CN101845549A - Method for cleaning and converting stone coal - Google Patents

Method for cleaning and converting stone coal Download PDF

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Publication number
CN101845549A
CN101845549A CN201010203166A CN201010203166A CN101845549A CN 101845549 A CN101845549 A CN 101845549A CN 201010203166 A CN201010203166 A CN 201010203166A CN 201010203166 A CN201010203166 A CN 201010203166A CN 101845549 A CN101845549 A CN 101845549A
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naoh
solution
cleaning
stone coal
nano
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周宏明
郑诗礼
李荐
刘芙蓉
郭雁军
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Central South University
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Central South University
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Priority to CN2011101316633A priority patent/CN102260801B/en
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    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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Abstract

The invention relates to a method for cleaning and converting stone coal, which can produce vanadium pentoxide and calcium silicate serving as intermediates for preparing a series of vanadium products and white carbon black. The method comprises the following steps of: ball-milling the stone coal and oxidizing and roasting the milled stone coal at a high temperature; decomposing the roasted material with NaOH+NaNO3 sub-molten salt; separating the decomposition product by dilution to obtain high-concentration NaOH alkaline solution and solid phase containing sodium silicate and sodium vanadate; returning the alkaline solution to the decomposition step of the sub-molten salt for recycling; separating the solid phase containing sodium silicate and sodium vanadate in hot water by leaching to obtain the solution containing sodium silicate and sodium vanadate and slag phase containing iron, magnesium and calcium; adjusting the pH value of the liquid phase with acid and then adding ammonium chloride into the liquid phase to precipitate vanadium so as to obtain ammonium metavanadate precipitate and sodium silicate liquid phase; adding calcium hydroxide into the sodium silicate liquid phase to obtain calcium silicate precipitate and NaOH solution; concentrating the NaOH solution and then returning the concentrated NaOH solution to the decomposition step of the sub-molten salt; and calcining the ammonium metavanadate to obtain V2O5 product. Compared with a conventional sodium chloride high-temperature roasting process, the process eliminates the pollution of chlorine gas and hydrogen chloride, has overall vanadium recovery of over 75 percent which is increased by over 30 percent compared with the conventional sodium chloride roasting process, has silicon recovery of over 80 percent and has good economic benefit and environmental benefit.

Description

A kind of method for cleaning and converting stone coal
Technical field
The invention belongs to the hydrometallurgy field, be specifically related to be suitable for, be particularly suited for from difficulty decomposition bone coal raw material, extracting V from containing the raw material of vanadium 2O 5, and the high-efficiency cleaning production method of the intermediate Calucium Silicate powder of preparation white carbon black.
Background technology
Traditional process for extracting vanadium from stone coal is sodium roasting-acidleach-extraction process, calcification baking-acid leaching process, the direct acidleach of bone coal and alkali soaking technology etc.Sodium roasting-acidleach-extraction process is simple, and cost is low, but roasting process can cause the pollution of chlorine and hydrogenchloride, and the yield of vanadium is low, has only about 45%, and use gradually is under an embargo.Reduce though calcification baking-acid leaching process baking flue gas pollutes, the acid consumption is bigger, and the subsequent disposal more complicated, the cost height.Directly acid leaching process can be avoided smoke pollution, and the leaching yield of vanadium can reach 60-70%, use more, but the long 36-48h of extraction time.Oxygen presses acid leaching process can accelerate the decomposition rate of bone coal, but the industrializing implementation difficulty of this technology is bigger.In recent years, with the increase of vanadium goods demand, the reasonable utilization of bone coal has put on the agenda.
In recent years, under the pressure of environmental protection pressure, the waste gas that Chinese patent (CN 101176837 A) produces at rotary kiln baking in the traditional technology sodium roasting technology, adopt dry gas cleaning, press three classes, six grades of turbulence foam absorption tower waters, 10% sodium hydrogen carbonate solution and saturated limewaters again as the toxic substances such as dust, sulfurous gas, chlorine and hydrogenchloride in the middle of the absorption agent processing waste gas, go effect preferably.Chinese patent (CN 101054630A) carries out the comprehensive regulation at the waste that traditional technology sodium roasting technology produces, and water or milk of lime absorb sulfurous gas, chlorine and hydrogenchloride etc., with negative pressure water absorption of N H 3Chinese patent (CN101069807A) adopts milk of lime or Wingdale breast as the scavenging agent of baking flue gas, obtains higher resource utilization.Though these methods all have effect preferably on the bone coal baking flue gas is handled, these methods all belong to the cost height generally, and little end treatment produces effects.
Summary of the invention
The purpose of this invention is to provide a kind of defective that can overcome on the prior art, efficiently realize the method that the bone coal cleaning transforms, can make Vanadium Pentoxide in FLAKES and Calucium Silicate powder intermediate as serial vanadium product of preparation and white carbon black.This method can reduce the discharging of toxic chlorine, hydrogenchloride etc., eliminate " three wastes " pollution from beginning of production to environment, and increase substantially the vanadium recovery in the bone coal, obtain good economic benefit and environmental benefit, this is that traditional sodium roasting method is unrivaled.
According to NaOH+NaNO 3Inferior molten salt system has good fluidity, the chemical property that characteristics that reactive behavior is high and the vanadic acid sodium solubleness in NaOH solution reduces with the increase of NaOH concentration, and the technological method of formation is described in detail as follows:
(1): bone coal is advanced planetary high-energy ball milling, and the ball milling time is 16-36h, and the stone coal powder behind the ball milling is crossed 350 mesh standard sieves.
(2): the bone coal behind mistake 350 mesh standard sieves that step (1) is obtained places retort furnace to carry out oxidizing roasting, and maturing temperature is 800～900 ℃, and roasting time is 1-5h.
(3): the bone coal after the oxidizing roasting that step (2) is obtained is at NaOH+NaNO 3Decompose NaOH+NaNO during decomposition in the inferior molten salt solution 3Inferior molten salt solution mass concentration is 50～75%, and decomposition temperature is 150～250 ℃, and the resolving time is 1.5-3h, NaOH+NaNO 3With the alkali ore deposit mass ratio of bone coal be 3: 1～6: 1, NaNO 3At NaOH+NaNO 3Mass ratio in the inferior molten salt solution is 2%～6%.
(4): use H 2O or dilute NaOH solution in temperature be under 20 ℃～110 ℃ the condition dilution bone coal at NaOH+NaNO 3Degradation production in the inferior fused salt, obtaining concentration is the NaOH diluent of 550～750g/L and the solid phase that contains vanadic acid sodium and water glass, the NaOH diluent returns inferior fused salt decomposition step.
(5): the solid product H that step (4) is contained vanadic acid sodium and water glass 2O heats leaching, and vanadic acid sodium and the water glass of Yi Rong change solution over to, separates with insoluble sodium aluminium silicate and iron magnesium calcium slag, and extraction temperature is 60～100 ℃, and leach liquor NaOH concentration is 60～150g/L.
(6): add the nitre acid for adjusting pH value in the solution that contains vanadic acid sodium and water glass that step (5) is obtained to 8-9, add ammonium chloride then, obtain the ammonium meta-vanadate precipitation and contain the solution of water glass.
(7): the ammonium meta-vanadate precipitation that step (6) is obtained is carried out high-temperature calcination and is decomposed and obtain V 2O 5Product can be used to prepare the intermediate of vanadium product.
(8): add Ca (OH) in the solution that contains water glass that step (6) is obtained 2, obtaining precipitated calcium silicate and the solution that contains NaOH, precipitated calcium silicate can be used as the raw material for preparing white carbon black, after the solution of NaOH carries out evaporation concentration, returns inferior fused salt decomposition step.
Advantage of the present invention is:
(1): the present invention proposes NaOH+NaNO 3Sub-molten salt method is handled bone coal, compares with traditional sodium roasting or calcification baking method, from the pollution that beginning of production has been stopped chlorine and hydrogenchloride, has huge environmental benefit.
(2): the present invention improves more than 30% than traditional sodium roasting method the vanadium recovery in the bone coal, reaches more than 75%, has greatly improved resource utilization.
(3): the present invention has greatly reduced starting material ground and has consumed owing to realized the internal recycling of decomposition media, and NaOH does not have process loss, and alkali consumption is the 0.3kg/kg ore deposit, and production cost reduces greatly.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
By following example in detail the present invention, but can not think a kind of restriction:
Embodiment 1:
The alkali lye that reactor is returned in circulation adds 2% NaNO through heat temperature raising to 150 ℃ 3, NaOH+NaNO 3Inferior fused salt mass concentration is 50%.350 mesh sieves will be crossed behind the bone coal ball milling 36h, again at 750 ℃ of following oxidizing roasting 5h, by alkali ore deposit mass ratio is 6: 1, under agitation the stone coal powder of handling well is joined in the reactor, complete hybrid reaction is 3 hours under 150 ℃, obtain degradation production, the dilute with water degradation production, dilution back NaOH concentration is 556g/L, temperature is 30 ℃, separate alkali lye and the solid phase that contains vanadic acid sodium, alkali lye returns inferior fused salt decomposition step through dehydration by evaporation, contains the solid phase water extraction of vanadic acid sodium, leaching liquid contains NaOH 61g/L, temperature is 60 ℃, and behind the leaching 30min, filtered while hot obtains containing the solution and the iron magnesium calcium slag precipitation of vanadic acid sodium and water glass.Add nitric acid and make the pH value of sodium vanadate solution transfer to 8, add ammonium chloride, obtain the solution that ammonium meta-vanadate precipitates and contain water glass, contain in the solution of water glass and add Ca (OH) 2, obtaining precipitated calcium silicate and the solution that contains NaOH, precipitated calcium silicate can be used as the raw material for preparing white carbon black, after the solution of NaOH carries out evaporation concentration, returns inferior fused salt decomposition step, and the ammonium meta-vanadate precipitation is carried out the high-temperature calcination decomposition and is obtained V 2O 5Product can be used to prepare the intermediate of vanadium product.The total yield of vanadium is 78%, the V of gained 2O 5Content be 98.6%, the content of Calucium Silicate powder is 98.4%.
