CN101380510A - Chromic slag wet method detoxifcation and resource comprehensive utilization new technique - Google Patents
Chromic slag wet method detoxifcation and resource comprehensive utilization new technique Download PDFInfo
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Abstract
A new harmless comprehensive utilization technique for wet processing chromic slag comprises steps as follows: ball milling chromic slag to 80-200 meshes, adding water to prepare slurry, immersing the slurry in hydrochloric acid solution, regulating the pH to 5-6, performing solid-liquid separation with filter press, in the immersion liquid after separation, the hexavalent chrome is reduced to trivalent chromium, adding sodium hudroxide aqueous solution, regulating the pH to 4-6, roughly preparing chromic hydroxide, adding sulfuric acid into filtrate, regulating the pH to 5-6, removing the calcium coprecipitated with magnesium in the rest filtrate, preparing the 2-water calcium sulphate whisker, adding alkali to the filtrate after filter-pressing to regulate the pH to 9-12 to synthesize super-fine magnesium hydroxide powder; the solution after filter-pressing is concentrated to prepare sodium chloride. The main contents of extracts within the chromic slag treated by wet processing all can meet primary, secondary or even accredited national or ministerial standard. The technique can thoroughly detoxicate Cr<6+> in chromic slag and can prepare nine products, includiing chromic hydroxide, magnesium hydroxide, ammonium hydroxide, silicon dioxide, magnetic ferrous ferricoxide, 2-water calcium sulphate, corundum intermediate, sodium chloride, and tailings-chromite; and the extracts after processing chromic slag have high quality.
Description
One technical field
The present invention relates to a kind of comprehensive resources and utilize again, particularly a kind of utilization again that utilizes chromite ore to produce the industrial waste ballast chromium slag that discharges in the product process.
Two technical backgrounds
The chromic salts industry is the indispensable important industry of the national economic development, utilizes chromite ore to produce that industrial waste ballast----the chromium slag as dischargings such as chemical industry, metallurgy industries is a kind of hazardous solid waste of severe toxicity in the process of product.Oxious component in the chromium slag mainly is hexavalent chromiums such as water-soluble chromic acid sodium, solubility in acid calcium chromate.Dust, water body, soil that contains hexavalent chromium etc. all can cause severe contamination and harm to ecological environment.
Handling the chromium slag and always be the problem of the headache of chromic salts industry, also is world-famous puzzle.Russia, the U.S., comprise Brazil, South Africa, these chromium salt production big countries, also do not find real economic, effective, a practical technology so far.How to bury or the making cement mineralizer with a large amount of wastelands of oneself.
The pollution problem of thoroughly administering the chromium slag has obtained the great attention of country and each province and city government, but produces little effect.
Make a general survey of domestic and international chromium residue detoxifying technology, the representative patented technology that following type is arranged:
For example: " carbonating detoxification chromium slag-magnesium extracts-does the collaborative detoxifcation-scum of wet method and prepares the new process of ferritic zero-emission green chemical industry ".The comprehensive utilization of resources rate is not high, and does not see operation.And " inorganic chromium saltworks chromium slag for comprehensive utilizes technology " propose to reclaim the slag brick-making technology after chromium cast iron contained, the melting.Extract very little, economy is relatively poor.Also having a kind of patent No. is that zero-emission of 200710078681.3 chromium poison and resource are utilized new method fully, by to chromium slag concentrated acid resolution process, Cr poisonous in the chromium slag
6+Be reduced into Cr
3+, the preparation chromium hydroxide.This method extract is technical grade, and in the patent silica is stayed extraction in the residue, handles not exclusively, do not reach whole utilizations of resource, formaldehyde that the more important thing is this technology usefulness severe toxicity easily damages the workman as chromic reducing agent, and is inadvisable.Or the like.
All there is certain limitation in above-mentioned chromium slag treatment technology, and the detoxifcation that has is not thorough, has secondary pollution; The chromium slag consumption that has is few, and the disposal cycle is long, and progress is slow; Some fully utilizes product, as with chromium slag as cement mineralizer, the influence of environment be it be unclear that.Except that above shortcoming was arranged, also have a same shortcoming: resource utilization was low excessively, and economic benefit is too poor, is not suitable for large-scale production.
