天然微藻水热炭理化特性及热解动力学研究
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摘要
为探索天然微藻资源化的利用途径,该文以天然栅藻为原料,采用傅立叶转换红外线光谱分析, X射线衍射分析,X射线荧光光谱分析,环境扫描电子显微镜与热重分析仪对水热炭进行测试分析。研究结果表明,随着水热温度的升高,水热炭产率从47.29%(180℃)降低至43.01%(240%);水热炭的O/C摩尔比从1.45减小至0.28,碳化程度加强,水热炭具有应用于固体燃料的潜力。鉴于水热炭含有大量灰分,其热值为8.43～9.67 MJ/kg,因此脱灰预处理是必要的过程。经过水热碳化处理,天然栅藻的比表面积从4.36 m~2/g增加到35.26 m~2/g。热解动力学结果表明随着水热温度的提高,水热炭的热稳定性增强。研究结果对天然微藻的资源化利用提供了一定的理论参考。
In order to explore the utilization of natural microalgae, the natural Scenedesmus was selected to carry out hydrothermal carbonization experiments, and the characterization of its hydrochars was determined using Fourier transform infrared spectroscopy, X-ray diffraction analysis, X-ray fluorescence spectroscopy, environmental scanning electron microscopy and thermogravimetric analyzer. The results showed that the ash content of natural Scenedesmus was 44.66%, and the lipid and protein content of natural Scenedesmus were 1.4% and 15.1%, respectively. The natural microalgae ash components were mostly water-insoluble components. The main components included(Mg0.064 Ca0.936 CO3), SiO2, NaCl, Al2 O3, CaSO4, Mg3 S2 O8(OH)2. After hydrothermal carbonization treatment, NaCl was dissolved in water, and the water-insoluble components were enriched in hydrochars. Compared with the natural Scenedesmus, the ash content of hydrochars increased, in the range from 57.41% to 71.47%. It was worth noting that the natural Scenedesmus and its derived hydrochars had no fixed carbon. With the increase of hydrothermal temperature, the hydrothermal carbon yield decreased from 47.29%(180℃) to 43.01%(240℃). This phenomenon was on account of the organic components in the natural Scenedesmus underwent hydrolysis, dehydration, decarboxylation, aromatization, condensation and polymerization. The carbon remaining ratio was the largest, the oxygen was the smallest, and the remaining ratios of carbon, hydrogen and oxygen decreased as the hydrothermal temperature increased. For HC-240, the removal rates of H and O were 69.88% and 93.88%, respectively, and the C remaining ration rate was 33.97%. The O/C molar ratio of hydrochars decreased from 1.45 to 0.28. Dehydration and decarboxylation were the main pathways in hydrothermal carbonization of the natural Scenedesmus, and the demethylation pathway was negligible. Oxygen was removed in the form of H2 O and CO2. The degree of carbonization was enhanced and hydrochars had the potential to be applied to solid fuels. Since hydrochars contained a large amount of ash, its calorific value was in the range of 8.43-9.67 MJ/kg. Hence, the pretreatment of deashing was a necessary process. The hydrothermal carbonization treatment effectively improved the pore structure of hydrochars, and the absorption-desorption capacity of hydrochars was obviously enhanced. Compared with natural Scenedesmus(4.36 m~2/g), the specific surface area of hydrochars was in the range of 28.7-35.26 m~2/g. The natural Scenedesmus had a dense block-like without pores or pathways. However, the morphologies of hydrochars changed significantly. The fragmentation and porosity of hydrochars increased, which attributed to the release of volatile matter during hydrothermal carbonization process and chemical bond decomposition of feedstock. The thermogravimetric analysis experiments were carried out to reveal the pyrolysis characteristics of hydrochars. It was found that the weight loss peak at 300 ℃ gradually disappeared with the increased of hydrothermal temperature. This was owing to the degree of natural Scenedesmus increased and the volatile matter content decreased. When the hydrothermal temperature was higher than 220 ℃, the maximum weight loss rate peak moved to the high temperature zone. The pyrolysis kinetics results showed that the thermal stability of hydrochars increased with the increase of hydrothermal temperature. The hydrochars were more hydrophobic than that of the natural Scenedesmus. The research results provide a theoretical reference for the resource utilization of natural microalgae.
