CN104310438B - A kind of system and method for continous way preparing potassium nitrate by means of double decomposition - Google Patents
A kind of system and method for continous way preparing potassium nitrate by means of double decomposition Download PDFInfo
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- CN104310438B CN104310438B CN201410532143.7A CN201410532143A CN104310438B CN 104310438 B CN104310438 B CN 104310438B CN 201410532143 A CN201410532143 A CN 201410532143A CN 104310438 B CN104310438 B CN 104310438B
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- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D9/00—Nitrates of sodium, potassium or alkali metals in general
- C01D9/08—Preparation by double decomposition
Abstract
The present invention relates to a kind of system and method for continous way preparing potassium nitrate by means of double decomposition. This system comprises dissolving tank, potassium nitrate vacuum crystallization device, a thickener, centrifuge, mixing tank for coating colors, concentrating and preheating device, adverse current triple effect enrichment facility, vacuum continuous crystalizer, secondary thickener and a secondary centrifuging machine. The invention still further relates to the method for continous way preparing potassium nitrate by means of double decomposition. The system and method for continous way preparing potassium nitrate by means of double decomposition of the present invention, adopt new potassium nitrate vacuum crystallization mentality of designing, more accurate to crystallization process control, the Quality and yield of potassium nitrate crystal is more stable, and can continuous dosing, continuous discharge, realized serialization production.
Description
Technical field
The system and method that the present invention relates to a kind of continous way preparing potassium nitrate by means of double decomposition, belongs to chemical production technical field.
Background technology
Domestic preparing potassium nitrate by means of double decomposition mainly adopts sodium nitrate-potassium chloride method and ammonium nitrate-potassium chloride method. The former cost of materialHigher, byproduct sodium chloride economic worth is lower. The extensive use of ammonium nitrate-potassium chloride metathesis process, again taking four one-step circulation methods as main:In circulating mother liquor, add water and potassium chloride, when temperature reduces, potassium nitrate crystal is separated out. In mother liquor, add ammonium nitrate, then through steamingSend out concentrated after, crystallisation by cooling, separates out ammonia chloride crystal. Mother liquor after separation returns as circulating mother liquor.
At present, domestic existing preparing potassium nitrate by means of double decomposition combined producting ammonium chloride there is no realizes the operating procedure of continous way completely, as withLower two kinds of representational technological processes:
Chinese patent literature CN1827526A (application number 200510094223.X) discloses a kind of process for preparing potassium nitrate by double decompositionMethod, raw material potassium chloride and ammonium nitrate and fresh water (FW) complete after preparation with certain proportion, send in vacuum cooling crystallizer nitreAcid potassium crystallization is also grown up; Crystal solution through thickener thickening again through centrifuge continuous separate from going out product potassium nitrate. Isolated motherLiquid through with reactant liquor heat exchange after send into natural-circulation evaporator evaporation and concentration; Solution after concentrated is through cold crystallization, thickener thickeningIsolate continuously ammonium chloride byproduct through centrifuge again, gained secondary mother liquid returns to make-up tank. This potassium nitrate crystal technique is behaviour in batchesDo, belong to Batch Process technique; When ammonium chloride evaporating and concentrating process, adopt backward feed, an effect normal pressure, two effect negative pressure economic benefits and social benefits concentrate,Improved steam utilization, but its two effect temperature at 125-130 DEG C, temperature is higher, and the corrosion resistance of equipment material is requiredHarsh; The latent heat of indirect steam does not make full use of. And after the method is concentrated, adopt the intermittence with outer circulation water heat exchange cold crystallizationFormula mode of operation, efficiency is lower.
Chinese patent literature CNCN101628723A (application number 200910044146.5) discloses metathesis reaction and has generated nitric acidThe method of potassium and ammonium chloride, at the temperature of 110 DEG C, by ammonium nitrate and potassium chloride, the ratio that is 1:2 by ammonium ion and chlorionExample is water-soluble, continues to add potassium chloride and water, heats while stirring, reaches the hypersaturated state of potassium nitrate, stops heating and makes solutionIn vacuum cooling crystallizer, be cooled to 36-40 DEG C and separate out potassium nitrate crystals, the centrifuge of putting into liner filter cloth obtains Temperature,The mother liquor I separating is another common saturation point of potassium nitrate, ammonium chloride, by the dry finished product nitre of obtaining after cold water washing for TemperatureAcid potassium, in mother liquor I and cleaning solution, adds ammonium nitrate, and adjustment solution concentration reaches the saturation state of ammonium chloride, at Vacuum ConcentrationIn device, carry out negative pressure evaporation, the centrifugal ammonium chloride of separating out that leaches, obtains solid ammonium chloride product. The method mainly exists as followsDefect: 1. the control of primary crystallization temperature is high, and product yield is low. 2., after after primary crystallization being separated, mother liquor mixes with ammonium nitrate, adoptWith and to flow double-effect evaporation concentrated, but it is high to be difficult to overcome two effect material viscosity, the coefficient of heat transfer reduces and the vaporising device that causes is produced energyThe problem of the decline of power. 3. the concentrated rear conventional type of cooling decrease temperature crystalline that adopts of ammonium chloride, belongs to intermittent operation mode, and efficiency is lowUnder.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of system and method for continous way preparing potassium nitrate by means of double decomposition is provided, canReach minimizing energy consumption, reduce equipment loss, expand production capacity, reduce work production intensity, the object of enhancing productivity.
