CN102910660B - Method for producing alum by utilizing alunite - Google Patents
Method for producing alum by utilizing alunite Download PDFInfo
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- CN102910660B CN102910660B CN201210437753.XA CN201210437753A CN102910660B CN 102910660 B CN102910660 B CN 102910660B CN 201210437753 A CN201210437753 A CN 201210437753A CN 102910660 B CN102910660 B CN 102910660B
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- 229940037003 alum Drugs 0.000 title claims abstract description 56
- 229910052934 alunite Inorganic materials 0.000 title claims abstract description 34
- 239000010424 alunite Substances 0.000 title claims abstract description 34
- KPZTWMNLAFDTGF-UHFFFAOYSA-D trialuminum;potassium;hexahydroxide;disulfate Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Al+3].[Al+3].[Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O KPZTWMNLAFDTGF-UHFFFAOYSA-D 0.000 title claims abstract description 34
- 238000004519 manufacturing process Methods 0.000 title abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000002386 leaching Methods 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 21
- 235000011126 aluminium potassium sulphate Nutrition 0.000 claims abstract description 15
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims abstract description 15
- 229910052939 potassium sulfate Inorganic materials 0.000 claims abstract description 15
- 235000011151 potassium sulphates Nutrition 0.000 claims abstract description 15
- GRLPQNLYRHEGIJ-UHFFFAOYSA-J potassium aluminium sulfate Chemical compound [Al+3].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRLPQNLYRHEGIJ-UHFFFAOYSA-J 0.000 claims abstract description 13
- 229940050271 potassium alum Drugs 0.000 claims abstract description 12
- 238000002425 crystallisation Methods 0.000 claims abstract description 11
- 230000008025 crystallization Effects 0.000 claims abstract description 11
- 238000000926 separation method Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000006297 dehydration reaction Methods 0.000 claims description 25
- 230000018044 dehydration Effects 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 15
- 238000001816 cooling Methods 0.000 claims description 13
- 235000011149 sulphuric acid Nutrition 0.000 claims description 11
- 239000001117 sulphuric acid Substances 0.000 claims description 11
- 238000010276 construction Methods 0.000 claims description 7
- 238000000354 decomposition reaction Methods 0.000 claims description 7
- 238000004090 dissolution Methods 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 230000008020 evaporation Effects 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 5
- 239000010413 mother solution Substances 0.000 claims description 5
- 238000005188 flotation Methods 0.000 claims description 4
- 238000009413 insulation Methods 0.000 claims description 4
- 239000006210 lotion Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- 229910052782 aluminium Inorganic materials 0.000 claims description 3
- 239000004411 aluminium Substances 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 3
- 238000006062 fragmentation reaction Methods 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 10
- 239000003245 coal Substances 0.000 abstract description 7
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 4
- 239000011707 mineral Substances 0.000 abstract description 4
- 239000002912 waste gas Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000007670 refining Methods 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 4
- 239000001120 potassium sulphate Substances 0.000 abstract 2
- 238000007654 immersion Methods 0.000 abstract 1
- 239000012452 mother liquor Substances 0.000 abstract 1
- 230000008569 process Effects 0.000 description 8
- 238000006722 reduction reaction Methods 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- -1 weight ratio) is 3-8 Chemical compound 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 2
- 229910001649 dickite Inorganic materials 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 1
- 239000002956 ash Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- VGIBGUSAECPPNB-UHFFFAOYSA-L nonaaluminum;magnesium;tripotassium;1,3-dioxido-2,4,5-trioxa-1,3-disilabicyclo[1.1.1]pentane;iron(2+);oxygen(2-);fluoride;hydroxide Chemical class [OH-].[O-2].[O-2].[O-2].[O-2].[O-2].[F-].[Mg+2].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[Al+3].[K+].[K+].[K+].[Fe+2].O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2.O1[Si]2([O-])O[Si]1([O-])O2 VGIBGUSAECPPNB-UHFFFAOYSA-L 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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Abstract
The invention relates to a method for producing alum by utilizing alunite, comprising the steps that alunite mineral powder is selected and used, the mineral powder is dehydrated by microwave roasting, sulfuric acid solution is leached and dissolved out, the filtering separation is carried out, the leaching agent is evaporated and concentrated, and the leaching agent is cooled and alum is crystallized. Potassium sulphate is added to the leaching agent, and potassium alum is completely produced; potassium sulphate is not added to the leaching agent, potassium alum is produced, and aluminum sulfate is co-produced; and crystallization mother liquor is recycled. Compared with the existing alum refining technology adopting 'water immersion method' and a vertical coal kiln, the method for producing alum by utilizing alunite has the beneficial effects that the utilization rate of resources is improved, the yield of alum is increased, the production cycle of the alum is shortened, energy sources are saved, the production cost is reduced, waste residues and waste gases are reduced, and the environment is protected.
