US2178685A - Decolorizing titanium tetrachloride - Google Patents
Decolorizing titanium tetrachloride Download PDFInfo
- Publication number
- US2178685A US2178685A US188574A US18857438A US2178685A US 2178685 A US2178685 A US 2178685A US 188574 A US188574 A US 188574A US 18857438 A US18857438 A US 18857438A US 2178685 A US2178685 A US 2178685A
- Authority
- US
- United States
- Prior art keywords
- titanium
- tetrachloride
- decolorizing
- titanium tetrachloride
- color
- Prior art date
- 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
Links
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 title description 23
- KPZGRMZPZLOPBS-UHFFFAOYSA-N 1,3-dichloro-2,2-bis(chloromethyl)propane Chemical compound ClCC(CCl)(CCl)CCl KPZGRMZPZLOPBS-UHFFFAOYSA-N 0.000 description 19
- 238000000034 method Methods 0.000 description 14
- 238000010438 heat treatment Methods 0.000 description 9
- 239000010936 titanium Substances 0.000 description 9
- 229910052719 titanium Inorganic materials 0.000 description 9
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 8
- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 description 7
- 150000003609 titanium compounds Chemical class 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- -1 titanium trichloride Chemical compound 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- MJGFBOZCAJSGQW-UHFFFAOYSA-N mercury sodium Chemical compound [Na].[Hg] MJGFBOZCAJSGQW-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910001023 sodium amalgam Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- MTAYDNKNMILFOK-UHFFFAOYSA-K titanium(3+);tribromide Chemical compound Br[Ti](Br)Br MTAYDNKNMILFOK-UHFFFAOYSA-K 0.000 description 1
- SOBXOQKKUVQETK-UHFFFAOYSA-H titanium(3+);trisulfate Chemical compound [Ti+3].[Ti+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O SOBXOQKKUVQETK-UHFFFAOYSA-H 0.000 description 1
- HUYLAMJIPCOVOM-UHFFFAOYSA-K triiodotitanium Chemical compound [Ti+3].[I-].[I-].[I-] HUYLAMJIPCOVOM-UHFFFAOYSA-K 0.000 description 1
Classifications
-
- 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
Definitions
- This invention relates to'the decolorizing oftitanium tetrachloride; 'W'hile'pure titanium tetrachloride is a water White liquid, the product which is obtainedbychlorination of titanium compounds and the commercial products generally available on the market have a distinct"'yellowish cast.
- decolorizing this liquid has been attempted by treatment with certain metals, suchas reduced'iron or sodium amalgam.
- Some decolorizing may be secured in this manner, but in general, it is found that the treated liquid does not remain colorless permanently and that it is contaminated with metallic impurities. This is highly, undesirable" when titanium tetrachloride is being decomposed into ti- ,tanium dioxide pigment, since the metallic impurities tend'to' reduce the whiteness of the pigment produced.
- titanium tetrachloride may be decoloriz ed to form a water white liquid by treatment with lower valent titanium compounds.
- chlorides of titanium such as titanium trichloride, or titanium dichloride.
- other titanium compounds which may be found suitable are titanium tribromide, titanium triiodide, titanous sulfate, etc.
- the treatment may be secured by any convenient method which will insure the required contact. I have found that very satisfactory results may be obtained by vigorously agitating a mixture of titanium tetrachloride and titanium trichloride while heating under a reflux condenser and subsequently distilling and condensing the titanium tetrachloride.
- the concentration of the lower valent titanium salt required depends to a great extent upon the color of the'product being treated. In general, it is preferred to maintain an excess of this salt, and it has been determined that concentrations in excess of about 2.0% titanium trichloride yield satisfactory products in most cases.
- ampZ'-I- 1 OO-parts of yellow'titanium'tetraq a parts of titanium trichloride were vigorously agitatedand heated undera reflux condenser ,at a temperature of 135 C. for a period of The treated mixture was then dis-. 15
- Example IL parts of yellow titanium tetrachloride and 3; parts of titanium trichloride ondenser at a t mperature "of l35f C fora 0
- the treated-mixture was an atrr'iosphere'of dryCOa
- the product produced was Water white.
- Example lIL-lOO parts of yellow titanium 25 tetrachloride and 5 parts of titanium dichloride were vigorously agitated and heated under a re flux condenser at a temperature of C. for a period of two hours. The treated mixture was then distilled rapidly in an atmosphere of dry 30 nitrogen. The product produced was water white.
- Thetitanium compound may be introduced into the tetrachloride in any convenient manner.
- I may reduce a 35 portion of the tetrachloride by suitable means, for example, by introduction of hydrogen, thereby generating the lower valent chloride in situ.
