US3139325A - Process for the production of titanium and zirconium hydrogen peroxide products - Google Patents

Process for the production of titanium and zirconium hydrogen peroxide products Download PDF

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Publication number
US3139325A
US3139325A US93326A US9332661A US3139325A US 3139325 A US3139325 A US 3139325A US 93326 A US93326 A US 93326A US 9332661 A US9332661 A US 9332661A US 3139325 A US3139325 A US 3139325A
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United States
Prior art keywords
titanium
hydrogen peroxide
zirconium
hydroxide
group
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
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US93326A
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English (en)
Inventor
Takada Koji
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Toyo Kinzoku kagaku KK
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Toyo Kinzoku kagaku KK
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/56Electroplating: Baths therefor from solutions of alloys
    • C25D3/565Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of zinc
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B15/00Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
    • C01B15/055Peroxyhydrates; Peroxyacids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00Compounds of zirconium
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G25/00Compounds of zirconium
    • C01G25/02Oxides
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/22Electroplating: Baths therefor from solutions of zinc
    • C25D3/24Electroplating: Baths therefor from solutions of zinc from cyanide baths
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/26Electroplating: Baths therefor from solutions of cadmium
    • C25D3/28Electroplating: Baths therefor from solutions of cadmium from cyanide baths
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/56Electroplating: Baths therefor from solutions of alloys

Definitions

  • the main object of the invention is to provide a novel process for the production of titanium and zirconium compound, especially adapted to add to the coating bath in the above proposed coating process.
  • Tetrahyroxide of titanium or zirconium can be obtained, when a solution of tetravalent salts of titanium or zirconium, such as, for instance, titanium tetrafluoride, zirconium tetrafluoride or the like, is subjected to a hydrol ysis in the presence of an alkali.
  • the thus obtained tetrahydroxides are variable in their chamical and physical properties, depending upon the temperature and other conditions during the hydrolysis to a substantial degree.
  • the fluorides, chlorides, sulphates and the like are preferably used as the above mentioned tetravalent salts of titanium or zirconium, while salts of weak acids are liable to be subjected to hydrolysis and thus to form an unwanted titanium or zirconium compounds such as oxy-compounds.
  • solutions of tetravalent compounds of titanium or zirconium, if diluted, are susceptible to hydrolysis. It is thus preferable in the present process to employ concentrations of these solutions lying in the neighborhood of the saturation point.
  • the hydrolysis of tetravalent titanium and zirconium salt is carried out at a temperature lower than 10 C.
  • the temperature of the hydrolyte increases substantially and if the reaction temperature should become higher than 10 C., the produced hydroxides would provide such chemically inactive acids as meta-titanic acid or meta-zirconic acid, which adversely affects the production of the desired stable addition compounds with hydrogen peroxide.
  • the hydrolysis is carried out under suflicient cooling to produce highly reactive hydroxides or ortho-titanic or ortho-zirconic acid, thus capable of producing stable addition compounds with hydrogen peroxide.
  • hydroxides are brought into reaction with the equivalent quantity of hydrogen peroxide, a paste-like substance consisting of titanium or zirconium hydroxide-hydrogen peroxide addition compound is formed, as the case may be.
  • the above mentioned additional compounds dissolve in an alkaline solution to form the peroxide of sodium pertitanate or perziconate, as the case may be.
  • the addition compounds are not only highly stable and persist for long intervals, but also dissolve stably in an alkaline coating bath containing cadmium or zinc, from which the desired alloy coating containing titanium or zirconium can be produced in the conventional way.
  • Example 1 A saturated aqueous solution of titanium tetrafluoride was ice-cooled and kept at a temperature lower than 5 C. An equivalent quantity of caustic soda was added and the resulting mixture was permitted to hydrolyze. The thus produced precipitate was then filtered and mixed with an equivalent quantity of hydrogen peroxide (of 35% concentration) containing 5% of sodium pyrophosphate, thus forming titanium hydroxide-hydrogen peroxide addition compound, which is highly stable. This addition compound was then dissolved in a conventional cyanate bath containing cadmium or zinc, therefrom a titantium alloy coating was produced in the conventional way.
  • Example 2 A saturated aqueous solution of zirconium tetrachloride was ice-cooled and kept at 3 C, and then subjected to hydrolysis in the presence of ammonia and centrifuged. The thus separated precipitate is reacted with an equivalent quantity of hydrogen peroxide (of 35% concentration) containing 3% of sodium pyrophosphate, thus forming zirconium hydroxide-hydrogen peroxide addition compound.
  • This compound together with the titanium additional compound obtained in Example 1 was dissolved in a conventional zinc cyanide and subjected to an electrolysis, thus obtaining a ternary alloy coating containing zinc, titanium and zirconium.
  • Process for the production of titanium and zirconium addition products particularly suited to be added to a plating bath containing a cyanide selected from the group consisting of cadmium cyanide and zinc cyanide comprising: preparing a substantially saturated aqueous solution of a salt of a tetravalent metal selected from the group consisting of titanium and zirconium, said salt being selected from the group consisting of the fluorides, chlorides and sulfates of said tetravalent metal; adding an alkali selected from the group consisting of alkali metal hydroxides and ammonium hydroxide to said aqueous salt solution while maintaining the solution and resulting products at a temperature below 10 C.; physically separating the thereby produced precipitated hydroxide from the remaining liquid; then reacting said hydroxide with a chemically equivalent quantity of hydrogen peroxide in the presence of between 1% and 5% by weight of sodium pyrophosphate based on the hydrogen peroxide; and recovering the metal hydroxide-hydrogen peroxid
  • Schurnb et aL Hydrogen Peroxide, Reinhold Publish- References Clted the file of this Patent ing Corporation, New York, No. 128, pages 540 and UNITED STATES PATENTS 10 541 (-1955).
  • Blumenthal The Chemical Behavior of Zirconium, 1,624,162 Boer P 1927 D. Van Nostrand Co., 111e,, New York, 1958, pages 198- 2,1'41,1s9 Lind Dec.27,1938 2m

