CN1020271C - Technology and apparatus for united production of salt and potassium chloride - Google Patents

Technology and apparatus for united production of salt and potassium chloride Download PDF

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Publication number
CN1020271C
CN1020271C CN 89104904 CN89104904A CN1020271C CN 1020271 C CN1020271 C CN 1020271C CN 89104904 CN89104904 CN 89104904 CN 89104904 A CN89104904 A CN 89104904A CN 1020271 C CN1020271 C CN 1020271C
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salt
bittern
potassium chloride
evaporation
halogen
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CN 89104904
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CN1048685A (en
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王炳全
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PIZOWO CHEMICAL PLANT DALIAN
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PIZOWO CHEMICAL PLANT DALIAN
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D3/00Halides of sodium, potassium or alkali metals in general
    • C01D3/04Chlorides
    • C01D3/06Preparation by working up brines; seawater or spent lyes

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  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The present invention relates to an association technology of table salt and potassium chloride, which is a method that bittern which is obtained after the seawater is dried in the sun to manufacture sea salt is processed through evaporative crystallization, separation and bittern blending and is used for preparing sodium chloride and potassium chloride at the same time. In the technology, crystallized table salt is taken out in continuous multiple effect evaporation, and then, bittern-blending evaporation liquor is used for preparing the potassium chloride. The present invention mainly uses multiple-effect evaporating equipment with double effects, and the technology is mainly applied to the salt chemical production.