In order to explore the utilization of natural microalgae, the natural Scenedesmus was selected to carry out hydrothermal carbonization experiments, and the characterization of its hydrochars was determined using Fourier transform infrared spectroscopy, X-ray diffraction analysis, X-ray fluorescence spectroscopy, environmental scanning electron microscopy and thermogravimetric analyzer. The results showed that the ash content of natural Scenedesmus was 44.66%, and the lipid and protein content of natural Scenedesmus were 1.4% and 15.1%, respectively. The natural microalgae ash components were mostly water-insoluble components. The main components included(Mg0.064 Ca0.936 CO3), SiO2, NaCl, Al2 O3, CaSO4, Mg3 S2 O8(OH)2. After hydrothermal carbonization treatment, NaCl was dissolved in water, and the water-insoluble components were enriched in hydrochars. Compared with the natural Scenedesmus, the ash content of hydrochars increased, in the range from 57.41% to 71.47%. It was worth noting that the natural Scenedesmus and its derived hydrochars had no fixed carbon. With the increase of hydrothermal temperature, the hydrothermal carbon yield decreased from 47.29%(180℃) to 43.01%(240℃). This phenomenon was on account of the organic components in the natural Scenedesmus underwent hydrolysis, dehydration, decarboxylation, aromatization, condensation and polymerization. The carbon remaining ratio was the largest, the oxygen was the smallest, and the remaining ratios of carbon, hydrogen and oxygen decreased as the hydrothermal temperature increased. For HC-240, the removal rates of H and O were 69.88% and 93.88%, respectively, and the C remaining ration rate was 33.97%. The O/C molar ratio of hydrochars decreased from 1.45 to 0.28. Dehydration and decarboxylation were the main pathways in hydrothermal carbonization of the natural Scenedesmus, and the demethylation pathway was negligible. Oxygen was removed in the form of H2 O and CO2. The degree of carbonization was enhanced and hydrochars had the potential to be applied to solid fuels. Since hydrochars contained a large amount of ash, its calorific value was in the range of 8.43-9.67 MJ/kg. Hence, the pretreatment of deashing was a necessary process. The hydrothermal carbonization treatment effectively improved the pore structure of hydrochars, and the absorption-desorption capacity of hydrochars was obviously enhanced. Compared with natural Scenedesmus(4.36 m~2/g), the specific surface area of hydrochars was in the range of 28.7-35.26 m~2/g. The natural Scenedesmus had a dense block-like without pores or pathways. However, the morphologies of hydrochars changed significantly. The fragmentation and porosity of hydrochars increased, which attributed to the release of volatile matter during hydrothermal carbonization process and chemical bond decomposition of feedstock. The thermogravimetric analysis experiments were carried out to reveal the pyrolysis characteristics of hydrochars. It was found that the weight loss peak at 300 ℃ gradually disappeared with the increased of hydrothermal temperature. This was owing to the degree of natural Scenedesmus increased and the volatile matter content decreased. When the hydrothermal temperature was higher than 220 ℃, the maximum weight loss rate peak moved to the high temperature zone. The pyrolysis kinetics results showed that the thermal stability of hydrochars increased with the increase of hydrothermal temperature. The hydrochars were more hydrophobic than that of the natural Scenedesmus. The research results provide a theoretical reference for the resource utilization of natural microalgae.
引文
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[2]Bhattacharya S,Maurya R,Mishra S K,et al.Solar driven mass cultivation and the extraction of lipids from chlorella variabilis:A case study[J].Algal Research,2016(14):137-142.
