CN105727576A - Continuous evaporative crystallization system and method for one-step production of large-grain-size food-grade potassium chloride crystals - Google Patents

Continuous evaporative crystallization system and method for one-step production of large-grain-size food-grade potassium chloride crystals Download PDF

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CN105727576A
CN105727576A CN201610247323.XA CN201610247323A CN105727576A CN 105727576 A CN105727576 A CN 105727576A CN 201610247323 A CN201610247323 A CN 201610247323A CN 105727576 A CN105727576 A CN 105727576A
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potassium chloride
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iii
separation chamber
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CN105727576B (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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  • Crystallography & Structural Chemistry (AREA)
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Abstract

The invention relates to a continuous evaporative crystallization system and method for one-step production of large-grain-size food-grade potassium chloride crystals. The system consists of an evaporation system and a crystallization system and can achieve the production of large-grain-size food-grade potassium chloride in a one-step continuous mode. The method comprises the steps that a potassium chloride solution performs heating concentration through the evaporation system and then is pumped to the crystallization system for continuous evaporative crystallization so as to obtain potassium chloride crystal slurry, and the potassium chloride crystal slurry is discharged out and delivered to a cache tank for caching after grain growing is completed. The conditions include that a feed potassium chloride liquid directly flows into a separation chamber circulating pipeline to be mixed with a large amount of concentrated potassium chloride liquid, a high-temperature and high-saturation solution is prepared through two-effect heat exchange and then is mixed with the large amount of concentrated potassium chloride liquid, the temperature and pressure of a potassium chloride material are improved through externally-cycled heat exchange, the mixture is delivered to a crystallizer for flash evaporation and concentration, and the potassium chloride crystals crystallize and dissolve out. The food-grade potassium chloride crystals obtained by means of the method are large in average grain size, uniform in grain size distribution and high in yield.

Description

One step produces the continuous evaporative crystallization system and method for big particle diameter food-grade potassium chloride crystal
Technical field
The invention belongs to evaporative crystallization technique field, be specifically related to an a kind of step and produce the continuous evaporative crystallization system and method for big particle diameter food-grade potassium chloride crystal.
Background technology
Food-grade potassium chloride is white powder or colourless crystallization, odorless, and salty in the mouth is nontoxic, soluble in water, be dissolved in glycerol, be slightly soluble in ethanol.Food-grade potassium chloride is mainly used to produce Cardia Salt, to meet the direct kalium replenishment of human body, substitutes Sal as savory agent and nutritional supplement with part, it is prevented that people's excess ingestion Sal;Pharmaceutically being available for taking orally, it is also possible to preparation water injection, play supplementary or balanced human's potassium deficiency effect, health can also manufacture diuretic, prevent kaliopenia medicine.In addition, potassium chloride is the same with Sal be can be used in the food such as agricultural production, Aquatic product, livestock products, fermentation, seasoning, canned food, instant food, can be added in proportion in various food, food tissue state, color, smell and taste and raw-food material cost control are played indispensable effect.
Food-grade potassium chloride crystal product produces and mainly includes dissolving, crystallization, separation, dry and five operations of packaging, namely the saturated solution of preparation potassium chloride is first dissolved by technical grade potassium chloride, then saturated solution is delivered to crystalline element and is evaporated crystallization, obtain potassium chloride magma, potassium chloride magma is delivered to centrifuge again be centrifuged separating, dry, pack for sale.Wherein, the evaporative crystallization of potassium chloride is most important, most crucial operation, evaporative crystallization obtains the quality of potassium chloride product, directly influence the granularity of food-grade potassium chloride product, purity and outward appearance, therefore strictly control potassium chloride multiple-effect evaporation crystallization processes flow process is needed, 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 still ", this covering device is evaporation and Crystallization Procedure to be separated, first Klorvess Liquid multiple-effect evaporation is concentrated, then concentrated solution is obtained potassium chloride product by the production that cools.Along with industrially scalable constantly expands, food-grade potassium chloride crystallization processes equipment needed thereby and manual operation are all relatively larger, impact due to manual operation unstable factor, easily cause that edible potassium chloride crystal product crystal is tiny, particle size distribution is uneven, crystal product coalescence serious, cause subsequent handling to separate, washing, dry difficulty and increase, it is impossible to meet food potassium chloride producer to Potassium Chloride Product granularity and purity requirement.
