CN105366736A - Titanium white by-product copperas dehydration and drying method - Google Patents
Titanium white by-product copperas dehydration and drying method Download PDFInfo
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Abstract
The invention discloses a titanium white by-product copperas dehydration and drying method. The method comprises adding titanium white by-product copperas into water or copperas crystallization mother liquor, carrying out stirring heating to a temperature of 50-110 DEG C so that the titanium white by-product copperas is dissolved and the solution is saturated, adding a reducer into the solution to reduce Fe<3+> in the solution, carrying out stirring cooling crystallization, carrying out filtration to obtain recrystallized copperas, transferring the recrystallized copperas into a converter, carrying out first-stage drying dehydration, adding the first-stage drying dehydration product into a second-stage converter, carrying out second-stage drying dehydration to obtain a second-stage drying dehydration product, adding sodium hydroxide into the crystallization mother liquor to adjust pH so that titanium in the mother liquor is precipitated and crystallizes, and carrying out filtration to obtain titanium slag and a titanium precipitation liquid. The titanium white by-product copperas is dissolved in water or copperas mother liquor, through reduction of Fe<3+> and cooling crystallization, free water and free acid in the titanium white by-product copperas are removed, and through control of recrystallized copperas granularity, the copperas is dried and recrystallized by a two-stage method. The method has the advantages of fast dehydration rate, low energy consumption, high product quality and no waste liquid discharge.
Description
Technical field
The present invention relates to the dehydration of a kind of titanium white by product thing green vitriol and dry method, realize the recovery of the dehydration of titanium white by product thing green vitriol and titanium in dry and titanium white green vitriol.
Background technology
Ferrous sulfate (green vitriol) is a kind of important industrial chemicals, has extensive use.Industrial for the manufacture of various molysite, bodied ferric sulfate, ink, iron pigment, magnetic etc.Ferrous sulfate produces ferriferous oxide both low prices, nontoxic again, therefore applied widely in the catalyst, as ferric oxide in chemical fertilizer industry, be used as desulfurization catalyst, the alkyl cyclic ethylene in organic synthesis, heterocycle spin alkylating hydrocarbons, be used as catalyzer in the hydration hydroxylation of coal etc.Agriculturally be used as green manure, iron be plant-growth, grow, bloom, the requisite micronutrient element of result, plant Pressure trunk injection, ferrous sulfate is conventional green manure, to the north of China the Yellow River, use ferrous sulfate to have great importance in alkaline soil; As weedicide, liverwort, lichens on radical cure trunk; With used as pesticides, cure mainly wheat smut, the canker of control orchard pest and fruit tree.Pharmaceutically be used as local convergence agent and hematinic, its iron content is the raw material of synthesis hemoglobin in body; It is also the widely used additive of feed etc.At dye industry, green vitriol is also used as mordant etc.In addition ferrous sulfate can also be used for removing fishy smell, bedroom peculiar smell etc.In sewage disposal, ferrous sulfate application is more extensive, mainly as flocculation agent when being used alone, is the most widely used inorganic flocculating agent, with hydrogen peroxide conbined usage as the organic pollutant of Fenton reagent for decolorization and degradation difficult degradation.
Because green vitriol contains many, the easy cakings of crystal water and easy oxidized variable color, goes bad, affects and pulverize and flowing property, green vitriol (iron vitriol) is moisture up to 45.39% in addition, and green vitriol transportation cost is high.Therefore, the use of ferrous sulfate is limited.Green vitriol, through dehydration, not only can improve the chemical stability of product, improves use properties, reduces transportation cost, can also expand its purposes.Green vitriol is through drying and dehydrating, and green vitriol dehydration is four aqueous ferrous sulfates, reduces crystal water 19.45%, its stable in properties, still has good water-soluble.Green vitriol prepares ferrous sulfate monohydrate (FeSO through drying and dehydrating
4h
2o), crystal water decreases 38.90%, and ferrous sulfate monohydrate is typical additives in feed and medicine.