Description
Technical field
The invention belongs to alum production field, relate in particular to a kind of method of utilizing alunite to produce alum.
Background technology
Alunite is non-water-soluble potassium aluminium sulfate mineral, will be to ore roasting (dehydration, pyrolysis or reduction pyrolysis), its ore structure is changed, improve chemical reactivity, then carry out wet processes, i.e. ore roasting and grog leaching are the basic working methods of the various processing technology routines of alunite comprehensive utilization.
Dehydration reaction 2KA1
3(S0
4)
2(OH)
6=K
2sO
4a1
2(S0
4)
3+ 2A1
20
3+ 6H
2o (1)
Pyrolytic reaction K
2sO
4a1
2(S0
4)
3=K
2sO
4+ A1
2o
3+ 3S0
3(2)
Reduction reaction K
2sO
4a1
2(S0
4)
3+ 3CO=K
2sO
4+ A1
2o
3+ 3S0
2+ 3CO
2(3)
Utilize alunite to produce the method for alum, ore roasting dewatering process is gordian technique.
1 mol rock alum K
2sO
4a1
2(S0
4)
34A1 (0H)
3dehydration reaction obtains 1 mol alumen exsiccatum K
2sO
4a1
2(SO
4)
3.And the other 2 mol A1 that dehydration reaction produces
20
3convert Tai-Ace S 150 to by sulfuric acid process, add potassium sulfate to generate potassium alum.Otherwise 2 mol A1
20
3stay in leached mud.
Existing " water seaoning " produces the method for alum, and master operation is for selecting alunite lump ore, ore roasting, water-sprinkling weathering, the stripping of heating, alum crystallization.Ore roasting adopts the roasting of vertical coal kiln, ore grade 50% left and right, and lump ore 5 one 15cm, coal ore is than 1:20,550-700 DEG C of maturing temperatures, roasting time 3-4 days.There is following subject matter in the method:
(1), ore resource utilization ratio is low.Ore total loss rate is 49.16%.
(2), alum yields poorly.Alunite ore grade is 51.79%, produces 1 ton of alum with 3.32 tons of ores, and it is 30.12% that ore goes out alum rate, and the ore grade rate of recovery is 50.84 %.
(3) waste residue waste gas is many.Produce 1 ton of alum, produce 0.15 ton, ashes, 0.82 ton, alum slurry, 1.82 tons of alum slags, alum cigarette 0.18 ten thousand m
3.
(4) the alum production cycle is long, energy consumption is high.100 1 120 days alum production cycles, wherein, ore roasting 3 one 4 days, water-sprinkling weathering 80 1 100 days, alum crystallization 15 1 18 days.Producing 1 ton of alum energy consumption is coal 451kg, electric 24lKwh.
Produce the major cause of the problems referred to above: the one, sinter process unreasonable (dehydration rate too low " half-cooked ", rate of decomposition higher " burning ", A1
2o
3phase transformation " is burnt to death "), A1 in ore
2o
3be not fully utilized, solubility rate is on the low side.The 2nd, hydrolysis reaction produces insolubles, sneaks in alum slurry, alum slag and causes A1
2o
3loss.The 3rd, K in leach liquor
2sO
4/ A1
2(SO
4)
3ratio imbalance, affects alum percent crystallization in massecuite.
Summary of the invention
Technical problem to be solved by this invention is: a kind of method of utilizing alunite breeze to produce alum is provided; the method can shorten the alum production cycle, improve resource utilization, reduce production costs, energy-saving and emission-reduction, protection of the environment, and existing to overcome " water seaoning " produces the above-mentioned subject matter that the method for alum exists.
