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化学进展 2021, Vol. 33 Issue (11): 2150-2162 DOI: 10.7536/PC210420 前一篇   

• 综述 •

生物质水热液化水相产物形成机理及资源回收

徐永洞, 刘志丹*()   

  1. 中国农业大学水利与土木工程学院环境增值能源实验室 农业农村部设施农业工程重点实验室 北京 100083
  • 收稿日期:2021-04-15 修回日期:2021-06-07 出版日期:2021-07-29 发布日期:2021-07-29
  • 通讯作者: 刘志丹
  • 基金资助:
    国家自然科学基金项目(U1562107); 国家自然科学基金项目(51861125103)
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Formation Mechanism and Resource Recovery Perspectives of Aqueous Phase from Hydrothermal Liquefaction of Biomass

Yongdong Xu, Zhidan Liu()   

  1. Laboratory of Environment-Enhancing Energy (E2E), Key Laboratory of Agricultural Engineering in Structure and Environment of Ministry of Agriculture and Rural Affairs, College of Water Resources and Civil Engineering, China Agricultural University, Beijing 100083, China
  • Received:2021-04-15 Revised:2021-06-07 Online:2021-07-29 Published:2021-07-29
  • Contact: Zhidan Liu
  • Supported by:
    National Natural Science Foundation of China(U1562107); National Natural Science Foundation of China(51861125103)

生物质水热液化转化为生物原油是极具潜力的可再生液体燃料制备途径。但水热液化水相产物产量大、成分复杂,具有较高的环境风险,限制了水热液化的绿色发展。论文以本课题组近10年(2012—2021)的研究积累为核心,综述了水热液化水相产物的形成机理、理化特性和资源回收路径。本文介绍了水相副产物形成的影响因素,总结了不同反应变量下水热转化和元素迁移途径;综述了水相生物转化的途径和研究进展,包括好氧微生物降解、微藻养殖、厌氧处理和微生物电化学等,介绍了膜分离和吸附等物理方法用于水相物质分离、获得高价值组分的研究,论述了利用水相制备农业杀菌剂的潜力。最后对水相的处理原则和研究方向进行展望,以期为水热液化水相的处理和资源回收提供参考。

关键词： 水热液化, 水相产物, 形成机理, 生物处理, 资源回收

The conversion of biomass into biocrude oil by hydrothermal liquefaction (HTL) is a potential way to produce renewable liquid fuels. However, the aqueous phase (HTL-AP) by-products have high yields, complex compositions and high environmental risk which limit the green development of hydrothermal liquefaction technology. Based on the relevant research of our research group in recent 10 years (2012-2021), this paper summarizes the formation mechanism, characteristics and resource recovery path of HTL-AP. The factors affecting the formation of HTL-AP were introduced, and the ways of compound transformation and element migration in different hydrothermal reaction variables were summarized. The approaches and research progress of aqueous biotransformation, including aerobic microbial degradation, microalgae culture, anaerobic treatment and microbial electrochemistry, were reviewed. The physical methods such as membrane separation and adsorption were introduced to separate aqueous substances and obtain high-value components. The potential of using HTL-AP to prepare agricultural fungicides was discussed. Finally, the treatment principle and research direction are prospected in order to provide reference for the treatment and resource recovery of HTL-AP.

