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 PDFInfo
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- 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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- Prior art keywords
- titanium
- hydrogen peroxide
- zirconium
- hydroxide
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- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 title claims description 22
- 229910052719 titanium Inorganic materials 0.000 title claims description 22
- 239000010936 titanium Substances 0.000 title claims description 22
- 238000000034 method Methods 0.000 title claims description 14
- 230000008569 process Effects 0.000 title claims description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- RQFMCJMUOOBOCQ-UHFFFAOYSA-N OO.[Zr] Chemical compound OO.[Zr] RQFMCJMUOOBOCQ-UHFFFAOYSA-N 0.000 title description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 26
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 13
- 229910052726 zirconium Inorganic materials 0.000 claims description 13
- 150000003839 salts Chemical class 0.000 claims description 11
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 6
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 6
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 6
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 5
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- GTLDTDOJJJZVBW-UHFFFAOYSA-N zinc cyanide Chemical compound [Zn+2].N#[C-].N#[C-] GTLDTDOJJJZVBW-UHFFFAOYSA-N 0.000 claims description 4
- NHMJUOSYSOOPDM-UHFFFAOYSA-N cadmium cyanide Chemical compound [Cd+2].N#[C-].N#[C-] NHMJUOSYSOOPDM-UHFFFAOYSA-N 0.000 claims description 3
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 3
- XFXPMWWXUTWYJX-UHFFFAOYSA-N Cyanide Chemical compound N#[C-] XFXPMWWXUTWYJX-UHFFFAOYSA-N 0.000 claims description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims description 2
- QOSATHPSBFQAML-UHFFFAOYSA-N hydrogen peroxide;hydrate Chemical compound O.OO QOSATHPSBFQAML-UHFFFAOYSA-N 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 238000007747 plating Methods 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims 1
- 150000001875 compounds Chemical class 0.000 description 11
- 238000000576 coating method Methods 0.000 description 9
- 230000007062 hydrolysis Effects 0.000 description 8
- 238000006460 hydrolysis reaction Methods 0.000 description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 5
- 239000002253 acid Substances 0.000 description 5
- -1 on the one hand Chemical compound 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- 229910052725 zinc Inorganic materials 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 229910052793 cadmium Inorganic materials 0.000 description 4
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 description 4
- 150000007513 acids Chemical class 0.000 description 3
- 150000004679 hydroxides Chemical class 0.000 description 3
- 150000003755 zirconium compounds Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000012670 alkaline solution Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 150000002222 fluorine compounds Chemical class 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XROWMBWRMNHXMF-UHFFFAOYSA-J titanium tetrafluoride Chemical class [F-].[F-].[F-].[F-].[Ti+4] XROWMBWRMNHXMF-UHFFFAOYSA-J 0.000 description 2
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SYSQUGFVNFXIIT-UHFFFAOYSA-N n-[4-(1,3-benzoxazol-2-yl)phenyl]-4-nitrobenzenesulfonamide Chemical class C1=CC([N+](=O)[O-])=CC=C1S(=O)(=O)NC1=CC=C(C=2OC3=CC=CC=C3N=2)C=C1 SYSQUGFVNFXIIT-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 150000003754 zirconium Chemical class 0.000 description 1
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 description 1
- OMQSJNWFFJOIMO-UHFFFAOYSA-J zirconium tetrafluoride Chemical class F[Zr](F)(F)F OMQSJNWFFJOIMO-UHFFFAOYSA-J 0.000 description 1
- HAIMOVORXAUUQK-UHFFFAOYSA-J zirconium(iv) hydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Zr+4] HAIMOVORXAUUQK-UHFFFAOYSA-J 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/565—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of zinc
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/055—Peroxyhydrates; Peroxyacids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/22—Electroplating: Baths therefor from solutions of zinc
- C25D3/24—Electroplating: Baths therefor from solutions of zinc from cyanide baths
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/26—Electroplating: Baths therefor from solutions of cadmium
- C25D3/28—Electroplating: Baths therefor from solutions of cadmium from cyanide baths
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: 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)
- Metallurgy (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electrolytic Production Of Non-Metals, Compounds, Apparatuses Therefor (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
United States Patent 3,139,325 PROCES FOR THE PRODUCTION OF TITANIUM AND ZIRCONIUM HYDROGEN PEROXIDE PRODUCTS K 7i Takada, Shinjuku-ku, Tokyo, Japan, assignor to Toyo Kinzokukagaku Kabushikikaisha, Tokyo, Japan No Drawing. Filed Mar. 6, 1961, Ser. No. 93,326 Claims priority, application Japan Jan. 28, 1961 4 Claims. (Cl. 23-14) The invention relates to a novel process for the production of titanium and zirconium compounds, for use in the formation of alloy coatings consisting of cadmium or zinc, on the one hand, and titanium or zirconium, on the other hand.
