Preparation method of oxidation-modified thermal cracking carbon black

A technology of thermal cracking carbon black and oxidative modification, applied in the direction of fibrous fillers, etc., can solve the problems of poor effect of oxidatively modified thermal cracking carbon black, difficult oxidative modification, etc., and achieves low cost, improved adsorption capacity, and high reactivity. improved effect

Active Publication Date: 2014-07-16
BEIJING UNIV OF CHEM TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It is precisely because of the particularity of the thermal cracking carbon black structure that the oxidant is not easy to penetrate into the interior of the carbon black particles, making oxidation modification relatively difficult or oxidation only occurs on the surface of the carbon black, resulting in a poor effect of oxidation modification thermal cracking carbon black

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  • Preparation method of oxidation-modified thermal cracking carbon black
  • Preparation method of oxidation-modified thermal cracking carbon black
  • Preparation method of oxidation-modified thermal cracking carbon black

Examples

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Effect test

Embodiment 1

[0023] (1) Calcination of carbon black: Take 5g of thermal cracking carbon black N990, place it in a muffle furnace, calcinate at 600°C for 11h, and cool to room temperature.

[0024] (2) Oxidation of carbon black: 2.5g of the above carbon black, 5g of NaNO 3 with 150ml concentrated H 2 SO 4 (Mass concentration is 98%, the same below) mixed in a three-necked flask, stirred evenly and then filtered under reduced pressure for 30min, and added 15g KMnO to the three-necked flask in 5 times within 1h 4 During this period, the temperature in the flask was controlled at 0°C to 5°C, and then the reaction temperature was raised to 35°C, kept for 6 hours, and then 200ml of deionized water was added to control the heating rate, during which the reaction temperature in the flask was guaranteed to be lower than 100°C, and then the temperature was raised to 90℃~100℃ and keep for 20min. After stopping the heating, add 700ml of deionized water to the three-necked flask, and add hydrogen pe...

Embodiment 2

[0028] (1) Calcination of carbon black: Take 5g of thermal cracking carbon black N990, put it in a muffle furnace, calcinate at 900°C for 6.5h, and then cool to room temperature.

[0029] (2) Oxidation of carbon black: 2.5g of the above carbon black, 1g of NaNO 3 with 100ml concentrated H 2 SO 4 Mix in a three-necked flask, stir evenly, and perform vacuum filtration for 10 minutes. Within 1 hour, add 3 g of KMnO to the three-necked flask 4 During this period, the temperature in the flask is controlled at 0°C to 5°C, then the reaction temperature is raised to 20°C, and kept for 1 hour, then 100ml of deionized water is added to control the heating rate, during which the reaction temperature in the flask is guaranteed to be lower than 100°C, and then the temperature is raised to 90℃~100℃ and keep for 10min. After stopping the heating, add 500ml deionized water to the three-necked flask, and add 30% hydrogen peroxide to make the solution turn bright yellow. The above solution ...

Embodiment 3

[0033] (1) Calcination of carbon black: Take 10 g of thermal cracking carbon black N990, put it in a muffle furnace, calcinate at 1000°C for 4 hours, and cool to room temperature.

[0034] (2) Oxidation of carbon black: 2.5g of the above carbon black, 3g of NaNO 3 with 200ml concentrated H 2 SO 4 Mix in a three-necked flask, stir evenly and carry out vacuum filtration for 60min, add 9g KMnO to the three-necked flask in 3 times within 1h 4During the period, the temperature in the flask was controlled at 0°C to 5°C, and then the reaction temperature was raised to 50°C, kept for 10 hours, and then 300ml of deionized water was added to control the heating rate, during which the reaction temperature in the flask was guaranteed to be lower than 100°C, and then the temperature was raised to 90℃~100℃ and keep for 60min. After stopping the heating, add 1000ml deionized water to the three-necked flask, and add 30% hydrogen peroxide to make the solution turn bright yellow. The above ...

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Abstract

The invention discloses a preparation method of oxidation-modified thermal cracking carbon black, belonging to the technical field of carbon material preparation. The preparation method comprises the following steps: with thermal cracking carbon black as a raw material, calcining at high temperature; carrying out carbon black oxidization by taking KMnO4, NaNO3 and concentrated H2SO4 as oxidants; carrying out suction filtration at reduced pressure on the reaction system before oxidation reaction; and then carrying out posttreatment on the oxidized carbon black by using ultrasonic or cell disruption. According to the preparation method, graphene microcrystals are peeled from the surface of the carbon black by controlling the calcining time, the calcining temperature, oxidation conditions and the like to destroy the regularity degree of the graph microcrystals on the surface of the thermal cracking carbon black, and thus the reaction activity and the adsorption capability of the thermal cracking carbon black are improved.

Description

technical field [0001] The invention belongs to the technical field of carbon materials, and relates to a method for oxidatively modifying thermal cracking carbon black. Background technique [0002] As a carbon material, carbon black is one of the most traditional and important fillers in the rubber industry. It is the second rubber raw material after raw rubber. It has the functions of reinforcing rubber, coloring, conductivity, antistatic, and ultraviolet absorption. . Thermal cracking carbon black is produced by pyrolysis of natural gas isolated from air and heated to 1300 ° C. It is composed of a large number of spherical and elliptical carbons and a small amount of welded particles. It has the characteristics of large particle size, small specific surface area, and low structure. [0003] The graphite layer plane of thermal cracking carbon black is very orderly, there is no reaction site to react with the elastomer, and the surface hardly contains oxygen-containing fu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09C1/56
Inventor 刘力赵泽丽吕晓茵
Owner BEIJING UNIV OF CHEM TECH
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