CN112143262A - Rare earth composite coated titanium dioxide and preparation method and application thereof - Google Patents
Rare earth composite coated titanium dioxide and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses rare earth composite coated titanium dioxide and a preparation method and application thereof, belonging to the technical field of titanium dioxide production. The method comprises the following steps: rolling and grinding the titanium dioxide crude product, then feeding the ground titanium dioxide crude product into a pulping tank, simultaneously adding desalted water and a dispersing agent, uniformly stirring to obtain titanium dioxide crude product slurry, and wet-grinding the obtained slurry by using a ball mill; grinding the slurry by a sand mill; transferring the ground slurry into a surface treatment tank for inorganic surface treatment; transferring the obtained slurry into a plate-and-frame filter press for filter pressing, and washing with desalted water to obtain a filter cake; and drying the filter cake to obtain titanium white powder, and carrying out organic coating on the titanium white powder through an air flow crushing process to obtain a titanium white finished product. Compared with the conventional product, the titanium dioxide prepared by the invention has better whiteness and stronger light resistance, and has better application performance in an application system.
Description
Technical Field
The invention belongs to the technical field of titanium dioxide production, and particularly relates to rare earth composite coated titanium dioxide and a preparation method and application thereof.
Background
TiO2Commonly known as titanium dioxide, is the top-grade white pigment which is most widely applied in the world and is mainly applied to the fields of coating, plastics, papermaking, chemical fibers, food, daily chemicals and the like. The crystal forms of the titanium dioxide comprise the following three types: rutile, anatase and brookite types. Among them, rutile type is the most stable crystalline form of titanium dioxide, its structure is compact, and compared with other crystalline forms, its application range is wider, and it is better in public praise, and because rutile type titanium dioxide has excellent optical property it is the best white pigment.
However, titanium dioxide is extracted from titanium ore, and the essential impurity ions exist in the titanium dioxide, so that the whiteness of the titanium dioxide is not particularly ideal, and the titanium dioxide contains an optical active point, so that the titanium dioxide is easy to yellow and pulverize under long-time ultraviolet irradiation, the durability of the titanium dioxide is poor, and meanwhile, nano particles are easy to agglomerate during photodegradation, so that the transparency of the titanium dioxide is poor, and the using effect of the titanium dioxide is directly influenced, so that the improvement of the whiteness and the light resistance of the titanium dioxide is of great significance.
In order to solve the above problems, titanium dioxide manufacturers have been looking for a method of improving light resistance. These methods include US patents US5976237A, US5785748A, US2004025749A, US4461810A, US4447270A, chinese patents CN101186334A, CN101857736A, CN104179066A, CN1067967A, CN101723446A, CN101235223A, etc.; in addition, Chinese patent CN100547037A adopts inorganic and organic composite coating, and adopts a method of cerium oxide and silicon oxide or aluminum oxide or zirconium oxide composite coating for inorganic coating; the product of Chinese patent CN101143978A is cerium oxide (CeO) because of being coated with cerium oxide2) It is yellow in color, so that the gloss (i.e., brightness) of the product is low. Chinese patent CN110669359A discloses a surface treatment process of special titanium dioxide for papermaking, which comprises the following steps: adding the dispersing agent into the titanium dioxide slurry after sanding, stirring and dispersingSieving to obtain TiO in the slurry2The amount of the titanium dioxide particles is 200-400 g/L, the surfaces of the titanium dioxide particles are coated with cerium phosphate, silicon dioxide and phosphorus pentoxide, finally, the surfaces of the titanium dioxide particles are coated with aluminum oxide by the cocurrent flow of alkaline aluminum and acidic aluminum, solid-liquid separation is carried out, and the solid is treated to obtain a finished product. Chinese patent CN109824083A discloses a method for improving the weather resistance of titanium dioxide produced by a chlorination process, which comprises the following steps: 1) pulping titanium dioxide base material by chlorination process at 50-100 deg.C, adding Al during pulping process3+Fixing agent to prepare slurry with the concentration of 300-800g/L, and adjusting the pH value of the slurry to 3.0-11.2; 2) homogenizing the slurry obtained in the step 1) for 4-6h at the temperature of 40-90 ℃; 3) grinding and grading the slurry obtained in the step 2), and controlling the particle size of the titanium dioxide to be 0.28-0.40 mu m; 4) carrying out inorganic coating on the slurry obtained in the step 3); 5) washing, purifying, drying and crushing the slurry obtained in the step 4) to obtain a titanium dioxide finished product.
The above-mentioned publications are continuously improving titanium dioxide, but these solutions are all in need of improvement, thereby improving the light resistance.
Disclosure of Invention
1. Problems to be solved
Aiming at the problems that the existing titanium dioxide has poor light resistance and yellowing and darkening after long-term use and cannot meet the requirements in some application fields, the invention provides the rare earth composite coated titanium dioxide and the preparation method and application thereof, and the light resistance of the titanium dioxide is improved.
