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Hollow organic microporous nanosphere cross-linked network and synthesis method and application thereof

A technology of cross-linked network and synthesis method, applied in the field of cross-linked network of hollow organic microporous nanospheres and its synthesis, can solve the problems of large size and uneven size distribution of COF spheres.

Active Publication Date: 2017-12-22
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the size of COF spheres synthesized by this method is large (0.5–4 μm) and the size distribution is not uniform

Method used

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  • Hollow organic microporous nanosphere cross-linked network and synthesis method and application thereof
  • Hollow organic microporous nanosphere cross-linked network and synthesis method and application thereof
  • Hollow organic microporous nanosphere cross-linked network and synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0104] The synthesis of embodiment 1 diblock copolymer (PLA-b-PS)

[0105] Firstly, polylactic acid was synthesized by ring-opening polymerization method, and then polylactic acid was modified with a chain transfer agent at the end, and finally polystyrene was connected by reversible addition-fragmentation chain transfer polymerization method to obtain a diblock copolymer PLA-b-PS.

[0106] Its synthesis process is shown in formula (VI):

[0107]

[0108] Wherein, n=150, m=250.

[0109] Specifically include the following steps:

[0110] (a-1) Synthesis of PLA

[0111] Benzyl alcohol (10 μl), D,L-lactide (1.3 g), and stannous octoate (19 mg) were added to the reaction tube, and the tube was sealed at 130° C. for 3 hours. After the reaction was completed, it was dissolved in 20 ml of dichloromethane, precipitated in methanol, collected and dissolved in dichloromethane, precipitated in methanol again, and repeated three times in sequence. The finally obtained white product...

Embodiment 2

[0118] Example 2 Synthesis of Hollow Organic Microporous Nanosphere Crosslinked Network

[0119] Dissolve the two-block copolymer PLA-b-PS synthesized in Example 1 in carbon tetrachloride, then add a certain amount of anhydrous aluminum chloride, and place it in a closed container at 90°C for 24 hours. After the reaction, respectively The obtained solid was washed three times with a mixed solution of 95% ethanol and water (4:1) and methanol, and finally vacuum-dried at room temperature for 24 hours to obtain the hollow organic microporous nanosphere cross-linked network. Specifically include the following steps:

[0120] Diblock copolymer PLA-b-PS (700 mg) was dissolved in 7 ml of carbon tetrachloride, and after complete dissolution, 2.5 g of anhydrous aluminum chloride was added. After stirring for 5 minutes, tighten the lid to close the reactor, move it into a 90°C oil bath, and let it stand for 24 hours to react. After the reaction solution is cooled to room temperature, ...

Embodiment 3

[0124] The synthesis of embodiment 3 different molecular weight diblock copolymers PLA-b-PS

[0125] (a) PLA 60 The synthesis of D, L-lactide, benzyl alcohol, and the molar ratio of stannous octoate are controlled in the ratio of 60:1:0.5, and the reaction time is 0.5 hour. Other reaction conditions are the same as in Example 1, and polymerization can be obtained Polylactic acid with a degree of 60.

[0126] (b) PLA 60 -b-PS 60 Synthesis of PLA 60 -TC, AIBN, the molar ratio of styrene is controlled in the ratio of 1:0.1:400, and the reaction time is 6 hours, and other reaction conditions are the same as embodiment 1, can obtain diblock copolymer PLA 60 -b-PS 60 .

[0127] (c) PLA 150 -b-PS 130 Synthesis of PLA 150 -TC, AIBN, the molar ratio of styrene is controlled in the ratio of 1:0.1:1000, and the reaction time is 7 hours, and other reaction conditions are the same as Example 1, can obtain diblock copolymer PLA 150 -b-PS 130 .

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Abstract

The invention discloses a diblock copolymer and a synthesis method thereof, wherein the diblock copolymer is synthesized through ring-opening polymerization and reversible addition-fragmentation chain transfer polymerization. The invention also discloses a synthesis method of a hollow organic microporous nanosphere cross-linked network from the diblock copolymer, and the hollow organic microporous nanosphere cross-linked network is prepared by Friedel-Crafts hyper-cross-linking reaction from the diblock copolymer under the action of a catalyst. The prepared cross-linked network is obtained by mutual crosslinking accumulation of hollow nanospheres as a structural unit; the spherical shells of the hollow nanospheres comprise super-cross-linked polystyrene; the diameter of the hollow nanosphere is 30 to 40 nm, the thickness is 6-7 nm; the specific surface area of the hollow organic microporous nanosphere cross-linked network is 582-806 m<2>g<-1>, the micropore area is 102-217 m<2>g<-1>, and the total pore volume is 0.77-1.28 m<3>g<-1>. The method has the advantages of simple operation, mild reaction conditions, no precious metal participation and low cost. The obtained hollow organic microporous nanosphere cross-linked network is controllable and uniform in size, and has a high specific surface area.

Description

technical field [0001] The invention belongs to the field of polymer synthesis and the field of porous polymer materials, and in particular relates to a crosslinked network of hollow organic microporous nanospheres and its synthesis method and application. Background technique [0002] Porous polymers have received increasing attention due to their good porosity, large specific surface area, and easy processability. In addition, stronger covalent bridging bonds endow porous polymers with higher chemical and thermal stability. Because of this, porous polymers can be used for gas storage and separation, as carriers for controlled release of drugs, as catalysts or catalyst carriers themselves, as carriers of small biological molecules or cells, filtration and separation membranes , proton exchange membranes, electrode materials for energy storage. [0003] However, the microstructure of porous polymers often determines their properties and applications. In other words, porou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F293/00C08G63/08C08J3/24C08G83/00B01J20/26B01J20/28B01J20/30B01D53/02
CPCB01D53/02B01D2257/504B01J20/264B01J20/267B01J20/28014C08F293/005C08G63/08C08G83/008C08J3/24C08J2353/00Y02C20/40Y02P20/151
Inventor 黄琨何紫东王天琪徐洋周铭洪
Owner EAST CHINA NORMAL UNIV
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