agent during crushing to obtain a finished product. The invention adds dispersant, zirconium compound, two different aluminum salt compounds and organic treating agent into titanium dioxide slurry, forms nanometer coating layer by physical and chemical adsorption on titanium dioxide particle surface, then through three washing, flash evaporation drying and crushing to obtain final product. Compared with the existing sulfuric acid method, the prepared titanium dioxide has good dispersibility and covering power and good application performance.

Description

Preparation method of zirconium-aluminum coated rutile titanium dioxide
Technical Field
The invention belongs to the technical field of titanium dioxide production, and relates to a preparation method of zirconium-aluminum coated rutile titanium dioxide.
Background
Titanium dioxide, the chemical name of which is titanium dioxide, has two crystal forms of rutile type and anatase type in industrial application. The uncoated rutile primary product has poor dispersibility when applied in an oily or aqueous system, the surface of the rutile primary product needs to be subjected to inorganic coating in order to improve the application performance of the rutile primary product, and when the uncoated rutile primary product is applied in a specific system, the surface of the rutile primary product needs to be subjected to organic coating in order to improve the application performance of the rutile titanium dioxide in the specific system. The rutile type titanium dioxide inorganic coating process mainly comprises a silicon-aluminum coating, a zirconium-silicon-aluminum coating, a phosphorus-aluminum coating, an aluminum coating and the like according to coating auxiliary agents, and a plurality of organic treating agents selected for organic coating comprise hydroxymethyl alkanes, alcamines, organic silanes and the like.
Since the production processes adopted by various companies are different, the product performances are also different, and patent CN201110099500 is that the surface of a rutile primary product is subjected to silicon and aluminum inorganic coating and organic coating, and the product has better dispersibility and weather resistance. Chinese patent CN201010228742 is an organic coating of silicon and aluminum inorganic coating agents on the surface of a rutile primary product, and the product has high covering power, high whiteness and basic weather resistance. Patent CN104119702 discloses a zirconium-aluminum coating process for rutile titanium dioxide with high gloss and high weatherability, which avoids flocculation and precipitation caused by pH change crossing isoelectric point due to directly adding acidic solution in the zirconium coating process, and simultaneously ensures uniform dispersion of zirconium, and effectively improves the gloss and weatherability of rutile titanium dioxide. Chinese patent CN103555001 discloses a coating method of titanium dioxide, which adopts low-alkalinity sodium metaaluminate to carry out zirconium-aluminum coating, silicon-aluminum coating and aluminum coating, improves the brightness of products and reduces the dosage of acid substances. Chinese patent CN104356693 discloses a zirconium-aluminum coating method for sulfuric acid process titanium dioxide, which comprises the steps of firstly adding zirconium salt, adjusting pH value, fully dispersing, and adding aluminum salt for three times, so as to improve the glossiness, covering power, weather resistance and the like of the titanium dioxide.
These studies have shown that oxides of silicon, aluminum, zirconium, phosphorus, etc. can be obtained under different conditions of raw materials, different pH, different temperature, etc., and the crystal structure of the oxides is only coated with aluminum (see document "XRD identification of aluminum oxide and aluminum hydroxide"), the aluminum oxide and hydroxide have various crystal forms, and the crystal forms have completely different uses, wherein the crystal form of aluminum hydroxide includes α -Al (OH)3, which belongs to monoclinic system and has a hexagonal plate shape and a prism shape when the crystals are intact, β -Al (OH)3 belongs to orthorhombic system, β' -Al (OH)3 belongs to triclinic system, diaspore belongs to orthorhombic system, boehmite, and orthorhombic system, etc., and meanwhile, the continuous or discontinuous, loose, and other coating effects of the film layer, and the application effects of the compact and different application systems are obviously different, which are obviously different in the existing patents, even if the coating raw materials, the coating film layers, etc. are close to each other field, the application performance is obviously different after different combinations are used.