2. Technical scheme
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the preparation method of the rare earth composite coated titanium dioxide comprises the steps of pulping, grinding (dry grinding by a rolling mill and wet grinding by a colloid mill, a ball mill and a sand mill), inorganic surface treatment, washing, drying, jet milling and packaging, and specifically comprises the following steps:
s101, rolling and grinding the titanium dioxide crude product, then feeding the ground titanium dioxide crude product into a pulping tank, simultaneously adding desalted water and a dispersing agent, uniformly stirring to obtain titanium dioxide crude product slurry, wet grinding the obtained slurry by a ball mill, carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to the pulping tank for circular grinding, and controlling 325-mesh screen residue;
step S102, grinding the slurry obtained in the step S101 through a sand mill; carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to a sand mill for circular grinding, and controlling the screen residue of 325 meshes;
step S103, transferring the ground slurry obtained in the step S102 to a surface treatment tank, performing inorganic surface treatment, curing, and transferring the obtained surface treatment clinker to a treated tank;
(1) diluting the ground slurry to 320g/L of 300-;
(2) phosphate solution and CeCl3Adding the solution into the slurry in a parallel flow manner, and curing for 30 minutes; it should be noted that, by adopting the parallel flow process, the pH value in the coating process is stable, and the stable environment ensures the uniformity and the integrity of the coating film;
(3) adjusting the pH value to 7.0-7.5 by using a dilute alkali solution with the mass fraction of 12%, and curing for 30 minutes; the dilute alkali solution can be a sodium hydroxide solution with the mass fraction of 12%. In some cases, the dilute alkali solution can also be a mixed solution of sodium hydroxide and cationic guar gum with the mass fraction of 12%, wherein the mass percentage content of the cationic guar gum is 5000ppm, the film forming property of the parallel flow coating can be improved under the alkalescent condition, and the dispersed coating of the core points can be realized, so that the core points continue to grow, and a continuous, uniform and compact film layer can be formed.
(4) Performing secondary parallel flow coating and Al2(SO4)3Solution with NaAlO2Adding the solution in a parallel flow manner, controlling the pH value to be 6.5-7.5, and curing for 40 minutes;
(5) adjusting the pH value to 6.0-6.5, curing for 30 minutes to obtain clinker, and transferring the clinker into a treated groove;
step S104: transferring the slurry obtained in the step S103 to a plate-and-frame filter press for filter pressing, washing with desalted water, washing to remove redundant salt ions, controlling the end-point conductivity to be below 100 mu S/cm, and controlling the solid content to be 65% -75% to obtain a filter cake;
step S105: transferring the obtained filter cake to flash evaporation drying for drying to obtain powder;
step S106: and (5) performing jet milling on the powder obtained in the step (S105), and performing organic coating by using a conventional coating agent to obtain a titanium dioxide finished product.
In one possible embodiment of the invention, the concentration of the titanium dioxide crude slurry in the step S101 is controlled to be 700-900g/L, the pressure of the cyclone is 0.25-0.4MPa, and the 325-mesh screen residue after cyclone is less than 0.5%; the dispersant is PAAS (sodium polyacrylate) or hexametaphosphoric acid, and the addition amount is TiO2The meter is controlled between 0.2% and 2.0%.
In one possible embodiment of the invention, in the step S102, the flow rate of the sand mill is controlled to be 7-10t/h, the pressure of the cyclone is 0.25-0.4MPa, and the 325-mesh residue after the cyclone is controlled to be below 0.1%.
In one possible embodiment of the present invention, the phosphate in step S103 is disodium hydrogen phosphate, sodium phosphate or a mixture thereof, and the main content P is2O5The concentration is 40g/L, and the coating amount is TiO2Calculated as 0.8 to 2.0 percent.
In one possible embodiment of the present invention, CeO is used in step S1032The concentration of the main content is 30g/L, and the coating amount is TiO2Calculated as 0.2% -0.5%; CeCl3Solution addition and flow: the addition amount and flow rate of the phosphate solution are 3: 1.
in one possible embodiment of the present invention, Al in step S1032(SO4)3The main content concentration of the solution is 90-100g/L, and the acid content is 220-240 g/L; NaAlO2The main content concentration of the solution is 90-100g/L, and the alkali content is 200-220 g/L; NaAlO2Solution addition and flow: al (Al)2(SO4)3The addition amount and flow rate of the solution are 1: 0.8-1.0.
In one possible embodiment of the present invention, the concentration of the dilute alkali in step S103 is 10% -15%; al (Al)2O3Coating amount of (2) with TiO23.0-4.0% in terms of weight; the titanium dioxide has a water content of less than 1%, a pH of 6.5-8.5 and a resistivity of more than 150 μ s.m.
