CN1041114C - Method and equipment for producing titanium-rich material - Google Patents
Method and equipment for producing titanium-rich material Download PDFInfo
- Publication number
- CN1041114C CN1041114C CN94111054A CN94111054A CN1041114C CN 1041114 C CN1041114 C CN 1041114C CN 94111054 A CN94111054 A CN 94111054A CN 94111054 A CN94111054 A CN 94111054A CN 1041114 C CN1041114 C CN 1041114C
- Authority
- CN
- China
- Prior art keywords
- tower body
- ilmenite
- fluidization
- leaching
- tower
- 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 - Fee Related
Links
Images
Landscapes
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method and equipment for producing a titanium-rich material by treating ilmenite with dilute hydrochloric acid. The method adopts primary ilmenite or ilmenite sand with low weathering degree, and adopts 18-20% hydrochloric acid to carry out multistage countercurrent normal-pressure leaching and washing in a fluidized leaching device consisting of two fluidization towers and two circulating grooves after oxidation roasting treatment, wherein the pulverization rate is less than 1%, and the primary ilmenite with maintained granularity and TiO content is obtained2More than 90 percent of titanium-rich material, the yield is higher than 94 percent, the fluidized leaching device has simple structure, easy manufacture, convenient operation, high running efficiency and good working environment.
Description
What the present invention relates to is a kind of method and device thereof of producing rich titanium material with dilute hydrochloric acid processing ilmenite.
Method and equipment thereof that existing dilute hydrochloric acid is handled the rich titanium material of ilmenite production are ilmenite to be carried out reducing roasting handle.In pressure is boiled the ball cylinder, press and soak, 0.5～2.5% of adding ore deposit amount sulfuric acid or vitriol in leaching process.When this method was used for the low placer of the abundantest primary ilmenite of reserves or rate of decay, efflorescence was serious, and process has some setbacks, and product is not popular with users.Pressure is soaked equipment and material is required high, presses and soaks that hydrogen chloride gas leaks in the process, contaminate environment, etching apparatus and buildings.(see United States Patent (USP) 4019898, Lammartion, N.R, ChemicalEnginering 1976, V83, No.11,100～101) and for example the metallurgical office of Zigong City coal wait unit directly to boil the leaching of ball cylinder with pressure with the Flos Bombacis Malabarici concentrated ilmenite, produce 4～7 microns fine powders in the process, take out of with mother liquor and wash water, therefrom reclaim these fine powders again, make titanium yellow powder, drag-out accounts for 26.86% of total rich titanium material, makes in the coarse fodder remaining fine powder amount reduce to 4.15%.This method, efflorescence is serious, and the thickness material separates bad, particularly reclaims the fine powder difficulty from solution and wash water, adds and press the problem of soaking equipment itself that the industrialization difficulty is big.(see the pressurization of choosing-smelting associating dilute hydrochloric acid leach the Flos Bombacis Malabarici ilmenite concentrate and produce artificial rutile, commerical test report, the metallurgical office of Zigong City coal etc., 1984.11).
Purpose of the present invention is exactly to be that seeking a kind of efflorescence normal pressure that prevents for primary ilmenite and the low ferrotianium placer dilute hydrochloric acid method of rate of decay leaches method and the equipment thereof of producing rich titanium material.
For achieving the above object, technical scheme of the present invention is: the ferrotianium placer that primary ilmenite or rate of decay is low, through oxidizing roasting handle, cooling, the hydrochloric acid with 18～20%, in fluidization leaching device, carry out the multistage counter current normal pressure and leach, wash, filter, dry or be sintered into rich titanium material product based on two fluidization column.The percentage composition of its raw material is: TiO
240～53, ∑ Fe28～37, Fe
2+22～32%, MgO 0.1～7, CaO 0.1～1.4, SiO
21～3, Al
2O
30.25～1.5, size composition is 0.04～0.6 millimeter.
Technical process of the present invention as shown in Figure 1.The drawing label is that 1a～oxidizing roasting, 2a-fluidization are leached, 3a-filtration washing, 4a-oven dry or calcining.Key step division of the present invention is as follows:
One, oxidizing roasting is handled.
