改性TiO_2可见光催化剂的制备及其光催化性能研究
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摘要
光催化氧化是一种绿色高效的高级氧化技术，具有分解水制氢、光催化合成和光降解有机污染物等作用，在解决温室效应、能源问题和环境问题方面有重要的应用前景。TiO2因其具有活性高、稳定性好、安全无毒等优点而被作为一种常用的光催化剂。但是TiO2对光的吸收仅限于紫外光区（Eg=3.2eV），对于可见光或太阳光的吸收利用率很低，提高光能利用效率的关键在于突破催化剂的禁带宽度，使其响应光谱向可见光扩展。对TiO2的光敏化是延伸其激发波长的一个重要手段。
本论文针对拓展催化剂的可见光吸收性能，利用工业有机颜料和石墨烯（GE）对TiO2进行了改性并对改性后的催化剂的可见光催化性能进行了研究。另外，本文还对苯酚选择性氧化和羟基化的实验条件进行了探讨。论文主要由以下三部分内容：
（1）工业有机颜料敏化改性TiO2复合催化剂降解有机污染物研究
通过溶剂热法制备了具有可见光响应的BYH3G/TiO2复合催化剂。利用X射线衍射（XRD）、扫描电子显微镜（SEM）、傅立叶变换红外光谱（FT-IR）、紫外可见漫反射光谱（UV-vis DRS）、N2吸附-脱附（BET和BJH）等测试手段对所制备的催化剂进行了表征。分别以罗丹明B（RB）、酸性铬蓝K（ACBK）、甲基橙（MO）等为目标降解物，研究了催化剂在可见光下对有机污染物的光催化降解性能。实验结果表明，颜料的复合有效的拓展了催化剂的可见光吸收性能。在可见光照射下，RB、ACBK、MO的降解率分别为93.5%，94.6%和89.2%，而同样的实验条件下，三种目标降解物的降解率分别为24.8%，34.8%和9.4%；催化剂反复使用四次催化活性没有明显降低，证明复合光催化剂具有很好的稳定性。还分别用颜料红254、颜料红151、颜料红179、酞菁绿G、颜料红122对TiO2进行敏化改性，在降解MO和RB试验中都表现了比纯TiO2更好的可见光降解效率。探讨了制备的光催化剂对有机污染物的降解机理。
（2）石墨烯/TiO2复合催化剂的制备及其降解有机污染物性能研究
以商业P25粉（TiO2）和氧化石墨为前驱物，先后在180℃水热和450℃高温下，制得了GE/TiO2复合催化剂。利用XRD、SEM、FT-IR、UV-vis DRS等测试手段对所制备的催化剂进行了表征。
从吸附能力上，GE/TiO2对RB、MB和MO比改性前的纯TiO2都有所提高，在可见光下，纯TiO2对RB和MB具有一定的降解效果，但是对MO溶液效果却很弱，GE/TiO2的可见光催化性能相对于纯TiO2有了较大提高。而在紫外光照射下降解速率远远高于可见光，在紫外光照射下，光照70min后MO的降解率达到95.6%，60min后RB的降解率达到99.1%，70min后MB的降解率达到99.4%。探讨了GE/TiO2复合催化剂对有机污染物的降解机理。
（3）苯酚光催化氧化羟基化制备邻苯二酚（CAL）和对苯二酚（HQE）
分别以纯TiO2、GE/TiO2和BYH3G/TiO2为催化剂对苯酚进行光催化羟基化反应。在可见光照射下仅以BYH3G/TiO2为催化剂时检测到少量的CAL和HQE的生成。在紫外光照射下，GE/TiO2和BYH3G/TiO2均显示出较好的光催化活性和较高羟基化选择性。实验考察了催化剂用量、光照时间和H2O2用量对苯酚光催化羟基化反应的影响。以TiO2为催化剂时，苯酚最高转化率为66.9%，CAL和HQE的收率分别为12.6%和4.6%，反应选择性为25.7%；以GE/TiO2为催化剂时，苯酚的最高转化率为92.1%，CAL和HQE收率分别为19.8%和11.2%，反应选择性为33.6%。以BYH3G/TiO2为催化剂时，苯酚最高的转化率为63.0%，CAL和HQE的收率分别为28.7%和27.6%，反应选择性高达89.3%。从CAL和HQE的高收率的角度考虑，BYH3G/TiO2的羟基化效果最好，GE/TiO2次之，纯TiO2最差。推测了光催化羟基化的反应机理。
Photocatalytic oxidation, one of advanced oxidation technologies, has importantroles to water-splitting for hydrogen production, photocatalytic synthesis and thedegradation of organic contaminants. Photocatalytic oxidation has importantapplication feature in global warming, energy problems and environmental issues, etc.The widely explored TiO2has been accepted as an excellent photocatalyst among thesemiconductors due to its advantages of stability, low toxicity and high activity.However, the large band–gap energy (3.2eV) of TiO2considerably limits theutilization of natural solar light or artificial visible light. Photosensitization isconsidered to be an efficient and general method to modify the photoresponseproperties of TiO2.
