椰衣微波热解工艺的响应面法优化及液体产物组成分析

doi:10.3969/j.issn.1673-5854.2020.04.007

Abstract

Abstract:

The Box-Behnken experimental design was used to optimize the microwave pyrolysis process of the coconut clothes by response surface method (RSM). The effects of microwave pyrolysis temperature, nitrogen flow rate, heating rate and pyrolysis time on liquid yield were investigated. The results showed that the regression equation model fitted well and was significant. The influence order of various factors on liquid product yield was microwave pyrolysis temperature > nitrogen flow rate > pyrolysis time > heating rate. The optimum conditions were temperature 550℃, nitrogen flow rate 80 mL/min, heating rate 20℃/min and pyrolysis time 20 min. According to this process, the obtained yield of liquid product value was 38.28%. The analyses of properties and composition of liquid product showed that the water content in the liquid product was 14.32%, the pH value was 3.78, and the maximum heating value under the best pyrolysis conditions was 24.61 MJ/kg.By GC-MS analysis of bio-oil, under the optimal conditions, the liquid product was composed of phenols, aldehydes, acids, ketones and so on, and their contents were 84.35%, 6.01%, 3.37%, 2.05%. The phenols included phenol(33.51%), p-cresol(9.71%), 2-methoxyphenol(10.99%) and 4-ethyl-2-methoxyphenol(5.57%).

Key words: coconut clothes, microwave pyrolysis, liquid product, response surface method

CLC Number:

TQ35

Qiqi DAI,Xiaocui WEI,Hongbiao TANG,Jin LI,Jinjing WANG. Optimization of Microwave Assisted Pyrolysis of Coconut Clothes by Response Surface Method and Analysis of Liquid Product Composition[J]. Biomass Chemical Engineering, 2020, 54(4): 42-48.

Figures/Tables 5

Table 1

Table 2

Fig.1

Table 3

Table 4

GC-MS properties analysis of bio-oil"

编号No.	组成composition	分子式molecular formula	不同温度下GC含量/% GC content under different temperature
编号No.	组成composition	分子式molecular formula	500 ℃	550 ℃	600 ℃
1	乙酸acetic acid	C₂H₄O₂	2.49	3.37	2.65
2	3-甲醛3-furmaldehyde	C₅H₄O₂	4.65	6.01	4.95
3	3-呋喃甲醇3-furanmethanol	C₅H₆O₂	1.16	2.11	1.43
4	5-甲基-2-呋喃甲醛2-furancarboxaldehyde, 5-methyl-	C₆H₆O₂	1.17	1.07	1.04
5	苯酚phenol	C₆H₆O	26.96	33.51	27.71
6	2-甲基苯酚phenol, 2-methyl-	C₇H₈O	1.24	3.75	3.85
7	对甲酚p-cresol	C₇H₄O	2.95	9.71	10.32
8	2-甲氧基苯酚phenol, 2-methoxy-	C₇H₈O₂	3.61	10.99	9.94
9	2-甲基苯并呋喃benzofuran, 2-methyl-	C₉H₁₀O	—	—	1.12
10	3，5-二甲基苯酚phenol, 3, 5-dimethyl-	C₈H₁₀O	1.49	3.77	4.21
11	4-乙基苯酚phenol, 4-ethyl-	C₈H₁₀O	2.90	2.49	2.82
12	2, 4-二甲基苯酚phenol, 2, 4-dimethyl-	C₈H₁₀O	2.60	—	—
13	2-甲氧基-5-甲基苯酚phenol, 2-methoxy-5-methyl-	C₈H₁₀O₂	3.91	3.51	3.65
14	邻苯二酚catechol	C₆H₆O₂	2.51	3.09	3.32
15	2, 3-二氢苯并呋喃benzofuran, 2, 3-dihydro-	C₈H₁₀O	0.97	—	1.08
16	4-乙基-2-甲氧基苯酚phenol, 4-ethyl-2-methoxy-	C₉H₁₂O₂	6.66	5.57	5.93
17	1-(2-羟基-5-甲基苯基)-乙酮ethanone, 1-(2-hydroxy-5-methylphenyl)-	C₉H₁₀O₂	2.33	2.05	2.71
18	2, 6-二甲氧基苯酚phenol, 2, 6-dimet hoxy-	C₈H₁₀O₃	4.73	4.44	4.70
19	2-甲氧基-4-丙基苯酚phenol, 2-methoxy-4-propyl-	C₁₀H₁₄O₂	1.02	—	0.91
20	2, 6-二甲氧基-4-甲基苯酚phenol, 2, 6-dimethoxy-4-methyl-	C₉H₁₂O₃	1.19	—	1.14
21	反异丁香酚trans-isoeugenol	C₁₀H₁₂O₂	2.60	2.00	2.52
22	5-叔丁基邻苯三酚5-tert-butylpyrogallol	C₁₀H₁₄O₃	—	1.53	1.92
23	4-羟基-3-甲氧基苯丙酮acetone, 4-hydroxy-3-methoxy-phenyl-	C₁₀H₁₂O₃	1.36	1.04	1.46
24	2, 6-二甲氧基-4-(2-丙烯基)-苯酚phenol, 2, 6-dimethoxy-4-(2-propenyl)-	C₁₁H₁₂0₃	1.04	—	1.00
合计sum up	酮类ketones		2.33	2.05	2.71
	酸类acids		2.18	3.37	2.65
	醛类aldehydes		5.82	6.01	5.63
	酚类phenols		80.40	84.35	82.78

