电子捕获剂协同载贵金属TiO_2光催化降解典型制药污染物
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摘要
针对近年来制药废水带来的环境问题日益严重的情况,结合越来越受到关注的TiO_2光催化法,本文制备了系列载贵金属催化剂,并系统地研究了添加不同电子捕获剂(H_2O_2,KBrO_3,K_2S_2O_8)协同载贵金属TiO_2光催化降解典型制药废水污染物(苯酚,吡啶,硝基苯,β-lactam类抗生素阿莫西林)相关活性及影响因素,得到了一系列富有意义的结果。研究内容主要包括:
第一,通过光沉积法成功的将不同贵金属负载在锐钛矿相TiO_2(M/TiO_2)上,并对各种催化剂进行了性能表征。其中,通过紫外可见分光光度计地检测,结果表明:在紫外光区域,M/TiO_2与TiO_2对光的吸收差别不大,各催化剂对可见光地吸收强弱顺序为: Au/TiO_2 > Ru/TiO_2 > Ag/TiO_2 > Pt/TiO_2 > Ir/TiO_2 > Pd/TiO_2 > Rh/TiO_2 > TiO_2;通过BET地检测,结果表明,负载各种贵金属对TiO_2的比表面积并未产生明显的影响,这主要是由于贵金属的负载量很少而且分布均匀;通过电子扫描电镜地检测及能谱地分析,结果表明:用光沉积法能够将贵金属均匀分散的负载在TiO_2表面,能很好的抑制团聚作用,得到分散度很好的催化剂。
第二,开展了电子捕获剂协同载贵金属TiO_2光催化降解苯酚的实验研究,结果表明:H_2O_2最利于协同TiO_2光催化去除苯酚;H_2O_2协同M/TiO_2光催化降解苯酚的活性顺序为: Ag/TiO_2 > Ir/TiO_2 > Pd/TiO_2 > Rh/TiO_2 > Pt/TiO_2 > Ru/TiO_2 > Au/TiO_2;在最优条件下( Ag/TiO_2载Ag量0.5%,催化剂浓度0.10g/L,H_2O_2投加量50mM,pH值为5),3小时光催化降解率达到57%,比TiO_2的降解率提高了35%。
第三,开展了电子捕获剂协同载贵金属TiO_2光催化降解吡啶的实验研究,结果表明:KBrO_3最利于协同TiO_2光催化去除吡啶;KBrO_3协同M/TiO_2光催化降解吡啶的活性顺序为: Ag/TiO_2 > Au/TiO_2 > Pd/TiO_2 > Pt/TiO_2≈TiO_2 > Ir/TiO_2 > Rh/TiO_2≈Ru/TiO_2;在最优条件下(Ag/TiO_2载Ag量0.5%,催化剂浓度0.10g/L,KBrO_3投加量10mM,pH值为9),3小时光催化降解率达到62%,比TiO_2的降解率提高23%。
第四,开展了电子捕获剂协同载贵金属TiO_2光催化降解硝基苯的实验研究,结果表明:KBrO_3最利于协同TiO_2光催化去除硝基苯;KBrO_3协同M/TiO_2光催化降解苯酚的活性顺序为: Au/TiO_2 > Ag/TiO_2≈TiO_2 > Ir/TiO_2 > Ru/TiO_2 > Pd/TiO_2 > Pt/TiO_2 > Rh/TiO_2;在最优条件下(Au/TiO_2载Au量0.1%,催化剂浓度0.10g/L,KBrO_3投加量5mM,pH值为3),6小时光催化降解率达到95%,比TiO_2的降解率提高17%。
第五,开展了电子捕获剂协同载贵金属TiO_2光催化降解β-lactam类抗生素阿莫西林的实验研究,结果表明:KBrO_3最利于协同TiO_2光催化降解阿莫西林;KBrO_3协同M/TiO_2光催化降解阿莫西林的活性顺序为: Rh/TiO_2 > Pd/TiO_2 > Ag/TiO_2 > Au/TiO_2≈Ir/TiO_2 > TiO_2 > Pt/TiO_2 > Ru/TiO_2;在最优条件下( Rh/TiO_2载Rh量0.1%,催化剂浓度0.15g/L,KBrO_3投加量0.5mM,pH值为5),2小时光催化降解率达到100%,比TiO_2的降解率提高80%。
第六,开展了UV+TiO_2、捕获剂+UV+TiO_2、贵金属/TiO_2+UV+捕获剂三种催化体系对四种污染物光催化降解动力学的研究,分析结果表明三种催化体系都比较符合一级反应动力学模型,遵循一级反应动力学规律,相关系数都比较高,而且反应速率常数K逐步增大,说明添加电子捕获剂并负载贵金属的确能有效提高光催化反应的速率。
In recent years, environmental problems caused by medical waste are more and more serious, combined with the strong oxidizing ability of the TiO_2 photocatalytic method, we have system studied of adding different electron capture agents (H_2O_2, KBrO_3, K_2S_2O_8) Collaborative TiO_2 loaded with precious metals photocatalytic degradation of typical medical waste water pollutants contained phenol, pyridine, nitrobenzene,β-lactam antibiotic amoxicillin.
