CN103787396A - Method for preparing high-purity potassium alum and aluminum sulfate from alunite ore - Google Patents
Method for preparing high-purity potassium alum and aluminum sulfate from alunite ore Download PDFInfo
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- CN103787396A CN103787396A CN201410039642.2A CN201410039642A CN103787396A CN 103787396 A CN103787396 A CN 103787396A CN 201410039642 A CN201410039642 A CN 201410039642A CN 103787396 A CN103787396 A CN 103787396A
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Abstract
The invention relates to a method for preparing high-purity potassium alum and aluminum sulfate from alunite ore. The method comprises the following steps: firstly, roasting the alunite ore to remove crystal water; secondly, performing sulfuric acid leaching on dehydrated alunite to obtain aluminum and potassium, and crystallizing the potassium alum in leaching liquid; thirdly, adding a certain quantity of acid into crystallization mother liquid, returning to a circulating leaching process, and crystallizing the potassium alum in circulating leaching liquid; and finally, crystallizing the aluminum sulfate in potassium alum crystallization mother liquid circulated for a certain number of times. The purpose of the invention is to provide the method for preparing the high-purity potassium alum and the aluminum sulfate from the alunite ore, which is simple in process, low in production cost and easy to industrialize in allusion to the comprehensive utilization problem of the alunite ore.
Description
One. technical field
The present invention relates to precious metals metallurgy industry, particularly comprehensive recovery, separation, the method for purification of valuable metal in a kind of ore, be specifically related to a kind of method of preparing high purity potassium alum and Tai-Ace S 150 from alumstone ore.
Two. background technology
Mineral Resources in China lacks, and Al, K are the Important Mineral Resources of China, wherein the narrow resources of Jia Shi China.Alumstone ore is more and more subject to the attention of research both at home and abroad as the potential resources of Al, K.At present, fully utilize alumstone ore both at home and abroad and all there is no economy, technical rational processing alunite technique.China is alunite reserves big countries, has a large amount of primary and association alumstone ores, and alum ore deposit, Wenzhou is described as " world's alum all ", and alunite reserves account for 60% of world's total reserves.Mixed Microbial Populations in Zijinshan Copper Mine is the super-huge copper mine of China, and wherein association has a large amount of alumstone ores, but the alumstone ore of current China is not all utilized effectively or utilising efficiency is very low.
In alumstone ore sulfuric acid leaching-crystallization processes process, aluminium, potassium crystallization alum process are a kind of naturally separation, scavenging process, have unique advantage compared with other techniques.But due to mAl/mK=3 in alumstone ore, and mAl/mK=1 in leach-crystallization alum, therefore there is the superfluous problem of Al in leach liquor, for the not effective means improvement at present of this problem, alum ore deposit, Wenzhou adopts methods such as reducing Al leaching yield that aluminium is leached less, causes the lower and wasting of resources of the rate of recovery of Al, K.
Patent of invention " a kind of method from association alunite mine tailing extraction aluminium potassium ", propose to adopt acid-soluble roasting-water logging technique to prepare the method for alum, Tai-Ace S 150 product.In patent prospectus first by sulfuric acid stripping at present alumstone ore 360 ℃, then to the crystalline sulfuric acid aluminium that adds water in Leaching Systems, leached mud water logging post crystallization alum, crystallization alum mother liquid evaporation crystalline sulfuric acid aluminium.But can find out from this Patent Prospectus content and data, this invention is inconsistent and cannot realize crystallization alum separates with the effective of crystalline sulfuric acid aluminium, and the product obtaining is the mixture of alum and Tai-Ace S 150 or other material impurities.Such as disclosed Al2O3 content in Al2 (SO4) the 3 ˙ 17H2O products of the first step crystallization in prospectus is 22.5%, and should be 15.74% according to Al2O3 actual content in product standard cubage Al2 (SO4) 3 ˙ 17H2O; In the alum product that second step crystallization obtains, Al2O3, K2O, SO3 content are respectively 20.86%, 20.79%, 55.84%, and should be respectively 10.76%, 9.91%, 33.75% according to Al2O3, K2O, SO3 actual content in product standard potassium alum; The mixture especially obtaining in the 3rd step crystallization, and in all crystallizations, the foreign matter content such as Fe2O3 is all higher, and Fe2O3 and other impurity minimum content are all more than 2%.In products obtained therefrom, product purity and foreign matter content do not meet the standard-required of any product.In addition, this technique exists 360 ℃ of acid-soluble roastings that energy consumption is high, technique be to the problems such as equipment requirements height, industrial cannot enforcement.And high temperature is acid-soluble enters in solution the impurity such as Fe, Si major part in alumstone ore, bring difficulty to follow-up filtration and separation, thereby cause product foreign matter content to meet the demands.
