CN109321002B - Preparation method of titanium dioxide silicon zirconium aluminum ternary coating film by chlorination process - Google Patents
Preparation method of titanium dioxide silicon zirconium aluminum ternary coating film by chlorination process Download PDFInfo
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Abstract
The invention relates to a preparation method of a titanium dioxide silicon zirconium aluminum ternary coating film by a chlorination method, which comprises the following steps: A. preparing titanium dioxide into suspension with the concentration of 500-600 g/L by using distilled water, adjusting the pH value to 9.5-10.5 by using NaOH aqueous solution, adding sodium metasilicate, and stirring to prepare titanium dioxide slurry; B. grinding and dispersing the slurry for 60-80 min by using a sand mill; C. pumping the ground and dispersed slurry into a coating tank, and heating to 60-80 ℃; D. adding a zirconium sulfate aqueous solution and an aluminum sulfate aqueous solution in a concurrent flow manner, and stirring at a constant temperature; adjusting the pH value to 7.0-8.0 by NaOH, and preserving heat, stirring and curing for 90-120 min; E. filtering and washing the cured silicon-zirconium-aluminum coated titanium dioxide by using distilled water at the temperature of 50-60 ℃; F. and carrying out flash drying and airflow crushing on the filtered and washed silicon-zirconium-aluminum ternary coated titanium dioxide to obtain the silicon-zirconium-aluminum ternary coated titanium dioxide. The method has the advantages of simple process, simple operation, energy conservation and environmental protection, and the titanium dioxide after ternary coating has good glossiness, water dispersibility and weather resistance.
Description
Technical Field
The invention belongs to the technical field of chemical production, and particularly relates to a preparation method of a titanium dioxide silicon zirconium aluminum ternary coating film by a chlorination process.
Background
The titanium dioxide has excellent whiteness, decolorization, weather resistance, heat resistance and chemical stability, particularly no toxicity, and can be widely applied to the fields of coatings, plastics, papermaking, printing ink, chemical fibers, rubber, cosmetics, foods, medicines and the like. The main production process of titanium dioxide is sulfuric acid process and chlorination process, the sulfuric acid process is a traditional process, the method has the advantages of complex operation, long flow and great environmental pollution, the chlorination process has advanced production technology, great production capacity, low comprehensive energy consumption, good product quality, recyclable chlorine gas, simple process, realization of intelligent operation and great reduction of human resources, and becomes the mainstream trend of the titanium dioxide production process in the world at present.
Because titanium dioxide has higher photochemical activity, photochemical reaction can occur under the condition of illumination, organic substances can be damaged, the weather resistance of the material is weakened, and phenomena of easy pulverization, yellowing, cracking, shedding and the like occur, so that the service life and the performance of the product are seriously influenced. Meanwhile, because titanium dioxide is a hydrophilic and oleophobic substance, the titanium dioxide which is not coated on the surface has poor dispersibility in various solvents and water-based coatings. The preparation process of the titanium dioxide can not change the photochemical defect, only can reduce the photochemical activity, and in order to improve the dispersibility, the optical stability, the weather resistance and other properties of the titanium dioxide and endow the titanium dioxide with new application properties, the surface of the titanium dioxide needs to be subjected to coating treatment.
The most widely used inorganic coating at home and abroad is oxide of silicon, aluminum, zirconium, cerium, manganese and the like, namely, acidic or alkaline coating agent is added into titanium dioxide slurry with a certain concentration, and then neutralized by alkali or acid, so that the coating agent is precipitated on the particle surface in the form of hydrated oxide under a certain condition, but the use of single oxide as a film forming substance has many defects and cannot meet the use requirement of improving weather resistance and dispersibility, and binary or multi-component composite coating is often carried out. Because the composite coating process is complex and difficult to realize, few researchers are at home and abroad.
Disclosure of Invention
The invention aims to provide a preparation method of a silicon-zirconium-aluminum ternary coating film of titanium dioxide produced by a chlorination method, which is used for carrying out silicon-zirconium-aluminum ternary coating on rutile titanium dioxide produced by the chlorination method, optimizing the coating process and improving the glossiness, water dispersibility and high weather resistance of the coated titanium dioxide.