In this thesis, using commercial organic pigments and graphene as modifier tomodify TiO2to expand visible light absorption performance of TiO2. The structuresand property of modified catalyst were studied. There are three main parts in thisthesis:
(1) TiO2photocatalyst sensitized with commercial organic pigment wasconveniently prepared and characterized by FT-IR, UV-Vis, XRD, SEM and N2adsorption-desorption isotherms. The adsorption capacities and photocatalyticactivities of the new photocatalyst were evaluated by photocatalytic degradation ofseveral kinds of representative pollutants under visible light irradiation. The resultsindicated that the new photocatalyst extends the photoresponse of TiO2from the UVto the visible region. The degradation rates of dyes RB (Rhodamine B), ACBK (AcidChrome Blue K) and MO (Methyl Orange) were24.8%,34.8%and9.4%respectivelyat their initial pH values in a fixed time under visible light irradiation with pure TiO2as the catalyst, while the degradation rates reach up to93.5%,94.6%and89.2%respectively in the present of BYH3G/TiO2(Benzimidazolone Yellow H3G/TiO2)under the same conditions. There was no appreciable loss of photocatalytic activityobserved when the photocatalyst was used four times, which demonstrates excellentstability and recyclability factors. Furthermore, sensitized TiO2with Pigment Red254,Pigment Red151, Pigment Red179, Phthalocyanine Green G, Pigment Red122wereprepared, and they all display better visible light catalytic activity than pure TiO2inthe degradation of MO and RB test under visible light irradiation. The mechanism ofaction was also discussed.
(2) Graphene/TiO2(GE/TiO2) was prepared by hydrothermal treating of a mixedsuspension of TiO2and graphite oxide. The prepared catalyst was characterized byFT-IR, UV-Vis, XRD and SEM. The adsorption capacity of GE/TiO2for RB、MB(Methlyene Blue) and MO was better than pure TiO2. Pure TiO2has a little bit ofdegradation capacity for RB and MB, but has no degradation capacity for MO, thevisible-light degradation ability of GE/TiO2was better than the pure TiO2. In addition,the degradation rate in the presence of UV light was far better than that of visible light.The degradation rate of MO was95.6%in70min under UV light irradiation, thedegradation rate of RB was99.1%in60min, and the degradation rate of MB was99.4%in70min. The mechanism of action was also discussed.
(3) Phenol photocatalytic oxidation experiment was carried out under ultravioletand visible light irradiation with the pure TiO2, GE/TiO2and BYH3G/TiO2catalysts.Under visible light irradiation, phenol was relatively stable and only a little catecholwas produced when use BYH3G/TiO2as the catalyst. While under UV-lightirradiation, there were obvious photocatalytic oxidations for phenol, and most phenolwas hydroxylated to pyrocatechol (CAL) and hydroquinone (HQE), others werephotocatalytic oxidized into benzoquinone or other materials. The effects of variousparameters on photocatalytic oxidation of phenol were studied. When using TiO2ascatalyst, the highest conversion of phenol was66.9%, and the yield of CAL and HQEwere12.6%and4.6%respectively, and the selectivity of the reaction was25.7%.Using GE/TiO2as catalyst, the highest conversion of phenol was92.1%, and the yieldof CAL and HQE yield were19.8%and11.2%, the selectivity was33.6%. UsingBYH3G/TiO2as catalyst, the highest conversion of phenol was63%, the yield ofCAL and HQE can reach28.7%and27.6%respectively, and the selectivity of thereaction was up to89.3%. From high yield of CAL and HQE perspective,BYH3G/TiO2was the best hydroxylation catalyst, the second was GE/TiO2, and theworst was pure TiO2. The mechanism of photocatalysis of the catalysts was inferred.
