CN101134680A - Method for extracting active potassium from potash feldspar under normal pressure - Google Patents

Method for extracting active potassium from potash feldspar under normal pressure Download PDF

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CN101134680A
CN101134680A CNA2007100254934A CN200710025493A CN101134680A CN 101134680 A CN101134680 A CN 101134680A CN A2007100254934 A CNA2007100254934 A CN A2007100254934A CN 200710025493 A CN200710025493 A CN 200710025493A CN 101134680 A CN101134680 A CN 101134680A
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potassium
felspar sand
active potassium
active
reaction
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CN100564324C (en
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韩效钊
阎勇
吴春燕
徐超
陈敏
王忠兵
刘荃
张燕燕
于红
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Hefei University of Technology
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Abstract

The process of extracting active potassium from potash feldspar at normal pressure replaces potassium from low grade potash feldspar with inorganic salt in the system comprising dilute acid solution and swelled high hydroscopic resin network. The process includes mixing feldspar powder, with inorganic salt and high hydroscopic resin in the weight ratio of 1 to 5-12 to 0.05-0.25; adding inorganic acid solution in the solid/liquid ratio of 1 to 20-50 and reacting at 150-250 deg.c for 1-4 hr; adding water to dilute after reaction to leach out the replaced potassium, separating, concentrating and drying to obtain potash fertilizer containing K2O not less than 25 %. The process has potassium extracting rate not lower than 70 %. The present invention extracts active potassium from potash feldspar at low temperature and normal pressure on the principle that water has raised boiling water in high molecular network.