The technical scheme adopted by the invention is as follows: the preparation method of the chlorination-process titanium dioxide silicon zirconium aluminum ternary coating comprises the following steps:
A. preparing slurry: preparing titanium dioxide prepared by a chlorination method into a titanium dioxide suspension with the concentration of 500-600 g/L by using distilled water, adjusting the pH value of the titanium dioxide suspension to 9.5-10.5 by using a NaOH aqueous solution, adding a dispersing agent sodium metasilicate, and stirring at the rotating speed of 300-400 r/min for 20-30 min to prepare titanium dioxide slurry;
B. grinding the slurry: b, grinding and dispersing the titanium dioxide slurry prepared in the step A for 60-80 min by using a sand mill;
C. heating the slurry: pumping the ground and dispersed titanium dioxide slurry into a coating tank, and heating to 60-80 ℃;
D. coating with silicon, zirconium and aluminum: by combining two peristaltic pumps simultaneouslyAqueous zirconium sulfate solution and aqueous aluminum sulfate solution are fed in a stream, the amount of the aqueous zirconium sulfate solution being ZrO2Calculated as TiO in the slurry22.0-3.0% of the mass, and the addition amount of the aluminum sulfate aqueous solution is Al2O3Calculated as TiO in the slurry22.5-3.5% of the mass, keeping the temperature at 60-80 ℃ in the adding process, and stirring at the rotating speed of 600-800 r/min; after the addition, adjusting the pH value of the slurry to 7.0-8.0 by using a NaOH aqueous solution, and continuing to preserve heat, stir and cure for 90-120 min to generate silicon-zirconium-aluminum coated titanium dioxide;
E. filtering and washing: filtering and washing the cured silicon-zirconium-aluminum coated titanium dioxide by using distilled water at the temperature of 50-60 ℃ until the conductivity of the filtrate is less than 10 mu s/cm;
F. drying and crushing: and carrying out flash drying and airflow crushing on the filtered and washed silicon-zirconium-aluminum ternary coated titanium dioxide to obtain the silicon-zirconium-aluminum ternary coated titanium dioxide.
The sodium metasilicate is added in SiO2Calculated as TiO in the slurry22.0-3.0% by mass of zirconium sulfate aqueous solution, the concentration of zirconium sulfate aqueous solution being ZrO 22Calculated as 80-100 g/L, the concentration of the aluminum sulfate aqueous solution is Al2O3The concentration is 90-110 g/L, and the concentration of the sodium hydroxide aqueous solution is 100-200 g/L. And D, simultaneously adding the zirconium sulfate aqueous solution and the aluminum sulfate aqueous solution in parallel by using a peristaltic pump for 40-60 min. And B, the average particle size of the titanium dioxide in the ground titanium dioxide slurry is less than or equal to 1.0 mu m. And F, the average grain diameter of the silicon-zirconium-aluminum ternary coated titanium dioxide prepared in the step F is less than or equal to 0.30 mu m. The titanium dioxide is rutile titanium dioxide prepared by a chlorination method.
The technical indexes of the rutile type titanium dioxide prepared by the chlorination method are as follows: TiO 22The content is more than or equal to 92 weight percent, the average grain diameter is less than or equal to 5.0 mu m, and rutile TiO2The content is more than or equal to 97 wt%, the pH value is 6.5-8.5, the screen residue (45 mu m) is less than or equal to 0.06%, the L value is more than or equal to 97%, the water dispersibility is more than or equal to 49%, and the reynolds number of the decoloring force is more than or equal to 1300.
Compared with the prior art, the invention has the beneficial effects that: the rutile titanium dioxide produced by the chlorination process is subjected to silicon-zirconium-aluminum ternary coating surface treatment, so that the catalytic activity of the titanium dioxide is reduced, the water dispersibility of the titanium dioxide is improved, and the improvement on the water dispersibility of the titanium dioxideThe weather resistance and the chalking resistance are improved. Secondly, in the preparation of the slurry, NaOH is used for adjusting the pH value of the slurry, and sodium metasilicate serving as a dispersing agent is added, so that the dispersing effect of titanium dioxide in water is optimized, no precipitate is formed, and the uniformity of the coating is ensured. In addition, sodium metasilicate is also used as grinding aid and SiO2Coating agent, under the condition of 60-80 ℃, when the zirconium sulfate solution and the aluminum sulfate solution are gradually added in parallel, the pH value of the solution is gradually reduced, and sodium metasilicate begins to hydrolyze to form SiO2The coating is precipitated on the surface of the titanium dioxide. And thirdly, adding a mixed solution of zirconium sulfate and aluminum sulfate into the slurry in a parallel flow manner, adjusting the pH value of the slurry to 7.0-8.0 by using a NaOH aqueous solution at the temperature of 60-80 ℃, carrying out coprecipitation chemical reaction on zirconium oxide and aluminum oxide, and then curing to form a silicon-zirconium-aluminum ternary coating on the surface of titanium dioxide. And fourthly, the coating production period is short, the energy consumption is reduced, and the production cost is saved.
