Method for preparing silica gel supported dithiocarbamate heavy metal chelating resin

A technology of dithioamino and chelating resins, which is applied in chemical instruments and methods, and other chemical processes, can solve the problems of low adsorption capacity of chelating resins and low number of dithiocarbamate functional groups, and achieve improved Large adsorption capacity, large adsorption capacity, and good mechanical strength

Inactive Publication Date: 2011-05-18
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the amino compounds reacted with carbon disulfide reported in the literature are polyamines with small molecular weight, such as ethylenediamine, diethylenetriamine, triethylenetetramine, etc. High, resulting in low adsorption of chelating resins (M.E.Mahmoud, Selective solid phase extraction ofmercury(II) by silica gel-immobilized-dithiocarbamate derivatives, Anal.Chim.Acta.1999,398:297-304; S.G.Renaudin, R.Schneiderb , A.Walcarius, Synthesis of newdithiocarbamate-based organosilanes for grafting on silica, Tetrahedron Lett.2007, 48: 2113-2116)

Method used

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  • Method for preparing silica gel supported dithiocarbamate heavy metal chelating resin
  • Method for preparing silica gel supported dithiocarbamate heavy metal chelating resin
  • Method for preparing silica gel supported dithiocarbamate heavy metal chelating resin

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Embodiment 1 adopts different inert organic solvents to prepare silica gel-loaded dithiocarbamate chelating resin

[0021] (1) Take 30g of chromatographic silica gel in a 500ml three-necked bottle, add 1mol / L HNO 3 The solution was 200ml, mechanically stirred at 50°C for 6h, and after the reaction, the solid product was obtained by suction filtration, which was washed with deionized water and methanol until neutral, and dried at room temperature for 12h to obtain activated silica gel.

[0022] (2) Take 20g of the activated silica gel obtained in step (1), 150ml of cyclohexane, heptane, toluene or xylene and add it to a 500ml three-necked flask, stir mechanically, and heat the reaction system in an oil bath to 80-140°C; 80ml Mix cyclohexane, heptane, toluene or xylene with 20ml of γ-chloropropyltriethylsilane evenly and drop them into the three-neck bottle drop by drop. During the whole reaction process, keep the system temperature at 80-140°C and reflux under nitrogen a...

Embodiment 2

[0027] Embodiment 2 adopts different polyamine compounds to prepare silica gel-loaded dithiocarbamate chelating resin

[0028] (1) Take 30g of chromatographic silica gel in a 500ml three-necked bottle, add 1mol / L HNO 3 The solution was 200ml, mechanically stirred at 50°C for 6h, and after the reaction, the solid product was obtained by suction filtration, which was washed with deionized water and methanol until neutral, and dried at room temperature for 12h to obtain activated silica gel.

[0029] (2) Take 20g of the activated silica gel obtained in step (1) and 150ml of toluene into a 500ml three-necked flask, mechanically stir, and heat in an oil bath to raise the temperature of the reaction system to 110°C; mix 80ml of toluene with 20ml of γ-chloropropyltriethylsilane After uniformity, it was dropped into a three-necked bottle drop by drop. During the whole reaction process, the temperature of the system was kept at 110° C., and the nitrogen atmosphere was refluxed for 48 h...

Embodiment 3

[0034] Example 3 Controlling the different pH values ​​of the reaction system to prepare silica gel-loaded dithiocarbamate chelating resins

[0035] (1) Take 30g of chromatographic silica gel in a 500ml three-necked bottle, add 1mol / L HNO 3 The solution was 200ml, mechanically stirred at 50°C for 6h, and after the reaction, the solid product was obtained by suction filtration, which was washed with deionized water and methanol until neutral, and dried at room temperature for 12h to obtain activated silica gel.

[0036] (2) Take 20g of the activated silica gel obtained in step (1) and 150ml of toluene into a 500ml three-necked flask, mechanically stir, and heat in an oil bath to raise the temperature of the reaction system to 110°C; mix 80ml of toluene with 20ml of γ-chloropropyltriethylsilane After uniformity, it was dropped into a three-necked bottle drop by drop. During the whole reaction process, the temperature of the system was kept at 110° C., and the nitrogen atmosphere...

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Abstract

The invention relates to a method for preparing heavy metal chelating resin, in particular to a method for preparing silica gel supported dithiocarbamate heavy metal chelating resin and adsorption of heavy metals such as lead, cadmium, copper, mercury and the like by the resin. The method comprises the following steps of: reacting carbon disulfide with a polyamine compound to generate a dithiocarbamate compound; and grafting the dithiocarbamate compound onto the surface of silicon dioxide, wherein a halogen group is modified on the surface of the silicon dioxide. By the method, the adsorption capacity of dithiocarbamate chelating resin is effectively improved; and the problem that silica gel is dissolved due to too high alkalinity of a reaction system (pH value is more than 11), or the dithiocarbamate compound cannot be generated through reaction due to too low alkalinity (the pH value is less than 10) when a dithiocarbamate functional group is prepared by reacting the silica gel with the carbon disulfide in the conventional synthetic route is solved, wherein an amino group is modified on the surface of the silica gel.

Description

technical field [0001] The invention relates to a preparation method of a heavy metal chelating resin, in particular to a preparation method of a silica gel-loaded dithiocarbamate heavy metal chelating resin and its adsorption to heavy metals such as lead, cadmium, copper and mercury. Background technique [0002] Due to their high toxicity, heavy metals are not easy to be metabolized in the environment, and are easy to be enriched by organisms and have a biomagnification effect, which not only seriously pollutes water bodies, but also seriously threatens the survival of humans and animals. For water bodies polluted by heavy metals, the treatment technologies that can be used include chemical precipitation, reverse osmosis, electrolytic extraction, ion exchange and adsorption methods, etc. Among these methods, the adsorption method has attracted extensive attention because of its high working efficiency, easy operation, and no pollution to the environment. As a kind of adso...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/392B01J20/26B01J20/30
Inventor 胡慧萍白蓝付翁程喜梁诸葛雷熊蕾陈启元
Owner CENT SOUTH UNIV
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