CN109251062A - The nitrophosphate fertilizer and preparation method thereof of low water insoluble matter content - Google Patents
The nitrophosphate fertilizer and preparation method thereof of low water insoluble matter content Download PDFInfo
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- CN109251062A CN109251062A CN201811207938.5A CN201811207938A CN109251062A CN 109251062 A CN109251062 A CN 109251062A CN 201811207938 A CN201811207938 A CN 201811207938A CN 109251062 A CN109251062 A CN 109251062A
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- nitrophosphate fertilizer
- insoluble matter
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- fertilizer
- low water
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B11/00—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes
- C05B11/04—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid
- C05B11/06—Fertilisers produced by wet-treating or leaching raw materials either with acids in such amounts and concentrations as to yield solutions followed by neutralisation, or with alkaline lyes using mineral acid using nitric acid (nitrophosphates)
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/36—Nitrates
- C01F11/38—Preparation with nitric acid or nitrogen oxides
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- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a kind of nitrophosphate fertilizer of low water insoluble matter content, the weight ratio that water-insoluble accounts for nitrophosphate fertilizer in nitrophosphate fertilizer is less than or equal to 0.2%, and the ratio that the weight of the acid non-soluble substance in water-insoluble accounts for water-insoluble weight is less than or equal to 50%.The present invention controls the size of the content of insoluble matter and insoluble matter particle in the nitrophosphate fertilizer of low water insoluble matter content, and product has preferably water-soluble.
Description
Technical field
The present invention relates to the nitrophosphate fertilizer of nitrophosphate fertilizer preparation technical field more particularly to a kind of low water insoluble matter content and
Preparation method.
Background technique
Nitrophosphate fertilizer refers to the phosphate rock decomposition powder with nitric acid or based on nitric acid, the nitrogen generated after ammoniated treatment
Phosphorus binary compound fertilizer.Phosphate Fertilizer Production process specifically includes that the acid of phosphorus ore, acid non-soluble substance separation, calcium nitrate Crystallization Separation, mother
Liquefied ammonia neutralization, the concentration of NP slurry, granulation, drying, screening, the conversion of packaging and calcium nitrate prepare ammonium nitrate etc..
At present nitrophosphate process production compound fertilizer in due to phosphorus ore raw material can not acidolysis acid non-soluble substance and preparation process
The calcium phosphate precipitation of middle generation leads in compound fertilizer that the insoluble content of water is exceeded, cannot achieve complete water-soluble.
In order to promoted preparation nitrophosphate fertilizer water solubility, there are many technologies new try and change to preparation process
Into.For example use is proposed in No. 201410033591.2 water soluble phosphorous fertilizers and preparation method thereof " with-XH base of class hydroxylcontaining materials
The crystallization of calcium oxide, magnesia, iron oxide, silica in group's filling ground phosphate rock lacks, and crystal structure is made irreversibility occur
It destroys, gradually becomes amorphous structure and fall into；Then carrying out ionization polarization again makes Ca in ground phosphate rock2+、Mg2+、Fe3+、Si4+Polarization,
Ionic bond strength reduction forms R-Ca2+、R-Mg2+、R-Fe3+、R-Si4+The soluble cation of mode ".This method is in discomfort
It is prepared for nitrophosphate fertilizer, because the impurity such as main Ca, Mg, Fe are that acid-soluble substances mass-energy is dissolved, and class hydroxylcontaining materials
What organic phase will affect acidolysis reaction in acid hemolysis process cause acidolysis insufficient, increases subsequent insoluble matter instead.
Another No. 201610948999.1 patents propose a kind of " life of high-concentration water-soluble nitrophosphate fertilizer appropriate
Production method " proposes addition resin adsorption process, to reach the metal ions such as the calcium and magnesium aluminium removed in solution in preparation, keeps away
Exempt from the phosphatic deposit buildup of calcium and magnesium ferro-aluminum；Although reducing obtained fertilizer metal salt insoluble matter by adsorbing exchange, by
Based on reversible requirement is precipitated in implementation, reaction solution control is acid condition, the oxidation and acidity of nitric acid under acid condition
Catalysis makes resin activity radical oxidation and catalytic decomposition；Resin activity group in actual implementation is caused to be used for exchange adsorption calcium and magnesium aluminium
Iron efficiency is extremely low, also easily generates organic resin constituent in fertilizer, and insoluble matter eradicating efficacy is not clearly.