In one possible embodiment of the inventionThe amount of the organic coating agent added in step S106 is TiO2Calculated as 0.3 to 1.0 percent.
The invention also provides a product obtained by the method.
The invention also provides application of the product in paint, plastic, printing ink and papermaking.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) as is well known, the surface of titanium dioxide is coated with hydrated oxides such as silicon, aluminum, zirconium and the like, so that a barrier can be formed between the titanium dioxide and a medium, and the oxidative degradation of matrix organic matters by nascent oxygen is prevented; the existing coating technology comprises the following steps: 1) the single coating agent has very limited performance effects of improving the weather resistance, brightness, whiteness and the like of the rutile titanium dioxide; 2) in the production process of rutile titanium dioxide, generally, two or more than two inorganic surface treatment agents such as silicon, aluminum, zirconium and the like are used for coating, namely mixing and coating rutile titanium dioxide particles; 3) transition metal, silicon and aluminum oxide mixed coating titanium dioxide, such as rare metals zirconium and cerium, for example, Chinese patent CN105199434A discloses a surface treatment method of titanium dioxide, which comprises the following steps: preparing a rutile type titanium dioxide primary product into a dissolving pulp, dispersing the dissolving pulp by using a dispersing agent, stirring and heating to a set temperature, adding a proper amount of trivalent soluble cerium salt to adjust the mixture to an acid environment, maintaining the pH value within the range of 4-6, adding one or mixture of sodium aluminate solution and phosphoric acid or disodium hydrogen phosphate and the rest of cerium salt solution in a concurrent flow manner, and forming a first layer of mixed coating film of cerium phosphate and aluminum phosphate after curing; adjusting and maintaining the pH value within the range of 7-9.5, adding a sodium aluminate solution and sulfuric acid or hydrochloric acid in a concurrent flow manner, and forming a second-layer boehmite alumina coating film after curing; filtering and washing with deionized water, drying, and pulverizing to obtain the final product. Compared with the method disclosed by the patent, the obtained product has higher whiteness and light resistance, and has smaller color difference after long-time sunlight irradiation, and the product can be used in the fields of coating, plastics, printing ink, paper making and the like;
(2) according to the preparation method of the rare earth composite coated titanium dioxide, the coating adopts a parallel flow process, the pH value in the coating process is stable, and the stable environment ensures the uniformity and the integrity of the coating film;
(3) the preparation method of the rare earth composite coated titanium dioxide has good dispersibility.
Drawings
FIG. 1 is a flow chart of the preparation method of the rare earth composite coated titanium dioxide.
Detailed Description
Exemplary embodiments of the present invention are described in detail below. Although these exemplary embodiments are described in sufficient detail to enable those skilled in the art to practice the invention, it should be understood that other embodiments may be realized and that various changes to the invention may be made without departing from the spirit and scope of the present invention. The following more detailed description of the embodiments of the invention is not intended to limit the scope of the invention, as claimed, but is presented for purposes of illustration only and not limitation to describe the features and characteristics of the invention, to set forth the best mode of carrying out the invention, and to sufficiently enable one skilled in the art to practice the invention. Accordingly, the scope of the invention is to be limited only by the following claims.
The following detailed description and example embodiments of the invention are set forth.
As shown in figure 1, the preparation method of the rare earth composite coated titanium dioxide comprises pulping, grinding (dry grinding by a rolling mill and wet grinding by a colloid mill, a ball mill and a sand mill), inorganic surface treatment, washing, drying, jet milling, organic coating and packaging.