China's ferrous sulfate is mainly derived from titanium white by product thing green vitriol, and current China produces titanium dioxide per year and reaches more than 1,000,000 tons, and one ton of titanium white produces 3.5 tons of green vitriols, calculates titanium powder industry in China accordingly and just about produces 3,500,000 tons of green vitriols every year.Titanium white by product thing green vitriol FeSO
47H
2o content is generally 90%, reaches 10% containing free-water, titaniferous liquid 0.2%, and other foreign matter content is high, uses because which limit it.Moreover, titanium white by product thing green vitriol amount is too large, can digest without any industry, the normal mode process adopting stacking and landfill.Therefore, its titanium white green vitriol has become the important factor of restriction titanium white development.In gas washing in SA production, green vitriol and sulfurous iron ore multifuel combustion after dehydration, not only reduce sulfurous iron ore usage quantity, and greatly can improve grade of sulfate cinder iron, add the added value of slag, obtain industrial application at sulfuric acid industry.The application of dehydration green vitriol in sulfuric acid industry, will become the important channel solving titanium white green vitriol.
At present, the dehydration of titanium white green vitriol and drying often adopt that Rotary drying dewaters, warm air drying is dewatered and fluidized-bed fluidized drying dewaters.Constant pressure and dry dewaters and warm air drying is dewatered, and not only time of drying is long, and produce caking phenomenon, production capacity is low.Fluidized-bed fluidized drying dehydration dewatering speed is very fast, but power consumption is large.Adopt vacuum-drying rate of drying to accelerate, can caking phenomenon be overcome, but complicated operation, and production capacity is low.Adopt dehydration in sulphuric acid soln to produce ferrous sulfate monohydrate, produce a large amount of sulfuric acid waste and be difficult to process and small-scale production.The method of above-mentioned convection drying titanium white green vitriol, because titanium white green vitriol is high containing free-water, lump and contain free sulfuric acid, making dehydration difficult with drying, energy consumption increase.And the heat steam that above-mentioned drying means drying produces is not utilized.
Existing method existing defects needs to improve.
Summary of the invention
The dehydration of a kind of titanium white by product thing of the present invention green vitriol and dry method, titanium white green vitriol free-water and free acid is removed by recrystallization, control recrystallization green vitriol granularity, accelerate dewatering speed, caking phenomenon when efficiently solving drying, and pass through the utilization of two sections of hot gas latent heat, significantly reduce energy consumption.Meanwhile, by reduction Fe
3+not only reclaim titanium in mother liquor with the neutralizing hydrolysis of titanium white green vitriol solution, improve the quality of dehydration green vitriol.
The object of this invention is to provide the dehydration of a kind of titanium white by product thing green vitriol and dry method, realize the recovery of titanium in the utilization of titanium white green vitriol and titanium white green vitriol.
Technical scheme of the present invention is:
The dehydration of titanium white by product thing green vitriol and a dry method, add in water solvent by titanium white by product thing green vitriol, be heated to 50 ~ 110 DEG C and make titanium white by product thing green vitriol dissolve and reach capacity, add Fe in reductive agent reducing solution under stirring
3+, cooling under stirring, crystallization, filtration obtain recrystallization green vitriol and crystalline mother solution.Sieved through 30 eye mesh screens by recrystallization green vitriol, screen overflow adds in converter and carries out first paragraph drying and dehydrating, is proceeded in converter by one section of drying and dehydrating product to carry out second segment drying and dehydrating and obtain two-stage drying dewatered product.Crystalline mother solution adds sodium hydroxide and regulates titanium in crystalline mother solution pH value precipitated crystal mother liquor, filters and obtains liquid after titanium slag and heavy titanium.
The reductive agent added is iron filings and iron sheet, and the amount of iron filings and iron sheet that adds is for reducing Fe completely
3+doubly, crystallisation by cooling temperature is-5 ~ 30 DEG C to the 1-1.2 of required theoretical amount;
Sieved through 30 eye mesh screens by recrystallization green vitriol, screen underflow, as crystal seed, adds reduction Fe when crystallisation by cooling
3+in rear saturated copperas solution;
One section of drying temperature is 50 ~ 120 DEG C, and one section of drying and dehydrating product controls as the ferrous sulfate containing 4-7 crystal water; Two-stage drying temperature is 120 ~ 300 DEG C, and two-stage drying dewatered product controls the ferrous sulfate for 1-4 crystal water; The waste heat hot gas produced in two-stage drying converter return one section dry time, one section of converter adopts outer hot mode to heat;
It is 3.0 ~ 5.0 that sodium hydroxide regulates crystalline mother solution pH value to control, and the titanium slag that filtration obtains is for recovery Pd; The water solvent dissolving titanium white by product thing green vitriol is liquid after water, crystalline mother solution and heavy titanium.
