Process for modifying reaction at surface of separating film of polymer

A grafting reaction and separation membrane technology, applied in semi-permeable membrane separation, chemical instruments and methods, membrane technology, etc., can solve problems such as large application limitations, limited depth and degree of grafting, and limited separation membranes. Clean processing, easy control of grafting degree, good repeatability

Inactive Publication Date: 2005-06-08
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The traditional free radical reaction is difficult to meet the above conditions, and the application limitations are relatively large
Relying solely on the irradiation of UV, plasma or other high-energy rays, although free radicals can be generated on the surface of the membrane and undergo grafting reactions, this method is limited to the outer surface of the separation membrane, and the depth and degree of grafting are limited.

Method used

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  • Process for modifying reaction at surface of separating film of polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Fix the PVDF microporous membrane (flat membrane, 10 cm × 20 cm) on a support with a certain shape, and place it in 1000ml cylindrical supercritical CO 2 The reactor (φ68mm / 400mm) is airtight, and then the temperature is raised to 35°C, pressurized to 9MPa, pre-soaked for 0.5 hours, open the pressure reducing valve to slowly drain the CO 2 , For the next step of grafting reaction. Then in CO 2 Under the atmosphere, 50 g of a mixed monomer of styrene (St) and maleic anhydride (MAH) (molar ratio 1:1) and 0.28 g of azoisobutyronitrile (AIBN) were sequentially added to the reactor, and the reactor was sealed. Open CO 2 The intake valve is pressurized, and at the same time the temperature is raised to a supercritical state (temperature 60°C, pressure 7.38MPa), constant temperature and constant pressure reaction for 1 hour. Open the pressure reducing valve and slowly vent until the pressure in the reactor is zero. Take out the grafted modified membrane and soak it in acetone for ...

Embodiment 2

[0028] The operation is the same as in Example 1. The modified base film is changed to PAN microporous film, the graft comonomer is changed to 1.6g itaconic anhydride (ITA), the initiator is changed to 0.03g benzoyl peroxide (BPO), and the reaction is closed. kettle. Open CO 2 The intake valve is pressurized, and the temperature is raised to a supercritical state (temperature 80°C, pressure 20MPa), and reacts at constant temperature and pressure for 10 hours. The grafted modified membrane was characterized by ATR-IR, XPS, elemental analysis and scanning electron microscopy, and the grafting rate was 6.8%.

Embodiment 3

[0030] Fix the PP dense non-porous membrane (flat membrane, 10 cm × 20 cm) on a support with a certain shape, and place it in supercritical CO 2Pre-soak in the reactor for 1 hour, and the operation is the same as in Example 1. Take out the PP microporous film, quickly put it into the plasma generator, adjust the vacuum to 20Pa under argon atmosphere, and irradiate 100W plasma for 10-20 minutes. After plasma irradiation The membrane is exposed to the air for 15 minutes, and then quickly moved into the supercritical CO 2 In the reactor; in CO 2 Under the atmosphere, 3.4 g of hydroxyethyl methacrylate monomer (HEMA) was sequentially added to the reaction kettle, and the reaction kettle was sealed. Open CO 2 The intake valve is pressurized, and the temperature is raised to a supercritical state (temperature 60°C, pressure 30MPa), and reacts at constant temperature and pressure for 4 hours. Open the pressure reducing valve and slowly exhaust until the pressure of the reactor is zero, t...

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Abstract

A process for modifying the surface of polymer separating membrane by graft reaction includes such steps as immersing the membrane to be modified in supercritical CO2, triggering by free radical trigger or peroxide radical generated by high-energy radiation, diffusing various functional free-radical monomers onto the external and internal surfaces of said membrane by supercritical CO2 fluid, and graft reaction at proper temp and under proper pressure.

Description

Technical field [0001] The invention relates to a graft reaction technology for surface modification of a polymer separation membrane material, in particular to a method for introducing functional molecules on the surface of a polymer separation membrane through a graft reaction. Background technique [0002] In recent decades, membrane separation technology as a separation, purification, concentration and purification technology with high efficiency, high selectivity, low energy consumption and low pollution, not only its technology itself has been developed rapidly, but also its application fields are also greatly improved. Expansion, especially in the fields of sewage treatment and reuse, food, biotechnology and clinical medicine, has shown a strong momentum of development. In the study of membrane separation technology, the core issue is the preparation of separation membranes with excellent performance. Due to the good processability and controllability of synthetic polymers...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/78
Inventor 徐又一邱广明朱宝库
Owner ZHEJIANG UNIV
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