- the compound may be added in the form of a solid or as a solution as desired. Aqueous solutions of the compound preferably should be avoided due to the rapidity with which the tetrachloride hydrolyzes.
- a method of decolorizing colored titanium tetrachloride which comprises contacting the same with a lower valent titanium compound in an amount sufficient and for the time required 65 same with a lower valent titanium-chloride in an amount sufiicient and for the time required to remove at least a substantial portion of the color from the tetrachloride.v Y H 4. A method of decolorizing colored titanium tetrachloride which comprises contacting the Same with titanium trichloride in an amount sufficient and for the time required to remove at least a substantial portion of the color from" the tetrachloride.
- a method of decoloriz'ing colored titanium tetrachloride which comprises heating the same in the presence oi a lower valent titanium compound'iri an amount sufiicient to remove atleast asiibstantial portion of the color from the tetrachloride arid subseqiiently distilling the heated titanium tetraehloride 7.
- a method of decolorizing colored t tan um tetrachloride which comprises heating the same ifi'thepfes'ence Ora lower valent titanium halide in an amount sufiicient to remove at least a substa'ntial portion of the color from the tetrachloride and subsequently distilling the heated titanium tetrachloride.
- a method of decoloriiingcolored titanium tetrachl(' rid 'e which comprises heating the same in the presence of a lower valent titanium chlo ride in an amount suflicient to remove at least a substantial portion of the color from the tetrachloride and subsequently distilling the heated titanium tetrachloride.
- a method of decolorizing colored titanium tetrachloride which comprises heating the same in the presence of titanium trichloride in an *amount sufllcient to remove at least a substantial portion of the color from the tetrachloride and subsequently distilling the heated titanium tetrachloride.
- a method of decolorizing colored titanium tetrachloride which comprises heating the same in the presence of titanium dichloride in an amount sufficient to remove at least a substantial' portion of the color from the tetrachloride and subsequently distilling the heated titanium tetrachloride.
- a method of decolorizing colored titanium tetrachloride which comprises heating the same in the presence of titanium dichloride in an amount sufficient to remove at least a substantial portion of the color from the tetrachloride and subsequently distilling the heated titanium tetrachloride and decolorizing further quantities of titanium tetrachloride by treating said quantities f with the residue from said distillation.
- a method of de'colorizing colored titanium tetrachloride which comprises heating the same with a lower valent titanium compound in an amount sufficient and for thetime required to remove at least a substantial portion of the color from the tetrachloride.
- a method of decolorizin'g colored titamum tetrachloride which comprises heating the same with titanium trichloride in an amount sufficient and for the time required to remove at least a substantial portion of the color from the tetrachloride.
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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)
Description
Patented Nov. 7, 1939 I nEooLoRi'zmo. 1 I oHLoaInn j Frederick-Gage, Akron, 0hio,= assignor to'Pittsv burgh Plate Glass Company, Allegheny County, a
" Pa, a corporati'on of Pennsylv nia l No Drawing. Applicati lil ebr ll a 't i3, I938,
'13 Claims. teller-ti),
This invention relates to'the decolorizing oftitanium tetrachloride; 'W'hile'pure titanium tetrachloride is a water White liquid, the product which is obtainedbychlorination of titanium compounds and the commercial products generally available on the market have a distinct"'yellowish cast. Prior to this'invention, decolorizing this liquidhas been attempted by treatment with certain metals, suchas reduced'iron or sodium amalgam. Some decolorizing may be secured in this manner, but in general, it is found that the treated liquid does not remain colorless permanently and that it is contaminated with metallic impurities. This is highly, undesirable" when titanium tetrachloride is being decomposed into ti- ,tanium dioxide pigment, since the metallic impurities tend'to' reduce the whiteness of the pigment produced.
'l'naccordance with my invention, I have found that titanium tetrachloride may be decoloriz ed to form a water white liquid by treatment with lower valent titanium compounds. I have found that especially effective results may be obtained by treatment with chlorides of titanium, such as titanium trichloride, or titanium dichloride. other titanium compounds which may be found suitable are titanium tribromide, titanium triiodide, titanous sulfate, etc. However, it is preferred to use the lower valent chlorides of titanium in order to avoid contamination of the material.
The treatment may be secured by any convenient method which will insure the required contact. I have found that very satisfactory results may be obtained by vigorously agitating a mixture of titanium tetrachloride and titanium trichloride while heating under a reflux condenser and subsequently distilling and condensing the titanium tetrachloride.
