CN102312102A - Comprehensive utilization method for titanium-contained blast furnace slag - Google Patents
Comprehensive utilization method for titanium-contained blast furnace slag Download PDFInfo
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Abstract
The invention relates to a comprehensive utilization method for titanium-contained blast furnace slag, which belongs to the technical field of chemical industry. The invention aims to improve the comprehensive utilization value of the titanium-contained blast furnace slag, fully utilize resources and eliminate potential safety hazard and environmental pollutions. The comprehensive utilization method for the titanium-contained blast furnace slag comprises the following steps: (a) acid leaching; (b) adding water to a material leached under an acidic condition in the step (a) to carry out water leaching, and filtering; (c) washing and drying a filter cake 1 filtered in the step (b) to obtain a titanium-rich product; (d) regulating the pH of a filtrate 1 filtered in the step (b) to be 6-7, and filtering; (e) washing and purifying a filter cake 2 filtered in the step (d) to obtain an aluminum hydroxide product; (f) regulating the pH of a filtrate 2 filtered in the step (d) to be not less than 12, and filtering; (g) washing and roasting a filter cake 3 filtered in the step (f) to obtain a magnesium oxide product; (h) carrying out evaporation concentration on a filtrate 3 filtered in the step (f), and then filtering; and (i) carrying out centrifuge dripping on a filter cake 4 filtered in the step (h) to obtain a calcium chloride product. By adopting the comprehensive utilization method for the titanium-contained blast furnace slag, the treatment speed is high, byproducts are rich, and metals contained in the titanium-contained blast furnace slag are totally utilized.
Description
Technical field
The present invention relates to a kind of method of comprehensive utilization of titanium-containing blast furnace slag, belong to the chemical industry technical field.
Background technology
Titanium is very wide in distributed in nature, accounts for 0.61% of earth's crust gross weight.China's Sichuan Panzhihua Region is contained has abundant titanium deposit, is the important place of production of China's titanium resource.Titanium metal is mainly used in aircraft industry, is characterized in that hardness is big, light weight, heat-resisting, anticorrosive.Chemical property not too live to be dialled, and valency mainly contains two, three, tetravalence, and wherein titanic is the most stable, and representative oxide compound is titanium oxide (TiO
2), be white indissoluble thing, and have significant amphoteric properties.
Titanium-containing blast furnace slag is mainly derived from Sichuan Flos Bombacis Malabarici vanadium titano-magnetite, and this iron ore is after ore dressing, smelting, and about 50% titanium gets in the blast-furnace smelting slag, forms the titanium-containing blast furnace slag of titaniferous amount about 20%.Can not sell that (industrial request for utilization reaches TiO as rich titanium ore
2>=35%), can not sell as cement additire again and (build slag requirement TiO
2≤1%), thus form the open-air place of solid trade refuse bulk deposition.Along with the continuous exploitation of Flos Bombacis Malabarici vanadium titano-magnetite, this type blast furnace slag totally reaches more than 8,000 ten thousand tons, and with annual 2～3,000,000 tons of speed in continuous increase.For solving scoriaceous pollution of this type and comprehensive utilization of resources, manufacturing enterprise and scientific research institutions have all carried out a large amount of research, and main achievement concentrates on: (1) is as material of construction; Like operating mine slag cement, concrete, ceramic tile, sytull etc., though this type technology can the mass consumption titanium-containing blast furnace slag, because the titaniferous amount is too high; The inaccessible national standard of quality product; And because the local market capacity is little, factors such as outward transport cost height have seriously restricted applying of this type slag treatment technology; (2) produce and contain titanium alloy, smelt like silicothermic process and produce the silicon titanium and contain gold, the fusion electrolysis legal system is equipped with silicon titanium aluminum alloy, and this type technical finesse blast furnace quantity of slag is limited, and then current consumption is big, and production cost is high, is difficult to obtain economic benefit; (3) hydrometallurgy is produced titaniferous compound, produces white titanium pigment as adopting sulfuric acid process, extracts aluminium, titanium, scandium in the titanium-containing blast furnace slag with sulfuric acid process; Produce aluminum oxide with the ammonium sulfate doctor treatment, produce artificial rutile etc. behind the acid hydrolysis solution dealuminzation, this type technology process route is complicated; Product is single; No economic benefit can be sayed, and a large amount of acid and chlorine of using in producing, and brings serious environmental problem.Therefore present titanium-containing blast furnace slag treatment technology ubiquity the problem of deficiency in economic performance.
