CN101913633A - Extraction technology of alumina and potassium sulfate from alunite by using hot-pressing leaching process - Google Patents
Extraction technology of alumina and potassium sulfate from alunite by using hot-pressing leaching process Download PDFInfo
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Abstract
The invention discloses an extraction technology of alumina and potassium sulfate from alunite by using a hot-pressing leaching process, comprising the following steps: mixing the alunite with a potassium hydroxide solution to prepare pulp; transferring the pulp into a hot-pressing system, carrying out hot-pressing leaching at 100-300 DEG C, cooling the obtained leaching solution, and carrying out solid-liquid separation; transferring the leaching solution after solid-liquid separation into a desiliconization system for desiliconizing at 80-200 DEG C, and filtering and separating to obtain a desiliconized extracting solution and silica slag; transferring the desiliconized extracting solution into an acid regulating system, keeping adding sulfuric acid to the acid regulating system while stirring until white precipitate in the desiliconized extracting solution is not generated any more and disappears, and then filtering and separating out a solution mainly containing the potassium sulfate; transferring the solution mainly containing the potassium sulfate into a crystallization system, evaporating and crystallizing the solution mainly containing the potassium sulfate in the crystallization system, and filtering and separating to obtain potassium sulfate crystal. The extraction technology of the invention has lower production cost and relatively short process flow.
Description
Technical field
The present invention relates to the alunite treatment process, in particular to utilizing the hot pressing extract technology to extract aluminum oxide and vitriolate of tartar from alunite.
Background technology
Alunite is meant the Sulfates rock alum.At present, domestic and international exploitation great majority to alunite are conceived to extract aluminium, potassium, sulphur.Mainly contain reduction heat solution, solvay soda process, card human relations nit acid system, UG method, decomposition for ammonium sulfate, thermal decomposition method etc. than typical method.In addition, also have Repone K sintering process, sulfurization roasting method, sour ammonia process, aquation method etc.
The reduction heat solution is by reductive method after the alunite roasting.At first, from Tai-Ace S 150, get rid of SO
3, and then handle the reductive alumstone ore with alkali lye.This method exists environmental pollution serious, and energy consumption is bigger, and production cost is higher, technical process complexity, shortcoming such as aluminium, the potassium rate of recovery are lower.
Solvay soda process is that ammonium sulfate, vitriolate of tartar, sodium sulfate enter solution, all aluminum oxide are stayed in the slag with the dehydration alunite of ammonia solution leaching through 520 ℃ of following roastings, and slag separates back alkaline solution stripping with sulfate liquor.Dissolution fluid through desiliconization, after separating aluminium hydroxide+again through calcination get aluminum oxide, filtrate is processed into potassium nitrogen mixed fertilizer.This method exists silicon to separate comparatively difficulty, and solid-liquid separation is difficult, and yield is lower, deficiencies such as cost up; In addition, this method needs a large amount of ammonia, and can only obtain potassium nitrogen mixed fertilizer.
Card human relations nit acid system is with the dehydration alunite after the sulfuric acid to leach roasting, separates behind the insoluble slag Fe in the solution
3+Be reduced into Fe
2+And carry out the alum crystallization.Alum dissolving is sent to is hydrolyzed into alkali formula alum well in the potheater and reclaims diluted acid.Alkali formula alum is emitted sulfur-containing smoke gas through the aluminum oxide well that is sintered into sulfur acid potassium.Flue gas reclaims system sulfuric acid, and aluminum oxide is through the washing and recycling vitriolate of tartar.This method corrosion resistant problem of equipment material aborning never obtains fine solution, deironing difficulty in the aluminum salt solution. and the large usage quantity of acid and acid group are difficult for reclaiming.
The UG method is that the dehydration alunite is pulverized, and logical ammonia treatment in water mixes fertilizer with extracting potassium ammonia after the Tai-Ace S 150 decomposition fully.Salic slag feeds sulfur dioxide treatment, obtains alkali formula aluminium sulfite solution and the slag that contains residual aluminum oxide.The latter separates with vitriolization with leach liquor and becomes alum liquor.With above-mentioned two kinds contain aluminum solutions merge reaction and the basic aluminium sulphate precipitation is made aluminium salt raw material or further is processed into metallurgical-grade aluminum oxide.This method can not get potassium product, and the technical process complexity, and it is higher to produce the aluminum oxide cost, and environmental pollution is serious.
