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Preparation method of silica bonding sulfur-containing terminal group PAMAM dendrimer adsorption agent

A dendrimer and adsorbent technology, applied in the field of chemistry, can solve the problem of non-recyclable use, etc., and achieve the effects of large adsorption capacity, mild reaction conditions and simple operation

Inactive Publication Date: 2015-05-27
LUDONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, PAMAM dendrimers and their metal ion complexes are generally soluble in water and different organic solvents, so they cannot be recycled, so they need to be bonded to silica gel, cross-linked polystyrene, chitosan and other carriers

Method used

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  • Preparation method of silica bonding sulfur-containing terminal group PAMAM dendrimer adsorption agent
  • Preparation method of silica bonding sulfur-containing terminal group PAMAM dendrimer adsorption agent
  • Preparation method of silica bonding sulfur-containing terminal group PAMAM dendrimer adsorption agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Under nitrogen protection, SiO was added to the three-necked flask respectively 2 -10 g of G0, 1.1553 g of methyl isothiocyanate, 100 ml of absolute ethanol, and the reaction mixture was mechanically stirred at 50°C for 24 hours. After the reaction was completed, it was cooled to 25°C, the product was filtered out, and the product was transferred to a Soxhlet extractor, extracted with absolute ethanol for 12 hours, and finally vacuum-dried at 50°C and 0.09Mpa for 48 hours to obtain the 0th generation silica gel Bonded Sulfur-Ended PAMAM Dendrimer Adsorbent SiO 2 -G0-MITC, the structure is shown below.

[0033]

[0034] figure 1 for SiO 2 - Infrared spectrum of G0-MITC, by figure 1 It can be seen at 1381cm -1 The characteristic absorption peak of C=S bond appears at , which proves that the 0th generation silica gel bond-loaded PAMAM dendrimers with sulfur end groups were successfully synthesized, but due to the 1110cm -1 The absorption peak of Si-O-Si is partic...

Embodiment 2

[0036] Under nitrogen protection, SiO was added to the three-necked flask respectively 2-G 1.010 g, methyl isothiocyanate 6.5808 g, absolute ethanol 100 ml, the reaction mixture was mechanically stirred for 36 hours at 60°C. After the reaction was completed, it was cooled to 25°C, the product was filtered out, and the product was transferred to a Soxhlet extractor for extraction with absolute ethanol for 12 hours, and finally vacuum-dried at 50°C and 0.09Mpa for 48 hours to obtain the 1.0-generation silica gel bond Sulfur-loaded PAMAM dendrimer adsorbent on SiO 2 -G1.0-MITC, the structure is shown below.

[0037]

[0038] figure 2 SiO shown 2 -Infrared spectrum of G1.0-MITC, by figure 2 It can be seen at 1381cm -1 The characteristic absorption peak of C=S bond appeared at , which proved that the 1.0th generation silica gel bond-supported PAMAM dendrimers were successfully synthesized.

Embodiment 3

[0040] Under nitrogen protection, SiO was added to the three-necked flask respectively 2 -2.010 g of G, 13.6734 g of methyl isothiocyanate, 150 ml of absolute ethanol, and the reaction mixture was mechanically stirred for 48 hours at 50°C. After the reaction was completed, it was cooled to 25°C, the product was filtered out, and the product was transferred to a Soxhlet extractor for extraction with absolute ethanol for 12 hours, and finally vacuum-dried at 50°C and 0.09Mpa for 48 hours to obtain the 2.0-generation silica gel bond Sulfur-loaded PAMAM dendrimer adsorbent on SiO 2 -G2.0-MITC, the structure is shown below.

[0041] image 3 for SiO 2 -Infrared spectrum of G2.0-MITC, it can be seen from the figure at 1381cm -1 The characteristic absorption peak of C=S bond appeared at , which proved that the 2.0 generation silica gel bond-supported PAMAM dendrimers were successfully synthesized.

[0042]

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Abstract

The invention relates to a preparation method of a silica bonding sulfur-containing terminal group PAMAM dendrimer adsorption agent. The method comprises the steps of loading PAMAM by utilizing generation-0 silica, generation-1.0 silica or generation-2.0 silica, adopting 100 to 300 mL of anhydrous alcohol as a solvent, adding methyl-isorhodanate, heating and stirring for reaction, cooling to 25 DEG C after the reaction is completed, filtering to obtain a product, transferring the product into a Soxhlet extractor, extracting for at least 12 hours by utilizing anhydrous alcohol, carrying out vacuum drying for 48 to 72 hours so as to obtain a generation-0, a generation-1.0 or a generation-2.0 silica bonding sulfur-containing terminal group PAMAM dentrimer adsorption agent. The prepared adsorption agent adopts silica as a carrier and the sulfur-containing terminal group PAMAM dendrimer as a functional group, is good in adsorption effect on Hg(II) and can be widely used for removing, selectively adsorbing and concentrating and recycling the Hg(II) ions in water.

Description

technical field [0001] The invention relates to a preparation method of a silica gel bond-loaded sulfur-containing end-group PAMAM dendrimer adsorbent, belonging to the field of chemistry. Background technique [0002] The pollution of heavy metal ions to the environment, especially the pollution of water, is a major challenge facing human beings, and has long been a major problem affecting the survival of human beings and other organisms. Among many metal ions, Hg(II) is the most serious and harmful. Hg(II) is difficult to be biodegraded and toxic, and can enter the human body through the food chain, causing multi-system damage to the body, mainly neurotoxicity and renal toxicity, and posing a huge threat to human health. The removal of Hg(II) by adsorption technology can improve the pollution control efficiency, especially in the treatment of low-concentration Hg(II)-containing wastewater. The search for cost-effective Hg(II) adsorption materials has important applicatio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/30C02F1/28C02F1/62
CPCB01J20/265C02F1/288
Inventor 牛余忠曲荣君陈厚孙昌梅张盈
Owner LUDONG UNIVERSITY
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