CN109825701B - Method for preparing titanium-rich material by leaching ilmenite with titanium white waste hydrochloric acid by chlorination process and comprehensively utilizing titanium-rich material - Google Patents
Method for preparing titanium-rich material by leaching ilmenite with titanium white waste hydrochloric acid by chlorination process and comprehensively utilizing titanium-rich material Download PDFInfo
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Abstract
The invention belongs to the technical field of new materials, and particularly relates to a method for preparing a titanium-rich material by leaching ilmenite with titanium white waste hydrochloric acid by a chlorination process and comprehensively utilizing the titanium-rich material. The method comprises leaching and filtering ilmenite, drying and calcining a filter cake to prepare a titanium-rich material, recycling a washing liquid, and concentrating a mother solution to prepare iron oxide red and ammonium chloride. The method comprehensively utilizes the waste hydrochloric acid discharged in the production of titanium dioxide by a chlorination process, reduces environmental pollution and treatment cost, realizes a new method for preparing a titanium-rich material and byproducts of iron oxide red and ammonium chloride by using the waste hydrochloric acid, can radically solve the problem that the waste hydrochloric acid of the titanium dioxide by the chlorination process cannot be recycled, realizes the reutilization of wastes, has simple process flow and operation, is easy to realize, accords with the carbon footprint and life cycle theory advocated internationally at present, and has good economic benefit and social benefit.
Description
Technical Field
The invention belongs to the technical field of new materials, and particularly relates to a method for preparing a titanium-rich material by leaching ilmenite with titanium white waste hydrochloric acid by a chlorination process and comprehensively utilizing the titanium-rich material.
Background
The titanium deposit can be divided into rock ore and sand ore, wherein the rock ore is primary ore, the sand ore is secondary ore, and the rock ore belongs to sedimentary rock deposit. The rock ore mainly contains titaniferous iron ore, the rutile content is low, the FeO content is high, and the content of FeO is generally as follows: fe2O3In the range of 2.9-5.8. Impurity SiO in rock ore2And Al2O3High content, mixed oxides of vanadium, chromium, copper, cobalt and the like, compact mineral phase structure and separation of TiO2And other components are difficult, the Panzhihua mineral deposit in China belongs to rock ore, and the content of calcium and magnesium is high.
Placer ore contains minerals such as ilmenite and rutile, and TiO is common2High grade, badly oxidized placer, iron oxide lost after weathering, TiO2Free to form rutile ore, FeO will be weathered further to form Fe2O3，Fe2O3The content of (A) is high and reaches FeO: fe2O3Less than 1, the content of impurities MnO in the placer is higher, and the placer is also associated with monazite, zirconite and the like. As most of the placer is naturally weathered, the mineral structure is loose, and TiO2Easy enrichment of, TiO of beneficiated rutile and ilmenite2High grade, large mineral particles.
At present, titanium dioxide production technologies are divided into a chlorination method and a sulfuric acid method, wherein the production capacity of the chlorination method accounts for about 56% globally, the production capacity of Chinese titanium dioxide is mainly based on the sulfuric acid method, and the production capacity of the chlorination method accounts for about 6.5% of the total production capacity of the domestic titanium dioxide. However, compared with the sulfuric acid method, the chlorination method has the advantages of short flow, good product quality, less three-waste emission and the like, so the production technology of titanium dioxide by the chlorination method is the national development technology process at present. But the production technology of titanium dioxide by chlorination method in China is always kept secret. The integrity and the technical advancement of the domestic chlorination process are far from foreign countries. The decomposition medium adopted in the production process of the chlorination method is chlorine, one part of the chlorine is recycled in a system, the other part of the chlorine can be discharged only in the form of hydrochloric acid, and the discharged waste hydrochloric acid is neutralized at present, so that a large amount of waste salt is generated after neutralization and cannot be utilized, the development of the chlorination method is limited, the environmental risk is caused, and the defects that the chlorination method cannot be stockpiled and the like because the silver and other ions are removed as precipitates by the chlorination method, and other ions are all soluble substances and are unstable in storage are caused. How to comprehensively utilize the part of waste hydrochloric acid, changing waste into valuable and comprehensively utilizing the waste hydrochloric acid is a future breakthrough point of the titanium dioxide production technology by the chlorination process.
