CN108083877A - A kind of method that calcium nitrate using Phosphate Fertilizer Nitrate with Frozen Method process by-product produces calcium nitrate-urea as raw material - Google Patents
A kind of method that calcium nitrate using Phosphate Fertilizer Nitrate with Frozen Method process by-product produces calcium nitrate-urea as raw material Download PDFInfo
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- CN108083877A CN108083877A CN201711383504.6A CN201711383504A CN108083877A CN 108083877 A CN108083877 A CN 108083877A CN 201711383504 A CN201711383504 A CN 201711383504A CN 108083877 A CN108083877 A CN 108083877A
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- nitrate
- calcium nitrate
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05C—NITROGENOUS FERTILISERS
- C05C5/00—Fertilisers containing other nitrates
- C05C5/04—Fertilisers containing other nitrates containing calcium nitrate
Abstract
The present invention relates to the methods that calcium nitrate-urea production technical field, especially a kind of calcium nitrate using Phosphate Fertilizer Nitrate with Frozen Method process by-product produce calcium nitrate-urea as raw material.During freezing produces nitrophosphate fertilizer, after the by-product calcium nitrate of generation is by neutralizing purification, pressure filtration washing, concentration, spray drying treatment, synthetic reaction is carried out with urea melt, obtain calcium nitrate-urea, product physical property is preferable, intensity stabilization, it is nonhygroscopic, therefore hardened dusting, and calcium nitrate-urea product total nitrogen content ＞ 31%, acyl state nitrogen content 15~28% are not easy, nitrate nitrogen is 3~12%, water-soluble calcium 4~12%, unit of the product nutrient cost is relatively low, and product price is easily received by market；And effectively prevent " in existing compound fertilizer granules process of producing product, when ammonium nitrate is mixed with urea, the gradual dusting of meeting, strength reduction, so as to influence fertilizer quality in the particle short time " the defects of.
Description
Technical field
It is especially a kind of with Phosphate Fertilizer Nitrate with Frozen Method process by-product the present invention relates to calcium nitrate-urea production technical field
The method that calcium nitrate produces calcium nitrate-urea for raw material.
Background technology
Freezing production nitrophosphate fertilizer is in nineteen twenty-eight, and Odda Smelt companies of Norway put forward, and use nitric acid point
Phosphorus ore is solved, obtains acid hydrolysis solution, and acid hydrolysis solution is fallen into substantial amounts of calcium nitrate by freezing separation, is then processed into fertilizer again,
Sale so that the production of Phosphate Fertilizer Nitrate with Frozen Method has obtained commercial practice.It is and continuous with Phosphate Fertilizer Nitrate with Frozen Method technology
Development so that in nineteen thirty-seven, the Lonza companies of Switzerland propose to manufacture the side of nitro calcium superphosphate with 70% decomposing phosphorite by using nitric acid powder
Method, product contain 8%N, 16%P205.There is extremely strong hygroscopicity, in addition product is always supported in product when containing nitric acid hydrate of calcium
The problems such as point content is low, nitrogen dioxide effusion is serious in production, and do not promote and apply.Between 1942-1945, Norsk Hydro
The Phosphate Fertilizer Production of company is interrupted and stopped production due to war, raw material.It resumes production after the war, at 1950, freezing nitric acid phosphorus
The yield of fertilizer is 40,000 tons/year.Or so nineteen fifty, German BASF companies, the Dutch State Mines of Holland and France
Some chemical plant all develop the freezing and mixed acid process nitrophosphate fertilizer technology of oneself in succession.Because most companies technical foundation all
It is related to the Odda techniques of freezing deliming, therefore, Phosphate Fertilizer Nitrate with Frozen Method is referred to as Odda methods by fertilizer circle.
