氨基硅油的生态毒性及其在废水中的脱除与降解研究
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摘要
中国作为全球纺织品生产和消费大国,纺织印染产业在国民经济中占有重要地位。氨基硅油(Poly(dimethylaminostyrene), PDMAS)作为重要的纺织印染助剂,生产和使用量都十分巨大,在生产和使用过程中氨基硅油可随废水排放进入环境,威胁环境安全。曾同样作为重要纺织印染助剂的二甲基硅油(Polydimethylsiloxane, PDMS),在环境行为等方面已有较为系统的研究报道,但针对氨基硅油的研究国内外却开展不多。鉴于此,本论文较为系统的研究了氨基硅油环境生态毒性、氨基硅油ASBR厌氧生物降解性、氨基硅油Fenton氧化脱除机制与降解途径,主要研究结果如下：
1、氨基硅油的发光菌发光抑制、蚯蚓急性毒性、白菜种子发芽和根伸长抑制等毒性试验结果表明：对于各检测终点,在氨基硅油微乳液暴露浓度为0.05～2.5mg/mL及氨基硅油暴露浓度为0.01-1.0mg/g范围内,均有明显的剂量-效应关系。同时,氨基硅油的氨值和粘度在三种毒性测试试验中表现出不尽相同的影响：高氨值氨基硅油微乳液比低氨值氨基硅油微乳液对发光细菌表现出更显著的发光强度抑制作用,这可能与氨基硅油侧链上氨烃基及其质子化过程的作用有关；氨基硅油粘度不同则对发光细菌的发光抑制没有显著的影响。氨基硅油的粘度显著影响了氨基硅油对蚯蚓的毒性作用,高粘度的氨基硅油比低粘度的氨基硅油表现出更高的蚯蚓减重率和更低的蚯蚓存活率,而氨基硅油的氨值高低则对蚯蚓的减重和存活没有显著影响。氨基硅油的氨值、粘度对种子发芽和根伸长的抑制作用均不产生显著的影响。
2、氨基硅油的ASBR厌氧生物降解实验发现：ASBR反应器模拟厌氧降解过程中,仅有不高于9.5%的氨基硅油随出水排出反应器进入环境,大部分氨基硅油被留滞或积累在反应器内(反应器壁及污泥吸附),最终通过污泥排入环境。ASBR反应器进出水和污泥中有机物分子量和官能团的检测表明,较高分子量的氨基硅油更多被滞留或积累在反应器内,且氨基硅油在ASBR厌氧生物处理过程中未发生明显的降解过程。此外,厌氧摇瓶降解性检验实验进一步验证,在厌氧生物处理过程中氨基硅油基本不能被有效生物降解。
3、氨基硅油Fenton氧化降解与脱除机制研究发现：Fenton试剂氧化技术可以有效处理氨基硅油微乳液废水,其COD去除率达到80%左右；在Fenton试剂氧化作用下,氨基硅油主要通过絮凝吸附作用得到脱除,但是因氧化作用而产生的降解反应对氨基硅油的脱除起到了关键作用；且在此过程中,氨基硅油的分子量与COD去除率表现出较好的相关性,较高分子量的氨基硅油样本的去除效率较高。在Fenton试剂氧化过程中,氨基硅油的降解途径表现为：a)氨基硅油首先在低pH值条件下发生环化反应；b)随后由于羟基自由基的氧化作用发生侧链的断链反应；c)与此同时,氨基硅油主链在羟基自由基的氧化作用下发生无规断链反应,氨基硅油的平均分子量明显降低。此外,反应过程中的H2O2、Fe2+、ORP、pH值等参数的变化趋势显示：氨基硅油的氨值和分子量明显影响了Fenton氧化反应体系中H202的消耗,同时Fenton氧化降解过程产生的中间活性产物显著影响了Fenton反应的进程。
总之,相对于二甲基硅油,氨基硅油表现出较为明显的生态急性毒性。同时,氨基硅油主要通过污水处理过程的污泥处置进入环境,仅有少量的氨基硅油随废水排放进入环境水体和沉积物中,并且在污水生化处理过程中氨基硅油不能被有效的生物降解。Fenton试剂产生的氧化作用可以破坏氨基硅油的分子结构,并通过絮凝和吸附作用有效脱除废水中的氨基硅油。这些研究结果可以为氨基硅油的安全使用和氨基硅油微乳液废水的有效处理提供理论依据和技术支持。
As an important global textile production and consumption country, China has contributed greatly to the whole national economies in terms of textile printing and dyeing industries, and the production and use quantity of poly(dimethylaminostyrene)(PDMAS), as an important textile additive in the textile printing and dyeing industries, accounted for a great proportion in the world. The rapid development of technologies producing PDMAS has greatly promoted the development of overall field of textile chemicals and textile printing and dyeing industry, resulting in the discharge of a large number of PDMAS pollutants, generated in the production and use procedures, into the environment together with the wastewater treatment process effluent, with a potential threat to the environment. Unlike the systematic study of polydimethylsiloxane (PDMS) in the environmental behaviors, the environmental problems of PDMAS, neither in the scientific nor industry community, have not attracted sufficient attention.