In addition, the high titanium slag is mainly prepared by an electric furnace smelting method and the artificial rutile is prepared by a reduction corrosion method in the current generation. The electric furnace smelting method for preparing the high titanium slag adopts a smelting generation process, and has the advantages of simplicity, easiness, large-scale equipment, less three wastes, easiness in processing and recycling and the like. But the production process technology has limited capability of removing calcium and magnesium; the reduction corrosion method is a high-grade ilmenite suitable for weathering and successfully researched by Australian CSIRO, and has high temperature requirement for strong reduction and great technical difficulty.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing a titanium-rich material by leaching ilmenite with titanium white waste hydrochloric acid by a chlorination process and comprehensively utilizing the titanium-rich material. The method better utilizes the titanium dioxide waste hydrochloric acid produced by the chlorination process to produce the rich titanium material, and comprehensively recycles the residual waste hydrochloric acid and the mixed chloride.
The method for preparing the titanium-rich material and comprehensively utilizing the ilmenite through hydrochloric acid leaching of titanium white waste by a chlorination process comprises leaching and filtering the ilmenite, drying and calcining a filter cake to prepare the titanium-rich material, recycling a washing liquid, and concentrating a mother liquor to prepare iron oxide red and ammonium chloride.
Wherein:
the leaching and filtering of the ilmenite comprise the following specific steps: mixing ilmenite and titanium white waste hydrochloric acid obtained by a chlorination process according to a certain mass-volume ratio, leaching the waste hydrochloric acid under the condition of stirring, and filtering the mixture while the mixture is hot after leaching.
The mass concentration of the titanium white waste hydrochloric acid produced by the chlorination method is 20-25%, and the mass volume ratio G isTiO2:VHClThe stirring speed is controlled to be 30-60 r/min, the stirring time is controlled to be 5-9 hours, and the stirring temperature is controlled to be 30-80 ℃.
The preparation of the titanium-rich material by drying and calcining the filter cake is specifically as follows: the filtrate after filter cake filtration is processed by Ca2+、Mg2+FeCl obtained after ion impurity removal process3And FeCl2The mother liquor is used for the preparation of iron oxide red and ammonium chloride; and washing the filter cake after filter pressing for 2-3 times by using tap water, then placing the filter cake in a muffle furnace for drying and calcining, and recycling the washed washing liquid.
The temperature of drying and calcining is within 350-450 ℃, and the drying time is 2-4 hours.
The washing liquid recycling method specifically comprises the following steps: and returning the washing liquid to the leaching process of the ilmenite, and using the washing liquid to prepare waste hydrochloric acid, so that the mass concentration of the waste hydrochloric acid is controlled within the range of 20-25%, and the waste hydrochloric acid is used as a leaching liquid.
The concentration of the mother liquor for preparing the iron oxide red and the ammonium chloride is specifically as follows: will pass through Ca2+、Mg2+FeCl obtained after ion impurity removal process3And FeCl2Further adopting steam as mother liquor for concentration, carrying out air oxidation, adding an ammonium bicarbonate solution, reacting until pink ferric carbonate appears, standing for 30-60 min, filtering, washing and precipitating, and placing the precipitate in a muffle furnace for drying and calcining to obtain iron oxide red; and concentrating the filtered and washed solution at the temperature of 80-95 ℃ until crystals appear, then cooling to room temperature, and crystallizing to obtain an ammonium chloride product.
The steam concentration is adopted to control the total Fe concentration within the range of 80-160 g/LPerforming air oxidation for 30-60 min, and then performing oxidation according to V (FeCI)3)/V(NH4HCO3) 1: adding an ammonium bicarbonate solution according to the volume ratio of 2.6-3.8, wherein the concentration of the ammonium bicarbonate solution is 100-180 g/L.
And (3) raising the calcination temperature from room temperature to 650 ℃, preserving the heat at 650 ℃ for 30-50 min, naturally cooling to room temperature, and grinding to obtain the iron oxide red.
The invention mainly utilizes the waste hydrochloric acid generated in the production process of titanium dioxide by a chlorination method to comprehensively utilize the waste hydrochloric acid to prepare a titanium-rich material, and then recycles the residual waste hydrochloric acid and the chloride.