For making the iron iron ore have stronger anti-efflorescence ability, can suppress the chemical atomizing that titanium causes because of homogeneous nucleation effectively in hydrolytic process, and for to make the titanium on the ore particle in the hydrolysis settled layer, have stronger intensity, alleviate efflorescence because of mechanical effect, this technology is at first carried out raw material oxidizing roasting and is handled in rotary kiln or fluidizing furnace, fuel can be oils or coal gas, its maturing temperature is 425～875 ℃, furnace exhaust gas oxygen is 5～20%, the residence time is 3～30 minutes, can make 5～35% ferrous oxidation become ferric iron, roasting material is cooled to 85 ℃ in air, carry out acidleach to send into the hypomere operation.
Two, multistage counter current normal pressure liquid stateization leaching.
Multistage counter current can be strengthened leaching process, and leaching velocity that also can satisfaction guaranted under normal pressure can keep contacting the first time with acid than isostatic speed of response, particularly ore deposit simultaneously in whole process, and to be unlikely decomposition rate too fast owing to acidity is hanged down.The matrix of titanium hydrolyzate is destroyed easily cause the settling efflorescence that comes off.In addition, in the fluidization bed of certain voidage, the impact that titanium hydrolysis settled layer is subjected to, collision mechanical effect such as mill is little and alleviate its efflorescence effectively.So this technology will be cooled to the oxidizing roasting material below 85 ℃, directly add in the fluidized bed from cat head, solution is gone into from column bottoms pump, and solution leaches by the fluidization bed continuously, and the bed porosity is 0.61～0.74.Use mother liquor that the final stage of batch of material leached as leach liquor, form the dense multistage counter current in earlier rare back and leach mode.With three sections is example, every section leach liquor concentration of hydrochloric acid is followed successively by 5～10%, 10～18%, 18～20%, temperature in the bed is hanged down 2～5 ℃ than the boiling point of solution under this state, leaching intrasystem vapour pressure is normal pressure, total extraction time is 6～9 hours, liquid-solid 2.8～4.0 (cubic meter/tons) that turn to.Pulverization ratio is less than 1%, and rich titanium material keeps the granularity of ilmenite, TiO
2Greater than 90%, be to produce TiCl
4, the high quality raw material of titanium yellow powder, welding electrode foreskin and ceramic industry.Yield from ilmenite to rich titanium material is greater than 94%.
The present invention aims at the structural representation of device shown in Fig. 2 a that multistage fluidization extract technology provides, and it is mainly constructed and is: two fluidization column are formed by connecting by two groups of pumps, two heat exchangers and pipe valve and two circulation grooves.Switching effect by some valves, each tower all can be formed the same form two cover leaching systems with each groove, this tower, groove alternately connect, form multistage counter current and leach and wash, and two cover system commissure effects have joint to finish leaching process one by one again and again with beating.Its drawing label is 1,6-fluidization column, 2,5-interchanger, 3,4-pump, 7,8-circulation groove, 9～16-valve.
Three sections adverse currents of this technology leach and the function mode of first wash is: Open valve (13) and (9) are valve-off (14) simultaneously, (15), (10) and (11), ejector priming (3), the solution of groove (7) [last consignment of carries out second section solution that leached in tower (6)] is through heat exchanger (2), pump into fluidization column (1), material adds from cat head, solution carries out first section leaching by the fluidization bed, meanwhile, tower (6), groove (8), the system that pump (4) and interchanger (5) are formed carries out the 3rd section leaching to the last consignment of ore deposit, soaks two systems of certain hour and finishes this section leaching simultaneously; Open valve (15) and (11), shut-off valve (13) and (9), use the 3rd section solution that leached in last consignment of ore deposit instead and carry out second section leaching, meanwhile, open the water valve (not marking among the figure) that leads to pump (4), open the bleed valve (not marking) of tower (6) upflow tube, carry out washing in the tower, washing wash water acidity reduces to below 0.1%, material in the tower (6) is put into storage tank (not marking), and used for filtering, groove (7) is 18～22% in complex acid concentration, treat that tower (1) leaches into to give and fix time open valve (13) and (9), close (15) and (11), groove (7) solution pumps into tower (1) and carries out the 3rd section leaching.Meanwhile, open valve (16) and (12), groove (8) solution pump into tower (6), and next batch of material is carried out first section leaching, after treating that two systems have leached certain hour to two batch of materials, change washing and second section leaching respectively over to, arrive this, finished one and embathed the cycle.By the switching of valve, the tower groove is alternately connected like this, both formed multistage counter current and leached and washing, make two to embathe system's commissure operation again, finished the process of embathing one by one rhythmically again and again.
