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Preparation method of ultra-high crosslinking type adsorptive resin modified by N-methyl acetamido

A methylacetamide-based, ultra-high cross-linking technology, applied in chemical instruments and methods, adsorption water/sewage treatment, alkali metal oxides/hydroxides, etc., can solve the reduction of resin specific surface area, adverse adsorption, functional The problem of weak interaction between the base nitrogen atom and the adsorbate can achieve the effect of improving the ability of selective adsorption and improving the adsorption capacity.

Inactive Publication Date: 2012-02-15
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the adsorption site of the polar adsorption of the ultra-high cross-linked adsorption resin modified by dimethylamine and trimethylamine is nitrogen atom. On the one hand, due to steric hindrance, the functional group nitrogen atom of the resin has weak interaction ability with the adsorbate; On the one hand, because the trimethylamine-modified resin contains quaternary amino groups and has strong polarity, the specific surface area of ​​the resin decreases sharply, which is not conducive to adsorption.

Method used

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  • Preparation method of ultra-high crosslinking type adsorptive resin modified by N-methyl acetamido
  • Preparation method of ultra-high crosslinking type adsorptive resin modified by N-methyl acetamido
  • Preparation method of ultra-high crosslinking type adsorptive resin modified by N-methyl acetamido

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Experimental program
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Effect test

Embodiment 1

[0049] Friedel-Crafts reaction: In a 250ml three-necked bottle, add 22.5g of dry chlorine balls with a chlorine content of 17.3% and a crosslinking degree of 6% (provided by Hebei Langfang Electric Power Resin Factory), add 120ml of dichloroethane, and swell at room temperature 17h; warm up to 50°C, add 5.4g FeCl 3 , stirred until the FeCl 3 Dissolve completely, gradually raise the temperature to 85°C, and react at a constant stirring speed for 9 hours to obtain an ultra-high cross-linked adsorption resin. After the reaction, the mother liquor was poured out, washed alternately with 1% hydrochloric acid aqueous solution and ethanol for several times until the eluate was clear, then transferred to a Soxhlet extractor, and extracted with ethanol for 8 hours. The resin was transferred and dried under vacuum. The determination of chlorine content records that the residual chlorine content of resin is 3.25%, adopts Brunauer-Emmett-Teller (BET) model fitting N 2 Adsorption-desorp...

Embodiment 2

[0053] Friedel-Crafts: In a 250ml three-necked bottle, add 20.0g of dry chlorine balls with a chlorine content of 17.3% and a cross-linking degree of 6%, add 120ml of dichloroethane, and swell at room temperature for 13 hours; warm up to 50°C, add 4.8 g FeCl 3 , stirred until the FeCl 3 Completely dissolve, then gradually raise the temperature to 90°C, and react for 6 hours at a certain stirring speed to obtain an ultra-high cross-linked adsorption resin. After the reaction, pour out the reaction mother liquor, alternately wash with 1% aqueous hydrochloric acid water and ethanol several times until the eluate is clear, then transfer to a Soxhlet extractor, and extract with ethanol for 10 h. The resin was transferred and dried under vacuum. Determination of chlorine content The measured residual chlorine content of the resin is 6.15%, and the specific surface area of ​​the resin is 908.5m 2 / g, the pore volume is 0.5256cm 3 / g.

[0054] Amination reaction: In a 250ml three...

Embodiment 3

[0057] Friedel-Crafts: In a 250ml three-neck bottle, add 21.5g of dry chlorine balls with a chlorine content of 17.3% and a cross-linking degree of 6%, add 120ml of dichloroethane, and swell at room temperature for 15 hours; heat up to 50°C, add 5.2 g FeCl 3 , stirred until the FeCl 3 Dissolve completely, gradually raise the temperature to 83°C, and react for 8 hours at a certain stirring speed to obtain an ultra-high cross-linked adsorption resin. Determination of chlorine content The measured residual chlorine content of the resin is 4.17%, and the specific surface area of ​​the resin is 988.5m 2 / g, the pore volume is 0.6088cm 3 / g.

[0058] Amination reaction: In a 250ml three-necked flask, add 18.6g of ultra-high cross-linking resin and 80.0 ml of methylamine aqueous solution, raise the temperature to 80°C, and react for 15 hours to obtain methylamine-modified ultra-high cross-linking adsorption resin. The determination of chlorine content shows that the residual chlo...

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Abstract

The invention relates to a preparation method of ultra-high crosslinking type adsorptive resin modified by N-methyl acetamido. Lewis acid is added into a chlorine ball swollen in a solvent to be as a catalyst, and Friedel-Crafts reaction is carried out at 80 to 100 DEG C so as to obtain the ultra-high crosslinking type adsorptive resin; and the obtained resin is further aminated and acetylated soas to prepare the ultra-high crosslinking type adsorptive resin modified by the N-methyl acetamido. According to the preparation method of the ultra-high crosslinking type adsorptive resin modified by the N-methyl acetamido, the surface of the ultra-high crosslinking type adsorptive resin is loaded with the N-methyl acetamido, which can obviously enhance the adsorption capacity of the resin to weak polar and polar substances (such as phenol and salicylic acid). The ultra-high crosslinking type adsorptive resin modified by the N-methyl acetamido has an extensive application prospect in the fields of the treatment, the recycle and the like of phenols and organic acid wastewater.

Description

technical field [0001] The invention relates to a preparation method of an N-methylacetamide modified ultra-high cross-linked adsorption resin. Background technique [0002] In the early 1970s, Davankov et al. synthesized a class of porous polymer adsorbents, which were prepared by crosslinking linear polystyrene or recrosslinking low crosslinked polystyrene through the Friedel-Crafts reaction. . Due to the high degree of cross-linking of this kind of resin, it is called ultra-high cross-linking adsorption resin. The structure and performance of ultra-high cross-linked adsorption resin are very different from the polymer adsorbent prepared by copolymerization reaction. It is a kind of high-efficiency adsorbent and has important application prospects in the treatment and recycling of fine organic chemical wastewater. [0003] However, the skeleton structure of ultra-highly cross-linked adsorption resins is hydrophobic polystyrene. On the one hand, its strong hydrophobicity ...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30C02F1/28
Inventor 黄健涵
Owner CENT SOUTH UNIV
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