光催化合成萘酚的研究
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摘要
萘酚(1-萘酚、2-萘酚),是重要的精细化工中间体,广泛应用于医药、农药、染料、香料制造等行业。TiO_2作为光催化剂,在芳香化合物光催化羟基化方面的应用越来越受到重视。
利用P-25型TiO_2对萘进行光催化,在不加H_2O_2的体系中,萘的转化率很低,仅有2%左右,加入适当浓度的H_2O_2,萘的转化率能提高至19.6%,1-萘酚的收率为2.5%左右。
利用Photo-Fenton反应和Photo-Fenton-like反应对萘进行了光催化羟基化反应。考察了Fe~(2+)或者Fe~(3+)初始浓度、H_2O_2初始浓度、反应时间等不同因素对反应的影响。Fenton-like反应对萘的光催化羟基化比Fenton反应快。萘的转化率很大程度上取决于Fe~(2+)或者Fe~(3+)的初始浓度以及H_2O_2的初始浓度。在合适的Fe~(2+)或者Fe~(3+)以及H_2O_2初始浓度的情况下,萘的转化率能达到80%以上,1-萘酚收率4.6%。不管在Photo-Fenton反应还是Photo-Fenton-like反应体系中,紫外光照射对萘的转化率影响很小。
利用浸渍法制备了Fe~(3+)、Cu~(2+)、Ag~+掺杂P-25型TiO_2,发现经过掺杂催化剂晶型没有发生变化。Fe~(3+)掺杂P-25光催化活性比P-25稍高,而Cu~(2+)、Ag~+掺杂P-25光催化剂以及通过溶胶-凝胶法制备的Fe~(3+)、Cu~(2+)、Ag~+掺杂的锐钛矿型TiO_2,光催化活性均比P-25低。经过H_2O_2改性的锐钛矿型TiO_2和P-25相比,萘的转化率基本一致,但生成萘酚的选择性高。
实验中制备的纳米CdS、介孔分子筛MCM-41对萘的光催化有一定活性,但萘的转化率5%左右,1-萘酚收率1.4%左右,都低于P-25的光催化活性。
Naphthol(1-naphthol, 2-naphthol), is an important fine chemical intermediate, widely used in medicine, pesticides, dyes, perfume manufacturing industry. Titanium dioxide catalysts have attracted a great deal of attention as a photocatalyst of hydroxylation of aromatic compounds.
Hydroxylation of naphthalene in the presence of P-25 TiO_2 as photocatalyst was investigated. In the absence of H_2O_2, the naphthalene conversion was rather low, while proper H_2O_2 was added to the reaction system, naphthalene conversion, as well as 1-naphthol yield, enhanced rapidly.
Hydroxylation of naphthalene using Photo-Fenton(Fe~(2+)/H_2O_2) or Photo-Fenton-like(Fe~(3+)/H_2O_2) reactions was investigated under neutral conditions. The effects of different systems variable initial concentration of Fe~(2+)or Fe~(3+), initial concentration of H_2O_2, reaction time were studied. Hydroxylation of naphthalene in Photo-Fenton-like reaction was faster than Fenton reaction.
The naphthalene conversion was strongly dependent on the initial concentration of Fe~(2+) or Fe~(3+), the initial concentration of H_2O_2. High naphthalene conversion was achieved at proper concentrations of Fe~(2+)/Fe~(3+)and H_2O_2. The UV irradiation had little effect on overall naphthalene conversion in the Fenton reaction or Fenton-like reaction.
Fe~(3+), Cu~(2+), Ag~+-doped P-25 was prepared by impregnation method. Compared metal-doped TiO_2 to P-25, there was no change in crystal form. While photocatlytic hydroxylation of naphthalene, Fe~(3+)-doped P-25 photocatalytic activity was higher than the P-25, followed by Cu~(2+)-doped P-25 and Ag~+-doped P-25. We also prepared Fe~(3+), Cu~(2+), Ag~+-doped anatase TiO_2 through the sol-gel method. Their photocatalytic activities were lower than P-25. The anatase TiO_2 modified by H_2O_2 is almost the same in the naphthalene conversion, but the selectivity of 1-naphthol increased.
