响应面法优化设计木质素基活性炭的制备

doi:10.3969/j.issn.0253-2417.2020.03.015

Abstract

Abstract:

Lignin-based activated carbon was prepared from corn cob lignin by using phosphoric acid activation method.Taking methylene blue adsorption value (MB) as the index, the interaction during the preparation of activated carbon were explored by Plackett-Burman design, the steepest climbing test, and the center composite design method.The results showed that the three most important factors obtained by Plackett-Burman design were immersion ratio, activation temperature, and activation time.The best center region was determined through the steepest climbing test.The optimal process conditions obtained by the center composite design (CCD) and response surface analysis (RSM) were impregnation ratio 3:1(g:g), activation temperature 563℃, and activation time 2.75 h. The verification experiment was performed under the above optimized process of 60% phosphoric acid mass fraction, 12 h immersion time, 90℃ immersion temperature. The pore size of the lignin-based activated carbon was mainly concentrated at 2-10 nm, the BET specific surface area was 1 436 m²/g, total pore volume was 1.041 cm³/g, the micropore pore volume was 0.385 6 cm³/g and the methylene blue adsorption value (MB)was 240 mg/g.

Key words: phosphoric acid activation, lignin, activated carbon, mesopores

CLC Number:

TQ35

Xinglong HOU,Qi GUO,Xiaopeng JIAN,Dichao WU,Wei XU,Junli LIU. Optimization of Design of Lignin-based Activated Carbon Based on Response Surface Methodology[J]. Chemistry and Industry of Forest Products, 2020, 40(3): 115-122.

