CN115367793A - Method for preparing titanium dioxide from titanyl dichloride solution - Google Patents
Method for preparing titanium dioxide from titanyl dichloride solution Download PDFInfo
- Publication number
- CN115367793A CN115367793A CN202211108703.7A CN202211108703A CN115367793A CN 115367793 A CN115367793 A CN 115367793A CN 202211108703 A CN202211108703 A CN 202211108703A CN 115367793 A CN115367793 A CN 115367793A
- Authority
- CN
- China
- Prior art keywords
- solution
- titanium dioxide
- titanyl
- preheated
- seed
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
Abstract
The invention discloses a method for preparing titanium dioxide by using a titanium oxychloride solution, which comprises the following steps: the method comprises the following steps: preheating 8-12% alkali liquor to 83-85 ℃, preheating 190-200 g/L titanyl sulfate solution to 83-85 ℃, adding the preheated titanyl sulfate solution into the preheated alkali liquor, uniformly stirring, heating the mixed solution to 95-98 ℃, preserving heat to obtain a seed crystal solution, and detecting the stability of the seed crystal solution; step two: adding the crystal seed solution with qualified stability into a titanium oxychloride solution preheated to 88-92 ℃, heating to 95-98 ℃, preserving heat for 90-120 min, and obtaining a titanium dioxide precursor through solid-liquid separation; step three: and (4) calcining the titanium dioxide precursor obtained in the step two under the condition of adding a salt treating agent to obtain the titanium dioxide. The method uses titanyl sulfate to prepare seed crystal to induce titanyl dichloride to perform precipitation reaction, so that the hydrolysate has uniform particle size distribution and high hydrolysis speed, and the obtained product has better quality.
Description
Technical Field
The invention belongs to the technical field of titanium dioxide preparation, and particularly relates to a method for preparing titanium dioxide from a titanium oxychloride solution.
Background
The hydrochloric acid method for preparing titanium white isScientists innovate and develop a method which has relatively low reaction temperature, full recycling of hydrochloric acid and chlorine elements and only produces titanium pigment and ferric trichloride. The hydrochloric acid method for preparing titanium white is explored for decades, and a laboratory kilogram-level and scale-up test is completed, but industrialization is not realized all the time. There are three main reasons that restrict its development: the first aspect is that the hydrochloric acid and chlorine elements are not recycled completely; the second aspect is that the extractant has high cost and contains harmful components to human body; the third aspect is that the quality of the prepared product can not be compared with that of the titanium white prepared by a chlorination method or the titanium white prepared by a sulfuric acid method. The global hydrochloric acid method titanium white preparation process can be divided into 3 types, which are respectively a method (ANI method) of Altair nanometer material company in the United states, a method (CTL method) of titanium Limited Canada and a method (ZLC method) of Zhangluo. The three processes are different in extraction, and have great difference in preparing hydrated titanium dioxide by adopting the titanium oxychloride solution after impurity removal. The American ANI method adopts spray high-temperature hydrolysis, namely, the titanyl dichloride solution after impurity removal is conveyed to an atomizing device, atomized into liquid drops under the action of compressed air and then enters a drying zone, the titanyl dichloride solution is contacted with hot air, and free hydrochloric acid contained in the seed crystal solution is rapidly volatilized, so that the acidity of the seed crystal solution is reduced. At lower acidity, the TiOCl contained in the seed solution 2 And H 2 O undergoes hydrolysis reaction to generate amorphous TiO 2 And collected by a product collection device at the bottom of the drying zone, but spray hydrolysis optimization was not achieved. The Canadian CTL process precipitates hydrous titanium dioxide by heating a solution of titanyl dichloride in a stirred tank reactor with steam heating to convert the titanyl dichloride to hydrous titanium dioxide as the temperature of the solution increases to 90-100 ℃. The Chinese ZLC method adopts a high-temperature precipitation mode for hydrolysis. Compared with spray hydrolysis, the precipitation hydrolysis has low requirements on equipment and is convenient for scale-up.
In view of this, the prior art is in need of improvement.
Disclosure of Invention
In view of the problems of the prior art, the invention provides a method for preparing titanium dioxide by using a titanyl dichloride solution which has low equipment requirement, is convenient for scale-up and has excellent quality of the generated product.