Description

Technology and apparatus for united production of salt and potassium chloride
Salt, potassium chloride co-production process is the bittern after seawater shines system sea salt, through evaporation, crystallization, separate, convert halogen, washing, decomposition, produce the method for sodium-chlor, Repone K simultaneously.Used major equipment is the mother liquor after consecutive evaporation concentrates bittern and separates salt simultaneously, forms the multifunctional evaporating equipment of coproduction flow process.
Existing technology of producing Repone K with bittern, write as leather nest chemical plant, Luda, Liaoning department of chemistry of college of education, " sea salt Chemical Manufacture ABC " book that light industry press publishes in April, 1978, the process of producing potassium chloride by halogen conversion method of record is according to the explained hereafter Repone K of converting halogen, evaporation, insulation sedimentation, crystallisation by cooling, decomposition washing.Isolated sal amarum when converting halogen, sodium chloride content is low, impurity is many.The also low industrial salt of grade just that sal amarum adds that the water spray washing obtains again.Convert halogen earlier, increase feed concentration revaporization moisture content, make the elevation of boiling point, heating evaporation heat exchange weak effect, energy consumption increases.What adopted is general two to imitate evaporation equipments, and the equipment drainage conduit is positioned at the bottom cone, and drainage conduit is easily stopped up, and liquid level between each is imitated, feeding discharging material control effect are bad.Other has 84 years the 2nd phases of " sea salt and chemical industry " magazine, new sodium-chlor, sal epsom, the Repone K joint process of visiting a literary composition record of salinization technological transformation inquired into, exploratory production craft step has only been proposed simply, be that first evaporation concentration bittern separates salt, mother liquor after the separation salt cools off the sal epsom of extracting again, and mother liquor is fit to convert halogen production Repone K again behind the separating magnesium sulphate.This technology is separated out with salt in a large number in order to prevent high and tow temperature salt, the evaporation dump temperature is the highest can only be about 111 ℃.After the mother liquor that cooling off extracts isolates sal epsom was converted halogen with old halogen, also further heating evaporation concentrated.The reheat evaporation of cooling back, energy loss.This technology does not propose salt purifying process process, the Repone K that contains in the salt, and sal epsom etc. can not reclaim extraction, make extraction yield reduce.Though this technology proposes to use triple effect evaporation equipment, the heat energy between two cover evaporation equipments can not utilize mutually, and material balance, thermal equilibrium are wayward.Also will convert halogen equipment between two cover evaporation equipments, overall device is many, complex structure.
More than in two kinds of technology, used bittern will shine through multiple, be concentrated to 30 ° of Be~31Be.It is bigger to shine the seepage losses of process raw material again, has reduced the extraction yield of total raw material, and Repone K, salt and other material output reduce.
The object of the present invention is to provide a kind of significant loss few, extraction yield is higher, the bittern coproduction salt of save energy, the processing method of Repone K; Provide technology employed coproduction multifunctional evaporating equipment.
Salt, potassium chloride co-production process of the present invention be with bittern through evaporation, crystallization, separate, convert the method that halogen is produced sodium-chlor, Repone K simultaneously.This technology still adopts bittern to go out salt through the heating evaporation crystallization, and salt is separated.The characteristics of this technology are: convert halogen when the mother liquor after the separation salt continues heating evaporation, old halogen is mixed with mother liquor, rather than convert halogen again after cooling off the sal epsom of extracting; Convert the halogen complete evaporation of liquid and settlement separately go out high and tow temperature salt (mixing salt) and isolate carnallitite through crystallisation by cooling again through being incubated, carnallitite is produced Repone K through decomposing washing.This technology is to take out crystallization salt in the middle of bittern mother liquor consecutive evaporation, converts halogen when taking out the mother liquid evaporation after the crystallization salt, to the mixed solution heating evaporation of mother liquor, old halogen.The technological process that do not cool in evaporative process has been saved energy consumption.Vaporization temperature before separating salt can reduce the subsidiary Repone K that folds not too together.Convert halogen in the time of heating evaporation, not only can guarantee magnesium potassium ratio, Repone K is separated out in the minimizing evaporation, can prevent that again the mixed liquor temperature from reducing, and separates out part Repone K, thereby reduces the loss of Repone K, improves the extraction yield of Repone K.