This thesis systematically studied the environmental behavior and degradation (removal) mechanism of PDMAS in the soil and water from three research perspectives:a) ecological toxicity of PDMAS, b) biodegradability of PDMAS in ASBR anaerobic reactor, and c) PDMAS's degradation mechanism and pathways in microemulsion by Fenton reagent. The major findings are:
1. Three acute toxicities were carried out in this study. They were the luminescence inhibition of luminous bacteria in the PDMAS emulsion, the inhibition of the cabbage seed germination and root elongation, the earthworm survival and weight loss in the soil which were contaminated by the PDMAS, respectively. These acute toxicity tests showed that within the PDMAS microemulsion exposure concentration range of0.05-2.5mg/mL and PDMAS exposure concentration range of0.01～1.0mg/g, they all have significant dose-response relationships at the each test. Relatively higher concentrations of PDMAS samples showed more obvious toxic effects. Meanwhile, the three test methods also showed slightly different toxic effects of ammonia value and viscosity of PDMAS. In the detection concentration range of the PDMAS emulsion, the PDMAS emulsion of higher ammonia values had more significant luminescence inhibition of photobacterium phosphorem (strain T3), because of the proton process of ammonia alkyl side chain of PDMAS. However, the viscosity of PDMAS had no significant effects on luminescence inhibition. The soil samples contaminated by higher viscosity PDMAS have higher weight loss rates and lower survival rates of earthworms (E. foetida), and the ammonia value of PDMAS did not significantly affect the weight loss and survival of earthworms. The soil samples contaminated by different ammonia value and viscosity of PDMAS did not have a significant impact on the inhibition of seed germination and root elongation.
2. The long-term biodegradability experiments of PDMAS in a ASBR reactor showed:only less than9.5%of the PDMAS entry into the environment together with the water discharge from the reactor, while most of the PDMAS were lagged or accumulated in the reactor (reactor wall and sludge adsorption), and later discharged into the environment with the sludge. The organic matters'analysis (average molecular weight and functional group) results of the ASBR reaction in the effluent and sludge showed that the higher molecular weight of the PDMAS had more retention or accumulation in the reactor anaerobic, and biological treatment process would had no significant degradation process. Mean the while; the further anaerobic shake flask experiments verified the very low biodegradability of PDMAS in the anaerobic biological treatment process.
3. The results of PDMAS's degradation mechanism and pathways in microemulsion by Fenton reagent showed that Fenton reagent oxidation technology is a suitable choice for physic-chemical pretreatment of PDMAS emulsion wastewater with COD removal efficiency reached about80%. Under the Fenton reaction conditions, PDMAS was removed primarily through flocculation and adsorption, coupling with a key process of oxidation. It was also observed that the molecular weight of the PDMAS was correlated to the COD removal efficiency in some extent, that is, the PDMAS samples in high molecular weight was removed with a slightly higher COD removal efficiency. The degradation pathway of the PDMAS under Fenton reagent oxidation process was as follows:a) firstly, the cyclization reaction of the PDMAS occurs under low pH conditions; b) the subsequent occurrence is side-chain scission due to oxidation of the hydroxyl radical reaction; c)simultaneously, the main chain scission reaction happens randomly. In addition, changes of the concentration of H2O2and Fe2+, and the value of ORP and pH in the Fenton reaction process verified that the molecular weight and ammonia values of the PDMAS affects the consumption of H2O2in the Fenton oxidation process, and intermediates affect the process of the Fenton reaction in the degradation process. These findings and laws further verified the PDMAS removal mechanism and degradation pathways.