Accompanying drawing 2b is the fluidization column structural representation, and its drawing label is:
20-nozzle, the 21-awl end, 22-tower body, 23-troclia, 24-upflow tube, 25-overflow weir, 26-charge cavity, 27-guide ring.The material of this technology adds from cat head, the nozzle (20) of leach liquor at the bottom of the tower pumps into, passed through (21) at the bottom of the awl of sieve plate effect, after adjusting the cross section flow velocity, enter tower body (22), leach by the fluidization bed, in troclia (23), clarify through guide ring (27), after compiling by overflow weir (25), flow to circulation groove by upflow tube (24), the nozzle bore be on the tower body diameter 4～12%, tower body (22) is up big and down small garden tube, cone angle is 0～10 °, and the cone angle at the awl end is 10～40 °, and the overflow weir diameter is 1～4 times of diameter on the tower body, 0～3 guide ring is installed in the tower body troclia, ring spacing be on the tower body diameter 1/15～1/6, whole tower is made by general steel plate, is lined with acid proof offset plate or acid-proof ceramic tile in the tower.
Embathe device with this fluidization and the high reduced ilmenite of rate of decay is carried out three sections adverse current normal pressures of dilute hydrochloric acid leach and first wash, Pulverization ratio is less than 0.3%, rich titanium material TiO
2Greater than 95%.Acidleach of the present invention and washing process all do not have hydrogen chloride gas leakage, good operational environment, convenience, equipment operation normal, leach containing mineral material 1 such as chromium, manganese, barium, iron～section, leaching and washing is same is suitable for.
Embodiment one
With the Flos Bombacis Malabarici concentrated ilmenite is raw material, and its percentage composition is TiO
246.43, ∑ Fe32.06, Fe
2+25.30, Mg5.95, CaO 1.17, SiO
22.32, Al
2O
31.25, sreen analysis sees Table 1.This raw material in rotary kiln under 750 ℃ the temperature condition, oxidizing roasting 10 minutes, fuel is 7% for the coal gas of heating up water, tail gas oxygen level, Fe
2+19.20%, when roasting material is cooled to 85 ℃ in air, utilizes fluidization of the present invention to leach device and carry out three sections adverse current normal pressures leachings, it is 2 listed that its condition sees Table, leach product behind washing and filtering, calcination becomes rutile under 960 ℃ of conditions, and its product percentage composition is TiO
292.27, TFe2.78, MgO+CaO0.56, Al
2O
30.13, SiO
22.15 the loss that fine powder causes is 0.17%, direct yield is 94.50%, and the rutile of table 1 is listed in the screen analysis of rutile in.
Embodiment 2
With the Guangxi beach placer is raw material, and its percentage composition is: TiO
258.73, ∑ Fe26.35, Fe
2+6.24, Mg0.1, CaO 0.28, SiO
21.02, Al
2O
31.25 sreen analysis is as shown in table 3.Oxidizing roasting under 900 ℃ condition. make Fe
2+Reach its roasting condition of 25.95%. and leaching condition with embodiment one, behind washing and filtering, be sintered into rutile under 960 ℃, its composition is TiO
292.27%, TFe2.78%, MgO+CaO 0.56%, Al
2O
30.13%, SiO
22.15%, the loss that fine powder causes is that 0.17% direct yield is 94.50%, and the screening of rutile is torn open and listed table 3 in.