In order to achieve the purpose, the invention adopts the following technical scheme:
according to the present invention, there is provided a process for preparing titanium dioxide from a solution of titanyl dichloride, the process comprising the steps of: the method comprises the following steps: preheating 8-12 wt% alkali liquor to 83-85 deg.c, preheating 190-200 g/L titanyl sulfate solution to 83-85 deg.c, adding the preheated titanyl sulfate solution into the preheated alkali liquor, stirring, heating the mixed liquid to 95-98 deg.c, maintaining the temperature to obtain crystal seed solution and detecting the stability of the crystal seed solution; step two: adding the crystal seed solution with qualified stability into a titanium oxychloride solution preheated to 88-92 ℃, wherein the titanium oxychloride solution has the metering concentration of 50-60 g/L by titanium dioxide, heating to 95-98 ℃, preserving heat for 90-120 min, and obtaining a titanium dioxide precursor through solid-liquid separation; step three: and (4) calcining the titanium dioxide precursor obtained in the step two under the condition of adding a salt treating agent to obtain the titanium dioxide.
According to one embodiment of the invention, in the first step, the titanyl sulfate solution is an aqueous solution of a mixture of titanyl sulfate and titanium sulfate produced by reacting sulfuric acid with a titanium raw material in the production of titanium white by a sulfate process.
According to one embodiment of the present invention, in the first step, if 10ml of the seed solution is diluted with distilled water at 25 ℃ until just before cloudiness occurs, the volume of water required is 120ml to 130ml, and the seed solution is considered to be stable.
According to an embodiment of the invention, in the first step, the alkali solution is selected from a sodium hydroxide solution, a potassium hydroxide solution or ammonia water.
According to one embodiment of the invention, in step one, the ratio of the alkali solution to the titanyl sulfate solution is alkali/TiO 2 The alkali/TiO is calculated by mass ratio 2 ＝0.14～0.27。
According to an embodiment of the present invention, in the second step, the crystal seed solution with qualified stability and the titanium oxychloride are both measured by titanium dioxide, and the TiO in the crystal seed solution 2 With TiO in solution of titanium oxychloride 2 The mass ratio is 2-5%.
According to one embodiment of the invention, in the first step, the preheated titanyl sulfate solution is added into the preheated alkali liquor within 2min, and after the titanyl sulfate solution and the alkali liquor are uniformly stirred, the mixed liquor is heated to 95-98 ℃ within 2-3 min.
According to one embodiment of the invention, in the second step, the seed crystal solution with qualified stability is added into the titanium oxychloride solution preheated to 88-92 ℃ within 2-3 min.
According to an embodiment of the present invention, in step three, the salt treatment agent is an aluminum-based formulation composed of potassium hydroxide, phosphoric acid and aluminum sulfate or a zinc-based formulation composed of potassium hydroxide, phosphoric acid and zinc sulfate.
According to one embodiment of the invention, in the third step, the maximum calcination temperature is 920-990 ℃ and the calcination time is 7-12 h when the aluminum salt treating agent formula is used, and the maximum calcination temperature is 820-890 ℃ and the calcination time is 7-12 h when the zinc salt treating agent formula is used.
By adopting the technical scheme, the invention has the following beneficial effects:
the invention creatively provides a method for preparing titanium dioxide by using a titanyl dichloride solution, which induces the titanyl dichloride to generate a precipitation reaction by using a seed crystal prepared by using titanyl sulfate, so that the particle size distribution of a hydrolysate is uniform, the hydrolysis speed is high, and the quality of the obtained hydrated titanium dioxide is good. The method provided by the invention has low requirements on equipment and is convenient for scale up.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to specific embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
As required, detailed embodiments of the present invention are disclosed in the present specification; however, it is to be understood that the disclosed embodiments are merely exemplary of the invention that may be embodied in various and alternative forms. In the following description, various operating parameters and components are described in various embodiments as contemplated. These specific parameters and components are used in this specification as examples only and are not meant to be limiting.