The method for preparing the titanium-rich material by leaching ilmenite with the waste hydrochloric acid of titanium white produced by the chlorination process and comprehensively utilizing the ilmenite has the main principle that the first step is to remove iron and other impurities in the ilmenite, so that the grade of titanium dioxide is improved as much as possible. The high pulverization rate of the hydrochloric acid method causes the fineness of the product to be fine and the production and filtration cost to be high, so that how to reduce the high pulverization rate in the hydrochloric acid leaching process is the most important research, and the reason of the serious pulverization phenomenon caused in the hydrochloric acid leaching process is mainly that the titanium dioxide particles generated by hydrolysis are too fine, the specific surface area is large, the surface free energy is high, the adsorption among the particles is serious and spherical particles are formed due to the existence of hydrolysis reaction.
The hydrochloric acid leaching of ilmenite is a complex heterogeneous reaction, the reaction products being various complexes containing chloride.
FeTiO3+6H+→Fe2++Ti4++3H2O
2FeO·TiO2+6HCl＝＝2FeCl2+TiO2+TiOCl2+3H2O
2MgO·TiO2+6HCl＝＝2MgCl2+TiO2+TiOCl2+3H2O
2CaO·TiO2+6HCl＝＝2CaCl2+TiO2+TiOCl2+3H2O
2Fe2O3·TiO2+14HCl＝＝4FeCl3+TiO2+TiOCl2+7H2O
In the leaching process of the dilute hydrochloric acid, part of titanium is dissolved and then hydrolyzed, and the hydrolysis reaction is as follows:
TiOCl2+(X+1)H2O＝＝TiO2·xH2O+2HCl
the invention removes FeO, CaO, MgO and Fe in the ilmenite by directly leaching the ilmenite with hydrochloric acid2O3And the inclusion oxide with poor stability is subjected to the treatment so as to improve the grade of the titanium dioxide.
The leaching condition in the hydrochloric acid leaching process is explored, the occurrence of hydrolysis reaction is reduced, the high pulverization rate is reduced, and the improvement of TiO2The quality method. Creatively exploring, leaching ilmenite by adopting a normal-pressure leaching process, wherein the mass concentration of titanium white waste hydrochloric acid produced by a chlorination method is 20-25%, and the mass-volume ratio of the titanium white waste hydrochloric acid to the titanium white waste hydrochloric acid is GTiO2:VHClThe ratio of the TiO to the TiO is 1: 2-5, the reaction time is controlled to be 5-9 hours, the reaction temperature is controlled to be 30-80 ℃, and the prepared TiO is prepared2The content is within the range of 80-90%.
The iron and titanium components are dissolved into the solution at the same speed in the initial leaching stage, after a period of reaction, the iron is continuously dissolved, the titanium is hydrolyzed and precipitated, so that the concentration of the titanium in the solution is reduced, and finally, the titanium reaches an equilibrium level, and the time for reaching the equilibrium is reduced by selecting leaching conditions, so that the phenomenon of high pulverization rate in the hydrochloric acid leaching process is reduced, and the prepared TiO is prepared2The mass content is within the range of 80-90%.
The property of the surface of the ore and the leaching mode have great influence on the generation of the titanium-rich material, and the ilmenite subjected to mild reduction can change the property of the surface of the ore and improve the generation of the titanium-rich material.
After filter pressing to obtain a filter cake, the filtrate is oxidized by aeration to remove Ca2+、Mg2+Plasma impurities.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention relates to a method for preparing a titanium-rich material by leaching ilmenite with waste hydrochloric acid of titanium white produced by a chlorination process and comprehensively utilizing the titanium white produced by the chlorination processWaste hydrochloric acid is used as leaching reagent, and leached TiO2The content of the iron oxide red reaches 80-90%, filter cakes obtained after filter pressing are further processed to prepare titanium-rich ore or artificial rutile, and the filtrate is subjected to impurity removal to prepare iron oxide red and ammonium chloride, wherein Fe in the iron oxide red2O3The mass content of (A) is more than 90%, and the mass content of ammonium chloride in the ammonium chloride crystal is more than 97%.
(2) The method comprehensively utilizes the waste hydrochloric acid discharged in the production of titanium dioxide by a chlorination process, reduces environmental pollution and treatment cost, realizes a new method for preparing a titanium-rich material and byproducts of iron oxide red and ammonium chloride by using the waste hydrochloric acid, can radically solve the problem that the waste hydrochloric acid of the titanium dioxide by the chlorination process cannot be recycled, realizes the reutilization of wastes, has simple process flow and operation, is easy to realize, accords with the carbon footprint and life cycle theory advocated internationally at present, and has good economic benefit and social benefit.
Drawings
FIG. 1 is a process flow chart for preparing a titanium-rich material and comprehensively recycling the material by leaching ilmenite with titanium white waste hydrochloric acid by a chlorination method.
