CN101891296A - A kind of ozonation water treatment method using the Y-type zeolite of supporting rare earth oxide CeO2 and La2O3 as a catalyst - Google Patents
A kind of ozonation water treatment method using the Y-type zeolite of supporting rare earth oxide CeO2 and La2O3 as a catalyst Download PDFInfo
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- 239000010457 zeolite Substances 0.000 title claims abstract description 31
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910021536 Zeolite Inorganic materials 0.000 title claims abstract description 29
- 238000006385 ozonation reaction Methods 0.000 title claims abstract description 23
- 229910001404 rare earth metal oxide Inorganic materials 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000003054 catalyst Substances 0.000 title abstract description 9
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 title 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 title 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 title 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 title 1
- 230000003197 catalytic effect Effects 0.000 claims abstract description 20
- 239000002957 persistent organic pollutant Substances 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 4
- 238000010525 oxidative degradation reaction Methods 0.000 claims 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 abstract description 15
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 238000013019 agitation Methods 0.000 abstract 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 20
- 238000006243 chemical reaction Methods 0.000 description 7
- 238000003756 stirring Methods 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 239000002351 wastewater Substances 0.000 description 5
- 239000003344 environmental pollutant Substances 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 2
- 238000007210 heterogeneous catalysis Methods 0.000 description 2
- 238000007172 homogeneous catalysis Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000011949 solid catalyst Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 229910021193 La 2 O 3 Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000033558 biomineral tissue development Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000002144 chemical decomposition reaction Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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Abstract
本发明提出了一种利用负载稀土氧化物的Y型沸石作为催化剂的臭氧化水处理方法，其特征在于将人工合成而又负载稀土氧化物的Y型沸石(又称分子筛)添加到臭氧化水处理体系中，搅拌条件下通入臭氧，进行臭氧化处理；负载过程并没有降低表面积，通常BET比表面积仍可达500m2g-1以上，并且负载后提高了表面羟基密度，有助于获得更好的催化性能。The present invention proposes a method for treating ozonated water using Y-type zeolite loaded with rare earth oxides as a catalyst. In the treatment system, ozone is introduced under agitation for ozonation treatment; the loading process does not reduce the surface area, usually the BET specific surface area can still reach more than 500m 2 g -1 , and the surface hydroxyl density is increased after loading, which helps to obtain Better catalytic performance.
Description
技术领域technical field
本发明提出一种利用负载稀土氧化物的Y型沸石作为催化剂、催化臭氧化降解水中有机污染物、从而消除污染的水处理方法，属于环境催化和水处理领域。The invention proposes a water treatment method that uses Y-type zeolite loaded with rare earth oxides as a catalyst to catalyze ozonation to degrade organic pollutants in water, thereby eliminating pollution, and belongs to the field of environmental catalysis and water treatment.
背景技术Background technique
芳香类污染物是工业废水中常见的污染物，是石油化工、化学、制药等行业中常见的原材料，具有毒性大、难降解等特点。近来，关于水中芳香类有机污染物的化学降解方法的研究引起了广泛关注。Aromatic pollutants are common pollutants in industrial wastewater, and are common raw materials in petrochemical, chemical, pharmaceutical and other industries. They are highly toxic and difficult to degrade. Recently, research on chemical degradation methods of aromatic organic pollutants in water has attracted widespread attention.
催化臭氧化作为方便实用的高级氧化技术，在水处理中具有重要的应用前景。催化臭氧化可以分为均相催化和多相催化，前者是溶液体系中的离子发挥催化作用，而后者是依靠固体催化剂表面发挥催化作用。同均相催化相比较，多相催化的一个优势是避免了溶解的离子带来的二次污染，因为许多金属离子也是环境有害的。为了提高臭氧化效率，人们开发了多种固体催化剂。然而从实际应用的角度来看，高效稳定的多相催化材料依然是比较少见的，开发活性高、性能稳定的臭氧化催化剂，对于提高催化臭氧化的实际应用价值是非常重要的。As a convenient and practical advanced oxidation technology, catalytic ozonation has an important application prospect in water treatment. Catalytic ozonation can be divided into homogeneous catalysis and heterogeneous catalysis. The former is catalyzed by ions in the solution system, while the latter is catalyzed by the surface of a solid catalyst. One advantage of heterogeneous catalysis over homogeneous catalysis is the avoidance of secondary pollution from dissolved ions, since many metal ions are also environmentally harmful. In order to improve ozonation efficiency, various solid catalysts have been developed. However, from the perspective of practical application, highly efficient and stable heterogeneous catalytic materials are still relatively rare. It is very important to develop ozonation catalysts with high activity and stable performance to improve the practical application value of catalytic ozonation.