Example 1
The preparation method of the rare earth composite coated titanium dioxide comprises the steps of pulping, rolling, grinding, dry grinding, inorganic surface treatment, washing, drying, jet milling and packaging, and specifically comprises the following steps:
s101, rolling and grinding the titanium dioxide crude product, then feeding the ground titanium dioxide crude product into a pulping tank, simultaneously adding desalted water and a dispersing agent, uniformly stirring to obtain titanium dioxide crude product slurry, wet grinding the obtained slurry by a ball mill, carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to the pulping tank for circular grinding, and controlling 325-mesh screen residue; controlling the concentration of the titanium dioxide crude product slurry to be 900g/L, controlling the pressure of a swirler to be 0.4MPa, and controlling the 325-mesh screen residue to be 0.4 percent after swirling; the dispersant is PAAS, and the addition amount is controlled to be 2.0 percent;
step S102, grinding the slurry obtained in the step S101 through a sand mill; carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to a sand mill for circular grinding, and controlling the screen residue of 325 meshes; the flow rate of the sand mill is controlled to be 10t/h, the pressure of the cyclone is 0.4MPa, and the 325-mesh screen residue is 0.08 percent after the cyclone is carried out;
step S103, transferring the ground slurry obtained in the step S102 to a surface treatment tank, performing inorganic surface treatment, curing, and transferring the obtained surface treatment clinker to a treated tank;
(1) diluting the ground slurry to 320g/L, and heating to 50 ℃;
(2) phosphate solution and CeCl3Adding the solution into the slurry in a parallel flow manner, and curing for 30 minutes; wherein the phosphate is disodium hydrogen phosphate, sodium phosphate or their mixture, and has main content of P2O5The concentration is 40g/L, and the coating amount is TiO22.0% in terms of weight; CeO (CeO)2The concentration of the main content is 30g/L, and the coating amount is TiO2Calculated as 0.5%; CeCl3Solution addition and flow: the addition amount and flow rate of the phosphate solution are 3: 1;
(3) adjusting the pH value to 7.5 by using a sodium hydroxide solution with the mass fraction of 12% and cationic guar gum with the mass percentage content of 5000ppm, and curing for 30 minutes;
(4) performing secondary parallel flow coating and Al2(SO4)3Solution with NaAlO2Adding the solution in a parallel flow manner, controlling the pH value to be 7.5, and curing for 40 minutes; al (Al)2O3Coating amount of (2) with TiO2Calculated as 4.0%; the titanium dioxide has the water content of 0.8 percent, the pH value of 8.5 and the resistivity of 156 mu s.m; al (Al)2(SO4)3The main content concentration of the solution is 100g/L, and the acid content is 240 g/L; NaAlO2The main content concentration of the solution is 100g/L, and the alkali content is 220 g/L; NaAlO2Solution addition and flow: al (Al)2(SO4)3The addition amount and flow rate of the solution are 1: 0.8;
(5) adjusting the pH value to 6.5, curing to obtain clinker, and transferring the clinker into a treated groove;
step S104: transferring the slurry obtained in the step S103 to a plate-and-frame filter press for filter pressing, washing with desalted water, washing to remove redundant salt ions, controlling the end-point conductivity to be 85 mu S/cm, and controlling the solid content to be 75% to obtain a filter cake;
step S105: transferring the obtained filter cake to flash evaporation drying for drying to obtain powder;
step S106: performing jet milling on the powder obtained in the step S105, and performing organic coating, wherein the addition amount of the organic coating agent is TiO2Calculated as 1.0 percent, and obtaining a titanium dioxide finished product.
Example 2
The preparation method of the rare earth composite coated titanium dioxide of the embodiment specifically comprises the following steps:
s101, rolling and grinding the titanium dioxide crude product, then feeding the ground titanium dioxide crude product into a pulping tank, simultaneously adding desalted water and a dispersing agent, uniformly stirring to obtain titanium dioxide crude product slurry, wet grinding the obtained slurry by a ball mill, carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to the pulping tank for circular grinding, and controlling 325-mesh screen residue; controlling the concentration of the titanium dioxide crude product slurry to be 700g/L, controlling the pressure of the cyclone to be 0.25MPa, and controlling the 325-mesh screen residue to be 0.5 percent after cyclone; the dispersant is hexametaphosphate, and the addition amount is controlled to be 0.2 percent;
step S102, grinding the slurry obtained in the step S101 through a sand mill; carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to a sand mill for circular grinding, and controlling the screen residue of 325 meshes; the flow rate of the sand mill is controlled to be 7t/h, the pressure of the cyclone is 0.25MPa, and the 325-mesh screen residue is 0.09 percent after the cyclone is carried out;
step S103, transferring the ground slurry obtained in the step S102 to a surface treatment tank, performing inorganic surface treatment, curing, and transferring the obtained surface treatment clinker to a treated tank;
(1) diluting the ground slurry to 300g/L, and heating to 45 ℃;
(2) phosphate solution and CeCl3Adding the solution into the slurry in a parallel flow manner, and curing for 30 minutes; wherein the phosphate is disodium hydrogen phosphate, sodium phosphate or their mixture, and has main content of P2O5The concentration is 40g/L, and the coating amount is TiO2Calculated as 0.8%; CeO (CeO)2The concentration of the main content is 30g/L, and the coating amount is TiO2Calculated as 0.2%; CeCl3Solution addition and flow: the addition amount and flow rate of the phosphate solution are 3: 1;
(3) adjusting the pH value to 7.0 by using a sodium hydroxide solution with the mass fraction of 12%, and curing for 30 minutes;
(4) performing secondary parallel flow coating and Al2(SO4)3Solution with NaAlO2Adding the solution in a parallel flow manner, controlling the pH value to be 6.5, and curing for 40 minutes; al (Al)2O3Coating amount of (2) with TiO2Calculated as 3.0%; the titanium dioxide has the water content of 0.8 percent, the pH value of 6.5 and the resistivity of more than 150 mu s.m; al (Al)2(SO4)3The main content concentration of the solution is 90g/L, and the acid content is 220 g/L; NaAlO2The main content concentration of the solution is 90g/L, and the alkali content is 200 g/L; NaAlO2Solution addition and flow: al (Al)2(SO4)3The addition amount and flow rate of the solution are 1: 0.8;
(5) adjusting the pH value to 6.0, curing to obtain clinker, and transferring the clinker into a treated groove;
step S104: transferring the slurry obtained in the step S103 to a plate-and-frame filter press for filter pressing, washing with desalted water, washing to remove redundant salt ions, controlling the end-point conductivity to be 90 mu S/cm, and controlling the solid content to be 65% to obtain a filter cake;
step S105: transferring the obtained filter cake to flash evaporation drying for drying to obtain powder;
step S106: and (5) performing jet milling on the powder obtained in the step (S105), and performing organic coating, wherein the addition amount of the organic coating agent is 0.3%, so as to obtain a titanium dioxide finished product.