The invention provides a method for preparing titanium dioxide by using a titanium oxychloride solution, which comprises the following steps: the method comprises the following steps: preheating 8-12% alkali liquor to 83-85 ℃, preheating 190-200 g/L titanyl sulfate solution to 83-85 ℃, adding the preheated titanyl sulfate solution into the preheated alkali liquor, uniformly stirring, heating the mixed solution to 95-98 ℃, preserving heat to obtain a seed crystal solution, and detecting the stability of the seed crystal solution; step two: adding the crystal seed solution with qualified stability into a titanium oxychloride solution preheated to 88-92 ℃, wherein the titanium oxychloride solution has the metering concentration of 50-60 g/L by titanium dioxide, heating to 95-98 ℃, preserving heat for 90-120 min, and obtaining a titanium dioxide precursor through solid-liquid separation; step three: and (4) calcining the titanium dioxide precursor obtained in the step two under the condition of adding a salt treating agent to obtain the titanium dioxide. In the invention, the titanyl sulfate is used for preparing the seed crystal to induce the titanyl dichloride to generate the titanium dioxide, so that the particle size distribution of the hydrolysate is uniform, the hydrolysis speed is high, and the quality of the obtained titanium dioxide is good. The chemical reaction for preparing the seed crystal by the titanyl sulfate is TiOSO 4 +2NaOH+H 2 O＝Ti(OH) 4 +Na 2 SO 4 In Ti (OH) 4 Under the induction action, the titanyl dichloride generates hydrolysis reaction TiOCl 2 +H 2 O＝TiO 2 +2HCl。
The "titanyl sulfate solution" referred to in the present invention is an aqueous solution of a mixture of titanyl sulfate and titanium sulfate produced by reacting sulfuric acid with a titanium raw material in the production of titanium white by a sulfuric acid method. The "lye" referred to in the present invention is selected from the group consisting of sodium hydroxide solution, potassium hydroxide solution or ammonia. The alkali liquor can be prepared by self-preparation of a commercially available solid medicine and desalted water, or can be prepared by dilution of a commercially available liquid medicine. The 'titanium oxychloride solution' mentioned in the invention is obtained by reacting titanium concentrate with hydrochloric acid and then removing impurities, and can be simply written as TiO in titanium concentrate 2 +2HCl＝TiOCl 2 +H 2 O。
In the method, the standard that the stability of the crystal seed solution is qualified is as follows: when 10ml of the seed crystal solution is diluted with distilled water at 25 ℃ until just turbidity appears, the volume of the required water is 120ml to 130ml, that is, if 10ml of the seed crystal solution is diluted with distilled water at 25 ℃ until just turbidity appears, the volume of the required water is 120ml to 130ml, the stability of the seed crystal solution is considered to be qualified.
In the first step of the invention, the ratio of the alkali liquor to the titanyl sulfate solution is alkali/TiO 2 The alkali/TiO is calculated by mass ratio 2 = 0.14-0.27, the preheated titanyl sulfate solution is added into the preheated alkali liquor within 2min, and the mixed solution is heated to 95 ℃ -98 ℃ within 2-3 min after the titanyl sulfate solution and the alkali liquor are uniformly stirred.
In the second step of the invention, the crystal seed solution with qualified stability and the titanium oxychloride are both measured by titanium dioxide, and TiO in the crystal seed solution 2 With TiO in solution of titanium oxychloride 2 The mass ratio is 2-5%, and the seed crystal solution with qualified stability is added into the titanium oxychloride solution preheated to 88-92 ℃ within 2-3 min.
In the third step of the invention, when the aluminum salt treating agent is used, the highest calcining temperature is within the range of 920-990 ℃, and the calcining time is generally 7-12 h from low temperature to high temperature by adopting a rotary kiln; when the zinc salt treating agent is used, the highest calcining temperature is 820-890 ℃, and the calcining is generally carried out for 7-12 h from low temperature to high temperature by adopting a rotary kiln.
In the invention, the concentration of the alkali liquor is selected to be 8-12% so as to ensure that the reaction temperature is in a controllable range; in the invention, the alkali liquor and the titanyl sulfate solution are respectively preheated to 83-85 ℃, and the titanyl sulfate solution can not be hydrolyzed in advance in the temperature range, and the proper reaction rate after being mixed with the alkali liquor can be ensured; in the invention, the preheated titanyl sulfate solution needs to be added into the preheated alkali liquor within 2 minutes, the uniformity of the seed crystal is deteriorated when the time exceeds 2 minutes, and the addition of the titanyl sulfate solution into the alkali liquor is to ensure that the reaction grows in an alkaline environment, but not in an acidic environment; in the invention, the aim of detecting the stability of the crystal seed solution is to verify that the crystal seeds reach the standardThe qualification verification proves that TiOSO with proper proportion occurs in the mixed solution 4 +2NaOH+H 2 O＝Ti(OH) 4 +Na 2 SO 4 And (4) reacting.
