Preparation method and application of a mesoporous ferrous disulfide/silica microsphere composite solid-phase iron source

A microsphere and mesoporous technology is applied in the field of treatment of refractory organic pollutants, which can solve the problems of rapid loss of mineral iron sources, less surface active adsorption sites, incomplete degradation of pollutants, etc., so as to avoid secondary environmental pollution problems, Enhanced removal effect, wide-ranging effect

Active Publication Date: 2018-06-22
SOUTH CHINA SEA INST OF OCEANOLOGY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the invention is to overcome the existing solid-phase iron source heterogeneous Fenton oxidation system due to Fe 2+ The excessive ion release rate leads to incomplete degradation of pollutants, the rapid loss of mineral iron source itself and the lack of active adsorption sites on the mineral surface, which cannot be combined with H 2 o 2 and other defects that fully contact and react with pollutants, and provide a mesoporous FeS 2 / SiO 2 Microsphere composite solid-phase iron source and its preparation method, and its application to the treatment of organic pollutants in water bodies

Method used

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Embodiment 1

[0028] Example 1: Mesoporous FeS 2 / SiO2 Microsphere composite catalyst (mesoporous FeS 2 / SiO 2 Preparation of Microsphere Composite Solid Phase Iron Source)

[0029] First crush, grind, sieve and wash the massive pyrite to obtain the pretreated FeS 2 particles. Then 0.2g of dodecylamine was dissolved in ethanol, and 0.5g of pretreated FeS was added under the condition of stirring. 2 The particles formed a mixture and kept stirring for 10 min. Then, add 1.2 g of tetraethyl orthosilicate to the above mixture and keep stirring for 180 minutes to form a solid gel, use centrifugation to separate the solid gel, wash the impurities on the surface of the solid gel with ethanol, and place the solid gel in a vacuum desiccator Keep at 60°C for 240min, and finally place it in a muffle furnace for calcination and keep at 600°C for 240min to remove the template to obtain mesoporous FeS 2 / SiO 2 Microsphere composite solid phase iron source.

[0030] Mesoporous SiO 2 Preparation m...

Embodiment 2

[0032] Add the mesoporous FeS prepared in Example 1 to the water containing ciprofloxacin 2 / SiO 2 Microsphere composite solid-phase iron source, with H 2 o 2 A new Fenton oxidation system was jointly constructed for the removal of ciprofloxacin in water. The specific steps of the method for removing ciprofloxacin are as follows: a 100mL Erlenmeyer flask is used as a reactor, and 50mL of water with a concentration of ciprofloxacin of 0.10mM is used as the treatment object, and the pH of the water is adjusted to 3.0. Adding mesoporous FeS to the reactor 2 / SiO 2 The microspheres were compounded with a solid-phase iron source so that the final concentration was 1.25g / L, and then added H 2 o 2 , so that the final concentration was 3 mM, and the reactor was placed on a magnetic stirrer to maintain uniform stirring, and the reaction time was 60 min.

Embodiment 3

[0047] This embodiment is basically the same as Example 2, except that the pH of the water in the reactor is adjusted to 2, 3, 5, 7 and 9 respectively, and all the other conditions are the same as those in Example 2 to measure the removal of ciprofloxacin in the water. Effect. The result is as figure 1 shown. Depend on figure 1 It can be seen that under this new Fenton oxidation system, the removal rate of ciprofloxacin decreases with the increase of pH. During the reaction period of 60 minutes, the removal rate of ciprofloxacin reached the maximum (nearly 100%) in the range of pH 2-3. Subsequently, the removal rate of ciprofloxacin showed a trend of rapid decline with the increase of pH.

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Abstract

A preparation method for a mesoporous iron disulfide / silica microsphere composite solid-phase iron source, and an application thereof, using a sol-gel process on a natural pyrite surface to form a mesoporous SiO2 microsphere structure and prepare a mesoporous FeS2 / SiO2 microsphere composite solid-phase iron source, and combining same with H2O2 to form a new Fenton oxidation system, for use in removing ciprofloxacin from bodies of water. The mesoporous FeS2 / SiO2 microsphere compound solid-phase iron source can both effectively control an iron release rate of a mineral, lowering loss of a mineral iron source itself and operating costs caused by high use of H2O2, and also avoid problems of secondary environmental pollution caused by high release of Fe3+. In addition, the present invention can also increase a number of active sites of contact between H2O2 and pollutants, further promoting full performance of a catalytic reaction and a ciprofloxacin degradation reaction in the system, finally realizing continuous and efficient ciprofloxacin removal.

Description

technical field [0001] The invention belongs to the field of treatment of refractory organic pollutants, in particular to a mesoporous FeS 2 / SiO 2 The preparation method of the microsphere composite solid-phase iron source and its application in the removal of refractory organic pollutants. Background technique [0002] Fenton oxidation is an advanced oxygen water treatment technology with simple operation process and thorough reaction. It has been widely used in the treatment of polluted water bodies such as chemical industry, pharmaceuticals, printing and dyeing, coking and tanning. However, the traditional homogeneous Fenton oxidation method has some defects. For example, it is greatly affected by the pH of the environment, and the reaction can only be carried out under acidic conditions, resulting in a narrow range of pH values ​​for its application, and the pH value needs to be adjusted repeatedly during the reaction process; 2 o 2 with Fe 2+ fast response, Fe 2+ ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G49/12C02F1/72C02F101/30
CPCC01G49/12C01P2004/32C01P2004/80C02F1/722C02F1/725C02F2101/30C02F2305/026
Inventor 刁增辉徐向荣左林子刘锦军胡咏霞
Owner SOUTH CHINA SEA INST OF OCEANOLOGY - CHINESE ACAD OF SCI
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