Summary of the invention
It is an object of the invention to provide an a kind of step and produce the continuous evaporative crystallization system and method for big particle diameter food-grade potassium chloride crystal, reduce hand labor intensity, improve production efficiency and energy utilization rate so that the food-grade potassium chloride crystal arrived is bigger, even particle size distribution, production cost reduces.
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;
Described vapo(u)rization system includes III effect circulating pump, III imitates heat exchanger, III imitates separation chamber and III imitates discharging pump, I imitates circulating pump, I effect heat exchanger, I imitate separation chamber;
Described crystal system includes II and imitates circulating pump, II effect heat exchanger, II effect crystallizer, II effect transfering material pump and crystallization discharging pump;
nullRaw material is connected to III and imitates the circulating line of separation chamber,It is delivered to III by circulating line and imitates heat exchanger and III effect separation chamber charging aperture,III is imitated separation chamber's discharging opening and is connected III effect pump entry,III is imitated circulating-pump outlet and is connected with III effect heat exchanger charging aperture,III is imitated heat exchanger discharging opening and is connected with III effect separation chamber's recycle feed mouth,III is imitated separation chamber's bottom discharge mouth and is connected III effect discharging pump entrance,III is imitated discharging pump outlet and is connected to II effect crystallizer circulating line,II is imitated transfering material pump outlet and is connected to I effect separation chamber circulating line,It is delivered to I by circulating line and imitates heat exchanger and I effect separation chamber charging aperture,I is imitated separation chamber's discharging opening and is connected I effect pump entry,I is imitated circulating-pump outlet and is connected with I effect heat exchanger charging aperture,I is imitated heat exchanger discharging opening and is connected with I effect separation chamber's recycle feed mouth,I imitate circulating line draw branch road be connected to II imitate crystallizer circulating line carry out crystallization,I is imitated separation chamber's overhead vapor outlet and is connected to II effect heat exchanger shell pass import,The overhead vapor outlet of III effect separation chamber is connected to surface condenser and cools down;
Klorvess Liquid after concentration is delivered to II and imitates the circulating line of crystallizer, it is delivered to II through circulating line and imitates heat exchanger and II effect crystallizer, II is imitated crystallizer circulating line discharging opening and is connected to the entrance of II effect circulating pump, II effect circulation delivery side of pump connects II and imitates the charging aperture of heat exchanger, II imitates the circulating line charging aperture of the discharging opening connection II effect crystallizer of heat exchanger, II is imitated the overhead vapor outlet of crystallizer separation chamber and is connected III effect heat exchanger steam inlet, and II is imitated crystallizer crystallisation chamber bottom discharge mouth and connected crystallization discharging pump.Crystallisation cycle pipeline draws branch road imitates transfering material pump to II, imitates transfering material pump by II and is delivered to I effect separation chamber circulating line.
I imitates heat exchanger, II imitates heat exchanger, III is imitated heat exchanger shell pass outlet condensed water and is connected to condensed water bucket buffer memory.