Example 3
The preparation method of the rare earth composite coated titanium dioxide of the embodiment specifically comprises the following steps:
s101, rolling and grinding the titanium dioxide crude product, then feeding the ground titanium dioxide crude product into a pulping tank, simultaneously adding desalted water and a dispersing agent, uniformly stirring to obtain titanium dioxide crude product slurry, wet grinding the obtained slurry by a ball mill, carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to the pulping tank for circular grinding, and controlling 325-mesh screen residue; controlling the concentration of the titanium dioxide crude product slurry to be 800g/L, controlling the pressure of a swirler to be 0.3MPa, and controlling the 325-mesh screen residue to be 0.4 percent after swirling; the dispersant is PAAS, and the addition amount is controlled to be 0.8 percent;
step S102, grinding the slurry obtained in the step S101 through a sand mill; carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to a sand mill for circular grinding, and controlling the screen residue of 325 meshes; the flow rate of the sand mill is controlled to be 8t/h, the pressure of the cyclone is 0.35MPa, and the residue of the 325-mesh sieve after cyclone is controlled to be 0.05 percent;
step S103, transferring the ground slurry obtained in the step S102 to a surface treatment tank, performing inorganic surface treatment, curing, and transferring the obtained surface treatment clinker to a treated tank;
(1) diluting the ground slurry to 310g/L, and heating to 48 ℃;
(2) phosphate solution and CeCl3Adding the solution into the slurry in a parallel flow manner, and curing for 30 minutes; wherein the phosphate is disodium hydrogen phosphate, sodium phosphate or their mixture, and has main content of P2O5The concentration is 40g/L, and the coating amount is TiO2Calculated as 0.9%; CeO (CeO)2The concentration of the main content is 30g/L, and the coating amount is TiO2Calculated as 0.4%; CeCl3Solution addition and flow: the addition amount and flow rate of the phosphate solution are 3: 1;
(3) adjusting the pH to 7.0 by using a sodium hydroxide solution with the mass fraction of 12% and cationic guar gum with the mass percentage content of 5000ppm, and curing for 30 minutes;
(4) performing secondary parallel flow coating and Al2(SO4)3Solution with NaAlO2Adding the solution in a parallel flow manner, controlling the pH value to 7.0, and curing for 40 minutes; al (Al)2O3Coating amount of (2) with TiO2Calculated as 3.5%; the water content of the titanium pigment is 0.08 percent, the pH value is 7,the resistivity is more than 150 mu s.m; al (Al)2(SO4)3The main content concentration of the solution is 95g/L, and the acid content is 230 g/L; NaAlO2The main content concentration of the solution is 95g/L, and the alkali content is 210 g/L; NaAlO2Solution addition and flow: al (Al)2(SO4)3The addition amount and flow rate of the solution are 1: 0.9;
(5) adjusting the pH value to 6.0, curing to obtain clinker, and transferring the clinker into a treated groove;
step S104: transferring the slurry obtained in the step S103 to a plate-and-frame filter press for filter pressing, washing with desalted water, washing to remove redundant salt ions, controlling the end-point conductivity to be 80 mu S/cm, and controlling the solid content to be 70% to obtain a filter cake;
step S105: transferring the obtained filter cake to flash evaporation drying for drying to obtain powder;
step S106: and (5) performing jet milling on the powder obtained in the step (S105), and performing organic coating, wherein the addition amount of the organic coating agent is 0.6%, so as to obtain a titanium dioxide finished product.