The nitric acid decomposed solution of phosphorus ore is cooled to 10~-5 DEG C by Phosphate Fertilizer Nitrate with Frozen Method, 60~85% with Ca (NO3)2·
4H2O crystal forms are precipitated, and the mother liquor after separation is neutralized with ammonia, and reaction equation is：
HNO3+H3PO4+H2SiF6+4Ca(NO3)2+9NH3+2H2O→CaHPO4+3CaF2+SiO2+9NH4NO3；Neutralize slip
Concentrated, granulation is dried and sieved up to nitrophosphate fertilizer product.And for freezing during, crystallize four water nitric acid of precipitation
Calcium component typically changes into ammonium nitrate using ammonium carbonate reaction, is added in neutralize slip, to improve its mobility；Or
It is to be directly added into ammonium carbonate or ammonium nitrate production calcium ammonium nitrate product, which is 15.5%, but its easy moisture absorption
It is hardened so that it needs to be coated on particle surface using package oil, causes cost higher, and also its calcium content reaches 18%, much
Higher than crops to the demand of calcium constituent so that obtained product quality is poor.
In consideration of it, generally require the calcium ammonium nitrate of preparation and urea is compound fertile as crops, and by ammonium nitrate
During calcium and urea progress are compound, due to the presence of two kinds of ingredients of ammonium nitrate and urea, the composite fertilizer prepared can be caused
In very short time dusting occurs for grain, influences the qualities such as intensity, the fertilizer efficiency of fertilizer product.
Based on this, this researcher passes through in production practices, to the by-product of Phosphate Fertilizer Nitrate with Frozen Method production process by-product-
Calcium nitrate is used, and produces calcium nitrate-urea composite fertilizer, largely improves the quality of composite fertilizer, improves simultaneously
The intensity of fertiliser granulates.
The content of the invention
In order to solve the above technical problems existing in the prior art, the present invention provides one kind with Phosphate Fertilizer Nitrate with Frozen Method work
The method that the calcium nitrate of skill by-product produces calcium nitrate-urea for raw material.
It is achieved particular by following technical scheme：
A kind of calcium nitrate using Phosphate Fertilizer Nitrate with Frozen Method process by-product as raw material produce calcium nitrate-urea method, including with
Lower step：
(1) in Phosphate Fertilizer Nitrate with Frozen Method production process, the calcium nitrate for freezing the acquisition of deliming process is crystallized, water is added to be made into
Solution obtains calcium nitrate solution；
(2) lime or milk of lime are added in into calcium nitrate solution, is neutralized, press filtration obtains filtrate and filter cake；
(3) filter cake with wash water is washed, dried up, the washing lotion return neutralization purification tank preparation calcium nitrate of filter press discharge is molten
Liquid, the neutralization slag that filter press is drawn off return to nitrophosphate fertilizer waste water recovery system recycling phosphorus；The filtrate of filter press discharge is concentrated, spray
Mist is dried, and obtains calcium nitrate, is sent into synth sink；
(4) Urea is melted, obtains molten mass, and add in synth sink, synthetic reaction occurs with calcium nitrate, through supercooling
But, cure, is broken, obtain agramon nitric acid calcium product or using high tower or slurry-spraying pelletizing, cooling, curing, obtaining granular
Calcium nitrate-urea product or after synthetic reaction adds in sylvite, and mixing is granulated, and obtains nitrogen, the production of potassium binary compound fertilizer
Product.
It is preferred that the step (2), under conditions of calcium nitrate solution is stirred continuously, adds in lime or milk of lime neutralizes,
So that pH value is 6-7.
It is preferred that the step (2), reaction temperature is 25-105 DEG C, time 0.5-2h.
It is preferred that the filtrate concentration, is to concentrate the filtrate to moisture content as 16-22%.
It is preferred that the synthetic reaction, temperature is 125-165 DEG C, residence time 0.25-0.5h.
It is preferred that the urea, addition is (60-120) with spray drying resulting material mass ratio:(41-50).
It is preferred that the step (3), is by after spray drying resulting material melting, is sent into synth sink.
It is preferred that the sylvite for one kind in potassium chloride, potassium nitrate, potassium dihydrogen phosphate, potassium hydrogen phosphate, potassium phosphate etc. or
Person is a variety of.
