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Preparation method of hollow nanometer hydrous zirconium oxide loaded millimeter-level polymer sphere

A hydrated zirconia, hollow nanotechnology, applied in chemical instruments and methods, water pollutants, other chemical processes, etc., can solve the problems that limit the large-scale practical application of nano-adsorbents, are difficult to separate and recycle, and are unfavorable for adsorption beds. application and other problems, to overcome the difficulty of recycling and reuse, easy industrial expansion of production, and fast adsorption rate

Inactive Publication Date: 2017-12-26
NANJING UNIV OF SCI & TECH
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] However, nano-adsorbents are difficult to separate and recycle from the solution due to their nano-scale properties and sizes, and may cause secondary pollution to the environment, which limits the large-scale practical application of nano-adsorbents.
The zirconia nanospheres synthesized in Document 1 have the disadvantage of being easily lost without immobilization, which is not conducive to the application of the actual adsorption bed (Su Y, et al.Strong adsorption of phosphate by amorphous zirconium oxidenanoparticles[J].Water research,2013 ,47(14):5018-5026.)
Document 2 synthesized hollow nanometer hydrated zirconia balls, which were also loaded with Fe3O4 for recycling, but in practical applications, there are still problems of loss and secondary pollution (Pan S, et al.Nanosized yolk–shell Fe 3 O 4@Zr(OH)x spheres efficient removal of Pb(II)from aqueous solution[J].Journal of hazardous materials,2016,309:1-9.)

Method used

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  • Preparation method of hollow nanometer hydrous zirconium oxide loaded millimeter-level polymer sphere
  • Preparation method of hollow nanometer hydrous zirconium oxide loaded millimeter-level polymer sphere
  • Preparation method of hollow nanometer hydrous zirconium oxide loaded millimeter-level polymer sphere

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Embodiment 1

[0039] In step 1, add 130 mL of absolute ethanol to 20 mL of H 2 O and 50 mL of ammonia water were stirred at 30° C. to obtain mixed solution 1. 10 mL of TEOS was added to 190 mL of anhydrous ethanol, and after stirring uniformly, it was added to mixed solution 1. After rapid stirring for 1 minute, the stirring was continued at 30° C. for 20 hours. After the reaction, centrifuge and dry to obtain nano-silica balls.

[0040] In step 2, the silica and 0.83 mL of H 2O and 0.83 g of Brij35 were added to 333 mL of absolute ethanol, sonicated for 2 hours and then stirred for 30 minutes to obtain mixed solution 2. Take 5mL of n-butoxide zirconium solution and add it to 25mL of absolute ethanol, after stirring evenly, suck it up with a syringe, adjust the speed of the syringe pump to 0.3mL / min, drop it into mixed solution 2, and continue to stir at 30°C for 8 hours. After the reaction, centrifuge, age in deionized water for 24 hours, centrifuge again, and reflux for 3 to 4 days. T...

Embodiment 2

[0045] In step 1, add 130 mL of absolute ethanol to 20 mL of H 2 O and 50 mL of ammonia water were stirred at 30° C. to obtain mixed solution 1. 10 mL of TEOS was added to 190 mL of anhydrous ethanol, and after stirring uniformly, it was added to mixed solution 1. After rapid stirring for 1 minute, the stirring was continued at 30° C. for 20 hours. After the reaction, centrifuge and dry to obtain nano-silica balls.

[0046] In step 2, the silica and 0.83 mL of H 2 O and 0.83 g of Brij35 were added to 333 mL of absolute ethanol, sonicated for 2 hours and then stirred for 30 minutes to obtain mixed solution 2. Take 5mL of n-butoxide zirconium solution and add it to 25mL of absolute ethanol, after stirring evenly, suck it up with a syringe, adjust the speed of the syringe pump to 0.3mL / min, drop it into mixed solution 2, and continue to stir at 30°C for 8 hours. After the reaction, centrifuge, age in deionized water for 24 hours, centrifuge again, and reflux for 3 to 4 days. ...

Embodiment 3

[0049] In step 1, add 130 mL of absolute ethanol to 20 mL of H 2 O and 50 mL of ammonia water were stirred at 30° C. to obtain mixed solution 1. 10 mL of TEOS was added to 190 mL of anhydrous ethanol, and after stirring uniformly, it was added to mixed solution 1. After rapid stirring for 1 minute, the stirring was continued at 30° C. for 20 hours. After the reaction, centrifuge and dry to obtain nano-silica balls.

[0050] In step 2, the silica and 0.83 mL of H 2 O and 0.83 g of Brij35 were added to 333 mL of absolute ethanol, sonicated for 2 hours and then stirred for 30 minutes to obtain mixed solution 2. Take 5mL of n-butoxide zirconium solution and add it to 25mL of absolute ethanol. After stirring evenly, suck it up with a syringe, adjust the speed of the syringe pump to 0.25mL / min, drop it into mixed solution 2, and continue stirring at 30°C for 8 hours. After the reaction, centrifuge, age in deionized water for 24 hours, centrifuge again, and reflux for 3 to 4 days....

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Abstract

The invention discloses a preparation method of a hollow nanometer hydrous zirconium oxide loaded millimeter-level polymer sphere. According to the method, a non-solvent induced phase separation method in the field of membrane separation is used for preparing the hollow nanometer hydrous zirconium oxide loaded millimeter-level polymer sphere; concretely, the hollow nanometer hydrous zirconium oxide sphere is prepared by using a nanometer silicon dioxide sphere as a template; a millimeter-level polymer sphere with the very-narrow particle size distribution is obtained through an injection pump extrusion process; few pore-foaming agents are added, so that the developed pore structure is formed; good sphericity degree and strength are maintained. The loaded hollow nanometer hydrous zirconium oxide prepared by the method has great adsorption capacity and little adsorption capacity loss, can be easily recovered and repeatedly utilized, and is also applicable to relatively harsh application environment; the adsorbent loss is relatively low under the extremely low pH condition; wide application prospects are realized in the field of heavy metal water pollution treatment.

Description

technical field [0001] The invention belongs to the technical field of heavy metal water pollution control, and in particular relates to a preparation method of a hollow nanometer hydrated zirconia millimeter-sized polymer ball. Background technique [0002] Heavy metal pollution has become one of the most harmful water pollution problems in recent years because of its strong toxicity, persistence and enrichment. At present, the commonly used methods for removing heavy metals in wastewater include chemical precipitation, ion exchange, ion flotation, electrolysis, electrodialysis, reverse osmosis, ferrite and adsorption. Adsorption is considered to be one of the most economically feasible, environmentally friendly and efficient technologies. Therefore, the development and research of high-performance adsorbents that are easy to store, low-cost, effective and reusable are a hot research topic at home and abroad. [0003] Nanomaterials, as emerging adsorbents for water treatm...

Claims

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Application Information

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IPC IPC(8): B01J20/02B01J20/30C02F1/28C02F101/20
Inventor 李健生魏国平齐俊文李阳沈家明刘郁歆王连军孙秀云沈锦优韩卫清
Owner NANJING UNIV OF SCI & TECH
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