CN101812595A - Method for producing artificial rutile from titanium slag - Google Patents
Method for producing artificial rutile from titanium slag Download PDFInfo
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- CN101812595A CN101812595A CN201010170363A CN201010170363A CN101812595A CN 101812595 A CN101812595 A CN 101812595A CN 201010170363 A CN201010170363 A CN 201010170363A CN 201010170363 A CN201010170363 A CN 201010170363A CN 101812595 A CN101812595 A CN 101812595A
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Abstract
A method for producing artificial rutile from titanium slag relates to a method for preparing artificial rutile from titanium slag smelted in an electric furnace, a blast furnace and the like as a raw material through alkali roasting, water washing and hydrochloric acid leaching. The method is characterized by comprising the following steps: (1) mixing titanium slag with alkali, and roasting; (2) performing multi-stage countercurrent washing and solid-liquid separation on the roasted product, and evaporating and concentrating washing water to realize alkali circulation; (3) will be washedLeaching the substance with dilute hydrochloric acid solution to remove impurities; (4) and (3) carrying out solid-liquid separation on the leached ore pulp, washing slag, drying and calcining to prepare the artificial rutile, and circularly regenerating hydrochloric acid. The method has simple process and equipment, easy solving of leaching equipment and materials, high removal rate of impurities such as calcium, magnesium, iron, aluminum and the like, and TiO product2High content, realizes the recycling of alkali and hydrochloric acid and has obvious environmental protection effect. The titanium slag suitable for the invention can be produced in various grades by smelting equipment such as an electric furnace, a blast furnace and the like, and has strong adaptability to raw materials.
Description
Technical field
A kind of method of producing synthetic rutile by using titania slag, relating to a kind of titanium slag that melts out with electric furnace, blast furnace etc. is raw material, is preparing the method for artificial rutile through alkali roasting-water washing-hydrochloric acid extract technology.
Background technology
Owing to reasons such as raw material and smelting technique make the grade of titanium slag lower, and domestic titanium slag major part can not reach the grade requirement, mainly as the raw material of Titanium White Production By Sulfuric Acid Process.The main drawback of Titanium White Production By Sulfuric Acid Process is that the waste discharge amount is bigger.According to statistics, every production 1t titanium dioxide will be discharged the sulfuric acid 8～10t about 20%, ferrous sulfate crystal 2 .5～3.5t, and about acid waste water (below 5%) 200t, acid waste residue 500～600kg, waste gas 2 * 10
4～4 * 10
4m
3, environmental pollution is quite serious.Chlorination process is produced not only good product quality of titanium dioxide, and " three wastes " are few in the production process, administer easily, therefore adopts chlorination process to produce titanium dioxide, is the inexorable trend of social and economic development, is the developing direction of China's titanium industry.
The melting titanium slag is prepared into TiO
2Content is greater than 92% artificial rutile, and to satisfy the preparing titanium white through chlorination process powder or to adopt fluidizing chlorination to prepare the ingredient requirement of titanium sponge, it has great significance to the titanium industry development of China.
According to the document record, the U.S., Norway, Russia etc. have all carried out enrichment and separating treatment research to the electrosmelting titanium slag.
(1) U.S. just successfully worked out a kind of method for preparing artificial rutile from ilmenite as far back as 1972.Ilmenite is reduced into the pig iron and titanium slag with coal or coke earlier in electric furnace, TiO in the artificial rutile of titanium slag gained after the acidleach concentration and separation is handled
2Content adds up to 94.4～96.8%, and the rate of recovery of titanium is 77～88%.Titanium in the ilmenite more than 90% reclaims with the form of titania.
(2) the mid-80, Norway smelts the TiO that contains that from ilmenite
2Produce artificial rutile in 75% the titanium slag and carried out systematic research.Main impure MgO, FeO, CaO and SiO
2This titanium slag resulting artificial rutile product after separating treatment contains TiO
292～94%, foreign matter content and granularity all can satisfy the requirement of fluidized bed chlorination, are better than natural rutile on the chlorination performance.