Contents

1 Introduction

2 Formation mechanism of HTL-AP

2.1 Hydrothermal reaction conditions

2.2 Raw material conversion path

2.3 Element migration path

3 Physical and chemical methods

3.1 Separation of organic elements

3.2 Separation of inorganic elements

3.3 Mixed component utilization

4 Biological treatment method

4.1 Cytotoxicity

4.2 Aerobic biological treatment

4.3 Microalgae treatment

4.4 Anaerobic fermentation

4.5 Microbial electrochemistry

5 Challenges and prospects of HTL-AP resource recovery

5.1 Challenges of HTL-AP resource recovery

5.2 Prospects of HTL-AP resource recovery

6 Conclusion

Key words: hydrothermal liquefaction, aqueous products, formation mechanism, biological treatment, resource recovery
()
图1 水热液化反应过程及两条产物分离路径
Fig. 1 Hydrothermal liquefaction reaction process and two product separation paths
图2 不同温度条件下模型化合物混合原料水热液化水相产物主要物质
Fig. 2 Main components of HTL-AP of mixed feedstocks of model compounds at different temperatures
表1 不同原料来源的水热液化水相性质[22,33,34]
Table 1 Typical characteristics of HTL-AP from HTL of various feedstock[22,33,34]
Composition Feedstock Operating Conditions pH COD (g·L-1) TOC (g·L-1) TN (g·L-1) TP (g·L-1)
Lignocellulose Con silage 220 ℃, 6 h 3.8 41.4 15.7 0.7 0.2
Suga beet waste 338 ℃ 4.7 110.4 - - -
Rice straw 170~330 ℃, 30 min 3.7 ~5.6 14.3~29.0 3.9 ~ 10.3 - -
Cornstalk 260 ℃, 0 h - 76.19 28.6 - -
Sludge Sewage sludge 140~320 ℃, 15~240 min; - 17.5~105.6 4.9~13.7 - -
Municipal sludge 225~275 ℃, 15~60 min - - 2.487 0.514 0.048
Swine manure - 5.6 104.1 - 5.36 1
Swine manure 270 ℃, 1 h - 39.8 - 1.85 -
Swine manure - 4.5 33 11.1 0.9 <0.01
Human feces 280 ℃, 1 h - 52.6 - 1.16 -
Algae Microalgae mixture 350 ℃, 1 h 4.7~6.8 - - 3.6~14.6 0.32~1.05
Tetraselmis sp. 350 ℃, 10 min - - 19 52 -
Tetraselmis 343~350 ℃, 7.6~7.9 43.8~94.9 - - -
Chlorella 350 ℃, 0~60 min, 8.0~8.6 - 6.99-13.09 - -
Chlorella 1067 300 ℃, 30 min 7.82 75.5 31.1 20.2 -
Chlorella pyrenoidosa 260~300 ℃, 30~90 min 7.77~8.29 62.7~104 - 11.0~31.7 5.4~18.9
Nannochloropsis sp. 344~362 ℃ 7.48~7.72 59.9~125.5 - 5.4~11.0 0.15
Spirulina 300 ℃, 30 min 8.64 143.8 - 21.3 1.37e
Spirulina sp. 220 ℃, 60 min 8.24 185.1 78.96 21.53 1.14
Spirulina powder 300 ℃, 30 min 7.8 89 - 22.98 4.4
Scenedesmus almeriensis 350 ℃, 15 min - - 12.57 5.3 -
N. gaditana 350 ℃, 15 min, 8.2~8.6 - 11.37~14.10 4.22~5.42 -
图3 C和N元素在水热液化产物中的分布[32]
Fig.3 Carbon and nitrogen distribution during HTL of manures[32]. (a) Carbon and nitrogen balance during HTL of manures; (b) Organic groups in the aqueous phase from HTL of livestock manures identified by GC-MS analysis. Copyright 2018, ACS Society
表2 微藻在不同原料来源的水热液化水相中的生长性能[33]
Table 2 Microalgae cultivation of HTL-AP from HTL of diverse biomass[33]
Feed of
HTL-AP		 Cultivation species Cultivation Conditions Performance
Dilution pH T
(℃)		 D
(days)		 ESC LS
S. platensis Chlorella 10~500 × 7.5 25 12 aeration (air
with 5% CO2)		 24 h illumination (80~110 μmol·m-2·s-1) Maximum biomass productivities (0.035 g·L-1·d-1, 0.52 g·L-1) in mediumby 500 × No growth in medium by 10 ×
C. reinhardtii C. reinhardtii 140 × 7.2~
7.4		 25 7 aeration (air
with 2% CO2)		 24 h illumination (130 μE·m-2·s-1) Optimized dilution rate was 25 ×
All grew well excepted one using ethyl ether extraction