Raw material is connected to III and imitates the circulating line of separation chamber, sequentially enters II and imitates crystallizer and I effect separation chamber, then imitate crystallizer from I effect separation chamber's entrance II, is cross-flow passes with steam;
Or raw material is connected to III and imitates the circulating line of separation chamber, sequentially enter II and imitate separation chamber and I effect crystallizer, imitate in crystallizer at I and carry out crystallization, be counter-current flow with steam;
Or raw material is connected to I and imitates the circulating line of separation chamber, sequentially enter II and imitate separation chamber and III effect crystallizer, imitate in crystallizer at III and carry out crystallization, be 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:
By vapo(u)rization system heating, Klorvess Liquid is concentrated into potassium chloride mass percent concentration is 30% ~ 36%, then potassium chloride concentrate pump is delivered to crystal system and carry out continuous evaporative crystallization, obtaining potassium chloride magma through evaporative crystallization, the discharge of potassium chloride magma is delivered to buffer tank buffer memory after terminating by growing the grain;
The condition of potassium chloride continuous evaporative crystallization includes: charging potassium chloride feed liquid is directly entered separation chamber's circulating line, mix with a large amount of potassium chloride concentrated solutions, imitate heat exchange by two and form high temperature height saturated solution, then it is allowed to mix with a large amount of potassium chloride magma, potassium chloride temperature of charge and pressure is improved by external circulation heat exchanging, send into crystallizer flash concentration, so as to crystallization potassium chloride.
Evaporation and concentration afterchlorinate potassium temperature is 55 ~ 110 DEG C.
The mass ratio of system circulating load and inlet amount is (50 ~ 150): 1.
The potassium chloride time of staying in a crystallizer is 1 ~ 4h.
Potassium chloride discharging magma solid content is percent by volume 15 ~ 40%.
A step produces the food-grade potassium chloride crystal that the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal produces as mentioned.
The invention have the advantages that
Crystallizer of the present invention can make region that degree of supersaturation produces and crystal growth district be respectively placed in two places of crystallizer, and crystal is fluidized suspension in circulating mother liquor, provides good condition for crystal growth, it is possible to produces that granularity is bigger and uniform crystal.
The invention provides an a kind of step and produce the Continuous Cooling Crystallization system and method for big particle diameter food-grade potassium chloride crystal, the crystallization operation of " multiple-effect evaporation "+" the crystallisation by cooling still " of the application of instead of over, stabilize input and output material and evaporative crystallization flow process, can effectively ensure that the stability of product quality, substantially increase the production efficiency of food-grade potassium chloride.
Continuous evaporative crystallization system provided by the invention is reasonable in design, and it is less expensive to build the equipment cost that this system adopts, crystalline mother solution infinite reflux, it is achieved crystallization process material is without waste, process stabilizing, and interference is few, is beneficial to consecutive production.This system repeatedly utilizes vaporization and the condensation of indirect steam, it is possible to substantially reduce raw steam consumption, thus improve the economy of vaporising device;And the operation of evaporation, concentration and crystallization can be completed in same crystallizer.
Accompanying drawing explanation
Fig. 1 is system composition and process flow diagram (cross-flow);
Fig. 2 is the structural representation of crystallizer;
Fig. 3 be according to embodiments of the present invention 1 method produce the food-grade potassium chloride Lens capsule figure that obtains;
Fig. 4 be according to embodiments of the present invention 1 method produce the potassium chloride photo that obtains;
Fig. 5 be according to embodiments of the present invention 2 method produce the food-grade potassium chloride Lens capsule figure that obtains;
Fig. 6 be according to embodiments of the present invention 2 method produce the potassium chloride photo that obtains;
Fig. 7 be according to embodiments of the present invention 3 method produce the food-grade potassium chloride Lens capsule figure that obtains;
Fig. 8 be according to embodiments of the present invention 3 method produce the potassium chloride photo that obtains;
Fig. 9 be according to embodiments of the present invention 4 method produce the food-grade potassium chloride Lens capsule figure that obtains;
Figure 10 be according to embodiments of the present invention 4 method produce the potassium chloride photomacrograph that obtains;
Figure 11 is system composition and process flow diagram (adverse current);
Figure 12 is system composition and process flow diagram (following current).
In figure, 1-I imitates circulating pump, and 2-I imitates heat exchanger, and 3-I imitates separation chamber, and 4-II imitates circulating pump, 5-II imitates heat exchanger, and 6-II imitates crystallizer, 7-crystallization discharging pump, and 8-II imitates transfering material pump, 9-III imitates circulating pump, and 10-III imitates heat exchanger, and 11-III imitates separation chamber, and 12-III imitates discharging pump.
