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Preparation method of oxygen-free zirconium tetrafluoride applied to nuclear fission energy-- thorium-based molten salt reactor

A technology of zirconium oxytetrafluoride and molten salt reactor, which is applied in zirconium halide, nuclear power generation, reactor fuel material, etc. Easy to mix, environmentally friendly, simple raw materials

Active Publication Date: 2021-07-06
刘明钢 +5
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this invention is to provide a kind of preparation method that is applied to nuclear fission energy thorium-based molten salt reactor anaerobic zirconium tetrafluoride, overcomes existing dry method and sublimation The environmental unfriendly problem existing in the production method of zirconium tetrafluoride and the technical problem that the oxygen content and purity of zirconium tetrafluoride produced by wet method are not up to standard

Method used

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  • Preparation method of oxygen-free zirconium tetrafluoride applied to nuclear fission energy-- thorium-based molten salt reactor
  • Preparation method of oxygen-free zirconium tetrafluoride applied to nuclear fission energy-- thorium-based molten salt reactor
  • Preparation method of oxygen-free zirconium tetrafluoride applied to nuclear fission energy-- thorium-based molten salt reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0055] This embodiment prepares oxygen-free zirconium tetrafluoride through the following steps:

[0056] Step 1, preparation of ZrF 4 .H 2 O crude product;

[0057] Step 1.1, add hydrofluoric acid with a mass concentration of 45%-50% and a mass of 3000 grams into the polytetrafluoroethylene reaction kettle, heat it to 65°C, and then quickly add it to the hydrofluoric acid at one time while stirring 750 grams of zirconium dioxide; wherein the mass ratio of the total mass of zirconium dioxide to the mass concentration of 45%-50% hydrofluoric acid is 1:2.0;

[0058] Step 1.2, wait for the reaction solution to boil, maintain the reaction temperature at 100°C, and continue the reaction for 45 minutes;

[0059] Step 1.3, add 750 grams of zirconium dioxide to the reaction solution again, keep the reaction temperature at 100°C, and continue the reaction for 40 minutes. After the reaction is complete, let it stand for 30 to 40 minutes; filter and collect the filtrate, which is ZrF ...

Embodiment 2

[0077] This example prepares oxygen-free zirconium tetrafluoride through the following steps. The difference from Example 1 is that the mass ratio of the total mass of zirconium dioxide to hydrofluoric acid with a mass concentration of 45%-50% is 1:2.2:

[0078] Step 1, preparation of ZrF 4 .H 2 O crude product;

[0079] Step 1.1, add hydrofluoric acid with a mass concentration of 45%-50% and a mass of 3000 grams into the polytetrafluoroethylene reaction kettle, heat it to 65°C, and then quickly add it to the hydrofluoric acid at one time while stirring 682 grams of zirconium dioxide; wherein the mass ratio of the total mass of zirconium dioxide to the mass concentration of 45%-50% hydrofluoric acid is 1:2.2;

[0080] Step 1.2, wait for the reaction solution to boil, maintain the reaction temperature at 100°C, and continue the reaction for 45 minutes;

[0081] Step 1.3, add 682 grams of zirconium dioxide to the reaction solution again, keep the reaction temperature at 100°C...

Embodiment 3

[0097] This example prepares oxygen-free zirconium tetrafluoride through the following steps. The difference from Example 1 is that the mass ratio of the total mass of zirconium dioxide to hydrofluoric acid with a mass concentration of 45%-50% is 1:1.8:

[0098] Step 1, preparation of ZrF 4 .H 2 O crude product;

[0099] Step 1.1, add hydrofluoric acid with a mass concentration of 45%-50% and a mass of 3000 grams into the polytetrafluoroethylene reaction kettle, heat it to 65°C, and then quickly add it to the hydrofluoric acid at one time while stirring 833 grams of zirconium dioxide; wherein the mass ratio of the total mass of zirconium dioxide to the mass concentration of 45%-50% hydrofluoric acid is 1:1.8;

[0100] Step 1.2, wait for the reaction solution to boil, maintain the reaction temperature at 100°C, and continue the reaction for 45 minutes;

[0101] Step 1.3, add 833 grams of zirconium dioxide to the reaction solution again, keep the reaction temperature at 100°C...

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Abstract

The invention relates to a preparation method of zirconium tetrafluoride, in particular to a preparation method of oxygen-free zirconium tetrafluoride applied to nuclear fission energy, namely a thorium-based molten salt reactor. The method solves the technical problems that existing dry methods and sublimation methods for producing zirconium tetrafluoride are not environment-friendly and that the oxygen content and the purity of zirconium tetrafluoride produced by a wet method do not reach the standard. The preparation method comprises the following steps: by taking ZrO2 and HF as raw materials, carrying out a complete reaction on ZrO2 by adjusting a material ratio and selecting a special charging mode and reaction temperature and time, and completely converting ZrO2 into ZrF4. H2O; then conducting concentration and centrifugation to obtain a refined ZrF4. H2O product; then converting ZrF4. H2O into ZrF4, wherein a by-product ZrOF2 is generated; and then adding NH4HF2 so as to completely convert the by-product into ZrF4. According to the invention, raw materials used for preparing the oxygen-free zirconium tetrafluoride are simple and easy to obtain, impurities are easy to remove, a reaction temperature zone is low, less waste water and waste gas are generated in the reaction process, and a reaction process is environmentally friendly; and the oxygen content of the finally prepared oxygen-free zirconium tetrafluoride product is 200-500 ppm, and the purity of the product is larger than or equal to 99.99%, so the index requirement of the thorium-based molten salt reactor for fluoride salt is met.

Description

technical field [0001] The invention relates to a preparation method of zirconium tetrafluoride, in particular to a preparation method of oxygen-free zirconium tetrafluoride applied to nuclear fission energy thorium-based molten salt reactors. Background technique [0002] Thorium-based molten salt reactor is a liquid fuel reactor that uses thorium-uranium nuclear fuel cycle, uses fluoride salt as coolant, melts natural nuclear fuel and convertible nuclear fuel in high-temperature fluoride salt, and carries nuclear fuel for circulation inside and outside the reactor . Since the coolant is fluoride salt, it becomes solid after cooling, which makes the nuclear fuel neither easy to leak nor interact with groundwater to cause ecological disasters. At the same time, the location of the reactor is more free, and can be built in non-shore areas and underground at a depth of tens of meters. [0003] Thorium-based molten salt reactors have special and strict requirements on the oxy...

Claims

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Application Information

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IPC IPC(8): C01G25/04G21C3/54
CPCC01G25/04G21C3/54C01P2002/72Y02E30/30
Inventor 刘明钢闫宏伟黄雪锋田厦李洋洋丁杰魏文丽张晓红
Owner 刘明钢
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