CN107128953A - A kind of method for producing fused salt level potassium nitrate - Google Patents
A kind of method for producing fused salt level potassium nitrate Download PDFInfo
- Publication number
- CN107128953A CN107128953A CN201710464258.0A CN201710464258A CN107128953A CN 107128953 A CN107128953 A CN 107128953A CN 201710464258 A CN201710464258 A CN 201710464258A CN 107128953 A CN107128953 A CN 107128953A
- Authority
- CN
- China
- Prior art keywords
- potassium nitrate
- fused salt
- potassium
- salt level
- material liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
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
- C01D9/18—Preparation in the form of shaped products, e.g. granules
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
- C01P2006/82—Compositional purity water content
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a kind of method for producing fused salt level potassium nitrate, comprise the following steps：Step S1 neutralization steps：Potassium hydroxide solution mixes generation neutralization reaction generation potassium nitrate with salpeter solution, obtains the first potassium nitrate material liquid, the ratio between amount of material of potassium hydroxide and nitric acid is 1:1.01~1.02；Step S2 evaporization process：It is 65~70% that first potassium nitrate material liquid, which is evaporated, and is concentrated into the mass percent concentration of potassium nitrate, obtains the second potassium nitrate material liquid；Step S3 slurry-spraying pelletizing processes：Slurry-spraying pelletizing is carried out to the second potassium nitrate material liquid, end-product fused salt level potassium nitrate is made.Method of the present invention can directly produce the potassium nitrate of high-purity fused salt rank, with extraordinary industrial value.And process operating process of the present invention is simple efficiently, easily realize automated production, high safety, it is adaptable to which the continuous-stable of high-purity grade of potassium nitrate is quickly produced.
Description
Technical field
The present invention relates to the technical field of potassium nitrate preparing technology, and in particular to a kind of side for producing fused salt level potassium nitrate
Method.
Background technology
Fused salt is the molten mass formed after salt melts, is generally made up of metal cation and metalloid anion, is planted
Class is enriched.According to mass ratio it is 6 by sodium nitrate and potassium nitrate：4 Molten Binary Salts constituted, fusing point is 160 degrees Celsius, work temperature
Degree proves to be suitable for the ripe heat-storage medium of solar-thermal generating system up to 560 DEG C, through real case.Itself and traditional hydrocarbonization
The heat transfer mediums such as compound and conduction oil are compared, with cost is low, long lifespan, heat exchange property is good, operating temperature is high, heat flux is high,
The advantage such as pressure is low, nonflammable, pollution-free, therefore with application prospect widely.
Potassium nitrate as above-mentioned Molten Binary Salts constituent, its main production method have sodium nitrate-potassium chloride conversion method,
Ammonium nitrate-potassium chloride conversion method, ammonium nitrate-potassium chloride ions exchange process, nitric acid and potassium hydroxide or potassium carbonate neutralisation.
Wherein, although the utilization rate of sodium nitrate-potassium chloride conversion method raw material is high, the price of raw material sodium nitrate is higher,
And resource is nervous, the value of byproduct sodium chloride is again relatively low, and mother liquor need to be discharged periodically.Ammonium nitrate-potassium chloride conversion method
The utilization rate of middle raw material is also higher, and byproduct ammonium chloride is recyclable, the whole basic non-environmental-pollution of technique, and process equipment is simple,
It is easy to operate, but the preparation-obtained product appearance of this kind of method, content are poor, it is necessary to it could be improved by recrystallization
The quality of final products potassium nitrate.The equipment that ammonium nitrate-potassium chloride ions exchange process is used is relatively simple, and can realize continuous
Operation, but the method shortcoming be exchange potassium nitrate concentration it is low, evaporation cost is high, and it is low to reclaim obtained ammonium chloride concentration, evaporation
High energy consumption, requires high to equipment material, is unsuitable for widely used.Neutralisation refers to anti-using nitric acid and potassium hydroxide or potassium carbonate
The reaction of potassium nitrate should be generated, the operating process of this method is relatively simple, but the potassium nitrate prepared using the neutralisation
The requirement of fused salt can not be met, therefore the preparation of fused salt can not be directly applied to.
In summary, the preparation method of existing potassium nitrate can not also directly produce the potassium nitrate of fused salt level, and base
It is with the obvious advantage in being widely used for fused salt, therefore it is that current urgent need is solved to work out the preparation method of the potassium nitrate of fused salt level
Industrial problem.
The content of the invention
It is an object of the invention to provide a kind of method for producing fused salt level potassium nitrate, for solving existing potassium nitrate
The problem of production method can not produce the potassium nitrate available for fused salt market.