Term explanation:
Ammonium chloride mother liquor: ammonium chloride mother liquor of the present invention refers in double decomposition process for producing potassium nitrate and produces after ammonium chloride crystalsRaw solution, comprises potassium chloride, ammonium nitrate, potassium nitrate, ammonium chloride component in solution.
Technical scheme of the present invention is as follows:
A system for continous way preparing potassium nitrate by means of double decomposition, comprises dissolving tank, potassium nitrate vacuum crystallization device, a stiffDevice, centrifuge, mixing tank for coating colors, concentrating and preheating device, adverse current triple effect enrichment facility, vacuum continuous crystalizer, secondary thickenerWith secondary centrifuging machine; The discharging opening of described dissolving tank is connected with the charging aperture of potassium nitrate vacuum crystallization device, potassium nitrate vacuum-junctionThe discharging opening of brilliant device is connected with the charging aperture of a thickener, the charging aperture of the discharging opening of a thickener and a centrifugeBe connected, the liquid outlet opening of a centrifuge is connected with the charging aperture of mixing tank for coating colors, the discharging opening of mixing tank for coating colors and concentrating and preheating deviceCharging aperture be connected, the discharging opening of concentrating and preheating device is connected with the charging aperture of adverse current triple effect enrichment facility, adverse current triple effect is concentratedThe discharging opening of device is connected with the charging aperture of vacuum continuous crystalizer, the discharging opening of vacuum continuous crystalizer and secondary thickenerCharging aperture is connected, and the discharging opening of secondary thickener is connected with the charging aperture of secondary centrifuging machine, the liquid discharging of secondary centrifuging machineMouth is connected with the charging aperture of dissolving tank;
Described adverse current triple effect enrichment facility comprise an effect enrichment facility, two effect enrichment facilities, triple effect enrichment facilities, vacuum system,Vacuum condenser and concentrating and preheating device, an effect enrichment facility comprises an effect heater, an effect separation chamber, effect circulating pump and an effectDischarging pump, two effect enrichment facilities comprise two effect heaters, two effect separation chambers, two effect circulating pumps and two effect discharging pumps, triple effect is concentratedDevice comprises triple effect heater, triple effect separation chamber, triple effect circulating pump and triple effect discharging pump; The charging aperture of one effect circulating pump and an effectThe bottom of separation chamber is connected, and the discharging opening of an effect circulating pump is connected with bottom and an effect discharging pump of an effect heater respectively,The discharging opening of one effect discharging pump is connected with the charging aperture of vacuum continuous crystalizer, an effect heater top and an effect bottom, separation chamberBy pipeline communication, an effect top, separation chamber is connected with two effect heater tops by pipeline;
The charging aperture of two effect circulating pumps is connected with the bottom of two effect separation chambers, and the discharging opening of two effect circulating pumps heats with two effects respectivelyThe bottom of device and two effect discharging pumps are connected, and the discharging opening of two effect discharging pumps is connected with the bottom of an effect heater, two effect heatingDevice top and two effect bottoms, separation chamber are by pipeline communication, and two effect tops, separation chamber are connected with triple effect heater top by pipelineLogical;
The charging aperture of triple effect circulating pump is connected with the bottom of triple effect separation chamber, and the discharging opening of triple effect circulating pump heats with triple effect respectivelyThe bottom of device and triple effect discharging pump are connected, and the discharging opening of triple effect discharging pump is connected with the bottom of two effect heaters, triple effect heatingDevice top and bottom, triple effect separation chamber are by pipeline communication, and top, triple effect separation chamber is by the steam inlet of pipeline and concentrating and preheating deviceBe connected; Concentrating and preheating device is connected with triple effect heater bottom and vacuum condenser by pipeline, and vacuum condenser passes through pipelineBe connected with vacuum system.
Preferred according to the present invention, described potassium nitrate vacuum crystallization device is connected by discharging pump by 2～10 vacuum crystallizersConnect, vacuum crystallizer comprises crystallizer, condenser and vacuum, and the upper end of crystallizer is connected with upper end of condenser by pipelineLogical, condenser lower end is connected with vacuum by pipeline, and the discharging opening that is arranged at crystallizer lower end is connected with discharging pump.
Preferred according to the present invention, described vacuum continuous crystalizer is DTB crystallizer, OSLO crystallizer.
Preferred according to the present invention, described potassium nitrate vacuum crystallization device is connected in series by discharging pump by 6 vacuum crystallizers.
Preferred according to the present invention, described vacuum is vavuum pump.
A method of utilizing said system continous way preparing potassium nitrate by means of double decomposition, step is as follows:
In dissolving tank, add circulating mother liquor, water and potassium chloride, heating for dissolving, makes mixed solution, and described circulating mother liquor isAmmonium chloride mother liquor, in mixed solution, the mol ratio of ammonium ion and chlorion is 1:(1～1.2), mixed solution enters nitric acid successivelyPotassium vacuum crystallization device, a thickener, a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, and wetting phase potassium nitrate is through dryDry, the cooling potassium nitrate that obtains; The potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors, then adds ammonium nitrate to chlorine in mixing tank for coating colorsChange ammonium and reach capacity, after mixing, feed liquid enters adverse current triple effect enrichment facility after the preheating of concentrating and preheating device, is concentrated into densityBe 1.30～1.37g/cm3After, send into the crystallization of vacuum continuous crystalizer, then pass through successively secondary thickener, secondary centrifuging machine, warpCentrifugation ammonia chloride crystal, separates the ammonium chloride mother liquor obtaining and adds in dissolving tank and recycle.
