CN101108738A - Manufacturing technique of potassium muriate heat of evaporation separating cooling crystallization process - Google Patents

Manufacturing technique of potassium muriate heat of evaporation separating cooling crystallization process Download PDF

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Publication number
CN101108738A
CN101108738A CNA2007100659362A CN200710065936A CN101108738A CN 101108738 A CN101108738 A CN 101108738A CN A2007100659362 A CNA2007100659362 A CN A2007100659362A CN 200710065936 A CN200710065936 A CN 200710065936A CN 101108738 A CN101108738 A CN 101108738A
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China
Prior art keywords
evaporation
solid
potassium
bittern
cooling
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CNA2007100659362A
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Chinese (zh)
Inventor
费宣
邢伟
王雁彬
闫光文
高松
何乾
苏勇
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YUNNAN ZHONGLIAO MINING DEVELOPMENT INVESTMENT Co Ltd
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YUNNAN ZHONGLIAO MINING DEVELOPMENT INVESTMENT Co Ltd
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Application filed by YUNNAN ZHONGLIAO MINING DEVELOPMENT INVESTMENT Co Ltd filed Critical YUNNAN ZHONGLIAO MINING DEVELOPMENT INVESTMENT Co Ltd
Priority to CNA2007100659362A priority Critical patent/CN101108738A/en
Publication of CN101108738A publication Critical patent/CN101108738A/en
Pending legal-status Critical Current

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  • Fertilizers (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

A potassium chloride evaporation thermal separation and cooling crystallization process is provided. The technological process of the invention is that the potassium-rich bittern unsaturated gained by well drilling thermosol and is directly adopted to be led into the evaporation system; the bittern is heated to 70 DEG C. to 120 DEG C. by steam; the control separator of the evaporation system has internal pressure between -0.05MPa to -0.09MPa; the sodium chloride reaches the oversaturated state through evaporation for 10min to 40min; the slurry forming the solid liquid through natural crystallization is first sent into a buffer vessel to settle for a short time, and the thermal filtering separation is carried out by centrifugal separation method under high temperature of 60 DEG C. to 100 DEG C., and then the cooling crystallization is carried out with temperature controlled between 10 DEG C. and 30 DEG C., and then solid liquid separation is carried out by centrifugal separation method to gain solid potassium chloride. The invention has the excellent advantages of being reliable in technology, comforming to the national standard, being short in process flow, low in production cost, free from pollution effluent and good in environment protection.

