CN105967231A - Method for extracting TiO2 from white clay - Google Patents
Method for extracting TiO2 from white clay Download PDFInfo
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- CN105967231A CN105967231A CN201610456901.0A CN201610456901A CN105967231A CN 105967231 A CN105967231 A CN 105967231A CN 201610456901 A CN201610456901 A CN 201610456901A CN 105967231 A CN105967231 A CN 105967231A
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- 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
- C01G23/053—Producing by wet processes, e.g. hydrolysing titanium salts
- C01G23/0532—Producing by wet processes, e.g. hydrolysing titanium salts by hydrolysing sulfate-containing salts
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention relates to a method for extracting TiO2 from white clay. The method comprises steps as follows: (1), an alkaline solution is added to the white clay, Al2O3 and SiO2 are leached, and filter residues a are collected; (2), the filter residues a are leached in a leaching liquid, CaO, MgO, Fe2O3, Na2O, K2O and the like are removed, and secondary filter residues b are collected; (3), sulfuric acid is added to the filter residues b, TiO2 is extracted, and a filtrate c is obtained; (4), the filtrate c is heated and concentrated, pH of the filtrate is regulated to 2.5-4.0 with the alkaline solution, then the filtrate is mixed with hot water, the mixed solution is heated to be boiled, TiOSO4 is hydrolyzed, solids obtained through hydrolysis are calcined, and TiO2 with the purity higher than 94% is obtained finally. According to the method for extracting TiO2 from the white clay, CO2 in the white clay can be effectively extracted, the process of the method is simple, the product purity is higher, the white clay is comprehensively utilized, the economic benefit is produced, and the method plays an important role in the aspects of increase of economic output and reduction of environmental pollution.
Description
Technical field
The present invention relates to the extracting method of titanium dioxide, be specifically related to a kind of method extracting titanium dioxide from white clay.
Background technology
Titanium is one of element abundant in the earth's crust, in terms of titanium dioxide, accounts for the 1.06% of earth's crust weight.Titanium and alloy thereof have strong corrosion resistance (corrosion rate in the seawater is bordering on zero), high intensity, high-low temperature resistant, light and nonmagnetic, and there is the excellent properties such as hydrogen storage, marmem and superconduction, be therefore national defense industry, space flight, biomedical material, chemical industry, electric power and the preferred material in anticorrosive high-abrasive material field.Therefore, titanium application in modern society is quite varied.In recent years, along with the rutile as titanium resource is petered out and rise in price, the research extracting titanium from the rich titanium waste residue that cheap ilmenite and commercial production produce the most progressively is carried out.
At present, the raw material extracting titanium is mainly titanium-containing blast furnace slag, the side-product that it is discharged when being to smelt vanadium titano-magnetite from blast furnace.Process titanium-containing blast furnace slag and need high-temperature process, pre-oxidation and pressure leaching etc..These methods not only flow process is complex, and there is the problems such as energy consumption is high, equipment requirements is harsh.As patent documentation CN101781717B describes a kind of method of the portly compound of separation and Extraction from Ti-containing slag: add acidic oxide in the presence of a reducing agent, crystallisation by cooling after mixing under high temperature (about 1300 DEG C).Although the method technological process is short, equipment simple, but reaction temperature is high, and energy consumption is big, and in its end-product, dioxy turns to content and is only more than 70%, and extraction effect is the most undesirable.
The garbage that flyash discharges as coal-burning power plant, annual discharge capacity is up to more than one hundred million ton.Owing to it contains Al2O3、SiO2、Fe2O3、CaO、MgO、TiO2Etc. multiple can be as the composition of the raw material of industry, it has been expanded and has studied widely by the scientific research institution of lot of domestic and international.At present, most commonly seen is exactly extraction aluminium oxide from flyash.In numerous extracting method, pioneering " a step acid pasting technique " (the patent documentation CN102145905A) of Shenhua Group owing to technological process is short, dissolution rate high and be gradually widely used.But, this method can produce substantial amounts of tailings after carrying aluminum and be commonly called as white clay, easily environment is caused secondary pollution.