To achieve these goals, the present invention provides following technical scheme：A kind of method for producing fused salt level potassium nitrate, bag
Include following steps：
Step S1 neutralization steps：
Potassium hydroxide solution is mixed to form reaction solution with salpeter solution, wherein, the thing of the potassium hydroxide and the nitric acid
The ratio between amount of matter is 1:1.01~1.02,
Neutralization reaction generation potassium nitrate occurs in the reaction solution, the first potassium nitrate material liquid is obtained；
Step S2 evaporization process：
Concentration is evaporated to the first potassium nitrate material liquid, the second potassium nitrate material liquid is obtained,
Wherein, the mass percent concentration of potassium nitrate is 65~70% in the second potassium nitrate material liquid；
Step S3 slurry-spraying pelletizing processes：
Slurry-spraying pelletizing is carried out to the second potassium nitrate material liquid, so that end-product fused salt level potassium nitrate is made.
Preferably, in the step S1, participate in neutralization reaction potassium hydroxide solution mass percent concentration for 31~
33%, chloride mass percent concentration is less than 0.005%, and the mass percent concentration of sodium is less than 0.5%；
The mass percent concentration for participating in the salpeter solution of neutralization reaction is 43~48%, and amounts of ammonium salt is less than 100ppm.
Preferably, in step S1, the pH value of the first potassium nitrate material liquid is 6.4~6.7, the quality percentage of potassium nitrate
Specific concentration is 30~35%.
Preferably, in the step S2, the evaporization process is carried out in quadruple effect falling film evaporation device.
Preferably, the slurry-spraying pelletizing process in the step S3 comprises the following steps：
A. the mass percent concentration obtained by cooling step S2 is 65~70% the second potassium nitrate material liquid, to temperature
For 103~105 DEG C when, be input in spray gun；
B. start spray gun, make to be atomized to form potassium nitrate granules from the material that spray gun sprays, and cause potassium nitrate granules simultaneously
Moisture is removed in thermal current；
C. cool down, sieve potassium nitrate granules, end-product fused salt level potassium nitrate is made.
Further, the particle diameter of the fused salt level potassium nitrate in the step S3c obtained by screening is 2~4mm.
Further, potassium nitrate granules of the screening gained particle diameter less than 2mm are input in comminutor in fact in the step S3c
It is again inputted into after existing granulation operations in step S3, screening gained particle diameter is more than 4mm potassium nitrate granules warp in the step S3c
Pulverizer is input in comminutor after crushing and realizes granulation operations, and is again inputted into step S3.
Further, in the granulation operations, the discharging opening of comminutor is provided with Venturi scrubber, the comminutor
Dust sequentially enter Venturi scrubber and vapo(u)rization system, to reclaim solid nitric acid potassium, the solid nitric acid potassium of recovery enters step
Handled in rapid S3c.
Preferably, the water content of the potassium nitrate granules is made to be less than 0.05% in the step S3b in thermal current.
Compared to prior art, the method for production fused salt level potassium nitrate of the present invention has the advantage that：The present invention
Potassium nitrate is prepared with reference to neutralisation, and the series of processing steps to neutralized reaction product potassium nitrate is provided, so as to directly produce
The potassium nitrate of high-purity fused salt rank, with extraordinary industrial value.And process operating process letter of the present invention
Single efficient, each step and parameter are very easy to control, automated production, security can be realized to it using each machinery equipment
By force, it is adaptable to which the continuous-stable of high-purity grade of potassium nitrate is quickly produced, with higher economic benefit, beneficial to large-scale promotion.
In addition, the method for present invention production fused salt level potassium nitrate is high to the utilization rate of raw material, high yield rate is effectively reduced
The production cost of fused salt level potassium nitrate.
Embodiment
The invention provides many applicable creative concepts, the creative concept can be reflected in a large number of on specific
Hereinafter.Specific embodiment described in following embodiments of the present invention is only as embodiment of the invention
Exemplary illustration, and be not meant to limit the scope of the invention.
With reference to specific embodiment, the invention will be further described.
The present invention provides a kind of method for producing fused salt level potassium nitrate, comprises the following steps：
Step S1 neutralization steps：
The neutralization step is using potassium hydroxide solution and salpeter solution as raw material, and the salpeter solution employed in it is dilute
Nitric acid, mass percent concentration is 43~48%, and amounts of ammonium salt is less than 100ppm.Hydroxide in the potassium hydroxide solution used
The mass percent concentration of potassium is 31~33%, and chloride mass percent concentration is less than 0.005%, and the mass percent of sodium is dense
Degree is less than 0.5%.
