IP Library Granted Patent US 8,057,770
Granted Patent B2
US 8,057,770 · App. 12/589,736 · Granted Nov 15, 2011

Process for hydrothermal production of sodium silicate solutions and precipitated silicas

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 8,057,770
App. No.
12/589,736
Granted
Nov 15, 2011
Kind
B2
Abstract

A method is provided for treating silica sand scrubs (SSS) generated and accumulated as waste in the chloride manufacturing process of titanium dioxide pigment. A hydrothermal process is used to produce sodium silicate solutions of modulus 3.0 to 3.8, and precipitated silicas. In some embodiments, the process uses two specific principal reaction stages. A sodium silicate solution having a low SiO 2 :Na 2 O molar ratio, in the range from 2.0 to 2.8, is first produced by reaction of the SSS, as a cost-effective SiO 2 source, with aqueous caustic soda. The conversion of this intermediate sodium silicate solution of low modulus to a high SiO 2 :Na 2 O molar ratio is made possible by using a SiO 2 source that is prepared as precipitated amorphous silica from the intermediate sodium silicate solution produced above.

Claims (20)

1. A sodium silicate solution produced by a method comprising the steps of:

(i) manufacturing titanium dioxide, wherein the manufacturing comprises generating a waste product, the waste product comprising a precursor solid silica source;

(ii) collecting the waste product;

(iii) exfoliating and removing at least about 85% by weight titanium dioxide particles adhering to the surface of the precursor solid silica source of the collected waste product, to form cleaned silica;

(iv) producing an intermediate sodium silicate solution by a hydrothermal fusion reaction of the cleaned silica with a caustic soda in an autoclave;

(v) forming an amorphous silica source by transposing the SiO 2 content of the intermediate sodium silicate of step (iv) by a separate precipitation process; and

(vi) dissolving the amorphous silica provided in step (v) in the intermediate sodium silicate solution of step (iv) and raising the SiO 2 :Na 2 O molar ratio to result in a high modulus sodium silicate solution,

wherein the high modulus sodium silicate solution is characterized by a Ti content of from 100 ppm to 1400 ppm and the following properties:

a physical form of a clear and colorless liquid;

a density of from 1.35 kg/L to 1.45 kg/L;

a minimum content of 27.2% by weight of SiO 2 ;

a maximum content of 9.0% by weight of Na 2 O; and

a SiO 2 :Na 2 O molar ratio of from 3.0:1 to 3.8:1.

2. The sodium silicate solution of claim 1 , wherein the SiO 2 :Na 2 O molar ratio is about 3.52:1.

3. The sodium silicate solution of claim 1 , wherein the precursor solid silica source of the waste product collected in step (ii) comprises silica sand scrubs from a titanium dioxide manufacturing process using chloride.

4. The sodium silicate solution of claim 1 , wherein the hydrothermal fusion reaction of step (iv) comprises reacting the precursor solid silica source of the waste product collected in step (ii) with a caustic soda in a closed autoclave pressure reactor, at a temperature range of from about 180° C. to about 300° C., and under a saturated steam.

5. The sodium silicate solution of claim 4 , wherein the caustic soda comprises an aqueous sodium hydroxide solution, and the amounts of the precursor solid silica source and the aqueous sodium hydroxide solution are such that the molar ratio of SiO 2 in the precursor solid silica source to dissolved Na 2 O in the aqueous sodium hydroxide solution is in a range of from about 2.0 to about 2.8, with respect to 1.

6. The sodium silicate solution of claim 4 , wherein the aqueous sodium hydroxide solution comprises dissolved Na 2 O in an amount stoichiometrically equivalent to a molar ratio of SiO 2 : Na 2 O in a range of from about 3.0 to about 3.8, with respect to 1, and the aqueous sodium hydroxide solution comprises from about 10% to about 50% by weight sodium hydroxide.

7. The sodium silicate solution of claim 1 , wherein the intermediate sodium silicate solution is produced in step (iv) by a hydrothermal fusion reaction of an aqueous sodium hydroxide solution with the cleaned silica formed in step (iii) in an autoclave pressure vessel at a temperature in the range of from about 180° C. to about 300° C., and under a saturated steam.

8. The sodium silicate solution of claim 7 , wherein the aqueous sodium hydroxide solution comprises from about 15% to about 30% by weight sodium hydroxide.

Assignments (6)
SECURITY INTEREST Recorded Sep 26, 2025
From: TRONOX LLC
To: WILMINGTON TRUST, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 072942/0255 →
RELEASE OF SECURITY INTEREST Recorded Apr 7, 2022
From: WILMINGTON TRUST, NATIONAL ASSOCIATION
To: TRONOX LLC
Reel/Frame 059629/0581 →
SECURITY INTEREST Recorded Mar 12, 2021
From: TRONOX LLC
To: HSBC BANK USA, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 055579/0619 →
SECURITY INTEREST Recorded May 1, 2020
From: TRONOX LLC
To: WILMINGTON TRUST, NATIONAL ASSOCIATION, AS COLLATERAL AGENT
Reel/Frame 052554/0529 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 25, 2019
From: THE NATIONAL TITANIUM DIOXIDE CO. LTD. (CRISTAL)
To: TRONOX LLC
Reel/Frame 049583/0638 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 20, 2019
From: TRABZUNI, FADI MOHAMMED SAEED; EL DEKKI, HASSAN MOENES; GOPALKRISHNAN, CHATHANGAT CHEROOLIL
To: THE NATIONAL TITANIUM DIOXIDE CO. LTD. (CRISTAL)
Reel/Frame 049539/0787 →