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Method for preparing rare earth element sulfide

A technology of rare earth elements and sulfides, applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve problems such as darkening, dark product body color, high impurity C content, etc. Short and low reaction temperature effect

Active Publication Date: 2011-02-09
YPB TECH BEIJING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But there is a fatal problem that some organic matter will be pyrolyzed into C and remain in the product. The high content of impurity C will easily cause the product to turn black or dark, and its application is very limited.

Method used

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  • Method for preparing rare earth element sulfide
  • Method for preparing rare earth element sulfide
  • Method for preparing rare earth element sulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Gd(NO 3 ) 3 ·H 2 O (4.5125g, 10mmol), o-phenanthroline (phen, 1.97g, 10mmol), NaS 2 CN(C 2 h 5 ) 2 ·3H 2 O (6.76g, 30mmol) was dissolved in 50ml, 50ml, and 150ml of acetonitrile respectively, and was dissolved completely by ultrasonication. Gd(NO 3 ) 3 ·H 2 O in acetonitrile and NaS 2 CN(C 2 h 5 ) 2 ·3H 2 O was mixed with acetonitrile solution, and the resulting precipitate was removed by rapid filtration. Add the acetonitrile solution of triethyl orthoformate (3.3g) and o-phenanthroline to the filtrate, let it stand for about 10min, after the precipitate is precipitated, filter it under reduced pressure, drain it, wash it twice with acetonitrile, and dissolve the solid in 20ml of chloroform, filter, get the filtrate, and naturally evaporate the solvent at room temperature to obtain the product, place it in a desiccator, and then obtain the dry precursor (attached figure 1 , 2 ). Then add the de-C agent S to the dried precursor product, the amount of t...

Embodiment 2

[0069] Gd(NO 3 ) 3 ·H 2 O (1.6g, 3mmol), o-phenanthroline (0.6g, 3mmol), NaS 2 CN(C 2 h 5 ) 2 ·3H 2 O (4.06g, 18mmol) was dissolved in 15ml, 15ml, and 90ml of acetonitrile respectively, and was dissolved completely by ultrasonication. Gd(NO 3 ) 3 ·H 2 O in acetonitrile and NaS 2 CN(C 2 h 5 ) 2 ·3H 2 O and acetonitrile were mixed, and the resulting precipitate was removed by rapid filtration. Add the acetonitrile solution of triethyl orthoformate (3.3g) and o-phenanthroline to the filtrate, let it stand for about 10min, after the precipitate is precipitated, filter it under reduced pressure, drain it, and place it in a vacuum desiccator to obtain dry and dry of the mixed precursor and then dry the precursor product in S v / Ar atmosphere at 1000 ° C for 240 min to obtain the composite sulfide NaGdS 2 Sample (attached Figure 4 ). In order to improve the crystallinity of the product, an appropriate amount of flux can also be added, and the flux is A 2 CO 3 、A...

Embodiment 3

[0071] Gd(NO 3 ) 3 ·H 2 O (4.5125g, 10mmol), o-phenanthroline (phen, 1.97g, 10mmol), NaS 2 CN(C 2 h 5 ) 2 ·3H 2 O (6.76g, 30mmol) was dissolved in 50ml, 50ml, and 150ml of acetonitrile respectively, and was dissolved completely by ultrasonication. Gd(NO 3 ) 3 ·H2 O in acetonitrile and tri-NaS 2 CN(C 2 h 5 ) 2 ·3H 2 O and acetonitrile were mixed, and the resulting precipitate was removed by rapid filtration. Add the acetonitrile solution of triethyl orthoformate (3.3g) and o-phenanthroline to the filtrate, let it stand for about 10min, after the precipitate is precipitated, filter it under reduced pressure, drain it, wash it twice with acetonitrile, and dissolve the solid in 20ml of chloroform, filter, take the filtrate, and naturally evaporate the solvent at room temperature to obtain the product, and place it in a desiccator to obtain a dry precursor. Then the dried precursor product was mixed with an equimolar ratio of Zn(S 2 CN(C 2 h 5 ) 2 ) 2 Mixed, in ...

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Abstract

The invention discloses a method for preparing rare earth element sulfide. The pure rare earth element sulfide is obtained by thermally decomposing Re-S key-containing rare earth element coordination compound which serves as a precursor or the Re-S key-containing rare earth element coordination compound and S-containing coordination compounds of elements in I, II and IIIA families which serve as the precursor for 10 to 1,000min in the presence of a decarbonizing agent in the atmosphere of N2 and / or Ar at the temperature of 250 to 1,500 DEG C. If the Re-S key-containing rare earth element coordination compound is used as the precursor, singular rare earth element sulfide is prepared by thermal decomposition; and if the Re-S key-containing rare earth element coordination compound and S-containing coordination compounds of the elements in I, II and IIIA families are used as the precursor, compound rare earth element sulfide is prepared by the thermal decomposition. The Re-S key-containing rare earth element coordination compound in the precursor is the coordination compound consisting of different rare earth elements and is thermally decomposed to form the compound sulfide containing different rare earth elements. The method has a simple process and eliminates the influences of residual C; and products of the method have uniform grain size and bright body color.

Description

technical field [0001] The invention belongs to the technical field of rare earth element sulfides and composite sulfides, and relates to a preparation method thereof. At the same time, it involves its application in the fields of optical materials, thermoelectric materials, pigments, and luminescent materials. Background technique [0002] Rare earth element sulfides and their complex sulfides have good development prospects in the fields of optical materials, thermoelectric materials, advanced refractory materials, and pigments due to their high melting point, good chemical stability, non-toxicity, and environmental protection. [0003] However, due to the oxophilicity of rare earth elements, the preparation of pure single-phase rare earth element sulfides has always been difficult. At present, the main preparation methods are: [0004] [1] Elemental direct synthesis method, that is, the rare earth element metal is directly reacted with S vapor or metal sulfide at high t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
Inventor 罗昔贤马禄斌张明
Owner YPB TECH BEIJING
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