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A kind of preparation method of hybrid porous polymer based on cage and ladder structure silsesquioxane

A technology of silsesquioxane and porous polymer, which is applied in the field of preparation of hybrid porous polymers, can solve problems such as insufficient research on porous materials, and achieves easy control of preparation process conditions, simple preparation steps and good chemical stability and thermal stability

Active Publication Date: 2020-05-26
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, the research on porous materials based on LTSs is still insufficient, and there are no relevant reports in the literature; the hybrid materials obtained by combining cage-type and ladder-type silsesquioxanes are expected to show some more superior properties, so this project research is necessary

Method used

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  • A kind of preparation method of hybrid porous polymer based on cage and ladder structure silsesquioxane
  • A kind of preparation method of hybrid porous polymer based on cage and ladder structure silsesquioxane
  • A kind of preparation method of hybrid porous polymer based on cage and ladder structure silsesquioxane

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Embodiment 1

[0048] A kind of preparation method based on the hybrid porous polymer (LCHPP) of cage type and ladder structure silsesquioxane, comprises steps:

[0049] (1) Add 0.632g of octavinylsilsesquioxane (OVS) with a cage structure, 0.291g of dodecylphenyl substituted tricyclic Trapezoidal silsesquioxane (PLS), 25mL 1,2-dichloroethane, stirred for 15 minutes, added 0.200g of anhydrous aluminum trichloride, stirred at room temperature for 30 minutes, then heated to 85°C, reacted for 24h; After the end, the reaction system was naturally cooled to room temperature, suction filtered, and the obtained solid was washed with methanol, tetrahydrofuran, chloroform, and acetone for 3 times respectively to obtain solid I;

[0050] (2) Soxhlet extract the obtained solid I with methanol and dichloromethane for 24 hours respectively, and vacuum-dry the obtained solid at 80° C. for 24 hours to obtain LCHPP.

[0051] The specific surface area of ​​the product obtained in this embodiment is 1273m 2...

Embodiment 2

[0060] A kind of preparation method based on the hybrid porous polymer (LCHPP) of cage type and ladder structure silsesquioxane, comprises steps:

[0061] (1) Add 0.632g of octavinylsilsesquioxane (OVS) with a cage structure, 0.437g of dodecylphenyl substituted tricyclic Trapezoidal silsesquioxane (PLS), 25ml 1,2-dichloroethane, stirred for 15 minutes, added 0.200g of anhydrous aluminum trichloride, stirred at room temperature for 30 minutes, then heated to 85°C, reacted for 24h; After the end, the reaction system was naturally cooled to room temperature, suction filtered, and the obtained solid was washed with methanol, tetrahydrofuran, chloroform, and acetone for 3 times respectively to obtain solid I;

[0062] (2) Soxhlet extract the obtained solid I with methanol and dichloromethane for 24 hours respectively, and vacuum-dry the obtained solid at 80° C. for 24 hours to obtain LCHPP.

[0063] The specific surface area of ​​the product obtained in this embodiment is 834m 2 ...

Embodiment 3

[0065] A kind of preparation method based on the hybrid porous polymer (LCHPP) of cage type and ladder structure silsesquioxane, comprises steps:

[0066] (1) Add 0.632g of octavinylsilsesquioxane (OVS) with a cage structure, 0.218g of dodecylphenyl substituted tricyclic Trapezoidal silsesquioxane (PLS), 25mL 1,2-dichloroethane, stirred for 15 minutes, added 0.200g of anhydrous aluminum trichloride, stirred at room temperature for 30 minutes, then heated to 85°C, reacted for 24h; After the end, the reaction system was naturally cooled to room temperature, suction filtered, and the obtained solid was washed with methanol, tetrahydrofuran, chloroform, and acetone for 3 times respectively to obtain solid I;

[0067] (2) Soxhlet extract the obtained solid I with methanol and dichloromethane for 24 hours respectively, and vacuum-dry the obtained solid at 80° C. for 24 hours to obtain LCHPP.

[0068] The specific surface area of ​​the product obtained in this embodiment is 1028m 2...

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Abstract

The invention provides a preparation method of a hybrid porous polymer based on cage and ladder type structure silsesquioxane. The method includes the steps of: dissolving cage structure octavinyl silsesquioxane (OVS) and dodecaphenyl substituted tricyclic trapezoid silsesquioxane (PLS) in an organic solvent, adding a catalyst, stirring the substances uniformly, and carrying out heating reaction;at the end of the reaction, performing cooling to room temperature, filtering and washing to obtain a solid I; subjecting the obtained solid I to soxhlet extraction, and then performing vacuum drying.The preparation steps adopted by the invention are simple, the preparation process conditions are easy to control, and the used raw materials are easily available; the obtained hybrid porous polymerhas high specific surface area, large pore volume, and good chemical stability and thermal stability, and has good adsorption capacity when applied to adsorption of dyes and heavy metal ions.

Description

technical field [0001] The invention relates to a preparation method of a hybrid porous polymer based on cage-type and ladder-structure silsesquioxane, and belongs to the technical field of polymer material preparation. Background technique [0002] In recent years, porous materials, as an important field of materials science, have attracted much attention due to their excellent properties, and have been widely used in catalysis, adsorption, separation, gas storage and other fields. Based on various practical requirements in different application fields, the design and synthesis of new porous materials with special chemical, mechanical or physical properties is becoming more and more important. Among many raw materials for the synthesis of porous materials, silsesquioxane is considered to be an ideal building block for hybrid porous materials due to its special molecular-level organic-inorganic hybrid structure. The composition of silsesquioxane is [RSiO 1.5 ] n (R is an ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/44C08J9/28C08L83/10C02F1/28C02F101/38
CPCC02F1/285C02F2101/308C02F2101/38C08G77/44C08J9/28C08J2383/10
Inventor 刘鸿志杜雅静
Owner SHANDONG UNIV
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