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High-molecular functional polymer with self-microporous structure and super-assembly preparation method of high-molecular functional polymer

A technology of high molecular function and microporous structure, which is applied in the field of preparation of high molecular functional polymers and their super-assembly, can solve the problems of few types and single preparation methods, and achieve few preparation steps, simple operation and good π-conjugation structure effect

Inactive Publication Date: 2021-02-05
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although high-molecular-functional polymers with self-microporous structures have great application potential in the membrane separation of some high-energy-consuming gases and organic vapors, there are few known types of high-molecular-functional polymers with self-microporous structures. , single preparation method and other defects

Method used

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  • High-molecular functional polymer with self-microporous structure and super-assembly preparation method of high-molecular functional polymer
  • High-molecular functional polymer with self-microporous structure and super-assembly preparation method of high-molecular functional polymer
  • High-molecular functional polymer with self-microporous structure and super-assembly preparation method of high-molecular functional polymer

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Experimental program
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preparation example Construction

[0023] The above polymer functional polymer SBIDI is prepared by the following super-assembly preparation method, which specifically includes the following steps:

[0024] Step 1, under nitrogen protection, 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetraalkyl-1,1'-spirobisindene and 2,3,5 , 6-Tetrafluoroterephthalonitrile is added to the organic solvent at a molar ratio of 1.0:(0.8-1.2), and then an organic base or an inorganic base is added to obtain a mixed solution. Among them, the organic solvent is 1,4-dioxane, toluene, xylene, N,N-dimethylacetamide (DMAc), butyl acetate, dimethylsulfoxide (DMSO), N-methylpyrrolidone ( One or more of NMP). The organic base or inorganic base is piperidine, potassium tert-butoxide (t-BuOK), triethylenediamine (DABCO), 1,8-diazabicycloundec-7-ene (DBU), sodium carbonate one or more of .

[0025] Step 2, after replacing the mixed solution with nitrogen three times, react at a predetermined temperature for a predetermined time, and cool to room temp...

Embodiment 1

[0029] The preparation reaction formula of the macromolecule functional polymer SBIDI with self-microporous structure in embodiment one is as follows:

[0030]

[0031] Its specific super-assembly preparation method includes the following steps:

[0032] Step 1, under the protection of nitrogen, 3.4g (10.0mmol) of 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethyl-1,1'-spirobis Add indene (1a in the reaction formula) and 2.0g (10.0mmol) of 2,3,5,6-tetrafluoroterephthalonitrile (2 in the reaction formula) to a 100mL three-necked reaction flask, and then add 1, 20 mL of 4-dioxane was added, and 4.3 g (50.0 mmol) of piperidine was added to obtain a mixed solution.

[0033] Step 2: After the above mixed solution was replaced with nitrogen three times, the reaction system was reacted at 40° C. for 72 hours, and cooled to room temperature to obtain a reaction solution.

[0034] Step 3: filter the reaction solution under reduced pressure to remove the solvent 1,4-dioxane, and rinse th...

Embodiment 2

[0036] The preparation reaction formula of the macromolecule functional polymer SBIDI with self-microporous structure in embodiment two is as follows:

[0037]

[0038] Its specific super-assembly preparation method includes the following steps:

[0039]Step 1, under the protection of nitrogen, 6.8g (20.0mmol) of 5,5',6,6'-tetrahydroxy-3,3,3',3'-tetramethyl-1,1'-spirobis Add indene (1a) and 4.0g (20.0mmol) 2,3,5,6-tetrafluoroterephthalonitrile (2) into a 250mL three-necked reaction flask, then add 40mL of dried toluene, and then add 6.7g ( 60.0mmol) of t-BuOK to obtain a mixed solution.

[0040] Step 2: After the above mixed solution was replaced with nitrogen three times, the reaction system was reacted at 80° C. for 24 hours, and cooled to room temperature to obtain a reaction solution.

[0041] Step 3: filter the reaction solution under reduced pressure to remove the solvent toluene, and rinse the filter cake with ethanol (20 mL×1 time). Then the yellow filter cake wa...

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Abstract

The invention provides a high-molecular functional polymer with a self-microporous structure and a super-assembly preparation method thereof, and the method comprises the following steps: step 1, adding 5, 5', 6, 6'-tetrahydroxy 3, 3, 3', 3'-tetraalkyl-1, 1'-spirobisindene and 2, 3, 5, 6-tetrafluoroterephthalonitrile into an organic solvent, and then adding an organic base or an inorganic base toobtain a mixed solution; step 2, reacting the mixed solution at a preset temperature for a preset time, and cooling to obtain a reaction solution; and step 3, sequentially filtering, washing, filtering and drying the reaction solution to obtain the high-molecular functional polymer with the self-microporous structure. The method has the advantages of few preparation steps, large number of bonds, simplicity in operation and easiness in separation and purification of the product. The high-molecular functional polymer has the following advantages: the high-molecular functional polymer has a goodpi conjugated structure and good solubility and stability; and the compound has a cyano functional group and is expected to be further modified and functionalized.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a high molecular functional polymer with self-microporous structure and a super-assembly preparation method thereof. Background technique [0002] High molecular functional polymers with self-microporous structure are a special class of polymers with very high specific surface area (S BET >200m 2 / g). Due to the distorted structure of molecules in three-dimensional space, the polymer will produce a large number of micropores (the size of the pores is generally below 3nm), which provides a very good channel for material transmission. [0003] In 2004 (Chem.Commun., 2004, 230-231; Adv.Mater., 2004, 16, 456-459.) the Mckeown and Budd research team of the University of Manchester reported a new type of self-polymerizing microporous polymer (PIM 1-6), wherein the specific surface area of ​​PIM 1 is as high as 800m 2 / g or more, the oxygen transmission rate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/40
CPCC08G65/40
Inventor 孔彪李继超李勇高翔杨波
Owner FUDAN UNIV