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A kind of preparation method of porous nitrogen-containing flexible long-chain bridged polysilsesquioxane

A polysilsesquioxane, nitrogen-flexible technology, applied in chemical instruments and methods, silicon-organic compounds, water/sludge/sewage treatment, etc. question

Inactive Publication Date: 2018-02-09
LUDONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Our research group has synthesized a series of polyamine bridged polysilsesquioxane adsorption materials using epoxy group-containing silane coupling agents and polyamines as raw materials. During the synthesis, it was found that due to the flexibility of the bridging group The hydrogen bond between the sex and the hydroxyl group makes the entanglement between the bridges very serious. It is necessary to add the porogen cetyltrimethylammonium bromide (CTAB) and tetraethoxysilane as a skeleton support to obtain Porous materials, and the addition of these reagents, although increasing the specific surface area of ​​the material, reduces the content of functional groups in the material, thereby reducing the adsorption performance of the material
And the porogen CTAB needs to be removed in the later stage of synthesis, the process is cumbersome, and the residual CTAB will also affect the performance of the material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] Add 100 ml of ethanol, 22 ml of 3-chloropropyltrimethoxysilane and 10 ml of diethylenetriamine into a three-neck flask, mechanically stir and reflux for 12 h under nitrogen protection at 70 °C to obtain diethylenetriamine bridged single The solid ethanol solution was placed in a sealed polypropylene bottle for storage.

[0009] Add 4ml of sodium hydroxide solution with a concentration of 0.014g / ml to 40ml of the ethanol solution of the above-mentioned monomers, and naturally gel at room temperature. After the gel was completed, it was aged at 70°C for 4 hours and at 85°C for 4 days, then the gel was taken out, ground, and dried at room temperature. The dried gel was extracted in a Soxhlet extractor for 72 hours, using absolute ethanol (270 ml) and hydrochloric acid (37%, 15 ml) as solvents. Afterwards, the product was dried in a vacuum oven at 60°C to obtain a pale yellow bridged polysilsesquioxane product with a specific surface area of ​​up to 215 m 2 g -1 .

Embodiment 2

[0011] Add 100 ml of ethanol, 22 ml of 3-chloropropyltrimethoxysilane and 5 ml of diethylenetriamine into a three-neck flask, mechanically stir and reflux for 12 h under the protection of nitrogen at 85 °C to obtain diethylenetriamine bridged single The solid ethanol solution was placed in a sealed polypropylene bottle for storage.

[0012] Add 2ml of 0.014g / ml sodium hydroxide solution to 40ml of the ethanol solution of the above-mentioned monomers, and naturally gel at 30°C. After the gel was completed, it was aged at 70°C for 4 hours and at 85°C for 4 days, then the gel was taken out, ground, and dried at room temperature. The dried gel was extracted in a Soxhlet extractor for 72 hours, using absolute ethanol (270 ml) and hydrochloric acid (37%, 15 ml) as solvents. Afterwards, put the product in a vacuum oven at 60°C and dry it to obtain a pale yellow bridged polysilsesquioxane product with a specific surface area of ​​up to 220 m 2 g -1 .

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Abstract

The invention discloses a preparation method for porous fiber-bridged polysilsesquioxane with nitrogenous flexible long chains. The method comprises the steps that 3-chloro trimethoxy silane and diethylenetriamine are subjected to a reaction to obtain a fiber-bridged monomer with nitrogenous flexible long chains; natural gelling, extraction and drying are performed at the certain temperature under the action of the catalyst to obtain a final product. The preparation method is simple, no additional pore-foaming agent needs to be added, the product nitrogen functional group is high in content, the specific surface area and the porosity are high, and the excellent adsorption performance for Au3+ and Ag+ is achieved.

Description

technical field [0001] The invention relates to a preparation method of a porous nitrogen-containing flexible long-chain bridged polysilsesquioxane adsorbent and a product thereof. Background technique [0002] Adsorbent material is a kind of material that utilizes the adsorption-desorption effect of the material itself to achieve the purpose of separation and purification of substances, and has a wide range of applications. It is generally believed that an ideal adsorption material should have high porosity, high adsorption capacity, high selectivity and high stability under harsh conditions, and in order to facilitate future large-scale industrial production and reduce production costs, its synthesis method should be as simple as possible , with good reproducibility, and the physicochemical properties and structure-adsorption properties of the final product can be regulated during the synthesis process. From this perspective, bridged polysilsesquioxanes become an attracti...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/30C02F1/28C02F1/62C07F7/21
CPCB01J20/22B01J2220/4812C02F1/285C07F7/21
Inventor 孙昌梅金梦曲荣君
Owner LUDONG UNIVERSITY