The present invention will be specifically described below with reference to specific examples.
Example 1
A process for preparing titanium dioxide from a solution of titanyl dichloride, the process comprising the steps of:
A. adding desalted water and caustic soda flakes into a dilute caustic soda preparation tank to prepare 10% dilute caustic soda solution, and taking 0.48m 3 The prepared NaOH dilute alkali solution with the concentration of 10 percent is put into an alkali solution heating tank and preheated to 85 ℃, and the amount of the NaOH dilute alkali solution is measured to be 1.35m 3 A195 g/L strength titanyl sulfate pump was pumped into the seed solution preheat tank and preheated to 85 deg.C (in this example, the ratio of NaOH to titanyl sulfate solution was NaOH/TiO) 2 Mass ratio was 0.202).
B. Adding the preheated titanyl sulfate solution with the concentration of 195g/L into the preheated NaOH solution with the concentration of 10 percent within 2 minutes, quickly and uniformly stirring, carrying out partial neutralization, heating the mixed solution to 96 ℃ within 2 minutes, preserving the temperature, and detecting the stability of the seed crystal solution;
C. the measuring volume is 263.25m 3 The titanyl dichloride solution was preheated to 90 deg.C (in this example, tiO in the seed solution) 2 With TiO in solution of titanium oxychloride 2 2 percent of mass ratio) and 50g/L (by TiO) of titanium oxychloride solution 2 Metering), when the stability of the seed crystal solution in the step B reaches 125ml/10ml, adding the seed crystal solution into the preheated titanyl dichloride solution within 2 minutes;
D. uniformly mixing titanyl sulfate with qualified stability and titanyl dichloride solution, rapidly heating to 96 ℃ within 3 minutes, preserving heat for 120 minutes, and finishing hydrolysis;
E. and filtering and washing the mixed solution, and separating out the solution to obtain the titanium dioxide precursor.
F. And (3) after the titanium dioxide precursor is pretreated, calcining to obtain a titanium dioxide product.
Practice ofExample 2
A process for preparing titanium dioxide from a solution of titanyl dichloride, the process comprising the steps of:
A. will be 0.0242m 3 Placing 50% alkali solution into the seed crystal preparation tank, and adding 0.145m 3 Diluting sodium hydroxide with process water to concentration of about 10%, adding the prepared 10% NaOH dilute alkali solution into an alkali solution heating tank, preheating to 84 deg.C, and measuring to obtain 0.675m solution 3 The 195g/L seed solution was pumped into a seed solution preheating tank and preheated to 84 deg.C (in this example, the ratio of NaOH to titanyl sulfate solution was NaOH/TiO) 2 Mass ratio was 0.140).
B. Adding the preheated seed crystal solution with the concentration of 195g/L into the preheated NaOH solution with the concentration of 10% within 2 minutes, quickly and uniformly stirring, carrying out partial neutralization, heating the mixed solution to 97 ℃ within 2 minutes, carrying out heat preservation, and detecting the stability of the seed crystal solution;
C. measuring volume of 131.6m 3 The titanyl dichloride solution was preheated to 90 deg.C (in this example, tiO in the seed solution) 2 With TiO in solution of titanyl dichloride 2 2 percent of mass ratio), and the concentration of the titanium oxychloride solution is 50g/L (by TiO) 2 Metering), when the stability of the seed crystal solution in the step B reaches 125ml/10ml, adding the seed crystal solution into the preheated titanyl dichloride solution within 2 minutes;
D. uniformly mixing the crystal seed solution with qualified stability and the titanium oxychloride solution, quickly heating to 96 ℃ within 3 minutes, preserving the temperature for 120 minutes, and finishing hydrolysis;
E. and filtering and washing the mixed solution, and separating out the solution to obtain the titanium dioxide precursor.
F. After the titanium dioxide precursor is pretreated, the titanium dioxide precursor is calcined to obtain a titanium dioxide product.