Description

A kind of method of in potassium felspar sand, extracting active potassium under the normal pressure
One, technical field
The present invention relates to a kind of method of extracting active inorganic elements in mineral, exactly is a kind of method of extracting active potassium in potassium felspar sand.
Two, background technology
China's potassium resource is not abundant, soluble potassium resource wretched insufficiency.1.16 hundred million tons of Qinghai sylvite reserves (KCl meter), potassium-rich brine ore bed KCl average grade 1.29%; 2.5 hundred million tons of Lop Nur, Xinjiang sylvite reserves (KCl meter), bittern KCl average grade 1.40%.China's soluble potassium salt reserves per capita only is 1/14 of world average level; And potassium application is to improve the crop quality greatest factor, causes a large amount of import potash fertilizer of having to, and at present, the external interdependency of China's potash fertilizer reaches more than 80%.
The explored water-soluble sylvite in the world mainly concentrates on a few countries such as Canada, Russia, Byelorussia, Germany, Israel, Jordan, though world's sylvite output greater than consumption, Potash Resources has monopoly, can form monopoly price.Therefore, improve China's potash fertilizer degree of self-sufficiency utmost point important meaning is arranged.
China's insoluble low grade potassium ore reserves surpasses 5,000,000,000 t K 2O (rolling over 8,000,000,000 t KCl), and be distributed widely in the agriculture production area.Wherein, based on potassium felspar sand, China's extracting potassium from potash feldspar technical study work starts from the fifties end, owing to lack mechanism research, technology development work is made slow progress.Typical at present operational path has: (1) vaporization at high temperature method is with the stove of preparing burden in proportion after the fragmentations such as potassium felspar sand, Wingdale, rhombspar, fluorite and coke.Fire box temperature is up to 1600 ℃, the K that evaporates 2CO in O and the stove 2Effect generates K 2CO 3(2) high-temperature sintering process is potassium felspar sand, additive to be mixed levigate, and the fusion roasting reaches the purpose of carrying potassium in High Temperature Furnaces Heating Apparatus, and temperature is about 1000 ℃.(3) fluorine decomposition method, be with fluorochemical or fluorine-containing auxiliary agent in inorganic acid medium, in decomposing of potassium feldspar below 200 ℃, process side reaction product potassium silicofluoride is water insoluble, simultaneously, the fluorine serious corrosion.(4) microbiological degradation method is to utilize auxiliary material and potassium felspar sand generation biochemical reactions such as microbial bacterial.This method advantage is that flow process is short, three-waste free discharge.But the fecundity of bacterial classification and vitality a little less than, be difficult to survive under field conditions (factors), also need to adopt genetically engineered further to screen and cultivate new bacterial strain.(5) hydro-thermal reaction method is in about 200 ℃, and additive and potassium felspar sand react under hydrothermal condition, need pressure exerting device.
The applicant has carried out fundamental research to potassium felspar sand, thereby the structure and the character of potassium felspar sand has been had deep understanding.Aluminium in the potassium felspar sand and silicon are all formed the coordination tetrahedron with oxygen, form firm tetrahedral network structure, and its chemical property stabilizer pole is not decomposed by any soda acid except that hydrofluoric acid under the normal temperature.But have bigger space in the potassium felspar sand structure significantly, under certain conditions, Ca 2+, Na +Deng the network-modifying ion K that can replace in the potassium felspar sand structure +
Three, summary of the invention
The present invention uses this reaction mechanism of ion-exchange the potassium in the potassium felspar sand to be changed into the active potassium that can be absorbed by crop, its objective is the low-grade potassium felspar sand of development and use, technical problem to be solved is to realize ion-exchange in normal pressure, free-floride and unlimited system.
The present invention makes ion-exchanger with the potassium of displacement in the potassium felspar sand with inorganic salt, and to be potassium felspar sand finish replacement(metathesis)reaction with inorganic salt to the scheme of design in dilute acid soln and the swollen High hydrophilous resin network system and realize effectively separating.
Technical scheme of the present invention comprises the pulverizing of raw material potassium felspar sand ore and mixing, swelling, reaction, lixiviate, separation, concentrate and unit process such as drying, and described mixing is meant that breeze, inorganic salt and High hydrophilous resin obtain compound by 1: 5~12: 0.05~0.25 quality than ground and mixed successively; Described swelling is exactly that to add concentration in compound be the mineral acid of 1~7wt%, the solid-liquid mass ratio with breeze count 1: 20~50; Described reaction is 150~250 ℃ and stirred 1~4 hour down; Reaction finishes back thin up lixiviate and goes out by metathetical potassium, separate at last, remove concentrate behind the exchanger, dry, obtain K 2The potash fertilizer of O 〉=25%.
The preferred breeze of the ratio of mixture of compound: inorganic salt: High hydrophilous resin is 1: 6~10: 0.10~0.20.
Preferred 2~the 6wt% of the concentration of mineral acid, solid-to-liquid ratio is in breeze preferred 1: 25~45.
Preferred 200~250 ℃ of reactions of temperature of reaction 2~3 hours.
High hydrophilous resin optimization polypropylene acid series is or/and polyacrylamide series High hydrophilous resin.Inorganic salt are selected from calcium chloride or sodium-chlor or sodium sulfate.
The mineral acid preferably phosphoric acid.
High hydrophilous resin has the network size structure, adsorbable own wt more than hundreds of times and even thousand times water and swelling, even being adsorbed extruding by network, water do not run off yet, can not vaporize more than 100 ℃ yet, can constitute the hydro-thermal reaction system of following 100 ℃~250 ℃ and open (uncovered) of normal pressure, thereby make inorganic salt under normal pressure, displace potassium in the potassium felspar sand.This process can be expressed from the next:
Figure A20071002549300041
The comparative advantages of present method and prior art are that prior art all is at high temperature or in the middle low temperature closed system to carry out, and often needs to use fluorine-containing auxiliary agent in the middle low temperature system.Present method is not used fluorine-containing auxiliary agent, the interior water boiling point rising principle of macromolecule network of utilizing high-absorbent material suction back swelling to form, and low-temperature atmosphere-pressure opens wide system is carried potassium system potash fertilizer in potassium felspar sand purpose in the realization.Potassium extraction yield 〉=70% in the potassium felspar sand.Present method has been opened up a new way for development and use China low grade potassium feldspar mineral.
Four, specific implementation method
Non-limiting examples is described below
1, raw material is prepared
Get ball milling after the potassium felspar sand fragmentation, it is standby to cross 200 mesh sieves.
Get industrial phosphoric acid, industrial calcium chloride, polyacrylic resin, standby;
2, preparation process
Get feldspar in powder, calcium chloride and sodium polyacrylate by 1: 8: 0.15 ground and mixed, obtaining compound drops in the extraction unit, stir the phosphoric acid solution that adds 40 part 4% down then and make the abundant swelling of polyacrylic resin, heating makes the swelling system be constant at 220 ℃, reaction 2h.Reaction end back adds a certain amount of water in reaction system and violent stirring makes by metathetical potassium automatic network internal diffusion to solution centrifugation; And in parting liquid, add in the proper amount of sodium hydroxide solution and acid solution and be settled out calcium; Cross the solution concentration drying that filters to remove behind the calcium hydroxide and obtain potash fertilizer, wherein K 2O 〉=25%.

