Rice Science ›› 2021, Vol. 28 ›› Issue (5): 501-510.DOI: 10.1016/j.rsci.2021.07.010
• Research Paper • Previous Articles Next Articles
Montipó Sheila1,2(
), Roslander Christian1, Camassola Marli2, Galbe Mats1, Wallberg Ola1
Received:2020-07-26
Accepted:2021-01-05
Online:2021-09-28
Published:2021-09-28
Montipó Sheila, Roslander Christian, Camassola Marli, Galbe Mats, Wallberg Ola. Steam Pretreatment of Rice Hulls to Release Fermentable Saccharides: An Approach to Improve Recovery of (Hemi)Cellulosic Sugars Through Multivariate Design[J]. Rice Science, 2021, 28(5): 501-510.
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| Pretreatment | Temperature (ºC) a | Time (min) a | Severity log(R′0) | Water-insoluble solid constituent (%) | Solid recovery (%) | Enzymatic hydrolysis | ||||
|---|---|---|---|---|---|---|---|---|---|---|
| Cellulose | Hemicellulose | Klason lignin b | Ash | Glucose (g/L) c | Yield (%) d | |||||
| 1 | 192 (-1) | 2.3 (-1) | 1.4 | 42.4 ± 0.1 | 5.9 ± 0.3 | 25.9 ± 0.5 | 23.3 ± 0.1 | 62.4 | 10.5 ± 0.0 | 44.9 ± 0.1 |
| 2 | 218 (+1) | 2.3 (-1) | 2.1 | 43.4 ± 0.1 | 3.4 ± 0.1 | 26.5 ± 0.4 | 26.1 ± 0.2 | 60.9 | 19.4 ± 0.0 | 81.4 ± 0.1 |
| 3 | 192 (-1) | 7.8 (+1) | 1.9 | 44.3 ± 0.1 | 4.4 ± 0.1 | 26.6 ± 0.6 | 24.6 ± 0.1 | 63.2 | 13.0 ± 0.1 | 53.4 ± 0.5 |
| 4 | 218 (+1) | 7.8 (+1) | 2.6 | 41.0 ± 0.0 | 2.9 ± 0.0 | 30.0 ± 0.1 | 26.6 ± 0.2 | 57.1 | 18.6 ± 0.1 | 82.5 ± 0.6 |
| 5 | 183 (-1.41) | 5.0 (0) | 1.6 | 43.0 ± 0.4 | 5.2 ± 0.3 | 26.0 ± 0.2 | 23.7 ± 0.1 | 65.2 | 10.5 ± 0.1 | 44.2 ± 0.5 |
| 6 | 227 (+1.41) | 5.0 (0) | 2.7 | 39.2 ± 0.1 | 2.6 ± 0.2 | 31.0 ± 0.2 | 27.1 ± 0.1 | 55.2 | 19.5 ± 0.2 | 90.3 ± 0.7 |
| 7 | 205 (0) | 1.1 (-1.41) | 1.3 | 41.4 ± 0.4 | 7.0 ± 0.2 | 25.1 ± 0.7 | 23.0 ± 0.2 | 65.0 | 10.4 ± 0.1 | 45.7 ± 0.6 |
| 8 | 205 (0) | 8.9 (+1.41) | 2.2 | 45.1 ± 0.0 | 3.4 ± 0.1 | 25.7 ± 0.0 | 25.1 ± 0.1 | 65.1 | 16.1 ± 0.3 | 64.7 ± 1.2 |
