CN113353977A - Method for preparing titanium dioxide by using ilmenite - Google Patents
Method for preparing titanium dioxide by using ilmenite Download PDFInfo
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- CN113353977A CN113353977A CN202110772828.9A CN202110772828A CN113353977A CN 113353977 A CN113353977 A CN 113353977A CN 202110772828 A CN202110772828 A CN 202110772828A CN 113353977 A CN113353977 A CN 113353977A
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- ilmenite
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 89
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 42
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 44
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 42
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- 239000011343 solid material Substances 0.000 claims abstract description 24
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 17
- 239000003513 alkali Substances 0.000 claims abstract description 16
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 230000008569 process Effects 0.000 claims abstract description 11
- 229910010270 TiOCl2 Inorganic materials 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 238000001354 calcination Methods 0.000 claims description 19
- 230000035484 reaction time Effects 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000005272 metallurgy Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 18
- 239000000047 product Substances 0.000 description 16
- 239000012065 filter cake Substances 0.000 description 12
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 230000001276 controlling effect Effects 0.000 description 8
- 238000010992 reflux Methods 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 229910052719 titanium Inorganic materials 0.000 description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 6
- 230000007935 neutral effect Effects 0.000 description 6
- 238000004064 recycling Methods 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000007062 hydrolysis Effects 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000377 silicon dioxide Substances 0.000 description 3
- 235000012239 silicon dioxide Nutrition 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- JUWGUJSXVOBPHP-UHFFFAOYSA-B titanium(4+);tetraphosphate Chemical compound [Ti+4].[Ti+4].[Ti+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O JUWGUJSXVOBPHP-UHFFFAOYSA-B 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910005451 FeTiO3 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- -1 firstly Chemical compound 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 150000002506 iron compounds Chemical class 0.000 description 1
- 229910052592 oxide mineral Inorganic materials 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- 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
- C01G23/0538—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing chloride-containing salts in the presence of seeds
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for preparing titanium dioxide by utilizing ilmenite, and relates to the technical field of metallurgy. The method for preparing titanium dioxide by using ilmenite comprises the following steps: mixing ilmenite with alkali liquor for reaction, performing solid-liquid separation to obtain a first solid material, and mixing the first solid material with a hydrochloric acid solution for reaction to form TiOCl2The solution is mixed with phosphoric acid and then undergoes hydrolysis reaction. The method provided by the invention has the characteristics of easily obtained raw materials and simple process route, can obtain titanium dioxide with better purity, and provides a new path for preparing titanium dioxide.
Description
Technical Field
The invention relates to the technical field of metallurgy, in particular to a method for preparing titanium dioxide by utilizing ilmenite.
Background
Titanium dioxide (TiO)2) Is a white pigment with excellent performance, and is widely applied to the industries of coating, plastics, papermaking and the like. Ilmenite, also known as titanomagnetite, is an oxide mineral of iron and titanium and is the main ore for extracting titanium, and the main component of ilmenite is FeTiO3The impurities include silicon, aluminum, etc. The ilmenite can be used for preparing titanium dioxide, so that the economic value of the titanium dioxide can be improved, and the requirement of the industry on a titanium raw material can be met.
At present, the method for producing titanium dioxide mainly comprises a sulfuric acid method and a chlorination method, wherein the chlorination method has high requirements on raw materials, the sulfuric acid method has a long process route, and both the two methods have certain problems.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a method for preparing titanium dioxide by using ilmenite, which aims to prepare titanium dioxide by using a simpler method and is easy for industrial production.
The invention is realized by the following steps:
the embodiment of the invention provides a method for preparing titanium dioxide by using ilmenite, which comprises the following steps:
mixing ilmenite with alkali liquor for reaction, performing solid-liquid separation to obtain a first solid material, and mixing the first solid material with a hydrochloric acid solution for reaction to form TiOCl2The solution is mixed with phosphoric acid and then undergoes hydrolysis reaction.
