IP Library Granted Patent US 8,419,897
Granted Patent B2
US 8,419,897 · App. 13/302,471 · Granted Apr 16, 2013

Method for producing crude tall oil by soap washing with calcium carbonate removal

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Quick Facts
Patent No.
US 8,419,897
App. No.
13/302,471
Granted
Apr 16, 2013
Kind
B2
Abstract

A method for producing crude tall oil from black liquor soap while removing calcium carbonate and lignates is disclosed. Black liquor soap is first combined with an alkaline ash medium having a lower concentration of lignates and inorganic solids than the black liquor soap, to form washed tall oil soap, fortified brine, lignates, and calcium carbonate. The washed tall oil soap is then separated from the fortified brine, lignates, and calcium carbonate, by centrifugation, decantation, filtration, settling, or a combination of these techniques. Acidification of the washed tall oil soap gives crude tall oil and a spent acid mixture. The crude tall oil is separated from the spent acid. The spent acid is made alkaline, and at least a portion of it is returned for use as alkaline wash medium. The method avoids accumulation of calcium sulfate in acidulation units.

Claims (21)

1. A method for producing crude tall oil from black liquor soap while removing calcium and lignates, comprising:

(a) combining a black liquor soap comprising tall oil soap, lignates. and inorganic solids comprising calcium carbonate, with an alkaline wash medium, wherein the alkaline wash medium has a pH from 10 to 14 and a lower concentration of lignates and inorganic solids than the black liquor soap, at a temperature within the range of 25° C. to 100° C. to produce a mixture comprising washed tall oil soap, fortified brine, lignates, and calcium carbonate; wherein the alkaline wash medium has a lignate content <1.0 wt. % and a filterable inorganic solids content <200 ppm:

(b) separating the mixture by centrifugation, decantation, filtration, settling, or a combination of these techniques to provide, in addition to the washed tall oil soap:

(i) a solid phase comprising calcium carbonate, and a liquid phase comprising fortified brine; or

(ii) an unclarified, fortified brine phase;

(c) acidifying the washed tall oil soap isolated in step (b) to give crude tall oil and a spent acid mixture; and

(d) isolating the crude tall oil.

2. The method of claim 1 further comprising

(e) adjusting the pH of the spent acid mixture to be within the range of pH =10 to 14 and returning at least a portion of it to step (a) as alkaline wash medium.

3. The method of claim 1 further comprising transferring the fortified brine to a weak black liquor storage unit.

4. The method of claim 1 further comprising washing the solid phase with water to give calcium carbonate and an aqueous lignate phase.

5. The method of claim 4 further comprising converting the calcium carbonate to lime for use in a Kraft process.

6. The method of claim 4 further comprising recovering lignates from the aqueous lignate phase for use as a biofuel component.

7. The method of claim 1 wherein the unclarified, fortified brine phase is sent to a transfer point in a Kraft plant that is downstream from a multi-effect evaporator system and upstream from a recovery boiler in the plant's liquor system.

8. The method of claim 7 wherein the transfer point is upstream from or directly into either a liquor concentrator or a direct contact evaporator and is upstream from the recovery boiler.

9. The method of claim 1 wherein the unclarified, fortified brine phase is clarified by centrifugation, decantation, filtration, settling, or a combination of these techniques to remove calcium carbonate and recover a clarified, fortified brine.

10. The method of claim 9 wherein the clarified, fortified brine is sent to a transfer point in a Kraft plant that is downstream from a multi-effect evaporator system and upstream from a recovery boiler in the plant's liquor system.

11. The method of claim 1 wherein the amount of alkaline wash medium is within the range of 1 to 60 wt. % based on the combined amounts of black liquor soap and alkaline wash medium.

12. The method of claim 1 wherein the alkaline wash medium has a lignate content within the range of 0.01 to 0.9 wt. % and a filterable inorganic solids content within the range of 10 to 175 ppm.

