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High-thermal stability two-component organic gel and preparation method thereof

A high thermal stability, organogel technology, applied in the field of supramolecular chemistry and functional materials, can solve problems such as thermal stability performance of gelling factors, complex preparation of gelling factors, complex chemical structure, etc., and achieve high gelation. -The effect of solution phase transition temperature, simple preparation method and fast preparation process

Active Publication Date: 2018-01-09
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Modification of known high-efficiency gelling factors often has a complex chemical structure and requires many synthesis steps, so the preparation of gelling factors is complicated and the cycle is long, which limits its practicability.
[0006] Timme, A. et al reported a gel factor N 1 , N 3 , N 5 -Tris(2-ethylhexyl)benzene-1,3,5-tricarboxamide (Chemistry-A European Journal, 2012, 18, 8329-8339.), but only involved its chemical structure and properties in terms of liquid crystals, Not related to the thermal stability of the gelling factor

Method used

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  • High-thermal stability two-component organic gel and preparation method thereof
  • High-thermal stability two-component organic gel and preparation method thereof
  • High-thermal stability two-component organic gel and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Weigh 856mg of 2-ethylhexylamine, 500mg of trimesoyl chloride, and 670mg of triethylamine, dissolve them in 150mL of dry chloroform, and stir at 35°C for 12h. After the reaction solution was lowered to room temperature, extracted three times with deionized water, collected the organic phase, dried with anhydrous sodium sulfate, filtered and spin-dried the solvent under reduced pressure to obtain the first gel factor N 1 , N 3 , N 5 - Tris(2-ethylhexyl)benzene-1,3,5-tricarboxamide 813mg white powder solid, yield 79%.

[0035] figure 1 for N 1 , N 3 , N 5-Proton NMR spectrum of tris(2-ethylhexyl)benzene-1,3,5-tricarboxamide. The * in the spectrogram indicates the solvent peak, and all the characteristic peaks are given clear assignments, and there are no miscellaneous peaks in the spectrogram, which proves that the prepared first gel factor has a high purity.

Embodiment 2

[0037] Weigh 9.5mg of the first gelling factor and 0.5mg of the second gelling factor into a screw-top vial with a diameter of 12mm, add 1mL of toluene, heat to 85°C and ultrasonically until the gelling factor is completely dissolved in toluene, then cool naturally To room temperature, let it stand for 9h to form a stable organogel.

[0038] The vial was placed upside down in a vacuum oven and heated at a rate of 12°C / h, and the gel-solution phase transition temperature of the organogel was measured to be 73°C.

[0039] Using the first gelling factor alone, an organogel is formed in toluene under the same conditions, and its gel-solution phase transition temperature is 51°C.

Embodiment 3

[0041] Weigh 11.4mg of the first gelling factor and 0.6mg of the second gelling factor into a screw-top vial with a diameter of 12mm, add 1mL of toluene, heat at 88°C and use strong ultrasonic waves until the gelling factor is completely dissolved in toluene, then cool naturally to After standing at room temperature for 8 hours, a stable organic gel was formed.

[0042] The vial was placed upside down in a vacuum oven and heated at a rate of 12°C / h, and the gel-solution phase transition temperature of the organogel was measured to be 77°C.

[0043] Using the first gelling factor alone, an organogel was formed in toluene under the same conditions, and its gel-solution phase transition temperature was measured to be 54°C.

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Abstract

The invention discloses a high-thermal stability two-component organic gel. The high-thermal stability two-component organic gel is a mixed system which is prepared from N<1>,N<3>,N<5>-tris(2-ethylhexyl)phenyl-1,3,5-triformamide serving as a first gel factor, triethylamine hydrochloride serving as a second gel factor and a low-polarity organic solvent. According to the two-component organic gel disclosed by the invention, a porous three-dimensional reticular super-molecular structure is constructed through a synergistic effect between the first gel factor and the second gel factor; the formedorganic gel has high thermal stability, namely, gel-solution phase transition.

Description

technical field [0001] The invention belongs to the technical field of supramolecular chemistry and functional materials, and relates to an organic gel, in particular to an organic gel with high thermal stability and a preparation method of the organic gel. Background technique [0002] Some small organic molecules can form stable organic gels when they exist at very low concentrations (even below 1wt%) in organic solvents. These small organic molecules that can gel organic solvents are called gels. factor. Through non-covalent interactions such as hydrogen bonds, π-π stacking, and van der Waals forces, this type of gel factor can self-assemble into fibrous structures of various sizes, which are stacked and entangled with each other, and finally form an ordered three-dimensional network structure. At the same time, the three-dimensional network structure can wrap the organic solvent in it, so that the system loses its fluidity and forms an organic gel. As physical gels, or...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J13/00
Inventor 杨海宽赵鸿黄朝海卞成明
Owner ZHONGBEI UNIV
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