Embodiment 2:
The alkali lye that reactor is returned in circulation adds 4% NaNO through heat temperature raising to 200 ℃ 3, NaOH+NaNO 3Inferior fused salt mass concentration is 68%.350 mesh sieves will be crossed behind the bone coal ball milling 24h, again at 800 ℃ of following oxidizing roasting 3h, by alkali ore deposit mass ratio is 5: 1, under agitation the stone coal powder of handling well is joined in the reactor, complete hybrid reaction is 2 hours under 200 ℃, obtain degradation production, the dilute with water degradation production, dilution back NaOH concentration is 632g/L, temperature is 80 ℃, separate alkali lye and the solid phase that contains vanadic acid sodium, alkali lye returns inferior fused salt decomposition step through dehydration by evaporation, contains the solid phase water extraction of vanadic acid sodium, leaching liquid contains NaOH 103g/L, temperature is 80 ℃, and behind the leaching 40min, filtered while hot obtains containing the solution and the iron magnesium calcium slag precipitation of vanadic acid sodium and water glass.Add nitric acid and make the pH value of sodium vanadate solution transfer to 9, add ammonium chloride, obtain the solution that ammonium meta-vanadate precipitates and contain water glass, contain in the solution of water glass and add Ca (OH) 2, obtaining precipitated calcium silicate and the solution that contains NaOH, precipitated calcium silicate can be used as the raw material for preparing white carbon black, after the solution of NaOH carries out evaporation concentration, returns inferior fused salt decomposition step, and the ammonium meta-vanadate precipitation is carried out the high-temperature calcination decomposition and is obtained V 2O 5Product can be used to prepare the intermediate of vanadium product.The total yield of vanadium is 81%, the V of gained 2O 5Content be 98.8%, the content of Calucium Silicate powder is 98.3%.
Embodiment 3:
The alkali lye that reactor is returned in circulation adds 6% NaNO through heat temperature raising to 250 ℃ 3, NaOH+NaNO 3Inferior fused salt mass concentration is 75%.350 mesh sieves will be crossed behind the bone coal ball milling 12h, again at 850 ℃ of following oxidizing roasting 1h, by alkali ore deposit mass ratio is 3: 1, under agitation the stone coal powder of handling well is joined in the reactor, complete hybrid reaction is 1.5 hours under 250 ℃, obtain degradation production, the dilute with water degradation production, dilution back NaOH concentration is 746g/L, temperature is 110 ℃, separate alkali lye and the solid phase that contains vanadic acid sodium, alkali lye returns inferior fused salt decomposition step through dehydration by evaporation, contains the solid phase water extraction of vanadic acid sodium, leaching liquid contains NaOH 138g/L, temperature is 100 ℃, and behind the leaching 30min, filtered while hot obtains containing the solution and the iron magnesium calcium slag precipitation of vanadic acid sodium and water glass.Add nitric acid and make the pH value of sodium vanadate solution transfer to 9, add ammonium chloride, obtain the solution that ammonium meta-vanadate precipitates and contain water glass, contain in the solution of water glass and add Ca (OH) 2, obtaining precipitated calcium silicate and the solution that contains NaOH, precipitated calcium silicate can be used as the raw material for preparing white carbon black, after the solution of NaOH carries out evaporation concentration, returns inferior fused salt decomposition step, and the ammonium meta-vanadate precipitation is carried out the high-temperature calcination decomposition and is obtained V 2O 5Product can be used to prepare the intermediate of vanadium product.The total yield of vanadium is 78%, the V of gained 2O 5Content be 98.5%, the content of Calucium Silicate powder is 98.2%.

