A kind of preparation method of high-purity cesium sulfate

A cesium sulfate, high-purity technology, applied in chemical instruments and methods, rubidium/cesium/francium compounds, alkali metal compounds, etc., can solve problems such as easy decomposition of carbonic acid, safety accidents, increased costs, etc., to achieve loose process control, The effect of reducing operating requirements and improving product quality stability

Active Publication Date: 2015-08-19
HUBEI BAIJIERUI ADVANCED MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Existing technology generally adopts cesium carbonate and sulfuric acid neutralization to produce cesium sulfate, but this technology has following deficiencies in use: 1, raw material uses cesium carbonate, and cost is high; 2, in neutralization preparation process, because product carbonic acid is Binary weak acid, the neutralizing solution is acidic, need to add cesium hydroxide to adjust the pH value, which increases the cost, and the carbonic acid is easy to decompose, when the carbon dioxide escapes, the reaction is violent and easy to cause safety accidents

Method used

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  • A kind of preparation method of high-purity cesium sulfate

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Embodiment 1

[0026] A kind of preparation method of high-purity cesium sulfate, its step is as follows:

[0027] 1. Acid leaching cesium garnet: put cesium garnet powder into 35wt% sulfuric acid for acid leaching, the liquid-solid mass ratio is 3:1, the reaction temperature is 130°C, the reaction time is 4h, and then keep above 90°C and filter to obtain acid leaching liquid;

[0028] 2. Naturally cool the pickling solution to room temperature to sink alum, centrifuge, separate the mother liquor and discharge it after neutralization treatment, add pure water to the separated cesium alum crystals for two recrystallizations, and the liquid-solid mass ratio of each recrystallization is 8: 1. After adding pure water to dissolve each time, heat, evaporate and concentrate to a temperature of 110°C, the volume is one-third of the original volume, and then naturally cool to room temperature to crystallize, and the recrystallized mother liquor returns to step 1;

[0029] 3. Dissolve the refined ces...

Embodiment 2

[0035] A kind of preparation method of high-purity cesium sulfate, its step is as follows:

[0036] 1. Acid leaching cesium garnet: put cesium garnet powder into 35wt% sulfuric acid for acid leaching, the liquid-solid mass ratio is 3:1, the reaction temperature is 130°C, the reaction time is 4h, and then keep above 90°C and filter to obtain acid leaching liquid;

[0037] 2. Naturally cool the pickling solution to room temperature to sink alum, centrifuge, separate the mother liquor and discharge it after neutralization treatment, add pure water to the separated cesium alum crystals for two recrystallizations, and the liquid-solid mass ratio of each recrystallization is 8: 1. After adding pure water to dissolve each time, heat, evaporate and concentrate to a temperature of 115°C, and the volume is one-third of the original volume, then naturally cool to room temperature to crystallize, and return the recrystallized mother liquor to step 1;

[0038] 3. Dissolve the refined cesi...

Embodiment 3

[0044] A kind of preparation method of high-purity cesium sulfate, its step is as follows:

[0045] 1. Acid leaching cesium garnet: put cesium garnet powder into 35wt% sulfuric acid for acid leaching, the liquid-solid mass ratio is 3:1, the reaction temperature is 130°C, the reaction time is 4h, and then keep above 90°C and filter to obtain acid leaching liquid;

[0046] 2. Naturally cool the pickling solution to room temperature to sink alum, centrifuge, separate the mother liquor and discharge it after neutralization treatment, add pure water to the separated cesium alum crystals for two recrystallizations, and the liquid-solid mass ratio of each recrystallization is 8: 1. After adding pure water to dissolve each time, heat, evaporate and concentrate until the temperature is 120°C, the volume is one-third of the original volume, and then naturally cool to room temperature to crystallize, and the recrystallized mother liquor returns to step 1;

[0047] 3. Dissolve the refine...

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Abstract

The invention belongs to the technical field of preparation methods of inorganic compound caesium sulfate, and particularly discloses a preparation method of high-purity caesium sulfate. The preparation method comprises the following steps: processing pollucite through acid leaching, vitriol sedimentation, re-crystallization and calcium oxide conversion to obtain a caesium sulfate conversion liquid, removing the impurities of the caesium sulfate conversion liquid by virtue of oxalic acid to obtain a caesium sulfate dilute solution, and finally evaporating, crystallizing and drying the caesium sulfate dilute solution to obtain the caesium sulfate finished product. The production process is simple in flow, and the preparation method is suitable for the industrial production; the raw material pollucite is a main raw material for producing the cesium salt, the market source is wide, and the raw material is easy to obtain; by comprising two-step impurity removal, the process is easier to control, the operation requirement is lowered, and the product quality stability is greatly improved.

Description

technical field [0001] The invention relates to the technical field of preparation methods of inorganic compound cesium sulfate, in particular to a preparation method of high-purity cesium sulfate. 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 sulfate is a colorless orthorhombic or white needle-like crystal, soluble in water, insoluble in alcohol and acetone, as a preparation Take the basic raw materials of various cesium salts. Mainly used for analytical reagents, trace analysis of lead, trivalent chromium; special glass; ceramics; catalyst additives. Cesium sulfate has been used as an analytical reagent and some catalysts for many years. Existing technology generally adopts cesium carbonate and sulfuric acid neutralization to produce cesium sulfate, but this technology has following deficiencies in use: ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01D17/00
Inventor 赵正红吴满梅陈凯李兴
Owner HUBEI BAIJIERUI ADVANCED MATERIALS
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