Using hydrometallurgical processes to handle titanium-containing blast furnace slag at present all is sulfuric acid process usually.This method sulfuric acid consumption is very big, and be about 5 times of titaniferous amount in the blast furnace slag, and cause many problems thus: 1. the sulfuric acid consumption is too big, and production cost is too high, and consuming can not balance with output, and no economic benefit can be sayed; 2. the leaching yield of titanium (about 80%) on the low side is that the blast furnace slag after handling still contains higher titanium, can not be used as cement producting material, causes the accumulation of a large amount of solid waste; 3. owing to calcium content in the titanium-containing blast furnace slag is high, produce a large amount of calcium sulfate sub products behind the sulphur acid leaching residue, no industrial utilization is worth, and forms the secondary pollution of solid waste; 4. during the sulfuric acid to leach blast furnace slag, with producing a large amount of methane and hydrogen sulfide poison gas, harm health of operators, pollution surrounding enviroment; 5. the great deal of high concentration vitriolic uses treatment facility is required height, and investment is big.For this reason, we have researched and developed this salt acid treatment process, and main ingredient in the titanium-containing blast furnace slag is reclaimed comprehensively; Can realize the comprehensive utilization of resource like this; Obtain considerable economic, can make full use of the various acid and the auxiliary material of interpolation again, realize the cleaner production of zero release.
Summary of the invention
Technical problem to be solved by this invention is in order to improve the comprehensive utilization value of titanium-containing blast furnace slag, to make full use of resource and get rid of potential safety hazard and environmental pollution.
Technical scheme of the present invention:
The main chemical compositions of titanium-containing blast furnace slag according to the invention has TiO
2, SiO
2, CaO, MgO, full iron, Al
2O
3, Na
2O, K
2O, MnO, P
2O
5
The method of comprehensive utilization of titanium-containing blast furnace slag of the present invention is accomplished by following steps:
A, employing hydrochloric acid leaching titanium-containing blast furnace slag; The consumption of hydrochloric acid is pressed cations metering input in the titanium-containing blast furnace slag; The most of solution that gets into of metals ions such as calcium, magnesium, aluminium, sodium, potassium; After reaction finished, leaching liquid pH was beneficial to subsequent technique and separates, extracts white lake and magnesium hydroxide products between 2-3;
Material after b, the step a acidleach (solidliquid mixture material) adds water and carries out water extraction, filters;
The purpose of water extraction is further metals ions such as calcium, magnesium, aluminium, sodium, potassium to be got into solution.
Filter cake washing after c, step b filter, drying obtain rich titanium products;
D, step b filtrate filtered are regulated pH=6-7, filter;
Obtain the white lake product after filter cake washing after e, steps d are filtered, the purification;
F, steps d filtrate filtered are regulated pH >=12, filter;
Filter cake washing calcining after g, step f filter obtains magnesium oxide product;
H, step f filtrate filtered evaporation concentration after-filtration;
Filter cake centrifuge dripping after i, step h filter obtains the U-Ramin MC product.
In the above-mentioned steps, step h filtrate filtered can be used as b step water extraction water and recycles; Simultaneously, the wash water liquid after step c filter cake is washed can be used as b step water extraction water and recycles.
Increase the preserved material joining day: get or add soluble chloride during water extraction for increasing preserved material in acidleach, the add-on that increases preserved material is the 0.8-1.2% of blast furnace slag (1% is good).Test shows, increases preserved material and when water extraction, adds, and effect is best.
Increasing preserved material is soluble chlorides such as sodium-chlor, Repone K, directly uses technical grade product to get final product.