Figures/Tables 8

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Fig.1

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References 26

1	迟慧智.木质素基活性炭热解活化工艺及其吸附性能研究[D].杨凌:西北农林科技大学, 2018.
	CHI H Z.Preparation and adsorption of lignin-based activated carbon in pyrolysis processing[D]. Yangling: Northwest A&F University, 2018.
2	张芝兰, 陆雍森. 木质素混凝剂的性质及其应用研究[J]. 水处理技术, 1997, (1): 40- 46.
	ZHANG Z L , LU Y S . Study of coagulation mechanism of lignin and its application[J]. Technology of Water Treatment, 1997, (1): 40- 46.
3	贾清超, 毛翠平, 武书彬. 木质素液化产物制备非离子表面活性剂的研究[J]. 造纸科学与技术, 2016, 35 (3): 28- 33, 38.
	JIA Q C , MAO C P , WU S B . Preparation of non-ionic surfactant from phenolic products of alkali lignin liquefication[J]. Paper Science and Technology, 2016, 35 (3): 28- 33, 38.
4	徐若愚, 张静, 龚方红. 酸木质素改性酚醛树脂胶粘剂的研究[J]. 林业实用技术, 2011, (11): 60- 62.
	XU R Y , ZHANG J , GONG F H . Study of acid lignin modified phenolic resin adhesive[J]. Practical Forestry Technology, 2011, (11): 60- 62.
5	张桂梅, 廖双泉, 蔺海兰, 等. 木质素的提取方法及综合利用研究进展[J]. 热带农业科学, 2005, 25 (1): 66- 70, 76. doi: 10.3969/j.issn.1009-2196.2005.01.017
	ZHANG G M , LIAO S Q , LIN H L , et al. Progress in studying the extraction and comprehensive utilization of lignin[J]. Chinese Journal of Tropical Agriculture, 2005, 25 (1): 66- 70, 76. doi: 10.3969/j.issn.1009-2196.2005.01.017
6	巨敏, 翁彩珠, 刘军海. 木质素在农业中的应用[J]. 现代农业, 2011, (1): 27- 28.
	JU M , WENG C Z , LIU J H . Application of lignin in agriculture[J]. Modern Agriculture, 2011, (1): 27- 28.
7	宋曜光, 刘军利, 许伟, 等. 模板法制备木质素基中孔炭材料研究进展[J]. 生物质化学工程, 2018, 52 (1): 64- 72. doi: 10.3969/j.issn.1673-5854.2018.01.009
	SONG Y G , LIU J L , XU W , et al. Research progress on synthesis of lignin-derived mesoporous carbon materials via template strategy[J]. Biomass Chemical Engineering, 2018, 52 (1): 60- 68. doi: 10.3969/j.issn.1673-5854.2018.01.009
8	申朋飞, 朱颖颖, 李信宝, 等. 植物基活性炭的制备及吸附应用研究进展[J]. 化工进展, 2019, 38 (8): 3763- 3773.
	SHEN P F , ZHU Y Y , LI X B , et al. Review on preparation of plant-based activated carbon and its adsorption application[J]. Chemical Industry and Engineering Progress, 2019, 38 (8): 3763- 3773.
9	于华阳, 孙国钰, 周帆, 等. 黑液木质素制备活性炭及其电化学性能研究[J]. 现代化工, 2018, 38 (3): 114- 118.
	YU H Y , SUN G Y , ZHOU F , et al. Preparation of activated carbon from black liquor lignin and characterization of its electrochemical properties[J]. Modern Chemical Industry, 2018, 38 (3): 114- 118.
10	袁康帅, 郭大亮, 张子明, 等. 碱木质素基多孔炭材料的制备及其在超级电容器中的应用[J]. 中国造纸, 2019, 38 (6): 47- 53.
	YAUN K S , GUO D L , ZHANG Z M , et al. Preparation of alkaline lignin-based porous carbon material and its application in supercapacitors[J]. China Pulp & Paper, 2019, 38 (6): 47- 53.
11	李松.膨胀石墨/活性炭用于船舶舱底水处理的研究[D].厦门:集美大学, 2016.
	LI S.Research on expansion graphite/activated carbon for bilge water treatment of ships[D]. Xiamen: Jimei University, 2016.
12	ARIYADEJWANICH P , TANTHAPANICHAKOON W , NAKAGAWA K , et al. Preparation and characterization of mesoporous activated carbon from waste tires[J]. Carbon, 2003, 41 (1): 157- 164. doi: 10.1016/S0008-6223(02)00267-1
13	SAYGǦILI H , GÜZEL F . High surface area mesoporous activated carbon from tomato processing solid waste by zinc chloride activation:Process optimization, characterization and dyes adsorption[J]. Journal of Cleaner Production, 2016, 113, 995- 1004. doi: 10.1016/j.jclepro.2015.12.055
