Soluble poly (siloxane-co-imide) block copolymer film and preparation and application thereof

A technology of block copolymer and siloxane diamine is applied in the field of preparation of soluble polyblock copolymer film, which can solve the problems of inability to make a self-supporting film, low gas permeability selectivity, difficulty in ultra-thinning, etc. The effect of low, good permeability and strong solubility

Inactive Publication Date: 2021-06-01
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since the climax of gas separation membrane research was set off in the 1970s, almost all existing polymer materials that can be formed into membranes have faced common problems in gas separation: membranes with good gas permeability

Method used

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  • Soluble poly (siloxane-co-imide) block copolymer film and preparation and application thereof
  • Soluble poly (siloxane-co-imide) block copolymer film and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] A 100ml dry four-neck flask equipped with a mechanical stirrer, a thermometer, a nitrogen inlet and a water separator was placed in a constant temperature water bath. At room temperature, add 50ml of N-methylpyrrolidone under nitrogen protection, add 1.222g of 2,6-diaminotoluene (0.011mol) under mechanical stirring, stir until completely dissolved, then add dropwise amodimethicone ( Molecular weight 2500) 5.000g (0.002 mol), after all dissolved, add bisphenol A dianhydride 6.763g (0.013 mol) in three times. React at 20°C for 4-24 hours to obtain a polyamic acid solution; then add 6.636 g (0.065 moles) of acetic anhydride and 6.577 g (0.065 moles) of triethylamine for chemical imidization, and react for 10-24 hours at room temperature to polymerize The product was settled in anhydrous methanol, washed three times with anhydrous methanol, air-dried at room temperature for 1 hour, and then dried in a vacuum oven at 100-250°C for 24-48 hours to remove residual moisture and ...

Embodiment 2

[0039] A 100ml dry four-neck flask equipped with a mechanical stirrer, a thermometer, a nitrogen inlet and a water separator was placed in a constant temperature water bath. At room temperature, add 50 ml of N-methylpyrrolidone under nitrogen protection, add 1.667 g of 2,6-diaminotoluene (0.0136 moles) under mechanical stirring, stir until completely dissolved, then add dropwise amino-terminated polydimethylsiloxane ( Molecular weight 2500) 2.500g (0.001 mole), after all dissolved, add bisphenol A dianhydride 7.647g (0.0147 mole) in three times. React at 20°C for 4-24 hours to obtain a polyamic acid solution; then add 7.453 g (0.073 moles) of acetic anhydride and 7.387 g (0.073 moles) of triethylamine for chemical imidization, and react for 10-24 hours at room temperature to polymerize The product was settled in anhydrous methanol, washed three times with anhydrous methanol, air-dried at room temperature for 1 hour, and then dried in a vacuum oven at 100-250°C for 24-48 hours ...

Embodiment 3

[0043] A 100ml dry four-neck flask equipped with a mechanical stirrer, a thermometer, a nitrogen inlet and a water separator was placed in a constant temperature water bath. At room temperature, add 50 ml of N-methylpyrrolidone under nitrogen protection, add 1.875 g of 2,6-diaminotoluene (0.0154 moles) under mechanical stirring, stir until completely dissolved, then add dropwise amodimethicone ( Molecular weight 2500) 12.50g (0.005 mol), after all dissolved, add bisphenol A dianhydride 10.608g (0.0159 mol) in three times. React at 20°C for 4-24 hours to obtain a polyamic acid solution; then add 8.168g (0.08 moles) of acetic anhydride and 8.095g (0.08 moles) of triethylamine for chemical imidization, and react for 10-24 hours at room temperature to polymerize The product was settled in anhydrous methanol, washed three times with anhydrous methanol, air-dried at room temperature for 1 hour, and then dried in a vacuum oven at 100-250°C for 24-48 hours to remove residual moisture ...

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Abstract

The invention relates to a preparation method of a soluble poly (siloxane-co-imide) block copolymer for gas separation. The preparation method comprises the following steps: polymerizing diaminosiloxane, aromatic diamine and aromatic dianhydride monomers in an aprotic polar solvent, and carrying out chemical imidization to obtain the poly (siloxane-co-imide) block copolymer. The prepared poly (siloxane-co-imide) block copolymer has good solubility in an aprotic polar solvent, an asymmetric membrane is prepared by adopting a phase inversion technology, and after solidification in a solidification medium, post-treatment is performed to obtain the asymmetric flat membrane with a compact skin layer. Compared with other traditional polymer membrane materials, the soluble poly (siloxane-co-imide) block copolymer can be widely applied to separation of various gases, such as separation of oxygen/nitrogen in air, separation of nitrogen/hydrogen, separation of carbon dioxide and methane in a natural gas purification process and the like.

Description

technical field [0001] The invention relates to the technical field of polymer materials, in particular to the preparation of a soluble poly(siloxane-co-imide) block copolymer membrane and its application in the field of gas separation. Background technique [0002] The key to the membrane separation technology of gas mixture is the selection of membrane material. Since the climax of gas separation membrane research was set off in the 1970s, almost all existing polymer materials that can be formed into membranes have faced common problems in gas separation: membranes with good gas permeability have low selectivity; The same is true. However, the membrane materials required in the industry for separating gas mixtures should have high selectivity and high gas permeation rate at the same time, and it is also hoped that they can be easily processed into membranes. Aromatic polyimide has become a commercial membrane separation material because of its excellent heat resistance a...

Claims

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Application Information

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IPC IPC(8): B01D71/80B01D67/00B01D69/06B01D69/02B01D53/22
CPCB01D53/228B01D67/0011B01D67/0013B01D69/02B01D69/06B01D71/80B01D2325/023Y02C20/40
Inventor 王丽娜介兴明刘丹丹曹义鸣
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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