Further, the hydrochloric acid consumption is among the step a: the volume ratio of titanium-containing blast furnace slag solid weight and hydrochloric acid liquid:
S (g): L (mL) 1: 1.8-2.2 is good, and the hydrochloric acid consumption is very few, influences the leaching of CaO, MgO etc., and the hydrochloric acid consumption is too much, TiO
2Lose more.Show that through test of many times the hydrochloric acid consumption was best with 1: 2, TiO in immersion liquid this moment
2Rate of loss is less than 1%, and almost 100% leaches Al
2O
3Leaching is also up to 87%.
Titanium-containing blast furnace slag and hydrochloric acid reaction are violent, and utmost point short period of time internal reaction can be accomplished.Therefore the acidolysis time unsuitable long, with the acidolysis time: 10～30min is advisable, and surpasses 30min, and the leaching rate of titanium can descend, less than 10min, reaction not exclusively, and the leaching rate of titanium also descends.
Among the step b amount of water of water extraction with solid-liquid weightmeasurement ratio (S (g): L (mL)) with 1: 4.5-5.5 is advisable, and is at 1: 5 best.Hypervolia is unfavorable for the extraction of follow-up calcium, magnesium, aluminium product, and the water yield is too small, and leaching liquid viscosity increases, and is unfavorable for solid-liquid separation.
The water extraction time is good with 9-12, is best with 10min.Surpass 10min, the leaching rate of titanium can descend, and less than 10min, reaction is incomplete, and the leaching rate of titanium also descends.
The present invention adopts multiple-effect separating agent unslaked lime to separate.Steps d is regulated potential of hydrogen and is adopted unslaked lime to be adjusted to pH=6-7.The potential of hydrogen of regulating step f adopts unslaked lime to be adjusted to pH to pH >=12.
Process characteristic of the present invention:
1. processing speed is fast, acidolysis 15min, and water logging 10min can realize solid-liquid separation, so day output is big.
2. technological design is operated at normal temperatures and pressures, and energy consumption is low, and safety performance is high.
3. use the preserved material that increases of research and development voluntarily, make titanium-containing blast furnace slag titaniferous amount be prone to reach rich titanium slag standard.
4. sub product is abundant, and titanium-containing blast furnace slag institute containing metal is almost all utilized.
5. technology does not have the discharging of waste residue and waste liquid, reaches the zero emission requirement basically.
6. the technology required equipment is simple, and the investment of founding the factory is little, and speed is fast.
Description of drawings
Fig. 1 is the comprehensive utilization process schema of titanium-containing blast furnace slag of the present invention
Embodiment
Below adopting the mode of specific embodiment that the present invention is done further detailed description, is limitation of the present invention but should not be construed as.
The titanium-containing blast furnace slag that following examples adopted is through complete chemical analysis and X-fluorescent spectroscopy, and the chemical ingredients of titanium-containing blast furnace slag is seen table 1.
The main chemical compositions of table 1 titanium-containing blast furnace slag
Visible by table 1, main valuable metal is titanium, aluminium, magnesium, calcium in the titanium-containing blast furnace slag, and the meaning of implementing comprehensive utilization is very big; The maximum quicklime that distributes if it is best to produce U-Ramin MC, is prone to sell, valency is high; Secondly titanium oxide can be considered under low-cost condition, it to be enriched to 35%, sells the production again of carrying out titanium products with rich titanium ore; The content of aluminium sesquioxide can obtain white lake through simple adjustment potential of hydrogen after the solid-liquid separation greater than 10%; Magnesian content 7.51%; Also have comprehensive utilization value, can continue to regulate potential of hydrogen and obtain magnesium hydrate precipitate, obtain light magnesium oxide through calcining again through carrying mother liquor behind the aluminium; Last remaining mother liquor mainly contains U-Ramin MC, obtains technical grade product through evaporation concentration.Whole operational path such as Fig. 1.
1, the screening of acidolysis time
Acidolysis is for the salt that effectively decomposes in the titanium-containing blast furnace slag gets into solution, and titanium is retained in the titanium-containing blast furnace slag, reaches the purpose of separation and concentration.According to the order of metal activity, the hydrochloric acid decomposing oxidation magnesium that should take the lead in.Next is quicklime and aluminum oxide, is titanium oxide at last.The acidolysis time is difficult for long, otherwise the titanium loss amount is very big.Carried out the experiment of acidolysis different time for this reason, tested the content of titanium, calcium, magnesium, aluminium in the acid hydrolysis solution respectively, the result sees table 2.
