竹粉乙醇-苯酚加压液化工艺研究及产物表征

doi:10.3969/j.issn.0253-2417.2016.04.015

林产化学与工业 ›› 2016, Vol. 36 ›› Issue (4): 105-112.doi: 10.3969/j.issn.0253-2417.2016.04.015

竹粉乙醇-苯酚加压液化工艺研究及产物表征

马艳¹, 谭卫红¹, 冯国东¹, 徐俊明^1,2, 王奎¹, 应浩¹, 蒋剑春^1,2

1. 中国林业科学研究院林产化学工业研究所;生物质化学利用国家工程实验室;国家林业局林产化学工程重点开放性实验室;江苏省生物质能源与材料重点实验室, 江苏南京 210042;
2. 江苏强林生物能源材料有限公司, 江苏溧阳 213364

收稿日期:2015-07-21 出版日期:2016-08-25 发布日期:2016-09-01
通讯作者: 蒋剑春,男,研究员,博士,博士生导师,研究领域为生物质能源与炭材料;E-mail:bio-energy@163.com。 E-mail:bio-energy@163.com
作者简介:马艳(1983-),女,山东聊城人,博士生,从事生物油分离应用方面的研究;E-mail:mayan23@163.com
基金资助:
“十二五”农村领域国家科技计划课题（2014BAD02B01）

Liquefaction of Bamboo Powder in Ethanol-phenol under High Pressure and Product Characterization

MA Yan¹, TAN Wei-hong¹, FENG Guo-dong¹, XU Jun-ming^1,2, WANG Kui¹, YING Hao¹, JIANG Jian-chun^1,2

1. Institute of Chemical Industry of Forest Products, CAF;National Engineering Lab. for Biomass Chemical Utilization;Key and Open Lab. of Forest Chemical Engineering, SFA;Key Lab. of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China;
2. Jiangsu Qianglin Bio-energy and Bio-materials Co., Ltd., Liyang 213364, China

Received:2015-07-21 Online:2016-08-25 Published:2016-09-01

摘要/Abstract

摘要： 以乙醇-苯酚为液化剂，浓硫酸为催化剂，采用高温高压（3.8 MPa）的方法对竹粉进行了液化处理。通过响应面分析法确定最佳液化工艺条件为：在苯酚和竹粉质量比（酚固比）为1：1、乙醇和竹粉质量比（醇固比）为18：1，浓硫酸用量（以竹粉质量计）5%，反应温度200℃，反应时间70 min时，液化率达98.5%。液化残渣的红外光谱（FT-IR）、扫描电镜（SEM）和热重分析（TG）结果证实了竹粉中化学组分的分子结构发生了明显的变化，复合溶剂液化使芳环上有不同取代基的化合物形成，液化残渣主要由木质素及其衍生物构成；竹粉液体产物（生物质油）的GC-MS分析结果表明，生物质油的成分比较复杂，主要包括酯、酚和酮等化合物，平台化合物乙酰丙酸乙酯GC含量为10.11%。

关键词: 竹粉, 液化, 响应面分析

Abstract: The liquefaction of bamboo powder was investigated in ethanol-phenol under high pressure using H₂SO₄ as catalyst. The liquefaction conditions were optimized by response surface analysis and its result was analyzed using Design-Expert 8.0.6 software. The effects conditions were investigated by a five level three-factor Box-Behnken design. The results showed that the liquefaction rate reached 98.5% under the optimum conditions, i.e., mass ratio of phenol and bamboo powder 1:1, ethanol and bamboo powder 18:1, sulfuric acid amount 5％,reaction temperature 200℃ and reaction time 70 min.The product analysis showed that the bamboo powder could be effectively degraded in blended solvents. The FT-IR, SEM and TG results of residue indicated that the molecular structure of bamboo powder present significant change via liquefaction and the compounds with different substituent on aromatic ring were obtained. The GC-MS analysis showed that the oil produced by this way was complex in composition with some major compounds such as alcohols, phenols, ketones and esters, and the GC content of ethyl levulinate reached 10.11%.

Key words: bamboo powder, liquefaction, response surface

中图分类号:

TQ35
TK6

马艳, 谭卫红, 冯国东, 徐俊明, 王奎, 应浩, 蒋剑春. 竹粉乙醇-苯酚加压液化工艺研究及产物表征[J]. 林产化学与工业, 2016, 36(4): 105-112.

MA Yan, TAN Wei-hong, FENG Guo-dong, XU Jun-ming, WANG Kui, YING Hao, JIANG Jian-chun. Liquefaction of Bamboo Powder in Ethanol-phenol under High Pressure and Product Characterization[J]. Chemistry and Industry of Forest Products, 2016, 36(4): 105-112.

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竹粉乙醇-苯酚加压液化工艺研究及产物表征

Liquefaction of Bamboo Powder in Ethanol-phenol under High Pressure and Product Characterization

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