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Method for preparing hafnium tetrachloride

A technology of hafnium tetrachloride and carbon tetrachloride, which is applied in the field of preparation of nuclear grade hafnium oxide to prepare hafnium tetrachloride, can solve the problems of excessive iron, chromium and nickel elements, unsatisfactory particle size and high chlorination reaction temperature. problems, to achieve the effect of reducing dust emissions, good product quality, and reducing the number of equipment

Inactive Publication Date: 2017-05-24
郑旭
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method is much more advanced than the former, but because there is no suitable equipment and process for crushing hafnium oxide and carbon powder, the particle size often fails to meet the requirements, resulting in more dust or slag floating backward in the furnace, forcing the producer to increase the distribution. The carbon ratio increases the cost. At the same time, the aisle is blocked due to the accumulation of carbon powder, and production needs to be stopped. In addition, the chlorination reaction temperature is relatively high, which causes corrosion of the equipment, and the iron, chromium, and nickel elements in the product often exceed the standard.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: The chlorination system of the present invention consists of a chlorination furnace, a first condenser, a second condenser and their interconnected aisles, all the way to the tail gas outlet, and its control pressure is ±50Pa (relative to atmospheric pressure). The inner diameter of the reaction section of the chlorination furnace is 200mm.

[0029] Control the crushed particle size of hafnium oxide at -325 ~ 500 mesh, after drying, put it into the boiling chlorination furnace for chlorination, the operation steps are as follows:

[0030] 1. Before the chlorination reaction, the microwave drying temperature of hafnium oxide is 420K, and it is dehydrated by microwave;

[0031] 3. When the temperature in the reaction zone of the chlorination furnace reaches 920K, add baked hafnium oxide into the chlorination furnace;

[0032] 4. The feeding rate of hafnium oxide into the chlorination furnace is 28kg / h; the carbon tetrachloride gas pressure is 0.25MPa, and t...

Embodiment 2

[0036] Embodiment 2: The chlorination system of the present invention is composed of a chlorination furnace, a first condenser, a second condenser, and the passages connected to each other, until the tail gas outlet, and its control pressure is ±50Pa (relative to atmospheric pressure). The inner diameter of the reaction section of the chlorination furnace is 200mm.

[0037] Control the crushed particle size of hafnium oxide at -325~500 mesh, after drying, put it into boiling chlorination furnace for chlorination, the operation steps are as follows:

[0038] 1. Before the chlorination reaction, the microwave drying temperature of hafnium oxide is 420K, and it is dehydrated by microwave;

[0039] 2. When the temperature in the reaction zone of the chlorination furnace reaches 870K, add the dried hafnium oxide into the chlorination furnace;

[0040] 3. The feeding speed is 26kg / h, carbon tetrachloride is fed 22kg / h per hour, and the carbon tetrachloride gas pressure is 0.25MPa ...

Embodiment 3

[0044] Embodiment 3: The chlorination system of the present invention is composed of a chlorination furnace, a first condenser, a second condenser and their interconnected aisles, until the tail gas outlet, and its control pressure is ±50Pa (relative to atmospheric pressure). The inner diameter of the reaction section of the chlorination furnace is 200mm. Control the particle size of the hafnium oxide at -325 to 600 mesh, after drying, put it into the boiling chlorination furnace for chlorination, the operation steps are as follows:

[0045] 1. Before the chlorination reaction, the microwave drying temperature of hafnium oxide is 420K, and it is dehydrated by microwave;

[0046] 2. When the temperature in the reaction zone of the chlorination furnace reaches 800K, add the dried mixture into the chlorination furnace;

[0047] 3. The feed rate is 25kg / h, the chlorine gas is injected at 21kg / h per hour, and the carbon tetrachloride gas pressure is 0.25MPa;

[0048] 4. The fluid...

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Abstract

The invention discloses a method for preparing hafnium tetrachloride. The method includes the following technological steps that hafnium oxide is smashed, the smashed hafnium oxide is dried, the dried hafnium oxide is added into a chlorination furnace, carbon tetrachloride is added for chlorination, and after a reaction is carried out, hafnium tetrachloride gas generated in a boiling fluidized bed is condensed through a condensing device, then solid hafnium tetrachloride is obtained, and tail gas is washed through a leaching tower to be discharged. The method is short in technological process, carbon powder is canceled, the production technology process of coarse hafnium tetrachloride is greatly shortened, and energy consumption is reduced; the quality of the product is good; the metal recovery rate is high; the carbon tetrachloride is selected as a carbon source and a chlorinating agent, the set number of used devices is reduced, the chlorinating agent is safer in using, purchasing is convenient and fast, dust discharging is reduced, and resources are saved.

Description

technical field [0001] The invention relates to a method for preparing hafnium tetrachloride, in particular to a method for preparing hafnium tetrachloride from nuclear grade hafnium oxide. [0002] technical background [0003] Hafnium is a rare metal material. Hafnium has a high melting point and is a trace additive for aviation, aerospace, and hard alloys. With the development of national defense industry, large-scale modernization of machinery special processing industry. High-purity hafnium is an important metal material that is indispensable for aviation and aviation special alloys and machining. Hafnium has been used as an alloy additive. Adding a small amount of hafnium can improve the strength and heat resistance of insoluble alloys, such as (Nb-30Hf-15W-1.5Zr) (Nb-10W-10Hf-0.07Y) (Nb-10Hf-1Ti), etc. , is a mature aviation and aerospace material. In addition, hafnium is also an additive in the structure of conventional weapons, or a trace additive in hydromagnetic...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G27/04
CPCC01G27/04C01P2006/80C01P2006/82
Inventor 郑旭
Owner 郑旭
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