CN1094466C - Method of extracting potassium chloride from mixed ore of sylvine and carnallite - Google Patents

Method of extracting potassium chloride from mixed ore of sylvine and carnallite Download PDF

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CN1094466C
CN1094466C CN99114004A CN99114004A CN1094466C CN 1094466 C CN1094466 C CN 1094466C CN 99114004 A CN99114004 A CN 99114004A CN 99114004 A CN99114004 A CN 99114004A CN 1094466 C CN1094466 C CN 1094466C
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ore
carnallitite
sylvite
ore deposit
repone
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CN1259486A (en
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宋文义
刘毓
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LIANYUNGANG DESIGN INST MINIST
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Abstract

The present invention relates to a method for extracting potassium chloride from the mixed ore of sylvinite and carnallite. After the mixed ore is pulverized, saturated bittern is added to the pulverized mixed ore until the ore milling concentration thereof is 40 to 70%, and the mixed ore is ground to ore pulp with the particle diameter less than or equal to 3mm; the right amount of fresh water for dissolving magnesium chloride is calculated according to the content of the magnesium chloride, and based on 1.1 to 1.3 times of the calculated value, the fresh water is added in the ore pulp; then, the saturated bittern is added again for regulating the pulp density to 20 to 40% for flotation, and the solid potassium chloride product is obtained after filtering and drying. Environment pollution caused by waste tail salt and the mixed ore precipitated from the unsaturated bittern is eliminated, and the present invention has the advantages of low cost, obvious benefits, simple manufacturing process, low energy consumption and no pollution.