We loaded the precious metal on the surface of anatase TiO_2 using light deposition method, and then characterized by a variety of means to characterize their properties. UV-vis diffuse reflectance spectra showed that: in the UV region, the light absorbed by TiO_2 or M/TiO_2 is not very different, in the visible region, the absorption from strong to weak as: Au/TiO_2 > Ru/TiO_2 > Ag/TiO_2 > Pt/TiO_2 > Ir/TiO_2 > Pd/TiO_2 > Rh/TiO_2 > TiO_2; BET analysis showed that: loading all kinds of precious metals did not produce significant effects on the specific surface area of TiO_2, for the load of precious metals rarely and well distribution;Scanning electron microscopy and EDS analysis showed that: the precious metal can be extremely dispersed on the surface of TiO_2 by the light deposition method and inhibit the agglomeration of the nanosized precious metal to get a good dispersion and uniform distribution.
We have studied the photocatalytic degradation of typical medical waste water pollutants phenol by adding electron capture agents collaborative TiO_2 loaded with precious metals. The results showed that the most favorable electron capture agents was H_2O_2; when the different precious metals loading on TiO_2 and H_2O_2 was added, the activity order of phenol removal was: Ag/TiO_2 > Ir/TiO_2 > Pd/TiO_2 > Rh/TiO_2 > Pt/TiO_2 > Ru/TiO_2 > Au/TiO_2. The favorable loading amount of the best precious metal Ag was 0.5%; the optimal dosage of catalyst was 0.02g; the best dosage of H_2O_2 was 50mM;the optimal pH was 5. Under these optimal conditions, the photocatalytic degradation rate reachs 57% in 3 hours, increased by 35% compared with the degradation rate of TiO_2 + UV system.
We have studied the photocatalytic degradation of typical medical waste water pollutants pyridine by adding electron capture agents collaborative TiO_2 loaded with precious metals. The results showed that the most favorable electron capture agents was KBrO_3; when the different precious metals loading on TiO_2 and KBrO_3 was added, the activity order of pyridine removal was: Ag/TiO_2 > Au/TiO_2 > Pd/TiO_2 > Pt/TiO_2 TiO_2 > Ir/TiO_2 > Rh/TiO_2 Ru/TiO_2. The favorable loading amount of the best precious metal Ag was 0.5%; the optimal dosage of catalyst was 0.02g; the best dosage of KBrO_3 was 10mM;the optimal pH was 9. Under these optimal conditions, the photocatalytic degradation rate reachs 62% in 3 hours, increased by 23% compared with the degradation rate of TiO_2 + UV system.
