Recovery of high-purity lignin via simultaneous liquid-phase acidification and solvation

Patent metadata

Field	Value
Publication number	US-2023339999-A1
Application number	US-202318303024-A
Country	US
Kind code	A1
Filing date	Apr 19, 2023
Priority date	Apr 20, 2022
Publication date	Oct 26, 2023
Grant date	—

Abstract

Methods for recovering lignins are described that include simultaneous acidification and solvation of lignin. A single step process is described that includes combining a lignin-containing feed with a solvent solution that includes both an organic solvent and a strong acid. Upon formation and heating of the resulting mixture, lignin in the feed can be acidified from the salt form to the acid form in conjunction with solvation of the acidified lignin through the creation of both a liquified lignin-rich liquid phase and a solvent-rich liquid phase in a liquid/liquid equilibrium (LLE).

First claim

What is claimed is:

1 . A method for lignin recovery comprising:
combining a feed containing lignin and one or more impurities with a solvent solution to form a mixture, the solvent solution including a strong acid at a normality of from about 0.25 N to about 4 N, and an organic solvent, the solvent solution including the organic solvent in an amount of from about 20 wt.% to about 90 wt.% of the solvent solution; heating and agitating the mixture, upon which the mixture separates to form a liquid/liquid equilibrium including a liquified lignin-rich phase comprising a first portion of the lignin and a solvent-rich phase comprising a second portion of the lignin; collecting the first portion, wherein the lignin of the first portion will have a higher number average molecular weight as compared to the lignin of the second portion.

2 . The method of claim 1 , wherein the lignin of the first portion is reduced in content of the impurities as compared to the feed.

3 . The method of claim 1 , further comprising pre-treating a lignin-containing material to form the feed.

4 . The method of claim 3 , the pre-treating comprising carbonating a black liquor by a process that includes contacting a black liquor with carbon dioxide.

5 . The method of claim 3 , the pre-treating comprising contacting a black liquor with sulfuric acid.

6 . The method of claim 1 , further comprising further processing the first portion of the lignin or the second portion of the lignin.

7 . The method of claim 6 , the further processing comprising contacting the lignin of the first portion or the lignin of the second portion with an organic solvent in a single or multi-stage treatment process.

8 . The method of claim 7 , the impurities comprising sodium, and wherein following the further processing, the lignin of the first portion has a sodium content of about 100 ppm or less.

9 . The method of claim 6 , the further processing comprising washing the lignin of the first portion or the lignin of the second portion.

10 . The method of claim 1 , the strong acid comprising sulfuric acid.

11 . The method of claim 1 , the organic solvent comprising an organic acid, an aliphatic alcohol, a ketone, an ether, ethyl acetate, or a mixture thereof.

12 . The method of claim 11 , the organic solvent comprising acetic acid, ethanol, methanol, or any combination thereof.

13 . The method of claim 1 , the organic solvent constituting from about 45 wt.% to about 70 wt.% of the solvent solution.

14 . The method of claim 1 , the strong acid having a normality of from about 0.5 N to about 3 N.

15 . The method of claim 1 , wherein the feed and the solvent solution are combined such that the wt./wt. ratio of the total solvent content to the lignin plus impurities content in the mixture as formed is from about 3:1 to about 20:1.

16 . The method of claim 15 , wherein the feed and the solvent solution are combined such that the wt./wt. ratio of the total solvent content to the lignin plus impurities content in the mixture as formed is about 6:1.

17 . The method of claim 1 , wherein the mixture is heated to a temperature of from about 30° C. to about 250° C.

18 . The method of claim 17 , wherein the mixture is heated under increased pressure.

19 . The method of claim 1 , wherein the impurities comprise sodium and ash, the lignin of the first portion containing about 1 wt.% or less ash and a total metals content of about 2,000 ppm or less.

Assignees

• Univ Clemson

Inventors

• Thies Mark C
• Fitzgerald Carter L

Classifications

• D21C11/0007

  Recovery of by-products, i.e. compounds other than those necessary for pulping, for multiple uses or not otherwise provided for (volatile compounds obtained by decomposition of spent liquors in order to regenerate them D21C11/125; compounds obtained by fractionating the liquors in order to regenerate them D21C11/0042) · CPC title

• C07G1/00 Primary

  Low-molecular-weight derivatives of lignin (high-molecular-weight derivatives of lignin {C08H6/00}) · CPC title

• B01D11/0488

  Flow sheets · CPC title

• B01D11/0492

  Applications, solvents used · CPC title

• B01D11/0288

  Applications, solvents · CPC title