Method for preparing high-purity anhydrous strontium iodide

Abstract

The invention relate to a method for preparing high-purity anhydrous strontium iodide. The method comprises the following steps: dropwise adding hydroiodic acid into a reaction vessel containing an aqueous solution containing a strontium compound under stirring until the pH of the solution is 5-6 to obtain an iodide-strontium aqueous solution; regulating the pH value of the iodide-strontium aqueous solution to 7-9 for filtering; after concentrating filtrate to near saturation, quickly lowering the temperature to 0-4 DEG C and precipitating crystal substances; filtering to obtain the crystal substances dissolving in water, and obtaining a purified iodide-strontium aqueous solution; heating the purified strontium iodide aqueous solution to 150-200 DEG C under the flowing inert shielding gas, and preserving heat for 1-30 hours to dehydrate to obtain a SrI2.xH2O white flurry material, wherein x is less than or equal to 1; grinding the white flurry material into powder in an anhydrous and oxygen-free inert atmosphere, and putting in a glass vessel; under vacuum, heating the glass vessel to 350-450 DEG C and preserving heat for 1-20 hours to remove crystal water in the powder, and naturally lowering the temperature to room temperature in the condition of keeping vacuum; heat-sealing the glass vessel in the condition of keeping vacuum.

Description

technical field

[0001] The present invention relates to a kind of preparation method of high-purity anhydrous strontium iodide, more specifically, the present invention relates to a kind of preparation method of high-purity anhydrous strontium iodide raw material for single crystal growth, belongs to halide material preparation field, especially It is the field of preparation of halide raw materials for crystal growth. Background technique

[0002] Inorganic scintillators can be used to quickly, sensitively and accurately determine the gamma-ray characteristics of highly enriched uranium, weapon-grade plutonium, radioactive sources and other special nuclear materials. Radiation detection fields such as testing and nuclear non-proliferation verification have a wide range of applications. In recent years, with the increasingly serious situation of global nuclear safety and terrorism, and the improvement of people's awareness of radiation environmental safety, the demand for h...

Examples

preparation example Construction

[0030] The invention provides a preparation method of high-purity strontium iodide. The preparation method mainly includes: a reaction step of reacting a strontium-containing compound with hydroiodic acid to generate strontium iodide; a purification step of purifying the generated strontium iodide to obtain a flaky hydrous crystal; removing the hydrous crystal in an inert atmosphere. Most of the water of crystallization, obtain the first water removal step of strontium iodide containing a small amount of water of crystallization; and remove the remaining small amount of water of crystallization under vacuum conditions to obtain the second water removal step of anhydrous strontium iodide.

[0031] figure 1 A specific process flow diagram of an example of the present invention is shown. Such as figure 1 As shown, the preparation method of the present invention may specifically include the following steps.

[0032] (1) Add a certain amount of deionized water into the reaction ...

Embodiment 1

[0041] (1) Add 5.4 grams of deionized water to a 250ml glass beaker and weigh strontium carbonate (SrCO 3 ) Put 7.38 grams of raw materials in a reaction vessel, add hydroiodic acid with a purity of not less than 99.9% dropwise, and stir with a magnetic stirrer to completely react strontium carbonate and hydroiodic acid until the solution is clear and the pH value is 5.5 , stop adding hydroiodic acid;

[0042] (2) Adjust the pH value of the solution to 7.5 by adding a small amount of ammonia water, and filter to remove impurities; stir and heat the obtained strontium iodide aqueous solution at 100°C±2°C until the solution is concentrated to 2 / 5 of the initial capacity , stop heating and immediately put the glass beaker into ice cubes, so that the temperature of the solution in the beaker is rapidly reduced to 2-3 ° C, and a large number of flaky crystals are precipitated in the solution;

[0043] (3) The crystals were separated from the mother liquor by vacuum filtration to o...