Raw material potassium hydroxide solution is added in neutralization kettle jointly with salpeter solution, forms reaction solution, neutralizes the hydrogen-oxygen in kettle
It is 1 to change the ratio between amount of material of potassium and nitric acid:1~1.02, the micro- excess of nitric acid of reaction solution in kettle is preferably neutralized, hydrogen-oxygen can be promoted
Change the reaction of potassium, reduce the content of potassium hydroxide impurity in the first potassium nitrate material liquid that neutralized reaction is formed.
Neutralization reaction in above-mentioned neutralization kettle is：KOH+HNO3=KNO3+H2O, generates potassium nitrate solution, question response liquid
PH value is 6.4~6.7, when the mass percent concentration of potassium nitrate is 30~35%, obtains the first qualified potassium nitrate material liquid.
Step S2 evaporization process：
Concentration is evaporated to the first potassium nitrate material liquid obtained by step S1, so as to obtain mass percent concentration and be
65~70% the second potassium nitrate material liquid.
It is noted that the step S2 evaporization process in the present embodiment is carried out in quadruple effect falling film evaporation device.It is many
Effect falling film evaporation device is to add feed liquid from the upper tube box of falling film evaporation device heating chamber, through liquid distribution and film formation device,
It is evenly distributed in each heat exchanger tube, under gravity and vacuum induced and airflow function, is flowed from top to bottom into uniformly membranaceous.Flowing
During, feed liquid is vaporized by shell side heating medium heating, and the steam of generation enters in the separation chamber of evaporator jointly with liquid phase, gas
Liquid is through being sufficiently separated, and steam enters lower 1st effective evaporator as heating medium, so as to realize that multiple-effect is operated, liquid phase is then by separation chamber
Discharge.Quadruple effect falling film evaporation device employed in the present embodiment is the multiple-effect falling film vaporising device for including four evaporators.
The present embodiment uses quadruple effect falling film evaporation device, and steam homogeneous heating, feed liquid is evaporated for liquid film type, when heat transfer efficiency height, heating
Between it is short, evaporation process is carried out in the presence of vacuum, both ensure that the hygienic requirements of material, also ensure that environmental requirement, simultaneously
Greatly reduce evaporating temperature.
Temperature of the first potassium nitrate material liquid in quadruple effect falling film evaporation device gradually rises, and quadruple effect falling film evaporation device goes out
The temperature of the second potassium nitrate material liquid is 120~130 DEG C at mouthful, and mass percent concentration is 65~70%.
Pass through above-mentioned quadruple effect falling film evaporation device, it is ensured that the evaporation effect of the second potassium nitrate material liquid in the present embodiment,
And reduce the loss of potassium nitrate in evaporation process by controlling the outlet temperature of quadruple effect falling film evaporation device, and cause the simultaneously
Potassium nitrate content in dinitric acid potassium material liquid is very high, so that the more conducively realization of later stage slurry-spraying pelletizing process.
It is noted that the efficient utilization in order to realize resource, reduces the production cost of the present embodiment, via this step
The condensed water of S2 evaporization process can be used for potassium nitrate Venturi scrubber in step S3.
Step S3 slurry-spraying pelletizing processes：
Slurry-spraying pelletizing is carried out to the second potassium nitrate material liquid end-product fused salt level potassium nitrate is made.
Slurry-spraying pelletizing process refers to the moisture in slurry by being ejected into an equipment, with the method for heating, taking out pressure, makes
After moisture vaporization and separation in slurry, the solid that retaining to gasify forms granular process.
Specifically, the slurry-spraying pelletizing process comprises the following steps：
A. the mass percent concentration obtained by cooling step S2 is 65~70% the second potassium nitrate material liquid, to temperature
For 103~105 DEG C when, be input in spray gun；
B. start spray gun, make to be atomized to form potassium nitrate granules from the material that spray gun sprays, and cause potassium nitrate granules simultaneously
Moisture is removed in thermal current；
C. cool down, sieve potassium nitrate granules, end-product fused salt level potassium nitrate is made.
Further, in step b, the material sprayed through spray gun after atomization, is constantly sprayed in comminutor at nozzle
On the material curtain that returning charge is formed, potassium nitrate granules are constantly formed and grown up on material curtain, while, cocurrent enters in this operation
Thermal current, so as to remove the moisture in formed potassium nitrate granules, is preferably less than the water content in potassium nitrate granules
0.05%.
