Preparation method of silica gel-bonded polyamidoamine (PAMAM) dendrimer adsorbent

A dendrimer-loaded polyamide technology, which is applied in chemical instruments and methods, adsorption water/sewage treatment, water/sludge/sewage treatment, etc. Problems such as low metal ion adsorption and steric hindrance can reduce reaction cost, improve porosity and increase crosslinking degree

Inactive Publication Date: 2014-11-05
LUDONG UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is an important problem in the synthesis process: cross-linking occurs between the amino group and the imino molecule and within the molecule. The cross-linking problem not only reduces the functional groups immobilized on the surface of the silica gel, but also seriously affects the chelation between the functional groups of the dendrim

Method used

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  • Preparation method of silica gel-bonded polyamidoamine (PAMAM) dendrimer adsorbent
  • Preparation method of silica gel-bonded polyamidoamine (PAMAM) dendrimer adsorbent
  • Preparation method of silica gel-bonded polyamidoamine (PAMAM) dendrimer adsorbent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Dissolve 38 mL of redistilled methyl acrylate in 40 mL of methanol, and 35 mL of 3-aminopropyltriethoxysilane in 40 mL of methanol. Among them, the molar ratio of ester group to amine group is 5:2. At 0°C, under the protection of nitrogen, with magnetic stirring, slowly drop the methanol solution of aminopropyltrimethoxysilane into the methanol solution of methyl acrylate for about 2 hours After the dropwise addition was completed. Subsequently, at 0° C., the reaction was stirred for 0.5 hours, and then stirred and reacted at room temperature for 24 hours under nitrogen protection. After the reaction, the mixture was evaporated with a rotary evaporator at 40° C. to remove the solvent and excess methyl acrylate, and the final product was a G0.5PAMAM dendrimer. Dissolve 115mL of ethylenediamine in 120mL of methanol, and 25g of G0.5PAMAM dendrimer in 30mL of methanol. The molar ratio of amine groups to ester groups is about 25:1. 0°C, under nitrogen protection, magnet...

Embodiment 2

[0028] (1) Same as step (1) in Example 1 to obtain a G1.0 PAMAM dendrimer.

[0029] (2) Put 0.3620g of cetyltrimethylammonium bromide and 0.05g of sodium hydroxide into a three-necked bottle filled with 20ml of warm water, stir until it becomes clear, and then add G1.0 PAMAM dendrimers Bulk and tetraethoxysilane were added to the above clear liquid in a molar ratio of 1:6. At room temperature (25° C.), the stirring was continued, and the stirring reaction was continued for 24 hours after a white gel was formed. Subsequently, the above-mentioned white precipitated gel was transferred to a polypropylene bottle, heated at 70°C for 2h, then aged at 85°C for 4 days, filtered with suction, washed with water (washed with water until there was only a small amount of foam), and dried at room temperature. The obtained sample was transferred to a Soxhlet extractor, using absolute ethanol (210 mL) and hydrochloric acid (10 ml, 37 wt %) as solvents, and extracted under reflux for 72 h. T...

Embodiment 3

[0031] (1) Same as step (1) in Example 1 to obtain G2.0 PAMAM dendrimers.

[0032] (2) At 25°C, mix the G2.0 PAMAM-type dendrimer monomer and tetraethoxysilane at a molar ratio of 1:10, stir mechanically for 2 hours, then add 7ml of water, and dropwise add 4.5ml of NH 4 Solution F (0.014g / mL), continue to react for 24h after forming a white gel. After the reaction, the sample was aged at 40° C. for 48 h, filtered with suction, and dried at room temperature. Transfer the dried sample to a Soxhlet extractor and extract it with absolute ethanol for 48 hours, and dry the sample in a vacuum oven at 60°C for 48 hours, and the obtained product is marked as G2.0-TEOS-1 / 10.

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Abstract

The invention relates to a preparation method of a silica gel-bonded polyamidoamine (PAMAM) dendrimer adsorbent. The preparation method comprises the following steps that 1, an amino functional group-containing silane coupling agent as a central nucleus and methyl acrylate undergo a Michael addition reaction to produce a semi-generation product G0.5 containing ester groups as terminal groups, the semi-generation product G0.5 and ethanediamine undergo an amidation reaction to produce a whole-generation product G1.0 containing amino groups as terminal group, and the Michael addition reaction and the amidation reaction are repeated to produce G0.5-G4.0 PAMAM dendrimers, and 2, the G0.5-G4.0 PAMAM dendrimers and a silica gel precursor tetraethoxysilane are mixed according to a mole ratio of 1: 1 to 1: 16 and undergo a synthesis reaction by a sol-gel method, and the reaction system respectively undergoes hydrolysis copolycondensation reactions in the presence of a pore forming agent and in the absence of the pore forming agent so that the silica gel-bonded PAMAM dendrimer adsorbent are obtained. The silica gel-bonded PAMAM dendrimer adsorbent has a large metal ion adsorption capacity, can be used for treatment on heavy metal ion wastewater and has a unique advantage in practical application.

Description

technical field [0001] The invention relates to a preparation method of a polyamide-amine (PAMAM) dendrimer adsorbent supported by a silica gel bond, and belongs to the field of polymer material synthesis. Background technique [0002] The heavy metal ions dissolved in industrial wastewater have great harm to organic life even at low concentrations. Therefore, the recovery and elimination of heavy metal ions has become a topic of concern. Various conventional separation methods, such as ion exchange, chemical precipitation, solvent extraction and adsorption, are applied in this field. Among them, chelation adsorption materials are a kind of adsorption functional materials that can form multi-coordination compounds with metal ions. , has a wide range of applications. Inexpensive silica gel has excellent thermodynamic and mechanical properties, stable chemical properties, large surface area, wide pore size range, good adsorption effect, etc., and there are a lot of silanol on...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J20/26B01J20/30C02F1/28C02F1/62
Inventor 曲荣君孙晓梅张盈孙昌梅纪春暖陈厚殷平
Owner LUDONG UNIVERSITY
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