CN112239227B - Preparation method of conductive titanium dioxide - Google Patents
Preparation method of conductive titanium dioxide Download PDFInfo
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- CN112239227B CN112239227B CN202011178005.5A CN202011178005A CN112239227B CN 112239227 B CN112239227 B CN 112239227B CN 202011178005 A CN202011178005 A CN 202011178005A CN 112239227 B CN112239227 B CN 112239227B
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- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
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- C01G23/00—Compounds of titanium
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- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
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- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/08—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances oxides
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Abstract
The invention relates to a preparation method of conductive titanium dioxide in the technical field of titanium dioxide preparation, which comprises the steps of preparing titanium dioxide slurry, heating the slurry to 40-60 ℃, simultaneously adding a metered lithium salt solution, a ferrous sulfate solution and a phosphate-containing solution, wherein the phosphate-containing solution adopts phosphoric acid and/or a phosphate solution, the addition amount of the lithium salt, the ferrous sulfate, the phosphoric acid and/or the phosphate is respectively 3-15 wt% of titanium dioxide, adjusting the pH value of the slurry to 8.0-10.0 by using inorganic alkali solution, carrying out hydrothermal reaction at the temperature of 150-400 ℃, and adjusting the pH value of the slurry to 7-10 when the temperature of the slurry is reduced to below 80 ℃; adding zinc salt solution into the slurry, wherein the addition amount of zinc salt is 1-20wt% of titanium dioxide, sieving, washing with water, drying and crushing. The invention combines the conductivity of lithium iron phosphate with the titanium pigment production process, realizes the comprehensive utilization of waste byproducts, perfects the industrial chain of ferrotitanium and reduces the production cost.
Description
Technical Field
The invention relates to the technical field of titanium dioxide preparation, and in particular relates to a preparation method of conductive titanium dioxide.
Background
The conductive titanium dioxide has the characteristics of no toxicity, no smell, acid resistance, alkali resistance, salt resistance, organic solvent resistance, light resistance, stability below 800 ℃, no oxidation and incombustibility, and flame retardant effect. The conductive titanium dioxide has the advantages of less light absorption, high scattering capability, good optical properties such as luster, whiteness, decolorizing capacity, covering power and the like, and is widely applied to various industrial departments such as petroleum, chemical industry and the like and daily life of people.
At present, the conductive titanium dioxide in the market is mainly prepared by coating antimony doped tin oxide (ATO) on the surface of titanium dioxide, the rare cost of the raw material is high, the coating process is complex, and the high-end conductive titanium dioxide is mainly dependent on foreign import, monopoly and high price.
The lithium iron phosphate has good lattice stability, wide raw material sources, low price, no toxicity, no environmental pollution and relatively high safety performance when being used as a novel lithium ion battery electrode material. Although the conductivity of lithium iron phosphate is poor, the conductivity of lithium iron phosphate can be improved by surface coating, which is mainly improved by increasing the electrical contact between active material particles and between active material and conductive agent. How to combine the conductivity of lithium iron phosphate with the production process of titanium dioxide, so that the byproduct ferrous sulfate in the production of titanium dioxide is used for the production of conductive titanium dioxide, the green recycling of waste byproducts is realized, the industrial chain of ferrotitanium is perfected, and the production cost is reduced, which is a technical problem to be solved in the field.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of conductive titanium dioxide, which comprises the following steps:
step 1), preparing titanium dioxide slurry;
step 2), heating the slurry in the step 1 to 40-60 ℃, and simultaneously adding a metered lithium salt solution, a ferrous sulfate solution and a phosphate-containing solution into the slurry, wherein the phosphate-containing solution adopts phosphoric acid and/or a phosphate solution; wherein the addition amount of lithium salt, ferrous sulfate, phosphoric acid and/or phosphate is respectively 3-15 wt% of the total content of titanium dioxide in the slurry, the addition time is 60-120 min, and the homogenization is carried out for 30min;
step 3), regulating the pH value of the slurry obtained in the step 2 to 8.0-10.0 by using inorganic alkali solution, and homogenizing for 1h;
step 4), carrying out hydrothermal reaction on the slurry obtained in the step 3 at the temperature of 150-400 ℃ for 3-10 h;
step 5), when the temperature of the slurry after the reaction in the step 4 is reduced to below 80 ℃, regulating the pH value of the slurry to 7-10;
step 6), adding zinc salt solution into the slurry obtained in the step 5, wherein the addition amount of the zinc salt accounts for 1-20wt% of the total content of titanium dioxide in the slurry based on zinc oxide, and homogenizing for 1h;
step 7), carrying out suction filtration and water washing on the slurry obtained in the step 6;
step 8), drying and crushing the slurry treated in the step 7, and packaging the product.