Through analyze find, white clay be mainly composed of SiO2And Al2O3, sum of the two accounts for more than the 80% of total content, shows higher resource and be worth in terms of sial resource reutilization.The most existing substantial amounts of document is about utilizing it to carry out the synthesis of the high value added product such as molecular sieve and alumina silicate glass, and for therefrom extracting the report that the research of rare valuable metal is not the most correlated with further.In the case of Resources is petered out, the comprehensive utilization of this type of resource will cause to be paid close attention to widely.In flyash, the content of titanium is relatively low, and only 1.84%, unsuitable extracting directly.But titanium dioxide does not dissolves in hydrochloric acid, is enriched with in the tailings i.e. white clay of acidity extraction aluminium oxide, and therefore from white clay, recovery Pd has higher production value and Significance for Environment.
Summary of the invention
It is an object of the invention to provide a kind of method extracting titanium dioxide with white mud as a raw material, the purity of the titanium dioxide that the method flow process is simple, economic and obtained is high.
The present invention extracts the method for titanium dioxide from white clay and comprises the following steps:
(1) adding alkaline solution in white clay, reaction, by Al2O3、SiO2Leach, filter, collect filtering residue a；
(2) filtering residue a is leached in acid leaching liquid, make CaO, MgO, Fe2O3、Na2O, K2O enters in solution, filters, and collects secondary filtering residue b；
(3) in filtering residue b, add sulphuric acid, make TiO2It is dissolved in leaching liquid, generates TiOSO4, filter, obtain titaniferous filtrate c；
(4) filtrate c heating is concentrated, add alkaline solution regulation filtrate pH to 2.5～4.0, then gained filtrate is mixed with hot water, be heated to boiling, TiOSO4Hydrolyzing, the solid obtained by calcining hydrolysis i.e. obtains titanium dioxide solids.
Wherein, before step (1), also include the step that white clay is washed to neutrality, dry for standby.
Alkaline solution described in the most above-mentioned (1) step is NaOH or KOH；Concentration is 3mol/L～6mol/L, preferably 5mol/L；Solid-liquid mass ratio during leaching is 1:(5～8), preferably 1:7；Leaching temperature is 50～90 DEG C, preferably 80 DEG C；Leaching time is 3～7h, preferably 4h.Al in gained filtrate3+、Si4+The study on the synthesis of molecular sieve can be made further.
Leaching liquid described in the most above-mentioned (2) step be concentration be the hydrochloric acid solution of 5mol/L～8mol/L, preferably 6mol/L；Solid-liquid mass ratio during leaching is (1:3)～(1:6), preferably 1:4；Leaching temperature is 50～80 DEG C, preferably 60 DEG C；Leaching time is: 2～4h, preferably 3h.
The sulfuric acid concentration of the most above-mentioned (3) step is 85%～92%, and solid-liquid mass ratio is 1:3～5, leaching time 0.5～1h, and the extraction rate recording Ti is 85%～90%.
The most above-mentioned (4) step regulates alkali liquor added by pH and includes ammonia, NaHCO3、Na2CO3, NaOH, KOH, KHCO3、K2CO3、(NH4)2CO3、NH4HCO3, preferably ammonia.Further, by the volume concentration 30%～60% of filtrate c in (4) step, thickening temperature is 60～80 DEG C, and hot water temperature is 80～100 DEG C, and titanium liquid is 1:2～1:5 with the volume ratio of hot water, preferably 1:3, hydrolysis time 2h～5h, preferably 3h, calcining heat is 750 DEG C～900 DEG C, calcination time 1h～2h, gained TiO2Purity 94%.
The inventive method step is simple, it is possible to efficiently extracting the titanium in white clay, gained titanium dioxide purity is higher, it is achieved that refuse reclamation, and provides substantial amounts of titanium material for commercial production, improves economic benefit；In addition the Al in the inventive method gained by-product3+、Si4+Also can make the study on the synthesis of molecular sieve further, improve the utilization rate of white clay.