(3) 1997 years Russia produce artificial rutile to the titanium slag of titanomagnetite concentrate (40% iron, 15～17% titanium dioxide) production and study.The content of titanium dioxide (55～65%) of the titanium slag that electrosmelting titanomagnetite concentrate obtains is than smelting titanic iron ore concentrate low 20～25%.Owing to be rich in the silicate composition in the titanium slag, therefore directly the efficient by chlorination process or sulfuric acid process production titanium dioxide is all too low.Because very tiny, the heterogeneous coexistence of crystallization of slag, the glass mutual-assistance slag that produces during cooling are difficult to pulverize, each alternate liberation degree is little, so the ore dressing separation has very big technical difficulty.The Russia metallurgist has studied the physical chemistry rule of producing artificial rutile by enrichment with anosovite type titanium slag, and the final titanium slag that obtains that separates contains titanium dioxide 85%～95%.In addition, Russia has also carried out the technical scale experiment that two-step approach is smelted titanium slag to v-ti magnetite concentrate, and the degree of metalization of rotary kiln prereduction is 90%.Smelt the titanium slag that in the heating of superpower closed electric furnace through the furnace charge of prereduction and contain TiO
272%, after ore dressing separated, the anosovite product that obtains enrichment contained TiO
2＞92%, other Chemical Composition satisfies the technological standard of titanium slag, and product is used for producing TiCl
4Isolated lightweight part is applied in refractory materials production.
(4) nineteen eighty-two, the patent of application such as Gerald W.Elger has been introduced at 600～1100 ℃ and has been used SO
3Gas and titanium slag reaction make the alkaline-earth metal in the titanium slag form sulfide, and water leaches and removes sulfide then, can obtain to satisfy the used artificial rutile of fluidizing chlorination.
(5) nineties in last century, the patent of applications such as Michel Gueguin has been introduced the method with producing synthetic rutile by using titania slag, earlier titanium slag at a certain temperature with chlorine reaction, then leach with hydrochloric acid, acquisition can be used for the artificial rutile of chlorination production titanium dioxide.
(6) 1999 years, J.P.VAN DYK etc. proposed by adding phosphoric acid salt (as P
2O
5) the oxidation titanium slag, use H then
3PO
4Leach, can make TiO
2Content is brought up to more than 94%, TiO
2The rate of recovery can arrive 77～88%.
(7) 2004 years, Jacobus Philippus Van Dyk etc. proposed oxidation-reduction-method of pickling enrichment titanium slag.700～950 ℃ of temperature, oxidation titanium slag 30min in the oxidizing atmosphere; Then 700～950 ℃ of temperature, reduction-oxidation titanium slag 5min in the reducing atmosphere; Leach with hydrochloric acid or sulfuric acid at last and can obtain TiO
2Content is greater than 90% rich titanium material.
The domestic present Research of China:
(1) to the nineties in last century, the Sui Zhitong of Northeastern University professor is in conjunction with composing the resource characteristics of depositing multiple valuable element in China's complex ore, and the comprehensive utilization at secondary resource after its choosing, the smelting has proposed " selectivity is separated out technology ".Basic fundamental thought is: 1. create the proper physical electrochemical conditions, impel the valuable element that intersperses among in each mineral facies under the driving of chemical potential gradient, optionally shift and be enriched in the mineral facies of design, finish " selective enrichment "; 2. rationally control correlative factor, promote " selectivity is separated out and grown up " of enrichment phase; 3. the modification slag after will handling is finished " selective separation " of " enrichment phase " through ore grinding and sorting.Its technological line is: selective enrichment → selectivity is separated out and is grown up → selective separation.
(2) people such as Northeastern University's tension force utilizes the principle of the titanium slag of traditional type ore deposit hot stove reduction preparation based on " selectivity is separated out ", by preoxidation, add modified methods such as additive and high-temperature heat treatment, can make most TiO in the anosovite
2Under the driving of chemical potential gradient, selective enrichment is in the rutile phase, and separates out and alligatoring.Be insoluble to dilute hydrochloric acid according to rutile, and most of impurity is dissolved in diluted acid in the slag, carries out selective separation with diluted acid.The modification slag is after acid dipping separation, and product is a rutile, TiO
2Content can reach more than 95%.