Detailed Description
The present invention is further described below with reference to examples.
Example 1
A process for preparing the rich-Ti material from the ilmenite by hydrochloric acid leaching of waste titanium white by chlorination method includes such steps as leaching and filtering ilmenite, baking filter cake to obtain rich-Ti material, cyclic use of washing liquid, and concentrating mother liquid to obtain iron oxide red and ammonium chloride.
(1) Controlling the mass concentration of titanium dioxide waste hydrochloric acid in the chlorination process at 20%, and controlling the mass volume ratio of the titanium dioxide waste hydrochloric acid to ilmenite at GTiO2:VHClMixing in the ratio of 1 to 2, stirring at 30r/min for 5 hr at 30 deg.c, leaching with waste hydrochloric acid, and hot filtering.
(2) Drying and calcining the filter cake to prepare a titanium-rich material: the filtrate after filter cake filtration is processed by Ca2+、Mg2+FeCl obtained after ion impurity removal process3And FeCl2The mother liquor enters the preparation process of iron oxide red and ammonium chloride. And washing the filtered filter cake for 2 times by using tap water, and recycling the washed washing liquid. And (3) placing the filter cake in a muffle furnace for drying and calcining, wherein the temperature is controlled within 350 ℃, and the drying time is 4 hours.
(3) The washing solution was returned to the leaching step, and used to prepare waste hydrochloric acid with a concentration of 20% for use as a leaching solution.
(4) Concentrating the mother liquor to prepare iron oxide red and ammonium chloride: will pass through Ca2+、Mg2+FeCl obtained after ion impurity removal process3And FeCl2The mother liquor was further concentrated with steam to control the total Fe concentration within the range of 80g/L, and after air oxidation for 30min, the ammonium bicarbonate solution concentration was controlled within the range of 100g/L as V (FeCl)3)/V(NH4HCO3) Adding ammonium bicarbonate solution at a volume ratio of 1/2.6 to ensure that the ammonium bicarbonate solution is excessive, reacting until pink ferric carbonate appears, standing for 30min, filtering, washing and precipitating, drying and calcining the precipitate in a muffle furnace, raising the calcining temperature from room temperature to 650 ℃, keeping the temperature at 650 ℃ for 30min, naturally cooling to room temperature, and grinding to obtain the iron oxide red.
And (3) concentrating the filtered and washed solution at the temperature of 80 ℃ until crystals appear, then slowly cooling, and crystallizing to obtain the ammonium chloride product.
Example 2
A process for preparing the rich-Ti material from the ilmenite by hydrochloric acid leaching of waste titanium white by chlorination method includes such steps as leaching and filtering ilmenite, baking filter cake to obtain rich-Ti material, cyclic use of washing liquid, and concentrating mother liquid to obtain iron oxide red and ammonium chloride.
(1) Controlling the mass concentration of titanium dioxide waste hydrochloric acid in the chlorination process at 25%, and controlling the mass volume ratio of the titanium dioxide waste hydrochloric acid to ilmenite at GTiO2:VHClMixing in the ratio of 1 to 5, stirring at 60r/min for 9 hr at 80 deg.c, leaching with waste hydrochloric acid, and hot filtering.
(2) Drying of the filter cakeCalcining to prepare a titanium-rich material: the filtrate after filter cake filtration is processed by Ca2+、Mg2+FeCl obtained after ion impurity removal process3And FeCl2The mother liquor enters the preparation process of iron oxide red and ammonium chloride. And washing the filtered filter cake for 3 times by using tap water, and recycling the washed washing liquid. And (3) placing the filter cake in a muffle furnace for drying and calcining, wherein the temperature is controlled within 450 ℃, and the drying time is 2 hours.
(3) The washing solution was returned to the leaching step, and used to prepare waste hydrochloric acid with a concentration of 25% for use as a leaching solution.
(4) Concentrating the mother liquor to prepare iron oxide red and ammonium chloride: will pass through Ca2+、Mg2+FeCl obtained after ion impurity removal process3And FeCl2The mother liquor of (2) was further concentrated with steam to control the total Fe concentration within the range of 160g/L, and after air oxidation for 60min, the ammonium bicarbonate solution concentration was controlled within the range of 180g/L as V (FeCI)3)/V(NH4HCO3) Adding ammonium bicarbonate solution at a volume ratio of 1/3.8 to ensure that the ammonium bicarbonate solution is excessive, reacting until pink ferric carbonate appears, standing for 60min, filtering, washing and precipitating, drying and calcining the precipitate in a muffle furnace, raising the calcining temperature from room temperature to 650 ℃, keeping the temperature at 650 ℃ for 50min, naturally cooling to room temperature, and grinding to obtain the iron oxide red.
