Rice Science ›› 2019, Vol. 26 ›› Issue (5): 319-330.DOI: 10.1016/j.rsci.2019.08.006
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B. Pedroso Giovanni, R. Philippsen Michael, F. Saldanha Loisleini, B. Araujo Raiara, F. Martins Ayrton()
Received:
2018-08-15
Accepted:
2018-10-29
Online:
2019-09-28
Published:
2019-05-24
B. Pedroso Giovanni, R. Philippsen Michael, F. Saldanha Loisleini, B. Araujo Raiara, F. Martins Ayrton. Strategies for Fermentable Sugar Production by Using Pressurized Acid Hydrolysis for Rice Husks[J]. Rice Science, 2019, 26(5): 319-330.
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Acid | Factor | Level | ||||
---|---|---|---|---|---|---|
-1.68 | -1 | 0 | 1 | 1.68 | ||
HCl | Concentration (%) | 0.8 | 1.5 | 2.5 | 3.5 | 4.2 |
Time (min) | 28 | 35 | 45 | 55 | 62 | |
Temperature (ºC) | 128 | 135 | 145 | 155 | 162 | |
H2SO4 | Concentration (%) | 0.8 | 1.5 | 2.5 | 3.5 | 4.2 |
Time (min) | 28 | 35 | 45 | 55 | 62 | |
Temperature (ºC) | 128 | 135 | 145 | 155 | 162 | |
H3PO4 | Concentration (%) | 0.9 | 1.9 | 3.4 | 4.9 | 6 |
Time (min) | 28 | 35 | 45 | 55 | 62 | |
Temperature (ºC) | 128 | 135 | 145 | 155 | 162 | |
HNO3 | Concentration (%) | 0.6 | 1.4 | 2.6 | 3.8 | 4.5 |
Time (min) | 28 | 35 | 45 | 55 | 62 | |
Temperature (ºC) | 128 | 135 | 145 | 155 | 162 |
Table 1 Central composite rotational design values for yield determination of glucose, xylose and arabinose through acid hydrolysis of rice husks.
Acid | Factor | Level | ||||
---|---|---|---|---|---|---|
-1.68 | -1 | 0 | 1 | 1.68 | ||
HCl | Concentration (%) | 0.8 | 1.5 | 2.5 | 3.5 | 4.2 |
Time (min) | 28 | 35 | 45 | 55 | 62 | |
Temperature (ºC) | 128 | 135 | 145 | 155 | 162 | |
H2SO4 | Concentration (%) | 0.8 | 1.5 | 2.5 | 3.5 | 4.2 |
Time (min) | 28 | 35 | 45 | 55 | 62 | |
Temperature (ºC) | 128 | 135 | 145 | 155 | 162 | |
H3PO4 | Concentration (%) | 0.9 | 1.9 | 3.4 | 4.9 | 6 |
Time (min) | 28 | 35 | 45 | 55 | 62 | |
Temperature (ºC) | 128 | 135 | 145 | 155 | 162 | |
HNO3 | Concentration (%) | 0.6 | 1.4 | 2.6 | 3.8 | 4.5 |
Time (min) | 28 | 35 | 45 | 55 | 62 | |
Temperature (ºC) | 128 | 135 | 145 | 155 | 162 |
Factor | Level | ||
---|---|---|---|
-1 | 0 | 1 | |
Concentration (%) | 1 | 2.5 | 4 |
Temperature (ºC) | 40 | 60 | 80 |
Table 2 Factorial design for the best detoxification conditions of rice husk hydrolysates.
