CN105727576B - One step produces the continuous evaporative crystallization system and method for big particle diameter food-grade potassium chloride crystal - Google Patents

One step produces the continuous evaporative crystallization system and method for big particle diameter food-grade potassium chloride crystal Download PDF

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CN105727576B
CN105727576B CN201610247323.XA CN201610247323A CN105727576B CN 105727576 B CN105727576 B CN 105727576B CN 201610247323 A CN201610247323 A CN 201610247323A CN 105727576 B CN105727576 B CN 105727576B
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potassium chloride
iii
separation chamber
crystal
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CN105727576A (en
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郭坤
杜宏德
刘胜
赵仕哲
梁恺
王辉
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Xian Aerospace Huawei Chemical and Biologic Engineering Co Ltd
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Xian Aerospace Huawei Chemical and Biologic Engineering Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D1/00Evaporating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D9/00Crystallisation
    • B01D9/0004Crystallisation cooling by heat exchange
    • 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
    • C01D3/14Purification

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Abstract

The present invention relates to the continuous evaporative crystallization system and method that a step produces big particle diameter food-grade potassium chloride crystal, system is made up of vapo(u)rization system and crystal system two parts, can a step continuously realize the production of large grained food grade potassium chloride, method includes:Klorvess Liquid is heated by vapo(u)rization system and concentrated, crystal system is then pumped to and carries out continuous evaporative crystallization, potassium chloride magma is obtained, the discharge of potassium chloride magma is delivered to buffer tank caching by growing the grain after terminating;Condition includes:Charging potassium chloride feed liquid is directly entered separation chamber's circulating line, mixed with a large amount of potassium chloride concentrates, the high saturated solution of high temperature is formed by two effect heat exchange, then it is allowed to be mixed with a large amount of potassium chloride magmas, potassium chloride temperature of charge and pressure are improved by external circulation heat exchanging, crystallizer flash concentration is sent into, crystallization separates out potassium chloride.The method provided according to the present invention, obtained food-grade potassium chloride crystal particle mean size is big, even particle size distribution, and yield is high.

Description

One step produce big particle diameter food-grade potassium chloride crystal continuous evaporative crystallization system and Method
Technical field
The invention belongs to evaporative crystallization technique field, and in particular to an a kind of step produces big particle diameter food-grade potassium chloride crystal Continuous evaporative crystallization system and method.
Background technology
Food-grade potassium chloride is white powder or colourless crystallization, and odorless, taste is salty, nontoxic, it is soluble in water, be dissolved in glycerine, it is micro- It is dissolved in ethanol.Food-grade potassium chloride is mainly used to produce Cardia Salt, and potassium is directly mended to meet human body, increases as savory agent and nutrition Tonic prevents people's excess ingestion salt partly to substitute salt;Pharmaceutically it is available for taking orally, water injection can also be prepared, rises To the effect of supplement or balanced human's potassium deficiency, health can also manufacture diuretics, prevent potassium deficiency disease drug.In addition, potassium chloride with Salt equally can be used in the food such as agricultural production, aquatic products, livestock products, fermentation, seasoning, can, instant food, can add in proportion In various food, indispensable effect is played to food tissue state, color, smell and taste and raw-food material cost control.
The production of food-grade potassium chloride crystal product mainly includes dissolving, crystallization, separation, dry and five processes of packaging, i.e., The saturated solution for preparing potassium chloride is dissolved by industrial grade potassium chloride first, saturated solution is then delivered to crystalline element and steamed Hair crystallization, obtains potassium chloride magma, then potassium chloride magma is delivered into centrifuge being centrifuged, and dries, and packs for sale.Its In, the evaporative crystallization of potassium chloride is most important, most crucial process, and evaporative crystallization obtains the quality of potassium chloride product, directly The granularity for having influence on food-grade potassium chloride product, purity and outward appearance are connect, therefore need to strictly control potassium chloride multiple-effect evaporation to crystallize work Skill flow, to obtain meeting the food-grade potassium chloride crystal product of user's request.
