Post on 30-Dec-2015
description
transcript
1
NREL Update—CAFI 2 Teleconference
Rick ElanderNational Renewable Energy Laboratory
National Bioenergy CenterGolden, CO
February 18, 2004
Biomass Refining CAFI
2
Outline
• Dilute Acid Pretreated Corn Stover Data
• Dilute Acid Pretreated Hybrid Poplar Data (Bench Scale-Steam Gun)
• Description of Dilute Acid Pretreated Hybrid Poplar (Pilot Scale-Sunds Reactor)– Data not yet available
Biomass Refining CAFI
3
Dilute Acid Pretreated Corn Stover• Feedstock: 2nd pass corn stover from Kramer farm (Wray, CO)
– Collected using high rake setting to avoid soil pick-up– Milled to pass 0.25 inch screen (Mitts and Merril knife mill)
– Pretreated in Sunds vertical reactor, with and without hot washing
Biomass Refining CAFI
Component Composition (wt %)
Sucrose 2.2Glucan 34.4Xylan 22.8
Arabinan 4.2Mannan 0.6Galactan 1.4
Lignin 11.0Protein 2.3Acetyl 5.6Ash 6.1
Uronic Acids 3.8Extractives 8.5
4
Biomass Refining CAFI
Pilot Scale Sunds Vertical Reactor
Steam, Hot Water, Hot Acid, Alkali, or Solvent, Hot Air
Pneumapress Filter
Pressurized Solids Tank (Jaygo Reactor)
Steam, Hot Water, Hot Acid or Alkali
High Solids Discflo Pump and Heated Transfer Line
Optional “Hot-Washing” in Pneumapress Filter
5
Dilute Acid Pretreated Corn StoverPretreatment Conditions:1. Typical “mid severity” condition in the Sunds vertical pretreatment reactor (190 C, ~ 1.5 minute
residence time in “flowthrough mode”, 0.045 g sulfuric acid/g dry feedstock, 30% insoluble solids) 2. “Low severity” condition in the Sunds vertical pretreatment reactor (180 C, ~ 1.5 minute residence
time in “flowthrough mode”, 0.03 g sulfuric acid/g dry feedstock, 25% insoluble solids) 3. “Low severity” condition in the Sunds vertical pretreatment reactor (180 C, ~ 1.5 minute residence
time in “flowthrough mode”, 0.03 g sulfuric acid/g dry feedstock, 25% insoluble solids) and hot washed in Pneumapress pressure belt filter with hot water.
Biomass Refining CAFI
6
Dilute Acid Pretreated Corn Stover—Pretreated Solids Composition and
Component Solubilization
Biomass Refining CAFI
Pretreated Solids Composition (wt %)
Amount of Original Component Remaining After Pretreatment
(%)Pretreated Solids
Composition (wt %)
Amount of Original Component Remaining After
Pretreatment (%)Pretreated Solids
Composition (wt %)
Amount of Original Component Remaining After Pretreatment
(%)Glucan 59.5 78.2 57.7 84.7 59.3 93.4Xylan 4.9 13.0 10.5 24.9 9.3 27.2
Arabinan 1.4 22.2 1.3 24.8 0.8 20.1Mannan 0.9 20.2 0.8 29.1 0.8 57.4Galactan 0.9 27.8 0.8 25.1 0.5 22.8
Lignin 29.5 82.4 22.7 81.2 22.5 n/aProtein 2.2 n/a 2.5 n/a 1.9 n/aAcetyl 0.0 n/a nd n/a 1.4 n/a
Ash 4.3 n/a 3.7 n/a 4.6 n/a
Mass % of feedstock remaining insoluble after pretreatment: 46.5
Mass % of feedstock remaining insoluble after pretreatment: 55.9
Mass % of feedstock remaining insoluble after pretreatment: 54.5
Sample 3
Low Severity Sunds Hot Wash, CS040427-J
Sample 2
Low Severity Sunds, 031209CS #7DALW-CSR-180C-1.5m-0.030H2SO4:Dry wt-25% solids-4/27/04-J
Sample 1
Mid Severity Sunds, 031209CS Mix 2-5 DALW-CSR-190C-1.5m-0.045H2SO4:Dry wt-30% solids-12/9/03-Mix 2:5 DALW-CSR-180C-1.5m-0.030H2SO4:Dry wt-25% solids-12/9/03-#7
7
Dilute Acid Pretreated Hybrid Poplar (Bench Scale-Steam Gun)
• Feedstock: USDA-supplied hybrid poplar (Alexandria, MN)– Debarked, chipped, and milled to pass 0.25 inch screen (Mitts and Merril knife mill)
– Pre-impregnated with H2SO4 and pretreated in 4 L NREL steam gun
