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Preparation of high-purity anhydrous lanthanum bromide or cerium bromide with temperature programmed method

A temperature-programmed, water lanthanum bromide technology, used in chemical instruments and methods, inorganic chemistry, rare earth metal compounds, etc.

Active Publication Date: 2013-07-03
BAOTOU JINGRUI NEW MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These documents do not report the actual water content in the anhydrous rare earth bromide obtained, because the water content is required to be less than 0.1% when preparing the scintillation crystal material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0007] 100kg LaBr 3 ·6H 2 O crystals and 80kg of ammonium bromide crystals are mixed evenly in a mixer, and the mixed materials are respectively put into porcelain bowls, and then the porcelain bowls containing materials are evenly placed in a programmed temperature-increasing furnace, and vacuumed by a vacuum pump with water. , when the vacuum degree reaches 0.08Pa, set the heating program to start heating. The heating program is: room temperature to 180°C, the heating rate is 1.33°C / min, the heating time is 2 hours, and the holding time at 180°C is 2 hours; 180°C to 300°C ℃, the heating rate is 0.5°C / min, the heating time is 4 hours, and the holding time at 300°C is 4 hours; 300°C~360°C, the heating rate is 0.5°C / min, the heating time is 2 hours, and the holding time at 360°C is 2 hours; 360°C~410°C, heating rate is 0.42°C / min, heating time is 2 hours, holding time at 410°C is 6 hours, when the temperature of the furnace body naturally drops to 50°C, the material is dischar...

Embodiment 2

[0009] 100kg CeBr 3 ·6H 2 O crystals and 80kg of ammonium bromide crystals are mixed evenly in a mixer, and the mixed materials are respectively put into porcelain bowls, and then the porcelain bowls containing materials are evenly placed in a programmed temperature-increasing furnace, and vacuumed by a vacuum pump with water. , when the vacuum degree reaches 0.08Pa, set the heating program to start heating. The heating program is: room temperature to 180°C, the heating rate is 1.33°C / min, the heating time is 2 hours, and the holding time at 180°C is 2 hours; 180°C to 300°C ℃, the heating rate is 0.5°C / min, the heating time is 4 hours, and the holding time at 300°C is 4 hours; 300°C~360°C, the heating rate is 0.5°C / min, the heating time is 2 hours, and the holding time at 360°C is 2 hours; 360°C to 410°C, the heating rate is 0.42°C / min, the heating time is 2 hours, and the holding time at 410°C is 6.2 hours. When the temperature of the furnace body naturally drops to 50°C, th...

Embodiment 3

[0011] 100kg CeBr 3 ·6H 2 O crystals and 80kg of ammonium bromide crystals are mixed evenly in a mixer, and the mixed materials are respectively put into porcelain bowls, and then the porcelain bowls containing materials are evenly placed in a programmed temperature-increasing furnace, and vacuumed by a vacuum pump with water. , when the vacuum degree reaches 0.08Pa, set the heating program to start heating. The heating program is: room temperature to 180°C, the heating rate is 1.33°C / min, the heating time is 2 hours, and the holding time at 180°C is 2 hours; 180°C to 300°C ℃, the heating rate is 0.5°C / min, the heating time is 4 hours, and the holding time at 300°C is 4 hours; 300°C~360°C, the heating rate is 0.5°C / min, the heating time is 2 hours, and the holding time at 360°C is 2 hours; 360°C~410°C, heating rate is 0.42°C / min, heating time is 2 hours, holding time at 410°C is 6.3 hours, when the temperature of the furnace body naturally drops to 50°C, the material is disch...

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Abstract

The invention relates to preparation of high-purity anhydrous lanthanum bromide or cerium bromide with a temperature programmed method, belonging to the field of preparation of rare earth materials. A method used in the invention comprises the following steps of: dissolving lanthanum carbonate or cerium carbonate of which the chlorine ion content is less than 20 ppm with 40 percent hydrobromic acid, concentrating and crystalizing to obtain LaBr3.6H2O or CeBr3.6H2O, wherein the weight ratio of the lanthanum carbonate or cerium carbonate to the hydrobromic acid is 1:1.6; and mixing the LaBr3.6H2O or CeBr3.6H2O with NH4Br in the weight ratio of 1:0.8 in a mixer, vacuumizing with a water jet pump, setting a temperature raising program for heating when the vacuum degree is 0.08 Pa, controlling segmental temperature raising speed and heat preserving time when the temperature is between the room temperature and 410 DEG C, analyzing and detecting whether the water content of obtained anhydrous lanthanum bromide or cerium bromide is less than 0.1 percent, and adding into water for dissolving quickly, wherein an aqueous solution obtained after dissolving is clear and transparent, product purity is more than 99 percent, and yield is more than 99 percent. The method is applied to a production line in which 75 kilograms of anhydrous lanthanum bromide or cerium bromide is produced in every batch with an industrial scale temperature programmed furnace.

Description

technical field [0001] The invention relates to a method for preparing high-purity anhydrous lanthanum bromide or cerium bromide by a temperature-programmed method, and belongs to the field of rare earth material preparation. Background technique [0002] High-purity anhydrous lanthanum bromide and cerium bromide are used in applications such as scintillation crystal materials and organic synthesis catalysts. The preparation methods of anhydrous lanthanum bromide and cerium bromide include hydrobromide dehydration method and oxide bromination method. Literature Yang Dongmei's "direct preparation of anhydrous lanthanum bromide from lanthanum oxide", Journal of Materials and Metallurgy, 2003, 2 (2): 113-114, provides a method for preparing anhydrous lanthanum bromide, using lanthanum oxide, Al Powder and bromine are directly reacted, and then by chemically transporting the product to obtain anhydrous lanthanum bromide, the anhydrous lanthanum bromide obtained by this method c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
Inventor 张瑞祥郝先库马显东许宗泽胡珊珊刘海旺王士智
Owner BAOTOU JINGRUI NEW MATERIAL
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