| 9 | 205 (0) | 5.0 (0) | 2.1 | 44.5 ± 0.3 | 3.6 ± 0.1 | 25.0 ± 0.2 | 24.9 ± 0.2 | 66.3 | 15.3 ± 0.1 | 62.6 ± 0.5 |
| 10 | 205 (0) | 5.0 (0) | 2.1 | 43.5 ± 1.8 | 3.5 ± 0.1 | 26.0 ± 0.3 | 25.5 ± 0.1 | 66.3 | 16.6 ± 0.1 | 69.2 ± 0.3 |
| 11 | 205 (0) | 5.0 (0) | 2.1 | 45.1 ± 0.4 | 3.5 ± 0.3 | 25.8 ± 0.5 | 25.6 ± 0.0 | 62.5 | 16.6 ± 0.0 | 67.0 ± 0.1 |
| Pretreatment | pH | Liquor constituent (g/L) | ||||||||
| Glucose | Xylose | Galactose | Arabinose | Mannose | Formic acid | Acetic acid | 5-HMF | Furfural | ||
| 1 | 1.7 | 9.7 ± 0.7 | 27.2 ± 1.8 | 2.2 ± 0.0 | 3.6 ± 0.4 | 0.5 ± 0.0 | 0.3 ± 0.0 | 2.9 ± 0.4 | 0.1 ± 0.0 | 0.4 ± 0.0 |
| 2 | 1.7 | 19.4 ± 0.9 | 29.1 ± 1.5 | 2.6 ± 0.0 | 3.4 ± 0.3 | 0.8 ± 0.0 | 0.5 ± 0.0 | 5.2 ± 0.3 | 0.8 ± 0.0 | 2.1 ± 0.0 |
| 3 | 1.7 | 15.2 ± 0.9 | 30.1 ± 1.5 | 2.5 ± 0.0 | 3.5 ± 0.3 | 0.6 ± 0.0 | 0.4 ± 0.0 | 4.7 ± 0.3 | 0.4 ± 0.0 | 1.4 ± 0.0 |
| 4 | 1.8 | 17.9 ± 0.7 | 13.6 ± 0.5 | 1.1 ± 0.0 | 2.3 ± 0.0 | 0.8 ± 0.0 | 0.6 ± 0.0 | 5.0 ± 0.2 | 1.9 ± 0.0 | 4.0 ± 0.2 |
| 5 | 1.6 | 10.0 ± 0.7 | 27.6 ± 1.5 | 1.9 ± 0.0 | 3.4 ± 0.4 | 0.5 ± 0.0 | 0.2 ± 0.0 | 3.4 ± 0.4 | 0.1 ± 0.0 | 0.6 ± 0.0 |
| 6 | 1.8 | 18.4 ± 0.8 | 11.7 ± 0.5 | 0.8 ± 0.0 | 2.2 ± 0.0 | 0.8 ± 0.0 | 0.7 ± 0.0 | 5.3 ± 0.3 | 2.2 ± 0.0 | 4.4 ± 0.2 |
| 7 | 1.9 | 2.9 ± 0.0 | 15.8 ± 0.6 | 0.4 ± 0.0 | 1.7 ± 0.0 | 0.0 ± 0.0 | 0.2 ± 0.0 | 1.4 ± 0.0 | 0.1 ± 0.0 | 0.2 ± 0.0 |
| 8 | 1.8 | 13.2 ± 0.4 | 19.7 ± 0.6 | 1.7 ± 0.0 | 2.4 ± 0.0 | 0.7 ± 0.0 | 0.4 ± 0.0 | 4.1 ± 0.2 | 0.7 ± 0.0 | 2.4 ± 0.0 |
| 9 | 1.7 | 9.3 ± 2.8 | 27.8 ± 7.9 | 2.1 ± 0.7 | 3.1 ± 1.0 | 0.6 ± 0.0 | 0.4 ± 0.2 | 4.4 ± 1.4 | 0.3 ± 0.0 | 1.4 ± 0.4 |
| 10 | 1.7 | 13.7 ± 3.7 | 28.9 ± 7.6 | 2.4 ± 0.7 | 3.4 ± 1.0 | 0.7 ± 0.0 | 0.4 ± 0.2 | 5.0 ± 1.3 | 0.5 ± 0.0 | 1.9 ± 0.3 |
| 11 | 1.7 | 13.2 ± 0.9 | 30.4 ± 1.7 | 2.6 ± 0.3 | 3.5 ± 0.3 | 0.8 ± 0.0 | 0.4 ± 0.0 | 5.0 ± 0.3 | 0.5 ± 0.0 | 1.6 ± 0.0 |
Table 1 Rice hull compositions obtained after SO2-catalyzed steam pretreatments.
