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Method for preparing water-soluble lanthanum trifluoride nanoparticles

A technology of lanthanum trifluoride and nano-particles, which is applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve the problems of difficult dispersion, inclusions, and large particles of rare earth fluorides, and achieve easy removal and reduced preparation costs Effect

Active Publication Date: 2015-05-20
青岛康普顿石油化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main disadvantage of this preparation method is that the generated ammonium nitrate, sodium nitrate or sodium chloride, ammonium chloride, etc. are easily mixed in lanthanum trifluoride nanoparticles, which affects the purity of the product
In addition, the generated waste liquid contains a large amount of these salts and cannot be discharged directly, which increases the cost of large-scale production
Another technical bottleneck restricting the application of nanoparticles is their dispersibility. This is due to the high surface energy of nanoparticles, which are easy to agglomerate and difficult to disperse in liquid media, thus restricting their large-scale application.
[0003] In the previous work, the inventors of this patent application used in-situ surface modification technology to prepare organically dispersed lanthanum trifluoride nanoparticles (Chinese patent ZL200610107264.2), but the prepared product is not water-soluble, and there is no solution The problem of a large amount of salt in the waste liquid
Chinese patent (CN1907859A) invented a method for preparing rare earth fluorides using rare earth oxides as raw materials, without any other by-products such as inorganic salts. It is an environmentally friendly preparation method, but the prepared rare earth fluorides have large particles , much larger than the nanoscale

Method used

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  • Method for preparing water-soluble lanthanum trifluoride nanoparticles
  • Method for preparing water-soluble lanthanum trifluoride nanoparticles
  • Method for preparing water-soluble lanthanum trifluoride nanoparticles

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Add 200ml of distilled water, 1g of lanthanum hydroxide, and 3.5g of thiophosphoric acid containing polyether chains into a 500ml flask, heat the above mixture to 55°C in a water bath, slowly drop in stoichiometric hydrofluoric acid under stirring, and react at a constant temperature 5h, then decompression distillation removes water, and the 3.3g white viscous thing that obtains is the target product water-soluble lanthanum trifluoride nanoparticles, and its XRD pattern and transmission electron microscope pattern, infrared spectrogram and thermogravimetric analysis pattern are respectively as follows figure 1 , 2 , 3, 4 shown.

[0040] The structural formula of the polyether chain-containing thiophosphoric acid used in the present embodiment is n=20.

[0041] Dissolve 1 g of the water-soluble lanthanum trifluoride nanoparticles prepared in this example in 10 g of water to observe its water solubility. It is found that the sample is completely dissolved, and the solu...

Embodiment 2

[0047] Add 200ml of distilled water, 1g of lanthanum hydroxide, and 0.5g of thiophosphoric acid containing polyether chains into a 500ml flask, cool the above mixture to 5°C in an ice-water bath, slowly drop in stoichiometric hydrofluoric acid under stirring, and keep the temperature constant Reaction 24h. Then decompression distillation removes water, and the white viscous thing that obtains is target product water-soluble lanthanum trifluoride nanoparticles, and its XRD pattern is consistent with figure 1 same.

[0048] The structural formula of the polyether chain-containing thiophosphoric acid used in the present embodiment is where R=CH 2 , n=20.

[0049] Dissolve 1 g of the water-soluble lanthanum trifluoride nanoparticles prepared in this example in 10 g of water to observe its water solubility. It is found that the sample is completely dissolved, and the solution is transparent in color, and there is no precipitation after standing for one month.

Embodiment 3

[0051] Add 200ml of distilled water, 1g of lanthanum hydroxide, and 0.5g of polyether chain-containing thiophosphoric acid into a 500ml flask, heat the above mixture to 35°C in a water bath, slowly drop in stoichiometric hydrofluoric acid under stirring, and react at constant temperature 12h. Then decompression distillation removes water, and the white viscous thing that obtains is target product water-soluble lanthanum trifluoride nanoparticles, and its XRD pattern is consistent with figure 1 same.

[0052] The structural formula of the polyether chain-containing thiophosphoric acid used in the present embodiment is where R=C 12 h 25 , R*=CH 3 , n=6.

[0053] Dissolve 1 g of the water-soluble lanthanum trifluoride nanoparticles prepared in this example in 10 g of water to observe its water solubility. It is found that the sample is completely dissolved, and the solution is transparent in color, and there is no precipitation after standing for one month.

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Abstract

The invention belongs to the technical field of novel functional nano materials and in particular relates to a method for preparing water-soluble lanthanum trifluoride nanoparticles. The preparation method comprises the following steps of: adding a lanthanum source and a surface modifier into water, uniformly mixing, dropwise adding hydrofluoric acid, fully reacting for 1-24 hours under the condition of 5-100 DEG C, removing water and obtaining the water-soluble lanthanum trifluoride nanoparticles. The preparation method has the characteristics of simple process and equipment, cheap and readily available raw materials, low cost, high yield and the like and is suitable for large-scale industrial production, and the prepared water-soluble lanthanum trifluoride nanoparticles are uniform in particle size and have high water solubility.

Description

technical field [0001] The invention belongs to the technical field of preparation of novel functional nanometer materials, and in particular relates to a preparation method of water-soluble lanthanum trifluoride nanoparticles. Background technique [0002] Lanthanum trifluoride nanoparticles have a wide range of applications in the fields of luminescent materials, solid lubrication, catalysis, and polymer-based self-lubricating materials. Its preparation is mainly based on the metathesis reaction between soluble lanthanum salts, such as lanthanum nitrate, lanthanum chloride, etc. and ammonium fluoride, sodium fluoride, etc. :6661-6665, Journal of Alloys and Compounds, 2009, 487(1-2):298-303, Journal of Colloid and Interface Science, 2000, 226(1):65-70). The main disadvantage of this preparation method is that the generated ammonium nitrate, sodium nitrate or sodium chloride, ammonium chloride, etc. are easily mixed in the lanthanum trifluoride nanoparticles, which affects ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00B82Y30/00
Inventor 张晟卯张杰张玉娟张治军
Owner 青岛康普顿石油化工有限公司