生物炭对西唯因与阿特拉津环境行为的影响
摘要
生物炭是动植物残体经缺氧热解形成的一种富含碳物质,由于在生物质资源化、减缓气候变化、提高土壤肥力等诸方面表现出的良好潜能,生物炭作为一种新型多功能材料迅速成为研究的热点。由于含有多孔及高度芳香结构,生物炭对各类污染物表现出较强的吸附能力,必将影响其环境行为、归宿及生态风险。
本论文系统研究了不同结构生物炭对两种典型农药一阿特拉津和西维因的吸附、水解及微生物降解等环境行为的影响及其微观机制。首先,利用猪粪、玉米秸秆、水稻秸秆等三种农业废弃物,通过不同的热解温度制备了物质组成和结构不同的生物炭并对生物炭进行了除灰处理,得到性质各异生物炭十余种,对不同生物炭的有机与无机部分的含量、化学组成与结构特征；孔性质与比表面积等性质进行了表征。在此基础上,研究了不同种类生物炭对两种农药的吸附作用机理,深入探讨了生物炭有机部分、无机部分、孔结构及生物碳表面化学作用等在吸附过程中所起的作用。研究了不同种类生物炭对两种农药的水解催化作用,通过逐步分析背景溶液,生物炭悬浊液以及生物炭浸出液中农药的水解,从OH-、表面矿物以及金属离子等方面探讨生物炭促进农药水解的机理。研究了生物炭对土壤中农药降解的影响,并向生物炭与土壤混合体系中接种筛选的对农药降解特异性微生物菌群,以促进土壤中农药的生物降解,通过不同的实验设计,综合分析了生物炭对土壤中农药去除的影响及途径。通过以上研究得到以下结论：
(1)生物炭由脂肪炭和芳香碳组成的有机部分,以及磷酸盐、碳酸盐和其他无机矿物组成的无机部分共同构成。有机碳表面含有羟基,羧基以及羰基等基团。不同原料和温度制备的生物炭物质组成和结构有较大差异。猪粪制备的生物炭含有较高的灰分,而秸秆制备的生物炭灰分较低,且温度越高灰分含量越多。而高温使生物炭孔比例增加,比表面积显著升高。
(2)生物炭可有效地吸附西维因,吸附等温线符合Freundlich方程,且吸附表现为非线性。低浓度时,初级生物炭有机碳标化分配系数(Koc)为10265-104.48L/kg。除灰后生物炭的吸附性能显著提高,低浓度时Koc为103·64-104.74L/kg。不同来源和温度制备的生物炭组成和结构具有差异性,其对西维因的吸附能力和吸附机制不同。猪粪生物炭(PBC)中无机部分对吸附的综合作用表现为阻碍作用；而玉米秸秆生物炭(MBC)和水稻秸秆生物炭(RBC)中无机部分在低温时表现为阻碍作用,而高温时表现出促进作用。生物炭对西维因的吸附是疏水性作用、孔填充作用、无机灰分以及特殊作用力等综合作用的结果,生物炭对西维因的吸附亲和性与生物碳的极性,芳香度以及疏水基团等单一因素没有明显的相关性。
(3)生物炭对阿特拉津的等温吸附也表现为非线性吸附,但吸附亲和能力要弱于对西维因的吸附。高浓度时初级生物炭的Koc为101.90-103.10L/kg。除灰后生物炭的吸附性能显著提高,高浓度时Koc为102.63-103.10L/kg。生物炭对阿特拉津的吸附是疏水性作用、孔填充作用、无机灰分以及特殊作用力等综合作用。与生物炭对西维因的吸附作用类似,生物炭对阿特拉津的吸附亲和与生物炭的极性没有明显的相关性。
(4)西维因在碱性(pH=9.1)条件下水解迅速,18h就水解80%以上；而在中性条件下较稳定。不同生物炭悬浊液中西维因的水解差异很大,7d水解率为21.9%-90.6%,西维因在生物炭悬浊液中的水解与体系pH呈正相关。除了pH对于水解的催化作用外,生物炭表面矿物以及释放到溶液中的过渡金属离子都可促进水解,而吸附降低了西维因分子的可及性,减弱水解。西维因在各生物炭实验组中的水解动力学过程大部分符合拟一级过程。
(5)阿特拉津在环境中较稳定,在碱性(pH=9.1)条件下,7d水解率仅为16.1%。阿特拉津在生物炭悬浊液中的水解程度比西维因弱,7d仅水解了2.6%-63.4%。阿特拉津的水解与生物炭的无机部分含量呈正相关。阿特拉津在生物炭悬浊液中的水解主要受生物炭表面和pH的影响,而金属离子的对水解的贡献较差。阿特拉津在各生物炭实验体系中的水解动力学过程大部分符合拟一级动力学。
(6)在灭菌的生物炭-土壤体系中,土壤pH升高,农药的降解主要是生物炭的催化水解作用。土壤中农药的降解趋势表现为PBC>RBC>MBC,与悬浊液中农药的水解趋势类似。未灭菌体系中,化学降解与微生物降解并存,添加高含量的高温生物炭的土壤pH的升高更显著,催化了水解,降低了土著微生物的降解能力,因此,农药的降解主要为水解。而添加高含量的低温生物炭的土壤,吸附作用降低了农药的生物有效性,对土壤中农药的降解有阻碍作用。而添加有机碳含量高的MBC,对土壤pH改变较小,为微生物提供所需的营养物质,促进微生物生长,提高了降解能力。活性污泥筛选的农药降解菌群能够有效地降解西维因和阿特拉津,且西维因降解菌群的降解能力强于阿特拉津降解菌群。加入外源微生物的土壤中,西维因40d降解率为79.8%；而添加微生物的土壤-生物炭体系,降解率为64.9%-82.9%,不同的生物炭分别表现出促进和抑制作用；对于阿特拉津也有同样的规律,这是生物炭影响水解、微生物生长以及化合物生物有效性的综合结果。
Biochars are materials produced by pyrolyzing biomass under limited oxygen. Due to its promising feature in recycling biomass waste, attenuating climate change, and improving soil fertility, biochar has quickly become a research hotspot as a novel functional material with multiple applications. Due to the highly porous structure and aromaticity, biochars show great adsorptive capacity for various pollutants, and hence influencing their environmental behavior, fate, and eco-risk.
