CN106518222B - A kind of viscosity reducing process of Phosphate Fertilizer Nitrate with Frozen Method neutralize slip - Google Patents
A kind of viscosity reducing process of Phosphate Fertilizer Nitrate with Frozen Method neutralize slip Download PDFInfo
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- CN106518222B CN106518222B CN201610949066.4A CN201610949066A CN106518222B CN 106518222 B CN106518222 B CN 106518222B CN 201610949066 A CN201610949066 A CN 201610949066A CN 106518222 B CN106518222 B CN 106518222B
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- mother liquor
- resin
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- calcium
- nitrate
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B3/00—Fertilisers based essentially on di-calcium phosphate
Abstract
A kind of viscosity reducing process of Phosphate Fertilizer Nitrate with Frozen Method neutralize slip, the viscosity reducing process is on the basis of Phosphate Fertilizer Nitrate with Frozen Method process flow, increase resins exchange process, to remove the calcium and magnesium ferro-aluminum metal ion in defluorinate mother liquor, achievees the purpose that neutralization mother liquor slurry viscosity reduction；Present approach reduces the viscosity of neutralize slip, and low-cost, easy to operate, without secondary pollution, products obtained therefrom good physical and chemical, water-soluble strong, wide adaptation range meets the needs of water-fertilizer integral.
Description
Technical field
The present invention relates to a kind of production methods of high-concentration water-soluble nitrophosphate fertilizer, especially a kind of to utilize low-grade phosphate ore
Produce the viscosity reducing process of high-concentration water-soluble nitrophosphate fertilizer neutralize slip.
Technical background
Phosphate Fertilizer Nitrate with Frozen Method production technology is one kind using nitric acid, phosphorus ore and ammonia as raw material, is produced after chilled crystallization
The production technology of nitrophosphate fertilizer, such as Jing Hongjian, the north Chen Mingliang, Chen Jingyu etc. Phosphate Fertilizer Nitrate with Frozen Method production technology [M]
Capital: Chemical Industry Press, 2002, production procedure includes phosphorus ore acid hydrolysis, acid non-soluble substance precipitation and separation, freezing and crystallizing, nitric acid
Calcium filtering, mother liquid ammonia neutralization, neutralize slip evaporation, biaxial granulation, drying and cooling technique, while in order to which by-product is effectively treated
Calcium nitrate also has calcium nitrate treatment process and digests the cement plant of byproduct.Such resulting nitrophosphate fertilizer of production technology
As a kind of high-concentration phosphate compound fertilizers, because of its good physical property and agricultural effect, and it is widely used in cereal crops and economy
Crop production, it is deep in agricultural production to be liked.But recently as the continuous decline of phosphorus ore grade, calcium iron magnalium etc. in phosphorus ore
The content of metal constantly rises, so that when by neutralization step, a series of liquid phase chemistry can occur with ammonia for slurry anti-
It answers, generates a large amount of spawn, lead to steeply rising for neutralize slip viscosity, bring very big difficulty to neutralization operation, very
The stage that can not be operated may extremely be reached, system is caused to be forced to stop, be less able to satisfy the requirement of high-tower granulation.So not only
Great economic loss, a large amount of manpower and material resources of consumption can be brought to will have a direct impact on nitrophosphate fertilizer for cleaning equipment
It is normal production and product quality.Therefore more and more people begin to focus on neutralize phosphoric acid variation and influence because
Element, such as it is existing report [Pan Peihua influence neutralize slip viscosity the reason of simply analyse [J] chemical fertilizer industry, 1999,6 (26):
43-45] and [Campbell G R, Leong Y K, Berndt C C, et al. Ammonium phosphate
slurry rheology and particle properties—the influence of Fe (III) and Al
(III) impurities, solid concentration and degree of neutralization[J].
Chemical engineering science, 2006,61 (17): 5856-5866.], report Ca, Mg and Fe in phosphorus ore
The improvement situation of slurry viscosity after influence of the metal ions such as aluminium to neutralize slip viscosity, and removal, but there is no so far
A kind of open source literature report for removing the metal ions such as Ca, Mg and Fe aluminium and reducing phosphoric acid.
Summary of the invention
The invention solves concrete technical problems be how to eliminate Ca, Mg and Fe aluminum metal ion pair neutralize slip in phosphorus ore
The influence of viscosity, the purpose is to provide a kind of viscosity reducing process of Phosphate Fertilizer Nitrate with Frozen Method neutralize slip.
