CN107459058B - Method for producing synthetic rutile by using titanium concentrate - Google Patents
Method for producing synthetic rutile by using titanium concentrate Download PDFInfo
- Publication number
- CN107459058B CN107459058B CN201610384797.9A CN201610384797A CN107459058B CN 107459058 B CN107459058 B CN 107459058B CN 201610384797 A CN201610384797 A CN 201610384797A CN 107459058 B CN107459058 B CN 107459058B
- Authority
- CN
- China
- Prior art keywords
- titanium
- liquid
- titanium concentrate
- solid
- washing
- 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.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/0475—Purification
Landscapes
- 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)
- Inorganic Compounds Of Heavy Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a method for producing artificial rutile by using titanium concentrate, which takes the titanium concentrate as a raw material and carries out mechanical activation, roasting treatment and magnetismSelecting, removing impurities by hot acid, washing with water, and calcining to obtain the synthetic rutile. The method can convert the titanium concentrate into the artificial rutile type titanium-rich material without electric furnace smelting, and the byproduct magnetite can be effectively utilized. TiO can be obtained after the treatment by the method2The artificial rutile type titanium-rich material with the content of more than 90 percent has the titanium recovery rate of 85 percent, is a novel method for effectively enriching titanium concentrate, and has the advantages of short process flow, less equipment investment, low energy consumption, less byproducts, less environmental pollution and the like.
Description
Technical Field
The invention belongs to the field of metallurgy, and relates to a method for producing synthetic rutile by using titanium concentrate.
Background
The titanium resource of China is rich, the ilmenite ore is mainly used except a small amount of ilmenite, the defects of the ilmenite ore in China are low grade and high impurity content, the requirement of chlorination process titanium white on raw materials cannot be directly met, and the demand for high-grade rich titanium materials is increased along with the rapid development of chlorination process titanium white and sea brocade titanium industries in China. Therefore, an economic and reasonable titanium raw material treatment method is sought, and the processing of abundant ilmenite resources in China into titanium-rich materials is an urgent priority for the development of titanium white and titanium material industries in China.
At present, the rutile type titanium dioxide is mainly produced by a sulfuric acid method and a chlorination method. The sulfuric acid method is to adopt concentrated sulfuric acid to carry out acidolysis on titaniferous raw materials such as ilmenite or acid-soluble titanium slag and the like to obtain titanyl sulfate solution, then the titanium solution is purified, concentrated and washed by water to obtain amorphous metatitanic acid, and the obtained metatitanic acid is filtered, washed and calcined at high temperature to obtain rutile titanium dioxide powder products. The chlorination process uses rutile or high titanium slag as raw material, and produces rutile type titanium dioxide finished product after chlorination, refining, oxidation and surface treatment.
The research institute of comprehensive utilization of mineral products of Chinese geological academy of sciences proposes a method for preparing a titanium-rich material from high-impurity ilmenite concentrate, and the technical route is as follows: the method comprises the steps of raw ore, magnetic separation, tailings, flotation, ilmenite concentrate, roasting, magnetic separation, reduction smelting, titanium slag, purification and titanium-rich material production.
Pan steel provides a method for smelting acid-soluble titanium slag by utilizing the molten reduction of vanadium-titanium-iron concentrate. The method comprises the following steps: mixing the vanadium-titanium-iron ore concentrate with the titanium ore concentrate, and adding a carbonaceous reducing agent and a binder to form a mixture; reducing the mixture, and then carrying out slag-iron separation treatment to obtain semisteel and titanium slag; spraying water on the surface of the titanium slag obtained by slag iron separation treatment, so that the temperature of the titanium slag rapidly crosses a temperature range of 600-850 ℃ in the cooling process to form acid-soluble titanium slag.
Chinese patent 201210155641.5 discloses a method for preparing titanium-rich material, etc., which comprises mixing titanium concentrate with a reducing agent, pelletizing, pre-reducing, and then smelting in an electric furnace. This approach notwithstanding the TiO2The grade is high, but the process is complex, and various additives and numerous devices are needed.
Chinese patent 201110094970.9 discloses a method for preparing a titanium-rich material from high-impurity ilmenite concentrate, which comprises the steps of calcining the titanium concentrate by a rotary kiln, then carrying out magnetic separation, and then reducing by a submerged arc furnace to finally obtain the titanium-rich material. Although pelletizing is omitted, the method does not carry out pre-reduction on the titanium concentrate, so that the reaction in the reduction stage is insufficient, and TiO is generated2Low grade, high energy consumption and the like.
