CN104261437B - A kind ofly produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining - Google Patents
A kind ofly produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining Download PDFInfo
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- CN104261437B CN104261437B CN201410530993.3A CN201410530993A CN104261437B CN 104261437 B CN104261437 B CN 104261437B CN 201410530993 A CN201410530993 A CN 201410530993A CN 104261437 B CN104261437 B CN 104261437B
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- C—CHEMISTRY; METALLURGY
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- 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
- C01D9/10—Preparation by double decomposition with ammonium nitrate
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Abstract
The present invention relates to a kind ofly produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining, this system comprises Production of Potassium Nitrate system and liquid ammonium nitrate production system, and described Production of Potassium Nitrate system comprises dissolving tank, potassium nitrate vacuum crystallization device, a thickener, centrifuge, mixing tank for coating colors, concentrating and preheating device, forced circulation adverse current triple effect enrichment facility, vacuum continuous crystalizer, secondary thickener and a secondary centrifuging machine; Liquid ammonium nitrate production system comprise ammonia evaporator, gas ammonia filter, ammonia preheater, tubular reactor, in and scrubbing tower and flash tank, the present invention has developed and has a set ofly produced with liquid ammonium nitrate the continous way Production of Potassium Nitrate new technology combining, improve the production efficiency of process for producing potassium nitrate, more accurate to crystallization process control, the Quality and yield of potassium nitrate crystal is more stable.
Description
Technical field
The present invention relates to a kind ofly produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining, belong to chemical production technicalField.
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 solid ammonium nitrate, thenAfter evaporation and concentration, crystallisation by cooling, separate 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. When the method evaporating and concentrating process, adoptWith backward feed, an effect normal pressure, two effect negative pressure economic benefits and social benefits are concentrated, have improved steam utilization, but its two effects temperature is at 125-130 DEG C,Temperature is higher, requires stricter to the corrosion resistance of equipment material; And after the method is concentrated, adopt and outer circulation water heat exchange cold analysis knotBrilliant intermittent operation mode, efficiency is lower.
Chinese patent literature CN101628723A (application number 200910044146.5) discloses metathesis reaction and has generated potassium nitrateWith the method for ammonium chloride, at the temperature of 110 DEG C, by ammonium nitrate and potassium chloride, the ratio that is 1:2 in ammonium ion and chlorionWater-soluble, continue to add potassium chloride and water, heat while stirring, reach the hypersaturated state of potassium nitrate, stop heating solution is existedIn 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, separatesMother liquor I be another common saturation point of potassium nitrate, ammonium chloride, by the dry finished product potassium nitrate of obtaining after cold water washing for Temperature,In mother liquor I and cleaning solution, add ammonium nitrate, adjustment solution concentration reaches the saturation state of ammonium chloride, in vacuum concentrating apparatusCarry out negative pressure evaporation, the centrifugal ammonium chloride of separating out that leaches, obtains solid ammonium chloride product. Primary crystallization is separated stepmother by the methodAfter liquid mixes with ammonium nitrate solid, adopt and flow double-effect evaporation to concentrate, but it is high to be difficult to overcome two effect material viscosity, the coefficient of heat transfer fallsThe problem of the decline of the low and vaporising device production capacity that causes. The method adopts type of cooling decrease temperature crystalline, belongs to intermittent operationMode, inefficiency.
Ammonium nitrate high temperature, high pressure and have can be oxidized material exist under can blast, therefore ammonium nitrate is in the time of production and applicationHave certain danger, in particularly on September 30th, 2002, the General Office of the State Council has issued the Office of the State Council and has sent out [2002] No. 52 " about enteringOne step is strengthened the notice of civil detonation article safety management ", strengthen the management and control to agricultural ammonium nitrate. And existing potassium nitrate four stepsIn round-robin method, be main mainly with adding ammonium nitrate solid greatly, as Chinese patent literature CN101628723A (application number200910044146.5) disclosed metathesis reaction generates method, the Chinese patent literature of potassium nitrate and ammonium chlorideThe method of CN101643226A (application number 200910115875.5) disclosed Production of Potassium Nitrate by Double Decomposition-Circulation Method and ammonium chloride is equalTo add ammonium nitrate solid after a mother liquid evaporation after potassium nitrate crystal is concentrated. Chinese patent literature CN101643226A (ShenPlease number 011108280.1) method, the Chinese patent literature CN101643226A (Shen of disclosed a kind of process for preparing potassium nitrate by double decompositionPlease number 01106898.1) ammonium nitrate solid adds nitre by the method for disclosed raising solid phase potassium nitrate concentration and product potassium nitrate qualityEvaporation and concentration again in a mother liquor after acid potassium crystallization. Chinese patent literature CN100374372A (application number200510094223.X) method of disclosed a kind of process for preparing potassium nitrate by double decomposition by adding ammonium nitrate in primary crystallization mother liquorLiquid, has avoided the danger of ammonium nitrate solid in storage, transport, use procedure. But the ammonium nitrate solution using in embodimentConcentration is low, causes enormous pressure to subsequent evaporation is concentrated, and energy consumption is higher, and the production technology of ammonium nitrate solution unexposed.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of and liquid ammonium nitrate and produce the continous way Production of Potassium Nitrate system combiningSystem, can reach minimizing energy consumption, realizes the serialization production that DCS controls, and expands Production of Potassium Nitrate scale, improves production safetyObject with efficiency.