Factor | Level | ||
---|---|---|---|
-1 | 0 | 1 | |
Concentration (%) | 1 | 2.5 | 4 |
Temperature (ºC) | 40 | 60 | 80 |
Analyst | Time (min) a | Regression equation | Linear range (g/L) | r2 | LOD | LOQ |
---|---|---|---|---|---|---|
Glucose | 11.3 | y = 322.15x + 1646.41 | 0.25-2.00 | 0.999 | 7 | 23 |
Xylose | 12.2 | y = 312.35x - 152.25 | 0.25-2.00 | 0.999 | 7.5 | 25 |
Arabinose | 13.4 | y = 324.30x - 704.10 | 0.25-2.00 | 0.998 | 7 | 23 |
Fructose | 12.6 | y = 334.87x - 2345.60 | 0.25-2.00 | 0.999 | 7.5 | 25 |
Rhamnose | 12.8 | y = 302.34x - 2976.68 | 0.25-2.00 | 0.999 | 7.5 | 25 |
Formic acid | 16.8 | y = 99.79x - 1707.91 | 0.50-1.00 | 0.999 | 16.5 | 55 |
Acetic acid | 18.2 | y = 128.54x - 1642.79 | 0.50-1.00 | 0.999 | 16.5 | 55 |
Table 3 Analytical figure-of-merit for the high performance liquid chromatography coupled to a refractive index detector (HPLC-RID) determinations.
Analyst | Time (min) a | Regression equation | Linear range (g/L) | r2 | LOD | LOQ |
---|---|---|---|---|---|---|
Glucose | 11.3 | y = 322.15x + 1646.41 | 0.25-2.00 | 0.999 | 7 | 23 |
Xylose | 12.2 | y = 312.35x - 152.25 | 0.25-2.00 | 0.999 | 7.5 | 25 |
Arabinose | 13.4 | y = 324.30x - 704.10 | 0.25-2.00 | 0.998 | 7 | 23 |
Fructose | 12.6 | y = 334.87x - 2345.60 | 0.25-2.00 | 0.999 | 7.5 | 25 |
Rhamnose | 12.8 | y = 302.34x - 2976.68 | 0.25-2.00 | 0.999 | 7.5 | 25 |
Formic acid | 16.8 | y = 99.79x - 1707.91 | 0.50-1.00 | 0.999 | 16.5 | 55 |
Acetic acid | 18.2 | y = 128.54x - 1642.79 | 0.50-1.00 | 0.999 | 16.5 | 55 |
Component | Hydrolysis products and subproducts (%) | |||
---|---|---|---|---|
Natural RH | Heat block | Stove | Microwave | |
Glucose | 35.7 | 17.2 | 22.7 | 27.3 |
Xylose | 14.8 | 2.3 | 13.6 | 14.3 |
Arabinose | 3.6 | 0.7 | 3.3 | 2.9 |
Soluble lignin | 4.2 | 0.1 | 0.2 | 0.1 |
Insoluble lignin | 23.7 | 49.7 | 31.7 | 26.2 |
Extractive | 1 | 0 | 0 | 0 |
Ash | 17.2 | 30.5 | 28.8 | 29.6 |
Total | 100.2 | 100.5 | 100.3 | 100.4 |
Table 4 Characterization of rice husk (RH) and resulting hydrolysis products and sub-products.
Component | Hydrolysis products and subproducts (%) | |||
---|---|---|---|---|
Natural RH | Heat block | Stove | Microwave | |
Glucose | 35.7 | 17.2 | 22.7 | 27.3 |
Xylose | 14.8 | 2.3 | 13.6 | 14.3 |
Arabinose | 3.6 | 0.7 | 3.3 | 2.9 |
Soluble lignin | 4.2 | 0.1 | 0.2 | 0.1 |
Insoluble lignin | 23.7 | 49.7 | 31.7 | 26.2 |
Extractive | 1 | 0 | 0 | 0 |
Ash | 17.2 | 30.5 | 28.8 | 29.6 |
Total | 100.2 | 100.5 | 100.3 | 100.4 |
Acid | Sugar | P value | R² | Adjusted R² | Mean | P- | Polynomial equation a |
---|---|---|---|---|---|---|---|
SE | value | ||||||
