IP Library Granted Patent US 9,617,162
Granted Patent B2
US 9,617,162 · App. 15/089,629 · Granted Apr 11, 2017

Continuous silica production process and silica product prepared from same

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Quick Facts
Patent No.
US 9,617,162
App. No.
15/089,629
Granted
Apr 11, 2017
Kind
B2
Abstract

Disclosed herein is a continuous process for preparing a silica product, comprising: (a) continuously feeding an acidulating agent and an alkali metal silicate into a loop reaction zone comprising a stream of liquid medium; wherein at least a portion of the acidulating agent and the alkali metal silicate react to form a silica product in the liquid medium of the loop reaction zone; (b) continuously recirculating the liquid medium through the loop reaction zone; and (c) continuously discharging from the loop reaction zone a portion of the liquid medium comprising the silica product. Silica products and dentifrice compositions comprising the silica products are also disclosed. A continuous loop reactor is also disclosed.

Claims (38)

1. A continuous process for preparing a silica product, comprising:

(a) continuously feeding an acidulating agent and an alkali metal silicate into a loop reaction zone comprising a stream of liquid medium; wherein at least a portion of the acidulating agent and the alkali metal silicate react to form a silica product in the liquid medium of the loop reaction zone;

(b) continuously recirculating the liquid medium through the loop reaction zone; and

(c) continuously discharging from the loop reaction zone a portion of the liquid medium comprising the silica product;

wherein the loop reaction zone comprises a continuous loop of one or more loop reactor pipes.

2. The process of claim 1 , wherein the process further comprises controlling a temperature of the liquid medium with a heat exchanger in thermal communication with at least a portion of the one or more loop reactor pipes.

3. The process of claim 1 , wherein the acidulating agent and the alkali metal silicate are fed into the loop reaction zone at different points along the loop reaction zone.

4. The process of claim 1 , wherein the portion of the liquid medium discharged from the loop reaction zone is discharged in a volumetric rate proportional to the amount of the acidulating agent and the alkali metal silicate fed into the loop reaction zone.

5. The process of claim 1 , wherein the portion of the liquid medium discharged from the loop reaction zone is discharged in a volumetric rate equal to the amount of the acidulating agent and the alkali metal silicate fed into the loop reaction zone.

6. The process of claim 1 , wherein the process is carried out in a continuous single loop reactor.

7. The process of claim 1 , wherein the liquid medium is recirculated through the loop reaction zone at a rate in a range from 15 L/min to 100 L/min.

8. A continuous process for preparing a silica product, comprising:

(a) continuously feeding an acidulating agent and an alkali metal silicate into a loop reaction zone comprising a stream of liquid medium; wherein at least a portion of the acidulating agent and the alkali metal silicate react to form a silica product in the liquid medium of the loop reaction zone;

(b) continuously recirculating the liquid medium through the loop reaction zone; and

(c) continuously discharging from the loop reaction zone a portion of the liquid medium comprising the silica product;

wherein the liquid medium is recirculated through the loop reaction zone at both:

(1) a pH in a range from 2.5 to 10, and

(2) a rate of from 97 vol. % to 645 vol. % per minute, based on the volume of the liquid medium in the loop reaction zone.

9. The process of claim 8 , wherein the pH is in a range from 6 to 10.

10. The process of claim 8 , wherein the pH is in a range from 7 to 10.

11. The process of claim 8 , wherein:

the alkali metal silicate comprises sodium silicate; and

the acidulating agent comprises sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, or combinations thereof.

12. The process of claim 8 , wherein:

the alkali metal silicate comprises sodium silicate; and

the acidulating agent comprises an acidic solution of aluminum sulfate.

13. The process of claim 8 , wherein the portion of the liquid medium discharged from the loop reaction zone is discharged in a volumetric rate proportional to the amount of the acidulating agent and the alkali metal silicate fed into the loop reaction zone.

14. The process of claim 8 , wherein the liquid medium comprising the silica product is recirculated through the loop reaction zone from 10 to 200 times prior to being discharged from the loop reaction zone.

15. A continuous process for preparing a silica product, comprising:

(a) continuously feeding an acidulating agent and an alkali metal silicate into a loop reaction zone comprising a stream of liquid medium; wherein at least a portion of the acidulating agent and the alkali metal silicate react to form a silica product in the liquid medium of the loop reaction zone;

(b) continuously recirculating all of the liquid medium through the loop reaction zone; and

(c) continuously discharging from the loop reaction zone a portion of the liquid medium comprising the silica product.

16. The process of claim 15 , wherein steps (a)-(c) are carried out simultaneously.

17. The process of claim 15 , wherein the liquid medium is recirculated through the loop reaction zone at a rate of from 97 vol. % to 645 vol. % per minute, based on the volume of the liquid medium in the loop reaction zone.

18. The process of claim 15 , wherein the liquid medium comprising the silica product is recirculated through the loop reaction zone from 10 to 200 times prior to being discharged from the loop reaction zone.

19. The process of claim 15 , wherein a pump is utilized to recirculate the liquid medium through the loop reaction zone.

20. The process of claim 15 , wherein the silica product comprises silica or sodium aluminosilicate.

21. The method of claim 1 , wherein the mean number of times the liquid medium is recirculated through the loop reaction zone is from 10 to 200.

Assignments (2)
CHANGE OF NAME Recorded Dec 20, 2019
From: EVONIK DEGUSSA GMBH
To: EVONIK OPERATIONS GMBH
Reel/Frame 051382/0001 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Oct 25, 2017
From: J.M. HUBER CORPORATION
To: EVONIK DEGUSSA GMBH
Reel/Frame 043944/0334 →