The main mode of production of current food-grade potassium chloride is " multiple-effect evaporation "+" crystallisation by cooling kettle ", the covering device be by Evaporation and Crystallization Procedure are separated, and are first concentrated Klorvess Liquid multiple-effect evaporation, then by concentrate by cooling Production obtains potassium chloride product.As industrially scalable constantly expands, equipment needed for food-grade potassium chloride crystallization processes With manually operate all than larger, due to the influence of artificial fluctuation of service factor, easily cause edible potassium chloride crystal product brilliant Body is tiny, size distribution is uneven, crystal product coalescence is serious, causes subsequent handling separation, washing, drying difficulty increase, it is impossible to Food potassium chloride producer is met to Potassium Chloride Product granularity and purity requirement.
The content of the invention
It is an object of the invention to provide the continuous evaporative crystallization system that an a kind of step produces big particle diameter food-grade potassium chloride crystal System and method, reduce hand labor intensity, improve production efficiency and energy utilization rate, so as to get food-grade potassium chloride crystal compared with Greatly, even particle size distribution, production cost reduction.
The technical solution adopted in the present invention is:
One step produces the continuous evaporative crystallization system of big particle diameter food-grade potassium chloride crystal, it is characterised in that:
Including vapo(u)rization system and crystal system two parts;
The vapo(u)rization system includes III effects circulating pump, III effects heat exchanger, III effect separation chambers and III effects discharging pump, I effects Circulating pump, I effects heat exchanger, I effects separation chamber;
The crystal system includes II effects circulating pump, II effects heat exchanger, II effects crystallizer, II effect transfering material pumps and crystallization discharging Pump;
Raw material is connected to the circulating line that III imitates separation chamber, and being delivered to III by circulating line imitates heat exchanger and III effects Separation chamber's charging aperture, III effect separation chamber's discharging opening connection III effect pump entries, III effect circulating-pump outlets are imitated with III to exchange heat Device charging aperture is connected, and III is imitated heat exchanger discharging opening and is connected with III effect separation chamber's recycle feeds mouthful, III effect separation chamber's bottom discharges Mouth connection III effect discharging pump intakes, III imitates the pump discharge that discharges and is connected to II effect crystallizer circulating lines, the outlet of II effect transfering material pumps I effect separation chamber's circulating lines are connected to, being delivered to I by circulating line imitates heat exchanger and I effect separation chamber's charging apertures, I effect separation Room discharging opening connection I effect pump entries, I is imitated circulating-pump outlet and is connected with I effect heat exchanger charging apertures, I effect heat exchanger discharging openings Mouthful be connected with I effect separation chamber's recycle feeds, I effect circulating lines, which draw branch road and are connected to II and imitate the circulating line of crystallizer, to be tied Crystalline substance, I effect separation chamber's overhead vapors outlet is connected to II effect heat exchanger shell pass imports, III effect separation chamber's overhead vapor outlet connections Cooled down to surface condenser;
Klorvess Liquid after concentration is delivered to the circulating line that II imitates crystallizer, and II effect heat exchange is delivered to through circulating line Device and II effect crystallizers, II effect crystallizer circulating line discharging openings are connected to the entrance that II imitates circulating pump, and II imitates going out for circulating pump Mouth connection II imitates the charging aperture of heat exchanger, the circulating line charging aperture of the discharging opening connection II effect crystallizers of II effect heat exchangers, II Imitate crystallizer separation chamber overhead vapor outlet connection III effect heat exchanger steam inlets, II effect crystallizer crystallisation chamber bottom discharges mouthful Connection crystallization discharging pump.Crystallisation cycle pipeline draws branch road imitates transfering material pump to II, and being delivered to I effects separation chamber by II effect transfering material pumps follows Endless tube road.
I effects heat exchanger, II effects heat exchanger, III effect heat exchanger shell pass outlet condensed water are connected to condensed water bucket caching.
Raw material is connected to the circulating line that III imitates separation chamber, sequentially enters II effect crystallizers and I effects separation chamber, then imitate from I Separation chamber enters II and imitates crystallizer, is in cross-flow passes with steam;
Or raw material is connected to the circulating line that III imitates separation chamber, II effect separation chambers and I effect crystallizers are sequentially entered, in I effects Crystallized in crystallizer, be in counter-current flow with steam;
Or raw material is connected to the circulating line that I imitates separation chamber, II effect separation chambers and III effect crystallizers are sequentially entered, in III Crystallized in effect crystallizer, be in co-current flow with steam.