At present, in the coating preparation process of titanium dioxide, particularly in titanium dioxide prepared by using zirconium-aluminum coating, a method of coating aluminum by using a single raw material is often adopted, namely, one of raw materials such as aluminum sulfate and sodium metaaluminate is coated under a certain pH condition, and the crystal form of aluminum hydroxide obtained by the product is mainly one of an amorphous structure and a boehmite structure. The aluminum hydroxide obtained by coating has single crystal form, and the dispersibility and the covering power of the titanium dioxide product are not ideal or the two cannot be considered at the same time. Researchers use a water-based emulsion paint test system to perform application tests on a large number of zirconium-aluminum coated titanium dioxide products, and the results show that the existing zirconium-aluminum coated titanium dioxide products have the dispersibility of more than 35 microns (the smaller the dispersibility value is, the better the dispersibility value is), the covering power (the contrast ratio method) of less than 86.5 percent (the larger the contrast ratio is, the better the contrast ratio is), the indexes of the products such as the dispersibility, the covering power and the like are not ideal, and the application requirements of increasingly improved water-based emulsion paints and other systems, especially high-end paint systems, can not be met.
Disclosure of Invention
1. The technical problem to be solved is as follows:
the existing titanium dioxide prepared by zirconium-aluminum coating adopts a single raw material to coat aluminum, and the aluminum hydroxide obtained by coating has a single crystal form, so that the dispersibility and the covering power of the titanium dioxide product are not ideal, or the two cannot be considered at the same time.
2. The technical scheme is as follows:
in order to solve the problems, the invention provides a preparation method of zirconium-aluminum coated rutile titanium dioxide, which comprises the following steps: the first step is as follows: preparing titanium dioxide slurry with aluminum hydroxide of a boehmite structure deposited on the surface; the second step is that: cooling the titanium dioxide slurry in the first step to 60-65 ℃, then adding an acidic aluminum-containing compound to adjust the pH of the titanium dioxide slurry to 6.5-7.5 to obtain aluminum hydroxide with an amorphous structure, wherein the aluminum hydroxide with the amorphous structure is deposited on the surfaces of titanium dioxide particles in the titanium dioxide slurry, and the third step is as follows: and (3) carrying out filter pressing on the titanium dioxide slurry obtained in the second step to form a filter cake, drying the filter cake, then crushing, and synchronously adding an organic auxiliary agent during crushing to obtain a finished product.
The PH value of the titanium dioxide slurry in the first step is 8.5-9.5.
In the second step, the acidic aluminum-containing compound is one or a mixture of aluminum sulfate, aluminum chloride and aluminum nitrate, and the addition amount of the acidic aluminum-containing compound is Al2O3/TiO2The mass fraction of (A) is 1.2-1.6%.
In the second step, the titanium dioxide slurry in the first step is cooled to 60-65 ℃, the pH value is adjusted to 5.0-6.0, then an acidic aluminum-containing compound is added, the pH value is maintained to be 5.0-6.0, homogenization is carried out for 20-40 min, the pH value of the titanium dioxide slurry is adjusted to be 6.5-7.5, and homogenization is carried out for 20-40 min.
The resistivity of the filter cake is 100-150 omega.m
Titanium dioxide slurry as described in the first stepObtained by the following steps: the method comprises the following steps: step S01: preparing a rutile type titanium dioxide primary product, diluting the rutile type titanium dioxide primary product until the concentration is 300-350 g/l in terms of titanium dioxide, adjusting the pH value of the titanium dioxide slurry to 9.0-10.0, and adding a dispersing agent, wherein the adding amount of the dispersing agent is TiO2The mass fraction of (A) is 0.05-0.25%; step S02: heating the titanium dioxide slurry obtained in the step S01 to 55-60 ℃, adding a zirconium-containing compound and an alkali liquor in a concurrent flow manner, then adjusting the pH of the titanium dioxide slurry to 8.0-9.0, and homogenizing for 20-40 min, wherein the zirconium-containing compound is added in an amount of ZrO2/ TiO2The mass fraction is 0.4-1.0%; step S03: heating the titanium dioxide slurry obtained in the step S02 to 65-70 ℃, adjusting the pH of the titanium dioxide slurry to 9.5-10.5 within 30-45 min by using alkali liquor, adding the dispersing agent, and homogenizing for 20-40 min, wherein the adding amount of the dispersing agent is TiO2The mass fraction of (A) is 0.05-0.10%; step S04: adding an alkaline aluminum-containing compound and an acid solution in parallel, homogenizing for 20-40 min while maintaining the pH of the titanium dioxide slurry at 8.5-9.5 in the titanium dioxide slurry obtained in the step S03, wherein the amount of the alkaline aluminum-containing compound added is Al2O3/TiO2The mass fraction of the slurry is 1.2-1.6%, and the titanium dioxide slurry with the boehmite structure deposited on the surface is prepared.
