CN103011206B - Method utilizing alunite in flotation tailing to produce potassium sulfate and auxiliary products thereof - Google Patents
Method utilizing alunite in flotation tailing to produce potassium sulfate and auxiliary products thereof Download PDFInfo
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Abstract
The invention provides a method utilizing alunite in flotation tailing to produce potassium sulfate and auxiliary products thereof. The method fully utilizes secondary resources, changes waste into treasure, achieves minimizing, harmlessness and recycling of solid waste, improves comprehensive utilizing level of tailings in China, relieves an acute contradiction of supply and demand of potassium sulfate, reduces loss on foreign exchange caused by mass importation of the potassium sulfate, improves guarantee age limit of kalium and the international competitiveness of the kalium salt industry, completely solves the key scientific and technical problem of economic, clean efficient and comprehensive utilization of the alunite in flotation, the tailings are utilized as resources, establishes tailing comprehensive utilization technical demonstration project, and promotes the development of the comprehensive utilization technique of the tailing in China.
Description
One. technical field
The present invention relates to a kind of method that comprehensive utilization of tailing utilizes, relate in particular to a kind of method of utilizing the alunite in flotation tailing to produce potassium sulfate and byproduct thereof.
Two. background technology
Mineral resources are one of the mankind's important means of production of depending on for existence, and its main feature is non-renewable and irreplaceability in a short time.Mineral resources are basic materials of China's industrial development, and at present more than 90% energy of China and approximately 80% the raw material of industry are from mineral resources, and the raw mineral materials that drops into every year national economy running exceedes 5,000,000,000 t.China is mineral resources big producing countries, but mineral resources are relatively less per capita, and the level of comprehensive utilization that improves mineral resources and mine tailing is even more important.China's Agenda 21 has been listed " disposal, management and the resource demonstration project of mine tailing " in the preference plan of pioneer field, indicates that China has brought up to considerable position the exploitation of Mine Tailing Resource and environmental protection.12655 of the existing Tailings Dams of China, wherein third-class above big-and-middle-sized Tailings Dam is 533, account for sum 4.2%, four, 12122 of small-sized Tailings Dams such as 5, account for 95.8% of sum.By being 10,000,000,000 t to China's mine tailing accumulation in the end of the year 2009 volume of cargo in storage.And national output 11.92 hundred million t in 2009 increase by 8.4% than last year, comprehensive utilization of tailing total amount is 1.6 hundred million t, comprehensive utilization ratio be 13.3% lower than developed country more than 50% advanced level.
According to the nonmetal supply and demand situation report of country, China's two kinds of nonmetallic minerals the most in short supply are sylvite and diamond.Sylvite is always paid attention to by various countries, and sylvite is in the world mainly derived from soluble potassium salt deposit.According to the U.S. adjust office 2005 statistics, world's sylvite reserves are about 8,300,000,000 tons (K2O), basic reserves are about 17,000,000,000 tons.By the current level of production, existing proved reserves can be exploited more than 300 years for the world.But the distribution of world's sylvite is very unbalanced, the overwhelming majority on the Northern Hemisphere, between all spend at north latitude 40～60 degree of 33 world-class sylvite basins and the famous large ore deposit of having found at present.Press reserves, Canada ranked first, account for 53% of the world, Russia ranked second, account for 22%, Byelorussia and Germany ranked third respectively and the 4th, respectively account for 9%, above-mentioned four countries total accounts for 93% of world's gross reserves, and China's sylvite reserves are 8,000,000 tons (K2O), basis reserves are 45,000 ten thousand tons (K2O), be respectively 0.096% and 2.65% of whole world reserves and basic reserves, although China's sylvite output had larger growth in recent years, however, the interdependency of sylvite import still remains on more than 70%, and the population ratio in this and the world 1/5 is extremely inharmonious.