The present thesis systematically studied the impacts and mechanisms behind on the adsorption, hydrolysis, and biodegradation of two typical pesticides, carbaryl and atrazine, by different biochars. To do so, different biochars with varied composition and structure, were derived from pig-manure, maize straw, and rice straw under different pyrolysis temperatures, and the present biochars were further deashed by acid. The structure characteristics, such as the content and constitutes of organic and inorganic moieties, specific surface area and pore structure, and chemical surface functional groups,were measured. Moreover, the adsorption of the two pesticides on the original biochars and deashed biochars were studied, and relationships between adsorption affinity and structural parametersof biochars were analyzed to elucidate their functions in adsorption. The hydrolysis of carbaryl and atrazine were studied in suspensions of different biochars. The mechanism of the catalytic hydrolysis were discussed by analyzing the effects of elevated solution pH, mineral surface, and dissolvedmetal ions step by step. Finally, the degradation of pesticides in soil amended withbiochars were studied under different designs. Exogenous mixed bacteriawere added to strengthen the biodegradation of the pesticides. The influence and pathways behind of biochars on pesticide removal were discussed. Through theresearchabove, some main results obtainedwere as followed:
(1) The biochars consisted of organic moiety including aliphatic carbon and aromatic carbon and inorganic moiety containing phosphate, carbonate, and other minerals. In addition, chemical functional groups, such as hydroxyl, carboxyl and carbonyl, also bound on the surface of bio chars. Great difference existed in composition and structure of various biochars derived from different feedstocks and temperatures. Biochars derived from pig-manure contained high content of ash, however, biochars derived from straws had low ash contents, and biochars derived from maize straw contained lower ash than that those derived from rice straw. The ash contents of biochars increased with elevated pyrolyzing temperature. Porosity and specific surface area also increased with increasing temperature.