Phosphoric | Glucose | < 0.005 | 0.83 | 0.774 | 0.128 | 0.956 | y = 0.992 + 0.419x1 - 0.092x12 + 0.133x1x3 - 0.075x2x3 |
Xylose | < 0.005 | 0.902 | 0.827 | 0.246 | 0.082 | y = 10.890 + 2.502x1 - 1.314x12 + 0.749x2 + 0.387x3 - 0.349x32 - 2.901x1x3 - 0.805x2x3 | |
Arabinose | > 0.005 | 0.445 | 0.256 | 0.003 | 0.009 | y = 1.120 + 0.052x1 - 0.038x2 + 0.088x3 - 0.070x1x3 | |
Nitric | Glucose | < 0.005 | 0.894 | 0.812 | 0.035 | 0.903 | y = 1.327 + 0.191x12 - 0.091x22 + 0.127x3 + 0.152x32 - 0.062x1x2 + 0.066x1x3 + 0.057x2x3 |
Xylose | < 0.005 | 0.977 | 0.963 | 0.188 | 0.656 | y = 10.56 - 0.269x1 - 0.305x2 - 0.264x22 - 1.894x3 - 0.782x32 - 1.159x1x3 | |
Arabinose | < 0.005 | 0.854 | 0.788 | 0.031 | 0.666 | y = 1.003 - 0.114x1 - 0.113x2 - 0.304x3 + 0.074x32 - 0.782x1x3 + 0.087x2x3 | |
Hydrochloric | Glucose | < 0.005 | 0.898 | 0.838 | 0.422 | 0.162 | y = 4.310 + 1.628x1 + 0.788x2 + 2.395x3 + 0.991x32 + 1.544x1x2 - 1.520x2x3 |
Xylose | < 0.005 | 0.964 | 0.936 | 0.935 | 0.394 | y = 9.158 - 3.117x1 - 1.111x2 - 0.705x22 - 3.205x3 - 1.183x32 - 2.256x1x2 - 1.874x2x3 | |
Arabinose | < 0.005 | 0.808 | 0.692 | 0.069 | 0.378 | y = 1.804 - 0.330x1 - 0.186x12 - 0.248x22 - 0.420x3 - 0.193x32 - 0.212x1x2 | |
Sulfuric | Glucose | < 0.005 | 0.976 | 0.963 | 0.587 | 0.716 | y = 3.373 + 1.176x1 + 0.598x2 + 3.075x3 + 1.232x32 + 0.900x1x3 - 0.795x2x3 |
Xylose | < 0.005 | 0.926 | 0.882 | 1.383 | 0.473 | y = 10.218 - 1.811x1 - 0.665x12 - 3.523x3 - 1.407x32 - 0.991x1x3 - 1.262x2x3 | |
Arabinose | < 0.005 | 0.948 | 0.918 | 0.009 | 0.428 | y = 1.209 - 0.097x2 - 0.080x22 - 0.384x3 - 0.095x1x2 - 0.174x1x3 - 0.115x2x3 |
Table 5 Polynomial equations and model adjustment values for the pressurized acid hydrolysis of rice husks by ANOVA analysis.
Acid | Sugar | P value | R² | Adjusted R² | Mean | P- | Polynomial equation a |
---|---|---|---|---|---|---|---|
SE | value | ||||||
Phosphoric | Glucose | < 0.005 | 0.83 | 0.774 | 0.128 | 0.956 | y = 0.992 + 0.419x1 - 0.092x12 + 0.133x1x3 - 0.075x2x3 |
Xylose | < 0.005 | 0.902 | 0.827 | 0.246 | 0.082 | y = 10.890 + 2.502x1 - 1.314x12 + 0.749x2 + 0.387x3 - 0.349x32 - 2.901x1x3 - 0.805x2x3 | |
Arabinose | > 0.005 | 0.445 | 0.256 | 0.003 | 0.009 | y = 1.120 + 0.052x1 - 0.038x2 + 0.088x3 - 0.070x1x3 | |
Nitric | Glucose | < 0.005 | 0.894 | 0.812 | 0.035 | 0.903 | y = 1.327 + 0.191x12 - 0.091x22 + 0.127x3 + 0.152x32 - 0.062x1x2 + 0.066x1x3 + 0.057x2x3 |
Xylose | < 0.005 | 0.977 | 0.963 | 0.188 | 0.656 | y = 10.56 - 0.269x1 - 0.305x2 - 0.264x22 - 1.894x3 - 0.782x32 - 1.159x1x3 | |
Arabinose | < 0.005 | 0.854 | 0.788 | 0.031 | 0.666 | y = 1.003 - 0.114x1 - 0.113x2 - 0.304x3 + 0.074x32 - 0.782x1x3 + 0.087x2x3 | |