Example 4
The preparation method of the rare earth composite coated titanium dioxide of the embodiment specifically comprises the following steps:
s101, rolling and grinding the titanium dioxide crude product, then feeding the ground titanium dioxide crude product into a pulping tank, simultaneously adding desalted water and a dispersing agent, uniformly stirring to obtain titanium dioxide crude product slurry, wet grinding the obtained slurry by a ball mill, carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to the pulping tank for circular grinding, and controlling 325-mesh screen residue; controlling the concentration of the titanium dioxide crude product slurry to be 750g/L, controlling the pressure of a swirler to be 0.32MPa, and controlling the 325-mesh screen residue to be 0.3 percent after swirling; the dispersant is PAAS, and the addition amount is controlled to be 1.0 percent;
step S102, grinding the slurry obtained in the step S101 through a sand mill; carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to a sand mill for circular grinding, and controlling the screen residue of 325 meshes; the flow rate of the sand mill is controlled to be 9t/h, the pressure of the cyclone is 0.3MPa, and the residue of the 325-mesh sieve after cyclone is controlled to be 0.04 percent;
step S103, transferring the ground slurry obtained in the step S102 to a surface treatment tank, performing inorganic surface treatment, curing, and transferring the obtained surface treatment clinker to a treated tank;
(1) diluting the ground slurry to 310g/L, and heating to 45 ℃;
(2) phosphate solution and CeCl3Adding the solution into the slurry in a parallel flow manner, and curing for 30 minutes; wherein the phosphate is disodium hydrogen phosphate, sodium phosphate or their mixture, and has main content of P2O5The concentration is 40g/L, and the coating amount is TiO2Calculated as 0.8%; CeO (CeO)2The concentration of the main content is 30g/L, and the coating amount is TiO2Calculated as 0.4%; CeCl3Solution addition and flow: the addition amount and flow rate of the phosphate solution are 3: 1;
(3) adjusting the pH value to 7.5 by using a sodium hydroxide solution with the mass fraction of 12%, and curing for 30 minutes;
(4) performing secondary parallel flow coating and Al2(SO4)3Solution with NaAlO2Adding the solution in a parallel flow manner, controlling the pH value to 7.5, and curing for 40 minutes; al (Al)2O3Coating amount of (2) with TiO2Calculated as 3.5%; the titanium dioxide has the water content of 0.9 percent, the pH value of 7.5 and the resistivity of more than 150 mu s.m; al (Al)2(SO4)3The main content concentration of the solution is 100g/L, and the acid content is 240 g/L; NaAlO2The main content concentration of the solution is 100g/L, and the alkali content is 220 g/L; NaAlO2Solution addition and flow: al (Al)2(SO4)3The addition amount and flow rate of the solution are 1: 1.0;
(5) adjusting the pH value to 6.5, curing to obtain clinker, and transferring the clinker into a treated groove;
step S104: transferring the slurry obtained in the step S103 to a plate-and-frame filter press for filter pressing, washing with desalted water, washing to remove redundant salt ions, controlling the end-point conductivity to be 100 mu S/cm, and controlling the solid content to be 65% to obtain a filter cake;
step S105: transferring the obtained filter cake to flash evaporation drying for drying to obtain powder;
step S106: and (5) performing jet milling on the powder obtained in the step (S105), and performing organic coating, wherein the addition amount of the organic coating agent is 0.7%, so as to obtain a titanium dioxide finished product.
Example 5
The preparation method of the rare earth composite coated titanium dioxide of the embodiment specifically comprises the following steps:
s101, rolling and grinding the titanium dioxide crude product, then feeding the ground titanium dioxide crude product into a pulping tank, simultaneously adding desalted water and a dispersing agent, uniformly stirring to obtain titanium dioxide crude product slurry, wet grinding the obtained slurry by a ball mill, carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to the pulping tank for circular grinding, and controlling 325-mesh screen residue; controlling the concentration of the titanium dioxide crude product slurry to be 850g/L, controlling the pressure of a swirler to be 0.3MPa, and controlling the 325-mesh screen residue to be 0.2% after swirling; the dispersant is PAAS, and the addition amount is controlled to be 0.8%;
step S102, grinding the slurry obtained in the step S101 through a sand mill; carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to a sand mill for circular grinding, and controlling the screen residue of 325 meshes; the flow rate of the sand mill is controlled to be 8t/h, the pressure of the cyclone is 0.25MPa, and the residue of the 325-mesh sieve after cyclone is controlled to be 0.06 percent;
step S103, transferring the ground slurry obtained in the step S102 to a surface treatment tank, performing inorganic surface treatment, curing, and transferring the obtained surface treatment clinker to a treated tank;
(1) diluting the ground slurry to 320g/L, and heating to 50 ℃;
(2) phosphate solution and CeCl3Adding the solution into the slurry in a parallel flow manner, and curing for 30 minutes; wherein the phosphate is disodium hydrogen phosphate, sodium phosphate or their mixture, and has main content of P2O5The concentration is 40g/L, and the coating amount is 1.5 percent; CeO (CeO)2The concentration of the main content is 30g/L, and the coating amount is 0.4%; CeCl3Solution addition and flow: the addition amount and flow rate of the phosphate solution are 3: 1;
(3) adjusting pH to 7.0 with dilute alkali solution, and aging for 30 min;
(4) performing secondary parallel flow coating and Al2(SO4)3Solution with NaAlO2Adding the solution in parallel, controlling pH to 6.5, aging for 40 minA clock; al (Al)2O3The coating amount of (2) was 3.0%; the water content of the titanium dioxide is less than 1 percent, the pH value is 6.5, and the resistivity is more than 150 mu s.m; al (Al)2(SO4)3The main content concentration of the solution is 90g/L, and the acid content is 220 g/L; NaAlO2The main content concentration of the solution is 90g/L, and the alkali content is 200 g/L; NaAlO2Solution addition and flow: al (Al)2(SO4)3The addition amount and flow rate of the solution are 1: 0.8;
(5) adjusting the pH value to 6.0, curing to obtain clinker, and transferring the clinker into a treated groove;
step S104: transferring the slurry obtained in the step S103 to a plate-and-frame filter press for filter pressing, washing with desalted water, washing to remove redundant salt ions, controlling the end-point conductivity to be 90 mu S/cm, and controlling the solid content to be 70% to obtain a filter cake;
step S105: transferring the obtained filter cake to flash evaporation drying for drying to obtain powder;
step S106: and (5) performing jet milling on the powder obtained in the step (S105), and performing organic coating, wherein the addition amount of the organic coating agent is 0.6%, so as to obtain a titanium dioxide finished product.
