Method of preparing titanium nitride-coated carbon black material through alkoxide hydrolysis

A technology for coating carbon black and titanium nitride with titanium nitride is applied in chemical instruments and methods, fibrous fillers, inorganic pigment treatment, etc. Improve chemical stability and thermal stability, improve thermal stability, good effect of purity

Active Publication Date: 2016-06-15
HEFEI GENIUS NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, silicon dioxide cannot form a dense film layer on the surface of carbon black, so it cannot greatly improve the thermal stability of carbon black materials.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Mix 5mL methoxyethanol and 6mL tetraisopropyl titanate with 160mL anhydrous isopropanol and 3mL distilled water, and then reflux the mixture at 80°C for 4 hours to hydrolyze to form TiO particles 2 ;

[0023] (2) Put 15g of carbon black with a particle size of 35nm into the above solution; adjust the pH value to about 7 with a small amount of ammonia water, gradually heat to 80°C and reflux for 3 hours, and the TiO produced by hydrolysis 2 Depositing carbon black particles coated with titanium dioxide on the surface of carbon black;

[0024] (3) The titanium dioxide-coated carbon black particles prepared above were centrifugally filtered, washed 5 times with ethanol, and dried at room temperature for 6 hours;

[0025] (4) Nitriding the dry titanium dioxide-coated carbon black particles at 900°C, using ammonia gas as the reducing agent, and the nitriding time is 3 hours, and the titanium nitride-coated particles coated with titanium nitride on the surface can be obt...

Embodiment 2

[0027] (1) Add 5mL of methoxyethanol and 6mL of tetraisopropyl titanate to 120mL of anhydrous isopropanol and 5mL of distilled water for mixing, and then reflux the mixed solution at 85°C for 3 hours to hydrolyze to generate granular TiO 2 ;

[0028] (2) Put 8g of carbon black with a particle size of 50nm into the above solution; adjust the pH value to about 7 with a small amount of ammonia water, gradually heat to 80°C and reflux for 2.5 hours, and the TiO2 generated by hydrolysis is deposited on the surface of the carbon black to obtain a titanium dioxide coating. Coated carbon black particles;

[0029] (3) The titanium dioxide-coated carbon black particles prepared above were centrifuged and washed with ethanol for 3 times, and dried at room temperature for 4 hours;

[0030] (4) Nitriding the dry titanium dioxide-coated carbon black particles at 850°C, using ammonia gas as a reducing agent, and the nitriding time is 4 hours, and the titanium nitride-coated particles coated...

Embodiment 3

[0032] (1) For every 5mL of methoxyethanol and 4mL of tetraisopropyl titanate, add 180mL of anhydrous isopropanol and 10mL of distilled water for mixing, and then reflux the mixed solution at 70°C for 2 hours to hydrolyze to form TiO particles 2 ;

[0033] (2) Take 25g of carbon black with a particle size of 15nm and put it into the above solution; adjust the pH value to about 7 with a small amount of ammonia water, gradually heat to 80°C and reflux for 2 hours, and the TiO2 generated by hydrolysis is deposited on the surface of the carbon black to obtain titanium dioxide coating carbon black particles;

[0034] (3) The titanium dioxide-coated carbon black particles prepared above were centrifuged and washed with ethanol for 8 times, and dried at room temperature for 8 hours;

[0035] (4) Nitriding the dry titanium dioxide-coated carbon black particles at 800°C, using ammonia gas as the reducing agent, and the nitriding time is 2 hours, and the titanium nitride-coated particl...

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PUM

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Abstract

The invention provides a method of preparing a titanium nitride-coated carbon black material through alkoxide hydrolysis. The method includes the following steps: (1) adding methoxyl ethanol and tetraisopropyl titanate into anhydrous isopropyl alcohol and distilled water, mixing the components and performing a reflux reaction; (2) adding the carbon black, regulating the pH value to neutralization, and performing the reflux reaction for 2-4 h; (3) centrifugally filtering, washing and drying a product to obtain TiO2-coated carbon black particles; and (4) performing nitridation for 2-5 h by feeding ammonia gas at 800-1000 DEG C to prepare the titanium nitride-coated carbon black material, of which the surface is coated by the titanium nitride. In the method, firstly the carbon black is coated by the TiO2 to form the TiO2-coated carbon black material to improve chemical stability, and then the outer surface of the carbon black is coated by the titanium nitride, thereby greatly improving the thermal stabilities of the carbon black and the titanium nitride, so that the titanium nitride-coated carbon black material has excellent stability even at more than 1000 DEG C.

Description

technical field [0001] The invention belongs to the technical field of inorganic material modification, and in particular relates to a method for preparing a titanium nitride-coated carbon black material by an alkoxide hydrolysis method. Background technique [0002] Black is an important color of ceramic products. Most of the black pigments commonly used in ceramics are spinel structures. Among them, cobalt oxide is an important part of obtaining black ceramics. However, its high price limits the wide application of black ceramics. [0003] At present, the best material to replace cobalt oxide is carbon black. Carbon black has high coloring ability, but carbon black itself will oxidize and fail at 500-600°C. Therefore, if carbon black is used in ceramic pigments, it must be treated first. It is coated to increase its thermal stability. At present, silica is often used to coat carbon black materials, which can stably increase its initial oxidation temperature to above 600...

Claims

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Application Information

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IPC IPC(8): C09C1/48C09C3/06C04B41/86
Inventor 杨桂生计娉婷
Owner HEFEI GENIUS NEW MATERIALS
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