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Method for preparing lanthanum subcarbonate nana-/micro-crystal by double hydrolysis regulation

A technology of lanthanum carbonate sodium and double hydrolysis, which is applied in chemical instruments and methods, rare earth metal compounds, inorganic chemistry, etc., can solve the problems of unfavorable environmental protection, rational application of resources, difficult control of product shape, high production cost, etc., and facilitate industrialization The operation and product processing are convenient and simple, and the effect of little environmental pollution

Inactive Publication Date: 2008-10-08
TONGJI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Although the above-mentioned method provides the approach of synthesizing rare earth basic carbonate nanomaterials, there are still deficiencies: the addition of rare earth salts brings more by-products, and the shape of the product is not easy to control, and the adjustment of the acidity of the solution will cause The production cost is high and the process is complicated, which is not conducive to environmental protection and rational application of resources

Method used

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  • Method for preparing lanthanum subcarbonate nana-/micro-crystal by double hydrolysis regulation
  • Method for preparing lanthanum subcarbonate nana-/micro-crystal by double hydrolysis regulation
  • Method for preparing lanthanum subcarbonate nana-/micro-crystal by double hydrolysis regulation

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Effect test

Embodiment 1

[0024] Embodiment 1: prepare helical rod-shaped lanthanum hydroxycarbonate

[0025] (1) Add 1×10 -3 mol of La 2 o 3 , 3×10 -2 mol glycine, after adding deionized water to make the filling degree of the reactor reach 60-80%, seal the reactor;

[0026] (2) Transfer the reaction kettle to a temperature-controlled furnace, control the reaction temperature to 200° C., and heat at this temperature for 8, 15, 24, 32, and 48 hours respectively.

[0027] (3) After the reaction was completed, the reactor was taken out and cooled to room temperature naturally.

[0028] (4) Take out the precipitate obtained in the reaction, wash it three times with deionized water and absolute ethanol alternately, and centrifuge after each washing to obtain the desired product.

[0029] Fig. 1 shows the X-ray powder diffraction patterns (a-e are respectively 8, 15, 24, 32, 48h) of the product obtained under different reaction times. It can be seen that the crystal form of the obtained product is the...

Embodiment 2

[0030] Embodiment 2: prepare round cake shape and spiral bar shape lanthanum carbonate basic

[0031] (1) Add 1×10 -3 mol of La 2 o 3 , 3×10 -2 mol glycine, after adding deionized water to make the filling degree of the reactor reach 60-80%, seal the reactor;

[0032] (2) Transfer the reactor to a temperature-controlled furnace, and control the reaction temperature to 160, 180, and 200° C. for 32 hours, respectively.

[0033] (3) After the reaction was completed, the reactor was taken out and cooled to room temperature naturally.

[0034] (4) Take out the precipitate obtained in the reaction, wash it three times with deionized water and absolute ethanol alternately, and centrifuge after each washing to obtain the desired product.

[0035] Figure 3 shows the SEM photos of the products generated by controlling the reaction temperature at 160, 180, 200, and 220°C (A-D) for a reaction time of 32 hours. It can be seen from the figure that the product obtained with the increase...

Embodiment 3

[0036] Embodiment 3: prepare helical rod-shaped lanthanum hydroxycarbonate

[0037] (1) Add 1×10 -3 mol of La 2 o 3 , 4×10 -2 mol glycine, after adding deionized water to make the filling degree of the reactor reach 60-80%, seal the reactor;

[0038] (2) Then, the reaction kettle was transferred to a temperature-controlled furnace, and the reaction time was controlled to be 32 hours, and the reaction temperatures were respectively controlled to be 160, 180, and 200° C. under the reaction time.

[0039] (3) After the reaction was completed, the reactor was taken out and cooled to room temperature naturally.

[0040] (4) Take out the precipitate obtained in the reaction, wash it three times with deionized water and absolute ethanol alternately, and centrifuge after each washing to obtain the desired product. The SEM photo of the product shows that the product is in the shape of a micron-sized spiral rod. The average length of the product obtained at 160° C. is about 1.5 μm...

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Abstract

The invention belongs to the micron-nanometer material preparation technique and the hydro-thermal synthesis technique field, in particular relates to a process for preparing a basic sodium lanthanum carbonate / micron crystal by means of double-hydrolytic regulation. The process has the specific steps that: a lanthanum oxide and an ammonium bicarbonate or a glycin being taken as precursors and a deionized water as a solvent are positioned in a hydrothermal reaction kettle in proportion, the mole ratio of the lanthanum oxide and the glycin or the ammonium bicarbonate is 1:20 to 1:45, and the added quantity of the deionized water is between 50 and 80 percent of the volume of a container; the hydrothermal reaction kettle provided with mixtures is put into a box-type resistance furnace for being heated to the temperature of between 150 and 220 DEG C, and the container is taken out after the 8 to 48h heating at such a temperature and is cooled naturally to the room temperature; and the needed product is obtained after washing and centrifugal separation. The preparing process has advantages of simple process, easy building of the whole preparing system, simple and convenient operation, easy control of conditions, low cost, easy control of the appearance and size of the product, high purity, good crystallinity and convenient and brief product treatment, and is applied to the mass industrial production.

Description

technical field [0001] The invention belongs to the field of micro / nano material preparation technology and hydrothermal synthesis technology, and specifically relates to a method for preparing basic lanthanum carbonate nano / micro crystals through double hydrolysis regulation. Background technique [0002] Rare earth elements are favored in phosphors because of their unique 4f-layer electronic structure and the excellent performance of excitation light in line spectrum or narrow band spectrum. Currently, rare earth compounds are attracting more and more attention due to their wide applications in photocatalysis, biomarkers and magnetism. These properties often depend on the composition, crystal form, morphology and size of rare earth compounds. Therefore, the synthesis of micro / nano rare earth compounds with different crystal shapes, shapes and sizes is a widely pursued goal. The reported method of synthesizing basic rare earth carbonates is mainly a solution method, using...

Claims

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Application Information

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IPC IPC(8): C01F17/00
Inventor 吴庆生谢劲松张达袁品仕
Owner TONGJI UNIV
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