微波热解污水污泥过程中氮转化途径及调控策略
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摘要
微波高温热解污水污泥具有污泥高效减容、重金属有效固定、副产物资源利用等优点，引起了国内外学者的高度关注。污泥中50%-80%的N在高温热解过程中转化为含氮气体，降低了生物燃气品质，造成了环境的二次污染。本文考察了含氮污染气体生成的影响因素，构建了切合污泥化学组分和官能团特征的含氮模型化合物，解析了污水污泥微波热解过程含氮化合物转化途径，明确了矿物添加剂抑制含氮污染气体产生机制并提出含氮污染气体选择性转化生成N2的污染控制措施。
本研究通过序批实验考察了微波热解污水污泥过程失重规律，结果表明微波热解过程中蛋白质、糖类和脂类有机物的分解反应阶段相互叠加，而传统热解过程中三类有机物的分解反应呈现明显的三阶段特征。利用FTIR分析了气态含氮化合物的主要成分，结果显示NH_3和HCN是主要气态含氮化合物，两者含量分别占含氮气体总量的70%和10%。考察了热解终温、污泥含水率、升温速率和微波能吸收物质对NH_3和HCN产率的影响，实验结果表明热解温度、升温速率、污泥含水率和微波能吸收物质是影响NH_3和HCN形成的主要因素。微波热解污泥过程中，热解终温、升温速率和污泥含水率的增加均促进NH_3和HCN的生成。
XPS分析表明污泥氮的主要存在形式为无机铵态氮，蛋白质氮和碱性杂环氮（吡咯和吡啶），定量分析表明蛋白质氮是污泥氮的主要存在形式，其含量占污泥总氮含量的90%。采用异硫氰酸苯酯（PITC）柱前衍生化反相高效液相色谱法（RP-HPLC）检测污泥蛋白质氨基酸组成及含量，结果表明精氨酸、甘氨酸、脯氨酸等八种氨基酸的含量占到氨基酸总量的82%以上。利用谷氨酸、精氨酸、赖氨酸、脯氨酸、苏氨酸、丙氨酸、亮氨酸和甘氨酸构建了理论模型化合物，各组分质量比为15：6：6：16：21：6：21：9，同时根据污泥氨基酸组成和比例相似原则筛选出又一种有机聚合肽链形式的大豆蛋白模型化合物。通过对两种含氮模型化合物的微波热解产气特性对比发现，大豆蛋白与脱灰污泥的含氮气体产率相似度>80%，大豆蛋白作为污泥含氮模型化合物更合理。微波热解大豆蛋白模型化合物发现了三种重要含氮中间产物，分别为胺态氮、含氮杂环和腈类氮化合物。微波热解模型化合物的氮转化途径分析表明，三类中间产物贡献了97%以上的（NH_3+HCN）总产量。
利用XPS、GC-MS等分析手段，研究了含氮官能团在微波热解污水污泥三相产物中的转化规律，并分析了微波热解污泥过程中含氮化合物的转化途径。在温度低于300℃时，污泥中的无机氮和小部分的蛋白质氮分解生成NH_3。在300-500℃时，污泥中大量的蛋白质热裂解生成了焦油中的胺类化合物，并伴随着大量NH_3生成。500-800℃时，焦油中的胺态-N大量裂解生成含氮杂环-N和腈类-N化合物，并伴随着NH_3和HCN的大量产生。微波热解污水污泥NH_3和HCN生成途径分析表明，污泥热解过程中的二次裂解反应是生成NH_3和HCN的主要途径，胺态氮、含氮杂环和腈类氮化合物的裂解反应贡献了热解全部（HCN+NH_3）产量的80%以上，因此可以考虑通过控制三类含氮中间产物的产生来减少NH_3和HCN的释放。
通过对比污水污泥和酸洗脱灰污泥的热解产气特性，确定了污泥内在矿物质对NH_3和HCN生成的抑制作用。考察了外加矿物质种类、添加量及加载方式对NH_3和HCN产率的影响，结果表明添加量20%的Fe2O3和CaO对NH_3和HCN的抑制效果分别达到50%和80%。与直接机械混合法相比，化学沉淀法加载Fe盐对含氮气体抑制效果更好。GC-MS分析了污水污泥和矿物质污泥的热解气态和焦油产物组分，发现了矿物质不影响300-500℃阶段胺态氮化合物的生成反应，而抑制了500-800℃阶段含氮杂环-N和腈类-N化合物的生成过程，导致焦油中含氮杂环-N和腈类-N化合物含量大量减少，继而使得含氮杂环-N和腈类-N化合物热解生成的HCN含量大量下降。铁和钙元素结合含氮中间产物生成一种Fe-N-Ca络合物质，微波非热效应降低了此反应的活化能，因而促进NH_3和HCN生成N_2和H_2。
Microwave pyrolysis is considered as a potential alternative technology due to itseffective reduction of sludge, stability of heavy metals and high added value ofbyproducts. However,50%-80%of nitrogen in the sludge is converted to thenitrogen-containing gases during microwave pyrolysis of sewage sludge, reducing thequality of bio-gas and causing secondary pollution of environment. This paper discussedthe influences of process conditions on the formation of NH_3and HCN, built thenitrogen-containing model compounds meeting sludge characteristics and investigatedthe nitrogen conversion pathways during microwave pyrolysis of sewage sludge. Theinhibition mechanism of inorganic additives on the formation of NH_3and HCN was alsoconducted and the strategies for the selective conversion of NH_3and HCN into N2wereproposed.
