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Method for preparing nuclear-grade sponge zirconium and nuclear-grade sponge hafnium

A nuclear-grade sponge zirconium and nuclear-grade technology, which is applied in the field of preparing nuclear-grade zirconium sponge and nuclear-grade hafnium sponge, can solve the problem that the zirconium-hafnium extraction and separation device cannot be produced normally, does not meet the national environmental protection requirements, and the product quality cannot reach high-purity oxygen Zirconium chloride quality standards and other issues

Inactive Publication Date: 2017-02-22
郭爽
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  • Claims
  • Application Information

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Problems solved by technology

[0003] However, the process method used for the extraction and separation of zirconium and hafnium, whether it is MIBK-NH 4 SCN method, or N235-H 2 SO 4 method, TBP-HCl-HNO 3 However, all the "three wastes" cannot be processed, and the environmental pollution is serious. It does not meet the national environmental protection requirements, resulting in the failure of the normal production of the zirconium and hafnium extraction and separation devices, which fundamentally restricts the development of the nuclear-grade sponge zirconium industry.
[0004] Zirconium oxychloride is the basic raw material of zirconium chemical industry, and the annual market consumption has reached 200,000 tons. However, zirconium oxychloride is produced by "alkali fusion method". The production cost is high, the environmental pollution is serious, and the product quality cannot reach high purity. The quality standard of zirconium oxychloride, with the strengthening of the national environmental protection policy, the "alkali fusion method" zirconium oxychloride is about to come to an end, and the chloride method zirconium oxychloride is a sunrise industry, which will definitely replace the alkali fusion method zirconium oxychloride

Method used

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  • Method for preparing nuclear-grade sponge zirconium and nuclear-grade sponge hafnium
  • Method for preparing nuclear-grade sponge zirconium and nuclear-grade sponge hafnium
  • Method for preparing nuclear-grade sponge zirconium and nuclear-grade sponge hafnium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] The processing device and process method of nuclear-grade zirconium sponge and nuclear-grade hafnium sponge (see figure 1 )

[0052] 1. Preparation of each stage of extraction

[0053] Feed solution preparation: measure and dissolve the zirconium oxychloride in the raw material, hydrolyze the zirconium tetrachloride, control the ZrO2 concentration in the feed liquid of the two obtained solutions to 80-95g / l, filter through a ceramic membrane filter, and use nitric acid and hydrochloric acid to prepare a qualified feed liquid with 8N acidity;

[0054] Preparation of lotion: use recovered hydrochloric acid, nitric acid mixture, hydrochloric acid, and nitric acid to prepare a mixed pickling solution with 5N acidity;

[0055] TBP organic phase preparation: 60% tributyl phosphate (TBP) and 40% kerosene by weight percentage, prepare TBP organic phase;

[0056] Saturated acid preparation: nitric acid is prepared into TBP saturated acid with 6N acidity;

[0057] Alkaline p...

Embodiment 2

[0203] Obtaining of the above-mentioned embodiment raw material: the method for producing high-purity zirconium oxychloride

[0204] 1. Boiling chlorination reaction

[0205] Zircon sand, silicon powder, petroleum coke and chlorine gas, the ratio is 0.8~1.2:0.1~0.4:0.4~0.5:2.8~3.0, and chlorine gas is introduced into the chlorination furnace at a gas velocity of 0.06~0.16m / s. The boiling chlorination reaction is carried out at 650-1100°C, which is an autothermal reaction, and the temperature of the expansion section is controlled at 380-500°C to generate zirconium tetrachloride and silicon tetrachloride.

[0206] Chlorination reaction equation:

[0207] ZrSiO 4 +4C+4Cl 2 =ZrCl 4 +SiCl 4 +4CO (1)

[0208] ZrSiO 4 +2C+4Cl 2 =ZrCl 4 +SiCl 4 +2CO 2 (2)

[0209] Si+2Cl 2 = SiCl 4 (3)

[0210] 2. Condensation and separation of the mixed gas after the reaction

[0211] The mixed gas after the reaction enters the fourth-stage condenser, and is cooled by circulating w...

Embodiment 3

[0230] Preparation of silica by gas phase method:

[0231] 1. Fumed silica synthesis and treatment

[0232]The refined silicon tetrachloride from the high-purity zirconium oxychloride process enters the silicon tetrachloride vaporizer for vaporization, and is vaporized with hot water in the vaporizer. The vaporization temperature is controlled at 70-80°C, and the hydrogen and air from the hydrochloric acid electrolysis device are heated The device is preheated to 120-130°C, and the three gases enter the reaction gas homogenizer for homogenization. The ratio of silicon tetrachloride: hydrogen: air (molar ratio) is 1:2-4:9-11, Enter the multi-layer burner on the upper part of the silica high-temperature reactor, form a stable flame after burning, and generate gas-phase silicon dioxide and hydrogen chloride water vapor in the silica high-temperature reactor, and the temperature in the silica high-temperature reactor is controlled at 800~1000℃, after passing through the reaction-...

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Abstract

The invention relates to nuclear-grade sponge zirconium, in particular to a method for preparing nuclear-grade sponge zirconium and nuclear-grade sponge hafnium. Chlorine generated by hydrochloric acid electrolysis is used for producing zirconium tetrachloride and zirconium oxychloride by a zircon sand boiling chlorination method; zirconium and hafnium are seperated to obtain zirconium oxide and hafnium oxide through a TBP-Hcl-HNO3 extraction method; and then, the chlorination and the purification are performed to obtain the nuclear-grade sponge zirconium and the nuclear-grade sponge hafnium. The method radically solves the environmental protecting environment difficultly treated in the zirconium oxychloride industry and the nuclear-grade sponge zirconium industry, and realizes complete industry chain circulation for combined production of the zirconium oxychloride industry, the gas-phase method silicon dioxide industry, the nuclear-grade sponge zirconium industry and the hydrochloric acid electrolysis industry.

Description

technical field [0001] The invention relates to nuclear-grade sponge zirconium, in particular to a method for preparing nuclear-grade sponge zirconium and nuclear-grade sponge hafnium. Background technique [0002] The main purpose of nuclear-grade zirconium sponge is the core cladding and grid of nuclear reactors. Nuclear-grade zirconium sponge is a strategic material and a necessary material for nuclear power. The annual demand in China has reached more than 1,000 tons, and the annual demand in the world has reached 8,000 tons. As mentioned above, any country with a nuclear power plant must master such an important strategic material technology. From this point of view, it is very necessary for China to establish its own nuclear-grade zirconium sponge industry. [0003] However, the process method used for the extraction and separation of zirconium and hafnium, whether it is MIBK-NH 4 SCN method, or N235-H 2 SO 4 method, TBP-HCl-HNO 3 However, all the "three wastes" ca...

Claims

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Application Information

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IPC IPC(8): C22B34/14C22B3/38C01G25/04C01B33/18
CPCC01B33/18C01G25/04C22B34/14C22B3/3846Y02P10/20
Inventor 郭爽
Owner 郭爽
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