In patent of invention " a kind of extracting vanadium from stone coal aluminium, potassium comprehensive recovering process ", disclose in addition one and added sylvite or containing potassium material, make aluminium unnecessary in solution generate potassium alum in leach liquor, thereby realized recovery or the removal of unnecessary aluminium.Also have this method of employing in alunite acidleach-Study on Crystallization field, but the value of the additives such as the K2SO4 adding is much larger than the value of the potassium alum generating, and potassium alum exists the problem that dimensions of market is little, therefore the method loses more than gain.
Both at home and abroad the problems that particularly comprehensive utilization of China's alumstone ore exists, make the difficult problem that alumstone ore always cannot efficient recovery based on above-mentioned, and the present invention proposes a kind of method of preparing high purity potassium alum and Tai-Ace S 150 from alumstone ore.The comprehensive leaching yield that adopts Al of the present invention, K respectively 92%, more than 97%, the potassium alum purity 99.56% obtaining, in Tai-Ace S 150 on Al2O3 content 15.95%.Technique of the present invention is simple, production cost is low, be easy to industrialization.
Three. summary of the invention
The object of a kind of method of preparing high purity potassium alum and Tai-Ace S 150 from alumstone ore of the present invention is intended to provide for an alumstone ore comprehensive utilization difficult problem that a kind of technique is simple, production cost is low, be easy to the industrialized method of preparing high purity potassium alum and Tai-Ace S 150 from alumstone ore.
The present invention realizes according to following know-why; 1. mAl/mK=3 in alumstone ore, and mAl/mK=1 in leach-crystallization alum.In Leaching Systems, Al is excessive, excessive Al can with SO42-crystalline sulfuric acid aluminium; 2. potassium alum and Tai-Ace S 150 crystallization there are differences.In leach liquor, first potassium alum crystallization is carried out, and Tai-Ace S 150 crystallization starts after in solution, Al3+ concentration exceedes finite concentration; 3. leach liquor circulating leaching-crystallisation process enrichment Al3+, lowers K+ content.Owing to all having the Al3+ of 60% left and right excessive in solution after each crystalline potassium alum, in the each circulating leaching-crystallisation process of leach liquor crystalline mother solution, Al3+/K+ ratio all obtains a certain proportion of increase, when realizing the crystallization of Tai-Ace S 150 in crystalline mother solution when Al3+>60g/L, K+<0.3g/L.
Technical scheme of the present invention, detailed process condition is as follows:
1, first, alumstone ore roasting is removed to crystal water, secondly, will dewater alunite sulfuric acid leaching aluminium and potassium, leach liquor crystalline potassium alum; Then, crystalline mother solution is added after a certain amount of acid and returned and pay for the acid flow process circulating leaching of few sand, circulating leaching liquid crystalline potassium alum; Finally, certain number of times post crystallization potassium alum mother liquor crystallization Tai-Ace S 150 that will circulate;
2, alumstone ore is raw ore or association alumstone ore, 500～550 ℃ of alunite maturing temperatures, 1～2 hour time.70～80 ℃ of dehydration alunite extraction temperatures, 1～2 hour time, liquid-solid ratio 5～7, sulfuric acid consumption 300～400kg/t alumstone ore;
3, crystalline potassium alum Recycling Mother Solution leaching number of times is 2～4 times, Al3+>60g/L, K+<0.3g/L in the front last crystalline potassium alum mother liquor of crystalline sulfuric acid aluminium, crystallization time 24～48 hours, crystallization mode is in spontaneous nucleation or evaporative crystallization.