We have studied the photocatalytic degradation of typical medical waste water pollutants nitrobenzene by adding electron capture agents collaborative TiO_2 loaded with precious metals. The results showed that the most favorable electron capture agents was KBrO_3; when the different precious metals loading on TiO_2 and KBrO_3 was added, the activity order of nitrobenzene removal was:Au/TiO_2 > Ag/TiO_2≈TiO_2 > Ir/TiO_2 > Ru/TiO_2 > Pd/TiO_2 > Pt/TiO_2 > Rh/TiO_2. The favorable loading amount of the best precious metal Au was 0.1%; the optimal dosage of catalyst was 0.02g; the best dosage of KBrO_3 was 5mM;the optimal pH was 3. Under these optimal conditions, the photocatalytic degradation rate reachs 95% in 6 hours, increased by 17% compared with the degradation rate of TiO_2 + UV system.
We have studied the photocatalytic degradation of typical medical waste water pollutantsβ-lactam antibiotics amoxicillin by adding electron capture agents collaborative TiO_2 loaded with precious metals. The results showed that the most favorable electron capture agents was KBrO_3; when the different precious metals loading on TiO_2 and KBrO_3 was added, the activity order of amoxicillin removal was: Rh/TiO_2 > Pd/TiO_2 > Ag/TiO_2 > Au/TiO_2 Ir/TiO_2 > TiO_2 > Pt/TiO_2 > Ru/TiO_2. The favorable loading amount of the best precious metal Rh was 0.1%; the optimal dosage of catalyst was 0.03g; the best dosage of KBrO_3 was 0.5mM;the optimal pH was 5. Under these optimal conditions,the photocatalytic degradation rate reachs 100% in 2 hours, increased by 80% compared with the degradation rate of TiO_2 + UV system.
Finaly, for each pollutant were carried out three different comparative experiments of photocatalytic degradation: "without electron scavenger, TiO_2 withnot precious metals "; "with electron capture agent, TiO_2 withnot precious metals "; "with electron capture agent, TiO_2 loaded with precious metals ". The results show that for phenol, loading properly amount of Ag on TiO_2 and adding right amount of H_2O_2 can significantly increase the degradation rate of TOC contaminants; while for the other three pollutants, adding TiO_2 electron capture agent and load on precious metals does not increase TOC degradation rate, but it also can promote the pollutants to the transformation of small molecule intermediates. Kinetic analysis showed that three kinds of catalyst systems are consistent with the first order kinetic model, following the first order reaction rule, and the reaction rate constant K gradually increase, that add an electron capture agent and load the precious metals indeed effectively improve the photocatalytic reaction rate.