| Pretreatment | Temperature (ºC) a | Time (min) a | Severity log(R′0) | Water-insoluble solid constituent (%) | Solid recovery (%) | Enzymatic hydrolysis | ||||
|---|---|---|---|---|---|---|---|---|---|---|
| Cellulose | Hemicellulose | Klason lignin b | Ash | Glucose (g/L) c | Yield (%) d | |||||
| 1 | 192 (-1) | 2.3 (-1) | 1.4 | 42.4 ± 0.1 | 5.9 ± 0.3 | 25.9 ± 0.5 | 23.3 ± 0.1 | 62.4 | 10.5 ± 0.0 | 44.9 ± 0.1 |
| 2 | 218 (+1) | 2.3 (-1) | 2.1 | 43.4 ± 0.1 | 3.4 ± 0.1 | 26.5 ± 0.4 | 26.1 ± 0.2 | 60.9 | 19.4 ± 0.0 | 81.4 ± 0.1 |
| 3 | 192 (-1) | 7.8 (+1) | 1.9 | 44.3 ± 0.1 | 4.4 ± 0.1 | 26.6 ± 0.6 | 24.6 ± 0.1 | 63.2 | 13.0 ± 0.1 | 53.4 ± 0.5 |
| 4 | 218 (+1) | 7.8 (+1) | 2.6 | 41.0 ± 0.0 | 2.9 ± 0.0 | 30.0 ± 0.1 | 26.6 ± 0.2 | 57.1 | 18.6 ± 0.1 | 82.5 ± 0.6 |
| 5 | 183 (-1.41) | 5.0 (0) | 1.6 | 43.0 ± 0.4 | 5.2 ± 0.3 | 26.0 ± 0.2 | 23.7 ± 0.1 | 65.2 | 10.5 ± 0.1 | 44.2 ± 0.5 |
| 6 | 227 (+1.41) | 5.0 (0) | 2.7 | 39.2 ± 0.1 | 2.6 ± 0.2 | 31.0 ± 0.2 | 27.1 ± 0.1 | 55.2 | 19.5 ± 0.2 | 90.3 ± 0.7 |
| 7 | 205 (0) | 1.1 (-1.41) | 1.3 | 41.4 ± 0.4 | 7.0 ± 0.2 | 25.1 ± 0.7 | 23.0 ± 0.2 | 65.0 | 10.4 ± 0.1 | 45.7 ± 0.6 |
| 8 | 205 (0) | 8.9 (+1.41) | 2.2 | 45.1 ± 0.0 | 3.4 ± 0.1 | 25.7 ± 0.0 | 25.1 ± 0.1 | 65.1 | 16.1 ± 0.3 | 64.7 ± 1.2 |
| 9 | 205 (0) | 5.0 (0) | 2.1 | 44.5 ± 0.3 | 3.6 ± 0.1 | 25.0 ± 0.2 | 24.9 ± 0.2 | 66.3 | 15.3 ± 0.1 | 62.6 ± 0.5 |
| 10 | 205 (0) | 5.0 (0) | 2.1 | 43.5 ± 1.8 | 3.5 ± 0.1 | 26.0 ± 0.3 | 25.5 ± 0.1 | 66.3 | 16.6 ± 0.1 | 69.2 ± 0.3 |
| 11 | 205 (0) | 5.0 (0) | 2.1 | 45.1 ± 0.4 | 3.5 ± 0.3 | 25.8 ± 0.5 | 25.6 ± 0.0 | 62.5 | 16.6 ± 0.0 | 67.0 ± 0.1 |
| Pretreatment | pH | Liquor constituent (g/L) | ||||||||
| Glucose | Xylose | Galactose | Arabinose | Mannose | Formic acid | Acetic acid | 5-HMF | Furfural | ||
| 1 | 1.7 | 9.7 ± 0.7 | 27.2 ± 1.8 | 2.2 ± 0.0 | 3.6 ± 0.4 | 0.5 ± 0.0 | 0.3 ± 0.0 | 2.9 ± 0.4 | 0.1 ± 0.0 | 0.4 ± 0.0 |
| 2 | 1.7 | 19.4 ± 0.9 | 29.1 ± 1.5 | 2.6 ± 0.0 | 3.4 ± 0.3 | 0.8 ± 0.0 | 0.5 ± 0.0 | 5.2 ± 0.3 | 0.8 ± 0.0 | 2.1 ± 0.0 |
| 3 | 1.7 | 15.2 ± 0.9 | 30.1 ± 1.5 | 2.5 ± 0.0 | 3.5 ± 0.3 | 0.6 ± 0.0 | 0.4 ± 0.0 | 4.7 ± 0.3 | 0.4 ± 0.0 | 1.4 ± 0.0 |