Preferred according to the present invention, the heating-up temperature of described heating for dissolving is 65～90 DEG C.
Preferred according to the present invention, described potassium nitrate vacuum crystallization device is six grades of vacuum that 6 vacuum crystallizers are composed in seriesCrystallizer, 65～80 DEG C of the temperature of one-level vacuum crystallizer, vacuum is 0.010～0.030MPa, secondary vacuum crystallizerTemperature is 50～65 DEG C, and vacuum is 0.007～0.010MPa, and the temperature of three grades of vacuum crystallizers is 42～50 DEG C, vacuumBe 0.006～0.007MPa, the temperature of level Four vacuum crystallizer is 35～42 DEG C, and vacuum is 0.003～0.006MPa, fiveThe temperature of level vacuum crystallizer is 25～35 DEG C, and vacuum is 0.0023～0.003MPa, and the temperature of six grades of vacuum crystallizers is15～25 DEG C, vacuum is 0.0010～0.0023MPa.
Preferred according to the present invention, described ammonium nitrate is that ammonium nitrate solid or mass concentration are not less than 65% ammonium nitrate solution.
Preferred according to the present invention, in the effect of one in described adverse current triple effect enrichment facility enrichment facility, temperature is 110～115 DEG C,Vacuum is 0.18～0.25MPa, and in two effect enrichment facilities, temperature is 90～100 DEG C, and vacuum is 0.08～0.10MPa, threeIn effect enrichment facility, temperature is 60～80 DEG C, and vacuum is 0.01～0.05MPa.
Preferred according to the present invention, in described vacuum continuous crystalizer, temperature is 50～70 DEG C, and vacuum is 0.07～0.10MPa.
A method for continous way preparing potassium nitrate by means of double decomposition, step is as follows:
(1) ammonium chloride mother liquor, water and potassium chloride are mixed, be heated to 65～90 DEG C of dissolvings, make ammonium ion and chlorionMol ratio be 1:1～1.2, make mixed solution;
(2) mixed solution step (1) being made carries out six grades of vacuum crystallizations, 65～80 DEG C of the temperature of one-level vacuum crystallizer,Vacuum is 0.020～0.040MPa, and the temperature of secondary vacuum crystallizer is 50～65 DEG C, and vacuum is 0.012～0.020MPa,The temperature of three grades of vacuum crystallizers is 42～50 DEG C, and vacuum is 0.008～0.012MPa, and the temperature of level Four vacuum crystallizer is35～42 DEG C, vacuum is 0.004～0.008MPa, and the temperature of Pyatyi vacuum crystallizer is 25～35 DEG C, and vacuum is0.0023～0.004MPa, the temperature of six grades of vacuum crystallizers is 15～25 DEG C, vacuum is 0.0010～0.0023MPa; AgainThrough stiff, centrifugal, make potassium nitrate crystal and potassium nitrate mother liquor;
(3) in the potassium nitrate mother liquor making to step (2), add ammonium nitrate, Chlorine in Solution ammonium is reached capacity, be heated to50～80 DEG C, concentrated through adverse current triple effect, triple effect thickening temperature is 70～80 DEG C, and two effect thickening temperatures are 90～100 DEG C, an effectThickening temperature is 110～115 DEG C, and being concentrated into density is 1.30～1.37g/cm3, be 50～70 DEG C in temperature, vacuum is 0.07～Crystallization under the condition of 0.10MPa, through stiff, centrifugal, make ammonia chloride crystal and ammonium chloride mother liquor, ammonium chloride mother liquor participates in stepSuddenly the reaction cycle utilization of (1).
Above-mentioned preparation and method are as do not specified, all by state of the art.
Beneficial effect
1, the system and method for continous way preparing potassium nitrate by means of double decomposition of the present invention, adopts new potassium nitrate vacuum crystallizationMentality of designing, more accurate to crystallization process control, the Quality and yield of potassium nitrate crystal is more stable, and can continuous dosing,Continuous discharge, has realized serialization production.
2, the present invention is applied to vacuum continuous crystalizer in the technical process of producing potassium nitrate side product sodium chloride first, more traditionalThe heat exchange type of cooling is compared, and saves the production time, raises the efficiency, and has realized serialization production.
3, the present invention adopts adverse current triple effect concentration technology concentrated to chloride slip, has not only reduced cost of investment, and concentratedTemperature is low, has alleviated the corrosion of slip to equipment, has saved steam use amount, has reduced energy consumption.
4, adverse current triple effect concentration technology of the present invention adopts forced circulation concentrated, by controlling higher velocity in pipes, reduces heat exchangeScale formation in device.
5, the system and method for continous way preparing potassium nitrate by means of double decomposition of the present invention, has realized the serialization of a whole set of technique,Expand production capacity, reduced work production intensity, improved the production efficiency of process for producing potassium nitrate.
6, the concentrated and continuous vacuum continuous crystalizer of the present invention adopts adverse current triple effect forced circulation has improved ammonium chloride productStability, has increased ammonium chloride yield.
