Silica-based spherical particulates and methods of preparing the same

Patent metadata

Field	Value
Publication number	US-10486973-B2
Application number	US-201715802511-A
Country	US
Kind code	B2
Filing date	Nov 3, 2017
Priority date	Nov 18, 2016
Publication date	Nov 26, 2019
Grant date	Nov 26, 2019

Abstract

Spherically-shaped silica can include a precipitated silica powder having a d50 particle size selected within a range of greater than 20 μm and up to 80 μm, a di-octyl adipate oil absorption selected within a range of from 150 ml/100 g to 500 ml/100 g, an average circularity selected within a range of from 0.70 to 1.0, and an angle of repose, of less than 30°. A process of preparing spherically-shaped silica powder is also included.

First claim

The invention claimed is:

1. Spherically-shaped silica comprising:
a d 50 particle size selected within a range of greater than 20 μm and up to 80 μm;
a di-octyl adipate oil absorption selected within a range of from 150 ml/100 g to 500 ml/100 g;
an average circularity selected within a range of from 0.70 to 1.0; and
an angle of repose of less than 30°,
wherein the spherically-shaped silica is a precipitated silica powder.

2. The spherically-shaped precipitated silica of claim 1 , wherein the spherically-shaped silica comprises an average tamped density of greater than 150 g/l.

3. The spherically-shaped precipitated silica of claim 1 , wherein the spherically-shaped silica comprises an average tamped density of greater than 250 g/l.

4. The spherically-shaped precipitated silica of claim 1 , wherein the spherically-shaped silica comprises a BET surface area of 80 to 600 m 2 /g.

5. The spherically-shaped precipitated silica of claim 1 , wherein the spherically-shaped silica comprises a CTAB surface area of 80 to 500 m 2 /g.

6. The spherically-shaped precipitated silica of claim 1 , wherein the spherically-shaped silica comprises a d 10 particle size selected within a range of greater than 3 μm and up to 40 μm.

7. The spherically-shaped precipitated silica of claim 1 , wherein the spherically-shaped silica comprises a d 90 particle size selected within a range of greater than 40 μm and up to 90 μm.

8. The spherically-shaped precipitated silica of claim 1 , wherein at least 90 weight % of a sample of the spherically-shaped silica passes through a 200-mesh sieve.

9. The spherically-shaped precipitated silica of claim 1 , wherein the spherically-shaped silica comprises a bulk density selected within a range of at least 5 lb/ft 3 and up to 30 lb/ft 3 .

10. The spherically-shaped precipitated silica of claim 1 , wherein the spherically-shaped silica has an average circularity selected within a range of from 0.70 to 0.95.

11. A process of preparing spherically-shaped precipitated silica powder comprising:
a) preparing a first alkali metal silicate aqueous solution;
b) preparing a second alkali metal silicate aqueous solution having a pH of greater than 7 with the first alkali metal silica aqueous solution and water;
c) simultaneously adding the first alkali metal silicate aqueous solution and an acidifying agent to the second aqueous alkali metal silicate aqueous solution to form a silica suspension comprising precipitated silica;
d) aging the silica suspension at a pH within a range of from 7 to 14; and
e) washing and drying the precipitated silica,
wherein the total time for steps c) and d) is less than 150 minutes, and
wherein the second alkali metal silicate aqueous solution has an alkalinity AZ value selected within a range of from 1 to 40.

12. The process of claim 11 , further comprising adding an additional acidifying agent after the aging such that the pH of the suspension is less than 7.

13. The process of claim 11 , wherein the drying of the precipitated silica comprises dispersing the silica in an aqueous medium and spray drying the dispersed silica.

14. The process of claim 13 , wherein the precipitated silica is dispersed in the aqueous medium to form a solution with a solids content of less than 20%.

15. The process of claim 11 , wherein at least one of steps a) through d) are performed at a temperature selected within a range of from 100° F. to 220° F.

16. The process of claim 11 , wherein the first alkali metal silicate aqueous solution and the acidifying agent are simultaneously added in step c) over a time period within a range from 2 to 90 minutes.

17. The process of claim 11 , wherein the silica suspension is aged in step d) for a period of time selected within a range from 1 minute to 120 minutes.

18. The process of claim 11 , wherein at least one of the first and second alkali metal silicate aqueous solutions is represented by x(SiO 2 )Na 2 O, wherein x is a value selected within a range of from 1 to 4.

19. The process of claim 18 , wherein the first alkali metal silicate aqueous solution has a concentration of less than 85 g/L Na 2 O.

20. The process of claim 11 , wherein an alkalinity AZ value of the second alkali metal silicate aqueous solution decreases during the simultaneous addition step c).

21. The process of claim 11 , wherein an alkalinity AZ value of the second alkali metal silicate aqueous solution is maintained during the simultaneous addition step c).

22. The process of claim 11 , wherein the spherically-shaped precipitated silica is formed in the absence of additional mechanical grinding or milling.

23. The process of claim 11 , wherein the first alkali metal silicate aqueous solution and the acidifying agent are simultaneously added once in a single step.

24. A composition comprising the spherically-shaped silica of claim 1 .

25. The composition of claim 24 , wherein the composition is a rubber composition.

26. The composition of claim 24 , wherein the composition is a coating composition.

27. The composition of claim 24 , wherein the composition is a porous polymer membrane composition.

28. The composition of claim 24 , wherein the composition is a carrier or adsorbent composition.

Assignees

• Ppg Ind Ohio Inc

Inventors

• Zhang Xiaofeng
• Kollah Raphael O

Classifications

• C09C1/3018

  Grinding · CPC title

• C01B33/193 Primary

  of aqueous solutions of silicates · CPC title

• C01B33/18

  Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof (preparation of aerogels by dehydrating gels C01B33/158; treatment to enhance the pigmenting or filling properties C09C) · CPC title

• C01P2004/51

  Particles with a specific particle size distribution · CPC title

• C01P2006/12

  Surface area · CPC title