Disclosure of Invention
Aiming at the problems, the method for producing the artificial rutile by the titanium concentrate is provided, and aims to solve the problems of high energy consumption, high pollution, high production cost and the like of the traditional electric furnace smelting or tunnel kiln reduction.
The technical scheme of the invention is as follows: a method for producing synthetic rutile from titanium concentrate, which is characterized by comprising the following steps:
(1) uniformly mixing the titanium concentrate and an activating agent according to a certain proportion, and adding the mixture into a ball mill for mechanical crushing and activation;
(2) adding a certain amount of additives into the activated material, uniformly mixing, containing the mixture by using a crucible, and putting the mixture into a roasting furnace for high-temperature roasting;
(3) grinding the roasted material, washing with hot water according to a certain liquid-solid ratio, and evaporating and concentrating the washing water to recover the additive;
(4) dissolving impurities in the washed product by using a dilute hydrochloric acid solution, carrying out solid-liquid separation after the reaction is finished, and circularly regenerating hydrochloric acid;
(5) washing the solid phase after the removal of impurities by hot acid with hot water again;
(6) and drying and calcining the solid material after the water washing treatment to obtain the synthetic rutile.
The activating agents in the step (1) are NaOH and Na during mechanical crushing and activation2CO3、NaHCO3And one or more of CaO, the mixing mass ratio of the titanium concentrate to the activating agent is 1: 1-5: 1, the activation time is 1-3 hours, and the granularity is controlled to be 100-300 meshes after mechanical activation. And (3) adding one or more additives selected from phosphate, borate, sulfate and carbonate during high-temperature roasting in the step (2), wherein a graphite crucible is selected during roasting, the roasting temperature is controlled to be 800-1000 ℃, the time is controlled to be 1.5-2.5 hours, and the roasted material needs to be subjected to magnetic separation treatment. And (4) washing the nonmagnetic material obtained in the step (3) with hot water at the temperature of 70-90 ℃ for 10-40 minutes according to the liquid-solid ratio of 3: 1-5: 1. And (4) carrying out hot acid impurity removal on the materials washed in the step (4) by using 10-30% of dilute hydrochloric acid solution at the temperature of 75-110 ℃ for 30-60 minutes according to the liquid-solid ratio of 3: 1-5: 1, and recovering hydrochloric acid from the liquid phase after impurity removal. And (5) washing the solid-phase material subjected to the hot acid impurity removal in the step (5) with hot water at the temperature of 50-80 ℃ according to the liquid-solid ratio of 3: 1-5: 1. And (4) drying the solid-phase material washed by water in the step (6), and calcining at 600-800 ℃ for 1-2 hours to obtain the artificial rutile.
Compared with the prior art, the method provided by the invention has the following advantages:
(1) the synthetic rutile obtained by the method meets the requirement of producing titanium white by a chlorination process, and has wide adaptability.
(2) The invention does not use high energy consumption equipment such as an electric furnace or a tunnel kiln;
(3) the invention does not add carbonaceous reducing agent and does not contain CO2Discharging;
(4) the titanium concentrate deforms under the action of mechanical force to generate a large amount of lattice distortion, so that the reaction activity is improved;
(5) the ilmenite phase is prevented from being converted into a ferrobrookite phase through roasting treatment, the enrichment of impurities such as calcium, magnesium, manganese and the like in the minerals is inhibited, and iron grains grow and are easy to separate from titanium.
(6) The filtrate after the impurity removal by the hot acid is a low-acidity solution, and the recycling is simple, so that the acid consumption is greatly reduced, and the environmental pollution is reduced.
(7) The invention has short process flow, less equipment investment, low energy consumption, less byproducts and less environmental pollution, and meets the requirements of energy conservation, emission reduction and clean metallurgy.
