CN103447090A - P-methyl benzoic acid uranyl complex photocatalyst - Google Patents
P-methyl benzoic acid uranyl complex photocatalyst Download PDFInfo
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- CN103447090A CN103447090A CN2013103139079A CN201310313907A CN103447090A CN 103447090 A CN103447090 A CN 103447090A CN 2013103139079 A CN2013103139079 A CN 2013103139079A CN 201310313907 A CN201310313907 A CN 201310313907A CN 103447090 A CN103447090 A CN 103447090A
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 30
- LPNBBFKOUUSUDB-UHFFFAOYSA-N p-toluenecarboxylic acid Natural products CC1=CC=C(C(O)=O)C=C1 LPNBBFKOUUSUDB-UHFFFAOYSA-N 0.000 title claims abstract description 15
- -1 uranyl p-toluate Chemical compound 0.000 claims abstract description 13
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 5
- 239000013078 crystal Substances 0.000 claims description 4
- 125000005289 uranyl group Chemical group 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 abstract description 6
- 239000000975 dye Substances 0.000 abstract description 5
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 4
- 238000000926 separation method Methods 0.000 abstract description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 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 description 6
- 229940043267 rhodamine b Drugs 0.000 description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000003912 environmental pollution Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- COQLPRJCUIATTQ-UHFFFAOYSA-N Uranyl acetate Chemical compound O.O.O=[U]=O.CC(O)=O.CC(O)=O COQLPRJCUIATTQ-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000003933 environmental pollution control Methods 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 239000000447 pesticide residue Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 238000001144 powder X-ray diffraction data Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 150000003462 sulfoxides Chemical class 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 229910002007 uranyl nitrate Inorganic materials 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
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Abstract
本发明公开了一种对甲基苯甲酸铀酰配合物光催化剂,该对甲基苯甲酸铀酰配合物光催化剂分子式为[(UO2)(C2H6SO)(p–CH3–C6H4–COO)2]2,式中p–CH3–C6H4–COOH为对甲基苯甲酸;该对甲基苯甲酸铀酰配合物光催化剂可降解染料和有机污染物,且该对甲基苯甲酸铀酰配合物光催化剂可用离心分离方法回收再利用,避免该催化剂可能引起的二次污染。
The invention discloses a uranyl p-toluate complex photocatalyst, the photocatalyst molecular formula of the uranyl p-toluate complex is [(UO 2 )(C 2 H 6 SO)(p-CH 3 - C 6 H 4 –COO) 2 ] 2 , where p–CH 3 –C 6 H 4 –COOH is p-toluic acid; the photocatalyst of the p-toluic acid uranyl complex can degrade dyes and organic pollutants , and the uranyl p-toluate complex photocatalyst can be recovered and reused by centrifugal separation, so as to avoid secondary pollution that may be caused by the catalyst.
Description
技术领域technical field
本发明涉及光催化剂,具体涉及一种对甲基苯甲酸铀酰配合物光催化剂。The invention relates to a photocatalyst, in particular to a photocatalyst of p-toluic acid uranyl complex.
背景技术Background technique
随着工业进程的发展,人们的生活水平得到了大幅度提高,但与此同时也给人们赖以生存的环境带来了破坏性的影响。每年都会有大量的染料、激素、残余农药等对我们的健康有极大威胁的有害物质不断地排入江河湖海,这些有害物质给生物的生存带来了极大的影响。如何低能耗,低耗费,高效能的去除工业废水中的染料等有毒物质已成为人们关注的焦点,而使用光催化剂来解决这一问题无疑是最佳的选择。由于光催化技术具有可以直接利用太阳能来解决能源的枯竭和地球环境污染等问题的潜在应用,因而光催化剂的制备引起了人们的极大兴趣。对环境污染问题,各国环境科学工作者在光催化这一领域进行了广泛而深入的探索,取得了许多可喜的成绩,并在环保方面得到了应用。尤其是光催化技术可以将水中的许多有机污染物降解为CO2和H2O等简单的无机物,具有能耗低、操作简便、反应条件温和,催化剂可回收再利用无二次污染和分解速度快等优点,成为新的高效节能的环境污染治理技术,如公开号为CN1618518的发明专利申请,就公开了以TiO2和ZnO为原料的复合光催化剂,可用于治理环境污染。针对这一问题,本发明开发出一种光催化降解性能良好的铀酰配合物光催化剂。With the development of industrial processes, people's living standards have been greatly improved, but at the same time, it has also brought destructive effects on the environment on which people live. Every year, a large amount of harmful substances such as dyes, hormones, and pesticide residues that pose a great threat to our health are continuously discharged into rivers, lakes and seas. These harmful substances have brought a great impact on the survival of organisms. How to remove toxic substances such as dyes in industrial wastewater with low energy consumption, low consumption and high efficiency has become the focus of attention, and using photocatalysts to solve this problem is undoubtedly the best choice. Since photocatalytic technology has the potential application of directly using solar energy to solve the problems of energy depletion and global environmental pollution, the preparation of photocatalysts has aroused great interest. Regarding the problem of environmental pollution, environmental scientists from various countries have conducted extensive and in-depth explorations in the field of photocatalysis, and have achieved many gratifying achievements, which have been applied in environmental protection. In particular, photocatalytic technology can degrade many organic pollutants in water into simple inorganic substances such as CO 2 and H 2 O. It has low energy consumption, simple operation, mild reaction conditions, and the catalyst can be recycled and reused without secondary pollution and decomposition. The advantages such as fast speed have become a new high-efficiency and energy-saving environmental pollution control technology. For example, the invention patent application with the publication number CN1618518 discloses a composite photocatalyst using TiO2 and ZnO as raw materials, which can be used to control environmental pollution. To solve this problem, the present invention develops a uranyl complex photocatalyst with good photocatalytic degradation performance.