Summary of the invention
The main purpose of the present invention is to provide a kind of nitrophosphate fertilizer preparation methods of low water insoluble matter content, it is intended to reduce
Insolubles content in nitrophosphate fertilizer product promotes the water solubility of fertilizer.
To achieve the above object, the nitrophosphate fertilizer of low water insoluble matter content provided by the invention, water is insoluble in nitrophosphate fertilizer
The weight ratio that object accounts for nitrophosphate fertilizer is less than or equal to 0.2%, and the weight of the acid non-soluble substance in water-insoluble accounts for water-insoluble weight
Ratio is less than or equal to 50%.
Preferably, the acid non-soluble substance includes silica and calcium sulfate.
Preferably, the nitrophosphate fertilizer includes ammonium nitrate, ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate, calcium monohydrogen phosphate, phosphorus
One of acid dihydride calcium is a variety of.
Preferably, the water content in nitrophosphate fertilizer is lower than 2%, and nitrophosphate fertilizer is graininess.
The nitrophosphate fertilizer of low water insoluble matter content of the invention, by the content of insoluble matter in control acid hydrolysis solution and insoluble
The size of object particle, can influence the content of the insoluble matter in subsequent fertilizer product, and product has preferably water-soluble.
The present invention further also proposes that the preparation method of the nitrophosphate fertilizer of the above low water insoluble matter content, method include as follows
Step:
Phosphorus ore raw material nitric acid solution is obtained into phosphorus ore acid hydrolysis slurry；
Phosphorus ore acid hydrolysis slurry is separated by solid-liquid separation, acid hydrolysis solution is obtained, the condition that is separated by solid-liquid separation guarantees that the acid in acid hydrolysis solution is insoluble
Object content accounts for weight ratio≤5% of acid hydrolysis solution；
The acid hydrolysis solution is subjected to freezing and crystallizing and obtains crystallization nitric acid calcium precipitate, separation crystallization nitric acid calcium precipitate obtains decalcification
Mother liquor；
The decalcification mother liquor is neutralized with alkaline matter, obtains neutralizing mother liquor,
Mother liquor will be neutralized to be separated by solid-liquid separation, obtain and neutralize mother liquid filtrate,
It mother liquid filtrate will be neutralized is concentrated and is heated up and melting and be granulated, and obtain the described in any item nitre of claim 1-5
Sour phosphate fertilizer.
Preferably, mother liquor will be neutralized to be separated by solid-liquid separation, obtains and neutralizes mother liquid filtrate, the condition of separation of solid and liquid guarantees to neutralize
Solid content in mother liquid filtrate is lower than 0.1%.
Preferably, by the alkaline matter be the solution comprising ammonium ion, potassium hydroxide, sodium hydroxide, liquefied ammonia, ammonium hydroxide or
One of ammonia is a variety of.
Preferably, the diameter of particle neutralized in mother liquid filtrate is less than 0.8 μm.
Preferably, mother liquor will be neutralized to carry out being separated by solid-liquid separation filter device used being plate filter, plate filter
The filter medium number of plies is not less than 18 layers.
Preferably, by the pH of neutralized mother liquor less than 7.
The content for starching insoluble matter in control acid hydrolysis solution when separating in the present invention by original acidolysis, eliminates the parent nucleus of sediment
On the one hand amount inhibits the amount of mutual adsorpting aggregation generation precipitating between insoluble microparticle in subsequent process, on the other hand can reduce
Insoluble matter suspended particulates own growth degree, to reduce the insolubles content in the nitrophosphate fertilizer of preparation；Product has more
Good water solubility.Wherein, the weight ratio that water-insoluble accounts for nitrophosphate fertilizer in the nitrophosphate fertilizer product finally prepared is less than or equal to
0.2%, the ratio that wherein acid non-soluble substance accounts for water-insoluble is less than or equal to 50%.