One step produces the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal, it is characterised in that:
Comprise the following steps:
It is 30% ~ 36% that Klorvess Liquid is concentrated into potassium chloride mass percent concentration by vapo(u)rization system heating, then Potassium chloride concentrate pump is delivered into crystal system and carries out continuous evaporative crystallization, potassium chloride magma, growing the grain are obtained through evaporative crystallization The discharge of potassium chloride magma is delivered to buffer tank caching after end;
The condition of potassium chloride continuous evaporative crystallization includes:Charging potassium chloride feed liquid is directly entered separation chamber's circulating line, with A large amount of potassium chloride concentrates mixing, the high saturated solution of high temperature is formed by two effect heat exchange, then allows itself and a large amount of potassium chloride magmas Liquid is mixed, and potassium chloride temperature of charge and pressure are improved by external circulation heat exchanging, sends into crystallizer flash concentration, is allowed to crystallization and is separated out Potassium chloride.
It is 55 ~ 110 DEG C to be concentrated by evaporation afterchlorinate potassium temperature.
The mass ratio of system circulation amount and inlet amount is(50~150):1.
The residence time is 1 ~ 4h to potassium chloride in a crystallizer.
Potassium chloride discharging magma solid content is percent by volume 15 ~ 40%.
A step produces the food-grade of the continuous evaporative crystallization method production of big particle diameter food-grade potassium chloride crystal as mentioned Potassium chloride.
The present invention has advantages below:
Crystallizer of the present invention can make the region that degree of supersaturation is produced be respectively placed in crystallizer with crystal growth area Two at, crystal fluidized suspension in circulating mother liquor provides good condition for crystal growth, can produce granularity larger And uniform crystal.
The invention provides Continuous Cooling Crystallization system and the side that an a kind of step produces big particle diameter food-grade potassium chloride crystal Method, the crystallization operation of " multiple-effect evaporation "+" the crystallisation by cooling kettle " for the application of instead of over, stabilizes input and output material and evaporative crystallization stream Journey, can effectively ensure that the stability of product quality, substantially increase the production efficiency of food-grade potassium chloride.
Continuous evaporative crystallization system design that the present invention is provided rationally, builds the equipment cost that the system used relatively low Honest and clean, crystalline mother solution infinite reflux realizes crystallization process material without waste, process stabilizing, interference is few, beneficial to consecutive production.This is System repeatedly using the vaporization and condensation of indirect steam, can substantially reduce raw steam consumption, so as to improve vaporising device Economy;And the operation of evaporation, concentration and crystallization can be completed in same crystallizer.
Brief description of the drawings
Fig. 1 is that system is constituted and process flow diagram(Cross-flow);
Fig. 2 is the structural representation of crystallizer;
Fig. 3 is that obtained food-grade potassium chloride Lens capsule figure is produced according to the method for the embodiment of the present invention 1;
Fig. 4 is that obtained potassium chloride photo is produced according to the method for the embodiment of the present invention 1;
Fig. 5 is that obtained food-grade potassium chloride Lens capsule figure is produced according to the method for the embodiment of the present invention 2;
Fig. 6 is that obtained potassium chloride photo is produced according to the method for the embodiment of the present invention 2;
Fig. 7 is that obtained food-grade potassium chloride Lens capsule figure is produced according to the method for the embodiment of the present invention 3;
Fig. 8 is that obtained potassium chloride photo is produced according to the method for the embodiment of the present invention 3;
Fig. 9 is that obtained food-grade potassium chloride Lens capsule figure is produced according to the method for the embodiment of the present invention 4;
Figure 10 is that obtained potassium chloride photomacrograph is produced according to the method for the embodiment of the present invention 4;
Figure 11 is that system is constituted and process flow diagram(Countercurrently);
Figure 12 is that system is constituted and process flow diagram(Following current).
In figure, 1- I effect circulating pumps, 2- I effect heat exchangers, 3- I effects separation chamber, 4-II effect circulating pumps, 5- II effect heat exchange Device, 6- II effect crystallizers, 7- crystallization discharging pumps, 8-II effect transfering material pumps, 9- III effect circulating pumps, 10-III effect heat exchangers, 11- III imitates separation chamber, 12-III effect discharging pumps.
Embodiment
With reference to embodiment, the present invention will be described in detail.
