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Preparation method of magnetic nano solid-phase extracting agent for Pb<2+> separation

A solid-phase extractant, magnetic nanotechnology, applied in chemical instruments and methods, ion exchange, ion exchange regeneration, etc., can solve the problems of unstable nano-extractant, inability to completely remove, high processing cost, and achieve good stability and Acid and alkali resistance, improving atom utilization, and the effect of large chemical adsorption capacity

Inactive Publication Date: 2014-03-05
UNIV OF SHANGHAI FOR SCI & TECH
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  • Application Information

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Problems solved by technology

Among them, the treatment cost of ion exchange method and membrane separation method is relatively high, and it is easy to cause secondary pollution; most of the chemical precipitation method and adsorption method can only transfer the position where heavy metal ions exist or transfer their physical and chemical forms, but cannot completely remove them. Heavy metal ions, and the adsorption is a variety of heavy metal ions, after elution is still a mixed solution, for specific heavy metal ions (especially Pb 2+ ) recovery and reuse is still relatively difficult; when the normal temperature ferrite method is used to treat heavy metal ion wastewater, the type of heavy metal ion in the wastewater has a greater impact on the properties of the magnetic product, and the closer the radius of the heavy metal ion is to the iron ion, the metal in the obtained magnetic product The higher the recovery rate, the stability of the magnetic product and its saturation magnetic susceptibility, the higher the adsorption and removal of other heavy metal ions; the method of magnetic separation method docking magnetic species, the selection of magnetic species and the recovery of magnetic species are still to be studied. Improvement; Nanoparticles can have adsorption capacity for many kinds of ions at the same time, but most of them are non-magnetic nanoparticles, which undoubtedly increases the difficulty of recovery of heavy metal ions, and most of them use hydrogen bonding or direct coating, so that Nano-extractants are unstable, poor acid and alkali resistance, small adsorption capacity, and poor reusability; although magnetic nanoparticles have been reported for the adsorption of heavy metal ions, these adsorbents are mostly non-specific, with poor selectivity and small adsorption capacity , which is not conducive to specific heavy metal ions (especially Pb 2+ ), and the recovery and activation of magnetic nano solid phase extraction agent is still in the immature stage

Method used

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  • Preparation method of magnetic nano solid-phase extracting agent for Pb&lt;2+&gt; separation
  • Preparation method of magnetic nano solid-phase extracting agent for Pb&lt;2+&gt; separation
  • Preparation method of magnetic nano solid-phase extracting agent for Pb&lt;2+&gt; separation

Examples

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Effect test

example 1

[0030] with 1gFe 3 o 4 Nanoparticles are used as precursors, deionized water and ethanol are used as solvents, and the volume ratio of ethanol and deionized water is 4:1. After mixing evenly, heat in a constant temperature stirring water bath in a reaction vessel, and add 25% volume fraction of NH at 30°C. 3 h 2 O, accounting for 5% of the total volume, after heating at a constant temperature of 45°C for 30 minutes, add A---tetraethyl silicate dropwise, accounting for 1% of the total volume, and add B---γ-chloropropane after 1 hour of reaction Triethoxysilane, accounting for 1% of the total fraction, heated to 60°C and refluxed for 1 hour, cooled, washed, dried, and then added to the chloroform solvent again, and then added 0.1g C---dithizone, 40 Stir at constant temperature for 12-24 hours; after washing and drying, it can be used for Pb 2+ Separation of magnetic nano solid phase extraction agent. The relationship between the adsorption time of the product and the content...

example 2

[0032] with 1gFe 3 o 4 Nanoparticles are used as precursors, deionized water and ethanol are used as solvents, and the volume ratio of ethanol and deionized water is 4:1. After mixing evenly, heat in a constant temperature stirring water bath in a reaction vessel, and add 25% volume fraction of NH at 30°C. 3 h 2 O, accounting for 5% of the total volume, after heating at a constant temperature of 45°C for 30 minutes, add A---tetrabutyl silicate dropwise, accounting for 1% of the total volume, and add B---γ-chloropropane after 1 hour of reaction Triethoxysilane, accounting for 2% of the total fraction, heated to 60°C and refluxed for 1 hour, cooled and washed, then added to chloroform solvent again, added 0.2g C---dithizone, stirred at 40°C 12-24 hours; after washing and drying, it can be used for Pb 2+ Separation of magnetic nano solid phase extraction agent. The relationship between the adsorption time of the product and the content of lead ions in the mother liquor is sho...

example 3

[0034] with 1gFe 3 o 4 Nanoparticles are used as precursors, deionized water and ethanol are used as solvents, and the volume ratio of ethanol and deionized water is 4:1. After mixing evenly, heat in a constant temperature stirring water bath in a reaction vessel, and add 25% volume fraction of NH at 30°C. 3 h 2 O, accounting for 5% of the total volume, after heating at a constant temperature of 45°C for 30 minutes, add A---tetrabutyl silicate dropwise, accounting for 1% of the total volume, and add B---γ-chloropropane after 1 hour of reaction Triethoxysilane, accounting for 3% of the total volume, heated to 60°C and refluxed for 1 hour, cooled and washed, then added to chloroform solvent again, added 0.3g C---dithizone, stirred at 40°C 12-24 hours; after washing and drying, it can be used for Pb 2+ Separation of magnetic nano solid phase extraction agent.

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Abstract

The invention relates to a preparation method of a magnetic nano solid-phase extracting agent for Pb2+ separation, which comprises the following steps of: taking Fe3O4 nano particles as a magnetic nucleus, taking the mixed liquid of deionized water and ethanol as a solvent, adding 25 percent of stronger ammonia water accounting for 5 percent of the fraction of the total volume, stirring at constant temperature in a reaction container after mixing evenly, dripping A after heating in a water bath for 30 minutes, adding B after reacting for 1 hour, heating up to 60 DEG C, cooling after refluxing for 1 hour, washing, adding into an ethanol solvent or a chloroform solvent after drying, then adding C and stirring at constant temperature of 40 DEG C for 12 to 24 hours; and washing so as to obtain the magnetic nano solid-phase extracting agent for the Pb2+ separation after drying at low temperature. The modifier A contains ester orthosilicate, the modifier B contains a silica coupling agent with chlorine functionalization, and the modifier C is dithizone. The magnetic nano solid-phase extracting agent prepared by the preparation method of the magnetic nano solid-phase extracting agent for the Pb2+ separation has large adsorption quantity, high rate, a simple process and low cost, is green, is friendly to the environment and is suitable for large-scale industrial production.

Description

technical field [0001] The present invention relates to a kind of for Pb 2+ The preparation method of the separated magnetic nanometer solid phase extractant. It is used to adsorb heavy metal ions from wastewater containing heavy metal ions. Background technique [0002] The technologies for treating heavy metal ion wastewater developed by scientific researchers in many countries include: ① chemical precipitation method; ② redox method; ③ air flotation method; ④ electrolytic reduction method; Evaporation and solidification method; ⑦Ion exchange method; ⑧Solvent extraction method; ⑨Liquid membrane, ultrafiltration membrane, reverse osmosis, electrodialysisMagnetic separation method, ferrite method, nano solid extractant method, magnetic nano solid extractant Law. Among them, the treatment cost of ion exchange method and membrane separation method is relatively high, and it is easy to cause secondary pollution; most of the chemical precipitation method and adsorption meth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30B01D15/08C02F1/28C02F1/62
Inventor 马杰成国良徐音辰李继龙季婷婷
Owner UNIV OF SHANGHAI FOR SCI & TECH