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Naphthyl methyl imidazole modified silica gel adsorbent and preparation method and application of naphthyl methyl imidazole modified silica gel adsorbent

A naphthylmethylimidazole, silica gel adsorption technology, applied in chemical instruments and methods, adsorption water/sewage treatment, other chemical processes, etc., can solve the problems of failing to give full play to the designability of ionic liquids, lack of structure and performance relationship, etc. , to achieve the effect of novel structure, high enrichment factor and large adsorption capacity

Inactive Publication Date: 2015-03-04
HENAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, little research has been done in this area, and it is still in the stage of optimizing conditions such as the synthesis and application of new materials. The designability of ionic liquids has not been fully utilized, and the understanding of the relationship between its structure and performance is lacking.

Method used

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  • Naphthyl methyl imidazole modified silica gel adsorbent and preparation method and application of naphthyl methyl imidazole modified silica gel adsorbent
  • Naphthyl methyl imidazole modified silica gel adsorbent and preparation method and application of naphthyl methyl imidazole modified silica gel adsorbent
  • Naphthyl methyl imidazole modified silica gel adsorbent and preparation method and application of naphthyl methyl imidazole modified silica gel adsorbent

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Add the solution of imidazole (2.119g, 31mmol) in 1,4-dioxane (50mL) to the suspension of oil-free NaH (1.364g, 34mmol) in 1,4-dioxane (100mL) , stirred at 90°C for 1h, then added 1-chloromethylnaphthalene (5g, 28mmol) in 1,4-dioxane (50mL) dropwise to the above solution, and stirred the mixed solution at 90°C for 22h to prepare Brown solution, remove the solvent by rotary evaporation, add 100mL distilled water to the residue, wash with CH 2 Cl 2 (3*50mL) extraction, extract with anhydrous MgSO 4 Dry, rotary evaporate to remove CH 2 Cl 2 Afterwards, the product 1-(1-naphthylmethyl)imidazole was obtained.

[0023]

[0024] (2) Mix 3-chloropropyltriethoxysilane and 1-(1-naphthylmethyl)imidazole at a molar ratio of 1:1.2, then react at 80°C for 24 hours to obtain 1-(1-naphthalene Methyl)-3-triethoxysilylpropylimidazole.

[0025]

[0026] (3) React 5g of activated silica gel with 4.2g of 1-(1-naphthylmethyl)-3-triethoxysilylpropylimidazole in toluene (60mL) ...

Embodiment 2

[0034] Adsorption selectivity experiment

[0035] Experimental conditions: mass of naphthalenemethylimidazole modified silica gel adsorbent: 25mg, initial concentration of phenol solution: 50mg / L, solution volume: 50mL, temperature: 30°C, stirring speed: 160rpm, time: 3h. Table 1 shows the adsorption results of the naphthalenemethylimidazole-modified silica gel adsorbent on different phenolic substances under the same conditions. As shown in Table 1, the naphthalenemethylimidazole-modified silica gel adsorbent selectively adsorbs 2,4-dinitrophenol, And the adsorption capacity is large.

[0036] Table 1 Adsorption results of different phenols by naphthalenemethylimidazole modified silica gel adsorbent under the same conditions

[0037] Adsorbent Adsorption capacity (mg / g) 2,4-Dinitrophenol 66.2 p-Chlorophenol 14.7 3-Aminophenol 14.5 1-naphthol 13.6 2-naphthol 9.38 2-Nitrophenol 7.74 3-Nitrophenol 1.42 4-Nitrophenol 10...

Embodiment 3

[0039] Adsorption Kinetic Analysis

[0040] Experimental conditions: mass of naphthalenemethylimidazole modified silica gel adsorbent: 25mg, initial concentration of 2,4-dinitrophenol solution: 50mg / L, solution volume: 50mL, temperature: 30°C, stirring speed: 160rpm. Such as image 3 It can be seen that the adsorption rate of 2,4-dinitrophenol on the silica gel adsorbent modified by naphthalenemethylimidazole is fast, and the adsorption capacity reaches 66 mg / g in 10 minutes, which is close to the saturated adsorption.

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Abstract

The invention discloses a naphthyl methyl imidazole modified silica gel adsorbent and a preparation method and application of the naphthyl methyl imidazole modified silica gel adsorbent. The technical scheme provided by the invention is characterized in that the naphthyl methyl imidazole modified silica gel adsorbent has the following structure as shown in the specification. The invention also discloses the preparation method of the naphthyl methyl imidazole modified silica gel adsorbent and the application of the naphthyl methyl imidazole modified silica gel adsorbent in a separation enrichment solution-2, 4-dinitrophenol. The naphthyl methyl imidazole modified silica gel adsorbent is simple in preparation process, novel in structure, high in multiple of enrichment on 2, 4-dinitrophenol in the solution, easy to elute, high in adsorption efficiency and adsorption quantity, and invariable in recovery rate after being used for multiple times.

Description

technical field [0001] The invention belongs to the technical field of ionic liquid modified silica gel adsorbent, in particular to a naphthalenemethylimidazole modified silica gel adsorbent and its preparation method and application. Background technique [0002] For solid phase extraction technology, instruments and devices have become more and more mature, while new solid phase extraction adsorbents are still being researched and developed. The current development of solid-phase extraction adsorbents focuses on expanding the range of use of adsorbents on the one hand, and developing adsorbents with high selectivity on the other hand. [0003] The new materials prepared by grafting ionic liquids onto solid supports (silicon-based materials or polymers) through chemical bonding can not only retain the original properties of ionic liquids, but also give full play to the properties of solid support materials. This new type of material has attracted attention in the fields of...

Claims

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Application Information

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IPC IPC(8): B01J20/22B01J20/30C02F1/28C02F1/58C02F101/38
CPCB01J20/22B01J2220/4812C02F1/285C02F2101/345
Inventor 王治科叶存玲武海丽范顺利王雪源
Owner HENAN NORMAL UNIV
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