Technical scheme of the present invention is as follows:
Produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining, comprise Production of Potassium Nitrate system and liquid nitreAcid ammonium production system, described Production of Potassium Nitrate system comprises dissolving tank, potassium nitrate vacuum crystallization device, thickener,Inferior centrifuge, mixing tank for coating colors, concentrating and preheating device, adverse current triple effect enrichment facility, vacuum continuous crystalizer, secondary thickener and secondaryCentrifuge; The discharging opening of described dissolving tank is connected with the charging aperture of potassium nitrate vacuum crystallization device, potassium nitrate vacuum crystallization deviceDischarging opening be connected with the charging aperture of a thickener, the discharging opening of a thickener is connected with the charging aperture of a centrifuge,The liquid outlet opening of a centrifuge is connected with the charging aperture of mixing tank for coating colors, the charging aperture of the discharging opening of mixing tank for coating colors and concentrating and preheating deviceBe connected, the discharging opening of concentrating and preheating device is connected with the charging aperture of adverse current triple effect enrichment facility, the going out of adverse current triple effect enrichment facilityMaterial mouthful is connected with the charging aperture of vacuum continuous crystalizer, the charging aperture phase of the discharging opening of vacuum continuous crystalizer and secondary thickenerBe communicated with, the discharging opening of secondary thickener is connected with the charging aperture of secondary centrifuging machine, the liquid outlet opening of secondary centrifuging machine and dissolvingThe charging aperture of groove is connected;
Described liquid ammonium nitrate production system comprises ammonia evaporator, gas ammonia filter, ammonia preheater, tubular reactor, neutralizationScrubbing tower and flash tank, described tubular reactor is provided with the first import, the second import, the first outlet and the second outlet, dodgesSteam groove and be provided with the first charging aperture, the second charging aperture and discharging opening, the discharging opening of ammonia evaporator is communicated with the import of gas ammonia filter,The outlet of gas ammonia filter is communicated with the import of ammonia preheater, and the outlet of ammonia preheater is communicated with the first charging aperture of tubular reactor,The second charging aperture by tubular reactor passes into rare nitric acid to tubular reactor, the first outlet of tubular reactor and neutralization washingThe import of tower is communicated with, in be connected with the first charging aperture of flash tank with washing pump in passing through with the outlet of scrubbing tower, tubular reactorSecond outlet be communicated with the second charging aperture of flash tank, the outlet of flash tank is communicated with mixing tank for coating colors in Production of Potassium Nitrate system, sudden strain of a muscleSteaming groove material out finally flows in the mixing tank for coating colors in Production of Potassium Nitrate system;
Described adverse current triple effect enrichment facility is forced circulation adverse current triple effect enrichment facility, comprise an effect forced circulation enrichment facility,Two effect forced circulation enrichment facilities, triple effect forced circulation enrichment facility, vacuum system, condenser and concentrating and preheating device, an effect is strongCirculation enrichment facility processed comprises an effect heater, an effect separation chamber, an effect circulating pump and an effect discharging pump, and two effect forced circulation are denseCompression apparatus comprises two effect heaters, two effect separation chambers, two effect circulating pumps and two effect discharging pumps, triple effect forced circulation enrichment facility bagDraw together 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 effect separation chamberBottom be connected, the discharging opening of an effect circulating pump is connected with the bottom of an effect heater and an effect discharging pump respectively, one imitates outThe discharging opening of material pump is connected with the charging aperture of vacuum continuous crystalizer, and an effect heater top and an effect bottom, separation chamber are by pipeRoad is communicated with, and 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 pipeline;
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 connected with concentrating and preheating device by pipeline; DenseContracting preheater is connected with triple effect heater bottom and condenser by pipeline, and condenser is connected with vacuum system by pipeline.
Described flash tank can be primary flash tank, can be also the series connection of two-stage flash groove.
Described potassium nitrate vacuum crystallization device is the device of 2～10 grades of cascaded structures, and every one-level cascaded structure comprises crystallizer, coldCondenser, vavuum pump and discharging pump, the upper end of crystallizer is communicated with the upper end of condenser by pipeline, and the lower end of condenser is by pipeRoad is connected with vavuum pump, and the lower end of condenser is also connected with tank by condensing water conduit, the lower end of crystallizer by pipeline with go outMaterial pump connects, and the discharging opening of discharging pump is connected with next stage crystallizer charging aperture, the discharging opening of dissolving tank and first order cascaded structureCrystallizer charging aperture connect, afterbody discharging pump is connected with the charging aperture of a thickener. Every grade of condenser lower end hasCondensing water conduit leads to tank, can be used as cycling use of water and returns to potassium chloride dissolving tank. N (1 < N < 10) level potassium nitrate vacuum crystallizationDevice is transferred to N+1 level potassium nitrate vacuum crystallization device by discharging pump by material, and afterbody potassium nitrate vacuum crystallization device is logicalCross discharging pump pump to thickener. Every grade of condenser lower end has condensing water conduit to lead to tank, can be used as cycling use of water and returns to dissolvingGroove. Can control every grade of temperature in potassium nitrate vacuum crystallization device by controlling the vacuum of every grade of potassium nitrate vacuum crystallization device,To ensure the Quality and yield of potassium nitrate crystal.
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 the device of 6 grades of cascaded structures.
The method that the continous way Production of Potassium Nitrate system of utilizing above-mentioned and liquid ammonium nitrate to produce to combine is produced potassium nitrate, stepRapid as follows:
In dissolving tank, add circulating mother liquor, water and potassium chloride, Steam Heating is dissolved, and makes mixed solution, described circulation motherLiquid is ammonium chloride mother liquor, and in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1～1.2, and 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;
Liquefied ammonia enters ammonia evaporator and is evaporated to gas ammonia, and gas ammonia, after gas ammonia filter filters, then enters ammonia preheater, and gas ammonia existsAmmonia preheater is heated to enter the rare nitric acid passing into the second charging aperture in tubular reactor after 90～150 DEG C and pressurizes neutralization insteadShould, the reactant liquor that reaction generates enters flash tank, utilizes reaction heat to carry out flash distillation concentrate, makes ammonium nitrate solution;
After making potassium nitrate mother liquor that ammonium nitrate solution goes out with centrifugation and mixing in mixing channel, feed liquid is through concentrating and preheating deviceAfter preheating, enter forced circulation adverse current triple effect enrichment facility, being concentrated into density is 1.30～1.37g/cm3After, send into vacuum and tie continuouslyBrilliant device crystallization, then pass through successively secondary thickener, secondary centrifuging machine, through centrifugation ammonia chloride crystal, separate the chlorination obtainingAmmonium mother liquor adds in dissolving tank and recycles.
Preferred according to the present invention, the heating-up temperature that in dissolving tank, Steam Heating is dissolved is 65～90 DEG C.
Preferred according to the present invention, described potassium nitrate vacuum crystallization device is the device of 6 grades of cascaded structures; Wherein, one-level knotIn brilliant device, temperature is controlled at 65～80 DEG C, and vacuum is 0.020～0.040MPa; In secondary crystallization device, temperature is controlled at 50～65 DEG C,Vacuum is 0.012～0.020MPa; In three grades of crystallizers, temperature is controlled at 42～50 DEG C, and vacuum is 0.005～0.012MPa;In level Four crystallizer, temperature is controlled at 35～42 DEG C, and vacuum is 0.003～0.005MPa; In Pyatyi crystallizer, temperature is controlled at25～35 DEG C, vacuum is 0.0020～0.003MPa; In six grades of crystallizers, temperature is controlled at 15～25 DEG C, and vacuum is0.0010～0.0020MPa。
Preferred according to the present invention, passing into rare nitric acid mass concentration in tubular reactor is 40～60wt%, the reaction of tubular reactorPressure is 0.2～0.6MPa, and reaction temperature relies on exothermic heat of reaction to provide, and the concentration of flash liquid, controls by the temperature of indirect steamSystem.
Preferred according to the present invention, the described ammonium nitrate solution mass concentration obtaining from flash tank concentrate is 75%～95wt%.