发明内容Contents of the invention
本发明的目的，是提供一种新型、稳定的催化材料及其使用方法，以提高催化臭氧化的实用价值。The purpose of the present invention is to provide a novel and stable catalytic material and its application method, so as to improve the practical value of catalytic ozonation.
Y型沸石材料是一类众所周知的多孔材料，被广泛应用为吸附材料或者催化剂载体，然而并未在臭氧化水处理中得到应用。我们已经提出将Y沸石作为臭氧化催化材料，研究了其使用方法，取得了良好的效果(中国专利，公开号：CN 101585577A)。在进一步的研究中发现，负载稀土氧化物的Y沸石在催化臭氧化中表现了更好的催化性能，因此本发明提出以负载稀土氧化物的Y型沸石作为催化剂、催化臭氧化降解水中有机污染物。Y-type zeolite materials are a well-known class of porous materials, which are widely used as adsorption materials or catalyst supports, but have not been applied in ozonated water treatment. We have proposed Y zeolite as the ozonation catalytic material, studied its application method, and achieved good results (Chinese patent, publication number: CN 101585577A). In further research, it was found that Y zeolite loaded with rare earth oxides showed better catalytic performance in catalytic ozonation, so the present invention proposes to use Y-type zeolite loaded with rare earth oxides as a catalyst to catalyze ozonation to degrade organic pollution in water things.
本发明的具体内容包括：Concrete content of the present invention includes:
(1)提出了一种利用负载稀土氧化物的Y型沸石作为催化剂的臭氧化水处理方法，其特征在于将人工合成而又负载稀土氧化物的Y型沸石(又称分子筛)添加到臭氧化水处理体系中，搅拌条件下通入臭氧，进行臭氧化处理；(1) Propose a kind of ozonation water treatment method that utilizes the Y-type zeolite of loading rare earth oxide as catalyst, it is characterized in that artificially synthesized and the Y-type zeolite (also known as molecular sieve) of loading rare earth oxide is added to ozonation In the water treatment system, ozone is introduced under stirring conditions for ozonation treatment;
(2)臭氧化处理完毕，通过静置、离心、过滤等方法，将负载稀土氧化物的Y型沸石分离出来，用于下一次的催化过程；(2) After the ozonation treatment is completed, the Y-type zeolite loaded with rare earth oxides is separated by standing, centrifuging, filtering and other methods, and is used for the next catalytic process;
上述臭氧化处理过程通常在5-35℃室温条件下进行，添加沸石与所处理水的质量相对比例通常在0.001-0.05之间。所用的Y型沸石可以是钠型的，也可以是经过离子交换后变为氢型的；所用的Y型沸石结构中硅铝的相对含量可以不同，在本发明的方法中负载稀土氧化物后都可以用作催化材料。本发明中负载的稀土氧化物是指CeO2和La2O3。The above ozonation treatment process is usually carried out at room temperature of 5-35° C., and the relative mass ratio of added zeolite to treated water is usually between 0.001-0.05. The Y-type zeolite used can be sodium-type, or it can become hydrogen-type after ion exchange; the relative content of silicon-alumina in the Y-type zeolite structure used can be different, after the rare earth oxide is loaded in the method of the present invention can be used as catalytic materials. The supported rare earth oxides in the present invention refer to CeO 2 and La 2 O 3 .
