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A kind of epoxy cyclohexane modified side chain liquid crystal polyether chelating resin and its preparation method and application

A technology of epoxy cyclohexane and chelating resin, applied in chemical instruments and methods, other chemical processes, water/sludge/sewage treatment, etc., can solve the problems of low adsorption capacity, affecting service life, poor mechanical strength, etc.

Active Publication Date: 2020-10-09
ZHENGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In terms of the structural manifestation of the chelating function of polyether chelating resins, traditional polyether molecules mostly use the oxygen atom at the junction of the side chain mesogenic group and the main chain as a coordination group, but because the electrons of the oxygen atom can be in the benzene ring Delocalization on the surface, resulting in weak coordination ability, the use effect is still not ideal
Although Zhang Shuangqing et al. introduced the pyrrole ring at the end of the mesogenic group, the pyrrole ring is a single coordination atom and requires multiple nitrogen atoms on the pyrrole ring to coordinate with the metal ion, so its coordination amount is limited, and the adsorption capacity lower
And affected by the molecular weight and structure of the main chain and the coordination competition of oxygen atoms in the original structure, it is not a terminal group with independent chelating ability, so its ion selectivity is usually negatively interfered
[0005] In addition, traditional polyethers are highly flexible chain structures that are polymerized from linear monomers, and their mechanical strength is poor, which leads to greater wear and tear of the resin in the subsequent application process and affects the service life

Method used

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  • A kind of epoxy cyclohexane modified side chain liquid crystal polyether chelating resin and its preparation method and application
  • A kind of epoxy cyclohexane modified side chain liquid crystal polyether chelating resin and its preparation method and application
  • A kind of epoxy cyclohexane modified side chain liquid crystal polyether chelating resin and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] The preparation method of chelating resin A comprises the steps:

[0060] (1) Polyether preparation:

[0061] Take 40mL CH respectively 2 Cl 2 , 0.01mol ethylene glycol, 0.009mol boron trifluoride ether in a flask, in a cold water bath, mechanically stirred at 0 ℃ for 30min. Measure 0.2 mol of epoxycyclohexane (CHO) and 0.3 mol of epichlorohydrin (ECH) and mix well, then transfer to a constant pressure dropping funnel and slowly drop into the reaction flask, and continue to react at 0°C for 5.5 hours. Add a large amount of water, stir vigorously for 5 minutes, separate the oil phase, and wash the product three times with water, then dissolve it with dichloromethane, use dichloromethane to take out the water and catalyst initiator in the product by atmospheric distillation, and then distill under reduced pressure to remove the residual dichloromethane to obtain copolyether.

[0062] (2) Biphenol sodium salt preparation:

[0063] Weigh 0.02 mol each of p-hydroxybiphe...

Embodiment 2

[0072] The preparation of chelating resin B (each intermediate preparation process is the same as resin A, i.e. step 1)-step 4) with embodiment 1)

[0073] Step 5) Measure 25ml DMSO to dissolve 0.05mol chloromethylated resin, put it in a round bottom flask, add 0.1mol ethylenediaminetriacetic acid sodium salt saturated aqueous solution, react in an oil bath at 100°C for 20h, add water to precipitate, filter Separation, washing with water several times to remove unreacted chelating agent, adding concentrated HCl with pH=1 to acidify after drying, washing to neutrality, wrapping with filter paper, extracting with ethanol Soxhlet for 48 hours, and obtaining side chain polyether liquid crystal chelating resin after drying , after drying, chelate resin B is obtained, and the structural formula is as follows:

[0074]

Embodiment 3

[0076] The preparation of chelating resin C comprises the steps:

[0077] (1) Preparation of polyether

[0078] Measure 0.01mol of ethylene glycol, 0.009mol of boron trifluoride ether and 30mL of chloroform into a flask, and mechanically stir for 30min at room temperature. Measure 0.2mol of CHO and 0.3mol of β-chloroethyl glycidyl ether, mix well, transfer to a constant pressure dropping funnel and slowly drop into the reaction bottle, and continue to react at 10°C for 10h. Add methanol to terminate the reaction, and add a large amount of solvent to dissolve the polymer. After washing and separating for many times, add methanol and pressurize distillation to remove impurities to obtain epoxycyclohexane-β-chloroethyl glycidyl ether copolyether.

[0079] (2) biphenol sodium salt is prepared with the step 2 of embodiment 1);

[0080] (3) Grafted biphenol

[0081]Weigh 0.001mol epoxycyclohexane-β-chloroethyl glycidyl ether copolyether with an electronic balance and place it in ...

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Abstract

The invention discloses a preparation method of a cyclohexane oxide modified side chain liquid crystal polyether chelating resin and an application of the cyclohexane oxide modified side chain liquidcrystal polyether chelating resin to treatment of Cu<2+> containing wastewater and belongs to the technical fields of preparation and application of functional polymer materials. The invention specifically relates to a chelating resin capable of trapping and recovering metal ions, and the chelating agent is prepared by taking chain polyether obtained by copolymerizing cyclohexane oxide serving asa modified monomer and a chlorine-containing ethylene oxide monomer as a main chain, introducing a rigid mesocrystal element with a large length-to-diameter ratio to the tail end of a side chain of the polyether, then, introducing chloromethyl to the mesocrystal element by chloromethylation, and finally, grafting a chelating group. The chelating resin meeting a actual application requirement is prepared by reasonably matching the kinds and structures of the polyether serving as the main chain, the mesocrystal element and the chelating group, the chelating resin is enabled to have relatively high mechanical strength and long service life while a certain flexibility of a polyether chain is retained.

Description

technical field [0001] The invention belongs to the technical field of preparation and application of functional materials, in particular to a side-chain liquid crystal polyether chelating resin with epoxy cyclohexane as the key modified comonomer, its preparation method and its application to Cu-containing 2+ Wastewater treatment field. Background technique [0002] Chelating resins are a class of polymer materials that are based on cross-linked polymers and connected with special groups to achieve their specific functions. Most of the traditional chelating resins use body-shaped cross-linked polystyrene as the matrix, and there are many types of such chelating resins. However, due to the high rigidity of polystyrene resin, it is difficult to form an orderly arrangement, so that the selectivity of the matrix to ions is very small, and only chelating groups play a role. Xu Yuwu and others have done some research on the preparation and application of linear polyether resins...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/06C08G65/24C08G65/323C08G65/331C08G65/333C08G65/338B01J20/26B01J20/30C02F1/28C02F101/20
CPCB01J20/262C02F1/285C02F2101/20C08G65/06C08G65/24C08G65/323C08G65/331C08G65/3317C08G65/33396C08G65/338
Inventor 梁政勇王爽石文锐
Owner ZHENGZHOU UNIV