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Preparation method of high-purity anhydrous rare earth chloride

A water chlorination, high-purity technology, applied in the preparation/processing of rare earth metal compounds, rare earth metal halides, rare earth metal chlorides, etc., can solve the problem that the finished product is easy to deliquescence, only within 2%, and the process control is complex and other problems, to achieve the effects of low moisture content and oxygen content, less control of technical indicators, and high process fault tolerance

Active Publication Date: 2021-04-06
包头市明芯科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The amount of other non-rare earth impurities brought in by this method cannot be controlled, and only industrial-grade anhydrous rare earth chloride can be produced. At the same time, the process control is complicated, and the minimum water content can only be within 2%. Only about 1% can be achieved, which cannot meet the requirements of high-purity products
[0003] The existing anhydrous rare earth chloride production processes all use rare earth chloride as raw material and ammonium chloride as auxiliary material for high-temperature vacuum dehydration. Complex, easy to generate chlorine oxides in the dehydration process, and the finished product is very easy to deliquescence, which brings great difficulties to the preparation, packaging, storage, and crystal growth of anhydrous rare earth chloride. Rare earth chloride hydrochloride cannot meet the high-purity anhydrous rare earth chloride that meets the demand for scintillator production in the high-end market
Due to the high price of high-purity anhydrous rare earth chloride scintillators demanded by scintillators, it seriously hinders the development of anhydrous rare earth chloride scintillator industry

Method used

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  • Preparation method of high-purity anhydrous rare earth chloride

Examples

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Comparison scheme
Effect test

Embodiment 1

[0033] Weigh 20 kg of high-purity lanthanum carbonate with ∑ non-rare earth impurities≦100ppm and ∑ non-lanthanum rare earth impurities≦100ppm, and perform the following operations under a slight negative pressure: specifically, the heating rate is 5°C / min, and the temperature is raised to 150°C in the first step. Heat preservation for 60 minutes; second step, heat up to 200°C, heat preservation for 45 minutes; third step, heat up to 250°C, heat preservation for 60 minutes; fourth step, heat up to 300°C, heat preservation for 45 minutes; fifth step, heat up to 350°C, heat preservation for 60 minutes Minutes later, 6.7kg of anhydrous hydrogen chloride gas was introduced under the condition of dynamic heat preservation, and the ventilation rate was 2kg / h. After the ventilation is over, stop the temperature rise, cool to room temperature under the protection of dry nitrogen, and then use a vacuum suction machine to suck the reactants into the storage tank under the protection of d...

Embodiment 2

[0035] Weigh 50kg of high-purity cerium carbonate with ∑ non-rare earth impurities≦100ppm and ∑ non-cerium rare earth impurities≦100ppm, and perform the following operations under a slight negative pressure: specifically, the heating rate is 5°C / min, and the temperature is raised to 150°C in the first step. Heat preservation for 60 minutes; second step, heat up to 200°C, heat preservation for 45 minutes; third step, heat up to 250°C, heat preservation for 60 minutes; fourth step, heat up to 300°C, heat preservation for 45 minutes; fifth step, heat up to 350°C, heat preservation for 60 minutes Minutes later, 16.7kg of anhydrous hydrogen chloride gas was introduced under the condition of dynamic heat preservation, and the ventilation rate was 5kg / h. After aeration, stop heating, cool to room temperature under the protection of dry nitrogen, then utilize vacuum feeder to suck the reactants in the storage tank under the protection of dry nitrogen, and finally analyze and pack to ob...

Embodiment 3

[0037]Weigh 50 kg of high-purity neodymium carbonate with ∑ non-rare earth impurities≦100ppm and ∑ non-neodymium rare earth impurities≦100ppm, and perform the following operations under a slight negative pressure: specifically, the heating rate is 5°C / min, and the temperature is raised to 150°C in the first step. Heat preservation for 60 minutes; second step, heat up to 200°C, heat preservation for 45 minutes; third step, heat up to 250°C, heat preservation for 60 minutes; fourth step, heat up to 300°C, heat preservation for 45 minutes; fifth step, heat up to 350°C, heat preservation for 60 minutes Minutes later, 16kg of anhydrous hydrogen chloride gas was fed under the condition of dynamic heat preservation, and the ventilation rate was 5kg / h. After the ventilation is over, stop the temperature rise, cool to room temperature under the protection of dry nitrogen, and then use a vacuum suction machine to suck the reactants into the storage tank under the protection of dry nitrog...

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Abstract

The invention discloses a preparation method of high-purity anhydrous rare earth chloride, which comprises the following steps: heating and dehydrating high-purity water-containing rare earth carbonate under micro negative pressure to obtain a raw material anhydrous rare earth carbonate; putting the crude anhydrous rare earth carbonate obtained in the previous step into a rotary atmosphere furnace for micro-negative pressure suction, and gradually raising the temperature step by step; after the technical requirements are met, slowly opening an anhydrous hydrogen chloride storage tank, and giving a flow rate according to the technical requirements, so that anhydrous rare earth carbonate is subjected to chlorination reaction under pure anhydrous hydrogen chloride; introducing anhydrous hydrogen chloride gas of which the theoretical amount is 105-130%, controlling the reaction rate to be 1kg-20kg / h ventilation, and cooling to room temperature under the protection of nitrogen after the ventilation is finished; sucking the reacted product into a storage container for inspection under the protection of dry nitrogen by using a vacuum suction machine, and collecting the finished anhydrous rare earth chloride under the condition of isolating water and oxygen. The method is low in process cost, simple in process control, environment-friendly, safe and easy for industrial production.

Description

technical field [0001] The invention relates to the technical field of preparation of rare earth compounds, in particular to a preparation method of high-purity anhydrous rare earth chloride. Background technique [0002] Anhydrous rare earth chloride is used to prepare high-purity metals, rare earth element organic compounds, pharmaceutical additives, organic synthesis catalysts, and desiccants. Existing data inquiries show that all methods use aqueous rare earth chloride mixed with ammonium chloride and then carry out high temperature Vacuum dehydration and other methods in the system. The amount of other non-rare earth impurities brought in by this method cannot be controlled, and only industrial-grade anhydrous rare earth chloride can be produced. At the same time, the process control is complicated, and the minimum water content can only be within 2%. Only about 1% can be achieved, which cannot meet the requirements of high-purity products. [0003] The existing anhyd...

Claims

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Application Information

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IPC IPC(8): C01F17/271C01F17/10
CPCC01F17/271C01F17/10C01P2006/80C01P2006/82C01P2004/61
Inventor 冀代明王新政
Owner 包头市明芯科技有限公司
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