Claims (7)

  1. One kind in potassium felspar sand normal pressure extract down the method for active potassium, with the potassium felspar sand is raw material, comprise pulverizing, mixing, swelling, reaction, leaching, separation, concentrate and dry, it is characterized in that: described mixing is exactly that potassium felspar sand breeze, inorganic salt and High hydrophilous resin are compared ground and mixed by 1: 5~12: 0.05~0.25 quality successively; Described swelling is exactly that to add concentration in compound be the inorganic acid solution of 1~7wt%, the solid-liquid mass ratio with breeze count 1: 20~50; Described reaction is 150~250 ℃ stirred 1~4 hour down, and described inorganic salt are selected from calcium chloride or sodium-chlor or sodium sulfate.
  2. 2. the method for the active potassium of extraction according to claim 1 is characterized in that: the mass ratio of potassium felspar sand breeze, inorganic salt and High hydrophilous resin is 1: 6~10: 0.10~0.20.
  3. 3. the method for the active potassium of extraction according to claim 1 and 2 is characterized in that: inorganic acid concentration is 2~6wt%.
  4. 4. the method for the active potassium of extraction according to claim 3 is characterized in that: the solid-to-liquid ratio that in compound, adds inorganic acid solution with breeze count 1: 25~45.
  5. 5. according to the method for claim 1 or the active potassium of 4 described extractions, it is characterized in that: reaction is 2~3 hours in the time of 200~250 ℃.
  6. 6. the method for the active potassium of extraction according to claim 5 is characterized in that: described High hydrophilous resin is selected from polyacrylic acid series resin or polyacrylamide series plastics.
  7. 7. according to the method for claim 1 or the active potassium of 6 described extractions, it is characterized in that: described mineral acid is a phosphoric acid.
CNB2007100254934A 2007-07-31 2007-07-31 A kind of method of in potassium felspar sand, extracting active potassium under the normal pressure Expired - Fee Related CN100564324C (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102432367A (en) * 2011-09-21 2012-05-02 安徽华岳矿物材料有限公司 Method for preparing mineral potash fertilizer with potassium feldspar
CN102701253A (en) * 2012-06-08 2012-10-03 四川大学 CO2 mineralization method capable of co-producing potassium-enriched solution by high temperature method
CN103172409A (en) * 2011-12-22 2013-06-26 清华大学 Process for preparing non-soluble potassium fertilizer by using potassium-bearing minerals
CN104671919A (en) * 2014-12-25 2015-06-03 牛政 Fertilizer processing process
CN105084395A (en) * 2015-08-05 2015-11-25 铜仁市万山区盛和矿业有限责任公司 Method for producing soluble potassium through potassium feldspar
CN111087204A (en) * 2019-12-31 2020-05-01 山西凯迪建材有限公司 Mineral admixture ternary cementing material and preparation method thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102432367A (en) * 2011-09-21 2012-05-02 安徽华岳矿物材料有限公司 Method for preparing mineral potash fertilizer with potassium feldspar
CN103172409A (en) * 2011-12-22 2013-06-26 清华大学 Process for preparing non-soluble potassium fertilizer by using potassium-bearing minerals
CN103172409B (en) * 2011-12-22 2014-07-23 清华大学 Process for preparing non-soluble potassium fertilizer by using potassium-bearing minerals
CN102701253A (en) * 2012-06-08 2012-10-03 四川大学 CO2 mineralization method capable of co-producing potassium-enriched solution by high temperature method
CN102701253B (en) * 2012-06-08 2014-05-14 四川大学 CO2 mineralization method capable of co-producing potassium-enriched solution by high temperature method
CN104671919A (en) * 2014-12-25 2015-06-03 牛政 Fertilizer processing process
CN105084395A (en) * 2015-08-05 2015-11-25 铜仁市万山区盛和矿业有限责任公司 Method for producing soluble potassium through potassium feldspar
CN111087204A (en) * 2019-12-31 2020-05-01 山西凯迪建材有限公司 Mineral admixture ternary cementing material and preparation method thereof

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