CN101817561A - Method for pollution-free production of sodium chromate by pressure leaching of chromite - Google Patents
Method for pollution-free production of sodium chromate by pressure leaching of chromite Download PDFInfo
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- CN101817561A CN101817561A CN 201010146648 CN201010146648A CN101817561A CN 101817561 A CN101817561 A CN 101817561A CN 201010146648 CN201010146648 CN 201010146648 CN 201010146648 A CN201010146648 A CN 201010146648A CN 101817561 A CN101817561 A CN 101817561A
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Abstract
The invention belongs to the field of chromite hydrometallurgy and chromium chemical industry, and in particular relates to a method for the pollution-free production of sodium chromate by pressure leaching of chromite. The method comprises the following steps of: 1) reacting the chromite with oxidizing gas in solution of NaOH; 2) diluting the product obtained by the step 1) and making subcrystalline sodium chromate to fully enter a liquid phase; 3) performing solid-liquid separation on the solid-liquid mixed slurry obtained by the step 2); 4) adding calcium oxide into the obtained diluent for removing impurities; and 5) evaporating and crystallizing the obtained solution without the impurities to obtain a sodium chromate crystal and crystallization mother solution; after the solid-liquid separation, rinsing the sodium chromate crystal by using saturated solution of sodium chromate; and drying to obtain a qualified sodium chromate product. The method has the advantages of simple reaction system component, no difficultly separated phase introduced in the system, contribution to high-efficiency separation of the sodium chromate, great reduction in reaction temperature, low energy consumption, effective reduction in production cost of the sodium chromate, and high chromium leaching yield.
Description
Technical field
The invention belongs to chromite hydrometallurgy and chromaking worker field, particularly a kind of method of pollution-free production of sodium chromate by pressure leaching of chromite.
Background technology
Sodium chromate is important industrialization chemical product, is the requisite of producing other chromium cpds.Chromite is the direct sources of producing Sodium chromate.
Chromite in becoming the ore deposit process, chromium and other metallic elements formed the chromohercynite structure ((Mg, Fe) (Cr, Al)
2O
4).This feasible method with mechanical ore grinding and ore dressing is difficult to make chromium to separate.The existing method with chromite production Sodium chromate of China has mainly contained calcium roasting method and calcium-free roasting method.Chromite uses traditional when having calcium roasting method technology to smelt, and the chromium transformation efficiency is low, only is about 75%, and bed drain purge is big, content of 6-valence Cr ions height in the slag, and environmental pollution is serious; Optimize the calcium-free roasting method that tradition has the calcium roasting method to form, compare with the calcium roasting method is arranged, chromium leaching yield height, that bed drain purge is little, slag contains sexavalent chrome is low, but facility investment is big, the body of heater ring formation is serious in the roasting process, and now u.s.a. and japan can industrialization, but the domestic heavy industrialization of still being unrealized.
In recent years, Chinese Academy Of Sciences Process Engineering Research Institute has made big quantity research to the liquid phase method process for cleanly preparing of chromic salts, has developed sub-molten salt method and molten-salt growth method series chromium-salt clean production process.CN1410358 utilizes the KOH fused salt under the effect of oxygenant, and chromite is decomposed in liquid-phase oxidation, the transformation efficiency height, and bed drain purge is little.At present, this technology has been built up the ton demonstration project.But the finished product of this technology are chromic oxide, can't satisfy the requirement of market to the Sodium chromate series product.CN1226512 replaces KOH with NaOH, has specifically introduced NaOH fused salt liquid phase oxygenolysis chromite and has produced the Sodium chromate cleaning procedure.This method is used the NaOH fused salt, and alkali ore deposit ratio is 3: 1～6: 1, and the NaOH temperature of molten salt is 500～550 ℃, and the reaction times is 6 hours, and the crystallization of dilution postcooling obtains the mixed crystal of Sodium chromate and sodium aluminate, further separates Sodium chromate and sodium aluminate again.The shortcoming of this method is to use the NaOH fused salt to require the temperature of reaction height, need evaporate during the recycle of dilution alkali lye and put forward highly basic concentration, the energy consumption height; Concentration of lye after the dilution is still very high, and soltion viscosity is big, the solid-liquid separation difficulty; And under the high temperature high alkali environment, equipment corrosion is serious; And the mixed crystal that obtains needs further to separate, and technical process is long.