Drawings
Fig. 1 is a process flow diagram of a process for producing synthetic rutile from titanium concentrate.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention clearer, the following detailed description of the present invention is given with reference to specific examples:
example 1
Referring to figure 1, conditions: taking Ti02Adding 50g of activating agent into 100g of 44.53 percent titanium concentrate, and finely grinding the mixture by using a ball mill until the content of the activating agent is more than 96 percent and less than 0.074 mm; then evenly mixing the mixture with an additive according to the mass ratio of 10:1, and roasting for 2 hours at the roasting temperature of 950 ℃; washing the roasted material for lh by using deionized water at the temperature of 85 ℃ according to the liquid-solid ratio of 5: 1; washing, performing liquid-solid separation, evaporating and concentrating a liquid phase to recover an additive, and pickling a solid phase for 2 hours at 105 ℃ by using a hydrochloric acid solution with the mass concentration of 15% according to the liquid-solid ratio of 4:1 under normal pressure; evaporating a liquid phase obtained by solid-liquid separation of the ore pulp after acid washing to recover hydrochloric acid, and washing the solid phase after acid washing with deionized water at 90 ℃ according to a liquid-solid ratio of 5: 1; washing with water, performing liquid-solid separation, drying and calcining the solid phase to obtain Ti02Synthetic rutile in an amount of 92.62%.
Example 2
Referring to figure 1, conditions: taking Ti02Adding 25g of activating agent into 100g of 44.53 percent titanium concentrate, and finely grinding the mixture by using a ball mill until the content of the activating agent is more than 96 percent and less than 0.074 mm; then evenly mixing the mixture with an additive according to the mass ratio of 15:1, and roasting for 2 hours at the roasting temperature of 950 ℃; washing the roasted material for lh by using deionized water at the temperature of 85 ℃ according to the liquid-solid ratio of 5: 1; after washingPerforming liquid-solid separation, evaporating and concentrating a liquid phase to recover the additive, and pickling a solid phase for 2 hours at 105 ℃ and normal pressure by using a hydrochloric acid solution with the mass concentration of 15% according to the liquid-solid ratio of 4: 1; evaporating a liquid phase obtained by solid-liquid separation of the ore pulp after pickling to recover hydrochloric acid, and washing a solid phase after pickling with deionized water at 90 ℃ according to a liquid-solid ratio of 5: 1; washing with water, performing liquid-solid separation, drying and calcining the solid phase to obtain Ti02Synthetic rutile with a content of 82.93%.
Example 3
Referring to figure 1, conditions: taking Ti02100g of titanium concentrate with the content of 44.53 percent, adding 100g of activating agent, and finely grinding the mixture by using a ball mill until the content of more than 96 percent is less than 0.074 mm; then evenly mixing the mixture with an additive according to the mass ratio of 5:1, and roasting for 2 hours at the roasting temperature of 950 ℃; washing the roasted material for lh by using deionized water at the temperature of 85 ℃ according to the liquid-solid ratio of 5: 1; washing, performing liquid-solid separation, evaporating and concentrating a liquid phase to recover an additive, and pickling a solid phase for 2 hours at 105 ℃ by using a hydrochloric acid solution with the mass concentration of 15% according to the liquid-solid ratio of 4:1 under normal pressure; evaporating a liquid phase obtained by solid-liquid separation of the ore pulp after pickling to recover hydrochloric acid, and washing a solid phase after pickling with deionized water at 90 ℃ according to a liquid-solid ratio of 5: 1; washing with water, performing liquid-solid separation, drying and calcining the solid phase to obtain Ti02Synthetic rutile with a content of 85.12%.
Example 4
Referring to figure 1, conditions: taking Ti02Adding 50g of activating agent into 100g of 44.53 percent titanium concentrate, and finely grinding the mixture by using a ball mill until the content of the activating agent is more than 96 percent and less than 0.074 mm; then evenly mixing the mixture with an additive according to the mass ratio of 10:1, and roasting for 2 hours at the roasting temperature of 850 ℃; washing the roasted material for lh by using deionized water at the temperature of 85 ℃ according to the liquid-solid ratio of 5: 1; washing, performing liquid-solid separation, evaporating and concentrating a liquid phase to recover an additive, and pickling a solid phase for 2 hours at 105 ℃ by using a hydrochloric acid solution with the mass concentration of 15% according to the liquid-solid ratio of 4:1 under normal pressure; evaporating a liquid phase obtained by solid-liquid separation of the ore pulp after acid washing to recover hydrochloric acid, and washing a solid phase after acid washing with deionized water at 90 ℃ according to a liquid-solid ratio of 5: 1; after the water washing is finished, liquid-solid separation is carried out, and the solid phase is dried and calcined to obtain Ti02Synthetic rutile with a content of 76.48%.