The preparation method of the chloride-process titanium dioxide silicon zirconium aluminum ternary coating adopts the simultaneous parallel flow addition of the zirconium sulfate aqueous solution and the aluminum sulfate aqueous solution, and the coprecipitation chemical reaction is carried out to carry out the silicon zirconium aluminum ternary coating on the rutile-type titanium dioxide produced by the chloride process, so that the technical process is simple, the operation is simple and convenient, the energy is saved, the environment is protected, the quality of the titanium dioxide is improved, and the titanium dioxide after the ternary coating has good glossiness, water dispersibility and weather resistance.
Detailed Description
The present invention will be described in detail with reference to examples. The scope of protection of the invention is not limited to the embodiments, and any modification made by those skilled in the art within the scope defined by the claims also falls within the scope of protection of the invention.
Example 1
The invention relates to a preparation method of a titanium dioxide silicon zirconium aluminum ternary coating by a chlorination method, which comprises the following steps:
A. preparing slurry: preparing titanium dioxide prepared by chlorination method into titanium dioxide suspension with concentration of 500g/L by using distilled water, adjusting pH value of the titanium dioxide suspension to 9.5 by using NaOH aqueous solution with concentration of 100g/L, adding dispersing agent sodium metasilicate, and adding SiO2Calculated as TiO in the slurry2Quality of2.0 percent of the titanium dioxide slurry, and then stirring the mixture for 20min at the rotating speed of 300r/min to prepare titanium dioxide slurry;
B. grinding the slurry: b, grinding and dispersing the titanium dioxide slurry prepared in the step A for 60min by using a sand mill, wherein the average particle size of the ground titanium dioxide is less than or equal to 1.0 mu m;
C. heating the slurry: b, pumping the titanium dioxide slurry ground in the step B into a coating tank, and heating to 60 ℃;
D. coating with silicon, zirconium and aluminum: adding zirconium sulfate aqueous solution into the mixture by a peristaltic pump, wherein the adding amount is ZrO2Calculated as TiO in the slurry22.0% by mass, concentration of zirconium sulfate aqueous solution as ZrO2The weight is 80 g/L; simultaneously, a peristaltic pump is used for adding aluminum sulfate aqueous solution in parallel flow, and the adding amount is Al2O3Calculated as TiO in the slurry22.5% by mass, the concentration of the aluminum sulfate aqueous solution being Al2O3The volume is 90g/L, the parallel flow adding time of the zirconium sulfate solution and the aluminum sulfate solution is 40min, the adding process is kept at 60 ℃, and the stirring is carried out at the rotating speed of 600 r/min; after the addition, the pH value of the slurry is adjusted to 7.0 by using a NaOH aqueous solution with the concentration of 100g/L, and the slurry is continuously stirred and aged for 90min under the condition of heat preservation to generate silicon-zirconium-aluminum coated titanium dioxide;
E. filtering and washing: d, filtering and washing the aged silicon-zirconium-aluminum coated titanium dioxide in the step D by using distilled water at 50 ℃ until the conductivity of the filtrate is less than 10 mu s/cm;
F. drying and crushing: and E, carrying out flash drying and airflow crushing on the silicon-zirconium-aluminum ternary coated titanium dioxide filtered and washed in the step E to obtain the silicon-zirconium-aluminum ternary coated titanium dioxide.