采用上述负载稀土氧化物的Y型沸石作为催化剂后，在相同的臭氧投入量情况下，对有机污染物的降解速率有所加快，矿化程度显著提高。具体提高程度与加入的催化剂相对比例以及反应条件(包括温度、搅拌速率、污染物浓度、臭氧投入量、水体pH等)有关。After adopting the above-mentioned Y-type zeolite loaded with rare earth oxides as a catalyst, under the same input amount of ozone, the degradation rate of organic pollutants is accelerated, and the degree of mineralization is significantly improved. The specific improvement degree is related to the relative proportion of catalyst added and reaction conditions (including temperature, stirring speed, pollutant concentration, ozone input amount, water pH, etc.).
与现有处理方法相比较，本发明提出的水处理方法具有显著的特点：Compared with existing treatment methods, the water treatment method proposed by the present invention has remarkable characteristics:
(1)负载稀土氧化物的Y型沸石是一类多孔材料，负载过程并没有降低表面积，通常BET比表面积仍可达500m2g-1以上，颗粒尺度较小(微米级别)，在水中具有较好的分散性，并且负载后提高了表面羟基密度，这对于提高催化性能是非常关键的。正是因为如此优势，在使用中较小的投入量即可取得较好的催化效果；(1) The Y-type zeolite loaded with rare earth oxides is a kind of porous material, and the loading process does not reduce the surface area. Usually, the BET specific surface area can still reach more than 500m 2 g -1 , and the particle size is small (micron level). Better dispersibility, and increased surface hydroxyl density after loading, which is very critical for improving catalytic performance. It is precisely because of this advantage that a relatively small amount of input can achieve a better catalytic effect in use;
(2)负载稀土氧化物的Y型沸石具有较好的机械强度，在催化臭氧化条件下显示了较好的稳定性，重复使用多次，催化效果能够得到较好的保持，这对于其实际应用是另一个关键因素。(2) The Y-type zeolite loaded with rare earth oxides has good mechanical strength, shows good stability under catalytic ozonation conditions, and can be reused many times, and the catalytic effect can be well maintained. Application is another key factor.
(3)负载稀土氧化物的Y型沸石对水中苯酚的吸附性能非常微弱，其催化作用主要来自沸石表面促进臭氧分子的分解，因此污染物分子对其影响非常小，这也是其稳定性好的原因之一。(3) Y-type zeolite loaded with rare earth oxides has very weak adsorption performance on phenol in water, and its catalytic effect mainly comes from the surface of zeolite to promote the decomposition of ozone molecules, so pollutant molecules have very little influence on it, which is also its good stability one of the reasons.
(4)负载稀土氧化物的Y型沸石材料目前已经实现商品化，价格相对便宜，为其实用提供了重要的保障。(4) The Y-type zeolite material loaded with rare earth oxides has been commercialized at present, and the price is relatively cheap, which provides an important guarantee for its practicality.
附图说明Description of drawings
附图1是实施例1中苯酚随时间的变化曲线图。Accompanying drawing 1 is the variation curve graph of phenol with time in embodiment 1.
附图2是实施例2中苯酚随时间的变化曲线图。Accompanying drawing 2 is the variation graph of phenol with time in embodiment 2.
附图3是实施例3中苯酚随时间的变化曲线图。Accompanying drawing 3 is the variation curve graph of phenol with time in embodiment 3.
附图4是实施例4中苯酚随时间的变化曲线图。Accompanying drawing 4 is the change curve graph of phenol with time in embodiment 4.
具体实施方式Detailed ways
本发明以处理含苯酚水为例，来说明其催化效果与实施方式，但本发明的范围不限于此。The present invention takes the treatment of phenol-containing water as an example to illustrate its catalytic effect and implementation, but the scope of the present invention is not limited thereto.