In step S01, the rutile type titanium dioxide powder is obtained by calcining, grinding, wet grinding, and water separation and classification.
The dispersant is sodium polyacrylate.
The zirconium-containing compound is one or more of zirconium oxychloride and zirconium sulfate.
The alkaline aluminum-containing compound is at least one of sodium metaaluminate and potassium metaaluminate.
3. Has the advantages that:
the invention adds inorganic dispersant, zirconium-containing compound, two different aluminum salt compounds and organic treating agent into titanium dioxide slurry in sequence, forms a nano-scale coating layer by physical and chemical adsorption on the surface of titanium dioxide particles, and then prepares the final product by the procedures of three-washing, flash evaporation drying, airflow pulverization and the like. Compared with the rutile titanium dioxide produced by the existing sulfuric acid method, the prepared titanium dioxide has good dispersibility and covering power and good application performance.
Drawings
FIG. 1 is an electron microscope image of a titanium white powder coated with a film layer.
Detailed Description
The present invention will be described in detail below with reference to the drawings and examples.
Example 1
Calcining, wet grinding, water-selecting and grading to obtain titanium dioxide slurry, diluting to 300 g/l, regulating pH value of titanium dioxide slurry to 10.0 by using alkali solution, adding sodium polyacrylate as dispersing agent, and adding TiO2Is 0.1% by mass. Then, the obtained titanium dioxide slurry is heated to 50 ℃ by introducing steam, and zirconium sulfate and sodium hydroxide solution are added in a concurrent manner, wherein the adding amount of the zirconium sulfate is ZrO2/ TiO2The mass fraction is 0.6%, the time is controlled at 50min, after the zirconium sulfate is added, the PH of the slurry is adjusted to 8.0 by dilute sulfuric acid, and the slurry is homogenized for 30 min. Then, the titanium dioxide slurry is heated to 68 ℃, the PH of the titanium dioxide slurry is adjusted to 9.5 within 40min by using sodium hydroxide solution, and then sodium polyacrylate is added, and the amount of added TiO is equal to that of added sodium polyacrylate2Is 0.05% by mass. After the addition of the sodium polyacrylate is completed, homogenization is carried out for 30 min. Under the condition that the pH value of the titanium dioxide slurry is 9.5, sodium metaaluminate and dilute sulfuric acid are added into the titanium dioxide slurry in a concurrent flow manner, wherein the adding amount of the sodium metaaluminate is Al2O3/TiO2The mass fraction of the sodium metaaluminate is 1.5 percent, the time is controlled to be about 50min, and the sodium metaaluminate is homogenized for 30min after being added. Then, the titanium dioxide slurry is cooled to 65 ℃, the PH value of the titanium dioxide slurry is adjusted to 5.5 by dilute sulfuric acid, and aluminum sulfate and sodium hydroxide solution are added into the titanium dioxide slurry in a concurrent flow manner, wherein the adding amount of the aluminum sulfate is Al2O3/TiO2The mass fraction of the aluminum sulfate is 1.5 percent, the time is controlled to be about 50min, and after the aluminum sulfate is added, the aluminum sulfate is homogenized for 30 min. The pH of the resulting titanium dioxide slurry was adjusted to 7.0 and homogenized for 30 min. Filter-pressing the titanium dioxide slurry to form a filter cake, wherein the resistivity of the filter cake is 100 omega.m, and dryingAfter drying, carrying out jet milling, and synchronously adding organic auxiliary agent in the jet milling, wherein the addition amount of the organic auxiliary agent/TiO2The mass fraction of the product is 0.3 percent, and a finished product is prepared. As shown in fig. 1.
