CN106000467A - 一种用于降解罗丹明b的光催化剂及其制备方法 - Google Patents
一种用于降解罗丹明b的光催化剂及其制备方法 Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 30
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229940043267 rhodamine b Drugs 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 230000000593 degrading effect Effects 0.000 title abstract 2
- 238000006731 degradation reaction Methods 0.000 claims abstract description 18
- 230000015556 catabolic process Effects 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 15
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 6
- 239000005711 Benzoic acid Substances 0.000 claims description 6
- 235000010233 benzoic acid Nutrition 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229940099596 manganese sulfate Drugs 0.000 claims description 5
- 235000007079 manganese sulphate Nutrition 0.000 claims description 5
- 239000011702 manganese sulphate Substances 0.000 claims description 5
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 5
- 239000011572 manganese Substances 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 3
- QNRATNLHPGXHMA-XZHTYLCXSA-N (r)-(6-ethoxyquinolin-4-yl)-[(2s,4s,5r)-5-ethyl-1-azabicyclo[2.2.2]octan-2-yl]methanol;hydrochloride Chemical group Cl.C([C@H]([C@H](C1)CC)C2)CN1[C@@H]2[C@H](O)C1=CC=NC2=CC=C(OCC)C=C21 QNRATNLHPGXHMA-XZHTYLCXSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000007146 photocatalysis Methods 0.000 claims 1
- 239000002351 wastewater Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000000975 dye Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- -1 benzoate anions Chemical class 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- GIVPFNWTXATYKC-UHFFFAOYSA-N 4-[[3,5-bis[(4-carboxyphenoxy)methyl]-2,4,6-trimethylphenyl]methoxy]benzoic acid Chemical compound CC1=C(COC=2C=CC(=CC=2)C(O)=O)C(C)=C(COC=2C=CC(=CC=2)C(O)=O)C(C)=C1COC1=CC=C(C(O)=O)C=C1 GIVPFNWTXATYKC-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229950000845 politef Drugs 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
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- 238000005070 sampling Methods 0.000 description 1
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- 239000006228 supernatant Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
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- B01J31/22—Organic complexes
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Abstract
本发明涉及废水染料处于领域，特别涉及一种用于降解罗丹明B的光催化剂及其制备方法。一种用于降解罗丹明B的光催化剂，该光催化剂化学式为C33H24O9Mn。本发明的光催化剂制备方法简单，可重复性强，容易工业化生产。本发明的光催化剂结构稳定，不但可以对罗丹明B进行吸附，而且在紫外光的作用下还能对罗丹明B进行降解。
Description
技术领域
本发明涉及废水染料处于领域，特别涉及一种用于降解罗丹明B的光催化剂及其制备方法。
背景技术
