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Novel immobilized 8-hydroxyquinoline type chelate adsorption material and preparation method thereof

A hydroxyquinoline-type, chelating adsorption technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of small adsorption capacity and low bonding amount of 8-hydroxyquinoline, and achieve a simple and high-quality preparation process. Coordination and complexation ability, the effect of easy preparation process

Inactive Publication Date: 2014-12-03
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Purpose of the present invention: In order to solve the existing chelating adsorption materials, the bonding amount of 8-hydroxyquinoline on the substrate surface is low, and the adsorption capacity is small, providing a stable performance, good rigidity, and a variety of heavy metal adsorption , a new type of immobilized 8-hydroxyquinoline chelate adsorption material with large adsorption capacity and easy regeneration and elution and its preparation method. The chelate adsorption material can be efficiently applied to remove metal ion pollution and trace metal enrichment in water set analysis

Method used

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  • Novel immobilized 8-hydroxyquinoline type chelate adsorption material and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Example 1: In a four-necked flask, add 1.0 g of amino-containing silane coupling agent-modified silica gel particles, 5 mL of hydroxyethyl methacrylate and 100 mL of DMF and H 2 Mixed solvent of O (V:V=1:1), blow nitrogen for 30min, heat up to 30°C, add 0.0537g of ammonium persulfate aqueous solution to the reaction system, react at constant temperature for 12h, filter with suction, and extract the filter cake with methanol Dry at 70°C for 24 hours to obtain silica gel particles PHEMA / SiO grafted with polyhydroxyethyl methacrylate 2 . The graft rate of poly(hydroxyethyl methacrylate) is 41.3%.

[0020] In the four-neck flask, add 0.5g grafted particle PHEMA / SiO 2 , 1.82g 5-chloromethyl-8-hydroxyquinoline CHQ and 20mL dimethyl sulfoxide, heated to 90°C, and added 1.5gNa 2 CO 3 , N 2 Under the atmosphere, react at constant temperature for 6 hours, filter, wash with water, wash with absolute ethanol, and dry to obtain the functional composite particle HQ-PHEMA / SiO wit...

Embodiment 2

[0021] Example 2: In a four-necked flask, add 1.0 g of amino-containing silane coupling agent-modified silica gel particles, 4.5 mL of hydroxyethyl methacrylate and 100 mL of DMF and H 2 Mixed solvent of O (V:V=1:1), blow nitrogen for 30min, heat up to 25°C, add 0.0483g of ammonium persulfate aqueous solution to the reaction system, react at constant temperature for 14h, filter with suction, and extract the filter cake with methanol Dry at 70°C for 24 hours to obtain silica gel particles PHEMA / SiO grafted with polyhydroxyethyl methacrylate 2 . The graft rate of poly(hydroxyethyl methacrylate) is 35.6%.

[0022] In the four-neck flask, add 0.5g grafted particle PHEMA / SiO 2 , 1.82g 5-chloromethyl-8-hydroxyquinoline CHQ and 20mL nitrobenzene, heated to 80°C, and added 1.4g NaHCO 3 , N 2 Under the atmosphere, react at constant temperature for 7 hours, filter, wash with water, wash with absolute ethanol, and dry to obtain the functional composite particle HQ-PHEMA / SiO with 8-hy...

Embodiment 3

[0023] Example 3: In a four-necked flask, add 1.0 g of amino-containing silane coupling agent-modified silica gel particles, 5.5 mL of hydroxyethyl methacrylate and 90 mL of DMF and H 2Mixed solvent of O (V:V=1:1), blow nitrogen for 30min, heat up to 35°C, add 0.0591g of ammonium persulfate aqueous solution to the reaction system, react at constant temperature for 12h, filter with suction, and extract the filter cake with methanol Dry at 70°C for 24 hours to obtain silica gel particles PHEMA / SiO grafted with polyhydroxyethyl methacrylate 2 . The graft rate of poly(hydroxyethyl methacrylate) is 39.8%.

[0024] In the four-neck flask, add 0.5g grafted particle PHEMA / SiO 2 , 1.82g 5-chloromethyl-8-hydroxyquinoline CHQ and 20mL N,N-dimethylformamide, heated to 100°C, and added 1.5g NaHCO 3 , N 2 Under the atmosphere, react at constant temperature for 5 hours, filter, wash with water, wash with absolute ethanol, and dry to obtain the functional composite particle HQ-PHEMA / SiO w...

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Abstract

The invention belongs to the field of chelate resin materials, and particularly relates to a novel immobilized 8-hydroxyquinoline type chelate adsorption material and a preparation method thereof. 0.95-1.85mmol / g of ligand 8-hydroxyquinoline is bonded to the surface of a silica gel micro-particle modified by hydroxyethyl methacrylate (HEMA). The preparation method includes the steps: grafting the hydroxyethyl methacrylate on the surface of the silica gel micro-particle modified by amino containing silane coupling agents; and fixing the ligand 8-hydroxyquinoline on the surface of the silica gel micro-particle modified by polymer. The material is large in 8-hydroxyquinoline bonding quantity, simple in synthesis process, moderate in condition, short in time, easy to control and fine in mechanical property, is repeatedly used, has a high coordinated complexing capacity for metal ions, can enrich and recycle various precious metal ions, particularly has excellent adsorption and selection performances for heavy metals such as copper, nickel and lead, and can be used for purifying industrial wastewater.

Description

technical field [0001] The invention belongs to the technical field of chelating adsorption materials, and in particular relates to a novel immobilized 8-hydroxyquinoline type chelating adsorption material and a preparation method thereof. Background technique [0002] Chelating adsorption materials (including chelating resins) are solid (particle) materials that have chelating functional groups for metal ions bonded to the surface of a solid substrate. There are many types of chelating functional groups, such as 8-hydroxyquinoline type, iminoacetic acid type, Schiff base type, salicylic acid type, and amidoxime type. Among these types of chelating groups, 8-hydroxyquinoline is a strong chelating ligand, and Goswami A and Wang Z et al. found that it interacts with Fe 3+ Ions and Ga 3+ The coordination constants of the ions are as high as 10 38 with 10 49 [Goswami A, Singh A K, Venkataramani B. Talanta, 2003, 60: 1141; Wang Z, J Miao, F S C Lee, Wang X R. Chinese Journa...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26
Inventor 高保娇李延斌王蕊欣房晓琳喻龙
Owner ZHONGBEI UNIV
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