Detailed description of the invention
Below in conjunction with detailed description of the invention, 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 still ", also concentrates by Klorvess Liquid multiple-effect evaporation, then by the production that cools, concentrated solution is obtained potassium chloride product.The food-grade potassium chloride crystal product particle size distribution that this mode of production obtains is uneven, and crystal product coalescence is serious;And because increasing a crystallization kettle being specifically designed to crystallization, the destructive increase of crystal, power consumption are increased, so that production efficiency is very low, production cost is higher.
In order to solve the Processes and apparatus problem occurred in food-grade potassium chloride crystal production, the invention provides a kind of continuous evaporative crystallization system producing big particle diameter food-grade potassium chloride crystal, including vapo(u)rization system and crystal system two parts:
Described vapo(u)rization system includes III effect circulating pump 9, III imitates heat exchanger 10, III imitates separation chamber 11 and III imitates discharging pump 12, I imitates circulating pump 1, I effect heat exchanger 2, I imitate separation chamber 3;Described crystal system includes II and imitates circulating pump 4, II effect heat exchanger 5, II effect crystallizer 6, II effect transfering material pump 8 and crystallization discharging pump 7.
nullRaw material is connected to III and imitates the circulating line of separation chamber 11,It is delivered to III by circulating line and imitates heat exchanger 10 and III effect separation chamber 11 charging aperture,III is imitated separation chamber 11 discharging opening and is connected III effect circulating pump 9 entrance,III effect circulating pump 9 exports and is connected with III effect heat exchanger 10 charging aperture,III is imitated heat exchanger 10 discharging opening and is connected with III effect separation chamber 11 recycle feed mouth,III is imitated separation chamber 11 bottom discharge mouth and is connected III effect discharging pump 12 entrance,III is imitated discharging pump 12 outlet and is connected to II effect crystallizer 6 circulating line,II is imitated transfering material pump 8 outlet and is connected to I effect separation chamber 3 circulating line,It is delivered to I by circulating line and imitates heat exchanger 2 and I effect separation chamber 3 charging aperture,I is imitated separation chamber 3 discharging opening and is connected I effect circulating pump 1 entrance,I effect circulating pump 1 exports and is connected with I effect heat exchanger 2 charging aperture,I is imitated heat exchanger 2 discharging opening and is connected with I effect separation chamber 3 recycle feed mouth,I imitate circulating line draw branch road be connected to II imitate crystallizer 6 circulating line carry out crystallization,I is imitated separation chamber 3 overhead vapor outlet and is connected to II effect heat exchanger 5 shell side import,The overhead vapor outlet of III effect separation chamber 11 is connected to surface condenser and cools down.
Klorvess Liquid after concentration is delivered to II and imitates the circulating line of crystallizer 6, it is delivered to II through circulating line and imitates heat exchanger 5 and II effect crystallizer 6, II is imitated crystallizer 6 circulating line discharging opening and is connected to the entrance of II effect circulating pump 4, II effect circulation delivery side of pump connects II and imitates the charging aperture of heat exchanger 5, II imitates the circulating line charging aperture of the discharging opening connection II effect crystallizer 6 of heat exchanger 5, II is imitated the overhead vapor outlet of crystallizer 6 separation chamber and is connected III effect heat exchanger 10 steam inlet, and II is imitated crystallizer 6 crystallisation chamber bottom discharge mouth and connected crystallization discharging pump 7.Crystallisation cycle pipeline draws branch road imitates transfering material pump 8 to II, imitates transfering material pump 8 by II and is delivered to I effect separation chamber 3 circulating line.
I imitates heat exchanger 2, II imitates heat exchanger 5, III is imitated heat exchanger 10 shell-side outlet condensed water and is connected to condensed water bucket buffer memory.