Performance testing
Respectively preparing the titanium dioxide finished products obtained in the embodiments 1-5 of the invention into water-based paint and oil-based paint, wherein the water-based paint and the oil-based paint are both in the prior art, and the formula of the water-based paint is provided by the Suzu corporation; oil paint formulations are supplied by Xuanwei corporation.
Putting the glass fiber into an ultraviolet artificial aging box for aging test for a certain time, and testing the color and the glossiness every preset time, wherein the specific color difference and the glossiness change are as follows:
preparing a sample: the coating is well prepared and then scraped on a standard test board, the standard test board is dried according to the national standard requirement, the gloss and the hue are detected, the test board is put in QUV for testing, the test standard is that the test board is taken out after AASTMG154 reaches the specified test total time, the gloss and the hue of the test board are detected, the appearance (whether cracking, rusting and the like) of the test board is evaluated, compared with the previous test data, the Delta E, the light loss rate and the like are calculated, and the aging condition is judged according to the national standard requirement. Wherein, the comparison sample is water paint or oil paint without the titanium dioxide.
Firstly, water-based paint:
(1) the water paint sample is put into QUV for 300h, 600h, 900h, 1200h and 1500h, and the color difference data are respectively measured as shown in the following table 1:
TABLE 1 color difference data for waterborne coatings of examples 1-5
And (3) analysis: the color difference of the ultraviolet artificial aging box after irradiation for 300h, 600h, 900h, 1200h and 1500h can be seen, compared with a comparison sample, the color difference of the product of the invention during each irradiation time period is better than that of the comparison sample, and particularly after irradiation for 1500h, the color difference of the comparison sample is far greater than that of the product of the patent. The product of the invention can be completely used for water-based paint and is far better than a comparison sample.
(2) The water-based paint panels were placed in QUV for 300h, 600h, 900h, 1200h, 1500h and measured for 60 ° gloss, respectively, as shown in table 2:
TABLE 2 waterborne coatings from examples 1-5 have 60 ° gloss data
And (3) analysis: the initial gloss of the comparison sample is similar to that of six samples of the product of the invention, the data deviation is not large after the illumination for 300h, but the gloss of the product of the invention is not changed greatly after the illumination for 600h, and is slightly reduced, while the reduction of the comparison sample is more, which shows that the light resistance of the product of the invention is far better than that of the comparison sample in gloss, the product of the invention can be used for water paint, and the light resistance is better.
Secondly, oil paint:
(1) the oil paint sample plate was placed in QUV for 300h, 600h, 900h, 1200h, 1500h, and the color difference data were measured as shown in table 3:
TABLE 3 color difference data for oil-based paints of examples 1-5
And (3) analysis: the color difference of the ultraviolet artificial aging box after irradiation for 300h, 600h, 900h, 1200h and 1500h can be seen, compared with a comparison sample, the color difference of the product of the invention during each irradiation time period is better than that of the comparison sample, particularly, after the irradiation for 900h, the color difference of the comparison sample is obviously greater than that of the product of the patent, and after the irradiation for 1500h, the product of the invention is obviously superior to that of the comparison sample. The product of the invention can be completely used for oil paint.