Three summary of the invention
The objective of the invention is to: design a kind of chromic slag wet method detoxifcation and comprehensive utilization of resources new technology; under normal temperature, normal pressure, adopt new technology the chromium quarrel is carried out wet method detoxifcation and comprehensive utilization of resources; hexavalent chromium causes severe contamination and harm to ecological environment in reduction and the minimizing chromium slag; reach the protection environment; reduce cost the purpose of comprehensive utilization of resources.
Concrete grammar of the present invention is: the innoxious comprehensive utilization of resources new technology of a kind of chromic slag wet method, with chromium slag ball milling to 80～200 orders, after adding water slurrying, in hydrochloric acid solution, carry out soaking, regulating PH is 5～6, carry out Separation of Solid and Liquid with filter press, after a immersion liquid after the separation is trivalent chromium with the sulphite reduction of hexavalent chromium, add caustic-soda aqueous solution, adjusting PH is 4---6, rough chromium hydroxide, and adding sulfuric acid accent PH in the filtrate is 5～6, remove in the residual filtrate and the calcium magnesium co-precipitation, preparation sulfate dihydrate calcium pyroborate; It is 9---12 that the press filtration rear filtrate adds alkali adjusting PH, the synthesizing superfine magnesium hydrate powder; Solution concentration after the press filtration prepares sodium chloride;
One soaks hydrochloric acid for dreg solution carries out secondary pickling, and control PH 0.5～1.0 carries out Separation of Solid and Liquid, and after two immersion liquid after the Separation of Solid and Liquid were trivalent chromium with the sulphite reduction of hexavalent chromium earlier, adding alkali, to transfer PH be 3----4.5, precipitates iron hydroxide; Filter cake adds aquation and opens and divalent iron salt synthesizing superfine magnetic ferroferric oxide again after press filtration; Filtrate is settled out aluminium hydroxide after adding alkali accent PH3.5----5; After the press filtration rear filtrate adds alkali accent PH6-7, the synthetic corundum intermediate.Two soak slag puts into aqueous slkali and carries out alkali and soak, and after the press filtration Separation of Solid and Liquid, filter cake is chromite sand (being tailings); Filtrate adds after the steric hindrance agent adds acid again and transfer PH8-9, and synthetic silicic acid colloidal sol is through ageing, drying, calcine and then obtain the silica superfine powder.
Press filtration after the crude product chromium hydroxide added sulfuric acid and keep PH1-1.5 high-speed stirred, its filter cake promptly is a calcium sulphate dihydrate; Its filtrate adds caustic-soda aqueous solution, keeps PH5.8-6.0 high-speed stirred filter pressing to get the elaboration chromium hydroxide.
Adopt new technology of the present invention, after hexavalent chromium and magnesium, calcium, iron, aluminium ion and sodium metasilicate (solution) at utmost leach in the chromium slag of wet method pulverizing, in the solution of " co-precipitation ", at first select for use sulphite that Cr VI (severe toxicity) is reduced into trivalent chromium; React by inorganic chemistry again, it is acid-base reaction, complex reaction, redox reaction, cause precipitation or precipitation dissolving, by the control pH value, realize " fractional precipitation " that the hydroxide of synthetic chromium, magnesium, iron, aluminium is again by " precipitation conversion reaction ", " recrystallization " synthetic sulfate dihydrate calcium pyroborate, Fe 3 O 4 magnetic powder body and corundum intermediate; According to " sol-gel processing " theory, select the steric hindrance agent for use again, utilize " co-precipitation " method, the synthetic silicic acid gel is prepared nano silicon.Best remaining tailings is that chromite sand is 1.3-1.5% only after employing this method, and chromite sand returns chromium salt factory and utilizes.
