A Method for Preparing Porous Covalent Organic Materials Using Hypergravity

A technology of covalent organic and hypergravity method, which is applied in the field of preparing porous covalent organic materials and producing porous covalent organic materials, can solve the problem of lack of mass production technology of porous covalent organic materials, difficult industrialization of porous covalent organic materials, The problem of low mixing rate of materials can achieve the effect of strengthening the microscopic mass transfer and micro mixing process, shortening the reaction time and improving the production efficiency.

Active Publication Date: 2017-07-18
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
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Problems solved by technology

[0009] 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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  • A Method for Preparing Porous Covalent Organic Materials Using Hypergravity
  • A Method for Preparing Porous Covalent Organic Materials Using Hypergravity
  • A Method for Preparing Porous Covalent Organic Materials Using Hypergravity

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Experimental program
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Effect test

Embodiment 1

[0037] Carry out the disposition of reaction mass in the glove box, two (1,5-cyclooctadiene) nickels and 6.4g of catalyst 11.25g are added in 800ml N, N'-dimethylformamide, and then Add 5 mL of 1,5-cyclooctadiene and stir for at least 30 minutes to dissolve 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 when the ...

Embodiment 2

[0051] Except following change, all the other are the same as embodiment 1.

[0052] Use a peristaltic pump to feed into the reactor, 100ml each time

[0053] 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

[0055] Except following change, all the other are the same as embodiment 1.

[0056] Add catalyst bis(1,5-cyclooctadiene)nickel 11.25g and 2,2'-bipyridine 6.4g into 800ml N,N'-dimethylformamide, then add 5ml 1,5-cyclooctadiene Alkenes, stirred 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.

[0057] 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.

[0058] 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 a hypergravity method, belonging to the technical field of porous covalent organic material preparation. The present invention strengthens the microscopic mixing and mass transfer process under the supergravity field. Preferably, the material in the supergravity rotating bed cavity is sucked into the rotating bed rotor through the rotating inner spiral tube, and the material is sheared by the high-speed rotating filler in the rotor. Mix, react. Compared with the reaction under normal gravity field, the invention can greatly improve the reaction rate and shorten the reaction time. In addition, for air-sensitive reaction systems, the present invention can achieve anhydrous and oxygen-free reaction conditions without the need for a glove box, and compared with small-dose preparation in a glove box, the present invention has a larger preparation amount and higher production efficiency high.

Description

[0001] field of invention [0002] 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. [0003] technical background [0004] 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...

Claims

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Application Information

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Patent Type & Authority Patents(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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