The features and advantages of the invention are:
1. utilize alumstone ore acidleach process Al surplus, crystallization difference principle and circulating leaching enrichment Al3+, lower the leaching process natures such as K+ content, adopt first circulating leaching, separation, process of enriching to prepare potassium alum, Tai-Ace S 150 product;
2. the present invention only adopts a kind of leaching agent of leaching agent sulfuric acid, in process, adds without any other reagent or additive;
3. the present invention utilize potassium alum, Tai-Ace S 150 crystallisation process be with solution in foreign ion natural separation, scavenging process, realized a step and prepared high purity potassium alum, the Tai-Ace S 150 product that conformance with standard requires.
The comprehensive leaching yield that adopts Al of the present invention, K respectively 92%, more than 95%, the potassium alum purity 99.56% obtaining, in Tai-Ace S 150 on Al2O3 content 15.95%.Potassium alum, Tai-Ace S 150 indices meet respectively GB1895-2004 foodstuff additive, the technical requirements of HG/T2225-2001 acceptable end product.
Four. embodiment
Example 1: get Purple Mountain association alumstone ore 100g in crucible and be placed in retort furnace roasting dehydration under 550 ℃ of temperature, time 2 h condition, then under sulfuric acid consumption 400kg/t alumstone ore, 80 ℃ of temperature, liquid-solid ratio 5 conditions, leach dehydration alum, leach liquor spontaneous nucleation potassium alum, after adding a certain amount of acid, crystalline potassium alum mother liquor returns to leaching, circulating leaching liquid crystalline potassium alum, post crystallization potassium alum mother liquor crystallization Tai-Ace S 150 so circulates 3 times.Dehydration alunite circulating leaching-crystallization trial result is as shown in table 1, the different circulating leaching number of times of dehydration alunite crystallization alum, Tai-Ace S 150 purity are as shown in table 2, crystalline potassium alum multielement analysis result is as shown in table 3, and crystalline sulfuric acid aluminium multielement analysis result is as shown in table 4.From table 3, table 4 result, the potassium alum of preparation, Tai-Ace S 150 indices meet respectively GB1895-2004 foodstuff additive, the technical requirements of HG/T2225-2001 acceptable end product
Example 2: get Purple Mountain association alumstone ore 100g and be placed in retort furnace roasting dehydration under 550 ℃ of temperature, 1.5 hours time condition in crucible, then under sulfuric acid consumption 350kg/t alumstone ore, temperature 70 C, liquid-solid ratio 7 conditions, leach dehydration alum, leach liquor spontaneous nucleation gallium alum, after crystalline potassium alum, mother liquor returns to leaching after adding a certain amount of acid, circulating leaching liquid crystalline potassium alum, post crystallization mother liquor crystallization Tai-Ace S 150 so circulates 4 times.The potassium alum purity 99.48% obtaining, Al2O3 content 16.05% in crystalline sulfuric acid aluminium.Crystalline potassium alum, Tai-Ace S 150 are carried out to chemical detection according to GB1895-2004, HG/T2225-2001 respectively, and potassium alum, Tai-Ace S 150 indices meet respectively GB1895-2004 foodstuff additive, the technical requirements of HG/T2225-2001 acceptable end product.
Example 3: get the primary alumstone ore 100g in alum ore deposit, Wenzhou roasting dehydration under 500 ℃ of temperature, 1 hour time condition in retort furnace, then under sulfuric acid consumption 300kg/t alumstone ore, 80 ℃ of temperature, liquid-solid ratio 6 conditions, leach dehydration alum, leach liquor spontaneous nucleation gallium alum, after crystalline potassium alum, mother liquor returns to leaching after adding a certain amount of acid, circulating leaching liquid crystalline potassium alum, so 3 post crystallization mother liquor crystallization Tai-Ace S 150 of circulation, crystalline potassium alum purity 99.50%, Al2O3 content 15.98% in crystalline sulfuric acid aluminium.Crystalline potassium alum, Tai-Ace S 150 are carried out to chemical detection according to GB1895-2004, HG/T2225-2001 respectively, and potassium alum, Tai-Ace S 150 indices meet respectively GB1895-2004 foodstuff additive, the technical requirements of HG/T2225-2001 acceptable end product.
