Method for producing high purity lignin

Patent metadata

Field	Value
Publication number	US-10072037-B2
Application number	US-201715648661-A
Country	US
Kind code	B2
Filing date	Jul 13, 2017
Priority date	Jan 24, 2013
Publication date	Sep 11, 2018
Grant date	Sep 11, 2018

Abstract

The method is for separation of lignin from original black liquor (BLIN) that has a first precipitation stage (PR) for precipitation of lignin by a first acidification using acidifier AC1, preferably using CO2, at alkaline conditions, then separating a lignin cake with subsequent suspension of the lignin cake in a strong acid in order to leach our metals from the lignin followed by dewatering and obtaining a clean lignin product LP. The process further is improved by intensified hydrolysis of lignin cake such that most of the carbohydrates are broken down to dissolvable monomers that could be separated from the lignin in the filtrate from a filtering stage subsequent to the hydrolysis. The improved hydrolysis could reduce as much as 90% of the carbohydrate content using a moderately increased temperature and increased charge of acidifier while avoiding any larger lignin yield losses.

First claim

I claim:

1. A method for separation of lignin from original black liquor (BL IN ) having a first alkaline pH value, comprising the following stages in sequence:
in a first precipitation stage (PR), adding an acidifier charge to an original black liquor in order to decrease a pH value of the original black liquor to a second pH level initiating precipitation of lignin so that the second pH level is above a pH value of 7 and below 11.5,
in a subsequent first separation stage (FP 1 ), separating a precipitated lignin as a lignin cake (LIG 1 ) with a content of carbohydrates from a remaining liquid phase of the original black liquor still kept in a pH range from neutral to alkaline,
mixing a lignin from the lignin cake with a content of carbohydrates in a subsequent stage with a second acidifier added to the lignin cake forming an acidic slurry establishing a pH value in a range of 1-3,
establishing a reaction temperature in a range of 100-140° C. in the acidic slurry,
maintaining the acidic slurry at the reaction temperature for a reaction time period during which at least 60% of the content of carbohydrates is hydrolyzed, the reaction time period being in a range of 10-30 minutes resulting in a P-factor of less than 20,
rapidly cooling the acidic slurry to reduce a temperature of the acidic slurry in 10 seconds to 2 minutes to a temperature in a range of 40-60° C., and
in a subsequent second separation stage, separating a treated and cooled lignin content from the acidic slurry and carbohydrates dissolved in the acidic slurry forming a low carbohydrate lignin cake.

2. A method according to claim 1 wherein the reaction temperature in the acidic slurry is in a range of 135-140° C.

3. A method according to claim 1 wherein after the acidic slurry is rapidly cooled to a cooling temperature of 50-60° C.

4. A method according to claim 3 wherein the acidic slurry is cooled to the cooling temperature in 10 seconds to 1 minute.

5. A method according to claim 4 wherein the acidic slurry is cooled to the cooling temperature in 20-40 seconds.

Assignees

• Valmet Oy

Inventors

• Tikka Panu

Classifications

• D21C11/04

  of alkali lye · CPC title

• D21C11/0042

  Fractionating or concentration of spent liquors by special methods (concentration by evaporation D21C11/10) · CPC title

• 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