To solve the above-mentioned problems and purpose is achieved through the following technical solutions.
A kind of viscosity reducing process of Phosphate Fertilizer Nitrate with Frozen Method neutralize slip, the viscosity reducing process are that Phosphate Fertilizer Nitrate with Frozen Method is raw
Neutralization mother liquor during production controls reaction temperature, reaction time and reaction environment, removal neutralizes female through resins exchange process
Calcium and magnesium ferro-aluminum metal ion in liquid reduces slurry viscosity；
The resins exchange process follows these steps to carry out:
1) resin adsorption
It is 1000 mm that mother liquor, which will be neutralized, and be placed in diameter by top-feed mouth, and potassium type resin layer height is the tree of 2000 mm
In Ester exchange tower, using calcium, magnesium, aluminium and the iron ion in the potassium ion and mother liquor in resin mother liquid flow rate be 2-6 BV/h,
Temperature is 30-60 DEG C, and pH value react 2-4 hours under conditions of being 4-6, progress ion exchange, calcium, magnesium in mother liquor to be neutralized,
When aluminium and iron ion removing rate respectively reach 90%, 80%, 70% and 80%, neutralize slip is flowed out by resin exchange tower bottom discharge port
And it is sent into neutralization step；
2) resin regeneration
After resin exchange tower adsorption saturation, by the neutralization mother liquor discharge port for neutralizing mother liquor feed opening and its bottom at top
It closes, while potassium nitrate solution being passed into resin exchange tower by the regeneration feed opening of resins exchange tower bottom, it is full to absorption
Potassium type resin with after is 10-20% in nitric acid potassium concn；The dosage of potassium nitrate is 0.7-0.9 times of phosphorus ore quality；Temperature is
It is reacted 3-6 hours under conditions of 10-40 DEG C, the calcium of potassium type resin adsorption, magnesium, iron and aluminium ion is cemented out into shape by potassium ion
At regenerated liquid, a portion is back in resin exchange tower as returning charge reacts potassium type resin, and another part is sent to
Calcium ammonium nitrate production process；Exist in liquid to be regenerated without calcium, magnesium, iron and aluminium plasma, closes regenerated liquid inlet and outlet, open and neutralize
Mother liquor feed opening recycles the resin adsorption process in previous step.
Wherein, the resin exchange tower is to be provided with three, wherein a main pair one is standby.
Realize a kind of viscosity reducing process of Phosphate Fertilizer Nitrate with Frozen Method neutralize slip provided by aforementioned present invention, central scope
It is by the neutralization mother liquor in Phosphate Fertilizer Nitrate with Frozen Method production process through resins exchange process, the original being exchanged with each other using interionic
Reason, by controlling reaction temperature, reaction time and the reaction environment of process, to remove the gold such as the calcium and magnesium ferro-aluminum neutralized in mother liquor
Belong to ion, to achieve the purpose that reduce slurry viscosity.
Compared with prior art, major advantage with have the active effect that first is that be utilized resins exchange method eliminate it is de-
Calcium and magnesium ferro-aluminum metal ion in fluorine mother liquor, reduces the viscosity of slurry, reduce subsequent neutralization step produce load and
Difficulty, it is low-cost, it is easy to operate；It is relatively independent, have a style of one's own second is that increased resins exchange production process method is simple, very
It is easy to realize technological transformation on existing Phosphate Fertilizer Nitrate with Frozen Method device；Third is that the potassium type tree utilized in resins exchange process
Rouge not only ensure that the removal to calcium and magnesium ferro-aluminum plasma in slurry, but also to introduce in neutralize slip crop growth necessary
Potassium ion, to improve the fertilizer and utilization scope of product；Fourth is that resulting neutralize slip viscosity is small after resins exchange, it is miscellaneous
Matter is few, and water-soluble strong, with its neutralized resulting nitrophosphate fertilizer product good physical and chemical, wide adaptation range can facilitate crop
Punching applies, trickle irrigation, top dressing, soilless cultivation etc., meets the needs of water-fertilizer integral.
Detailed description of the invention
Fig. 1 is the integrated artistic flow diagram of this viscosity reducing process.
Fig. 2 is the resins exchange flow diagram of this viscosity reducing process.
Fig. 3 be this viscosity reducing process resins exchange to the adsorption effect of calcium and magnesium ferro-aluminum with the variation table figure of mother liquor viscosity.