Example 3
A process for preparing titanium dioxide from a solution of titanyl dichloride, the process comprising the steps of:
A. 0.028m 3 Adding 50% alkali solution into the seed crystal preparation tank, and adding 0.145m 3 Diluting sodium hydroxide with process water to concentration of about 10%, adding the prepared 10% NaOH dilute alkali solution into an alkali solution heating tank, preheating to 83 deg.C, and measuring to obtain 0.675m solution 3 The seed solution having a concentration of 195g/L was pumped into a seed solution preheating tank and preheated to 83 deg.C (in this example, the ratio of NaOH to titanyl sulfate solution was NaOH/TiO 2 Mass ratio was 0.162).
B. Adding the preheated seed crystal solution with the concentration of 195g/L into the preheated NaOH solution with the concentration of 10% within 2 minutes, quickly and uniformly stirring, carrying out partial neutralization, heating the mixed solution to 97 ℃ within 2 minutes, carrying out heat preservation, and detecting the stability of the seed crystal solution;
C. the volume is measured to be 65.8m 3 The titanyl dichloride solution was preheated to 90 deg.C (in this example, tiO in the seed solution) 2 With TiO in solution of titanium oxychloride 2 4 percent of mass ratio) and the concentration of the titanium oxychloride solution is 50g/L (by TiO) 2 Metering), when the stability of the seed crystal solution in the step B reaches 125ml/10ml, adding the seed crystal solution into the preheated titanyl dichloride solution within 2 minutes;
D. uniformly mixing the crystal seed solution with qualified stability and the titanium oxychloride solution, quickly heating to 96 ℃ within 3 minutes, preserving the temperature for 120 minutes, and finishing hydrolysis;
E. and filtering and washing the mixed solution, and separating out the solution to obtain the titanium dioxide precursor.
F. And (3) after the titanium dioxide precursor is pretreated, calcining to obtain a titanium dioxide product.
Example 4
A process for preparing titanium dioxide from a solution of titanyl dichloride, the process comprising the steps of:
A. adding desalted water and caustic soda flakes into a dilute caustic soda preparation tank to prepare 8% dilute caustic soda solution, and taking 1.180m 3 The prepared NaOH dilute alkali solution with the concentration of 8 percent is put into an alkali solution heating tank and preheated to 83 ℃, and the amount of the NaOH dilute alkali solution is measured to be 1.9m 3 Titanyl sulfate having a concentration of 200g/L was pumped into the seed solution preheating tank and preheated to 83 deg.C (in this example, the ratio of NaOH to titanyl sulfate solution was NaOH/TiO) 2 Mass ratio was 0.27).
B. Adding the preheated titanyl sulfate solution with the concentration of 200g/L into the preheated NaOH solution with the concentration of 8% within 2 minutes, quickly and uniformly stirring, carrying out partial neutralization, heating the mixed solution to 98 ℃ within 2 minutes, carrying out heat preservation, and detecting the stability of the seed crystal solution;
C. the measuring volume is 126.67m 3 The titanyl dichloride solution was preheated to 92 deg.C (in this example, tiO in the seed solution) 2 With TiO in solution of titanyl dichloride 2 5 percent of mass ratio) and 60g/L (by TiO) of titanium oxychloride solution 2 Metering), when the stability of the seed crystal solution in the step B reaches 130ml/10ml, adding the seed crystal solution into the preheated titanyl dichloride solution within 2 minutes;
D. uniformly mixing titanyl sulfate with qualified stability and titanyl dichloride solution, rapidly heating to 98 ℃ within 3 minutes, preserving the temperature for 105 minutes, and finishing hydrolysis;
E. and filtering and washing the mixed solution, and separating out the solution to obtain the titanium dioxide precursor.
F. After the titanium dioxide precursor is pretreated, the titanium dioxide precursor is calcined to obtain a titanium dioxide product.
Example 5
A process for preparing titanium dioxide from a solution of titanyl dichloride, the process comprising the steps of:
A. adding desalted water and flake caustic soda into a dilute caustic soda preparation tank to prepare dilute caustic soda solution with the concentration of 12 percent, and taking 0.504m 3 Placing prepared NaOH dilute alkali solution with concentration of 12% into an alkali solution heating tank, preheating to 85 deg.C, and measuring to obtain 2m 3 Titanyl sulfate having a concentration of 190g/L was pumped into the seed solution preheating tank and preheated to 85 deg.C (in this example, the ratio of NaOH to titanyl sulfate solution was NaOH/TiO) 2 Mass ratio was 0.18).