Description

Manufacturing technique of potassium muriate heat of evaporation separating cooling crystallization process
Technical field: the invention belongs to salt chemical engineering and potassium chloride fertilizer technical field of producing.
Background technology: sylvite production has very long history, and great majority are raw material with the sylvite all, mainly adopt floatation process.The floatation process technology is a most widely used production technology during current sylvite is produced.Mainly be to be that sylvite or carnallitite are ground into certain particle, add chemical flotation agent, utilize the different wetting ability of mineral substance (degree that ore is wetted), carry out separating process solid materials.The salt lake potash fertilizer of Xing Qiing is raw material with the salt lake intercrystalline bittern subsequently, and by the spontaneous evaporation of evaporating brine of big area salt pan, the carnallitite that obtains carries out flotation, obtains Repone K through the filter solid-liquid separation.Above-mentioned production technique great majority all need the big area salt pan to evaporate brine, and technical process is longer, invest bigger, higher to the carnallitite specification of quality, and, used after the flotation agent, the discharging of waste water brings very big influence to environmental protection problem.So this technology only is applicable to that usually some are more remote, the area that environmental protection requirement is relatively low.And present under the situation of paying attention to environment protection day by day, this technology has belonged to the technology of careful employing.
Summary of the invention: purpose of the present invention just in order to overcome the weak point that above-mentioned existing Repone K production technique exists, and provides a kind of manufacturing technique of potassium muriate heat of evaporation separating cooling crystallization process.Processing method of the present invention is: directly adopt the unsaturated potassium-rich brine that the drilling well thermosol is obtained to introduce vapo(u)rization system, with steam bittern is heated to 70~120 ℃, the control separator internal pressure that makes vapo(u)rization system-0.05~-0.09MPa between, evaporation through 10~40 minutes, make sodium-chlor reach hypersaturated state, again spontaneous nucleation is come out to form solid-liquid slip together and send into a dashpot earlier, carry out the short period of time sedimentation, under 60~100 ℃ high temperature, adopt centrifugal separation to carry out heat filtering and separate; Carry out crystallisation by cooling then, the temperature of crystallisation by cooling is controlled at 10~30 ℃, and subcooling obtains the solid potassium chloride crystallization, re-uses centrifugal separation and carries out solid-liquid separation, obtains solid Repone K.This Repone K product meets the requirement of standard GB 6549-1996, and promptly potassium oxide content is greater than 54%, and most of product has surpassed the superior product standard, and potassium oxide content is greater than 62%.Subcooling obtains the solid potassium chloride crystallization, and through the whizzer solid-liquid separation, solid materials can reach the product requirement of qualified Repone K.And the magnesium chloride solubleness in the bittern is bigger, still is deposited in the mother liquor, can deliver to the down-hole as weighting material.
The beneficial effect of the invention is: technology is reliable, obtains solid Repone K product and meets national standard; Technical process is short, greatly reduces production cost; The non-pollution discharge thing is particularly conducive to environment protection.
Further set forth content of the present invention below in conjunction with drawings and Examples.
Description of drawings: Fig. 1 is a specific embodiment of the invention process flow sheet.
Embodiment: embodiment one is about about 60 ℃ from the brine temperature of adopting defeated halogen operation and sending here, and bittern is introduced into dashpot, and typical component is (%): NaCl8.40, KCl7.60, MgCl 213.80.With the bittern transferpump undersaturated bittern is delivered to vapo(u)rization system, with steam bittern is heated to 100 ℃, control separator internal pressure is at-0.05MPa, through the evaporation of 15 fens clock times, make sodium-chlor reach hypersaturated state, spontaneous nucleation comes out to form solid-liquid slip together; Slip is introduced into a subsider, carries out the short period of time sedimentation, carries out heat filtering with whizzer and separate under 80 ℃ temperature, and slip is separated into Industrial Salt and mother liquor.Mother liquor carries out crystallisation by cooling by crystallizer again, and the temperature of crystallisation by cooling is controlled at 30 ℃, and re-use whizzer the mother liquor of crystallisation by cooling is carried out solid-liquid separation, thus the qualified Repone K product that obtains, and meet the requirement of standard GB 6549-1996.
Embodiment two is about about 60 ℃ from the brine temperature of adopting defeated halogen operation and sending here, and typical component is (%): NaCl8.40, KCl7.60, MgCl 213.80.With the bittern transferpump undersaturated bittern is delivered to vapo(u)rization system, with steam bittern is heated to 78 ℃, control separator internal pressure is at-0.08MPa, through the evaporation of 30 fens clock times, make sodium-chlor reach hypersaturated state, spontaneous nucleation comes out to form solid-liquid slip together; Slip is introduced into a subsider, carries out the short period of time sedimentation, carries out heat filtering with whizzer and separate under 60 ℃ temperature.The temperature of crystallisation by cooling is controlled at 20 ℃, uses whizzer to carry out solid-liquid separation, and the qualified Repone K product that obtains meets the requirement of standard GB 6549-1996, records chemical constitution: NaCl2.44%, KCl95.13%, MgCl 20.22%, H 2O2.16%.KCE content is amounted to potassium oxide and is about 60%.
Embodiment three is about about 60 ℃ from the brine temperature of adopting defeated halogen operation and sending here, and typical component is (%): NaCl8.40, KCl7.60, MgCl 213.80.With the bittern transferpump undersaturated bittern is delivered to vapo(u)rization system, with steam bittern is heated to 120 ℃, control separator internal pressure is at-0.09MPa, through the evaporation of 40 fens clock times, make sodium-chlor reach hypersaturated state, spontaneous nucleation comes out to form solid-liquid slip together; Slip is introduced into a dashpot, carries out the short period of time sedimentation, carries out heat filtering with whizzer and separate under 70 ℃ temperature.The temperature of crystallisation by cooling is controlled at 10 ℃, uses whizzer to carry out solid-liquid separation, and the qualified Repone K product that obtains meets the requirement of standard GB 6549-1996.
Potassium-rich brine comes from adopting defeated halogen operation, enters dashpot.Potassium-rich brine is delivered to the opening for feed of vaporizer bottom with the bittern transferpump.The vaporizer steam heating, constantly circulation, the high-temperature bittern through evaporation and concentrating is pumped into the separation buffer jar with high-temperature bittern, carries out solid-liquid separation to the heat filtering machine again.Solid is byproduct industrial salt (an industrial sodium-chlor), and liquid flows automatically to mother liquor tank, is pumped into cooling crystallizer with mother liquor again.In overcooled mother liquor, a large amount of solid potassium chlorides crystallize out, and carry out solid-liquid separation with whizzer again.The chemical ingredients of solid materials has reached the requirement of qualified Repone K product, for packaged convenience, can further carry out drying with hot air fluidized bed, and packing enters finished goods warehouse then.Also can directly pack and enter the finished goods warehouse pile.Liquid returns adopts defeated halogen operation, be made into leaching solution after, inject the down-hole through heating.