The extraction owner content of this technology wet-treating chromium slag all reaches GB or ministry standard I and II even superfine standard.In order to reduce cost, available lime replaces caustic soda.This technology not only makes Cr in the chromium slag
6+Thoroughly detoxifcation also can be prepared 9 kinds of products, is respectively chromium hydroxide, magnesium hydroxide, aluminium hydroxide, silica, magnetic ferroferric oxide, calcium sulphate dihydrate, corundum intermediate, sodium chloride, tailings--chromite sand; Wherein preceding four kinds of products are nanometer or nanometer materials, Cr in all over products
6+Residual quantity all is lower than more than national standard (GB5085.3-1996) 7.5-375 times.Extract quality quality height after the chromium slag is handled, scientific and technological added value height, in demand.The chromium slag secondary resource rate of recovery has realized really that up to more than 99.95% the chromium slag thoroughly detoxifies and resource is all utilized.In a word, this technology makes the chromium slag thoroughly detoxify at normal temperatures and pressures, realized the harmless treatment of chromium slag, have great social benefit and environmental benefit, simultaneously, because make chromium slag resource obtain farthest utilizing again, and the product quality better that extracts, the price height makes treatment of chromate slag have bigger economic benefit.
Four description of drawings
Fig. 1 is a process chart
Five specific embodiments
The innoxious comprehensive utilization of resources new technology of a kind of chromic slag wet method, with chromium slag ball milling to 80～200 orders, one soaks in hydrochloric acid solution, and regulating PH is 5～6, carry out Separation of Solid and Liquid with filter press, after a immersion liquid after the separation is trivalent chromium with the sulphite reduction of hexavalent chromium, add caustic-soda aqueous solution, adjusting PH is 4---6, rough chromium hydroxide, adding sulfuric acid in the filtrate, to transfer PH be 5～6, removes in the residual filtrate and the calcium magnesium co-precipitation, preparation sulfate dihydrate calcium pyroborate; It is 9---12 that the press filtration rear filtrate adds alkali adjusting PH, the synthesizing superfine magnesium hydrate powder; Solution concentration prepares sodium chloride after the press filtration;
One soaks hydrochloric acid for dreg solution carries out secondary pickling, and control PH 0.5～1.0 carries out Separation of Solid and Liquid, and after two immersion liquid after the Separation of Solid and Liquid were trivalent chromium with the sulphite reduction of hexavalent chromium earlier, adding alkali, to transfer PH be 3----4.5, precipitates iron hydroxide; Filter cake adds aquation and opens and divalent iron salt synthesizing superfine magnetic ferroferric oxide again after press filtration; Filtrate is settled out aluminium hydroxide after adding alkali accent PH3.5----5; After the press filtration rear filtrate adds alkali accent PH6-7, the synthetic corundum intermediate.Two soak slag puts into aqueous slkali and carries out alkali and soak, and after the press filtration Separation of Solid and Liquid, filter cake is chromite sand (being tailings); After adding the steric hindrance agent in the filtrate for example polyethylene glycol adding acid again and transfers PH8-9, synthetic silicic acid colloidal sol is through ageing, drying, calcine and then obtain the silica superfine powder.
Press filtration after the crude product chromium hydroxide added sulfuric acid and keep PH1-1.5 high-speed stirred, its filter cake promptly is a calcium sulphate dihydrate; Its filtrate adds caustic-soda aqueous solution, keeps PH5.8--6.0 high-speed stirred filter pressing to get the elaboration chromium hydroxide.The also available quick lime of caustic soda described in the reaction replaces.