Table 4

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来源 source	平方和 sum of square	自由度 degree of freedom	均方 square	F值 F value	P值 P value	显著性¹⁾ significant degree
模型model	254.53	14	18.18	44.63	< 0.0001	**
X₁	175.28	1	175.28	430.30	x0.0001	**
X₂	9.26	1	9.26	22.74	0.0103	*
X₃	0.11	1	0.11	0.28	0.1723
X₄	0.24	1	0.24	0.58	0.1077
X₁X₂	2.66	1	2.66	6.52	0.0229	*
X₁X₃	1.95	1	1.95	4.78	0.0463	*
X₁X₄	2.28	1	2.28	5.6	0.0330	*
X₂X₃	0.00225	1	0.00225	0.00552	0.9816
X₂X₄	1.28	1	1.28	3.13	0.0984
X₃X₄	0.25	1	0.25	0.61	0.4464
X₁²	215.96	1	215.96	530.15	< 0.0001	**
X₂²	22.68	1	22.68	55.69	< 0.0001	**
X₃²	4.01	1	4.01	9.85	0.0073	**
X₄²	3.83	1	3.83	9.41	0.0083	**
残差residual	5.7	14	0.41
失拟项lack of fit	5.33	10	0.53	5.76	0.053
纯误差pure error	0.37	4	0.093
总和cor total	260.23	28
R²	0.9890

热解温度/℃ pyrolysis temperature	含水量/% water content	黏度/ (m²·s^-1) viscosity	pH值 pH value	元素分析elemental analysis/%					n(H)/ n(C)	平均分子式 average molecular formula	高位热值/ (MJ·kg^-1) high heating value
热解温度/℃ pyrolysis temperature	含水量/% water content	黏度/ (m²·s^-1) viscosity	pH值 pH value	C	H	O	N	S	n(H)/ n(C)	平均分子式 average molecular formula	高位热值/ (MJ·kg^-1) high heating value
500	15.21	225.8	3.86	52.27	6.90	27.90	4.42	0	1.58	CH_1.58O_0.40N_0.07	23.63
550	14.32	214.6	3.78	56.11	6.32	23.54	5.73	0	1.35	CH_1.35O_0.31N_0.0₉	24.61
600	14.02	211.0	3.80	53.96	5.95	27.66	6.21	0	1.32	CH_1.32O_0.38N_0.10	22.89

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Optimization of Microwave Assisted Pyrolysis of Coconut Clothes by Response Surface Method and Analysis of Liquid Product Composition

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序号 No.	X₁ 热解温度/℃ pyrolysis temperature	X₂ 氮气流速/(mL·min^-1) nitrogen flow rate	X₃ 升温速率/(℃·min^-1) heating rate	X₄ 热解时间/min pyrolysis time	Y 液体产物产率/% liquid yield
1	550	80	20	25	38.51
2	550	80	15	30	36.25
3	550	100	20	20	34.88
4	600	100	20	25	32.02
5	550	100	25	25	36.08
6	550	100	20	30	37.39
7	500	80	25	25	29.56
8	500	80	15	25	31.05
9	600	80	20	30	34.28
10	550	60	25	25	35.89
11	550	80	25	30	37.62
12	550	80	20	25	38.08
13	550	80	20	25	38.02
14	550	60	15	25	35.09
15	550	80	20	25	38.49
16	550	80	20	25	38.73
17	500	60	20	25	28.28
18	500	100	20	25	31.98
19	500	80	20	20	30.62
20	600	80	20	20	32.02
21	550	80	15	20	36.98
22	550	60	20	20	34.98
23	600	80	15	25	32.45
24	550	60	20	30	35.23
25	600	80	25	25	33.75
26	500	80	20	30	29.86
27	550	100	15	25	35.25
28	600	60	20	25	31.58
29	550	80	25	20	37.35