Example 2
The method comprises the following steps:
A. preparing slurry: preparing titanium dioxide prepared by chlorination process into 550g/L titanium dioxide suspension with distilled water, adjusting pH of the titanium dioxide suspension to 10.0 with 150g/L NaOH aqueous solution, adding sodium metasilicate as dispersant, adding SiO2Measured as TiO in the slurry22.5 percent of the mass, and then stirring the mixture for 25min at the rotating speed of 350r/min to prepare titanium dioxide slurry;
B. grinding the slurry: b, grinding and dispersing the titanium dioxide slurry prepared in the step A for 70min by using a sand mill, wherein the average particle size of the ground titanium dioxide is less than or equal to 1.0 mu m;
C. heating the slurry: b, pumping the titanium dioxide slurry ground in the step B into a coating tank, and heating to 70 ℃;
D. coating with silicon, zirconium and aluminum: adding zirconium sulfate aqueous solution into the mixture by a peristaltic pump, wherein the adding amount is ZrO2Calculated as TiO in the slurry22.5% by mass, concentration of zirconium sulfate aqueous solution as ZrO2The weight is 90 g/L; simultaneously, a peristaltic pump is used for adding aluminum sulfate aqueous solution in parallel flow, and the adding amount is Al2O3Calculated as TiO in the slurry23.5% by mass, the concentration of the aluminum sulfate aqueous solution being Al2O3The volume is 100g/L, the parallel flow adding time of the zirconium sulfate solution and the aluminum sulfate solution is 40min, the adding process is kept at 70 ℃, and the stirring is carried out at the rotating speed of 700 r/min; after the addition, the pH value of the slurry is adjusted to 7.5 by using a NaOH aqueous solution with the concentration of 150g/L, and the slurry is continuously stirred and aged for 100min under the condition of heat preservation to generate silicon-zirconium-aluminum coated titanium dioxide;
E. filtering and washing: d, filtering and washing the aged silicon-zirconium-aluminum coated titanium dioxide in the step D by using distilled water at 55 ℃ until the conductivity of the filtrate is less than 10 mu s/cm;
F. drying and crushing: and E, carrying out flash drying and airflow crushing on the silicon-zirconium-aluminum ternary coated titanium dioxide filtered and washed in the step E to obtain the silicon-zirconium-aluminum ternary coated titanium dioxide.
Example 3
The method comprises the following steps:
A. preparing slurry: preparing titanium dioxide prepared by chlorination method into titanium dioxide suspension with concentration of 600g/L by using distilled water, adjusting pH value of the titanium dioxide suspension to 10.5 by using NaOH aqueous solution with concentration of 200g/L, adding dispersing agent sodium metasilicate, and adding SiO2Calculated as TiO in the slurry23.0 percent of the mass, and then stirring the mixture for 30min at the rotating speed of 400r/min to prepare titanium dioxide slurry;
B. grinding the slurry: b, grinding and dispersing the titanium dioxide slurry prepared in the step A for 80min by using a sand mill, wherein the average particle size of the ground titanium dioxide is less than or equal to 1.0 mu m;
C. heating the slurry: b, pumping the titanium dioxide slurry ground in the step B into a coating tank, and heating to 80 ℃;
D. coating with silicon, zirconium and aluminum: adding zirconium sulfate aqueous solution into the mixture by a peristaltic pump, wherein the adding amount is ZrO2Calculated as TiO in the slurry23.0% by mass, concentration of zirconium sulfate aqueous solution as ZrO2The weight is 100 g/L; simultaneously, a peristaltic pump is used for adding aluminum sulfate aqueous solution in parallel flow, and the adding amount is Al2O3Calculated as TiO in the slurry23.5% by mass, the concentration of the aluminum sulfate aqueous solution being Al2O3The adding time is 60min, the temperature is kept at 80 ℃ in the adding process, and the stirring is carried out at the rotating speed of 800 r/min; after the addition, the pH value of the slurry is adjusted to 8.0 by using a NaOH aqueous solution with the concentration of 200g/L, and the slurry is continuously kept at the temperature and stirred for curing for 110min to generate silicon-zirconium-aluminum coated titanium dioxide;
E. filtering and washing: d, filtering and washing the aged silicon-zirconium-aluminum coated titanium dioxide in the step D by using distilled water at the temperature of 60 ℃ until the conductivity of the filtrate is less than 10 mu s/cm;
F. drying and crushing: and E, carrying out flash drying and airflow crushing on the silicon-zirconium-aluminum ternary coated titanium dioxide filtered and washed in the step E to obtain the silicon-zirconium-aluminum ternary coated titanium dioxide.