Decomposition for ammonium sulfate carries out the solid phase thermolysis with the alunite of ammonium sulfate and dehydration, leaches after the slagging-off filtrate Fe
3+Be reduced into Fe
2+And carry out the alum crystallization.Use in the ammonia then and potassium ammonium mixing alum, make aluminium salt wherein be converted into Al (OH)
3, the Al that dissolution fluid leaches (OH)
3Through calcine aluminum oxide, filtrate gets potassium-nitrogen fertilizer through evaporative crystallization.It is reasonable inadequately that this method exists energy consumption to use, and the rate of decomposition that gas-solid is decomposed is not high, and the mother liquor after the crystallization deironing is difficult to recycle, production metallurgy level Al
2O
3Problem such as be difficult to break even economically.
Thermal decomposition method adopts high temperature fast dewatering disaggregating treatment alumstone ore, and Tai-Ace S 150 is decomposed, and trioxygen-containing sulphur flue gas is used for making sulfuric acid, grog water extraction vitriolate of tartar, after the filtration, solid phase through deironing, mend aluminium, join alkali and synthesize the 4A zeolite.It is unfriendly to environment that the main weak point that this method exists is to produce harmful smoke, and potassium, aluminium utilization ratio are not high.
From the above, problem such as the treatment process cost height of present alumstone ore, seriously polluted, utilization ratio.
Summary of the invention
Main purpose of the present invention is to provide a kind of alunite treatment process, one of to address the above problem at least.
According to an aspect of the present invention, utilize the hot pressing extract technology to may further comprise the steps: alunite and potassium hydroxide solution are modulated into ore pulp from alunite extraction aluminum oxide and vitriolate of tartar; Described ore pulp is sent into hot-pressing system, under 100 ℃～300 ℃ conditions, carry out hot pressing and leach, dissolution fluid is cooled off, carry out solid-liquid separation; Send the desiliconization system with the leach liquor after the solid-liquid separation, carry out desiliconization under 80～200 ℃ of conditions, filtering separation obtains desiliconization seminal fluid and white residue; Described desiliconization seminal fluid is sent into the acid adjustment system, under agitation condition, in described acid adjustment system, add sulfuric acid, add acid when white precipitate can not produce and disappear in described desiliconization seminal fluid and stop, carrying out filtering separation; The solution that filters to isolate based on vitriolate of tartar send crystal system, in described crystal system described solution based on vitriolate of tartar is carried out evaporative crystallization, obtains potassium sulfate crystal after the filtering separation.
Preferably, after the desiliconization seminal fluid in the acid adjustment system stops to add sulfuric acid and carries out filtering separation, sedimentary aluminium hydroxide is washed behind certain number of times the calcining of carrying out aluminium hydroxide under 800 ℃～1300 ℃ of temperature, obtain metallurgical grade product aluminum oxide.
Preferably, with after the hot wash 3 to 7 times, will send hot-pressing system to be used for modulating ore pulp in described sedimentary aluminium hydroxide with washing lotion.
Preferably, after filtering separation obtains potassium sulfate crystal, with obtaining vitriolate of tartar after a certain amount of hot wash.
Preferably, with the potassium sulfate crystal washing of a certain amount of hot water after to filtering separation 1 to 3 time, washing lotion after the washing and crystallization concentrated solution return described acid adjustment system.
Preferably, the concentration mass percent of described ore pulp is 1%-60%.
Preferably, the concentration of potassium hydroxide mass percent of described ore pulp is 1%-60%.
Preferably, alunite and potassium hydroxide solution are modulated into described ore pulp, wherein, described potassium hydroxide solution concentration mass percent is more than 1%.
Preferably, described ore pulp is sent into hot-pressing system, under 100 ℃～300 ℃ conditions, carry out hot pressing and leached 1 minute to 300 minutes.
Preferably, the described leach liquor after the solid-liquid separation is sent into the desiliconization system, under 80～200 ℃ of conditions, carry out desiliconization in 1 minute to 300 minutes.
By the present invention, adopt the hot pressing extract technology to handle alunite, solved roasting energy consumption height, technical process complexity in the prior art, operational difficulty, problem such as environmental pollution is serious one of at least.And then reached and generated that this is lower, technical process is short relatively, eco-friendly effect.
Description of drawings
Accompanying drawing described herein is used to provide further understanding of the present invention, constitutes the application's a part, and illustrative examples of the present invention and explanation thereof are used to explain the present invention, do not constitute improper qualification of the present invention.In the accompanying drawings:
Fig. 1 is that the heat pressing process that utilizes according to the embodiment of the invention extracts aluminum oxide and vitriolate of tartar schema from alunite.
