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Preparation method of hydrogen bond acceptor oxygen atom-rich super-crosslinked polymer and application of super-crosslinked polymer

A polymer and super-crosslinking technology, applied in the direction of alkali metal oxides/hydroxides, separation methods, alkali metal compounds, etc., can solve the problem of difficult to obtain super-crosslinked polymers, limited improvement ability, limited modification ability, etc. problems, to achieve the effect of improving selective adsorption capacity, increasing selective adsorption capacity, and improving selective adsorption

Inactive Publication Date: 2020-04-21
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation process is more complicated, and highly toxic chloromethyl ether is used as a cross-linking agent. The results of their adsorption properties show that this type of polymer is suitable for substances of different sizes and different polarities (such as: aniline, salicylic acid, phenol, etc.) etc.) have a certain adsorption capacity, but the adsorption selectivity is not obvious
[0005] Although the hypercrosslinked polymers of the prior art have certain adsorption properties to aniline, salicylic acid or phenol, etc., the adsorption effect is poor (the amount of adsorption is small, and the time to reach adsorption equilibrium is long), and the adsorption selectivity is poor.
The main reason is (1) The polymer cross-linking is too high, the porosity is dense, and only small molecules (such as N 2 etc.), and polar molecules with relatively large molecular size are not easy to diffuse into the pores, resulting in poor adsorption effect of polystyrene hypercrosslinked polymers on polar molecules; (2) existing hypercrosslinked polymers The precursor polymer is mainly modified by amination reaction, and the functional group is modified only by residual chlorine, the amount of functional group modification is small, the modification ability is limited, and the process is more complicated
Therefore, the existing hypercrosslinked polymers not only have limited improvement ability, but also it is difficult to adjust the pore structure, and it is difficult to obtain hypercrosslinked polymers with high selective adsorption effect.

Method used

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  • Preparation method of hydrogen bond acceptor oxygen atom-rich super-crosslinked polymer and application of super-crosslinked polymer
  • Preparation method of hydrogen bond acceptor oxygen atom-rich super-crosslinked polymer and application of super-crosslinked polymer
  • Preparation method of hydrogen bond acceptor oxygen atom-rich super-crosslinked polymer and application of super-crosslinked polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1) Preparation of precursor polymers rich in hydrogen bond acceptor oxygen atoms:

[0039] Add 20 g of chloromethylated polystyrene low-crosslinked polymer to N,N-dimethylformamide (DMF), and seal and swell overnight at room temperature. Install a reflux condenser and a mechanical stirrer, add phenol and 10g of basic catalyst K at room temperature 2 CO 3 , stirred for 30 minutes until completely dissolved, raised the temperature to 90-95°C, and reacted at this temperature for 24 hours, washed the obtained product alternately with hot water, cold water, and absolute ethanol for 3-4 times until colorless, and then washed with ethanol, The volume ratio of methanol and water is 1:1:1, extracting in a Soxhlet extractor for 8-24 hours, ordinary drying for 12 hours, and then vacuum drying for 24 hours to obtain the precursor polymer P;

[0040] 2) Friedel-Crafts alkylation reaction:

[0041] Add 10 g of precursor polymer P and 120 mL of 1,2-dichloroethane into a dry three-n...

Embodiment 2

[0052] 1) Preparation of precursor polymers rich in hydrogen bond acceptor oxygen atoms:

[0053] Add 20 g of chloromethylated polystyrene low-crosslinked polymer to N,N-dimethylformamide (DMF), and seal and swell overnight at room temperature. Install reflux condenser and mechanical stirrer, add naphthol and 10g basic catalyst K at normal temperature 2 CO 3 , stirred for 30 minutes until completely dissolved, raised the temperature to 90-95°C, and reacted at this temperature for 24 hours, washed the obtained product alternately with hot water, cold water, and absolute ethanol for 3-4 times until colorless, and then washed with ethanol, The volume ratio of methanol and water was 1:1:1, extracted in a Soxhlet extractor for 8-24 hours, dried for 12 hours in a normal way, and then dried in vacuum for 24 hours to obtain the precursor polymer P; infrared characterization showed that the precursor polymer P was -1 The absorption peak corresponding to the C-Cl stretching vibration ...

Embodiment 3

[0063] 1) Preparation of precursor polymers rich in hydrogen bond acceptor oxygen atoms:

[0064] Add 20 g of chloromethylated polystyrene low-crosslinked polymer to N,N-dimethylformamide (DMF), and seal and swell overnight at room temperature. Install reflux condenser and mechanical stirrer, add catechol and 10g basic catalyst Na at normal temperature 2 CO 3 , stirred for 30 minutes until completely dissolved, raised the temperature to 90-95°C, and reacted at this temperature for 24 hours, washed the obtained product alternately with hot water, cold water, and absolute ethanol for 3-4 times until colorless, and then washed with ethanol, The volume ratio of methanol and water was 1:1:1, extracted in a Soxhlet extractor for 8-24 hours, dried for 12 hours in a normal way, and then dried in vacuum for 24 hours to obtain the precursor polymer P; infrared characterization showed that the precursor polymer P was -1 The absorption peak corresponding to the C-Cl stretching vibration...

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Abstract

The invention relates to a preparation method of a hydrogen bond acceptor oxygen atom-rich super-crosslinked polymer and an application of the super-crosslinked polymer. The preparation method comprises the following steps: (1) preparation of a precursor polymer: carrying out a nucleophilic substitution reaction process on chloromethylated polystyrene and a phenol compound in an alkaline environment, and introducing a monomer containing hydrogen bond acceptor oxygen atoms into a polymer skeleton, and (2) preparation of a super-crosslinked polymer: carrying out a Friedel-Crafts alkylation reaction on the precursor polymer prepared in the step (1) and an external crosslinking agent under the catalysis of Lewis acid, and weaving a precursor polymer skeleton. The super-crosslinked polymer prepared by the method can realize regulation and control of the pore structure size, has a high-selectivity adsorption effect on aromatic organic compounds with specific molecular sizes, is easy to eluteafter adsorption, can be repeatedly used, and can be widely applied to the fields of chemical analysis, drug separation and purification, environmental pollution treatment and the like.

Description

technical field [0001] The invention belongs to the technical field of functional polymer synthesis, and in particular relates to a preparation method of a hypercrosslinked polymer rich in hydrogen bond acceptor oxygen atoms and an application of the hypercrosslinked polymer. Background technique [0002] Hypercrosslinked polymers, as a class of classic microporous organic polymers, have flourished in recent years. Their synthesis is mainly through the Friedel-Crafts reaction, forming a large number of rigid cross-linking bridges between polymer chains or aromatic monomers to produce highly cross-linked polymer networks. The Friedel-Crafts reaction is one of the electrophilic substitution reactions. The reaction conditions are in some inert solvents (1,2-dichloroethane, nitrobenzene, cycloethane), with Lewis acid (FeCl 3 , AlCl 3 ) as a catalyst and dissolved in the above solvents, at a certain temperature, catalytically active groups (chloromethyl, vinyl, acyl halide, etc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/00C08J3/24C08F8/02C08F8/00C08F112/08B01J20/26B01J20/28B01J20/30B01J20/34C02F1/28C08L25/06C02F101/34C02F101/38
CPCB01J20/267B01J20/28061B01J20/28064B01J20/28073B01J20/28076B01J20/28083B01J20/3475C02F1/285C02F2101/34C02F2101/345C02F2101/38C08F8/00C08F8/02C08J3/24C08J9/00C08J2325/06C08F112/08
Inventor 黄健涵王悠桑亚非王立志张都肖覃舒哲刘又年
Owner CENT SOUTH UNIV
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