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Preparation of macrocyclic molecule-modified nano silica capillary chromatographic column

A nano-silica, capillary chromatographic column technology, applied in ion exchange, other chemical processes, ion-exchange regeneration, etc., can solve the problems of reports on the preparation of nano-silica capillary chromatographic columns without macrocyclic molecules, and achieve separation. Simple and convenient, good application prospects

Inactive Publication Date: 2017-01-04
ANQING NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] According to the current literature and patent review, there is no report on the preparation of nano-silica capillary column modified by macrocyclic molecules

Method used

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  • Preparation of macrocyclic molecule-modified nano silica capillary chromatographic column
  • Preparation of macrocyclic molecule-modified nano silica capillary chromatographic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] 1. Weigh 5.0g of nano-silica (40-60nm) into a glass sand core funnel, rinse with 1.0mol / L NaOH, deionized water, 1.0mol / L HCl, and high-purity water for 20 minutes each, and take it out at 110°C Dry for 10h. Then add 42mL of silylating reagent 3-aminopropyltriethoxysilane (APTS) methanol solution (1:1, V / V), and stir electromagnetically at a constant temperature of 55°C for 24h.

[0015] 2. Acylation modification of macrocyclic molecule (MCM): Weigh 3.42g macrocyclic molecule into a 150mL round-bottomed distillation flask, add 30mL absolute ethanol to dissolve it, then add 1.5mL dichlorooxalic acid, 1 drop of N , N-dimethylformamide, electromagnetic stirring (200 rpm) reflux for 4 hours, cooled to 0 ° C, filtered, washed with absolute ethanol to obtain macrocyclic acid chlorides.

[0016] 3. Add 3.0 g of macrocyclic molecular acid chloride, 20 mL of absolute ethanol, and 1 drop of glacial acetic acid to the product of step 1, and stir electromagnetically (rotating at 2...

Embodiment 2

[0018] 1. Weigh 10g of nano-silica (40-60nm) into a glass sand core funnel, wash with 1.0mol / L NaOH, deionized water, 1.0mol / L HCl, and high-purity water for 20 minutes each, and take it out at 110°C Dry for 10h. Then add 42mL of silylating reagent 3-aminopropyltriethoxysilane (APTS) methanol solution (1:1, V / V), and stir electromagnetically at a constant temperature of 55°C for 24h.

[0019] 2. Acylation modification of macrocyclic molecule (MCM): Weigh 6.84g of macrocyclic molecule and put it into a 150mL round-bottomed distillation flask, add 60mL absolute ethanol to dissolve it, then add 3.0mL dichlorooxalic acid, 1 drop of N , N-dimethylformamide, electromagnetic stirring (200 rpm) reflux for 4 hours, cooled to 0 ° C, filtered, washed with absolute ethanol to obtain macrocyclic acid chlorides.

[0020] 3. Add 6.0 g of macrocyclic acid chloride, 40 mL of absolute ethanol, and 1 drop of glacial acetic acid to the product of step 1, and stir it electromagnetically (rotating...

Embodiment 3

[0022] 1. Weigh 20g of nano-silica (40-60nm) into a glass sand core funnel, rinse with 1.0mol / L NaOH, deionized water, 1.0mol / LHCl, and high-purity water for 20 minutes, take it out and dry it at 110°C 10h. Then add 42mL of silylating reagent 3-aminopropyltriethoxysilane (APTS) methanol solution (1:1, V / V), and stir electromagnetically at a constant temperature of 55°C for 24h.

[0023] 2. Acylation modification of macrocyclic molecule (MCM): Weigh 13.68g of macrocyclic molecule and put it into a 150mL round bottom distillation flask, add 120mL absolute ethanol to dissolve it, then add 6.0mL dichlorooxalic acid, 1 drop of N , N-dimethylformamide, electromagnetic stirring (200 rpm) reflux for 4 hours, cooled to 0 ° C, filtered, washed with absolute ethanol to obtain macrocyclic acid chlorides.

[0024] 3. Add 12.0 g of macrocyclic molecular acid chloride, 40 mL of absolute ethanol, 1 drop of glacial acetic acid to the product of step 1, and stir electromagnetically (rotating a...

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Abstract

The invention belongs to the interdisciplinary field of inorganic chemistry and organic chemistry and discloses preparation of a macrocyclic molecule-modified nano silica capillary chromatographic column. Nano silica is modified first with silylation reagent APTS, macrocyclic molecules are then reacted with dichloride oxalate, separating and purifying are carried out to obtain macrocyclic molecule acyl chloride, and the macrocyclic molecule acyl chloride is then reacted with the modified nano silica to obtain the macrocyclic molecule-modified nano silica; the macrocyclic molecule-modified nano silica is charged into a capillary chromatographic column through a column charging pump, nitrogen flushing is carried out, and the temperature 280 DEG C is held for 12 h to obtain the capillary chromatographic column. The capillary chromatographic column prepared herein has an important application prospect in terms of separation, purification and chiral enantiomer separation.

Description

technical field [0001] The invention belongs to the interdisciplinary technical field of inorganic chemistry and organic chemistry, and relates to the preparation of a macrocyclic molecule-modified nano-silica color capillary column. Background technique [0002] There are many kinds of liquid chromatography columns, which are usually divided into ①conventional analytical columns with an inner diameter of 2-5mm and a column length of 10-30cm; ②narrow-diameter columns with an inner diameter of 1-2mm and a column length of 10-20cm; ③capillary columns (also known as micro column microcolumn), inner diameter 0.2-0.5mm; ④ semi-preparative column, inner diameter > 5mm; ⑤ laboratory preparation column, inner diameter 20-40mm, column length 10-30cm; Various columns are suitable for separating different kinds of substances due to their chemical bonding of different kinds of compounds. [0003] There are tens of thousands of compounds of various structures. If they can be chemical...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/281B01J20/30B01D15/08
CPCB01J20/281B01D15/08B01J2220/54B01J2220/84
Inventor 董彦杰章丹王钧伟何承东张元广
Owner ANQING NORMAL UNIV
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