Brief description of the drawings:
Fig. 1 is the process flow diagram of continous way double decomposition Production of Potassium Nitrate of the present invention;
Fig. 2 is potassium nitrate vacuum crystallization device schematic diagram of the present invention;
Wherein: A, crystallizer, B, condenser, C, vavuum pump, D, discharging pump;
Fig. 3 is that adverse current triple effect forced circulation of the present invention is concentrated, vacuum continuous crystallisation device schematic diagram;
Wherein: 1, vacuum system, 2, triple effect separation chamber, 3, triple effect heater, 4, two effect separation chambers, 5, two effect heatingDevice, 6, an effect separation chamber, 7, an effect heater, 8, triple effect circulating pump, 9, triple effect discharging pump, 10, two effect circulating pumps,11, two effect discharging pumps, 12, an effect circulating pump, 13, an effect discharging pump, 14, vacuum condenser, 15, concentrating and preheating device.
Detailed description of the invention
Below in conjunction with embodiment, technical scheme of the present invention is described further, but scope of the present invention is not limited to this.
The raw material using in embodiment is common commercially available.
Embodiment 1
A system for continous way preparing potassium nitrate by means of double decomposition, comprises dissolving tank, potassium nitrate vacuum crystallization device, a stiffDevice, centrifuge, mixing tank for coating colors, concentrating and preheating device, adverse current triple effect enrichment facility, vacuum continuous crystalizer, secondary thickenerWith secondary centrifuging machine; The discharging opening of described dissolving tank is connected with the charging aperture of potassium nitrate vacuum crystallization device, potassium nitrate vacuum-junctionThe discharging opening of brilliant device is connected with the charging aperture of a thickener, the charging aperture of the discharging opening of a thickener and a centrifugeBe connected, the liquid outlet opening of a centrifuge is connected with the charging aperture of mixing tank for coating colors, the discharging opening of mixing tank for coating colors and concentrating and preheating deviceCharging aperture be connected, the discharging opening of concentrating and preheating device is connected with the charging aperture of adverse current triple effect enrichment facility, adverse current triple effect is concentratedThe discharging opening of device is connected with the charging aperture of vacuum continuous crystalizer, the discharging opening of vacuum continuous crystalizer and secondary thickenerCharging aperture is connected, and the discharging opening of secondary thickener is connected with the charging aperture of secondary centrifuging machine, the liquid discharging of secondary centrifuging machineMouth is connected with the charging aperture of dissolving tank;
Described potassium nitrate vacuum crystallization device is connected in series by discharging pump by 6 vacuum crystallizers, and vacuum crystallizer comprises knotBrilliant device A, condenser B and vavuum pump C, the upper end of crystallizer A is connected with condenser B upper end by pipeline, condenser BLower end is connected with vavuum pump C by pipeline, and the discharging opening that is arranged at crystallizer A lower end is connected with discharging pump D;
Described adverse current triple effect enrichment facility comprises an effect enrichment facility, two effect enrichment facilities, triple effect enrichment facility, vacuum system1, vacuum condenser 14 and concentrating and preheating device 15, one effect enrichment facilities comprise an effect heater 7, an effect separation chamber 6, an effectCirculating pump 12 and effect discharging pump 13, two effect enrichment facilities comprise two effect heaters 5, two effect separation chambers 4, two effect circulating pumps10 and two imitate discharging pump 11, and triple effect enrichment facility comprises triple effect heater 3, triple effect separation chamber 2, triple effect circulating pump 8 and triple effectDischarging pump 9; The charging aperture of one effect circulating pump 12 is connected with the bottom of an effect separation chamber 6, the discharging opening of an effect circulating pump 12Be connected with bottom and an effect discharging pump 13 of an effect heater 7 respectively, discharging opening and the vacuum of an effect discharging pump 13 are tied continuouslyThe charging aperture of brilliant device is connected, and effect heater 7 tops and effect 6 bottoms, separation chamber are by pipeline communication, and one imitates separation chamber 6Top is connected with two effect heater 5 tops by pipeline;
Two effect circulating pumps 10 charging apertures with two effect separation chambers 4 bottoms be connected, two imitate circulating pumps 10 discharging opening respectively withThe bottom of two effect heaters 5 and two effect discharging pumps 11 are connected, the end of the discharging opening of two effect discharging pumps 11 and an effect heater 7Portion is connected, and two effect heater 5 tops and two effect 4 bottoms, separation chamber are by pipeline communication, and two effect 4 tops, separation chamber are by pipeRoad is connected with triple effect heater 3 tops;
The charging aperture of triple effect circulating pump 8 is connected with the bottom of triple effect separation chamber 2, and the discharging opening of triple effect circulating pump 8 is respectively with threeBottom and the triple effect discharging pump 9 of effect heater 3 are connected, and the discharging opening of triple effect discharging pump 9 and two is imitated the bottom phase of heaters 5Connect, triple effect heater 3 tops and 2 bottoms, triple effect separation chamber are by pipeline communication, 2 tops, triple effect separation chamber by pipeline withThe steam inlet of concentrating and preheating device 15 is connected; Concentrating and preheating device 15 is by pipeline and triple effect heater 3 bottoms and vacuum condensationDevice 14 is connected, and vacuum condenser 14 is connected with vacuum system 1 by pipeline;
Described vacuum continuous crystalizer is DTB crystallizer, OSLO crystallizer.