In order to solve the deficiency of CN1226512, CN101659444 has proposed to have added NaNO in system
3To replace the technology of part NaOH.This technological reaction temperature is 280～400 ℃, and transformation efficiency contains the chromium rate less than 0.5% greater than 99% in the slag; NaNO in system
3Only as catalysts, self does not consume.But the weak point of this technology is to have introduced NaNO
3, make Na
2CrO
4Crystalline extraction process complexity, difficulty are big; And SODIUMNITRATE easily resolves into Sodium Nitrite in reaction process, and is difficult to remove, and makes the industrialization of this technology be subjected to very big constraint.Along with the progress of Materials science, the development of metallurgical equipment needs a kind ofly more to optimize, efficiently with the process for cleanly preparing of preparing sodium chromate from chromite.
Summary of the invention
Therefore, purpose of the present invention is just at above-mentioned the deficiencies in the prior art part, and what provide is a kind of according to the chromite mineralogical character, chromite is pressurizeed leach the method for producing Sodium chromate.
Principle of the present invention be chromite in autoclave, react at 180～320 ℃ with certain density NaOH solution, oxidizing gas, make trivalent chromium be oxidized to sexavalent chrome and generate Sodium chromate, the chemical reaction that wherein relates to has:
Sodium chromate clean preparation method of the present invention is: chromite is oxygenolysis in NaOH solution and oxidizing atmosphere, makes chromium with Na
2CrO
4Form enter solution, the dilution after-filtration remove tailings, carry out evaporative crystallization again and obtain the Sodium chromate product.
Method according to pollution-free production of sodium chromate by pressure leaching of chromite of the present invention may further comprise the steps:
1) chromite carries out the heated oxide reaction with oxidizing gas in NaOH solution, and the concentration of NaOH is 30%wt～80%wt, and the mass ratio of NaOH and chromite is 2: 1～10: 1, obtains containing Na after the reaction
2CrO
4, the solution of NaOH and other water-soluble impurity and rich iron tailings, crystals of sodium chromate solidliquid mixture;
2) dilution step 1) product that obtains, make the Sodium chromate of partial crystallization all enter liquid phase, obtain containing NaOH, Na
2CrO
4And the solution of water-soluble impurity component and the solid-liquid mixed slurry of rich iron tailings;
3) with step 2) the solid-liquid mixed slurry that obtains carries out solid-liquid separation, and obtain rich iron tailings respectively and contain NaOH, Na
2CrO
4And the diluting soln of water-soluble impurity component;
4) in the diluent that step 3) obtains, add the calcium oxide removal of impurities, obtain removal of impurities liquid and calcic waste residue after the solid-liquid separation;
5) the removal of impurities solution evaporation crystallization that step 4) is obtained obtains crystals of sodium chromate and crystalline mother solution, and crystals of sodium chromate can obtain qualified Sodium chromate product after drying with saturated chromium acid sodium solution drip washing after the solid-liquid separation.
Method according to pollution-free production of sodium chromate by pressure leaching of chromite of the present invention, wherein, described step also comprises the step that rich iron tailings that step 3) is obtained carries out the multi-stage countercurrent washing with clear water, therefore, can be with clear water or the above-mentioned washings dilution step 1 that obtains) product that obtains.
According to the method for pollution-free production of sodium chromate by pressure leaching of chromite of the present invention, wherein, described step also comprises after the crystalline mother solution that step 5) is obtained is transferred alkali returns the oxygenolysis that step 1) is used for chromite.
According to the method for pollution-free production of sodium chromate by pressure leaching of chromite of the present invention, preferably, the temperature of reaction of the oxidizing reaction in the step 1) is 180 ℃～320 ℃.
According to the method for pollution-free production of sodium chromate by pressure leaching of chromite of the present invention, preferably, the reaction times of the oxidizing reaction in the step 1) is 0.5～10.0 hour.
According to the method for pollution-free production of sodium chromate by pressure leaching of chromite of the present invention, preferably, in step 1), the dividing potential drop of oxidizing gas is 0.1MPa～5.0MPa,
According to the method for pollution-free production of sodium chromate by pressure leaching of chromite of the present invention, wherein, in step 1), described oxidizing gas is air, oxygen, oxygen-rich air, ozone and composition thereof.