Description

From the mix method of ore deposit extracting Repone K of sylvite with carnallitite
The present invention relates to a kind of extracting method of alkali metal compound, particularly extract the method for Repone K.
In the prior art, the process of producing Repone K with potassium chloride-type brine is: potassium chloride-type brine is shone evaporation concentration to the sodium-chlor drop out point through the beach, separate bittern, with isolated bittern beach shine to the carnallitite point be E point bittern, separate E point bittern again, continuing the beach solarization and make carnallitite, is raw material with the carnallitite again, therefrom extracts Repone K.The problem of its existence is: after extracting Repone K, the tail washings beach of discharge is shone into a large amount of tail salt and is gone out of use; Moreover, shining evaporation concentration through the beach to sodium-chlor point at bittern, carnallitite point bittern is that the mineral that E point bittern is separated out before are called the mixing ore deposit that unsaturated bittern is separated out.The mixing ore deposit that these depleted tail salt and unsaturated bittern are separated out all is potassium magnesium mixed salt mineral, all belongs to the ore deposit of mixing of sylvite and carnallitite, and the content of its useful composition Repone K fluctuates in the 5%-30% scope.But their xln granularity is very big, and hardness is big, and valuable mineral and gangue mineral symbiosis are tight, and for a long time, people can't separate the useful composition Repone K in the mixed mineral of these sylvites and carnallitite effectively.Thereby they all are abandoned as waste material.At present, as the area, salt lake, Qinghai of China, pile up like a mountain in the mixing ore deposit that discarded tail salt that the factory of Repone K discharges in the process of producing Repone K and unsaturated bittern are separated out, can't handle, both pollute environment, wasted resource again, become puzzlement people a great problem for many years.
The objective of the invention is at the deficiencies in the prior art, proposed a kind of from the method for effectively extracting Repone K the ore deposit of mixing of sylvite with carnallitite.
The objective of the invention is to reach by following technical scheme, the present invention is a kind of from the mix method of ore deposit extracting Repone K of sylvite with carnallitite, be characterized in the sylvite of salt-field collection and carnallitite mixed the ore deposit after fragmentation, add Repone K, sodium-chlor, the saturated bittern that magnesium chloride is all saturated transfers to the ore milling concentration of 40-70% by weight percentage, be milled to the ore pulp that solid grain size is less than or equal to 3 millimeters, sample examination obtains the content of magnesium chloride in the solid-like, according to quaternary salt-water system phasor, calculate the theoretical value of the fresh water amount of just dissolving magnesium chloride, 1.1-1.3 by this theoretical value doubly adds fresh water in the good ore pulp of mill, decompose solid-phase chlorination magnesium wherein, add Repone K in the material after decomposing again, sodium-chlor, the saturated bittern that magnesium chloride is all saturated, size mixing by weight percentage to the pulp density of 20%-40% and carry out flotation, with the concentrate foam that floatingly selects after filtration, drying obtains the solid potassium chloride product.
The present invention repeatedly carries out beneficiation test through the mixing ore deposit that the discarded tail salt and the unsaturated bittern of the discharge of area, salt lake, China Qinghai Repone K factory are separated out, work out the particle size range of sylvite and the best material ore dressing that mixes the ore deposit of carnallitite, make the Repone K monomer in the ore deposit of mixing of sylvite and carnallitite separate grain and come out.Simultaneously, reasonably controlled the fresh water amount that has added when decomposing magnesium chloride, made the sylvite effectively be separated to liquid phase, and that Repone K farthest remains on is solid-state with the magnesium chloride that mixes in the ore deposit of carnallitite, guaranteed that Repone K can obtain efficient recovery in the floatation process, the rate of recovery reaches higher scope.
Purpose of the present invention can also further reach by following scheme.Aforesaid from the mix method of ore deposit extracting Repone K of sylvite with carnallitite, be characterized in, in floatation process, collecting agent is selected stearylamine for use, consumption is that sylvite of gathering per ton uses 50-150 gram stearylamine with the ore deposit of mixing of carnallitite, inhibitor is selected carboxymethyl cellulose for use, and consumption is a sylvite of gathering per ton.Use 20-100 gram carboxymethyl cellulose with the ore deposit of mixing of carnallitite, flotation flowsheet is that one-level is roughly selected, one-level is scanned, secondary is selected.Adopt such flotation mode further to improve the rate of recovery of Repone K, reduced production cost again.
Purpose of the present invention can also further reach by following scheme.The aforesaid method of extracting Repone K the ore deposit of mixing from sylvite and carnallitite, the mother liquor that is characterized in the filtrate of concentrate after the flotation and mine tailing recycle as saturated bittern or shine through the beach and separate out new sylvite and do the new raw material use with the ore deposit of mixing of carnallitite.
The present invention compared with prior art, because the mixing ore deposit that the raw materials for production that use are separated out as the discarded tail salt and the unsaturated bittern of Repone K factory, not only removed the pollution of mixing ore deposit that discarded tail salt and unsaturated bittern separates out to environment, solved a puzzlement people hang-up for many years, and made full use of resource, turn waste into wealth, the cost of the Repone K product of producing is very low.Its economic benefit and social benefit are very remarkable.Technological process of the present invention is simple simultaneously, and facility investment is few, and energy consumption is low, and is pollution-free.Adopt technical process of the present invention, the purity of the Repone K product that obtains reaches 85%, and the yield of Repone K all reaches 45%.
Fig. 1 is a process flow diagram of the present invention.Fig. 2 is Na, K, Mg//Cl-H 2O quaternary salt-water system isothermal phase diagram.