The method of existing production food-grade potassium chloride crystal is " multiple-effect evaporation "+" crystallisation by cooling kettle ", also i.e. by potassium chloride Solution multiple-effect evaporation is concentrated, and concentrate then is obtained into potassium chloride product by the production that cools.The mode of production is obtained The food-grade potassium chloride crystal product size distribution arrived is uneven, and crystal product coalescence is serious;And used because increase by one is special In the crystallization kettle of crystallization, destructive increase, power consumption increase to crystal so that production efficiency is very low, production cost compared with It is high.
It is raw the invention provides one kind in order to solve the problems, such as the Processes and apparatus occurred in food-grade potassium chloride crystal production Produce the continuous evaporative crystallization system of big particle diameter food-grade potassium chloride crystal, including vapo(u)rization system and crystal system two parts:
The vapo(u)rization system includes III effects circulating pump 9, III effects heat exchanger 10, III effect separation chambers 11 and III effect discharging pumps 12nd, I imitates circulating pump 1, I effects heat exchanger 2, I effects separation chamber 3;The crystal system include II effect circulating pump 4, II effect heat exchanger 5, II effects crystallizer 6, II effect transfering material pumps 8 and crystallization discharging pump 7.
Raw material is connected to the circulating line that III imitates separation chamber 11, and being delivered to III by circulating line imitates the He of heat exchanger 10 III imitates the charging aperture of separation chamber 11, and the III effect discharging opening of the separation chamber 11 connection III effect entrances of circulating pump 9, III effect circulating pumps 9 are exported It is connected with the III effect charging apertures of heat exchanger 10, III is imitated the discharging opening of heat exchanger 10 and is connected with the III effect recycle feeds of separation chamber 11 mouthful, The III effect bottom discharge of the separation chamber 11 mouthful connection III effect entrances of discharging pump 12, the outlet of III effect discharging pumps 12 is connected to II effect crystallizations The circulating line of device 6, II effect transfering material pumps 8 outlet is connected to the I effect circulating lines of separation chamber 3, and I effect heat exchange is delivered to by circulating line Device 2 and the I effect charging apertures of separation chamber 3, the I effect discharging opening of the separation chamber 3 connection I effect entrances of circulating pump 1, I are imitated the outlet of effect circulating pump 1 with I The charging aperture of heat exchanger 2 is connected, and I is imitated the discharging opening of heat exchanger 2 and is connected with the I effect recycle feeds of separation chamber 3 mouthful, and I effect circulating lines draw branch The circulating line that road is connected to II effect crystallizers 6 is crystallized, and the outlet of the I effect overhead vapors of separation chamber 3 is connected to II effect heat exchangers 5 Shell side import, the III effect overhead vapors of separation chamber 11 outlet is connected to surface condenser and cooled down.
Klorvess Liquid after concentration is delivered to the circulating line that II imitates crystallizer 6, and being delivered to II effects through circulating line changes Hot device 5 and II imitate crystallizer 6, and the II effect circulating line discharging openings of crystallizer 6 are connected to the entrance that II imitates circulating pump 4, II effect circulations The outlet connection II of pump imitates the charging aperture of heat exchanger 5, and the discharging opening connection II of II effect heat exchangers 5 imitates the circulating line of crystallizer 6 Charging aperture, the separation chamber's overhead vapor outlet connection III effect steam inlets of heat exchanger 10 of II effects crystallizer 6, II effect crystallizers 6 are crystallized Room bottom discharge mouthful connection crystallization discharging pump 7.Crystallisation cycle pipeline draws branch road imitates transfering material pump 8 to II, and it is defeated to imitate transfering material pump 8 by II Deliver to the I effect circulating lines of separation chamber 3.
I effects heat exchanger 2, II effects heat exchanger 5, the III effect shell-side outlet condensed waters of heat exchanger 10 are connected to condensed water bucket caching.
Raw material is connected to the circulating line that III imitates separation chamber 11, sequentially enters II effect crystallizers 6 and I effects separation chamber 3, then Enter II from I effects separation chamber 3 and imitate crystallizer 6, be in cross-flow passes with steam;Or raw material is connected to the circulation that III imitates separation chamber 11 Pipeline, sequentially enters II effect separation chambers 6 and I effect crystallizers 3, is crystallized in I effect crystallizers, is in counter-current flow with steam; Or raw material is connected to the circulating line that I imitates separation chamber 3, II effect separation chambers 6 and III effect crystallizers 11 are sequentially entered, imitates and ties in III Crystallized in brilliant device, be in co-current flow with steam.
