A kind of triptycene functional material, preparation method and application thereof
A functional material, triptycene technology, applied in the field of gas chromatography, can solve problems such as affecting separation and detection, and achieve the effects of low raw material cost, good solubility, and good thermal stability
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Embodiment 1
[0053] A preparation method of triptycene functional material, the specific steps of the preparation method are as follows:
[0054] (1) Anthracene and p-benzoquinone were dissolved in xylene at a molar ratio of 1:1, heated to reflux for 4 hours, cooled for 1 hour, and the solid product was collected by filtration and recrystallized in xylene to obtain triptycene-p-benzoquinone.
[0055] (2) Dissolve triptycene-p-benzoquinone in glacial acetic acid solvent, heat and reflux for 1h, during the reaction, add dropwise hydrobromic acid in an equimolar amount to triptycene-p-quinone, continue to react for 1h, and cool After 1 h, the solid product was collected by filtration to obtain triptycene-p-benzodihydroquinone (TP-2OH).
[0056](3) Under the protection of nitrogen, dissolve TPGS-1000 and triethylamine in dichloromethane at a molar ratio of 1:35, stir at 25°C, add p-toluenesulfonyl chloride, the mixture of TPGS-1000 and p-toluenesulfonyl chloride Molar ratio is 1:2, reacts 24h...
Embodiment 2
[0062] The TPT chromatographic column that embodiment 1 makes is applied in gas chromatography analysis, to containing heptanone, heptanal, octanone, octanal, nonanone, nonanal, octanol, tridecane, methyl nonanoate, nonyl Alcohol, tetradecane, methyl decanoate, decanol, pentadecane and methyl undecanoate were separated. The chromatographic conditions are as follows: nitrogen with a purity of 99.99% is the carrier gas, the flow rate is 0.6mL / min, the temperature is programmed to rise from 40°C to 160°C (heating rate is 10°C / min), the inlet temperature is 250°C, and the detector temperature is 300°C.
[0063] Separation result as figure 2 As shown, the chromatographic peaks 1 to 15 in the figure are: heptanone, heptanal, octanone, octanal, nonanone, nonanal, octanol, tridecane, methyl nonanoate, nonanol, tetradecane, Methyl Decanoate, Decyl Alcohol, Pentadecane and Methyl Undecanoate. Depend on figure 2 It can be seen that the TPT chromatographic column can separate various...
Embodiment 3
[0065] The TPT chromatographic column prepared in Example 1 was applied to gas chromatographic analysis to separate samples containing thiophene, pyridine, 3-picoline, pyrrole and pyrazole. The chromatographic conditions are as follows: nitrogen with a purity of 99.99% is the carrier gas, the flow rate is 1mL / min, the temperature is programmed to rise from 40°C to 160°C (heating rate is 10°C / min), the inlet temperature is 250°C, and the detector temperature is 300°C.
[0066] Separation result as image 3 As shown, the chromatographic peaks 1 to 5 in the figure are successively: thiophene, pyridine, 3-picoline, pyrrole and pyrazole. Depend on image 3 It can be seen that the TPT chromatographic column can baseline-separate 5 kinds of heterocyclic components, and the basic components (pyridine, 3-picoline, pyrazole) that are easily adsorbed or tailed (pyridine, 3-picoline, pyrazole) all obtain symmetrical chromatographic peaks, indicating that The TPT chromatographic column h...
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