Preferred according to the present invention, gas ammonia and the rare nitric acid technique containing ammonia or nitric acid that neutralization reaction is discharged in tubular reactor is steamedRare nitric acid or ammonia stripping during vapour enters and scrubbing tower for, the rare ammonium nitrate solution obtaining after washing by pump into flash distillation with washing pumpGroove, process steam can be used as the thermal source of flash vaporization or supplies outward.
Preferred according to the present invention, temperature in the effect of one in described forced circulation adverse current triple effect enrichment facility forced circulation enrichment facilityDegree is 110～115 DEG C, and vacuum is 0.18～0.25MPa, and in two effect forced circulation enrichment facilities, temperature is 90～100 DEG C, trueReciprocal of duty cycle is 0.08～0.10MPa, and in triple effect forced circulation 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.
Preferred according to the present invention, this technique can realize automation control by DCS system is installed.
With the method that liquid ammonium nitrate is produced the continous way potassium nitrate combining, step is as follows:
(1) ammonium chloride mother liquor, water and potassium chloride are mixed, are steam heated to 65～90 DEG C of dissolvings, make mixed solution,In mixed solution, the mol ratio of ammonium ion and chlorion is 1:1～1.2,
(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 0.005～0.012MPa, and the temperature of level Four vacuum crystallizer is35～42 DEG C, vacuum is 0.003～0.005MPa, and the temperature of Pyatyi vacuum crystallizer is 25～35 DEG C, vacuum is 0.0020～0.0030MPa, the temperature of six grades of vacuum crystallizers is 15～25 DEG C, vacuum is 0.0010～0.0020MPa;
(3) material after step (2) vacuum crystallization is entered to thickener one time, make the out water content control of material of thickenerBuilt in 40～50%, then once centrifugal, make potassium nitrate crystal and potassium nitrate mother liquor;
(4) liquefied ammonia is evaporated to gas ammonia after being heated to 5～15 DEG C, and then gas ammonia is heated to 90～150 DEG C at ammonia preheater after filteringAfter enter in tubular reactor and rare nitric acid neutralization reaction of pressurizeing, the molar ratio of controlling gas ammonia and nitric acid is 0.8～1.2: 1.The reactant liquor flash distillation concentrate that reaction generates, makes the ammonium nitrate solution that mass concentration is 75%-95wt%;
(5) after step (4) being made to potassium nitrate mother liquor that ammonium nitrate solution makes with step (3) and mixing in mixing channel,Ammonium nitrate solution and potassium nitrate mother liquor ratio are (5～10): 1, and concentrated through forced circulation adverse current triple effect, triple effect thickening temperature is 70～80 DEG C, two effect thickening temperatures are 90～100 DEG C, and an effect thickening temperature is 110～115 DEG C, be concentrated into density and be 1.30～1.37g/cm3, water content 50～80%, is 50～70 DEG C in temperature, crystallization under the condition that vacuum is 0.07～0.10MPa,Then enter secondary thickener, make thickener out the moisture mass content of material be controlled at 30～45%, then secondary centrifuging,Make ammonia chloride crystal and ammonium chloride mother liquor, ammonium chloride mother liquor participates in the reaction cycle utilization of step (1).
In above preparation method not special instruction all according to prior art.
The present invention has the following advantages and beneficial effect:
1, the present invention has developed and has a set ofly produced with liquid ammonium nitrate the continous way Production of Potassium Nitrate new technology combining, and has improved potassium nitrateThe production efficiency of production technology, avoids the danger in the purchase of raw material ammonium nitrate, transport, storage, greatly reduces production cost.
2, the present invention adopts brand-new potassium nitrate vacuum crystallization design, more accurate to crystallization process control, the quality of potassium nitrate crystalMore stable with output.
3, adopt flash process to produce ammonium nitrate solution, the explosion danger of having avoided traditional mode of production device to cause, and the nitric acid of producingAmmonium salt solution concentration is high, and little to follow-up concentration technology pressure, the time of staying is short, little to equipment corrosion, capable of reducing energy consumption.
4, the present invention adopts adverse current triple effect concentration technology concentrated to chloride slip, has not only reduced thickening temperature, has alleviated slipTo the corrosion of equipment, also greatly save steam use amount, reduce energy consumption.
5, adverse current triple effect concentration technology of the present invention adopts forced circulation concentrated, by controlling higher velocity in pipes, reduces heat exchangerInterior scale formation.
6, the present invention is applied to vacuum continuous crystalizer in the crystallization process of ammonium chloride, and more traditional heat exchange type of cooling is compared, realShow continued operation, saved the production time, raised the efficiency.
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 forced circulation adverse current triple effect enrichment facility of the present invention, 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 heaters,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, condenser, 15, concentrating and preheating device, 16, vacuumContinuous crystalizer.
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
Produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining, comprise Production of Potassium Nitrate system and liquid nitreAcid ammonium production system, described Production of Potassium Nitrate system comprises dissolving tank, potassium nitrate vacuum crystallization device, thickener,Inferior centrifuge, mixing tank for coating colors, concentrating and preheating device, adverse current triple effect enrichment facility, vacuum continuous crystalizer, secondary thickener and secondaryCentrifuge; The discharging opening of described dissolving tank is connected with the charging aperture of potassium nitrate vacuum crystallization device, potassium nitrate vacuum crystallization deviceDischarging opening be connected with the charging aperture of a thickener, the discharging opening of a thickener is connected with the charging aperture of a centrifuge,The liquid outlet opening of a centrifuge is connected with the charging aperture of mixing tank for coating colors, the charging aperture of the discharging opening of mixing tank for coating colors and concentrating and preheating deviceBe connected, the discharging opening of concentrating and preheating device is connected with the charging aperture of adverse current triple effect enrichment facility, the going out of adverse current triple effect enrichment facilityMaterial mouthful is connected with the charging aperture of vacuum continuous crystalizer, the charging aperture phase of the discharging opening of vacuum continuous crystalizer and secondary thickenerBe communicated with, the discharging opening of secondary thickener is connected with the charging aperture of secondary centrifuging machine, the liquid outlet opening of secondary centrifuging machine and dissolvingThe charging aperture of groove is connected; Potassium nitrate vacuum crystallization device is the device of 6 grades of cascaded structures, and every one-level cascaded structure comprises crystallizationDevice A, condenser B, vavuum pump C and discharging pump D, the upper end of crystallizer A is communicated with the upper end of condenser B by pipeline,The lower end of condenser B is connected with vavuum pump C by pipeline, and the lower end of condenser B is also connected with tank by condensing water conduit,The lower end of crystallizer A is connected with discharging pump D by pipeline, and the discharging opening of discharging pump D is connected with next stage crystallizer charging aperture,The discharging opening of dissolving tank is connected with the charging aperture of the crystallizer of first order cascaded structure, afterbody discharging pump and a thickenerCharging aperture connects. Every grade of condenser lower end has condensing water conduit to lead to tank, can be used as cycling use of water and returns to potassium chloride dissolving tank.N (1 < N < 10) level potassium nitrate vacuum crystallization device is transferred to N+1 level potassium nitrate vacuum crystallization device by discharging pump by material,Afterbody potassium nitrate vacuum crystallization device passes through discharging pump pump to thickener. Every grade of condenser lower end has condensing water conduit to lead toTank, can be used as cycling use of water and returns to dissolving tank. Can control often by the vacuum of controlling every grade of potassium nitrate vacuum crystallization deviceTemperature in level potassium nitrate vacuum crystallization device, to ensure the Quality and yield of potassium nitrate crystal.