Specific embodiment
The realization, the function and the advantages of the object of the present invention will further illustrate in conjunction with the embodiments.It should be appreciated that herein
Described specific embodiment is only used to explain the present invention, is not intended to limit the present invention.
The present invention provides a kind of nitrophosphate fertilizer preparation method of low water insoluble matter content, for using phosphorus ore be raw material produce with
Nitrophosphate fertilizer product is prepared, method and step includes:
Phosphorus ore raw material nitric acid solution is obtained phosphorus ore acid hydrolysis slurry by S10；And be separated by solid-liquid separation phosphorus ore acid hydrolysis slurry, it obtains
Obtain acid non-soluble substance and acid hydrolysis solution；
S20, by acid hydrolysis solution, freezing and crystallizing obtains crystallization nitric acid calcium precipitate under low temperature, and separation crystallization calcium nitrate obtains decalcification
Mother liquor；
S30 neutralizes decalcification mother liquor with alkaline matter, obtains neutralizing mother liquor.
Wherein, rate-determining steps S10 is separated by solid-liquid separation the acid in condition guarantee acid hydrolysis solution not in whole implementation in the present invention
Molten object content accounts for weight ratio≤5% of acid hydrolysis solution.
The content for starching insoluble matter in control acid hydrolysis solution when separating in the present invention by original acidolysis, eliminates the parent nucleus of sediment
On the one hand amount inhibits the amount of mutual adsorpting aggregation generation precipitating between insoluble microparticle in subsequent process, on the other hand can reduce
Insoluble matter suspended particulates own growth degree, to reduce the insolubles content in the nitrophosphate fertilizer of preparation.
Wherein, the alkaline matter of step S30 is the solution comprising ammonium ion, potassium hydroxide, sodium hydroxide, liquefied ammonia, ammonium hydroxide
Or one of ammonia or a variety of.
It can further include after step S30:
Step S40 is separated by solid-liquid separation the neutralization mother liquor of step S30, obtains mother liquid filtrate and insoluble matter precipitating, solid-liquid
Isolated condition guarantees that insolubles content is lower than 0.1% in mother liquid filtrate after guaranteeing separation.
Simultaneously in order to guarantee isolated quality, the step of being separated by solid-liquid separation packet is starched to phosphorus ore acid hydrolysis during step S10
It includes:
Phosphorus ore acid hydrolysis slurry is first placed in subsider and carries out settlement treatment, obtains supernatant and sediment by S11；
S12, then supernatant is passed through plate filter and is filtered, collection filtrate is acid hydrolysis solution.
By the initial gross separation and fine separation of the two steps, the content of acid non-soluble substance in acid hydrolysis solution then can control
Account for weight ratio≤2% of acid hydrolysis solution.The sedimentation time of step S11 controls 2~3 hours, and sedimentation is abundant.
Meanwhile further for subsequent insoluble matter particle growth size is reduced, the amount of insoluble matter is reduced, is gone back in step S10
The diameter of particle of acid non-soluble substance is less than 0.8 μm in control acid hydrolysis solution that can be profound；By the partial size for inhibiting primary particle
Size can influence the amount that the mutual flocculating setting of subsequent insoluble matter forms insoluble precipitating.Equally, the neutralization that step S30 is obtained is female
Diameter of particle in liquid filtrate is less than 0.8 μm.
The diameter of particle of the acid non-soluble substance of certain step S10 can by the aperture of the filter medium of plate filter come
Control, by the filtration media pore diameters of the step S12 plate filter used less than 0.8 μm, while the filter medium number of plies is not less than
18 layers；Can then guarantee it is subsequent obtain acidolysis slurry in insoluble matter particle partial size and be in require size.