Embodiment one.The following examples have further described summary of the invention of the present invention.In the present embodiment, the tail salt solution that raw materials for production are selected from Qinghai potash fertilizer plant Repone K flotation mill shines the tail salt of system through spontaneous evaporation, be sylvite and the ore deposit of mixing of carnallitite, its major ingredient that mixes the ore deposit is: contain Repone K 26.85%, sodium chloride-containing 61.08%, contain magnesium chloride 5.76%, sulfur acid calcium 1.56%.The sylvite of salt-field collection is restrained behind the crusher machine of broken ore deposit with the ore deposit 300 of mixing of carnallitite, add Repone K, sodium-chlor, the saturated bittern that magnesium chloride is all saturated transfers to 60% ore milling concentration by weight percentage, be milled to the ore pulp that solid grain size is less than or equal to 0.15 millimeter through ore mill, the content that the resampling chemical examination obtains magnesium chloride in the solid-like is 5.76%, according to quaternary salt-water system phasor, the theoretical value that calculates the fresh water amount of just dissolving magnesium chloride is 20 grams, 1.2 times by this theoretical value add fresh water 24 grams in the good ore pulp of mill, decompose solid-phase chlorination magnesium wherein, add Repone K in the material after decomposing again, sodium-chlor, the saturated bittern that magnesium chloride is all saturated, size mixing by weight percentage to 30% pulp density and carry out flotation, in floatation process, collecting agent is selected stearylamine for use, consumption is that sylvite of gathering per ton uses 150 gram stearylamines with the ore deposit of mixing of carnallitite, inhibitor is selected carboxymethyl cellulose for use, consumption is that sylvite of gathering per ton uses 100 gram carboxymethyl celluloses with the ore deposit of mixing of carnallitite, and flotation flowsheet is that one-level is roughly selected, one-level is scanned, secondary is selected.The mother liquor of the filtrate of concentrate and mine tailing recycles as saturated bittern or separates out new sylvite through the beach solarization and do the new raw material use with the ore deposit of mixing of carnallitite after the flotation.With the concentrate foam that floatingly selects after filtration, drying, obtain the solid potassium chloride product, gained 83.24 gram Repone K products, purity reaches 90%, the Repone K rate of recovery is 93%.
Embodiment two.The following examples continue to describe summary of the invention of the present invention, in the present embodiment, raw materials for production are selected from east, Qinghai high-quality Repone K factory and shine the mixing ore deposit that unsaturated bittern is separated out in the pond in advance, it also is sylvite and the ore deposit of mixing of carnallitite, its major ingredient that mixes the ore deposit is: contain Repone K 14.85%, sodium chloride-containing 48.40%, contain magnesium chloride 10.19%, sulfur acid calcium 1.44%, the sylvite of gathering is restrained behind the crusher machine of broken ore deposit with the ore deposit 300 of mixing of carnallitite, add Repone K, sodium-chlor, the saturated bittern that magnesium chloride is all saturated transfers to 40% ore milling concentration by weight percentage, be milled to the ore pulp that solid grain size is less than or equal to 0.7 millimeter through ore mill, the content that the resampling chemical examination obtains magnesium chloride in the solid-like is 10.19%, according to quaternary salt-water system phasor, the theoretical value that calculates the fresh water amount of just dissolving magnesium chloride is 55 grams, 1.1 times by this theoretical value add fresh water 60.5 grams in the good ore pulp of mill, decompose solid-phase chlorination magnesium wherein, add Repone K in the material after decomposing again, sodium-chlor, the saturated bittern that magnesium chloride is all saturated, size mixing by weight percentage to 20% pulp density and carry out flotation, in floatation process, collecting agent is selected stearylamine for use, consumption is that sylvite of gathering per ton uses 50 gram stearylamines with the ore deposit of mixing of carnallitite, inhibitor is selected carboxymethyl cellulose for use, consumption is that sylvite of gathering per ton uses 20 gram carboxymethyl celluloses with the ore deposit of mixing of carnallitite, and flotation flowsheet is that one-level is roughly selected, one-level is scanned, secondary is selected.With the concentrate foam that floatingly selects after filtration, drying, obtain the solid potassium chloride product, gained 30.06 gram Repone K products, purity reaches 88.93%, the Repone K rate of recovery is 60%.
Embodiment three.The following examples continue to describe summary of the invention of the present invention.In the present embodiment, in the present embodiment, the tail salt solution that raw materials for production are selected from salt lake, Qinghai Repone K flotation mill shines the tail salt of system through spontaneous evaporation, it is sylvite and the ore deposit of mixing of carnallitite, its major ingredient that mixes the ore deposit is: contain Repone K 26.17%, sodium chloride-containing 62.3%, contain magnesium chloride 5.31%, sulfur acid calcium 1.65%, the sylvite of gathering is restrained behind the crusher machine of broken ore deposit with the ore deposit 300 of mixing of carnallitite, add Repone K, sodium-chlor, the saturated bittern that magnesium chloride is all saturated transfers to 70% ore milling concentration by weight percentage, be milled to the ore pulp that solid grain size is less than or equal to 3 millimeters through ore mill, the content that the resampling chemical examination obtains magnesium chloride in the solid-like is 5.31%, according to quaternary salt-water system phasor, the theoretical value that calculates the fresh water amount of just dissolving magnesium chloride is 21.5 grams, 1.3 times by this theoretical value add fresh water 27.95 grams in the good ore pulp of mill, decompose solid-phase chlorination magnesium wherein, add Repone K in the material after decomposing again, sodium-chlor, the saturated bittern that magnesium chloride is all saturated, size mixing by weight percentage to 40% pulp density, carry out conventional flotation by the method for prior art.With the concentrate foam that floatingly selects after filtration, drying, obtain the solid potassium chloride product, gained 41.6 gram Repone K products, purity reaches 85.95%, the Repone K rate of recovery is 45.5%.