Adverse current triple effect enrichment facility is forced circulation adverse current triple effect enrichment facility, comprises an effect forced circulation enrichment facility, two effects by forceCirculation enrichment facility processed, triple effect forced circulation enrichment facility, vacuum system 1, condenser 14 and concentrating and preheating device 15, one effects are strongCirculation enrichment facility processed comprises that an effect heater 7, an effect separation chamber 6, an effect circulating pump 12 and effect discharging pump 13, two effects are strongCirculation enrichment facility processed comprises two effect heaters 5, two effect separation chambers 4, two effect circulating pumps 10 and two effect discharging pumps 11, and triple effect is strongCirculation enrichment facility processed comprises triple effect heater 3, triple effect separation chamber 2, triple effect circulating pump 8 and triple effect discharging pump 9; One effect circulationThe charging aperture of pump 12 with one effect separation chamber 6 bottom be connected, one effect circulating pump 12 discharging opening respectively with an effect heater 7Bottom and one effect discharging pump 13 be connected, one effect discharging pump 13 discharging opening be connected with the charging aperture of vacuum continuous crystalizer,One effect heater 7 tops and effect 6 bottoms, separation chamber are by pipeline communication, and effect 6 tops, separation chamber add by pipeline and two effectsHot device 5 tops are connected;
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 condenser 14Be connected, condenser 14 is connected with vacuum system 1 by pipeline.
Described liquid ammonium nitrate production system comprises ammonia evaporator, gas ammonia filter, ammonia preheater, tubular reactor, neutralizationScrubbing tower and flash tank, described tubular reactor is provided with the first import, the second import, the first outlet and the second outlet, dodgesSteam groove and be provided with the first charging aperture, the second charging aperture and discharging opening, the discharging opening of ammonia evaporator is communicated with the import of gas ammonia filter,The outlet of gas ammonia filter is communicated with the import of ammonia preheater, and the outlet of ammonia preheater is communicated with the first charging aperture of tubular reactor,The second charging aperture by tubular reactor passes into rare nitric acid to tubular reactor, the first outlet of tubular reactor and neutralization washingThe import of tower is communicated with, in pass through with the outlet of scrubbing tower in washing pump and flash tank the first charging aperture be connected, pipe reactionThe second outlet of device is communicated with the second charging aperture of flash tank, and the outlet of flash tank is communicated with mixing tank for coating colors in Production of Potassium Nitrate system,Flash tank material out finally flows in the mixing tank for coating colors in Production of Potassium Nitrate system.
Described vacuum continuous crystalizer is DTB crystallizer, OSLO crystallizer.
Embodiment 2
Utilize described in embodiment 1 and to produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining and produce continuously potassium nitrateMethod, step is as follows:
(1) in dissolving tank, add circulating mother liquor, water and potassium chloride, mix, be steam heated to 75 DEG C of dissolvings, makeMixed solution, described circulating mother liquor is ammonium chloride mother liquor, in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1,
(2) mixed solution enters potassium nitrate vacuum crystallization device successively, and potassium nitrate vacuum crystallization device is the dress of 6 grades of cascaded structuresPut; The temperature 70 C of one-level vacuum crystallizer, vacuum is 0.035MPa, the temperature of secondary vacuum crystallizer is 55 DEG C, trueReciprocal of duty cycle is 0.018MPa, and the temperature of three grades of vacuum crystallizers is 42 DEG C, and vacuum is 0.010MPa, level Four vacuum crystallizerTemperature is 35 DEG C, and vacuum is 0.003MPa, and the temperature of Pyatyi vacuum crystallizer is 25 DEG C, and vacuum is 0.003MPa, sixThe temperature of level vacuum crystallizer is 15 DEG C, and vacuum is 0.001MPa;
(3) material after step (2) vacuum crystallization is entered to thickener one time, make thickener out material containing water qualityContent is controlled at 40%, and then, through a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, wetting phase potassium nitrate drying,The cooling potassium nitrate that obtains, the potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors;
(4) liquefied ammonia enters ammonia evaporator and is heated to 10 DEG C and is evaporated to gas ammonia, and gas ammonia, after gas ammonia filter filters, then entersAmmonia preheater, gas ammonia is heated to enter after 90 DEG C at ammonia preheater the mass concentration passing into the second charging aperture in tubular reactor65% rare nitric acid neutralization reaction of pressurizeing, controlling ammonia is 1:1 with the mol ratio of nitric acid, the reactant liquor of reaction generation enters sudden strain of a muscleSteam groove, utilize reaction heat to carry out flash distillation concentrate, obtain the ammonium nitrate solution that mass concentration is 80wt%; In tubular reactor, dischargeAmmonia enter in and the rare nitric acid of scrubbing tower wash, the ammonium nitrate solution obtaining after washing enters flash tank. The technique of flash tankSteam is condensed into process condensate water circulation through evaporative condenser and uses.
(5) the potassium nitrate mother liquor that the ammonium nitrate solution that mass concentration step (4) being made is 80wt% and step (3) makeAfter mixing in mixing tank for coating colors, the mass ratio of ammonium nitrate solution and potassium nitrate mother liquor is 5:1, and feed liquid is through the preheating of concentrating and preheating deviceAfter enter forced circulation adverse current triple effect enrichment facility, being concentrated into density is 1.35g/cm3After, control an effect forced circulation enrichment facilityMiddle temperature is 110 DEG C, and in two effect forced circulation enrichment facilities, temperature is 90 DEG C, and in triple effect forced circulation enrichment facility, temperature is75 DEG C, then send into the crystallization of DTB vacuum continuous crystalizer, 60 DEG C of crystallization temperatures, vacuum is 0.10MPa, then passes through secondaryThickener, make thickener out the water content of material be controlled at 40%, then secondary centrifuging machine, through centrifugation ammonium chloride crystalline substanceBody, separates the ammonium chloride mother liquor obtaining and adds in dissolving tank and recycle. Gained potassium nitrate product K2O：44.0wt％，Cl-：1.6wt%, ammonium chloride product total nitrogen content is 25.3wt%.