(2) Carbaryl could be adsorbed efficiently by biochars. Adsorption isotherms were fitted by Freundlich equation with distict nonlinearity. In prisent biochars, the distribution coefficients normalized by organic carbon content (Koc) of biochars were102.65-104.48L/kg at low solute concentration. When the ash was removed, adsorption increased generally,the distribution coefficients normalized by organic carbon content (Koc) of biochars were103.64-104.74L/kg at low solute concentration Differences in composition and structure of biochars derived from different feedstocks and temperatures led to the differences in adsorption affinity and mechanism of the various biochars. Inorganic moiety of the biochars derived from pig-manure (PBC) had an apparently negative effect on adsorption. The inorganic moiety of biochars derived from maize straw (MBC) and rice straw (RBC) under low pyrolyzing temperature had negative effect on adsorption, however, that of MBC and RBC obtained under high pyrolyzing temperature had positive effect. Overall, the adsorption of carbaryl on biochar was controlled by hydrophobic effect, pore-filling effect, effects with inorganic ash and specific effect. No significant correlation could be found between adsorption affinity with any of single parameters of polarity, aromaticity, and hydrophobic functional groups.
(3) Adsorption isotherms of atrazine on biochars were fitted in Freundlich equation and displayed nonlinear trends. The Koc of biochars werel01.90-103.10L/kg at high solute concentration. After deashing treatment, The Koc of deashed biochars were102.63-103.10L/kg at high solute concentration. Mechanism of adsorption of atrazine on biochars was also a combination of hydrophobic effect, pore-filling effect, effects with inorganic moiety and specific effects. In addition, no significant correlation between polarity of biochars and adsorption affinity could be found for atrazine either.
(4) Rapid hydrolysis of carbaryl occurred in alkaline (pH=9.1) background solution with over80%lost in18h, however, it was stable in neutral background solution. Hydrolysis of carbaryl in suspensions of biochars varied a lot with7d hydrolysis ratio ranging from21.9%to90.6%, and biochars influenced hydrolysis through different ways. We found a positive correlation between carbaryl hydrolysis and the pH of the suspensions. Beside pH, surface minerals, metal ions, and adsorption of biochars also influenced hydrolysis ratio, with the former two factors having catalyzing effect and the latter one showing inhibitory effect. The hydrolysis of carbaryl in majority of the tested systems were fitted in pseudo-first order kinetic equation.
(5) Hydrolysis of atrazine only occurred in strong alkaline background solution, and only16.1%of atrazine was hydrolyzed at pH of9.1. The hydrolysis of atrazine in suspensions of biochars were generally weaker than those of carbaryl with7d hydrolysis ratio ranging from2.6%to63.4%. The hydrolysis of atrazine was positive correlated with the quantity of inorganic moiety, and surface minerals and carboxylic groups could enhance the OH" catalyzed hydrolysis of atrazine by forming H-bond with atrazine. The hydrolysis of atrazine in the suspensions of biochars were mainly influenced by mineral surface and solution pH, and the contribution of metal ions was very low. The hydrolysis of atrazine in majority of the tested systems were fitted in pseudo-first order kinetic equation.
(6) Enhanced hydrolysis of the pesticides were the dominating process for the degradation of pesticides in sterile systems of biochar-soil mixture. The order of degradation ratio of the pesticides in biochar-soil mixing system was PBC>RBC> MBC, which was the same with the hydrolysis of pesticides in biochar suspensions. In unsterile systems, the chemical degradation and biodegradation co-existed, and the impact of biochar addition on the pesticide removal varied a lot. Generally, the addition of biochars enhanced pesticides removal, however, the enhancement extent and mechanism were different. Enhanced hydrolysis of pesticides was the main degradation in the system containing higher dose of biochars pyrolyzed at higher temperature due to the elevated pH of the system, which is favorable for hydrolysis and unfavorable for the growth of microorganisms. However, degradation of pesticides were reduced due to the lowered bioavailability by adsorption in the system containing higher dose of biochars pyrolyzed at lower temperature. However, biodegradation were increased in the system amended with MBC containing more organic carbon, which could supply more nutrition to microorganisms and did not change pH too much. Mixed floras were obtained by screening from activated sludge, and the degradation of carbaryl by the mixed flora was stronger than that of atrazine. The40d degradation ratio of carbaryl was enhanced to79.8%in the soil bioaugmented with the mixed flora; while the degradation ratio ranged in64.9%-82.9%when amended by biochars. Both enhancement and inhibitory occurred by different biochars, and similar results were acquired for atrazine. This is due to that biochars could simultaneously affect the hydrolysis, the growth of microorganisms, and the bioavailability of the pesticides.
