Monomer for polymer gel, polymer gel and preparation method

A polymer gel and monomer technology, applied in the direction of sulfate ester preparation, chemical instruments and methods, alkali metal oxides/hydroxides, etc., can solve the problem of difficult to accurately predict solvent molecules and polymer main chain and side chain groups Group interaction etc.

Active Publication Date: 2021-07-23
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the design of most polymer gels focuses on the gelation of oil molecules (non-polar organic solvents), and there is little research on the formation of colloids in polar organic solvents other than water and alcohols (such as DMF, DMSO). , this is mainly due to the difficulty of accurately predicting the interaction of solvent molecules with the main chain and side chain groups of the polymer, which can make the orderly arrangement of solvent molecules and stabilize them in the polymer

Method used

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  • Monomer for polymer gel, polymer gel and preparation method
  • Monomer for polymer gel, polymer gel and preparation method
  • Monomer for polymer gel, polymer gel and preparation method

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0031] The synthesis of embodiment one TPC-OTBS

[0032]

[0033]4,4',4''-trihydroxytriphenylmethane (1.46 g, 5 mmol) and imidazole (1.36 g, 20 mmol) were placed in a 100 mL flask, 20 mL of dichloromethane was added, and stirred at room temperature for 15 minutes, The solid dissolved completely. Dissolve tert-butyldimethylsilyl chloride (TBSCl, 3.02 g, 20 mmol) in 10 mL of dichloromethane, and add it dropwise to the above-mentioned flask through a constant pressure dropping funnel, and keep regular stirring in the flask during the dropwise addition, 30 Minutes dropwise completed. The whole reaction was stirred for 12 hours at room temperature. Use TLC to detect the progress of the reaction. After the conversion of the raw materials, the solids are removed by filtration. After the filtrate is spin-dried, the crude product is purified by column chromatography. The developer is dichloromethane / petroleum ether (v / v=1 / 2), and the pure product It is a pure white solid (2.3 g, ...

Embodiment 2

[0034] Embodiment 2 TPC-OSO 2 Synthesis of F

[0035]

[0036] 4,4',4''-trihydroxytriphenylmethane (1.46 g, 5 mmol) was placed in a 1000 mL flask, 20 mL of dichloromethane was added, and triethylamine (2.1 g, 20 mmol), stirring continuously to dissolve all solids. Seal the flask, pump it to a vacuum with a water pump, and then inject sulfuryl fluoride gas with a 55 L air bag. The whole reaction system was kept sealed and stirred for 12 hours at room temperature. The degree of progress of the reaction was detected by TLC. After conversion of the raw materials, the solid was removed by filtration, and the crude product was purified by column chromatography after the filtrate was spin-dried. The developer was ethyl acetate / petroleum ether (v / v=1 / 4). The pure product is white fine crystals (2.5 g, yield: 93%) TPC-OSO 2 F. The NMR spectrum of the synthesized product is attached figure 2 . 1 H NMR (400 MHz, CDCl 3 ,ppm) δ 7.28 (d, J = 8.6 Hz, 6H), 7.16 (d, J = 8.7 Hz...

Embodiment 3

[0037] Example 3 Preparation of TPC-cPS-gel

[0038] At room temperature, weigh an equimolar amount of TPC-OSO 2 Add F (200 mg) and TPC-OTBS (235 mg) into a 20 mL sample bottle, use a pipette gun to measure 4 mL of DMF and add it to the sample bottle as a solvent, dissolve all solids by conventional ultrasound, and then add 50 ug of DBU, sonicate again to dissolve and disperse evenly, let the sample bottle stand for 24 hours, pour off the upper layer of liquid, take the lower layer of gel, it is TPC-cPS-gel, and the formed colorless gel does not settle by centrifugation. image 3 for TPC-OSO 2 F, FT-IR of TPC-OTBS, TPC-cPS-Gel, image 3 a. image 3 b is the in situ infrared image of TPC-cPS-Gel, image 3 c. image 3 d; at 1437cm -1 、1219cm -1 Two characteristic stretches are observed at , which correspond to the S=O symmetric and asymmetric stretching vibration peaks, 1012cm -1 、940cm -1 The absorption peak is the stretching peak of S-O, 816cm -1 The peak at is attri...

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Abstract

The invention discloses a monomer for polymer gel, the polymer gel and a preparation method. The preparation method comprises the following steps of: reacting 4, 4', 4''-trihydroxytriphenylmethane with tert-butyldimethylsilyl chloride to obtain TPC-OTBS; reacting 4, 4', 4''-trihydroxy triphenylmethane with sulfuryl fluoride in the presence of triethylamine to prepare TPC-OSO2F; and dissolving TPC-OTBS and TPC-OSO2F in DMF, adding DBU, carrying out uniform ultrasonic dispersion, and standing to obtain the polymer gel. The gel obtained by the invention can selectively adsorb an organic solvent through electrostatic interaction and Van der Waals force. SEM (scanning electron microscope) and TEM (transmission electron microscope) are used for characterizing the surface and internal morphology of a solid material, the porous morphology of the solid material is found, and pores are most macropores. The structure of cross-linked polysulfate is represented by infrared and nuclear magnetism, a solid nuclear magnetism fluorine spectrum and an XPS element prove that a monomer sulfonyl fluoride group is completely reacted, and the polymer gel has a better application prospect in the aspect of adsorption due to the interaction force between the cross-linked polysulfate and a solvent.

Description

technical field [0001] The invention belongs to material preparation technology, and in particular relates to a polymer gel and its preparation method and application. Background technique [0002] Polymer gel is a metastable equilibrium system formed by the interaction between gel factor and solvent (water or other organic solvents) through hydrogen bonding, π-π stacking or van der Waals force and electrostatic attraction. It is favored because of its wide application in chemical separation, environmental restoration, biomedicine and smart materials. The semi-solid organogel formed by the interaction of polymers and organic solvents is an important basic material for future all-solid electrolyte batteries and artificial muscles. However, how the polymer chain interacts with liquid organic solvent molecules to stabilize it in the polymer framework has always been a mystery. This brings difficulties to the rational design of polymer gels. Although traditionally hydrogen bo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C07C305/26C07C303/24C08G75/24B01J20/26B01J20/28B01J20/30
CPCC07F7/1804C07F7/188C07C305/26C07C303/24C08G75/24B01J20/264B01J20/28047
Inventor 路建美徐庆锋
Owner SUZHOU UNIV
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