Example 5
Referring to figure 1, conditions: taking Ti02Adding 50g of activating agent into 100g of 44.53 percent titanium concentrate, and finely grinding the mixture by using a ball mill until the content of the activating agent is more than 96 percent and less than 0.074 mm; then evenly mixing the mixture with an additive according to the mass ratio of 10:1, and roasting for 2 hours at the roasting temperature of 1050 ℃; washing the roasted material for lh by using deionized water at the temperature of 85 ℃ according to the liquid-solid ratio of 5: 1; washing, performing liquid-solid separation, evaporating and concentrating a liquid phase to recover an additive, and pickling a solid phase for 2 hours at 105 ℃ by using a hydrochloric acid solution with the mass concentration of 15% according to the liquid-solid ratio of 4:1 under normal pressure; evaporating a liquid phase obtained by solid-liquid separation of the ore pulp after acid washing to recover hydrochloric acid, and washing a solid phase after acid washing with deionized water at 90 ℃ according to a liquid-solid ratio of 5: 1; after the water washing is finished, liquid-solid separation is carried out, and the solid phase is dried and calcined to obtain Ti02Synthetic rutile with a content of 88.21%.
Example 6
Referring to figure 1, conditions: taking Ti02Adding 50g of activating agent into 100g of 44.53 percent titanium concentrate, and finely grinding the mixture by using a ball mill until the content of the activating agent is more than 96 percent and less than 0.074 mm; then evenly mixing the mixture with an additive according to the mass ratio of 10:1, and roasting for 2 hours at the roasting temperature of 950 ℃; washing the roasted material for lh by using deionized water at the temperature of 85 ℃ according to the liquid-solid ratio of 5: 1; washing, performing liquid-solid separation, evaporating and concentrating a liquid phase to recover an additive, and pickling a solid phase for 2 hours at 95 ℃ and normal pressure by using a hydrochloric acid solution with the mass concentration of 15% according to the liquid-solid ratio of 4: 1; evaporating a liquid phase obtained by solid-liquid separation of the ore pulp after acid washing to recover hydrochloric acid, and washing a solid phase after acid washing with deionized water at 90 ℃ according to a liquid-solid ratio of 5: 1; after the water washing is finished, liquid-solid separation is carried out, and the solid phase is dried and calcined to obtain Ti02Synthetic rutile with a content of 83.74%.
Claims (5)
1. A method for producing synthetic rutile by using titanium concentrate is characterized by mainly comprising the following steps:
(1) uniformly mixing the titanium concentrate and an activating agent according to a certain proportion, and adding the mixture into a ball mill for mechanical activation; the activating agent is NaOH or Na during mechanical activation2CO3、NaHCO3And one or more of CaO, the mixing mass ratio of the titanium concentrate to the activating agent is 1: 1-5: 1, the activating time is 1-3 hours, and the mixture is processed by a machineThe granularity is controlled between 100 meshes and 300 meshes after mechanical activation;
(2) adding a certain amount of additives into the activated material, uniformly mixing, containing the mixture by using a graphite crucible, and putting the mixture into a roasting furnace for high-temperature roasting; the additive added during high-temperature roasting is one or more of phosphate, borate, sulfate and carbonate;
(3) grinding the roasted material and then carrying out magnetic separation treatment;
(4) washing the obtained nonmagnetic material with water according to a certain liquid-solid ratio, and dissolving impurities by using a hot dilute hydrochloric acid solution;
(5) and washing the solid phase subjected to the impurity removal by hot acid with hot water, drying the washed solid phase material, and calcining the dried solid phase material at 600-800 ℃ for 1-2 hours to obtain the artificial rutile.
2. The method for producing artificial rutile by using titanium concentrate as claimed in claim 1, wherein a graphite crucible is selected during roasting, the roasting temperature is controlled to be 800-1000 ℃, the time is controlled to be 1.5-2.5 hours, and the roasted material needs to be subjected to magnetic separation treatment.
3. The method for producing the artificial rutile by using the titanium concentrate according to claim 1, wherein the obtained nonmagnetic material is washed with hot water at the temperature of 70-90 ℃ for 10-40 minutes according to the liquid-solid ratio of 3: 1-5: 1.