Crystallizer crystallisation chamber part is cone structure, the material formation supersaturated solution after flash distillation, then is entered by downspout Enter crystallisation chamber, supersaturated solution and the crystal contact of descending liquid bottom of the tube, promote crystal constantly to grow up, the crystallized device bottom of feed liquid Up flow, stir the crystal of bottom, while up flowing, power and crystal gravity, fluid resistance for up being walked with generation etc. The interaction of different active forces, realizes crystal classification, separation, so that crystal grain is suspended in liquid stream formation grading Fluid bed.Crystallisation chamber middle and upper part is predominantly located in compared with small particle crystal, the feed liquid rate of climb is slow, and crystal grain is deposited in small crystals form ;Middle particle diameter crystal grain is mainly distributed on crystallisation chamber middle and lower part, and feed liquid upflow velocity is larger, and crystal grain quantity is more, crystal growth It hurry up, the crystal grain of this part accounts for major part;Big particle diameter crystal grain is mainly distributed on crystallisation chamber bottom, and degree of supersaturation is high, in feed liquid Up-flow speed is fast, and crystal particle diameter is big, and growth rate is fast.
The step carried out using the said equipment produces the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal, bag Include following steps:
It is 30% ~ 36% that Klorvess Liquid is concentrated into potassium chloride mass percent concentration by vapo(u)rization system heating, then Potassium chloride concentrate pump is delivered into crystal system and carries out continuous evaporative crystallization, potassium chloride magma, growing the grain are obtained through evaporative crystallization The discharge of potassium chloride magma is delivered to buffer tank caching after end;
The condition of potassium chloride continuous evaporative crystallization includes:Charging potassium chloride feed liquid is directly entered separation chamber's circulating line, with A large amount of potassium chloride concentrates mixing, the high saturated solution of high temperature is formed by two effect heat exchange, then allows itself and a large amount of potassium chloride magmas Liquid is mixed, and potassium chloride temperature of charge and pressure are improved by external circulation heat exchanging, sends into crystallizer flash concentration, is allowed to crystallization and is separated out Potassium chloride.
It is 55 ~ 110 DEG C to be concentrated by evaporation afterchlorinate potassium temperature.The mass ratio of system circulation amount and inlet amount is(50~150): 1.The residence time is 1 ~ 4h to potassium chloride in a crystallizer.Potassium chloride discharging magma solid content is percent by volume 15 ~ 40%.
Hereinafter, the food-grade potassium chloride continuous evaporative crystallization method of the present invention is carried out by specific embodiment further Describe in detail.Wherein, the size distribution of potassium chloride is determined using Malvern Particle Size Analyzer dry method, and crystallogram is logical Cross determination of polarized light microscopy.Particle mean size refer to sieve lower accumulating weight than for 50% when screen size value.
Embodiment 1:
The present embodiment is used for the food-grade potassium chloride crystal and its production method for illustrating that the present invention is provided.
By Klorvess Liquid by feed pump be delivered to III imitate separation chamber circulating line, by III imitate heat exchanger and After III effect separation chamber's flash concentrations, the circulating line that material is delivered into II effect crystallizers by III effect discharging pumps further dodges Inspissation contracts, then through being delivered to the circulating line that I imitates separation chamber by II effect transfering material pumps after II imitates concentration, imitating heat exchanger by I changes Heat and I imitate separation chamber's high temperature flash concentration, then by pipeline pressure difference be delivered to II imitate crystallizer circulating line, through I effect and III effects two are imitated after heat exchanger heating concentration, and feed liquid is warming up to 88 DEG C or so, and potassium chloride concentration is 34%(w/w), then by chlorination The circulating line that potassium concentrate is delivered to II effect crystallizers is evaporated crystallization, and it is 100 times of inlet amount to keep internal circulating load, is maintained Citric acid feed temperature is 88 DEG C in crystallizer, and it is 30% to keep potassium chloride magma solid content in crystallizer, is circulated in a crystallizer Evaporate after 2h by discharge hole for discharge, be centrifuged, the circulating line that separation Mother liquor is back to II effect crystallizers continues Evaporative crystallization, so that potassium chloride is separated out completely.Obtained product particle mean size is 1.6mm, Granularity Distribution and crystal Photo is as shown in Figure 3 and Figure 4.