第一,通过光沉积法成功的将不同贵金属负载在锐钛矿相TiO_2(M/TiO_2)上,并对各种催化剂进行了性能表征。其中,通过紫外可见分光光度计地检测,结果表明:在紫外光区域,M/TiO_2与TiO_2对光的吸收差别不大,各催化剂对可见光地吸收强弱顺序为: Au/TiO_2 > Ru/TiO_2 > Ag/TiO_2 > Pt/TiO_2 > Ir/TiO_2 > Pd/TiO_2 > Rh/TiO_2 > TiO_2;通过BET地检测,结果表明,负载各种贵金属对TiO_2的比表面积并未产生明显的影响,这主要是由于贵金属的负载量很少而且分布均匀;通过电子扫描电镜地检测及能谱地分析,结果表明:用光沉积法能够将贵金属均匀分散的负载在TiO_2表面,能很好的抑制团聚作用,得到分散度很好的催化剂。
第二,开展了电子捕获剂协同载贵金属TiO_2光催化降解苯酚的实验研究,结果表明:H_2O_2最利于协同TiO_2光催化去除苯酚;H_2O_2协同M/TiO_2光催化降解苯酚的活性顺序为: Ag/TiO_2 > Ir/TiO_2 > Pd/TiO_2 > Rh/TiO_2 > Pt/TiO_2 > Ru/TiO_2 > Au/TiO_2;在最优条件下( Ag/TiO_2载Ag量0.5%,催化剂浓度0.10g/L,H_2O_2投加量50mM,pH值为5),3小时光催化降解率达到57%,比TiO_2的降解率提高了35%。
第三,开展了电子捕获剂协同载贵金属TiO_2光催化降解吡啶的实验研究,结果表明:KBrO_3最利于协同TiO_2光催化去除吡啶;KBrO_3协同M/TiO_2光催化降解吡啶的活性顺序为: Ag/TiO_2 > Au/TiO_2 > Pd/TiO_2 > Pt/TiO_2≈TiO_2 > Ir/TiO_2 > Rh/TiO_2≈Ru/TiO_2;在最优条件下(Ag/TiO_2载Ag量0.5%,催化剂浓度0.10g/L,KBrO_3投加量10mM,pH值为9),3小时光催化降解率达到62%,比TiO_2的降解率提高23%。
第四,开展了电子捕获剂协同载贵金属TiO_2光催化降解硝基苯的实验研究,结果表明:KBrO_3最利于协同TiO_2光催化去除硝基苯;KBrO_3协同M/TiO_2光催化降解苯酚的活性顺序为: Au/TiO_2 > Ag/TiO_2≈TiO_2 > Ir/TiO_2 > Ru/TiO_2 > Pd/TiO_2 > Pt/TiO_2 > Rh/TiO_2;在最优条件下(Au/TiO_2载Au量0.1%,催化剂浓度0.10g/L,KBrO_3投加量5mM,pH值为3),6小时光催化降解率达到95%,比TiO_2的降解率提高17%。
第五,开展了电子捕获剂协同载贵金属TiO_2光催化降解β-lactam类抗生素阿莫西林的实验研究,结果表明:KBrO_3最利于协同TiO_2光催化降解阿莫西林;KBrO_3协同M/TiO_2光催化降解阿莫西林的活性顺序为: Rh/TiO_2 > Pd/TiO_2 > Ag/TiO_2 > Au/TiO_2≈Ir/TiO_2 > TiO_2 > Pt/TiO_2 > Ru/TiO_2;在最优条件下( Rh/TiO_2载Rh量0.1%,催化剂浓度0.15g/L,KBrO_3投加量0.5mM,pH值为5),2小时光催化降解率达到100%,比TiO_2的降解率提高80%。
第六,开展了UV+TiO_2、捕获剂+UV+TiO_2、贵金属/TiO_2+UV+捕获剂三种催化体系对四种污染物光催化降解动力学的研究,分析结果表明三种催化体系都比较符合一级反应动力学模型,遵循一级反应动力学规律,相关系数都比较高,而且反应速率常数K逐步增大,说明添加电子捕获剂并负载贵金属的确能有效提高光催化反应的速率。
In recent years, environmental problems caused by medical waste are more and more serious, combined with the strong oxidizing ability of the TiO_2 photocatalytic method, we have system studied of adding different electron capture agents (H_2O_2, KBrO_3, K_2S_2O_8) Collaborative TiO_2 loaded with precious metals photocatalytic degradation of typical medical waste water pollutants contained phenol, pyridine, nitrobenzene,β-lactam antibiotic amoxicillin.
We loaded the precious metal on the surface of anatase TiO_2 using light deposition method, and then characterized by a variety of means to characterize their properties. UV-vis diffuse reflectance spectra showed that: in the UV region, the light absorbed by TiO_2 or M/TiO_2 is not very different, in the visible region, the absorption from strong to weak as: Au/TiO_2 > Ru/TiO_2 > Ag/TiO_2 > Pt/TiO_2 > Ir/TiO_2 > Pd/TiO_2 > Rh/TiO_2 > TiO_2; BET analysis showed that: loading all kinds of precious metals did not produce significant effects on the specific surface area of TiO_2, for the load of precious metals rarely and well distribution;Scanning electron microscopy and EDS analysis showed that: the precious metal can be extremely dispersed on the surface of TiO_2 by the light deposition method and inhibit the agglomeration of the nanosized precious metal to get a good dispersion and uniform distribution.
