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Method for preparing nano cerium sulfide by adopting liquid phase method

A technology of cerium sulfide and liquid phase method, which is applied in the field of preparation of nano-red cerium sulfide, can solve the problems of high toxicity of hydrogen sulfide gas, coarse cerium sulfide particles, low coloring rate, etc. Good uniformity and dispersion

Inactive Publication Date: 2017-02-22
湖南科莱新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The cerium sulfide synthesized by the solid phase method has coarse particles and low coloring rate; hydrogen sulfide gas is very toxic, not environmentally friendly, and it is difficult to react completely

Method used

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  • Method for preparing nano cerium sulfide by adopting liquid phase method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Weigh 50g of mica powder (10-50 microns) at room temperature and dissolve in 1000ml of deionized water, stir evenly to make a bottom solution; add 246g of cerium chloride (CeCl 3 ), 18g sodium sulfide (Na 2 S), heated in a water bath at 90°C, added dropwise sodium carbonate solution (10wt%) to control the pH value to 10, and vigorously stirred (2000rpm) for 2h to generate a sol. The sol was filtered, washed 3 times with absolute ethanol, put into a 90° C. 4 SCN) mixed evenly, then put into the vacuum furnace, evacuate, heat up to 800°C at a rate of 10°C / min (if the heating rate is too fast, the grains will grow thicker, and if the heating rate is too slow, the production cycle will be lengthened), keep warm for 2 hours, and cool naturally After crushing, Na-doped cerium sulfide can be obtained. Take 75g of the above-mentioned cerium sulfide and dissolve it in 500ml of absolute ethanol, add 40ml of ammonia water (32%), then add 3.5g of ammonium fluoride and 2g of PVP, ...

Embodiment 2

[0037] Weigh 40g of mica powder (10-50 microns) at room temperature and dissolve in 1000ml of deionized water, stir evenly to make a bottom solution; add 246g of cerium chloride (CeCl 3 ), 9g sodium sulfide (Na 2 S), 13g of calcium sulfide (CaS), heated in a water bath at 85°C, added dropwise a sodium carbonate solution (10wt%) to control the pH to 10, and vigorously stirred (2000rpm) for 2h to generate a sol. The sol was filtered, washed 3 times with absolute ethanol, put into a 90° C. 4 SCN) were mixed evenly, then put into a vacuum furnace, evacuated, heated to 850°C at a rate of 10°C / min, kept for 2h, cooled naturally, and pulverized to obtain Na and Ca-doped cerium sulfide. Take 75g of the above-mentioned cerium sulfide and dissolve it in 500ml of absolute ethanol, add 41ml of ammonia water (32%), then add 3.5g of ammonium fluoride and 2g of PVP, and stir at room temperature for 2h; dissolve 7.5g of zinc oxide in 500ml of absolute ethanol, add to the above solution, and...

Embodiment 3

[0041] Weigh 50g of mica powder (10-50 microns) at room temperature and dissolve in 1000ml of deionized water, stir evenly to make a bottom solution; add 246g of cerium chloride (CeCl 3 ), 18g sodium sulfide (Na 2 S), heated in a water bath at 90°C, added dropwise sodium carbonate solution (10wt%) to control the pH value to 10, and vigorously stirred (2000rpm) for 2h to generate a sol. The sol was filtered, washed 3 times with absolute ethanol, put into a 100°C oven for drying, took out after cooling and mixed with 85g ammonium thiocyanate (NH 4 SCN) were mixed evenly, then put into a vacuum furnace, evacuated, heated up to 900°C at a rate of 10°C / min, kept for 2h, cooled naturally, and pulverized to obtain Na-doped cerium sulfide. Take 75g of the above-mentioned cerium sulfide and dissolve it in 500ml of absolute ethanol, add 42ml of ammonia water (32%), then add 3.5g of ammonium fluoride and 2g of PVP, and stir at room temperature for 2h; dissolve 7.5g of zinc oxide in 500m...

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Abstract

The invention relates to a method for preparing nano cerium sulfide by adopting a liquid phase method. The method comprises the following steps that a water-soluble trivalent cerium salt and a water-soluble sulfide reacts in a base solution to generate sol, and then filtration and drying are performed, wherein the base solution is prepared from mica powder and water; the obtained product and ammonium thiocyanate are uniformly mixed, and calcination is performed at the temperature of 800-1000 DEG C; then fluoridation treatment is performed by using an affiliative fluorinating agent. The prepared nano cerium sulfide (gamma-Ce2S3) product is bright in color and strong in tinting strength, the tinting strength can be up to 85% of the tinting strength of a cadmium red pigment and is greatly better than iron oxide red, molybdate red, manganese red and other inorganic red pigment. The covering power can be up to the level of the cadmium-based red pigment, the particle size is uniform, the dispersibility is good, and temperature resistance and corrosion resistance are good.

Description

technical field [0001] The invention belongs to the technical field of synthesis of nano-rare earth materials, in particular to a nano-red cerium sulfide (γ-Ce 2 S 3 ) preparation method. Background technique [0002] Red pigments are usually divided into two categories: organic red pigments and inorganic red pigments. Organic red pigments have bright luster and strong tinting power, but their hiding power, heat resistance, light resistance and weather resistance are quite different from those of inorganic red pigments. [0003] Most of the currently used inorganic red pigments contain cadmium, lead, mercury and other heavy metal elements that are extremely harmful to the human body, and their application range is increasingly restricted by relevant regulations. [0004] Due to the growing environmental awareness of human beings, many countries have formulated strict regulations in recent years to restrict or prohibit the use of toxic pigments that pollute the environment...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
CPCC01F17/288C01P2002/72C01P2004/62
Inventor 张家松
Owner 湖南科莱新材料有限公司
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