(3) comrade Wang Yanzhong of Kunming University of Science and Technology has proposed the dilute hydrochloric acid selectivity and has leached the modification titanium slag at the titanium resource of Panzhihua Region, adopts ore deposit acid than 1g: 2ml, and concentration of hydrochloric acid is 20%, 145 ℃ of temperature of reaction, reaction times 7h, TiO
2Content can bring up to 91.2% by 73.87%, and the content of impurity CaO and MgO is less than 1.5% in the leached mud.Meet chlorination process and produce the requirement of titanium dioxide raw material.
(4) to utilize the method for sodium hydroxide clean production of titanium dioxide be to be raw material with the titanium slag to the patent 200610114130.3 of Chinese Academy of Sciences's process engineering institute, make the sodium hydroxide of itself and the 350-550 ℃ preparation intermediate product that reacts, then intermediate product is washed that (or carbonating), acid are molten, preparation anatase titanium dioxide or rutile titanium dioxide after the reduction, hydrolysis, calcining.
Summary of the invention
The prior art of domestic research is handled titanium slag and is needed pressing technology or high-temperature heat treatment, and energy consumption is big, cost is high and to the equipment requirements strictness.The objective of the invention is in order to overcome the deficiencies in the prior art, providing a kind of is raw material with the titanium slag, and technology and equipment are simple, Ca, Mg and Fe aluminium removal of impurity height, the TiO of artificial rutile
2The method of the producing synthetic rutile by using titania slag that content is high.Alkali circulation of the present invention, regeneration of hydrochloric acid and isolation technique have been simplified production process, have improved the technology operability, for the comprehensive utilization of low-grade titanium slag resource and the preparation of artificial rutile provide a valid approach.
The present invention seeks to be achieved through the following technical solutions.
The method of producing synthetic rutile by using titania slag is characterized in that the step of its process comprises:
(1) with titanium slag with after alkali mixes, carry out roasting;
(2) product of roasting carries out multi-stage countercurrent washing, solid-liquid separation, and washing evaporation concentration realizes the alkali circulation;
(3) product after will washing leaches removal of impurities with dilute hydrochloric acid solution;
(4) will leach that solid-liquid separation on ore pulp, wash heat are washed, dry, calcining, preparation artificial rutile, hydrochloric acid cyclic regeneration.
The method of producing synthetic rutile by using titania slag of the present invention, it is characterized in that with titanium slag blended alkali be NaOH, NaCO
3, Ca (OH)
2Or CaCO
3One or more mixtures, titanium slag is 2 with alkali mixing quality ratio: 1-10: 1; Maturing temperature is 400-1000 ℃, and roasting time is 0.5-6h.
The method of producing synthetic rutile by using titania slag of the present invention, it is characterized in that process water that product of roasting washs directly washing to neutral or be not more than sodium hydroxide or the sodium carbonate solution washing of 100g/l with concentration, liquid-solid ratio is 2: 1-8: 1, wash temperature is 25-95 ℃, washing time is 0.5-4h, is washed with water to neutrality after the filtration again.
The method of producing synthetic rutile by using titania slag of the present invention is characterized in that the process that product of roasting washs can carry out by multi-stage countercurrent.Wash water can be realized the alkali circulation by evaporation concentration.
The method of producing synthetic rutile by using titania slag of the present invention, product after it is characterized in that washing is under condition of normal pressure, is that the hydrochloric acid soln of 5%-22% leaches with mass concentration, and hydrochloric acid leachate is admittedly than being 2: 1-8: 1, extraction temperature is 25-95 ℃, and extraction time is 0.5-8h.
The method of producing synthetic rutile by using titania slag of the present invention is characterized in that its hydrochloric acid that leaches usefulness can be regeneration hydrochloric acid.The regeneration of hydrochloric acid technology of industrial application is subjected to the restriction of hydrochloric acid azeotropic point at present, and the concentration of regeneration hydrochloric acid generally is no more than 22%.Hydrochloric acid leaches when producing artificial rutile among the present invention, can realize that low-concentration hcl leaches, and has realized the regeneration and the circulation of hydrochloric acid.
Method of the present invention is at first to utilize the destruction of alkali realization to the titanium slag Solid solution, is implemented in the low-concentration hcl purpose that leaching is removed to metallic impurity such as iron calcium magnaliums under the condition of normal pressure then, thereby obtains high-grade artificial rutile.Technology of the present invention and equipment are simple, and leaching plant and material solve easily, and impurity such as Ca, Mg and Fe aluminium are removed rate height and product TiO
2The content height has been realized the regeneration of alkali circulation and hydrochloric acid, and environment protecting is remarkable.Be applicable to that titanium slag of the present invention can be the various grades that melting equipments such as electric furnace, blast furnace are produced, strong to the adaptability of raw material.