In summary, relative to the PDMS, PDMAS showed stronger acute toxicity, and presented a potential threat to the environment. We verified that that the PDMAS entry into the environment through the sludge disposal of wastewater treatment process, and only a small amount of the PDMAS entry into the environment through wastewater discharge, and little effective biodegradation was observed in the process of biochemical treatment. The PDMAS can be removed primarily by the flocculation and adsorption in the Fenton process. Oxidation broke the PDMAS structure (all of side-chains scission, main chain scission randomly and smaller molecular weight siloxane polymer generated), which greatly promoted the flocculation effect of the removal efficiency. The results from this study provide a theoretical base and technical support for the safe use and effective removal of PDMAS.
1、氨基硅油的发光菌发光抑制、蚯蚓急性毒性、白菜种子发芽和根伸长抑制等毒性试验结果表明：对于各检测终点,在氨基硅油微乳液暴露浓度为0.05～2.5mg/mL及氨基硅油暴露浓度为0.01-1.0mg/g范围内,均有明显的剂量-效应关系。同时,氨基硅油的氨值和粘度在三种毒性测试试验中表现出不尽相同的影响：高氨值氨基硅油微乳液比低氨值氨基硅油微乳液对发光细菌表现出更显著的发光强度抑制作用,这可能与氨基硅油侧链上氨烃基及其质子化过程的作用有关；氨基硅油粘度不同则对发光细菌的发光抑制没有显著的影响。氨基硅油的粘度显著影响了氨基硅油对蚯蚓的毒性作用,高粘度的氨基硅油比低粘度的氨基硅油表现出更高的蚯蚓减重率和更低的蚯蚓存活率,而氨基硅油的氨值高低则对蚯蚓的减重和存活没有显著影响。氨基硅油的氨值、粘度对种子发芽和根伸长的抑制作用均不产生显著的影响。
2、氨基硅油的ASBR厌氧生物降解实验发现：ASBR反应器模拟厌氧降解过程中,仅有不高于9.5%的氨基硅油随出水排出反应器进入环境,大部分氨基硅油被留滞或积累在反应器内(反应器壁及污泥吸附),最终通过污泥排入环境。ASBR反应器进出水和污泥中有机物分子量和官能团的检测表明,较高分子量的氨基硅油更多被滞留或积累在反应器内,且氨基硅油在ASBR厌氧生物处理过程中未发生明显的降解过程。此外,厌氧摇瓶降解性检验实验进一步验证,在厌氧生物处理过程中氨基硅油基本不能被有效生物降解。
3、氨基硅油Fenton氧化降解与脱除机制研究发现：Fenton试剂氧化技术可以有效处理氨基硅油微乳液废水,其COD去除率达到80%左右；在Fenton试剂氧化作用下,氨基硅油主要通过絮凝吸附作用得到脱除,但是因氧化作用而产生的降解反应对氨基硅油的脱除起到了关键作用；且在此过程中,氨基硅油的分子量与COD去除率表现出较好的相关性,较高分子量的氨基硅油样本的去除效率较高。在Fenton试剂氧化过程中,氨基硅油的降解途径表现为：a)氨基硅油首先在低pH值条件下发生环化反应；b)随后由于羟基自由基的氧化作用发生侧链的断链反应；c)与此同时,氨基硅油主链在羟基自由基的氧化作用下发生无规断链反应,氨基硅油的平均分子量明显降低。此外,反应过程中的H2O2、Fe2+、ORP、pH值等参数的变化趋势显示：氨基硅油的氨值和分子量明显影响了Fenton氧化反应体系中H202的消耗,同时Fenton氧化降解过程产生的中间活性产物显著影响了Fenton反应的进程。
总之,相对于二甲基硅油,氨基硅油表现出较为明显的生态急性毒性。同时,氨基硅油主要通过污水处理过程的污泥处置进入环境,仅有少量的氨基硅油随废水排放进入环境水体和沉积物中,并且在污水生化处理过程中氨基硅油不能被有效的生物降解。Fenton试剂产生的氧化作用可以破坏氨基硅油的分子结构,并通过絮凝和吸附作用有效脱除废水中的氨基硅油。这些研究结果可以为氨基硅油的安全使用和氨基硅油微乳液废水的有效处理提供理论依据和技术支持。
As an important global textile production and consumption country, China has contributed greatly to the whole national economies in terms of textile printing and dyeing industries, and the production and use quantity of poly(dimethylaminostyrene)(PDMAS), as an important textile additive in the textile printing and dyeing industries, accounted for a great proportion in the world. The rapid development of technologies producing PDMAS has greatly promoted the development of overall field of textile chemicals and textile printing and dyeing industry, resulting in the discharge of a large number of PDMAS pollutants, generated in the production and use procedures, into the environment together with the wastewater treatment process effluent, with a potential threat to the environment. Unlike the systematic study of polydimethylsiloxane (PDMS) in the environmental behaviors, the environmental problems of PDMAS, neither in the scientific nor industry community, have not attracted sufficient attention.