It has been already proposed by me to produce alloy coatings of the kind above referred to in such a way that a pertitanate and a perzirconate is dissolved in a conventional coating bath containing cadmium cyanide or zinc cyanide and the electrolysis is carried out with use of cadmium or zinc as anode.
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. Thus, there are a plurality of isomers of tetrahydroxides of titanium and zirconium. It is, therefore, the more specific object of the invention to provide a novel process for the production of such titanium or zirconium tetrahydroxide which easily reacts with hydrogen peroxide to form the corresponding addition product liable to solve stably in an alkaline solution and thereby to form the pertitanate or perzirconate. According to my profound experiments, salts of strong acids, such as,
for instance, 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. On the other hand, 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.
According to the invention, the hydrolysis of tetravalent titanium and zirconium salt is carried out at a temperature lower than 10 C. In the course of the alkaline hydrolysis, 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.
According to the invention, 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. When the thus produced 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.
3,139,325 Patented June 30, 1964 ice j In the process according to the invention, 1-5 of sodium pyrophosphate is added in the above mentioned stage to the hydrogen peroxide, which measure constitutes a feature of the invention. It was now found that the pyrophosphatereacts with hydrogen peroxide to form the peroxide of sodium pyrophosphate, which serves for stabilization of the titanium compound.
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.
The invention can be more fully understood with reference to the following several examples:
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.
Although for the purpose of explaining the invention certain particular examples thereof have been disclosed, obvious modifications will occur to a person skilled in the art, and it is not desired to be limited to the exact details described.
What is claimed and desired to be secured by Letters Patent is:
1. 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, said process 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 peroxide addition product, so produced.
a a 4, 2. The process of claim 1, where in the salt is titanium 2,150,060 Guttenberg et a1 Mar. 7, 1939 tetrafiuoride. 2,333,444 Robinson Nov. 2, 1943 3. The process of claim 1 wherein the salt is zir- OTHER REFERENCES coniurn tetrachloride.
4. The process of claim" 1 wherein the hydrolysis is 5 Mellon Comprehensive Treatls? 011 Inorganlc arm carried out in the presence of caustic soda addedto said B hcal CheImstry, Longmans, Green and Co., New York, aqueous salt sslution. V 1927, vol. VII, pages 130 t0.132.
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
Claims (1)
1. 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, SAID PROCESS 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 AND SAID TETRAVALENT METAL; ADDING AN ALKALI SELECTED FROM THE GROUP CONSISTING OF ALKALI METAL HYDROXIDES AND AMMINOUM 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 PEROXIDE ADDITION PRODUCT, SO PRODUCED.
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP252561 | 1961-01-28 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US3139325A true US3139325A (en) | 1964-06-30 |
Family
ID=11531779
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US93326A Expired - Lifetime US3139325A (en) | 1961-01-28 | 1961-03-06 | Process for the production of titanium and zirconium hydrogen peroxide products |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US3139325A (en) |
| CH (1) | CH427757A (en) |
| DE (1) | DE1253987B (en) |
| GB (1) | GB954089A (en) |
Cited By (3)
| 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)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59111921A (en) * | 1982-12-15 | 1984-06-28 | Sony Corp | Production of fine particles of barium zirconate |
Citations (4)
| 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 |
-
1961
- 1961-03-06 US US93326A patent/US3139325A/en not_active Expired - Lifetime
- 1961-08-12 DE DET20619A patent/DE1253987B/en active Pending
- 1961-08-18 GB GB29944/61A patent/GB954089A/en not_active Expired
- 1961-09-01 CH CH1020161A patent/CH427757A/en unknown
Patent Citations (4)
| 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)
| 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 (en) | 1967-11-09 |
| GB954089A (en) | 1964-04-02 |
| CH427757A (en) | 1967-01-15 |
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