Compared with prior art, the technique effect of the invention is embodied in：
During producing nitrophosphate fertilizer to freezing, the by-product calcium nitrate of generation is by neutralizing purification, pressure filtering cleaning
Wash, concentrate, after spray drying treatment, with fusing urea carry out synthetic reaction so that the calcium nitrate-urea product of acquisition it is strong
Degree is stablized, and calcium nitrate-urea, total nitrogen content ＞ 31%, wherein acyl state nitrogen content 15~28%, nitrate nitrogen for 3~
12%, water-soluble calcium 4~12%；Unit of the product nutrient cost is relatively low, and product price is easily received by market；And it effectively prevents
" in existing compound fertilizer granules process of producing product, it, can gradual powder in the particle short time when ammonium nitrate is mixed with urea
Change, strength reduction, so as to influence fertilizer quality " the defects of.
It is to carry out the calcium nitrate in Phosphate Fertilizer Nitrate with Frozen Method production process, crystallized out specifically in processing procedure
Water is added to be configured to starch, then adds in lime or milk of lime thereto, free nitric acid, phosphoric acid, fluosilicic acid in neutralization solution etc. will
Impurity component is removed, and obtains the higher calcium nitrate solution of purity, and by the solution by concentrating, spray drying melts it
Synthetic reaction is carried out with urea melt afterwards, effectively improves the nutrient of product, and the product prepared is not easy moisture absorption dusting, by force
Degree is stablized, and quality is more excellent.
Specifically in processing procedure, including following reaction：
N-process：
Ca(OH)2+2HNO3→Ca(NO3)2+2H2O；
Ca(OH)2+H3PO4→CaHPO4↓+2H2O；
H2SiF6+3Ca(OH)2→3CaF2↓+SiO2↓+4H2O；
Building-up process：
Ca(NO3)2+4CO(NH2)2→Ca(NO3)2+4CO(NH2)2。
Description of the drawings
Fig. 1 is the process flow chart of the invention.
Specific embodiment
It is limited technical scheme is further, but is required with specific embodiment below in conjunction with the accompanying drawings
The scope of protection is not only limited to made description.
Embodiment 1
As shown in Figure 1, by Phosphate Fertilizer Nitrate with Frozen Method production process, the thick nitre calcium of acquisition is crystallized (containing N 10.54%, P2O5
0.28%th, CaO19.70%, F 0.19%) 800kg send to neutralize purification tank, add in 150kg water be made into thick nitre calcium liquid, continuous
150kg milk of limes (CaO content~10%) are added under stirring condition, are neutralized to pH value 6~7,60~85 DEG C of reaction temperature, when
Between 1h, then pressure filtration washing, filter cake are washed with water, then are dried up with compressed air, then draw off neutralization slag, neutralize slag and return to nitric acid
Phosphate fertilizer waste water recovery system recycles phosphorus；Concentrating filter liquor, spray drying, obtains anhydrous nitric acid calcium 465kg, send to synth sink, then press
Calcium nitrate：Urea melt=164:240 mass ratio adds in urea melt and carries out synthetic reaction, directly cools and solidifies to obtain nothing
Water calcium nitrate-urea 1110kg, product contain total N 33.41%, NAcyl26.87%th, NNitre6.54%th, CaWater9.30%；After testing：It is worked as
Its product strength 26.82N places 10 days product strength 26.85N, and one month product rheobase sheet of placement is unchanged, maintains
26.81 between~26.83N.In process of production, researcher passes through the thick nitre calcium obtained to embodiment 1, is directly over concentrating,
After drying process, itself and urea melt are subjected to synthetic reaction, obtained product total nitrogen content compares embodiment 1 low 5 hundred
Branch, and also low 3.1 percentage points of the content of water-soluble calcium, and the intensity that its same day produces is in 24.45N, placement
Decline 20% within 10 days, after placing one month, the basic dusting of product.