Embodiment 2
A method of utilizing the system continous way preparing potassium nitrate by means of double decomposition described in embodiment 1, step is as follows:
In dissolving tank, add circulating mother liquor, water and potassium chloride, be steam heated to 75 DEG C and also stir and make it to dissolve completely, make mixedClose solution, described circulating mother liquor is ammonium chloride mother liquor, and in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1, mixesSolution enters in six grades of series connection vacuum crystallization devices of potassium nitrate successively, controls the temperature 70 C of one-level vacuum crystallizer, and vacuum is0.035MPa, the temperature of secondary vacuum crystallizer is 55 DEG C, and vacuum is 0.018MPa, and the temperature of three grades of vacuum crystallizers is42 DEG C, vacuum is 0.010MPa, and the temperature of level Four vacuum crystallizer is 35 DEG C, and vacuum is 0.007MPa, Pyatyi vacuumThe temperature of crystallizer is 25 DEG C, and vacuum is 0.005MPa, and the temperature of six grades of vacuum crystallizers is 15 DEG C, and vacuum is0.004MPa. Then by a thickener, a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, wetting phase potassium nitrate warpDry, the cooling potassium nitrate that obtains; The potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors, and then adding mass concentration is 65%Ammonium nitrate solution reaches capacity to ammonium chloride in mixing tank for coating colors, and after mixing, feed liquid enters adverse current three after the preheating of concentrating and preheating deviceEffect enrichment facility, being concentrated into density is 1.35g/cm3After, controlling temperature in an effect enrichment facility is 110 DEG C, vacuum is0.23MPa, in two effect enrichment facilities, temperature is 90 DEG C, and vacuum is 0.09MPa, and in triple effect enrichment facility, temperature is 75 DEG C,Vacuum is 0.03MPa; Then send into the crystallization of DTB vacuum continuous crystalizer, 60 DEG C of crystallization temperatures, then pass through secondary stiffDevice, then secondary centrifuging machine, through centrifugation ammonia chloride crystal, separates the ammonium chloride mother liquor obtaining and adds circulation profit in dissolving tankWith.
After testing, gained potassium nitrate product K2O：44.0wt％，Cl-: 1.6wt%, ammonium chloride product total nitrogen content is 25.3wt%.
Embodiment 3
A method of utilizing the system continous way preparing potassium nitrate by means of double decomposition described in embodiment 1, step is as follows:
In dissolving tank, add circulating mother liquor, water and potassium chloride, be steam heated to 80 DEG C and also stir and make it to dissolve completely, make mixedClose solution, described circulating mother liquor is ammonium chloride mother liquor, and in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1.1, mixedClose solution and enter successively in six grades of series connection vacuum crystallization devices of potassium nitrate, 75 DEG C of the temperature of control one-level vacuum crystallizer, vacuumFor 0.030MPa, the temperature of secondary vacuum crystallizer is 60 DEG C, and vacuum is 0.015MPa, the temperature of three grades of vacuum crystallizersBe 45 DEG C, vacuum is 0.008MPa, and the temperature of level Four vacuum crystallizer is 38 DEG C, and vacuum is 0.006MPa, and Pyatyi is trueThe temperature of empty crystallizer is 30 DEG C, and vacuum is 0.0028MPa, and the temperature of six grades of vacuum crystallizers is 20 DEG C, and vacuum is0.0023MPa. Then by a thickener, a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, wetting phase potassium nitrateDrying, the cooling potassium nitrate that obtains; The potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors, and then adding mass concentration is 80%Ammonium nitrate solution reach capacity to ammonium chloride in mixing tank for coating colors, after mixing, feed liquid enters adverse current after the preheating of concentrating and preheating deviceTriple effect enrichment facility, being concentrated into density is 1.36g/cm3After, controlling temperature in an effect enrichment facility is 115 DEG C, vacuum is0.20MPa, in two effect enrichment facilities, temperature is 95 DEG C, and vacuum is 0.085MPa, and in triple effect enrichment facility, temperature is 80 DEG C,Vacuum is 0.03MPa; Then send into the crystallization of OSLO vacuum continuous crystalizer, 60 DEG C of crystallization temperatures, then pass through secondary stiffDevice, then secondary centrifuging machine, through centrifugation ammonia chloride crystal, separates the ammonium chloride mother liquor obtaining and adds circulation profit in dissolving tankWith.
After testing, gained potassium nitrate product K2O：44.2wt％，Cl-: 0.9wt%, ammonium chloride product total nitrogen content is 25.6wt%.