Description of drawings
Fig. 1 is the principle process flow sheet of the inventive method.
Embodiment
Producing the method for artificial rutile, is titanium slag and alkali (NaOH, the NaCO with size fractionated
3, Ca (OH)
2, CaCO
3) one or more mixtures press mass ratio 2: 1-10: 1 mixes, and at maturing temperature 400-1000 ℃ of following roasting time 0.5-6h; Water or concentration are not more than 100g/l sodium hydroxide or sodium carbonate solution is 2 in liquid-solid ratio: 1-8 then: 1, and wash temperature is 25-95 ℃ of following washing time 0.5-4h, the washing slurry filtration also is washed to neutrality, or realizes by the multi-stage countercurrent washing.Wash water can be realized the alkali circulation by evaporation concentration.
After the solid-liquid separation with mass concentration be the hydrochloric acid soln of 5-22% under condition of normal pressure, carry out one-level and leach, hydrochloric acid leachate is admittedly than being 2: 1-8: 1, extraction temperature 25-95 ℃, extraction time 0.5-8h; Leach spent acid through regeneration of hydrochloric acid technology regeneration hydrochloric acid, thereby realize the regeneration and the circulation of hydrochloric acid.Hydrochloric acid leaches the slag that solid-liquid separation on ore pulp is come out, through washing, dry, calcining, preparation artificial rutile.
With following indefiniteness embodiment method of the present invention is further described, helping understanding content of the present invention and advantage thereof, and as the qualification to protection domain of the present invention, protection scope of the present invention is determined by claims.
Embodiment 1
Get TiO
2The electro-titanium slag 100g of content 72%, fine grinding less than 0.074mm, mixes by mass ratio with sodium hydroxide more than 96% at 2: 1, and at 1000 ℃ of following roasting time 2h of maturing temperature; Roasting sample water is 1: 1 in liquid-solid ratio, and wash temperature is 25 ℃ of following washing time 1h, and the washing slurry filtration also repeatedly washs to neutral.Sample mass concentration after the washing be 18% hydrochloric acid soln under condition of normal pressure, carry out one-level and leach, hydrochloric acid leachate is admittedly than being 4: 1,95 ℃ of extraction temperatures, extraction time 4h; Hydrochloric acid leaches the slag that solid-liquid separation on ore pulp is come out, through washing, dry, calcining, preparation artificial rutile.The TiO of artificial rutile
2Content 92.15%.
Embodiment 2
Get TiO
2The electro-titanium slag 100g of content 81% directly mixes by mass ratio with sodium hydroxide without fine grinding at 4: 1, and at 800 ℃ of following roasting time 1h of maturing temperature; The roasting sample is 2: 1 with the 100g/l sodium hydroxide solution in liquid-solid ratio, and wash temperature is 95 ℃ of following washing time 0.5h, and the washing slurry filtration also repeatedly washs to neutral.Sample mass concentration after the washing be 22% hydrochloric acid soln under condition of normal pressure, carry out one-level and leach, hydrochloric acid leachate is admittedly than being 2: 1,85 ℃ of extraction temperatures, extraction time 6h; Hydrochloric acid leaches the slag that solid-liquid separation on ore pulp is come out, through washing, dry, calcining, preparation artificial rutile.The TiO of artificial rutile
2Content 93.18%.
Embodiment 3
Get TiO
2The electro-titanium slag 100g of content 72%, fine grinding less than 0.074mm, mixes by mass ratio with 1: 1 sodium hydroxide of mass ratio and sodium carbonate mixture more than 70% at 8: 1, and at 400 ℃ of following roasting time 6h of maturing temperature; The roasting sample is 8: 1 with the 5g/l sodium hydroxide solution in liquid-solid ratio, and wash temperature is 25 ℃ of following washing time 2h, and the washing slurry filtration also is washed to neutrality.Sample mass concentration after the washing be 15% hydrochloric acid soln under condition of normal pressure, carry out one-level and leach, hydrochloric acid leachate is admittedly than being 6: 1,65 ℃ of extraction temperatures, extraction time 8h; Hydrochloric acid leaches the slag that solid-liquid separation on ore pulp is come out, through washing, dry, calcining, preparation artificial rutile.The TiO of artificial rutile
2Content 93.3%.