Embodiment
The hot pressing extract technology is used for bauxite the earliest and extracts aluminum oxide, and the hot pressing leaching-out technique is in the application of succeeding of uranium ore, nickel boring the ground, tungsten aluminium ore, copper nickel, zink sulphide and difficult-treating gold mine subsequently.But, openly do not adopt hot-pressing technique to handle the technical scheme of alumstone ore so far in the prior art.To adopt hot pressing to leach in following examples handles alunite.
Need to prove, all are mass percents at the per-cent described in following examples.
Embodiment one
It is lower that present embodiment has proposed a kind of production cost, and technical process is short, environmental friendliness, and easily the hot pressing extract technology of industrializing implementation is handled the method that alunite is produced aluminum oxide and vitriolate of tartar.This method has overcome alunite and has handled roasting energy consumption height, technical process complexity in the prior art, operational difficulty, shortcoming such as environmental pollution is serious.
In the present embodiment alunite being carried out hot pressing with potassium hydroxide solution leaches.Leaching slurry separates the back after filtration and goes out aluminium hydroxide with sulfuric acid precipitation, and the aluminium hydroxide that filters to isolate obtains the finished product aluminum oxide through calcining, and mother liquor obtains the finished product vitriolate of tartar through evaporating, concentrating and crystallizing.Comprise the steps:
The first step: alunite, potassium hydroxide solution are added in the surge tank, and being modulated into concentration of potassium hydroxide is 1%～40%, and pulp density is 1%～60% qualified ore pulp.
Preferably, in this step, alunite and concentration can be modulated into the qualified ore pulp of pulp density position 1%～60% greater than 1% potassium hydroxide solution.
Second one: send hot-pressing system with qualified slurry, under 100 ℃～300 ℃ conditions, carry out hot pressing leach (for example, the back of 1min～300min) to dissolution fluid cool off, solid-liquid separation.
The 3rd step: separation solution is 80 ℃～200 ℃ of temperature, time (for example, 1min～300min) carry out desiliconization under the condition.
The 4th step: the desiliconization seminal fluid send the acid adjustment groove, slowly adds in groove under agitation condition till sulfuric acid white precipitate in seminal fluid no longer produces and disappear, and the aluminium in the seminal fluid is separated out with the form precipitation of aluminium hydroxide, filters and realizes that aluminium potassium separates.
The 5th step: aluminium hydroxide is sent back in the rotary kiln under 800 ℃～1300 ℃ of temperature and is obtained the finished product aluminum oxide in calcining.
The 6th step: send based on the solution of vitriolate of tartar and to carry out evaporating, concentrating and crystallizing in the crystallizer, the agricultural potassium sulfate product that obtains complying with the national standard requirements.
Following examples two to embodiment four combine the foregoing description one and preferred embodiment, Fig. 1 is that the heat pressing process that utilizes according to the embodiment of the invention extracts aluminum oxide and vitriolate of tartar schema from alunite, wherein, 1 is that alunite, 2 is that potassium hydroxide solution, 3 is that water, 4 is that desiliconization seminal fluid, 6 is that aluminium hydroxide, 7 is that aluminum oxide, 8 is a vitriolate of tartar for soaking slag, 5.Below the technical process adopted of each embodiment may further comprise the steps:
The first step: the qualified ore pulp that at first alunite and concentration is modulated into pulp density position 1%～60% greater than 1% potassium hydroxide solution; Send hot-pressing system with qualified slurry then, carrying out after 1min～300min is leached in hot pressing dissolution fluid being cooled off, realize solid-liquid separation under 100 ℃～300 ℃ conditions.
Second step: the hot pressing leach liquor send the desiliconization system, carries out desiliconization 1min～300min under 80～200 ℃ of conditions, and filtering separation obtains desiliconization seminal fluid and white residue then.The white residue that exists with the silicate form adds the desiliconization system as the desiliconization crystal seed, and seminal fluid send the acid adjustment groove to handle.
The 3rd step: under suitable agitation condition, slowly in the acid adjustment groove, add sulfuric acid, add acid when white precipitate can not produce and disappear in seminal fluid and stop.At this moment, the aluminium in the seminal fluid is separated out with the form precipitation of aluminium hydroxide.The mother liquor that filters to isolate based on vitriolate of tartar send crystal system, and precipitated aluminium hydroxide is calcined with sending rotary kiln back to after the hot wash 3～7 times, and washing lotion send hot-pressing system to be used for sizing mixing.
The 4th step: under 800 ℃～1300 ℃ of temperature, carry out the calcining of aluminium hydroxide, obtain metallurgical grade product aluminum oxide.