Claims (1)

1. manufacturing technique of potassium muriate heat of evaporation separating cooling crystallization process, it is characterized in that, technological process of the present invention is: the unsaturated potassium-rich brine that directly adopts the drilling well thermosol to obtain is introduced vapo(u)rization system, with steam bittern is heated to 70~120 ℃, the control separator internal pressure that makes vapo(u)rization system-0.05~-0.09MPa between, evaporation through 10~40 minutes, make sodium-chlor reach hypersaturated state, again spontaneous nucleation is come out to form solid-liquid slip together and send into a dashpot earlier, carry out the short period of time sedimentation, under 60~100 ℃ high temperature, adopt centrifugal separation to carry out heat filtering and separate; Carry out crystallisation by cooling then, the temperature of crystallisation by cooling is controlled at 10~30 ℃, re-uses centrifugal separation and carries out solid-liquid separation, obtains solid Repone K.
CNA2007100659362A 2007-06-05 2007-06-05 Manufacturing technique of potassium muriate heat of evaporation separating cooling crystallization process Pending CN101108738A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2465203C2 (en) * 2011-01-13 2012-10-27 Закрытое акционерное общество ВНИИ Галургии (ЗАО ВНИИ Галургии) Method of producing potassium chloride
CN103086402A (en) * 2013-01-22 2013-05-08 齐保冉 Environment-friendly treating device and process for concentrated waste liquor obtained after evaporation of pesticide and resin chemicals
CN103193252A (en) * 2013-04-24 2013-07-10 化工部长沙设计研究院 Method for producing potassium chloride by adopting carnallite hot-melt brine
CN110002776A (en) * 2019-03-25 2019-07-12 浙江红狮环保股份有限公司 A kind of online dry method dechlorination process
CN114735722A (en) * 2022-03-11 2022-07-12 苏州乔发环保科技股份有限公司 Potassium-rich low-sodium salt recycling process

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RU2465203C2 (en) * 2011-01-13 2012-10-27 Закрытое акционерное общество ВНИИ Галургии (ЗАО ВНИИ Галургии) Method of producing potassium chloride
CN103086402A (en) * 2013-01-22 2013-05-08 齐保冉 Environment-friendly treating device and process for concentrated waste liquor obtained after evaporation of pesticide and resin chemicals
CN103086402B (en) * 2013-01-22 2014-02-26 齐保冉 Environment-friendly treating device and process for concentrated waste liquor obtained after evaporation of pesticide and resin chemicals
CN103193252A (en) * 2013-04-24 2013-07-10 化工部长沙设计研究院 Method for producing potassium chloride by adopting carnallite hot-melt brine
CN103193252B (en) * 2013-04-24 2014-06-25 化工部长沙设计研究院 Method for producing potassium chloride by adopting carnallite hot-melt brine
CN110002776A (en) * 2019-03-25 2019-07-12 浙江红狮环保股份有限公司 A kind of online dry method dechlorination process
CN114735722A (en) * 2022-03-11 2022-07-12 苏州乔发环保科技股份有限公司 Potassium-rich low-sodium salt recycling process

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