Embodiment 4
A method of utilizing the system continous way preparing potassium nitrate by means of double decomposition described in embodiment 1, step is as follows:
In dissolving tank, add circulating mother liquor, water and potassium chloride, be steam heated to 90 DEG C and also stir and make it to dissolve completely, make mixedClose solution, described circulating mother liquor is ammonium chloride mother liquor, and in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1.2, mixedClose solution and enter successively in six grades of series connection vacuum crystallization devices of potassium nitrate, 80 DEG C of the temperature of control one-level vacuum crystallizer, vacuumFor 0.020MPa, the temperature of secondary vacuum crystallizer is 65 DEG C, and vacuum is 0.012MPa, the temperature of three grades of vacuum crystallizersBe 50 DEG C, vacuum is 0.007MPa, and the temperature of level Four vacuum crystallizer is 42 DEG C, and vacuum is 0.005MPa, and Pyatyi is trueThe temperature of empty crystallizer is 35 DEG C, and vacuum is 0.0025MPa, and the temperature of six grades of vacuum crystallizers is 25 DEG C, and vacuum is0.0020MPa. Then by a thickener, a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, wetting phase potassium nitrateDrying, the cooling potassium nitrate that obtains; The potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors, and then adding mass concentration is 70%Ammonium nitrate solution reach capacity to ammonium chloride in mixing tank for coating colors, after mixing, feed liquid enters adverse current after the preheating of concentrating and preheating deviceTriple effect enrichment facility, being concentrated into density is 1.37g/cm3After, controlling temperature in an effect enrichment facility is 115 DEG C, vacuum is0.22MPa, in two effect enrichment facilities, temperature is 100 DEG C, and vacuum is 0.08MPa, and in triple effect enrichment facility, temperature is 80 DEG C,Vacuum is 0.04MPa; Then send into the crystallization of OSLO vacuum continuous crystalizer, 50 DEG C of crystallization temperatures, then pass through secondary stiffDevice, then secondary centrifuging machine, through centrifugation ammonia chloride crystal, separates the ammonium chloride mother liquor obtaining and adds circulation profit in dissolving tankWith.
After testing, gained potassium nitrate product K2O：44.9wt％，Cl-: 0.6wt%, ammonium chloride product total nitrogen content is 25.1wt%.
Embodiment 5
A method of utilizing the system continous way preparing potassium nitrate by means of double decomposition described in embodiment 1, step is as follows:
In dissolving tank, add circulating mother liquor, water and potassium chloride, be steam heated to 65 DEG C and also stir and make it to dissolve completely, make mixedClose solution, described circulating mother liquor is ammonium chloride mother liquor, and in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1, mixesSolution enters in six grades of series connection vacuum crystallization devices of potassium nitrate successively, controls the temperature 60 C of one-level vacuum crystallizer, and vacuum is0.040MPa, the temperature of secondary vacuum crystallizer is 55 DEG C, and vacuum is 0.019MPa, and the temperature of three grades of vacuum crystallizers is45 DEG C, vacuum is 0.011MPa, and the temperature of level Four vacuum crystallizer is 40 DEG C, and vacuum is 0.007MPa, Pyatyi vacuumThe temperature of crystallizer is 30 DEG C, and vacuum is 0.0038MPa, and the temperature of six grades of vacuum crystallizers is 20 DEG C, and vacuum is0.0022MPa. Then by a thickener, a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, wetting phase potassium nitrateDrying, the cooling potassium nitrate that obtains; The potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors, and then adding mass concentration is 85%Ammonium nitrate solution reach capacity to ammonium chloride in mixing tank for coating colors, after mixing, feed liquid enters adverse current after the preheating of concentrating and preheating deviceTriple effect enrichment facility, being concentrated into density is 1.34g/cm3After, controlling temperature in an effect enrichment facility is 110 DEG C, vacuum is0.25MPa, in two effect enrichment facilities, temperature is 90 DEG C, and vacuum is 0.08MPa, and in triple effect enrichment facility, temperature is 70 DEG C,Vacuum is 0.03MPa; Then send into the crystallization of OSLO vacuum continuous crystalizer, 65 DEG C of crystallization temperatures, then pass through secondary stiffDevice, then secondary centrifuging machine, through centrifugation ammonia chloride crystal, separates the ammonium chloride mother liquor obtaining and adds circulation profit in dissolving tankWith.
After testing, gained potassium nitrate product K2O：44.5wt％，Cl-: 1.1wt%, ammonium chloride product total nitrogen content is25.5wt％。
Embodiment 6
A method of utilizing the system continous way preparing potassium nitrate by means of double decomposition described in embodiment 1, step is as follows:
In dissolving tank, add circulating mother liquor, water and potassium chloride, be steam heated to 70 DEG C and also stir and make it to dissolve completely, make mixedClose solution, described circulating mother liquor is ammonium chloride mother liquor, and in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1.1, mixedClose solution and enter successively in six grades of series connection vacuum crystallization devices of potassium nitrate, 65 DEG C of the temperature of control one-level vacuum crystallizer, vacuumFor 0.038MPa, the temperature of secondary vacuum crystallizer is 55 DEG C, and vacuum is 0.018MPa, the temperature of three grades of vacuum crystallizersBe 42 DEG C, vacuum is 0.010MPa, and the temperature of level Four vacuum crystallizer is 38 DEG C, and vacuum is 0.006MPa, and Pyatyi is trueThe temperature of empty crystallizer is 30 DEG C, and vacuum is 0.0035MPa, and the temperature of six grades of vacuum crystallizers is 23 DEG C, and vacuum is0.0020MPa. Then by a thickener, a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, wetting phase potassium nitrateDrying, the cooling potassium nitrate that obtains; The potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors, and then adding mass concentration is 85%Ammonium nitrate solution reach capacity to ammonium chloride in mixing tank for coating colors, after mixing, feed liquid enters adverse current after the preheating of concentrating and preheating deviceTriple effect enrichment facility, being concentrated into density is 1.32g/cm3After, controlling temperature in an effect enrichment facility is 115 DEG C, vacuum is0.20MPa, in two effect enrichment facilities, temperature is 90 DEG C, and vacuum is 0.09MPa, and in triple effect enrichment facility, temperature is 70 DEG C,Vacuum is 0.02MPa; Then send into the crystallization of OSLO vacuum continuous crystalizer, 55 DEG C of crystallization temperatures, then pass through secondary stiffDevice, then secondary centrifuging machine, through centrifugation ammonia chloride crystal, separates the ammonium chloride mother liquor obtaining and adds circulation profit in dissolving tankWith.