Example 2
Calcining, wet grinding, water separating and grading to obtain titanium dioxide slurry, diluting to 350 g/l, regulating pH value of titanium dioxide slurry to 9.5 with sodium hydroxide solution, adding sodium polyacrylate as dispersant and TiO2Is 0.15% by mass. Then, the obtained titanium dioxide slurry is heated to 55 ℃ by introducing steam, and zirconium sulfate and sodium hydroxide solution are added in a concurrent manner, wherein the adding amount of the zirconium sulfate is ZrO2/ TiO2The mass fraction is 0.4%, the time is controlled at 50min, after the zirconium sulfate is added, the PH of the slurry is adjusted to 8.5 by dilute sulfuric acid, and the slurry is homogenized for 30 min. Then, the titanium dioxide slurry is heated to 65 ℃, the PH of the titanium dioxide slurry is adjusted to 10.5 within 40min by using sodium hydroxide solution, and then sodium polyacrylate is added, wherein the addition amount is TiO2Is 0.1% by mass. After the addition of the sodium polyacrylate is completed, homogenization is carried out for 30 min. Under the condition that the pH value of the titanium dioxide slurry is 9.5, sodium metaaluminate and dilute sulfuric acid are added into the titanium dioxide slurry in a concurrent flow manner, wherein the adding amount of the sodium metaaluminate is Al2O3/TiO2The mass fraction of the sodium metaaluminate is 1.4 percent, the time is controlled to be about 50min, and the sodium metaaluminate is homogenized for 20min after being added. Then, the titanium dioxide slurry is cooled to 60 ℃, the pH value of the titanium dioxide slurry is adjusted to 6.0 by dilute sulfuric acid, and aluminum sulfate and sodium hydroxide solution are added into the titanium dioxide slurry in a concurrent flow manner, wherein the adding amount of the aluminum sulfate is Al2O3/TiO2The mass fraction of the aluminum sulfate is 1.4 percent, the time is controlled to be about 50min, and after the aluminum sulfate is added, the aluminum sulfate is homogenized for 30 min. Then the pH of the obtained titanium dioxide slurry is adjusted to 6.5, and the titanium dioxide slurry is homogenized for 30 min. Filter-pressing the titanium dioxide slurry to form a filter cake, drying the filter cake to obtain a filter cake with the resistivity of 150 omega, jet milling the filter cake, and synchronously adding the organic auxiliary agent in the jet milling process, wherein the addition amount of the organic auxiliary agent/TiO2The mass fraction of the product is 0.6 percent, and a finished product is prepared. As shown in fig. 1.
Example 3
Calcining, wet grinding,Water selecting and grading to obtain titanium dioxide slurry, diluting to 330 g/l, regulating pH value of titanium dioxide slurry to 11.0 by using sodium hydroxide solution, adding sodium polyacrylate as dispersant, and adding TiO2Is 0.15% by mass. Then, the obtained titanium dioxide slurry is heated to 60 ℃ by introducing steam, and zirconium sulfate and sodium hydroxide solution are added in a concurrent manner, wherein the adding amount of the zirconium sulfate is ZrO2/TiO2The mass fraction is 0.4%, the time is controlled at 50min, after the zirconium sulfate is added, the PH of the slurry is adjusted to 9.0 by dilute sulfuric acid, and the slurry is homogenized for 30 min. Then, the titanium dioxide slurry is heated to 70 ℃, the PH of the titanium dioxide slurry is adjusted to 10 within 40min by using sodium hydroxide solution, and then sodium polyacrylate is added, wherein the addition amount is TiO2The mass fraction of (A) is 0.1%, and homogenizing for 30 min. Under the condition that the pH value of the titanium dioxide slurry is 10, adding sodium metaaluminate and dilute sulfuric acid into the titanium dioxide slurry in a concurrent flow manner, wherein the adding amount of the sodium metaaluminate is Al2O3/TiO2The mass fraction of the sodium metaaluminate is 1.6 percent, the time is controlled to be about 50min, and the sodium metaaluminate is homogenized for 40min after being added. Then, the titanium dioxide slurry is cooled to 65 ℃, diluted sulfuric acid is used for adjusting the pH value to 5.0, and aluminum sulfate and sodium hydroxide solution are added into the titanium dioxide slurry in a concurrent flow mode, wherein the adding amount of the aluminum sulfate is Al2O3/TiO2The mass fraction of the aluminum sulfate is 1.5 percent, the time is controlled to be about 50min, and the aluminum sulfate is homogenized for 30min after being added. Then the pH of the obtained titanium dioxide slurry is adjusted to 7.5, and the titanium dioxide slurry is homogenized for 40 min. Filter-pressing the titanium dioxide slurry to form a filter cake, wherein the resistivity of the filter cake is 130 omega, drying, and then carrying out jet milling, wherein organic auxiliary agent is synchronously added during jet milling, and the addition amount of the organic auxiliary agent/TiO is used as the addition amount2The mass fraction of the product is 0.8 percent, and a finished product is prepared. As shown in fig. 1.
