US20130280149A1 - Purification of Titanium Tetrachloride - Google Patents

Purification of Titanium Tetrachloride Download PDF

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Publication number
US20130280149A1
US20130280149A1 US13/838,254 US201313838254A US2013280149A1 US 20130280149 A1 US20130280149 A1 US 20130280149A1 US 201313838254 A US201313838254 A US 201313838254A US 2013280149 A1 US2013280149 A1 US 2013280149A1
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US
United States
Prior art keywords
feedstock
sorbent material
impurity
oxychlorides
chlorides
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Abandoned
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US13/838,254
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English (en)
Inventor
Bela Derecskei
Alexandre Jean Fines
Alastair Valentine
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Ineos Pigments USA Inc
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Cristal USA Inc
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Publication date
Application filed by Cristal USA Inc filed Critical Cristal USA Inc
Priority to US13/838,254 priority Critical patent/US20130280149A1/en
Publication of US20130280149A1 publication Critical patent/US20130280149A1/en
Assigned to CRISTAL USA INC. reassignment CRISTAL USA INC. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: DERECSKEI, Bela, FINES, ALEXANDRE J., VALENTINE, ALASTAIR
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G23/00—Compounds of titanium
    • C01G23/02—Halides of titanium
    • C01G23/022—Titanium tetrachloride
    • C01G23/024—Purification of tetrachloride
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Definitions