Embodiment one
Chromium slag ball milling to 80～200 kilograms of chromium slags of 200 purposes are put in the agitator tank; Again 400 kilograms of hydrochloric acid are slowly added with 800 kilograms of pure water dilution backs and carry out " acidleach " i.e. acidleach for the first time in the agitator tank.The solution pH value is controlled at 5～6 in jar, stir the back and carry out Separation of Solid and Liquid with plate and frame filter press, filtrate imports the synthetic agitator tank of reduction, add sodium sulfite solution, make hexavalent chrome reduction become trivalent chromium, slowly add a certain amount of caustic-soda aqueous solution, to keep pH value be 6 and stir the back press filtration and obtain chromium hydroxide (crude product).After filtrate imported synthesis tank, adding 1:4 milk of lime adjusting pH value was to enter filter press after 11 stirrings.Its filtrate imports crystallizing evaporator and produces sodium chloride (crude product); Its filter cake adds in the synthesis tank, and adds the sulfuric acid (SILVER REAGENT) of 30% concentration, and pH value is remained on 2-1.5, after the high-speed stirred, gets calcium sulphate dihydrate (crude product) through filter pressing; Filtrate imports in the synthesis tank, adds sodium hydrate aqueous solution, and keeping pH value is 11, and filter pressing gets magnesium hydroxide (crude product) after stirring.Press filtration after the crude product chromium hydroxide adds 30% SILVER REAGENT sulfuric acid and keeps PH1-1.5 high-speed stirred, its filter cake promptly is a calcium sulphate dihydrate; Its filtrate adds the SILVER REAGENT caustic-soda aqueous solution, keeps PH5.8--6.0 high-speed stirred filter pressing to get the elaboration chromium hydroxide, promptly gets chromium hydroxide superfine powder finished product in 24 hours 90 ℃ of dryings.The crude product calcium sulphate dihydrate cleans, promptly gets the elaboration calcium sulphate dihydrate after 125 ℃ of dryings through three pure water.Press filtration after the crude product magnesium hydroxide adds 3 sulfuric acid and keeps pH value 1-1.5 high-speed stirred, filter cake promptly is a calcium sulphate dihydrate; Filtrate keeps PH11 after adding the SILVER REAGENT caustic-soda aqueous solution, the high-speed stirred press filtration, and its filter cake is the elaboration magnesium hydroxide after 150 ℃ of dryings after 12 hours; Filtrate imports crystallizing evaporator and reclaims sodium chloride.
Two acidleach i.e. acidleach for the second time.Soak the back filter cake with one and add in the agitator tank,, carry out press filtration after 1 hour PH of high-speed stirred is stabilized in 0.5-1.0 with adding in the agitator tank after 1200 kilograms of pure water and 400 kilograms of mixed in hydrochloric acid.Filter cake is waited until alkali and is soaked usefulness; Filtrate is handled in the following order: adding a small amount of caustic-soda aqueous solution reduction of hexavalent chromium under the high speed fine jade changes is three prices, again the concentration caustic-soda aqueous solution is slowly added in the agitator tank when non-hexavalent chromium reacts in affirmation solution, and PH is remained on the pressure worry of the back of stirring below 3.4.Filter cake is iron hydroxide; Filtrate imports in the agitator tank and adds caustic-soda aqueous solution, and making PH is 4.7, stirs the back and presses worry.Filter cake is aluminium hydroxide; Filtrate imports in the agitator tank again and to add caustic-soda aqueous solution and slowly add in the agitator tank PH and be controlled at 5.6 and stir the back and press and consider.Filter cake is chromium hydroxide (crude product); Filtrate imports in the synthesis tank, adds caustic-soda aqueous solution and PH is controlled at 6.5, stirs the back pressure and considers, and filter cake is the corundum intermediate; Filtrate imports and to add 1:4 milk of lime in the agitator tank and regulate PH and 11 carry out the co-precipitation of calcium magnesium, below extracts calcium sulphate dihydrate, magnesium hydroxide, sodium chloride respectively by technology described in aforementioned " acidleach ".The iron hydroxide filter cake is added 60 kilograms of pure water stir and melt the back and add solution of ferrous chloride, through stirring after, slowly add caustic-soda aqueous solution and keep PH6.5, press filtration and after abundant the flushing, filter cake is tri-iron tetroxide; Through 75 ℃ of drying pickling after 12 hours, washing, promptly get the ultra-fine magnetic powder of tri-iron tetroxide after 48 hours through 75 ℃ of dryings again.