发明内容Contents of the invention
本发明所要解决的技术问题是提供一种可降解染料和有机污染物的对甲基苯甲酸铀酰配合物光催化剂。The technical problem to be solved by the invention is to provide a uranyl p-toluate photocatalyst capable of degrading dyes and organic pollutants.
本发明解决上述技术问题所采用的技术方案为:一种对甲基苯甲酸铀酰配合物光催化剂,其分子式为[(UO2)(C2H6SO)(p–CH3–C6H4–COO)2]2,式中p–CH3–C6H4–COOH为对甲基苯甲酸。The technical scheme adopted by the present invention to solve the above technical problems is: a photocatalyst of uranyl p-toluate complex, the molecular formula of which is [(UO 2 )(C 2 H 6 SO)(p-CH 3 -C 6 H 4 -COO) 2 ] 2 , where p-CH 3 -C 6 H 4 -COOH is p-toluic acid.
该对甲基苯甲酸铀酰配合物光催化剂晶体的晶胞参数为: β=99.13(3)°。为单斜晶系,属于C2/c空间群。The unit cell parameters of the uranyl p-toluate complex photocatalyst crystal are: β=99.13(3)°. It is monoclinic and belongs to C2/c space group.
与现有技术相比,本发明的优点在于一种对甲基苯甲酸铀酰配合物光催化剂,该光催化剂的分子式为[(UO2)(C2H6SO)(p–CH3–C6H4–COO)2]2,分子式中C2H6SO为二甲基亚砜,p–CH3–C6H4–COOH为对甲基苯甲酸。该对甲基苯甲酸铀酰配合物光催化剂可降解染料和有机污染物,且该对甲基苯甲酸铀酰配合物光催化剂可用离心分离方法回收再利用,避免该催化剂可能引起的二次污染。Compared with the prior art, the present invention has the advantage of a photocatalyst of uranyl p-toluate complex, the molecular formula of the photocatalyst is [(UO 2 )(C 2 H 6 SO)(p-CH 3 - C 6 H 4 -COO) 2 ] 2 , in the molecular formula, C 2 H 6 SO is dimethyl sulfoxide, and p-CH 3 -C 6 H 4 -COOH is p-toluic acid. The uranyl p-toluate complex photocatalyst can degrade dyes and organic pollutants, and the uranyl p-toluate complex photocatalyst can be recovered and reused by centrifugal separation to avoid secondary pollution that may be caused by the catalyst .
附图说明Description of drawings
图1为本发明的光催化剂的分子结构图;Fig. 1 is the molecular structure figure of photocatalyst of the present invention;
图2为本发明的光催化剂的PXRD图谱与单晶模拟PXRD图谱的对比图;Fig. 2 is the contrast figure of the PXRD collection of illustrative plates of photocatalyst of the present invention and single crystal simulation PXRD collection of collections;
图3为本发明的光催化剂对罗丹明B的光催化降解曲线图。Fig. 3 is a graph showing photocatalytic degradation of rhodamine B by the photocatalyst of the present invention.
具体实施方式Detailed ways
以下结合附图实施例对本发明作进一步详细描述。The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.