The thermogravimetric analysis was conduced by the batch experiments, indicatingthat the thermal decomposition reactions of protein, carbohydrate and lipid occurredsimultaneously in the microwave pyrolysisin comparison with the conventionalpyrolysis system. FTIR analysis showed that NH_3and HCN were the majornitrogen-containing gases accounting for about70%and10%of total gas-N yields,respectively. The influences of temperature, moisture content of sludge, heating rate andmicrowave absorbers on the formation of NH_3and HCN during microwave pyrolysis ofsewage sludge were stuied. The results showed that NH_3and HCN yields increased withthe increase of temperature, heating rate, moisture content of sludge during pyrolysis.
XPS analysis showed that the inorganic ammonium nitrogen, protein nitrogen andheterocyclic nitrogen (pyrrole and pyridine) were the main nitrogen functionalities inthe sludge. The steam distillation and Kjeldahl nitrogen determination analysis revealedthat the protein nitrogen was the major nitrogen form in the sludge, accounting foraround90%of total nitrogen in sewage sludge. PITC-RP-HPLC analysis showed thatthe contents of nine kinds of amino acids, such as arginine, glycine, proline and so on,accounted for above82%of the total. A theoretical model compound of arginine: lysine:proline: threonine: alanine: leucine: glycine=15:6:6:16:21:6:21:9was establishedaccording to their pyrolysis characteristics. Meanwhile, an organic polymeric peptidechain model compound soybean protein was selected according to the similar sludgeamino acid compositions. Microwave pyrolysis of two nitrogen-containing modelcompounds showed that the soybean protein was more proper as the sludge-N modelcompound. Three important intermediates, including the amine-N, heterocyclic-N andnitrile-N compounds, were identified during microwave pyrolysis of soybean proten,which contributed to more than97%of the total (NH_3+HCN) productions.
The nitrogen distributions and evolution of nitrogen functionalities in the char, tarand gas fractions were conducted by XPS and GC-MS. The nitrogen conversions inrelation to NH_3and HCN were investigated during microwave pyrolysis of sewagesludge. At temperatures below300℃, the thermal decomposition of inorganic nitrogencompounds contributed to the release of NH_3. In the temperature ranges of300-500℃,the thermal cracking of labile proteins contributed to the formation of amine-Ncompounds in the tars further generating NH_3. The cracking of nitrile-N andheterocyclic-N compounds resulted from the dehydrogenation and polymerization ofamine-N compounds led to the formation of NH_3and HCN at temperatures of500-800℃. The analysis on nitrogen conversin mechanism revealed that the secondarycracking reactions was the major pathway for the production of NH_3and HCN duringthe sludge pyrolysis. Specifically, the cracking of amine-N, heterocyclic-N and nitrile-Ncompounds contributed to above80%of the total (HCN+NH_3) productions.Consequently, it was considered that it might be able to reduce the NH_3and HCNemissions by controlling the production of three nitrogen-containing intermediates.
Conparing the release of gas-N by pyrolysis of sewage sludge and demineralizedsludge, the inhibition of the intrinsic minerals on the formation of NH_3and HCN wasconfirmed. The experiments on the added mineral species, mineral/sludge ratio andloaded methods demonstrated that addition of20%Fe2O3and20%CaO in the sludgecould inhibited the formation NH_3and HCN by approximately50%and80%,respectively. Additionally, compared with the direct mixing method, the chemicalprecipitation loading of Fe salt possessed better inhibitory effect on thenitrogen-containing gases. GC-MS analysis on the tar-N compositions produced frommicrowave pyrolysis of sewage sludge and minerals added sludge showed that mineralsdid not inhibit the formation of amine-N compounds (300-500℃), while inhibit theformation of heterocyclic-N and nitrile-N compounds (500-800℃). Thus, this resultedin the significant decrease of heterocyclic-N and nitrile-N compounds, leading to thedecline of HCN yields during pyrolysis. The formation of N2was ascribed to theintermediate mechanism in the presence of inorganic minerals (such as the interstitial Feand Ca nitride species). The non-thermal microwave effects directly coupled to energymodes within the molecules and caused the reactive molecular oscillation and rotationreducing the reaction activation energy. As a consequence, the microwave irradiationpromoted higher productions of N2.