Claims (7)

1. a method for cleaning and converting stone coal is characterized in that, may further comprise the steps:
(1) bone coal is advanced planetary high-energy ball milling and be placed on oxidizing roasting in the retort furnace, the bone coal after the oxidizing roasting is at NaOH+NaNO 3Decompose NaOH+NaNO in the inferior molten salt solution 3Mass concentration is 50～75%, and temperature is 150～250 ℃, and the resolving time is 1.5-3h, NaOH+NaNO 3With the alkali ore deposit mass ratio of bone coal be 3: 1～6: 1, NaNO 3At NaOH+NaNO 3Mass ratio in the inferior molten salt solution is 2%～6%;
(2) use H 2O or dilute NaOH solution dilution bone coal are at NaOH+NaNO 3Degradation production in the inferior molten salt solution obtains NaOH diluent and the solid phase that contains vanadic acid sodium and water glass;
(3) will contain the solid product H of vanadic acid sodium and water glass 2O heats leaching; Add the nitre acid for adjusting pH value in the leaching liquid that obtains to 8-9, add ammonium chloride then, obtain the solution that ammonium meta-vanadate precipitates and contain water glass;
(4) the ammonium meta-vanadate precipitation that step (3) is obtained is carried out the high-temperature calcination decomposition and is obtained V 2O 5Product; Add Ca (OH) in the solution that contains water glass that step (3) is obtained 2, obtaining precipitated calcium silicate and the solution that contains NaOH, precipitated calcium silicate is as the raw material of preparation white carbon black.
2. method for cleaning and converting stone coal according to claim 1 is characterized in that, the ball milling time is 16-36h in the described step (1), and the stone coal powder behind the ball milling is crossed 350 mesh standard sieves.
3. method for cleaning and converting stone coal according to claim 1 is characterized in that, described oxidizing roasting temperature is 800～900 ℃, and roasting time is 1-5h.
4. method for cleaning and converting stone coal according to claim 1 is characterized in that, the NaOH diluent that obtains in the described step (2) returns the inferior molten salt solution decomposition step of step (1).
5. method for cleaning and converting stone coal according to claim 1 is characterized in that, described step is used H in (2) 2O or dilute NaOH solution be diluted in temperature be under 20 ℃～110 ℃ the condition dilution bone coal at NaOH+NaNO 3Degradation production in the inferior molten salt solution, the time is 0.5-1 hour, obtaining concentration is the NaOH diluent of 550～750g/L and the solid phase of water glass.
6. method for cleaning and converting stone coal according to claim 1 is characterized in that, contains the solid product H of vanadic acid sodium and water glass in the described step (3) 2O heating leaching temperature is 60～100 ℃, and NaOH concentration is 60～150g/L in the leaching liquid.
7. method for cleaning and converting stone coal according to claim 1 is characterized in that, after the solution that contains NaOH that obtains in the described step (4) carries out evaporation concentration, returns the inferior fused salt decomposition step of step (1).
CN201010203166A 2010-06-18 2010-06-18 Method for cleaning and converting stone coal Pending CN101845549A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102226237A (en) * 2011-05-12 2011-10-26 杨暖 Method for extracting ammonium metavanadate, silica white and coal powder from vanadium-containing coal gangue
CN102534267A (en) * 2012-02-06 2012-07-04 四川省达州钢铁集团有限责任公司 Vanadium extracting method
CN102732739A (en) * 2012-06-08 2012-10-17 武汉理工大学 Method for extracting V2O5 from vanadium-containing shale by using chlorination evaporation
CN105152205A (en) * 2015-09-22 2015-12-16 中国华电工程(集团)有限公司 Method and device for recycling Ti and V from waste flue gas denitrification catalyst
CN108149015A (en) * 2018-01-15 2018-06-12 东北大学 A kind of method of valuable constituent element in oxygen-enriched Selectively leaching extraction vanadium titano-magnetite
CN108300874A (en) * 2018-01-15 2018-07-20 东北大学 A kind of method of high titanium slag Selectively leaching upgrading
CN108300875A (en) * 2018-01-15 2018-07-20 东北大学 A kind of oxygen-enriched Selectively leaching ilmenite concentrate prepares high purity Ti O2Method

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CN101693947A (en) * 2009-10-22 2010-04-14 湖南大学 Additive and method for extracting vanadium by roasting stone coal ores, and preparation method thereof
CN101705377A (en) * 2009-11-24 2010-05-12 锦州金业化工冶金技术咨询有限公司 Method for extracting vanadium from stone coal by wet-process enrichment and pyrogenic-process conversion

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Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102226237A (en) * 2011-05-12 2011-10-26 杨暖 Method for extracting ammonium metavanadate, silica white and coal powder from vanadium-containing coal gangue
CN102534267A (en) * 2012-02-06 2012-07-04 四川省达州钢铁集团有限责任公司 Vanadium extracting method
CN102732739A (en) * 2012-06-08 2012-10-17 武汉理工大学 Method for extracting V2O5 from vanadium-containing shale by using chlorination evaporation
CN102732739B (en) * 2012-06-08 2013-09-18 武汉理工大学 Method for extracting V2O5 from vanadium-containing shale by using chlorination evaporation
CN105152205A (en) * 2015-09-22 2015-12-16 中国华电工程(集团)有限公司 Method and device for recycling Ti and V from waste flue gas denitrification catalyst
CN108149015A (en) * 2018-01-15 2018-06-12 东北大学 A kind of method of valuable constituent element in oxygen-enriched Selectively leaching extraction vanadium titano-magnetite
CN108300874A (en) * 2018-01-15 2018-07-20 东北大学 A kind of method of high titanium slag Selectively leaching upgrading
CN108300875A (en) * 2018-01-15 2018-07-20 东北大学 A kind of oxygen-enriched Selectively leaching ilmenite concentrate prepares high purity Ti O2Method
WO2019137544A1 (en) * 2018-01-15 2019-07-18 东北大学 Method for extracting valent component in vanadium titanium magnetite by means of oxygen-rich selective leaching

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