And (3) concentrating the filtered and washed solution at the temperature of 95 ℃, and then slowly cooling and crystallizing to obtain an ammonium chloride product.
Example 3
A process for preparing the rich-Ti material from the ilmenite by hydrochloric acid leaching of waste titanium white by chlorination method includes such steps as leaching and filtering ilmenite, baking filter cake to obtain rich-Ti material, cyclic use of washing liquid, and concentrating mother liquid to obtain iron oxide red and ammonium chloride.
(1) Controlling the mass concentration of the titanium dioxide waste hydrochloric acid in the chlorination process within 22 percent, and controlling the mass concentration of the titanium dioxide waste hydrochloric acid and the titanium concentrate to be G according to the mass-volume ratioTiO2:VHClMixing in the range of 1:3, stirring at 40r/min for 6 hr,controlling the temperature within 50 ℃, leaching the waste hydrochloric acid, and filtering while the waste hydrochloric acid is hot after leaching.
(2) Drying and calcining the filter cake to prepare a titanium-rich material: the filtrate after filter cake filtration is processed by Ca2+、Mg2+FeCl obtained after ion impurity removal process3And FeCl2The mother liquor enters the preparation process of iron oxide red and ammonium chloride; and washing the filtered filter cake for 2 times by using tap water, and recycling the washed washing liquid. And (3) placing the filter cake in a muffle furnace for drying and calcining, wherein the temperature is controlled within 400 ℃, and the drying time is 3 hours.
(3) The washing solution was returned to the leaching step, and used as a leaching solution by preparing waste hydrochloric acid with a concentration of 22%.
(4) Concentrating the mother liquor to prepare iron oxide red and ammonium chloride: will pass through Ca2+、Mg2+FeCl obtained after ion impurity removal process3And FeCl2The mother liquor is further concentrated by steam to control the total Fe concentration within the range of 100g/L, and after air oxidation is carried out for 40min, an excessive ammonium bicarbonate solution is added, the concentration of the ammonium bicarbonate solution is controlled within the range of 120g/L, and the solution is concentrated according to V (FeCl)3)/V(NH4HCO3) Adding ammonium bicarbonate solution at a volume ratio of 1/3.0, reacting until pink iron carbonate appears, standing for 50min, filtering, washing, precipitating, oven drying and calcining the precipitate in a muffle furnace, raising the calcining temperature from room temperature to 650 ℃, keeping the temperature at 650 ℃ for 40min, naturally cooling to room temperature, and grinding to obtain iron oxide red.
And (3) concentrating the filtered and washed solution at the temperature of 90 ℃, and then slowly cooling and crystallizing to obtain an ammonium chloride product.
The raw ilmenite and the products recovered synthetically were subjected to content detection analysis, in which for the mass content analysis of the recovered products (titanium-rich material, red iron oxide, ammonium chloride), 4 measurements were made per example, averaged to reduce the detection error.
Table 1 examples 1-3 ilmenite composition analysis table
| Item | TiO2％ | Tfe％ | FeO％ | Fe2O3％ |
| Example 1 | 46.72 | 33 | 36.78 | 6.29 |
| Example 2 | 46.84 | 34.43 | 37.72 | 7.29 |
| Example 3 | 47.81 | 34.42 | 38.01 | 6.95 |
TABLE 2 Mass analysis tables of titanium-rich materials prepared in examples 1 to 3
Table 3 table for mass analysis of iron oxide red prepared in examples 1 to 3
TABLE 4 Mass analysis of ammonium chloride prepared in examples 1 to 3
Claims (5)
1. A method for preparing a titanium-rich material by leaching ilmenite with titanium white waste hydrochloric acid by a chlorination process and comprehensively utilizing the titanium-rich material is characterized by comprising the following steps of: comprises leaching and filtering ilmenite: mixing ilmenite and titanium white waste hydrochloric acid obtained by a chlorination process according to a certain mass-volume ratio, leaching the waste hydrochloric acid under the condition of stirring, and filtering the mixture while the mixture is hot after the leaching is finished; drying and calcining the filter cake to prepare a titanium-rich material, recycling washing liquor, and concentrating mother liquor to prepare iron oxide red and ammonium chloride;
wherein: the mass concentration of the titanium white waste hydrochloric acid produced by the chlorination method is 20-25%, and the mass volume ratio G isTiO2:VHClThe stirring speed is controlled to be 30-60 r/min, the stirring time is controlled to be 5-9 hours, and the stirring temperature is controlled to be 30-80 ℃;
the drying and calcining temperature is 350-450 ℃, and the drying time is 2-4 hours;
the concentration of the mother liquor for preparing the iron oxide red and the ammonium chloride is specifically as follows: will pass through Ca2+、Mg2+FeCl obtained after impurity removal process3And FeCl2Further concentrating with steam as mother liquor, air oxidizing, adding ammonium bicarbonate solution, reacting until pink ferric carbonate appears, standing for 30-60 min, filtering, washing, precipitating, and placing the precipitate in a muffle furnaceDrying and calcining to obtain iron oxide red; and concentrating the filtered and washed solution at the temperature of 80-95 ℃ until crystals appear, then cooling to room temperature, and crystallizing to obtain an ammonium chloride product.
