CN112239227A - Preparation method of conductive titanium dioxide - Google Patents
Preparation method of conductive titanium dioxide Download PDFInfo
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- CN112239227A CN112239227A CN202011178005.5A CN202011178005A CN112239227A CN 112239227 A CN112239227 A CN 112239227A CN 202011178005 A CN202011178005 A CN 202011178005A CN 112239227 A CN112239227 A CN 112239227A
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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
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0536—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts
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- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- 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 metered lithium salt solution, ferrous sulfate solution and phosphate radical-containing solution, wherein the phosphate radical-containing solution is phosphoric acid and/or phosphate solution, the addition amount of the lithium salt, the ferrous sulfate, the phosphoric acid and/or the phosphate is 3-15 wt% of the 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 a zinc salt solution into the slurry, wherein the addition amount of the zinc salt is 1-20 wt% of the titanium dioxide, and sieving, washing, drying and crushing the mixture. The invention combines the conductivity of lithium iron phosphate with the production process of titanium dioxide, realizes the comprehensive utilization of waste byproducts, perfects the ferrotitanium industrial chain 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 is characterized by no toxicity, no odor, acid resistance, alkali resistance, salt resistance, organic solvent resistance, light resistance, stability below 800 ℃, no oxidation, no combustion and flame retardant effect. The conductive titanium dioxide has the advantages of less light absorption, large scattering capacity, good optical properties such as luster, whiteness, achromatism, 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 raw material is rare, the manufacturing cost is high, the coating process is complex, and the high-end conductive titanium dioxide mainly depends on foreign import, technical monopoly and high price.
The lithium iron phosphate has good lattice stability, is used as a novel lithium ion battery electrode material, has wide raw material source, low price, no toxicity, no environmental pollution and relatively high safety performance. Although lithium iron phosphate has poor conductivity, the conductivity of lithium iron phosphate can be improved by surface coating, which is mainly improved by improving electrical contact between active material particles and between the active material and the conductive agent. How to combine the conductivity of lithium iron phosphate with the titanium dioxide production process, so that the by-product ferrous sulfate in the titanium dioxide production is used for the production of the conductive titanium dioxide, the green cyclic utilization of the waste by-product is realized, the ferrotitanium industrial chain is perfected, and the production cost is reduced, which is a technical problem to be solved urgently in the field.
Disclosure of Invention
In order to solve the technical problem, 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 obtained in the step 1 to 40-60 ℃, and simultaneously adding metered lithium salt solution, ferrous sulfate solution and phosphate radical-containing solution into the slurry, wherein the phosphate radical-containing solution is phosphoric acid and/or phosphate solution; wherein the adding amount of the lithium salt, the ferrous sulfate, the phosphoric acid and/or the phosphate is 3-15 wt% of the total content of the titanium dioxide in the slurry, the adding time is 60-120 min, and the homogenization is performed for 30 min;
step 3), adjusting the pH value of the slurry obtained in the step 2 to 8.0 to 10.0 by using an inorganic alkali solution, and homogenizing for 1 hour;
step 4), carrying out hydrothermal reaction on the slurry obtained in the step 3 at the temperature of 150-400 ℃, wherein the reaction time is 3-10 h;
step 5), when the temperature of the slurry after the reaction in the step 4 is reduced to be below 80 ℃, adjusting the pH of the slurry to be 7-10;
step 6), adding a zinc salt solution into the slurry obtained in the step 5, wherein the adding amount of the zinc salt accounts for 1-20 wt% of the total content of titanium dioxide in the slurry in terms of zinc oxide, and homogenizing for 1 h;
step 7), carrying out suction filtration and washing on the slurry obtained in the step 6;
and 8) drying, crushing and packaging the slurry treated in the step 7.
Preferably, the base material of the titanium dioxide slurry in the step 1 is a chlorination-process base material and/or a sulfuric-acid-process base material, the concentration of the slurry is 250-450 g/L, the particle size is 0.25-0.40 μm after grinding, and the particle size distribution is less than or equal to 1.45.