B. Adding the preheated titanyl sulfate solution with the concentration of 190g/L into the preheated NaOH solution with the concentration of 12% within 2 minutes, quickly and uniformly stirring, carrying out partial neutralization, heating the mixed solution to 95 ℃ within 2 minutes, preserving heat, and detecting the stability of the seed crystal solution;
C. the volume of the sample is taken to be 211.1m 3 The titanyl dichloride solution was preheated to 88 deg.C (in this example, tiO in the seed solution) 2 With TiO in solution of titanium oxychloride 2 3 percent of mass ratio) and 60g/L (by TiO) of titanium oxychloride solution 2 Metering), when the stability of the seed crystal solution in the step B reaches 120ml/10ml, adding the seed crystal solution into the preheated titanyl dichloride solution within 2 minutes;
D. uniformly mixing titanyl sulfate with qualified stability and titanyl dichloride solution, quickly heating to 95 ℃ within 3 minutes, preserving heat for 90 minutes, and finishing hydrolysis;
E. and filtering and washing the mixed solution, and separating out the solution to obtain the titanium dioxide precursor. F. After the titanium dioxide precursor is pretreated, the titanium dioxide precursor is calcined to obtain a titanium dioxide product.
Claims (10)
1. A method for preparing titanium dioxide from a titanyl dichloride solution, which is characterized by comprising the following steps:
the method comprises the following steps: preheating 8-12% alkali liquor to 83-85 ℃, preheating 190-200 g/L titanyl sulfate solution to 83-85 ℃, adding the preheated titanyl sulfate solution into the preheated alkali liquor, uniformly stirring, heating the mixed solution to 95-98 ℃, preserving heat to obtain a seed crystal solution, and detecting the stability of the seed crystal solution;
step two: adding the crystal seed solution with qualified stability into a titanium oxychloride solution preheated to 88-92 ℃, wherein the titanium oxychloride solution has the metering concentration of 50-60 g/L by titanium dioxide, heating to 95-98 ℃, preserving heat for 90-120 min, and obtaining a titanium dioxide precursor through solid-liquid separation;
step three: and (4) calcining the titanium dioxide precursor obtained in the step two under the condition of adding a salt treating agent to obtain the titanium dioxide.
2. The method for preparing titanium dioxide from a titanyl dichloride solution as set forth in claim 1, wherein in the first step, the titanyl sulfate solution is an aqueous solution of a mixture of titanyl sulfate and titanium sulfate produced by reacting sulfuric acid with a titanium raw material in the preparation of titanium white by a sulfate process.
3. The method for preparing titanium dioxide from a titanyl dichloride solution according to claim 1, wherein in the step one, if 10ml of the seed solution is diluted with distilled water at 25 ℃ until the volume of the required water is 120ml to 130ml immediately before turbidity appears, the stability of the seed solution is considered to be acceptable.
4. The method for preparing titanium dioxide from titanyl dichloride solution according to claim 1, wherein in step one, the alkali solution is selected from sodium hydroxide solution, potassium hydroxide solution or ammonia water.
5. The method of claim 4, wherein in step one, the ratio of the lye to the titanyl sulfate solution is based on alkali/TiO 2 The alkali/TiO is calculated by mass ratio 2 ＝0.14～0.27。
6. The method for preparing titanium dioxide from titanyl dichloride solution according to claim 1, wherein in step two, the seed solution with qualified stability and the titanyl dichloride are both metered by titanium dioxide, and TiO in the seed solution 2 With TiO in solution of titanium oxychloride 2 The mass ratio is 2-5%.
7. The method for preparing titanium dioxide from titanyl dichloride solution according to claim 1, wherein in the first step, preheated titanyl sulfate solution is added into preheated alkali liquor within 2min, and after the titanyl sulfate solution and the alkali liquor are uniformly stirred, the mixed solution is heated to 95-98 ℃ within 2-3 min.
8. The method for preparing titanium dioxide from titanyl dichloride solution according to claim 1, wherein in step two, the seed crystal solution with qualified stability is added into the titanyl dichloride solution preheated to 88-92 ℃ within 2-3 min.