Hydrochloric | Glucose | < 0.005 | 0.898 | 0.838 | 0.422 | 0.162 | y = 4.310 + 1.628x1 + 0.788x2 + 2.395x3 + 0.991x32 + 1.544x1x2 - 1.520x2x3 |
Xylose | < 0.005 | 0.964 | 0.936 | 0.935 | 0.394 | y = 9.158 - 3.117x1 - 1.111x2 - 0.705x22 - 3.205x3 - 1.183x32 - 2.256x1x2 - 1.874x2x3 | |
Arabinose | < 0.005 | 0.808 | 0.692 | 0.069 | 0.378 | y = 1.804 - 0.330x1 - 0.186x12 - 0.248x22 - 0.420x3 - 0.193x32 - 0.212x1x2 | |
Sulfuric | Glucose | < 0.005 | 0.976 | 0.963 | 0.587 | 0.716 | y = 3.373 + 1.176x1 + 0.598x2 + 3.075x3 + 1.232x32 + 0.900x1x3 - 0.795x2x3 |
Xylose | < 0.005 | 0.926 | 0.882 | 1.383 | 0.473 | y = 10.218 - 1.811x1 - 0.665x12 - 3.523x3 - 1.407x32 - 0.991x1x3 - 1.262x2x3 | |
Arabinose | < 0.005 | 0.948 | 0.918 | 0.009 | 0.428 | y = 1.209 - 0.097x2 - 0.080x22 - 0.384x3 - 0.095x1x2 - 0.174x1x3 - 0.115x2x3 |
Acid | Sugar | P-value | R² | Adjusted R² | Mean SE | P- | Polynomial equation a |
---|---|---|---|---|---|---|---|
value | |||||||
Hydrochloric (Lab stove) | Glucose | < 0.005 | 0.62 | 0.504 | 0.022 | 0.069 | y = 1.092 + 0.221x1 - 0.247x12 + 0.427x2 - 0.391x32 |
Xylose | < 0.005 | 0.83 | 0.698 | 0.123 | 0.013 | y = 11.516 + 1.705x1 - 2.093x12 + 2.914x2 - 2.512x22 + 1.086x3 - 2.940x32 - 1.517x2x3 | |
Arabinose | < 0.005 | 0.781 | 0.65 | 0.025 | 0.202 | y = 1.637 + 0.173x1 - 0.159x12 + 0.342x - 0.171x22 - 0.293x32 - 0.120x1x3 | |
Sulfuric | Glucose | < 0.005 | 0.591 | 0.405 | 0.044 | 0.032 | y = 1.905 + 0.172x1 - 0.691x12 + 0.279x2 - 0.611x22 + 0.761x3 |
(Lab stove) | Xylose | < 0.005 | 0.919 | 0.857 | 0.129 | 0.026 | y = 12.86 + 1.484x1 - 2.962x12 + 2.459x2 - 3.086x22 + 1.348x3 - 3.886x32 + 1.687x2x3 |
Arabinose | < 0.005 | 0.951 | 0.922 | 0.065 | 0.864 | y = 1.913 + 0.158x1 - 0.289x12 + 0.325x2 - 0.386x22 + 0.265x3 + 0.518x32 | |
Hydrochloric (MW oven) | Glucose | < 0.005 | 0.739 | 0.621 | 0.569 | 0.185 | y = 3.562 + 0.636x2 + 0.895x22 - 0.642x3 - 0.856x32 - 2.149x1x3 |
Xylose | > 0.005 | 0.564 | 0.303 | 3.73 | 0.004 | y = 7.835 - 1.662x1 - 1.178x22 - 1.795x3 - 1.101x32 - 1.546x1x2 - 1.408x1x3 | |
Arabinose | < 0.005 | 0.634 | 0.468 | 0.136 | 0.686 | y = 1.127 - 0.218x1 - 0.222x3 - 0.137x32 + 0.235x1x2 + 0.089x1x3 | |
Sulfuric | Glucose | < 0.005 | 0.829 | 0.752 | 1.091 | 0.349 | y = 6.971 + 1.002x1 - 1.720x12 + 0.790x22 + 2.003x32 + 0.941x1x3 |
(MW oven) | Xylose | > 0.005 | 0.504 | 0.206 | 2.07 | 0.002 | y = 4.461 - 1.377x1 - 1.749x12 - 0.992x2 - 1.347x3 - 1.184x1x2 - 1.035x2x3 |
Arabinose | > 0.005 | 0.438 | 0.181 | 0.17 | 0.001 | y = 0.786 - 0.205x1 + 0.137x12 - 0.111x3 + 0.146x1x + 0.181x2x3 |
Table 6 Polynomial equations and model adjustment values for the acid hydrolysis of rice husks by ANOVA analysis in the microwave (MW) oven and laboratory (lab) stove.