  • the presently disclosed and claimed inventive process(es), procedure(s), method(s), product(s), result(s) and/or concept(s) (collectively hereinafter referenced to as the “presently disclosed and claimed inventive concept(s)”) relates generally to processes and systems for purifying titanium tetrachloride. More specifically, the presently disclosed and claimed inventive concept(s) relates to the removal of chloride or oxychloride metal contaminants from titanium tetrachloride using a sorbent material.
  • Titanium tetrachloride (TiCl 4 ) is produced from the chlorination of titaniferous ores.
  • the manufacture of high purity TiCl 4 has become more challenging due to the limited supply, and resulting high costs, of high purity titanium ores. While the use of lower cost and more abundant lower grade ores would be preferable, such would require additional steps or unit operations, such as more extensive distillation, to manufacture the same purity of TiCl 4 . It is generally desirable to keep this purification process simple and of low cost.
  • a titanium tetrachloride purification process comprises:
  • the sorbent material comprises a member selected from the group consisting of an alumino-silicate, activated alumina, ultrafine TiO2, and combinations thereof
  • the at least one impurity comprises a member selected from the group consisting of carbonyl sulfide, sulfur dioxide, phosgene, hydrogen sulfide, carbon disulfide, chlorides of: aluminum, carbon, gallium, indium, tin, thallium, lead, bismuth, polonium, boron, silicon, germanium, arsenic, antimony, tellurium, zirconium, hafnium, iron, chromium, copper, magnesium, vanadium, nickel, thorium, uranium, oxychlorides of: aluminum, bismuth, arsenic, antimony, zirconium, ha
  • FIG. 1 is a chart showing % impurity removal from TiCl 4 for various zeolites and impurities.
  • inventive concept(s) Before explaining at least one embodiment of the inventive concept(s) disclosed herein in detail, it is to be understood that the presently disclosed and claimed inventive concept(s), process(es), methodology(ies) and/or outcome(s) is not limited in its application to the details of construction and the arrangement of the components or steps or methodologies set forth in the following description or illustrated in the drawings.
  • inventive concept(s), process(es), methodology(ies) and/or outcome(s) disclosed herein is capable of other embodiments or of being practiced or carried out in various ways.
  • the titaniferous ores useful in the presently disclosed and claimed inventive concept(s) can be any titaniferous ores capable of being chlorinated to produce sufficient quantities of TiCl 4 .
  • a feedstock comprising titanium tetrachloride and at least one impurity can be contacted, preferably in a contacting vessel, with a sorbent material comprising a member selected from the group consisting of an alumino-silicate, activated alumina, ultrafine TiO2, and combinations thereof to form a product stream.
  • the sorbent material can further comprise activated carbon.
  • the at least one impurity can be any impurity commonly present in a titanium tetrachloride stream obtained from the chlorination of a titaniferous ore.
  • impurities include or comprise carbonyl sulfide, sulfur dioxide, phosgene, hydrogen sulfide, carbon disulfide, chlorides of: aluminum, carbon, gallium, indium, tin, thallium, lead, bismuth, polonium, boron, silicon, germanium, arsenic, antimony, tellurium, zirconium, hafnium, iron, chromium, copper, magnesium, vanadium, nickel, thorium, uranium, and oxychlorides of: aluminum, bismuth, arsenic, antimony, zirconium, hafnium, chromium, vanadium, uranium, either individually or in combination of two or more thereof and combinations thereof.
  • chlorides of tin are generally present as an impurity in the form of SnCl 4 , but can also include SnCl 2 . The product stream is then withdrawn from the contacting vessel.
  • the feedstock may be in various forms.
  • the feedstock may be in the form of a vapor or liquid, either individually or in a combination thereof.
  • the titanium tetrachloride comprises an anhydrous form when contacted with the alumino-silicate.
  • the titanium tetrachloride comprises an aqueous form when contacted with the alumino-silicate.
  • the at least one impurity can be present in the feedstock in the range of from about 0.1 to about 10,000 ppmw, or from about 5 to about 1000 ppmw.
  • the resulting product stream can contain less than about 80 weight %, or less than about 50 weight %, or less than about 20 weight % of the impurity(ies) contained in the feedstock.
  • impurities include or comprise chlorides of tin, arsenic, antimony, zirconium, and oxychlorides of arsenic, antimony, zirconium, either individually or in combinations of two or more thereof.
  • the feedstock can comprise in the range of from about 1 to about 500 ppmw, or from about 1 to about 200 ppmw, of combined chlorides of tin comprising tin dichloride.
  • the product stream can contain less than about 20 weight %, or less than about 10 weight %, of the tin dichloride contained in the feedstock.
  • the feedstock can comprise in the range of from about 0.1 to about 500, or from about 1 to about 200 ppmw, or from about 0.1 to about 20 ppmw, of combined chlorides and oxychlorides of arsenic.
  • the product stream can contain less than about 20 weight %, or less than about 10 weight %, of the combined chlorides and oxychlorides of arsenic contained in the feedstock.
  • the feedstock can comprise in the range of from about 0.1 to about 500, or from about 1 to about 200 ppmw, or from about 0.1 to about 20 ppmw, of combined chlorides and oxychlorides of antimony.
  • the product stream can contain less than about 20 weight %, or less than about 10 weight %, of the combined chlorides and oxychlorides of antimony contained in the feedstock.
  • the feedstock can comprise in the range of from about 0.1 to about 100 ppmw, or from about 0.1 to about 10 ppmw, of combined chlorides and oxychlorides of zirconium.
  • the product stream can contain less than about 20 weight %, or less than about 10 weight %, of the combined chlorides and oxychlorides of zirconium contained in the feedstock.
  • the alumino-silicate can have a surface area greater than about 200 m 2 /g, or greater than about 600 m 2 /g. Also, the alumino-silicate can have an average channel size in the range of from about 4.5 to about 9.5 ⁇ , or in the range of from about 6.5 to about 7.5 ⁇ ; and can have an alkali content in the range of from about 0.02 to about 0.2 wt %, or in the range of from about 0.025 to about 0.04.
  • the silica to alumina ratio of the alumino-silicate can be in the range of from about 30 to about 100, or from about 60 to about 85. More particularly, the alumino-silicate includes or comprises a zeolite material, more particularly a faujasite zeolite.
  • the contacting of the sorbent material with the feedstock can comprise contacting the sorbent material with the feedstock in a single vessel; removing the sorbent material from the vessel; and disposing the sorbent material once spent. This cycle can then be repeated.
  • the contacting of the sorbent material with the feedstock can comprise i) contacting the sorbent material with the feedstock in a single vessel until the sorbent material is spent forming a spent sorbent material; stopping contact with the feedstock in step a) until the spent sorbent material is regenerated into a regenerated sorbent material; and iii) contacting the regenerated sorbent material with the feedstock. This cycle can then be repeated.
  • the contacting of the sorbent material with the feedstock can comprise contacting the sorbent material with the feedstock in a system containing multiple vessels, and wherein the contacting of the sorbent material with the feedstock can comprise sequentially charging the feedstock to the vessels and regenerating the sorbent material in each of the vessels upon becoming spent. This cycle can then be repeated.
  • the regeneration of the sorbent material can be accomplished by contacting the spent sorbent material with a flow of either inert gas or TiCl 4 , or mixtures thereof, at elevated temperatures.
  • a titanium ore of relatively low grade such as, but not limited to, a titanium ore comprising titanium oxide, iron oxide, and at least 3 wt %, or at least 4 wt %, of the at least one impurity, can be chlorinated to form the feedstock.
  • the product stream can be reacted with oxygen to form pigmentary titanium dioxide.
  • the product stream can also be reacted with a metal selected from the group consisting of sodium, magnesium, or combinations thereof, to form titanium metal.
  • the alumino-silicate can be selected for the removal of a specific one of the impurities or specific groups of the impurities based on: i) the geometric size of the impurity or impurities, ii) the channel size of the alumino-silicate material, iii) at least one property of the alumino-silicate material such as, but not limited to, polarity, and iv) combinations thereof.
  • Table 1 lists approximate molecular diameters for various impurities, for titanium tetrachloride, and the approximate average channel size for a faujasite zeolite (FAU).
  • Zeolite 1 Product designation CP 811C-300 Zeolite 2—Product designation CP 814C Zeolite 3—Product designation CBV-901