Example 4
Calcining, wet grinding, water separating and grading to obtain titanium dioxide slurry, diluting to 330 g/l, regulating pH value of titanium dioxide slurry to 10.0 by using sodium hydroxide solution, adding sodium polyacrylate as dispersing agent, adding P2O5/TiO2Is 0.2% by mass. Then, the obtained titanium dioxide slurry is heated by introducing steam to the titanium dioxide slurryZirconium sulfate and sodium hydroxide solution are added at 60 ℃ in parallel, and the adding amount of the zirconium sulfate is ZrO2/TiO2The mass fraction is 0.6%, the time is controlled at 50min, after the zirconium sulfate is added, the PH of the slurry is adjusted to 8.5 by dilute sulfuric acid, and the slurry is homogenized for 30 min. Then, the titanium dioxide slurry is heated to 65 ℃, the PH of the titanium dioxide slurry is adjusted to 10 within 40min by using sodium hydroxide solution, and then sodium polyacrylate is added, wherein the addition amount is TiO2The mass fraction of (A) is 0.05%, and the homogenization is carried out for 30 min. Under the condition that the pH value of the titanium dioxide slurry is 10, adding sodium metaaluminate and dilute sulfuric acid into the titanium dioxide slurry in a concurrent flow manner, wherein the adding amount of the sodium metaaluminate is Al2O3/TiO2The mass fraction of the sodium metaaluminate is 1.3 percent, the time is controlled to be about 50min, and the sodium metaaluminate is homogenized for 40min after being added. Then, the titanium dioxide slurry is cooled to 65 ℃, diluted sulfuric acid is used for adjusting the pH value to 5.0, and aluminum sulfate and sodium hydroxide solution are added into the titanium dioxide slurry in a concurrent flow mode, wherein the adding amount of the aluminum sulfate is Al2O3/TiO2The mass fraction of the aluminum sulfate is 1.3 percent, the time is controlled to be about 50min, and after the aluminum sulfate is added, the aluminum sulfate is homogenized for 30 min. Then the pH of the obtained titanium dioxide slurry is adjusted to 7.0, and the titanium dioxide slurry is homogenized for 40 min. Filter-pressing the titanium dioxide slurry to form a filter cake, drying the filter cake to obtain a filter cake with the resistivity of 110 omega, jet milling the filter cake, and synchronously adding the organic auxiliary agent in the jet milling process, wherein the addition amount of the organic auxiliary agent/TiO2The mass fraction of the product is 0.5 percent, and a finished product is prepared. As shown in fig. 1.
Example 5
Calcining, wet grinding, water separating and grading to obtain titanium dioxide slurry, diluting to 330 g/l, regulating pH value of titanium dioxide slurry to 10.5 with sodium hydroxide solution, adding sodium polyacrylate as dispersant and TiO2Is 0.15% by mass. Then, the obtained titanium dioxide slurry is heated to 50 ℃ by introducing steam, and zirconium sulfate and sodium hydroxide solution are added in a concurrent manner, wherein the adding amount of the zirconium sulfate is ZrO2/TiO2The mass fraction is 0.5%, the time is controlled at 50min, after the zirconium sulfate is added, the PH of the slurry is adjusted to 8.0 by dilute sulfuric acid, and the slurry is homogenized for 30 min. Then, the titanium dioxide slurry is heated to 68 ℃, and is adjusted within 40min by using sodium hydroxide solutionAdjusting the pH of the titanium dioxide slurry to 10.5, adding sodium polyacrylate in an amount of TiO2The mass fraction of (A) is 0.1%, and homogenizing for 30 min. Under the condition that the pH value of the titanium dioxide slurry is 10.5, sodium metaaluminate and dilute sulfuric acid are added into the titanium dioxide slurry in a concurrent flow manner, wherein the adding amount of the sodium metaaluminate is Al2O3/TiO2The mass fraction of the sodium metaaluminate is 1.3 percent, the time is controlled to be about 50min, and the sodium metaaluminate is homogenized for 30min after being added. Then, the titanium dioxide slurry is cooled to 65 ℃, diluted sulfuric acid is used for adjusting the pH value to 6.0, and aluminum sulfate and sodium hydroxide solution are added into the titanium dioxide slurry in a concurrent flow mode, wherein the adding amount of the aluminum sulfate is Al2O3/TiO2The mass fraction of the aluminum sulfate is 1.3 percent, the time is controlled to be about 50min, and after the aluminum sulfate is added, the aluminum sulfate is homogenized for 30 min. Then the pH of the obtained titanium dioxide slurry is adjusted to 7.0, and the titanium dioxide slurry is homogenized for 30 min. Filter-pressing the titanium dioxide slurry to form a filter cake, wherein the resistivity of the filter cake is 140 omega.m, drying, and then carrying out jet milling, wherein organic auxiliary agent is synchronously added during jet milling, and the addition amount of the organic auxiliary agent/TiO2The mass fraction of the product is 0.5 percent, and a finished product is prepared. As shown in fig. 1.
