IP Library Granted Patent US 7,250,144
Granted Patent B2
US 7,250,144 · App. 11/126,941 · Granted Jul 31, 2007

Perchlorate removal from sodium chlorate process

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Quick Facts
Patent No.
US 7,250,144
App. No.
11/126,941
Granted
Jul 31, 2007
Kind
B2
Abstract

Novel methods for the removal of sodium perchlorate from electrolytic processes for the production of sodium chlorate have been discovered, allowing sodium chlorate production processes to proceed with low levels of sodium perchlorate. A portion of the mother liquor from the sodium chlorate crystallization is fed to a secondary crystallization step to concentrate sodium perchlorate in a second mother liquor. In this manner, at least a portion of the sodium perchlorate in the sodium chlorate production process is isolated in the second mother liquor, which can be removed from the sodium chlorate production process. The process is run until the concentration of sodium perchlorate in the second mother liquor reaches a desired concentration, at which point at least a portion of the second mother liquor can be removed, thereby removing a portion of the sodium perchlorate from the sodium chlorate production process. The removal of sodium perchlorate from the electrolytic production process allows extended process operating time, improved raw material utilization, and improved reaction efficiency.

Claims (23)

1. A method comprising:

electrolyzing an aqueous solution containing sodium chloride to form an aqueous solution containing sodium chlorate and sodium chloride;

crystallizing sodium chlorate from the aqueous solution containing sodium chlorate and sodium chloride to form a mother liquor and sodium chlorate crystals;

separating the sodium chlorate crystals from the mother liquor;

recycling the mother liquor; and

maintaining a sodium perchlorate concentration in the mother liquor below about 1 g/L.

2. The method of claim 1 , wherein the sodium chlorate is produced in a closed loop system and wherein the sodium perchlorate concentration in the mother liquor is maintained below about 1 g/L by segregating sodium perchlorate produced in the electrolysis step, and continuously or from time to time removing a sufficient amount of the segregated sodium perchlorate to maintain the sodium perchlorate concentration in the mother liquor below about 1 g/L.

3. The method of claim 2 , wherein the sodium perchlorate concentration is maintained below about 0.46 g/L.

4. The method of claim 1 , wherein the sodium perchlorate concentration is maintained below about 0.46 g/L.

5. A method comprising:

electrolyzing an aqueous solution containing sodium chloride to form an aqueous solution containing sodium chlorate and sodium chloride;

crystallizing sodium chlorate from the aqueous solution containing sodium chlorate and sodium chloride to form a first mother liquor and a first amount of sodium chlorate crystals;

separating the first amount of sodium chlorate crystals from the first mother liquor;

separating the first mother liquor into a first stream and a second stream;

recycling the first stream;

crystallizing sodium chlorate from at least a portion of the second stream to form a second mother liquor and a second amount of sodium chlorate crystals;

separating the second amount of sodium chlorate crystals from the second mother liquor;

washing the second amount of sodium chlorate crystals with a portion of the second stream from the first mother liquor not fed to the secondary crystallization step or with the second mother liquor;

returning the spent wash stream from the washing step to the secondary crystallization step; and

removing at least a portion of the second mother liquor when the second mother liquor reaches a certain concentration of sodium perchlorate.

6. The method of claim 5 , wherein the certain concentration of sodium perchlorate in the removed second mother liquor is less than about 1000 g/L.

7. The method of claim 5 , wherein the certain concentration of sodium perchlorate in the removed second mother liquor is at least about 750 g/L.

8. A solution concentrated in sodium perchlorate, wherein the solution corresponds to the removed second mother liquor and is produced by the method of claim 5 .