Titanium white by product thing green vitriol to be added after water or crystalline mother solution or heavy titanium in liquid, be heated to 50 ~ 110 DEG C under stirring and make titanium white by product thing green vitriol dissolve and reach capacity, add and reduce Fe completely
3+fe in 1-1.2 times of reductive agent iron powder of required theoretical amount and iron sheet reducing solution
3+, add screen underflow that 30 mesh sieves divide under stirring as crystal seed, crystallisation by cooling at-5 ~ 30 DEG C, filter and obtain recrystallization green vitriol.The screen overflow that recrystallization green vitriol 30 mesh sieve divides is added in converter and carries out two-stage drying.Crystalline mother solution add sodium hydroxide regulate mother liquor pH value precipitated crystal to filter after titanium in mother liquor, filter and obtain liquid after titanium slag and heavy titanium.One section of drying temperature is 50 ~ 120 DEG C, and one section of drying and dehydrating product is the ferrous sulfate containing 4-7 crystal water; Two-stage drying temperature is 120 ~ 300 DEG C, the ferrous sulfate of two-stage drying dewatered product 1-4 crystal water; One section of converter adopts external-heat, and the waste heat hot gas produced in two-stage drying converter returns one section of drying as outer heat.
Advantage of the present invention is:
(1) remove titanium white green vitriol free-water and free acid by recrystallization, control recrystallization green vitriol granularity, accelerate dewatering speed, caking phenomenon when efficiently solving drying.
(2) by the quickening of dewatering speed and the utilization of two sections of hot gas latent heat, energy consumption is significantly reduced.
(3) by reduction Fe
3+not only reclaim titanium in mother liquor with the neutralizing hydrolysis of titanium white green vitriol solution, and improve the quality of dehydration green vitriol, add economic benefit.
embodiment:
The present invention can implement by the technical scheme described in summary of the invention.
The dehydration of titanium white by product thing green vitriol and a dry method, add in water solvent by titanium white by product thing green vitriol, be heated to 50 ~ 110 DEG C and make titanium white by product thing green vitriol dissolve and reach capacity, add Fe in reductive agent reducing solution under stirring
3+, cooling under stirring, crystallization, filtration obtain recrystallization green vitriol and crystalline mother solution.Sieved through 30 eye mesh screens by recrystallization green vitriol, screen overflow adds in converter and carries out first paragraph drying and dehydrating, is proceeded in converter by one section of drying and dehydrating product to carry out second segment drying and dehydrating and obtain two-stage drying dewatered product.Crystalline mother solution adds sodium hydroxide and regulates titanium in crystalline mother solution pH value precipitated crystal mother liquor, filters and obtains liquid after titanium slag and heavy titanium.
The reductive agent added is iron filings and iron sheet, and the amount of iron filings and iron sheet that adds is for reducing Fe completely
3+doubly, crystallisation by cooling temperature is-5 ~ 30 DEG C to the 1-1.2 of required theoretical amount;
Sieved through 30 eye mesh screens by recrystallization green vitriol, screen underflow, as crystal seed, adds reduction Fe when crystallisation by cooling
3+in rear saturated copperas solution;
One section of drying temperature is 50 ~ 120 DEG C, and one section of drying and dehydrating product controls as the ferrous sulfate containing 4-7 crystal water; Two-stage drying temperature is 120 ~ 300 DEG C, and two-stage drying dewatered product controls the ferrous sulfate for 1-4 crystal water; The waste heat hot gas produced in two-stage drying converter return one section dry time, one section of converter adopts outer hot mode to heat;
It is 3.0 ~ 5.0 that sodium hydroxide regulates crystalline mother solution pH value to control, and the titanium slag that filtration obtains is for recovery Pd; The water solvent dissolving titanium white by product thing green vitriol is liquid after water, crystalline mother solution and heavy titanium.