Embodiment 2
As shown in Figure 1, by Phosphate Fertilizer Nitrate with Frozen Method production process, the thick nitre calcium of acquisition is crystallized (containing N 10.54%, P2O5
0.28%th, CaO19.70%, F 0.19%) 800kg send to neutralize purification tank, add in 150kg water be made into thick nitre calcium liquid, continuous
150kg milk of limes (CaO content~10%) are added under stirring condition, are neutralized to pH value 6~7,60~85 DEG C of reaction temperature, when
Between 1h, then pressure filtration washing, filter cake are washed with water, then are dried up with compressed air, then draw off neutralization slag, neutralize slag and return to nitric acid
Phosphate fertilizer recycles phosphorus；Concentrating filter liquor, spray drying, obtains calcium nitrate 518kg and send to synth sink, then by calcium nitrate：Urea melt=
182:240 ratios add in urea melt carry out synthetic reaction, directly cool and solidify a water calcium nitrate-urea 1175kg, product contain
N 32.48%, NAcyl26.06%th, NNitre6.42%th, CaWater9.10%；Its same day product strength 9.72N, places 10 days product strengths
It is unchanged to place a month product rheobase sheet by 9.75N.
In process of production, researcher passes through the thick nitre calcium obtained to embodiment 1, is directly over concentrating, after drying process,
Itself and urea melt are subjected to synthetic reaction, obtained product total nitrogen content compares 1 low 7.8 percentage point of embodiment, and
Also low 2.87 percentage points of the content of water-soluble calcium, and the intensity that its same day produces, in 9.56N, placement declines for 10 days
20%, after placing one month, intensity has dropped 60%, maintains between 9.68~9.73N.
Embodiment 3
By water calcium nitrate-urea (N 32.48%, a N made from embodiment 2Acyl26.06%th, NNitre6.42%th, CaWater
9.10%) melt 1340kg, then by a water calcium nitrate-urea melt：Potassium chloride=67：33 ratio adds in potassium chloride 660kg
Mixing granulation contains N 21.65%, N to get nitrogen, potassium binary compound fertilizer 1978kg, productAcyl17.33%th, NNitre4.32%th, K2O
20.28%th, CaWater6.06%；Its same day product strength 34.68N, places 14 days product strength 34.65N, places a month product
Intensity is substantially unchanged.
For that during potassium chloride is added, other sylvite can also be used to add, such as：Potassium nitrate, biphosphate
One or more in potassium, potassium hydrogen phosphate, potassium phosphate etc..
In certain embodiments, the step (2), under conditions of calcium nitrate solution is stirred continuously, add in lime or
Milk of lime so that pH value 6-7.
In certain embodiments, the step (2), reaction temperature are 25-105 DEG C, time 0.5-2h.
In certain embodiments, filtrate concentration is to concentrate the filtrate to moisture content as 16-22%.
In certain embodiments, the synthetic reaction, temperature are 125-165 DEG C, residence time 0.25-0.5h.
In certain embodiments, the urea, addition are (60-120) with spray drying resulting material mass ratio:
(41-50)。
In certain embodiments, the step (3) are after spray drying resulting material is prepared into molten mass, to be sent into
Synth sink.
In above choice of parameters implementation process, the calcium nitrate-urea that is obtained, total nitrogen content ＞ 31%, wherein acyl
State nitrogen content 15~28%, nitrate nitrogen are 3~12%, water-soluble calcium 4~12%.Product strength is on the day of, after 14 days, after 1 month
Substantially it is unchanged, illustrate technical solution of the present invention ideal, improve the quality of fertilizer product and the intensity of particle.
In addition, when selecting other sylvite such as potassium sulfate, potassium hydroxide, potassium carbonate, saleratus, potassium sulfite, gained
Product quality can be a bit weaker, as total nitrogen content be less than 30% or acyl state nitrogen content be less than 15%.
It is 50 selecting urea addition and calcium nitrate spray-dried granules material ratio:40 or 120:When 30, can also it cause
Product quality and intensity are affected.
Meanwhile reaction temperature is too low and the reaction time is too short, can so that reaction is incomplete, and if temperature is excessively high, the time
Too long, overreact can cause the result of quality and stability difference.
Granule strength more than the invention is measured using fertiliser granulates intensity measuring device, is specifically used
The detection of the similar strengths analyzers such as YHKC-3A types automatic detector for strength of particles.