Accompanying drawing explanation
Fig. 1 is the flow chart of embodiment of the present invention.
Detailed description of the invention
The white clay used in following instance is the tailings that the method recorded according to patent documentation CN102145905A obtains after Junger coalfield flyash extracts aluminium oxide, and its specific chemical composition is shown in Table one.
The chemical component table (wt%) of table one white clay
| SiO2 | Al2O3 | TiO2 | CaO | MgO | Fe2O3 | K2O | Na2O | LOI | Amount to |
| 68.36 | 12.83 | 4.01 | 0.47 | 0.28 | 0.27 | 0.10 | 0.30 | 13.26 | 99.88 |
In conjunction with drawings and Examples, the detailed description of the invention of the present invention is further described, but the invention is not restricted among the practical range of the following stated.
Embodiment 1 uses the inventive method to extract titanium
Titaniferous white clay, through being washed to neutrality, is dried.Using the sodium hydroxide solution of 5mol/L as leaching reagent, leaching solid-liquid mass ratio is 1:7, in temperature 80 DEG C, stirring, leaches 4h, by Al2O3、SiO2Leach, filter, wash, obtain filtering residue a.Being dissolved in the hydrochloric acid of 6mol/L by filtering residue a, solid-liquid mass ratio is 1:4, temperature 60 C, stirring, reacts 3h, makes CaO, MgO, Fe2O3、Na2O, K2O enters in solution, filters, washes, obtains filtering residue b.Being dissolved in the concentrated sulphuric acid of 92% by filtering residue b, solid-liquid mass ratio is 1:3, stirring, reacts 0.5h, makes TiO2It is dissolved in leaching liquid, generates TiOSO4, filter, in ICP-OES measures filtrate, the extraction rate of titanium is 90%.Filtrate being heated at a temperature of 75 DEG C, volume concentration 50%, drip ammonia, the pH=2.68 of regulation filtrate, then mix with the volume ratio of 1:3 with 100 DEG C of hot water, stirring, boil, stop after reaction 3h, hydrolysis generates the hydration TiO of white2Precipitation.Precipitation is filtered, wash, dry after under the conditions of 900 DEG C calcine 1h, obtain the TiO that purity is 96.2%2。
Embodiment 2 uses the inventive method to extract titanium
Titaniferous white clay, through being washed to neutrality, is dried.Using the sodium hydroxide solution of 5mol/L as leaching reagent, leaching solid-liquid mass ratio is 1:5.5, in temperature 80 DEG C, stirring, leaches 4h, filters, washes, stays slag a.Being dissolved in the hydrochloric acid of 6mol/L by filtering residue a, solid-liquid mass ratio is 1:4, temperature 60 C, stirring, reacts 3h, filters, washes, stays slag b.Being dissolved in the concentrated sulphuric acid of 92% by filtering residue b, solid-liquid mass ratio is 1:3, stirring, reacts 0.5h, filters, and in ICP-OES measures filtrate, the extraction rate of titanium is 87%.Filtrate being heated at a temperature of 60 DEG C, volume concentration 40%, drip ammonia, the pH=3.15 of regulation filtrate, then mix with the volume ratio of 1:3 with 90 DEG C of hot water, stirring, stop after boiling reaction 3h, hydrolysis generates the hydration TiO of white2Precipitation.Precipitation is filtered, wash, dry after under the conditions of 900 DEG C calcine 1h, obtain the TiO that purity is 95.1%2。
Embodiment 3 uses the inventive method to extract titanium