Embodiment 3
Utilize described in embodiment 1 and to produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining and produce continuously potassium nitrateMethod, step is as follows:
(1) in dissolving tank, add circulating mother liquor, water and potassium chloride, mix, be steam heated to 80 DEG C of dissolvings, makeMixed solution, described circulating mother liquor is ammonium chloride mother liquor, in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1.1,
(2) mixed solution enters potassium nitrate vacuum crystallization device successively, and potassium nitrate vacuum crystallization device is the dress of 6 grades of cascaded structuresPut; 75 DEG C of the temperature of one-level vacuum crystallizer, vacuum is 0.030MPa, the temperature of secondary vacuum crystallizer is 60 DEG C, trueReciprocal of duty cycle is 0.015MPa, and the temperature of three grades of vacuum crystallizers is 45 DEG C, and vacuum is 0.008MPa, level Four vacuum crystallizerTemperature is 38 DEG C, and vacuum is 0.004MPa, and the temperature of Pyatyi vacuum crystallizer is 30 DEG C, and vacuum is 0.0028MPa,The temperature of six grades of vacuum crystallizers is 20 DEG C, and vacuum is 0.0013MPa;
(3) material after step (2) vacuum crystallization is entered to thickener one time, make thickener out material containing water qualityContent is controlled at 50%, and then, through a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, wetting phase potassium nitrate drying,The cooling potassium nitrate that obtains, the potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors;
(4) liquefied ammonia enters ammonia evaporator and is heated to 15 DEG C and is evaporated to gas ammonia, and gas ammonia, after gas ammonia filter filters, then entersAmmonia preheater, gas ammonia is heated to enter after 100 DEG C at ammonia preheater the mass concentration passing into the second charging aperture in tubular reactor40% rare nitric acid neutralization reaction of pressurizeing, controlling ammonia is 0.9:1 with the mol ratio of nitric acid, the reactant liquor of reaction generation entersFlash tank, utilizes reaction heat to carry out flash distillation concentrate, obtains the ammonium nitrate solution that mass concentration is 78wt%; In tubular reactor, arrangeDuring the ammonia going out enters, wash with rare nitric acid with scrubbing tower, the ammonium nitrate solution obtaining after washing enters flash tank. The work of flash tankSkill steam is condensed into process condensate water circulation through evaporative condenser and uses.
(5) the potassium nitrate mother liquor that the ammonium nitrate solution that mass concentration step (4) being made is 78wt% and step (3) makeAfter mixing in mixing tank for coating colors, the mass ratio of ammonium nitrate solution and potassium nitrate mother liquor is 9:1, and feed liquid is through the preheating of concentrating and preheating deviceAfter enter forced circulation adverse current triple effect enrichment facility, being concentrated into density is 1.35g/cm3, water content is 65%, control an effect and forceIn circulation enrichment facility, temperature is 115 DEG C, and in two effect forced circulation enrichment facilities, temperature is 95 DEG C, the concentrated dress of triple effect forced circulationPutting middle temperature is 80 DEG C, then sends into the crystallization of OSLO vacuum continuous crystalizer, 70 DEG C of crystallization temperatures, and vacuum is 0.075MPa,Pass through again secondary thickener, make thickener out the water content of material be controlled at 35%, then secondary centrifuging machine, through centrifugal pointFrom ammonia chloride crystal, separate the ammonium chloride mother liquor obtaining and add in dissolving tank and recycle.
Gained potassium nitrate product K2O：44.2wt％，Cl-: 0.9wt%, ammonium chloride product total nitrogen content is 25.6wt%.
Embodiment 4
Utilize described in embodiment 1 and to produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining and produce continuously potassium nitrateMethod, step is as follows:
(1) in dissolving tank, add circulating mother liquor, water and potassium chloride, mix, be steam heated to 90 DEG C of dissolvings, makeMixed solution, described circulating mother liquor is ammonium chloride mother liquor, in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1.2,
(2) mixed solution enters potassium nitrate vacuum crystallization device successively, and potassium nitrate vacuum crystallization device is the dress of 6 grades of cascaded structuresPut; 80 DEG C of the temperature of one-level vacuum crystallizer, vacuum is 0.020MPa, the temperature of secondary vacuum crystallizer is 65 DEG C, trueReciprocal of duty cycle is 0.012MPa, and the temperature of three grades of vacuum crystallizers is 50 DEG C, and vacuum is 0.007MPa, level Four vacuum crystallizerTemperature is 42 DEG C, and vacuum is 0.005MPa, and the temperature of Pyatyi vacuum crystallizer is 35 DEG C, and vacuum is 0.003MPa, sixThe temperature of level vacuum crystallizer is 25 DEG C, and vacuum is 0.0020MPa;
(3) material after step (2) vacuum crystallization is entered to thickener one time, make thickener out material containing water qualityContent is controlled at 45%, and then, through a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, wetting phase potassium nitrate drying,The cooling potassium nitrate that obtains, the potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors;
(4) liquefied ammonia enters ammonia evaporator and is heated to 15 DEG C and is evaporated to gas ammonia, and gas ammonia, after gas ammonia filter filters, then entersAmmonia preheater, gas ammonia is heated to enter after 100 DEG C at ammonia preheater the mass concentration passing into the second charging aperture in tubular reactor56% rare nitric acid neutralization reaction of pressurizeing, controlling ammonia is 1.1:1 with the mol ratio of nitric acid, the reactant liquor of reaction generation entersFlash tank, utilizes reaction heat to carry out flash distillation concentrate, obtains the ammonium nitrate solution that mass concentration is 95wt%; In tubular reactor, arrangeDuring the ammonia going out enters, wash with rare nitric acid with scrubbing tower, the ammonium nitrate solution obtaining after washing enters flash tank. The work of flash tankSkill steam is condensed into process condensate water circulation through evaporative condenser and uses.
(5) the potassium nitrate mother liquor that the ammonium nitrate solution that mass concentration step (4) being made is 95wt% and step (3) make existsAfter mixing in mixing tank for coating colors, the mass ratio of ammonium nitrate solution and potassium nitrate mother liquor is 8:1, and feed liquid is after the preheating of concentrating and preheating deviceEnter forced circulation adverse current triple effect enrichment facility, being concentrated into density is 1.36g/cm3, water content is 60%, control an effect and force to followIn ring enrichment facility, temperature is 115 DEG C, and in two effect forced circulation enrichment facilities, temperature is 100 DEG C, triple effect forced circulation enrichment facilityMiddle temperature is 80 DEG C, then sends into the crystallization of OSLO vacuum continuous crystalizer, 70 DEG C of crystallization temperatures, and vacuum is 0.08MPa,Pass through again secondary thickener, make thickener out the water content of material be controlled at 35%, then secondary centrifuging machine, through centrifugal pointFrom ammonia chloride crystal, separate the ammonium chloride mother liquor obtaining and add in dissolving tank and recycle.