Table 2 acidolysis time synopsis
Visible by table 2, along with the acidolysis time increases, the leaching rate of calcium, magnesium, aluminium is not had obvious influence, but titanium there is significantly sacrificing.Therefore, the acidolysis time is advisable with 10～30min.Following examples all adopt 15 minutes acidolysis time.
2, the screening of water extraction condition
2.1 the water logging time
With the acidolysis time is that the acid hydrolysis solution of 15min carries out the water extraction reaction.Compared the leaching situation of 10min, 30min, 3h, 8h, 24h under the equal price modification through test, shown that after acidolysis the water extraction metal-salt can be accomplished in the short period of time at the utmost point.Behind the water logging 24h, concentration of metal ions only has faint increase in the leaching liquid, and the leaching rate of aluminium reduces with the leaching time increase on the contrary.Moreover leaching time length is unfavorable for industrial production, is that 10min is advisable so the water extraction time is confirmed in actual production.The best leaching time 10min that following examples water extraction time adopting process is confirmed.
2.2 the solid-to-liquid ratio of water extraction reaction
Solid-liquid weightmeasurement ratio S (g): L (mL) S: L=1 has been compared in experiment: 2.5,1: 5,1: 7.5,1: 10; The result shows that small volume solid-to-liquid ratio ore pulp viscosity is big; Be difficult for to filter, be amplified to more than 1: 5, filter stopping state be improved significantly; But the excessive extraction that is unfavorable for subsequent product of volume, so confirm that solid-to-liquid ratio is 1: 5.
3, the screening of hydrochloric acid consumption
Adopt following different hydrochloric acid consumption, with the 15 minutes acidolysis time (do not add and increase preserved material), the water extraction time is 10min, and water extraction solid-liquid volume ratio is 1: 5 processing titanium-containing blast furnace slag, adopts diantipyrylmethane colorimetric method for determining TiO
2EDTA complexometric titration CaO, MgO; NaF replacement-EDTA replacement titration Al
2O
3Content, the result is as shown in table 3.
The experiment of table 3 hydrochloric acid consumption
Can know by table 3, the hydrochloric acid consumption with S (g): L (mL)=1: 2 for well, TiO in immersion liquid this moment
2Rate of loss is less than 1%, and CaO, MgO be 100% leaching almost, Al
2O
3Leaching is also up to 87%, and is highly beneficial for from solution, extracting various products successively.Titanium-contained slag moisture absorption that it should be noted that this method enrichment is very serious, and water-content is the major cause that causes present rich titanium slag product also below standard (>=35%) up to 30.34%.The hydrochloric acid consumption is excessive, is higher than 1: 2, and the titanium in the titanium-contained slag generates the solubility titanium salt, is dissolved in the water, and causes damage.
4, increase the test of preserved material consumption
The effect that increases preserved material mainly contains two aspects, and the one, increase the leaching of salt in the titanium-containing blast furnace slag, the 2nd, suppress TiO
2Stripping.Carry out following experiment for this reason, taken by weighing the 10g test portion, wherein contained TiO
22.024g, press S (g): L (mL)=1: 2, add 1/4 water (being 20mL hydrochloric acid+5mL water) in the acid solution, acidolysis 15min adds 5 times of water yields leaching 10min then, and the sodium-chlor that drop into different amounts are for increasing preserved material, and suction filtration carries out TiO in immersion liquid and the product respectively
2Analysis.The result sees table 4.