Embodiment 4
Get TiO
2The electro-titanium slag 100g of content 72%, fine grinding less than 0.074mm, mixes by mass ratio with yellow soda ash more than 90% at 10: 1, and at 700 ℃ of following roasting time 4h of maturing temperature; The roasting sample is 4: 1 with the 50g/l sodium hydroxide solution in liquid-solid ratio, and wash temperature is 55 ℃ of following washing time 4h, and the washing slurry filtration also is washed to neutrality.Sample mass concentration after the washing be 18% hydrochloric acid soln under condition of normal pressure, carry out one-level and leach, hydrochloric acid leachate is admittedly than being 8: 1,65 ℃ of extraction temperatures, extraction time 5h; Hydrochloric acid leaches the slag that solid-liquid separation on ore pulp is come out, through washing, dry, calcining, preparation artificial rutile.The TiO of artificial rutile
2Content 94.3%.
Embodiment 5
Get TiO
2The electro-titanium slag 100g of content 72%, fine grinding less than 0.074mm, mixes by mass ratio with calcium hydroxide more than 50% at 3: 1, and at 600 ℃ of following roasting time 4h of maturing temperature; The roasting sample is 8: 1 with the 15g/l sodium hydroxide solution in liquid-solid ratio, and wash temperature is 85 ℃ of following washing time 2h, and the washing slurry filtration also is washed to neutrality.Sample mass concentration after the washing be 20% hydrochloric acid soln under condition of normal pressure, carry out one-level and leach, hydrochloric acid leachate is admittedly than being 5: 1,95 ℃ of extraction temperatures, extraction time 6h; Hydrochloric acid leaches the slag that solid-liquid separation on ore pulp is come out, through washing, dry, calcining, preparation artificial rutile.The TiO of artificial rutile
2Content 95.2%.
Embodiment 6
Get TiO
2The electro-titanium slag 100g of content 72%, fine grinding less than 0.074mm, mixes by mass ratio with lime carbonate more than 90% at 2: 1, and at 400 ℃ of following roasting time 6h of maturing temperature; Roasting sample 30g/l sodium hydroxide solution is 4: 1 in liquid-solid ratio, and wash temperature is 45 ℃ of following washing time 1h, and the washing slurry filtration also is washed to neutrality.Sample mass concentration after the washing be 16% hydrochloric acid soln under condition of normal pressure, carry out one-level and leach, hydrochloric acid leachate is admittedly than being 2: 1,85 ℃ of extraction temperatures, extraction time 2h; Hydrochloric acid leaches the slag that solid-liquid separation on ore pulp is come out, through washing, dry, calcining, preparation artificial rutile.The TiO of artificial rutile
2Content 94.8%.
Embodiment 7
Get TiO
2The electro-titanium slag 100g of content 81%, fine grinding less than 0.074mm, mixes by mass ratio with 2: 1 sodium hydroxide of mass ratio and calcium carbonate mixture more than 96% at 4: 1 again, and at 950 ℃ of following roasting time 0.5h of maturing temperature; Roasting sample water is 5: 1 in liquid-solid ratio, and wash temperature is 75 ℃ of following washing time 2h, and the washing slurry filtration also is washed to neutrality.Sample mass concentration after the washing be 18% hydrochloric acid soln under condition of normal pressure, carry out one-level and leach, hydrochloric acid leachate is admittedly than being 2: 1,25 ℃ of extraction temperatures, extraction time 4h; Hydrochloric acid leaches the slag that solid-liquid separation on ore pulp is come out, through washing, dry, calcining, preparation artificial rutile.The TiO of artificial rutile
2Content 93.6%.