Titanium white by product thing green vitriol to be added after water or crystalline mother solution or heavy titanium in liquid, be heated to 50 ~ 110 DEG C under stirring and make titanium white by product thing green vitriol dissolve and reach capacity, add and reduce Fe completely
3+fe in 1-1.2 times of reductive agent iron powder of required theoretical amount and iron sheet reducing solution
3+, add screen underflow that 30 mesh sieves divide under stirring as crystal seed, crystallisation by cooling at-5 ~ 30 DEG C, filter and obtain recrystallization green vitriol.The screen overflow that recrystallization green vitriol 30 mesh sieve divides is added in converter and carries out two-stage drying.Crystalline mother solution add sodium hydroxide regulate mother liquor pH value precipitated crystal to filter after titanium in mother liquor, filter and obtain liquid after titanium slag and heavy titanium.One section of drying temperature is 50 ~ 120 DEG C, and one section of drying and dehydrating product is the ferrous sulfate containing 4-7 crystal water; Two-stage drying temperature is 120 ~ 300 DEG C, the ferrous sulfate of two-stage drying dewatered product 1-4 crystal water; One section of converter adopts external-heat, and the waste heat hot gas produced in two-stage drying converter returns one section of drying as outer heat.
Embodiment 1:
Take titanium white green vitriol 1600g, titanium white green vitriol calculates FeSO with total iron
47H
2o content is 90.83%, and titanium content is 0.30%, adds in 720mL60 DEG C of tap water under stirring, keeps constant temperature, after dissolving completely, according to reduction Fe
3+1.10 times of required iron powder theoretical amount add iron powder 6.20g, after iron powder complete reaction, stir lower natural cooling crystallization, are cooled to room temperature 24 DEG C.Centrifuging, obtains recrystallization green vitriol 966g, crystalline mother solution 950mL, the total concentration of iron 1.79mol/L of crystalline mother solution, titanium 5.05g/L.Recrystallization green vitriol is through 30 mesh sieve, and screen underflow is zero.
It is in the converter of 10cm that screen overflow 966g recrystallization green vitriol is added internal diameter, and heat 80 DEG C and carry out after one section of dry 4h being greyish-green particle, dewatered product is FeSO
45.5H
2o.Proceeding two-stage drying temperature is 200 DEG C, and two-stage drying 1h is canescence particle, and dewatered product is FeSO
41.5H
2o.
It is 4.30 that sodium hydroxide regulates crystalline mother solution pH value to control, and filters and obtains 43.60g titanium slag, and after drying, titanium slag Ti, Fe, S mass percentage is respectively 11.12%, 20.03%, 18.60%.
Embodiment 2:
Take titanium white green vitriol 3200g, titanium white green vitriol calculates FeSO with total iron
47H
2o content is 91.23%, and titanium content is 0.28%, adds in 1440mL tap water under stirring, is heated to 80 DEG C and keeps constant temperature, after dissolving completely, according to reduction Fe
3+1.15 times of required iron powder theoretical amount add iron powder 13.30g, after iron powder complete reaction, stir lower crystallisation by cooling, add ice cube and keep cooling temperature to be 0 DEG C in water.Centrifuging, obtains recrystallization green vitriol 2500g, crystalline mother solution 1450mL, the total concentration of iron 1.19mol/L of crystalline mother solution, titanium 6.10g/L.Recrystallization green vitriol is through 30 mesh sieve, and screen underflow is 150g.
It is in the converter of 10cm that screen overflow 2350g recrystallization green vitriol is added internal diameter, and heat 120 DEG C and carry out after one section of dry 4h being greyish-green particle, dewatered product is FeSO
45H
2o.Proceed two-stage drying, drying temperature is 180 DEG C, and two-stage drying 2h is canescence particle, and dewatered product is FeSO
4h
2o.
It is 4.00 that sodium hydroxide regulates crystalline mother solution pH value to control, and filters and obtains 63.12g titanium slag, and after drying, titanium slag Ti, Fe, S mass percentage is respectively 13.94%, 18.93%, 21.01%.