Table 1
| Sieve mesh | +60 | -60 +90 | -90 +110 | -110 +130 | -130 +150 | -150 +190 | -190 |
| Ilmenite | 4.5 | 28.51 | 9.5 | 20.7 | 9.6 | 16.0 | 17.0 |
| Rutile | 0.4 | 19.8 | 12.6 | 28.1 | 10.0 | 10.7 | 18.2 |
Table 2
| Job step | Strength of solution % | Extraction temperature ℃ | Apparent velocity cm/s | Extraction time (hour) |
| First section second section the 3rd section | 8.75 12.69 20.00 | 117 112 106 | 0.4～0.45 0.3～0.4 0.2～0.3 | 3 3 3 |
Table 3
| Sieve mesh | +40 | -40 +60 | -60 +80 | -80 +100 | -100 +140 | -140 +200 | -200 |
| Ilmenite | 1.84 | 31.91 | 49.85 | 12.35 | 3.16 | 0.81 | 0.07 |
| Rutile | 0.20 | 30.89 | 51.63 | 13.77 | 3.03 | 0.44 | 0.04 |
Acidleach and washing process all do not have hydrogen chloride gas to leak, good operational environment, and it is intact, easy to operate to leach device, works well.
Claims (3)
1. handle the method that ilmenite is produced rich titanium material with dilute hydrochloric acid for one kind, it is characterized in that: adopt the oxidizing roasting in rotary kiln or fluidizing furnace of the low titanium placer of primary ilmenite or rate of decay to handle, its temperature is 425～875 ℃, the content of furnace exhaust gas oxygen is 5～20%, roasting 3～30 minutes, after making 5～35% ferrous oxidation become ferric iron, roasting material is cooled in air below 85 ℃; Cooled roasting material, carrying out the fluidization of three sections adverse current normal pressures in the fluidization leaching device with two fluidization column and two circulation groove compositions invades out, the solution salt acid concentration of every section leaching is followed successively by 5～10%, 10～18%, 18～20%, back one section mother liquor that leached of using batch of material earlier is as leach liquor, the voidage of fluidization bed is 0.61～0.74, extraction temperature is than low 2～5 ℃ of the solution boiling point under this state, and liquid-solid ratio is 2.8～4.0 cubic metres/ton.Carry out washing in the tower after the 3rd section leaching, total extraction time is 6～9 hours, and Pulverization ratio is less than 1%, leach material after filtration, wash, dry or be sintered into rich titanium material product.
2. the method for the rich titanium material of production according to claim 1 is characterized in that: ∑ Fe28～37%, Fe in the content of the ferrotianium placer that primary ilmenite or rate of decay are low
2+22～32%, mineral granularity is 0.04～0.6 millimeter.
3. device that is used for the described method of claim 1, it is characterized in that:, be formed by connecting with two circulation grooves (7) and (8) by two groups of pumps (3) and (4), two interchanger (2) and (5), pipe valve (9) and (16) by two fluidization column (1) and (6); Valve by pipe valve (9) and (16) switches, and the same form two cover leaching systems are formed with groove (7) and (8) respectively in tower (1) and (6); Fluidization column (1) and (6) mainly are made up of tower body (22), spray group (20), the awl end (21), upflow tube (24), guide ring (27), overflow weir parts such as (25); Tower body (22) is 0～10 ° for up big and down small cylinder, cone angle, the diameter of spray group (20) be tower body (22) go up diameter 4～12%, the cone angle of the awl end (21) is 10～40 °, overflow weir (25) diameter is that tower body (22) is gone up 1～4 times of diameter, tower body (22) troclia is equipped with 0～3 guide ring (27), ring spacing is 1/15～1/6 of the last diameter of tower body (22), tower body (22) surrounds with general steel plate, and the tower body liner is acidproof offset plate or acid-proof ceramic tile.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94111054A CN1041114C (en) | 1994-06-29 | 1994-06-29 | Method and equipment for producing titanium-rich material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN94111054A CN1041114C (en) | 1994-06-29 | 1994-06-29 | Method and equipment for producing titanium-rich material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1114364A CN1114364A (en) | 1996-01-03 |
| CN1041114C true CN1041114C (en) | 1998-12-09 |
Family
ID=5034961
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN94111054A Expired - Fee Related CN1041114C (en) | 1994-06-29 | 1994-06-29 | Method and equipment for producing titanium-rich material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1041114C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1320141C (en) * | 2005-06-16 | 2007-06-06 | 昆明理工大学 | Method for preparing rutile type titanium-rich material from primary titanium-rich material |
