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Hafnium tetrachloride preparation method

A technology of hafnium tetrachloride and hafnium oxide, applied in the field of preparation of hafnium tetrachloride by fluidized bed chlorination, which can solve the problems of difficult control of impurities, long production cycle, and low recovery rate, so as to shorten the production process and reduce dust Emissions, small footprint effect

Inactive Publication Date: 2015-06-10
CHINA NUCLEAR JINGHUAN ZIRCONIUM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The existing hafnium oxide chlorination process is complex. Firstly, hafnium oxide and carbon powder are ground to a certain particle size, and then mixed according to the ratio of hafnium oxide: carbon powder: pulp = 4.325: 1: 1.1, and the balls are mixed and put into a coking furnace for coking. , after coking for 10 hours, put the ball into the vertical immobilization furnace heated to 800°C, seal the upper cover, connect the aisle, and inject chlorine gas at the bottom to start production
This method has a long cycle, and the recovery rate decreases after several processes.
Moreover, the vertical fixed chlorination furnace is made of quartz knots, which has poor sealing performance, easy to leak, harsh production environment, and difficult to control impurities, low product quality, long production cycle and low output.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Example 1: The present invention consists of a chlorination furnace, a first condenser, a second condenser, a third condenser and the interconnected aisle, until the tail gas outlet constitutes a chlorination system. system , and its control pressure is ±50Pa (relative to atmospheric pressure). The inner diameter of the reaction section of the chlorination furnace is 200 mm.

[0033] Control the pulverized particle size of hafnium oxide at -325~500 mesh, control the pulverized particle size of carbon powder at -100~200 mesh, mix well, add boiling chlorination furnace for chlorination, the operation steps are as follows:

[0034] 1. The ratio of hafnium oxide to carbon powder is 100:9 to make a mixture;

[0035] 2. Before the chlorination reaction, the microwave drying temperature of the mixture is 420-470K, and the mixture is dehydrated by microwave;

[0036] 3. When the temperature in the reaction zone of the chlorination furnace reaches 1050K±100K, add the dried m...

Embodiment 2

[0041] Example 2: The present invention consists of a chlorination furnace, a first condenser, a second condenser, a third condenser and the interconnected aisle, until the tail gas outlet constitutes a chlorination system. system , and its control pressure is ±50Pa (relative to atmospheric pressure). The inner diameter of the reaction section of the chlorination furnace is 200 mm.

[0042] Control the pulverized particle size of hafnium oxide at -325~500 mesh, control the pulverized particle size of carbon powder at -100~200 mesh, mix well, add boiling chlorination furnace for chlorination, the operation steps are as follows:

[0043] 1. The ratio of hafnium oxide to carbon powder is 100:9 to make a mixture;

[0044] 2. Before the chlorination reaction, the microwave drying temperature of the mixture is 420-470K, and the mixture is dehydrated by microwave;

[0045] 3. When the temperature in the reaction zone of the chlorination furnace reaches 1050K±100K, add the dried ...

Embodiment 3

[0050] Example 3: The present invention consists of a chlorination furnace, a first condenser, a second condenser, a third condenser and the interconnected aisle, until the tail gas outlet constitutes a chlorination system. system , and its control pressure is ±50Pa (relative to atmospheric pressure). The inner diameter of the reaction section of the chlorination furnace is 200 mm.

[0051] Control the pulverized particle size of hafnium oxide at -325~500 mesh, control the pulverized particle size of carbon powder at -100~200 mesh, mix well, add boiling chlorination furnace for chlorination, the operation steps are as follows:

[0052] 1. The ratio of hafnium oxide to carbon powder is 100:10 to make a mixture;

[0053] 2. Before the chlorination reaction, the microwave drying temperature of the mixture is 420-470K, and the mixture is dehydrated by microwave;

[0054] 3. When the temperature in the reaction zone of the chlorination furnace reaches 1050K±100K, add the dried...

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Abstract

The invention discloses a hafnium tetrachloride preparation method which includes the processing steps that hafnium oxide and carbon powder are smashed, the smashed hafnium oxide and the smashed carbon powder are evenly mixed into a mixture, microwave drying and dehydration are carried out on the mixture, the dried mixture is added into a chlorination furnace, chlorine is added for chlorination, after an reaction, hafnium tetrachloride gas generated by a fluidized bed passes a condenser, then solid hafnium tetrachloride is obtained, and tail gas is exhausted after leaching in a channel. The method is short in process procedure, the metal recycle rate is high, the yield of the single furnace is high, occupied area is small, equipment is small in number, concentrated and easy to manage, environmental protection is facilitated, no chlorine leaks due to new process material matching, materials are conveyed in a closed condition, powder emission is reduced, and resources are saved.

Description

technical field [0001] The invention relates to a method for preparing hafnium tetrachloride by ebullating bed chlorination, in particular to a method for preparing hafnium tetrachloride from nuclear-grade hafnium oxide. technical background [0002] Hafnium is a rare metal material. Because it is not easy to extract and the quantity is small, high-purity hafnium is mainly used as a control material for nuclear reactors, and high-purity hafnium can be processed into rods, plates, wires, Tubes are also the research and development objects of new alloys. Due to the high melting point of hafnium, it is a trace additive for aviation, aerospace, and hard alloys. With the development of large-scale modernization of the national defense industry and the special machinery 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 amo...

Claims

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Application Information

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IPC IPC(8): C01G27/04
CPCC01G27/04C01P2006/80
Inventor 郑旭
Owner CHINA NUCLEAR JINGHUAN ZIRCONIUM IND
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