C. sorokiniana C. sorokiniana, C. vulgaris or G. sulphuraria 0~30 × - 26 or 42 10 aeration (air
with 0.5%
CO2)		 12 h on/
off illumination		 Growth rate depended on HTL feed and aqueous separation
Heterotrophic mode was dominant in 10~50×media
Nannochloropsis sp. or
Chlorella sp.		 C. vulgaris 3.5~
52.6 ×		 7.0~7.5 26 11 no aeration 12 h on/off
illumination (170
μmol·m-2·s-1)		 Autotrophic mode was dominant in 100~200×media
Mixotrophic mode
G. sulphuraria G. sulphuraria 12.5~
100 ×		 - 40 3 2%~3% CO2 14 h on/10 h
off illumination		 P. tricornutum did not grow satisfactorily
Maximum biomass concentration (13.4 g·L-1) and productivity (~1 g·L-1·d-1)
N. gaditana N. gaditana or P. tricornutum 377, 392
or 571 ×		 7.8 - 14 ambient air 24 h illumination (125
μmol·m-2·s-1)		 Photosynthetic efficiency was up to ~9%
Much lower growth than that in AM-14
图4 HTL-AP吸附处理后厌氧发酵
Fig.4 Anaerobic fermentation of HTL-AP after adsorption[76]. (a) zeolite adsorption and anaerobic digestion; (b) Gas chromatography-mass spectrometer (GC-MS) chromatograms for zeolite-adsorbed and raw HTL-AP. Copyright 2018, Elsevier
图5 利用HTL-AP产生生物氢烷系统中微生物分布[80]
Fig.5 Taxonomic classification of microbial community in biohythane and biomethane systems for HTL-AP treatment[80]. At the phylum (A, C) and family (B, D) levels through Illumina Miseq sequencing. Copyright 2016, Springer
图6 MEC用于HTL-AP处理[84]
Fig.6 MEC system used for HTL-AP treatment[84]. Copyright 2018, Elsevier
表3 HTL-AP处理技术现状对比
Table 3 Comparison of the state of technology of different HTL-AP treatment approaches.
Technology Category Approaches Advantages Challenges
Biotechnology Algae Cultivation Nutrients are reused
Biomass generation
Mild treatment conditions		 Low COD removal efficiency
Needs economic evaluation
Large dilution ratio demand
Risk of heavy meatal accumulation
Aerobic Biodegradation Biomass generation
Mild treatment conditions		 Large dilution ratio demand
High aeration energy consumption
Anaerobic Fermentation Energettically positive
Low operating cost
Large capacity		 Long processing cycle
Large dilution ratio requirement
Microbial Electrochemical Technology Energettically positive
High removal rate of
toxic substances
Low sludge production		 Long processing cycle
Small capacity
Physicochemical Technology Chemical Sedimentation High separation efficiency of
inorganic substances		 Needs additional chemicals
High sludge production
Low removal rate of organic substances
Membrane Separation Concentrate the aqueous phase
Separation of organic and
inorganic substances		 Difficult to obtain specific substances
Limited efficiency of small molecule organic substances
Adsorption-desorption Obtain specific substances Low treatment efficiency
Needs economic evaluatio
Complex process
Gasification Efficient removal of
organic substances
Fast conversion process		 High energy demand
High pressure and temperature
Limited removal rate of inorganic substances
Recycle for HTL Water conservation
Concentrate the aqueous phase
No additional treatment
technology required		 May restrain the oil production rate
High energy requirement
Prominent Pathway Bactericidal Insecticide High value-added utilization Needs evaluation of biosafety, economy and effectiveness
Unstable bactericidal properties
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