本研究通过序批实验考察了微波热解污水污泥过程失重规律，结果表明微波热解过程中蛋白质、糖类和脂类有机物的分解反应阶段相互叠加，而传统热解过程中三类有机物的分解反应呈现明显的三阶段特征。利用FTIR分析了气态含氮化合物的主要成分，结果显示NH_3和HCN是主要气态含氮化合物，两者含量分别占含氮气体总量的70%和10%。考察了热解终温、污泥含水率、升温速率和微波能吸收物质对NH_3和HCN产率的影响，实验结果表明热解温度、升温速率、污泥含水率和微波能吸收物质是影响NH_3和HCN形成的主要因素。微波热解污泥过程中，热解终温、升温速率和污泥含水率的增加均促进NH_3和HCN的生成。
XPS分析表明污泥氮的主要存在形式为无机铵态氮，蛋白质氮和碱性杂环氮（吡咯和吡啶），定量分析表明蛋白质氮是污泥氮的主要存在形式，其含量占污泥总氮含量的90%。采用异硫氰酸苯酯（PITC）柱前衍生化反相高效液相色谱法（RP-HPLC）检测污泥蛋白质氨基酸组成及含量，结果表明精氨酸、甘氨酸、脯氨酸等八种氨基酸的含量占到氨基酸总量的82%以上。利用谷氨酸、精氨酸、赖氨酸、脯氨酸、苏氨酸、丙氨酸、亮氨酸和甘氨酸构建了理论模型化合物，各组分质量比为15：6：6：16：21：6：21：9，同时根据污泥氨基酸组成和比例相似原则筛选出又一种有机聚合肽链形式的大豆蛋白模型化合物。通过对两种含氮模型化合物的微波热解产气特性对比发现，大豆蛋白与脱灰污泥的含氮气体产率相似度>80%，大豆蛋白作为污泥含氮模型化合物更合理。微波热解大豆蛋白模型化合物发现了三种重要含氮中间产物，分别为胺态氮、含氮杂环和腈类氮化合物。微波热解模型化合物的氮转化途径分析表明，三类中间产物贡献了97%以上的（NH_3+HCN）总产量。
利用XPS、GC-MS等分析手段，研究了含氮官能团在微波热解污水污泥三相产物中的转化规律，并分析了微波热解污泥过程中含氮化合物的转化途径。在温度低于300℃时，污泥中的无机氮和小部分的蛋白质氮分解生成NH_3。在300-500℃时，污泥中大量的蛋白质热裂解生成了焦油中的胺类化合物，并伴随着大量NH_3生成。500-800℃时，焦油中的胺态-N大量裂解生成含氮杂环-N和腈类-N化合物，并伴随着NH_3和HCN的大量产生。微波热解污水污泥NH_3和HCN生成途径分析表明，污泥热解过程中的二次裂解反应是生成NH_3和HCN的主要途径，胺态氮、含氮杂环和腈类氮化合物的裂解反应贡献了热解全部（HCN+NH_3）产量的80%以上，因此可以考虑通过控制三类含氮中间产物的产生来减少NH_3和HCN的释放。
通过对比污水污泥和酸洗脱灰污泥的热解产气特性，确定了污泥内在矿物质对NH_3和HCN生成的抑制作用。考察了外加矿物质种类、添加量及加载方式对NH_3和HCN产率的影响，结果表明添加量20%的Fe2O3和CaO对NH_3和HCN的抑制效果分别达到50%和80%。与直接机械混合法相比，化学沉淀法加载Fe盐对含氮气体抑制效果更好。GC-MS分析了污水污泥和矿物质污泥的热解气态和焦油产物组分，发现了矿物质不影响300-500℃阶段胺态氮化合物的生成反应，而抑制了500-800℃阶段含氮杂环-N和腈类-N化合物的生成过程，导致焦油中含氮杂环-N和腈类-N化合物含量大量减少，继而使得含氮杂环-N和腈类-N化合物热解生成的HCN含量大量下降。铁和钙元素结合含氮中间产物生成一种Fe-N-Ca络合物质，微波非热效应降低了此反应的活化能，因而促进NH_3和HCN生成N_2和H_2。
Microwave pyrolysis is considered as a potential alternative technology due to itseffective reduction of sludge, stability of heavy metals and high added value ofbyproducts. However,50%-80%of nitrogen in the sludge is converted to thenitrogen-containing gases during microwave pyrolysis of sewage sludge, reducing thequality of bio-gas and causing secondary pollution of environment. This paper discussedthe influences of process conditions on the formation of NH_3and HCN, built thenitrogen-containing model compounds meeting sludge characteristics and investigatedthe nitrogen conversion pathways during microwave pyrolysis of sewage sludge. Theinhibition mechanism of inorganic additives on the formation of NH_3and HCN was alsoconducted and the strategies for the selective conversion of NH_3and HCN into N2wereproposed.