Raw material is connected to III and imitates the circulating line of separation chamber 11, sequentially enters II and imitates crystallizer 6 and I effect separation chamber 3, then enter II effect crystallizer 6 from I effect separation chamber 3, is cross-flow passes with steam;Or raw material is connected to III and imitates the circulating line of separation chamber 11, sequentially enter II and imitate separation chamber 6 and I effect crystallizer 3, imitate in crystallizer at I and carry out crystallization, be counter-current flow with steam;Or raw material is connected to I and imitates the circulating line of separation chamber 3, sequentially enter II and imitate separation chamber 6 and III effect crystallizer 11, imitate in crystallizer at III and carry out crystallization, be co-current flow with steam.
Crystallizer crystallisation chamber part is cone structure, material after flash distillation forms supersaturated solution, crystallisation chamber is entered again through downspout, crystal contact bottom supersaturated solution and downspout, promote that crystal is constantly grown up, up flow bottom the crystallized device of feed liquid, stir the crystal of bottom, up flow simultaneously, along with the interaction producing the different active forces such as the power up walked and crystal gravity, fluid resistance, realize crystal classification, separation, so that crystal grain is suspended in liquid stream and forms the fluid bed of grading.Less particle diameter crystal is predominantly located in crystallisation chamber middle and upper part, and the feed liquid rate of climb is slow, and crystal grain exists with small crystals form;Middle particle diameter crystal grain is mainly distributed on crystallisation chamber middle and lower part, and feed liquid upflow velocity is relatively big, and crystal grain quantity is many, and crystal growth is fast, and the crystal grain of this part accounts for major part;Big particle diameter crystal grain is mainly distributed on bottom crystallisation chamber, and degree of supersaturation is high, and feed liquid upflow velocity is fast, and crystal particle diameter is big, and growth rate is fast.
Adopt the step that the said equipment carries out to produce the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal, comprise the following steps:
By vapo(u)rization system heating, Klorvess Liquid is concentrated into potassium chloride mass percent concentration is 30% ~ 36%, then potassium chloride concentrate pump is delivered to crystal system and carry out continuous evaporative crystallization, obtaining potassium chloride magma through evaporative crystallization, the discharge of potassium chloride magma is delivered to buffer tank buffer memory after terminating by growing the grain;
The condition of potassium chloride continuous evaporative crystallization includes: charging potassium chloride feed liquid is directly entered separation chamber's circulating line, mix with a large amount of potassium chloride concentrated solutions, imitate heat exchange by two and form high temperature height saturated solution, then it is allowed to mix with a large amount of potassium chloride magma, potassium chloride temperature of charge and pressure is improved by external circulation heat exchanging, send into crystallizer flash concentration, so as to crystallization potassium chloride.
Evaporation and concentration afterchlorinate potassium temperature is 55 ~ 110 DEG C.The mass ratio of system circulating load and inlet amount is (50 ~ 150): 1.The potassium chloride time of staying in a crystallizer is 1 ~ 4h.Potassium chloride discharging magma solid content is percent by volume 15 ~ 40%.
Hereinafter, by specific embodiment, the food-grade potassium chloride continuous evaporative crystallization method of the present invention is described in further detail.Wherein, the particle size distribution of potassium chloride adopts Malvern Particle Size Analyzer dry method to measure, and crystallogram is by determination of polarized light microscopy.Particle mean size refers to that the lower accumulating weight ratio of sieve is screen size value when 50%.
Embodiment 1:
The present embodiment is used for food-grade potassium chloride crystal provided by the invention and production method thereof are described.
nullKlorvess Liquid is delivered to III by feed pump and imitates the circulating line of separation chamber,After III imitates heat exchanger and III imitates separation chamber's flash concentration,Material is imitated discharging pump by III and is delivered to the further flash concentration of circulating line of II effect crystallizer,Again through being delivered to the circulating line of I effect separation chamber by II effect transfering material pump after II effect concentration,Imitate heat exchanger heat exchange by I and I imitates separation chamber's high temperature flash concentration,Then pass through pipeline pressure reduction and be delivered to the circulating line of II effect crystallizer,After I effect and III effect two effect heat exchanger heating concentration,Feed liquid is warming up to about 88 DEG C,Potassium chloride concentration is 34%(w/w),The circulating line that then potassium chloride concentrated solution is delivered to II effect crystallizer is evaporated crystallization,Keep circulating load to be inlet amount 100 times,Maintaining citric acid feed temperature in crystallizer is 88 DEG C,Keeping potassium chloride magma solid content in crystallizer is 30%,Discharge hole for discharge is passed through in a crystallizer after circulating and evaporating 2h,It is centrifuged separating,After separation, mother solution is back to II and imitates the circulating line continuation evaporative crystallization of crystallizer,So that potassium chloride precipitates out completely.The product particle mean size obtained be 1.6mm, Granularity Distribution and crystallogram as shown in Figure 3 and Figure 4.