Since the tetrachloride is readily hydrolyzed in a moist atmosphere, it is preferred to carry this process out in the presence of a dry inert gas. Dry carbon dioxide or nitrogen are suitable for this purpose although other gases may be resorted to. I
The concentration of the lower valent titanium salt required depends to a great extent upon the color of the'product being treated. In general, it is preferred to maintain an excess of this salt, and it has been determined that concentrations in excess of about 2.0% titanium trichloride yield satisfactory products in most cases.
The time for which the mixture is refluxed likewise dependsupon the degree of coloration of the product being treated. In general, refluxing QchIOride'and WQ 'h r "tilled rapidly an atmosphere of dry C02. The
were vigorouslyag'itated and heatedl under a"rej'iicr p mow-15 1.0. then distill ed i apidlyln' 'pensed with. The, residue remaining after dis- 5 tillation will;in -general,contain'more or. less .titanous salts and may Ice-reused in aysubseduent treatment offurtheramounts of titanium tetrachloride. p Y N v 1 Thefollowing examples-are illustrat ,ive: 10 'Ea. ampZ'-I- 1 OO-parts of yellow'titanium'tetraq a parts of titanium trichloridewere vigorously agitatedand heated undera reflux condenser ,at a temperature of 135 C. for a period of The treated mixture was then dis-. 15
product produced was water-white.
"Example "IL parts of yellow titanium tetrachloride and 3; parts of titanium trichloride ondenser at a t mperature "of l35f C fora 0 The treated-mixture was an atrr'iosphere'of dryCOa The product produced was Water white.
Example lIL-lOO parts of yellow titanium 25 tetrachloride and 5 parts of titanium dichloride were vigorously agitated and heated under a re flux condenser at a temperature of C. for a period of two hours. The treated mixture was then distilled rapidly in an atmosphere of dry 30 nitrogen. The product produced was water white.
Thetitanium compound may be introduced into the tetrachloride in any convenient manner. By one very efiective method, I may reduce a 35 portion of the tetrachloride by suitable means, for example, by introduction of hydrogen, thereby generating the lower valent chloride in situ. However, the compound may be added in the form of a solid or as a solution as desired. Aqueous solutions of the compound preferably should be avoided due to the rapidity with which the tetrachloride hydrolyzes.
Although the invention has been described in connection with the specific details of certain embodiments thereof, it is not intended that such details shall be regarded as limitations uponthe scope of the invention except insofan as in-- cluded in the accompanying claims.
I claim:
1. A method of decolorizing colored titanium tetrachloride which comprises contacting the same with a lower valent titanium compound in an amount sufficient and for the time required 65 same with a lower valent titanium-chloride in an amount sufiicient and for the time required to remove at least a substantial portion of the color from the tetrachloride.v Y H 4. A method of decolorizing colored titanium tetrachloride which comprises contacting the Same with titanium trichloride in an amount sufficient and for the time required to remove at least a substantial portion of the color from" the tetrachloride.
5. .A method of decoloriz ing colored titanium tetrachloride which comprises contacting the same with titanium dichloride in an amount sufficient and for the time required to remove at least a substantial portion of the color from the tetrachloride.
.6. A method of decoloriz'ing colored titanium tetrachloride which comprises heating the same in the presence oi a lower valent titanium compound'iri an amount sufiicient to remove atleast asiibstantial portion of the color from the tetrachloride arid subseqiiently distilling the heated titanium tetraehloride 7. A method of decolorizing colored t tan um tetrachloride which comprises heating the same ifi'thepfes'ence Ora lower valent titanium halide in an amount sufiicient to remove at least a substa'ntial portion of the color from the tetrachloride and subsequently distilling the heated titanium tetrachloride.
8. A method of decoloriiingcolored titanium tetrachl(' rid 'e which comprises heating the same in the presence of a lower valent titanium chlo ride in an amount suflicient to remove at least a substantial portion of the color from the tetrachloride and subsequently distilling the heated titanium tetrachloride.
9. A method of decolorizing colored titanium tetrachloride which comprises heating the same in the presence of titanium trichloride in an *amount sufllcient to remove at least a substantial portion of the color from the tetrachloride and subsequently distilling the heated titanium tetrachloride.
10. A method of decolorizing colored titanium tetrachloride which comprises heating the same in the presence of titanium dichloride in an amount sufficient to remove at least a substantial' portion of the color from the tetrachloride and subsequently distilling the heated titanium tetrachloride.
11. A method of decolorizing colored titanium tetrachloride which comprises heating the same in the presence of titanium dichloride in an amount sufficient to remove at least a substantial portion of the color from the tetrachloride and subsequently distilling the heated titanium tetrachloride and decolorizing further quantities of titanium tetrachloride by treating said quantities f with the residue from said distillation.