Technology of the present invention does not have particular requirement to the concentration of raw material bittern.Can use the bittern after the multiple solarization, also can directly use the clarification bittern after sea salt is shone in the field, beach, needn't carry out multiple solarization.Do not shine the seepage losses of process raw material again, not only improve the output of salt, Repone K, also can increase again the output of the bromine produced, magnesium chloride, anhydrous nitre, improved total extraction yield.Shine without multiple, the bittern boiling point that concentration is lower is low, the heating evaporation good effect of heat exchange.In the evaporation of salt precipitation phase, magnesium chloride is difficult for separating out, and has guaranteed to separate out the quality of salt.Isolated salt can further improve the quality of salt through the bittern countercurrent washing.Washing melts the impurity that is attached between salt grain surface and seam, takes away the sal epsom of particulate.Countercurrent washing liquid preferably sends back in the raw material bittern together heating evaporation, and the various materials that reclaim washings and wash out further improve extraction yield.Salt slurry after the back washing promptly can be made into the smart salt of secondary by general separating and dehydrating, drying.Salt is starched isolated liquid and can be mixed with the bittern that is used for back washing, returns in the back washing liquid, does not lose the useful matter in the liquid.Owing to adopted countercurrent washing salt, the heating evaporation discharge concentration of separating before the salt can be at 33~34Be, thereby increases the crystallization extraction yield of salt.
Convert halogen process part for further minimizing and separate out Repone K, the old halogen of converting halogen can pass through preheating.Preferably use the water of condensation preheating of vaporizer, generally can be preheating to about 90 ℃, thereby effectively utilized heat energy, saved energy consumption, improved the extraction yield of Repone K.Convert halogen and generally use crystallisation by cooling to isolate the old halogen of carnallitite, old halogen proportion is generally 36 ± 1Be '.The magnesium potassium ratio of converting halogen is still between 11~12.For guaranteeing in the end to evaporate and be incubated in the settling process, be difficult for separating out Repone K, the dump temperature of converting the halogen evaporation is the same with the evaporation dump temperature of general production Repone K, can be at 126 ± 1 ℃.Discharge concentration is at 36 ± 0.5 ° of B ' e.
In order to save energy consumption,, adopt two one multiple-effect evaporation of imitating according to process characteristic of the present invention.Last effect evaporation of salt crystallization before mother liquor after the separation salt is converted the halogen evaporation and separated salt all is an effect evaporation.These two steam that evaporate are all entered the 2nd effect evaporator heating of crystallization salt.Can make full use of heat energy like this, and form a whole set of consecutive evaporation process.
In order to guarantee the feed liquid balancing control of continuous heating evaporation, control the evaporation liquid level easily and effectively, the equipment that salt, potassium chloride co-production process of the present invention is used is controlled the countercurrent multi-effect evaporation equipment (having selected the multifunctional evaporating equipment and the liquid level controlling method of No. 88106806 Chinese invention patent application technology for use) of liquid level automatically for upflow tube.This multifunctional evaporating equipment last evaporator still is equipped with the bittern feed-pipe.1st effective evaporator still is equipped with the overflow drainage conduit, and other multiple-effect evaporators respectively are equipped with the upflow tube that is communicated with the fresh feed pump import.This multifunctional evaporating equipment constructional feature is: 1st effective evaporator is steam inlet tube, goes out pipe two vaporizers in parallel respectively that the steam of two vaporizers goes out the pipe parallel connection and is communicated with the 2nd effect evaporator steam inlet tube; In two vaporizers, a vaporizer overflow drainage conduit is connected with separator, and feed-pipe is communicated with the 2nd effect evaporator drainage conduit, and the feed liquid of 2nd effect evaporator is forwarded in this vaporizer, is discharged to separator behind the heating evaporation again; In two vaporizers, another vaporizer mother liquor feed-pipe is communicated with the liquid discharge pipe of separator, and the mother liquor after the separation salt is transported to this vaporizer, and this vaporizer has the input tube of old halogen, simultaneously in the old halogen input vaporizer.This equipment makes amount and the vaporization temperature of converting halogen evaporative crystallization high and tow temperature salt, by giving the steam of 2nd effect evaporator, directly influences the amount and the vaporization temperature of evaporative crystallization salt, makes the mother liquid evaporation amount and the vaporization temperature mutual restriction of separating the salt front and back, keeps balance.This equipment make the evaporative crystallization mixing salt exhaust vapour obtain utilizing at 2nd effect evaporator, heat energy is effectively utilized.Convert in the mother liquid evaporation device of halogen after separating salt and carry out, saved the independent halogen equipment of converting.Old halogen, mother liquor mixed solution obtain timely heating evaporation, have solved the material balance of converting between halogen steam output and the evaporative crystallization salinity.The equipment that the present invention is used, the salt comb of its separator can be communicated with the back washing bucket, the salt comb is fed the back washing bucket, the relative position of back washing bucket has also fed the bittern input tube, and the feed-pipe of last evaporator is communicated with the liquid discharge pipe of back washing bucket, back washing liquid is input in the last evaporator, with raw material bittern heating evaporation.