Preferably, the lithium salt solution in the step 2 is 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 is one or more of a phosphoric acid solution with the concentration of 40-200 g/L, a sodium hydrogen phosphate solution and a sodium dihydrogen phosphate solution; the concentration of the ferrous sulfate solution is 40-200 g/L.
Preferably, the inorganic alkali solution in the step 3 is a lithium hydroxide solution, a sodium hydroxide solution or a potassium hydroxide solution with a concentration of 100-300 g/L.
Preferably, 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.
Preferably, when the spray drying is performed in step 8, the spray drying and the air jet mill are used for combined drying and pulverization.
The operation steps and parameters that are 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 a metal oxide (namely zinc oxide) on the surface of the lithium iron phosphate so as to improve the electric contact among active substance particles and between the active substance 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 dioxide byproduct of a sulfuric acid process, so that the waste byproduct is comprehensively utilized, the improvement of a ferrotitanium industrial chain is facilitated, and the green cycle development is realized.
(3) The invention has the advantages of cheap and easily obtained raw materials, short process flow and simple operation.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Examples 1 to 4 are provided to illustrate the preparation method of the novel conductive titanium dioxide of the present invention.
Example 1
Preparing titanium dioxide slurry with the concentration of 400g/L by using a sulfuric acid method titanium dioxide base material, and grinding until the particle size D50 is 0.390 mu m and the particle size distribution is less than 1.45; raising the temperature of the slurry to 50 ℃, simultaneously adding a lithium bicarbonate solution with the concentration of 200g/L, a phosphoric acid solution with the concentration of 80g/L and a ferrous sulfate solution with the concentration of 200g/L, wherein the adding amount of lithium bicarbonate, phosphoric acid and ferrous sulfate is 3 wt% of the total content of titanium dioxide in the slurry, adding for 60min, and homogenizing for 30 min; adjusting the pH value of the slurry to 8.0 by using a sodium hydroxide solution, and carrying out hydrothermal reaction at the temperature of 300 ℃ for 3 h; cooling to 80 ℃, adjusting the pH value of the slurry to 9.0, adding a zinc sulfate solution with the concentration of 100g/L, wherein the addition amount of the zinc sulfate is 8 wt% of the total content of the titanium dioxide in the slurry, and homogenizing for 1 h; sieving, washing with water, drying, and pulverizing to obtain the final product.
Example 2
Preparing titanium dioxide slurry with the concentration of 350g/L by using a sulfuric acid method titanium dioxide base material, and grinding until the particle size D50 is 0.380 mu m and the particle size distribution is less than 1.45; heating the slurry to 40 ℃, simultaneously adding 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, wherein the adding amount of lithium sulfate, sodium hydrogen phosphate and ferrous sulfate is 10 wt% of the total content of titanium dioxide in the slurry, adding for 60min, and homogenizing for 30 min; adjusting the pH value of the slurry to 8.5 by using a sodium hydroxide solution, and carrying out hydrothermal reaction at the temperature of 250 ℃ for 8 h; cooling to 70 ℃, adjusting the pH value of the slurry to 8.5, adding a zinc sulfate solution with the concentration of 100g/L, wherein the addition amount of the zinc sulfate is 5 wt% of the total content of the titanium dioxide in the slurry, and homogenizing for 1 h; sieving, washing with water, drying, and pulverizing to obtain the final product.
Example 3
Preparing titanium dioxide slurry with the concentration of 300g/L by using a chlorination-process titanium dioxide base material, and grinding until the particle size D50 is 0.350 mu m and the particle size distribution is less than 1.45; heating the slurry to 60 ℃, simultaneously adding 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, wherein the adding amounts of the lithium bicarbonate, the sodium dihydrogen phosphate and the ferrous sulfate are 12 wt% of the total content of the titanium dioxide in the slurry, adding for 60min, and homogenizing for 30 min; adjusting the pH value of the slurry to 9.0 by using a sodium hydroxide solution, and carrying out hydrothermal reaction at the temperature of 400 ℃ for 6 hours; cooling to 80 ℃, adjusting the pH value of the slurry to 8.5, adding a zinc sulfate solution with the concentration of 100g/L, wherein the addition amount of the zinc sulfate is 3 wt% of the total content of the titanium dioxide in the slurry, and homogenizing for 1 h; sieving, washing with water, drying, and pulverizing to obtain the final product.