Embodiment 2:
The present embodiment is used for the food-grade potassium chloride crystal and its production method for illustrating that the present invention is provided.
By Klorvess Liquid by feed pump be delivered to III imitate separation chamber circulating line, by III imitate heat exchanger and After III effect separation chamber's flash concentrations, the circulating line that material is delivered into II effect crystallizers by III effect discharging pumps further dodges Inspissation contracts, then through being delivered to the circulating line that I imitates separation chamber by II effect transfering material pumps after II imitates concentration, imitating heat exchanger by I changes Heat and I imitate separation chamber's high temperature flash concentration, then by pipeline pressure difference be delivered to II imitate crystallizer circulating line, through I effect and III effects two are imitated after heat exchanger heating concentration, and feed liquid is warming up to 88 DEG C or so, and potassium chloride concentration is 34%(w/w), then by chlorination The circulating line that potassium concentrate is delivered to II effect crystallizers is evaporated crystallization, and it is 150 times of inlet amount to keep internal circulating load, is maintained Citric acid feed temperature is 89 DEG C in crystallizer, and it is 25% to keep potassium chloride magma solid content in crystallizer, is circulated in a crystallizer Evaporate after 1h by discharge hole for discharge, be centrifuged, the circulating line that separation Mother liquor is back to II effect crystallizers continues Evaporative crystallization, so that potassium chloride is separated out completely.Obtained product particle mean size is 1.6mm, Granularity Distribution and crystal Photo is as shown in Figure 5 and Figure 6.
Embodiment 3:
The present embodiment is used for the edible potassium chloride crystal and its production method for illustrating that the present invention is provided.
By Klorvess Liquid by feed pump be delivered to III imitate separation chamber circulating line, by III imitate heat exchanger and After III effect separation chamber's flash concentrations, the circulating line that material is delivered into II effects separation chamber by III effect discharging pumps further dodges Inspissation contract, then II imitate concentration after pass through by II imitate transfering material pump be delivered to I effect crystallizer circulating line be evaporated crystallization, through II Feed liquid is warming up to 110 DEG C or so after effect separation chamber and III effects separation chamber are concentrated by evaporation, and potassium chloride concentration is 36%(w/w), material Crystallization is evaporated into the I circulating lines for imitating crystallizer, it is 50 times of inlet amount to keep internal circulating load, maintains lemon in crystallizer Sour feed temperature is 100 DEG C or so, and it is 15% to keep potassium chloride magma solid content in crystallizer, in a crystallizer circulating and evaporating 3h Afterwards by discharge hole for discharge, it is centrifuged, the circulating line that separation Mother liquor is back to I effect crystallizers continues to evaporate knot Crystalline substance, so that potassium chloride is separated out completely.Obtained product particle mean size is 1.4mm, and Granularity Distribution and crystallogram are such as Shown in Fig. 7 and Fig. 8.
Embodiment 4:
The present embodiment is used for the food-grade potassium chloride crystal and its production method for illustrating that the present invention is provided.
Klorvess Liquid is delivered to the circulating line that I imitates separation chamber by feed pump, heat exchanger and I effects point are imitated by I After the high temperature flash concentration of room, the circulating line that material is delivered into II effects separation chamber by I effect circulating pumps further flashes dense Contracting, then II imitate concentration after pass through by II imitate transfering material pump be delivered to III effect crystallizer circulating line be evaporated crystallization, imitated through I Feed liquid is warming up to 55 DEG C or so after separation chamber and II effects separation chamber are concentrated by evaporation, and potassium chloride concentration is 30%(w/w), material enters I The circulating line of effect crystallizer is evaporated crystallization, and it is 150 times of inlet amount to keep internal circulating load, maintains citric acid material in crystallizer Liquid temperature degree is 55 DEG C or so, and it is 40% to keep potassium chloride magma solid content in crystallizer, is passed through in a crystallizer after circulating and evaporating 4h Discharge hole for discharge, is centrifuged, and the circulating line that separation Mother liquor is back to III effect crystallizers continues evaporative crystallization, with Potassium chloride is set to separate out completely.Obtained product particle mean size is 1.6mm, Granularity Distribution and crystallogram such as Fig. 9 with Shown in Figure 10.