Compared with the prior art the present invention has following advantage:
1. the raw material bittern needn't not only improve sodium-chlor, Repone K output, and improve the output of the magnesium chloride of further extraction, anhydrous nitre, bromine etc. through multiple solarization, minimizing significant loss.
2. convert halogen, heating evaporation and carry out simultaneously, simplified technological process.Technological process increases the extraction yield of sodium-chlor, Repone K to some extent, energy efficient, reduces cost, and has increased the economic benefit of producing.
3. this processing unit is simple, and less investment has improved equipment, energy utilization rate.Operation of equipment is convenient, is convenient to grasp use.
Accompanying drawing has been represented the main technique and the equipment flowsheet of salt, potassium chloride co-production process of the present invention.
Further specify Processes and apparatus of the present invention below in conjunction with accompanying drawing.Import in the third effect evaporators 7 by feed-pipe 5 through the clarifying 28-31 of saturated sedimentation ° Be bittern, after heating evaporation falls part moisture content, be transported in the 2nd effect evaporator by transfering material pump 3 between imitating and feeding discharging material pipe.Continue heating evaporation and fall after the part moisture content, again by transfering material pump 6 and the feeding discharging material pipe that is communicated with between imitating be transported in the vaporizer 1 in two 1st effective evaporators 1,2, continue heating evaporation and fall part moisture content.Progressively evaporative crystallization is separated out salt.The heating of vaporizer 1 is to give birth to steam heating by the boiler that steam inlet tube imports.And two, triple-effect evaporator heating is that the steam of imitating evaporation before being imported by steam duct heats.When the feed liquid of 1st effective evaporator 1 reaches 33.5 ± 0.5B ' e, by upflow tube 9 in the vaporizer 1 and discharge pump 10 be discharged to carry out salt in wet cyclone 11 or the airtight settlement separator, mother liquor separates.The feed liquid that has a large amount of salt grains is separated into stiff salt slurry and mother liquor.Mother liquor enters in the vaporizer 2 through the liquid discharge pipe 12 of separator and 1st effective evaporator 2 feed-pipes 4 that are communicated with.In this simultaneously, through 36 ° of old halogen of B ' e of 90 ± 2 ℃ of water of condensation preheater 13 preheatings, the old halogen input tube 14 by vaporizer 2 enters vaporizer 2, mixes with mother liquor, converts halogen in vaporizer 2, and is heated evaporation.Guaranteed that mixeding liquid temperature can bust, Repone K has been reduced separate out.The old halogen that is blended into will make magnesium potassium ratio be stabilized in 11~12 scopes.Water of condensation preheater 13 is connected on old halogen input tube 14 and and imitates condensed water discharge pipe road 15.Boiling point is discharged to the insulation settling vessel to the feed liquid that is higher than overflow port continuously by the upflow tube in the vaporizer 2 16 under 126 ± 1 ℃ of (normal pressure) conditions in guaranteeing vaporizer 2, and the technology of finishing by evaporation in the general producing potassium chloride by halogen conversion method is produced Repone K again.Sedimentation goes out crystalline high and tow temperature salt (claiming mixing salt again) in the insulation settling vessel.Sedimentation goes out mother liquor behind the high and tow temperature salt again through cooling, and enters in another settlement separator, and the carnallitite that crystallisation by cooling is gone out is settlement separate to come out.Carnallitite dissolves other materials (based on sodium-chlor, magnesium chloride) through washing several times again, obtains Repone K.Make the Repone K of finished product again through glue dries.
Stiff salt slurry upper end in salt comb 17 is discharged to vertical back washing bucket 18 that separator 11 separates.19 outlets of bittern input tube are positioned at the bottom of the back washing bucket, to going up spray feed bittern, the salt slurry that back washing is sunk down.The floating low weight sal epsom particle of proportion of washing off of bittern, melt away the soluble impurity that is attached between salt grain surface and brilliant seam, and with they triple-effect evaporator feed-pipes 5 by liquid discharge pipe 20 on the back washing bucket and connection, be discharged in the triple-effect evaporator 7, with raw material bittern heating evaporation together, make washings obtain reclaiming.Macrobead salt is deposited to back washing bucket bottom through back washing.And deliver in the thickening wet cyclone by row salt pipe 21 and transferpump 22, carry out spinning liquid many from, table salt is made in isolated salt drying dehydration.The isolated liquid of spinning liquid is discharged to bittern input tube 19 by comb.
One imitates the steam inlet tube D of two vaporizer 1,2 interchanger 01, D 02Parallel connection together is communicated with the Boiler Steam comb.The steam comb D of vaporizer 1,2 evaporator rooms 11, D 12Also in parallel, and be communicated with the steam inlet tube of 2nd effect evaporator interchanger.The steam comb D of 2nd effect evaporator evaporation 20Be communicated with the steam inlet tube of triple-effect evaporator well heater.Use this cover Processes and apparatus, can reduce multiple solarization process seepage losses 25%, thereby volume increase Repone K, sodium-chlor and after the bromine, magnesium chloride, anhydrous nitre that produce again each 25%.The production of Repone K per ton can obtain six tons of civilian table salts of secondary, and the output value can increase by 40%, and benefit can increase by 36%.

