IP Library Granted Patent US 9,097,996
Granted Patent B2
US 9,097,996 · App. 13/810,834 · Granted Aug 4, 2015

Silicon dioxide powder having special surface properties and toner composition containing said powder

View Patent ↗
Loading inventors, assignments & file history…
Monitor This Case
Get email alerts when status or documents change.
Order Certified Copies
Most orders are placed with the USPTO same day — all within 24 business hours.
Order via The Patent Place →
Pre-filled with this patent's details
Quick Facts
Patent No.
US 9,097,996
App. No.
13/810,834
Granted
Aug 4, 2015
Kind
B2
Abstract

The invention relates to silicon dioxide powder which is present in the form of aggregated primary particles having an average diameter of at least 40 nm and a ratio of the BET surface area to the STSA surface area of at least 3.5. The invention also relates to a toner composition containing said silicon dioxide powder.

Claims (44)

1. A silica powder, in a form of aggregated primary particles having a mean diameter of at least 40 nm and a ratio of a BET surface area to a STSA surface area of at least 3.5.

2. The silica powder of claim 1 , wherein

the BET surface area is 100 to 400 m 2 /g.

3. The silica powder of claim 1 , having

a thickening action based on the STSA surface area of more than 8 mPas·g/m 2 .

4. The silica powder of claim 1 , having

a micropore volume of at least 0.07 cm 3 /g.

5. The silica powder of claim 1 , having a

fractal dimension Dm of at least 2.80.

6. The silica powder of claim 1 , wherein a

DBP absorption based on the STSA surface area is 3.5 g/100 g m 2 g −1 or higher.

7. A process for preparing the silica powder of claim 1 , the process comprising

a) supplying a mixture comprising one or more hydrolysable and/or oxidizable silicon compounds, an oxygen-comprising gas and a primary combustion gas which reacts with the oxygen-comprising gas to form water, to a flame burning from a burner in a flame tube,

b) separately introducing one or more secondary combustion gases into the flame tube from a tube surrounding the burner, and

c) at a later time, supplying one or more tertiary combustion gases to a reaction mixture within the flame tube, and

d) then removing at least one solid from the reaction mixture, where

gamma 1 <1, gamma 2 <1 and gamma 3 <1 and

gamma 1/2 =gamma 1 +gamma 2 <1

gamma total =gamma 1 +gamma 2 +gamma 3 >1 and

lambda 1 >1 where

gamma 1 =primary combustion gas/stoichiometrically required combustion gas

gamma 2 =secondary combustion gas/stoichiometrically required combustion gas

gamma 3 =tertiary combustion gas/stoichiometrically required combustion gas and

lambda 1 =oxygen in the oxygen-containing gas/stoichiometrically required oxygen.

8. The process of claim 7 , wherein

gamma 1 >gamma 2 .

9. The process of claim 7 , wherein

(i) gamma 1 <gamma 3 , (ii) gamma 2 <gamma 3 , or both (i) and (ii).

10. The process of claim 7 , wherein

0.2≦gamma 1 ≦0.6 and 0.4≦gamma 3 ≦0.8.

11. The process of claim 7 , wherein the

secondary combustion gas, the tertiary combustion gas, or both, are supplied by a ring nozzle.

12. The process of claim 7 , wherein

1<lambda 1 ≦10.

13. The process of claim 7 , further comprising introducing

a further oxygen-comprising gas into the flame tube.

14. A process for preparing a surface-modified silica powder in a form of aggregated primary particles, a surface of which or parts thereof is covered by chemically bound linear and/or branched alkylsilyl groups having 1 to 20 carbon atoms, the process comprising spraying the silica powder of claim 1 with one or more surface-modifying agents which are optionally dissolved in an organic solvent and have linear and/or branched alkylsilyl groups having 1 to 20 carbon atoms, and subsequently thermally treating the sprayed silica powder at a temperature of 120 to 400° C. over a period of 0.5 to 8 hours, optionally under a protective gas.

15. The process of claim 14 , wherein

the surface-modifying agent is at least one selected from the group consisting of hexamethyldisilazane, dimethyldimethoxysilane, dimethyldiethoxysilane, trimethylmethoxysilane, methyltrimethoxysilane, butyltrimethoxysilane, dimethyldichlorosilane, trimethylchlorosilane and a silicone oil.

16. A surface-modified silica powder in a form of aggregated primary particles, a surface of which or parts thereof is covered by chemically bound linear and/or branched alkylsilyl groups having 1 to 20 carbon atoms, obtained by the process of claim 14 .

17. A toner composition comprising the silica powder of claim 1 .

18. The silica powder of claim 1 , wherein the aggregated primary particles have a mean diameter of 40 to 70 nm.

19. The silica powder of claim 1 , wherein the ratio of the BET surface area to the STSA surface area is in a range of 3.5 to 7.

20. The silica powder of claim 1 , having a micropore volume of 0.07 to 0.09 cm 3 /g.

Assignments (2)
CHANGE OF NAME Recorded Jan 31, 2020
From: EVONIK DEGUSSA GMBH
To: EVONIK OPERATIONS GMBH
Reel/Frame 051765/0166 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Apr 3, 2013
From: HILLE, ANDREAS
To: EVONIK DEGUSSA GMBH
Reel/Frame 030140/0329 →