The technical solution adopted in the present invention is: adopt alunite breeze microwave calcining dehydration Production By Sulfuric Acid Process alum, specifically comprise following implementation step:
(1), select alunite breeze:
By alumstone ore fragmentation, levigate or flotation acquisition alunite breeze, ore grade >=45%, ore powder granularity 80-200 orders (0.175-0.074mm);
(2), breeze microwave calcining dehydration:
By microwave thermal construction equipment roasting dehydration for breeze, ore grog dehydration rate >=90 %, rate of decomposition≤5 %,
A1
2o
3solubility rate>=90%;
(3), sulphuric acid soln leaches stripping, filtering separation:
The alunite (grog) that will dewater leaches stripping with sulphuric acid soln, insulation is filtered, solid-liquid separation, leached mud hot wash, washing lotion is incorporated to leach liquor, wherein, liquid-solid ratio (sulphuric acid soln/dehydration alunite, weight ratio) is 3-8, and sulfuric acid (100%) consumption is theoretical amount 100-130%, leaching stripping temperature >=90 DEG C, leaching dissolution time >=0.5h;
(4) leach liquor evaporation concentration, the crystallization of cooling down alum:
By the leach liquor evaporation concentration of heating, the crystallization of cooling down alum, crystalline mother solution returns to leaching stripping, recycle; Former liquid temp >=80 DEG C of alum, alum original liquid concentration >=25 %, cooling termination temperature≤25 DEG C;
Wherein, add potassium sulfate in leach liquor, all generate potassium alum, potassium sulfate consumption is theoretical amount 100 one 120%; In leach liquor, do not add potassium sulfate, generate potassium alum co-producing sulfuric acid aluminium.
Preferred version is: in described step (1), ore grade is 50%-65%; In described step (2), the microwave frequency of microwave thermal construction equipment is 2450MHz, microwave irradiation time>=10min, and ore grog dehydration rate is 95 1 99 %, rate of decomposition is 2 one 5 %, A1
2o
3solubility rate is 90 one 95%; In described step (3), leaching stripping temperature is 90 1 100 DEG C, and leaching dissolution time is 0.5 1 3.0h; In described step (4), the former liquid temp of alum is 80-95 DEG C, and alum original liquid concentration is 25-28%, and cooling termination temperature is 15-25 DEG C.
Beneficial effect of the present invention: the present invention, with the comparison of existing " water seaoning " vertical coal kiln refining alum technology, has the following advantages:
The one, adopt microwave thermal construction equipment to replace vertical coal kiln to carry out alunite roasting dehydration, maturing temperature is even, it is controlled that temperature is adjustable, roasting time is short, the alum production cycle shortens to 3 one 5 days in 100 1 120 days from existing " water seaoning ", and can produce continuously, do not exist mineral dehydration rate too low " half-cooked, rate of decomposition is higher " burning ", A1
2o
3phase transformation " is burnt to death ", improves the utilization ratio of ore, increases alum output, and ore total loss rate is reduced to 29 % from 49 % of existing " water seaoning ", and the ore grade rate of recovery is brought up to more than 70% from existing " water seaoning " 50% left and right.And microwave thermal construction equipment and the comparison of existing vertical coal kiln, save the energy, reduces production costs, and reduces waste residue waste gas, protection of the environment.
The 2nd, the leaching medium of choose reasonable dehydration alunite (grog), adopts sulphuric acid soln leaching stripping to replace " water seaoning " to use water extraction stripping.
First the other 2 mol Al that, sulphuric acid soln leaching produces alunite dehydration reaction
2o
3convert Tai-Ace S 150 to, the Al in ore
2o
3be fully utilized, solubility rate is high.Specific as follows:
(1) sulfuric acid process, adds potassium sulfate in leach liquor, generate 3 mol potassium alums.
K?
2SO
4·A1
2?(SO
4）
3＋2A1
2O
3?+?6H
2SO
4?+2K
2SO
4?+?66H
2O?=?3K
2SO
4·A1
2?(SO
4)?
3·24H
2O
(2) sulfuric acid process, does not add potassium sulfate in leach liquor, generate 1 mol potassium alum coproduction 2 mol Tai-Ace S 150.