Gained potassium nitrate product K2O：44.9wt％，Cl-: 0.6wt%, ammonium chloride product total nitrogen content is 25.1%.
Embodiment 5
Utilize described in embodiment 1 and to produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining and produce continuously potassium nitrateMethod, step is as follows:
(1) in dissolving tank, add circulating mother liquor, water and potassium chloride, mix, be steam heated to 65 DEG C of dissolvings, makeMixed solution, described circulating mother liquor is ammonium chloride mother liquor, in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1,
(2) mixed solution enters potassium nitrate vacuum crystallization device successively, and potassium nitrate vacuum crystallization device is the dress of 6 grades of cascaded structuresPut; The temperature 60 C of one-level vacuum crystallizer, vacuum is 0.040MPa, the temperature of secondary vacuum crystallizer is 55 DEG C, trueReciprocal of duty cycle is 0.019MPa, and the temperature of three grades of vacuum crystallizers is 45 DEG C, and vacuum is 0.011MPa, level Four vacuum crystallizerTemperature is 40 DEG C, and vacuum is 0.0045MPa, and the temperature of Pyatyi vacuum crystallizer is 30 DEG C, and vacuum is 0.0028MPa,The temperature of six grades of vacuum crystallizers is 20 DEG C, and vacuum is 0.0012MPa;
(3) material after step (2) vacuum crystallization is entered to thickener one time, make thickener out material containing water qualityContent is controlled at 45%, and then, through a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, wetting phase potassium nitrate drying,The cooling potassium nitrate that obtains, the potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors;
(4) liquefied ammonia enters ammonia evaporator and is heated to 20 DEG C and is evaporated to gas ammonia, and gas ammonia, after gas ammonia filter filters, then entersAmmonia preheater, gas ammonia is heated to enter after 150 DEG C at ammonia preheater the mass concentration passing into the second charging aperture in tubular reactor56% rare nitric acid neutralization reaction of pressurizeing, controlling ammonia is 0.8:1 with the mol ratio of nitric acid, the reactant liquor of reaction generation entersFlash tank, utilizes reaction heat to carry out flash distillation concentrate, obtains the ammonium nitrate solution that mass concentration is 85wt%; In tubular reactor, arrangeDuring the ammonia going out enters, wash with rare nitric acid with scrubbing tower, the ammonium nitrate solution obtaining after washing enters flash tank. The work of flash tankSkill steam is condensed into process condensate water circulation through evaporative condenser and uses.
(5) the potassium nitrate mother liquor that the ammonium nitrate solution that mass concentration step (4) being made is 85wt% and step (3) makeAfter mixing in mixing tank for coating colors, the mass ratio of ammonium nitrate solution and potassium nitrate mother liquor is 9:1, and feed liquid is through the preheating of concentrating and preheating deviceAfter enter forced circulation adverse current triple effect enrichment facility, being concentrated into density is 1.37g/cm3, water content is 60%, control an effect and forceIn circulation enrichment facility, temperature is 110 DEG C, and in two effect forced circulation enrichment facilities, temperature is 90 DEG C, the concentrated dress of triple effect forced circulationPutting middle temperature is 70 DEG C, then sends into the crystallization of OSLO vacuum continuous crystalizer, 65 DEG C of crystallization temperatures, and vacuum is 0.09MPa,Pass through again secondary thickener, make thickener out the water content of material be controlled at 40%, then secondary centrifuging machine, through centrifugal pointFrom ammonia chloride crystal, separate the ammonium chloride mother liquor obtaining and add in dissolving tank and recycle.
Gained potassium nitrate product K2O：44.5wt％，Cl-: 1.1wt%, ammonium chloride product total nitrogen content is 25.5wt%
Embodiment 6
Utilize described in embodiment 1 and to produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining and produce continuously potassium nitrateMethod, step is as follows:
(1) in dissolving tank, add circulating mother liquor, water and potassium chloride, mix, be steam heated to 70 DEG C of dissolvings, makeMixed solution, described circulating mother liquor is ammonium chloride mother liquor, in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1.1,
(2) mixed solution enters potassium nitrate vacuum crystallization device successively, and potassium nitrate vacuum crystallization device is the dress of 6 grades of cascaded structuresPut; 65 DEG C of the temperature of one-level vacuum crystallizer, vacuum is 0.038MPa, the temperature of secondary vacuum crystallizer is 55 DEG C, trueReciprocal of duty cycle is 0.018MPa, and the temperature of three grades of vacuum crystallizers is 42 DEG C, and vacuum is 0.010MPa, level Four vacuum crystallizerTemperature is 38 DEG C, and vacuum is 0.004MPa, and the temperature of Pyatyi vacuum crystallizer is 30 DEG C, and vacuum is 0.0025MPa,The temperature of six grades of vacuum crystallizers is 23 DEG C, and vacuum is 0.0018MPa;
(3) material after step (2) vacuum crystallization is entered to thickener one time, make thickener out material containing water qualityContent is controlled at 70%, and then, through a centrifuge, centrifugation goes out wetting phase potassium nitrate crystal, wetting phase potassium nitrate drying,The cooling potassium nitrate that obtains, the potassium nitrate mother liquor that centrifugation goes out enters mixing tank for coating colors;
(4) liquefied ammonia enters ammonia evaporator and is heated to 8 DEG C and is evaporated to gas ammonia, and gas ammonia, after gas ammonia filter filters, then enters ammoniaPreheater, gas ammonia is heated to enter after 130 DEG C at ammonia preheater the mass concentration 56% passing into the second charging aperture in tubular reactorRare nitric acid neutralization reaction of pressurizeing, controlling ammonia is 1.2:1 with the mol ratio of nitric acid, the reactant liquor of reaction generation enters flash distillationGroove, utilizes reaction heat to carry out flash distillation concentrate, obtains the ammonium nitrate solution that mass concentration is 90wt%; In tubular reactor, dischargeDuring ammonia enters, wash with rare nitric acid with scrubbing tower, the ammonium nitrate solution obtaining after washing enters flash tank. The technique of flash tank is steamedGas is condensed into process condensate water circulation through evaporative condenser and uses.
(5) the potassium nitrate mother liquor that the ammonium nitrate solution that mass concentration step (4) being made is 90wt% and step (3) makeAfter mixing in mixing tank for coating colors, the mass ratio of ammonium nitrate solution and potassium nitrate mother liquor is 10:1, and feed liquid is pre-through concentrating and preheating deviceAfter heat, enter forced circulation adverse current triple effect enrichment facility, being concentrated into density is 1.30g/cm3, water content is 80%, controls an effect strongIn circulation enrichment facility processed, temperature is 115 DEG C, and in two effect forced circulation enrichment facilities, temperature is 90 DEG C, and triple effect forced circulation is concentratedIn device, temperature is 70 DEG C, then sends into the crystallization of OSLO vacuum continuous crystalizer, 55 DEG C of crystallization temperatures, and vacuum is 0.09MPa,Pass through again secondary thickener, make thickener out the water content of material be controlled at 32%, then secondary centrifuging machine, through centrifugal pointFrom ammonia chloride crystal, separate the ammonium chloride mother liquor obtaining and add in dissolving tank and recycle.