| JP5792727B2 (en) * | 2009-09-02 | 2015-10-14 | シャ，リーリン | Concentrated titanium hydrochloric acid extraction residue, its use and method for preparing titanium pigment |
| CN101723448B (en) * | 2009-12-29 | 2013-11-06 | 攀钢集团研究院有限公司 | Method for preparing titaniferous solution |
| CN102765750A (en) * | 2012-05-19 | 2012-11-07 | 河南佰利联化学股份有限公司 | Preparation method of titanium-rich material |
| CN103352129A (en) * | 2013-06-17 | 2013-10-16 | 中国船舶重工集团公司第七二五研究所 | Method for improving quality of titanium concentrate |
| CN103482696B (en) * | 2013-09-02 | 2015-04-29 | 攀钢集团攀枝花钢铁研究院有限公司 | Method and device for preparing titanium solution from fluidized acidolysis titanium-containing material |
| CN103910382B (en) * | 2014-04-01 | 2015-07-22 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing artificial rutile |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4119696A (en) * | 1977-11-14 | 1978-10-10 | Uop Inc. | Production of titanium metal values |
-
1994
- 1994-06-29 CN CN94111054A patent/CN1041114C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4119696A (en) * | 1977-11-14 | 1978-10-10 | Uop Inc. | Production of titanium metal values |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1114364A (en) | 1996-01-03 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100500893C (en) | Copper cobalt alloy separation and recovery method | |
| CN101967563A (en) | Method for wet-process vanadium extraction by using vanadium- and titanium-containing converter slag | |
| CN102745743B (en) | Method for preparing artificial rutile by titanium slags | |
| CN1041114C (en) | Method and equipment for producing titanium-rich material | |
| CN1057130C (en) | Vanadium pentoxide extracting method from stone coal vanadium ore | |
| CN1244498C (en) | Manufacture of high grade artificial rutile from low grade primary greporite | |
| CN101851004B (en) | Method for producing artificial rutile by using residual slope accumulated ilmenite | |
| CN109136537A (en) | The technique that vanadium titano-magnetite prepares liquid vanadium extraction acceptable material and direct vanadium extraction | |
| CN107043128A (en) | A kind of method that iron salt solutions lixiviation process prepares synthetic rutile | |
| CN1006635B (en) | Method for preparing titanium white power using iron-smelting blast-furnace slag containing titanium | |
| CN105110300B (en) | The method that a kind of compound manganese ore of Containing Sulfur manganese extracts manganese and sulphur | |
| CN109971910A (en) | Using the method for calcium system processing vanadium extraction from molten iron | |
| CN112209446B (en) | Method for recycling Cr-containing tungsten carbide waste and application thereof | |
| CN205773419U (en) | A kind of hydrochloric acid method titanium white production system | |
| CN112266013A (en) | System and process for producing titanium tetrachloride from high-calcium magnesium titanium dioxide | |
| CN1254023A (en) | Leaching-out method for extracting vanadium from vanadium-containg ore calcines and its application in stone-coal calcination-direct vanadium-extracting process | |
| CN115232961B (en) | Method for extracting vanadium by decalcification of calcified vanadium extraction tailings | |
| CN1772964A (en) | Process for producing Mg rare earth intermediate alloy by Submerged Liquid Cathode electrolysis under low-temperature | |
| CN103145181B (en) | Three-phase fluidized continuous reaction device for preparing rutile by hydrochloric acid leaching method | |
| CN1025499C (en) | Method of extracting nicotine from waste tobacco powder | |
| CN109179496A (en) | High-grade titanium dioxide and preparation method thereof | |
| CN105886772A (en) | Comprehensive recycling method of waste rare-earth type Y-type molecular sieve catalyst | |
| CN1258642A (en) | Continuous precipitation process of prodcing globular ammonium polyvanadate | |
| CN100526486C (en) | Method of oxidizing transforming leaching vanadium from stone coal under pressure field | |
| CN101100709B (en) | Method for reclaiming chromium in vanadium oxides producing process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |