CN104310440B - 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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- CN104310440B CN104310440B CN201410531096.4A CN201410531096A CN104310440B CN 104310440 B CN104310440 B CN 104310440B CN 201410531096 A CN201410531096 A CN 201410531096A CN 104310440 B CN104310440 B CN 104310440B
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- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 title claims abstract description 247
- 235000010333 potassium nitrate Nutrition 0.000 title claims abstract description 121
- 239000004323 potassium nitrate Substances 0.000 title claims abstract description 121
- 238000000034 method Methods 0.000 title claims abstract description 45
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 24
- 230000000694 effects Effects 0.000 claims abstract description 188
- 238000002425 crystallisation Methods 0.000 claims abstract description 58
- 239000002562 thickening agent Substances 0.000 claims abstract description 56
- 230000008025 crystallization Effects 0.000 claims abstract description 54
- 238000002156 mixing Methods 0.000 claims abstract description 31
- 230000002411 adverse Effects 0.000 claims abstract description 27
- 239000011248 coating agent Substances 0.000 claims abstract description 25
- 238000000576 coating method Methods 0.000 claims abstract description 25
- 239000003086 colorant Substances 0.000 claims abstract description 25
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical group [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 113
- 235000019270 ammonium chloride Nutrition 0.000 claims description 55
- 239000012452 mother liquor Substances 0.000 claims description 48
- 238000007599 discharging Methods 0.000 claims description 45
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 239000007788 liquid Substances 0.000 claims description 32
- 239000012043 crude product Substances 0.000 claims description 29
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 23
- 239000013078 crystal Substances 0.000 claims description 20
- 239000011552 falling film Substances 0.000 claims description 20
- 239000000243 solution Substances 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 16
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 15
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 11
- 241000370738 Chlorion Species 0.000 claims description 10
- 238000005119 centrifugation Methods 0.000 claims description 9
- 239000000460 chlorine Substances 0.000 claims description 9
- 238000004891 communication Methods 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 9
- 239000012047 saturated solution Substances 0.000 claims description 9
- 230000008719 thickening Effects 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 229910052801 chlorine Inorganic materials 0.000 claims description 7
- 239000012141 concentrate Substances 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 239000010413 mother solution Substances 0.000 claims description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 239000000047 product Substances 0.000 description 22
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 239000006227 byproduct Substances 0.000 description 8
- 238000001704 evaporation Methods 0.000 description 7
- 230000008020 evaporation Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000013461 design Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 238000005649 metathesis reaction Methods 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- IRPDISVJRAYFBI-UHFFFAOYSA-N nitric acid;potassium Chemical compound [K].O[N+]([O-])=O IRPDISVJRAYFBI-UHFFFAOYSA-N 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C01D9/10—Preparation by double decomposition with ammonium nitrate
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/164—Ammonium chloride
-
- C—CHEMISTRY; METALLURGY
- 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
- C01D9/16—Purification
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of system and method for continous way preparing potassium nitrate by means of double decomposition.This system comprises dissolving tank, saltpetre vacuum crystallization device, thickener, whizzer, rinse bath, secondary dissolving tank, filter, vacuum continuous crystallizer, secondary thickener, secondary centrifuging machine, mixing tank for coating colors, concentrating and preheating device, adverse current triple effect concentrating unit, secondary vacuum continuous crystallizer, three thickeners, No. three whizzers.Continous way Production of Potassium Nitrate system and method for the present invention, expands throughput, reduces work production intensity, improves the production efficiency of process for producing potassium nitrate.
Description
Technical field
The present invention relates to a kind of system and method for continous way preparing potassium nitrate by means of double decomposition, belong to chemical production technical field.
Background technology
Domestic preparing potassium nitrate by means of double decomposition mainly adopts SODIUMNITRATE-Repone K method and ammonium nitrate-Repone K method.The former cost of material is higher, and byproduct sodium chloride economic worth is lower.Ammonium nitrate-Repone K metathesis process widespread use, again based on four one-step circulation methods: add water and Repone K in circulating mother liquor, when temperature reduces, potassium nitrate crystal is separated out.In mother liquor, add ammonium nitrate, then after evaporation concentration, 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 the operating procedure realizing continous way completely, as following two kinds of representational technical process:
Chinese patent literature CN1827526A (application number 200510094223.X) discloses a kind of method of process for preparing potassium nitrate by double decomposition: after raw material Repone K and ammonium nitrate and process water complete preparation in certain proportion, send in vacuum cooling crystallizer, potassium nitrate crystal is separated out and is grown up; Crystal solution is continuously separated out product saltpetre through whizzer again through thickener thickening.Isolated mother liquor through with reaction solution heat exchange after send into natural-circulation evaporator evaporation concentration, adopt backward feed, an effect normal pressure, two effect negative pressure economic benefits and social benefits concentrate; Solution after concentrated is continuously separated out ammonium chloride byproduct through whizzer again through cold crystallization, thickener thickening, and gained secondary mother liquid returns Preparation tank.Repeat this working cycle, namely constantly obtain solid nitric acid potassium and solid ammonium chloride successively.This potassium nitrate crystal process lot operates, and belongs to batch production process; Adopt backward feed during ammonium chloride evaporating and concentrating process, an effect normal pressure, two effect negative pressure economic benefits and social benefits concentrate, and improve steam utilization, but its two effects temperature is at 125-130 DEG C, and temperature is higher, requires harsher to the erosion resistance of equipment material; The latent heat of secondary steam does not make full use of.And the method concentrates the batch operation mode of rear employing and outer circulation water heat exchange cold crystallization, efficiency is lower.
Chinese patent literature CN101628723A discloses the method (application number is 200910044146.5) that replacement(metathesis)reaction generates saltpetre and ammonium chloride: at the temperature of 110 DEG C, by ammonium nitrate and Repone K, be that the ratio of 1:2 is water-soluble in ammonium ion and chlorion, continue to add Repone K and water, heat while stirring, reach the hypersaturated state of saltpetre, stop heating making solution in vacuum cooling crystallizer, be cooled to 36-40 DEG C and separate out potassium nitrate crystals, the whizzer putting into liner filter cloth obtains Temperature, the mother liquor I be separated is saltpetre, another common saturation point of ammonium chloride, finished product saltpetre is obtained by dry after Temperature cold water washing, to mother liquor I with washings, add ammonium nitrate, adjustment strength of solution reaches the state of saturation of ammonium chloride, negative pressure evaporation is carried out in vacuum concentrating apparatus, the centrifugal ammonium chloride leaching precipitation, obtain solid ammonium chloride product.Mainly there is following defect in the method: 1. primary crystallization temperature controls high, and product yield is low.2. after after being separated by primary crystallization, mother liquor mix with ammonium nitrate, to adopt and to flow double-effect evaporation concentrated, but it is high to be difficult to overcome two effect material viscosity, coefficient of heat transfer reduction and the problem of the decline of evaporation unit throughput that causes.3. the concentrated rear employing conventional chilling mode decrease temperature crystalline of the method ammonium chloride, belongs to batch operation mode, inefficiency.
Chinese patent literature CN101643226 discloses the method (application number 200910115875.5) of Production of Potassium Nitrate by Double Decomposition-Circulation Method and ammonium chloride: with Repone K, ammonium nitrate, the aqueous solution for raw material, controls Cl in reaction soln
-with or NH
4 +concentration is respectively 16%-22%, 7-12%, and reaction soln temperature is 80-100 DEG C; Work in-process potassium nitrate crystal; Potassium nitrate crystal rinses; Multiple junction reacts; Filter, clean Cl in body refuse, saltpetre finished product cerium sulphate crystal xln finished product
-(in muriate)≤0.01%, NH
4 +(in ammonium salt)≤0.05%; And above-mentioned xln finished product is carried out processed to water content≤3%, finally carry out being dried to saltpetre water content≤0.1% and be saltpetre finished product; Above-mentioned each step filtrate recovery is carried out evaporation concentration, adds ammonium nitrate reaction, point ammonium process, crystallizing and drying prepares ammonium chloride product, and the filtrate cycle of process is to step (1).The method utilizes the flushing relief liquor of different concns to rinse work in-process, finished product and ammonium chloride, technical grade saltpetre can be prepared, but its work in-process and finished product saltpetre and ammonium chloride are all decrease temperature crystallines in crystallization water cooler, and obviously belong to periodical operation, efficiency is lower.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of system and method for continous way preparing potassium nitrate by means of double decomposition, minimizing energy consumption can be reached, reduce equipment loss, expand production capacity, reduce work production intensity, the object of enhancing productivity.
Term illustrates:
Ammonium chloride mother liquor: ammonium chloride mother liquor of the present invention refers to the solution produced after ammonium chloride crystals in double decomposition process for producing potassium nitrate, comprises Repone K, ammonium nitrate, saltpetre, 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, saltpetre vacuum crystallization device, thickener, whizzer, rinse bath, secondary dissolving tank, filter, vacuum continuous crystallizer, secondary thickener, secondary centrifuging machine, mixing tank for coating colors, concentrating and preheating device, adverse current triple effect concentrating unit, secondary vacuum continuous crystallizer, three thickeners, No. three whizzers, the discharge port of a described dissolving tank is connected with the opening for feed of saltpetre vacuum crystallization device, the discharge port of saltpetre vacuum crystallization device is connected with the opening for feed of a thickener, the discharge port of a thickener is connected with the opening for feed of a whizzer, the solids exit mouth of a whizzer is connected with the opening for feed of rinse bath, the liquid outlet opening of rinse bath is connected with one of opening for feed of mixing tank for coating colors, the solids exit mouth of rinse bath is connected with the opening for feed of secondary dissolving tank, the discharge port of secondary dissolving tank is connected with the opening for feed of filter, the discharge port of filter is connected with the opening for feed of a vacuum continuous crystallizer, the discharge port of a vacuum continuous crystallizer is connected with the opening for feed of secondary thickener, the discharge port of secondary thickener is connected with the opening for feed of secondary centrifuging machine, the liquid outlet opening of secondary centrifuging machine is connected with one of opening for feed of mixing tank for coating colors, the liquid outlet opening of a whizzer is connected with one of opening for feed of mixing tank for coating colors, the discharge port of mixing tank for coating colors is connected with the opening for feed of concentrating and preheating device, the discharge port of concentrating and preheating device is connected with the opening for feed of adverse current triple effect concentrating unit, the discharge port of adverse current triple effect concentrating unit is connected with the opening for feed of secondary vacuum continuous crystallizer, the discharge port of secondary vacuum continuous crystallizer is connected with the opening for feed of three thickeners, the discharge port of three thickeners is connected with the opening for feed of No. three whizzers, the liquid outlet opening of No. three whizzers is connected with the opening for feed of a dissolving tank,
Described saltpetre vacuum crystallization device is the device of 2 ~ 10 grades of cascaded structures, every one-level cascaded structure comprises crystallizer, condenser, vacuum, discharging pump and tank, the upper end of described crystallizer is communicated with the upper end of condenser by pipeline, the lower end of described condenser is connected with vacuum by pipeline, the lower end of described condenser is also connected with tank by condensing water conduit, the lower end of described crystallizer is connected with discharging pump by pipeline, the discharge port of a described dissolving tank is connected with the opening for feed of first step crystallizer, described last step discharging pump is connected with the opening for feed of a thickener.
Described adverse current triple effect concentrating unit comprises an effect falling film concentrating device, two effect falling film concentrating device, triple effect falling film concentrating device, concentrating and preheating device, vacuum cooler-condenser and vacuum, one effect falling film concentrating device comprises an effect well heater, an effect separate chamber, an effect recycle pump and an effect discharging pump, two effect falling film concentrating devices comprise two effect well heaters, two effect separate chambers, two effect recycle pumps and two effect discharging pumps, and triple effect falling film concentrating device comprises triple effect well heater, triple effect separate chamber, triple effect cycle pump and triple effect discharging pump;
The bottom that the opening for feed of one effect recycle pump imitates discharging pump respectively opening for feed, with one imitates separate chamber is connected with a bottom of imitating well heater, the discharge port that one discharge port and two of imitating recycle pump imitates discharging pump is connected with an opening for feed of imitating well heater top respectively, the discharge port of one effect discharging pump is connected with the opening for feed of secondary vacuum continuous crystallizer, one effect well heater and an effect bottom, separate chamber are by pipeline communication, and an effect top, separate chamber is imitated well heater top by pipeline and two and is connected;
The bottom that the opening for feeds of two effect recycle pumps imitate discharging pump respectively opening for feed, two with two imitates separate chamber is connected with two bottoms of imitating well heater, the two effect discharge ports of recycle pump are connected with two opening for feeds of imitating well heater top respectively with the discharge port of triple effect discharging pump, two effect well heaters and two effect bottoms, separate chamber are by pipeline communication, and two effect tops, separate chamber are connected with triple effect well heater top by pipeline;
The opening for feed of triple effect cycle pump respectively with the opening for feed of triple effect discharging pump, the bottom of triple effect separate chamber is connected with the bottom of triple effect well heater, the discharge port of triple effect cycle pump is connected with the opening for feed at triple effect well heater top respectively with the discharge port of concentrating and preheating device, pipeline communication is passed through in triple effect well heater and bottom, triple effect separate chamber, top, triple effect separate chamber by pipeline respectively with concentrating and preheating device steam-in, vacuum cooler-condenser top is connected, concentrating and preheating device condensate outlet is connected with condenser lower end by pipeline, condenser discharge port is connected with vacuum by pipeline.
Preferred according to the present invention, described vacuum continuous crystallizer is draft tube baffle crystallizer, OSLO crystallizer.
Preferred according to the present invention, described saltpetre vacuum crystallization device is the device of 6 grades of cascaded structures.
Preferred according to the present invention, described vacuum is vacuum pump.
Utilize a method for said system continous way preparing potassium nitrate by means of double decomposition, step is as follows:
Circulating mother liquor, water and Repone K is added in a dissolving tank, described circulating mother liquor is ammonium chloride mother liquor, heating material to 65 ~ 90 in a dissolving tank DEG C, between 1:1 ~ 1.2, are also stirred and material are dissolved completely by the molar ratio controlling ammonium ion and the chlorion added; Feed liquid enters saltpetre vacuum crystallization device, thickener, a whizzer successively, and centrifugation goes out saltpetre crude product; Saltpetre crude product after rinse bath, secondary dissolving tank, filter washing, dissolving, filtering, is sent into the crystallization of a vacuum continuous crystallizer, then is separated to obtain saltpetre through secondary thickener, secondary centrifuging machine successively successively; Centrifugal for mother liquor, wash-down water and saltpetre after the centrifugation of saltpetre crude product rear mother liquor is injected mixing tank for coating colors, add ammonium chloride in ammonium nitrate to mixing tank for coating colors to reach capacity, after mixing, feed liquid first enters adverse current triple effect concentrating unit after the preheating of concentrating and preheating device, and being concentrated into density is 1.30 ~ 1.37g/cm
3after, send into the crystallization of secondary vacuum continuous crystallizer, more successively through three thickeners, No. three whizzer separating ammonium chloride crystal, be separated the ammonium chloride mother liquor obtained and add recycle in a dissolving tank.
According to the present invention, preferably, the mode of a described dissolving tank heating is steam heating.
According to the present invention, preferably, described saltpetre vacuum crystallization device is the device of 6 grades of cascaded structures; Wherein, in first degree crystalline device, temperature controls at 65 ~ 80 DEG C, and vacuum tightness is 0.010 ~ 0.030MPa; In secondary crystallizer, temperature controls at 50 ~ 65 DEG C, and vacuum tightness is 0.007 ~ 0.010MPa; In three grades of crystallizers, temperature controls at 42 ~ 50 DEG C, and vacuum tightness is 0.006 ~ 0.007MPa; In level Four crystallizer, temperature controls at 35 ~ 42 DEG C, and vacuum tightness is 0.003 ~ 0.006MPa; In Pyatyi crystallizer, temperature controls at 25 ~ 35 DEG C, and vacuum tightness is 0.0023 ~ 0.003MPa; In six grades of crystallizers, temperature controls at 15 ~ 25 DEG C, and vacuum tightness is 0.0010 ~ 0.0023MPa.
Preferred according to the present invention, in secondary dissolving tank, saltpetre heating for dissolving becomes the saturated solution of 50-60 DEG C; In a described vacuum continuous crystallizer, Tc is 20-40 DEG C, and vacuum tightness is 0.002 ~ 0.07MPa.
Preferred according to the present invention, described ammonium nitrate is the ammonium nitrate solution that ammonium nitrate solid or mass concentration are not less than 65%.
Preferred according to the present invention, in an effect concentrating unit in described adverse current triple effect concentrating unit, temperature is 110 ~ 115 DEG C, vacuum tightness is 0.18 ~ 0.25MPa, in two effect concentrating uniies, temperature is 90 ~ 100 DEG C, vacuum tightness is 0.08 ~ 0.10MPa, in triple effect concentrating unit, temperature is 60 ~ 80 DEG C, and vacuum tightness is 0.01 ~ 0.05MPa.
In described secondary vacuum continuous crystallizer, Tc is 50-70 DEG C, and vacuum tightness 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 Repone K are mixed, be heated to 65 ~ 90 DEG C of dissolvings, make the mol ratio of ammonium ion and chlorion be 1:1 ~ 1.2, obtained mixing solutions;
(2) mixing solutions that step (1) is obtained is carried out six grades of vacuum continuous crystallisations, the temperature of one-level vacuum cyrsytalliser 65 ~ 80 DEG C, vacuum tightness is 0.010 ~ 0.030MPa, the temperature of secondary vacuum crystallizer is 50 ~ 65 DEG C, vacuum tightness is 0.007 ~ 0.010MPa, the temperature of three grades of vacuum cyrsytallisers is 42 ~ 50 DEG C, vacuum tightness is 0.006 ~ 0.007MPa, the temperature of level Four vacuum cyrsytalliser is 35 ~ 42 DEG C, vacuum tightness is 0.003 ~ 0.006MPa, the temperature of Pyatyi vacuum cyrsytalliser is 25 ~ 35 DEG C, vacuum tightness is 0.0023 ~ 0.003MPa, the temperature of six grades of vacuum cyrsytallisers is 15 ~ 25 DEG C, vacuum tightness is 0.0010 ~ 0.0023MPa, again through stiff, centrifugal, obtained saltpetre crude product and saltpetre crude product mother solution,
(3) the saltpetre crude product that step (2) is obtained becomes the saturated solution of 50-60 DEG C through the cold water washing of 0 ~ 20 DEG C, the heating for dissolving that adds water, after filtration, be 20-40 DEG C in temperature, vacuum tightness is crystallization under the condition of 0.002 ~ 0.07MPa, stiff, centrifugal, obtained saltpetre;
(4) in the obtained saltpetre crude product mother solution of step (2), add ammonium nitrate, Chlorine in Solution ammonium is reached capacity, is heated to 50 ~ 80 DEG C, concentrate through adverse current triple effect, triple effect thickening temperature is 60 ~ 80 DEG C, and vacuum tightness is 0.01 ~ 0.05MPa; Two effect thickening temperatures are 90 ~ 100 DEG C, and vacuum tightness is 0.08 ~ 0.10MPa; One effect thickening temperature is 110 ~ 115 DEG C, and vacuum tightness is 0.18 ~ 0.25MPa; Being concentrated into density is 1.30 ~ 1.37g/cm
3, be 50 ~ 70 DEG C in temperature, vacuum tightness is crystallization under the condition of 0.07 ~ 0.10MPa, and through stiff, centrifugal, obtained ammonia chloride crystal and ammonium chloride mother liquor, the reaction cycle that ammonium chloride mother liquor participates in step (1) utilizes.
Above-mentioned preparation and method as being not particularly illustrated, all by state of the art.
Beneficial effect:
1, continous way Production of Potassium Nitrate system and method for the present invention, expands throughput, reduces work production intensity, improves the production efficiency of process for producing potassium nitrate.
2, the present invention adopts the design of new saltpetre vacuum crystallization, and control more accurate to crystallisation process, the Quality and yield of potassium nitrate crystal is more stable, and can continuous dosing, continuous discharge, achieves continuous prodution.
3, the present invention adopts adverse current triple effect falling film concentration technique to concentrate chloride slip, not only reduce cost of investment, and thickening temperature is low, alleviates the corrosion of slip to equipment, also greatly saved steam usage quantity, reduced energy consumption.
4, vacuum continuous crystallizer is applied to and produces in saltpetre side product sodium chloride technological process by the present invention first, and more traditional heat exchange type of cooling is compared, and achieves operate continuously, saves the production time, raises the efficiency.
5, the adverse current triple effect falling film concentration that adopts of the present invention and continuous vacuum continuous crystallizer substantially increase the stability of ammonium chloride product, add ammonium chloride yield.
Accompanying drawing explanation
Fig. 1 is the process flow diagram of continous way double decomposition Production of Potassium Nitrate of the present invention;
Fig. 2 is saltpetre vacuum crystallization device schematic diagram of the present invention;
Fig. 3 is adverse current triple effect concentrating unit schematic diagram of the present invention;
In Fig. 2: A, crystallizer, B, condenser, C, vacuum, D, discharging pump.
In Fig. 3: 1, vacuum, 2, triple effect separate chamber, 3, triple effect well heater, 4, two effect separate chambers, 5, two effect well heaters, 6, one effect separate chamber, 7, an effect well heater, 8, triple effect cycle pump, 9, triple effect discharging pump, 10, two effect recycle pumps, 11 2 effect discharging pumps, 12, one effect recycle pump, 13, an effect discharging pump, 14, vacuum cooler-condenser, 15, concentrating and preheating device, 16, secondary vacuum continuous crystallizer, 17, ammonium chloride condenses device.
Embodiment
Bright in order to illustrate in greater detail we, provide following technological design embodiment.But scope of the present invention is not limited thereto.Being that raw material of the present invention is not done to illustrate is commercially available.
Embodiment 1
A system for continous way preparing potassium nitrate by means of double decomposition, comprises dissolving tank, saltpetre vacuum crystallization device, thickener, whizzer, rinse bath, secondary dissolving tank, filter, vacuum continuous crystallizer, secondary thickener, secondary centrifuging machine, mixing tank for coating colors, concentrating and preheating device, adverse current triple effect concentrating unit, secondary vacuum continuous crystallizer, three thickeners, No. three whizzers, the discharge port of a described dissolving tank is connected with the opening for feed of saltpetre vacuum crystallization device, the discharge port of saltpetre vacuum crystallization device is connected with the opening for feed of a thickener, the discharge port of a thickener is connected with the opening for feed of a whizzer, the solids exit mouth of a whizzer is connected with the opening for feed of rinse bath, the liquid outlet opening of rinse bath is connected with one of opening for feed of mixing tank for coating colors, the solids exit mouth of rinse bath is connected with the opening for feed of secondary dissolving tank, the discharge port of secondary dissolving tank is connected with the opening for feed of filter, the discharge port of filter is connected with the opening for feed of a vacuum continuous crystallizer, the discharge port of a vacuum continuous crystallizer is connected with the opening for feed of secondary thickener, the discharge port of secondary thickener is connected with the opening for feed of secondary centrifuging machine, the liquid outlet opening of secondary centrifuging machine is connected with one of opening for feed of mixing tank for coating colors, the liquid outlet opening of a whizzer is connected with one of opening for feed of mixing tank for coating colors, the discharge port of mixing tank for coating colors is connected with the opening for feed of concentrating and preheating device, the discharge port of concentrating and preheating device is connected with the opening for feed of adverse current triple effect concentrating unit, the discharge port of adverse current triple effect concentrating unit is connected with the opening for feed of secondary vacuum continuous crystallizer, the discharge port of secondary vacuum continuous crystallizer is connected with the opening for feed of three thickeners, the discharge port of three thickeners is connected with the opening for feed of No. three whizzers, the liquid outlet opening of No. three whizzers is connected with the opening for feed of a dissolving tank,
Described saltpetre vacuum crystallization device is the device of 2 ~ 10 grades of cascaded structures, every one-level cascaded structure comprises crystallizer A, condenser B, vacuum C, discharging pump D and tank, the upper end of described crystallizer A is communicated with by the upper end of pipeline with condenser B, the lower end of described condenser B is connected with vacuum C by pipeline, the lower end of described condenser B is also connected with tank by condensing water conduit, the lower end of described crystallizer A is connected with discharging pump D by pipeline, the discharge port of a described dissolving tank is connected with the opening for feed of first step crystallizer, described last step discharging pump is connected with the opening for feed of a thickener.
Described adverse current triple effect concentrating unit comprises an effect falling film concentrating device, two effect falling film concentrating device, triple effect falling film concentrating device, concentrating and preheating device 15, vacuum cooler-condenser 14 and vacuum 1, one effect falling film concentrating device comprises an effect well heater 7, and imitates separate chamber 6, effect recycle pump 12 and an effect discharging pump 13, two effect falling film concentrating devices comprise two effect well heaters 5, two and imitate separate chamber 4, two effect recycle pump 10 and two effect discharging pumps 11, and triple effect falling film concentrating device comprises triple effect well heater 3, triple effect separate chamber 2, triple effect cycle pump 8 and triple effect discharging pump 9;
The bottom that the opening for feed of one effect recycle pump 12 imitates discharging pump 13 respectively opening for feed, with one imitates separate chamber 6 is connected with a bottom of imitating well heater 7, the discharge port that the discharge port and two of one effect recycle pump 12 imitates discharging pump 11 imitates well heater 7 top respectively opening for feed with one is connected, the discharge port of one effect discharging pump 13 is connected with the opening for feed of secondary vacuum continuous crystallizer, one effect well heater 7 and an effect bottom, separate chamber 6 are by pipeline communication, and an effect top, separate chamber 6 is imitated well heater 5 top by pipeline and two and is connected;
The bottom that the opening for feeds of two effect recycle pumps 10 imitate discharging pump 11 respectively opening for feed, two with two imitates separate chamber 4 is connected with two bottoms of imitating well heater 5, the two effect discharge ports of recycle pump 10 are connected with the discharge port of triple effect discharging pump 9 imitates well heater 5 top respectively opening for feed with two, two effect well heaters 5 and two effect bottoms, separate chamber 4 are by pipeline communication, and two effect tops, separate chamber 4 are connected with triple effect well heater 3 top by pipeline;
The opening for feed of triple effect cycle pump 8 is connected with the bottom of triple effect well heater 3 with the opening for feed of triple effect discharging pump 9, the bottom of triple effect separate chamber 2 respectively, the discharge port of triple effect cycle pump 8 is connected with the opening for feed at triple effect well heater 3 top respectively with the discharge port of concentrating and preheating device 15, triple effect well heater 3 and bottom, triple effect separate chamber 2 are by pipeline communication, and top, triple effect separate chamber 2 is connected with concentrating and preheating device 15 steam-in, vacuum cooler-condenser 14 top respectively by pipeline.Concentrating and preheating device 15 is exported and is connected with condenser 14 lower end by pipeline, and condenser 14 is exported and is connected with vacuum 1 by pipeline.
Described vacuum continuous crystallizer is draft tube baffle crystallizer, OSLO crystallizer.
Embodiment 2
Ammonium chloride mother liquor, water and Repone K is added in a dissolving tank, the ratio of ammonium ion and chlorion is made to be 1:1, be steam heated to 75 DEG C and stir and make it to dissolve completely, feed liquid enters in six grades, saltpetre series connection vacuum crystallization device successively, it is 70 DEG C by controlling temperature in vacuum system pressure-controlling first degree crystalline device A1 at different levels, in secondary crystallizer A2, temperature is 55 DEG C, in three grades of crystallizer A3, temperature is 42 DEG C, in level Four crystallizer A4, temperature is 35 DEG C, in Pyatyi crystallizer A5, temperature is 25 DEG C, and in six grades of crystallizer A6, temperature is 15 DEG C.Material in 6th grade of crystallizer A6 by the 6th grade of discharging pump D6 by product pump to thickener, a whizzer, isolate saltpetre crude product; Saltpetre crude product 5 DEG C of cold water flush, heating for dissolving become 50 DEG C of saturated solutions, filtering and removing water-insoluble, send into DTB vacuum continuous crystallizer, temperature 40 DEG C, vacuum tightness is crystallization under 0.07MPa condition, then is separated to obtain saltpetre through secondary thickener, secondary centrifuging machine successively; Centrifugal for mother liquor, wash-down water and saltpetre after the centrifugation of saltpetre crude product rear mother liquor is injected mixing tank for coating colors, add wherein concentration be 65% ammonium nitrate solution mix, feed liquid first enters adverse current triple effect concentrating unit after the preheating of concentrating and preheating device, and the temperature controlling liquid in an effect, two effects, triple effect well heater by controlling the accurate control pressure of vacuum system is followed successively by 110 DEG C, 90 DEG C and 75 DEG C.Being concentrated into pulp density is 1.35g/cm
3, send into the crystallization of DTB secondary vacuum continuous crystallizer, Tc controls at 60 DEG C, and the slip after crystallization, more successively through three thickeners, No. three whizzer separating ammonium chloride crystal, is separated the ammonium chloride mother liquor obtained and adds recycle in a dissolving tank.
The potassium nitrate product KNO of gained
3: 99.6wt%, Cl
-: 0.012wt%, ammonium chloride product total nitrogen content is 25.3wt%.
Embodiment 3
Ammonium chloride mother liquor, water and Repone K is added in a dissolving tank, the ratio of ammonium ion and chlorion is made to be 1:1.1, be steam heated to 80 DEG C and stir and make it to dissolve completely, feed liquid enters in six grades, saltpetre series connection vacuum crystallization device successively, it is 75 DEG C by controlling temperature in vacuum system pressure-controlling first degree crystalline device A1 at different levels, in secondary crystallizer A2, temperature is 60 DEG C, in three grades of crystallizer A3, temperature is 45 DEG C, in level Four crystallizer A4, temperature is 38 DEG C, in Pyatyi crystallizer A5, temperature is 30 DEG C, and in six grades of crystallizer A6, temperature is 20 DEG C.Material in 6th grade of crystallizer A6 by the 6th grade of discharging pump D6 by product pump to thickener, a whizzer, isolate saltpetre crude product; Saltpetre crude product 12 DEG C of cold water flush, heating for dissolving become 55 DEG C of saturated solutions, filtering and removing water-insoluble, send into DTB vacuum continuous crystallizer, temperature 35 DEG C, vacuum tightness is crystallization under 0.05MPa condition, then is separated to obtain saltpetre through secondary thickener, secondary centrifuging machine successively; Centrifugal for mother liquor, wash-down water and saltpetre after the centrifugation of saltpetre crude product rear mother liquor is injected mixing tank for coating colors, add wherein concentration be 65% ammonium nitrate solution mix, feed liquid first enters adverse current triple effect concentrating unit after the preheating of concentrating and preheating device, and the temperature controlling liquid in an effect, two effects, triple effect well heater by controlling the accurate control pressure of vacuum system is followed successively by 115 DEG C, 95 DEG C and 80 DEG C.Being concentrated into pulp density is 1.36g/cm
3, send into the crystallization of DTB secondary vacuum continuous crystallizer, Tc controls at 70 DEG C, and the slip after crystallization, more successively through three thickeners, No. three whizzer separating ammonium chloride crystal, is separated the ammonium chloride mother liquor obtained and adds recycle in a dissolving tank.
The potassium nitrate product KNO of gained
3: 99.5wt%, Cl
-: 0.020wt%, ammonium chloride product total nitrogen content is 25.6wt%.
Embodiment 4
Ammonium chloride mother liquor, water and Repone K is added in a dissolving tank, the ratio of ammonium ion and chlorion is made to be 1:1.2, be steam heated to 90 DEG C and stir and make it to dissolve completely, feed liquid enters in six grades, saltpetre series connection vacuum crystallization device successively, it is 80 DEG C by controlling temperature in vacuum system pressure-controlling first degree crystalline device A1 at different levels, in secondary crystallizer A2, temperature is 65 DEG C, in three grades of crystallizer A3, temperature is 50 DEG C, in level Four crystallizer A4, temperature is 42 DEG C, in Pyatyi crystallizer A5, temperature is 35 DEG C, and in six grades of crystallizer A6, temperature is 25 DEG C.Material in 6th grade of crystallizer A6 by the 6th grade of discharging pump D6 by product pump to thickener, a whizzer, isolate saltpetre crude product; Saltpetre crude product 20 DEG C of cold water flush, heating for dissolving become 50 DEG C of saturated solutions, filtering and removing water-insoluble, send into DTB vacuum continuous crystallizer, at temperature 45 C, vacuum tightness is crystallization under 0.01MPa condition, then is separated to obtain saltpetre through secondary thickener, secondary centrifuging machine successively; Centrifugal for mother liquor, wash-down water and saltpetre after the centrifugation of saltpetre crude product rear mother liquor is injected mixing tank for coating colors, add wherein concentration be 65% ammonium nitrate solution mix, feed liquid first enters adverse current triple effect concentrating unit after the preheating of concentrating and preheating device, and the temperature controlling liquid in an effect, two effects, triple effect well heater by controlling the accurate control pressure of vacuum system is followed successively by 115 DEG C, 100 DEG C and 80 DEG C.Being concentrated into pulp density is 1.37g/cm
3, send into the crystallization of DTB secondary vacuum continuous crystallizer, Tc controls at 50 DEG C, and the slip after crystallization, more successively through three thickeners, No. three whizzer separating ammonium chloride crystal, is separated the ammonium chloride mother liquor obtained and adds recycle in a dissolving tank.
The potassium nitrate product KNO of gained
3: 99.8wt%, Cl
-: 0.007wt%, ammonium chloride product total nitrogen content is 25.1%.
Embodiment 5
Ammonium chloride mother liquor, water and Repone K is added in a dissolving tank, the ratio of ammonium ion and chlorion is made to be 1:1, be steam heated to 65 DEG C and stir and make it to dissolve completely, feed liquid enters in six grades, saltpetre series connection vacuum crystallization device successively, it is 60 DEG C by controlling temperature in vacuum system pressure-controlling first degree crystalline device A1 at different levels, in secondary crystallizer A2, temperature is 55 DEG C, in three grades of crystallizer A3, temperature is 45 DEG C, in level Four crystallizer A4, temperature is 40 DEG C, in Pyatyi crystallizer A5, temperature is 30 DEG C, and in six grades of crystallizer A6, temperature is 20 DEG C.Material in 6th grade of crystallizer A6 by the 6th grade of discharging pump D6 by product pump to thickener, a whizzer, isolate saltpetre crude product; Saltpetre crude product 10 DEG C of cold water flush, heating for dissolving become 50 DEG C of saturated solutions, filtering and removing water-insoluble, send into DTB vacuum continuous crystallizer, temperature 40 DEG C, vacuum tightness is crystallization under 0.07MPa condition, then is separated to obtain saltpetre through secondary thickener, secondary centrifuging machine successively; Centrifugal for mother liquor, wash-down water and saltpetre after the centrifugation of saltpetre crude product rear mother liquor is injected mixing tank for coating colors, add wherein concentration be 65% ammonium nitrate solution mix, feed liquid first enters adverse current triple effect concentrating unit after the preheating of concentrating and preheating device, and the temperature controlling liquid in an effect, two effects, triple effect well heater by controlling the accurate control pressure of vacuum system is followed successively by 110 DEG C, 90 DEG C and 70 DEG C.Being concentrated into pulp density is 1.34g/cm
3, send into the crystallization of DTB secondary vacuum continuous crystallizer, Tc controls at 65 DEG C, and the slip after crystallization, more successively through three thickeners, No. three whizzer separating ammonium chloride crystal, is separated the ammonium chloride mother liquor obtained and adds recycle in a dissolving tank.
The potassium nitrate product KNO of gained
3: 99.6wt%, Cl
-: 0.019wt%, ammonium chloride product total nitrogen content is 25.5wt%.
Embodiment 6
Ammonium chloride mother liquor, water and Repone K is added in a dissolving tank, the ratio of ammonium ion and chlorion is made to be 1:1.1, be steam heated to 70 DEG C and stir and make it to dissolve completely, feed liquid enters in six grades, saltpetre series connection vacuum crystallization device successively, it is 65 DEG C by controlling temperature in vacuum system pressure-controlling first degree crystalline device A1 at different levels, in secondary crystallizer A2, temperature is 55 DEG C, in three grades of crystallizer A3, temperature is 42 DEG C, in level Four crystallizer A4, temperature is 38 DEG C, in Pyatyi crystallizer A5, temperature is 30 DEG C, and in six grades of crystallizer A6, temperature is 23 DEG C.Material in 6th grade of crystallizer A6 by the 6th grade of discharging pump D6 by product pump to thickener, a whizzer, isolate saltpetre crude product; Saltpetre crude product 15 DEG C of cold water flush, heating for dissolving become 55 DEG C of saturated solutions, filtering and removing water-insoluble, send into DTB vacuum continuous crystallizer, temperature 35 DEG C, vacuum tightness is crystallization under 0.05MPa condition, then is separated to obtain saltpetre through secondary thickener, secondary centrifuging machine successively; Centrifugal for mother liquor, wash-down water and saltpetre after the centrifugation of saltpetre crude product rear mother liquor is injected mixing tank for coating colors, add wherein concentration be 65% ammonium nitrate solution mix, feed liquid first enters adverse current triple effect concentrating unit after the preheating of concentrating and preheating device, and the temperature controlling liquid in an effect, two effects, triple effect well heater by controlling the accurate control pressure of vacuum system is followed successively by 115 DEG C, 90 DEG C and 70 DEG C.Being concentrated into pulp density is 1.32g/cm
3, send into the crystallization of DTB secondary vacuum continuous crystallizer, Tc controls at 55 DEG C, and the slip after crystallization, more successively through three thickeners, No. three whizzer separating ammonium chloride crystal, is separated the ammonium chloride mother liquor obtained and adds recycle in a dissolving tank.
The potassium nitrate product KNO of gained
3: 99.3wt%, Cl
-: 0.04wt%, ammonium chloride product total nitrogen content is 25.3wt%.
Claims (10)
1. the system of a continous way preparing potassium nitrate by means of double decomposition, be characterised in that, comprise dissolving tank, saltpetre vacuum crystallization device, thickener, whizzer, rinse bath, secondary dissolving tank, filter, vacuum continuous crystallizer, secondary thickener, secondary centrifuging machine, mixing tank for coating colors, concentrating and preheating device, adverse current triple effect concentrating unit, secondary vacuum continuous crystallizer, three thickeners, No. three whizzers, the discharge port of a described dissolving tank is connected with the opening for feed of saltpetre vacuum crystallization device, the discharge port of saltpetre vacuum crystallization device is connected with the opening for feed of a thickener, the discharge port of a thickener is connected with the opening for feed of a whizzer, the solids exit mouth of a whizzer is connected with the opening for feed of rinse bath, the liquid outlet opening of rinse bath is connected with one of opening for feed of mixing tank for coating colors, the solids exit mouth of rinse bath is connected with the opening for feed of secondary dissolving tank, the discharge port of secondary dissolving tank is connected with the opening for feed of filter, the discharge port of filter is connected with the opening for feed of a vacuum continuous crystallizer, the discharge port of a vacuum continuous crystallizer is connected with the opening for feed of secondary thickener, the discharge port of secondary thickener is connected with the opening for feed of secondary centrifuging machine, the liquid outlet opening of secondary centrifuging machine is connected with one of opening for feed of mixing tank for coating colors, the liquid outlet opening of a whizzer is connected with one of opening for feed of mixing tank for coating colors, the discharge port of mixing tank for coating colors is connected with the opening for feed of concentrating and preheating device, the discharge port of concentrating and preheating device is connected with the opening for feed of adverse current triple effect concentrating unit, the discharge port of adverse current triple effect concentrating unit is connected with the opening for feed of secondary vacuum continuous crystallizer, the discharge port of secondary vacuum continuous crystallizer is connected with the opening for feed of three thickeners, the discharge port of three thickeners is connected with the opening for feed of No. three whizzers, the liquid outlet opening of No. three whizzers is connected with the opening for feed of a dissolving tank,
Described saltpetre vacuum crystallization device is the device of 2 ~ 10 grades of cascaded structures, every one-level cascaded structure comprises crystallizer, condenser, vacuum 1, discharging pump and tank, the upper end of described crystallizer is communicated with the upper end of condenser by pipeline, the lower end of described condenser is connected with vacuum 1 by pipeline, the lower end of described condenser is also connected with tank by condensing water conduit, the lower end of described crystallizer is connected with discharging pump by pipeline, the discharge port of a described dissolving tank is connected with the opening for feed of first step crystallizer, last step discharging pump is connected with the opening for feed of a thickener,
Described adverse current triple effect concentrating unit comprises an effect falling film concentrating device, two effect falling film concentrating device, triple effect falling film concentrating device, concentrating and preheating device, vacuum cooler-condenser and vacuum 2, one effect falling film concentrating device comprises an effect well heater, an effect separate chamber, an effect recycle pump and an effect discharging pump, two effect falling film concentrating devices comprise two effect well heaters, two effect separate chambers, two effect recycle pumps and two effect discharging pumps, and triple effect falling film concentrating device comprises triple effect well heater, triple effect separate chamber, triple effect cycle pump and triple effect discharging pump;
The bottom that the opening for feed of one effect recycle pump imitates discharging pump respectively opening for feed, with one imitates separate chamber is connected with a bottom of imitating well heater, the discharge port that one discharge port and two of imitating recycle pump imitates discharging pump is connected with an opening for feed of imitating well heater top respectively, the discharge port of one effect discharging pump is connected with the opening for feed of secondary vacuum continuous crystallizer, one effect well heater and an effect bottom, separate chamber are by pipeline communication, and an effect top, separate chamber is imitated well heater top by pipeline and two and is connected;
The bottom that the opening for feeds of two effect recycle pumps imitate discharging pump respectively opening for feed, two with two imitates separate chamber is connected with two bottoms of imitating well heater, the two effect discharge ports of recycle pump are connected with two opening for feeds of imitating well heater top respectively with the discharge port of triple effect discharging pump, two effect well heaters and two effect bottoms, separate chamber are by pipeline communication, and two effect tops, separate chamber are connected with triple effect well heater top by pipeline;
The opening for feed of triple effect cycle pump respectively with the opening for feed of triple effect discharging pump, the bottom of triple effect separate chamber is connected with the bottom of triple effect well heater, the discharge port of triple effect cycle pump is connected with the opening for feed at triple effect well heater top respectively with the discharge port of concentrating and preheating device, pipeline communication is passed through in triple effect well heater and bottom, triple effect separate chamber, top, triple effect separate chamber by pipeline respectively with concentrating and preheating device steam-in, vacuum cooler-condenser top is connected, concentrating and preheating device condensate outlet is connected with condenser lower end by pipeline, condenser discharge port is connected with vacuum 2 by pipeline.
2. the system of a kind of continous way preparing potassium nitrate by means of double decomposition described in claim 1, is characterised in that, described vacuum continuous crystallizer is draft tube baffle crystallizer, OSLO crystallizer.
3. the system of a kind of continous way preparing potassium nitrate by means of double decomposition described in claim 1, is characterised in that, described saltpetre vacuum crystallization device is the device of 6 grades of cascaded structures; Described vacuum 1 and vacuum 2 are vacuum pump.
4. utilize a method for the arbitrary described system continous way preparing potassium nitrate by means of double decomposition of claim 1-3, be characterised in that, step is as follows:
Circulating mother liquor, water and Repone K is added in a dissolving tank, described circulating mother liquor is ammonium chloride mother liquor, heating material to 65 ~ 90 in a dissolving tank DEG C, between 1:1 ~ 1.2, are also stirred and material are dissolved completely by the molar ratio controlling ammonium ion and the chlorion added; Feed liquid enters saltpetre vacuum crystallization device, thickener, a whizzer successively, and centrifugation goes out saltpetre crude product; Saltpetre crude product after rinse bath, secondary dissolving tank, filter washing, dissolving, filtering, is sent into the crystallization of a vacuum continuous crystallizer, then is separated to obtain saltpetre through secondary thickener, secondary centrifuging machine successively successively; Centrifugal for mother liquor, wash-down water and saltpetre after the centrifugation of saltpetre crude product rear mother liquor is injected mixing tank for coating colors, add ammonium chloride in ammonium nitrate to mixing tank for coating colors to reach capacity, after mixing, feed liquid first enters adverse current triple effect concentrating unit after the preheating of concentrating and preheating device, and being concentrated into density is 1.30 ~ 1.37g/cm
3after, send into the crystallization of secondary vacuum continuous crystallizer, more successively through three thickeners, No. three whizzer separating ammonium chloride crystal, be separated the ammonium chloride mother liquor obtained and add recycle in a dissolving tank.
5. the method for a kind of continous way preparing potassium nitrate by means of double decomposition described in claim 4, is characterised in that, the mode of a described dissolving tank heating is steam heating.
6. the method for a kind of continous way preparing potassium nitrate by means of double decomposition described in claim 4, is characterised in that, described saltpetre vacuum crystallization device is the device of 6 grades of cascaded structures; Wherein, in first degree crystalline device, temperature controls at 65 ~ 80 DEG C, and vacuum tightness is 0.010 ~ 0.030MPa; In secondary crystallizer, temperature controls at 50 ~ 65 DEG C, and vacuum tightness is 0.007 ~ 0.010MPa; In three grades of crystallizers, temperature controls at 42 ~ 50 DEG C, and vacuum tightness is 0.006 ~ 0.007MPa; In level Four crystallizer, temperature controls at 35 ~ 42 DEG C, and vacuum tightness is 0.003 ~ 0.006MPa; In Pyatyi crystallizer, temperature controls at 25 ~ 35 DEG C, and vacuum tightness is 0.0023 ~ 0.003MPa; In six grades of crystallizers, temperature controls at 15 ~ 25 DEG C, and vacuum tightness is 0.0010 ~ 0.0023MPa.
7. the method for a kind of continous way preparing potassium nitrate by means of double decomposition described in claim 4, be characterised in that, in secondary dissolving tank, saltpetre heating for dissolving becomes the saturated solution of 50-60 DEG C; In a described vacuum continuous crystallizer, Tc is 20-40 DEG C, and vacuum tightness is 0.002 ~ 0.07MPa.
8. the method for a kind of continous way preparing potassium nitrate by means of double decomposition described in claim 4, is characterised in that, described ammonium nitrate is the ammonium nitrate solution that ammonium nitrate solid or mass concentration are not less than 65%.
9. the method for a kind of continous way preparing potassium nitrate by means of double decomposition described in claim 4, be characterised in that, in an effect concentrating unit in described adverse current triple effect concentrating unit, temperature is 110 ~ 115 DEG C, vacuum tightness is 0.18 ~ 0.25MPa, in two effect concentrating uniies, temperature is 90 ~ 100 DEG C, vacuum tightness is 0.08 ~ 0.10MPa, and in triple effect concentrating unit, temperature is 60 ~ 80 DEG C, and vacuum tightness is 0.01 ~ 0.05MPa;
In described secondary vacuum continuous crystallizer, Tc is 50-70 DEG C, and vacuum tightness is 0.07 ~ 0.10MPa.
10. a method for continous way preparing potassium nitrate by means of double decomposition, is characterised in that, step is as follows:
(1) ammonium chloride mother liquor, water and Repone K are mixed, be heated to 65 ~ 90 DEG C of dissolvings, make the mol ratio of ammonium ion and chlorion be 1:1 ~ 1.2, obtained mixing solutions;
(2) mixing solutions that step (1) is obtained is carried out six grades of vacuum continuous crystallisations, the temperature of one-level vacuum cyrsytalliser 65 ~ 80 DEG C, vacuum tightness is 0.010 ~ 0.030MPa, the temperature of secondary vacuum crystallizer is 50 ~ 65 DEG C, vacuum tightness is 0.007 ~ 0.010MPa, the temperature of three grades of vacuum cyrsytallisers is 42 ~ 50 DEG C, vacuum tightness is 0.006 ~ 0.007MPa, the temperature of level Four vacuum cyrsytalliser is 35 ~ 42 DEG C, vacuum tightness is 0.003 ~ 0.006MPa, the temperature of Pyatyi vacuum cyrsytalliser is 25 ~ 35 DEG C, vacuum tightness is 0.0023 ~ 0.003MPa, the temperature of six grades of vacuum cyrsytallisers is 15 ~ 25 DEG C, vacuum tightness is 0.0010 ~ 0.0023MPa, again through stiff, centrifugal, obtained saltpetre crude product and saltpetre crude product mother solution,
(3) the saltpetre crude product that step (2) is obtained becomes the saturated solution of 50-60 DEG C through the cold water washing of 0 ~ 20 DEG C, the heating for dissolving that adds water, after filtration, be 20-40 DEG C in temperature, vacuum tightness is crystallization under the condition of 0.002 ~ 0.07MPa, stiff, centrifugal, obtained saltpetre;
(4) in the obtained saltpetre crude product mother solution of step (2), add ammonium nitrate, Chlorine in Solution ammonium is reached capacity, is heated to 50 ~ 80 DEG C, concentrate through adverse current triple effect, triple effect thickening temperature is 60 ~ 80 DEG C, and vacuum tightness is 0.01 ~ 0.05MPa; Two effect thickening temperatures are 90 ~ 100 DEG C, and vacuum tightness is 0.08 ~ 0.10MPa; One effect thickening temperature is 110 ~ 115 DEG C, and vacuum tightness is 0.18 ~ 0.25MPa; Being concentrated into density is 1.30 ~ 1.37g/cm
3, be 50 ~ 70 DEG C in temperature, vacuum tightness is crystallization under the condition of 0.07 ~ 0.10MPa, and through stiff, centrifugal, obtained ammonia chloride crystal and ammonium chloride mother liquor, the reaction cycle that ammonium chloride mother liquor participates in step (1) utilizes.
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| CN110963511A (en) * | 2019-11-27 | 2020-04-07 | 新疆硝石钾肥有限公司 | System and method for producing optical glass-grade potassium nitrate by using sodium nitrate high-temperature mother liquor |
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| CN1304878A (en) * | 2001-02-28 | 2001-07-25 | 化学工业部连云港设计研究院 | Process for preparing potassium nitrate by metathesis method |
| CN1827526A (en) * | 2005-08-31 | 2006-09-06 | 东华工程科技股份有限公司 | Process for preparing potassium nitrate by double decomposition method |
| 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 |
| CN101643226A (en) * | 2009-09-02 | 2010-02-10 | 赵家春 | Method for producing nitrate and ammonium chloride with double decomposition circulation method |
| CN201458761U (en) * | 2009-08-18 | 2010-05-12 | 湖南丹化农资有限公司 | Vacuum cooling crystallization device for producing potassium nitrate |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1304878A (en) * | 2001-02-28 | 2001-07-25 | 化学工业部连云港设计研究院 | Process for preparing potassium nitrate by metathesis method |
| CN1827526A (en) * | 2005-08-31 | 2006-09-06 | 东华工程科技股份有限公司 | Process for preparing potassium nitrate by double decomposition method |
| 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 |
| CN201458761U (en) * | 2009-08-18 | 2010-05-12 | 湖南丹化农资有限公司 | Vacuum cooling crystallization device 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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