K?
2SO
4·A1
2?(SO
4）
3＋2A1
2O
3?+?6H
2SO
4?+54H
2O=?K
2SO
4·A1
2(SO
4)
3·24H
2O?+?2A1
2?(SO
4)
3·18H
2O
And (3) " water seaoning " generates 1 mol potassium alum, 2 mol A1
2o
3stay in leached mud.
K
2SO
4·A1
2?(SO
4）
3＋2A1
2O
3?+?24H
2O=?K
2SO
4·A1
2?(SO
4）
3·24H
2?O?+?2A1
2O
3
Secondly, " water seaoning " water-sprinkling weathering activity time is long, need 80-100 days, and sulfuric acid to leach dissolution time is only 0.5-3.0h, greatly shortens the production cycle.
Brief description of the drawings
Fig. 1 is the process flow diagram of an embodiment of the present invention.
Embodiment
Embodiment 1
The present embodiment embodiment comprises the steps:
(1), select alunite breeze:
By alumstone ore fragmentation, levigate or flotation acquisition alunite concentrate.Ore grade is 50-65%, and ore powder granularity is 80 1 200 orders (0.175 one 0.074mm).
(2), breeze microwave calcining dehydration:
By microwave thermal construction equipment roasting dehydration for breeze, microwave frequency is 2450MHz, and microwave output power is 1.0-5.0KW, and microwave irradiation time is 10 1 60min, and ore grog dehydration rate is 95-99 %, and rate of decomposition is 2-5 %, A1
2o
3solubility rate is 90-95 %.
(3), sulphuric acid soln leaches stripping, filtering separation:
The alunite (grog) that will dewater leaches stripping with sulphuric acid soln, insulation is filtered, solid-liquid separation, leached mud hot wash, washing lotion is incorporated to leach liquor, wherein, liquid-solid ratio (sulphuric acid soln/dehydration alunite, weight ratio) is 3-8, and sulfuric acid (100%) consumption is theoretical amount 100-130%, leaching stripping temperature is 90-100 DEG C, and leaching dissolution time is 0.5-3.0h.
(4), leach liquor evaporation concentration, the crystallization of cooling down alum:
By the leach liquor evaporation concentration of heating, the crystallization of cooling down alum, crystalline mother solution returns to leaching stripping, recycle, 80-95 DEG C of the former liquid temps of alum, alum original liquid concentration 25-28 %, 15-25 DEG C of cooling termination temperatures.
Wherein, add potassium sulfate in leach liquor, all generate potassium alum, potassium sulfate consumption is theoretical amount 100-120%.In leach liquor, do not add potassium sulfate, generate potassium alum co-producing sulfuric acid aluminium.
Embodiment 2
The present embodiment step is with embodiment 1.Select alunite concentrate (the alunite A1 in ore of flotation
2o
316.53%, dickite A1
2o
312.56 %, add up to A1
2o
329.09 %).Ore powder granularity 200 orders (0.074mm) left and right.100 grams of alunite breeze consumptions, breeze dewaters by microwave calcining, microwave irradiation time 30min.Sulfuric acid (98%) 40ml for dehydration alunite (grog), 500 grams of heating waters, the leaching stripping of heating, 100 DEG C of leaching stripping temperature, leaching dissolution time 2.0h.Insulation is filtered, solid-liquid separation.Leached mud hot wash, washing lotion is incorporated to leach liquor.In leach liquor, add sulfuric acid K42 gram, stirring and dissolving.The leach liquor evaporation concentration of heating, to alum original liquid concentration 26% left and right, the crystallization of cooling down alum, 20 DEG C of cooling termination temperatures, obtain 205 grams of potassium alums, crystalline mother solution recycle.
Embodiment 3
The present embodiment step and experiment condition are with embodiment 2.In leach liquor, do not add potassium sulfate, obtain 142 grams, potassium alum/Tai-Ace S 150, wherein 40 grams of potassium alums.Crystalline mother solution recycle.