Embodiment 8
Get TiO
2The electro-titanium slag 100g of content 81%, fine grinding less than 0.074mm, mixes by mass ratio with 1: 2 calcium hydroxide of mass ratio and calcium carbonate mixture more than 96% at 3: 1 again, and at 800 ℃ of following roasting time 4h of maturing temperature; The roasting sample is 3: 1 with the 50g/l sodium hydroxide solution in liquid-solid ratio, and wash temperature is 75 ℃ of following washing time 1h, and the washing slurry filtration also is washed to neutrality.Sample mass concentration after the washing be 10% hydrochloric acid soln under condition of normal pressure, carry out one-level and leach, hydrochloric acid leachate is admittedly than being 4: 1,95 ℃ of extraction temperatures, extraction time 0.5h; Hydrochloric acid leaches the slag that solid-liquid separation on ore pulp is come out, through washing, dry, calcining, preparation artificial rutile.The TiO of artificial rutile
2Content 92.9%.
Embodiment 9
Get TiO
2The electro-titanium slag 100g of content 81%, fine grinding less than 0.074mm, mixes by mass ratio with yellow soda ash more than 96% at 3: 1, and at 900 ℃ of following roasting time 2h of maturing temperature; Roasting sample water is 3: 1 in liquid-solid ratio, and wash temperature is 95 ℃ of following washing time 1h, and the washing slurry filtration also is washed to neutrality.Sample mass concentration after the washing be 25% hydrochloric acid soln under condition of normal pressure, carry out one-level and leach, hydrochloric acid leachate is admittedly than being 4: 1,70 ℃ of extraction temperatures, extraction time 8h; Hydrochloric acid leaches the slag that solid-liquid separation on ore pulp is come out, through washing, dry, calcining, preparation artificial rutile.The TiO of artificial rutile
2Content 93.9%.
Claims (6)
1. the method for producing synthetic rutile by using titania slag is characterized in that the step of its process comprises:
(1) with titanium slag with after alkali mixes, carry out roasting;
(2) product of roasting carries out multi-stage countercurrent washing, solid-liquid separation, and washing evaporation concentration realizes the alkali circulation;
(3) product after will washing leaches removal of impurities with dilute hydrochloric acid solution;
(4) will leach that solid-liquid separation on ore pulp, wash heat are washed, dry, calcining, preparation artificial rutile, hydrochloric acid cyclic regeneration.
2. the method for producing synthetic rutile by using titania slag according to claim 1, it is characterized in that with titanium slag blended alkali be NaOH, NaCO
3, Ca (OH)
2Or CaCO
3One or more mixtures, titanium slag is 2 with alkali mixing quality ratio: 1-10: 1; Maturing temperature is 400-1000 ℃, and roasting time is 0.5-6h.
3. the method for producing synthetic rutile by using titania slag according to claim 1, it is characterized in that process water that product of roasting washs directly washing to neutral or be not more than sodium hydroxide or the sodium carbonate solution washing of 100g/l with concentration, liquid-solid ratio is 2: 1-8: 1, wash temperature is 25-95 ℃, washing time is 0.5-4h, is washed with water to neutrality after the filtration again.
4. the method for producing synthetic rutile by using titania slag according to claim 1 is characterized in that the process that product of roasting washs can carry out by multi-stage countercurrent; Wash water carries out the alkali circulation by evaporation concentration.
5. the method for producing synthetic rutile by using titania slag according to claim 1, product after it is characterized in that washing is under condition of normal pressure, with mass concentration is that the hydrochloric acid soln of 5%-22% leaches, hydrochloric acid leachate is admittedly than being 2: 1-8: 1, extraction temperature is 25-95 ℃, and extraction time is 0.5-8h.
6. the method for producing synthetic rutile by using titania slag according to claim 1 is characterized in that its hydrochloric acid that leaches usefulness is regeneration hydrochloric acid.
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| CN102139918A (en) * | 2011-02-18 | 2011-08-03 | 昆明冶金研究院 | Method for preparing high-grade synthetic rutile |
| CN102745743A (en) * | 2012-08-08 | 2012-10-24 | 长沙矿冶研究院有限责任公司 | Method for preparing artificial rutile by titanium slags |
| CN102757091A (en) * | 2011-04-28 | 2012-10-31 | 中国科学院过程工程研究所 | Method for preparing high-concentration titanic liquid |
| CN102787194A (en) * | 2012-08-27 | 2012-11-21 | 攀枝花学院 | Method for preparing titanium-rich material by directly reducing molten slag from vanadium-titanium-ferrum concentrate |
| 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 |
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