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
  • Catalysts (AREA)
US13/838,254 2012-04-20 2013-03-15 Purification of Titanium Tetrachloride Abandoned US20130280149A1 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
US13/838,254 US20130280149A1 (en) 2012-04-20 2013-03-15 Purification of Titanium Tetrachloride

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US201261636156P 2012-04-20 2012-04-20
US13/838,254 US20130280149A1 (en) 2012-04-20 2013-03-15 Purification of Titanium Tetrachloride

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US14/395,742 Active 2033-10-25 US9731979B2 (en) 2012-04-20 2013-04-15 Purification of titanium tetrachloride

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US (2) US20130280149A1 (da)
EP (1) EP2838850B1 (da)
JP (1) JP6226208B2 (da)
CN (1) CN104379508B (da)
AU (1) AU2013249586B2 (da)
DK (1) DK2838850T3 (da)
ES (1) ES2902408T3 (da)
IN (1) IN2014DN08593A (da)
PL (1) PL2838850T3 (da)
SI (1) SI2838850T1 (da)
WO (1) WO2013158525A1 (da)

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CN103818952B (zh) * 2014-03-03 2015-07-08 攀钢集团攀枝花钢铁研究院有限公司 除去粗四氯化钛中钒杂质的方法及精制粗四氯化钛的方法
KR102516883B1 (ko) 2016-08-04 2023-04-03 삼성전자주식회사 차폐 구조를 포함하는 전자 장치
CN108328652A (zh) * 2018-03-28 2018-07-27 河南佰利联新材料有限公司 一种节能的四氯化钛精制方法
CN112758977B (zh) * 2020-12-31 2023-06-23 仙桃市中星电子材料有限公司 一种降低四氯化钛锡含量的方法
CN112645381A (zh) * 2020-12-31 2021-04-13 仙桃市中星电子材料有限公司 一种降低四氯化钛中碳含量的方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2834667A (en) * 1954-11-10 1958-05-13 Dominion Magnesium Ltd Method of thermally reducing titanium oxide
US3421917A (en) * 1966-04-28 1969-01-14 Dresser Ind Aluminosilicate refractory brick
US3760071A (en) * 1971-01-08 1973-09-18 Ppg Industries Inc PROCESS FOR TREATING BY-PRODUCT TITANIUM TETRACHLORIDE FROM PYROGENIC TiO{11 {11 PRODUCTION
JPS60264327A (ja) * 1984-06-14 1985-12-27 Mitsui Toatsu Chem Inc 四塩化チタンの脱色方法
US20070104638A1 (en) * 2005-04-11 2007-05-10 Cronin James T Process for purifying titanium chloride-containing feedstock
US7341665B2 (en) * 2003-12-22 2008-03-11 Enitecnologie S.P.A. Process for the treatment of contaminated water based on the use of apolar zeolites having different characteristics
US20140151303A1 (en) * 2010-11-05 2014-06-05 Eni S.P.A. Process for the treatment of contaiminated water by means of adsorption and nanofiltration