The invention has the following beneficial effects: the inventor optimizes the process route for preparing titanium dioxide by using ilmenite, firstly uses the mixing reaction of ilmenite and alkali liquor to dissolve impurities such as silicon dioxide, aluminum oxide and the like in ilmenite, obtains a first solid material mainly containing titanium and iron compounds after solid-liquid separation, and then uses the first solid material to be mixed with hydrochloric acid to form TiOCl2The solution, after mixing with phosphoric acid, is hydrolyzed to form titanium phosphate nuclei, on the basis of which titanium dioxide continues to form. The method provided by the invention has the characteristics of easily obtained raw materials and simple process route, can obtain titanium dioxide with better purity, and provides a new path for preparing titanium dioxide.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a scanning electron micrograph of a product prepared in example 1 of the present application;
FIG. 2 is a scanning electron micrograph of a product prepared in comparative example 1 of the present application;
FIG. 3 is a scanning electron micrograph of a product prepared in comparative example 2 of the present application;
FIG. 4 is a scanning electron micrograph of a product prepared in comparative example 3 of the present application;
FIG. 5 is a scanning electron micrograph of a product prepared in comparative example 4 of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The inventor optimizes the process route for preparing the titanium dioxide by utilizing the ilmenite, so that the titanium dioxide is prepared by a simpler process route, and the raw materials are easy to obtain, thereby being suitable for industrial application.
The embodiment of the invention provides a method for preparing titanium dioxide by using ilmenite, which comprises the following steps:
s1, separating impurities
After reacting ilmenite with alkali liquor, carrying out solid-liquid separation to obtain a first solid material so as to separate and obtain a solid material mainly containing titanium and iron, wherein impurities such as silicon dioxide, aluminum oxide and the like can be dissolved in the alkali liquor.
In the actual operation process, ilmenite and alkali liquor are mixed and reacted, after the reaction is finished, filtration and solid-liquid separation are carried out, liquid can be recycled, and the obtained filter cake is the first solid material. In some embodiments, the first solid material may be washed to neutrality to remove surface alkali solution, and then mixed with hydrochloric acid solution.
In some embodiments, the reaction temperature of the ilmenite and the alkali liquor is 70-80 ℃, the reaction time is 6-8h, and impurities are better dissolved in the alkali liquor and removed by regulating the reaction temperature and the reaction time. Specifically, the reaction temperature is 70 ℃, 75 ℃, 80 ℃ or the like, and may be any value between the above adjacent temperature values. The reaction time is 6h, 6.5h, 7h, 7.5h, 8h, etc., and may be any value between the above adjacent time values.
Further, the alkali solution is selected from at least one of a sodium hydroxide solution and a potassium hydroxide solution. The mass fraction of the alkali liquor is 10-30% (such as 10%, 15%, 20%, 25%, 30%, etc.), and the mass ratio of the alkali liquor to the ilmenite is 4-6:1 (such as 4:1, 5:1, 6: 1). The impurities are fully removed by controlling the dosage of the alkali liquor.
In some embodiments, the ilmenite may be ilmenite powder, to facilitate reaction completion.
S2, hydrolysis and cleavage
Mixing the first solid material with hydrochloric acid solution to react to form TiOCl2Then mixing with phosphoric acid and carrying out hydrolysis reaction, during which the TiOCl is added2The reaction is titanium dioxide. Phosphoric acid is utilized to carry out hydrolysis reaction to form titanium phosphate as crystal nucleus (iron is not hydrolyzed), titanium dioxide formed by hydrolysis grows on the crystal nucleus, and free phosphate ions play a role in controlling particle size and morphology.
In some embodiments, the mass ratio of hydrochloric acid in the hydrochloric acid solution to the first solid material is 1.8 to 3:1 (e.g., 1.8:1, 2:1, 2.5:1, 3:1, etc.), preferably 2 to 2.5: 1. Specifically, the mass fraction of the hydrochloric acid solution is 25-35% (e.g., 25%, 30%, 35%, etc.), and the mass ratio of the total amount of the hydrochloric acid solution to the first solid material is 6-10:1 (e.g., 6:1, 7:1, 8:1, 9:1, 10:1, etc.). The dosage of hydrochloric acid is controlled to fully convert titanium into TiOCl2And the utilization rate of raw materials is improved.
Further, the reaction temperature of the hydrolysis reaction is 100-110 ℃, the reaction time is 6-8h, the reaction rate is controlled by controlling the hydrolysis temperature, and if the temperature is too high, the reaction rate is too fast, which is not favorable for obtaining the titanium dioxide product with the purity and the particle size meeting the requirements; if the temperature is too low, the reaction does not proceed easily. Specifically, the hydrolysis reaction temperature may be 100 ℃, 105 ℃, 110 ℃ or the like, or may be any value between the above adjacent temperature values; the reaction time is 6h, 6.5h, 7h, 7.5h, 8h, etc., and may be any value between the above adjacent time values.
In a preferred embodiment, the reaction temperature of the hydrolysis reaction is 105-108 ℃, and the reaction time is 6.5-7.5h, so as to improve the purity and yield of the product.
Further, the mass ratio of the added phosphoric acid to the ilmenite is 0.05-1: 100; preferably 0.5-0.01: 100. The addition amount of phosphoric acid has a certain influence on the purity and influence of the product, and is preferably controlled within the above range.