At present, the production method of potassium sulfate is divided three classes substantially in the world, and approximately 10%～15% potassium sulfate is to be produced by sea lake salt bittern, 10% left and right be to utilize that sylvite ore is made of stones gets, approximately 75% potassium sulfate is to transform and produce with sulfuric acid or sulfate and potassium chloride.Sea lake salt bittern is produced and is existed technique to need evaporated water large, and energy consumption is high, potassium sulfate to obtain rate low, the product shortcoming such as serious that runs off.Sulfuric acid or sulfate and potassium chloride transform and produces is to throw people using potassium chloride as raw material, has increased the production cost of potassium sulfate, has reduced the market competitiveness of enterprise.The mid-50, the former Soviet Union adopts heat of reduction solution technique to realize the comprehensive utilization of alunite, year is produced aluminium oxide 160,000 t, potassium sulfate 170,000 t and sulfuric acid 350,000 t, this factory utilizes potassium hydroxide to carry out purifying crude sylvite in sylvite purification workshop section and produces potassium sulfate, although produce stable, potassium product quality is good, does not meet China's national situation but adopt potassium hydroxide purifying crude sylvite to produce potassium sulfate.Wenzhou chemical factory of China adopts heat of reduction solution that alunite is fully utilized and studied, Chinese style be installed on nineteen sixty start investment build, start test run October 16 nineteen sixty-five, be total to production standard potash fertilizer (25%K2O) 3085t by 1972, sulfuric acid (100%H2SO4) 2584t, aluminium hydroxide (primes) 2714t.The Ministry of Chemical Industry organized and identified by pilot scale in December, 1978, although the rate of recovery of aluminium oxide and potassium oxide, can decompose the key technical indexes such as SO3 overall utilization, alkaline consumption and all reach or connect former petrochemical industry portion requirement, but follow-uply produce potassium sulfate by evaporative crystallization, potassium sulfate average content is 65%, potassium, sodium separation difficulty, poor product quality.The molten alumina technology of producing of grain slag acid that professor Han Xiaozhao of HeFei University of Technology adopts high temperature fast dewatering---grog water logging potassium oxide---is processed alunite, and this technique dehydration sintering temperature is high, and energy consumption is large, requires high to equipment material.
In a word, China's mine tailing amount is large at present, and level of comprehensive utilization is low, and this has not only caused the significant wastage of resource, but also occupies a large amount of soils, contaminated environment, the destruction ecological balance, even causes security incident.In addition, China's arable land severe potassium deficiency, the Changjiang river areas to the south and East China generally need application of potash fertilizer, and China's potassium resource is very poor, potash fertilizer output is very low, the degree of self-sufficiency is about 20%, can not meet the needs of agricultural production far away, and the overwhelming majority needs dependence on import, externally interdependency is too high, China is in a disadvantageous position all the time in the international price negotiation of potash fertilizer, over the next several years in, the situation of potash fertilizer degree of self-sufficiency deficiency will continue.Therefore, be badly in need of a kind of method of utilizing the alunite in flotation tailing to produce potassium sulfate of exploitation, improve China's comprehensive utilization of tailing level and alleviate the outstanding contradiction of potassium sulfate supply and demand, reduce loss on foreign exchange that potassium sulfate relies on import in a large number, promote the guarantee time limit of potassium resource and the international competitiveness of Potash Industry, thoroughly solve the economy of alunite in mine tailing, a crucial Science and Technology difficult problem clean, high-efficiency comprehensive utilization is extremely urgent.
Three. summary of the invention
The invention provides a kind of method of utilizing the alunite in flotation tailing to produce potassium sulfate and byproduct thereof, its objective is that solution present stage China's comprehensive utilization of tailing level is low and potassium resource is very poor, potash fertilizer output and the degree of self-sufficiency are very low, the overwhelming majority needs dependence on import, externally interdependency is too high, over the next several years, the problem that the situation of potash fertilizer degree of self-sufficiency deficiency will continue.A kind of China's comprehensive utilization of tailing level and outstanding contradiction of alleviation potassium sulfate supply and demand of improving is proposed, reduce loss on foreign exchange, the guarantee time limit that promotes potassium resource and the international competitiveness of Potash Industry that potassium sulfate relies on import in a large number, thoroughly solve the economy of alunite in mine tailing, a crucial Science and Technology difficult problem for clean, high-efficiency comprehensive utilization, make Making Use of Tailings, provide the method for technical support for the high-efficiency vigorous exploitation of alunite in mine tailing provides the transformation of wide space and existing relevant enterprise.