Preferably, the base material of the titanium pigment slurry in the step 1 is a chloridizing base material and/or a sulfuric acid base material, the concentration of the slurry is 250-450 g/L, the particle size is 0.25-0.40 mu m after grinding, and the particle size distribution is less than or equal to 1.45.
Preferably, the lithium salt solution in the step 2 adopts one or more of a lithium chloride solution, a lithium nitrate solution, a lithium sulfate solution and a lithium bicarbonate solution with the concentration of 40-200 g/L; the phosphate radical-containing solution adopts one or more of a phosphoric acid solution, a sodium hydrogen phosphate solution and a sodium dihydrogen phosphate solution with the concentration of 40-200 g/L; the concentration of the ferrous sulfate solution is 40-200 g/L.
Preferably, the inorganic alkali solution in the step 3 adopts a lithium hydroxide solution, a sodium hydroxide solution or a potassium hydroxide solution with the concentration of 100-300 g/L.
Preferably, the zinc salt solution in the step 6 adopts zinc sulfate solution or zinc chloride solution with the concentration of 80-200 g/L, and the adding time is 30-60 min.
Preferably, in the spray drying in the step 8, the combination drying and pulverizing is performed by a spray dryer and an air flow pulverizer.
The operation steps and parameters not limited in the present invention can be performed by conventional technical means in the art, and are not described herein.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts a hydrothermal method to prepare uniform and compact lithium iron phosphate in a high-temperature and high-pressure environment, and coats metal oxide (namely zinc oxide) on the surface of the lithium iron phosphate so as to improve the electric contact between active substance particles and between active substances and a conductive agent, thereby ensuring that the titanium dioxide has excellent conductivity.
(2) The ferrous sulfate solution adopted by the invention is a titanium white byproduct of a sulfuric acid method, so that not only is waste byproducts comprehensively utilized, but also the industrial chain of ferrotitanium is perfected, and the green cyclic development is realized.
(3) The invention has the advantages of low-cost and easily-obtained raw materials, short process flow and simple operation.
Detailed Description
The technical solutions of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments.
Examples 1 to 4 illustrate the preparation of the novel conductive titanium pigment of the present invention.
Example 1
Preparing titanium dioxide slurry with the concentration of 400g/L by utilizing a sulfuric acid method titanium dioxide base material, and grinding until the particle size D50 is 0.390 mu m, wherein the particle size distribution is less than 1.45; the temperature of the slurry is raised to 50 ℃, and simultaneously, lithium bicarbonate solution with the concentration of 200g/L, phosphoric acid solution with the concentration of 80g/L and ferrous sulfate solution with the concentration of 200g/L are added, wherein the addition amount of the lithium bicarbonate, the phosphoric acid and the ferrous sulfate is 3wt% of the total content of titanium dioxide in the slurry, the adding time is 60min, and the homogenization is carried out for 30min; adjusting the pH value of the slurry to 8.0 by using sodium hydroxide solution, and carrying out hydrothermal reaction at the temperature of 300 ℃ for 3 hours; cooling to 80 ℃, regulating the pH of the slurry to 9.0, adding zinc sulfate solution with the concentration of 100g/L, wherein the addition amount of zinc sulfate is 8wt% of the total content of titanium dioxide in the slurry, and homogenizing for 1h; sieving, washing, drying and pulverizing to obtain the product.