In potassium nitrate product after cooling down operation in step S3c, potassium nitrate particle diameter d ＜ 1mm mass fraction for 5~
8%, 1mm≤potassium nitrate particle diameter d ＜ 2mm mass fraction are 35~45%, 2mm≤potassium nitrate particle diameter d≤4mm mass fraction
For 40~52%, potassium nitrate particle diameter d ＞ 4mm mass fraction is 0~3%.
The potassium nitrate granules that preferable particle size is 2~4mm in the present embodiment are as fused salt level potassium nitrate, and screening gained particle diameter is small
It is input in 2mm potassium nitrate granules in comminutor and realizes granulation operations, the potassium nitrate granules that screening gained particle diameter is more than 4mm is passed through
Pulverizer is input in comminutor after crushing and realizes granulation operations, and realization is reclaimed to potassium nitrate granules after screening.
The potassium nitrate good fluidity of 2~4mm particle diameters, high mechanical strength, cracky and generation dust, are not easy to store and make
With, beneficial to the operation and binary or the operation of the mixing match amount of polynary fused salt product system packed automatically, in addition, screening 2~
The potassium nitrate of 4mm particle diameters can control the overall material balance of slurry-spraying pelletizing system, the nitric acid less than 2mm as fused salt level potassium nitrate
K particle, which is input in comminutor, to be realized and is again inputted into after granulation operations in step S3, reaches stable yields and the purpose of high yield, greatly
It is input to after the 4mm size-reduced machine of potassium nitrate granules is crushed in comminutor and realizes granulation operations, and is again inputted into step S3
In, so as to the nucleus fines required for supplementing in slurry-spraying pelletizing operation.
It is noted that in granulation operations, the discharging opening of comminutor is provided with the powder in Venturi scrubber, comminutor
Dirt and the vapor of heat enter Venturi scrubber through air channel in the presence of air-introduced machine, and the material after processing enters back into evaporation system
System, to realize the recovery to solid nitric acid potassium, the solid nitric acid potassium of recovery enter cooled down in step S3c, screening process.
Venturi scrubber is also known as venturi tube duster, is made up of Venturi tube knockouts and demister, dedusting
Journey can be divided into the three phases such as atomization, cohesion and demisting, and the first two stage is carried out in Venturi tube knockouts, latter stage
Completed in demister.Venturi scrubber is a kind of reduced investment, the wet cleaning equipment of efficiency high, the cooling to high-temperature gas
Work well, be widely used in dedusting, the cooling of high-temperature flue gas, can also serve as gas absorber.
Above-mentioned vapo(u)rization system can directly use the thermal current atmosphere in step S3b, so as to realize the potassium nitrate to recovery
The water removal operation of grain.
The present embodiment combination neutralisation prepares potassium nitrate, and offer is to the series of processing steps of neutralized reaction product potassium nitrate,
So as to directly produce the potassium nitrate of high-purity fused salt rank, with extraordinary industrial value.And described in the present embodiment
Process operating process simple efficient, each step and parameter are very easy to control, it can be realized using each machinery equipment
Automated production, high safety, it is adaptable to which the continuous-stable of high-purity grade of potassium nitrate is quickly produced, with higher economic benefit,
Beneficial to large-scale promotion.
In addition, the method for the present embodiment production fused salt level potassium nitrate is high to the utilization rate of raw material, high yield rate, effectively reduction
The production cost of fused salt level potassium nitrate.
Three specific embodiments are as follows, so that the invention will be further described.
Embodiment one
Step S1 neutralization steps：
The mass percent concentration of raw material potassium hydroxide solution is 31.54%, and chloride mass percent concentration is
0.005%, the mass percent concentration of sodium is 0.32%.Potassium hydroxide solution input is neutralized in kettle.According to potassium hydroxide with
The ratio between amount of material of nitric acid is 1:1.01, it is 43% to addition mass percent concentration in kettle is neutralized, amounts of ammonium salt 90ppm's
Dilute nitric acid solution.Potassium hydroxide solution and dilute nitric acid solution form reaction solution in kettle is neutralized, and occur neutralization reaction to generate nitre
Sour potassium solution.When to the pH of reaction solution being 6.4, the concentration of potassium nitrate is 30%, that is, obtains the first potassium nitrate material liquid.
Step S2 is concentrated by evaporation：
Make the first potassium nitrate material liquid realize by quadruple effect falling film evaporation device to be concentrated by evaporation.Via quadruple effect in the present embodiment
The temperature of the second potassium nitrate material liquid is 125 DEG C obtained by vaporization chamber, and concentration is 65%.
Step S3 slurry-spraying pelletizings：
Second potassium nitrate material liquid is input in spray gun after being cooled to 103 DEG C, starts spray gun, makes the material sprayed from spray gun
Atomization forms potassium nitrate granules, and causes potassium nitrate granules to remove moisture in thermal current simultaneously, so that by resulting nitric acid
Water content in k particle is reduced to 0.05%.The uneven potassium nitrate granules of particle are obtained through cooling.
Potassium nitrate granules after slurry-spraying pelletizing are sieved, take 2mm -4mm to be packed, as end-product fused salt level
Potassium nitrate.
In addition, potassium nitrate granules of the screening gained particle diameter less than 2mm are input in comminutor and realize granulation operations, institute is sieved
Obtain to be input in comminutor after the size-reduced machine of potassium nitrate granules of the particle diameter more than 4mm is crushed and realize granulation operations, realize to through sieve
Potassium nitrate granules after point are reclaimed.
In granulation operations, the discharging opening of comminutor is provided with the dust in Venturi scrubber, comminutor and the water steaming of heat
Gas enters Venturi scrubber through air channel in the presence of air-introduced machine, and the material after processing enters back into vapo(u)rization system, with realization pair
The recovery of solid nitric acid potassium, the solid nitric acid potassium of recovery enter cooled down in step S3c, screening process, above-mentioned vapo(u)rization system
Thermal current in as step S3b.
By detection, in the fused salt level potassium nitrate prepared using method described in the present embodiment, contents on dry basis is：Nitric acid
Potassium content 97.80%；Nitric acid sodium content 2.3%, moisture 0.02%, Cl-Content is 0.005%, water insoluble matter content
0.003%, NO2 -Content 0.003%, OH-Content 0, the content of iron is 0.0001%, Ca2+Content be 0, Mg2+Content be
0, SO4 2-Content be 0.001%, CO3 2-Content be 0.003%, meet the standard of the potassium nitrate available for fused salt market.
Embodiment two
Step S1 neutralization steps：
The mass percent concentration of raw material potassium hydroxide solution is 32.14%, and chloride mass percent concentration is
0.004%, the mass percent concentration of sodium is 0.30%.Potassium hydroxide solution input is neutralized in kettle.According to potassium hydroxide with
The ratio between amount of material of nitric acid is 1:1.02, it is 45% to addition mass percent concentration in kettle is neutralized, amounts of ammonium salt 90ppm's
Dilute nitric acid solution.Potassium hydroxide solution and dilute nitric acid solution form peracid reaction solution in kettle is neutralized, and occur neutralization reaction with life
Into potassium nitrate solution.When to the pH of reaction solution being 6.7, the concentration of potassium nitrate is 33%, that is, obtains the first potassium nitrate material liquid.
Step S2 is concentrated by evaporation：
Making the first potassium nitrate material liquid, just body realizes evaporation and concentration by quadruple effect falling film evaporation device.In the present embodiment via
The temperature that the second potassium nitrate material liquid is obtained behind four-effect evaporation room is 130 DEG C, and concentration is 68.5%.
Step S3 slurry-spraying pelletizings：
Second potassium nitrate material liquid is input in spray gun after being cooled to 105 DEG C, starts spray gun, makes the material sprayed from spray gun
Atomization forms potassium nitrate granules, and causes potassium nitrate granules to remove moisture in thermal current simultaneously, so that by resulting nitric acid
Water content in k particle is reduced to 0.05%.The uneven potassium nitrate granules of particle are obtained through cooling.
Potassium nitrate granules after slurry-spraying pelletizing are sieved, take 2mm -4mm to be packed, as end-product fused salt level
Potassium nitrate.
In addition, potassium nitrate granules of the screening gained particle diameter less than 2mm are input in comminutor and realize granulation operations, institute is sieved
Obtain to be input in comminutor after the size-reduced machine of potassium nitrate granules of the particle diameter more than 4mm is crushed and realize granulation operations, realize to through sieve
Potassium nitrate granules after point are reclaimed.
In granulation operations, the discharging opening of comminutor is provided with the dust in Venturi scrubber, comminutor and the water steaming of heat
Gas enters Venturi scrubber through air channel in the presence of air-introduced machine, and the material after processing enters back into vapo(u)rization system, with realization pair
The recovery of solid nitric acid potassium, the solid nitric acid potassium of recovery enter cooled down in step S3c, screening process, above-mentioned vapo(u)rization system
Thermal current in as step S3b.