In figure: 1-phosphorus ore；2- nitric acid；3-acidolysis reactions；4-precipitation and separations；5- acid non-soluble substance；6-freezing and crystallizings；
The filtering of 7-nitre calcium；8-calcium nitrate；9-mother liquors；10-potassium nitrate；11-mother liquor defluorinates；12- is separated by solid-liquid separation；13-fluosilicic acid
Potassium；14-resins exchanges；15-nitric acid；16-mother liquors neutralize；17-nitric acid；18-ammonias；The evaporation of 19-slurries；20-make
Grain；21-is dry, cooling；22-water-soluble nitrophosphate fertilizers；23-resin regeneration liquid；The conversion of 24-nitre calcium.
Specific embodiment
A specific embodiment of the invention is made further instructions below.
Implement the present invention it is above-mentioned provided by a kind of viscosity reducing process of Phosphate Fertilizer Nitrate with Frozen Method neutralize slip, be
On the basis of the process flow of existing Phosphate Fertilizer Nitrate with Frozen Method production, be separated by solid-liquid separation 12 in mother liquor and 16 two
Resins exchange 14 is had additional between process, attached drawing 3 is shown in process flow.Nitric acid 2 and phosphorus ore 1 are stoichiometrically added in acidolysis slot
Acidolysis reaction 3 is carried out, the acid non-soluble substance 5 in acid hydrolysis solution is separated through precipitation and separation 4, then by isolated acid non-soluble substance 5
Acid hydrolysis solution is sent into freezing and crystallizing 6, and the calcium nitrate 8 after chilled crystallization is precipitated from acid hydrolysis solution and enters calcium nitrate filtering 7 and carries out
It is separated by solid-liquid separation, gained liquid is mother liquor 9；Mother liquor 9 will be through 11 process of mother liquor defluorinate and mother liquor before going to resins exchange 14
12 processes are separated by solid-liquid separation, the mother liquor 9 from calcium nitrate filtering 7 is sent in mother liquor defluorinate slot, are carried out by addition potassium nitrate 10
Mother liquor defluorinate reacts the fluosilicic acid ion in mother liquor 9 with potassium ion and generates the crystallization of potassium fluosilicate 13, will by separation of solid and liquid 12
System is discharged in potassium fluosilicate 13, is sent into resins exchange 14 in gained defluorinate with mother liquor, utilizes the ion exchange function of potassium type resin
It can be by the potassium ion exchange of calcium, magnesium, iron, aluminium ion and resin in mother liquor, wherein eliminating calcium, magnesium, iron, aluminum ions neutralization
Slurry is sent in mother liquor and 16 processes, and ammonia 18 and ammonium nitrate 17 is added in N-process according to the technique of Phosphate Fertilizer Nitrate with Frozen Method
Neutralization 16, evaporation 19 are carried out to mother liquor, are granulated 20, dry cooling 21, to obtain NPK nitrophosphate fertilizer, in the process we
To exchange resin method to the mother liquor after the removal rate of each metal ion species and removal metal ion in N-process medium viscosity
Variation is determined.Furthermore the potassium type resin of adsorption saturation then carries out 23 process of resin regeneration, with potassium nitrate to adsorption saturation
Potassium type resin afterwards is rinsed and impregnates, and the calcium of resin adsorption, magnesium, iron, aluminium ion are cemented out with potassium ion and formed again
Raw liquid 23 is sent to nitre calcium and converts 24 processes.
It is further illustrated below by specific embodiment.
Embodiment 1
The quality index of the phosphorus ore 1 of the present embodiment: P2O5 31.2%、CaO 44.4%、F 2.8%、AI 13.2%、 Fe2
(Al2O)3Amount to 2.5%, other impurities；The concentration of nitric acid 2 is 58%.