Acid | Sugar | P-value | R² | Adjusted R² | Mean SE | P- | Polynomial equation a |
---|---|---|---|---|---|---|---|
value | |||||||
Hydrochloric (Lab stove) | Glucose | < 0.005 | 0.62 | 0.504 | 0.022 | 0.069 | y = 1.092 + 0.221x1 - 0.247x12 + 0.427x2 - 0.391x32 |
Xylose | < 0.005 | 0.83 | 0.698 | 0.123 | 0.013 | y = 11.516 + 1.705x1 - 2.093x12 + 2.914x2 - 2.512x22 + 1.086x3 - 2.940x32 - 1.517x2x3 | |
Arabinose | < 0.005 | 0.781 | 0.65 | 0.025 | 0.202 | y = 1.637 + 0.173x1 - 0.159x12 + 0.342x - 0.171x22 - 0.293x32 - 0.120x1x3 | |
Sulfuric | Glucose | < 0.005 | 0.591 | 0.405 | 0.044 | 0.032 | y = 1.905 + 0.172x1 - 0.691x12 + 0.279x2 - 0.611x22 + 0.761x3 |
(Lab stove) | Xylose | < 0.005 | 0.919 | 0.857 | 0.129 | 0.026 | y = 12.86 + 1.484x1 - 2.962x12 + 2.459x2 - 3.086x22 + 1.348x3 - 3.886x32 + 1.687x2x3 |
Arabinose | < 0.005 | 0.951 | 0.922 | 0.065 | 0.864 | y = 1.913 + 0.158x1 - 0.289x12 + 0.325x2 - 0.386x22 + 0.265x3 + 0.518x32 | |
Hydrochloric (MW oven) | Glucose | < 0.005 | 0.739 | 0.621 | 0.569 | 0.185 | y = 3.562 + 0.636x2 + 0.895x22 - 0.642x3 - 0.856x32 - 2.149x1x3 |
Xylose | > 0.005 | 0.564 | 0.303 | 3.73 | 0.004 | y = 7.835 - 1.662x1 - 1.178x22 - 1.795x3 - 1.101x32 - 1.546x1x2 - 1.408x1x3 | |
Arabinose | < 0.005 | 0.634 | 0.468 | 0.136 | 0.686 | y = 1.127 - 0.218x1 - 0.222x3 - 0.137x32 + 0.235x1x2 + 0.089x1x3 | |
Sulfuric | Glucose | < 0.005 | 0.829 | 0.752 | 1.091 | 0.349 | y = 6.971 + 1.002x1 - 1.720x12 + 0.790x22 + 2.003x32 + 0.941x1x3 |
(MW oven) | Xylose | > 0.005 | 0.504 | 0.206 | 2.07 | 0.002 | y = 4.461 - 1.377x1 - 1.749x12 - 0.992x2 - 1.347x3 - 1.184x1x2 - 1.035x2x3 |
Arabinose | > 0.005 | 0.438 | 0.181 | 0.17 | 0.001 | y = 0.786 - 0.205x1 + 0.137x12 - 0.111x3 + 0.146x1x + 0.181x2x3 |
Fig. 3. Example of contour surfaces showing the optimal region of glucose production. A, Hydrolysis at a higher temperature and HCl concentration. B, Hydrolysis aiming for xylose production in a less severe optimal region.