本论文针对拓展催化剂的可见光吸收性能，利用工业有机颜料和石墨烯（GE）对TiO2进行了改性并对改性后的催化剂的可见光催化性能进行了研究。另外，本文还对苯酚选择性氧化和羟基化的实验条件进行了探讨。论文主要由以下三部分内容：
（1）工业有机颜料敏化改性TiO2复合催化剂降解有机污染物研究
通过溶剂热法制备了具有可见光响应的BYH3G/TiO2复合催化剂。利用X射线衍射（XRD）、扫描电子显微镜（SEM）、傅立叶变换红外光谱（FT-IR）、紫外可见漫反射光谱（UV-vis DRS）、N2吸附-脱附（BET和BJH）等测试手段对所制备的催化剂进行了表征。分别以罗丹明B（RB）、酸性铬蓝K（ACBK）、甲基橙（MO）等为目标降解物，研究了催化剂在可见光下对有机污染物的光催化降解性能。实验结果表明，颜料的复合有效的拓展了催化剂的可见光吸收性能。在可见光照射下，RB、ACBK、MO的降解率分别为93.5%，94.6%和89.2%，而同样的实验条件下，三种目标降解物的降解率分别为24.8%，34.8%和9.4%；催化剂反复使用四次催化活性没有明显降低，证明复合光催化剂具有很好的稳定性。还分别用颜料红254、颜料红151、颜料红179、酞菁绿G、颜料红122对TiO2进行敏化改性，在降解MO和RB试验中都表现了比纯TiO2更好的可见光降解效率。探讨了制备的光催化剂对有机污染物的降解机理。
（2）石墨烯/TiO2复合催化剂的制备及其降解有机污染物性能研究
以商业P25粉（TiO2）和氧化石墨为前驱物，先后在180℃水热和450℃高温下，制得了GE/TiO2复合催化剂。利用XRD、SEM、FT-IR、UV-vis DRS等测试手段对所制备的催化剂进行了表征。
从吸附能力上，GE/TiO2对RB、MB和MO比改性前的纯TiO2都有所提高，在可见光下，纯TiO2对RB和MB具有一定的降解效果，但是对MO溶液效果却很弱，GE/TiO2的可见光催化性能相对于纯TiO2有了较大提高。而在紫外光照射下降解速率远远高于可见光，在紫外光照射下，光照70min后MO的降解率达到95.6%，60min后RB的降解率达到99.1%，70min后MB的降解率达到99.4%。探讨了GE/TiO2复合催化剂对有机污染物的降解机理。
（3）苯酚光催化氧化羟基化制备邻苯二酚（CAL）和对苯二酚（HQE）
分别以纯TiO2、GE/TiO2和BYH3G/TiO2为催化剂对苯酚进行光催化羟基化反应。在可见光照射下仅以BYH3G/TiO2为催化剂时检测到少量的CAL和HQE的生成。在紫外光照射下，GE/TiO2和BYH3G/TiO2均显示出较好的光催化活性和较高羟基化选择性。实验考察了催化剂用量、光照时间和H2O2用量对苯酚光催化羟基化反应的影响。以TiO2为催化剂时，苯酚最高转化率为66.9%，CAL和HQE的收率分别为12.6%和4.6%，反应选择性为25.7%；以GE/TiO2为催化剂时，苯酚的最高转化率为92.1%，CAL和HQE收率分别为19.8%和11.2%，反应选择性为33.6%。以BYH3G/TiO2为催化剂时，苯酚最高的转化率为63.0%，CAL和HQE的收率分别为28.7%和27.6%，反应选择性高达89.3%。从CAL和HQE的高收率的角度考虑，BYH3G/TiO2的羟基化效果最好，GE/TiO2次之，纯TiO2最差。推测了光催化羟基化的反应机理。
Photocatalytic oxidation, one of advanced oxidation technologies, has importantroles to water-splitting for hydrogen production, photocatalytic synthesis and thedegradation of organic contaminants. Photocatalytic oxidation has importantapplication feature in global warming, energy problems and environmental issues, etc.The widely explored TiO2has been accepted as an excellent photocatalyst among thesemiconductors due to its advantages of stability, low toxicity and high activity.However, the large band–gap energy (3.2eV) of TiO2considerably limits theutilization of natural solar light or artificial visible light. Photosensitization isconsidered to be an efficient and general method to modify the photoresponseproperties of TiO2.