9. The method for preparing titanium dioxide from titanyl dichloride solution according to claim 1, wherein in step three, the salt treatment agent is an aluminum-based formulation consisting of potassium hydroxide, phosphoric acid and aluminum sulfate or a zinc-based formulation consisting of potassium hydroxide, phosphoric acid and zinc sulfate.
10. The method of claim 9, wherein in the third step, the maximum calcination temperature is 920 ℃ to 990 ℃ and the calcination time is 7 hours to 12 hours when using the aluminum salt treatment formulation, and the maximum calcination temperature is 820 ℃ to 890 ℃ and the calcination time is 7 hours to 12 hours when using the zinc salt treatment formulation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211108703.7A CN115367793A (en) | 2022-09-13 | 2022-09-13 | Method for preparing titanium dioxide from titanyl dichloride solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211108703.7A CN115367793A (en) | 2022-09-13 | 2022-09-13 | Method for preparing titanium dioxide from titanyl dichloride solution |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115367793A true CN115367793A (en) | 2022-11-22 |
Family
ID=84071288
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202211108703.7A Pending CN115367793A (en) | 2022-09-13 | 2022-09-13 | Method for preparing titanium dioxide from titanyl dichloride solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115367793A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834019A (en) * | 2006-04-05 | 2006-09-20 | 江苏太白集团有限公司 | Prepn. method of hydrolytic crystal seeds for producing titanium pigment |
| CN109911931A (en) * | 2019-04-16 | 2019-06-21 | 正太新材料科技有限责任公司 | A kind of preparation method of anatase thpe white powder |
-
2022
- 2022-09-13 CN CN202211108703.7A patent/CN115367793A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1834019A (en) * | 2006-04-05 | 2006-09-20 | 江苏太白集团有限公司 | Prepn. method of hydrolytic crystal seeds for producing titanium pigment |
| CN109911931A (en) * | 2019-04-16 | 2019-06-21 | 正太新材料科技有限责任公司 | A kind of preparation method of anatase thpe white powder |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101092245B (en) | Methods for preparing and using crystal seeds of rutile in high activity | |
| CN101565201B (en) | Preparation of white titanium pigment double action crystal seed from metatitanic acid | |
| CN107720801B (en) | A method of blanc fixe is prepared using titanium white waste acid | |
| CN110589884B (en) | Method for recycling waste and side-product titanium oxychloride | |
| NO130793B (en) | ||
| CN1843938A (en) | Method for preparing vanadium pentoxide | |
| CN104030346A (en) | Method for preparing high brightness rutile titanium dioxide | |
| CN103043715A (en) | Production method of titanium dioxide powder | |
| CN106829904B (en) | A kind of preparation method of graininess calcium phosphate dibasic anhydrous | |
| CN108516582B (en) | Preparation method of high-weather-resistance nano rutile titanium dioxide | |
| FI67358C (en) | SAOSOM ADSORPTIONSMEDEL OCH SAMLARREAGENS ANVAENDBAR TITANDIOXIDHYDRAT MED SPECIELL STRUKTUR | |
| CN115367793A (en) | Method for preparing titanium dioxide from titanyl dichloride solution | |
| US8268203B2 (en) | Method for producing microcrystalline titanium oxide | |
| JP6970174B2 (en) | The method for producing titanium dioxide and the resulting titanium dioxide | |
| CN109205663A (en) | Automatic growing crystal species and preparation method thereof are hydrolyzed in Producing Titanium Dioxide | |
| CN107572588B (en) | A kind of environment-friendly type sodium tungstate preparation process and its application | |
| AU2017284781B2 (en) | Production of nanoparticulate titanium dioxide | |
| US1851487A (en) | Preparation of titanium hydroxide | |
| CN109019680A (en) | A kind of Titanium Dioxide Produced by Chloride Procedure by-product hydrochloric acid production titanium dioxide method | |
| CN107043126A (en) | The method that dichloro oxygen titanium solution is prepared by metatitanic acid | |
| CN101786962A (en) | Method for producing amino acid chelate iron | |
| CN114573021A (en) | High-purity mixed crystal titanium dioxide and production method thereof | |
| US2998321A (en) | Solutions of titanium and aluminium salts | |
| US2055221A (en) | Process of producing titanium pigment | |
| CN115367792B (en) | Preparation method of sulfuric acid process titanium dioxide hydrolysis composite seed crystal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |