US3486847A - Process for automatically regulating the reduction of the iron and titanium values in a digestion liquor - Google Patents
Process for automatically regulating the reduction of the iron and titanium values in a digestion liquor Download PDFInfo
- Publication number
- US3486847A US3486847A US3486847DA US3486847A US 3486847 A US3486847 A US 3486847A US 3486847D A US3486847D A US 3486847DA US 3486847 A US3486847 A US 3486847A
- Authority
- US
- United States
- Prior art keywords
- reduction
- iron
- titanium
- digestion
- liquor
- 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
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/12—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08
- C22B34/1236—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching
- C22B34/1259—Obtaining titanium or titanium compounds from ores or scrap by metallurgical processing; preparation of titanium compounds from other titanium compounds see C01G23/00 - C01G23/08 obtaining titanium or titanium compounds from ores or scrap by wet processes, e.g. by leaching treatment or purification of titanium containing solutions or liquors or slurries
-
- G—PHYSICS
- G05—CONTROLLING; REGULATING
- G05D—SYSTEMS FOR CONTROLLING OR REGULATING NON-ELECTRIC VARIABLES
- G05D21/00—Control of chemical or physico-chemical variables, e.g. pH value
- G05D21/02—Control of chemical or physico-chemical variables, e.g. pH value characterised by the use of electric means
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Definitions
- the invention covers a process for the continuous and fully automatic reduction of the iron and titanium values in digestion of liquors produced from titanium ores, titanium ore concentrates and titanium slags with the aid of a regulating device which controls the rate of flow of the digestion liquor through a reductor filled with a reducing agent by measuring the oxidation-reduction potential of the liquor which is dependent upon the amount of tri-valent titanium ions formed during the reduction.
- the control of the Ti value must therefore always be carried out; it is mostly carried out by titration with an iron (III) sulfate solution of known content using thiocyanate solution as indicator.
- This analytical method of determination requires quite some time so that a rapid and/or continuous reduction is not very well controllable in this manner.
- FIGURE 1 is presented to show the rapid jump in potential which takes place in an iron sulfate-titanium sulfate solution when all of the iron values have been reduced to the ferrous state and a small amount of trivalent titanium is formed.
- FIGURE 2 represents a schematic drawing of apparatus for carrying out the continuous and automatic reduction of the iron sulfate-titanium sulfate solution to obtain the desirable degree of reduction.
- the degree of reduction is measured by the oxidation-reduction potential of the solution.
- the amount of Ti+ reduced to Ti+ is measured exactly and rapidly by a change in the potential.
- the dependence of the oxidation-reduction potential T i +/Ti is surprisingly large in the range up to about 5 g.p.l. Ti calculated as TiO so that it is easily possible to coordinate each measured potential with a definite content of Ti ions.
- the potential curve must, of course, be determined separately for each digestion liquor produced according to a particular digestion process from a particular titaniferous material. However with each identical starting material and identical digestion procedure, the same standardizing curve may be used each time.
- Such an automatic control of the continuous reduction may be carried out, for example, by means of the apparatus described in FIG. 2.
- the apparatus consists of a bufl er and mixing tank 2 fitted with a stirrer.
- the unreduced digestion liquor is fed into this mixing tank through the inlet 1.
- the amount of liquor fed may be regulated by valve V
- the sufi'iciently reduced liquor is transferred from the mixing tank into the clarifying tank through outlet 11, whereby the effluent amount may also be controlled by valve V
- the liquor is pumped through pipe 3 from the mixing tank 2 into the reductor 5 by means of pump 4 for reduction; the reductor has a vent 6.
- the amount flowing through is regulated by valve V From there the reduced solution flows through pipe 7 again into the mixing tank 2 into which the electrodes 8 connected with the potentiometer 9 are immersed directly in front of the outlet.
- the potentiometer is connected with the regulator 10 which controls the regulating valves V V and V
- the unreduced digestion liquor coming from the digestion tank is brought to the temperature necessary for reduction and collected in the mixing tank. From there it is pumped in portions into the reductor which is filled with loose scrap iron, where it emanates from a ring-shaped pipe with many bore holes like a sprinkler, and flows over the scrap iron.
- the reductor which is expediently suspended in an elevated frame, can be refilled with scrap iron from above.
- the reduced solution is recycled into the mixing tank again through the bottom outlet of the reductor and mixed there with the remaining solution.
- the potential of this solution measured by the oxidation-reduction electrode measuring device is indicated by the potentiometer and effects the control of the regulating valve V via the regulator, whereby the ratio of flow through the reductor to the total amount of flow through the mixing tank is regulated corresponding to the content of Ti ions.
- the regulator causes, furthermore, closing of the regulating valve V in the inlet of the mixing tank when the Ti ion content has been decreased below a certain minimum value, and a closing of the regulating valve V when the Ti ion content has risen above a certain value. Since in this case unreduced liquor is added without reduced liquor being removed, it may be necessary to close the influx to the tank by means of a floating hook-up at a certain level of filling.
- the electrode measuring combination may be immersed, instead of into the mixing tank directly before the outlet, into the outlet itself even before the regulating valve V
- the flow through the reductor may be carried out with potentiometric control in other form also in the main circuit and/ or shunt circuit.
- the redox electrode measuring combination may be the combination of a platinum electrode immersed into the measuring solution and a reference electrode which is separated from the measuring solution by a suitable salt bridge; as reference electrode, for example, a calomel electrode or another reference electrode which operates reversibly at elevated temperature is applicable.
- Reference electrodes need some attention in continuous operation.