Claims (7)

1, a kind of salt, potassium chloride co-production process in turn includes the following steps:
(1) bittern is isolated salt and mother liquor through heating evaporation,
(2) described salt bittern countercurrent washing,
(3) described mother liquor is converted halogen when continuing heating evaporation,
(4) convert the halogen complete evaporation of liquid through be incubated settlement separate go out high and tow temperature salt after, go out carnallitite through crystallisation by cooling again,
(5) carnallitite is produced Repone K through decomposing washing.
2, as the said salt, potassium chloride co-production process of claim 1, it is characterized in that: the bittern washings of countercurrent washing salt returns raw material bittern heating evaporation together.
3,, it is characterized in that bittern concentration is 28~31 ° of B ' e as the said salt, potassium chloride co-production process of claim 1.
4,, it is characterized in that the salt slurry parting liquid after the back washing mixes with the bittern that is used for back washing as the said salt, potassium chloride co-production process of claim 2.
5,, it is characterized in that heating evaporation adopts two one triple effect evaporation of imitating as the said salt, potassium chloride co-production process of one of claim 1 to 4.
6,, it is characterized in that converting the old halogen water of condensation preheating of halogen as the said salt, potassium chloride co-production process of claim 5.
7, the used equipment of salt, potassium chloride co-production process is the adverse current triple effect evaporation equipment that upflow tube is controlled liquid level automatically, it is characterized in that:
A. 1st effective evaporator is that steam inlet tube goes out pipe two vaporizers in parallel respectively, and steam in parallel goes out pipe and is communicated with at the 2nd effect evaporator steam inlet tube.
B. in two 1st effective evaporators, the overflow drainage conduit of a vaporizer is equipped with separator, and its feed-pipe is communicated with the 2nd effect evaporator drainage conduit, and the mother liquor feed-pipe that has another vaporizer of old halogen input tube is communicated with the liquid discharge pipe of described separator.
CN 89104904 1989-07-13 1989-07-13 Technology and apparatus for united production of salt and potassium chloride Expired - Fee Related CN1020271C (en)

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CN1020271C true CN1020271C (en) 1993-04-14

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1037338C (en) * 1993-06-29 1998-02-11 浙江大学 Method for producing multicomponent long effect compound fertilizer using k extracted from sea water with kieselguhr
CN102311131A (en) * 2010-07-09 2012-01-11 中国中轻国际工程有限公司 Process for co-producing potassium chloride and sodium chloride by sylvite brine evaporation method

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CN1056286C (en) * 1995-07-26 2000-09-13 李永康 Traditional Chinese medicine ointment for AIDS
CN100402427C (en) * 2005-06-01 2008-07-16 高崧耀 Method for producing potassium chloride crystal through solarization on large area of brine pan
CN102461860A (en) * 2010-11-17 2012-05-23 天津长芦汉沽盐场有限责任公司 Method for preparing edible salt from acrid bittern
CN104135904A (en) * 2012-01-19 2014-11-05 水技术国际公司 Settling chamber for separation of large, plugging particles upstream of a hydroclone
CN103496719A (en) * 2013-09-18 2014-01-08 天津长芦汉沽盐场有限责任公司 Method for improving granularity and purity of chemical salt byproducts of acrid bittern
CN105329918A (en) * 2015-12-02 2016-02-17 中盐工程技术研究院有限公司 Eleven-effect combined sodium and potassium preparation device
CN106693423A (en) * 2017-01-09 2017-05-24 中国海洋石油总公司 Bittern continuous evaporation system
CN112479231A (en) * 2020-12-21 2021-03-12 天津长芦汉沽盐场有限责任公司 Brine-blending method for producing potassium chloride by adopting triple-effect evaporation

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1037338C (en) * 1993-06-29 1998-02-11 浙江大学 Method for producing multicomponent long effect compound fertilizer using k extracted from sea water with kieselguhr
CN102311131A (en) * 2010-07-09 2012-01-11 中国中轻国际工程有限公司 Process for co-producing potassium chloride and sodium chloride by sylvite brine evaporation method

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