Claims (3)

1, a kind of from the mix method of ore deposit extracting Repone K of sylvite with carnallitite, it is characterized in that the sylvite of salt-field collection and carnallitite mixed the ore deposit after fragmentation, add Repone K, sodium-chlor, the saturated bittern that magnesium chloride is all saturated transfers to the ore milling concentration of 40-70% by weight percentage, be milled to the ore pulp that solid grain size is less than or equal to 3 millimeters, sample examination obtains the content of magnesium chloride in the solid-like, according to quaternary salt-water system phasor, calculate the theoretical value of the fresh water amount of just dissolving magnesium chloride, 1.1-1.3 by this theoretical value doubly adds fresh water in the good ore pulp of mill, decompose solid-phase chlorination magnesium wherein, add Repone K in the material after decomposing again, sodium-chlor, the saturated bittern that magnesium chloride is all saturated, size mixing by weight percentage to the pulp density of 20%-40% and carry out flotation, with the concentrate foam that floatingly selects after filtration, drying obtains the solid potassium chloride product.
2, according to claim 1 from the mix method of ore deposit extracting Repone K of sylvite with carnallitite, it is characterized in that in floatation process, collecting agent is selected stearylamine for use, consumption is that sylvite of gathering per ton uses 50-150 gram stearylamine with the ore deposit of mixing of carnallitite, inhibitor is selected carboxymethyl cellulose for use, consumption is that sylvite of gathering per ton uses 20-100 gram carboxymethyl cellulose with the ore deposit of mixing of carnallitite, and flotation flowsheet is that one-level is roughly selected, one-level is scanned, secondary is selected.
3, the method for extracting Repone K the ore deposit of mixing from sylvite and carnallitite according to claim 1, the mother liquor that it is characterized in that the filtrate of concentrate after the flotation and mine tailing recycle as saturated bittern or shine through the beach and separate out new sylvite and do the new raw material use with the ore deposit of mixing of carnallitite.
CN99114004A 1999-01-04 1999-01-04 Method of extracting potassium chloride from mixed ore of sylvine and carnallite Expired - Lifetime CN1094466C (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101774612B (en) * 2009-12-24 2011-08-17 中国科学院青海盐湖研究所 Method for producing potassium chloride by using direct flotation process of third solid sylvinite
CN101474598B (en) * 2009-01-23 2012-10-24 云南省化工研究院 Method for flotation of potassium chloride from potassium salt mine
US11851340B2 (en) 2020-05-06 2023-12-26 Qinghai Institute Of Salt Lakes, Chinese Academy Of Sciences Method for preparing potassium chloride from carnallite

Families Citing this family (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101905895A (en) * 2010-08-10 2010-12-08 山西大学 Method for producing potassium chloride by using sylvite as raw material
CN101982412B (en) * 2010-11-09 2012-07-04 化工部长沙设计研究院 Process for extracting KCl coarse grains by carrying out flotation on solid sylvinite primary ores
CN102942196B (en) * 2012-11-29 2014-10-15 中国科学院地质与地球物理研究所 Dressing method for dense medium in carnallite ore
CN103787696B (en) * 2014-02-19 2016-03-02 中国科学院青海盐湖研究所 A kind of preparation method containing potassic fertilizer and containing K composite fertilizer
CN107381601B (en) * 2017-09-12 2019-07-19 化工部长沙设计研究院 A kind of method of high boron carnallite production KCl
CN107758696B (en) * 2017-12-08 2019-09-17 中国科学院青海盐湖研究所 A method of potassium chloride is prepared from the solid mineral of the magnesium of ammonium containing potassium
CN108752058A (en) * 2018-07-16 2018-11-06 青海盐湖工业股份有限公司 A kind of method and apparatus for producing potash fertilizer using carnallite based on on-line checking
CN108821312A (en) * 2018-07-27 2018-11-16 茫崖兴元钾肥有限责任公司 A method of using making from brine for potassium chloride
CN109647631B (en) * 2018-12-28 2020-09-04 青海盐湖工业股份有限公司 Utilization method and utilization system of reverse flotation tail salt foam
CN110028084B (en) * 2019-04-11 2021-09-07 中蓝长化工程科技有限公司 Method for improving recovery rate of potassium chloride by using mine water

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CN1034562A (en) * 1987-09-09 1989-08-09 黄平利 Process technique of artificial amber
US5057208A (en) * 1984-09-25 1991-10-15 Kali Und Salz Aktiengesellschaft Method for the production of potassium chloride with K2 O content of more than 55 weight percent
CN1063663A (en) * 1992-03-05 1992-08-19 化学工业部化工矿山设计研究院 Potassium chloride preparing by chloride type patassium brine
CN1065053A (en) * 1992-04-25 1992-10-07 天津长芦汉沽盐场 Low energy-consumption production method of refined potassium chloride

Patent Citations (4)

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US5057208A (en) * 1984-09-25 1991-10-15 Kali Und Salz Aktiengesellschaft Method for the production of potassium chloride with K2 O content of more than 55 weight percent
CN1034562A (en) * 1987-09-09 1989-08-09 黄平利 Process technique of artificial amber
CN1063663A (en) * 1992-03-05 1992-08-19 化学工业部化工矿山设计研究院 Potassium chloride preparing by chloride type patassium brine
CN1065053A (en) * 1992-04-25 1992-10-07 天津长芦汉沽盐场 Low energy-consumption production method of refined potassium chloride

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101474598B (en) * 2009-01-23 2012-10-24 云南省化工研究院 Method for flotation of potassium chloride from potassium salt mine
CN101774612B (en) * 2009-12-24 2011-08-17 中国科学院青海盐湖研究所 Method for producing potassium chloride by using direct flotation process of third solid sylvinite
US11851340B2 (en) 2020-05-06 2023-12-26 Qinghai Institute Of Salt Lakes, Chinese Academy Of Sciences Method for preparing potassium chloride from carnallite

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