The present invention is a kind of utilizes the method that in flotation tailing, alunite is produced potassium sulfate and byproduct thereof, comprises following several step:
The first step: alunite flotation: flotation tailing pulp adopts sodium carbonate to regulate pH=9.0～9.5, then add successively scattered inhibitor waterglass 400g/t～800g/t to stir 2min～3min, collecting agent oleic acid 200g/t～400g/t and stir and carry out alunite after 1min～2min and roughly select 6min～9min, mine tailing is thrown tail; The alunite concentrate of roughly selecting adds waterglass 200g/t～400g/t and carries out selected 4min～6min for the first time, and selected chats is thrown tail for the first time; Selected alunite concentrate adds waterglass 100g/t～300g/t and carries out selected 3min～5min for the second time and obtain alunite concentrate for the first time, and selected chats returns to the alunite section of roughly selecting for the second time.
Second step: roasting: the alunite concentrate of first step flotation gained and reducing agent (affiliated reducing agent is coke or coal or black oil) are mixed and ball processed, be that 570 DEG C～650 DEG C, time 15min～30min, reducing agent consumption calculate by alunite grade in temperature, by carrying out roasting under 1～3 times of condition adding of theoretical requirement.Flue gas, through high efficiency cyclonic dust collector, hot electrostatic precipitator, the processing of high-efficient wet-type (venturi) smoke eliminator, finally adopts 3+2 double-absorption flow process to produce sulfuric acid.Roasting grog through good operational environment, automaticity is high, heat loss is little (hot scraper plate), and thermal material conveyer send the processing of shrend potassium sulfate operation.
The 3rd step: shrend potassium sulfate: second step gained thermal material uses shrend potassium sulfate 20min～60min(under the condition of L/S=3～5 under the condition of L/S=3～5, when thermal material shrend, temperature can maintain 75 DEG C～95 DEG C voluntarily, without other heating), after finishing, question response carries out Separation of Solid and Liquid, filtrate is sent potassium sulfate multi-effect evaporation system, after residue washing, Separation of Solid and Liquid, be aluminium oxide and aluminosilicate byproduct, take out to cement plant as cement producting material, cleaning solution returns for shrend potassium sulfate.
The 4th step: potassium sulfate---crystallisation by cooling: adopt 120 DEG C～140 DEG C saturated vapor evaporation and concentration the 3rd step gained leachate in multi-effect evaporator, be evaporated to potassium sulfate content in solution and be greater than 220g/L, then send cooler crystallizer to stir crystallisation by cooling this evaporated liquor, last Separation of Solid and Liquid obtains potassium product and crystalline mother solution, potassium sulfate is dried, packs, and crystalline mother solution returns to the 3rd potassium sulfate for shrend roasting grog.
Advantage of the present invention:
The method that a the present invention utilizes the alunite in mine tailing to produce potassium sulfate and byproduct thereof, make full use of secondary resource, turn waste into wealth, realize solid waste reducing, innoxious and resource, to implement the Party Central Committee until the important embodiment of the Developing Recycling Economy, Building up An Economization Soceity of cities and counties, promote the level of comprehensive utilization of China's mine tailing, alleviate the outstanding contradiction of potassium sulfate supply and demand, reduce the loss on foreign exchange that potassium sulfate relies on import in a large number, promote the guarantee time limit of potassium resource and the international competitiveness of Potash Industry, thoroughly solve the economy of alunite in mine tailing, clean, a crucial Science and Technology difficult problem for high-efficiency comprehensive utilization, make Making Use of Tailings, form comprehensive utilization of tailing show-how engineering, advance the development of China's comprehensive utilization of tailing technology.