Example 4
The method comprises the following steps:
A. preparing slurry: preparing titanium dioxide prepared by chlorination process into 550g/L titanium dioxide suspension with distilled water, adjusting pH of the titanium dioxide suspension to 10.5 with 200g/L NaOH aqueous solution, adding sodium metasilicate as dispersant, adding SiO2Calculated as TiO in the slurry22.5 percent of the mass, and then stirring the mixture for 25min at the rotating speed of 400r/min to prepare titanium dioxide slurry;
B. grinding the slurry: b, grinding and dispersing the titanium dioxide slurry prepared in the step A for 70min by using a sand mill, wherein the average particle size of the ground titanium dioxide is less than or equal to 1.0 mu m;
C. heating the slurry: b, pumping the titanium dioxide slurry ground in the step B into a coating tank, and heating to 75 ℃;
D、coating with silicon, zirconium and aluminum: adding zirconium sulfate aqueous solution into the mixture by a peristaltic pump, wherein the adding amount is ZrO2Calculated as TiO in the slurry23.0% by mass, concentration of zirconium sulfate aqueous solution as ZrO2The weight is 95 g/L; simultaneously, a peristaltic pump is used for adding aluminum sulfate aqueous solution in parallel flow, and the adding amount is Al2O3Calculated as TiO in the slurry23.0% by mass of aluminum sulfate aqueous solution, concentration of aluminum sulfate aqueous solution being Al2O3The volume is 105g/L, the parallel flow adding time of the zirconium sulfate solution and the aluminum sulfate solution is 55min, the adding process is kept at 75 ℃, and the stirring is carried out at the rotating speed of 750 r/min; after the addition, the pH value of the slurry is adjusted to 7.8 by using a NaOH aqueous solution with the concentration of 200g/L, and the slurry is continuously kept at the temperature and stirred for curing for 120min to generate silicon-zirconium-aluminum coated titanium dioxide;
E. filtering and washing: d, filtering and washing the aged silicon-zirconium-aluminum coated titanium dioxide in the step D by using distilled water at the temperature of 60 ℃ until the conductivity of the filtrate is less than 10 mu s/cm;
F. drying and crushing: and E, carrying out flash drying and airflow crushing on the silicon-zirconium-aluminum ternary coated titanium dioxide filtered and washed in the step E to obtain the silicon-zirconium-aluminum ternary coated titanium dioxide.
Comparative example 1 is a rutile titanium dioxide feedstock prepared by the chloride process used in the present invention.
The performance test results of the silicon-aluminum-zirconium ternary coated titanium dioxide prepared in the embodiments 1-4 of the invention and the titanium dioxide used in the comparative example 1 are shown in table 1.
TABLE 1 titanium dioxide Performance test results
The test results in Table 1 show that the silicon-aluminum-zirconium ternary coated titanium dioxide prepared by the preparation method of the chlorination-process titanium dioxide silicon-zirconium-aluminum ternary coating has good whiteness, glossiness, water dispersibility and decoloring capability.
Application test
The silicon-aluminum-zirconium ternary coated titanium dioxide prepared in the embodiments 1 to 4 and the titanium dioxide prepared in the comparative example 1 are applied to the aqueous acrylic resin coatingIn the material, the material is qualified by detection according to the standard HG/T4758-2014 and is used as a matrix coating for a test. The addition amounts of titanium dioxide were 5% by weight of the aqueous acrylic resin coating, and the weathering performance of the coating was tested with the pure aqueous acrylic resin coating as control example 1 of this test, the coating thickness being 0.1 mm. The test plate base material for preparing the coating and the surface treatment are carried out according to the national standard GB/T9271-2008, the weather resistance is tested according to GB/T1766-2008, the artificial accelerated aging is adopted, and the xenon lamp illumination intensity is 300W/m2And the illumination time is 200 h. The test results are shown in table 2.
TABLE 2 weather resistance test results for the coatings
As can be seen from the application test results in Table 2, the silicon-zirconium-aluminum ternary coated titanium dioxide prepared by the invention has obviously improved weather resistance on the water-based acrylic resin coating.