14	DENG H , YANG L , TAO G H , et al. Preparation and characterization of activated carbon from cotton stalk by microwave assisted chemical activation-Application in methylene blue adsorption from aqueous solution[J]. Journal of Hazardous Materials, 2009, 166 (2): 1514- 1521.
15	左宋林, 刘军利, 杨建校, 等. 磷酸活化法活性炭性质对亚甲基蓝吸附能力的影响[J]. 林产化学与工业, 2010, 30 (4): 1- 6.
	ZUO S L , LIU J L , YANG J X , et al. Effects of the properties of phosphoric acid-activated carbon on adsorption capacity of methylene blue[J]. Chemistry and Industry of Forest Products, 2010, 30 (4): 1- 6.
16	左宋林, 倪传根, 高尚愚. 磷酸活化工艺条件对活性炭性质的影响[J]. 林产工业, 2005, 32 (4): 29- 31.
	ZUO S L , NI C G , GAO S Y . The effect of activation technology on the properties of activated carbon with phosphoric acid[J]. China Forest Products Industry, 2005, 32 (4): 29- 31.
17	左宋林. 磷酸活化法活性炭孔隙结构的调控机制[J]. 新型炭材料, 2018, 33 (4): 289- 302.
	ZUO S L . A review of the control of pore texture of phosphoric acid-activated carbons[J]. New Carbon Materials, 2018, 33 (4): 289- 302.
18	DAYANA PRIYADHARSHINI S , BAKTHAVATSALAM A K . Optimization of phenol degradation by the microalga Chlorella pyrenoidosa using Plackett-Burman design and response surface methodology[J]. Bioresource Technology, 2016, 207, 150- 156. doi: 10.1016/j.biortech.2016.01.138
19	REDDY L V A , WEE Y J , YUN J S , et al. Optimization of alkaline protease production by batch culture of Bacillus sp.RKY3 through Plackett-Burman and response surface methodological approaches[J]. Bioresource Technology, 2008, 99 (7): 2242- 2249. doi: 10.1016/j.biortech.2007.05.006
20	冶鹏辉, 吴专丽, 周倩, 等. PB试验和BBD响应面优化酶解鱼鳞制备抗菌肽工艺[J]. 云南化工, 2019, 46 (5): 5- 7. doi: 10.3969/j.issn.1004-275X.2019.05.002
	YE P H , WU Z L , ZHOU Q , et al. Optimization of enzymatic hydrolysis of fish scales for preparing antimicrobial peptides by Plackett-Burman and Box-Behnken[J]. Yunnan Chemical Industry, 2019, 46 (5): 5- 7. doi: 10.3969/j.issn.1004-275X.2019.05.002
21	项国梁, 喻泽斌, 陈颖, 等. 响应面法优化甘蔗渣-污泥复合活性炭的制备工艺[J]. 环境工程学报, 2014, 8 (12): 5475- 5482.
	XIAGN G L , YU Z B , CHEN Y , et al. Optimizing the preparation of sugarcane bagasse-sludge compositional activated carbon by response surface methodology[J]. Chinese Journal of Environmental Engineering, 2014, 8 (12): 5475- 5482.
22	ZHOU J Y , YU X J , DING C , et al. Optimization of phenol degradation by Candida tropicalis Z-04 using Plackett-Burman design and response surface methodology[J]. Journal of Environmental Sciences, 2011, 23 (1): 22- 30.
23	程松, 张利波, 夏洪应, 等. 响应曲面法优化CO₂活化制备夏威夷坚果壳基活性炭[J]. 环境工程学报, 2015, 9 (9): 4495- 4502.
	CHENG S , ZHANG L B , XIA H Y , et al. Preparation of activated carbon from Hawaii nut shell via CO₂ activation using response surface methodology[J]. Journal of Environmental Engineering, 2015, 9 (9): 4495- 4502.
24	MOLINA-SABIO M , RODRÍGUEZ-REINOSO F , CATURLA F , et al. Porosity in granular carbons activated with phosphoric acid[J]. Carbon, 1995, 33 (8): 1105- 1113. doi: 10.1016/0008-6223(95)00059-M
25	JAGTOYEN M , DERBYSHIRE F . Activated carbons from yellow poplar and white oak by H₃PO₄ activation[J]. Carbon, 1998, 36 (7): 1085- 1097.
26	闫伟, 张艳, 杨建华, 等. 磷酸活化草浆黑液木质素制备活性炭的研究[J]. 林产化学与工业, 2011, 31 (5): 81- 84.
	YAN W , ZHANG Y , YANG J H , et al. Preparation of activated carbon from straw black liquor lignin impregnated by phosphoric acid[J]. Chemistry and Industry of Forest Products, 2011, 31 (5): 81- 84.

