Preparation method of POSS (polyhedral oligomeric silsesquioxane)-based porous material capable of simultaneously improving porosity and carbon dioxide storage volume

A carbon dioxide and porous material technology, applied in the field of preparation of POSS-based porous materials, can solve problems such as the reduction of porous properties, and achieve the effects of increased pore volume and carbon dioxide storage capacity, excellent porous properties and carbon dioxide storage properties, and simple preparation steps.

Active Publication Date: 2015-04-29
SHANDONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the disadvantages of reducing porosity while introducing functional groups such as amino groups to improve carbon dioxide storage capacity, the present invention provides a preparation method for POSS-based porous materials that simultaneously improve porosity and carbon dioxide storage capacity

Method used

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  • Preparation method of POSS (polyhedral oligomeric silsesquioxane)-based porous material capable of simultaneously improving porosity and carbon dioxide storage volume
  • Preparation method of POSS (polyhedral oligomeric silsesquioxane)-based porous material capable of simultaneously improving porosity and carbon dioxide storage volume
  • Preparation method of POSS (polyhedral oligomeric silsesquioxane)-based porous material capable of simultaneously improving porosity and carbon dioxide storage volume

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Embodiment 1

[0060] The preparation of the POSS-based porous material (HPP-1-EDA) of embodiment 1, ethylenediamine functionalization

[0061] The POSS-based porous material described in this embodiment is a POSS-based porous material (HPP-1 ), the reaction formula is as follows:

[0062]

[0063] The preparation steps are as follows:

[0064] In a 100 mL dry round bottom flask, were added octavinyl POSS (632 mg, 1 mmol), 2,7-dibromo-9-fluorenone (1.35 g, 4 mmol), palladium acetate (90 mg, 0.4 mmol) and tris(o Methylphenyl) phosphorus (126mg, 0.48mmol), then add 45mL N,N-dimethylformamide and 15mL triethylamine, after stirring at room temperature, bubble with argon for at least half an hour, slowly raise the temperature to 100 °C, stirred at 100 °C for 48h.

[0065] After the reaction is completed and the reaction system returns to room temperature, the solid is filtered with suction, and the filter cake is washed with water, tetrahydrofuran, chloroform, water, methanol and acetone in...

Embodiment 2

[0076] The preparation of the POSS-based porous material (HPP-1-DAH) of embodiment 2, hexamethylenediamine functionalization

[0077] In a 100mL round-bottomed flask, add 0.3g of the POSS-based porous material HPP-1 prepared in Example 1 and 6g of hexamethylenediamine, then add 50mL of tetrahydrofuran and 5 drops of formic acid, reflux for 36h, filter with suction, and wash the filter cake three times with tetrahydrofuran. 50 mL was used each time, and then the filter cake was vacuum-dried at 80° C. for 18 h. Finally, 0.32 g of brown solid HPP-1-DAH was obtained.

[0078] The reaction formula is as follows:

[0079]

[0080] The infrared spectrum of HPP-1-DAH is attached Figure 9 , compared with HPP-1, 1718cm -1 The stretching vibration of the carbon-oxygen double bond of the carbonyl group in fluorenone is significantly weakened, and the peaks at other positions do not change significantly. Its solid NMR carbon spectrum is shown in the appendix Figure 10 , compared ...

Embodiment 3

[0083] The preparation of the POSS-based porous material (HPP-2-EDA) of embodiment 3, ethylenediamine functionalization

[0084] The POSS-based porous material described in this embodiment is composed of eight iodine (bromo) phenyl POSS (POSS-Ph-X-1) and FO-B (OH) 2 (HPP-2) was prepared by Suzuki reaction; the reaction formula is as follows:

[0085]

[0086] The preparation steps are as follows:

[0087] In a dry 100 mL round bottom flask, POSS-Ph-X-1 (X=I: 1.22 g, 0.6 mmol; X=Br: 998 mg, 0.6 mmol) and 2,7-diboronic acid-9-fluorenone ( 604mg, 2.4mmol) was added to 10mL N,N-dimethylformamide, then tetrakis(triphenylphosphine)palladium (277mg, 0.24mmol) and potassium carbonate aqueous solution (2.0M, 0.20mL) were added, and stirred at room temperature After that, bubble with argon for at least 0.5h, slowly raise the temperature to 120°C, and stir at 120°C for 48h.

[0088] After the reaction was completed and the reaction system returned to room temperature, the reaction ...

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PUM

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Abstract

The invention relates to a preparation method of a POSS (polyhedral oligomeric silsesquioxane)-based porous material capable of simultaneously improving porosity and carbon dioxide storage volume. The preparation method comprises the following steps: (1) dispersing the POSS-based porous material in an organic solvent, adding a primary amine compound and an organic acid catalyst, and carrying out reflux reaction under a stirring condition for 12-48 hours, wherein the POSS-based porous material comprises a POSS unit and a fluorenone unit, and the primary amine compound at least comprises two amino groups; and (2) after reaction, filtering, washing the filter cake and drying in vacuum to obtain the material. Compared with a raw material POSS-based porous material, the POSS-based porous material prepared by the method has preferable porous performance and carbon dioxide storage performance, and the BET specific surface area, pore volume and carbon dioxide storage volume are improved to a certain extent.

Description

technical field [0001] The invention belongs to the field of polymer materials, and relates to a method for preparing a POSS-based porous material, in particular to a method for preparing a POSS-based porous material that can simultaneously improve porosity and carbon dioxide storage capacity. Background technique [0002] In recent years, porous materials based on polyhedral oligomeric silsesquioxane (POSS) have attracted great attention from researchers at home and abroad for their wide applications in gas storage and separation, adsorption and separation, optoelectronics, sensors, etc. . Compared with other porous materials composed of pure organic units, the introduction of POSS units is beneficial to improve the thermal stability and mechanical properties of the materials. [0003] The combustion of fossil fuels such as oil and coal emits a large amount of carbon dioxide into the atmosphere, causing a terrible greenhouse effect in the atmosphere and posing a huge threa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21B01J20/22B01D53/02
CPCY02C20/40
Inventor 王灯旭冯圣玉刘鸿志
Owner SHANDONG UNIV
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