The condition that the control of step S10 insoluble matter particle meets, it is subsequent to generate in step s 30 and in the process largely
Bulky grain insoluble matter precipitating, then the operation of step S40 being separated by solid-liquid separation to neutralization mother liquor, can will neutralize mother liquor and carry out
Being separated by solid-liquid separation filter device used is that plate filter mode carries out, and filtration media pore diameters are less than 0.8 μm, the filter medium number of plies
Not less than 18 layers.Meanwhile based on the usual working condition for reducing metal salt precipitate and generating, with ammonia to de- in step S30 implementation
When mother liquor of calcium carries out neutralization reaction, the pH control of reaction system is acidic environment, i.e. addition alkaline matter is anti-into reaction system
At once, stop being added when system pH reaches 5~7, that is, control the pH of neutralized mother liquor less than 7；It prevents from generating under alkaline system
It is irreversible to precipitate.The alkaline matter for wherein being used to be neutralized may include the solution, potassium hydroxide, hydroxide of ammonium ion
One of sodium, liquefied ammonia, ammonium hydroxide or ammonia are a variety of.
The process of low temperature decalcification includes: the acidolysis liquid cooling after being first separated by solid-liquid separation phosphorus ore acid hydrolysis liquid in the implementation of step S20
But it arrives temperature to be crystallized for -10 DEG C~0 DEG C, 60~85% calcium nitrate is with Ca (NO3)2·4H2O crystal form is precipitated；Then
Again cooling solution is subjected to vacuum filter at -2~1 DEG C, then obtains decalcification mother liquor.By first under the conditions of determining temperature
Freeze pre-crystallized precipitation, after under conditions of -2~1 DEG C the mode of vacuum filter promote the condensation and precipitation of crystal grain, to mention
It rises and removes ca efficiency.
Fertilizer finished product preparation after step S40 further include:
The mother liquid filtrate of step S40 is concentrated step S50, and pelletizer granulation is added after being warming up to molten condition, obtains
Nitrophosphate fertilizer.
The present invention also proposes the nitrophosphate fertilizer prepared by the nitrophosphate fertilizer preparation method of above-mentioned low water insoluble matter content,
It can by the content of the insoluble matter in control acid hydrolysis solution and the size of insoluble matter particle using above-mentioned preparation method of the invention
To influence the content of the insoluble matter in subsequent fertilizer product, product has preferably water-soluble.Wherein, guarantee that low water-insoluble contains
The weight ratio that water-insoluble accounts for nitrophosphate fertilizer in the nitrophosphate fertilizer product of amount is less than or equal to 0.2%, and wherein acid non-soluble substance accounts for water not
The ratio of molten object is less than or equal to 50%.
Certainly, according to the raw material of preparation and technique, acid non-soluble substance includes silica and calcium sulfate.
Final prepared nitrophosphate fertilizer includes ammonium nitrate, ammonium phosphate, ammonium hydrogen phosphate, ammonium dihydrogen phosphate, calcium monohydrogen phosphate, phosphorus
One of acid dihydride calcium is a variety of.
In order to guarantee the quality of fertilizer, the water content in nitrophosphate fertilizer is lower than 2%.
To make the nitrophosphate fertilizer preparation method details of the above-mentioned low water insoluble matter content of the present invention be more conducive to those skilled in the art
The understanding and implementation of member, and the verifying water-soluble effect of this case nitrophosphate fertilizer, come below by way of specific embodiment to this case
Above content be illustrated.
Embodiment 1
S10 will be added to acid according to stoichiometry 1.1:1 with the nitric acid of concentration 58% and mid low grade phosphate rock (100kg)
It carries out abundant acidolysis in solution slot, obtains phosphorus ore acid hydrolysis slurry (solid content is about 1.8% after measurement)；
The phosphorus ore acid hydrolysis slurry that step S10 acidolysis obtains is placed in subsider after carrying out sedimentation 3h, is separated by solid-liquid separation by S11
To supernatant and sediment；
S12, the supernatant that step S11 is obtained carry out refined filtration by plate filter.
