A kind of spherical covalent organic framework material and its preparation method and application
A covalent organic framework, spherical technology, applied in the field of chromatographic materials, can solve the problem that pure spherical COFs materials have not been reported, and achieve good application prospects, rapid separation, and the effect of expanding the range of pH use.
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Embodiment 1
[0026] Disperse 32.4 mg (0.24 mmol) terephthalaldehyde (, 56.2 mg (0.16 mmol) 1,3,5-tris(4-aminophenylbenzene) homogeneously in 25 mL (0.43 mol) of absolute ethanol at room temperature Ultrasonic to make it dispersed evenly, then quickly add 2 mL of 6mol / L acetic acid, and then ultrasonic for 3 minutes, then stand at room temperature for 24 hours to obtain a spherical covalent organic framework material. Add the obtained material to a Soxhlet extractor and reflux with tetrahydrofuran After washing for 24 hours, centrifuge and wash several times with ethanol, place in a vacuum oven at 120 °C for 24 hours to dry.
[0027] figure 1 It is a scanning electron micrograph of the spherical covalent organic framework material obtained in Example 1. It can be clearly seen from the figure that the particle size of the spherical covalent organic framework material is uniform, and the size is about 1 μm.
[0028] figure 2 It is a transmission electron microscope picture of the spherica...
Embodiment 2
[0033] The spherical covalent organic framework material prepared in Example 1 was used as a chromatographic stationary phase, and filled into an empty stainless steel short column with an inner diameter of 2.1 mm and a length of 50 mm by a dry filling method (stainless steel short columns need to be filled in sequence before filling). Ultrasonic cleaning several times with acetone and ethanol). When loading the column, one end of the empty column is tightened and connected to a vacuum source, and the other end is equipped with a funnel, and the dry spherical covalent organic framework material is slowly added to it, and the column wall is gently tapped from all directions to make the material fall into the column. After the filling is completed, the mobile phase (acetonitrile:water=90:10, v:v) with a flow rate of 0.5 mL / min is used to wash and balance for a long time on the high-performance liquid chromatograph to obtain a tightly packed and uniform chromatographic column. Fi...
Embodiment 3
[0036] In liquid chromatography (HPLC) mode, water was used as mobile phase A, acetonitrile was used as mobile phase B, and the chromatographic conditions were 55% B; the pump flow rate was 0.5 mL / min, and the detection wavelength was 214 nm; the determination of thiourea (10 ppm ) and toluene (50ppm), ethylbenzene (50ppm), propylbenzene (50ppm) single sample and mixed sample on the chromatographic column prepared in embodiment 2 separation situation, its chromatographic separation diagram is as follows Figure 7 shown.
[0037] Depend on Figure 7 It can be seen that the chromatographic column prepared by adopting the spherical covalent organic framework material of the present invention can realize effective separation of thiourea and toluene, ethylbenzene and propylbenzene.
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