Process for manufacturing lower chlorides of titanium

A preparation process, low-valent titanium chloride technology, applied in the direction of titanium trichloride, titanium halide, process efficiency improvement, etc., can solve the problems of expensive process, unmentioned reagent recovery and recycling, complex and other problems

Active Publication Date: 2013-09-11
凯基·霍尔穆斯吉·格哈达
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This makes the process more expensive and complex
Moreover, the process does not mention the recovery and recycling of reagents

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0067] Weigh 700 g of equimolar NaCl and KCl (308 parts of NaCl and 392 parts of KCl) into a clay-graphite reactor. The mixed salts are refined and dried by heating and passing through dry HCl. Finally, the reactor was purged of air with inert argon. The reactor was heated in an electric furnace, and the temperature was slowly raised to 750° C. under an argon atmosphere. About 1400g of titanium tetrachloride liquid is passed into a steel evaporator at a rate of 200g / h. Reducing gas H from cylinder 2 , bubbled through a titanium tetrachloride evaporator. TiCl 4 Steam and H 2 The mixture passes through a ceramic sparger and is bubbled in a molten salt bath. During reduction, TiCl 4 with H 2 The molar ratio was maintained at 1:1. Reduced TiCl 4 , to obtain TiCl in situ 3 , And with alkali metal chlorides, generate chlorine complexes. Condensation of unreacted TiCl 4 , Wash the by-product HCl with dilute lye. According to the change of normal concentration of lye, ca...

Embodiment 2

[0069] Place a graphite crucible in a steel reactor, and prepare 10kg of mixed salt, which contains 32mol% NaCl, 48mol% KCl and 20mol% CaCl 2 . The mixed salt was refined and degassed as described in Example 1. The mixed salts were melted under an inert atmosphere, and the melt temperature was maintained at 700 °C. In molten liquid, with TiCl 4 and H 2 The vapor mixture is bubbling. During reduction, by controlling the TiCl 4 Evaporation and H 2 gas flow rate, maintain TiCl 4 with H 2 The stoichiometric ratio is 1:4. The bubbling and dispersion of the vapor mixture is carried out by placing multiple ceramic dip tubes into the molten bath. Analysis of TiCl 3 content, it was found that the content was 30%, and the efficiency was 96.5%.

Embodiment 3

[0071] In a reduction reactor whose outer layer is clay graphite and inner brick lining, by adding 25mol% CaCl 2 And 75mol% KCl, the preparation of molten bath. The mixed salt (120 kg) was dried and melted with the help of a graphite resistance heater provided at the bottom of the reactor. Seal the reactor with a high temperature rope gasket to prevent gas leakage. During the reduction, the reactor temperature was maintained at 700°C. Through multiple clay-graphite dip tubes, adding TiCl 4 and H 2 Vapor to generate agitation and dispersion in the molten bath. Pass 4500g / h TiCl 4 , with a 1:4 molar ratio of reduced H 2 Together, restore. Unreacted TiCl 4 Condensates in multiple condensers and circulates back to the evaporator. Likewise, excess hydrogen passes through a series of HCl scrubbers and dehydration towers (with a concentrated sulfuric acid cycle) and is recycled back into the reaction system. TiCl 4 to TiCl 3 The conversion rate was confirmed to be 97%.

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PUM

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Abstract

A process for preparation of lower chlorides of titanium is provided, in which titanium tetrachloride (TiCl4) is reduced using a reducing agent in at least one molten alkali metal salt at a temperature of about 300 to about 1400 DEG C to obtain a reduced mass containing lower chlorides of titanium. A process for preparation of titanium metal from the lower chlorides of titanium is also provided.

Description

field of invention [0001] The present invention relates to the preparation of titanium chlorides in a medium containing an electrolyte suitable for the electrochemical production of high purity titanium metal. Background of the invention [0002] Titanium and its alloys have excellent properties such as hardness, corrosion resistance, and high-temperature strength. As strategic metals, they are widely used in many applications including defense and aerospace applications. At present, titanium is produced by metal thermal reduction process. These processes are accompanied by various disadvantages such as: i) these processes are batch processes; ii) these processes have low throughput and high energy consumption; and iii) these processes involve multi-stage treatments to remove impurities. There have been some attempted processes in the past, but none have yet been able to replace existing processes. [0003] In recent years, several other new electrochemical and reduction ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/02C25C3/28C22B34/12
CPCC01G23/02C01G23/026C22B34/1218C25C3/28Y02P10/20
Inventor 凯基·霍尔穆斯吉·格哈达
Owner 凯基·霍尔穆斯吉·格哈达
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