Method for synthesizing alizarin violet bond silica-gel soid-phase extraction agent

A technology of solid-phase extraction agent and bonded silica gel, which is applied in the field of synthesis of alizarin violet-bonded silica gel solid-phase extraction agent, can solve the problems of difficult control of experimental conditions, poor selectivity of solid-phase extraction agent, complex synthesis steps, etc. question

Inactive Publication Date: 2007-11-14
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the solid-phase extraction of lead is mostly established based on the principle of hydrophobic interaction. Metal ions react with chelating reagents and then are adsorbed on the solid to achieve the purpose of enrichment. This method has poor selectivity. , and the operation is complicated, and the experimental conditions are not easy to control
In some other solid-phase extraction agents for lead, organic chelating agents are also bonded to the surface of silica gel, but their synthesis steps are more complicated, and the selectivity of the selected solid-phase extraction agent is not very good, such as Talanta 58 (2002) 669-678, in this paper, 1,8-dihydroxyanthraquinone is connected to the surface of silica gel through two-step chemical reactions, and Pb is enriched when the pH is 6.0-7.5, Zn is enriched when the pH is 7.0-8.0, and Zn is enriched when the pH is 6.0-8.0. Cd is enriched at 8.0, and its enrichment rate is only 200 times; Talanta71 (2007) 1075-1082, in this paper, aminnothioamidoanthraquinone is linked to the surface of silica gel through a 4-step reaction, and Pb(II) is enriched at pH ≥ 3, Cu(II) and Cd(II), enrich Ni(II) and Co(II) at pH ≥ 4

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0006] A kind of solid-phase extractant-alizarin violet bonded silica gel that is selective to lead is synthesized, and its synthetic method comprises the following steps:

[0007] (1) Take 10g of 60-100 mesh silica gel, add it to a beaker, add 6mol / L hydrochloric acid to soak for 10-30 hours, then wash with water until neutral, then dry it in a vacuum oven at 85°C for 10 hours, and activate it for later use.

[0008] (2) Take the activated and pretreated silica gel, put it into a three-neck round bottom flask, add 50ml of anhydrous toluene, 10ml of silylating reagent aminopropyltriethoxysilane, and a little zeolite, and stir and reflux at 60°C for 6 hours. After cooling, filter with suction, wash the product successively with toluene, ethanol, and acetone until there is no colloid, and obtain aminopropyl silylated silica gel, filter the filter cake with suction, dry in vacuum at 60°C for 24 hours, and cool in a vacuum desiccator. Then store it in a normal desiccator for later...

Embodiment 2

[0011] A kind of solid-phase extractant-alizarin violet bonded silica gel that is selective to lead is synthesized, and its synthetic method comprises the following steps:

[0012] (1) Take 10g of 60-100 mesh silica gel, add it to a beaker, add 6mol / L hydrochloric acid to soak for 10-30 hours, then wash with water until neutral, then dry it in a vacuum oven at 110°C for 20 hours, and activate it for later use.

[0013] (2) Take the activated and pretreated silica gel, put it into a three-neck round bottom flask, add 50ml of anhydrous toluene, 10ml of silylating reagent aminopropyltriethoxysilane, and a little zeolite, and stir and reflux at 70°C for 8 hours. After cooling, filter with suction, wash the product successively with toluene, ethanol, and acetone until there is no colloid, and prepare aminopropyl silyl silica gel, filter the filter cake with suction, dry in vacuum at 80°C for 10 hours, and cool in a vacuum desiccator. Then store it in a normal desiccator for later u...

Embodiment 3

[0016] A kind of solid-phase extractant-alizarin violet bonded silica gel that is selective to lead is synthesized, and its synthetic method comprises the following steps:

[0017] (1) Take 10g of 60-100 mesh silica gel, add it to a beaker, add 6mol / L hydrochloric acid to soak for 10-30 hours, then wash with water until neutral, then dry it in a vacuum oven at 130°C for 8 hours, and activate it for later use.

[0018] (2) Take the activated and pretreated silica gel, put it into a three-neck round bottom flask, add 50ml of anhydrous toluene, 10ml of silylating reagent aminopropyltriethoxysilane, and a little zeolite, and stir and reflux at 90°C for 10 hours. After cooling, filter with suction, wash the product successively with toluene, ethanol, and acetone until there is no colloid, and obtain aminopropyl silylated silica gel, filter the filter cake with suction, dry in vacuum at 100°C for 8 hours, and cool in a vacuum desiccator. Then store it in a normal desiccator for late...

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Abstract

The present invention discloses a method for synthesizing alizarin purple bonded silica-gel solid-phase extracting agent. Said synthesis method includes the following steps: silica-gel activation step and silanization step, placing the aminopropyl silanized silica-gel obtained after silanization step into a flask, adding tetrahydrofuran solvent, N1N1-dicyclohexylcarbodiimide and alizarin purple, stirring them at normal temperature, filtering product, using absolute ethyl alcohol or acetone to wash product until the upper layer liquor is colorless, and drying so as to obtain the invented alizarin purple bonded silica-gel solid-phase extracting agent.

Description

Technical field: [0001] The invention relates to a general method of organic chemistry, in particular to a method for synthesizing an alizarin violet bonded silica gel solid-phase extraction agent. Background technique: [0002] Lead is a toxic heavy metal that exists widely in the environment, and its content has a significant impact on human health. Therefore, the determination of lead content and the treatment of actual samples contaminated by lead are of great significance. At present, the main methods for determining lead are spectral analysis methods such as atomic absorption method, atomic emission method, and spectrophotometry. However, when the content of lead ions in the actual sample is very low or the interference of the matrix substance is serious, the above method cannot be directly measured, and pre-treatment such as pre-separation and enrichment of the sample is required. The commonly used pretreatment techniques mainly include co-precipitation, electrodepos...

Claims

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Application Information

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Patent Type & AuthorityApplications(China)
IPC IPC(8): B01J20/286
Inventor樊静吴春来王键吉彭传云魏娅方梁峰
OwnerHENAN NORMAL UNIV