实施例1Example 1
称取0.5mmol醋酸双氧铀(UO2Ac2·2H2O)溶于10mL H2O中,溶解得黄色溶液,另称取1.5mmol对甲基苯甲酸(p–CH3–C6H4–COOH)溶于20mL水与甲醇的混合溶剂(V/V=1:1)中,搅拌溶解,随后加入0.5mL NaOH(1M);把上述两种溶液混合搅拌,溶液变浑浊,再滴加0.5mL NaOH(1M)后搅拌,过滤,得浅黄色澄清溶液,测得pH=5.47,滴加0.5mL二甲基亚砜(C2H6SO),2个月后得黄色产物,该黄色产物为分子式[(UO2)(C2H6SO)(p–CH3–C6H4–COO)2]2的一种对甲基苯甲酸铀酰配合物光催化剂。将黄色产物研磨成粉末,置于光催化剂反应器中,并将含有罗丹明B的水溶液注入其中,开启搅拌器,在氙灯500W紫外光照射下,200分钟可将水溶液中的罗丹明B降解94.1%,基本被降解完全,得到如图3所示的光催化降解曲线图,由图3可见,在500W氙灯照射没有催化剂的情况下,未加上述催化剂罗丹明B并没有发生降解,加入上述催化剂后,罗丹明B发生明显降解,200min后,基本被降解完全。铀酰配合物光催化剂可通过离心可以将催化剂回收再利用。采用Bruker D8Focus粉末衍射仪2θ角度范围为5–50°,以8°/min的扫描速度对该铀酰配合物光催化剂进行扫描,在室温下收集样品的粉末衍射图谱(PXRD),并与单晶模拟PXRD图对比,可以完美拟合,说明产物为纯相,纯度不低于99%。Weigh 0.5mmol of uranyl acetate (UO 2 Ac 2 2H 2 O) and dissolve it in 10mL of H 2 O to obtain a yellow solution, and weigh 1.5mmol of p-toluic acid (p-CH 3 -C 6 H 4 -COOH) was dissolved in 20mL of water and methanol mixed solvent (V/V=1:1), stirred to dissolve, and then 0.5mL NaOH (1M) was added; the above two solutions were mixed and stirred, the solution became cloudy, and then dripped Add 0.5mL NaOH (1M) and stir, filter to obtain a light yellow clear solution, the measured pH = 5.47, add dropwise 0.5mL dimethyl sulfoxide (C 2 H 6 SO), and obtain a yellow product after 2 months. The yellow product is a uranyl p-toluate photocatalyst with the molecular formula [(UO 2 )(C 2 H 6 SO)(p-CH 3 -C 6 H 4 -COO) 2 ] 2 . Grind the yellow product into powder, place it in a photocatalyst reactor, inject the aqueous solution containing Rhodamine B into it, turn on the agitator, and under the irradiation of 500W ultraviolet light from a xenon lamp, the Rhodamine B in the aqueous solution can be degraded by 94.1% in 200 minutes. %, is basically degraded completely, and the photocatalytic degradation curve shown in Figure 3 is obtained. It can be seen from Figure 3 that in the case of no catalyst under the irradiation of a 500W xenon lamp, Rhodamine B does not degrade without adding the above-mentioned catalyst. Adding the above-mentioned catalyst Rhodamine B was degraded obviously, and after 200 minutes, it was basically degraded completely. Uranyl complex photocatalysts can be recovered and reused by centrifugation. A Bruker D8Focus powder diffractometer with a 2θ angle range of 5–50° was used to scan the uranyl complex photocatalyst at a scanning speed of 8°/min. The powder diffraction pattern (PXRD) of the sample was collected at room temperature, and compared with a single The comparison of the crystal simulation PXRD patterns can be perfectly fitted, indicating that the product is a pure phase with a purity of not less than 99%.
实施例2Example 2
与实施例1基本相同,所不同的只是醋酸双氧铀由硝酸双氧铀替代,对甲基苯甲酸为1mmol,NaOH(1M)二次共滴加0.5mL,每次0.25mL,二甲基亚砜滴加量为1.0mL。光催化剂反应器中罗丹明B的水溶液由亚甲基橙或甲基蓝的水溶液替代。It is basically the same as Example 1, except that uranyl acetate is replaced by uranyl nitrate, p-toluic acid is 1mmol, NaOH (1M) is added dropwise 0.5mL twice, each 0.25mL, dimethyl The amount of sulfoxide added dropwise was 1.0 mL. The aqueous solution of rhodamine B in the photocatalyst reactor was replaced by the aqueous solution of methylene orange or methylene blue.
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CN107955026A (en) * | 2016-10-15 | 2018-04-24 | 宁波大学 | One kind one is hydrated malonic acid uranyl cadmium ferroelectric function material and preparation method thereof |
CN109107608A (en) * | 2017-06-23 | 2019-01-01 | 宁波大学 | A kind of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst and preparation method thereof |
CN109939739A (en) * | 2019-04-03 | 2019-06-28 | 东华理工大学 | A kind of 5-nitro-1,2,3-benzenetricarboxylic acid uranyl complex photocatalyst and preparation method thereof |
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CN109107608A (en) * | 2017-06-23 | 2019-01-01 | 宁波大学 | A kind of paranitrobenzoic acid Complexes of Uranyl photochemical catalyst and preparation method thereof |
CN111215145A (en) * | 2018-11-26 | 2020-06-02 | 宁波大学 | A kind of 2-nitroterephthalate uranyl complex photocatalyst |
CN109939739A (en) * | 2019-04-03 | 2019-06-28 | 东华理工大学 | A kind of 5-nitro-1,2,3-benzenetricarboxylic acid uranyl complex photocatalyst and preparation method thereof |
CN110003248A (en) * | 2019-04-03 | 2019-07-12 | 东华理工大学 | A kind of polycarboxylic acid Complexes of Uranyl photochemical catalyst and preparation method thereof |
CN110003248B (en) * | 2019-04-03 | 2022-09-02 | 东华理工大学 | Polycarboxylic acid uranyl complex photocatalyst and preparation method thereof |
CN114956252A (en) * | 2022-06-02 | 2022-08-30 | 华北电力大学 | Method for photocatalytic degradation of wastewater containing organic dye by using uranium-containing wastewater |
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