Table 4 increases the test of preserved material consumption
| Experiment numbers | 1 | 2 | 3 | 4 |
| Increase preserved material consumption (g) | 0 | 0.1 | 0.25 | 0.5 |
| Immersion liquid+wash water (mL) | 88 | 82 | 83 | 83 |
| TiO in the immersion liquid 2(mg/L) | 141.39 | 98.39 | 62.31 | 30.98 |
| Immersion liquid distributive law (%) | 0.61 | 0.40 | 0.24 | 0.13 |
| Product weight (g) | 6.40 | 5.33 | 5.85 | 6.05 |
| TiO in the product 2Content (%) | 30.45 | 36.66 | 33.25 | 31.88 |
| TiO in the product 2Distributive law (%) | 96.28 | 96.54 | 96.10 | 95.29 |
Can know that by table 4 it is very tangible increasing preserved material adding effect, increase preserved material experiment relatively with not containing, increase preserved material and account for when feeding intake 1% ratio, suppress TiO
2The situation of leaching is reduced to 0.42% by original loss 0.61%, and the leaching rate of salt obviously increases, and filter cake is reduced to 5.33g by former 6.40g, TiO
2Content is increased to 36.66% by 30.45% in product, reaches rich titanium slag and sells grade requirement.3, No. 4 tests show in the table 4, increase the preserved material consumption and can not increase the preserved material input amount greater than 1%, and the filter cake total amount also increases thereupon, causes TiO in the product
2Content reduce on the contrary, can not reach rich titanium slag grade requirement.
Embodiment
Take by weighing titanium-containing blast furnace slag 10g in the 150mL beaker, add (20mL hydrochloric acid+5mL water) and mix acid hydrolysis solution, acidolysis 15min; After increasing preserved material 0.1g and in 50mL water, dissolving, add and carry out salt leaching 10min in the acidolysis material, filter; Wash 2 times, merge leaching liquid and wash water, measurement volumes; Filter cake oven dry is weighed, and filter cake and liquid (leaching liquid and wash water) are carried out the analytical test of titanium, calcium, aluminium and magnesium respectively, investigates the distribution situation of these four principal elements in feed liquid and filter cake.The result sees table 5.
The material balance table of principal element in table 5 titanium-containing blast furnace slag
Can be known that by table 5 four distributions of main products in feed liquid and filter cake are equilibrated in the titanium-containing blast furnace slag, the total distributed rate is within the error allowed band.Through this art breading, TiO
2Basically all stay and burn in the slag, make and handle the requirement that the back titanium-containing blast furnace slag reaches rich titanium slag grade standard, can be used as rich titanium slag direct marketing; A large amount of CaO, MgO almost all is transferred in the immersion liquid in the burning slag.
Adopt multiple-effect separating agent unslaked lime to be adjusted to the pH=6-7 after-filtration leaching liquid, obtain the white lake product after filter cake washing, the purification;
Filtrating adopts multiple-effect separating agent unslaked lime to regulate pH >=12, and the filter cake washing calcining after the filtration obtains magnesium oxide product;
Filter cake centrifuge dripping after filtrating evaporation concentration, the filtration obtains the U-Ramin MC product.
With the rich titanium slag of above-mentioned acquisition, calcium chloride, Marinco H and white lake product, all reach national Industrial products standard-required through examining the quality of the production.
In a word, the present invention is with the comprehensive utilization process of hydrochloric acid system rapid method enforcement titanium-containing blast furnace slag, through the mixed economy cost analysis; It is reasonable to prove that this technology has a technical process; The comprehensive utilization of resources rate is high, and economic benefit is obvious, advantages such as no environment secondary pollution; Realized that country turns waste into wealth the policy goals of energy-saving and emission-reduction.
Claims (10)
1. the method for comprehensive utilization of titanium-containing blast furnace slag is characterized in that being accomplished by following steps:
A, acidleach: adopt the hydrochloric acid leaching titanium-containing blast furnace slag;
B, water logging: the material after the step a acidleach adds water and carries out water extraction, filters;
C, filter cake 1 are handled: filter cake 1 washing after step b filters, drying obtain rich titanium products;
D, filtrating 1 are handled: step b filtrate filtered 1 is regulated pH=6-7, filters;
E, filter cake 2 are handled: obtain the white lake product after filter cake 2 washings after steps d is filtered, the purification;
F, filtrating 2 are handled: steps d filtrate filtered 2 is regulated pH >=12, filters;
G, filter cake 3 are handled: the filter cake 3 washing calcinings after step f filters obtain magnesium oxide product;
H, filtrating 3 are handled: step f filtrate filtered 3 evaporation concentration after-filtration;
I, filter cake 4 are handled: filter cake 4 centrifuge drippings after step h filters obtain the U-Ramin MC product.
