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Large-granularity cesium iodide spherocrystal and preparation method thereof

A technology of cesium spherulites and large particle size, which is applied in the field of large particle size cesium iodide spherulites and its preparation, can solve problems such as easy agglomeration, achieve low hygroscopicity, simple preparation process and operation, and inhibit crystal nucleation.

Active Publication Date: 2020-08-07
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In order to overcome the defect that the existing products are easy to agglomerate and fill the technical gap, the invention provides a large-size cesium iodide spherulite and its preparation method

Method used

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  • Large-granularity cesium iodide spherocrystal and preparation method thereof
  • Large-granularity cesium iodide spherocrystal and preparation method thereof
  • Large-granularity cesium iodide spherocrystal and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] (1) Add cesium iodide powder into 80°C water to form a saturated solution, and the stirring rate is 700 rpm;

[0039] (2) Cool down from 80°C to 45°C at a cooling rate of 1°C / h;

[0040] (3) Cool down from 45°C to 30°C at a cooling rate of 1°C / h. Insert 4 times of temperature recovery operation, each temperature recovery is 1 °C, and the temperature recovery rate is 1 °C / h, specifically: 45 °C to 42 °C, temperature to 43 °C, temperature to 39 °C, temperature to 40 °C, temperature to 36 °C ℃, warm up to 37°C, cool down to 33°C, warm up to 34°C, cool down to 30°C;

[0041] (4) Continue constant temperature stirring for 2h;

[0042] (5) Filtrate, wash with acetone, and then dry at a temperature of 30° C. under normal pressure for 12 hours to obtain spherical cesium iodide crystals.

[0043] The average circularity of the product is 0.81; the average particle size is 112 μm; the angle of repose: 20°; the caking rate is 9.4%.

Embodiment 2

[0045] (1) Add cesium iodide powder into 70°C water to form a saturated solution, and the stirring rate is 600 rpm;

[0046] (2) Cool down from 70°C to 45°C at a cooling rate of 1°C / h;

[0047] (3) Cool down from 45°C to 30°C at a cooling rate of 2°C / h. Insert 4 times of temperature recovery operation, each temperature recovery is 1 °C, and the temperature recovery rate is 10 °C / h, specifically: 45 °C to 42 °C, temperature to 43 °C, temperature to 39 °C, temperature to 40 °C, temperature to 36 °C ℃, warm up to 37°C, cool down to 33°C, warm up to 34°C, cool down to 30°C;

[0048] (4) Continue constant temperature stirring for 1h;

[0049] (5) Filtrate, wash with acetone, and then dry at a temperature of 40° C. under normal pressure for 8 hours to obtain spherical cesium iodide crystals.

[0050] The average circularity of the product is 0.85; the average particle size is 180 μm; the angle of repose: 23°; the caking rate is 8.9%.

Embodiment 3

[0052] (1) Add cesium iodide powder into 60°C water to form a saturated solution, and the stirring rate is 600 rpm;

[0053] (2) Cooling from 60°C to 40°C at a cooling rate of 4°C / h;

[0054] (3) Cool down from 40°C to 28°C, the cooling rate is 2°C / h, no warm-up operation;

[0055] (4) Continue constant temperature stirring for 0.5h;

[0056] (5) Filtrate, wash with acetone, and then dry at a temperature of 50° C. under normal pressure for 4 hours to obtain spherical cesium iodide crystals.

[0057] The average circularity of the product is 0.78; the average particle size is 380 μm; the angle of repose: 22°; the caking rate is 7.2%.

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Abstract

The invention discloses a large-granularity cesium iodide spherocrystal and a preparation method thereof. The preparation method comprises the following steps: cooling a saturated cesium iodide solution from 50-80 DEG C to 35-45 DEG C at a cooling rate of 1-8 DEG C / h and a stirring rate of 400-700 revolutions / min, and then cooling the solution from 35-45 DEG C to 15-30 DEG C at a cooling rate of 1-4 DEG C / h, wherein multiple temperature returning operations may be conducted in the process of cooling to regulate the sphericity and granularity of the spherocrystal; continuing stirring at a constant temperature for 5 minutes to 2 hours; and successively carrying out filtering, washing and drying to obtain the cesium iodide spherocrystal. The spherocrystal has a particle size in a range of 100-1000 [mu]m, a roundness value of 0.7 or more, a repose angle of 25 degrees or less, and strong anti-caking ability, and solves a series of problems brought to production, transportation and sales dueto easy caking of cesium iodide. The preparation method is green, crystallization is performed in a pure water solution, additives and impurities are avoided, and the requirement for high purity of the product is met; and the preparation method is simple and efficient to operate and easy to implement on an industrial scale.

Description

technical field [0001] The invention belongs to the technical field of chemical engineering industrial crystallization, and in particular relates to a large-size cesium iodide spherulite and a preparation method thereof. Background technique [0002] Cesium iodide, CAS No. 7789-17-5, molecular formula CsI, molecular weight 259.8, colorless crystal or crystalline powder. Cesium iodide is usually used in X-ray image intensifier tubes, sodium / thallium doped cesium iodide scintillation crystal materials, special electric light source additives, special optical glass, analytical reagents, etc. [0003] Cesium iodide is soluble in water, easy to absorb moisture, and easy to deliquesce, which causes its crystal particles to be subject to fluctuations in humidity and temperature during storage, transportation, and sales, resulting in repeated moisture absorption and dehydration, which in turn triggers contact between crystals The process of dissolution and recrystallization occurs ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01D17/00
CPCC01D17/00C01P2004/32C01P2004/61
Inventor 龚俊波陈明洋余畅游姚孟惠刘岩博汤伟伟吴送姑杜世超高振国侯宝红尹秋响
Owner TIANJIN UNIV
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