磷在固体废物热处理过程中的迁移转化及再利用
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摘要
固体废物的热解和焚烧等热化学处理技术不仅可以大量削减废物总量,还能够实现其资源化利用。固体废物中含有不同比例的营养元素,其中磷是一个不可再生的营养元素,因而备受关注。它在热解产物中的分布和形态以及转化机制关系到它的再利用途径。本论文以污泥和塑料固体废物为研究对象,探索了磷在热化学处理过程中的迁移转化行为,并研究了热化学处理固体产物中的磷在环境中的释放规律。论文主要研究结果如下：
1.污泥经过热解或焚烧之后,其产物SSC/A中磷的形态较污泥中有显著的变化。热处理温度是影响这一变化的主要因素,而热处理氛围的影响相对很小。我们通过逐级提取,通过31P-NMR和XRD表征发现：在低温(400-600℃)热解的条件下,污泥中的磷倾向于转化为较为稳定的NaOH-P(主要为吸附在铝铁化合物上的磷)；而在高温条件下(700-800℃),污泥中的磷倾向于转化为更为稳定的HC1-P(即Ca、Mg-P的化合物)。
2.通过对磷酸三(丁氧基乙基)酯与木质素的共热解研究发现,在快速热解条件下,温度对生物炭上磷的分配比例(即生物炭上的磷占原始进料中磷的比例)起着关键作用,热解温度越高(从400到600℃),生物炭上磷的分配比例越低(从76.6%到51%)；在慢速热解条件下,生物炭中磷的比例几乎不受温度影响,且均在70%以上；CaCl2和MgCl2在热解过程中与磷生成Ca、Mg-P的化合物,从而显著增强生物炭对磷的固定作用。通过XPS表征,我们发现生物炭中磷的形态主要有正磷、焦磷(或P4O10)、以及一系列与生物炭上芳环相连的磷(Ar-P),其中以Ar-P最为稳定,很难被普通溶剂提取。快速热解的生物炭中可提取磷的比例要低于慢速热解生物炭中的磷的可提取比例,这是由于慢速热解生物炭上Ar-P含量高于快速热解的Ar-P含量的缘故。通过TG/FTIR/MS的分析,可以推断磷酸三(丁氧基乙基)酯和木质素热解中间产物之间的反应是导致磷固定在生物炭上的主要原因。
3.稻壳生物炭(磷含量为4.7mg Pg-1)中含有不同形态的含磷化合物,利用生物炭-水的释放体系,并结合实际的土壤环境条件研究了生物炭中磷在不同环境条件下的释放规律。结果显示,在纯水中(平衡pH值约为9.0)约有一半的磷在8h之内释放出来,所释放的磷的形态为正磷和焦磷；共存阴离子(Cl、NO3-或SO42-)能够促进正磷的释放,这是由阴离子之间的竞争作用和溶液中升高的离子强度导致的；然而,由于焦磷能够在溶液中形成稳定的配合物,其释放并不受共存阴离子的影响。霍格兰德营养液对磷的释放起到抑制作用,这是由于霍格兰德营养液中过剩的Ca2+、Mg2+和NH4+离子与生物炭释放的含磷化合物反应形成沉淀所致。
Thermal processing (pyrolysis or incineration) of solid wastes can substantially reduce the waste volume and simultaneously properly reuse the energy and resource contained in wastes. Phosphorus, one of the most important and nonrenewable nutrient elements contained in solid wastes, has received more interests. The distribution and form of P in biochar or ash (the solid product derived from the thermal treatment of solid wastes) are essential for the disposal (reutilization) of biochar or ash. Herein, the thermochemical behaviors of P in different solid wastes (e.g., sewage sludge and plastics) in thermal treatment were investigated. Moreover, the release of P from biochar of rice husk to the environment was also explored and the environmental factors affecting the release of P were evaluated.