Biomass Refining CAFI
Component Composition (wt %)Glucan 43.8Xylan 14.9
Arabinan 0.6Mannan 3.9Galactan 1.0
Lignin 29.1Protein ndAcetyl 3.6Ash 1.1
Uronic Acids ndExtractives 3.6
8
Dilute Acid Pretreated Poplar in Steam Gun
Biomass Refining CAFI
190 C
70 s
Acid Loading: 0.02 g H2SO4/g bone dry feedstock
190 C
120 s
200 C
70 s
200 C
120 s
9
Composition of Pretreated Solids from Dilute Acid Pretreated Hybrid Poplar (Bench
Scale-Steam Gun)
Biomass Refining CAFI
Pretreatment Conditionw
t % A
sh
wt %
Pro
tein
wt %
Lig
nin
wt %
Glu
can
wt %
Xyl
an
wt %
Gal
acta
n
wt %
Ara
bina
n
wt %
Man
nan
wt %
Uro
nic
acid
wt %
Ace
tate
Tota
l %
MP041004 A-G (190 C/70 s) 0.1 0.0 46.1 57.3 2.1 0.0 0.0 0.0 0.0 0.0 105.5MP041005 A-G (190 C/120 s) 0.0 0.0 42.5 60.3 1.8 1.0 0.0 0.0 0.0 0.0 105.6MP041005 H-N (200 C/70 s) 0.0 0.0 49.1 54.6 1.5 0.9 0.0 0.0 0.0 0.0 106.1MP041006 A-G (200 C/120 s) 0.0 0.0 59.3 44.3 0.7 0.3 0.0 0.0 0.0 0.0 104.6
10
Composition of Pretreated Liquids from Dilute Acid Pretreated Hybrid Poplar (Bench
Scale-Steam Gun)
Biomass Refining CAFI
Hydrolyzate pH 1.48 1.48 1.48 1.50Glucose Concentration as Cellobiose (g/L) 1.5 1.5 1.9 3.1 as Glucose Monomer (g/L) 43.4 42.5 47.2 66.2 as Total Monomer + Oligomer (g/L) 50.1 49.7 54.5 75.5Xylose Concentration as Monomer (g/L) 44.3 44.0 42.3 22.5 as Total Monomer + Oligomer (g/L) 44.7 45.2 43.7 21.1Galactose Concentration as Monomer (g/L) 4.1 4.0 3.9 2.6 as Total Monomer + Oligomer (g/L) 4.7 4.7 3.7 2.5Arabinose Concentration as Monomer (g/L) 2.3 2.3 2.2 1.1 as Total Monomer + Oligomer (g/L) 1.5 1.7 1.7 0.9Mannose Concentration as Monomer (g/L) 9.7 9.8 8.2 6.0 as Total Monomer + Oligomer (g/L) 10.5 10.2 9.4 5.7Soluble Lignin Concentration (g/L) 22.8 20.4 24.1 29.5Acetic Acid Concentration (g/L) 22.1 20.9 21.5 20.2Furfural Concentration (g/L) 8.7 7.7 8.7 12.2HMF Concentration (g/L) 1.8 1.6 1.9 3.8
11
Glucose and Xylose Component Balance from Dilute Acid Pretreated Hybrid Poplar
(Bench Scale-Steam Gun)
Biomass Refining CAFI
Glucose Component Balance as Glucan (% of original) 87.9 88.0 75.7 67.0 as Glucose Monomer (% of original) 20.7 19.6 24.4 29.4 as Glucose Oligomer (% of original) 3.2 3.4 4.3 4.5 as HMF (% of original) 0.4 0.4 0.5 0.8 Total (% of original) 112.2 111.4 104.9 101.7Xylose Component Balance as Xylan (% of original) 8.3 7.9 5.4 2.9 as Xylose Monomer (% of original) 61.8 56.5 62.4 28.9 as Xylose Oligomer (% of original) 0.6 1.5 2.9 -1.4 as Furfural (% of original) 19.5 18.0 22.0 28.3 Total (% of original) 90.2 83.9 92.7 58.7
12
Example of Detailed Component Balance from Dilute Acid Pretreated Hybrid Poplar
(Bench Scale-Steam Gun)
Biomass Refining CAFI
Pretreatment ConditionsPretreatment Temperature (deg C) 190Pretreatment Time (sec) 70Sulfuric Acid Loading 0.02 g acid/g B.D. feedstock
Sample Label (NREL nomenclature) MP-041004 a-gSample Label (CAFI nomenclature) DASE-POP1-190C-70s-0.02H2SO4:Dry wt-30% solids-10/4/04-N-A:G
Total pretreated mass output including rinsate (O.D. wt) (g) 2529.8Total charge of preimpregnated feedstock--wet wt. (g) 5950.0 Total wet wt of pretreated feedstock (g)--including steam condensate 8143.0Total feedstock input (O.D. wt) (g) 2664.4 Measured total dry solids of pretreated feedstock (wt%) 30.1
Feedstock mass solubilized in pretreatment (% of original feedstock) 29.5
Total SolublesRecovery Recovery