13. The method of claim 1 wherein step (a) is performed at a temperature within the range of 55° C. to 95° C.

14. The method of claim 1 wherein the alkaline wash medium has a pH within the range of 10.0 to 11.5.

Assignments (16)
RELEASE OF SECURITY INTEREST IN PATENTS Recorded Jul 24, 2024
From: GOLDMAN SACHS BANK USA, AS COLLATERAL AGENT
To: KRATON CHEMICAL, LLC; KRATON CORPORATION
Reel/Frame 068671/0836 →
CORRECTIVE ASSIGNMENT TO CORRECT THE PATENT NO. 8837224 TO PATENT NO. 7737224 PREVIOUSLY RECORDED AT REEL: 037448 FRAME: 0453. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT. Recorded Jun 11, 2022
From: KRATON POLYMERS U.S. LLC; ARIZONA CHEMICAL COMPANY, LLC
To: BANK OF AMERICA, N.A.
Reel/Frame 060344/0919 →
SECURITY INTEREST Recorded Mar 18, 2022
From: KRATON CHEMICAL, LLC; KRATON POLYMERS LLC; KRATON POLYMERS U.S. LLC
To: GOLDMAN SACHS BANK USA, AS COLLATERAL AGENT
Reel/Frame 059864/0455 →
SECURITY INTEREST Recorded Mar 18, 2022
From: KRATON CHEMICAL, LLC; KRATON POLYMERS LLC; KRATON POLYMERS U.S. LLC
To: GOLDMAN SACHS BANK USA, AS COLLATERAL AGENT
Reel/Frame 059525/0804 →
RELEASE OF SECURITY INTEREST Recorded Mar 16, 2022
From: BANK OF AMERICA, N.A.
To: KRATON POLYMERS U.S. LLC; KRATON CHEMICAL, LLC F/K/A ARIZONA CHEMICAL COMPANY, LLC; KRATON POLYMERS LLC; KRATON CORPORATION; KRATON CHEMICAL B.V.
Reel/Frame 059910/0017 →
RELEASE OF SECURITY INTEREST Recorded Mar 15, 2022
From: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS COLLATERAL AGENT
To: ARIZONA CHEMICAL COMPANY, LLC
Reel/Frame 059366/0727 →
SECURITY INTEREST Recorded Apr 16, 2020
From: KRATON POLYMERS U.S. LLC; KRATON CHEMICAL, LLC F/K/A ARIZONA CHEMICAL COMPANY, LLC; KRATON POLYMERS LLC; KRATON CORPORATION
To: BANK OF AMERICA, N.A.
Reel/Frame 053020/0101 →
CHANGE OF NAME Recorded Apr 1, 2020
From: ARIZONA CHEMICAL COMPANY, LLC
To: KRATON CHEMICAL, LLC
Reel/Frame 052282/0011 →
PATENT SECURITY AGREEMENT Recorded Jan 7, 2016
From: ARIZONA CHEMICAL COMPANY, LLC
To: CREDIT SUISSE AG, CAYMAN ISLANDS BRANCH, AS COLLATERAL AGENT
Reel/Frame 037457/0928 →
RELEASE OF SECURITY INTEREST IN PATENT RIGHTS Recorded Jan 6, 2016
From: ANTARES CAPITAL LP, AS SUCCESSOR TO GENERAL ELECTRIC CAPITAL CORPORATION
To: ARIZONA CHEMICAL COMPANY LLC
Reel/Frame 037451/0057 →
CORRECTIVE ASSIGNMENT TO CORRECT THE PATENT NUMBER 8837224 TO PATENT NUMBER 7737224 PREVIOUSLY RECORDED AT REEL: 037448 FRAME: 0453. ASSIGNOR(S) HEREBY CONFIRMS THE SECURITY INTEREST. Recorded Jan 6, 2016
From: KRATON POLYMERS U.S. LLC; ARIZONA CHEMICAL COMPANY, LLC
To: BANK OF AMERICA, N.A.
Reel/Frame 037448/0453 →
RELEASE OF SECURITY INTEREST IN INTELLECTUAL PROPERTY COLLATERAL AT REEL/FRAME NO. 33146/0361 Recorded Jan 6, 2016
From: GOLDMAN SACHS BANK USA
To: ARIZONA CHEMICAL COMPANY LLC
Reel/Frame 037451/0169 →
ASSIGNMENT OF INTELLECTUAL PROPERTY SECURITY AGREEMENT Recorded Oct 9, 2015
From: GENERAL ELECTRIC CAPITAL CORPORATION, AS RETIRING AGENT
To: ANTARES CAPITAL LP, AS SUCCESSOR AGENT
Reel/Frame 036827/0443 →
SECURITY INTEREST Recorded Jun 12, 2014
From: ARIZONA CHEMICAL COMPANY LLC
To: GENERAL ELECTRIC CAPITAL CORPORATION, AS FIRST LIEN COLLATERAL AGENT
Reel/Frame 033146/0333 →
SECURITY INTEREST Recorded Jun 12, 2014
From: ARIZONA CHEMICAL COMPANY LLC
To: GOLDMAN SACHS BANK USA, AS SECOND LIEN COLLATERAL AGENT
Reel/Frame 033146/0361 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jan 30, 2012
From: BOWLES, ROBERT E.; FORAN, C. DOUGLAS; GRIFFIN, JOSEPH H.; SWANN, F. EDWIN
To: ARIZONA CHEMICAL COMPANY, LLC
Reel/Frame 027621/0686 →