Preparation of pure titanium dioxide with anatase crystal structure from titanium oxychloride solution

• US 4,923,682 A
• Filed: 03/30/1989
• Issued: 05/08/1990
• Est. Priority Date: 03/30/1989
• Status: Expired due to Term

• Current Assignee: Tronox Pigments (Savannah), Inc. (Tronox Holdings Plc)
• Original Assignee: Kemira Oyj
• Inventors: Lawhorne, Earl R., Roberts, George L.
• Primary Examiner(s): Stoll, Robert L.
• Assistant Examiner(s): Bos, Steven J.
• Application Number:
  US07/331,628
• Time in Patent Office: 404 Days
• Field of Search: 423/612, 423/610, 423/611, 502/350, 106/436, 106/437
• US Class Current: 423/611
• CPC Class Codes: C01G 23/0536 by hydrolysing chloride-containing salts

Abstract

A method for producing titanium dioxide with an anatase crystal structure from a titanium oxychloride solution. Titanium tetrachloride is mixed with water to form titanium oxychloride, which in turn is mixed with an organic reagent, preferably sorbitol. The resulting solution is hydrolyzed, precipitated and calcined to form titanium dioxide with an anatase crystal structure.

Claims

1. A method for producing titanium dioxide with anatase crystal structure, comprising the steps of:

(a) providing a titanium oxychloride solution;

(b) providing a quantity of an organic reagent selected from the group consisting of sugar, polyhydric alcohols, starch and organic acids which readily form complexes with metal ions;

(c) adding said organic reagent in an amount equivalent to about 0.1 to about 10.0% by weight based on titanium dioxide concentration to said titanium oxychloride solution;

(d) providing a seed suspension of titanium dioxide;

(e) adding said seed suspension to the resultant solution from step (c);

(f) heating said resultant solution including said seed suspension to boiling and continuing boiling for a period sufficient to effect precipitation of titanium hydrolysate;

(g) recovering the precipitated titanium hydrolysate; and

(h) calcining said precipitated titanium hyrolystate to form an anatase titanium dioxide as the final product.

2. A method as claimed in claim 1, including the step of passing said titanium oxychloride solution through a column of activated charcoal and to remove impurities therein prior to step (b).

3. A method as claimed in claim 1, wherein said organic reagent is sorbitol.

4. A method as claimed in claim 1, wherein said organic acid is selected from citric, tartaric and gluconic acids, EDTA and salts of EDTA.

5. A method as defined in claim 1, wherein said organic reagent is selected from the group consisting of sorbitol, mannitol, or pentaerythritol.

6. A method as claimed in claim 1, wherein the amount of seed suspension added in step (e) is from about 0.1 to about 10.0% by weight based on titanium dioxide concentration in said solution.

7. A method as claimed in claim 1, wherein said heating step has a duration of from about 2 to about 5 hours.

8. A method as claimed in claim 1, wherein said calcination step is carried out at a temperature of from about 500°

C. to about 750°

C. for a period of from about 0.5 to about 2 hours.

9. A method as claimed in claim 1, wherein the concentration of said titanium oxychloride solution is from about 50 to about 300 g of titanium dioxide equivalent per liter of solution.

10. A method as claimed in claim 1, wherein said titanium oxychloride solution is obtained by providing a quantity of titanium tetrachloride and mixing said titanium tetrachloride with water to form said titanium oxychloride solution.

11. A method as claimed in claim 3, wherein the amount of sorbitol added is from about 2.5% to about 10% by weight based on equivalent titanium dioxide concentration in said solution.

12. A method as claimed in claim 1, wherein the concentration of said titanium oxychloride solution is from about 150 to about 255 g of titanium dioxide equivalent per liter of solution.

13. A method as claimed in claim 1, wherein the amount of seed suspension added in step (e) is from about 2% to about 5% by weight titanium dioxide based on titanium dioxide concentration in said solution.

14. A method as defined in claim 1, wherein the step of recovering the precipitated titanium hydrolysate includes filtering, washing and drying the hydrolysate precipitate before calcining.

15. A method as claimed in claim 1 wherein the final product of anatase titanium dioxide is at least 78.2% anatase.

16. A method as claimed in claim 1, including the step of treating said titanium oxychloride solution with gaseous hydrogen sulfide to remove impurities therein prior to step (b).

17. A method as claimed in claim 1, including the step of passing said titanium oxychloride solution through a column of activated charcoal and treating said titanium oxychloride solution with gaseous hydrogen sulfide to remove impurities therein prior to step (b).

18. A method as claimed in claim 12 wherein the final product of anatase titanium dioxide is at least 78.2% anatase.

19. A method for producing titanium dioxide with an anatase structure, comprising the steps of:

(a) providing a quantity of titanium tetrachloride;

(b) adding said titanium tetracholoride to water to form a titanium oxychloride solution containing from about 50 to about 300 g of titanium dioxide equivalent per liter of solution;

(c) providing a quantity of an organic reagent selected from the group consisting of sugar, polyhydric alcohols, starch, and organic acids which readily form complexes with metal ions;

(d) adding said organic reagent to said titanium oxychloride solution to form a resultant solution containing from about 0.1% to about 10.0% organic reagent by weight based on titaniam dioxide concentration in said solution;

(e) providing a seed suspension of titanium dioxide containing the equivalent of from about 0.1% to 10.0% by weight based on titanium dioxide concentration in said solution;

(f) adding said seed suspension to said resultant solution;

(g) heating said resultant solution to boiling and continuing boiling for a period sufficient to effect precipitation of titanium hydrolysate;

(h) recovering the precipitated titanium hydrolysate;

(i) calcining said precipitated titanium hydrolysate to form an anatase titanium dioxide as the final product.

20. A method as claimed in claim 19, wherein said organic reagent is selected from the group consisting of sorbitol, mannitol, or pentaerythritol.