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Preparation method and application of acetamide-modified ultra-high cross-linked adsorption resin

An ultra-high cross-linking and acetamide-based technology, which is applied in chemical instruments and methods, adsorption water/sewage treatment, and other chemical processes, can solve problems such as unsatisfactory adsorption effects, increase adsorption capacity and adsorption capacity, and reduce Adsorption steric hindrance, effect of increasing adsorption enthalpy

Inactive Publication Date: 2015-11-18
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In view of the defect that the modified cross-linked polystyrene in the prior art has an unsatisfactory adsorption effect on polar organic substances in water (such as: weakly polar phenol, highly polar salicylic acid), its application is limited. The purpose of the present invention is to provide a method for preparing acetamide-modified ultra-high cross-linked adsorption resin with simple process and low cost, with high specific surface area and large pore volume, and suitable pore size and polar pore structure.

Method used

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  • Preparation method and application of acetamide-modified ultra-high cross-linked adsorption resin
  • Preparation method and application of acetamide-modified ultra-high cross-linked adsorption resin
  • Preparation method and application of acetamide-modified ultra-high cross-linked adsorption resin

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Experimental program
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Effect test

Embodiment 1

[0040] Friedel-Crafts reaction: add 20.0g dry chloromethylated polystyrene (chlorine content is 17.3%, crosslinking degree is 6%) in 250mL there-necked flask, then add 120mL dichloroethane swelling agent to swell overnight; Heat up to 50°C, add 4.0g FeCl 3 and stirred until the FeCl 3 After complete dissolution, the temperature was raised to 80°C, and the reaction was carried out at this temperature for 8h. After the reaction is completed, pour out the reaction mother liquor, alternately wash with 1.0% hydrochloric acid solution and absolute ethanol until the eluate is clear, then transfer to a Soxhlet extractor, extract with absolute ethanol for 12 hours, and dry to obtain Super high cross-linked resin. The residual chlorine content of the resin is 3.35%, and the specific surface area of ​​the resin is 1032.6m 2 / g, the pore volume is 0.6729cm 3 / g.

[0041] Amination reaction: Dissolve 5.3g of hexamethylenetetramine and 6.3g of potassium iodide in a 250mL three-necked f...

Embodiment 2

[0047] Friedel-Crafts reaction: add 20.3g dry chloromethylated polystyrene (chlorine content is 17.3%, cross-linking degree is 6%) in 250mL there-necked flask, then add 120mL p-dichlorobenzene swelling agent to swell overnight; Heat up to 50°C, add 8.0g AlCl 3 and stirred until the AlCl 3 After complete dissolution, gradually raise the temperature to 85°C, and react at this temperature for 5h. After the reaction is completed, pour out the reaction mother liquor, alternately wash with 1.0% hydrochloric acid solution and absolute ethanol until the eluate is clear, then transfer to a Soxhlet extractor, extract with absolute ethanol for 12 hours, and dry to obtain Super high cross-linked resin. The residual chlorine content of the resin is 6.24%, and the specific surface area of ​​the resin is 1045.6m 2 / g, the pore volume is 0.7929cm 3 / g.

[0048] Amination reaction: Dissolve 10.2g of hexamethylenetetramine and 12.0g of potassium iodide in a 250mL three-necked flask with an...

Embodiment 3

[0051] Friedel-Crafts reaction: add 20.0g dry chloromethylated polystyrene (chlorine content is 17.3%, crosslinking degree is 6%) in 250mL there-necked flask, then add 120mL dichloroethane swelling agent to swell overnight; Heat up to 50°C, add 7.0g SnCl 4 and stirred until the SnCl 4 After complete dissolution, gradually raise the temperature to 80°C, and react at this temperature for 5h. After the reaction is completed, pour out the reaction mother liquor, alternately wash with 1.0% hydrochloric acid solution and absolute ethanol until the eluate is clear, then transfer to a Soxhlet extractor, extract with absolute ethanol for 12 hours, and dry to obtain Super high cross-linked resin. The residual chlorine content of the resin is 4.75%, and the specific surface area of ​​the resin is 976.5m 2 / g, the pore volume is 0.6485cm 3 / g.

[0052] Amination reaction: dissolve 10.5g of hexamethylenetetramine and 11.8g of potassium iodide in a 250mL three-necked flask with an appr...

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Abstract

The invention discloses a method for preparing acetamido-modified ultra-high crosslinking type adsorption resin and application of the resin. The preparation method comprises the following steps: with chloromethylated polystyrene as a raw material, and performing Friedel-Crafts reaction sequentially for crosslinking; and performing Delepine reaction to graft amino and acetylation to carry out amino acetylation, so as to prepare the acetamido-modified ultra-high crosslinking type adsorption resin with high specific surface area and pore volume, and appropriate aperture and polarity. The prepared acetamido-modified ultra-high crosslinking type adsorption resin can be applied to adsorption of a polar organic compound in water, especially has a selective adsorption effect on phenol and / or salicylic acid, and has a broad application prospect. The preparation method of the acetamido-modified ultra-high crosslinking type adsorption resin is simple in process, and low in cost, and can be applied to industrial production.

Description

technical field [0001] The invention relates to a preparation method and application of an acetamide-modified ultra-high cross-linking adsorption resin, which belongs to the field of polymer modification. Background technique [0002] In the early 1970s, Davankov et al crosslinked linear polystyrene or recrosslinked low crosslinked polystyrene through Friedel-Crafts reaction to form a class of porous polymers with unique structure and excellent performance. According to its preparation method, this type of reaction is called hypercrosslinking reaction (also known as Davankov hypercrosslinking reaction). The porous polymer prepared by ultra-high cross-linking reaction is called ultra-high cross-linked adsorption resin. Ultra-high cross-linked adsorbent resins are considered to be the third generation of adsorbent resins after gel-type and macroporous adsorbent resins. Ultra-high cross-linked adsorption resins usually have structural characteristics such as large specific su...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26B01J20/28B01J20/30C02F1/28C02F1/58
Inventor 黄健涵查宏伟杨丽李河冰伏振宇姚泽雷王小梅陈立妙刘又年
Owner CENT SOUTH UNIV