Embodiment 3:
Liquid 1L after heavy titanium in Example 2, be heated to 60 DEG C under stirring, add titanium white green vitriol 1800g, titanium white green vitriol calculates FeSO with total iron
47H
2o content is 91.23%, and titanium content is 0.28%, after keeping constant temperature to dissolve completely, according to reduction Fe
3+1.15 times of required iron powder theoretical amount add iron powder 7.50g, and after iron powder complete reaction, slowly add screen underflow 150g in embodiment 2, crystallisation by cooling under stirring, controlled cooling model Tc is 10 DEG C.Centrifuging, obtains recrystallization green vitriol 1593g, crystalline mother solution 980mL, titanium 4.05g/L in crystalline mother solution.Recrystallization green vitriol is through 30 mesh sieve, and screen underflow is zero.
It is in the converter of 10cm that screen overflow 1593g recrystallization green vitriol is added internal diameter, and heat 100 DEG C and carry out after one section of dry 5h being greyish-green particle, dewatered product is FeSO
44H
2o.Continue intensification and carry out two-stage drying, drying temperature is 220 DEG C, and two-stage drying 1h is canescence particle, and dewatered product is FeSO
4h
2o.
It is 4.80 that sodium hydroxide regulates crystalline mother solution pH value to control, and filters and obtains 33.12g titanium slag, and after drying, titanium slag Ti, Fe, S mass percentage is respectively 14.72%, 17.33%, 22.42%.
Claims (6)
1. the dehydration of titanium white by product thing green vitriol and a dry method, is characterized in that: add in water solvent by titanium white by product thing green vitriol, be heated to 50 ~ 110 DEG C and make titanium white by product thing green vitriol dissolve and reach capacity, add Fe in reductive agent reducing solution under stirring
3+cooling under stirring, crystallization, filtration obtain recrystallization green vitriol and crystalline mother solution, by recrystallization green vitriol through 30 orders (aperture is 550um) sieved through sieve, screen overflow adds in converter and carries out first paragraph drying and dehydrating, one section of drying and dehydrating product is proceeded in converter and carries out second segment drying and dehydrating and obtain two-stage drying dewatered product, crystalline mother solution adds sodium hydroxide and regulates titanium in crystalline mother solution pH value precipitated crystal mother liquor, filters and obtains liquid after titanium slag and heavy titanium.
2. a kind of titanium white by product thing green vitriol dehydration according to claim 1 and dry method, is characterized in that: the reductive agent added is iron filings and iron sheet, and the amount of iron filings and iron sheet that adds is for reducing Fe completely
3+doubly, crystallisation by cooling temperature is-5 ~ 30 DEG C to the 1-1.2 of required theoretical amount.
3. a kind of titanium white by product thing green vitriol dehydration according to claim 1 and dry method, it is characterized in that: sieved through 30 eye mesh screens by recrystallization green vitriol, screen underflow, as crystal seed, adds reduction Fe when crystallisation by cooling
3+in rear saturated copperas solution.
4. a kind of titanium white by product thing green vitriol dehydration according to claim 1 and dry method, is characterized in that: one section of drying temperature is 50 ~ 120 DEG C, and one section of drying and dehydrating product controls as the ferrous sulfate containing 4-7 crystal water; Two-stage drying temperature is 120 ~ 300 DEG C, and two-stage drying dewatered product controls the ferrous sulfate for 1-4 crystal water; The waste heat hot gas produced in two-stage drying converter return one section dry time, one section of converter adopts outer hot mode to heat.
5. a kind of titanium white by product thing green vitriol according to claim 1 dewaters and dry method, it is characterized in that: it is 3.0 ~ 5.0 that sodium hydroxide regulates crystalline mother solution pH value to control, and the titanium slag that filtration obtains is for recovery Pd.
6. a kind of titanium white by product thing green vitriol dehydration according to claim 1 and dry method, is characterized in that: the water solvent dissolving titanium white by product thing green vitriol is liquid after water, crystalline mother solution and heavy titanium.
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Cited By (2)
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| CN107720833A (en) * | 2017-11-15 | 2018-02-23 | 攀钢集团攀枝花钢铁研究院有限公司 | The process for effectively purifying of byproduct ferrous sulfate of titanium dioxide |
| CN115432739A (en) * | 2022-10-20 | 2022-12-06 | 江苏宇星科技有限公司 | Recrystallization purification process of titanium dioxide byproduct ferrous sulfate |
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