(wt%) Total (wt%) Total (g/L) (g/L) Total (g/L) (g/L) Total (% in feed) (% in feed)wt (g) wt (g) Monomeric Total sugar wt (g) Monomeric Total sugar wt (g)
43.80 1295.4 57.32 1138.4 43.41 50.10 305.0 0.85 0.98 4.0 112.6 23.93.94 116.5 0.00 0.0 9.74 10.50 63.9 0.44 0.47 2.0 66.1 56.51.02 30.2 0.00 0.0 4.07 4.69 28.6 0.19 0.22 0.9 97.6 97.6
14.85 447.1 2.07 37.0 44.28 44.69 272.1 1.64 1.66 6.8 83.1 62.40.61 18.4 0.00 0.0 2.30 1.53 9.3 0.00 0.00 0.0 50.7 50.7
Crude protein 0.00 0.0 0.00 0.029.12 775.9 46.06 824.1 22.82 22.82 138.9 124.1 17.9
3.56 94.9 0.00 0.0 0.0 0.03.62 96.5 0.00 0.0 22.12 134.7 0.97 4.0 143.81.07 28.5 0.06 1.1 3.8
8.71 53.0 0.67 2.81.78 10.8 0.20 0.8
Furfural included in xylan component balanceHMF included in glucan component balance
GalactanXylan
AshFurfural*HMF*
Component
Arabinan
Total LigninExtractivesAcetic acid*
GlucanMannan
Water-solubles (in pressate by HPLC) RinsateFeedstock
input Water-insolublesPretreated Solids Pretreated Liquids
13
Dilute Acid Pretreated Hybrid Poplar (Pilot Scale-Sunds Reactor)• Feedstock: USDA-supplied hybrid poplar (Alexandria, MN)
– Debarked, chipped, and milled to pass 0.25 inch screen (Mitts and Merril knife mill)• Utilized Sunds reactor, with and without Pneumapress hot washing• Pretreatment conducted at less severe conditions than steam gun runs, due to apparent “over-pretreatment”
– 175 C, ~ 1.5 minute residence time in “flowthrough mode”, 0.025 g sulfuric acid/g dry feedstock, 25% insoluble solids
• Five samples sent– Separation only (no washing)– Hot water washed– Hot dilute ethanol (0.5 wt%) washed– Hot dilute NaOH (0.2 wt%) washed– Hot dilute ethanol (0.5 wt%) and NaOH (0.2 wt%) washed
• Compositional analysis and mass balance data not yet available
Biomass Refining CAFI
14
CAFI Labeling Nomenclature for Previously Sent Samples
Biomass Refining CAFI
Date Shipped Sample ID as sent Sample ID--CAFI Nomenclature Sample Description031209 CS-Mix 2-5 DALW-CSR-190C-1.5m-0.045H2SO4:Dry wt-30% solids-12/9/03-Mix 2:5 Pretreated corn stover solids -mid severity031209 CS #7 DALW-CSR-180C-1.5m-0.030H2SO4:Dry wt-25% solids-12/9/03-#7 Pretreated corn stover solids-low severityCS-040427-J DALW-CSR-180C-1.5m-0.030H2SO4:Dry wt-25% solids-4/27/04-J Pretreated and hot washed corn stover solids
MP-041004a-g DASE-POP1-190C-70s-0.02H2SO4:Dry wt-30% solids-10/4/04-N-A:G Steam Gun Pretreated Minn. Poplar solids (190 C, 70 sec)MP-041005a-g DASE-POP1-190C-120s-0.02H2SO4:Dry wt-30% solids-10/5/04-N-A:G Steam Gun Pretreated Minn. Poplar solids (190 C, 120 sec)MP-041005 h-n DASE-POP1-200C-70s-0.02H2SO4:Dry wt-30% solids-10/5/04-N-H:N Steam Gun Pretreated Minn. Poplar solids (200 C, 70 sec)MP-041006 a-g DASE-POP1-200C-120s-0.02H2SO4:Dry wt-30% solids-10/6/04-N-A:G Steam Gun Pretreated Minn. Poplar solids (200 C, 120 sec)
MP-041214 b-c DALW-CSR-175C-1.5m-0.025H2SO4:Dry wt-25% solids-12/14/04-B:C Sunds Pretreated Minn. Poplar solids -air blow-downMP-041214 e-f DALW-CSR-175C-1.5m-0.025H2SO4:Dry wt-25% solids-12/14/04-E:F Sunds Pretreated Minn. Poplar solids - hot water washMP-041214 g-i DALW-CSR-175C-1.5m-0.025H2SO4:Dry wt-25% solids-12/14/04-G:I Sunds Pretreated Minn. Poplar solids- hot washed w/ 0.5% EthanolMP-041214 k-m DALW-CSR-175C-1.5m-0.025H2SO4:Dry wt-25% solids-12/14/04-K:M Sunds Pretreated Minn. Poplar solids- hot washed w/ 0.2% NaOHMP-041214 n-p DALW-CSR-175C-1.5m-0.025H2SO4:Dry wt-25% solids-12/14/04-N:P Sunds Pretreated Minn. Poplar solids- hot washed w/ 0.5% Ethanol and
0.2% NaOH
9/20/2004
11/2/2004
12/22/2004