Example 2
Preparing titanium dioxide slurry with the concentration of 350g/L by utilizing a sulfuric acid method titanium dioxide base material, and grinding until the particle size D50 is 0.380 mu m, wherein the particle size distribution is less than 1.45; the temperature of the slurry is raised to 40 ℃, and simultaneously, a lithium sulfate solution with the concentration of 120g/L, a sodium hydrogen phosphate solution with the concentration of 40g/L and a ferrous sulfate solution with the concentration of 160g/L are added, wherein the addition amounts of the lithium sulfate, the sodium hydrogen phosphate and the ferrous sulfate are all 10 weight percent of the total content of titanium dioxide in the slurry, the adding time is 60min, and the homogenization is carried out for 30min; adjusting the pH value of the slurry to 8.5 by using sodium hydroxide solution, and carrying out hydrothermal reaction at the temperature of 250 ℃ for 8 hours; cooling to 70 ℃, regulating the pH of the slurry to 8.5, adding zinc sulfate solution with the concentration of 100g/L, wherein the addition amount of zinc sulfate is 5wt% of the total content of titanium dioxide in the slurry, and homogenizing for 1h; sieving, washing, drying and pulverizing to obtain the product.
Example 3
Preparing titanium dioxide slurry with the concentration of 300g/L by using a titanium dioxide base material by a chlorination process, and grinding until the particle size D50 is 0.350 mu m, wherein the particle size distribution is less than 1.45; the temperature of the slurry is raised to 60 ℃, and simultaneously, a lithium bicarbonate solution with the concentration of 100g/L, a sodium dihydrogen phosphate solution with the concentration of 40g/L and a ferrous sulfate solution with the concentration of 120g/L are added, wherein the addition amounts of the lithium bicarbonate, the sodium dihydrogen phosphate and the ferrous sulfate are all 12 weight percent of the total content of titanium dioxide in the slurry, the addition time is 60min, and the homogenization is carried out for 30min; adjusting the pH value of the slurry to 9.0 by using sodium hydroxide solution, and carrying out hydrothermal reaction at 400 ℃ for 6 hours; cooling to 80 ℃, regulating the pH of the slurry to 8.5, adding zinc sulfate solution with the concentration of 100g/L, wherein the addition amount of zinc sulfate is 3wt% of the total content of titanium dioxide in the slurry, and homogenizing for 1h; sieving, washing, drying and pulverizing to obtain the product.
Example 4
Preparing titanium dioxide slurry with the concentration of 250g/L by using a titanium dioxide base material by a chlorination process, and grinding until the particle size D50 is 0.360 mu m, wherein the particle size distribution is less than 1.45; the temperature of the slurry is raised to 50 ℃, and simultaneously, a lithium sulfate solution with the concentration of 160g/L, a phosphoric acid solution with the concentration of 60g/L and a ferrous sulfate solution with the concentration of 120g/L are added, wherein the addition amounts of the lithium sulfate, the phosphoric acid and the ferrous sulfate are all 5wt% of the total content of titanium dioxide in the slurry, the adding time is 60min, and the homogenization is carried out for 30min; adjusting the pH value of the slurry to 9.5 by using sodium hydroxide solution, and carrying out hydrothermal reaction at 300 ℃ for 4 hours; cooling to 80 ℃, regulating the pH of the slurry to 8.5, adding zinc sulfate solution with the concentration of 100g/L, wherein the addition amount of zinc sulfate is 10wt% of the total content of titanium dioxide in the slurry, and homogenizing for 1h; sieving, washing, drying and pulverizing to obtain the product.