This thesis systematically studied the environmental behavior and degradation (removal) mechanism of PDMAS in the soil and water from three research perspectives:a) ecological toxicity of PDMAS, b) biodegradability of PDMAS in ASBR anaerobic reactor, and c) PDMAS's degradation mechanism and pathways in microemulsion by Fenton reagent. The major findings are:
1. Three acute toxicities were carried out in this study. They were the luminescence inhibition of luminous bacteria in the PDMAS emulsion, the inhibition of the cabbage seed germination and root elongation, the earthworm survival and weight loss in the soil which were contaminated by the PDMAS, respectively. These acute toxicity tests showed that within the PDMAS microemulsion exposure concentration range of0.05-2.5mg/mL and PDMAS exposure concentration range of0.01～1.0mg/g, they all have significant dose-response relationships at the each test. Relatively higher concentrations of PDMAS samples showed more obvious toxic effects. Meanwhile, the three test methods also showed slightly different toxic effects of ammonia value and viscosity of PDMAS. In the detection concentration range of the PDMAS emulsion, the PDMAS emulsion of higher ammonia values had more significant luminescence inhibition of photobacterium phosphorem (strain T3), because of the proton process of ammonia alkyl side chain of PDMAS. However, the viscosity of PDMAS had no significant effects on luminescence inhibition. The soil samples contaminated by higher viscosity PDMAS have higher weight loss rates and lower survival rates of earthworms (E. foetida), and the ammonia value of PDMAS did not significantly affect the weight loss and survival of earthworms. The soil samples contaminated by different ammonia value and viscosity of PDMAS did not have a significant impact on the inhibition of seed germination and root elongation.
2. The long-term biodegradability experiments of PDMAS in a ASBR reactor showed:only less than9.5%of the PDMAS entry into the environment together with the water discharge from the reactor, while most of the PDMAS were lagged or accumulated in the reactor (reactor wall and sludge adsorption), and later discharged into the environment with the sludge. The organic matters'analysis (average molecular weight and functional group) results of the ASBR reaction in the effluent and sludge showed that the higher molecular weight of the PDMAS had more retention or accumulation in the reactor anaerobic, and biological treatment process would had no significant degradation process. Mean the while; the further anaerobic shake flask experiments verified the very low biodegradability of PDMAS in the anaerobic biological treatment process.
3. The results of PDMAS's degradation mechanism and pathways in microemulsion by Fenton reagent showed that Fenton reagent oxidation technology is a suitable choice for physic-chemical pretreatment of PDMAS emulsion wastewater with COD removal efficiency reached about80%. Under the Fenton reaction conditions, PDMAS was removed primarily through flocculation and adsorption, coupling with a key process of oxidation. It was also observed that the molecular weight of the PDMAS was correlated to the COD removal efficiency in some extent, that is, the PDMAS samples in high molecular weight was removed with a slightly higher COD removal efficiency. The degradation pathway of the PDMAS under Fenton reagent oxidation process was as follows:a) firstly, the cyclization reaction of the PDMAS occurs under low pH conditions; b) the subsequent occurrence is side-chain scission due to oxidation of the hydroxyl radical reaction; c)simultaneously, the main chain scission reaction happens randomly. In addition, changes of the concentration of H2O2and Fe2+, and the value of ORP and pH in the Fenton reaction process verified that the molecular weight and ammonia values of the PDMAS affects the consumption of H2O2in the Fenton oxidation process, and intermediates affect the process of the Fenton reaction in the degradation process. These findings and laws further verified the PDMAS removal mechanism and degradation pathways.
In summary, relative to the PDMS, PDMAS showed stronger acute toxicity, and presented a potential threat to the environment. We verified that that the PDMAS entry into the environment through the sludge disposal of wastewater treatment process, and only a small amount of the PDMAS entry into the environment through wastewater discharge, and little effective biodegradation was observed in the process of biochemical treatment. The PDMAS can be removed primarily by the flocculation and adsorption in the Fenton process. Oxidation broke the PDMAS structure (all of side-chains scission, main chain scission randomly and smaller molecular weight siloxane polymer generated), which greatly promoted the flocculation effect of the removal efficiency. The results from this study provide a theoretical base and technical support for the safe use and effective removal of PDMAS.
引文
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