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A kind of preparation method of polyethylene polyamine modified ultra-high cross-linked adsorption resin

A polyethylene polyamine, ultra-high cross-linking technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of no mention, and achieve the effect of improving the ability of selective adsorption and improving the adsorption capacity

Inactive Publication Date: 2011-12-14
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Researchers from Nanjing University have applied for the patent of "A Synthesis Method of Ultra-high Cross-linked Weak Base Anion Exchange Resin with Dual Functions" (Patent No. ZL01134143.2) and "A Super-high Cross-linked Adsorption Resin Containing Quaternary Amino Compound Functions" Resin and its preparation method" patent (Patent No. 200610039861), they use dimethylamine and trimethylamine to aminate the post-crosslinking resin respectively, and can obtain ultra-high crosslinking resin modified with tertiary amine and quaternary amine functional groups type adsorption resin, but there is no mention of loading polyethylene polyamine functional groups on the surface of the resin

Method used

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  • A kind of preparation method of polyethylene polyamine modified ultra-high cross-linked adsorption resin
  • A kind of preparation method of polyethylene polyamine modified ultra-high cross-linked adsorption resin
  • A kind of preparation method of polyethylene polyamine modified ultra-high cross-linked adsorption resin

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Friedel-Crafts reaction: In a 250ml three-necked bottle, add 20.0g 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 5.0g FeCl 3 , stirred until the FeCl 3 Dissolve completely, gradually raise the temperature to 85°C, and carry out Friedel-Crafts reaction for 1 hour at a constant stirring speed 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.

[0051] Amination reaction: Into a 250ml three-neck flask, add 15.0g of ultra-high cross-linked adsorption resin prepared in Friedel-Crafts, add...

Embodiment 2

[0055] Friedel-Crafts reaction: In a 250ml three-neck flask, add 20.0g of dry chlorine balls with a chlorine content of 17.3% and a crosslinking degree of 6%, add 120ml of dichloroethane, and swell at room temperature for 13 hours; heat up to 50°C, add 4.8 g FeCl 3 , stirred until the FeCl 3 Dissolve completely, then gradually raise the temperature to 90°C, and carry out Friedel-Crafts reaction for 3 hours at a certain stirring speed to obtain an ultra-high cross-linking 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.

[0056] Amination reaction: In a 250ml three-necked flask, add 15.0g of ultra-high cross-linked adsorption resin obtained after Friedel-Crafts reaction, add 110ml of diethylenetriamine, and swell at room ...

Embodiment 3

[0060] Friedel-Crafts reaction: In a 250ml three-neck flask, add 20.5g of dry chlorine balls with a chlorine content of 17.3% and a crosslinking degree of 6%, add 120ml of dichloroethane, and swell at room temperature for 15 hours; heat up to 50°C, add 5g FeCl 3 , stirred until the FeCl 3 Dissolve completely, gradually raise the temperature to 83°C, and carry out Friedel-Crafts reaction at a certain stirring speed for 5 hours to obtain an ultra-high cross-linking adsorption resin. After the reaction, the resin was filtered out, washed several times with 1% hydrochloric acid aqueous solution and ethanol, then transferred to a Soxhlet extractor, and extracted with ethanol for 8.5 h. The resin was transferred and dried under vacuum.

[0061] Amination reaction: In a 250ml three-neck flask, add 15.0g of ultra-high cross-linked resin prepared in Friedel-Crafts, add 112ml of diethylenetriamine (resin:diethylenetriamine=1:7), and swell at room temperature for 15h . Raise the temp...

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Abstract

The invention discloses a preparation method of ultrahigh crosslinking type absorbent resin modified by polyethylene polyamine. The preparation method comprises the steps of: adding chloromethyl polystyrene resin well swelling in a solvent into lewis acid to serve as a catalyst, and performing Friedel-Crafts (F-S) reaction at the temperature of 80-100 DEG C for 0.5-0.9 h to obtain ultrahigh crosslinking type absorbent resin; and reacting the obtained resin with the polyethylene polyamine at the temperature of 100-140 DEC G for 15-22 h under the protection of N2 to prepare the ultrahigh crosslinking type absorbent resin modified by the polyethylene polyamine. According to the preparation method disclosed by the invention, the surface of the prepared ultrahigh crosslinking type absorbent resin is loaded with the polyethylene polyamine with different contents, the adsorbability of the resin to substances with weak polarity and polarity can be obviously improved, the F-C reaction time canbe simply controlled to realize selective absorption to different polarity substances such as naphthol, phenol, polyethylene polyamine and the like, and the preparation method has a wide application prospect in the fields of treatment and recycle of the phenol and organic acid wastewater.

Description

technical field [0001] The invention relates to a preparation method of a polyethylene polyamine-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 obtained by crosslinking linear polystyrene or recrosslinking low-crosslinked polystyrene through F-C reactions. Because the cross-linking degree of this kind of resin used as adsorbent is very high, it is called ultra-high cross-linked adsorbent 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 hydrop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F12/08C08F8/32C08J3/24B01J20/26B01J20/30
Inventor 黄健涵邓锐杰毛劲林晋晓英
Owner CENT SOUTH UNIV
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