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
  • Electroplating And Plating Baths Therefor (AREA)
US93326A 1961-01-28 1961-03-06 Process for the production of titanium and zirconium hydrogen peroxide products Expired - Lifetime US3139325A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP252561 1961-01-28

Publications (1)

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US3139325A true US3139325A (en) 1964-06-30

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US (1) US3139325A (de)
CH (1) CH427757A (de)
DE (1) DE1253987B (de)
GB (1) GB954089A (de)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4529487A (en) * 1983-09-29 1985-07-16 The Boeing Company Coating for increasing corrosion resistance and reducing hydrogen reembrittlement of metal articles
US4612236A (en) * 1983-09-29 1986-09-16 The Boeing Company Coating for increasing corrosion resistance and reducing hydrogen reembrittlement of metal articles
US6267944B1 (en) * 1999-07-05 2001-07-31 Morioki Sangyo Company Limited Method of preparing a solution for titania film

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59111921A (ja) * 1982-12-15 1984-06-28 Sony Corp ジルコニウム酸バリウム微粒子の製造方法

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1624162A (en) * 1924-08-13 1927-04-12 Philips Nv Process for converting hafnium and zirconium phosphates
US2141189A (en) * 1933-12-22 1938-12-27 Henkel & Cie Gmbh Bleaching and cleansing compositions
US2150060A (en) * 1935-06-15 1939-03-07 Firm Henkel & Cie Gmbh Stabilizing color binding agent
US2333444A (en) * 1943-11-02 Method op preparing stable deter

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2333444A (en) * 1943-11-02 Method op preparing stable deter
US1624162A (en) * 1924-08-13 1927-04-12 Philips Nv Process for converting hafnium and zirconium phosphates
US2141189A (en) * 1933-12-22 1938-12-27 Henkel & Cie Gmbh Bleaching and cleansing compositions
US2150060A (en) * 1935-06-15 1939-03-07 Firm Henkel & Cie Gmbh Stabilizing color binding agent

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4529487A (en) * 1983-09-29 1985-07-16 The Boeing Company Coating for increasing corrosion resistance and reducing hydrogen reembrittlement of metal articles
US4612236A (en) * 1983-09-29 1986-09-16 The Boeing Company Coating for increasing corrosion resistance and reducing hydrogen reembrittlement of metal articles
US6267944B1 (en) * 1999-07-05 2001-07-31 Morioki Sangyo Company Limited Method of preparing a solution for titania film

Also Published As

Publication number Publication date
DE1253987B (de) 1967-11-09
GB954089A (en) 1964-04-02
CH427757A (de) 1967-01-15

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