S3, post-processing
And after the hydrolysis reaction, carrying out solid-liquid separation to obtain a second solid material, and then washing, drying and calcining the second solid material to obtain a titanium dioxide product. Unreacted acid liquor is removed through water washing, and calcination is carried out after drying to remove moisture and improve crystallinity.
Furthermore, in the calcining process, the calcining temperature is controlled to be 750-850 ℃, and the calcining time is 4-6 min. Specifically, the calcination temperature may be 750 ℃, 800 ℃, 850 ℃ and the like, and the calcination time may be 4min, 5min, 6min and the like.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The embodiment provides a method for preparing titanium dioxide by using ilmenite, which comprises the following steps:
(1) putting ilmenite powder and 20% sodium hydroxide solution in a mass ratio of 1:5 into a reaction kettle, and reacting for 7 hours at the reflux temperature of 75 ℃. After the reaction is finished, filtering to carry out solid-liquid separation, recycling the liquid, and continuously washing the filter cake to be neutral by using water for later use.
(2) Adding the filter cake and 30% hydrochloric acid into a reaction kettle according to the mass ratio of 1:8, continuously adding phosphoric acid accounting for 0.05% of the mass of the ilmenite powder (namely the mass ratio of the added phosphoric acid to the ilmenite is 0.05:100), uniformly stirring, and reacting for 7 hours at the reflux temperature of 105 ℃.
(3) And after the reaction is finished, filtering to perform solid-liquid separation, recycling the filtrate, washing the filter cake to be neutral, drying, and calcining (controlling the calcining temperature to be 800 ℃ and the calcining time to be 5min) to obtain the titanium dioxide product.
Example 2
The embodiment provides a method for preparing titanium dioxide by using ilmenite, which comprises the following steps:
(1) putting ilmenite powder and 10% sodium hydroxide solution into a reaction kettle according to the mass ratio of 1:6, and reacting for 8 hours at the reflux temperature of 70 ℃. After the reaction is finished, filtering to carry out solid-liquid separation, recycling the liquid, and continuously washing the filter cake to be neutral by using water for later use.
(2) Putting the filter cake and 30% hydrochloric acid into a reaction kettle according to the mass ratio of 1:6 (namely the mass ratio of the filter cake to the pure hydrochloric acid is 1:1.8), continuously adding phosphoric acid accounting for 0.01% of the mass of the ilmenite powder (namely the mass ratio of the adding amount of the phosphoric acid to the ilmenite is 0.01:100), uniformly stirring, and reacting for 8 hours at the reflux temperature of 100 ℃.
(3) And after the reaction is finished, filtering to perform solid-liquid separation, recycling the filtrate, washing the filter cake to be neutral, drying, and calcining (controlling the calcining temperature to be 750 ℃ and the calcining time to be 6min) to obtain the titanium dioxide product.
Example 3
The embodiment provides a method for preparing titanium dioxide by using ilmenite, which comprises the following steps:
(1) putting ilmenite powder and 30% sodium hydroxide solution in a mass ratio of 1:4 into a reaction kettle, and reacting for 6 hours at the reflux temperature of 80 ℃. After the reaction is finished, filtering to carry out solid-liquid separation, recycling the liquid, and continuously washing the filter cake to be neutral by using water for later use.
(2) Putting the filter cake and 30% hydrochloric acid into a reaction kettle according to the mass ratio of 1:10 (namely the mass ratio of the filter cake to the pure hydrochloric acid is 1:3), continuously adding phosphoric acid accounting for 0.05% of the mass of the ilmenite powder (namely the mass ratio of the adding amount of the phosphoric acid to the ilmenite is 0.05:100), uniformly stirring, and reacting for 6 hours at the reflux temperature of 110 ℃.
(3) And after the reaction is finished, filtering to perform solid-liquid separation, recycling the filtrate, washing the filter cake to be neutral, drying, and calcining (controlling the calcining temperature to be 850 ℃ and the calcining time to be 4min) to obtain the titanium dioxide product.
Comparative example 1
This comparative example provides a process for preparing titanium dioxide using ilmenite, differing from example 1 only in that: the reflux temperature after the addition of phosphoric acid in step (2) was controlled to 120 ℃.
Comparative example 2
This comparative example provides a process for preparing titanium dioxide using ilmenite, differing from example 1 only in that: the reflux temperature after the addition of phosphoric acid in step (2) was controlled to 90 ℃.
