沉淀法回收生物油高温馏分中的酚类物质

赵欣; 李凯; 李明; 马善为; 朱锡锋

沉淀法回收生物油高温馏分中的酚类物质

基金项目:

国家重点基础研究发展规划 973计划, 2013CB228103

中国科学院重点部署项目 KGZD-EW-304-3

详细信息

中图分类号: TK6
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出版历程
- 收稿日期: 2015-09-18
- 修回日期: 2015-11-19

Separating phenols from high-temperature fraction of bio-oil by precipitation

More Information

Corresponding author: Tel: 0551-63600040, E-mail: xfzhu@ustc.edu.cn

摘要

摘要: 为了研究金属离子沉淀法对生物油高温馏分中酚类物质的回收, 提高生物油中化学物质的利用率, 利用气相色谱-质谱联用仪 (GC-MS) 从NaOH试剂浓度、反应温度和反应时间三个方面研究了镁离子对生物油中酚类物质的回收效果。结果表明, 镁离子与酚类物质形成了不溶物, 而且不同浓度的氢氧化钠溶液 (1.0-4.0 mol/L)、不同的反应温度 (25-85℃) 以及不同的反应时间 (5-35 min) 对实验结果有着不同程度的影响。结果表明, 在反应温度为25℃、氢氧化钠浓度为2.5 mol/L, 反应时间在20 min时为最佳反应条件。在此条件下, 对生物油高温馏分中对乙基苯酚的回收率可达34.97%。
- 生物油 /
- 酚类 /
- 镁离子 /
- 沉淀法 /
- 回收
Abstract: To improve the utilization of chemicals in bio-oil, recovery of phenolic compounds from high temperature bio-oil fractions by metal ion precipitation was studied.The effects of concentration of sodium hydroxide solution, reaction temperature and reaction time on the recovery of phenolic compounds by magnesium ion were examined using gas chromatography-mass spectrometry (GC-MS).The results demonstrate that the precipitation was formed instead of a salt of magnesium phenols.The optimum reaction conditions are reaction temperature of 25℃, 2.5 mol/L of sodium hydroxide solution, and reaction time of 20 min.In this case, the recovery of 4-ethylphenol from high temperature bio-oil fractions reaches 34.97%.
- bio-oil /
- phenol /
- magnesium ion /
- precipitation /
- recovery

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图 1 沉淀法回收生物油中酚类物质的工艺路线示意图

Figure 1. Extraction procedure of phenolic compounds from bio-oil

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图 2 不溶物的红外光谱谱图

Figure 2. FT-IR spectrum of the complex

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图 3 乙酸乙酯层的总离子色谱图

Figure 3. Total ion chromatogram of ethyl acetate layer

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图 4 在不同NaOH浓度下对乙基苯酚的萃取率和pH值

Figure 4. 4-ethylphenol extraction rate and pH value at various concentrations of sodium hydroxide solution

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图 5 在不同温度下对乙基苯酚的萃取率和pH值

Figure 5. 4-ethylphenol extraction rate and pH value at various temperatures

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图 6 在不同时间下对乙基苯酚的萃取率和pH值

Figure 6. 4-ethylphenol extraction rate and pH value at various reaction times

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表 1 生物油高温馏分中酚类物质的化学成分

Table 1. Chemical compositions of phenolic compounds from high temperature fractions of bio-oil

No.	Chemical compound	Molecular formula	Molecular weight /(g·mol^-1)	Structure	Peak area /%
1	phenol	C₆H₆O	94		4.47
2	phenol, 2-methyl-	C₇H₈O	108		5.67
3	phenol, 3-methyl-	C₇H₈O	108		6.56
4	phenol, 2-methoxy-	C₇H₈O₂	124		3.35
5	2, 5-xylenol	C₈H₁₀O	122		1.88
6	phenol, 4-ethyl-	C₈H₁₀O	122		21.5
7	phenol, 2-methoxy-4-methyl-	C₈H₁₀O₂	138		2.86
8	1, 2-benzenediol	C₆H₆O₂	110		3.41
9	phenol, 3-(1-methylethyl)-	C₉H₁₀O	134		3.05
10	phenol, 3-methyl-4-ethyl-	C₉H₁₀O	134		1.58
11	phenol, 4-isopropyl-	C₉H₁₂O	136		3.89
12	guaiacol, 4-ethyl-	C₉H₁₀O₂	150		3.75
13	1, 2-benzenediol, 4-methyl-	C₇H₈O₂	124		2.1
14	phenol, 4-sec-butyl-	C₁₀H₁₄O	150		2.37
15	phenol, 2, 6-dimethoxy-	C₈H₁₀O₃	154		3.15
16	guaiacol, 5-allyl-	C₁₀H₁₂O₂	164		2.51
17	phenol, 2-methoxy-4-propyl-	C₁₀H₁₄O₂	166		2.94
18	catechol, 4-ethyl-	C₈H₁₀O₂	138		2.2
19	guaiacol, 4-propenyl-	C₁₀H₁₂O₂	164		2.04

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表 2 乙酸乙酯层中的酚类化合物

Table 2. Phenolic compounds identified in the ethyl acetate layer

No.	Chemical compound	Molecular formula	Molecular weight /(g·mol^-1)	Structure	Peak area /%
1	phenol	C₆H₆O	94		5.48
2	phenol, 3-methyl-	C₇H₈O	108		6.47
3	guaiacol	C₇H₈O₂	124		4.03
4	phenol, 4-ethyl-	C₈H₁₀O	122		21.75
5	guaiacol, 4-methyl	C₈H₁₀O₂	138		3.74
6	catechol	C₆H₆O₂	110		3.19
7	phenol, 3-(1-methylethyl)-	C₉H₁₀O	134		3.95
8	phenol, 2-ethyl-5-methyl-	C₉H₁₂O	136		2.09
9	phenol, 4-propyl-	C₉H₁₂O	136		4.01
10	guaiacol, 4-ethyl-	C₉H₁₀O₂	150		5.6
11	catechol, 4-methyl-	C₈H₁₀O₂	138		1.77
12	phenol, 4-sec-butyl-	C₁₀H₁₄O	150		1.48
13	phenol, 2, 6-dimethoxy-	C₈H₁₀O₃	154		2.78
14	guaiacol, 5-allyl-	C₁₀H₁₂O₂	156		1.85
15	phenol, 2-methoxy-4-propyl-	C₁₀H₁₄O₂	166		3.96
16	catechol, 4-ethyl-	C₈H₁₀O₂	138		1.56
17	guaiacol, 4-propenyl-	C₉H₁₂O	136		2.1

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