S20, it is -5 DEG C that the acid hydrolysis solution of step S12, which is cooled to temperature, and cooling solution is then carried out vacuum mistake at 0 DEG C
Filter obtains decalcification mother liquor.
S30 is added gas ammonia into decalcification mother liquor and carries out neutralization reaction, obtains and neutralize mother liquor；And it is controlled in neutralization reaction anti-
Answering the pH of solution is 5.0.
S40 carries out filters pressing to the neutralization mother liquor of step S30, obtains mother liquid filtrate and insoluble matter precipitating.
The mother liquid filtrate of step S40 is concentrated into mass concentration >=97.5%, and is added after being warming up to molten condition by S50
Pelletizer is granulated, and obtains nitrophosphate fertilizer particle.
In order to verify the quality and effect of nitrophosphate fertilizer particle of the invention, the nitrophosphate fertilizer particle of preparation is subjected to water
It is molten, water insoluble matter content is measured, water-insoluble will be obtained and carry out acidolysis, measure the content of acid non-soluble substance.
In the nitrophosphate fertilizer particle of above-described embodiment 1, water insoluble matter content is.0.153%, acid non-soluble substance content is
0.068%.
The color of the nitrophosphate fertilizer particle prepared by embodiment 1 is whiter, and solution rate is fast in water, precipitates invisible
The conveyance conduit and spray hole of nitrophosphate fertilizer aqueous solution are not blocked, and the acid non-soluble substance content in water-insoluble is low, fertilizer solution acid
Still invisible precipitating after property.
And the fertiliser granulates that water-insoluble is exceeded, particulate matter sedimentation, and dissolved color are had in pipeline after dissolution
It is partially deep, illustrate that the fertilizer of the embodiment of the present invention has excellent water-soluble effect.
Embodiment 1 is repeated, adjustment neutralizes the pH value of mother liquor, and pH value is neutralized female within the scope of 4-7 by filtering
Liquid can realize that water insoluble matter content is lower than 0.2% in nitrophosphate fertilizer particle, and the amount of acid non-soluble substance accounts for the amount of water-insoluble
Ratio is lower than 50%.When pH is 6-7, the filter residue that neutralization mother liquor is obtained by filtration can be relatively more, because there is more phosphate in pH
Can be not soluble in water in the case where height, the yield of fertilizer can be relatively low, but the water-insoluble not influenced in nitrophosphate fertilizer particle contains
Amount and acid non-soluble substance content.
The above is only a preferred embodiment of the present invention, is not intended to limit the scope of the invention, all to utilize this hair
Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks
Domain is included within the scope of the present invention.
Claims (10)
1. a kind of nitrophosphate fertilizer of low water insoluble matter content, which is characterized in that water-insoluble accounts for nitrophosphate fertilizer in nitrophosphate fertilizer
Weight ratio is less than or equal to 0.2%, and the ratio that the weight of the acid non-soluble substance in water-insoluble accounts for water-insoluble weight is less than or equal to
50%.
2. nitrophosphate fertilizer according to claim 1, which is characterized in that the acid non-soluble substance includes silica and sulfuric acid
Calcium.
3. nitrophosphate fertilizer according to claim 1, it is characterised in that the nitrophosphate fertilizer includes ammonium nitrate, ammonium phosphate, phosphorus
One of sour hydrogen ammonium, ammonium dihydrogen phosphate, calcium monohydrogen phosphate, calcium dihydrogen phosphate are a variety of.
4. nitrophosphate fertilizer according to claim 1, it is characterised in that the water content in nitrophosphate fertilizer is lower than 2%, nitric acid phosphorus
Fertilizer is graininess.