Therefore, the method for pollution-free production of sodium chromate by pressure leaching of chromite according to a particular embodiment of the invention can may further comprise the steps:
1) chromite reacts with oxidizing gas in certain density NaOH solution, described oxidizing gas can be air, oxygen, oxygen-rich air, ozone and composition thereof, oxygen during reaction or the dividing potential drop of other oxidizing gas are 0.1MPa～5.0MPa, the mass ratio of NaOH and chromite is 2: 1～10: 1, the concentration of NaOH is 30%wt～80%wt, the temperature of reaction is 180 ℃～320 ℃, and the time of reaction is 0.5～10.0 hour, obtains containing Na after the reaction
2CrO
4, the solidliquid mixture that forms of the solution of NaOH and other water-soluble impurity and rich iron tailings, crystals of sodium chromate;
2) product that step 1) is obtained is with clear water or following steps 4) the washings dilution that obtains, make the Sodium chromate of partial crystallization all enter liquid phase, obtain containing NaOH, Na
2CrO
4And the solution of water-soluble impurity component and the solid-liquid mixed slurry of rich iron tailings;
3) with step 2) the solid-liquid mixed slurry that obtains carries out solid-liquid separation, and obtain rich iron tailings respectively and contain NaOH, Na
2CrO
4And the solution of water-soluble impurity component;
4) the rich iron tailings that obtains of step 3) is with the washing of clear water multi-stage countercurrent, and washings can be used as step 2) dilution;
5) diluent that step 3) is obtained adds the calcium oxide removal of impurities, obtains removal of impurities liquid and calcic waste residue after the solid-liquid separation;
What 6) step 5) is obtained contains NaOH, Na
2CrO
4Deng the solution evaporation crystallization, obtain crystals of sodium chromate and crystalline mother solution, crystals of sodium chromate can obtain qualified Sodium chromate product after drying with saturated chromium acid sodium solution drip washing after the solid-liquid separation;
7) crystalline mother solution that step 6) is obtained returns the oxygenolysis that step (1) is used for chromite after transferring alkali.
The present invention proposes the cleaning procedure of pressurization leaching chromite production Sodium chromate in autoclave, compare, obvious superiority is arranged with domestic and international existing production method:
1, from reaction system, the leach liquor composition is simple, does not introduce the difficult phase of separating in the system, and in reaction and leaching process, the water-soluble by product of generation is sodium aluminate, water glass, yellow soda ash, can add calcium oxide and remove, and helps the high efficiency separation of Sodium chromate.
2, from reaction conditions, to compare with traditional technology, temperature of reaction reduces greatly, and energy consumption is little, effectively reduces the production cost of Sodium chromate.
3, this invention chromium leaching yield height can reach more than 99%, and bed drain purge is little, and slag toxic content of 6-valence Cr ions is low, and the slag main component is a ferric oxide, easier realization comprehensive utilization.
4, the waste of this technology NaOH is little, only needs to buy small amount of alkali and just can meet the needs of production.
5, this technology self can realize the balance of water, and this technology both can be founded the factory separately, also can calcium sinter process, calcium-free roasting technology, liquid phase production technology be arranged with tradition and deposits, and is fit to that old factory transforms and the side area is newly-built separately.
6, this technology both can be founded the factory separately, also can calcium sinter process, calcium-free roasting technology, liquid phase production technology be arranged with tradition and deposited, and was fit to that old factory transforms and the side area is newly-built separately.
Description of drawings
Fig. 1 is the schematic flow sheet of method of the present invention
Embodiment
Embodiment 1
In autoclave, add the NaOH solution of chromite and 30%, alkali ore deposit ratio is 10: 1, is heated to 300 ℃, bubbling air in solution then, and stir, chromite is fully contacted with oxygen, hierarchy of control total pressure is 8MPa, is incubated 10 hours, and chromite and oxygen are fully reacted.Finally obtain containing NaOH and Na
2CrO
4Deng solution, crystals of sodium chromate and rich iron tailings, the transformation efficiency of principal element chromium is more than 99% in the chromite.Add the clear water diluted reaction mixture, solid-liquid separation obtains rich iron tailings and contains Na then
2CrO
4, NaOH etc. solution.With after adding an amount of calcium oxide removal of impurities in the solution, evaporative crystallization obtains crystals of sodium chromate again.Crystals of sodium chromate promptly obtains purity at the Sodium chromate product more than 99% after saturated chromium acid sodium solution drip washing and drying.Rich iron tailings can be used as the ferrous metallurgy raw material after the washing of three stage countercurrents.