After testing, gained potassium nitrate product K2O：44.7wt％，Cl-: 0.5wt%, ammonium chloride product total nitrogen content is 25.3wt%.
Claims (12)
1. a system for continous way preparing potassium nitrate by means of double decomposition, is characterized in that, comprises dissolving tank, potassium nitrate vacuum crystallizationDevice, thickener, centrifuge, mixing tank for coating colors, concentrating and preheating device, adverse current triple effect enrichment facility, vacuum continuous crystalizer,Secondary thickener and secondary centrifuging machine; The discharging opening of described dissolving tank is connected with the charging aperture of potassium nitrate vacuum crystallization device,The discharging opening of potassium nitrate vacuum crystallization device is connected with the charging aperture of a thickener, the discharging opening of a thickener with onceThe charging aperture of centrifuge is connected, and the liquid outlet opening of a centrifuge is connected with the charging aperture of mixing tank for coating colors, the going out of mixing tank for coating colorsMaterial mouthful is connected with the charging aperture of concentrating and preheating device, the charging aperture phase of the discharging opening of concentrating and preheating device and adverse current triple effect enrichment facilityBe communicated with, the discharging opening of adverse current triple effect enrichment facility is connected with the charging aperture of vacuum continuous crystalizer, vacuum continuous crystalizerDischarging opening is connected with the charging aperture of secondary thickener, and the discharging opening of secondary thickener is connected with the charging aperture of secondary centrifuging machineLogical, the liquid outlet opening of secondary centrifuging machine is connected with the charging aperture of dissolving tank;
Described adverse current triple effect enrichment facility comprises an effect enrichment facility, two effect enrichment facilities, triple effect enrichment facility, vacuum systemSystem, vacuum condenser and concentrating and preheating device, one effect enrichment facility comprise an effect heater, one effect separation chamber, one effect circulating pump andOne effect discharging pump, two effect enrichment facilities comprise two effect heaters, two effect separation chambers, two effect circulating pumps and two effect discharging pumps, triple effectEnrichment facility comprises triple effect heater, triple effect separation chamber, triple effect circulating pump and triple effect discharging pump; One effect circulating pump charging aperture withThe bottom of one effect separation chamber is connected, and the discharging opening of an effect circulating pump is imitated discharging pump phase with the bottom and of an effect heater respectivelyBe communicated with, the discharging opening of an effect discharging pump is connected with the charging aperture of vacuum continuous crystalizer, an effect heater top and an effect pointFrom bottom, chamber, by pipeline communication, an effect top, separation chamber is connected with two effect heater tops by pipeline;
The charging aperture of two effect circulating pumps is connected with the bottom of two effect separation chambers, and the discharging opening of two effect circulating pumps adds with two effects respectivelyThe bottom of hot device and two effect discharging pumps are connected, and the discharging opening of two effect discharging pumps is connected with the bottom of an effect heater, two effectsHeater top and two effect bottoms, separation chamber are by pipeline communication, and two effect tops, separation chamber are by pipeline and triple effect heater topBe connected;
The charging aperture of triple effect circulating pump is connected with the bottom of triple effect separation chamber, and the discharging opening of triple effect circulating pump adds with triple effect respectivelyThe bottom of hot device and triple effect discharging pump are connected, and the discharging opening of triple effect discharging pump is connected with the bottom of two effect heaters, triple effectHeater top and bottom, triple effect separation chamber are by pipeline communication, and top, triple effect separation chamber is by the steaming of pipeline and concentrating and preheating deviceVapour entrance is connected; Concentrating and preheating device is connected with triple effect heater bottom and vacuum condenser by pipeline, vacuum condenserBe connected with vacuum system by pipeline.
2. the system as claimed in claim 1, is characterized in that, described potassium nitrate vacuum crystallization device is by 2 ~ 10 vacuum-junctionsBrilliant device is connected in series by discharging pump, and vacuum crystallizer comprises crystallizer, condenser and vacuum, and the upper end of crystallizer is by pipeRoad is connected with upper end of condenser, and condenser lower end is connected with vacuum by pipeline, is arranged at the discharging of crystallizer lower endMouth is connected with discharging pump.
3. the system as claimed in claim 1, is characterized in that, described vacuum continuous crystalizer is DTB crystallizer, OSLO knotBrilliant device.
4. the system as claimed in claim 1, is characterized in that, described potassium nitrate vacuum crystallization device is by 6 vacuum crystallizationsDevice is connected in series by discharging pump.
5. system as claimed in claim 2, is characterized in that, described vacuum is vavuum pump.