[3]徐玉福,俞辉强,朱利华,等.小球藻粉水热催化液化制备生物油[J].农业工程学报,2012,28(19):194-199.Xu Yufu,Yu Huiqiang,Zhu Lihua,et al.Preparation of bio-fuel from Chlorella pyrenoidosa by hydrothermal catalytic liquefaction[J].Transactions of the Chinese Society of Agricultural Engineering(Transactions of the CSAE)2012.28(19):194-199.(in Chinese with English abstract)
[4]曲磊,崔翔,杨海平,等.微藻水热液化制取生物油的研究进展[J].化工进展,2018,37(8):2962-2969.Qu Lei,Cui Xiang,Yang Haiping,et al.Review on the preparation of bio-oil by microalgae hydrothermal liquefaction[J].Chemical Industry and Engineering Progress,2018,37(8):2962-2969.(in Chinese with English abstract)
[5]徐春明,焦志亮,王晓丹,等.微藻作原料生产生物柴油的研究现状和前景[J].现代化工,2015,35(8):1-5.Xu Chunming,Jiao Zhiliang,Wang Xiaodan,et al.Biodiesel production from microalgae:Current status and potential[J].Modern Chemical Industry,2015,35(8):1-5.(in Chinese with English abstract)
[6]张冀翔,蒋宝辉,王东,等.微藻水热液化生物油化学性质与表征方法综述[J].化工学报,2016(5):1644-1653.Zhang Yixiang,Jiang Baohui,Wang Dong,et al.Chemical properties and characterization methods for hydrothermalliquefaction bio-crude from microalgae:Areview[J].CIESC Journal,2016(5):1644-1653.(in Chinese with English abstract)
[7]Peterson A A,Vogel F,Lachance R P,et al.Thermochemical biofuel production in hydrothermal media:A review of suband supercritical water technologies[J].Energy&Environmental Science,2008,1(1):32-65.
[8]王定美,王跃强,袁浩然,等.水热炭化制备污泥生物炭的碳固定[J].化工学报,2013(7):2625-2632.Wang Dingmei,Wang Yueqiang,Yuan Haoran,et al.Carbon fixation of sludge biochar by hydrothermal carbonization[J].CIESC Journal,2013(7):2625-2632.(in Chinese with English abstract)
[9]Funke A,Ziegler F.Hydrothermal carbonization of biomass:A summary and discussion of chemical mechanisms for process engineering[J].Biofuels Bioproducts&Biorefining-Biofpr,2010,4(2):160-177.
[10]李音,单胜道,杨瑞芹,等.低温水热法制备竹生物炭及其对有机物的吸附性能[J].农业工程学报,2016,32(24):240-247.Li Yin,Shan Shengdao,Yang Ruiqin,et al.Preparation of bamboo biochars by low-temperature hydrothermal method and its adsorption of organics[J].Transactions of the Chinese Society of Agricultural Engineering(Transactions of the CSAE),2016,32(24):240-247.(in Chinese with English abstract)
[11]Cao X,Ro K S,Chappell M,et al.Chemical structures of swine-manure chars produced under different carbonization conditions investigated by advanced solid-state C-13 nuclear magnetic resonance(NMR)spectroscopy[J].Energy&Fuels,2011,25(1):388-397.
[12]Falco C,BaccileN,Titirici M M.Morphological and structural differences between glucose,cellulose and lignocellulosic biomass derived hydrothermal carbons[J].Green Chemistry,2011,13(11):3273-3281.
[13]Cheng F,Cui Z,Chen L,et al.Hydrothermal liquefaction of high-and low-lipid algae:Bio-crude oil chemistry[J].Applied Energy,2017,206:278-292.
[14]Heilmann S M,Davis H T,Jader L R,et al.Hydrothermal carbonization of microalgae[J].Biomass&Bioenergy,2010,34(6):875-882.
[15]Xu Q,Qian Q,Quek A,et al.Hydrothermal carbonization of macroalgae and the effects of experimental parameters on the properties of hydrochars[J].ACS Sustainable Chemistry&Engineering,2013,1(9):1092-1101.
[16]Park K Y,Lee K,Kim D.Characterized hydrochar of algal biomass for producing solid fuel through hydrothermal carbonization[J].Bioresource Technology,2018,258:119-124.
[17]Lee J,Lee K,Sohn D,et al.Hydrothermal carbonization of lipid extracted algae for hydrochar production and feasibility of using hydrochar as a solid fuel[J].Energy,2018,153:913-920.