By detection, in the fused salt level potassium nitrate prepared using method described in the present embodiment, contents on dry basis is：Nitric acid
Potassium content 98.10%；Nitric acid sodium content 1.7%, moisture 0.02%, Cl-Content is 0.003%, water insoluble matter content
0.003%, NO2 -Content 0.003%, OH-Content 0, the content of iron is 0.0002%, Ca2+Content be 0, Mg2+Content be
0, SO4 2-Content be 0.001%, CO3 2-Content be 0.004%, meet the standard of the potassium nitrate available for fused salt market.
Embodiment three
Step S1 neutralization steps：
The mass percent concentration of raw material potassium hydroxide solution is 31.78%, and chloride mass percent concentration is
0.005%, the mass percent concentration of sodium is 0.38%.Potassium hydroxide solution input is neutralized in kettle.According to potassium hydroxide with
The ratio between amount of material of nitric acid is 1:1.01, it is 48% to addition mass percent concentration in kettle is neutralized, amounts of ammonium salt 90ppm's
Dilute nitric acid solution.Potassium hydroxide solution and dilute nitric acid solution form peracid reaction solution in kettle is neutralized, and occur neutralization reaction with life
Into potassium nitrate solution.When to the pH of reaction solution being 6.4, the concentration of potassium nitrate is 35%, that is, obtains the first potassium nitrate material liquid.
Step S2 is concentrated by evaporation：
Making the first potassium nitrate material liquid, just body realizes evaporation and concentration by quadruple effect falling film evaporation device.In the present embodiment via
The temperature that the second potassium nitrate material liquid is obtained behind four-effect evaporation room is 125 DEG C, and concentration is 70%.
Step S3 slurry-spraying pelletizings：
Second potassium nitrate material liquid is input in spray gun after being cooled to 104 DEG C, starts spray gun, makes the material sprayed from spray gun
Atomization forms potassium nitrate granules, and causes potassium nitrate granules to remove moisture in thermal current simultaneously, so that by resulting nitric acid
Water content in k particle is reduced to 0.05%.The uneven potassium nitrate granules of particle are obtained through cooling.
Potassium nitrate granules after slurry-spraying pelletizing are sieved, take 2mm -4mm to be packed, as end-product fused salt level
Potassium nitrate.
In addition, potassium nitrate granules of the screening gained particle diameter less than 2mm are input in comminutor and realize granulation operations, institute is sieved
Obtain to be input in comminutor after the size-reduced machine of potassium nitrate granules of the particle diameter more than 4mm is crushed and realize granulation operations, realize to through sieve
Potassium nitrate granules after point are reclaimed.
In granulation operations, the discharging opening of comminutor is provided with the dust in Venturi scrubber, comminutor and the water steaming of heat
Gas enters Venturi scrubber through air channel in the presence of air-introduced machine, and the material after processing enters back into vapo(u)rization system, with realization pair
The recovery of solid nitric acid potassium, the solid nitric acid potassium of recovery enter cooled down in step S3c, screening process, above-mentioned vapo(u)rization system
Thermal current in as step S3b.
By detection, in the fused salt level potassium nitrate prepared using the present embodiment methods described, contents on dry basis is：Potassium nitrate
Content 97.50%；Nitric acid sodium content 2.3%, moisture 0.02%, Cl-Content is less than 0.004%, water insoluble matter content
0.003%, NO2 -Content 0.003%, OH-Content 0, the content of iron is 0.0001%, Ca2+Content be 0, Mg2+Content be
0, SO4 2-Content be 0.001%, CO3 2-Content be 0.002%, meet the standard of the potassium nitrate available for fused salt market.
It should be noted that the present invention will be described rather than limits the invention for above-described embodiment, and this
Art personnel can design alternative embodiment without departing from the scope of the appended claims.In claim
In, any reference symbol between bracket should not be configured to limitations on claims.Word "comprising" is not excluded for depositing
In element or step not listed in the claims.
Claims (9)
1. a kind of method for producing fused salt level potassium nitrate, it is characterised in that comprise the following steps：
Step S1 neutralization steps：
Potassium hydroxide solution is mixed to form reaction solution with salpeter solution, wherein, the material of the potassium hydroxide and the nitric acid
The ratio between amount is 1:1.01~1.02,
Neutralization reaction generation potassium nitrate occurs in the reaction solution, the first potassium nitrate material liquid is obtained；
Step S2 evaporization process：
Concentration is evaporated to the first potassium nitrate material liquid, the second potassium nitrate material liquid is obtained,
Wherein, the mass percent concentration of potassium nitrate is 65~70% in the second potassium nitrate material liquid；
Step S3 slurry-spraying pelletizing processes：
Slurry-spraying pelletizing is carried out to the second potassium nitrate material liquid, so that end-product fused salt level potassium nitrate is made.
