稀硫酸预处理对杂交狼尾草木质纤维素化学组分和表征结构的影响

doi:10.3864/j.issn.0578-1752.2020.21.019

Abstract

Abstract:

【Objective】 Study the effects of H₂SO₄ concentration, solid-liquid ratio, treatment time and temperature on lignocellulose degradation efficiency of hybrid pennisetum under dilute sulfuric acid pretreatment, analyze the mechanism of dilute sulfuric acid on lignocellulose degradation, and screen the best pretreatment process.【Method】 Four single factors: H₂SO₄ concentration (0.5%, 1.0%, 1.5%, 2.0%, 2.5%), solid-liquid ratio (1﹕6, 1﹕8, 1﹕10, 1﹕12, 1﹕14), time (15, 30, 45, 60, 90 min) and temperature (80, 100, 110, 120, 125℃) were tested. Five levels of each factor were selected and repeated three times to analyze the effects of single factor on solid decomposition rate, cellulose degradation rate, hemicellulose degradation rate, lignin removal rate and hydrolyzed sugar. On the basis of single factor experiment, L₈ (2⁴) orthogonal test with 4 factors and 2 levels was used to determine the main influencing factors, and SEM and XRD analysis were carried out for the hybrid pennisetum under the optimal processing conditions. 【Result】 The results of single factor test showed that the degradation rate of hemicellulose was higher than that of lignin under all factors. With the increase of H₂SO₄concentration, the degradation rate of cellulose and hemicellulose increased, and the lignin removal rate decreased; the yield of glucose produced by cellulose hydrolysis increased with the increase of concentration, but the content of xylose decreased gradually. The low concentration of H₂SO₄ (0.5%-1.5%) promoted the degradation and digestion of solid substances of hybrid pennisetum, increased concentration (>1.5%) further did not significantly change the solid degradation. The influence of solid-liquid ratio on each index was small,and when the solid-liquid ratio increased to 1﹕10, the solid decomposition rate, hemicellulose and lignin removal reached the maximum. The pretreatment time had no obvious effect on solid decomposition rate, hemicellulose and lignin degradation, but promoted hemicellulose degradation and glucose production. Temperature has obvious effects on solid decomposition rate, degradation of cellulose, hemicellulose and lignin, and yield of hydrolyzed sugar, and 100℃ is an important critical value, and effective degradation of lignocellulose need temperature above 100℃. The orthogonal test results showed that the factors affecting hemicellulose degradation were temperature - concentration - time - solid - liquid ratio. After pretreatment with dilute sulfuric acid, the structure of lignocellulose collapsed, non-cellulose was removed, cellulose bundles were exposed (SEM), and the degree of crystallization and polymerization of cellulose was increased (XRD). 【Conclusion】 Hemicellulose was mainly degraded by dilute sulfuric acid pretreatment, but lignin was poorly degraded. Temperature is the most important factor, followed by H₂SO₄ concentration. Under the influence of four factors, the optimum technological conditions are as follows: concentration 1.5%, solid-liquid ratio 1﹕6, time 15 min, temperature 120℃.

Key words: hybrid pennisetum, lignocellulose, dilute sulfuric acid pretreatment, optimal conditions

GAO FengQin,JING YuanYuan,DE Ying,WAN QiHao,LIU YingHao, . Effects of Dilute Sulfuric Acid Pretreatment on Chemical Composition and Characterization Structure of Hybrid Pennisetum (Pennisetum americanum×P.purpureum) Lignocellulose[J].Scientia Agricultura Sinica, 2020, 53(21): 4516-4526.

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References 37

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实验序号 Experiment No.	浓度 Concentration (%)	固液比 Solid-liquid ratio (g·mL^-1)	时间 Time (min)	温度 Temperature (℃)
1	1 (1.0)	1 (1﹕6)	1 (15)	1 (110)
2	1	1	1	2 (120)
3	1	2 (1﹕8)	2 (30)	1
4	1	2	2	2
5	2 (1.5)	1	2	1
6	2	1	2	2
7	2	2	1	1
8	2	2	1	2

项目Item	含量Content (%)
纤维素 Cellulose	35.57
半纤维素 Hemicellulose	27.65
木质素Lignin	11.23
中性洗涤纤维 Neutral detergent fiber, NDF	48.36
酸性洗涤纤维 Acid detergent fiber, ADF	76.45
粗灰分Ash	3.70
干物质Dry matter	95.20