Claims (9)
1. a kind of method that calcium nitrate using Phosphate Fertilizer Nitrate with Frozen Method process by-product produces calcium nitrate-urea as raw material, feature exist
In comprising the following steps：
(1) in Phosphate Fertilizer Nitrate with Frozen Method production process, the calcium nitrate for freezing the acquisition of deliming process is crystallized, water is added to be made into molten
Liquid obtains calcium nitrate solution；
(2) lime or milk of lime are added in into calcium nitrate solution, is neutralized, press filtration obtains filtrate and filter cake；
(3) filter cake with wash water is washed, dried up, the washing lotion of filter press discharge, which returns, neutralizes purification tank preparation calcium nitrate solution, pressure
The neutralization slag that filter is drawn off returns to nitrophosphate fertilizer waste water recovery system recycling phosphorus；The filtrate of filter press discharge is concentrated, spraying is dry
It is dry, calcium nitrate is obtained, is sent into synth sink；
(4) Urea is melted, obtains molten mass, and add in synth sink, synthetic reaction occurs with calcium nitrate, through supercooling, admittedly
Change, is broken, obtain agramon nitric acid calcium product or using high tower or slurry-spraying pelletizing, cooling, curing, obtaining Granular Urea
Nitric acid calcium product or after synthetic reaction adds in sylvite, and mixing is granulated, and obtains nitrogen, potassium binary compound fertilizer product.
2. calcium nitrate-urea is produced by raw material of the calcium nitrate of Phosphate Fertilizer Nitrate with Frozen Method process by-product as described in claim 1
Method, which is characterized in that the step (2) under conditions of calcium nitrate solution is stirred continuously, adds in lime or milk of lime,
PH value is neutralized to as 6-7.
3. urea nitric acid is produced by raw material of the calcium nitrate of Phosphate Fertilizer Nitrate with Frozen Method process by-product as claimed in claim 1 or 2
The method of calcium, which is characterized in that the step (2), reaction temperature are 25-105 DEG C, time 0.5-2h.
4. calcium nitrate-urea is produced by raw material of the calcium nitrate of Phosphate Fertilizer Nitrate with Frozen Method process by-product as described in claim 1
Method, which is characterized in that the filtrate concentration is to concentrate the filtrate to moisture content as 16-22%.
5. calcium nitrate-urea is produced by raw material of the calcium nitrate of Phosphate Fertilizer Nitrate with Frozen Method process by-product as described in claim 1
Method, which is characterized in that the synthetic reaction, temperature are 125-165 DEG C, residence time 0.25-0.5h.
6. calcium nitrate-urea is produced by raw material of the calcium nitrate of Phosphate Fertilizer Nitrate with Frozen Method process by-product as described in claim 1
Method, which is characterized in that the urea, addition are (60-120) with spray drying resulting material mass ratio:(41-50).
7. calcium nitrate-urea is produced by raw material of the calcium nitrate of Phosphate Fertilizer Nitrate with Frozen Method process by-product as described in claim 1
Method, which is characterized in that the step (3) is by after spray drying resulting material melting, is sent into synth sink.
8. calcium nitrate-urea is produced by raw material of the calcium nitrate of Phosphate Fertilizer Nitrate with Frozen Method process by-product as described in claim 1
Method, which is characterized in that the sylvite is one in potassium chloride, potassium nitrate, potassium dihydrogen phosphate, potassium hydrogen phosphate, potassium phosphate etc.
Kind is a variety of.
9. such as the calcium nitrate-urea of claim 1-8 any one of them method production, wherein total nitrogen content ＞ 31%, acyl state
Nitrogen content 15~28%, nitrate nitrogen are 3~12%, water-soluble calcium 4~12%.
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| CN201711383504.6A CN108083877A (en) | 2017-12-20 | 2017-12-20 | A kind of method that calcium nitrate using Phosphate Fertilizer Nitrate with Frozen Method process by-product produces calcium nitrate-urea as raw material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113603554A (en) * | 2021-07-30 | 2021-11-05 | 太原柏悟化工科技有限公司 | Production method of urea nitrophosphate fertilizer |
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