2. the method for production fused salt level potassium nitrate according to claim 1, it is characterised in that in the step S1, participate in
The potassium hydroxide solution of neutralization reaction includes potassium hydroxide, chloride and sodium, and the mass percent concentration of the potassium hydroxide is
31~33%, chloride mass percent concentration is less than 0.005%, and the mass percent concentration of sodium is less than 0.5%；
Participating in the salpeter solution of neutralization reaction includes nitric acid and ammonium salt, and the mass percent concentration of the nitric acid is 43~48%,
Amounts of ammonium salt is less than 100ppm.
3. the method for production fused salt level potassium nitrate according to claim 1, it is characterised in that in step S1, described first
The pH value of potassium nitrate material liquid is that the mass percent concentration of potassium nitrate in 6.4~6.7, the first potassium nitrate material liquid is 30
~35%.
4. the method for production fused salt level potassium nitrate according to claim 1, it is characterised in that described in the step S2
Evaporization process is carried out in quadruple effect falling film evaporation device.
5. the method for production fused salt level potassium nitrate according to claim 1, it is characterised in that the whitewashing in the step S3
Granulating working procedure comprises the following steps：
A. the mass percent concentration obtained by cooling step S2 is 65~70% the second potassium nitrate material liquid, is to temperature
At 103~105 DEG C, it is input in spray gun；
B. start spray gun, make to be atomized to form potassium nitrate granules from the material that spray gun sprays, and cause potassium nitrate granules in heat simultaneously
Moisture is removed in air-flow；
C. cool down, sieve potassium nitrate granules, end-product fused salt level potassium nitrate is made.
6. the method for production fused salt level potassium nitrate according to claim 5, it is characterised in that sieved in the step S3c
The particle diameter of the fused salt level potassium nitrate of gained is 2~4mm.
7. the method for production fused salt level potassium nitrate according to claim 6, it is characterised in that sieved in the step S3c
The potassium nitrate granules that gained particle diameter is less than 2mm are input in comminutor and realize and be again inputted into after granulation operations in step S3, institute
State in step S3c screening gained particle diameter and be more than after the size-reduced machine of 4mm potassium nitrate granules is crushed to be input to and realize and make in comminutor
Grain operation, and be again inputted into step S3.
8. the method for production fused salt level potassium nitrate according to claim 7, it is characterised in that in the granulation operations, make
The dust that the discharging opening of grain machine is provided with Venturi scrubber, the comminutor sequentially enters Venturi scrubber and evaporation is
System, to reclaim solid nitric acid potassium, the solid nitric acid potassium of recovery enters to be sieved in step S3c.
9. according to claim 5 production fused salt level potassium nitrate method, it is characterised in that in the step S3b
The water content of the potassium nitrate granules is set to be less than 0.05% in thermal current.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710464258.0A CN107128953A (en) | 2017-06-19 | 2017-06-19 | A kind of method for producing fused salt level potassium nitrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710464258.0A CN107128953A (en) | 2017-06-19 | 2017-06-19 | A kind of method for producing fused salt level potassium nitrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107128953A true CN107128953A (en) | 2017-09-05 |
Family
ID=59735337
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710464258.0A Pending CN107128953A (en) | 2017-06-19 | 2017-06-19 | A kind of method for producing fused salt level potassium nitrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107128953A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108017071A (en) * | 2017-12-08 | 2018-05-11 | 中国科学院青海盐湖研究所 | A kind of method that potassium is recycled in the tail washings from industry containing potassium |
| CN108584991A (en) * | 2018-05-04 | 2018-09-28 | 中国成达工程有限公司 | A kind of low chlorine photo-thermal fused salt production technology and process units |
| CN109384251A (en) * | 2018-12-12 | 2019-02-26 | 青海盐湖工业股份有限公司 | A kind of prilling process of potassium nitrate and its potassium nitrate granules of preparation |