The thermogravimetric analysis was conduced by the batch experiments, indicatingthat the thermal decomposition reactions of protein, carbohydrate and lipid occurredsimultaneously in the microwave pyrolysisin comparison with the conventionalpyrolysis system. FTIR analysis showed that NH_3and HCN were the majornitrogen-containing gases accounting for about70%and10%of total gas-N yields,respectively. The influences of temperature, moisture content of sludge, heating rate andmicrowave absorbers on the formation of NH_3and HCN during microwave pyrolysis ofsewage sludge were stuied. The results showed that NH_3and HCN yields increased withthe increase of temperature, heating rate, moisture content of sludge during pyrolysis.
XPS analysis showed that the inorganic ammonium nitrogen, protein nitrogen andheterocyclic nitrogen (pyrrole and pyridine) were the main nitrogen functionalities inthe sludge. The steam distillation and Kjeldahl nitrogen determination analysis revealedthat the protein nitrogen was the major nitrogen form in the sludge, accounting foraround90%of total nitrogen in sewage sludge. PITC-RP-HPLC analysis showed thatthe contents of nine kinds of amino acids, such as arginine, glycine, proline and so on,accounted for above82%of the total. A theoretical model compound of arginine: lysine:proline: threonine: alanine: leucine: glycine=15:6:6:16:21:6:21:9was establishedaccording to their pyrolysis characteristics. Meanwhile, an organic polymeric peptidechain model compound soybean protein was selected according to the similar sludgeamino acid compositions. Microwave pyrolysis of two nitrogen-containing modelcompounds showed that the soybean protein was more proper as the sludge-N modelcompound. Three important intermediates, including the amine-N, heterocyclic-N andnitrile-N compounds, were identified during microwave pyrolysis of soybean proten,which contributed to more than97%of the total (NH_3+HCN) productions.
The nitrogen distributions and evolution of nitrogen functionalities in the char, tarand gas fractions were conducted by XPS and GC-MS. The nitrogen conversions inrelation to NH_3and HCN were investigated during microwave pyrolysis of sewagesludge. At temperatures below300℃, the thermal decomposition of inorganic nitrogencompounds contributed to the release of NH_3. In the temperature ranges of300-500℃,the thermal cracking of labile proteins contributed to the formation of amine-Ncompounds in the tars further generating NH_3. The cracking of nitrile-N andheterocyclic-N compounds resulted from the dehydrogenation and polymerization ofamine-N compounds led to the formation of NH_3and HCN at temperatures of500-800℃. The analysis on nitrogen conversin mechanism revealed that the secondarycracking reactions was the major pathway for the production of NH_3and HCN duringthe sludge pyrolysis. Specifically, the cracking of amine-N, heterocyclic-N and nitrile-Ncompounds contributed to above80%of the total (HCN+NH_3) productions.Consequently, it was considered that it might be able to reduce the NH_3and HCNemissions by controlling the production of three nitrogen-containing intermediates.
Conparing the release of gas-N by pyrolysis of sewage sludge and demineralizedsludge, the inhibition of the intrinsic minerals on the formation of NH_3and HCN wasconfirmed. The experiments on the added mineral species, mineral/sludge ratio andloaded methods demonstrated that addition of20%Fe2O3and20%CaO in the sludgecould inhibited the formation NH_3and HCN by approximately50%and80%,respectively. Additionally, compared with the direct mixing method, the chemicalprecipitation loading of Fe salt possessed better inhibitory effect on thenitrogen-containing gases. GC-MS analysis on the tar-N compositions produced frommicrowave pyrolysis of sewage sludge and minerals added sludge showed that mineralsdid not inhibit the formation of amine-N compounds (300-500℃), while inhibit theformation of heterocyclic-N and nitrile-N compounds (500-800℃). Thus, this resultedin the significant decrease of heterocyclic-N and nitrile-N compounds, leading to thedecline of HCN yields during pyrolysis. The formation of N2was ascribed to theintermediate mechanism in the presence of inorganic minerals (such as the interstitial Feand Ca nitride species). The non-thermal microwave effects directly coupled to energymodes within the molecules and caused the reactive molecular oscillation and rotationreducing the reaction activation energy. As a consequence, the microwave irradiationpromoted higher productions of N2.
引文
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