It can be drawn by embodiments of the invention 1-4, the food-grade potassium chloride continuous evaporation knot provided using the present invention The food-grade potassium chloride crystal that brilliant production method is obtained, crystallization yield is high(In the case of material infinite reflux, crystallization yield is reachable 100%), plane of crystal is glossy, and coalescence is few, and even particle size distribution, product quality is higher.
The preferred embodiment of the present invention described in detail above, but the present invention is not limited to the tool in above-described embodiment Body details, the technical method progress simple deformation to the present invention falls within protection scope of the present invention.
Each detail described in above-mentioned embodiment, can pass through any appropriate mode in not contradiction Combination, to avoid repeating, the present invention is no longer illustrated to various possible combinations, and these possible combinations are same It should be regarded as content disclosed in this invention.
Presently preferred embodiments of the present invention is above are only, the protection domain being not intended to limit the invention, the art Personnel should be understood that any modification, equivalent substitution and improvements within the spirit and principles of the invention, being done etc., all should wrap It is contained within protection scope of the present invention.
Above-mentioned continuous evaporative crystallization system cannot be only used for the continuous evaporative crystallization of food-grade potassium chloride, it may also be used for six water Aluminium chloride, sodium chloride, sodium sulphate, ammonium sulfate, maltitol etc. be inorganic or crystallization of organic matter, and preceding system uses the continuous steaming Hair crystal system also should be regarded as content disclosed in this invention.
Present disclosure is not limited to cited by embodiment, and those of ordinary skill in the art are by reading description of the invention And any equivalent conversion taken technical solution of the present invention, it is that claim of the invention is covered.

Claims (9)

1. a step produces the continuous evaporative crystallization system of big particle diameter food-grade potassium chloride crystal, it is characterised in that:
Including vapo(u)rization system and crystal system two parts;
The vapo(u)rization system includes III and imitates circulating pump(9), III effect heat exchanger(10), III effect separation chamber(11)Imitate and discharge with III Pump(12), I effect circulating pump(1), I effect heat exchanger(2), I effect separation chamber(3);
The crystal system includes II and imitates circulating pump(4), II effect heat exchanger(5), II effect crystallizer(6), II effect transfering material pump(8)With Crystallize discharging pump(7);
Raw material is connected to III effects separation chamber(11)Circulating line, by circulating line be delivered to III imitate heat exchanger(10)With III imitates separation chamber(11)Charging aperture, III effects separation chamber(11)Discharging opening connection III effect circulating pumps(9)Entrance, III effect circulating pumps (9)Heat exchanger is imitated with III in outlet(10)Charging aperture is connected, III effect heat exchangers(10)Discharging opening imitates separation chamber with III(11)Circulation Charging aperture is connected, III effects separation chamber(11)Bottom discharge mouthful connection III effect discharging pumps(12)Entrance, III effect discharging pumps(12)Go out Mouth is connected to II effect crystallizers(6)Circulating line, II effect transfering material pumps(8)Outlet is connected to I effects separation chamber(3)Circulating line, leads to Cross circulating line and be delivered to I effect heat exchangers(2)Separation chamber is imitated with I(3)Charging aperture, I effects separation chamber(3)Discharging opening connection I effects are followed Ring pump(1)Entrance, I effect circulating pumps(1)Heat exchanger is imitated with I in outlet(2)Charging aperture is connected, I effect heat exchangers(2)Discharging opening is imitated with I Separation chamber(3)Recycle feed mouthful is connected, and I effect circulating lines draw branch road and are connected to II effect crystallizers(6)Circulating line tied Crystalline substance, I effects separation chamber(3)Overhead vapor outlet is connected to II effect heat exchangers(5)Shell side import, III effects separation chamber(11)Steam at top Vapor outlet is connected to surface condenser and cooled down;
Klorvess Liquid after concentration is delivered to II effect crystallizers(6)Circulating line, through circulating line be delivered to II effect heat exchange Device(5)Crystallizer is imitated with II(6), II effect crystallizers(6)Circulating line discharging opening is connected to II effect circulating pumps(4)Entrance, II Imitate the outlet connection II effect heat exchangers of circulating pump(5)Charging aperture, II effect heat exchanger(5)Discharging opening connection II effect crystallizer (6)Circulating line charging aperture, II effect crystallizer(6)Separation chamber's overhead vapor outlet connection III effect heat exchangers(10)Steam enters Mouthful, II effect crystallizers(6)Crystallisation chamber bottom discharge mouthful connection crystallization discharging pump(7);Crystallisation cycle pipeline draws branch road and turned to II effects Expect pump(8), transfering material pump is imitated by II(8)It is delivered to I effects separation chamber(3)Circulating line.
