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Nanometer spherical covalent organic framework as well as preparation method and application of nanometer spherical covalent organic framework with controllable particle size

A covalent organic framework, spherical technology, applied in the direction of nanotechnology, nanotechnology, nanomedicine, etc., can solve the problems of underdevelopment, cumbersome multi-step sequence, hindering biomedical applications, etc., and achieve the effect of simplifying synthesis

Active Publication Date: 2022-01-14
HUBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, methods to control the optimal particle size below 100 nm while achieving water-dispersibility and specific surface functions are still underdeveloped, which hampers many biomedical applications such as protein aggregation inhibition and drug delivery
At the same time, the typical synthesis process of COF NPs involves a cumbersome multi-step sequence, which requires step-by-step control of particle size and surface properties, and it is difficult to unify these two aspects in the same step.

Method used

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  • Nanometer spherical covalent organic framework as well as preparation method and application of nanometer spherical covalent organic framework with controllable particle size
  • Nanometer spherical covalent organic framework as well as preparation method and application of nanometer spherical covalent organic framework with controllable particle size
  • Nanometer spherical covalent organic framework as well as preparation method and application of nanometer spherical covalent organic framework with controllable particle size

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] This example provides a nano-spherical covalent organic framework, which achieves both size control and surface functionalization of COF NPs through an aspartic acid (Asp)-assisted synthesis method, such as figure 1 shown. The raw materials for its synthesis are 1,3,5-tris(4-aminophenyl)benzene (TAPB) and terephthalic acid (TPD).

[0045] Its concrete preparation method is:

[0046] 0.04 M D-Asp aqueous solution was added to ACN (1.5 mL) in TAPB (0.04 mmol) and TPD (0.06 mmol) solution, and a yellow amorphous solid was precipitated immediately at room temperature.

[0047] Then the precipitated yellow amorphous solid was centrifuged at 6000rpm for 10min, washed with ACN, and oven-dried at 60°C for 30min to obtain a powder sample nano-spherical covalent organic framework (D-Asp-COF).

[0048] The prepared D-Asp-COF was subjected to transmission electron microscopy, and its image was as follows Figure 4 , Figure 5 As shown in the scanning electron microscope, the imag...

Embodiment 2

[0050] In this example, the traditional use of acetic acid (HAv) as a catalyst, the prepared nano-spherical covalent organic framework was used as the control group, and the D-Asp-COF prepared above was used as the experimental group to test the water dispersibility and hydrophilicity:

[0051] In the control group, nanospherical covalent organic frameworks were prepared as follows:

[0052] The reaction raw materials 1,3,5-tris(4-aminophenyl)benzene (TAPB) and terephthalic acid (TPD) were placed in acetonitrile (ACN) / HAc system at room temperature for 10s, through the condensation reaction of reversible imine bonds , the yellow amorphous solid HAc-COF spheres were obtained.

[0053] Inspection process:

[0054] Stable HAc-COF and D-Asp-COF nanoparticle suspensions prepared under the same procedure, the two suspensions were placed under the same change and observed.

[0055] Test results such as figure 2 , the HAc-COF suspension started to precipitate after one day, while ...

Embodiment 3

[0058] This example is based on the preparation method of D-Asp-COF provided in Example 1, and the experiment of controlling its particle size is carried out:

[0059] (1) Change the batch feeding times of D-Asp (n times feeding, each round 1 / n, interval 10min) to control the particle size of D-Asp-cof balls. Preparation of D-Asp-COF spheres (TAPB: 16mM, 1mL; TPD: 24mM, 1mL LD-Asp (0.04M, 2.4mL) reacted for 200min to obtain 70nm COF spheres.

[0060] (2) Change the feeding speed: divided into one-time feeding and intermittent feeding, such as twice, three times, four times, etc. to control the feeding speed. Depending on the batch added, two growth modes were observed: growth of existing particles and nucleation of new particles.

[0061] (3) Change the initial monomer concentration: under the same conditions as other experiments, adjust the initial monomer concentration to control the particle size. When the amount of D-Asp increased from 1 equivalent to 4 equivalents, the ...

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Abstract

The invention discloses a nanometer spherical covalent organic framework. The specific structural formula of the nanometer spherical covalent organic framework is as shown in the specification. A specific preparation method of the nanometer spherical covalent organic framework comprises the following steps: 1) with 1,3,5-tris(4-aminophenyl) and terephthalic acid as reaction raw materials, D-aspartic acid as a catalyst and acetonitrile as a reaction solvent, carrying out reacting at room temperature for 8-20 seconds, and separating out a yellow amorphous solid; and 2) washing and drying the obtained yellow amorphous solid to obtain a product. A method for controlling a particle size based on the preparation method comprises the following steps: changing the batch charging frequency of the catalyst D-aspartic acid, adjusting the concentration of the initially added D-aspartic acid, and carrying out secondary forming. The nanometer spherical covalent organic framework can be made into drugs for treating related neurodegenerative diseases. The invention provides a strategy of utilizing asp to assist synthesis, the size control and surface functionalization of COF NPs are realized in the same experimental process, and the surface property and particle size of the COF ball can be shown through a relatively simple method.

Description

technical field [0001] The invention relates to the technical field of biological science and medicine, in particular to a nano-spherical covalent organic framework and a preparation method and application thereof with controllable particle size. Background technique [0002] Nanospherical covalent organic frameworks (COFs) have attracted much attention due to their uniform spherical morphology, multiscale particle size, and mesoporous microenvironment, making them excellent candidates for applications in numerous fields ranging from energy to biomedicine. However, their optimal synthesis and chemical modification often involves a lengthy multi-step sequence, with individual steps controlling particle size and surface properties. The current synthesis of uniform COF spheres is generally based on empirical screening of seed growth methods and reaction conditions, and acetic acid (HAc) has been shown to regulate the growth rate and provide size-controlled conditions for the fo...

Claims

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Application Information

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IPC IPC(8): C08G83/00A61P25/28B82Y5/00B82Y40/00
CPCC08G83/008A61P25/28B82Y5/00B82Y40/00
Inventor 汪航行毛樊高凯翔
Owner HUBEI UNIV
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