| CN111518525A (en) * | 2020-04-23 | 2020-08-11 | 青海盐湖工业股份有限公司 | Method and system for preparing binary molten salt |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070167A (en) * | 2007-06-14 | 2007-11-14 | 上海文通化工有限公司 | Potassium nitrate preparing technology |
| CN106276985A (en) * | 2016-07-22 | 2017-01-04 | 中国科学院青海盐湖研究所 | A kind of preparation method of potassium nitrate |
| CN106698483A (en) * | 2017-01-19 | 2017-05-24 | 青海盐湖工业股份有限公司 | Method for producing molten salt-grade sodium nitrate |
-
2017
- 2017-06-19 CN CN201710464258.0A patent/CN107128953A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101070167A (en) * | 2007-06-14 | 2007-11-14 | 上海文通化工有限公司 | Potassium nitrate preparing technology |
| CN106276985A (en) * | 2016-07-22 | 2017-01-04 | 中国科学院青海盐湖研究所 | A kind of preparation method of potassium nitrate |
| CN106698483A (en) * | 2017-01-19 | 2017-05-24 | 青海盐湖工业股份有限公司 | Method for producing molten salt-grade sodium nitrate |
Non-Patent Citations (1)
| Title |
|---|
| 逯亚平: "硝酸钾生产工艺及研究进展概述", 《化工管理》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108017071A (en) * | 2017-12-08 | 2018-05-11 | 中国科学院青海盐湖研究所 | A kind of method that potassium is recycled in the tail washings from industry containing potassium |
| CN108017071B (en) * | 2017-12-08 | 2019-09-17 | 中国科学院青海盐湖研究所 | A method of recycling potassium from the tail washings of industry containing potassium |
| CN108584991A (en) * | 2018-05-04 | 2018-09-28 | 中国成达工程有限公司 | A kind of low chlorine photo-thermal fused salt production technology and process units |
| CN108584991B (en) * | 2018-05-04 | 2020-07-21 | 中国成达工程有限公司 | Low-chlorine photo-thermal molten salt production process and production device |
| CN109384251A (en) * | 2018-12-12 | 2019-02-26 | 青海盐湖工业股份有限公司 | A kind of prilling process of potassium nitrate and its potassium nitrate granules of preparation |
| CN111518525A (en) * | 2020-04-23 | 2020-08-11 | 青海盐湖工业股份有限公司 | Method and system for preparing binary molten salt |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107128953A (en) | A kind of method for producing fused salt level potassium nitrate | |
| CN105308773B (en) | It is used to prepare the multistage process and system of battery unit material | |
| US8470055B2 (en) | Combined process for preparing calcined soda by applying surface engineering technology to natural soda preparation | |
| CN102424616B (en) | Full water-soluble urea-based composite fertilizer and preparation method thereof | |
| CN104445306B (en) | Manufacture the apparatus and method of magnesium sulfate | |
| CN103848670A (en) | Process for producing high-concentration compound fertilizer by virtue of concentrated ammonium phosphate slurry one-step method | |
| CN106698483B (en) | A method of producing fused salt grade sodium nitrate | |
| CN105236374B (en) | A kind of preparation method of granular diammonium phosphate | |
| CN105110819A (en) | Method used for producing sulfur-based urea compound fertilizer from ammonia desulphurization by-products | |
| CN1289443C (en) | Method and apparatus for producing calcium ammonium nitrate using by-product calcium nitrate of nitrate phosphatic fertilizer | |
| CN105503758A (en) | Melamine production system and technique | |
| CN104230429A (en) | Powdered water-soluble NPK composite fertilizer and preparation method thereof | |
| CN103391897A (en) | Manufacturing method and manufacturing device for multiple oxide | |
| CN103011114A (en) | Method of producing monopotassium phosphate | |
| CN105399455B (en) | A kind of system and method using chemical industry tail gas production compound fertilizer | |
| CN207391303U (en) | A kind of production system of urea nitrophosphate fertilizer product | |
| CN105347703B (en) | A kind of decomposition method of calcium carbonate and magnesium carbonate ore deposit | |
| CN100420694C (en) | Preparation method of crystalline xylosic alcohol powder | |
| CN109360951A (en) | A kind of preparation method of modified nickel ion doped | |
| CN101434519B (en) | Preparation of tetrabromobisphenol A bis(2,3-dibromopropyl)ether | |
| CN105271429A (en) | Method for preparing iron oxide red and hydrochloric acid from hot galvanized waste acid | |
| CN101343206B (en) | Process for preparing circular particle kalium based fertilizer | |
| EP3950593B1 (en) | Method for preparing ammonia by using ammonium salt and silicate | |
| CN203048601U (en) | Crystal ammonium phosphate cooling crystallization device | |
| CN208776330U (en) | A kind of four water-calcium nitrate fertilizer production system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170905 |