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Progress in Chemistry 2021, Vol. 33 Issue (11): 2150-2162 DOI: 10.7536/PC210420 Previous Articles   

• Review •

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: Revised: Online: Published:
  • Contact: Zhidan Liu
  • Supported by:
    National Natural Science Foundation of China(U1562107); National Natural Science Foundation of China(51861125103)
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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
Fig. 1 Hydrothermal liquefaction reaction process and two product separation paths
Fig. 2 Main components of HTL-AP of mixed feedstocks of model compounds at different temperatures
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 -
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
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
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
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
Fig.6 MEC system used for HTL-AP treatment[84]. Copyright 2018, Elsevier
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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