Finally, it is also to be noted that, what more than exemplify is only specific embodiments of the invention.Obviously, the invention is not restricted to above embodiment, can also have many changes and variation.Those skilled in the art can directly derive or associate all any amendments from content disclosed by the invention, is equal to replacement, change and improve etc. and all should think the scope of the present invention within.The present invention is also applicable to utilize containing A1
2o
3the clay such as dickite, illite class ore or containing A1
2o
3raw materials of slag produce within alum also should think the scope of the present invention.
Claims (2)
1. utilize alunite to produce a method for alum, comprise following implementation step:
(1), select alunite breeze:
By alumstone ore fragmentation, levigate or flotation acquisition alunite breeze, ore grade >=45%, ore powder granularity 80-200 orders;
(2), breeze microwave calcining dehydration:
By microwave thermal construction equipment roasting dehydration for breeze, ore grog dehydration rate>=90 %, rate of decomposition≤5 %, A1
2o
3solubility rate>=90%, the microwave frequency of microwave thermal construction equipment is 2450MHz, microwave output power>=1.0KW, microwave irradiation time>=10min;
(3), sulphuric acid soln leaches stripping, filtering separation:
The alunite sulphuric acid soln that will dewater leaches stripping, insulation is filtered, solid-liquid separation, leached mud hot wash, washing lotion is incorporated to leach liquor, wherein, sulphuric acid soln/dehydration alunite weight ratio is 3-8, the consumption of sulfuric acid (100%) is theoretical amount 100-130%, leaching stripping temperature >=90 DEG C, leaching dissolution time >=0.5h;
(4), leach liquor evaporation concentration, the crystallization of cooling down alum:
By the leach liquor evaporation concentration of heating, the crystallization of cooling down alum, crystalline mother solution returns to leaching stripping, recycle, former liquid temp >=80 DEG C of alum, alum original liquid concentration >=25 %, cooling termination temperature≤25 DEG C; Wherein, in leach liquor, add potassium sulfate, all generate potassium alum, 100-120 % that potassium sulfate consumption is theoretical amount; In leach liquor, do not add potassium sulfate, generate potassium alum co-producing sulfuric acid aluminium.
2. the method for utilizing alunite to produce alum according to claim 1, is characterized in that: in described step (1), ore grade is 50%-65%; In described step (2), ore grog dehydration rate is 95-99 %, and rate of decomposition is 2-5 %, A1
2o
3solubility rate is 90-95 %; In described step (3), leaching stripping temperature is 90-100 DEG C, and leaching dissolution time is 0.5-3.0h; In described step (4), the former liquid temp of alum is 80-95 DEG C, and alum original liquid concentration is 25-28%, and cooling termination temperature is 15-25 DEG C.
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| CN103787396A (en) * | 2014-01-27 | 2014-05-14 | 紫金矿业集团股份有限公司 | Method for preparing high-purity potassium alum and aluminum sulfate from alunite ore |
| CN103979592B (en) * | 2014-04-16 | 2016-02-10 | 广西冶金研究院 | A kind of method reclaiming aluminium from alumina producing waste red mud |
| CN104445331A (en) * | 2014-12-16 | 2015-03-25 | 兴安宸亿工贸有限公司 | Method for using wastewater and waste residues generated in alum production process |
| CN105129830A (en) * | 2015-02-15 | 2015-12-09 | 广西隆安瑞丰工贸有限公司 | Method for preparation of potassium alum from activated clay production mother liquor |
| CN105293553A (en) * | 2015-02-15 | 2016-02-03 | 广西隆安瑞丰工贸有限公司 | Method for preparing tschermigite by utilizing activated clay production wastewater |
| CN105271341A (en) * | 2015-02-15 | 2016-01-27 | 广西隆安瑞丰工贸有限公司 | Method for preparing potassium alum by utilization of activated clay production waste water |
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| CN102517461A (en) * | 2011-12-16 | 2012-06-27 | 紫金矿业集团股份有限公司 | Method for recycling gallium in alunite concentrate |
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|---|---|---|---|---|
| RU2013373C1 (en) * | 1991-11-05 | 1994-05-30 | Гакиф Закирович Насыров | Process for treating alunite ore to obtain alumopotassium alum and aluminium sulfate |
| CN101913633A (en) * | 2010-07-07 | 2010-12-15 | 紫金矿业集团股份有限公司 | Extraction technology of alumina and potassium sulfate from alunite by using hot-pressing leaching process |
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