[18]Marin-Batista J D,Villamil J A,Rodriguez J J,et al.Valorization of microalgal biomass by hydrothermal carbonization and anaerobic digestion[J].Bioresource Technology,2019,274:395-402.
[19]张进红,林启美,赵小蓉,等.水热炭化温度和时间对鸡粪生物质炭性质的影响[J].农业工程学报,2015,31(24):239-244.Zhang Jinhong,Lin Qimei,Zhao Xiaorong,et al.Effect of hydrothermal carbonization temperature and time on characteristics of bio-chars from chicken manure[J].Transactions of the Chinese Society of Agricultural Engineering(Transactions of the CSAE),2015,31(24):239-244.(in Chinese with English abstract)
[20]Kohansal K,Tavasoli A,Bozorg A.Using a hybrid-like supported catalyst to improve green fuel production through hydrothermal liquefaction of Scenedesmus obliquus microalgae[J].Bioresource Technology,2019,277:136-147.
[21]Channiwala S A,Parikh P P.A unified correlation for estimating HHV of solid,liquid and gaseous fuels[J].Fuel,2002,81(8):1051-1063.
[22]王庆峰.中高硫煤浮选脱硫脱灰试验研究[D].青岛:青岛理工大学,2013.Wang Qingfeng.Research on Desulphurization and Deashing for Medium-High Sulphur Coal with Flotation[D].Qingdao:Qingdao Technological University,2013.(in Chinese with English abstract)
[23]Jaber J O,Probert S D.Non-isothermal thermogravimetry and decomposition kinetics of two Jordanian oil shales under different processing conditions[J].Fuel Processing Technology,2000,63(1):57-70.
[24]White J E,Catallo W J,Legendre B L.Biomass pyrolysis kinetics:A comparative critical review with relevant agricultural residue case studies[J].Journal of Analytical and Applied Pyrolysis,2011,91(1):1-33.
[25]张进红,林启美,赵小蓉,等.不同炭化温度和时间下牛粪生物炭理化特性分析与评价[J].农业机械学报,2018,49(11):298-305.Zhang Jinhong,Lin Qimei,Zhao Xiaorong,et al.Physico-chemical characteristics and evaluation of cow manure hydrocharat different carbonization temperatures and durations[J].Journal of Agricultural Machinery,2018,49(11):298-305.(in Chinese with English abstract)
[26]马腾,郝彦辉,姚宗路,等.秸秆水热生物炭燃烧特性评价[J].农业机械学报,2018,49(12):340-346.Ma Teng,Hao Yanhui,Yao Zonglu,et al.Evaluation on combustion characteristics of straw hydrothermal bio-char[J].Journal of Agricultural Machinery,2018,49(12):340-346.(in Chinese with English abstract)
[27]张曾,单胜道,吴胜春,等.炭化条件对猪粪水热炭主要营养成分的影响[J].浙江农林大学学报,2018,35(3):398-404.Zhang Zeng,Shan Shengdao,Wu Shengchun,et al.Carbonization with main nutrients in pig manure hydrochar[J].Journal of Zhejiang A&F University,2018,35(3):398-404.(in Chinese with English abstract)
[28]He C,Zhao J,Yang Y,et al.Multiscale characteristics dynamics of hydrochar from hydrothermal conversion of sewage sludge under sub-and near-critical water[J].Bioresource Technology,2016,211:486-493.
[29]Van Krevelen D W.Graphical-statistical method for the study of structure and reaction processes of coal[J].Fuel,1950,29:228-269.
[30]Zhang B,Feng H,He Z,et al.Bio-oil production from hydrothermal liquefaction of ultrasonic pre-treated Spirulina platensis[J].Energy Conversion and Management,2018,159:204-212.
[31]Sabio E,Alvarez-Murillo A,Roman S,et al.Conversion of tomato-peel waste into solid fuel by hydrothermal carbonization:Influence of the processing variables[J].Waste Management,2016,47:122-132.
[32]Yuan J H,Xu R K,Zhang H.The forms of alkalis in the biochar produced from crop residues at different temperatures[J].Bioresource Technology,2011,102(3):3488-3497.
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