Comparative experiment
Calcining, wet grinding, water separating and grading to obtain titanium dioxide slurry, diluting to 330 g/l, regulating pH value of titanium dioxide slurry to 10.0 with sodium hydroxide solution, adding inorganic dispersant sodium hexametaphosphate, and adding sodium hexametaphosphate in the amount of P2O5/TiO2Is 0.2% by mass. Then, the obtained titanium dioxide slurry is heated to 55 ℃ by introducing steam, and zirconium sulfate and sodium hydroxide solution are added in a concurrent manner, wherein the adding amount of the zirconium sulfate is ZrO2/TiO2The mass fraction is 0.4%, the time is controlled at 50min, after the zirconium sulfate is added, the PH of the slurry is adjusted to 8.3 by dilute sulfuric acid, and the slurry is homogenized for 30 min. Then, the titanium dioxide slurry is cooled to 62 ℃, diluted sulfuric acid is used for adjusting the pH value to 5.5, and aluminum sulfate and sodium hydroxide solution are added into the titanium dioxide slurry in a concurrent flow mode, wherein the adding amount of the aluminum sulfate is Al2O3/TiO2The mass fraction of the aluminum sulfate is 3.0 percent, the time is controlled to be about 70min, and after the aluminum sulfate is added, the aluminum sulfate is homogenized for 50 min. Then adjusting the pH of the obtained titanium dioxide slurry to7.2, homogenizing for 40 min. Filter-pressing the titanium dioxide slurry to form a filter cake, wherein the resistivity of the filter cake is 140 omega.m, drying, and then carrying out jet milling, wherein organic auxiliary agent is synchronously added during jet milling, and the addition amount of the organic auxiliary agent/TiO2The mass fraction of the product is 0.5 percent, and a finished product is prepared.
The sample is subjected to application test analysis in a water-based emulsion paint system, and the test method comprises the following steps: the addition of the titanium dioxide formula is 10%, a vibrator is adopted for dispersing in the paint preparation process, the dispersion time is 40min, then a 100-micron wet grinding preparation device is used for preparing the film on the polyester film in the same direction, the dispersibility is tested, and the contrast ratio (covering power) is detected after drying. The results are shown in the following table:
sample name Dispersity mu m Contrast ratio (hiding power)%
Example 1 sample 25 87.48
Example 2 sample 25 87.51
Example 3 sample 25 87.45
Example 4 sample 25 87.48
Example 5 sample 25 87.42
Comparative experiment sample 35 86.21
Note: the lower the dispersion value, the better the product dispersion; the higher the contrast ratio, the better the product hiding.
According to the test results, the dispersibility and the covering power of the product are greatly improved, and the application performance of the product is well improved by using the sample prepared by the method.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. A preparation method of zirconium-aluminum coated rutile titanium dioxide comprises the following steps: the first step is as follows: preparing titanium dioxide slurry with aluminum hydroxide of a boehmite structure deposited on the surface; the second step is that: cooling the titanium dioxide slurry in the first step to 60-65 ℃, then adding an acidic aluminum-containing compound to adjust the pH of the titanium dioxide slurry to 6.5-7.5 to obtain aluminum hydroxide with an amorphous structure, wherein the aluminum hydroxide with the amorphous structure is deposited on the surfaces of titanium dioxide particles in the titanium dioxide slurry, and the third step is as follows: and (3) carrying out filter pressing on the titanium dioxide slurry obtained in the second step to form a filter cake, drying the filter cake, then crushing, and synchronously adding an organic auxiliary agent during crushing to obtain a finished product.