2. a step according to claim 1 produces the continuous evaporative crystallization system of big particle diameter food-grade potassium chloride crystal, its It is characterised by:
I imitates heat exchanger(2), II effect heat exchanger(5), III effect heat exchanger(10)Shell-side outlet condensed water is connected to condensed water bucket and delayed Deposit.
3. a step according to claim 1 produces the continuous evaporative crystallization system of big particle diameter food-grade potassium chloride crystal, its It is characterised by:
Raw material is connected to III effects separation chamber(11)Circulating line, sequentially enter II effect crystallizer(6)Separation chamber is imitated with I(3), Again separation chamber is imitated from I(3)Crystallizer is imitated into II(6), it is in cross-flow passes with steam;
Or raw material is connected to III effects separation chamber(11)Circulating line, sequentially enter II effect separation chamber(6)Crystallizer is imitated with I (3), crystallized in I effect crystallizers, be in counter-current flow with steam;
Or raw material is connected to I effects separation chamber(3)Circulating line, sequentially enter II effect separation chamber (6) and III imitate crystallizer (11), crystallized in III effect crystallizers, be in co-current flow with steam.
4. a step produces the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal, it is characterised in that:
Comprise the following steps:
It is 30% ~ 36% that Klorvess Liquid is concentrated into potassium chloride mass percent concentration by vapo(u)rization system heating, then by chlorine Change potassium concentrate pump and deliver to crystal system progress continuous evaporative crystallization, obtain potassium chloride magma through evaporative crystallization, growing the grain terminates The discharge of potassium chloride magma is delivered to buffer tank caching afterwards;
The condition of potassium chloride continuous evaporative crystallization includes:Charging potassium chloride feed liquid is directly entered separation chamber's circulating line, and a large amount of Potassium chloride concentrate is mixed, and is formed the high saturated solution of high temperature by two effect heat exchange, is then allowed it mixed with a large amount of potassium chloride magmas Close, potassium chloride temperature of charge and pressure are improved by external circulation heat exchanging, send into crystallizer flash concentration, be allowed to crystallization and separate out chlorination Potassium crystal.
5. a step according to claim 4 produces the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal, its It is characterised by:
It is 55 ~ 110 DEG C to be concentrated by evaporation afterchlorinate potassium temperature.
6. a step according to claim 4 produces the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal, its It is characterised by:
The mass ratio of system circulation amount and inlet amount is(50~150):1.
7. a step according to claim 4 produces the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal, its It is characterised by:
The residence time is 1 ~ 4h to potassium chloride in a crystallizer.
8. a step according to claim 4 produces the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal, its It is characterised by:
Potassium chloride discharging magma solid content is percent by volume 15 ~ 40%.
9. a step as claimed in claim 4 produces the continuous evaporative crystallization method production of big particle diameter food-grade potassium chloride crystal Food-grade potassium chloride crystal.
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CN106745078A (en) * 2016-12-13 2017-05-31 中蓝连海设计研究院 The method that food-grade potassium chloride is produced using calcining recrystallizing technology
CN107626112A (en) * 2017-10-27 2018-01-26 中国轻工业长沙工程有限公司 A kind of continuous production vacuum cooling crystallizer
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CN111039325B (en) * 2019-12-11 2022-06-10 天津科技大学 Continuous evaporation crystallization method of sodium molybdate dihydrate
CN113599858B (en) * 2021-08-11 2022-06-10 自然资源部天津海水淡化与综合利用研究所 Spiral-flow type fluidized bed cooling crystallization system

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