Method for preparing porous covalent organic material by using ultra-gravity method

A technology of covalent organic and high gravity method, which is applied in the field of preparation of porous covalent organic materials and production of porous covalent organic materials, can solve the shortage of mass production technology of porous covalent organic materials, the difficulty of industrialization of porous covalent organic materials, The problem of low material mixing rate can achieve the effect of strengthening micro mass transfer and micro mixing process, shortening reaction time and high production efficiency

Active Publication Date: 2015-12-30
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

[0007] However, the continuous and mass production process of porous covalent organic materials is relatively scarce, making it difficult for porous covalent organic materials to be industrialized
In the current preparation process of porous covalent organic materials, a magnetic heating stirrer is generally used, and the material mixing rate is low and the heating is uneven, resulting in long reaction time, high energy consumption, and low production efficiency.

Method used

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  • Method for preparing porous covalent organic material by using ultra-gravity method
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  • Method for preparing porous covalent organic material by using ultra-gravity method

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Effect test

Embodiment 1

[0035] Carry out the disposition of reaction material in the glove box, add catalyst 11.25g bis(1,5-cyclooctadiene) nickel and 6.4g2,2'-bipyridine in 800mlN,N'-dimethylformamide, then add 5mL of 1,5-cyclooctadiene was stirred for at least 30 minutes to dissolve it completely. Subsequently, 2.47 g of 1,3,5-tribromobenzene was added to the solution to obtain a purple solution. The reaction kettle is pumped and nitrogen reciprocated four times to ensure that the reaction kettle maintains an anhydrous and oxygen-free environment. The reactor was heated with a water bath circulation device and kept at 85°C. Connect the material bottle to the feed pipe, repeat the pumping and venting operations again to ensure that the connection pipeline reaches anhydrous and oxygen-free conditions, and use a peristaltic pump to pump all the materials into the cavity of the supergravity rotating bed. The rotation speed of the high-gravity rotating bed is set to 2000r / min, and the timing starts wh...

Embodiment 2

[0049] Except following change, all the other are the same as embodiment 1.

[0050] Use a peristaltic pump to feed into the reactor, 100ml each time

[0051] Set the rotation speed of the high-gravity rotary bed to 400r / min, 800r / min, 1200r / min, 1600r / min, 2000r / min, 2400r / min, 2800r / min, and start the high-gravity rotary bed equipment. Start the timing from the pump, and take the material from the feed port after 1 hour.

Embodiment 3

[0053] Except following change, all the other are the same as embodiment 1.

[0054] Add 11.25 g of catalyst bis(1,5-cyclooctadiene) nickel and 6.4 g of 2,2'-bipyridine into 800 ml of N,N'-dimethylformamide, then add 5 ml of 1,5-cyclooctadiene, Stir for at least 30 minutes to completely dissolve. Subsequently, 4.83 g of 1,3,5-tris((4-bromophenyl)ethynyl)benzene was added to the solution to obtain a purple solution.

[0055] The reactor was heated with an oil bath circulation device and kept at 105°C. The rotating speed of the high-gravity rotating bed is set at 2000r / min, and the running time is 1h.

[0056] After drying in vacuum, the material was soaked in ethanol for 24 h, and then washed with supercritical CO 2 Drying removes solvent molecules to ensure the integrity of the material skeleton.

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Abstract

The invention discloses a method for preparing a porous covalent organic material by using the ultra-gravity method, and belongs to the technical field of preparation of porous covalent organic materials. The method comprises the following steps: under a high gravity field, the micromixing and mass transferring process is strengthened, materials in a cavity of a preferable over-gravity rotary bed are sucked into a rotor of the rotary bed through a rotating inner spiral pipe, and the materials are sheared by, mixed and reacted with a filler rotating at a high speed in the rotor. Compared with reaction under a normal gravity filed, the method is greatly increased in reaction rate, and shortened in reaction time; besides, as for reaction systems sensitive to air, the water-free and oxygen-free reaction condition can also be achieved without a glove box, and compared with low-dosage preparation in the glove box, the method is greater in preparation amount and higher in production efficiency.

Description

field of invention [0001] The invention relates to a method for preparing porous covalent organic materials using a hypergravity method. Specifically, the present invention relates to a method for the continuous, mass production of porous covalent organic materials using a hypergravity rotating bed. According to the method of the invention, the production efficiency of the porous covalent organic material can be greatly improved, and the output thereof can be increased, which belongs to the technical field of preparation of the porous covalent organic material. technical background [0002] Porous materials have experienced the development process from natural acquisition to artificial synthesis, from inorganic porous materials to organic porous materials. Since 2005, porous covalent organic materials with pure organic components have become the research frontier in the field of porous materials, especially the crystalline covalent organic framework materials developed by Y...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G61/02
Inventor 向中华谢呈鹏郭佳宁陈建峰罗勇王洁欣万刚李阳
Owner BEIJING UNIV OF CHEM TECH
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