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Purification of titanium tetrachloride

a technology of titanium tetrachloride and titanium tetrachloride, which is applied in the field of titanium tetrachloride purification, can solve the problems of downstream process damage and fouling problems

Inactive Publication Date: 2006-03-09
EI DU PONT DE NEMOURS & CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

[0011] The present invention provides a method in the purification of a crude titanium tetrachloride chlorinator discharge from the carbochlorination of titanium containing materials to minimize the loss of raw materials resulting from passivation of aluminum chloride and vanadium oxychloride, comprising:

Problems solved by technology

They can have a detrimental impact on downstream processes.
Aluminum chloride, for example, is highly corrosive and attacks the metal materials of construction in the equipment downstream of its formation; thus, aluminum chloride must be rendered non-corrosive via treatment with a passivating agent early in the processing of making crude titanium tetrachloride.
Niobium and tantalum chlorides may condense downstream and cause fouling problems.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0038] A round bottomed flask was filled with 100 mL TiCl4, 0.92 g VOCl3 (5.31 mmol), and 0.174 g AlCl3 (1.30 mmol). The AlCl3 was handled air-free to avoid moisture contamination. The reaction mixture was heated to 100° C. Hydrogenated naphthenic oil (ERGON Incorporated's product brand Ergon H-750) was added (1.0333 g). The reaction mixture was held at temperature for 30 minutes. At this point, all of the VOCl3 was passivated, as measured by FTIR. To determine how much unreacted AlCl3 remained, 30 microliter (1.61 mmol) of water were added by syringe. Any AlCl3 in solution would react with the water before TiOCl2 was formed. A total of 1531 ppm TiOCl2 was generated from the water addition, as observed by FTIR. If all of the AlCl3 was present, only 280 ppm should have been observed. Since an extra 1301 ppm TiOCl2 (1.67 mmol) formed, all of the AlCl3 had already been passivated in the solution.

example 2

[0039] A round bottomed flask was filled with 100 mL TiCl4, 0.92 g VOCl3 (5.31 mmol), and 1.74 g AlCl3 (13.0 mmol). The AlCl3 was handled air-free to avoid moisture contamination. The reaction mixture was heated to 100° C. The oil from Example 1 was added (1.0401 g). The reaction mixture was held at temperature for 30 minutes. At this point, all of the VOCl3 was passivated, as measured by FTIR. To determine how much unreacted AlCl3 remained, 290 microliter (16.1 mmol) of water were added by syringe. A total of 6808 ppm TiOCl2 was generated from the water addition. If all of the AlCl3 was still present, only 2371 ppm TiOCl2 should have been observed. Since an extra 4437 ppm TiOCl2 (5.70 mmol) formed, part of the AlCl3 was passivated in the solution. The amount of AlCl3 reacted was stoichiometrically equivalent to the amount of oxygen initially present in solution as part of the VOCl3, within experimental error.

example 3

[0040] Water was added as an aluminum passivating agent to a crude TiCl4 stream containing metal chloride contaminants AlCl3 and VOCl3 produced by the chlorination of titanium-bearing ore, following discharge from the chlorinator and separation of condensable solids. Water addition was in control by the control method described in U.S. Pat. No. 6,562,312. The hydrogenated, naphthenic oil, from Example 1 (vanadium passivating agent) was added to the TiCl4 stream at the same location as the water addition. In contrast to operating the process in the absence of the vanadium passivating agent, the demand for aluminum passivating agent was reduced by 50% while reducing VOCl3 by 20% of its original concentration.

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Abstract

The present invention is a process for reducing raw material yield losses resulting from the passivation aluminum chloride and vanadium chlorides in the chlorinator discharge in a carbochlorination process for making titanium tetrachloride.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS [0001] Cross-reference is made to U.S. Provisional Application No. 60 / 439190 filed on Jan. 9, 2003, which is incorporated herein by reference in its entirety.BACKGROUND OF THE INVENTION [0002] This invention relates to a process for the removal of multiple metal chlorides from a crude titanium tetrachloride stream produced by chlorination of titanium-bearing compounds, and more particularly to a process wherein the removal of multiple metal chlorides occurs in a single reaction vessel. [0003] In the production of titanium tetrachloride, raw materials, including ilmenite or rutile ores or other titanium-containing materials such as those obtained from beneficiating these ores, are reacted with chlorine and carbon (carbochlorination) to yield a mixture of metal chlorides in a crude titanium tetrachloride stream, from which titanium tetrachloride of sufficient purity may be recovered that may be used as a starting material to make titanium metal ...

Claims

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Application Information

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Patent Type & Authority Applications(United States)
IPC IPC(8): C22B34/10C01G23/02
CPCC01G23/024C22B34/1295C22B34/1272C22B34/1222Y02P10/20
Inventor CRONIN, JAMES TIMOTHYELKINS, THOMAS SHIELDSHELBERG, LISA EDITHMIRABELLA, STEVE EDWARDMERKLE, JAMES ELLIOTT
Owner EI DU PONT DE NEMOURS & CO
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