Embodiment 2
In autoclave, add the NaOH solution of chromite and 50wt%, alkali ore deposit ratio is 6: 1, is heated to 280 ℃, aerating oxygen in solution then, and stir, chromite is fully contacted with oxygen, hierarchy of control total pressure is 6MPa, is incubated 8 hours, and chromite and oxygen are fully reacted.Finally obtain containing NaOH and Na
2CrO
4Deng solution, crystals of sodium chromate and rich iron tailings, the transformation efficiency of principal element chromium is more than 99% in the chromite.Add the clear water diluted reaction mixture, solid-liquid separation obtains rich iron tailings and contains Na then
2CrO
4, NaOH etc. solution, subsequent technique is with embodiment 1.
Embodiment 3
In autoclave, the NaOH solution that adds chromite and 80wt%, alkali ore deposit ratio is 2: 1, be heated to 200 ℃, in solution, feed ozone then, and stir, chromite is fully contacted with ozone, hierarchy of control total pressure is 0.5MPa, is incubated 0.5 hour, and chromite and ozone are fully reacted.Finally obtain containing NaOH and Na
2CrO
4Deng solution, crystals of sodium chromate and rich iron tailings, the transformation efficiency of principal element chromium is more than 99% in the chromite.Add the rich iron tailings washings diluted reaction mixture that obtains among the embodiment 2, solid-liquid separation obtains rich iron tailings and contains Na2CrO then
4, NaOH etc. solution, subsequent technique is with embodiment 1.
Embodiment 4
In autoclave, add chromite, 55wt%NaOH solution and Sodium chromate, alkali ore deposit ratio is 4: 1, be heated to 260 ℃, aerating oxygen in solution then, and stir, chromite is fully contacted with oxygen, hierarchy of control total pressure is 4MPa, is incubated 6 hours, and chromite and oxygen are fully reacted.Finally obtain containing NaOH and Na
2CrO
4Deng solution, crystals of sodium chromate and rich iron tailings, the transformation efficiency of principal element chromium is more than 99% in the chromite.With solid-liquid separation behind the clear water diluted reaction mixture, obtain rich iron tailings and contain Na
2CrO
4, NaOH etc. solution, subsequent technique is with embodiment 1.
Embodiment 5
Circulation turns back to the evaporative crystallization mother liquor of reactor, after mending alkali, add chromite, alkali ore deposit ratio is 4: 1, is heated to 260 ℃, aerating oxygen in solution then, and stir, chromite is fully contacted with oxygen, hierarchy of control total pressure is 4.5MPa, be incubated 5 hours, chromite and oxygen are fully reacted.Reaction conversion ratio is more than 99%.With carrying out solid-liquid separation behind the rich iron tailings washings diluted reaction mixture that obtains among the embodiment 4, obtain rich iron tailings and contain Na
2CrO
4, NaOH etc. solution, subsequent technique is with embodiment 1.
Claims (8)
1. the method for a pollution-free production of sodium chromate by pressure leaching of chromite is characterized in that, said method comprising the steps of:
1) chromite carries out the heated oxide reaction with oxidizing gas in NaOH solution, and the concentration of NaOH is 30%wt～80%wt, and the mass ratio of NaOH and chromite is 2: 1～10: 1, obtains containing Na after the reaction
2CrO
4, the solution of NaOH and other water-soluble impurity and rich iron tailings, crystals of sodium chromate solidliquid mixture;
2) dilution step 1) product that obtains, make the Sodium chromate of partial crystallization all enter liquid phase, obtain containing NaOH, Na
2CrO
4And the solution of water-soluble impurity component and the solid-liquid mixed slurry of rich iron tailings;
3) with step 2) the solid-liquid mixed slurry that obtains carries out solid-liquid separation, and obtain rich iron tailings respectively and contain NaOH, Na
2CrO
4And the diluting soln of water-soluble impurity component;
4) in the diluent that step 3) obtains, add the calcium oxide removal of impurities, obtain removal of impurities liquid and calcic waste residue after the solid-liquid separation;
5) the removal of impurities solution evaporation crystallization that step 4) is obtained obtains crystals of sodium chromate and crystalline mother solution, and crystals of sodium chromate can obtain qualified Sodium chromate product after drying with saturated chromium acid sodium solution drip washing after the solid-liquid separation.