Gained potassium nitrate product K2O：44.7wt％，Cl-: 0.5wt%, ammonium chloride product total nitrogen content is 25.3wt%.
Claims (10)
1. produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining for one kind, comprise Production of Potassium Nitrate system and liquid ammonium nitrate production system, described Production of Potassium Nitrate 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 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 is connected with the charging aperture of a centrifuge, 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 is connected with the charging aperture of concentrating and preheating device, the discharging opening of concentrating and preheating device is connected with the charging aperture of adverse current triple effect enrichment facility, the discharging opening of adverse current triple effect enrichment facility is connected with the charging aperture of vacuum continuous crystalizer, the discharging opening of vacuum continuous crystalizer is connected with the charging aperture of secondary thickener, the discharging opening of secondary thickener is connected with the charging aperture of secondary centrifuging machine, the liquid outlet opening of secondary centrifuging machine is connected with the charging aperture of dissolving tank,
Described liquid ammonium nitrate production system comprises ammonia evaporator, gas ammonia filter, ammonia preheater, tubular reactor, in and scrubbing tower and flash tank, described tubular reactor is provided with the first import, the second import, the first outlet and the second outlet, flash tank is provided with the first charging aperture, the second charging aperture and discharging opening, the discharging opening of ammonia evaporator is communicated with the import of gas ammonia filter, the outlet of gas ammonia filter is communicated with the import of ammonia preheater, the outlet of ammonia preheater is communicated with the first charging aperture of tubular reactor, the second charging aperture by tubular reactor passes into rare nitric acid to tubular reactor, the first outlet of tubular reactor with in be communicated with the import of scrubbing tower, in be connected with the first charging aperture of flash tank with washing pump in passing through with the outlet of scrubbing tower, the second outlet of tubular reactor is communicated with the second charging aperture of flash tank, the outlet of flash tank is communicated with mixing tank for coating colors in Production of Potassium Nitrate system, flash tank material out finally flows in the mixing tank for coating colors in Production of Potassium Nitrate system,
Described adverse current triple effect enrichment facility is forced circulation adverse current triple effect enrichment facility, comprise an effect forced circulation enrichment facility, two effect forced circulation enrichment facilities, triple effect forced circulation enrichment facility, vacuum system, condenser and concentrating and preheating device, one effect forced circulation enrichment facility comprises an effect heater, one effect separation chamber, one effect circulating pump and an effect discharging pump, two effect forced circulation enrichment facilities comprise two effect heaters, two effect separation chambers, two effect circulating pumps and two effect discharging pumps, triple effect forced circulation enrichment facility 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 is connected with the bottom of an effect separation chamber, the discharging opening of one 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, and an effect heater top and an effect bottom, separation chamber are by pipe
Road is communicated with, and 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, the discharging opening of two effect circulating pumps is connected with bottom and the two effect discharging pumps of two effect heaters respectively, the discharging opening of two effect discharging pumps is connected with the bottom of an effect heater, two effect heater tops and two effect bottoms, separation chamber are by pipeline communication, and two effect tops, separation chamber are connected with triple effect heater top by pipeline;
The charging aperture of triple effect circulating pump is connected with the bottom of triple effect separation chamber, the discharging opening of triple effect circulating pump is connected with bottom and the triple effect discharging pump of triple effect heater respectively, the discharging opening of triple effect discharging pump is connected with the bottom of two effect heaters, triple effect heater top and bottom, triple effect separation chamber are by pipeline communication, and top, triple effect separation chamber is connected with concentrating and preheating device by pipeline; Concentrating and preheating device is connected with triple effect heater bottom and condenser by pipeline, and condenser is connected with vacuum system by pipeline.
2. according to claim 1ly produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining, it is characterized in that, described potassium nitrate vacuum crystallization device is the device of 2 ~ 10 grades of cascaded structures, every one-level cascaded structure comprises crystallizer, condenser, vavuum pump and discharging pump, the upper end of crystallizer is communicated with the upper end of condenser by pipeline, the lower end of condenser is connected with vavuum pump by pipeline, the lower end of condenser is also connected with tank by condensing water conduit, the lower end of crystallizer is connected with discharging pump by pipeline, the discharging opening of discharging pump is connected with next stage crystallizer charging aperture, the discharging opening of dissolving tank is connected with the charging aperture of the crystallizer of first order cascaded structure, afterbody discharging pump is connected with the charging aperture of a thickener, every grade of condenser lower end has condensing water conduit to lead to tank, can be used as cycling use of water and return to potassium chloride dissolving tank, N (1 < N < 10) level potassium nitrate vacuum crystallization device is transferred to N+1 level potassium nitrate vacuum crystallization device by discharging pump by material, afterbody potassium nitrate vacuum crystallization device passes through discharging pump pump to thickener.
3. according to claim 1ly produce with liquid ammonium nitrate the continous way Production of Potassium Nitrate system combining, it is characterized in that, described vacuum continuous crystalizer is DTB crystallizer, OSLO crystallizer, and described potassium nitrate vacuum crystallization device is the device of 6 grades of cascaded structures.
4. utilize and produce with liquid ammonium nitrate the method that the continous way Production of Potassium Nitrate system that combines is produced potassium nitrate described in claim 1, step is as follows:
In dissolving tank, add circulating mother liquor, water and potassium chloride, Steam Heating is dissolved, make mixed solution, described circulating mother liquor is ammonium chloride mother liquor, in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1～1.2, mixed solution enters potassium nitrate vacuum crystallization device, a thickener, a centrifuge successively, and centrifugation goes out wetting phase potassium nitrate crystal, wetting phase potassium nitrate drying, the cooling potassium nitrate that obtains;
Liquefied ammonia enters ammonia evaporator and is evaporated to gas ammonia, gas ammonia is after gas ammonia filter filters, then enter ammonia preheater, gas ammonia is heated to enter after 90～150 DEG C the rare nitric acid passing into the second charging aperture in the tubular reactor neutralization reaction of pressurizeing at ammonia preheater, the reactant liquor that reaction generates enters flash tank, utilize reaction heat to carry out flash distillation concentrate, make ammonium nitrate solution; After making potassium nitrate mother liquor that ammonium nitrate solution goes out with centrifugation and mixing in mixing channel, feed liquid enters forced circulation adverse current triple effect enrichment facility after the preheating of concentrating and preheating device, and being concentrated into density is 1.30～1.37g/cm3After, send into the crystallization of vacuum continuous crystalizer, then pass through successively secondary thickener, secondary centrifuging machine, through centrifugation ammonia chloride crystal, separate the ammonium chloride mother liquor obtaining and add in dissolving tank and recycle.