Assignments (21)
ASSIGNMENT OF SECURITY INTEREST IN PATENT COLLATERAL RECORDED AT REEL/FRAME 044100/0339 Recorded Mar 12, 2021
From: BANK OF AMERICA, N.A.
To: HSBC BANK USA, NATIONAL ASSOCIATION, AS THE SUCCESSOR ADMINISTRATIVE AGENT AND COLLATERAL AGENT
Reel/Frame 055578/0880 →
RELEASE OF SECURITY INTEREST Recorded Mar 12, 2021
From: WELLS FARGO BANK, NATIONAL ASSOCIATION
To: TRONOX LLC
Reel/Frame 055583/0001 →
RELEASE OF SECURITY INTEREST Recorded Feb 23, 2021
From: MIDCAP BUSINESS CREDIT LLC
To: EMD ACQUISITION LLC
Reel/Frame 055374/0142 →
SECURITY INTEREST Recorded Dec 17, 2020
From: EMD ACQUISITION LLC
To: UNITY NATIONAL BANK OF HOUSTON
Reel/Frame 054677/0043 →
RELEASE OF SECURITY INTEREST Recorded Oct 15, 2019
From: WELLS FARGO BANK, N.A.
To: TRONOX LLC
Reel/Frame 050722/0291 →
RELEASE OF SECURITY INTEREST Recorded Oct 15, 2019
From: BANK OF AMERICA, N.A
To: TRONOX LLC
Reel/Frame 050722/0274 →
SECURITY INTEREST Recorded Aug 29, 2019
From: EMD ACQUISITION LLC
To: MIDCAP BUSINESS CREDIT LLC
Reel/Frame 050209/0822 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 2, 2019
From: TRONOX LLC
To: EMD ACQUISITION LLC
Reel/Frame 047879/0865 →
PATENT SECURITY AGREEMENT Recorded Oct 2, 2017
From: TRONOX LLC
To: BANK OF AMERICA, N.A., AS COLLATERAL AGENT
Reel/Frame 044100/0339 →
RELEASE OF SECURITY INTEREST IN INTELLECTUAL PROPERTY COLLATERAL AT REEL/FRAME NOS. 027682/0086 AND 030047/0422 Recorded Sep 26, 2017
From: GOLDMAN SACHS BANK USA, AS COLLATERAL AGENT
To: TRONOX LLC
Reel/Frame 044018/0893 →
SECURITY INTEREST Recorded Sep 25, 2017
From: TRONOX LLC
To: WELLS FARGO BANK, NATIONAL ASSOCIATION
Reel/Frame 043993/0340 →
RELEASE OF SECURITY INTEREST IN PATENTS Recorded Sep 25, 2017
From: UBS AG, STAMFORD BRANCH, AS COLLATERAL AGENT
To: TRONOX LLC; TRONOX WORLDWIDE LLC
Reel/Frame 043993/0306 →
PATENT SECURITY AGREEMENT Recorded Jul 18, 2012
From: TRONOX LLC; TRONOX WORLDWIDE LLC
To: UBS AG, STAMFORD BRANCH
Reel/Frame 028582/0669 →
RELEASE OF SECURITY INTEREST IN PATENTS Recorded Jul 12, 2012
From: WELLS FARGO CAPITAL FINANCE, LLC
To: TRONOX LLC; TRONOX WORLDWIDE LLC
Reel/Frame 028535/0362 →
RELEASE OF SECURITY INTEREST Recorded Feb 9, 2012
From: GOLDMAN SACHS LENDING PARTNERS LLC
To: TRONOX LLC
Reel/Frame 027682/0064 →
SECURITY AGREEMENT Recorded Feb 9, 2012
From: TRONOX LLC
To: GOLDMAN SACHS BANK USA, AS COLLATERAL AGENT
Reel/Frame 027682/0086 →
BANKRUPTCY COURT NOTICE CONFIRMING RELEASE OF LIENS EFFECTIVE 2/14/2011 Recorded Mar 24, 2011
From: LEHMAN COMMERCIAL PAPER, INC.
To: TRONOX LLC
Reel/Frame 026010/0684 →
SECURITY AGREEMENT Recorded Feb 22, 2011
From: TRONOX LLC; TRONOX PIGMENTS (SAVANNAH) INC.
To: WELLS FARGO CAPITAL FINANCE, LLC, AS AGENT
Reel/Frame 025822/0026 →
SECURITY AGREEMENT Recorded Feb 15, 2011
From: TRONOX LLC
To: GOLDMAN SACHS LENDING PARTNERS LLC, AS COLLATERAL AGENT
Reel/Frame 025795/0130 →
SECURITY AGREEMENT Recorded Aug 21, 2008
From: TRONOX LLC F/K/A KERR-MCGEE CHEMICAL LLC
To: LEHMAN COMMERCIAL PAPER INC.
Reel/Frame 021411/0792 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 2, 2005
From: SANDERS, KEENAN D.; PARTLOW, KEVIN E.
To: KERR-MCGEE CHEMICAL, LLC
Reel/Frame 016605/0191 →