Embodiment 2:
The present embodiment is used for food-grade potassium chloride crystal provided by the invention and production method thereof are described.
nullKlorvess Liquid is delivered to III by feed pump and imitates the circulating line of separation chamber,After III imitates heat exchanger and III imitates separation chamber's flash concentration,Material is imitated discharging pump by III and is delivered to the further flash concentration of circulating line of II effect crystallizer,Again through being delivered to the circulating line of I effect separation chamber by II effect transfering material pump after II effect concentration,Imitate heat exchanger heat exchange by I and I imitates separation chamber's high temperature flash concentration,Then pass through pipeline pressure reduction and be delivered to the circulating line of II effect crystallizer,After I effect and III effect two effect heat exchanger heating concentration,Feed liquid is warming up to about 88 DEG C,Potassium chloride concentration is 34%(w/w),The circulating line that then potassium chloride concentrated solution is delivered to II effect crystallizer is evaporated crystallization,Keep circulating load to be inlet amount 150 times,Maintaining citric acid feed temperature in crystallizer is 89 DEG C,Keeping potassium chloride magma solid content in crystallizer is 25%,Discharge hole for discharge is passed through in a crystallizer after circulating and evaporating 1h,It is centrifuged separating,After separation, mother solution is back to II and imitates the circulating line continuation evaporative crystallization of crystallizer,So that potassium chloride precipitates out completely.The product particle mean size obtained be 1.6mm, Granularity Distribution and crystallogram as shown in Figure 5 and Figure 6.
Embodiment 3:
The present embodiment is used for edible potassium chloride crystal provided by the invention and production method thereof are described.
nullKlorvess Liquid is delivered to III by feed pump and imitates the circulating line of separation chamber,After III imitates heat exchanger and III imitates separation chamber's flash concentration,Material is imitated discharging pump by III and is delivered to the further flash concentration of circulating line of II effect separation chamber,The circulating line that warp is delivered to I effect crystallizer by II effect transfering material pump after II effect concentration again is evaporated crystallization,After II imitates separation chamber and III imitates separation chamber's evaporation and concentration, feed liquid is warming up to about 110 DEG C,Potassium chloride concentration is 36%(w/w),Material enters the circulating line of I effect crystallizer and is evaporated crystallization,Keep circulating load to be inlet amount 50 times,Maintaining citric acid feed temperature in crystallizer is about 100 DEG C,Keeping potassium chloride magma solid content in crystallizer is 15%,Discharge hole for discharge is passed through in a crystallizer after circulating and evaporating 3h,It is centrifuged separating,After separation, mother solution is back to I and imitates the circulating line continuation evaporative crystallization of crystallizer,So that potassium chloride precipitates out completely.The product particle mean size obtained be 1.4mm, Granularity Distribution and crystallogram as shown in Figure 7 and Figure 8.