浓度 Concentration (%)	葡萄糖 Glucose (g·L^-1)	固液比 Solid-liquid ratio (g·mL^-1)	葡萄糖 Glucose (g·L^-1)	时间 Time (min)	葡萄糖 Glucose (g·L^-1)	温度 Temperature (℃)	葡萄糖 Glucose (g·L^-1)
0.5	0.77±0.03e	1﹕06	4.54±0.47a	15	1.98±0.09c	80	0.34±0.01e
1.0	2.04±0.16d	1﹕08	3.93±0.06b	30	2.56±0.40bc	100	0.96±0.05d
1.5	3.36±0.22c	1﹕10	3.36±0.22c	45	2.83±0.09bc	110	1.82±0.08c
2.0	3.72±0.25b	1﹕12	3.31±0.31cd	60	3.92±0.20ab	120	3.36±0.22b
2.5	4.26±0.22a	1﹕14	2.82±0.04d	90	4.68±0.22a	125	3.70±0.13a
浓度 Concentration (%)	木糖 Xylose (g·L^-1)	固液比 Solid-liquid ratio (g·mL^-1)	木糖 Xylose (g·L^-1)	时间 Time (min)	木糖 Xylose (g·L^-1)	温度 Temperature (℃)	木糖 Xylose (g·L^-1)
0.5	15.78±0.33a	1﹕06	13.23±0.22c	15	15.78±0.63a	80	19.80±0.21a
1.0	15.18±0.20a	1﹕08	15.66±0.76a	30	15.60±1.57a	100	16.50±0.36b
1.5	13.52±0.48b	1﹕10	14.81±0.25b	45	15.05±0.42a	110	16.33±0.33b
2.0	13.19±0.42b	1﹕12	14.44±0.22b	60	15.22±0.40a	120	13.98±0.65c
2.5	13.16±0.66b	1﹕14	14.35±0.43b	90	13.31±0.49b	125	13.47±0.37c

编号 Experiment No.		因子Factors				纤维素保留率Cellulose residual (%)	半纤维素降解率Himcellulose degradation (%)
编号 Experiment No.		浓度 Concentration (%)	固液比 Solid-liquid ratio (g·mL^-1)	时间 Time (min)	温度 Temperature (℃)	纤维素保留率Cellulose residual (%)	半纤维素降解率Himcellulose degradation (%)
1		1 (1.0)	1 (1﹕6)	1 (15)	1 (110)	93.38	58.12
2			1 (1﹕6)	1 (15)	2 (120)	93.77	65.50
3			2 (1﹕8)	2 (30)	1 (110)	98.46	63.11
4			2 (1﹕8)	2 (30)	2 (120)	93.80	80.78
5		2 (1.5)	1 (1﹕6)	2 (30)	1 (110)	99.96	71.13
6			1 (1﹕6)	2 (30)	2 (120)	92.95	85.74
7			2 (1﹕8)	1 (15)	1 (110)	91.15	67.15
8			2 (1﹕8)	1 (15)	2 (120)	91.05	85.73
纤维素保留率Cellulose residual (%)	K1	379.40	380.06	369.34	382.94	∑=754.51
	K2	375.11	374.45	385.17	371.57
	K1	94.85	95.01	92.33	95.74
	K2	93.78	93.61	96.29	92.89
R		1.07	1.40	3.96	2.84
半纤维素降解率Himcellulose degradation (%)	K1	267.51	280.48	276.50	259.51	∑=577.25
	K2	309.74	296.77	300.76	317.74
	K1	66.88	70.12	69.12	64.88
	K2	77.44	74.19	75.19	79.44
R		10.56	4.07	6.07	14.56

Effects of Dilute Sulfuric Acid Pretreatment on Chemical Composition and Characterization Structure of Hybrid Pennisetum (Pennisetum americanum×P.purpureum) Lignocellulose

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	浓度 Concentration (%)	固液比 Solid-liquid ratio (g·mL^-1)	时间 Time (min)	温度 Temperature (℃)
单因素水平 Levels of single factor	0.5	1﹕6	15	80
	1.0	1﹕8	30	100
	1.5	1﹕10	45	110
	2.0	1﹕12	60	120
	2.5	1﹕14	90	125
固定因子 Fixed factors	1﹕8 g·mL^-1 30 min 120℃	2.0% 30 min 120℃	2.0% 1﹕8 g·mL^-1 120℃	2.0% 1﹕8 g·mL^-1 30 min