罗丹明B（Rhodamine B）又称玫瑰红B，或碱性玫瑰精，俗称花粉红，是一种具有鲜桃红色的人工合成的染料。其属于三苯甲烷类染料，被广泛应用于纺织、印刷、食品和化妆品工业中。罗丹明B染料废水的色度高，可生化性差，如果不经过处理直接排放，会引起水体环境的持久恶化。现在处理罗丹明B的常见方法是光催化降解，光催化降解污染物是近些年发展起来的一种高效的绿色环保新技术。该方法通过光催化剂在可见光或者紫外光照下产生具有高活性的自由基来破坏有机物分子结构，最终达到降解有机物的目的。
发明内容
本发明所要解决的技术问题是提供一种用于降解罗丹明B的光催化剂。
本发明的另一个目的在于提供上述光催化剂的制备方法。
一种用于降解罗丹明B的光催化剂，该光催化剂化学式为C33H24O9Mn；其中，C33H24O9为4,4',4''-(((2,4,6-三甲基苯-1,3,5-三基)三(亚甲基))三(氧代))三苯甲酸根，所述光催化剂为正交晶系，Pmc21空间群，晶胞参数为a=11.334(7) Å，b=16.264(2) Å，c=14.951(3) Å，α=β =γ=90º，V=2756.01 (2) Å3。
制备上述的用于降解罗丹明B的光催化剂的方法为：将4,4',4''-(((2,4,6-三甲基苯-1,3,5-三基)三(亚甲基))三(氧代))三苯甲酸和硫酸锰溶于水和乙腈的混合溶液当中，其中水和乙腈体积比为1:2，用氨水将混合溶液的pH调节为7.5，在室温下搅拌形成混合液A，然后将所述混合液A在35℃下静置48小时得到混合液B，最后将所述混合液B水热反应36小时后得到所述光催化剂。
其中，所述所述4,4',4''-(((2,4,6-三甲基苯-1,3,5-三基)三(亚甲基))三(氧代))三苯甲酸英文为：4,4',4''-(((2,4,6-trimethylbenzene-1,3,5-triyl)tris(methylene))tris(oxy))tribenzoic acid，其结构式如下所示：
。
优选的，所述4,4',4''-(((2,4,6-三甲基苯-1,3,5-三基)三(亚甲基))三(氧代))三苯甲酸和硫酸锰的摩尔比为1:1。
优选的，所述的水热的温度为160℃。
本发明具有如下有益效果：
本发明的光催化剂制备方法简单，可重复性强，容易工业化生产。本发明的光催化剂结构稳定，不但可以对罗丹明B进行吸附，而且在紫外光的作用下还能对罗丹明B进行降解。
具体实施方式
下面结合实施例对本发明进行详细的说明，实施例仅是本发明的优选实施方式，不是对本发明的限定。
实施例1
将1mmol 4,4',4''-(((2,4,6-三甲基苯-1,3,5-三基)三(亚甲基))三(氧代))三苯甲酸和1mmol硫酸锰溶解于5mL水和10mL乙腈的混合溶液中，用氨水将混合溶液的pH调节为7.5，在室温下搅拌30分钟溶解后形成混合液A，然后将所述混合液A在35℃下静置48小时得到混合液B，随后将所述混合液B转移到聚四氟乙烯高压反应釜中，将其放在160℃烘箱中反36小时后降至室温过滤得到光催化剂，产率53.9%（基于锰）。
然后将所得的光催化剂进行单晶表征。
该光催化剂的X射线衍射数据是在Bruker Smart Apex CCD面探衍射仪上，用MoKα辐射(λ = 0.71073 Å)，以ω扫描方式收集并进行Lp因子校正，吸收校正使用SADABS程序。用直接法解结构，然后用差值傅立叶法求出全部非氢原子坐标，并用理论加氢法得到氢原子位置(C−H 1.083 Å)，用最小二乘法对结构进行修正。计算工作在PC机上用SHELXTL程序包完成。
经测试解析可知，该光催化剂化学式为C33H24O9Mn；其中，C33H24O9为4,4',4''-(((2,4,6-三甲基苯-1,3,5-三基)三(亚甲基))三(氧代))三苯甲酸根，所述光催化剂为正交晶系，Pmc21空间群，晶胞参数为a=11.334(7) Å，b=16.264(2) Å，c=14.951(3) Å，α=β =γ=90º，V=2756.01 (2) Å3，Z=2。
实施例2
将15mg实施例1中所得的光催化剂研磨成粉末后降解罗丹明B水溶液，罗丹明B水溶液浓度为20mg/L，体积为100mL，在315nm紫外光和搅拌的作用下于常温常压催化降解罗丹明B，定时取样离心分离得上清液并用紫外可见分光光度计在罗丹明B最大吸收波长处（552nm）测量吸光度，按吸光度-浓度工作曲线换算成罗丹明B水溶液的浓度，分别计算降解时间为5分钟、10分钟、20分钟的数据，最后将光催化剂离心分离重新进行上述催化降解过程，降解率如表1所示。
表1罗丹明B降解率表
从上表数据可知，本发明的光催化剂不但可以吸附一定量的罗丹明B，而且在紫外光的作用下可以有效降解罗丹明B染料。
以上所述实施例仅表达了本发明的实施方式，其描述较为具体和详细，但并不能因此而理解为对本发明专利范围的限制，但凡采用等同替换或等效变换的形式所获得的技术方案，均应落在本发明的保护范围之内。
Claims (5)
1.一种用于降解罗丹明B的光催化剂，其特征在于：该光催化剂化学式为C33H24O9Mn；其中，C33H24O9为4,4',4''-(((2,4,6-三甲基苯-1,3,5-三基)三(亚甲基))三(氧代))三苯甲酸根。
2.根据权利要求1所述的一种用于降解罗丹明B的光催化剂，其特征在于，所述光催化剂为正交晶系，Pmc21空间群，晶胞参数为a=11.334(7) Å，b=16.264(2) Å，c=14.951(3)Å，α=β =γ=90º，V=2756.01 (2) Å3。
3.一种制备权利要求1所述的用于降解罗丹明B的光催化剂的方法，其特征在于：将4,4',4''-(((2,4,6-三甲基苯-1,3,5-三基)三(亚甲基))三(氧代))三苯甲酸和硫酸锰溶于水和乙腈的混合溶液当中，其中水和乙腈体积比为1:2，用氨水将混合溶液的pH调节为7.5，在室温下搅拌形成混合液A，然后将所述混合液A在35℃下静置48小时得到混合液B，最后将所述混合液B水热反应36小时后得到所述光催化剂。
4.根据权利要求3所述的用于降解罗丹明B的光催化剂的方法，其特征在于：所述4,4',4''-(((2,4,6-三甲基苯-1,3,5-三基)三(亚甲基))三(氧代))三苯甲酸和硫酸锰的摩尔比为1:1。
5.根据权利要求3所述的用于降解罗丹明B的光催化剂的方法，其特征在于：所述的水热的温度为160℃。
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