本论文系统研究了不同结构生物炭对两种典型农药一阿特拉津和西维因的吸附、水解及微生物降解等环境行为的影响及其微观机制。首先,利用猪粪、玉米秸秆、水稻秸秆等三种农业废弃物,通过不同的热解温度制备了物质组成和结构不同的生物炭并对生物炭进行了除灰处理,得到性质各异生物炭十余种,对不同生物炭的有机与无机部分的含量、化学组成与结构特征；孔性质与比表面积等性质进行了表征。在此基础上,研究了不同种类生物炭对两种农药的吸附作用机理,深入探讨了生物炭有机部分、无机部分、孔结构及生物碳表面化学作用等在吸附过程中所起的作用。研究了不同种类生物炭对两种农药的水解催化作用,通过逐步分析背景溶液,生物炭悬浊液以及生物炭浸出液中农药的水解,从OH-、表面矿物以及金属离子等方面探讨生物炭促进农药水解的机理。研究了生物炭对土壤中农药降解的影响,并向生物炭与土壤混合体系中接种筛选的对农药降解特异性微生物菌群,以促进土壤中农药的生物降解,通过不同的实验设计,综合分析了生物炭对土壤中农药去除的影响及途径。通过以上研究得到以下结论：
(1)生物炭由脂肪炭和芳香碳组成的有机部分,以及磷酸盐、碳酸盐和其他无机矿物组成的无机部分共同构成。有机碳表面含有羟基,羧基以及羰基等基团。不同原料和温度制备的生物炭物质组成和结构有较大差异。猪粪制备的生物炭含有较高的灰分,而秸秆制备的生物炭灰分较低,且温度越高灰分含量越多。而高温使生物炭孔比例增加,比表面积显著升高。
(2)生物炭可有效地吸附西维因,吸附等温线符合Freundlich方程,且吸附表现为非线性。低浓度时,初级生物炭有机碳标化分配系数(Koc)为10265-104.48L/kg。除灰后生物炭的吸附性能显著提高,低浓度时Koc为103·64-104.74L/kg。不同来源和温度制备的生物炭组成和结构具有差异性,其对西维因的吸附能力和吸附机制不同。猪粪生物炭(PBC)中无机部分对吸附的综合作用表现为阻碍作用；而玉米秸秆生物炭(MBC)和水稻秸秆生物炭(RBC)中无机部分在低温时表现为阻碍作用,而高温时表现出促进作用。生物炭对西维因的吸附是疏水性作用、孔填充作用、无机灰分以及特殊作用力等综合作用的结果,生物炭对西维因的吸附亲和性与生物碳的极性,芳香度以及疏水基团等单一因素没有明显的相关性。
(3)生物炭对阿特拉津的等温吸附也表现为非线性吸附,但吸附亲和能力要弱于对西维因的吸附。高浓度时初级生物炭的Koc为101.90-103.10L/kg。除灰后生物炭的吸附性能显著提高,高浓度时Koc为102.63-103.10L/kg。生物炭对阿特拉津的吸附是疏水性作用、孔填充作用、无机灰分以及特殊作用力等综合作用。与生物炭对西维因的吸附作用类似,生物炭对阿特拉津的吸附亲和与生物炭的极性没有明显的相关性。
(4)西维因在碱性(pH=9.1)条件下水解迅速,18h就水解80%以上；而在中性条件下较稳定。不同生物炭悬浊液中西维因的水解差异很大,7d水解率为21.9%-90.6%,西维因在生物炭悬浊液中的水解与体系pH呈正相关。除了pH对于水解的催化作用外,生物炭表面矿物以及释放到溶液中的过渡金属离子都可促进水解,而吸附降低了西维因分子的可及性,减弱水解。西维因在各生物炭实验组中的水解动力学过程大部分符合拟一级过程。
(5)阿特拉津在环境中较稳定,在碱性(pH=9.1)条件下,7d水解率仅为16.1%。阿特拉津在生物炭悬浊液中的水解程度比西维因弱,7d仅水解了2.6%-63.4%。阿特拉津的水解与生物炭的无机部分含量呈正相关。阿特拉津在生物炭悬浊液中的水解主要受生物炭表面和pH的影响,而金属离子的对水解的贡献较差。阿特拉津在各生物炭实验体系中的水解动力学过程大部分符合拟一级动力学。
(6)在灭菌的生物炭-土壤体系中,土壤pH升高,农药的降解主要是生物炭的催化水解作用。土壤中农药的降解趋势表现为PBC>RBC>MBC,与悬浊液中农药的水解趋势类似。未灭菌体系中,化学降解与微生物降解并存,添加高含量的高温生物炭的土壤pH的升高更显著,催化了水解,降低了土著微生物的降解能力,因此,农药的降解主要为水解。而添加高含量的低温生物炭的土壤,吸附作用降低了农药的生物有效性,对土壤中农药的降解有阻碍作用。而添加有机碳含量高的MBC,对土壤pH改变较小,为微生物提供所需的营养物质,促进微生物生长,提高了降解能力。活性污泥筛选的农药降解菌群能够有效地降解西维因和阿特拉津,且西维因降解菌群的降解能力强于阿特拉津降解菌群。加入外源微生物的土壤中,西维因40d降解率为79.8%；而添加微生物的土壤-生物炭体系,降解率为64.9%-82.9%,不同的生物炭分别表现出促进和抑制作用；对于阿特拉津也有同样的规律,这是生物炭影响水解、微生物生长以及化合物生物有效性的综合结果。
Biochars are materials produced by pyrolyzing biomass under limited oxygen. Due to its promising feature in recycling biomass waste, attenuating climate change, and improving soil fertility, biochar has quickly become a research hotspot as a novel functional material with multiple applications. Due to the highly porous structure and aromaticity, biochars show great adsorptive capacity for various pollutants, and hence influencing their environmental behavior, fate, and eco-risk.