Comparative example 3
This comparative example provides a process for preparing titanium dioxide using ilmenite, differing from example 1 only in that: controlling the amount of the phosphoric acid added in the step (2) to be different, wherein the mass ratio of the amount of the phosphoric acid to the ilmenite is 0.005: 100.
Comparative example 4
This comparative example provides a process for preparing titanium dioxide using ilmenite, differing from example 1 only in that: controlling the amount of the phosphoric acid added in the step (2) to be different, wherein the mass ratio of the amount of the phosphoric acid to the ilmenite is 5: 100.
Test example 1
The purity and yield of the product obtained in the test example and the comparative example were determined. The results are shown in Table 1.
TABLE 1 purity and yield test results for titanium dioxide products
| Group of | Purity (%) | Yield (%) |
| Example 1 | 99.1％ | 99.8％ |
| Example 2 | 99.3％ | 99.7％ |
| Example 3 | 99.2％ | 99.5％ |
| Comparative example 1 | 99.1％ | 99.8％ |
| Comparative example 2 | 98.5％ | 99.0％ |
| Comparative example 3 | 98.5％ | 99.8％ |
| Comparative example 4 | 95.0％ | 99.8％ |
Test example 2
The morphology of the titanium dioxide products obtained in the test examples and comparative examples are shown in FIGS. 1-5.
As can be seen from the figure: the embodiment can prepare titanium dioxide with uniform particle size and morphology, and the titanium dioxide obtained at the hydrolysis temperature is too high or too low, has non-uniform size and serious agglomeration.
In summary, the embodiments of the present invention provide a method for preparing titanium dioxide by using ilmenite, wherein the inventor optimizes the process route for preparing titanium dioxide by using ilmenite, firstly, ilmenite is mixed with alkali solution for reaction, impurities such as silicon dioxide and aluminum oxide in ilmenite are dissolved, and a first solid material obtained after solid-liquid separation mainly contains titanium and iron,then the first solid material is mixed with hydrochloric acid to form TiOCl2Mixed with phosphoric acid and then hydrolyzed to form titanium phosphate nuclei, TiOCl in the hydrolysis reaction2Titanium dioxide is formed on the basis of the crystal nuclei. The method provided by the invention has the characteristics of easily obtained raw materials and simple process route, can obtain titanium dioxide with better purity, and provides a new path for preparing titanium dioxide.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A method for preparing titanium dioxide by using ilmenite is characterized by comprising the following steps:
mixing ilmenite and alkali liquor for reaction, then carrying out solid-liquid separation to obtain a first solid material, and mixing the first solid material with a hydrochloric acid solution for reaction to form TiOCl2Then mixing with phosphoric acid and carrying out hydrolysis reaction.
2. The method as claimed in claim 1, wherein the reaction temperature of the hydrolysis reaction is 100-110 ℃, and the reaction time is 6-8 h;
preferably, the reaction temperature of the hydrolysis reaction is 105-108 ℃, and the reaction time is 6.5-7.5 h.
3. The method according to claim 2, characterized in that the mass ratio of the added phosphoric acid to the ilmenite is 0.05-1: 100; preferably 0.05-0.1: 100.
4. The method according to claim 1, wherein the mass ratio of the hydrochloric acid solution to the first solid material is 1.8-3:1, preferably 2-2.5: 1.
5. The method according to claim 4, wherein the mass fraction of the hydrochloric acid solution is 25-35%, and the mass ratio of the total amount of the hydrochloric acid solution to the first solid material is 6-10: 1.
6. The method of claim 4, wherein the first solid material is washed with water to neutrality and then mixed with the hydrochloric acid solution.
7. The method according to claim 1, characterized in that the reaction temperature of the ilmenite and the lye is 70-80 ℃, the reaction time is 6-8 h;
preferably, the alkali solution is selected from at least one of a sodium hydroxide solution and a potassium hydroxide solution.
8. The method according to claim 7, characterized in that the mass fraction of the lye is 10-30%, the mass ratio of the lye to the ilmenite is 4-6: 1;
preferably, the ilmenite is ilmenite powder.
9. The method of claim 1, further comprising performing solid-liquid separation after the hydrolysis reaction to obtain a second solid material, and washing, drying and calcining the second solid material.
10. The method as claimed in claim 9, wherein the calcination process is performed at a calcination temperature of 750-850 ℃ for 4-6 min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114132960A (en) * | 2021-12-21 | 2022-03-04 | 湖北亚星电子材料有限公司 | Preparation method for purifying titanium dioxide by composite solid phase column |
| CN116062788A (en) * | 2023-01-17 | 2023-05-05 | 中国科学院赣江创新研究院 | Method for regulating granularity and morphology of metatitanic acid |
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