Preparation method of sulfydryl modified magnetic nano material for adsorbing mercury

A technology of mercapto modification and magnetic nanotechnology, which is applied in the field of preparation of magnetic ferric oxide nanomaterials, can solve problems such as poor selectivity and matrix interference, and achieve the effects of large adsorption capacity, good selectivity, and saving processing time and cost

Inactive Publication Date: 2019-11-22
合肥海关技术中心 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the shortcomings of poor selectivity and serious matrix interference in traditional mercury and organic mercury pretreatment, realize high selective adsorption and separation of inorganic mercury and methylmercury, so as to improve the sensitivity and accuracy of inorganic mercury and methylmercury detection methods ; The invention provides a method for preparing magnetic nanomaterials modified by sulfhydryl groups for adsorbing mercury

Method used

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  • Preparation method of sulfydryl modified magnetic nano material for adsorbing mercury

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] A kind of preparation operation steps of the mercapto-modified magnetic nanomaterials for adsorbing mercury are as follows:

[0020] (1) Synthesis of olefin-modified magnetic ferric iron tetroxide (Fe 3 o 4 )Nanoparticles:

[0021] 1g of magnetic ferric oxide (Fe 3 o 4 ) nanoparticles were dispersed in 100mL isopropanol and 8mL water, ultrasonically dispersed for 15min, and stirred at room temperature under nitrogen gas. Then add 10 mL of ammonia water (26% w / w), stir for 5 min, add 8 mL of allyltrimethoxysilane, heat to 45°C and stir for 12 h; the product is obtained by magnetic separation, washed three times with deionized water and once with ethanol, 60 ℃ and dried under vacuum for 12 hours to obtain olefin-modified magnetic ferric iron tetroxide (Fe 3 o 4 )Nanoparticles.

[0022] (2) Synthesis of sulfhydryl-modified ferric iron tetroxide Fe 3 o 4 @SiO 2 @SH nanoparticles:

[0023] 1g of olefin-modified magnetic ferric iron tetroxide (Fe 3 o 4 ) nanopart...

Embodiment 2

[0025] A kind of preparation operation steps of the mercapto-modified magnetic nanomaterials for adsorbing mercury are as follows:

[0026] (1) Synthesis of olefin-modified Fe 3 o 4 Nanoparticles:

[0027] 1g of magnetic iron tetroxide (Fe 3 o 4 ) nanoparticles were dispersed in 100mL isopropanol and 8mL water, ultrasonically dispersed for 15min, and stirred at room temperature under nitrogen gas. Then add 10 mL of ammonia water (26% w / w), stir for 5 min, add 8 mL of allyltrimethoxysilane, heat to 45°C and stir for 12 h. The product was obtained by magnetic separation, washed three times with deionized water, washed once with ethanol, and dried under vacuum at 60°C for 12 hours to obtain olefin-modified Fe 3 o 4 Nanoparticles.

[0028] (2) Synthesis of sulfhydryl-modified ferric iron tetroxide Fe 3 o 4 @SiO 2 @SH nanoparticles:

[0029] 1 g of olefin-modified Fe 3 o 4 Nanoparticles were dissolved in 100mL of toluene, nitrogen was blown, and stirred at room tempera...

Embodiment 3

[0031] A kind of preparation operation steps of the mercapto-modified magnetic nanomaterials for adsorbing mercury are as follows:

[0032] (1) Synthesis of olefin-modified Fe 3 o 4 Nanoparticles:

[0033] 1g of magnetic iron tetroxide (Fe 3 o 4 ) rice particles were dispersed in 100mL of isopropanol and 8mL of water, ultrasonically dispersed for 15min, and stirred at room temperature under nitrogen gas. Add 10 mL of ammonia water (26% w / w), stir for 5 min, add 8 mL of allyltrimethoxysilane, heat to 45°C and stir for 12 h. The product was obtained by magnetic separation, washed three times with deionized water, washed once with ethanol, and dried under vacuum at 60°C for 12 hours to obtain olefin-modified Fe 3 o 4 Nanoparticles.

[0034] (2) Synthesis of sulfhydryl-modified ferric iron tetroxide Fe 3 o 4 @SiO 2 @SH nanoparticles:

[0035] 1 g of olefin-modified Fe 3 o 4 Nanoparticles were dissolved in 100mL of toluene, nitrogen was blown, and stirred at room tempera...

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Abstract

The invention discloses a preparation method of a sulfydryl modified magnetic ferroferric oxide material. The preparation method comprises the following specific operation steps: modifying magnetic ferroferric oxide with trimethoxyvinylsilane to prepare olefin-modified magnetic ferroferric oxide, and then performing a reaction with ethanedithiol under the catalysis of azodiisobutyronitrile to synthesize sulfydryl-modified magnetic ferroferric oxide Fe3O4@SiO2@SH. According to the material, Fe3O4 is modified by the sulfydryl, so that the adsorption capacity on inorganic mercury and organic mercury is large, and the selectivity is good; by using the magnetic Fe3O4, the operation steps of column packing, centrifugation and filtration and the like in the purification process are simplified, and the treatment time and cost are saved.

Description

technical field [0001] The invention belongs to the field of enrichment, purification and detection of heavy metal mercury in food and environmental samples, and in particular relates to a preparation method of a sulfhydryl-modified magnetic ferric iron tetroxide nanometer material. Background technique [0002] In the natural environment, the main forms of mercury are elemental, organic mercury compounds mainly composed of short-chain alkylmercury and divalent inorganic mercury compounds, all of which are potentially harmful to the human body. Among mercury compounds, organic mercury is highly toxic, and methylmercury is the most toxic. It has high lipophilicity, is easily absorbed by organisms, accumulates in the body, and amplifies with the food chain, and the enrichment factor can reach 10 6 ~10 7 . Experiments have shown that low-dose mercury intake for a long time will cause harm to the human body, including nervous system damage, motor function and memory decline, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/10B01J20/28B01J20/30G01N1/40
CPCB01J20/103B01J20/28009B01J20/28016B01J20/28057B01J20/3085G01N1/405
Inventor 周典兵陈洪周丁磊韩芳吕亚宁宋伟刘宇欣郑平
Owner 合肥海关技术中心
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