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Method for preparing polyoxyethylene-introduced cross-linked modified polyimide gas separation membrane

A technology of gas separation membrane and polyimide, applied in semipermeable membrane separation, chemical instruments and methods, membrane technology, etc., can solve the problems of difficult to improve gas separation performance and decrease of polymer sieving ability, and achieve excellent CO2 gas separation performance, effect of separation performance improvement

Inactive Publication Date: 2010-06-16
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
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Problems solved by technology

However, many feed gases such as raw natural gas contain CO with high partial pressure and high content 2 The plasticizing phenomenon caused by the gas can greatly reduce the sieving ability of the polymer, so it is sometimes difficult to improve the separation performance of the gas only by improving the sieving ability of the polymerization (increasing the diffusion selectivity), especially in the gas. Contains a lot of CO 2 and other acidic gases

Method used

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  • Method for preparing polyoxyethylene-introduced cross-linked modified polyimide gas separation membrane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 1g of Matrimid and 1.185g of two-terminal amino polyethylene glycol molecular weight (2000) and add them to about 5g of THF respectively. After the two solutions are completely dissolved, mix and stir for 24 hours. The solution is cast on a flat plate and dried at 25°C. The film was placed in water for 2 days to remove unreacted cross-linking agent, and then baked in a vacuum oven at 100°C for 24 hours. The membrane was stored in a desiccator at room temperature, and the thickness of the obtained membrane was ~100 μm.

[0018] Test gas separation performance:

[0019] P CO2 = 59.2 Barrer

[0020] (1Barrer=10 -10 cm 3 (STP)cm / (cm 2 scmHg))

[0021] alpha CO2 / CH4 =17.6α CO2 / N2 =52.2α CO2 / H2 =5.9

Embodiment 2

[0023] Take 1g of Matrimid and 3.63g of two-terminal amino polyethylene glycol molecular weight (2000) and add them to about 10g of THF respectively. After the two solutions are completely dissolved, mix and stir for 24 hours. The film was placed in water for 2 days to remove unreacted cross-linking agent, and then baked in a vacuum oven at 100°C for 24 hours. The membrane was stored in a desiccator at room temperature, and the thickness of the obtained membrane was ~100 μm.

[0024] Test gas separation performance:

[0025] P CO2 = 115.2 Barrer

[0026] alpha CO2 / CH4 =16.9α CO2 / N2 =52.5α CO2 / H2 =7.3

Embodiment 3

[0028] Take 1g of Matrimid and 1.089g of two-terminal amino polyethylene glycol (molecular weight: 600) and add them to about 10g of THF respectively. After the two solutions are completely dissolved, mix and stir for 24 hours. The solution is cast on a flat plate and dried at 25°C. The film was placed in water for 2 days to remove unreacted cross-linking agent, and then baked in a vacuum oven at 100°C for 24 hours. The membrane was stored in a desiccator at room temperature, and the thickness of the obtained membrane was ~100 μm.

[0029] Test gas separation performance:

[0030] P CO2 = 1.47 Barrer

[0031] alpha CO2 / CH4 =23.18α CO2 / N2 =34.82α CO2 / H2 =0.65

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Abstract

The invention relates to polymer separation membrane technology, in particular to a method for preparing a polyoxyethylene-introduced cross-linked modified polyimide gas separation membrane. The method comprises the steps of: 1) performing a cross-linking reaction, namely dissolving polyimide and a cross-linking agent, namely polyether amine into a solvent respectively until a polymer and the cross-linking agent are completely dissolved, mixing two solutions, and then stirring the obtained solution for 5 to 30h to react; and 2) preparing a homogeneous membrane, namely dumping the solution on a polyethylene plate after a complete mixed reaction of the solution, performing drying and film formation at the temperature of between 25 and 60 DEG C, placing the obtained homogeneous membrane into water for 1 to 5 days to remove the unreacted cross-linking agent in the homogeneous membrane, and then placing the membrane into a vacuum baking oven to bake at the temperature of between 50 and 120 DEG C for 5 to 24h, wherein the obtained membrane thickness is between 50 and 150mu m. The method uses the special cross-linking agent, namely the polyether amine to perform comprehensive cross-linking modification on the polyimide, and obtains the homogeneous membrane with excellent CO2 gas separation performance.

Description

technical field [0001] The invention relates to polymer separation membrane technology, in particular to polyimide materials and polyether amine cross-linked modified membrane materials and a preparation method for a homogeneous membrane. The prepared homogeneous membrane is cross-linked by polyoxyethylene The modified polyimide gas separation membrane contains ether oxygen functional groups and has a cross-linked structure. Background technique [0002] CO 2 The separation and removal of is a separation process with great potential and industrial prospects. Hydrogen is one of the main energy sources in the future; at present, the main source of hydrogen is through the reforming of alkanes and the reaction of hydration gas, which produces CO 2 impurity gas, in order to obtain pure hydrogen source, CO 2 The removal is very important. Natural gas is one of the main energy and chemical raw materials in the world in recent decades, and natural gas products often contain a la...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/64B01D71/76
Inventor 曹义鸣赵红永介兴明丁晓莉刘健辉周美青
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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