Embodiment 4:
The present embodiment is used for food-grade potassium chloride crystal provided by the invention and production method thereof are described.
nullKlorvess Liquid is delivered to I by feed pump and imitates the circulating line of separation chamber,After I imitates heat exchanger and I imitates separation chamber's high temperature flash concentration,Material is imitated circulating pump by I and is delivered to the further flash concentration of circulating line of II effect separation chamber,The circulating line that warp is delivered to III effect crystallizer by II effect transfering material pump after II effect concentration again is evaporated crystallization,After I imitates separation chamber and II imitates separation chamber's evaporation and concentration, feed liquid is warming up to about 55 DEG C,Potassium chloride concentration is 30%(w/w),Material enters the circulating line of I effect crystallizer and is evaporated crystallization,Keep circulating load to be inlet amount 150 times,Maintaining citric acid feed temperature in crystallizer is about 55 DEG C,Keeping potassium chloride magma solid content in crystallizer is 40%,Discharge hole for discharge is passed through in a crystallizer after circulating and evaporating 4h,It is centrifuged separating,After separation, mother solution is back to III and imitates the circulating line continuation evaporative crystallization of crystallizer,So that potassium chloride precipitates out completely.The product particle mean size obtained be 1.6mm, Granularity Distribution and crystallogram as shown in Figure 9 and Figure 10.
Can be drawn by embodiments of the invention 1-4, adopt the food-grade potassium chloride crystal that food-grade potassium chloride continuous evaporative crystallization production method provided by the invention obtains, crystallization yield is high (in material infinite reflux situation, crystallization yield is up to 100%), plane of crystal is glossy, 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 detail in above-described embodiment, the technical method of the present invention is carried out simple deformation and falls within protection scope of the present invention.
Each detail described in above-mentioned detailed description of the invention, can be combined by the mode of any appropriate when not contradiction, for avoiding repeating, various possible compound modes are no longer illustrated by the present invention, and these possible compound modes should be regarded as content disclosed in this invention equally.
Above are only presently preferred embodiments of the present invention; not in order to limit the scope of the invention, described those skilled in the art should be understood that all within the spirit and principles in the present invention; any amendment of being made, equivalent replacement, improvement etc., should be included 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, can be additionally used in the inorganic or organic crystallizations such as Aluminum Chloride Hexahydrate, sodium chloride, sodium sulfate, ammonium sulfate, maltose alcohol, aforementioned system adopts this continuous evaporative crystallization system also to should be regarded as content disclosed in this invention.
Present disclosure is not limited to cited by embodiment, and the conversion of any equivalence that technical solution of the present invention is taked by those of ordinary skill in the art by reading description of the present invention, the claim being the present invention is contained.

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;
Described vapo(u)rization system includes III effect circulating pump (9), III effect heat exchanger (10), III imitates separation chamber (11) and III imitates discharging pump (12), I imitates circulating pump (1), I effect heat exchanger (2), I effect separation chamber (3);
Described crystal system includes II and imitates circulating pump (4), II effect heat exchanger (5), II effect crystallizer (6), II effect transfering material pump (8) and crystallization discharging pump (7);
nullRaw material is connected to III and imitates the circulating line of separation chamber (11),It is delivered to III by circulating line and imitates heat exchanger (10) and III effect separation chamber (11) charging aperture,III is imitated separation chamber (11) discharging opening and is connected III effect circulating pump (9) entrance,III is imitated circulating pump (9) outlet and is connected with III effect heat exchanger (10) charging aperture,III is imitated heat exchanger (10) discharging opening and is connected with III effect separation chamber (11) recycle feed mouth,III is imitated separation chamber (11) bottom discharge mouth and is connected III effect discharging pump (12) entrance,III is imitated discharging pump (12) outlet and is connected to II effect crystallizer (6) circulating line,II is imitated transfering material pump (8) outlet and is connected to I effect separation chamber (3) circulating line,It is delivered to I by circulating line and imitates heat exchanger (2) and I effect separation chamber (3) charging aperture,I is imitated separation chamber (3) discharging opening and is connected I effect circulating pump (1) entrance,I is imitated circulating pump (1) outlet and is connected with I effect heat exchanger (2) charging aperture,I is imitated heat exchanger (2) discharging opening and is connected with I effect separation chamber (3) recycle feed mouth,I imitate circulating line draw branch road be connected to II imitate crystallizer (6) circulating line carry out crystallization,I is imitated the outlet of separation chamber (3) overhead vapor and is connected to II effect heat exchanger (5) shell side import,III effect separation chamber (11) overhead vapor outlet is connected to surface condenser and cools down;
Klorvess Liquid after concentration is delivered to II and imitates the circulating line of crystallizer (6), it is delivered to II through circulating line and imitates heat exchanger (5) and II effect crystallizer (6), II is imitated crystallizer (6) circulating line discharging opening and is connected to the entrance of II effect circulating pump (4), II effect circulation delivery side of pump connects II and imitates the charging aperture of heat exchanger (5), II imitates the circulating line charging aperture of discharging opening connection II effect crystallizer (6) of heat exchanger (5), II is imitated the overhead vapor outlet of crystallizer (6) separation chamber and is connected III effect heat exchanger (10) steam inlet, II is imitated crystallizer (6) crystallisation chamber bottom discharge mouth and is connected crystallization discharging pump (7);Crystallisation cycle pipeline draws branch road imitates transfering material pump (8) to II, imitates transfering material pump (8) by II and is delivered to I effect 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, it is characterised in that:
I imitates heat exchanger (2), II imitates heat exchanger (5), III is imitated heat exchanger (10) shell-side outlet condensed water and is connected to condensed water bucket buffer memory.
