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Preparation method of PVDF-PAA (polyvinylidene fluoride-polyacrylic acid) block copolymer

A polyvinylidene fluoride and block copolymer technology, which is applied in the field of preparation of polyvinylidene fluoride-polyacrylic acid block copolymers, can solve the problems of few reports on block copolymers, and can improve the polymerization reaction rate and improve the Stain resistance, improved hydrophilicity

Active Publication Date: 2015-05-13
JUHUA GROUP TECH CENT +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

PVDF block copolymers are mainly prepared by step-by-step living radical polymerization. Although there have been research reports on block copolymers of PVDF and polystyrene, PVDF and poly(meth)acrylates, but about PVDF and hydrophilic polymers There are few reports on the composition of block copolymers, and the synthesis of block copolymers of PVDF and polyacrylic acid and its application in the modification of PVDF porous membranes have not been reported.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a 5L reactor, add 2000 ml of water, 5.0 g of ammonium perfluorooctanoate, 20.0 g of n-hexadecanol, and 15.2 g of ICF 2 CF 2 I, 3.2g of VA-044, pass into N 2 Row O 2 When the content is lower than 5ppm, stir at a high speed for 10min at 5°C to obtain a fine emulsion; raise the temperature to 45 o C, feed VDF monomer until the pressure inside the tank is 3.0 MPa, and start polymerization. When the pressure in the kettle drops by 0.1MPa, add VDF monomer until the pressure in the kettle is 3.0MPa, and repeat the operation. When the cumulative monomer pressure drop reaches 4.0MPa, stop supplementing VDF monomer, continue polymerization until the pressure drops to 1.5MPa, cool to room temperature to end polymerization, remove unreacted VDF monomer, and obtain active PVDF seed emulsion.

[0024] Add 40g of acrylonitrile into the kettle, stir and disperse at room temperature, and swell for 2h. The temperature was raised to 45°C to continue the reaction for 5h and then s...

Embodiment 2

[0028] In a 5L reactor, add 2000 ml of water, 5.0 g of ammonium perfluorooctanoate, 10.0 g of n-hexadecane, and 58 g of C 6 F1 3 I, 3.2g of VA-044, pass into N 2 Row O 2 When the content is lower than 5ppm, stir at 5°C for 10 minutes at high speed to obtain a fine emulsion; heat up to 50 o C, feed VDF monomer until the pressure inside the tank is 3.0 MPa, and start polymerization. When the pressure in the kettle drops by 0.1MPa, add VDF monomer until the pressure in the kettle is 3.0MPa, and repeat the operation. When the cumulative monomer pressure drop reaches 6.3MPa, stop supplementing VDF monomer, continue polymerization until the pressure drops to 1.5MPa, cool to room temperature to end polymerization, remove unreacted VDF monomer, and obtain active PVDF seed emulsion.

[0029] Add 200g of acrylonitrile into the kettle, stir and disperse at room temperature, and swell for 5h. The temperature was raised to 50° C. to continue the reaction for 10 h and then stopped. Ce...

Embodiment 3

[0033] In a 5L reactor, add 2000 ml of water, 8.0 g of ammonium perfluorooctanoate, 15.0 g of n-hexadecane, and 29.0 g of C 4 f 9 I, 4.0g APS, pass into N 2 Row O 2 When the content is lower than 5ppm, stir at a high speed for 10min at 5°C to obtain a fine emulsion; heat up to 80 o C, feed VDF monomer until the pressure inside the tank is 3.0 MPa, and start polymerization. When the pressure in the kettle drops by 1.0MPa, add VDF monomer until the pressure in the kettle is 3.0MPa, and repeat the operation. When the cumulative monomer pressure drop reaches 5.8MPa, stop supplementing VDF monomer, continue polymerization until the pressure drops to 1.5MPa, cool to room temperature to end polymerization, remove unreacted VDF monomer, and obtain active PVDF seed emulsion.

[0034] Add 100g of acrylonitrile into the kettle, stir and disperse at room temperature, and swell for 2 hours. The temperature was raised to 80° C. to continue the reaction for 5 h and then stopped. Centri...

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PUM

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Abstract

The invention discloses a preparation method of a PVDF-PAA (polyvinylidene fluoride-polyacrylic acid) block copolymer. The method comprises steps as follows: firstly, preparing a PVDF seed emulsion through iodine transfer active free-radical miniemulsion polymerization, then adding acrylonitrile monomers to continue polymerization to obtain a PVDF-PAN (polyacrylonitrile) block copolymer, and finally, hydrolyzing the PVDF-PAN block copolymer under an alkaline condition to obtain the PVDF-PAA block copolymer. The method is simple in process, the molecular weight of PVDF and PAA blocks as well as components of the block copolymer are convenient to control, and the prepared PVDF-PAA block copolymer can be applied to preparation of porous PVDF membranes with excellent stain resistance and stable membrane flux for sewage treatment.

Description

technical field [0001] The invention belongs to the field of chemical engineering and technology, in particular to a preparation method of polyvinylidene fluoride-polyacrylic acid block copolymer. Background technique [0002] Polyvinylidene fluoride (PVDF) is a thermoplastic fluoropolymer, and its output is second only to polytetrafluoroethylene and ranks second in fluoropolymers. The fluorine content of PVDF is as high as 59wt%. Due to the strong electronegativity of fluorine atoms, the small atomic radius (1.32?), the large C-F bond energy (485KJ / mol), and the symmetrical substitution distribution of fluorine atoms, PVDF is semi-crystalline and heat-resistant. , Excellent weather resistance and chemical corrosion resistance, hydrophobic and oleophobic, low surface energy, small dielectric constant and so on. Therefore, PVDF is widely used in construction, aerospace, electronics, chemical industry, environmental protection, new energy and other industries. [0003] Memb...

Claims

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Application Information

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IPC IPC(8): C08F293/00C08F220/44C08F8/12C08F2/28
Inventor 包永忠黄志辉付铁柱汪星平余晓斌郑明华王树华
Owner JUHUA GROUP TECH CENT
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