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Method for preparing dispersive type carbon black adopting surface graft modification method

A surface graft modification and dispersion technology, which is applied in the treatment of dyed polymer organic compounds, fibrous fillers, etc., can solve the problems of narrow application range, cumbersome steps, and many steps, and achieves wide application range and simple preparation process Effect

Inactive Publication Date: 2007-05-30
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

After introducing various initiating groups on the surface of carbon black, the initiating groups on the surface can initiate free radical polymerization, ring-opening polymerization, anionic polymerization and cationic polymerization of monomers. This method of grafting and modifying the surface of carbon black usually has cumbersome steps. , more stringent conditions
Graft modified carbon black is prepared by condensation reaction of functional groups on the surface of carbon black with polymers containing reactive end groups. This method of surface graft modified carbon black usually has many steps and has a narrow scope of application.

Method used

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  • Method for preparing dispersive type carbon black adopting surface graft modification method
  • Method for preparing dispersive type carbon black adopting surface graft modification method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1) Add 10mL of styrene (87.4mmol), 98.5mg of azobisisobutyronitrile (0.6mmol) and 103.8mg of HTEMPO (0.6mmol) into a 50ml three-necked flask. After deoxygenation, the reaction system is protected by argon and Under stirring, use an oil bath to heat, first react at 95°C for 1 hour, and then heat to 125°C to continue the reaction for 7 hours. After the reaction, the product is precipitated with ethanol, and finally dried in vacuum to obtain polystyrene with HTEMPO end groups.

[0038] 2) Add 50mg of carbon black, 5ml of N,N-dimethylformamide and 0.20g of polystyrene with HTEMPO end groups prepared into a 25ml two-necked flask. After deoxygenation, the reaction system is protected by argon. Under stirring, use an oil bath to heat and raise the temperature to 130°C for 24 hours. After the reaction, the obtained product is washed with tetrahydrofuran under ultrasound, and then centrifuged; the ultrasonic washing-centrifugal separation process is repeated 6 times, and finally the...

Embodiment 2

[0040] 1) Put 5mL styrene (43.7mmol), 0.4285g maleic anhydride (4.37mmol), 40mg benzoyl peroxide (0.165mmol) and 51.2mg HTEMPO (0.297mmol) into a 50ml three-necked flask, the reaction system After deoxygenation, under argon protection and stirring, use oil bath heating, first react at 100°C for 1 hour, and then heat to 125°C to continue the reaction for 7 hours. After the reaction, the product is precipitated with ethanol and finally dried in vacuum to obtain poly(styrene-co-maleic anhydride) with HTEMPO end groups.

[0041] 2) Add 50mg of carbon black, 5ml of N,N-dimethylformamide and 0.20g of poly(styrene-co-maleic anhydride) with HTEMPO end groups prepared into a 25ml two-necked flask, the reaction system is removed After oxygen, under argon protection and stirring, use an oil bath to heat, and raise the temperature to 130°C for 24 hours. After the reaction, the obtained product was washed with tetrahydrofuran under ultrasound, and then centrifuged; this ultrasound washing-cent...

Embodiment 3

[0043]1) Add 3mL 4-vinylpyridine (28.5mmol), 13.4mg benzoyl peroxide (0.0553mmol) and 12.4mg HTEMPO (0.0721mmol) into a 50ml three-necked flask. After deoxygenation, the reaction system is heated in argon. Under protection and stirring, use oil bath heating, first react at 100°C for 1 hour, and then heat to 125°C to continue the reaction for 7 hours. After the completion of the reaction, the product was precipitated with ether and finally dried under vacuum to obtain poly(4-vinylpyridine) with HTEMPO end groups.

[0044] 2) Add 50mg of carbon black, 5ml of N,N-dimethylformamide and 0.75g of poly(4-vinylpyridine) with HTEMPO end groups into a 25ml two-necked flask. After deoxygenation, the reaction system is protected under argon. Under stirring, use an oil bath to heat, and raise the temperature to 130°C to react for 12 hours. After the reaction, the obtained product was washed with N,N-dimethylformamide under ultrasound, and then centrifuged; this ultrasound washing-centrifugal s...

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Abstract

The invention discloses a making method of dispersing carbon black through surface grafting modifying method, which is characterized by the following: making a series of polymer with HTEMPO terminal group polymerized by controllable free radiacal; decomposing HTEMPO into polymer free radical under higher temperature; making non-paired electron on the surface of carbon black catch polymer free radical; obtaining the modified carbon black grafted by polymer; dispersing the modified carbon black in multiple organic solvents; applying in the PTC material, air-sensitive material and ink domain.

Description

Technical field [0001] The invention relates to a method for preparing dispersible carbon black by adopting a surface graft modification method. Background technique [0002] Carbon black is usually an aggregate of small carbon particles with a diameter of 10-400nm, mainly composed of carbon elements, with a carbon content of usually 90-99%, and a small amount of carboxyl groups, phenolic hydroxyl groups, quinone groups and lactone groups distributed on the surface And other functional groups. Carbon black has been widely used in the preparation of conductive composite materials, gas-sensitive materials, coatings and inks, and is an extremely important chemical raw material. A basic condition for carbon black to enter these systems is that carbon black can be well dispersed in these solvent systems or polymer systems. Generally, carbon black is difficult to disperse in these systems. Grafting modification on the surface of carbon black is one of the effective ways to improve the ...

Claims

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Application Information

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IPC IPC(8): C09C3/10C09C1/48C08F292/00
Inventor 杨强王立俞豪杰周峻峰
Owner ZHEJIANG UNIV
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