1. Investigations into the transformation and migration of P in the sewage sludge under various thermal treatment conditions show that the temperature significantly influenced the species and content of P in the sewage sludge char or ash (SSC/A), while the atmosphere of thermal treatment had a slight effect on the fate of P. The sequential extraction,31P-NMR, and XRD analysis indicate that P was mainly migrated to the medium-term plant available P pool (poolNaOH) when treating the sewage sludge at low temperatures (400-600℃), while it was migrated to long-term plant available P pool (poolhcl) when treated at high temperatures (700-800℃).
2. To investigate the behaviors. of tris(2-butoxyethyl) phosphate (TBEP) in co-pyrolysis, the mixture of TBEP and lignin was used to simulate the feedstock of the co-pyrolysis of wood biomass and waste plastics. In fast pyrolysis, the proportion of P distributed in char was significantly influenced by temperature. With an increase in temperature (400-500℃), the proportion of P distributed in char decreased from76.6%to51%. In slow pyrolysis, temperature had little effect on the proportion of P in char (all of them exceeded70%). The dose of CaCl2and MgCl2could significantly increase the P distributed in char through the formation of Ca, Mg-P compounds. The XPS analysis shows that the P species in char were orthophosphate, pyrophosphate (or P4O10), and the P associated with the aromatic rings in char (Ar-P), among which Ar-P was the most stable species and hardly to be extracted. Compared with the P in the char produced in fast pyrolysis, the P in the char derived from the slow pyrolysis could hardly be extracted, which was caused by the higher Ar-P content in the char of slow pyrolysis. The TG/FTIR/MS analysis suggests that the thermochemical reactions between the intermediates of both lignin and TBEP were responsible for the diversity of the P species in chars.
3. The effects of environmental (soil) conditions on the release of different P species from rice husk biochar in a biochar-water system were explored. About2.2mg g-1P in the form of inorganic orthophosphate and pyrophosphate was released from a raw biochar (contained4.7mg P g-1) at initial pH of9.0in the initial8h. The release of orthophosphate was significantly enhanced by the coexisting anions of Cl-, NO3-or SO42-, attributed to the effect of ion exchange competition and the elevated ionic strength, while the release of pyrophosphate (P2O74-) was not influenced by the introduction of anions, which might be attributed to the formation of stable complexes. The introduction of Hoagland nutrient solution led to the decrease in release of P due to the formation of precipitates between dissolved P and excessive Ca2+, Mg2+, and NH4+.
1.污泥经过热解或焚烧之后,其产物SSC/A中磷的形态较污泥中有显著的变化。热处理温度是影响这一变化的主要因素,而热处理氛围的影响相对很小。我们通过逐级提取,通过31P-NMR和XRD表征发现：在低温(400-600℃)热解的条件下,污泥中的磷倾向于转化为较为稳定的NaOH-P(主要为吸附在铝铁化合物上的磷)；而在高温条件下(700-800℃),污泥中的磷倾向于转化为更为稳定的HC1-P(即Ca、Mg-P的化合物)。
2.通过对磷酸三(丁氧基乙基)酯与木质素的共热解研究发现,在快速热解条件下,温度对生物炭上磷的分配比例(即生物炭上的磷占原始进料中磷的比例)起着关键作用,热解温度越高(从400到600℃),生物炭上磷的分配比例越低(从76.6%到51%)；在慢速热解条件下,生物炭中磷的比例几乎不受温度影响,且均在70%以上；CaCl2和MgCl2在热解过程中与磷生成Ca、Mg-P的化合物,从而显著增强生物炭对磷的固定作用。通过XPS表征,我们发现生物炭中磷的形态主要有正磷、焦磷(或P4O10)、以及一系列与生物炭上芳环相连的磷(Ar-P),其中以Ar-P最为稳定,很难被普通溶剂提取。快速热解的生物炭中可提取磷的比例要低于慢速热解生物炭中的磷的可提取比例,这是由于慢速热解生物炭上Ar-P含量高于快速热解的Ar-P含量的缘故。通过TG/FTIR/MS的分析,可以推断磷酸三(丁氧基乙基)酯和木质素热解中间产物之间的反应是导致磷固定在生物炭上的主要原因。
3.稻壳生物炭(磷含量为4.7mg Pg-1)中含有不同形态的含磷化合物,利用生物炭-水的释放体系,并结合实际的土壤环境条件研究了生物炭中磷在不同环境条件下的释放规律。结果显示,在纯水中(平衡pH值约为9.0)约有一半的磷在8h之内释放出来,所释放的磷的形态为正磷和焦磷；共存阴离子(Cl、NO3-或SO42-)能够促进正磷的释放,这是由阴离子之间的竞争作用和溶液中升高的离子强度导致的；然而,由于焦磷能够在溶液中形成稳定的配合物,其释放并不受共存阴离子的影响。霍格兰德营养液对磷的释放起到抑制作用,这是由于霍格兰德营养液中过剩的Ca2+、Mg2+和NH4+离子与生物炭释放的含磷化合物反应形成沉淀所致。