Fig. 4. Scanning electron microscopy images for rice husks.A and B are natural and residual rice husks treated by pressurized acid hydrolysis with 1.5% H2SO4 (65 min, 135 ºC), respectively.
Compound (g/L) | Untreated hydrolysate | Treated by active carbon | Treated by CaO | Treated by Ca(OH)2 |
---|---|---|---|---|
Glucose | 11.6 ± 0.4 | 10.7 ± 0.4 | 8.9 ± 0.4 | 10.4 ± 0.4 |
Xylose | 2.3 ± 0.1 | 1.7 ± 0.1 | 1.2 ± 0.1 | 1.5 ± 0.1 |
Arabinose | 0.7 ± 0.1 | 0.6 ± 0.1 | 0.5 ± 0.1 | 0.4 ± 0.1 |
Fructose | - | - | - | - |
Rhamnose | - | - | - | - |
Formic acid | 1.9 ± 0.4 | 1.5 ± 0.4 | 1.5 ± 0.4 | 1.5 ± 0.4 |
Acetic acid | 2.6 ± 0.3 | 1.8 ± 0.3 | 2.0 ± 0.3 | 1.9 ± 0.3 |
Table 7 Characterization of hydrolysates submitted to different detoxification processes.
Compound (g/L) | Untreated hydrolysate | Treated by active carbon | Treated by CaO | Treated by Ca(OH)2 |
---|---|---|---|---|
Glucose | 11.6 ± 0.4 | 10.7 ± 0.4 | 8.9 ± 0.4 | 10.4 ± 0.4 |
Xylose | 2.3 ± 0.1 | 1.7 ± 0.1 | 1.2 ± 0.1 | 1.5 ± 0.1 |
Arabinose | 0.7 ± 0.1 | 0.6 ± 0.1 | 0.5 ± 0.1 | 0.4 ± 0.1 |
Fructose | - | - | - | - |
Rhamnose | - | - | - | - |
Formic acid | 1.9 ± 0.4 | 1.5 ± 0.4 | 1.5 ± 0.4 | 1.5 ± 0.4 |
Acetic acid | 2.6 ± 0.3 | 1.8 ± 0.3 | 2.0 ± 0.3 | 1.9 ± 0.3 |
Agent | P-value | R² | Adjusted R² | Mean-square error | P value (lack of fit) | Polynomial equation a |
---|---|---|---|---|---|---|
Active carbon | < 0.005 | 0.999 | 0.996 | 0.2 | > 0.005 | y = 86.60 + 7.00x1 + 2.00x2 + 0.50x1x2 |
CaO | < 0.005 | 0.83 | 0.698 | 4.05 | > 0.005 | y = 67.80 - 1.75x1 + 13.25x2 + 1.25x1x2 |
Ca(OH)2 | < 0.005 | 0.781 | 0.65 | 0.45 | > 0.005 | y = 66.40 - 3.25x1 - 10.75x2 - 0.25x1x2 |
Table 8 Polynomial equations and model adjustment values for the rice husk hydrolysate detoxification by ANOVA analysis.
Agent | P-value | R² | Adjusted R² | Mean-square error | P value (lack of fit) | Polynomial equation a |
---|---|---|---|---|---|---|
Active carbon | < 0.005 | 0.999 | 0.996 | 0.2 | > 0.005 | y = 86.60 + 7.00x1 + 2.00x2 + 0.50x1x2 |
CaO | < 0.005 | 0.83 | 0.698 | 4.05 | > 0.005 | y = 67.80 - 1.75x1 + 13.25x2 + 1.25x1x2 |
Ca(OH)2 | < 0.005 | 0.781 | 0.65 | 0.45 | > 0.005 | y = 66.40 - 3.25x1 - 10.75x2 - 0.25x1x2 |
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