| 4 | 1.8 | 17.9 ± 0.7 | 13.6 ± 0.5 | 1.1 ± 0.0 | 2.3 ± 0.0 | 0.8 ± 0.0 | 0.6 ± 0.0 | 5.0 ± 0.2 | 1.9 ± 0.0 | 4.0 ± 0.2 |
| 5 | 1.6 | 10.0 ± 0.7 | 27.6 ± 1.5 | 1.9 ± 0.0 | 3.4 ± 0.4 | 0.5 ± 0.0 | 0.2 ± 0.0 | 3.4 ± 0.4 | 0.1 ± 0.0 | 0.6 ± 0.0 |
| 6 | 1.8 | 18.4 ± 0.8 | 11.7 ± 0.5 | 0.8 ± 0.0 | 2.2 ± 0.0 | 0.8 ± 0.0 | 0.7 ± 0.0 | 5.3 ± 0.3 | 2.2 ± 0.0 | 4.4 ± 0.2 |
| 7 | 1.9 | 2.9 ± 0.0 | 15.8 ± 0.6 | 0.4 ± 0.0 | 1.7 ± 0.0 | 0.0 ± 0.0 | 0.2 ± 0.0 | 1.4 ± 0.0 | 0.1 ± 0.0 | 0.2 ± 0.0 |
| 8 | 1.8 | 13.2 ± 0.4 | 19.7 ± 0.6 | 1.7 ± 0.0 | 2.4 ± 0.0 | 0.7 ± 0.0 | 0.4 ± 0.0 | 4.1 ± 0.2 | 0.7 ± 0.0 | 2.4 ± 0.0 |
| 9 | 1.7 | 9.3 ± 2.8 | 27.8 ± 7.9 | 2.1 ± 0.7 | 3.1 ± 1.0 | 0.6 ± 0.0 | 0.4 ± 0.2 | 4.4 ± 1.4 | 0.3 ± 0.0 | 1.4 ± 0.4 |
| 10 | 1.7 | 13.7 ± 3.7 | 28.9 ± 7.6 | 2.4 ± 0.7 | 3.4 ± 1.0 | 0.7 ± 0.0 | 0.4 ± 0.2 | 5.0 ± 1.3 | 0.5 ± 0.0 | 1.9 ± 0.3 |
| 11 | 1.7 | 13.2 ± 0.9 | 30.4 ± 1.7 | 2.6 ± 0.3 | 3.5 ± 0.3 | 0.8 ± 0.0 | 0.4 ± 0.0 | 5.0 ± 0.3 | 0.5 ± 0.0 | 1.6 ± 0.0 |
Fig. 1. Sugar recovery yields obtained using different catalyzed steam explosion conditions.GR-LIQ, Glucan recovery in the liquor; GR-WIS, Glucan recovery in the solid fraction; XR-LIQ, Xylan recovery in the liquor; XR-WIS, Xylan recovery in the solid fraction. 1?11 represent the pretreatment assays at 192 ºC for 2.3 min, 218 ºC for 2.3 min, 192 ºC for 7.8 min, 218 ºC for 7.8 min, 183 ºC for 5.0 min, 227 ºC for 5.0 min, 205 ºC for 1.1 min, 205 ºC for 8.9 min, 205 ºC for 5.0 min, 205 ºC for 5.0 min, 205 ºC for 5.0 min, respectively.
Fig. 2. Overall sugar yields from catalyzed steam pretreatment followed by enzymatic hydrolysis of solid fraction.G-WIS, Glucose in the solid fraction; X-LIQ, Xylose in the liquor; G-LIQ, Glucose in the liquor; X-WIS, Xylose in the solid fraction. 1?11 represent the pretreatment assays at 192 ºC for 2.3 min, 218 ºC for 2.3 min, 192 ºC for 7.8 min, 218 ºC for 7.8 min, 183 ºC for 5.0 min, 227 ºC for 5.0 min, 205 ºC for 1.1 min, 205 ºC for 8.9 min, 205 ºC for 5.0 min, 205 ºC for 5.0 min, 205 ºC for 5.0 min, respectively.