2. the method for pollution-free production of sodium chromate by pressure leaching of chromite according to claim 1 is characterized in that, described step comprises that also the rich iron tailings that step 3) is obtained carries out the step that multi-stage countercurrent washs with clear water.
3. the method for pollution-free production of sodium chromate by pressure leaching of chromite according to claim 1 is characterized in that, described step also comprises after the crystalline mother solution that step 5) is obtained is transferred alkali returns the oxygenolysis that step 1) is used for chromite.
4. the method for pollution-free production of sodium chromate by pressure leaching of chromite according to claim 1 is characterized in that, in described step 2) in, the washings dilution step 1 that obtains with clear water or claim 2) product that obtains.
5. the method for pollution-free production of sodium chromate by pressure leaching of chromite according to claim 1 is characterized in that, the temperature of reaction of the oxidizing reaction in the step 1) is 180 ℃～320 ℃.
6. the method for pollution-free production of sodium chromate by pressure leaching of chromite according to claim 1 is characterized in that, the reaction times of the oxidizing reaction in the step 1) is 0.5～10.0 hour.
7. the method for pollution-free production of sodium chromate by pressure leaching of chromite according to claim 1 is characterized in that, in step 1), the dividing potential drop of oxidizing gas is 0.1MPa～5.0MPa.
8. the method for pollution-free production of sodium chromate by pressure leaching of chromite according to claim 1 is characterized in that, in step 1), described oxidizing gas is air, oxygen, oxygen-rich air, ozone and composition thereof.
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Cited By (14)
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|---|---|---|---|---|
| CN102531056A (en) * | 2012-01-09 | 2012-07-04 | 中国科学院过程工程研究所 | Method for cleaner production of sodium vanadate and sodium chromate by pressure leaching of vanadium slag |
| CN103060838A (en) * | 2012-12-29 | 2013-04-24 | 中国科学院过程工程研究所 | Method for extracting chromium by electrochemically decomposing chromite in potassium hydroxide solution |
| CN103183384A (en) * | 2013-03-29 | 2013-07-03 | 中国科学院过程工程研究所 | Method for preroasting and intensifying chromite decomposed by sub-molten salt |
| CN103449522A (en) * | 2012-06-01 | 2013-12-18 | 中国科学院过程工程研究所 | Method for producing chromates through using chromium-containing waste residues |
| CN104341004A (en) * | 2013-07-25 | 2015-02-11 | 中国科学院过程工程研究所 | New process for preparing potassium chromate through pressurization leaching on chromite |
| CN104512930A (en) * | 2013-09-30 | 2015-04-15 | 湖北振华化学股份有限公司 | Method for producing chromate by liquid-phase catalytic oxidation of chromite |
| CN104512931A (en) * | 2013-09-30 | 2015-04-15 | 湖北振华化学股份有限公司 | Chromite decomposing method through pressurizing liquid-phase oxidizing method and device used in the chromite decomposing method through the pressurizing liquid-phase oxidizing method |
| CN104726705A (en) * | 2013-12-23 | 2015-06-24 | 中国科学院过程工程研究所 | Method for extracting chromium from chromite by leaching |
| CN104760997A (en) * | 2015-03-05 | 2015-07-08 | 重庆民丰化工有限责任公司 | Production method of sodium chromate with alkali liquid circulation and liquid phase oxidization |
| CN104843790A (en) * | 2015-05-22 | 2015-08-19 | 四川省银河化学股份有限公司 | Method for preparing sodium chromate from chromite by acid dissolution oxygenation |
| CN105366724A (en) * | 2015-12-24 | 2016-03-02 | 四川省银河化学股份有限公司 | Method for producing chromium oxide green through sodium circulation |
| CN106186068A (en) * | 2016-07-06 | 2016-12-07 | 于广新 | The clean preparation method of chromate is prepared in a kind of Continuous Liquid Phase oxidation |