Thermal processing (pyrolysis or incineration) of solid wastes can substantially reduce the waste volume and simultaneously properly reuse the energy and resource contained in wastes. Phosphorus, one of the most important and nonrenewable nutrient elements contained in solid wastes, has received more interests. The distribution and form of P in biochar or ash (the solid product derived from the thermal treatment of solid wastes) are essential for the disposal (reutilization) of biochar or ash. Herein, the thermochemical behaviors of P in different solid wastes (e.g., sewage sludge and plastics) in thermal treatment were investigated. Moreover, the release of P from biochar of rice husk to the environment was also explored and the environmental factors affecting the release of P were evaluated.
1. Investigations into the transformation and migration of P in the sewage sludge under various thermal treatment conditions show that the temperature significantly influenced the species and content of P in the sewage sludge char or ash (SSC/A), while the atmosphere of thermal treatment had a slight effect on the fate of P. The sequential extraction,31P-NMR, and XRD analysis indicate that P was mainly migrated to the medium-term plant available P pool (poolNaOH) when treating the sewage sludge at low temperatures (400-600℃), while it was migrated to long-term plant available P pool (poolhcl) when treated at high temperatures (700-800℃).
2. To investigate the behaviors. of tris(2-butoxyethyl) phosphate (TBEP) in co-pyrolysis, the mixture of TBEP and lignin was used to simulate the feedstock of the co-pyrolysis of wood biomass and waste plastics. In fast pyrolysis, the proportion of P distributed in char was significantly influenced by temperature. With an increase in temperature (400-500℃), the proportion of P distributed in char decreased from76.6%to51%. In slow pyrolysis, temperature had little effect on the proportion of P in char (all of them exceeded70%). The dose of CaCl2and MgCl2could significantly increase the P distributed in char through the formation of Ca, Mg-P compounds. The XPS analysis shows that the P species in char were orthophosphate, pyrophosphate (or P4O10), and the P associated with the aromatic rings in char (Ar-P), among which Ar-P was the most stable species and hardly to be extracted. Compared with the P in the char produced in fast pyrolysis, the P in the char derived from the slow pyrolysis could hardly be extracted, which was caused by the higher Ar-P content in the char of slow pyrolysis. The TG/FTIR/MS analysis suggests that the thermochemical reactions between the intermediates of both lignin and TBEP were responsible for the diversity of the P species in chars.
3. The effects of environmental (soil) conditions on the release of different P species from rice husk biochar in a biochar-water system were explored. About2.2mg g-1P in the form of inorganic orthophosphate and pyrophosphate was released from a raw biochar (contained4.7mg P g-1) at initial pH of9.0in the initial8h. The release of orthophosphate was significantly enhanced by the coexisting anions of Cl-, NO3-or SO42-, attributed to the effect of ion exchange competition and the elevated ionic strength, while the release of pyrophosphate (P2O74-) was not influenced by the introduction of anions, which might be attributed to the formation of stable complexes. The introduction of Hoagland nutrient solution led to the decrease in release of P due to the formation of precipitates between dissolved P and excessive Ca2+, Mg2+, and NH4+.
引文
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