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Method for preparing cesium nitrate by pollucite

A technology of cesium nitrate and cesium garnet, applied in chemical instruments and methods, rubidium/cesium/francium compounds, alkali metal compounds, etc., can solve problems such as hidden safety hazards in operation, harsh raw material requirements, complex technological processes, etc. The effect of improved quality stability, reduced material requirements, and simple process flow

Active Publication Date: 2014-01-15
HUBEI BAIJIERUI ADVANCED MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Existing technology generally adopts cesium carbonate mother liquor and nitric acid neutralization to produce cesium nitrate, but this technology has following deficiencies in use: 1, this technology is directly reacted by cesium carbonate and nitric acid neutralization, and cost is high and because reaction uses nitric acid Neutralization is easy to form acid mist, which makes the operation a safety hazard
2. When producing high-purity products, the process has almost strict requirements on raw materials, which are difficult to achieve by means of impurity removal.
In 1997, Xinjiang Institute of Nonferrous Metals used ion exchange technology to successfully convert cesium sulfate conversion liquid into high-purity cesium nitrate products with ion exchange resin, but the process is complicated and the production cost is high

Method used

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Examples

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Embodiment 1

[0028] A method for preparing cesium nitrate by cesium garnet, the steps are as follows:

[0029] 1. Put the cesium garnet powder into 35wt% sulfuric acid for acid leaching, the mass ratio of liquid to solid is 3:1, the reaction temperature is 130°C, the reaction time is 4h, keep above 90°C and filter to obtain the acid leaching solution;

[0030] 2. Cool the pickling solution to room temperature to sink alum, centrifuge, separate the mother liquor and discharge it after neutralization treatment. The separated crystals are added to tap water for two recrystallizations. The liquid-solid mass ratio of each recrystallization is 5.5:1. Heat tap water to dissolve, boil for half an hour, then cool to room temperature to crystallize, and return the recrystallized mother liquor to step 1;

[0031] 3. Add pure water to the recrystallized refined cesium alum according to the solid-liquid mass ratio of 1:2 to make a suspension, add lime slurry to remove Al 3+ Continue to react for 1 hou...

Embodiment 2

[0038] A method for preparing cesium nitrate by cesium garnet, the steps are as follows:

[0039] 1. Put the cesium garnet powder into 35wt% sulfuric acid for acid leaching, the mass ratio of liquid to solid is 3:1, the reaction temperature is 130°C, the reaction time is 4h, keep above 90°C and filter to obtain the acid leaching solution;

[0040] 2. Cool the pickling solution to room temperature to sink alum, centrifuge, separate the mother liquor and discharge it after neutralization treatment. The separated crystals are added to tap water for two recrystallizations. The liquid-solid mass ratio of each recrystallization is 5.5:1. Heat tap water to dissolve, boil for half an hour, cool to room temperature to crystallize, and return to step 1 for the recrystallized mother liquor;

[0041] 3. Add pure water to the recrystallized refined cesium alum according to the solid-liquid mass ratio of 1:2 to make a suspension, add lime slurry to remove Al 3+ Continue to react for 1 hour...

Embodiment 3

[0048] A method for preparing cesium nitrate by cesium garnet, the steps are as follows:

[0049]1. Put the cesium garnet powder into 35wt% sulfuric acid for acid leaching, the mass ratio of liquid to solid is 3:1, the reaction temperature is 130°C, the reaction time is 4h, keep above 90°C and filter to obtain the acid leaching solution;

[0050] 2. Cool the pickling solution to room temperature to sink alum, centrifuge, separate the mother liquor and discharge it after neutralization treatment. The separated crystals are added to tap water for two recrystallizations. The liquid-solid mass ratio of each recrystallization is 5.5:1. Heat tap water to dissolve, boil for half an hour, cool to room temperature to crystallize, and return to step 1 for the recrystallized mother liquor;

[0051] 3. Add pure water to the recrystallized refined cesium alum according to the solid-liquid mass ratio of 1:2 to make a suspension, add lime slurry to remove Al 3+ Continue to react for 1 hour ...

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Abstract

The invention belongs to the technical field of cesium nitrate preparations and particularly discloses a method for preparing cesium nitrate by pollucite. The method includes that the pollucite is subjected to acid leaching, jarosite precipitation, recrystallization and conversion to obtain a conversion solution of cesium sulfate, a dilute solution of the cesium nitrate is obtained after a double decomposition reaction of calcium nitrate and an impurity removing by adding barium hydroxide and carbon dioxide, and ultimately a finished product of the cesium nitrate is prepared by an evaporation crystallization and a drying. The direct recovery rate of the obtained cesium nitrate product is about 89%, the cesium nitrate content in a product mother liquor is approximately 10.27%, the cesium content in calcium sulfate of a conversion slag after being washed is about 0.48%, the cesium content in a barium sulfate slag is about 0.25%, and the total recovery rate of the mother liquor participating in the recycling is approximately 95.5%.

Description

technical field [0001] The invention relates to the technical field of preparation of cesium nitrate, in particular to a method for preparing cesium nitrate from cesium garnet. Background technique [0002] Cesium salt is widely used in the field of medicine and catalyst in today's industrial production; scintillation crystal optoelectronic industry and high energy physics industry, cesium nitrate crystal is a shiny hexagonal prism with a specific gravity of 3.64-3.68g / cm 3 , with a melting point of 414°C. Due to its chemical properties, it is often used as the basic raw material for the preparation of high-purity cesium salt, and is also used as a catalyst in organic industry. It is one of the main products in the cesium salt market. Existing technology generally adopts cesium carbonate mother liquor and nitric acid neutralization to produce cesium nitrate, but this technology has following deficiencies in use: 1, this technology is directly reacted by cesium carbonate and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D17/00
Inventor 赵正红纪东海罗钊
Owner HUBEI BAIJIERUI ADVANCED MATERIALS
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