The 5th step: in crystal system, the solution based on vitriolate of tartar is carried out evaporative crystallization.The potassium sulfate crystal of filtering separation gained with a certain amount of hot wash 1～3 time after, obtain qualified agricultural potassium sulfate product.Washing lotion and crystallization concentrated solution return the utilization of acid adjustment systemic circulation.
Below embodiment two to embodiment four is described respectively, simultaneously,, also enumerated a Comparative Examples for following each embodiment better is described.
Embodiment two
The potassium hydroxide solution of getting alunite 96.4g and 5% carries out hot pressing and leaches under the condition of liquid-solid ratio 3,140 ℃ of temperature, time 45min, obtain containing aluminium after the filtration realization solid-liquid separation and contain the potassium mother liquor.The solubility rate of aluminum oxide and potassium oxide is respectively 78.25% and 90.69% in this process.
After containing aluminium, potassium mother liquor and carrying out desiliconization, obtain siliceous modulus and add sulfuric acid precipitation aluminium hydroxide (the sulfuric acid add-on will make the aluminium hydroxide that is precipitated out not return molten), with the hot wash of 1.5 times of filtrate volumes, filter also that the aluminium hydroxide of dry gained obtains stair oxidation aluminium through 1100 ℃ of calcinings greater than 300 desiliconization seminal fluid.Washing lotion is sent the hot-pressing system recycle.
Solution based on vitriolate of tartar carries out evaporative crystallization under 90 ℃ of conditions.The potassium sulfate crystal of filtering separation gained obtains potassium product with after a spot of hot wash 1 time, and washing lotion and crystalline mother solution return the recycle of sulfuric acid precipitation aluminium hydroxide.Each technical indicator sees the following form 1.
Embodiment three
The potassium hydroxide solution of getting alunite 130g and 7% carries out hot pressing and leaches under the condition of liquid-solid ratio 3,150 ℃ of temperature, time 1h, obtain containing aluminium after the filtration realization solid-liquid separation and contain the potassium mother liquor.
Containing aluminium, potassium mother liquor is undertaken obtaining potassium product behind desiliconization, the heavy aluminium hydroxide of acid and the heavy aluminium mother liquid evaporation condensing crystal by the condition of embodiment 1.Each technical indicator sees the following form 1.
Embodiment four
The potassium hydroxide solution of getting alunite 130g and 10% carries out hot pressing and leaches under the condition of liquid-solid ratio 5,220 ℃ of temperature, time 1h, obtain containing aluminium after the filtration realization solid-liquid separation and contain the potassium mother liquor.
Contain and obtain potassium product after aluminium, potassium mother liquor are undertaken behind desiliconization, the heavy aluminium hydroxide of acid and the heavy aluminium mother liquid evaporation condensing crystal by the condition of embodiment 1.Each technical indicator sees the following form 1.
Comparative Examples
Get the first roasting 2h postcooling that under 580 ℃ of conditions, dewaters of alunite 343g, extraordinarily go into the S mixing by 1.5 of theory metering then and carry out reducing roasting 1.5h at 600 ℃, the gained grog is at L/S=4, leach 48h and 3.5h under room temperature and the 90 ℃ of conditions after, potassium oxide, leaching rate of alumina see Table 1.
Each embodiment of table 1 and Comparative Examples technical indicator gather
In sum, the foregoing description carries out the hot pressing leaching by alunite with potassium hydroxide solution.Have the following advantages:
(1) the leach liquor foreign matter content is lower, and aluminium potassium is easily separated, is that solution is produced aluminum oxide, vitriolate of tartar is created very strong condition, and vitriolate of tartar, alumina recovery rate height;
(2) do not produce smoke pollutions such as sulfurous gas, environmental friendliness;
(3) technical process is short, and easy to operate, comprehensive benefit is good, have a extensive future, and easy industrializing implementation.
The above is the preferred embodiments of the present invention only, is not limited to the present invention, and for a person skilled in the art, the present invention can have various changes and variation.Within the spirit and principles in the present invention all, any modification of being done, be equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. utilize the hot pressing extract technology to extract aluminum oxide and vitriolate of tartar, it is characterized in that, may further comprise the steps from alunite:
Alunite and potassium hydroxide solution are modulated into ore pulp;
Described ore pulp is sent into hot-pressing system, under 100 ℃～300 ℃ conditions, carry out hot pressing and leach, dissolution fluid is cooled off, carry out solid-liquid separation;
Send the desiliconization system with the leach liquor after the solid-liquid separation, carry out desiliconization under 80～200 ℃ of conditions, filtering separation obtains desiliconization seminal fluid and white residue;
Described desiliconization seminal fluid is sent into the acid adjustment system, under agitation condition, in described acid adjustment system, add sulfuric acid, add acid when white precipitate can not produce and disappear in described desiliconization seminal fluid and stop, carrying out filtering separation;
The solution that filters to isolate based on vitriolate of tartar send crystal system, in described crystal system described solution based on vitriolate of tartar is carried out evaporative crystallization, obtains potassium sulfate crystal after the filtering separation.