One alkali soaks.Be about to carry out alkali in diacid leaching cake input NaOH (about the 10 kilograms) aqueous solution and soak the back press filtration, filter cake is tailings, is the primary chromite sand of participating in reaction in the former chromium salt factory roasting technique.Filtrate adds 5000 milliliters of steric hindrance agent such as polyethylene glycol under high-speed stirred, regulating PH with hydrochloric acid again is 8～9 synthetic silicic acid colloidal sols, after ageing 1 day is spray-dried powder hydrochloric acid and pure water with 10% concentration after under 90 ℃ of conditions dry 48 hours cleaned 2--4 time repeatedly, when confirming the negative reaction of Cr VI again with the silicic acid gel ageing after 5 days under 90 ℃ of conditions drying 48 hours, move in the high temperature furnace 900 ℃ of calcinings 8 hours again, take out when naturally cooling to room temperature the silica superfine powder.It is the chromium salt factory raw material that alkali soaks back only surplus 1.3～1.5% tailings (chromite sand).
Claims (4)
1, the innoxious comprehensive utilization of resources new technology of a kind of chromic slag wet method, with chromium slag ball milling to 80～200 orders, after adding water slurrying, in hydrochloric acid solution, carry out soaking, regulating PH is 5～6, stir the back and carry out Separation of Solid and Liquid with filter press, it is characterized in that: after the immersion liquid after the separation is trivalent chromium with the sulphite reduction of hexavalent chromium, add caustic-soda aqueous solution, adjusting PH is 4---6, gets rough chromium hydroxide after the stirring, and adding sulfuric acid accent PH in the filtrate is 5～6, remove in the residual filtrate and the calcium magnesium co-precipitation, preparation sulfate dihydrate calcium pyroborate; It is 9---12 that the press filtration rear filtrate adds alkali adjusting PH, the synthesizing superfine magnesium hydrate powder; Solution concentration prepares sodium chloride after the press filtration;
One soaks hydrochloric acid for dreg solution carries out secondary pickling, and control PH 0.5～1.0 carries out Separation of Solid and Liquid, and after two immersion liquid after the Separation of Solid and Liquid were trivalent chromium with the sulphite reduction of hexavalent chromium earlier, adding alkali, to transfer PH be 3----4.5, precipitates iron hydroxide; Filter cake adds aquation and opens and divalent iron salt synthesizing superfine magnetic ferroferric oxide again after press filtration; Filtrate is settled out aluminium hydroxide after adding alkali accent PH3.5----5; After the press filtration rear filtrate adds alkali accent PH6-7, the synthetic corundum intermediate.
2, the innoxious comprehensive utilization of resources new technology of chromic slag wet method according to claim 1 is characterized in that: two soak slag puts into aqueous slkali and carries out alkali and soak, and after the press filtration Separation of Solid and Liquid, filter cake is chromite sand (being tailings); Filtrate adds after the steric hindrance agent adds acid again and transfer PH8-9, and synthetic silicic acid colloidal sol is through ageing, drying, calcine and then obtain the silica superfine powder.
3, the innoxious comprehensive utilization of resources new technology of chromic slag wet method according to claim 1 is characterized in that: the crude product chromium hydroxide is added sulfuric acid and keep PH1-1.5 to stir the back press filtration, its filter cake promptly is a calcium sulphate dihydrate; Its filtrate adds caustic-soda aqueous solution, keeps PH5.8--6.0 to stir filter pressing and gets the elaboration chromium hydroxide.
4, according to claim 2 or the innoxious comprehensive utilization of resources new technology of 3 described chromic slag wet methods, it is characterized in that: the also available quick lime of the caustic soda described in the reaction replaces.
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| CN110526292A (en) * | 2019-06-04 | 2019-12-03 | 河南金谷实业发展有限公司 | The technique of chromium is extracted in a kind of chromium pollutant |
| CN111139359A (en) * | 2020-01-16 | 2020-05-12 | 湖北振华化学股份有限公司 | Method for extracting chromium from chromium slag and pretreating chromium slag by acid leaching |
| CN111139359B (en) * | 2020-01-16 | 2022-02-25 | 湖北振华化学股份有限公司 | Method for extracting chromium from chromium slag and pretreating chromium slag by acid leaching |
| CN112607760A (en) * | 2020-12-25 | 2021-04-06 | 北京建筑材料科学研究总院有限公司 | Cement kiln bypass air-bleeding ash resource utilization system and method |
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