In this thesis, using commercial organic pigments and graphene as modifier tomodify TiO2to expand visible light absorption performance of TiO2. The structuresand property of modified catalyst were studied. There are three main parts in thisthesis:
(1) TiO2photocatalyst sensitized with commercial organic pigment wasconveniently prepared and characterized by FT-IR, UV-Vis, XRD, SEM and N2adsorption-desorption isotherms. The adsorption capacities and photocatalyticactivities of the new photocatalyst were evaluated by photocatalytic degradation ofseveral kinds of representative pollutants under visible light irradiation. The resultsindicated that the new photocatalyst extends the photoresponse of TiO2from the UVto the visible region. The degradation rates of dyes RB (Rhodamine B), ACBK (AcidChrome Blue K) and MO (Methyl Orange) were24.8%,34.8%and9.4%respectivelyat their initial pH values in a fixed time under visible light irradiation with pure TiO2as the catalyst, while the degradation rates reach up to93.5%,94.6%and89.2%respectively in the present of BYH3G/TiO2(Benzimidazolone Yellow H3G/TiO2)under the same conditions. There was no appreciable loss of photocatalytic activityobserved when the photocatalyst was used four times, which demonstrates excellentstability and recyclability factors. Furthermore, sensitized TiO2with Pigment Red254,Pigment Red151, Pigment Red179, Phthalocyanine Green G, Pigment Red122wereprepared, and they all display better visible light catalytic activity than pure TiO2inthe degradation of MO and RB test under visible light irradiation. The mechanism ofaction was also discussed.
(2) Graphene/TiO2(GE/TiO2) was prepared by hydrothermal treating of a mixedsuspension of TiO2and graphite oxide. The prepared catalyst was characterized byFT-IR, UV-Vis, XRD and SEM. The adsorption capacity of GE/TiO2for RB、MB(Methlyene Blue) and MO was better than pure TiO2. Pure TiO2has a little bit ofdegradation capacity for RB and MB, but has no degradation capacity for MO, thevisible-light degradation ability of GE/TiO2was better than the pure TiO2. In addition,the degradation rate in the presence of UV light was far better than that of visible light.The degradation rate of MO was95.6%in70min under UV light irradiation, thedegradation rate of RB was99.1%in60min, and the degradation rate of MB was99.4%in70min. The mechanism of action was also discussed.
(3) Phenol photocatalytic oxidation experiment was carried out under ultravioletand visible light irradiation with the pure TiO2, GE/TiO2and BYH3G/TiO2catalysts.Under visible light irradiation, phenol was relatively stable and only a little catecholwas produced when use BYH3G/TiO2as the catalyst. While under UV-lightirradiation, there were obvious photocatalytic oxidations for phenol, and most phenolwas hydroxylated to pyrocatechol (CAL) and hydroquinone (HQE), others werephotocatalytic oxidized into benzoquinone or other materials. The effects of variousparameters on photocatalytic oxidation of phenol were studied. When using TiO2ascatalyst, the highest conversion of phenol was66.9%, and the yield of CAL and HQEwere12.6%and4.6%respectively, and the selectivity of the reaction was25.7%.Using GE/TiO2as catalyst, the highest conversion of phenol was92.1%, and the yieldof CAL and HQE yield were19.8%and11.2%, the selectivity was33.6%. UsingBYH3G/TiO2as catalyst, the highest conversion of phenol was63%, the yield ofCAL and HQE can reach28.7%and27.6%respectively, and the selectivity of thereaction was up to89.3%. From high yield of CAL and HQE perspective,BYH3G/TiO2was the best hydroxylation catalyst, the second was GE/TiO2, and theworst was pure TiO2. The mechanism of photocatalysis of the catalysts was inferred.
引文
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