2. The method of claim 1, wherein: the PH value of the titanium dioxide slurry in the first step is 8.5-9.5.
3. The method of claim 1, wherein: in the second step, the acidic aluminum-containing compound is one or a mixture of aluminum sulfate, aluminum chloride and aluminum nitrate, and the addition amount of the acidic aluminum-containing compound is Al2O3/TiO2The mass fraction of (A) is 1.2-1.6%.
4. The method of claim 1, wherein: in the second step, the titanium dioxide slurry in the first step is cooled to 60-65 ℃, the pH value is adjusted to 5.0-6.0, then an acidic aluminum-containing compound is added, the pH value is maintained to be 5.0-6.0, homogenization is carried out for 20-40 min, the pH value of the titanium dioxide slurry is adjusted to be 6.5-7.5, and homogenization is carried out for 20-40 min.
5. The method of claim 1, wherein: the resistivity of the filter cake is 100-150 omega.
6. The method of any one of claims 1-5, wherein: the titanium dioxide slurry described in the first step is obtained by: the method comprises the following steps: step S01: preparing a rutile type titanium dioxide primary product, diluting the rutile type titanium dioxide primary product until the concentration is 300-350 g/l in terms of titanium dioxide, adjusting the pH value of the titanium dioxide slurry to 9.0-10.0, and adding a dispersing agent, wherein the adding amount of the dispersing agent is TiO2The mass fraction of (A) is 0.05-0.25%; step S02: heating the titanium dioxide slurry obtained in the step S01 to 55-60 ℃, adding a zirconium-containing compound and an alkali liquor in a concurrent flow manner, then adjusting the pH of the titanium dioxide slurry to 8.0-9.0, and homogenizing for 20-40 min, wherein the zirconium-containing compound is added in an amount of ZrO2/ TiO2The mass fraction is 0.4-1.0%; step S03: heating the titanium dioxide slurry obtained in the step S02 to 65-70 ℃, adjusting the pH of the titanium dioxide slurry to 9.5-10.5 within 30-45 min by using alkali liquor, adding the dispersing agent, and homogenizing for 20-40 min, wherein the adding amount of the dispersing agent is TiO2The mass fraction of (A) is 0.05-0.10%; step S04: adding an alkaline aluminum-containing compound and an acid solution in parallel, homogenizing for 20-40 min while maintaining the pH of the titanium dioxide slurry at 8.5-9.5 in the titanium dioxide slurry obtained in the step S03, wherein the amount of the alkaline aluminum-containing compound added is Al2O3/TiO2The mass fraction of the slurry is 1.2-1.6%, and the titanium dioxide slurry with the boehmite structure deposited on the surface is prepared.
7. The method of claim 6, wherein: in step S01, the rutile type titanium dioxide powder is obtained by calcining, grinding, wet grinding, and water separation and classification.
8. The method of claim 6, wherein: the dispersant is sodium polyacrylate.
9. The method of claim 6, wherein: the zirconium-containing compound is one or more of zirconium oxychloride and zirconium sulfate.
10. The method of claim 6, wherein: the alkaline aluminum-containing compound is at least one of sodium metaaluminate and potassium metaaluminate.
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CN114149698A (en) * 2021-12-18 2022-03-08 中信钛业股份有限公司 Preparation method of special titanium dioxide for outdoor building coating
CN114163844A (en) * 2021-12-19 2022-03-11 中信钛业股份有限公司 Production method of titanium dioxide pigment with high achromatism and high weather resistance
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CN114106590A (en) * 2021-11-30 2022-03-01 龙佰集团股份有限公司 Slurry titanium dioxide and preparation method thereof
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CN114539815A (en) * 2022-03-01 2022-05-27 昆明冶金研究院有限公司 High-covering high-dispersity modified micro silicon powder and preparation method thereof
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CN115418117B (en) * 2022-08-04 2023-09-22 上海颜钛实业有限公司 Production method of special titanium dioxide pigment for powder coating

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