The present thesis systematically studied the impacts and mechanisms behind on the adsorption, hydrolysis, and biodegradation of two typical pesticides, carbaryl and atrazine, by different biochars. To do so, different biochars with varied composition and structure, were derived from pig-manure, maize straw, and rice straw under different pyrolysis temperatures, and the present biochars were further deashed by acid. The structure characteristics, such as the content and constitutes of organic and inorganic moieties, specific surface area and pore structure, and chemical surface functional groups,were measured. Moreover, the adsorption of the two pesticides on the original biochars and deashed biochars were studied, and relationships between adsorption affinity and structural parametersof biochars were analyzed to elucidate their functions in adsorption. The hydrolysis of carbaryl and atrazine were studied in suspensions of different biochars. The mechanism of the catalytic hydrolysis were discussed by analyzing the effects of elevated solution pH, mineral surface, and dissolvedmetal ions step by step. Finally, the degradation of pesticides in soil amended withbiochars were studied under different designs. Exogenous mixed bacteriawere added to strengthen the biodegradation of the pesticides. The influence and pathways behind of biochars on pesticide removal were discussed. Through theresearchabove, some main results obtainedwere as followed:
(1) The biochars consisted of organic moiety including aliphatic carbon and aromatic carbon and inorganic moiety containing phosphate, carbonate, and other minerals. In addition, chemical functional groups, such as hydroxyl, carboxyl and carbonyl, also bound on the surface of bio chars. Great difference existed in composition and structure of various biochars derived from different feedstocks and temperatures. Biochars derived from pig-manure contained high content of ash, however, biochars derived from straws had low ash contents, and biochars derived from maize straw contained lower ash than that those derived from rice straw. The ash contents of biochars increased with elevated pyrolyzing temperature. Porosity and specific surface area also increased with increasing temperature.