Claims (5)
1. A preparation method of titanium dioxide silicon zirconium aluminum ternary coating by chlorination method is characterized in that: the method comprises the following steps:
A. preparing slurry: preparing titanium dioxide prepared by a chlorination method into a titanium dioxide suspension with the concentration of 500-600 g/L by using distilled water, adjusting the pH value of the titanium dioxide suspension to 9.5-10.5 by using a NaOH aqueous solution, adding a dispersing agent sodium metasilicate, and stirring at the rotating speed of 300-400 r/min for 20-30 min to prepare titanium dioxide slurry;
B. grinding the slurry: b, grinding and dispersing the titanium dioxide slurry prepared in the step A for 60-80 min by using a sand mill;
C. heating the slurry: pumping the ground and dispersed titanium dioxide slurry into a coating tank, and heating to 60-80 ℃;
D. coating with silicon, zirconium and aluminum: using two peristaltic pumps simultaneouslyAdding zirconium sulfate aqueous solution and aluminum sulfate aqueous solution in parallel, wherein the adding amount of the zirconium sulfate aqueous solution is ZrO2Calculated as TiO in the slurry22.0-3.0% of the mass, and the addition amount of the aluminum sulfate aqueous solution is Al2O3Calculated as TiO in the slurry22.5-3.5% of the mass, keeping the temperature at 60-80 ℃ in the adding process, and stirring at the rotating speed of 600-800 r/min; after the addition, adjusting the pH value of the slurry to 7.0-8.0 by using a NaOH aqueous solution, and continuing to preserve heat, stir and cure for 90-120 min to generate silicon-zirconium-aluminum coated titanium dioxide;
E. filtering and washing: filtering and washing the cured silicon-zirconium-aluminum coated titanium dioxide by using distilled water at the temperature of 50-60 ℃ until the conductivity of the filtrate is less than 10 mu s/cm;
F. drying and crushing: carrying out flash drying and airflow crushing on the filtered and washed silicon-zirconium-aluminum ternary coated titanium dioxide to prepare silicon-zirconium-aluminum ternary coated titanium dioxide;
the addition amount of the sodium metasilicate is SiO2Calculated as TiO in the slurry22.0-3.0% by mass of zirconium sulfate aqueous solution, the concentration of zirconium sulfate aqueous solution being ZrO 22Calculated as 80-100 g/L, the concentration of the aluminum sulfate aqueous solution is Al2O3The concentration is 90-110 g/L, and the concentration of the sodium hydroxide aqueous solution is 100-200 g/L;
the quality indexes of the titanium dioxide prepared by the chlorination method are as follows: TiO 22The content is more than or equal to 92 weight percent, the average grain diameter is less than or equal to 5.0 mu m, and rutile TiO2The content is more than or equal to 97 wt%, the pH value is 6.5-8.5, the sieve residue is less than or equal to 0.06% with the particle size of 45 mu m, the L value is more than or equal to 97%, the water dispersibility is more than or equal to 49%, and the reynolds number of the achromatism is more than or equal to 1300.
2. The preparation method of the chlorination-process titanium dioxide silicon zirconium aluminum ternary coating film according to claim 1, characterized in that: and D, simultaneously adding the zirconium sulfate aqueous solution and the aluminum sulfate aqueous solution in parallel by using a peristaltic pump for 40-60 min.
3. The preparation method of the chlorination-process titanium dioxide silicon zirconium aluminum ternary coating film according to claim 1, characterized in that: and B, grinding the titanium dioxide slurry in the step B to obtain the titanium dioxide slurry, wherein the average particle size of the titanium dioxide in the titanium dioxide slurry is less than or equal to 1.0 mu m.
4. The preparation method of the chlorination-process titanium dioxide silicon zirconium aluminum ternary coating film according to claim 1, characterized in that: and F, the average grain diameter of the silicon-zirconium-aluminum ternary coated titanium dioxide prepared in the step F is less than or equal to 0.30 mu m.
5. The preparation method of the chlorination-process titanium dioxide silicon zirconium aluminum ternary coating film according to claim 1, characterized in that: the titanium dioxide is rutile titanium dioxide prepared by a chlorination method.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811088102.8A CN109321002B (en) | 2018-09-18 | 2018-09-18 | Preparation method of titanium dioxide silicon zirconium aluminum ternary coating film by chlorination process |
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| CN201811088102.8A CN109321002B (en) | 2018-09-18 | 2018-09-18 | Preparation method of titanium dioxide silicon zirconium aluminum ternary coating film by chlorination process |
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| CN109321002B true CN109321002B (en) | 2020-12-04 |
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| CN108083331A (en) * | 2017-12-29 | 2018-05-29 | 广东惠云钛业股份有限公司 | A kind of preparation method of rutile titanium dioxide superfine powder |
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| CN108083331A (en) * | 2017-12-29 | 2018-05-29 | 广东惠云钛业股份有限公司 | A kind of preparation method of rutile titanium dioxide superfine powder |
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