5. the preparation method of the nitrophosphate fertilizer of the described in any item low water insoluble matter contents of claim 1-4, which is characterized in that side
Method includes the following steps:
Phosphorus ore raw material nitric acid solution is obtained into phosphorus ore acid hydrolysis slurry；
Phosphorus ore acid hydrolysis slurry is separated by solid-liquid separation, acid hydrolysis solution is obtained, separation of solid and liquid condition guarantees that the acid non-soluble substance in acid hydrolysis solution contains
Amount accounts for weight ratio≤5% of acid hydrolysis solution；
The acid hydrolysis solution is subjected to freezing and crystallizing and obtains crystallization nitric acid calcium precipitate, it is female that separation crystallization nitric acid calcium precipitate obtains decalcification
Liquid；
The decalcification mother liquor is neutralized with alkaline matter, obtains neutralizing mother liquor,
Mother liquor will be neutralized to be separated by solid-liquid separation, obtain and neutralize mother liquid filtrate,
It mother liquid filtrate will be neutralized is concentrated and is heated up and melting and be granulated, and obtain the described in any item nitric acid phosphorus of claim 1-5
Fertilizer.
6. the fertile preparation method of the nitric acid phosphorus of low water insoluble matter content as claimed in claim 5, which is characterized in that female by neutralizing
Liquid is separated by solid-liquid separation, and is obtained and is neutralized mother liquid filtrate, and the condition of separation of solid and liquid guarantees that the solid content neutralized in mother liquid filtrate is lower than
0.1%.
7. the nitrophosphate fertilizer preparation method of low water insoluble matter content as claimed in claim 5, which is characterized in that by the alkalinity
Substance is one of the solution comprising ammonium ion, potassium hydroxide, sodium hydroxide, liquefied ammonia, ammonium hydroxide or ammonia or a variety of.
8. such as the nitrophosphate fertilizer preparation method of the described in any item low water insoluble matter contents of claim 5-7, which is characterized in that institute
The diameter of particle in neutralization mother liquid filtrate is stated less than 0.8 μm.
9. the nitrophosphate fertilizer preparation method of low water insoluble matter content as claimed in claim 5, which is characterized in that mother liquor will be neutralized
It carries out being separated by solid-liquid separation filter device used being plate filter, the filter medium number of plies of plate filter is not less than 18 layers.
10. the nitrophosphate fertilizer preparation method of low water insoluble matter content as claimed in claim 5, which is characterized in that will be neutralized
The pH of mother liquor is less than 7, it is preferred that the pH for neutralizing mother liquor is 3-6.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486595A (en) * | 2009-02-25 | 2009-07-22 | 天脊煤化工集团股份有限公司 | Technological process for producing high concentration nitric-phosphate fertilizer |
| CN102351590B (en) * | 2011-07-18 | 2013-07-24 | 贵州省化工研究院 | Method for producing high-water solubility nitrophosphate fertilizer by phosphorite nitrolysis and calcium nitrate freezing |
| CN104107585A (en) * | 2014-07-03 | 2014-10-22 | 贵州省化工研究院 | Method for reinforced separation of acid-insoluble substances during decomposition of phosphate rock with nitric acid |
| CN105198503A (en) * | 2015-10-26 | 2015-12-30 | 天脊煤化工集团股份有限公司 | System and method for increasing nitric phosphate product P2O5 dissolvability in water |
-
2018
- 2018-10-17 CN CN201811207938.5A patent/CN109251062A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101486595A (en) * | 2009-02-25 | 2009-07-22 | 天脊煤化工集团股份有限公司 | Technological process for producing high concentration nitric-phosphate fertilizer |
| CN102351590B (en) * | 2011-07-18 | 2013-07-24 | 贵州省化工研究院 | Method for producing high-water solubility nitrophosphate fertilizer by phosphorite nitrolysis and calcium nitrate freezing |
| CN104107585A (en) * | 2014-07-03 | 2014-10-22 | 贵州省化工研究院 | Method for reinforced separation of acid-insoluble substances during decomposition of phosphate rock with nitric acid |
| CN105198503A (en) * | 2015-10-26 | 2015-12-30 | 天脊煤化工集团股份有限公司 | System and method for increasing nitric phosphate product P2O5 dissolvability in water |
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