2. the method for comprehensive utilization of titanium-containing blast furnace slag according to claim 1 is characterized in that: get or add soluble chloride for increasing preserved material during water extraction in acidleach, the add-on that increases preserved material is the 0.8-1.2% of blast furnace slag (1% is good).
3. the method for comprehensive utilization of titanium-containing blast furnace slag according to claim 2 is characterized in that: increase preserved material and when water extraction, add.
4. the method for comprehensive utilization of titanium-containing blast furnace slag according to claim 3 is characterized in that: the said preserved material that increases is at least a in sodium-chlor, the Repone K.
5. according to the method for comprehensive utilization of each described titanium-containing blast furnace slag of claim 1-4, it is characterized in that: the hydrochloric acid consumption is among the step a: the volume ratio of titanium-containing blast furnace slag solid weight and hydrochloric acid liquid:
S (g): L (mL)=1: 1.8-2.2, preferred 1: 2; Leaching time: 10～30min, preferred 15min.
6. according to the method for comprehensive utilization of each described titanium-containing blast furnace slag of claim 1-5, it is characterized in that:
The amount of water of water extraction was with solid-liquid weightmeasurement ratio S (g): L (mL)=1: 4.5-5.5, preferred 1: 5 among the step b; The water extraction time is with 9-12, preferred 10min.
7. according to the method for comprehensive utilization of each described titanium-containing blast furnace slag of claim 1-6, it is characterized in that: steps d is regulated potential of hydrogen and is adopted unslaked lime to be adjusted to pH=6-7.
8. according to the method for comprehensive utilization of each described titanium-containing blast furnace slag of claim 1-7, it is characterized in that: step f regulates potential of hydrogen and adopts unslaked lime to be adjusted to pH to pH >=12.
9. according to the method for comprehensive utilization of each described titanium-containing blast furnace slag of claim 1-8, it is characterized in that: the filtrating 4 that step h obtains after filtering is as b step water extraction water.
10. according to the method for comprehensive utilization of each described titanium-containing blast furnace slag of claim 1-9, it is characterized in that: the washing lotion that 1 washing of step c filter cake obtains is as b step water extraction water.
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| CN102698737A (en) * | 2012-05-25 | 2012-10-03 | 中国科学院过程工程研究所 | Method for preparing selective catalytic reduction SCR flue gas denitration catalyst and method for preparing raw material titanium-tungsten powder of SCR flue gas denitration catalyst |
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| CN103449495A (en) * | 2013-08-30 | 2013-12-18 | 遵宝钛业有限公司 | Method for preparing calcium chloride by hydrochloric acid recovered from production of titanium tetrachloride |
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| CN103952567A (en) * | 2014-05-13 | 2014-07-30 | 李翔 | Method for recycling titanium, silicon, aluminum, calcium and magnesium from titaniferous blast furnace slag by multistage acid leaching |
| CN103952568A (en) * | 2014-05-13 | 2014-07-30 | 李翔 | Method for treating titaniferous blast furnace slag |
| CN103952568B (en) * | 2014-05-13 | 2016-03-23 | 李翔 | The method of process titanium-containing blast furnace slag |
| CN103952567B (en) * | 2014-05-13 | 2016-05-25 | 李翔 | Utilize multistage acidleach to get the method that reclaims titanium, silicon, aluminium, calcium and magnesium from titanium-containing blast furnace slag |
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| CN107686897A (en) * | 2017-08-23 | 2018-02-13 | 攀枝花学院 | A kind of method that titanium is carried from titanium-containing blast furnace slag |
| CN107686897B (en) * | 2017-08-23 | 2019-05-10 | 攀枝花学院 | A method of mentioning titanium from titanium-containing blast furnace slag |
| CN113620628A (en) * | 2021-08-31 | 2021-11-09 | 西南科技大学 | Recycling method of chlorine element in titanium extraction slag |
| CN114438335A (en) * | 2021-12-29 | 2022-05-06 | 绵阳师范学院 | Titanium-containing blast furnace slag treatment method |
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