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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, which is applied in chemical instruments and methods, and other chemical processes, can solve the problems of resin specific surface area reduction, unfavorable adsorption, and weak interaction between functional group nitrogen atoms and adsorbates. , to achieve the effect of improving the ability of selective adsorption and improving the adsorption capacity

Inactive Publication Date: 2013-03-20
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
Comparison scheme
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 cross-linking degree of 6% (provided by Hebei Langfang Power Resin Factory), add 120ml of dichloroethane, and swell at room temperature 17h; heat up to 50℃, add 5.4g FeCl 3 , stirring until FeCl 3 It was completely dissolved, gradually heated up to 85°C, and reacted at a constant stirring speed for 9 hours to obtain an ultra-high cross-linked adsorption resin. After the reaction, the reaction mother liquor was poured out, washed alternately with 1% aqueous hydrochloric acid 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 out and dried in vacuo. Determination of chlorine content The residual chlorine content of the resin was 3.25%, and the Brunauer-Emmett-Teller (BET) model was used to fit N 2 Adsorption-desorption isotherm data...

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 13h; heat up to 50°C, add 4.8 g FeCl 3 , stirring until FeCl 3 It was completely dissolved, and then the temperature was gradually raised to 90 °C, and the reaction was carried out at a certain stirring speed for 6 hours to obtain an ultra-high cross-linked adsorption resin. After the reaction, the reaction mother liquor was poured out, washed alternately with 1% aqueous hydrochloric acid water and ethanol for several times until the eluate was clear, then transferred to a Soxhlet extractor and extracted with ethanol for 10 hours. The resin was transferred out and dried in vacuo. Determination of chlorine content The 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. ...

Embodiment 3

[0057] Friedel-Crafts: In a 250ml three-necked 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 15h; raise the temperature to 50°C, add 5.2 g FeCl 3 , stirring until FeCl 3 It was completely dissolved, gradually heated up to 83°C, and reacted for 8 hours at a certain stirring speed to obtain an ultra-high cross-linked adsorption resin. Determination of chlorine content The 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 bottle, add 18.6g of ultra-high cross-linking resin and 80.0ml of methylamine aqueous solution, raise the temperature to 80°C, and react for 15h to obtain a methylamine-modified ultra-high-crosslinking adsorption resin. Determination of chlorine content The residual chlorine content of the re...

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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 so as 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 cross-linked polystyrene through Friedel-Crafts reaction. . Due to the high degree of cross-linking of these resins, they are called ultra-high cross-linked adsorption resins. The structure and properties of ultra-highly cross-linked adsorbent resins are very different from those of polymer adsorbents prepared by copolymerization. [0003] However, the skeleton structure of the ultra-high cross-linked adsorption resin is all hydrophobic polystyrene. On the one hand, its strong hydrophobicity makes it need to be pretreated with a polar reagent (such as methanol) before use, which increases the complexity of the operation. On the other hand, t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/26
Inventor 黄健涵
Owner CENT SOUTH UNIV
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