3. a step according to claim 1 produces the continuous evaporative crystallization system of big particle diameter food-grade potassium chloride crystal, it is characterised in that:
Raw material is connected to III and imitates the circulating line of separation chamber (11), sequentially enters II and imitates crystallizer (6) and I effect separation chamber (3), then imitate crystallizer (6) from I effect separation chamber (3) entrance II, is cross-flow passes with steam;
Or raw material is connected to III and imitates the circulating line of separation chamber (11), sequentially enter II and imitate separation chamber (6) and I effect crystallizer (3), imitate in crystallizer at I and carry out crystallization, be counter-current flow with steam;
Or raw material is connected to I and imitates the circulating line of separation chamber (3), sequentially enter II and imitate separation chamber (6) and III effect crystallizer (11), imitate in crystallizer at III and carry out crystallization, be 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:
By vapo(u)rization system heating, Klorvess Liquid is concentrated into potassium chloride mass percent concentration is 30% ~ 36%, then potassium chloride concentrate pump is delivered to crystal system and carry out continuous evaporative crystallization, obtaining potassium chloride magma through evaporative crystallization, the discharge of potassium chloride magma is delivered to buffer tank buffer memory after terminating by growing the grain;
The condition of potassium chloride continuous evaporative crystallization includes: charging potassium chloride feed liquid is directly entered separation chamber's circulating line, mix with a large amount of potassium chloride concentrated solutions, imitate heat exchange by two and form high temperature height saturated solution, then it is allowed to mix with a large amount of potassium chloride magma, potassium chloride temperature of charge and pressure is improved by external circulation heat exchanging, send into crystallizer flash concentration, so as to crystallization potassium chloride.
5. a step according to claim 4 produces the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal, it is characterised in that:
Evaporation and concentration afterchlorinate potassium temperature is 55 ~ 110 DEG C.
6. a step according to claim 4 produces the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal, it is characterised in that:
The mass ratio of system circulating load 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, it is characterised in that:
The potassium chloride time of staying in a crystallizer is 1 ~ 4h.
8. a step according to claim 4 produces the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal, it is characterised in that:
Potassium chloride discharging magma solid content is percent by volume 15 ~ 40%.
9. a step as claimed in claim 4 produces the food-grade potassium chloride crystal that the continuous evaporative crystallization method of big particle diameter food-grade potassium chloride crystal produces.
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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
CN109911921A (en) * 2019-03-13 2019-06-21 上海中腾环保科技有限公司 Using the system and method for MVR evaporative crystallization technique consecutive production hydronium(ion) lithia
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CN111039325A (en) * 2019-12-11 2020-04-21 天津科技大学 Continuous evaporation crystallization method of sodium molybdate dihydrate
CN111039325B (en) * 2019-12-11 2022-06-10 天津科技大学 Continuous evaporation crystallization method of sodium molybdate dihydrate
CN113599858A (en) * 2021-08-11 2021-11-05 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
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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