B is flotation alunite from flotation tailing, saves 60%～70% the broken grinder order that accounts for conventional flotation totle drilling cost; Alunite concentrate and reducing agent mix rear employing ball baking modes processed, 600 DEG C of left and right are down in 900 DEG C of left and right of decomposition temperature when making can to decompose SO3 in alunite and more thoroughly decomposing, unique baking modes has not only shortened the reduction roasting time, also realize synchronously carrying out of dehydration and reduction, simplify technological process, reduced roasting energy consumption, saved equipment investment, reduce area of mill site, for the high-efficiency vigorous exploitation of alunite in mine tailing provides wide space.
C grog shrend liquid is potassium sulfate solution, and composition is single, and impurity content is few, only by evaporation---crystallisation by cooling can obtain the high-class product quality requirement of potassium sulfate for agricultural use.
The production line that d this method forms, technological process is short, simple to operate, invests littlely, and production cost is low, and instant effect has tremendous economic, society and environmental benefit.
Four. brief description of the drawings
Fig. 1 is a kind of process chart that utilizes alunite in flotation tailing to produce the method for potassium sulfate and byproduct thereof of the present invention.
Five. detailed description of the invention
Technique below in conjunction with embodiment to the present invention and effect are done further checking and are set forth, and can not limit the scope of the invention with this, and the technological process that example adopts as shown in Figure 1.
Embodiment 1
The essential mineral of certain flotation tailing is quartz, is secondly alunite and dickite, and a small amount of exists with forms such as sericite, feldspar, chlorite, allochites, and flotation tailing chemical analysis results is in table 1.
Certain flotation tailing essential element analysis result/% of table 1
Note: "
※" unit is g/t, lower with.
Utilize the method that in flotation tailing, alunite is produced potassium sulfate and byproduct thereof, comprise successively following step.
The first step: alunite flotation: flotation pulp is adopting sodium carbonate to adjust pH=9.0, then adds successively scattered inhibitor waterglass 500g/t to stir 3min, collecting agent oleic acid 200g/t and stirs and carry out alunite after 2min and roughly select 7min, and mine tailing is thrown tail; The alunite concentrate of roughly selecting adds waterglass 400g/t and carries out selected 4min for the first time, and selected chats is thrown tail for the first time; Selected alunite concentrate adds waterglass 300g/t and carries out selected 4min for the second time and obtain alunite concentrate for the first time, and selected chats returns to the alunite section of roughly selecting for the second time.
Second step: roasting: the alunite concentrate of first step flotation gained and coke blacking (granularity-200 order accounts for 70% left and right) are mixed and ball processed, are to dewater and reduction roasting under 620 DEG C, time 15min, the coke blacking addition condition of 1.5 times that is theoretical requirement in temperature simultaneously.Flue gas, through high efficiency cyclonic dust collector, hot electrostatic precipitator, the processing of high-efficient wet-type (venturi) smoke eliminator, finally adopts 3+2 double-absorption flow process to produce sulfuric acid.Roasting grog through good operational environment, automaticity is high, heat loss is little (hot scraper plate), and thermal material conveyer send the processing of shrend potassium sulfate operation.
The 3rd step: shrend potassium sulfate: second step gained thermal material is used shrend potassium sulfate 30min under 90 DEG C of temperature, L/S=3 condition, after finishing, question response carries out Separation of Solid and Liquid, filtrate is sent potassium sulfate multi-effect evaporation system, residue washing and carry out Separation of Solid and Liquid after obtain aluminium oxide and aluminosilicate byproduct, take out to cement plant as cement producting material, cleaning solution returns for shrend potassium sulfate.
The 4th step: potassium sulfate evaporation---crystallisation by cooling: adopt 140 DEG C of saturated vapor evaporation and concentration the 3rd step gained leachate in multi-effect evaporator, being evaporated to potassium sulfate content in solution is 225g/L left and right, then this evaporated liquor is sent cooler crystallizer to stir and be cooled to 30 DEG C, last Separation of Solid and Liquid obtains potassium product and crystalline mother solution, potassium sulfate is dried, packs, and crystalline mother solution returns to the 3rd potassium sulfate for shrend roasting grog.Technical data and technical indicator are in table 2.
The technical data of table 2 embodiment and technical indicator
Embodiment 2
The essential mineral of certain flotation tailing is quartz, calcedony, is secondly alunite, and other also has kaolin, sericite, feldspar etc., and flotation tailing chemical analysis results is in table 3.