- it is advantageous in certain cases to use the quite constant oxidation-reduction potential of the unreduced starting solution as reference potential i.e. to employ two platinum electrodes of which one is immersed in the unreduced digestion liquor and the other inthe reduced digestion liquor which is, as the case may be, connected with the unreduced liquor via a diaphragm. In this manner the reduction may be carried out up to a definite potential difference which must be determined empirically.
- the process according to the invention is not only limited to sulfuric acid digestion liquors. It may, in the same manner, be applied to hydrochloric acid solutions.
- one electrode is platinum and the other electrode is a calomel electrode.
Landscapes
- Engineering & Computer Science (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Geology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Automation & Control Theory (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Electrolytic Production Of Metals (AREA)
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DET0033053 | 1967-01-24 |
Publications (1)
Publication Number | Publication Date |
---|---|
US3486847A true US3486847A (en) | 1969-12-30 |
Family
ID=7557474
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
US3486847D Expired - Lifetime US3486847A (en) | 1967-01-24 | 1967-09-15 | Process for automatically regulating the reduction of the iron and titanium values in a digestion liquor |
Country Status (7)
Country | Link |
---|---|
US (1) | US3486847A (xx) |
BE (1) | BE709168A (xx) |
ES (1) | ES349610A1 (xx) |
FR (1) | FR1554954A (xx) |
GB (1) | GB1191981A (xx) |
NL (1) | NL6800989A (xx) |
NO (1) | NO119836B (xx) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3728431A (en) * | 1970-03-28 | 1973-04-17 | Bayer Ag | Production of titanyl sulfate solutions |
US3853984A (en) * | 1973-10-17 | 1974-12-10 | Huber Corp J M | Controlling the leaching of kaolin clay |
US3880653A (en) * | 1971-03-18 | 1975-04-29 | Falconbridge Nickel Mines Ltd | Chlorine leach process |
US3883421A (en) * | 1972-09-12 | 1975-05-13 | Dale Emerson Cutting | Measurement of oxidation reduction potential in ore beneficiation |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1333849A (en) * | 1917-10-12 | 1920-03-16 | Titan Co As | Solution of titanium and iron salts and the process of preparing same |
US1916236A (en) * | 1928-03-27 | 1933-07-04 | Titanium Pigment Co Inc | Method of precipitating titanium compounds |
US3199948A (en) * | 1961-06-28 | 1965-08-10 | Sincat Soc Ind Catanese S P A | Processing of kainitic minerals |
US3218131A (en) * | 1961-01-27 | 1965-11-16 | Independence Foundation | Process for recovery of titania values |
US3368870A (en) * | 1963-12-06 | 1968-02-13 | Soloducha Nicolas | Method of producing titanium hydroxide and high grade pigments produced therefrom |
-
1967
- 1967-09-15 US US3486847D patent/US3486847A/en not_active Expired - Lifetime
-
1968
- 1968-01-09 GB GB133268A patent/GB1191981A/en not_active Expired
- 1968-01-10 BE BE709168D patent/BE709168A/xx unknown
- 1968-01-15 NO NO0156/68A patent/NO119836B/no unknown
- 1968-01-22 ES ES349610A patent/ES349610A1/es not_active Expired
- 1968-01-22 FR FR1554954D patent/FR1554954A/fr not_active Expired
- 1968-01-23 NL NL6800989A patent/NL6800989A/xx unknown
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US1333849A (en) * | 1917-10-12 | 1920-03-16 | Titan Co As | Solution of titanium and iron salts and the process of preparing same |
US1916236A (en) * | 1928-03-27 | 1933-07-04 | Titanium Pigment Co Inc | Method of precipitating titanium compounds |
US3218131A (en) * | 1961-01-27 | 1965-11-16 | Independence Foundation | Process for recovery of titania values |
US3199948A (en) * | 1961-06-28 | 1965-08-10 | Sincat Soc Ind Catanese S P A | Processing of kainitic minerals |
US3368870A (en) * | 1963-12-06 | 1968-02-13 | Soloducha Nicolas | Method of producing titanium hydroxide and high grade pigments produced therefrom |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3728431A (en) * | 1970-03-28 | 1973-04-17 | Bayer Ag | Production of titanyl sulfate solutions |
US3880653A (en) * | 1971-03-18 | 1975-04-29 | Falconbridge Nickel Mines Ltd | Chlorine leach process |
US3883421A (en) * | 1972-09-12 | 1975-05-13 | Dale Emerson Cutting | Measurement of oxidation reduction potential in ore beneficiation |
US3853984A (en) * | 1973-10-17 | 1974-12-10 | Huber Corp J M | Controlling the leaching of kaolin clay |
Also Published As
Publication number | Publication date |
---|---|
FR1554954A (xx) | 1969-01-24 |
GB1191981A (en) | 1970-05-13 |
NO119836B (xx) | 1970-07-13 |
NL6800989A (xx) | 1968-07-25 |
BE709168A (xx) | 1968-05-16 |
ES349610A1 (es) | 1969-10-01 |
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Legal Events
Date | Code | Title | Description |
---|---|---|---|
AS | Assignment |
Owner name: NL CHEMICALS, INC., A CORP. OF DE., NEW YORK Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:NL INDUSTRIES, INC.;REEL/FRAME:004661/0323 Effective date: 19861118 Owner name: NL CHEMICALS, INC., 1230 AVENUE OF THE AMERICAS, N Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:NL INDUSTRIES, INC.;REEL/FRAME:004661/0323 Effective date: 19861118 |