CdS, as well as mesoporous molecular sieve MCM-41, was prepared in the experiments. Although they all had photocatalytic activity in hydroxylation of naphthalene, much lower than P-25 photocatalytic activity.
利用P-25型TiO_2对萘进行光催化,在不加H_2O_2的体系中,萘的转化率很低,仅有2%左右,加入适当浓度的H_2O_2,萘的转化率能提高至19.6%,1-萘酚的收率为2.5%左右。
利用Photo-Fenton反应和Photo-Fenton-like反应对萘进行了光催化羟基化反应。考察了Fe~(2+)或者Fe~(3+)初始浓度、H_2O_2初始浓度、反应时间等不同因素对反应的影响。Fenton-like反应对萘的光催化羟基化比Fenton反应快。萘的转化率很大程度上取决于Fe~(2+)或者Fe~(3+)的初始浓度以及H_2O_2的初始浓度。在合适的Fe~(2+)或者Fe~(3+)以及H_2O_2初始浓度的情况下,萘的转化率能达到80%以上,1-萘酚收率4.6%。不管在Photo-Fenton反应还是Photo-Fenton-like反应体系中,紫外光照射对萘的转化率影响很小。
利用浸渍法制备了Fe~(3+)、Cu~(2+)、Ag~+掺杂P-25型TiO_2,发现经过掺杂催化剂晶型没有发生变化。Fe~(3+)掺杂P-25光催化活性比P-25稍高,而Cu~(2+)、Ag~+掺杂P-25光催化剂以及通过溶胶-凝胶法制备的Fe~(3+)、Cu~(2+)、Ag~+掺杂的锐钛矿型TiO_2,光催化活性均比P-25低。经过H_2O_2改性的锐钛矿型TiO_2和P-25相比,萘的转化率基本一致,但生成萘酚的选择性高。
实验中制备的纳米CdS、介孔分子筛MCM-41对萘的光催化有一定活性,但萘的转化率5%左右,1-萘酚收率1.4%左右,都低于P-25的光催化活性。
Naphthol(1-naphthol, 2-naphthol), is an important fine chemical intermediate, widely used in medicine, pesticides, dyes, perfume manufacturing industry. Titanium dioxide catalysts have attracted a great deal of attention as a photocatalyst of hydroxylation of aromatic compounds.
Hydroxylation of naphthalene in the presence of P-25 TiO_2 as photocatalyst was investigated. In the absence of H_2O_2, the naphthalene conversion was rather low, while proper H_2O_2 was added to the reaction system, naphthalene conversion, as well as 1-naphthol yield, enhanced rapidly.
Hydroxylation of naphthalene using Photo-Fenton(Fe~(2+)/H_2O_2) or Photo-Fenton-like(Fe~(3+)/H_2O_2) reactions was investigated under neutral conditions. The effects of different systems variable initial concentration of Fe~(2+)or Fe~(3+), initial concentration of H_2O_2, reaction time were studied. Hydroxylation of naphthalene in Photo-Fenton-like reaction was faster than Fenton reaction.
The naphthalene conversion was strongly dependent on the initial concentration of Fe~(2+) or Fe~(3+), the initial concentration of H_2O_2. High naphthalene conversion was achieved at proper concentrations of Fe~(2+)/Fe~(3+)and H_2O_2. The UV irradiation had little effect on overall naphthalene conversion in the Fenton reaction or Fenton-like reaction.
Fe~(3+), Cu~(2+), Ag~+-doped P-25 was prepared by impregnation method. Compared metal-doped TiO_2 to P-25, there was no change in crystal form. While photocatlytic hydroxylation of naphthalene, Fe~(3+)-doped P-25 photocatalytic activity was higher than the P-25, followed by Cu~(2+)-doped P-25 and Ag~+-doped P-25. We also prepared Fe~(3+), Cu~(2+), Ag~+-doped anatase TiO_2 through the sol-gel method. Their photocatalytic activities were lower than P-25. The anatase TiO_2 modified by H_2O_2 is almost the same in the naphthalene conversion, but the selectivity of 1-naphthol increased.
CdS, as well as mesoporous molecular sieve MCM-41, was prepared in the experiments. Although they all had photocatalytic activity in hydroxylation of naphthalene, much lower than P-25 photocatalytic activity.
引文
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