序号 No.	X₁(g:g)	X₂/%	X₃/h	X₄/℃	X₅/h	X₆/℃	X₇	X₈	亚甲基蓝吸附值MB/(mg·g^-1)
序号 No.	X₁(g:g)	X₂/%	X₃/h	X₄/℃	X₅/h	X₆/℃	X₇	X₈	实验值 experimental value	预测值 predicted value
1	1:1	60	12	90	1	700	0	0	82.5	103.13
2	4:1	30	6	90	1	350	0	0	112.5	111.87
3	1:1	30	6	140	7	700	0	0	82.5	63.13
4	4:1	30	12	140	1	700	0	0	150.0	148.13
5	1:1	30	6	90	1	350	0	0	60.0	60.61
6	1:1	60	6	90	7	700	0	0	82.5	80.61
7	4:1	60	6	140	1	700	0	0	157.5	143.13
8	1:1	30	12	140	7	350	0	0	45.0	49.39
9	4:1	60	12	90	7	350	0	0	105.0	114.41
10	4:1	60	6	140	7	350	0	0	112.5	103.15
11	4:1	30	12	90	7	700	0	0	120.0	136.87
12	1:1	60	12	140	1	350	0	0	82.5	78.13

因子 factors	效应 effect	系数 coefficient	标准误差 standard error	T值 T value	P值 P value	显著性 significance
常量constant	198.76	99.38	2.13	46.55	0.000
X₁	53.76	26.88	2.13	12.59	0.001	**
X₂	8.76	4.38	2.13	2.05	0.133
X₃	11.26	5.63	2.13	2.63	0.078
X₄	-3.74	-1.87	2.13	-0.88	0.444
X₅	-16.24	-8.12	2.13	-3.81	0.032	*
X₆	26.24	13.12	2.13	6.15	0.009	**
X₇	-3.74	-1.87	2.13	-0.88	0.444
X₈	1.24	0.62	2.13	0.29	0.789

来源 source	自由度 df	平方和 SS	均方 MS	F值 F value	P值 P value	显著性 significance
模型model	8	12225.0	1528.12	27.94	0.010	*
X₁	1	8667.2	8667.19	158.49	0.001	**
X₂	1	229.7	229.69	4.20	0.133
X₃	1	379.7	379.69	6.94	0.078
X₄	1	42.2	42.19	0.77	0.444
X₅	1	792.2	792.19	14.49	0.032	*
X₆	1	2067.2	2067.19	37.80	0.009	**
X₇	1	42.2	42.19	0.77	0.444
X₈	1	4.7	4.69	0.09	0.789
误差error	3	164.1	54.69
合计total	11	12389.1

序号 No.	X₁(g:g)	X₅/h	X₆/℃	亚甲基蓝吸附值/(mg·g^-1) methylene blue adsorption
1	0.5:1	5	350	105
2	1.5:1	4	450	160
3	2.5:1	3	550	202.5
4	3.5:1	2	650	180
5	4.5:1	1	700	150

运行序号 run order	X₁(g:g)	X₅/h	X₆/℃	亚甲基蓝吸附值MB/(mg·g^-1)
运行序号 run order	X₁(g:g)	X₅/h	X₆/℃	实验值 experimental value	预测值 predicted value
1	3.0:1	3.5	575	97.5	94.88
2	2.5:1	3.0	550	210.0	207.33
3	3.5:1	3.0	550	180.0	182.96
4	2.5:1	3.0	550	105.0	106.17
5	2.5:1	3.0	550	165.0	169.81
6	3.0:1	2.5	525	180.0	179.95
7	2.5:1	3.0	550	210.0	207.33
8	2.5:1	2.0	500	202.5	204.67
9	2.5:1	3.0	550	202.5	207.33
10	2.5:1	4.0	600	165.0	168.81
11	2.5:1	3.0	550	210.0	207.33
12	1.5:1	3.0	550	120.0	123.02
13	2.0:1	3.5	575	127.5	126.73
14	2.0:1	2.5	525	120.0	118.39
15	2.5:1	3.0	550	202.5	207.33
16	3.0:1	3.5	575	202.5	200.22
17	2.0:1	3.5	575	165.0	160.83
18	2.5:1	3.0	550	210.0	207.33
19	2.0:1	2.5	525	150.0	148.05
20	3.0:1	2.5	525	225.0	221.54

Optimization of Design of Lignin-based Activated Carbon Based on Response Surface Methodology

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来源 source	自由度 df	平方和 SS	均方 MS	F值 F value	P值 P value
模型model	9	30302.23	3366.91	181.73	< 0.0001
X₁	1	4338.28	4338.28	234.16	< 0.0001
X₅	1	1551.59	1551.59	83.75	< 0.0001
X₆	1	4889.45	4889.45	263.91	< 0.0001
X₁X₅	1	2032.03	2032.03	109.68	< 0.0001
X₁X₆	1	2538.28	2538.28	137.00	< 0.0001
X₅X₆	1	2032.03	2032.03	109.68	< 0.0001
X₁²	1	5319.04	5319.04	287.09	< 0.0001
X₅²	1	763.62	763.62	41.22	< 0.0001
X₆²	1	8660.95	8660.95	467.47	< 0.0001
残差residual	10	185.27	18.53
失拟项lack of fit	5	110.27	22.05	1.47	0.3413
纯误差pure error	5	75.00	15.00
总变异cor total	19	30487.50