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Magnetic micro-sphere, method for preparing same and application of magnetic micro-sphere to treating antibiotic wastewater

A technology of antibiotic wastewater and magnetic microspheres, which is applied in water/sewage treatment, natural water treatment, chemical instruments and methods, etc., can solve the problems of harsh preparation conditions, high comprehensive cost, and difficulty in mass production, and achieve good reuse effects , good durability, simple operation effect

Inactive Publication Date: 2017-03-08
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Using various cheap materials or waste to prepare activated carbon adsorbents, such as wood chips, straw, fungal residue, excess sludge, etc., can reduce the cost of one-time use, but the disadvantage is that it cannot be reused, and the long-term calculation investment is relatively high
[0006] The preparation of porous nanomaterials, such as graphene, mesoporous silicon, carbon nanotubes, etc., can greatly improve the efficiency of adsorbing antibiotics, thereby prolonging the use time of adsorbents and reducing operating costs. The disadvantage is that the preparation conditions are harsh and mass production is difficult. In addition, Nor does it overcome the difficulty of adsorbent regeneration
[0007] Synthetic polymer porous microsphere materials, such as polyaniline, chitosan, polystyrene and other substances, can improve the adsorption performance, but the comprehensive cost caused by one-time use is still high
[0008] Synthetic iron-based magnetic adsorption materials, such as polystyrene magnetic microspheres, chitosan magnetic materials, etc., can use a magnetic field to separate and recover antibiotics after adsorption saturation, but there are still shortcomings in the regeneration performance of the adsorbent

Method used

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  • Magnetic micro-sphere, method for preparing same and application of magnetic micro-sphere to treating antibiotic wastewater
  • Magnetic micro-sphere, method for preparing same and application of magnetic micro-sphere to treating antibiotic wastewater
  • Magnetic micro-sphere, method for preparing same and application of magnetic micro-sphere to treating antibiotic wastewater

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preparation example Construction

[0038] The invention provides a kind of preparation method of magnetic microsphere, comprises the following steps:

[0039] (1) Adopt ethylenediamine and chloroacetic acid to modify chloromethyl polystyrene microspheres to obtain modified polystyrene microspheres;

[0040] Mixing ferric ammonium oxalate, surfactant, ion buffer and alcoholic organic solvent to obtain ferric ammonium oxalate solution;

[0041] (2) the modified polystyrene microspheres obtained by the step (1) are mixed with ferric ammonium oxalate solution, and pre-reaction is carried out under the condition of cutting off oxygen;

[0042] (3) performing a solvothermal reaction on the pre-reaction product obtained in the step (2) to obtain magnetic microspheres.

[0043] The invention adopts ethylenediamine and chloroacetic acid to modify the chloromethyl polystyrene microspheres to obtain the modified polystyrene microspheres. The invention adopts ethylenediamine and chloroacetic acid to modify the chlorometh...

Embodiment 1

[0086] (1) 2 g of commercially available chloromethyl polystyrene microspheres (PSC, CAS NO 55844-94-5, with a particle size of about 1 mm and a density of about 1.05 g / cm 3 ) in 20mL 1,4-dioxane for 2h, and then mixed with alkaline solution (2.5g sodium hydroxide, 0.1g phase transfer catalyst tetrabutylammonium bromide and 20mL water) and 25mL ethylene dioxane Mix the amines, heat in a water bath at 80-85°C, stir and react at 60rpm for 6h, filter the material obtained after the reaction, wash with water and methanol, and vacuum-dry for 4 days at a vacuum degree of 0.1MPa and 25°C , to obtain the precursor of modified polystyrene microspheres; 2.52g chloroacetic acid was neutralized with saturated sodium carbonate solution, and then mixed with alkaline solution (2.5g sodium hydroxide, 0.1g phase transfer catalyst tetrabutylammonium bromide and 20mL mixed solution of water) mixed with the obtained modified polystyrene microsphere precursor, heated in a water bath at 80-85° C., ...

Embodiment 2

[0093] With 100mg / L tetracycline aqueous solution as the antibiotic wastewater to be treated, the adsorption performance of the magnetic microspheres provided by the invention is verified, comprising the following steps:

[0094] The pH value of the tetracycline aqueous solution was adjusted to 6.5, based on the volume of the tetracycline aqueous solution, 2 g / L of the magnetic microspheres prepared in Example 1 were added, and the adsorption reaction was carried out at normal temperature and pressure, and the stirring rate was 60 rpm for 12 hours.

[0095] Sampling and analysis in the adsorption process, the results are as follows Figure 5 shown. Depend on Figure 5 From the curve shown in , it can be seen that the magnetic microspheres of the present invention have a certain adsorption performance for tetracycline, and 30% of tetracycline can be adsorbed within 2 hours.

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Abstract

The invention provides a method for preparing a magnetic micro-sphere. The method includes modifying a chloromethyl polystyrene micro-sphere by the aid of ethylenediamine and chloroacetate to obtain a modified polystyrene micro-sphere; mixing ammonium ferrie oxalate, surfactants, ion buffering agents and alcohol organic solvents with one another to obtain ammonium ferrie oxalate solution; mixing the modified polystyrene micro-sphere and the ammonium ferrie oxalate solution with each other to obtain a mixture and carrying out pre-reaction on the mixture under an oxygen isolation condition; carrying out solvothermal reaction on a pre-reaction product to obtain the magnetic micro-sphere. The method for preparing the magnetic micro-sphere has the advantages that the method is easy to implement and low in cost, antibiotic wastewater can be effectively treated by the magnetic micro-sphere prepared by the aid of the method, and the magnetic micro-sphere can be recycled; 90% of tetracycline can be adsorbed and degraded in 2 h under the condition that 2 g of magnetic micro-sphere and an appropriate quantity of hydrogen peroxide are added into each liter of to-be-treated antibiotic wastewater which is 100 mg / L tetracycline aqueous solution.

Description

technical field [0001] The invention relates to the technical field of environmental functional materials, in particular to a magnetic microsphere and its preparation method and application. Background technique [0002] my country is a big country in the production and consumption of antibiotics. In 2013, the output of antibiotics in my country was about 120,000 tons, and the export was 30,000 tons, accounting for 70% of the international market. The production and use of antibiotics, on the one hand, ensured the health and safety of the people, and at the same time brought more environmental problems. In the production process, a large amount of antibiotic raw materials and finished waste water are difficult to effectively treat, posing a threat to the water environment; in the process of use, residual human or veterinary antibiotics enter the environment, which can easily induce bacterial resistance and produce broad-spectrum resistance. Therefore, the treatment of antib...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30B01J31/26B01J35/08C02F1/28C02F1/72
CPCB01J20/06C02F1/28C02F1/722C02F1/725B01J20/265B01J20/28009B01J20/28021B01J31/26C02F1/285C02F1/281C02F2101/30C02F2103/343B01J2220/4812B01J2220/46B01J35/33B01J35/51
Inventor 邱勇李冰马俊俊
Owner TSINGHUA UNIV
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