2. The method for preparing the titanium-rich material and comprehensively utilizing the titanic iron ore by using the hydrochloric acid leaching of the chlorination process titanium dioxide waste as claimed in claim 1, is characterized in that: the preparation of the titanium-rich material by drying and calcining the filter cake comprises the following steps: and washing the filter cake after filter pressing for 2-3 times by using tap water, then placing the filter cake in a muffle furnace for drying and calcining, and recycling the washed washing liquid.
3. The method for preparing the titanium-rich material and comprehensively utilizing the titanic iron ore by using the hydrochloric acid leaching of the chlorination process titanium dioxide waste as claimed in claim 1, is characterized in that: the washing liquor recycling specifically comprises the step of returning the washing liquor to the leaching process of ilmenite, and using the washing liquor to prepare waste hydrochloric acid, so that the mass concentration of the waste hydrochloric acid is controlled within the range of 20-25% and the waste hydrochloric acid is used as leaching liquor.
4. The method for preparing the titanium-rich material and comprehensively utilizing the titanic iron ore by using the hydrochloric acid leaching of the chlorination process titanium dioxide waste as claimed in claim 1, is characterized in that: adopting steam concentration to control the total Fe concentration within the range of 80-160 g/L, carrying out air oxidation for 30-60 min, and then carrying out treatment according to V (FeCI)3)/V(NH4HCO3) 1: adding an ammonium bicarbonate solution according to the volume ratio of 2.6-3.8, wherein the concentration of the ammonium bicarbonate solution is 100-180 g/L.
5. The method for preparing the titanium-rich material and comprehensively utilizing the titanic iron ore by using the hydrochloric acid leaching of the chlorination process titanium dioxide waste as claimed in claim 1, is characterized in that: and (3) raising the calcination temperature from room temperature to 650 ℃, preserving the heat at 650 ℃ for 30-50 min, naturally cooling to room temperature, and grinding to obtain the iron oxide red.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1710122A (en) * | 2005-06-16 | 2005-12-21 | 昆明理工大学 | Method for preparing rutile type titanium-rich material from primary titanium-rich material |
| CN105621495A (en) * | 2014-10-31 | 2016-06-01 | 陕西启源科技发展有限责任公司 | Method for preparing high purity iron oxide red from picking waste liquid |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1710122A (en) * | 2005-06-16 | 2005-12-21 | 昆明理工大学 | Method for preparing rutile type titanium-rich material from primary titanium-rich material |
| CN105621495A (en) * | 2014-10-31 | 2016-06-01 | 陕西启源科技发展有限责任公司 | Method for preparing high purity iron oxide red from picking waste liquid |
Non-Patent Citations (1)
| Title |
|---|
| 国内外钛矿和富钛料生产现状及发展趋势;余家华等;《世界有色金属》;20030630(第6期);第4-8页 * |
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Denomination of invention: Preparation and Comprehensive Utilization of Titanium Rich Materials by Leaching Ilmenite from Titanium Dioxide Waste Hydrochloric Acid by Chlorination Method Effective date of registration: 20230803 Granted publication date: 20201030 Pledgee: China Construction Bank Corporation Zibo Boshan sub branch Pledgor: SHANDONG DOGUIDE GROUP Co.,Ltd. Registration number: Y2023980050752 |