Method for preparing self-dispersing nano carbon black based on a thiol-ene click reaction

Patent metadata

Field	Value
Publication number	US-10975245-B2
Application number	US-201816178299-A
Country	US
Kind code	B2
Filing date	Nov 1, 2018
Priority date	Dec 22, 2017
Publication date	Apr 13, 2021
Grant date	Apr 13, 2021

Abstract

Disclosed is a method for preparing self-dispersing nano carbon black based on a thiol-ene click reaction. A sol-gel technique is used to graft a coupling agent containing a carbon-carbon double bond onto the surface of the carbon black, and a functional molecular chain is grafted onto the surface of the carbon black by a thiol-ene click reaction with a mercapto compound. The self-dispersing nano carbon black is obtained after centrifugation, washing and drying. The method is simple and easy to operate, has a high grafting rate, and can prepare self-dispersing nano carbon black adaptable to different systems by selecting mercapto compounds with different functional groups.

First claim

What is claimed is:

1. A method for preparing a self-dispersing nano carbon black, comprising:
1) oxidatively modifying carbon black using a liquid phase oxidant to obtain an oxidized carbon black;
2) using a coupling reaction to obtain a modified carbon black containing a double bond on the surface, wherein the oxidized carbon black is dispersed into a coupling agent alcohol solution to a nanometer scale and react at 20-80° C., pH 8.5-9.0 adjusted by an alkaline agent, for 0.5-30 hr;
3) adding a functional group to the modified carbon black containing a double bond by a thiol-ene click reaction, wherein a mercapto compound is added to the modified carbon black containing a double bond, and an initiator is stepwisely added to initiate the thiol-ene click reaction; and
4) obtaining the self-dispersing nano carbon black after centrifugation, washing and drying.

2. The method of claim 1 , wherein the thiol-ene click reaction is performed at 50˜90° C. for 0.5 to 20 hours.

3. The method of claim 1 , wherein the oxidized carbon black is added in an amount of 0.1%-40% by mass of the coupling agent alcohol solution.

4. The method of claim 1 , wherein the alkaline agent is added in an amount of 0.1-10% by volume of the coupling agent alcohol solution.

5. The method of claim 1 , wherein the initiator is selected from the group consisting of potassium persulfate, ammonium persulfate, sodium persulfate, azobisisobutyronitrile, 2,2′-azobis(isobutyramidine) dihydrochloride, 2,2′-azobis[2-(2-imidazolin-2-yl)propane] dihydrochloride and benzoyl peroxide; and wherein the initiator is added in an amount of 0.5-15% by mass of the mercapto compound.

6. The method of claim 1 , wherein the coupling agent is selected from the group consisting of a silane coupling agent, a titanate coupling agent, an organic complexing coupling agent and an aluminate compound.

7. The method of claim 1 , wherein the liquid phase oxidant is a nitric acid solution, a hydrogen peroxide solution, a saturated ammonium persulfate solution, perchloric acid, a sodium hypochlorite aqueous solution, an isocyanate solution or a potassium permanganate solution.

Assignees

• Fu Shaohai
• Zhang Liping
• Wang Liangan
• Wang Chunxia
• Li Min
• Univ Jiangnan

Inventors

• Fu Shaohai
• Zhang Liping
• Wang Liangan
• Wang Chunxia
• Li Min

Classifications

• C09C3/08 Primary

  Treatment with low-molecular-weight {non-polymer} organic compounds {(C09C3/006, C09C3/048 take precedence)} · CPC title

• C09C1/56

  Treatment of carbon black {; Purification} · CPC title

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• C09C3/006

  Combinations of treatments provided for in groups C09C3/04 - C09C3/12 · CPC title

• C09C1/565 Primary

  comprising an oxidative treatment with oxygen, ozone or oxygenated compounds, e.g. when such treatment occurs in a region of the furnace next to the carbon black generating reaction zone · CPC title