Fig. 3. Pareto chart of standardized effects for rice hulls in terms of temperature (T) and time (t) for overall yield responses of glucose released in solid fraction (A) and xylose released in liquor (B). L, Linear variable; Q, Quadratic variable.
Fig. 4. Response surface method and contour curves.A, Response surface method using the desirability function to maximize yields in a single-step.B and C, Contour curves comprising the interactions between temperature and time for overall yields of glucose released in the solid fraction (B) and xylose released in the liquor after hydrolysis (C).
| Overall sugar yield | SV | SS | df | MS | F | F value | P value | R2 |
|---|---|---|---|---|---|---|---|---|
| Overall sugar yield | ||||||||
| G-WIS | Regression | 1 092.202 | 1 | 1 092.202 | 62.806 | F1, 9; 0.05 = 5.12 | < 0.0001 | 0.87466 |
| Error | 156.509 | 9 | 17.390 | |||||
| Total | 1 248.711 | 10 | ||||||
| X-LIQ | Regression | 1 402.769 | 2 | 701.385 | 25.595 | F2, 8; 0.05 = 4.46 | < 0.0001 | 0.86485 |
| Error | 219.223 | 8 | 27.403 | |||||
| Total | 1 621.992 | 10 | ||||||
| Sugar production | ||||||||
| Glucose | Regression | 1 587.981 | 2 | 793.991 | 138.455 | F2, 8; 0.05 = 4.46 | < 0.0001 | 0.97192 |
| Error | 45.877 | 8 | 5.734 | |||||
| Total | 1 633.858 | 10 | ||||||
Table S1 Analysis of variance for the overall sugar yields after pretreatment and for enzymatic saccharification.
| Overall sugar yield | SV | SS | df | MS | F | F value | P value | R2 |
|---|---|---|---|---|---|---|---|---|
| Overall sugar yield | ||||||||
| G-WIS | Regression | 1 092.202 | 1 | 1 092.202 | 62.806 | F1, 9; 0.05 = 5.12 | < 0.0001 | 0.87466 |
| Error | 156.509 | 9 | 17.390 | |||||
| Total | 1 248.711 | 10 | ||||||
| X-LIQ | Regression | 1 402.769 | 2 | 701.385 | 25.595 | F2, 8; 0.05 = 4.46 | < 0.0001 | 0.86485 |
| Error | 219.223 | 8 | 27.403 | |||||
| Total | 1 621.992 | 10 | ||||||
| Sugar production | ||||||||
| Glucose | Regression | 1 587.981 | 2 | 793.991 | 138.455 | F2, 8; 0.05 = 4.46 | < 0.0001 | 0.97192 |
| Error | 45.877 | 8 | 5.734 | |||||
| Total | 1 633.858 | 10 | ||||||
Fig. 5. Time course of glucose concentration (A) and yields (B and C) obtained after 96 h of enzymatic hydrolysis at different solid loadings and enzyme dosages.1, 13.5% water-insoluble solids (WIS) and 15.0 filter paper units (FPU)/g; 2, 20.5% WIS and 15.0 FPU/g; 3, 13.5% WIS and 25.0 FPU/g; 4, 20.5% WIS and 25.0 FPU/g; 5, 12.0% WIS and 20.0 FPU/g; 6, 22.0% WIS and 20.0 FPU/g; 7, 17.0% WIS and 13.0 FPU/g; 8, 17.0% WIS and 27.0 FPU/g; 9, 17.0% WIS and 20.0 FPU/g; 10, 17.0% WIS and 20.0 FPU/g; 11, 17.0% WIS and 20.0 FPU/g; 12, 17.0% WIS and 20.0 FPU/g.
Fig. S1. Chromatograms obtained from different treatment samples.A, Sample of standard solution of cellobiose, glucose, xylose, galactose, arabinose and mannose.B, Sample of pretreated biomass (pretreatment 2) and hydrolyzed with 5% solids load, 15 FPU/g, diluted three times in water. C, Sample of liquor resulting from pretreatment 2, diluted three times in water.1, Cellobiose; 2, Glucose; 3, Xylose; 4, Galactose; 5, Arabinose; 6, Mannose.
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