6. the system of the continous way preparing potassium nitrate by means of double decomposition described in a claim 1-3 any one is produced the side of potassium nitrateMethod, is characterized in that, step is as follows:
In dissolving tank, add circulating mother liquor, water and potassium chloride, heating for dissolving, makes mixed solution, and described circulating mother liquor isAmmonium chloride mother liquor, in mixed solution, the mol ratio of ammonium ion and chlorion is 1:(1～1.2), mixed solution enters nitric acid successivelyPotassium vacuum crystallization device, a thickener, a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, and wetting phase potassium nitrate is through dryDry, the cooling potassium nitrate that obtains; The potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors, then adds ammonium nitrate to chlorine in mixing tank for coating colorsChange ammonium and reach capacity, after mixing, feed liquid enters adverse current triple effect enrichment facility after the preheating of concentrating and preheating device, is concentrated into densityBe 1.30～1.37g/cm3After, send into the crystallization of vacuum continuous crystalizer, then pass through successively secondary thickener, secondary centrifuging machine, warpCentrifugation ammonia chloride crystal, separates the ammonium chloride mother liquor obtaining and adds in dissolving tank and recycle.
7. method as claimed in claim 6, is characterized in that, the heating-up temperature of described heating for dissolving is 65～90 DEG C.
8. method as claimed in claim 6, is characterized in that, described potassium nitrate vacuum crystallization device is 6 vacuum crystallizationsSix grades of vacuum crystallizers that device is composed in series, 65～80 DEG C of the temperature of one-level vacuum crystallizer, vacuum is 0.010～0.030MPa, the temperature of secondary vacuum crystallizer is 50～65 DEG C, vacuum is 0.007～0.010MPa, three grades of vacuum crystallizationsThe temperature of device is 42～50 DEG C, and vacuum is 0.006～0.007MPa, and the temperature of level Four vacuum crystallizer is 35～42 DEG C, trueReciprocal of duty cycle is 0.003～0.006MPa, and the temperature of Pyatyi vacuum crystallizer is 25～35 DEG C, vacuum is 0.0023～0.003MPa, the temperature of six grades of vacuum crystallizers is 15～25 DEG C, vacuum is 0.0010～0.0023MPa.
9. method as claimed in claim 6, is characterized in that, described ammonium nitrate is that ammonium nitrate solid or mass concentration are not littleIn 65% ammonium nitrate solution.
10. method as claimed in claim 6, is characterized in that, the concentrated dress of the effect of one in described adverse current triple effect enrichment facilityPutting middle temperature is 110～115 DEG C, and vacuum is 0.18～0.25MPa, and in two effect enrichment facilities, temperature is 90～100 DEG C, vacuumDegree is 0.08～0.10MPa, and in triple effect enrichment facility, temperature is 60～80 DEG C, and vacuum is 0.01～0.05MPa.
11. methods as claimed in claim 6, is characterized in that, in described vacuum continuous crystalizer, temperature is 50～70 DEG C, trueReciprocal of duty cycle is 0.07～0.10MPa.
The method of 12. 1 kinds of continous way preparing potassium nitrate by means of double decomposition, is characterized in that, step is as follows:
(1) ammonium chloride mother liquor, water and potassium chloride are mixed, be heated to 65～90 DEG C of dissolvings, make ammonium ion and chlorionMol ratio is 1:1～1.2, makes mixed solution;
(2) mixed solution step (1) being made carries out six grades of vacuum crystallizations, 65～80 DEG C of the temperature of one-level vacuum crystallizer,Vacuum is 0.020～0.040MPa, and the temperature of secondary vacuum crystallizer is 50～65 DEG C, vacuum is 0.012～0.020MPa, the temperature of three grades of vacuum crystallizers is 42～50 DEG C, vacuum is 0.008～0.012MPa, level Four vacuum crystallizationThe temperature of device is 35～42 DEG C, and vacuum is 0.004～0.008MPa, and the temperature of Pyatyi vacuum crystallizer is 25～35 DEG C, trueReciprocal of duty cycle is 0.0023～0.004MPa, and the temperature of six grades of vacuum crystallizers is 15～25 DEG C, vacuum is 0.0010～0.0023MPa; Through stiff, centrifugal again, make potassium nitrate crystal and potassium nitrate mother liquor;
(3) in the potassium nitrate mother liquor making to step (2), add ammonium nitrate, Chlorine in Solution ammonium is reached capacity, be heated to 50 ~80 DEG C, concentrated through adverse current triple effect, triple effect thickening temperature is 70～80 DEG C, and two effect thickening temperatures are 90～100 DEG C, the concentrated temperature of an effectDegree is 110～115 DEG C, and being concentrated into density is 1.30～1.37g/cm3, be 50～70 DEG C in temperature, vacuum is 0.07～Crystallization under the condition of 0.10MPa, through stiff, centrifugal, make ammonia chloride crystal and ammonium chloride mother liquor, ammonium chloride mother liquor participates in step(1) reaction cycle utilization.
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| CN201454126U (en) * | 2009-08-18 | 2010-05-12 | 湖南丹化农资有限公司 | Vacuum concentration device for separating ammonium chloride in production of potassium nitrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| AU1916200A (en) * | 1998-11-20 | 2000-06-13 | Board Of Trustees Of Michigan State University | Porous ceramic composites |
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| DE3413687A1 (en) * | 1983-04-11 | 1985-01-24 | Perstorp Ab, Perstorp | METHOD FOR THE MICROBIAL PRODUCTION OF POLYSACCHARIDES |
| CN101628723A (en) * | 2009-08-18 | 2010-01-20 | 湖南丹化农资有限公司 | Method for preparing potassium nitrate and ammonium chloride employing double decomposition reaction |
| CN201454126U (en) * | 2009-08-18 | 2010-05-12 | 湖南丹化农资有限公司 | Vacuum concentration device for separating ammonium chloride in production of potassium nitrate |
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