Example 4
Preparing titanium dioxide slurry with the concentration of 250g/L by using a chlorination-process titanium dioxide base material, and grinding until the particle size D50 is 0.360 mu m and the particle size distribution is less than 1.45; heating the slurry to 50 ℃, simultaneously adding 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, wherein the adding amount of lithium sulfate, phosphoric acid and ferrous sulfate is 5 wt% of the total content of titanium dioxide in the slurry, adding for 60min, and homogenizing for 30 min; adjusting the pH value of the slurry to 9.5 by using a sodium hydroxide solution, and carrying out hydrothermal reaction at the temperature of 300 ℃ for 4 h; cooling to 80 ℃, adjusting the pH value of the slurry to 8.5, adding a zinc sulfate solution with the concentration of 100g/L, wherein the addition amount of the zinc sulfate is 10 wt% of the total content of titanium dioxide in the slurry, and homogenizing for 1 h; sieving, washing with water, drying, and pulverizing to obtain the final product.
The products prepared in examples 1 to 4 and purchased foreign conductive titanium dioxide are used as standard samples to perform performance analysis tests, the performance tests are performed 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 |
| Film resistivity/omega 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 |
| Coverage rate/%) | 87.3 | 91.6 | 90.9 | 92.1 | 91.2 |
The data show that the conductivity, the coverage rate and the hue of the conductive titanium dioxide prepared by the method are superior to those of foreign conductive titanium dioxide serving as a standard sample.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, 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 illustrated 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 obtained in the step 1 to 40-60 ℃, and simultaneously adding metered lithium salt solution, ferrous sulfate solution and phosphate radical-containing solution into the slurry, wherein the phosphate radical-containing solution is phosphoric acid and/or phosphate solution; wherein the addition amounts of the lithium salt, the ferrous sulfate, the phosphoric acid and/or the phosphate are respectively 3-15 wt% of the total content of the titanium dioxide in the slurry, the addition time is 60-120 min, and the homogenization is performed for 30 min;
step 3), adjusting the pH value of the slurry obtained in the step 2 to 8.0 to 10.0 by using an inorganic alkali solution, and homogenizing for 1 hour;
step 4), carrying out hydrothermal reaction on the slurry obtained in the step 3 at the temperature of 150-400 ℃, wherein the reaction time is 3-10 h;
step 5), when the temperature of the slurry after the reaction in the step 4 is reduced to be below 80 ℃, adjusting the pH of the slurry to be 7-10;
step 6), adding a zinc salt solution into the slurry obtained in the step 5, wherein the adding amount of the zinc salt accounts for 1-20 wt% of the total content of titanium dioxide in the slurry in terms of zinc oxide, and homogenizing for 1 h;
step 7), carrying out suction filtration and washing on the slurry obtained in the step 6;
and 8) drying, crushing and packaging the slurry treated in the step 7.
2. The preparation method of the conductive titanium dioxide according to claim 1, characterized in that: the base material of the titanium dioxide slurry in the step 1 is a chlorination process base material and/or a sulfuric acid process 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 preparation method of the conductive titanium dioxide according to claim 1, characterized in that: the lithium salt solution in the step 2 is 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 is one or more of a phosphoric acid solution with the concentration of 40-200 g/L, a sodium hydrogen phosphate solution and a sodium dihydrogen phosphate solution; the concentration of the ferrous sulfate solution is 40-200 g/L.
4. The preparation method of the conductive titanium dioxide according to claim 1, characterized in that: the inorganic alkali solution in the step 3 is a lithium hydroxide solution, a sodium hydroxide solution or a potassium hydroxide solution with the concentration of 100-300 g/L.
5. The preparation method of the conductive titanium dioxide according to claim 1, characterized in that: and (3) adopting a zinc sulfate solution or a zinc chloride solution with the concentration of 80-200 g/L for the zinc salt solution in the step 6, and adding for 30-60 min.
6. The preparation method of the conductive titanium dioxide according to claim 1, characterized in that: and 8, when the spray drying is carried out in the step 8, carrying out combined drying and crushing by using a spray dryer and an airflow crusher.
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