Titaniferous white clay, through being washed to neutrality, is dried.Using the sodium hydroxide solution of 5mol/L as leaching reagent, leaching solid-liquid mass ratio is 1:6, in temperature 90 DEG C, stirring, leaches 4h, filters, washs, stays slag a.Being dissolved in the hydrochloric acid of 6mol/L by filtering residue a, solid-liquid mass ratio is 1:5, temperature 60 C, stirring, reacts 3h, filters, washs, stays slag b.Being dissolved in the concentrated sulphuric acid of 89% by filtering residue b, solid-liquid mass ratio is 1:3, stirring, reacts 1h, filters, and in ICP-OES measures filtrate, the extraction rate of titanium is 85.2%.Filtrate being heated at a temperature of 60 DEG C, volume concentration 60%, drip ammonia, the pH=4.0 of regulation filtrate, then mix with the volume ratio of 1:3 with 85 DEG C of hot water, stirring, stop after boiling reaction 3h, hydrolysis generates the hydration TiO of white2Precipitation.Precipitation is filtered, wash, dry after under the conditions of 850 DEG C calcine 1.5h, obtain the TiO that purity is 94.5%2。
Embodiment 4 uses the inventive method to extract titanium
Titaniferous white clay, through being washed to neutrality, is dried.Using the sodium hydroxide solution of 5mol/L as leaching reagent, leaching solid-liquid mass ratio is 1:7, in temperature 70 C, stirring, leaches 5h, filters, washs, stays slag a.Being dissolved in the hydrochloric acid of 6mol/L by filtering residue a, solid-liquid mass ratio is 1:5, temperature 60 C, stirring, reacts 3h, filters, washs, stays slag b.Being dissolved in the concentrated sulphuric acid of 90% by filtering residue b, solid-liquid mass ratio is 1:3, stirring, reacts 1h, filters, and in ICP-OES measures filtrate, the extraction rate of titanium is 87%.Filtrate being heated at a temperature of 70 DEG C, volume concentration 50%, drip ammonia, the pH=3.5 of regulation filtrate, then mix with the volume ratio of 1:3.5 with 90 DEG C of hot water, stirring, stop after boiling reaction 3h, hydrolysis generates the hydration TiO of white2Precipitation.Precipitation is filtered, wash, dry after under the conditions of 850 DEG C calcine 2h, obtain the TiO that purity is 95.5%2。
Embodiment 5 uses the inventive method to extract titanium
Titaniferous white clay, through being washed to neutrality, is dried.Using the sodium hydroxide solution of 6mol/L as leaching reagent, leaching solid-liquid mass ratio is 1:8, in temperature 60 C, stirring, leaches 6h, by Al2O3、SiO2Leach, filter, wash, obtain filtering residue a.Being dissolved in the hydrochloric acid of 5mol/L by filtering residue a, solid-liquid mass ratio is 1:6, temperature 60 C, stirring, reacts 3h, makes CaO, MgO, Fe2O3、Na2O, K2O enters in solution, filters, washes, obtains filtering residue b.Being dissolved in the concentrated sulphuric acid of 92% by filtering residue b, solid-liquid mass ratio is 1:2, stirring, reacts 0.5h, makes TiO2It is dissolved in leaching liquid, generates TiOSO4, filter, in ICP-OES measures filtrate, the extraction rate of titanium is 83.5%.Filtrate being heated at a temperature of 70 DEG C, volume concentration 30%, drip ammonia, the pH=4 of regulation filtrate, then mix with the volume ratio of 1:3 with 80 DEG C of hot water, stirring, boil, stop after reaction 3h, hydrolysis generates the hydration TiO of white2Precipitation.Precipitation is filtered, wash, dry after under the conditions of 750 DEG C calcine 1h, obtain the TiO that purity is 94.2%2。
Embodiment 6 uses the inventive method to extract titanium