Embodiment 2

[0049] (1) Add 54 grams of deionized water into a 1000ml glass beaker, weigh 51.81 grams of strontium oxide raw material with a purity of 99.99%, place it in a reaction vessel, and add hydroiodic acid with a purity higher than 99.9% dropwise for neutralization reaction , stirring by a magnetic stirrer makes the reaction complete, and stops adding hydroiodic acid when the pH value of the solution is 5.0;

[0050] (2) Adjust the pH value of the solution to 7.0 by adding a small amount of ammonia water, and filter to remove impurities; put the obtained strontium iodide aqueous solution into a quartz crucible, and use a water ring vacuum pump to evacuate the quartz crucible for 2 hours, so that The aqueous solution of strontium iodide is concentrated, and the quartz crucible containing the concentrated solution is immediately placed in ice cubes, so that the temperature of the concentrated solution is rapidly reduced to 1-2°C, and a large number of flaky crystals are precipitated i...

technical field

[0001] The present invention relates to a kind of preparation method of high-purity anhydrous strontium iodide, more specifically, the present invention relates to a kind of preparation method of high-purity anhydrous strontium iodide raw material for single crystal growth, belongs to halide material preparation field, especially It is the field of preparation of halide raw materials for crystal growth. Background technique

[0002] Inorganic scintillators can be used to quickly, sensitively and accurately determine the gamma-ray characteristics of highly enriched uranium, weapon-grade plutonium, radioactive sources and other special nuclear materials. Radiation detection fields such as testing and nuclear non-proliferation verification have a wide range of applications. In recent years, with the increasingly serious situation of global nuclear safety and terrorism, and the improvement of people's awareness of radiation environmental safety, the demand for h...

Examples

preparation example Construction

[0030] The invention provides a preparation method of high-purity strontium iodide. The preparation method mainly includes: a reaction step of reacting a strontium-containing compound with hydroiodic acid to generate strontium iodide; a purification step of purifying the generated strontium iodide to obtain a flaky hydrous crystal; removing the hydrous crystal in an inert atmosphere. Most of the water of crystallization, obtain the first water removal step of strontium iodide containing a small amount of water of crystallization; and remove the remaining small amount of water of crystallization under vacuum conditions to obtain the second water removal step of anhydrous strontium iodide.

[0031] figure 1 A specific process flow diagram of an example of the present invention is shown. Such as figure 1 As shown, the preparation method of the present invention may specifically include the following steps.

[0032] (1) Add a certain amount of deionized water into the reaction ...

Embodiment 1

[0041] (1) Add 5.4 grams of deionized water to a 250ml glass beaker and weigh strontium carbonate (SrCO 3 ) Put 7.38 grams of raw materials in a reaction vessel, add hydroiodic acid with a purity of not less than 99.9% dropwise, and stir with a magnetic stirrer to completely react strontium carbonate and hydroiodic acid until the solution is clear and the pH value is 5.5 , stop adding hydroiodic acid;

[0042] (2) Adjust the pH value of the solution to 7.5 by adding a small amount of ammonia water, and filter to remove impurities; stir and heat the obtained strontium iodide aqueous solution at 100°C±2°C until the solution is concentrated to 2 / 5 of the initial capacity , stop heating and immediately put the glass beaker into ice cubes, so that the temperature of the solution in the beaker is rapidly reduced to 2-3 ° C, and a large number of flaky crystals are precipitated in the solution;

[0043] (3) The crystals were separated from the mother liquor by vacuum filtration to o...

Embodiment 2

[0049] (1) Add 54 grams of deionized water into a 1000ml glass beaker, weigh 51.81 grams of strontium oxide raw material with a purity of 99.99%, place it in a reaction vessel, and add hydroiodic acid with a purity higher than 99.9% dropwise for neutralization reaction , stirring by a magnetic stirrer makes the reaction complete, and stops adding hydroiodic acid when the pH value of the solution is 5.0;

[0050] (2) Adjust the pH value of the solution to 7.0 by adding a small amount of ammonia water, and filter to remove impurities; put the obtained strontium iodide aqueous solution into a quartz crucible, and use a water ring vacuum pump to evacuate the quartz crucible for 2 hours, so that The aqueous solution of strontium iodide is concentrated, and the quartz crucible containing the concentrated solution is immediately placed in ice cubes, so that the temperature of the concentrated solution is rapidly reduced to 1-2°C, and a large number of flaky crystals are precipitated i...

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