| CN107902699A (en) * | 2017-11-14 | 2018-04-13 | 中国科学院过程工程研究所 | A kind of decomposition method of continuous pressure self-heating liquid phase oxidation chromite |
| CN110947319A (en) * | 2019-12-16 | 2020-04-03 | 重庆理工大学 | Dynamic and static combined stirring system and process for preparing chromium salt through chromite liquid-phase oxidation |
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| CN102531056A (en) * | 2012-01-09 | 2012-07-04 | 中国科学院过程工程研究所 | Method for cleaner production of sodium vanadate and sodium chromate by pressure leaching of vanadium slag |
| CN102531056B (en) * | 2012-01-09 | 2014-11-05 | 中国科学院过程工程研究所 | Method for cleaner production of sodium vanadate and sodium chromate by pressure leaching of vanadium slag |
| CN103449522A (en) * | 2012-06-01 | 2013-12-18 | 中国科学院过程工程研究所 | Method for producing chromates through using chromium-containing waste residues |
| CN103449522B (en) * | 2012-06-01 | 2016-03-09 | 中国科学院过程工程研究所 | A kind of chromium residue produces the method for chromic salt |
| CN103060838A (en) * | 2012-12-29 | 2013-04-24 | 中国科学院过程工程研究所 | Method for extracting chromium by electrochemically decomposing chromite in potassium hydroxide solution |
| CN103060838B (en) * | 2012-12-29 | 2015-12-23 | 中国科学院过程工程研究所 | In a kind of potassium hydroxide solution, electrochemical decomposition chromite extracts the method for chromium |
| CN103183384A (en) * | 2013-03-29 | 2013-07-03 | 中国科学院过程工程研究所 | Method for preroasting and intensifying chromite decomposed by sub-molten salt |
| CN103183384B (en) * | 2013-03-29 | 2016-08-10 | 中国科学院过程工程研究所 | The method that a kind of preroast strengthening sub-molten salt decomposes chromite |
| CN104341004A (en) * | 2013-07-25 | 2015-02-11 | 中国科学院过程工程研究所 | New process for preparing potassium chromate through pressurization leaching on chromite |
| CN104512930A (en) * | 2013-09-30 | 2015-04-15 | 湖北振华化学股份有限公司 | Method for producing chromate by liquid-phase catalytic oxidation of chromite |
| CN104512931A (en) * | 2013-09-30 | 2015-04-15 | 湖北振华化学股份有限公司 | Chromite decomposing method through pressurizing liquid-phase oxidizing method and device used in the chromite decomposing method through the pressurizing liquid-phase oxidizing method |
| CN104726705A (en) * | 2013-12-23 | 2015-06-24 | 中国科学院过程工程研究所 | Method for extracting chromium from chromite by leaching |
| CN104726705B (en) * | 2013-12-23 | 2017-06-06 | 中国科学院过程工程研究所 | A kind of chromite leaches the method for carrying chromium |
| CN104760997A (en) * | 2015-03-05 | 2015-07-08 | 重庆民丰化工有限责任公司 | Production method of sodium chromate with alkali liquid circulation and liquid phase oxidization |
| CN104843790A (en) * | 2015-05-22 | 2015-08-19 | 四川省银河化学股份有限公司 | Method for preparing sodium chromate from chromite by acid dissolution oxygenation |
| CN105366724B (en) * | 2015-12-24 | 2017-04-05 | 四川省银河化学股份有限公司 | A kind of method of sodium cyclic production chrome oxide green |
| CN105366724A (en) * | 2015-12-24 | 2016-03-02 | 四川省银河化学股份有限公司 | Method for producing chromium oxide green through sodium circulation |
| CN106186068A (en) * | 2016-07-06 | 2016-12-07 | 于广新 | The clean preparation method of chromate is prepared in a kind of Continuous Liquid Phase oxidation |
| CN107902699A (en) * | 2017-11-14 | 2018-04-13 | 中国科学院过程工程研究所 | A kind of decomposition method of continuous pressure self-heating liquid phase oxidation chromite |
| CN107902699B (en) * | 2017-11-14 | 2019-09-27 | 中国科学院过程工程研究所 | A kind of decomposition method of continuous pressure self-heating liquid phase oxidation chromite |
| CN110947319A (en) * | 2019-12-16 | 2020-04-03 | 重庆理工大学 | Dynamic and static combined stirring system and process for preparing chromium salt through chromite liquid-phase oxidation |
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