Preparation method and application of ionic liquid bonded silica adsorbent

A technology of ionic liquid and bonded silica gel, which is applied in the field of analytical chemical sample pretreatment, can solve problems such as difficult repeated use, easy loss of ionic liquid, and poor mechanical strength of materials, so as to reduce analysis cost, maximize flexibility, and improve The effect of precision

Inactive Publication Date: 2012-06-27
GUANGDONG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although ionic liquids can be modified onto the surface of the matrix material silica gel by a relatively simple physical loading method, the loaded ionic liquids are easily lost, and the mechanical strength of the material is poor, so it is difficult to reuse it many times.

Method used

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  • Preparation method and application of ionic liquid bonded silica adsorbent
  • Preparation method and application of ionic liquid bonded silica adsorbent
  • Preparation method and application of ionic liquid bonded silica adsorbent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 5.0 g of activated silica gel in a 150 mL round-bottomed flask, add 5 mL of excess 3-aminopropyltriethoxysilane, 0.5 mL of triethylamine as a catalyst, and 60 mL of dry toluene as a reaction solvent, magnetically stir and reflux for 24 Hour. The reaction was stopped, and after the reaction was cooled, suction filtration was performed. Then the product was washed with 150 mL of toluene, and then washed with 300 mL of ethanol and 500 mL of ultrapure water. Dry at 50°C for 8 hours.

[0022] Weigh 2.0 g of the silanized silica gel product synthesized in the previous step, 3.0 g of 1,3-di-n-butylimidazolium hexafluorophosphate ionic liquid, and 30 mL of dried toluene as a solvent, stir mechanically, and reflux for 24 hours. After stopping the reaction, wait to cool to room temperature, and filter with suction. First wash twice with 100mL of methanol, then wash with 1:1 ethanol and 500mL of water, and finally wash with 150mL of methanol, and dry the washed product in ...

Embodiment 2

[0024] Take 4.0 g of activated silica gel in a 150 mL round bottom flask, add 4 mL of 3-aminopropyltriethoxysilane, 0.5 mL of triethylamine as a catalyst, and 50 mL of dry toluene as a reaction solvent, and magnetically stir and reflux for 24 hours . Stop the reaction, and filter with suction after the reaction is cooled. Then the product was washed with 150 mL of toluene, and then washed with 300 mL of ethanol and 500 mL of ultrapure water. Dry at 50°C for 8 hours.

[0025] Weigh 2.0 g of the silanized silica gel product synthesized in the previous step, 3.0 g of 1-hexyl-3-methylimidazolium hexafluorophosphate ionic liquid, and 30 mL of dried toluene as a solvent, stir mechanically, and reflux for 36 hours. After stopping the reaction, wait to cool to room temperature, and filter with suction. Wash twice with 100mL of methanol, then wash with 1:1 ethanol and 500mL of water, and finally wash with 120mL of methanol, and dry the washed product in an oven at 60°C for 8 hours t...

Embodiment 3

[0027] Take 3.0 g of activated silica gel in a 150 mL round bottom flask, add 3 mL of 3-aminopropyltriethoxysilane, 0.5 mL of triethylamine as a catalyst, and 30 mL of dry toluene as a reaction solvent, and magnetically stir and reflux for 24 hours . Stop the reaction, and filter with suction after the reaction is cooled. Then the product was washed with 100 mL of toluene, and then washed with 200 mL of ethanol and 500 mL of ultrapure water. Dry at 50°C for 8 hours.

[0028] Weigh 2.0g of the silanized silica gel product synthesized in the previous step, 3.0g of 1-butyl-3-methylimidazolium bromide ionic liquid, 30mL of dried toluene as solvent, stir mechanically, and reflux for 36 hours. After stopping the reaction, wait to cool to room temperature, and filter with suction. First wash twice with 100mL of methanol, then wash with 1:1 ethanol and 500mL of water, and finally wash with 150mL of methanol, and dry the washed product in an oven at 60°C for 8 hours to obtain an ion...

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Abstract

The invention discloses a preparation method and an application of an ionic liquid bonded silica adsorbent. The preparation method takes silica as a carrier, takes 3-aminopropyltriethoxysilane as a coupling agent to synthesize alkylsilane epoxy silica, and reacted with ionic liquid like 1,3-di-n-butyl imidazole hexafluoride phosphate to obtain the ionic liquid bonded silica adsorbent; the ionic liquid is fixed on the solid phase carrier silica through a chemical modification mode, characteristics of the ionic liquid can be maintained, and the stability during the usage process can be substantially enhanced; thereby the analysis cost can be reduced, and the precision of the determination result can be improved. The ionic liquid adsorbent by the chemical modification possesses good adsorption function to the hydrophobic substances such as a heavy metal ion chelate, and is suitable for separation and enrichment of trace hydrophobic compounds in a water phase sample in the fields of environment, food and the like.

Description

technical field [0001] The invention belongs to the technical field of analytical chemical sample pretreatment, and in particular relates to a preparation method and application of an ionic liquid-bonded silica gel adsorbent. Background technique [0002] Solid-phase extraction has many advantages and is widely used, but there are few kinds of adsorbents for solid-phase extraction. Ionic liquids have the characteristics of non-volatile, non-flammable, strong solubility, and adjustable anion and cation structures. Although ionic liquids can be modified onto the surface of the matrix material silica gel by a relatively simple physical loading method, the loaded ionic liquids are easily lost, and the mechanical strength of the material is poor, making it difficult to reuse it many times. Therefore, it is necessary to develop a stable and efficient ionic liquid-modified solid-phase extraction adsorbent, and based on this, establish a corresponding solid-phase extraction applica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/22B01J20/30B01D15/08
Inventor 马晓国陈菊芳潘长桂
Owner GUANGDONG UNIV OF TECH
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