12. A method of de'colorizing colored titanium tetrachloride which comprises heating the same with a lower valent titanium compound in an amount sufficient and for thetime required to remove at least a substantial portion of the color from the tetrachloride.
v13. A method of decolorizin'g colored titamum tetrachloride which comprises heating the same with titanium trichloride in an amount sufficient and for the time required to remove at least a substantial portion of the color from the tetrachloride.
FREDERICK GAGE.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US188574A US2178685A (en) | 1938-02-03 | 1938-02-03 | Decolorizing titanium tetrachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US188574A US2178685A (en) | 1938-02-03 | 1938-02-03 | Decolorizing titanium tetrachloride |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2178685A true US2178685A (en) | 1939-11-07 |
Family
ID=22693714
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US188574A Expired - Lifetime US2178685A (en) | 1938-02-03 | 1938-02-03 | Decolorizing titanium tetrachloride |
Country Status (1)
| Country | Link |
|---|---|
| US (1) | US2178685A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2512807A (en) * | 1947-09-23 | 1950-06-27 | Nicholson Douglas Gillison | Purification of titanium halides |
| US2543591A (en) * | 1950-06-20 | 1951-02-27 | Stauffer Chemical Co | Purification of titanium tetrachloride |
| US2677592A (en) * | 1943-06-10 | 1954-05-04 | Atomic Energy Commission | Process of producing uranium tetrachloride |
| US2682451A (en) * | 1943-10-07 | 1954-06-29 | Atomic Energy Commission | Still |
| US2691571A (en) * | 1952-09-25 | 1954-10-12 | Du Pont | Titanium dioxide manufacture |
| US2706153A (en) * | 1951-04-19 | 1955-04-12 | Kennecott Copper Corp | Method for the recovery of titanium |
| US2725278A (en) * | 1943-12-13 | 1955-11-29 | Milton J Polissar | Manufacture of uranium tetrachloride |
| US2735746A (en) * | 1956-02-21 | Method of producing uranium tetrachloride | ||
| US2754255A (en) * | 1952-05-27 | 1956-07-10 | Nat Lead Co | Decolorizing titanium tetrachloride |
| US2890100A (en) * | 1957-01-31 | 1959-06-09 | Titanium Metals Corp | Purification of crude titanium tetrachloride |
| US2915364A (en) * | 1956-05-25 | 1959-12-01 | Clabaugh Wilbur Stanley | Preparation of pure titanium tetrachloride |
| US3253885A (en) * | 1963-05-23 | 1966-05-31 | Titanium Metals Corp | Purification of crude titanium tetrachloride |
-
1938
- 1938-02-03 US US188574A patent/US2178685A/en not_active Expired - Lifetime
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2735746A (en) * | 1956-02-21 | Method of producing uranium tetrachloride | ||
| US2677592A (en) * | 1943-06-10 | 1954-05-04 | Atomic Energy Commission | Process of producing uranium tetrachloride |
| US2682451A (en) * | 1943-10-07 | 1954-06-29 | Atomic Energy Commission | Still |
| US2725278A (en) * | 1943-12-13 | 1955-11-29 | Milton J Polissar | Manufacture of uranium tetrachloride |
| US2512807A (en) * | 1947-09-23 | 1950-06-27 | Nicholson Douglas Gillison | Purification of titanium halides |
| US2543591A (en) * | 1950-06-20 | 1951-02-27 | Stauffer Chemical Co | Purification of titanium tetrachloride |
| US2706153A (en) * | 1951-04-19 | 1955-04-12 | Kennecott Copper Corp | Method for the recovery of titanium |
| US2754255A (en) * | 1952-05-27 | 1956-07-10 | Nat Lead Co | Decolorizing titanium tetrachloride |
| US2691571A (en) * | 1952-09-25 | 1954-10-12 | Du Pont | Titanium dioxide manufacture |
| US2915364A (en) * | 1956-05-25 | 1959-12-01 | Clabaugh Wilbur Stanley | Preparation of pure titanium tetrachloride |
| US2890100A (en) * | 1957-01-31 | 1959-06-09 | Titanium Metals Corp | Purification of crude titanium tetrachloride |
| US3253885A (en) * | 1963-05-23 | 1966-05-31 | Titanium Metals Corp | Purification of crude titanium tetrachloride |
| DE1237081B (en) * | 1963-05-23 | 1967-03-23 | Nat Lead Co | Process for purifying titanium tetrachloride containing vanadyl chloride |
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