(2) Carbaryl could be adsorbed efficiently by biochars. Adsorption isotherms were fitted by Freundlich equation with distict nonlinearity. In prisent biochars, the distribution coefficients normalized by organic carbon content (Koc) of biochars were102.65-104.48L/kg at low solute concentration. When the ash was removed, adsorption increased generally,the distribution coefficients normalized by organic carbon content (Koc) of biochars were103.64-104.74L/kg at low solute concentration Differences in composition and structure of biochars derived from different feedstocks and temperatures led to the differences in adsorption affinity and mechanism of the various biochars. Inorganic moiety of the biochars derived from pig-manure (PBC) had an apparently negative effect on adsorption. The inorganic moiety of biochars derived from maize straw (MBC) and rice straw (RBC) under low pyrolyzing temperature had negative effect on adsorption, however, that of MBC and RBC obtained under high pyrolyzing temperature had positive effect. Overall, the adsorption of carbaryl on biochar was controlled by hydrophobic effect, pore-filling effect, effects with inorganic ash and specific effect. No significant correlation could be found between adsorption affinity with any of single parameters of polarity, aromaticity, and hydrophobic functional groups.
(3) Adsorption isotherms of atrazine on biochars were fitted in Freundlich equation and displayed nonlinear trends. The Koc of biochars werel01.90-103.10L/kg at high solute concentration. After deashing treatment, The Koc of deashed biochars were102.63-103.10L/kg at high solute concentration. Mechanism of adsorption of atrazine on biochars was also a combination of hydrophobic effect, pore-filling effect, effects with inorganic moiety and specific effects. In addition, no significant correlation between polarity of biochars and adsorption affinity could be found for atrazine either.
(4) Rapid hydrolysis of carbaryl occurred in alkaline (pH=9.1) background solution with over80%lost in18h, however, it was stable in neutral background solution. Hydrolysis of carbaryl in suspensions of biochars varied a lot with7d hydrolysis ratio ranging from21.9%to90.6%, and biochars influenced hydrolysis through different ways. We found a positive correlation between carbaryl hydrolysis and the pH of the suspensions. Beside pH, surface minerals, metal ions, and adsorption of biochars also influenced hydrolysis ratio, with the former two factors having catalyzing effect and the latter one showing inhibitory effect. The hydrolysis of carbaryl in majority of the tested systems were fitted in pseudo-first order kinetic equation.
(5) Hydrolysis of atrazine only occurred in strong alkaline background solution, and only16.1%of atrazine was hydrolyzed at pH of9.1. The hydrolysis of atrazine in suspensions of biochars were generally weaker than those of carbaryl with7d hydrolysis ratio ranging from2.6%to63.4%. The hydrolysis of atrazine was positive correlated with the quantity of inorganic moiety, and surface minerals and carboxylic groups could enhance the OH" catalyzed hydrolysis of atrazine by forming H-bond with atrazine. The hydrolysis of atrazine in the suspensions of biochars were mainly influenced by mineral surface and solution pH, and the contribution of metal ions was very low. The hydrolysis of atrazine in majority of the tested systems were fitted in pseudo-first order kinetic equation.
(6) Enhanced hydrolysis of the pesticides were the dominating process for the degradation of pesticides in sterile systems of biochar-soil mixture. The order of degradation ratio of the pesticides in biochar-soil mixing system was PBC>RBC> MBC, which was the same with the hydrolysis of pesticides in biochar suspensions. In unsterile systems, the chemical degradation and biodegradation co-existed, and the impact of biochar addition on the pesticide removal varied a lot. Generally, the addition of biochars enhanced pesticides removal, however, the enhancement extent and mechanism were different. Enhanced hydrolysis of pesticides was the main degradation in the system containing higher dose of biochars pyrolyzed at higher temperature due to the elevated pH of the system, which is favorable for hydrolysis and unfavorable for the growth of microorganisms. However, degradation of pesticides were reduced due to the lowered bioavailability by adsorption in the system containing higher dose of biochars pyrolyzed at lower temperature. However, biodegradation were increased in the system amended with MBC containing more organic carbon, which could supply more nutrition to microorganisms and did not change pH too much. Mixed floras were obtained by screening from activated sludge, and the degradation of carbaryl by the mixed flora was stronger than that of atrazine. The40d degradation ratio of carbaryl was enhanced to79.8%in the soil bioaugmented with the mixed flora; while the degradation ratio ranged in64.9%-82.9%when amended by biochars. Both enhancement and inhibitory occurred by different biochars, and similar results were acquired for atrazine. This is due to that biochars could simultaneously affect the hydrolysis, the growth of microorganisms, and the bioavailability of the pesticides.
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