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Metalothermic reduction of refractory metal oxides

A refractory metal and oxide technology, applied in the directions of chromium oxide/hydrate, low-value titanium oxide, titanium oxide/hydroxide, etc. The effect of metal oxide reduction

Inactive Publication Date: 2006-11-01
钽铌欧碧盛创新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] The present invention solves the problem of refractory metal oxide reduction by feeding a mixture of oxidizing and reducing agents directly into the reactor to achieve a self-sustaining highly exothermic reaction (continuous magnesium reduction)

Method used

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  • Metalothermic reduction of refractory metal oxides
  • Metalothermic reduction of refractory metal oxides
  • Metalothermic reduction of refractory metal oxides

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Such as figure 2 As shown, tantalum pentoxide was reduced by gaseous magnesium. The temperature in the magnesium melter is 975°C, while the temperature inside the furnace is maintained at 985°C to prevent condensation in the cold parts. The argon flow through the melter and furnace was 55 standard cubic feet per hour (scfh). The average feed rate of oxide was 1.5 kg / h. Reduction lasted 3 hours. After passivation, the receiver is opened and the product is leached with dilute sulfuric acid to remove residual magnesium and magnesium oxides. The blocks were then dried in an oven at 65°C and analyzed. The reduced powder has a surface area of ​​17m 2 / g, bulk density is 26.8g / in 3 , and the oxygen content is 13.2 W / W%. The inability to maintain consistent oxide and magnesium feed rates resulted in an unstable self-sustaining reaction during the run, whereby the reduction was only 60% complete.

Embodiment 2

[0054] The temperature of the reaction zone was estimated by energy balance calculations, and the results were plotted as a function of mixture feed rate in image 3 . The following assumptions were made:

[0055] (1) The energy loss value is estimated to be 30% of the energy input. This is a reasonable approximation for the furnace design utilized.

[0056] (2) The chemical reaction kinetics are instantaneous and independent of the oxide or magnesium particle size.

[0057] (3) The flow rate of argon is 1.8Nm 3 / hr.

[0058] (4) Furnace temperature is 1150°C.

[0059] image 3 Indicates that the reaction zone temperature can vary significantly with the feed rate. At a mixture feed rate of 7 kg / hr, the reaction zone temperature was indistinguishable from the furnace temperature, while at a feed rate of 30 kg / hr the reaction zone temperature exceeded the melting point of tantalum pentoxide. When the temperature of the reaction zone is above the melting point of the oxid...

Embodiment 3

[0061] Figure 4 represents the reduction of Ta with magnesium powder at several feed rates of the mixture 2 o 5 Furnace power readings in the process as a function of time. The curve represents the power value as a function of mixture feed rate. The higher the feed rate, the greater the reduction in power. In fact, at a mixture feed rate of 20 kg / hr, the electrical power input was reduced from 46% to 6%. In other words, the furnace does not supply energy to the system. This is strong evidence for a stable self-sustaining reaction in the reactor.

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Abstract

High purity refractory metals, valve metals, refractory metals oxides, valve metal oxides, or alloys thereof suitable for a variety of electrical, optical and mill product / fabricated parts usages are produced from their respective oxides by metalothermic reduction of a solid or liquid form of such oxide (18) using a reducing agent that establishes (after ignition) a highly exothermic reaction, the reaction preferably taking place in a continuously or step-wise moving oxide such as gravity fall (24) with metal retrievable at the bottom (30) and an oxide of the reducing agent being removable as a gas or in other convenient form and unreacted reducing agent derivatives being removable by leaching or like process.

Description

[0001] This application is a divisional application of the application number 01823433.X, the application date of the application number 01823433.X is October 11, 2001, and the applicant is H.C. Stark Company. field of invention [0002] The present invention relates to the reduction of corresponding metal oxides to produce tantalum, niobium and other difficult to Melting or valve metal powder (valve metal powder) and low-priced metal oxide (metal suboxide) powder or its alloys to obtain powders with desired morphology and other physical and electrical properties. Background of the invention [0003] Refractory metals belong to a group of elements that are difficult to separate in pure form due to the stability of their compounds such as oxides, chlorides, fluorides. Because the manufacture of refractory metals is very complex, we will use the metallurgy of extracting tantalum as an example to illustrate the development of this t...

Claims

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Application Information

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IPC IPC(8): B22F9/20C01G25/02B22F5/00C01G23/04C01G31/02C01G33/00C01G35/00C01G37/02C01G39/02C01G41/02H01G9/052
CPCB22F9/20B22F2998/00C01G23/043C01G31/02C01G33/00C01G37/02C01G39/02C01G41/02C01P2004/03C01P2004/04C01P2004/50C01P2004/52C01P2004/61C01P2004/62C01P2006/10C01P2006/12C01P2006/17C01P2006/34C01P2006/40C01P2006/80H01G9/0525B22F1/148B22F1/052
Inventor L·N·舍尔特尔T·B·特里普L·L·拉宁A·M·孔伦H·V·戈德伯格
Owner 钽铌欧碧盛创新材料有限公司
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