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Preparation method of rare earth sulfide compound

A rare earth sulfide and rare earth compound technology, applied in chemical instruments and methods, dyeing physical treatment, inorganic pigment treatment, etc. Brightness and tinting strength, lower reaction temperature, low cost effect

Active Publication Date: 2020-02-04
中科泽邦(青岛)新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

On the one hand, the grinding and crushing process will seriously damage the integrity of the rare earth sulfide grains, resulting in more defects on the surface of the particles and reducing the brightness of the material.
On the other hand, the particle size of the material obtained by grinding is uneven, and the particle shape is irregular, which seriously affects the coloring performance of the material.
Although the ground rare earth sulfide can also improve its coloring performance after being washed with fluoride ions, the fluorine washing process will bring about the problem of fluorine-containing wastewater treatment, which will increase the production cost.

Method used

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  • Preparation method of rare earth sulfide compound
  • Preparation method of rare earth sulfide compound
  • Preparation method of rare earth sulfide compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] Prepare the cerium sulfide composite as follows:

[0060] (1) Dissolve 0.02mol sodium fluoride, 0.010mol sodium carbonate and 1.0g PVP in 500ml deionized water and stir for 30min to obtain solution A1.

[0061] (2) Add 0.095 mol of 1000-mesh cerium carbonate and 0.4 mol of 500-mesh sulfur to solution A1, and stir for 60 minutes to obtain suspension B1.

[0062] (3) Set the nozzle temperature of the spray drying system to 120°C, and obtain C1 after the suspension B passes through the spray drying system.

[0063] (4) Put C in the corundum crucible A, then place the crucible in the large crucible B, put 400g of activated carbon particles around the crucible A, cover it, put it in a box-type electric furnace, and pass in nitrogen to drive out the furnace cavity air, heated to 700°C, and roasted for 150 minutes to obtain the primary product of cerium oxysulfide composite;

[0064] (5) Put the obtained primary product in a beaker, add 500ml of deionized water, stir for 60 ...

Embodiment 2

[0067] Prepare the cerium sulfide composite as follows:

[0068] (1) Dissolve 0.03mol of ammonium fluoride, 0.0015mol of sodium carbonate and 0.8g of PEG in 300ml of deionized water, and stir for 120min to obtain solution A2.

[0069] (2) Add 0.199 mol of 500-mesh cerium oxide and 0.40 mol of 1000-mesh sulfur to solution A2, and stir for 180 min to obtain suspension B2.

[0070] (3) Set the nozzle temperature of the spray drying system to 200° C., and obtain C2 after the suspension passes through the spray drying system.

[0071] (4) Put C2 in the corundum crucible A, then place the crucible in the large crucible B, put 600g of activated carbon particles around the crucible A, cover it, put it in a box-type electric furnace, and pass in argon to drive away the furnace cavity Inner air, heated up to 900°C, and roasted for 60 minutes to obtain the primary product of cerium oxysulfide composite;

[0072] (5) Put the obtained primary product in a beaker, add 300ml of deionized w...

Embodiment 3

[0075] Prepare the cerium sulfide composite as follows:

[0076] (1) Dissolve 0.01mol ammonium fluoride, 0.003mol sodium carbonate and 1.6g PVP in 400ml deionized water and stir for 90min to obtain solution A3.

[0077] (2) Add 0.099 mol of 800-mesh cerium carbonate and 1.0 mol of 800-mesh sulfur to solution A3, and stir for 90 minutes to obtain suspension B3.

[0078] (3) Set the nozzle temperature of the spray drying system to 150° C., and obtain C3 after the suspension B passes through the spray drying system.

[0079] (4) Put C3 in the corundum crucible A, then place the crucible in the large crucible B, put 500g of activated carbon powder around the crucible A, cover it, put it in the tube electric furnace, and let helium gas drive away the furnace cavity Inner air, heated up to 800°C, and roasted for 120 minutes to obtain the primary product of cerium sulfide composite;

[0080] (5) Put the obtained primary product in a beaker, add 500ml of deionized water, stir for 90...

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PUM

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Abstract

The invention relates to a preparation method of a rare earth sulfide compound. The preparation method comprises the following steps: (1) taking and uniformly mixing a soluble fluoride, a surfactant,a soluble alkaline sodium salt, a rare earth compound and sulfur in water to prepare a suspension A; (2) carrying out spray drying on the suspension A to obtain a product B; (3) calcining the productB in the presence of activated carbon and protective gas to obtain a primary product for the rare earth sulfide compound; and (4) washing the primary product for the rare earth sulfide compound with water, and drying the washed primary product to obtain the final product. The invention also relates to the rare earth sulfide compound prepared by the method, and an application of the rare earth sulfide compound as a coloring agent.

Description

technical field [0001] The invention relates to rare earth sulfides, in particular to a preparation method of a fluorine-containing rare earth sulfide compound, the rare earth sulfide compound prepared by the method and its use as a coloring agent. Background technique [0002] As a colorant, rare earth sulfides can replace the currently widely used organic pigments and pigments and other colorants that cannot meet environmental protection requirements due to their excellent coloring performance, non-toxic and harmless characteristics. Rare earth sulfides were included in the "List of Substitutes for Toxic and Hazardous Raw Materials Encouraged by the State" jointly promulgated by the Ministry of Science and Technology, the Ministry of Industry and Information Technology and the Ministry of Environmental Protection in 2016. [0003] The synthesis of rare earth sulfides can generally be prepared by using rare earth compounds as raw materials, hydrogen sulfide or carbon disulf...

Claims

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Application Information

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IPC IPC(8): C09C1/00C09C3/04C09C3/06
CPCC01P2004/61C01P2006/62C01P2006/63C01P2006/64C01P2006/65C09C1/00C09C3/006C09C3/043C09C3/06
Inventor 李成宇庞然张洪杰
Owner 中科泽邦(青岛)新材料有限公司
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