The products prepared in examples 1 to 4 and purchased foreign conductive titanium dioxide are used as standard samples for performance analysis and test, and the performance test is carried out by adopting a conventional method, and the results are shown in the following table 1:
| test index | Foreign standard sample | Example 1 | Example 2 | Example 3 | Example 4 |
| Volume resistivity/Ω·cm | 34 | 27 | 29 | 26 | 27 |
| Resistivity of paint film/Ω cm | 1.73 | 1.49 | 1.53 | 1.41 | 1.46 |
| Average particle diameter/. Mu.m | 0.423 | 0.392 | 0.377 | 0.352 | 0.369 |
| L | 88.97 | 90.13 | 91.29 | 90.94 | 91.07 |
| b | 2.49 | 2.36 | 2.17 | 2.16 | 2.25 |
| Cover rate/% | 87.3 | 91.6 | 90.9 | 92.1 | 91.2 |
As can be seen from the data, the conductivity, the coverage rate and the color phase of the conductive titanium dioxide prepared by the method are all superior to those of foreign conductive titanium dioxide serving as a standard sample.
The embodiments of the present invention have been described above, the description is illustrative, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (6)
1. The preparation method of the conductive titanium dioxide is characterized by comprising the following steps:
step 1), preparing titanium dioxide slurry;
step 2), heating the slurry in the step 1 to 40-60 ℃, and simultaneously adding a metered lithium salt solution, a ferrous sulfate solution and a phosphate-containing solution into the slurry, wherein the phosphate-containing solution adopts phosphoric acid and/or a phosphate solution; wherein the addition amount of lithium salt, ferrous sulfate, phosphoric acid and/or phosphate is respectively 3-15 wt% of the total content of titanium dioxide in the slurry, the addition time is 60-120 min, and the homogenization is carried out for 30min;
step 3), regulating the pH value of the slurry obtained in the step 2 to 8.0-10.0 by using inorganic alkali solution, and homogenizing for 1h;
step 4), carrying out hydrothermal reaction on the slurry obtained in the step 3 at the temperature of 150-400 ℃ for 3-10 hours;
step 5), when the temperature of the slurry after the reaction in the step 4 is reduced to below 80 ℃, regulating the pH value of the slurry to 7-10;
step 6), adding a zinc salt solution into the slurry obtained in the step 5, wherein the addition amount of the zinc salt accounts for 1-20wt% of the total content of titanium dioxide in the slurry according to zinc oxide, and homogenizing for 1h;
step 7), carrying out suction filtration and water washing on the slurry obtained in the step 6;
step 8), drying and crushing the slurry treated in the step 7, and packaging the product.
2. The method for preparing conductive titanium dioxide according to claim 1, wherein: the base material of the titanium pigment slurry in the step 1 is a chloridizing base material and/or a sulfuric acid base material, the concentration of the slurry is 250-450 g/L, the particle size is 0.25-0.40 mu m after grinding, and the particle size distribution is less than or equal to 1.45.
3. The method for preparing conductive titanium dioxide according to claim 1, wherein: the lithium salt solution in the step 2 adopts one or more of a lithium chloride solution, a lithium nitrate solution, a lithium sulfate solution and a lithium bicarbonate solution with the concentration of 40-200 g/L; the phosphate radical-containing solution adopts one or more of a phosphoric acid solution, a sodium hydrogen phosphate solution and a sodium dihydrogen phosphate solution with the concentration of 40-200 g/L; the concentration of the ferrous sulfate solution is 40-200 g/L.
4. The method for preparing conductive titanium dioxide according to claim 1, wherein: the inorganic alkali solution in the step 3 adopts a lithium hydroxide solution, a sodium hydroxide solution or a potassium hydroxide solution with the concentration of 100-300 g/L.
5. The method for preparing conductive titanium dioxide according to claim 1, wherein: and (3) the zinc salt solution in the step (6) is a zinc sulfate solution or a zinc chloride solution with the concentration of 80-200 g/L, and the adding time is 30-60 min.
6. The method for preparing conductive titanium dioxide according to claim 1, wherein: in the step 8, the spray dryer and the pneumatic pulverizer are used for combined drying and pulverizing.
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Address after: 454000 Fengfeng office, zhongzhan District, Jiaozuo City, Henan Province Applicant after: Longbai Group Co.,Ltd. Address before: 454000 Fengfeng office, zhongzhan District, Jiaozuo City, Henan Province Applicant before: LOMON BILLIONS GROUP Co.,Ltd. |
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