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XNH4Br.LaBr3.YH2O, preparation method and preparation method of anhydrous lanthanum bromide

A hydrated lanthanum bromide and ammonium bromide technology, applied in inorganic chemistry, chemical instruments and methods, rare earth metal compounds, etc., can solve problems such as high product cost, strict content control requirements, and restrictions on the development of lanthanum bromide scintillation crystals

Active Publication Date: 2015-03-18
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the strong hydrolysis of anhydrous lanthanum bromide at high temperature, its preparation process has extremely strict requirements on the control of oxygen and water vapor content in the surrounding environment, resulting in the current production process of high-purity anhydrous lanthanum bromide is complicated, the process control is difficult, and the product cost is very high. High, restricting the development of lanthanum bromide scintillation crystals

Method used

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  • XNH4Br.LaBr3.YH2O, preparation method and preparation method of anhydrous lanthanum bromide
  • XNH4Br.LaBr3.YH2O, preparation method and preparation method of anhydrous lanthanum bromide
  • XNH4Br.LaBr3.YH2O, preparation method and preparation method of anhydrous lanthanum bromide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0069] 15.14g lanthanum bromide heptahydrate (LaBr 3 ·7H 2 O) and 5.91g of ammonium bromide were mixed evenly and added to a 50mL corundum crucible. Cover the crucible with a lid and keep it at 120°C for 4.5 hours, then keep it at 450°C for 1.0 hour to get XNH 4 Br·LaBr 3 ·YH 2 O. Will get XNH 4 Br·LaBr 3 ·YH 2 After the surface of O is covered with 5mm thick alumina, it is first kept at 250°C for 3.5 hours, and then at 850°C for 0.5 hour, so that the upper layer of alumina and the lower layer of anhydrous lanthanum bromide with obvious stratification are obtained. In this embodiment, based on the addition of 1.00 parts by weight of lanthanum bromide without crystal water, the addition of ammonium bromide is 0.52 parts by weight, aluminum oxide is the covering, and the thickness of the covering is 5 mm.

[0070] The XNH obtained according to the above measurement method 4 Br·LaBr 3 ·YH 2 O and anhydrous lanthanum bromide were characterized, and the results are as fo...

Embodiment 2

[0073] 15.14g lanthanum bromide heptahydrate (LaBr 3 ·7H 2 O) and 70.88g of ammonium bromide were mixed evenly and added to a 100mL corundum crucible. Cover the crucible and keep it at 200°C for 3.0 hours, then keep it at 400°C for 5.5 hours to get XNH 4 Br·LaBr 3 ·YH 2 O. Will get XNH 4 Br·LaBr 3 ·YH 2 After the surface of O is covered with 10mm thick alumina, it is first kept at 500°C for 3.0 hours, and then at 850°C for 0.5 hour, so that the upper layer of alumina and the lower layer of anhydrous lanthanum bromide are obtained with obvious stratification. In this embodiment, based on the addition of 1.00 parts by weight of lanthanum bromide without crystal water, the addition of ammonium bromide is 6.24 parts by weight, alumina is the covering, and the thickness of the covering is 10 mm.

[0074] The XNH obtained according to the above measurement method 4 Br·LaBr 3 ·YH 2 O and anhydrous lanthanum bromide were characterized, and the results are as follows:

[00...

Embodiment 3

[0077] 13.25g hydrated lanthanum bromide (LaBr 3 3.5H 2 O) and 141.77g of ammonium bromide were mixed evenly and added to a 200mL corundum crucible. After the crucible was covered with a lid, it was incubated at 250°C for 3.5 hours, and then at 350°C for 5.5 hours to obtain XNH 4 Br·LaBr 3 ·YH 2 O. Will get XNH 4 Br·LaBr 3 ·YH 2 O was first incubated at 500°C for 3.0 hours, and then at 850°C for 3.0 hours, thus obtaining anhydrous lanthanum bromide. In this embodiment, based on the addition of 1.00 parts by weight of lanthanum bromide without crystal water, the addition of ammonium bromide is 12.48 parts by weight, XNH 4 Br·LaBr 3 ·YH 2 O is the cover, and the thickness of the cover is 18mm.

[0078] The XNH obtained according to the above measurement method 4 Br·LaBr 3 ·YH 2 O and anhydrous lanthanum bromide were characterized, and the results are as follows:

[0079] XNH 4 Br·LaBr 3 ·YH 2 The purity of O is 99.98%, the X value is 3.0, and the Y value is 0; ...

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Abstract

The invention discloses a double salt of XNH4Br.LaBr3.YH2O and a preparation method thereof. The method comprises: (1) well mixing hydrated lanthanum bromide with a molecular formula of LaBr3.mH2O with ammonium bromide, wherein m>0; (2) heating the mixture obtained in step (1) to obtain the double salt. The double salt of the invention is easy to dehydrate, is low in hydrolyzation degree in a heating dehydration process, and is suitable for preparing anhydrous lanthanum bromide with high purity.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic materials, in particular to XNH 4 Br·LaBr 3 ·YH 2 O, its preparation method and based on XNH 4 Br·LaBr 3 ·YH 2 O Process for the preparation of anhydrous lanthanum bromide. Background technique [0002] to Ce 3+ Ion-activated lanthanum bromide crystals (LaBr 3 : Ce 3+ ) is a new type of inorganic scintillation crystal developed in recent years. Compared with similar crystals, this crystal has the advantages of higher light yield, better energy resolution, faster decay time, and less nonlinear response; compared with traditional NaI(TI) crystals, Ce 3+ Ion-activated lanthanum bromide crystals have many excellent properties and have feasible prospects for industrialization and commercialization. be widely used. [0003] The preparation of anhydrous lanthanum bromide is one of the key links in the preparation of the above-mentioned lanthanum bromide crystal. The method fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
CPCC01F17/30C01P2002/72
Inventor 卢旭晨张志敏
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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