We have studied the photocatalytic degradation of typical medical waste water pollutants phenol by adding electron capture agents collaborative TiO_2 loaded with precious metals. The results showed that the most favorable electron capture agents was H_2O_2; when the different precious metals loading on TiO_2 and H_2O_2 was added, the activity order of phenol removal was: Ag/TiO_2 > Ir/TiO_2 > Pd/TiO_2 > Rh/TiO_2 > Pt/TiO_2 > Ru/TiO_2 > Au/TiO_2. The favorable loading amount of the best precious metal Ag was 0.5%; the optimal dosage of catalyst was 0.02g; the best dosage of H_2O_2 was 50mM;the optimal pH was 5. Under these optimal conditions, the photocatalytic degradation rate reachs 57% in 3 hours, increased by 35% compared with the degradation rate of TiO_2 + UV system.
We have studied the photocatalytic degradation of typical medical waste water pollutants pyridine by adding electron capture agents collaborative TiO_2 loaded with precious metals. The results showed that the most favorable electron capture agents was KBrO_3; when the different precious metals loading on TiO_2 and KBrO_3 was added, the activity order of pyridine removal was: Ag/TiO_2 > Au/TiO_2 > Pd/TiO_2 > Pt/TiO_2 TiO_2 > Ir/TiO_2 > Rh/TiO_2 Ru/TiO_2. The favorable loading amount of the best precious metal Ag was 0.5%; the optimal dosage of catalyst was 0.02g; the best dosage of KBrO_3 was 10mM;the optimal pH was 9. Under these optimal conditions, the photocatalytic degradation rate reachs 62% in 3 hours, increased by 23% compared with the degradation rate of TiO_2 + UV system.
We have studied the photocatalytic degradation of typical medical waste water pollutants nitrobenzene by adding electron capture agents collaborative TiO_2 loaded with precious metals. The results showed that the most favorable electron capture agents was KBrO_3; when the different precious metals loading on TiO_2 and KBrO_3 was added, the activity order of nitrobenzene removal was:Au/TiO_2 > Ag/TiO_2≈TiO_2 > Ir/TiO_2 > Ru/TiO_2 > Pd/TiO_2 > Pt/TiO_2 > Rh/TiO_2. The favorable loading amount of the best precious metal Au was 0.1%; the optimal dosage of catalyst was 0.02g; the best dosage of KBrO_3 was 5mM;the optimal pH was 3. Under these optimal conditions, the photocatalytic degradation rate reachs 95% in 6 hours, increased by 17% compared with the degradation rate of TiO_2 + UV system.
We have studied the photocatalytic degradation of typical medical waste water pollutantsβ-lactam antibiotics amoxicillin by adding electron capture agents collaborative TiO_2 loaded with precious metals. The results showed that the most favorable electron capture agents was KBrO_3; when the different precious metals loading on TiO_2 and KBrO_3 was added, the activity order of amoxicillin removal was: Rh/TiO_2 > Pd/TiO_2 > Ag/TiO_2 > Au/TiO_2 Ir/TiO_2 > TiO_2 > Pt/TiO_2 > Ru/TiO_2. The favorable loading amount of the best precious metal Rh was 0.1%; the optimal dosage of catalyst was 0.03g; the best dosage of KBrO_3 was 0.5mM;the optimal pH was 5. Under these optimal conditions,the photocatalytic degradation rate reachs 100% in 2 hours, increased by 80% compared with the degradation rate of TiO_2 + UV system.
Finaly, for each pollutant were carried out three different comparative experiments of photocatalytic degradation: "without electron scavenger, TiO_2 withnot precious metals "; "with electron capture agent, TiO_2 withnot precious metals "; "with electron capture agent, TiO_2 loaded with precious metals ". The results show that for phenol, loading properly amount of Ag on TiO_2 and adding right amount of H_2O_2 can significantly increase the degradation rate of TOC contaminants; while for the other three pollutants, adding TiO_2 electron capture agent and load on precious metals does not increase TOC degradation rate, but it also can promote the pollutants to the transformation of small molecule intermediates. Kinetic analysis showed that three kinds of catalyst systems are consistent with the first order kinetic model, following the first order reaction rule, and the reaction rate constant K gradually increase, that add an electron capture agent and load the precious metals indeed effectively improve the photocatalytic reaction rate.
引文
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