Multistage process with hydrothermal liquefaction

Abstract

The disclosure relates to a process for converting lignocellulosic feedstock (10) to renewable product (80), wherein the process comprises the following steps; treating (100) lignocellulosic feedstock (10) with aqueous solution (20) to obtain a mixture (30); heating (110) the mixture (30) of step (a) to a temperature between 290 and 340° C., under a pressure from 90 to 120 bar, to obtain a first product mix (40); separating aqueous phase (53) and oil phase (50), and optionally gas (51) and solids (52), of the first product mix (40) of step (b); and heating (130) the oil phase (50) of step (c) and solvent (60). The heating (130) is optionally followed by fractionation (200) to obtain a light fraction (90) and a heavy fraction (91) and optionally a bottom residue fraction (92) and/or a gaseous fraction.

1 . A process for converting lignocellulosic feedstock ( 10 ) to renewable product ( 80 ), characterized in that the process comprises the following steps,
 (a) treating ( 100 ) lignocellulosic feedstock ( 10 ) with aqueous solution ( 20 ), at a temperature between 180° C. and 245° C., under a pressure from 10 to 55 bar, for 10-180 min to obtain a mixture ( 30 );   (b) heating ( 110 ) the mixture ( 30 ) of step (a) at a temperature between 290 and 340° C., under a pressure from 70 to 160 bar, to obtain a first product mix ( 40 );   (c) separating ( 120 ) aqueous phase ( 53 ) and oil phase ( 50 ), and optionally gas ( 51 ) and/or solids ( 52 ), of the first product mix ( 40 ) of step (b) wherein the aqueous phase ( 53 ) is used in step (a) ( 100 ) as aqueous solution ( 20 ); and   wherein the aqueous phase pH is higher than 5.   
     
     
         2 . The process according to  claim 1 , characterized in that the process further comprises (d) heating ( 130 ) the oil phase ( 50 ) of step (c) and solvent ( 60 ) at a temperature between 360° C. to 450° C., under a pressure from 50 to 120 bar. 
     
     
         3 . The process according to  claim 1 , characterized in that the aqueous solution ( 20 ) in step (a) is black liquor, black liquor and water or water and alkaline salts. 
     
     
         4 . The process according to  claim 1 , characterized in that a ratio of dry biomass to total reaction mixture is lower than 0.43 by weight. 
     
     
         5 . The process according to  claim 1 , characterized in that said solvent ( 60 ) in the third step is crude tall oil, acid oil, vegetable oil, renewable hydrocarbons, oxygen containing hydrocarbons or mixtures thereof. 
     
     
         6 . The process according to  claim 1 , characterized in that the oil phase to solvent ratio is from 1:5 to 1.5:1 by weight. 
     
     
         7 . The process according to  claim 1 , characterized in that aqueous phase ( 53 ) of step (c) is recirculated back to step (b) ( 110 ). 
     
     
         8 . The process according to  claim 1 , characterized in that lignocellulosic feedstock ( 10 ) is energy crops, waste or residues of wood-processing, raw-material or residues of pulp- and papermaking, and/or residues of timber processes. 
     
     
         9 . The process according to  claim 1 , characterized in that step (d) ( 130 ) is followed by a step (e) ( 140 ) comprising separating aqueous phase ( 83 ), oil phase ( 80 ) and optionally gas ( 81 ) and/or solids ( 82 ) of the second product mix ( 70 ) of step (d) ( 130 ). 
     
     
         10 . The process according to  claim 8 , characterized in that aqueous phase ( 83 ) of step (e) ( 140 ) is used in step (a) ( 100 ) as aqueous solution ( 20 ) and/or is recirculated back to step (b) ( 110 ). 
     
     
         11 . The process according to  claim 1 , characterized in that step (d) ( 130 ) is followed by fractionation ( 200 ) to obtain a light fraction ( 90 ) and a heavy fraction ( 91 ) and optionally a bottom residue fraction ( 92 ) and/or a gaseous fraction. 
     
     
         12 . The process according to  claim 10 , characterized in that the light fraction ( 90 ) from said fractionation ( 200 ), or part of it, is directed to a hydroprocessing step. 
     
     
         13 . The process according to  claim 10 , characterized in that the light fraction ( 90 ), or part of it, is recycled to step (d) ( 130 ) as solvent ( 60 ). 
     
     
         14 . The process according to  claim 1 , characterized in that the treating of the lignocellulosic feedstock ( 10 ) with aqueous solution ( 20 ) in step (a) ( 100 ) is performed at a temperature from 200° C. to 220° C. and/or a pressure from 10 bar-20 bar for 10-80 minutes. 
     
     
         15 . The process according to  claim 1 , characterized in that heating the mixture ( 30 ) of step (a) ( 100 ) is performed at a temperature from 300° C. and 330° C., and/or at a pressure from 100 bar to 115 bar. 
     
     
         16 . The process according to  claim 1 , characterized in that the heating the oil phase ( 50 ) of step (c) ( 120 ) is performed at a temperature from 370° C. and 400° C. and/or at a pressure from 90-110 bar. 
     
     
         17 . The process according to  claim 1 , characterized in that the heating of step (b) ( 110 ) is performed for 3-60 minutes and/or of step (d) ( 130 ) is performed for 5-30 minutes. 
     
     
         18 . The process according to  claim 1 , characterized in that heat from one or more product streams is used to heat up feed streams. 
     
     
         19 . The process according to  claim 2 , wherein the alkaline salts are chosen from one or more of NaOH, K2CO 3 , KOH, and Na 2 CO 3 . 
     
     
         20 . The process according to  claim 3 , wherein the ratio of dry biomass to total reaction mixture is 0.015 to 0.43. 
     
     
         21 . The process according to  claim 3 , wherein the ratio of dry biomass to total reaction mixture is 0.1 to 0.25. 
     
     
         22 . The process according to  claim 1 , wherein the lignocellulosic feedstock is seeds and/or residues of wood processing. 
     
     
         23 . The process according to  claim 1 , wherein the lignocellulosic feedstock is seed crop, urban wood waste, lumber waste, wood chips, wood branches, bark, wood sawdust, straw, firewood and/or plywood residual. 
     
     
         24 . The process according to  claim 1 , wherein the lignocellulosic feedstock is Brassica carinata seed, wood chips, bark and/or sawdust. 
     
     
         25 . The process according to  claim 1 , characterized in that the treating of the lignocellulosic feedstock ( 10 ) with aqueous solution ( 20 ) in step (a) ( 100 ) is performed at a temperature from 200° C. to 220° C. and/or a pressure from 10 bar-20 bar for 50-70 minutes. 
     
     
         26 . The process according to  claim 15 , wherein the pressure is from 90 to below 100 bar.