Table 1 dewater alunite circulating leaching, enrichment, separating resulting
Table 2 dewater alunite circulating leaching crystallization alum, Tai-Ace S 150 purity check result/%
Table 3 crystalline potassium alum multielement analysis result/%
Table 4 Tai-Ace S 150 crystallization multielement analysis result/%
Claims (3)
1. the method for preparing high purity potassium alum and Tai-Ace S 150 from alumstone ore, is characterized in that: concrete steps comprise: first, alumstone ore roasting is removed to crystal water, secondly, will dewater alunite sulfuric acid leaching aluminium and potassium, leach liquor crystalline potassium alum; Then, crystalline mother solution is added after a certain amount of acid and returned and pay for the acid flow process circulating leaching of few sand, circulating leaching liquid crystalline potassium alum; Finally, certain number of times post crystallization potassium alum mother liquor crystallization Tai-Ace S 150 that will circulate.
2. the method for preparing high purity potassium alum and Tai-Ace S 150 from alumstone ore according to claim 1, it is characterized in that: alumstone ore is raw ore or association alumstone ore, alunite roasting condition is 500～550 ℃ of temperature, 1～2 hour time, and dehydration alunite leaching condition is 70～80 ℃ of temperature, 1～2 hour time, liquid-solid ratio 5～7, sulfuric acid consumption 300～400kg/t alumstone ore.
3. the method for preparing high purity potassium alum and Tai-Ace S 150 from alumstone ore according to claim 1, it is characterized in that: it is 2～4 times that crystalline potassium alum Recycling Mother Solution leaches number of times, Al3+>60g/L, K+<0.3g/L in the front last crystalline potassium alum mother liquor of crystalline sulfuric acid aluminium, crystallization time 24～48 hours, crystallization mode is in spontaneous nucleation or evaporative crystallization.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110510647A (en) * | 2019-09-24 | 2019-11-29 | 福州大学 | The method that production aluminium oxide, potassium sulfate and sulfuric acid are decomposed in potassium alum suspension roasting |
| CN112125325A (en) * | 2020-09-29 | 2020-12-25 | 福州大学 | Process for producing alumina by aluminosilicate mineral acid method |
| CN115304301A (en) * | 2022-08-11 | 2022-11-08 | 厦门兑泰新材料科技有限公司 | Exciting agent for exciting activity of alunite tailings entrained in copper ore and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102910660A (en) * | 2012-11-06 | 2013-02-06 | 傅培鑫 | Method for producing alum by utilizing alunite |
| CN103103339A (en) * | 2012-12-19 | 2013-05-15 | 紫金矿业集团股份有限公司 | Method for selectively recovering alum and gallium from alunite concentrate |
| CN103436717A (en) * | 2013-08-30 | 2013-12-11 | 紫金矿业集团股份有限公司 | Method for enriching gallium and comprehensively utilizing potassium and aluminum from alunite |
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2014
- 2014-01-27 CN CN201410039642.2A patent/CN103787396A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102910660A (en) * | 2012-11-06 | 2013-02-06 | 傅培鑫 | Method for producing alum by utilizing alunite |
| CN103103339A (en) * | 2012-12-19 | 2013-05-15 | 紫金矿业集团股份有限公司 | Method for selectively recovering alum and gallium from alunite concentrate |
| CN103436717A (en) * | 2013-08-30 | 2013-12-11 | 紫金矿业集团股份有限公司 | Method for enriching gallium and comprehensively utilizing potassium and aluminum from alunite |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110510647A (en) * | 2019-09-24 | 2019-11-29 | 福州大学 | The method that production aluminium oxide, potassium sulfate and sulfuric acid are decomposed in potassium alum suspension roasting |
| CN112125325A (en) * | 2020-09-29 | 2020-12-25 | 福州大学 | Process for producing alumina by aluminosilicate mineral acid method |
| CN115304301A (en) * | 2022-08-11 | 2022-11-08 | 厦门兑泰新材料科技有限公司 | Exciting agent for exciting activity of alunite tailings entrained in copper ore and preparation method thereof |
| CN115304301B (en) * | 2022-08-11 | 2023-07-21 | 厦门兑泰新材料科技有限公司 | Exciting agent for exciting activity of alunite tailings carried in copper ores and preparation method thereof |
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Application publication date: 20140514 |