IP Library Granted Patent US 6,838,068
Granted Patent B2
US 6,838,068 · App. 09/891,412 · Granted Jan 4, 2005

Silica gel

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Quick Facts
Patent No.
US 6,838,068
App. No.
09/891,412
Granted
Jan 4, 2005
Kind
B2
Abstract

A method of producing a silica gel by hydrolyzing a silicon alkoxide and subjecting the resulting hydrogel to a hydrothermal treatment substantially without aging it is described. Also described in a silica gel produced by such a method and a silica gel which has the following characteristics: (a) the pore volume is from 0.6 to 1.6 ml/g, (b) the specific surface area is from 300 to 900 m 2 /g, (c) the mode diameter (Dmax) of pores is less than 20 nm, (d) the volume of pores having diameters within ±20% of Dmax is at least 50% of the total pore volume, (e) it is amorphous, and (f) the content of metal impurities is at most 500 ppm.

Claims (60)

1. A method of producing a silica gel, which comprises:

hydrolyzing a silicon alkoxide, thereby forming a hydrogel; and

subjecting the hydrogel to a hydrothermal treatment substantially without aging the hydrogel, thereby producing said silica gel having the following characteristics:

(a) a pore volume ranging from 0 6 to 1.6 ml/g,

(b) a specific surface area ranging from 300 to 900 m 2 /g,

(c) a mode diameter (Dmax) of pores of less than 20 nm,

(d) a volume of pores having diameters within ±20% of Dmax of at least 50% of the total pore volume;

(e) it is amorphous, and

(f) the content of metal impurities is at most 500 ppm.

2. The method for producing a silica gel according to claim 1 , wherein a hydrogel having a breaking stress of at most 6 MPa is subjected to the hydrothermal treatment.

3. The method for producing a silica gel according to claim 1 , wherein the hydrothermal treatment is carried out at a temperature ranging from 50 to 150° C. for from 1 to 10 hours.

4. The method for producing a silica gel according to claim 1 , wherein an ammonia water is used for the hydrothermal treatment is conducted in ammonia water.

5. The method for producing a silica gel according to claim 1 , wherein hydrolysis of said silicon alkoxide is conducted in the absence of a template.

6. A silica gel, produced by a process comprising:

hydrolyzing a silicon alkoxide, thereby forming a hydrogel; and

subjecting the hydrogel to a hydrothermal treatment substantially without aging the hydrogel, thereby producing said silica gel having the following characteristic:

(a) a pore volume ranging from 0.6 to 1.6 ml/g,

(b) a specific surface area ranging from 300 to 900 m 2 /g,

(c) a mode diameter (Dmax) of pores of less than 20 nm,

(d) a volume of pores having diameters within ±20% of Dmax of at least 50% of the total pore volume;

(e) it is amorphous, and

(f) the content of metal impurities is at most 500 ppm.

7. The silica gel according to claim 6 , wherein a hydrogel having a breaking stress of at most 6 MPa is subjected to the hydrothermal treatment.

8. The silica gel according to claim 6 , wherein the hydrothermal treatment is carried out at a temperature ranging from 50 to 150° C. for from 1 to 10 hours.

9. The silica gel according to claim 6 , wherein the hydrothermal treatment is conducted in ammonia water.

10. The silica gel according to claim 6 , wherein the pore volume ranges from 0.8 to 1.6 ml/g.

11. The silica gel according to claim 6 , wherein the specific surface area ranges from 400 to 900 m 2 /g.

12. The silica gel according to claim 6 , wherein the mode diameter (Dmax) is at least 2 nm.

13. The silica gel according to claim 6 , wherein the volume of pores having diameters within ±20% of Dmax is at least 60% of the total pore volume.

14. The silica gel according to claim 6 , wherein the content of metal impurities is at most 10 ppm.

15. The silica gel according to claim 14 , wherein the content of metal impurities is at most 1 ppm.

16. The silica gel according to claim 6 , wherein the differential pore volume at the mode diameter (Dmax) ranges from 5.0 to 12.0 ml/g.

17. The silica gel according to claim 6 , wherein the value of Q4/Q3 in solid state Si-NMR is at least 1.3.

18. The silica gel according to claim 6 , wherein hydrolysis of said silicon alkoxide is conducted in the absence of a template.

19. The silica gel according to claim 6 , wherein hydrolysis of said silicon alkoxide is conducted in the absence of a template.

20. A silica gel which has the following characteristics:

(a) a pore volume ranging from 0.6 to 1.6 ml/g,

(b) a specific surface area ranging from 300 to 900 m 2 /g,

(c) a mode diameter (Dmax) of pores of less than 20 nm,

(d) a volume of pores having diameters within ±20% of Dmax of at least 50% of the total pore volume;

(e) it is amorphous, and

(f) the content of metal impurities is at most 500 ppm.

21. The silica gel according to claim 20 , wherein the pore volume ranges from 0.8 to 1.6 ml/g.

22. The silica gel according to claim 20 , wherein the specific surface area ranges from 400 to 900 m 2 /g.

23. The silica gel according to claim 20 , wherein the mode diameter (Dmax) is at least 2 nm.

24 .The silica gel according to claim 20 , wherein the volume of pores having diameters within ±20% of Dmax is at least 60% of the total pore volume.

25. The silica gel according to claim 20 , wherein the content of metal impurities is at most 10 ppm.

26. The silica gel according to claim 25 , wherein the content of metal impurities is at most 1 ppm.

27. The silica gel according to claim 20 , wherein the differential pore volume at the mode diameter (Dmax) ranges from 5.0 to 12.0 ml/g.

28. The silica gel according to claim 20 , wherein th value of Q4/Q3 in solid state Si-NMR is at least 1.3.

29. The silica gel according to claim 20 , which is produced by means of a step of hydrolyzing a silicon alkoxide.

30. A method of producing a silica gel, which comprises:

hydrolyzing a silicon alkoxide, thereby forming a hydrogel which has breaking stress of at most 6 MPa; and

subjecting the hydrogel to a hydrothermal treatment substantially without aging the hydrogel, thereby producing said silica gel having the following characteristics:

(a) a pore volume ranging from 0.6 to 1.6 ml/g,

(b) a specific surface area ranging from 300 to 900 m 2 /g,

(c) a mode diameter (Dmax) of pores of less than 20 nm,

(d) a volume of pores having diameters within ±20% of Dmax of at least 50% of the total pore volume;

(e) it is amorphous, and

(f) the content of metal impurities is at most 500 ppm.

Assignments (2)
CHANGE OF NAME Recorded Sep 5, 2017
From: MITSUBISHI RAYON CO., LTD.
To: MITSUBISHI CHEMICAL CORPORATION
Reel/Frame 043750/0834 →
MERGER Recorded Sep 4, 2017
From: MITSUBISHI CHEMICAL CORPORATION
To: MITSUBISHI RAYON CO., LTD.
Reel/Frame 043750/0207 →