实施例1Example 1
在200ml含苯酚初始浓度为100mg L-1的模拟废水中，添加负载稀土氧化物的Y型沸石1.0g，开动搅拌，在反应温度20℃下通入臭氧流量0.47mg min-1的臭氧，记录不同时间下苯酚的浓度。结果如图1所示，表明沸石的加入显著促进了苯酚的降解。In 200ml of simulated wastewater containing phenol with an initial concentration of 100mg L -1 , add 1.0g of Y-type zeolite loaded with rare earth oxides, start stirring, and inject ozone with an ozone flow rate of 0.47mg min -1 at a reaction temperature of 20°C, and record The concentration of phenol at different times. The results are shown in Fig. 1, indicating that the addition of zeolite significantly promoted the degradation of phenol.
实施例2Example 2
在200ml含苯酚初始浓度为100mg L-1的模拟废水中，添加负载稀土氧化物的Y型沸石1.0g，开动搅拌，在反应温度5℃下通入臭氧流量0.47mg min-1的臭氧，记录不同时间下苯酚的浓度。结果如图2所示，表明沸石的加入显著促进了苯酚的降解。In 200ml of simulated wastewater containing phenol with an initial concentration of 100mg L -1 , add 1.0g of Y-type zeolite loaded with rare earth oxides, start stirring, and inject ozone with an ozone flow rate of 0.47mg min -1 at a reaction temperature of 5°C, and record The concentration of phenol at different times. The results are shown in Fig. 2, indicating that the addition of zeolite significantly promoted the degradation of phenol.
实施例3Example 3
在200ml含苯酚初始浓度为100mg L-1的模拟废水中，添加负载稀土氧化物的Y型沸石1.0g，开动搅拌，在反应温度35℃下通入臭氧流量0.47mg min-1的臭氧，记录不同时间下苯酚的浓度。结果如图3所示，表明沸石的加入显著促进了苯酚的降解。In 200ml of simulated wastewater containing phenol with an initial concentration of 100mg L -1 , add 1.0g of Y-type zeolite loaded with rare earth oxides, start stirring, and inject ozone with an ozone flow rate of 0.47mg min -1 at a reaction temperature of 35°C, and record The concentration of phenol at different times. The results are shown in Fig. 3, indicating that the addition of zeolite significantly promoted the degradation of phenol.
实施例4Example 4
在200ml含苯酚初始浓度为100mg L-1的模拟废水中，添加负载稀土氧化物的Y型沸石1.0g，开动搅拌，在反应温度20℃下通入臭氧流量0.47mg min-1的臭氧60分钟，记录苯酚的浓度。反应结束后，将沸石滤出，再投入200ml含苯酚初始浓度为100mg L-1的模拟废水中，在反应温度20℃下通入臭氧流量047mg min-1的臭氧60分钟，记录苯酚的浓度。结果如图4所示，表明沸石的加入显著促进了苯酚的降解，并且在重复使用中催化活性保持较好的稳定性。In 200ml of simulated wastewater containing phenol with an initial concentration of 100mg L -1 , add 1.0g of Y-type zeolite loaded with rare earth oxides, start stirring, and pass ozone with an ozone flow rate of 0.47mg min -1 at a reaction temperature of 20°C for 60 minutes , record the concentration of phenol. After the reaction, the zeolite was filtered out, and then put into 200ml of simulated wastewater containing phenol with an initial concentration of 100mg L -1 , and ozone with an ozone flow rate of 047mg min -1 was introduced at a reaction temperature of 20°C for 60 minutes, and the concentration of phenol was recorded. The results are shown in Figure 4, indicating that the addition of zeolite significantly promoted the degradation of phenol, and the catalytic activity maintained good stability during repeated use.
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| CN105854925B (en) * | 2016-05-04 | 2018-10-19 | 北京高能时代环境技术股份有限公司 | A kind of support type ozone catalyst and its preparation and application |
| CN106964333A (en) * | 2017-04-05 | 2017-07-21 | 天津万峰环保科技有限公司 | The method that rare earth loaded catalyst for handling sewage and its preparation method and application and catalytic ozonation handle sewage |
| CN106964333B (en) * | 2017-04-05 | 2020-06-26 | 天津万峰环保科技有限公司 | Rare earth supported catalyst for treating sewage, preparation method and application thereof, and method for treating sewage by catalytic oxidation of ozone |
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