4. The method for producing artificial rutile by using titanium concentrate according to claim 1, wherein the material washed in the step (4) is subjected to hot acid impurity removal for 30-60 minutes by using 10-30% of dilute hydrochloric acid solution at the temperature of 75-110 ℃ according to the liquid-solid ratio of 3: 1-5: 1, and hydrochloric acid is recovered from the liquid phase after impurity removal.
5. The method for producing artificial rutile by using titanium concentrate according to claim 1, wherein the solid phase material after the hot acid impurity removal is washed by hot water at 50-80 ℃ according to a liquid-solid ratio of 3: 1-5: 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610384797.9A CN107459058B (en) | 2016-06-02 | 2016-06-02 | Method for producing synthetic rutile by using titanium concentrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610384797.9A CN107459058B (en) | 2016-06-02 | 2016-06-02 | Method for producing synthetic rutile by using titanium concentrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107459058A CN107459058A (en) | 2017-12-12 |
| CN107459058B true CN107459058B (en) | 2021-06-08 |
Family
ID=60544386
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610384797.9A Active CN107459058B (en) | 2016-06-02 | 2016-06-02 | Method for producing synthetic rutile by using titanium concentrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107459058B (en) |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014362A (en) * | 2013-01-16 | 2013-04-03 | 昆明冶金研究院 | Method for reducing content of calcium and magnesium in high-calcium-magnesium titanium slag |
| CN104860347B (en) * | 2015-05-15 | 2017-07-07 | 云南民族大学 | A kind of preparation method of synthetic rutile |
-
2016
- 2016-06-02 CN CN201610384797.9A patent/CN107459058B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN107459058A (en) | 2017-12-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101812595A (en) | Method for producing artificial rutile from titanium slag | |
| CN109022773B (en) | Method for comprehensively utilizing titanium concentrate | |
| CN105293564A (en) | Method for recycling zinc-containing dust ash in steel plant | |
| CN1069110C (en) | Technology for comprehensive utilization of V-Ti magnetite | |
| CN111534706A (en) | Method for preparing titanium-rich material from Panxi titanium concentrate | |
| CN103276227B (en) | Method for extracting vanadium from vanadium-titanium magnetite concentrates | |
| CN103088208A (en) | Method for treating manganese-containing and phosphorus-containing hematite | |
| CN102745743A (en) | Method for preparing artificial rutile by titanium slags | |
| WO2019137544A1 (en) | Method for extracting valent component in vanadium titanium magnetite by means of oxygen-rich selective leaching | |
| CN107285375A (en) | The method that low-grade titanium ore prepares high-grade artificial rutile | |
| WO2012171481A1 (en) | Hydrometallurgical process for complete and comprehensive recovery with substantially no wastes and zero emissions | |
| CN113862494B (en) | Preparation method of titanium-rich material and preparation method of titanium tetrachloride | |
| CN101851004B (en) | Method for producing artificial rutile by using residual slope accumulated ilmenite | |
| CN110735032B (en) | Vanadium-titanium-iron paragenetic ore treatment process | |
| CN109385533A (en) | The recoverying and utilizing method of titanium slag dedusting ash | |
| CN103074496B (en) | Method for separating and purifying magnesium dioxide from anode mud | |
| CN107460345A (en) | A kind of method for producing high titanium slag | |
| Ju et al. | An approach towards utilization of water-quenched blast furnace slag for recovery of titanium, magnesium, and aluminum | |
| CN117926027A (en) | Comprehensive utilization method of laterite nickel ore | |
| CN111348653B (en) | Method for preparing high-purity silicon, titanium white and high-purity fluoride by using titanium-containing slag and low-purity silicon material | |
| CN110396610B (en) | Method for treating titanium minerals and metal silicate minerals through ammonium salt pressure pyrolysis | |
| CN111534699A (en) | Method for recovering valuable substances from cemented carbide scrap | |
| CN107459058B (en) | Method for producing synthetic rutile by using titanium concentrate | |
| CN114480882B (en) | Method for fully utilizing ferrotitanium and vanadium resources in vanadium titano-magnetite | |
| CN114084902B (en) | Method for preparing titanium chloride slag from titanium concentrate |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20230516 Address after: 538000 Gongche Town, Gangkou District, Fangchenggang City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Yueqiao New Material Technology Co.,Ltd. Address before: 650033 No. 388, Xuefu Road, Wuhua District, Yunnan, Kunming Patentee before: KUNMING METALLURGY College |
|
| TR01 | Transfer of patent right |