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Method for preparing (Y1-xEux)2(OH)5NO3.nH2O oversized rare-earth layered hydroxide compound particles

A oxyhydroxide, 3.6H2O technology, applied in the field of material science, can solve the problems of not getting LRH pure phase particles, limiting the size of exfoliated nanosheets, etc., and achieve the effect of simple and easy technical solution and easy exfoliation treatment.

Active Publication Date: 2014-08-06
NORTHEASTERN UNIV LIAONING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the existing synthesis process generally uses the rare earth ion aqueous solution as the mother liquid (without adding mineralizer), alkali metal or ammonium hydroxide as the precipitant, and obtains LRH particles through synthetic methods such as hydrothermal or homogeneous precipitation, and the reaction temperature is generally It is lower than 120 oC, mainly because when the reaction temperature is higher than 120 oC, LRH pure-phase particles will not be obtained, and the size of LRH particles obtained by the existing synthesis process is less than 5 μm, which greatly limits the size of exfoliated nanosheets

Method used

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  • Method for preparing (Y1-xEux)2(OH)5NO3.nH2O oversized rare-earth layered hydroxide compound particles
  • Method for preparing (Y1-xEux)2(OH)5NO3.nH2O oversized rare-earth layered hydroxide compound particles
  • Method for preparing (Y1-xEux)2(OH)5NO3.nH2O oversized rare-earth layered hydroxide compound particles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Eu(NO 3 ) 3 ·6H 2 O and Y (NO 3 ) 3 ·6H 2 O is mixed with ammonium nitrate according to the molar ratio Y / Eu=19:1. The amount of ammonium nitrate added is based on molar ratio. Stir under pressure to become transparent, and prepare a solution with a total concentration of rare earth element ions of 0.10mol / L, then add ammonium hydroxide while stirring, and adjust the pH of the solution to 6.5 to obtain a suspension;

[0031] The above suspension was moved to a reaction kettle, and hydrothermally reacted at 200 o C for 24 hours;

[0032] After the reaction, the reactor was taken out, cooled to room temperature naturally, and the reaction product was centrifuged, cleaned, and dried at 60°C to obtain white powdery particles (Y 0.95 Eu 0.05 ) 2 (OH) 5 NO 3 · n h 2 O, n =1.5-1.8.

[0033] The obtained white powder particles have a side length of 20 μm, such as figure 1 (a) shown.

Embodiment 2

[0035] Eu(NO 3 ) 3 ·6H 2 O and Y (NO 3 ) 3 ·6H 2 O is mixed with ammonium nitrate according to the molar ratio Y / Eu=19:1, the amount of ammonium nitrate added is based on molar ratio, ammonium nitrate: (Eu+Y) ion=150:1, add deionized water, at room temperature Stir under pressure to become transparent, and prepare a solution with a total concentration of rare earth element ions of 0.10mol / L, then add ammonium hydroxide while stirring, and adjust the pH of the solution to 6.5 to obtain a suspension;

[0036] The above suspension was moved to a reaction kettle, and hydrothermally reacted at 200 o C for 24 hours;

[0037] After the reaction, the reactor was taken out, cooled to room temperature naturally, and the reaction product was centrifuged, cleaned, and dried at 60°C to obtain white powdery particles (Y 0.95 Eu 0.05 ) 2 (OH) 5 NO 3 · n h 2 O, n =1.5-1.8.

[0038] The obtained white powder particles have a side length of 300 μm, such as figure 1 (b) shown.

Embodiment 3

[0040] Eu(NO 3 ) 3 ·6H 2 O and Y (NO 3 ) 3 ·6H 2 O is mixed with ammonium nitrate according to the molar ratio Y / Eu=1:4, the amount of ammonium nitrate added is molar ratio, ammonium nitrate: (Eu+Y) ion=100:1, add deionized water, at room temperature Stir under pressure to become transparent, and prepare a solution with a total concentration of rare earth element ions of 0.08mol / L, then add ammonium hydroxide while stirring, and adjust the pH of the solution to 7.0 to obtain a suspension;

[0041] The above suspension was moved to a reaction kettle, and hydrothermally reacted at 120oC for 168 hours;

[0042] After the reaction finished, take out the reaction kettle, cool to room temperature naturally, the reaction product is through centrifugation, cleaning, and drying at 80oC to obtain white powdery particles (Y 0.2 Eu 0. 8 ) 2 (OH) 5 NO 3 · n h 2 O, n =1.5-1.8.

[0043] The obtained white powder particles have a side length of 10 μm, such as figure 2 As shown...

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Abstract

The invention belongs to the field of material science, and particularly relates to a method for preparing ultra-large size (Y1-xEux)2(OH)5NO3·nH2O rare earth layered hydroxide compound particles. The technical solution steps of the present invention are: mix Eu(NO3)3·6H2O, Y(NO3)3·6H2O or a mixture of the two in any proportion with ammonium nitrate, add deionized water, and prepare a rare earth element ion concentration of 0.02 -0.10mol / L solution, add ammonium hydroxide while stirring, adjust the pH of the solution to 6.5-7.0, and obtain a suspension. Move the suspension to a reaction kettle and conduct a hydrothermal reaction at 120-200oC 24-168 hour, the reaction product is centrifuged, washed and dried to obtain white powder particles (Y1-xEux)2(OH)5NO3·nH2O, where 0≤x≤1, n=1.5-1.8. The technical solution of the present invention is simple and easy to implement, and the obtained (Y1-xEux)2(OH)5NO3·nH2O particle size is relatively large, between 10 and 300 μm, which is easy to carry out subsequent peeling processing.

Description

technical field [0001] The invention belongs to the field of material science, in particular to a super-large size (Y 1-x Eu x ) 2 (OH) 5 NO 3 · n h 2 Preparation method of O rare earth layered hydroxide particles. Background technique [0002] With strippability, the general formula is Ln 8 (OH) 20 (A m- ) 4 / m · y h 2 O or Ln 2 (OH) 5 (A m- ) 1 / m ·( y / 4)H 2 O(Ln: rare earth ion; A: charge balance anion; m =1-3; y =6-7) rare earth layered hydroxide (Layered rare-earth hydroxide, LRH) is a new type of anionic layered compound, and there is only one rare earth metal ion in the LRH laminate. At present, LRH particles can be exfoliated into nanosheets with one or several layers of thickness by ion exchange, intercalation pillars, mechanical disturbance (such as ultrasonic waves), etc. Large-sized two-dimensional nanosheets can not only completely retain the exfoliated matrix. The structural characteristics of laminates, and the transparent fluorescent film ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
Inventor 李继光朱琦武晓鹂韩秀梅李晓东霍地刘绍宏孙伟孙旭东
Owner NORTHEASTERN UNIV LIAONING
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