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What are the mainstream industrial preparation routes for zirconium fluoride
info：www.hongjiafu.net | Release time：2026-10-26
There are four main preparation routes for industrial anhydrous zirconium fluoride. In China, ammonium fluorozirconate pyrolysis method and zirconia gas-phase fluorination method are commonly used for mass production. Hydrate salt dehydration and zirconium tetrachloride fluorination conversion are mostly used in high-purity or special scenarios
1. Ammonium fluorozirconate pyrolysis method
First, prepare ammonium hexafluorozirconate using zirconium oxychloride or zirconium oxide, hydrofluoric acid, and ammonia water. Alternatively, the intermediate ammonium fluorozirconate can be obtained by directly reacting ammonium hydrogen fluoride with zirconium oxide; Afterwards, it undergoes high-temperature thermal decomposition in an inert atmosphere of 400 to 500 degrees Celsius to produce zirconium fluoride, while releasing ammonia and hydrogen fluoride gases. The exhaust gas can be recycled and reused.
Advantages: The raw materials are easy to procure, and during the wet process, impurities such as hafnium, iron, and silicon can be separated in advance through crystallization purification. It is suitable for high-purity zirconium fluoride used in optical grade and molten salt reactors; The corrosion pressure of the equipment is relatively controllable.
Shortcoming: It will generate a large amount of fluorine-containing tail gas, and the investment in tail gas recovery equipment is relatively high; Improper temperature control during decomposition can easily result in residual oxygen and ammonium impurities.
2. Zirconia gas-phase fluorination method (direct fluorination of gaseous hydrogen fluoride)
Using zirconia powder as raw material, anhydrous hydrogen fluoride gas is introduced into a rotary furnace or fluidized bed equipment to directly undergo fluorination reaction at a high temperature of 500 to 650 degrees Celsius to produce zirconium fluoride. The product can also be further purified by sublimation.
Advantages: Short process flow, suitable for continuous large-scale production of industrial grade zirconium fluoride.
Shortcoming: Hydrogen fluoride has strong corrosiveness, and the reactor requires special corrosion-resistant materials such as Hastelloy and Monel alloy; Zirconia is prone to incomplete fluorination, resulting in a high oxygen content in the finished product, which requires high air flow distribution and temperature uniformity in the furnace.
3. Dehydration method of hydrated zirconium fluoride (wet precipitation+high-temperature removal of crystallization water)
Zirconia dissolves in concentrated hydrofluoric acid and precipitates zirconium fluoride with crystal water; First, perform low-temperature pre drying, then deeply dehydrate at high temperature under a hydrogen fluoride protective atmosphere to prevent hydrolysis and obtain anhydrous zirconium fluoride.
Advantages: The precipitation process is easy to purify and suitable for small-scale production of high-purity raw materials.
Shortcoming: The difficulty lies in the easy hydrolysis of materials. If the dehydration environment lacks hydrogen fluoride protection, it will generate zirconia fluoride and zirconia impurities, making it difficult to control the oxygen index at a low level; High energy consumption, rarely used for large-scale production.
4. Fluorination conversion method of zirconium tetrachloride (halogen exchange method)
Using zirconium tetrachloride as raw material, a halogen exchange reaction occurs with anhydrous hydrogen fluoride gas at around 300 degrees Celsius, where chlorine is replaced by fluorine to obtain zirconium fluoride and hydrogen chloride.
Advantages: Fast response speed, convenient to match with the zirconium metallurgy industry chain; After sublimation purification, the purity is very high.
Shortcomings: High cost of zirconium tetrachloride raw materials, strong corrosiveness of hydrogen chloride and hydrogen fluoride mixed flue gas, and high pressure for environmental protection treatment; It is generally only used for producing nuclear grade, high-purity small batch products and is not considered as the main production line for bulk production.
1. Ammonium fluorozirconate pyrolysis method
First, prepare ammonium hexafluorozirconate using zirconium oxychloride or zirconium oxide, hydrofluoric acid, and ammonia water. Alternatively, the intermediate ammonium fluorozirconate can be obtained by directly reacting ammonium hydrogen fluoride with zirconium oxide; Afterwards, it undergoes high-temperature thermal decomposition in an inert atmosphere of 400 to 500 degrees Celsius to produce zirconium fluoride, while releasing ammonia and hydrogen fluoride gases. The exhaust gas can be recycled and reused.
Advantages: The raw materials are easy to procure, and during the wet process, impurities such as hafnium, iron, and silicon can be separated in advance through crystallization purification. It is suitable for high-purity zirconium fluoride used in optical grade and molten salt reactors; The corrosion pressure of the equipment is relatively controllable.
Shortcoming: It will generate a large amount of fluorine-containing tail gas, and the investment in tail gas recovery equipment is relatively high; Improper temperature control during decomposition can easily result in residual oxygen and ammonium impurities.
2. Zirconia gas-phase fluorination method (direct fluorination of gaseous hydrogen fluoride)
Using zirconia powder as raw material, anhydrous hydrogen fluoride gas is introduced into a rotary furnace or fluidized bed equipment to directly undergo fluorination reaction at a high temperature of 500 to 650 degrees Celsius to produce zirconium fluoride. The product can also be further purified by sublimation.
Advantages: Short process flow, suitable for continuous large-scale production of industrial grade zirconium fluoride.
Shortcoming: Hydrogen fluoride has strong corrosiveness, and the reactor requires special corrosion-resistant materials such as Hastelloy and Monel alloy; Zirconia is prone to incomplete fluorination, resulting in a high oxygen content in the finished product, which requires high air flow distribution and temperature uniformity in the furnace.
3. Dehydration method of hydrated zirconium fluoride (wet precipitation+high-temperature removal of crystallization water)
Zirconia dissolves in concentrated hydrofluoric acid and precipitates zirconium fluoride with crystal water; First, perform low-temperature pre drying, then deeply dehydrate at high temperature under a hydrogen fluoride protective atmosphere to prevent hydrolysis and obtain anhydrous zirconium fluoride.
Advantages: The precipitation process is easy to purify and suitable for small-scale production of high-purity raw materials.
Shortcoming: The difficulty lies in the easy hydrolysis of materials. If the dehydration environment lacks hydrogen fluoride protection, it will generate zirconia fluoride and zirconia impurities, making it difficult to control the oxygen index at a low level; High energy consumption, rarely used for large-scale production.
4. Fluorination conversion method of zirconium tetrachloride (halogen exchange method)
Using zirconium tetrachloride as raw material, a halogen exchange reaction occurs with anhydrous hydrogen fluoride gas at around 300 degrees Celsius, where chlorine is replaced by fluorine to obtain zirconium fluoride and hydrogen chloride.
Advantages: Fast response speed, convenient to match with the zirconium metallurgy industry chain; After sublimation purification, the purity is very high.
Shortcomings: High cost of zirconium tetrachloride raw materials, strong corrosiveness of hydrogen chloride and hydrogen fluoride mixed flue gas, and high pressure for environmental protection treatment; It is generally only used for producing nuclear grade, high-purity small batch products and is not considered as the main production line for bulk production.
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