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A kind of preparation method of rare earth sulfide

A technology of rare earth sulfide and zinc sulfide, applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of unfavorable synthesis of rare earth sulfide, influence on the application of rare earth sulfide, incomplete reaction, etc., and achieve good power The effects of chemical reaction conditions, easy recycling, and easy operation

Active Publication Date: 2017-01-04
内蒙古中科宏特高新科技有限责任公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

h 2 S is not an effective source of sulfur and is more toxic than CS 2 Bigger, less reductive than CS 2
In addition, H 2 The thermal decomposition effect of S at low temperature is unfavorable for the synthesis of rare earth sulfides, H 2 S reacts incompletely at high temperature or contains impurities, which are not easy to remove in the post-processing process, which seriously affects the application of rare earth sulfides

Method used

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  • A kind of preparation method of rare earth sulfide

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Effect test

Embodiment 1

[0049] Rare earth metal samarium and zinc sulfide are respectively subjected to vacuum heating and dehydration treatment: the vacuum degree is 0.03Mpa, the temperature is 500 °C, the heating rate is 3 °C / min, and the treatment time is 1 hour; after the rare earth metal samarium and zinc sulfide are uniformly mixed, set aside In a graphite-heated closed reactor-vacuum carbon tube furnace metal molybdenum crucible, according to the molar ratio of rare earth metals and sulfides of 1:1, start the cooling water circulation system, and vacuumize, the vacuum degree is 0.07Pa, and the heating rate is 15 ℃ / min, keep the temperature at 1000℃ for 3h, and keep the vacuum degree of 10~10 -3 Between the Pa range, high-purity argon with a purity of ≥99.99% is filled as the protective gas. After the synthesis reaction is completed, the temperature is naturally lowered, and the furnace is cooled to below 100 ° C. After the product is taken out, Th 3 P 4 The rare earth sulfide with a cubic st...

Embodiment 2

[0051] The rare earth metal samarium and zinc sulfide are respectively subjected to vacuum heating and dehydration treatment: the vacuum degree is 0.05MPa; the temperature is 800 ° C; the heating rate is 15 ° C / min; the treatment time is 3 hours; In a graphite-heated closed reactor-vacuum carbon tube furnace metal molybdenum crucible, according to the molar ratio of rare earth metals and sulfides of 1:2, start the cooling water circulation system, and vacuumize, the vacuum degree is 0.08Pa, and the heating rate is 10°C / min, at a temperature of 1200°C, hold for 2 hours, and keep the vacuum degree at 10-10- 3 In the range of Pa, high-purity argon with a purity of ≥99.99% is filled as protective gas. After the synthesis reaction is completed, the temperature is naturally lowered, and cooled to below 100 °C with the furnace. Grinding process to obtain Th 3 P 4 type cubic structure of rare earth sulfides, the results of X-ray diffraction analysis are similar figure 1 . The rare...

Embodiment 3

[0053] Rare earth metal samarium and zinc sulfide are respectively subjected to vacuum heating and dehydration treatment: the degree of vacuum is 0.03MPa; the temperature is 800°C; the heating rate is 10°C / min; the treatment time is 3 hours; In a graphite-heated closed reactor-vacuum carbon tube furnace metal molybdenum crucible, according to the molar ratio of rare earth metals and sulfides of 1:3, start the cooling water circulation system, and vacuumize, the vacuum degree is 0.09Pa, and the heating rate is 3°C / min, keep the temperature at 1400°C for 3h, keep the vacuum degree in the range of 10-10-3Pa, fill with high-purity argon with a purity of ≥99.99% as a protective gas, and cool down naturally after the synthesis reaction. The furnace is cooled to below 100 ℃, and after taking out the product, it is subjected to the grinding process of the crusher and the sample preparation pulverizer to obtain Th 3 P 4 type cubic structure of rare earth sulfides, the results of X-ray...

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Abstract

The invention provides a preparation method of rare earth sulfide. The preparation method comprises the following steps of preprocessing, mixing and storing a rare earth metal simple substance and zinc sulfide in a sealed reactor, wherein the molar ratio of rare earth metal and the zinc sulfide is 1:(1-10); vacuumizing the reactor until the vacuum degree is 0.07-0.09 Pa; filling protective gas until the vacuum degree is 0.03-0.04 MPa; reacting for 1-3h under the temperature of 1000-1400 DEG C. The preparation method is safe, reliable and low in cost, and the synthetic ratio and the purity of a product are high.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, in particular, the invention relates to a preparation method of rare earth sulfide. Background technique [0002] Rare earth elements have a special 4f electronic structure and unique physical and chemical properties. They have a wide range of applications in light, sound, electricity, magnetism, heat and catalysis. Rare earth sulfides are a class of functional materials with complex structures, rich properties and wide applications. They have broad application prospects and unique advantages in the fields of inorganic pigments, thermoelectric materials, optical materials and magnetic materials, and have become a research field in the field of materials science. One of the hot spots. [0003] Because rare earth sulfides have a large oxygen affinity, it is difficult to synthesize high-purity rare earth sulfides. At present, rare earth sulfides are mainly synthesized by three methods: d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B22F1/02B22F9/20C01F17/00
Inventor 刘建钢姜银举翟纪敏张成边瑞峰刘明月
Owner 内蒙古中科宏特高新科技有限责任公司