5. according to claim 4 and liquid ammonium nitrate are produced the method that the continous way Production of Potassium Nitrate system that combines is produced potassium nitrate, it is characterized in that, the heating-up temperature that in dissolving tank, Steam Heating is dissolved is 65～90 DEG C.
6. according to claim 4 and liquid ammonium nitrate are produced the method that the continous way Production of Potassium Nitrate system that combines is produced potassium nitrate, it is characterized in that, described potassium nitrate vacuum crystallization device is the device of 6 grades of cascaded structures; Wherein, in one-level crystallizer, temperature is controlled at 65 ~ 80 DEG C, and vacuum is 0.020 ~ 0.040MPa; In secondary crystallization device, temperature is controlled at 50 ~ 65 DEG C, and vacuum is 0.012 ~ 0.020MPa; In three grades of crystallizers, temperature is controlled at 42 ~ 50 DEG C, and vacuum is 0.005 ~ 0.012MPa; In level Four crystallizer, temperature is controlled at 35 ~ 42 DEG C, and vacuum is 0.003 ~ 0.005MPa; In Pyatyi crystallizer, temperature is controlled at 25 ~ 35 DEG C, and vacuum is 0.0020 ~ 0.0030MPa; In six grades of crystallizers, temperature is controlled at 15 ~ 25 DEG C, and vacuum is 0.0010 ~ 0.0020MPa.
7. according to claim 4 and liquid ammonium nitrate are produced the method that the continous way Production of Potassium Nitrate system that combines is produced potassium nitrate, it is characterized in that, passing into rare nitric acid mass concentration in tubular reactor is 40 ~ 60wt%, the reaction pressure of tubular reactor is 0.2 ~ 0.6MPa, reaction temperature relies on exothermic heat of reaction to provide, the concentration of flash liquid, controls by the temperature of indirect steam.
8. according to claim 4 and liquid ammonium nitrate are produced the method that the continous way Production of Potassium Nitrate system that combines is produced potassium nitrate, it is characterized in that, the described ammonium nitrate solution mass concentration obtaining from flash tank concentrate is 75% ~ 95wt%, in in described forced circulation adverse current triple effect enrichment facility effect forced circulation enrichment facility, temperature is 110～115 DEG C, vacuum is 0.18～0.25MPa, in two effect forced circulation enrichment facilities, temperature is 90～100 DEG C, vacuum is 0.08～0.10MPa, in triple effect forced circulation enrichment facility, temperature is 60～80 DEG C, vacuum is 0.01～0.05MPa.
9. according to claim 4 and liquid ammonium nitrate are produced the method that the continous way Production of Potassium Nitrate system that combines is produced potassium nitrate, it is characterized in that, in described vacuum continuous crystalizer, temperature is 50～70 DEG C, and vacuum is 0.07～0.10MPa.
10. a production method of producing the continous way potassium nitrate combining with liquid ammonium nitrate, step is as follows:
(1) ammonium chloride mother liquor, water and potassium chloride are mixed, be steam heated to 65～90 DEG C of dissolvings, make mixed solution, in mixed solution, the mol ratio of ammonium ion and chlorion is 1:1～1.2,
(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, 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 0.005～0.012MPa, the temperature of level Four vacuum crystallizer is 35～42 DEG C, vacuum is 0.003～0.005MPa, the temperature of Pyatyi vacuum crystallizer is 25～35 DEG C, vacuum is 0.0020～0.0030MPa, the temperature of six grades of vacuum crystallizers is 15～25 DEG C, vacuum is 0.0010～0.0020MPa,
(3) material after step (2) vacuum crystallization is entered to thickener one time, make thickener out the water content of material be controlled at 40 ~ 50%, then once centrifugal, make potassium nitrate crystal and potassium nitrate mother liquor;
(4) liquefied ammonia is evaporated to gas ammonia after being heated to 5 ~ 15 DEG C, after gas ammonia filters, then after being heated to 90～150 DEG C, ammonia preheater enters in tubular reactor and rare nitric acid neutralization reaction of pressurizeing, the molar ratio of controlling gas ammonia and nitric acid is 0.8 ~ 1.2: 1, the reactant liquor flash distillation concentrate that reaction generates, makes the ammonium nitrate solution that mass concentration is 75%-95wt%;
(5) after step (4) being made to potassium nitrate mother liquor that ammonium nitrate solution makes with step (3) and mixing in mixing channel, ammonium nitrate solution and potassium nitrate mother liquor ratio are (5 ~ 10): 1, mass ratio, concentrated through forced circulation adverse current triple effect, triple effect thickening temperature is 70～80 DEG C, two effect thickening temperatures are 90～100 DEG C, and an effect thickening temperature is 110～115 DEG C, and being concentrated into density is 1.30～1.37g/cm3Water content 50 ~ 80%, it is 50～70 DEG C in temperature, vacuum is crystallization under the condition of 0.07～0.10MPa, then enter secondary thickener, make thickener out the moisture mass content of material be controlled at 30 ~ 45%, then secondary centrifuging, make ammonia chloride crystal and ammonium chloride mother liquor, ammonium chloride mother liquor participates in the reaction cycle utilization of step (1).
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| CN107715484B (en) * | 2017-11-29 | 2023-06-02 | 白银昌元化工有限公司 | Potassium permanganate three-effect forced circulation evaporation system |
| CN107973324A (en) * | 2018-01-18 | 2018-05-01 | 江西金利达钾业有限责任公司 | A kind of potassium nitrate semi-finished product separate pot |
| CN108083299B (en) * | 2018-01-18 | 2023-07-28 | 江西金利达钾业有限责任公司 | Potassium nitrate crystallization production system |
| CN109908613A (en) * | 2019-02-20 | 2019-06-21 | 浙江瀚普智慧科技有限公司 | A kind of multiple-effect evaporation coupling crystallization apparatus and its technique producing nitre sodium salt |
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| CN101628732A (en) * | 2008-07-16 | 2010-01-20 | 中国科学院福建物质结构研究所 | Method for quickly preparing nano titanium dioxide ball with adjustable internal cavity |
| CN201458761U (en) * | 2009-08-18 | 2010-05-12 | 湖南丹化农资有限公司 | Vacuum cooling crystallizer for producing potassium nitrate |
| CN101643226A (en) * | 2009-09-02 | 2010-02-10 | 赵家春 | Method for producing nitrate and ammonium chloride with double decomposition circulation method |
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