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* Cited by examiner, † Cited by third party
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US2207597A (en) * 1938-10-27 1940-07-09 Pittsburgh Plate Glass Co Decolorizing titanium tetrachloride
GB1360587A (en) * 1971-12-27 1974-07-17 Sir Soc Italiana Resine Spa Process for the purification of titanium tetrachloride
US4994191A (en) * 1989-10-10 1991-02-19 Engelhard Corporation Removal of heavy metals, especially lead, from aqueous systems containing competing ions utilizing wide-pored molecular sieves of the ETS-10 type
EP0457988A1 (en) * 1990-05-25 1991-11-27 Engelhard Corporation Removal of heavy metals from aqueous systems
US6395070B1 (en) * 1998-10-06 2002-05-28 Matheson Tri-Gas, Inc. Methods for removal of impurity metals from gases using low metal zeolites
US20020179427A1 (en) * 2001-05-21 2002-12-05 Goddard John Burnham Process for purifying titanium tetrachloride
US6770254B2 (en) * 2002-01-17 2004-08-03 Air Products And Chemicals, Inc. Purification of group IVb metal halides
US7368096B2 (en) * 2005-06-07 2008-05-06 E.I. Du Pont De Nemours And Company Process for separating solids from a purification purge stream
JP5083950B2 (ja) * 2007-07-02 2012-11-28 株式会社大阪チタニウムテクノロジーズ ＴｉＣｌ４製造方法

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2834667A (en) * 1954-11-10 1958-05-13 Dominion Magnesium Ltd Method of thermally reducing titanium oxide
US3421917A (en) * 1966-04-28 1969-01-14 Dresser Ind Aluminosilicate refractory brick
US3760071A (en) * 1971-01-08 1973-09-18 Ppg Industries Inc PROCESS FOR TREATING BY-PRODUCT TITANIUM TETRACHLORIDE FROM PYROGENIC TiO{11 {11 PRODUCTION
JPS60264327A (ja) * 1984-06-14 1985-12-27 Mitsui Toatsu Chem Inc 四塩化チタンの脱色方法
US7341665B2 (en) * 2003-12-22 2008-03-11 Enitecnologie S.P.A. Process for the treatment of contaminated water based on the use of apolar zeolites having different characteristics
US20070104638A1 (en) * 2005-04-11 2007-05-10 Cronin James T Process for purifying titanium chloride-containing feedstock
US20140151303A1 (en) * 2010-11-05 2014-06-05 Eni S.P.A. Process for the treatment of contaiminated water by means of adsorption and nanofiltration

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Publication number Publication date
SI2838850T1 (sl) 2022-02-28
CN104379508B (zh) 2017-04-19
PL2838850T3 (pl) 2022-03-07
EP2838850B1 (en) 2021-10-20
IN2014DN08593A (da) 2015-05-22
JP2015514671A (ja) 2015-05-21
JP6226208B2 (ja) 2017-11-08
EP2838850A1 (en) 2015-02-25
ES2902408T3 (es) 2022-03-28
CN104379508A (zh) 2015-02-25
US9731979B2 (en) 2017-08-15
WO2013158525A1 (en) 2013-10-24
EP2838850A4 (en) 2016-01-13
US20150064100A1 (en) 2015-03-05
AU2013249586A1 (en) 2014-11-06
AU2013249586B2 (en) 2016-08-25
DK2838850T3 (da) 2021-12-13

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Owner name: CRISTAL USA INC., MARYLAND

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:DERECSKEI, BELA;FINES, ALEXANDRE J.;VALENTINE, ALASTAIR;REEL/FRAME:033883/0012

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