Preparation method of binaphthyl-based network type polyimide resin and film and application of binaphthyl-based network type polyimide resin and film in gas separation

A technology of polyimide resin and binaphthalene, which is applied in the field of synthesis and film preparation, can solve the problems of difficult to meet the requirements of gas separation, difficult to control the pore size of polymer micropores, etc., and achieve excellent gas permeability and selectivity, The effect of preventing physical collapse of pores and high specific surface area

Active Publication Date: 2020-07-03
TIANJIN UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0008] The purpose of the present invention is to solve the problem that existing gas separation membrane materials are not easy to effectively regulate the pore size and distribution of polymers, and it is difficult to meet the actual gas separation requirements. It provides a binaphthyl network polyimide resin and Preparation method of thin film and its application in gas separation
The present invention also proposes a method for preparing a network-type polyimide resin film, which solves the problem of network-type polyimide resin film formation, and the polyimide film effectively improves the gas separation performance

Method used

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  • Preparation method of binaphthyl-based network type polyimide resin and film and application of binaphthyl-based network type polyimide resin and film in gas separation
  • Preparation method of binaphthyl-based network type polyimide resin and film and application of binaphthyl-based network type polyimide resin and film in gas separation
  • Preparation method of binaphthyl-based network type polyimide resin and film and application of binaphthyl-based network type polyimide resin and film in gas separation

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preparation example Construction

[0032] The preparation method of the gas separation membrane of the present invention mainly comprises the following steps: the preparation of the binaphthyl tetramine monomer, the preparation of the binaphthyl network polyamic acid resin and the binaphthyl network polyimide resin Film preparation. Concrete preparation steps are as follows:

[0033] (1) Preparation of 7,7'-dinitro-1,1'-binaphthol (compound 1)

[0034] Prepare a single-necked round bottom flask, add a certain amount of acetic acid and 1,1'-binaphthol, and stir vigorously for 10 minutes. Then fuming nitric acid (98%) was slowly added dropwise to the reaction solution, stirred at room temperature for 1 h, during which the color of the solution changed from white to black, and finally to green. The mixture was poured into ice water and stirred for 10 min, filtered and dried to obtain compound 1.

[0035] (2) Preparation of tetranitrobinaphthalene (compound 2)

[0036] Compound 1, K 2 CO 3 and anhydrous DMF w...

Embodiment 1

[0043] Embodiment 1: Preparation of binaphthyl network polyimide resin XS18

[0044] (1) Preparation of 7,7'-dinitro-1,1'-binaphthol (compound 1)

[0045] Add 1,1'-binaphthol (1.0g, 3.49mmol) and acetic acid (15mL) into a 25ml single-necked round bottom flask, stir at room temperature for 10min, then slowly add fuming nitric acid dropwise to the solution at 0°C (98%, 0.62 mL, 15.24 mmol). The resulting mixture was then stirred at room temperature for 1 h, during which time the solution color changed from white to black and finally green. The mixture was poured into ice water (500ml) and stirred for 10min, filtered and dried to obtain a green powder (compound 1) with a yield of 78%.

[0046] (2) Preparation of tetranitrobinaphthalene (compound 2)

[0047] Add compound 1 (7.00g, 18.61mmol), K 2 CO 3 (3.85 g, 27.92 mmol) and anhydrous DMF (200 mL), stirred at room temperature for 30 minutes until a homogeneous solution was obtained. 2-Chloro-5-nitrobenzotrifluoride (8.79 g,...

Embodiment 2

[0052] Example 2: Preparation of Bininaphthyl Network Polyimide Resin XS19

[0053] (1) Preparation of 7,7'-dinitro-1,1'-binaphthol (compound 1)

[0054] Add 1,1'-binaphthol (1.0g, 3.49mmol) and acetic acid (15mL) into a 25ml single-necked round bottom flask, stir at room temperature for 10min, then slowly add fuming nitric acid dropwise to the solution at 0°C (98%, 0.62 mL, 15.24 mmol). The resulting mixture was then stirred at room temperature for 1 h, during which time the solution color changed from white to black and finally green. The mixture was poured into ice water (500ml) and stirred for 10min, filtered and dried to obtain a green powder (compound 1) with a yield of 78%.

[0055] (2) Preparation of tetranitrobinaphthalene (compound 2)

[0056] Add compound 1 (7.00g, 18.61mmol), K 2 CO 3 (3.85 g, 27.92 mmol) and anhydrous DMF (200 mL), stirred at room temperature for 30 minutes until a homogeneous solution was obtained. 2-Chloro-5-nitrobenzotrifluoride (8.79 g, ...

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Abstract

The invention provides a preparation method of a binaphthyl-based network type polyimide resin and a film and an application of the binaphthyl-based network type polyimide resin and the film in gas separation. The binaphthyl-based network type polyimide resin and the film are mainly used for separation and purification of small molecular gases such as H2, O2, CO2, N2 and CH4. The polyimide acid resin is prepared by taking 1,1'-binaphthol as a raw material, nitrifying to generate 7,7'-dinitro-1,1'-binaphthol, performing etherification reaction on the 7,7'-dinitro-1,1 '-binaphthol and 2-chloro-5-nitrobenzotrifluoride under an alkaline condition, performing palladium carbon hydrogenation reduction to generate a tetramine compound, and performing polycondensation reaction with dianhydride at alow temperature. The polyamic acid resin can be prepared into a polyamic acid resin film simply and conveniently by adopting a solution processing method, and then the polyamic acid resin film is further heated for imidization, so that a polyimide film can be prepared. The obtained film can be used for gas separation and has good gas permeability and selectivity.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, relates to the synthesis of a binaphthyl network polyimide resin with excellent air permeability and selectivity, the preparation method and application of the film, and is suitable for H 2 Recovery, CO in natural gas 2 The removal of O in the air 2 enrichment and CO in flue gas 2 areas such as removal. Background technique [0002] With environmental pollution, energy and resource crisis, gas separation membrane technology has attracted international attention due to its excellent performance. This technology is a new type of green chemical separation technology that uses a specific gas separation membrane to separate and purify mixed gases. It belongs to a physical separation process without phase change. It has the advantages of simple process technology, low energy consumption, and high efficiency. It has been widely used in h 2 Recovery, CO in natural gas 2 The removal of O i...

Claims

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Application Information

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IPC IPC(8): C08G73/10C08L79/08C08J5/18B01D53/22C10L3/10C01B13/02
CPCC08G73/1071C08G73/1039C08G73/1007C08J5/18B01D53/228C10L3/104C01B13/0255C08J2379/08C01B2210/0028Y02P20/151
Inventor 薛松邓国雄骆江洲王一雷宗雪平
Owner TIANJIN UNIVERSITY OF TECHNOLOGY
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