Table 3 flotation tailing chemical composition analysis result/%
Utilize the method that in flotation tailing, alunite is produced potassium sulfate and byproduct thereof, comprise successively following step.
The first step: alunite flotation: flotation pulp is adopting sodium carbonate to adjust pH=9.5, then adds successively scattered inhibitor waterglass 500g/t to stir 3min, collecting agent oleic acid 400g/t and stirs and carry out alunite after 2min and roughly select 6min, and mine tailing is thrown tail; The alunite concentrate of roughly selecting adds waterglass 300g/t and carries out selected 4min for the first time, and selected chats is thrown tail for the first time; Selected alunite concentrate adds waterglass 200g/t and carries out selected 4min for the second time and obtain alunite concentrate for the first time, and selected chats returns to the alunite section of roughly selecting for the second time.
Second step: roasting: the alunite concentrate of first step flotation gained and coal dust (granularity-200 order accounts for 70% left and right) are mixed and ball processed, are to dewater and reduction roasting under 600 DEG C, time 30min, the coal dust addition condition of 2.5 times that is theoretical requirement in temperature simultaneously.Flue gas, through high efficiency cyclonic dust collector, hot electrostatic precipitator, the processing of high-efficient wet-type (venturi) smoke eliminator, finally adopts 3+2 double-absorption flow process to produce sulfuric acid.Roasting grog through good operational environment, automaticity is high, heat loss is little (hot scraper plate), and thermal material conveyer send the processing of shrend potassium sulfate operation.
The 3rd step: shrend potassium sulfate: second step gained thermal material is used shrend potassium sulfate 40min under 80 DEG C of temperature, L/S=4 condition, after finishing, question response carries out Separation of Solid and Liquid, filtrate is sent potassium sulfate multi-effect evaporation system, residue washing and carry out Separation of Solid and Liquid after obtain aluminium oxide and aluminosilicate byproduct, take out to cement plant as cement producting material, cleaning solution returns for shrend potassium sulfate.
The 4th step: potassium sulfate evaporation---crystallisation by cooling: adopt 140 DEG C of saturated vapor evaporation and concentration the 3rd step gained leachate in multi-effect evaporator, being evaporated to potassium sulfate content in solution is 230g/L left and right, then this evaporated liquor is sent cooler crystallizer to stir and be cooled to 30 DEG C, last Separation of Solid and Liquid obtains potassium product and crystalline mother solution, potassium sulfate is dried, packs, and crystalline mother solution returns to the 3rd potassium sulfate for shrend roasting grog.Technical data and technical indicator are in table 4.
Table 4 embodiment 2 technical datas and technical indicator
Claims (3)
1. utilize the method that in flotation tailing, alunite is produced potassium sulfate and byproduct thereof, it is characterized in that: specifically comprise the following steps:
The first step: alunite flotation: flotation tailing pulp adopts sodium carbonate to regulate, then adds that scattered inhibitor waterglass stirs, collecting agent oleic acid carries out alunite after stirring and roughly select and obtain alunite concentrate 1 successively, roughly selects the mine tailing of generation and throws tail; Alunite concentrate 1 adds waterglass and carries out the selected alunite concentrate 2 that obtains for the first time, and the chats of selected generation is for the first time thrown tail; Alunite concentrate 2 adds waterglass and carries out the selected alunite concentrate 3 that obtains for the second time, and the chats of selected generation for the second time returns to alunite and roughly selects workshop section;
Second step: roasting: the alunite concentrate of first step flotation gained 3 and reducing agent are mixed and ball processed, carry out roasting, flue gas is through high efficiency cyclonic dust collector, hot electrostatic precipitator, the processing of high-efficient wet-type smoke eliminator, finally adopt 3+2 double-absorption flow process to produce sulfuric acid, roasting grog send the processing of shrend potassium sulfate operation through thermal material conveyer;
The 3rd step: shrend potassium sulfate: second step gained thermal material shrend potassium sulfate, after finishing, question response carries out Separation of Solid and Liquid, filtrate is sent potassium sulfate multi-effect evaporation system, is aluminium oxide and aluminosilicate byproduct after residue washing, Separation of Solid and Liquid, and cleaning solution returns for shrend potassium sulfate;
The 4th step: potassium sulfate---crystallisation by cooling: adopt saturated vapor evaporation and concentration the 3rd step gained leachate in multi-effect evaporator, be evaporated to potassium sulfate content in solution and be greater than 220g/L, then send cooler crystallizer to stir crystallisation by cooling this evaporated liquor, last Separation of Solid and Liquid obtains potassium product and crystalline mother solution, potassium sulfate is dried, packs, and crystalline mother solution returns to shrend potassium sulfate workshop section as shrend liquid.