2. technology according to claim 1, it is characterized in that, after desiliconization seminal fluid in the acid adjustment system stops to add sulfuric acid and carries out filtering separation, sedimentary aluminium hydroxide is washed behind certain number of times the calcining of carrying out aluminium hydroxide under 800 ℃～1300 ℃ of temperature, obtain metallurgical grade product aluminum oxide.
3. technology according to claim 2 is characterized in that, with after the hot wash 3 to 7 times, will send hot-pressing system to be used for modulating ore pulp with washing lotion in described sedimentary aluminium hydroxide.
4. technology according to claim 1 is characterized in that, after filtering separation obtains potassium sulfate crystal, with obtaining vitriolate of tartar after a certain amount of hot wash.
5. technology according to claim 4 is characterized in that, with the potassium sulfate crystal washing of a certain amount of hot water after to filtering separation 1 to 3 time, washing lotion after the washing and crystallization concentrated solution return described acid adjustment system.
6. technology according to claim 1 is characterized in that, the concentration mass percent of described ore pulp is 1%-60%.
7. technology according to claim 6 is characterized in that, the concentration of potassium hydroxide mass percent of described ore pulp is 1%-60%.
8. according to claim 6 or 7 described technologies, it is characterized in that, alunite and potassium hydroxide solution are modulated into described ore pulp, wherein, described potassium hydroxide solution concentration mass percent is more than 1%.
9. technology according to claim 1 is characterized in that, described ore pulp is sent into hot-pressing system, carries out hot pressing and leached 1 minute to 300 minutes under 100 ℃～300 ℃ conditions.
10. technology according to claim 1 is characterized in that, the described leach liquor after the solid-liquid separation is sent into the desiliconization system, carries out desiliconization in 1 minute to 300 minutes under 80～200 ℃ of conditions.
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| CN201010224456.8A CN101913633B (en) | 2010-07-07 | 2010-07-07 | Extraction technology of alumina and potassium sulfate from alunite by using hot-pressing leaching process |
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Cited By (5)
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| CN102491806A (en) * | 2011-11-14 | 2012-06-13 | 山东瑞福锂业有限公司 | Process for preparing nitrogen-potassium compound fertilizer and aluminum hydroxide from mixed alum |
| CN102659156A (en) * | 2012-04-19 | 2012-09-12 | 中国科学院过程工程研究所 | Method for extracting aluminum potassium product from associated alum quarry tailings |
| CN102910660A (en) * | 2012-11-06 | 2013-02-06 | 傅培鑫 | Method for producing alum by utilizing alunite |
| CN103011206A (en) * | 2012-12-19 | 2013-04-03 | 紫金矿业集团股份有限公司 | Method utilizing alunite in flotation tailing to produce potassium sulfate and auxiliary products thereof |
| CN105217658A (en) * | 2015-10-29 | 2016-01-06 | 福州大学 | A kind of method of alunite direct weighting acid leaching extraction potassium aluminium |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102491806A (en) * | 2011-11-14 | 2012-06-13 | 山东瑞福锂业有限公司 | Process for preparing nitrogen-potassium compound fertilizer and aluminum hydroxide from mixed alum |
| CN102659156A (en) * | 2012-04-19 | 2012-09-12 | 中国科学院过程工程研究所 | Method for extracting aluminum potassium product from associated alum quarry tailings |
| CN102910660A (en) * | 2012-11-06 | 2013-02-06 | 傅培鑫 | Method for producing alum by utilizing alunite |
| CN102910660B (en) * | 2012-11-06 | 2014-06-18 | 傅培鑫 | Method for producing alum by utilizing alunite |
| CN103011206A (en) * | 2012-12-19 | 2013-04-03 | 紫金矿业集团股份有限公司 | Method utilizing alunite in flotation tailing to produce potassium sulfate and auxiliary products thereof |
| CN105217658A (en) * | 2015-10-29 | 2016-01-06 | 福州大学 | A kind of method of alunite direct weighting acid leaching extraction potassium aluminium |
| CN105217658B (en) * | 2015-10-29 | 2016-09-07 | 福州大学 | A kind of method of alunite direct weighting acid leaching extraction potassium aluminium |
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