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Template-free preparation method of hollow micro-spherical polymers with covalent organic frameworks (COFs)

A covalent organic framework and hollow microsphere technology, which is applied in the preparation of microspheres and microcapsule preparations, can solve the problems of low porosity and small pore size of COFs, and achieve the effects of short process, mild conditions and high yield

Inactive Publication Date: 2015-07-15
UNIV OF SCI & TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the above problems, the object of the present invention is to provide a method for preparing covalent organic framework hollow microspheres with simple process, mild conditions and short flow process, so as to improve the porosity of hollow microspheres of covalent organic framework porous polymer materials, Effectively solve the problems of too small pore size and low porosity of COFs prepared by direct synthesis, and promote the application of COFs in phase change energy storage and other fields

Method used

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  • Template-free preparation method of hollow micro-spherical polymers with covalent organic frameworks (COFs)
  • Template-free preparation method of hollow micro-spherical polymers with covalent organic frameworks (COFs)
  • Template-free preparation method of hollow micro-spherical polymers with covalent organic frameworks (COFs)

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preparation example Construction

[0015] Preparation of ligand four-armed aldehyde:

[0016]

[0017] Take by weighing 2g (5.16mmol) of pentaerythritol bromide, 2.52g (20.6mmol) of 4-hydroxybenzaldehyde and 8.55g (61.9mmol) of anhydrous potassium carbonate, join in the anhydrous DMF of 30ml, heat up to 100 while stirring ℃, keep warm and stir vigorously for 72h, cool to room temperature, use a rotary evaporator to remove most of the DMF, and then add a large amount of ice water to dissolve the K 2 CO 3 , extracted the product several times with chloroform, and then washed repeatedly with ice water until the solution was a light yellow colorless transparent liquid. Most of the chloroform was rotary evaporated, and vacuum-dried to obtain the product four-arm aldehyde.

Embodiment 1

[0019]

[0020] Add 0.111g (0.2mmol) of four-arm aldehyde and 0.074g (0.4mmol) benzidine to 10mL of 1,2-dichloroethane to prepare a homogeneous solution, and add 0.4mL of 3M acetic acid solution to the solution , evenly dispersed, sealed and placed in an oven at 85°C, kept for 72h, cooled, filtered and washed repeatedly with chloroform, dried at 120°C for 24h to obtain the covalent organic framework hollow microsphere polymer SBQB, its scanning electron microscope and Transmission electron microscope picture as figure 1 , figure 2 shown. Depend on figure 1 It can be seen that the diameter of the hollow spheres is 3-5 μm, most of the spheres are piled together, no monodisperse microspheres appear, and the surface of the microspheres is very short burrs similar to sea urchins. Depend on figure 2 It can be seen that there are still some holes on the surface of the prepared hollow spheres, and the size of the holes is 100-400nm. The infrared characterization figure ( i...

Embodiment 2

[0022]

[0023] Add 0.111g (0.2mmol) of four-arm aldehyde and 0.104g (0.4mmol) of 4,4'-diaminoterphenyl to 10mL of 1,2-dichloroethane to prepare a homogeneous solution, add 0.4mL of 3M acetic acid solution, evenly dispersed, sealed and placed in an oven at 65°C, kept for 48h, cooled, filtered and washed repeatedly with chloroform, dried at 120°C for 24h to obtain the covalent organic framework hollow microsphere polymer SBQBI.

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Abstract

The invention discloses a template-free preparation method of hollow micro-spherical polymers with covalent organic frameworks (COFs), belonging to the field of inorganic nonmetal materials. The template-free preparation method comprises the steps of firstly, adding an organic aldehyde ligand and an amine ligand into a solvent, adding a certain quantity of additives after dissolving and dispersing, and controlling the reaction temperature, the concentrations of the ligands and the reaction time to obtain a solid sediment; and filtering, washing and drying to obtain hollow microspheres with the COFs. The structural characteristics of the hollow microspheres with the COFs are simultaneously determined by the kinds of the ligands, the reaction time, the reaction temperature and the solvent in the reaction system. The template-free preparation method has the advantages that the application range of a direct synthesis method to COFs synthesis is widened, and the hollow appearances of the polymers are obtained; the prepared hollow microspheres have high porosity which can be up to 85%, and the thickness and surface polarity of a spherical shell can be controlled through regulating reaction conditions in the system; and the method disclosed by the invention is simple in reaction process, high in yield, mild in condition, short in process and suitable for industrial production.

Description

technical field [0001] The invention belongs to a preparation method of a polymer, in particular to a preparation method of a covalent organic skeleton hollow microsphere. Background technique [0002] Porous materials widely used in the fields of gas storage, molecular separation and adsorption, ion exchange, catalysis, and sensing have always attracted the attention of researchers all over the world. In particular, porous polymers are the most prominent, because compared with other porous materials, porous polymer materials have the advantages of controllable preparation process, large specific surface area, high porosity, and chemical modification. The preparation methods of porous polymer materials generally include hard template method, soft template method, interfacial polymerization method and direct synthesis method. The hard template method, soft template method and interfacial polymerization method are the most commonly used. When using these methods, it is neces...

Claims

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Application Information

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IPC IPC(8): B01J13/14C08G12/08
Inventor 王戈汤甲杨明谭丽范爽金召奎王静静底巴罗
Owner UNIV OF SCI & TECH BEIJING
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