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Cu3(BTC)2-modified capillary tube as well as preparation method and application thereof

A capillary, solution technology, applied in the field of chromatography

Active Publication Date: 2015-06-24
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

It has been widely used in catalysis, adsorption, gas storage and release, etc., but the use of Cu 3 (BTC) 2 The study of modified capillary has not been reported

Method used

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  • Cu3(BTC)2-modified capillary tube as well as preparation method and application thereof
  • Cu3(BTC)2-modified capillary tube as well as preparation method and application thereof
  • Cu3(BTC)2-modified capillary tube as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] (1) Pretreatment of capillary: first use CH 3 Wash the capillary with OH and secondary water for 5-15 minutes, then rinse the capillary with 1.5 mol / L NaOH solution for 10-20 minutes, then seal both ends of the capillary, and place it in an oven at 100°C for 2 hours. After the reaction, the capillary was cleaned successively with 0.5 mol / L HCl, secondary water and acetone, blown dry with nitrogen, and dried in an oven at 120°C for 1.5 h for later use;

[0025] (2) Preparation of γ-glycidyl etheroxypropyltrimethoxysilane-iminodiacetic acid sodium solution: Dissolve 2.12g of iminodiacetic acid sodium in 25mL of secondary water, adjust the pH of the solution with 10mol / L NaOH solution to After 11.0, add γ-glycidyloxypropyl trimethoxysilane in two batches: first slowly add 0.7mL of γ-glycidyloxypropyltrimethoxysilane to the above iminodiacetic acid in an ice-water bath Sodium solution, after mixing, transfer the system to a water bath at 65°C, stir and react for 6 h, then ...

Embodiment 2～6

[0030] The difference from Example 1 is that the steps (4) of Examples 2-6 are repeated 5, 10, 15, 20 and 25 times in sequence.

[0031] figure 2 It is the SEM picture of the inner wall of the capillary, wherein, A is a cross-sectional view, B is the inner wall of the bare capillary, and C-H correspond to Examples 1-6 in turn. by such as figure 2 It can be seen that the Cu on the inner wall of the capillary can be controlled by the number of modifications. 3 (BTC) 2 thickness of.

[0032] Table 1 Cu in the capillary of Examples 1-6 2+ Determination of content

[0033]

[0034] image 3 Capillary electrochromatographic separation of neutral small molecules by the capillary tubes of Examples 1-6 (corresponding to 3-LC, 5-LC, 10-LC, 15-LC, 20-LC, 25-LC respectively). 1. Benzene; 2. Naphthalene; 3. Acenaphthene; 4. Phenanthrene. Separation voltage: +20 kV. Detection wavelength: 214 nm. Capillary: total length 49.5 cm, effective length 41.0 cm. The sample solution ...

Embodiment 7

[0039] (1) Pretreatment of capillary: first use CH 3 Wash the capillary with OH and secondary water for 5-15 minutes, then rinse the capillary with 0.5 mol / L NaOH solution for 10-20 minutes, then seal both ends of the capillary, and place it in an oven at 100°C for 1.5 hours. After the reaction, the capillary was cleaned successively with 0.5 mol / L HCl, secondary water and acetone, blown dry with nitrogen, and dried in an oven at 120°C for 1.5 h for later use;

[0040] (2) Preparation of GLYMO-IDA solution: Dissolve 2.12g of sodium iminodiacetate in 25mL of secondary water, adjust the pH of the solution to 10.0 with 10mol / L NaOH solution, and then add γ-glycidyl etheroxypropyl in two batches Trimethoxysilane: slowly add 0.7mL γ-glycidyl etheroxypropyl trimethoxysilane to the above sodium iminodiacetate solution in an ice-water bath, and transfer the system to a 60°C water bath after mixing , after stirring and reacting for 6 h, transfer the system to an ice-water bath, then s...

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Abstract

The invention discloses a Cu3(BTC)2-modified capillary tube. The inner wall of the capillary tube is modified with a metal organic framework material Cu3(BTC)2. A preparation method for the Cu3(BTC)2-modified capillary tube comprises the following process: filling the capillary tube with a gamma-glycidoxy propyl trimethoxy silane-imino sodium diacetate solution, preserving the temperature at 90-100 DEG C for 10-12 hours, and then cleaning the capillary tube; at 60-80 DEG C, filling the capillary tube processed in the step (2) with a copper acetate alcohol solution, contacting for 10-20 minutes, cleaning the capillary tube with alcohol, filling the capillary tube with a trimesic acid alcohol solution, cleaning the capillary tube with alcohol after contacting for 20-40 minutes, and repeating the operation for 3-40 minutes. The capillary tube disclosed by the invention can be used for improving separating effects of neutral micromolecules of benzene, naphthalene, acenaphthene, phenanthrene and the like.

Description

technical field [0001] The invention belongs to the technical field of chromatography, in particular to a Cu 3 (BTC) 2 Modified capillaries, methods of preparation and applications thereof. Background technique [0002] Capillary electrochromatography (CEC) is an electrochromatographic separation method that integrates the high selectivity of high performance liquid chromatography (HPLC) and the high separation efficiency of capillary electrophoresis (CE), and has strong advantages in the analysis of complex samples. The commonly used open capillary column has the advantages of simple preparation process, no frit and particle filling in the preparation process, and simple equipment required. However, due to its low specific surface area and sample capacity, there are many problems in the separation and determination of trace analytes in complex matrices. problems, which limit the application of open capillary electrochromatography (OT-CEC). In order to solve the problems ...

Claims

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Application Information

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IPC IPC(8): B01D15/08B01J20/30B01J20/281C07C7/12C07C15/04C07C15/24C07C15/30C07C13/547
Inventor 陈兴国许银银
Owner LANZHOU UNIVERSITY
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