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Preparation method of porous aromatic framework compound constructed with benzene ring base blocks

A technology for porous aromatic skeletons and compounds, which is applied in the field of preparation of porous aromatic skeleton compounds constructed from benzene ring blocks, which can solve the problems of high price of reaction catalysts, complex and harsh reaction conditions, and low reaction yields, and achieve simple reaction methods Ease of operation, high application value and market value, and high reaction yield

Inactive Publication Date: 2015-08-26
苏州纳埃净化科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, these synthetic methods have many disadvantages in the reaction process, such as low reaction yield, complex and harsh reaction conditions, dangerous reactants, and high price of reaction catalysts, which have become major obstacles to the industrialization and cheap acquisition of porous aromatic skeleton compounds.

Method used

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  • Preparation method of porous aromatic framework compound constructed with benzene ring base blocks
  • Preparation method of porous aromatic framework compound constructed with benzene ring base blocks
  • Preparation method of porous aromatic framework compound constructed with benzene ring base blocks

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specific Embodiment 1

[0045] Specific embodiment one: the preparation method of polybiphenyl is as follows:

[0046] (1) Weighing: feed biphenyl (molecular weight 154.21) and aluminum trichloride (molecular weight 133.34) according to the mass ratio of 1:1, that is, the analytical balance accurately weighs 500 mg (3.750 mmol) of aluminum trichloride and After the biphenyl of 500mg (3.242mmol) (the ratio of the amount of substance of reactant and catalyst is 0.865:1 at this moment), put in the 250mL round-bottomed flask that has dried in advance, and described round-bottomed flask has very strong Sealing, can carry out anhydrous and oxygen-free operation;

[0047](2) Dissolution and reaction of the reactant: Accurately inject 100 mL of anhydrous chloroform (the concentration of the reactant biphenyl is 0.03242 mol / L) after dry pretreatment in the round bottom flask with a syringe, and then put A magnetic stirrer with a size of 1 cm was inserted to replace the gas in the round bottom flask, so that ...

specific Embodiment 2

[0052] Specific embodiment two: the preparation method of polym-terphenyl is as follows:

[0053] (1) Weighing: Feed m-terphenyl (molecular weight 230.30) and aluminum trichloride (molecular weight 133.34) in a mass ratio of 1:1, that is, accurately weigh 500 mg (3.750 mmol) of aluminum trichloride with an analytical balance and 500mg (2.171mmol) of m-terphenyl (at this time, the ratio of the amount of reactant and catalyst is 0.579), put it into the pre-dried 250mL round bottom flask, and the round bottom flask has a strong Sealing, can carry out anhydrous and oxygen-free operation;

[0054] (2) Dissolving and reacting of reactant: Accurately inject 100mL anhydrous chloroform (the amount concentration of reactant m-terphenyl) after dry pretreatment in the round-bottom flask with a syringe, and then A magnetic stirring bar with a size of 1 cm was put in to replace the gas in the round bottom flask, so that the internal reaction was carried out under the protection of nitrogen...

specific Embodiment 3

[0059] Specific embodiment three: the preparation method of poly-p-terphenyl is as follows:

[0060] (1) Weighing: Feed p-terphenyl (molecular weight 230.30) and aluminum trichloride (molecular weight 133.34) in a mass ratio of 2:1, that is, the analytical balance accurately weighs 1.000g (7.500mmol) of trichloride After aluminum and 2.000g (8.684mmol) p-terphenyl (the ratio of the amount of substance of reactant and catalyst is 1.158:1), put it into the pre-dried 250mL round-bottomed flask, the round-bottomed flask It has strong sealing performance and can be operated without water and oxygen;

[0061] (2) Dissolving and reaction of reactant: Accurately inject 100mL anhydrous trichloromethane (the amount concentration of reactant p-terphenyl) after dry pretreatment in the round-bottomed flask, then A magnetic stirring bar with a size of 1 cm was put in to replace the gas in the round bottom flask, so that the internal reaction was carried out under the protection of nitrogen...

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Abstract

The invention discloses a preparation method of a porous aromatic framework compound constructed with benzene ring base blocks. According to the preparation method, an aromatic rigid monomer with no substituent group and composed of and only of a plurality of benzene rings is adopted as a reactant; and Lewis acid is adopted as a catalyst. Especially, biphenyl, m-terphenyl, p-terphenyl, o-terphenyl or 1,3,5-triphenylbenzene are adopted as the reactant; aluminum trichloride is adopted as the catalyst, and the porous aromatic framework compound is prepared. The reaction raw materials and the catalyst used in the method are cheap and easy to obtain, such that cost is low. The yield of the reaction is extremely high; the reaction method is simple and feasible; and the reaction conditions are substantially easy to obtain. An obtained product has extremely high hydrogen adsorption property, such that the product has high application and market values. With the method, the application prospect of the type of aromatic framework compound is expanded.

Description

technical field [0001] The invention relates to a preparation method of a porous material, in particular to a preparation method of a porous aromatic skeleton compound constructed by a benzene ring block. Background technique [0002] In the past two decades, porous materials, as a rapidly developing new material, have attracted more and more attention from chemists and scientists, especially in gas adsorption, gas storage, gas separation, and chemical reaction catalysis. Good performance in all aspects. [0003] An earlier series of porous materials is the metal-organic framework series, which is a series of porous materials with adjustable pore diameters prepared by the coordination of inorganic metal ions and organic groups. In 2005, Yaghi and his collaborators believed that some porous organic materials connected by covalent bonds could be designed and synthesized by using topological structures, and good stability and regular framework structures could be obtained. Aft...

Claims

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Application Information

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IPC IPC(8): C08G61/10
Inventor 李莉娜
Owner 苏州纳埃净化科技有限公司
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