(2) The oily paint panels were placed in QUV for 300h, 600h, 900h, 1200h, 1500h and their 60 ° gloss was measured separately as shown in table 4:
TABLE 4 oily coating 60 ℃ gloss data for examples 1-5
And (3) analysis: the data show that the glossiness of the oil paint prepared by the product of the invention is not changed greatly after the oil paint is irradiated by an ultraviolet artificial aging box, and the glossiness is not changed greatly even after the oil paint is irradiated for 1500 hours. And the contrast sample is irradiated by ultraviolet light, and the glossiness is obviously reduced. The product of the invention is completely suitable for oil paint and is far better than a comparison sample.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the rare earth composite coated titanium dioxide comprises the steps of pulping, grinding, inorganic surface treatment, washing, drying, airflow crushing and organic coating, and is characterized by comprising the following steps:
s101, rolling and grinding the titanium dioxide crude product, then feeding the ground titanium dioxide crude product into a pulping tank, simultaneously adding desalted water and a dispersing agent, uniformly stirring to obtain titanium dioxide crude product slurry, wet grinding the obtained slurry by a ball mill, carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to the pulping tank for circular grinding, and controlling 325-mesh screen residue;
step S102, grinding the slurry obtained in the step S101 through a sand mill; carrying out cyclone classification, transferring screened qualified slurry into the next process, transferring unqualified slurry back to a sand mill for circular grinding, and controlling the screen residue of 325 meshes;
step S103, transferring the ground slurry obtained in the step S102 to a surface treatment tank, performing inorganic surface treatment, curing, and transferring the obtained surface treatment clinker to a treated tank;
(1) diluting the ground slurry to 320g/L of 300-;
(2) phosphate solution and CeCl3Adding the solution into the diluted slurry in a parallel flow manner, and curing for 30 minutes;
(3) adjusting the pH value to 7.0-7.5 by using a dilute alkali solution with the mass fraction of 12%, and curing for 30 minutes;
(4) performing secondary parallel flow coating and Al2(SO4)3Solution with NaAlO2Adding the solution in a parallel flow manner, controlling the pH value to be 6.5-7.5, and curing for 40 minutes;
(5) adjusting the pH value to 6.0-6.5, curing for 30 minutes to obtain clinker, and transferring the clinker into a treated groove;
s104, transferring the slurry obtained in the step S103 to a plate-and-frame filter press for filter pressing, washing with desalted water, washing to remove redundant salt ions, controlling the end-point conductivity to be below 100 mu S/cm, and controlling the solid content to be 65% -75% to obtain a filter cake;
s105, transferring the obtained filter cake to flash evaporation drying for drying to obtain powder;
and S106, performing jet milling on the powder obtained in the step S105, and performing organic coating to obtain a titanium dioxide finished product.
2. The preparation method of rare earth composite coated titanium dioxide according to claim 1, wherein in step S101, the concentration of the slurry of crude titanium dioxide is controlled at 700-900g/L, the pressure of the cyclone is 0.25-0.4MPa, and the residue of 325 mesh after cyclone is less than 0.5%; the dispersant is PAAS or hexametaphosphoric acid, and the addition amount is TiO2The meter is controlled between 0.2% and 2.0%.
3. The preparation method of the rare earth composite coated titanium dioxide according to claim 1, wherein in step S102, the flow rate of the sand mill is controlled to be 7-10t/h, the pressure of the cyclone is 0.25-0.4MPa, and the residue of the 325-mesh sieve after cyclone is controlled to be below 0.1%.
4. The method for preparing rare earth composite coated titanium dioxide according to claim 1, wherein the phosphate in step S103 is disodium hydrogen phosphate, sodium phosphate or a mixture of the two, and the main content P is2O5The concentration is 40g/L, and the coating amount is TiO2Calculated as 0.8 to 2.0 percent.
5. The preparation method of the rare earth composite coated titanium dioxide as claimed in claim 1, wherein CeO in step S1032The concentration of the main content is 30g/L, and the coating amount is TiO2Calculated as 0.2% -0.5%; phosphate solution with CeCl3The solution flow ratio is 1: 3.
6. the preparation method of the rare earth composite coated titanium dioxide according to claim 1, wherein Al in step S1032(SO4)3The main content concentration of the solution is 90-100g/L, and the acid content is 220-240 g/L; NaAlO2The main content concentration of the solution is 90-100g/L, and the alkali content is 200-220 g/L; NaAlO2Solution addition and flow: al (Al)2(SO4)3The addition amount and flow rate of the solution are 1: 0.8-1.0.
7. The preparation method of the rare earth composite coated titanium dioxide according to claim 1, wherein the concentration of the dilute alkali in the step S103 is 10-15%；Al2O3Coating amount of (2) with TiO23.0-4.0% in terms of weight; the titanium dioxide has a water content of less than 1%, a pH value of 6.5-8.5, and a resistivity of more than 150 μ s · m.
8. The preparation method of the rare earth composite coated titanium dioxide according to claim 2, wherein the amount of the organic coating agent added in step S106 is TiO2Calculated as 0.3 to 1.0 percent.
9. Titanium dioxide obtainable by the process according to any one of claims 1 to 8.
10. Use of the titanium dioxide according to claim 9 in coatings, plastics, inks, paper.
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