Titaniferous white clay, through being washed to neutrality, is dried.Using the sodium hydroxide solution of 6mol/L as leaching reagent, leaching solid-liquid mass ratio is 1:5, in temperature 80 DEG C, stirring, leaches 4h, by Al2O3、SiO2Leach, filter, wash, obtain filtering residue a.Being dissolved in the hydrochloric acid of 5mol/L by filtering residue a, solid-liquid mass ratio is 1:6, temperature 75 DEG C, stirring, reacts 3h, makes CaO, MgO, Fe2O3、Na2O, K2O enters in solution, filters, washes, obtains filtering residue b.Being dissolved in the concentrated sulphuric acid of 92% by filtering residue b, solid-liquid mass ratio is 1:2, stirring, reacts 0.5h, makes TiO2It is dissolved in leaching liquid, generates TiOSO4, filter, in ICP-OES measures filtrate, the extraction rate of titanium is 84.5%.Filtrate being heated at a temperature of 80 DEG C, volume concentration 60%, drip ammonia, the pH=3.8 of regulation filtrate, then mix with the volume ratio of 1:3 with 95 DEG C of hot water, stirring, boil, stop after reaction 3h, hydrolysis generates the hydration TiO of white2Precipitation.Precipitation is filtered, wash, dry after under the conditions of 800 DEG C calcine 1h, obtain the TiO that purity is 94.7%2。
Claims (8)
1. the method extracting titanium dioxide from white clay, comprises the following steps:
(1) adding alkaline solution in white clay, reaction, by Al2O3、SiO2Leach, filter, receive
Collection filtering residue a；
(2) filtering residue a is leached in acid leaching liquid, make CaO, MgO, Fe2O3、Na2O,
K2O enters in solution, filters, and collects secondary filtering residue b；
(3) in filtering residue b, add sulphuric acid, make TiO2It is dissolved in leaching liquid, generates TiOSO4,
Filter, obtain filtrate c；
(4) filtrate c heating is concentrated, regulate filtrate pH to 2.5～4.0 with alkaline solution, then
Mix with hot water, be heated to boiling, TiOSO4Hydrolyzing, the solid obtained by calcining hydrolysis is i.e.
Obtain titanium dioxide solids.
Method the most according to claim 1, it is characterised in that also wrapped before step (1)
Include the step that white clay is washed to neutrality, dry for standby.
Method the most according to claim 1 and 2, it is characterised in that described in step (1)
Alkaline solution is NaOH or KOH；Concentration is 3mol/L～6mol/L, preferably 5mol/L；Leaching
Solid-liquid mass ratio when taking is 1:(5～8), preferably 1:7；Leaching temperature is 50～90 DEG C, preferably
80℃；Leaching time is 3～7h, preferably 4h.
4. according to the method described in any one in claim 1-3, it is characterised in that step (2)
Described leaching liquid be concentration be the hydrochloric acid solution of 5mol/L～8mol/L, preferably 6mol/L；Leaching
Solid-liquid mass ratio when taking is (1:3)～(1:6), preferably 1:4；Leaching temperature is 50～80 DEG C,
Preferably 60 DEG C；Leaching time is: 2～4h, preferably 3h.
5. according to the method described in any one in claim 1-4, it is characterised in that step (3)
Sulfuric acid concentration be 85%～92%, solid-liquid mass ratio is 1:3～1:5, leaching time 0.5～1h.
6. according to the method described in any one in claim 1-5, it is characterised in that step (4)
Alkali liquor used by middle regulation pH includes ammonia, NaHCO3、Na2CO3, NaOH, KOH, KHCO3、
K2CO3、(NH4)2CO3、NH4HCO3, preferably ammonia.
7. according to the method according to any one of claim 1-6, it is characterised in that by step (4)
The volume concentration 30%～60% of described filtrate c, thickening temperature is 60～80 DEG C, and hot water temperature is
80～100 DEG C, described filtrate c is 1:2～1:5, preferably 1:3 with the volume ratio of hot water；Hydrolysis time
2～5h, preferably 3h.
8. according to the method described in any one in claim 1-7, it is characterised in that step (4)
Described in calcining heat be 750～900 DEG C, calcination time is 1～2h.
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Inventor after: Wang Liping Inventor after: Li Chao Inventor after: Chi Junzhou Inventor after: Wang Yongwang Inventor after: Chen Dong Inventor after: Wang Rui Inventor after: Dong Hong Inventor before: Wang Liping |
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Application publication date: 20160928 |