2. a kind of method that in flotation tailing, alunite is produced potassium sulfate and byproduct thereof of utilizing according to claim 1, is characterized in that:
Described alunite flotation is that flotation tailing pulp adopts sodium carbonate to regulate pH=9.0～9.5, then add successively scattered inhibitor waterglass 400g/t～800g/t to stir 2min～3min, collecting agent oleic acid 200g/t～400g/t and stir and under 1min～2min condition, roughly select 6min～9min and obtain alunite concentrate 1, roughly select the mine tailing of generation and throw tail; Alunite concentrate 1 is under 200g/t～400g/t condition, to carry out primary cleaning 4min～6min to obtain alunite concentrate 2 in waterglass addition, and the chats of selected generation is for the first time thrown tail; Alunite concentrate 2 is under 100g/t～300g/t condition, to carry out selected 3min～5min for the second time to obtain alunite concentrate 3 in waterglass addition, and the chats of selected generation is for the second time back to the alunite section of roughly selecting;
Described roasting is to adopt the alunite concentrate 3 of first step flotation gained to mix and ball processed with reducing agent, be that 570 DEG C～650 DEG C, time 15min～30min, reducing agent consumption calculate by alunite grade in temperature, by carrying out roasting under 1～3 times of condition adding of theoretical requirement;
Described shrend potassium sulfate is in L/S=3～5, under time 20min～60min condition, carries out, and after question response finishes, carries out Separation of Solid and Liquid;
Described potassium sulfate---when crystallisation by cooling, adopt multi-effect evaporator, under 120 DEG C～140 DEG C conditions of temperature, evaporate, when being greater than 220g/L, finishes potassium sulfate content evaporation when being evaporated in solution, and send cooler crystallizer to stir crystallisation by cooling this evaporation and concentration liquid, last Separation of Solid and Liquid obtains potassium product and crystalline mother solution, and crystalline mother solution returns to shrend potassium sulfate workshop section as shrend liquid.
3. a kind of method that in flotation tailing, alunite is produced potassium sulfate and byproduct thereof of utilizing according to claim 1 and 2, is characterized in that: affiliated reducing agent is coke or coal or black oil.
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| CN104313346B (en) * | 2014-10-30 | 2016-03-30 | 北京矿冶研究总院 | Process for recovering aluminum, potassium and gallium by quickly reducing and desulfurizing alunite at high temperature |
| CN104475268A (en) * | 2014-12-03 | 2015-04-01 | 紫金矿业集团股份有限公司 | Method for recycling alunite from copper ore flotation tailings |
| CN106115743A (en) * | 2016-06-21 | 2016-11-16 | 新疆景美诺农业科技有限公司 | Potassium sulfate purifying technique |
| CN106830015A (en) * | 2017-03-28 | 2017-06-13 | 北京科技大学 | A kind of method for promoting alunite thermal decomposition to extract potassium sulfate |
| CN106882814B (en) * | 2017-04-20 | 2019-02-22 | 紫金矿业集团股份有限公司 | The method for preparing industrial metasilicate with discarded copper and sulfide tailings |
| CN112371713B (en) * | 2020-10-21 | 2022-03-01 | 紫金矿业集团股份有限公司 | Method for in-situ treatment of tailings of biological heap leaching field by using copper sulfide ore flotation tailings |
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| CN101913633B (en) * | 2010-07-07 | 2014-12-10 | 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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