Stoichiometrically 1.2:1 is added to progress acidolysis reaction 3 in acidolysis slot for nitric acid 2 and phosphorus ore 1, and the acid in acid hydrolysis solution is insoluble
Object 5 is separated through precipitation and separation 4, and the acid hydrolysis solution for being completely separated acid non-soluble substance 5 is then sent into freezing and crystallizing 6, chilled
Crystallization calcium nitrate 8 is precipitated from acid hydrolysis solution and enters calcium nitrate filtering 7 and is separated by solid-liquid separation, and gained liquid is mother liquor 9, then
Mother liquor 9 is sent in mother liquor defluorinate slot 11, mother liquor defluorinate is carried out by addition potassium nitrate 10, makes the fluosilicic acid ion in mother liquor 9
It is reacted with potassium ion and generates potassium fluosilicate crystallization 13, process reaction condition is 10-50 DEG C of reaction temperature, and the reaction time, 0.5-1 was small
When, the additional amount of potassium nitrate according to potassium nitrate and fluosilicic acid molar ratio are as follows: KNO3/H2SiF6=2-4, wherein potassium fluosilicate is through solid
System is discharged after liquid separation 12, and is then sent into resins exchange 14 in defluorinate with mother liquor, utilizes the ion exchange function of potassium type resin
Can by mother liquor calcium, magnesium, iron, aluminium ion and resin potassium ion exchange, process reaction condition is that temperature is 40 DEG C, when reaction
Between 3 hours, pH value 5,4 BV/h of mother liquid flow rate；Calcium, magnesium, iron, aluminum ions neutralize slip is wherein eliminated to be sent in mother liquor
With 16 processes, according to Phosphate Fertilizer Nitrate with Frozen Method technique N-process be added ammonia 18 and ammonium nitrate 17 mother liquor is carried out in and
16, evaporation 19, be granulated 20, dry cooling 21, to obtain nitrophosphate fertilizer, wherein in neutralization step ammonia additive amount and phosphorus ore
Mass ratio is 0.10-0.18, and the additive amount and phosphorus ore quality ratio of ammonium nitrate are 0.05-0.70；We are to resin in the process
Exchange process to the mother liquor after the removal rates of each metal ion species and removal metal ion N-process medium viscosity variation into
It has gone measurement, has as a result seen attached list Fig. 3.Furthermore the potassium type resin of adsorption saturation then carries out 23 process of resin regeneration, with potassium nitrate pair
Potassium type resin after adsorption saturation is rinsed and impregnates, and the calcium of potassium type resin adsorption, magnesium, iron, aluminium ion are set with potassium ion
It swaps out to form regenerated liquid 23, is sent to nitre calcium and converts 24 processes.Step for regeneration reaction condition is nitric acid potassium concn 10%, potassium nitrate
Dosage be 0.8 times, 20 DEG C of temperature, the reaction time 4 hours of phosphorus ore quality.
Embodiment 2
The quality index of the phosphorus ore 1 of the present embodiment and the difference of embodiment one, quality index are as follows: P2O532.5%, CaO
47%, F 2.9%, AI 6.0%, Fe2(Al2O)32.2% is amounted to, other impurities；The concentration of nitric acid 2 is 58%.
Stoichiometrically 1.2:1 is added to progress acidolysis reaction 3 in acidolysis slot for nitric acid 2 and phosphorus ore 1, and the acid in acid hydrolysis solution is insoluble
Object 5 is separated through precipitation and separation 4, and the acid hydrolysis solution for being completely separated acid non-soluble substance 5 is then sent into freezing and crystallizing 6, chilled
Crystallization calcium nitrate 8 is precipitated from acid hydrolysis solution and enters calcium nitrate filtering 7 and is separated by solid-liquid separation, and gained liquid is mother liquor 9, then
Mother liquor 9 is sent in mother liquor defluorinate slot 11, mother liquor defluorinate is carried out by addition potassium nitrate 10, makes the fluosilicic acid ion in mother liquor 9
It is reacted with potassium ion and generates potassium fluosilicate crystallization 13, process reaction condition is 10-50 DEG C of reaction temperature, and the reaction time, 0.5-1 was small
When, the additional amount of potassium nitrate according to potassium nitrate and fluosilicic acid molar ratio are as follows: KNO3/H2SiF6=2-4, wherein potassium fluosilicate is through solid
System is discharged after liquid separation 12, and is then sent into resins exchange 14 in defluorinate with mother liquor, utilizes the ion exchange function of potassium type resin
Can by mother liquor calcium, magnesium, iron, aluminium ion and resin potassium ion exchange, process reaction condition is that temperature is 30 DEG C, when reaction
Between 2 hours, pH value 4,5 BV/h of mother liquid flow rate；Calcium, magnesium, iron, aluminum ions neutralize slip is wherein eliminated to be sent in mother liquor
With 16 processes, according to Phosphate Fertilizer Nitrate with Frozen Method technique N-process be added ammonia 18 and ammonium nitrate 17 mother liquor is carried out in and
16, evaporation 19, be granulated 20, dry cooling 21, to obtain nitrophosphate fertilizer, wherein in neutralization step ammonia additive amount and phosphorus ore
Mass ratio is 0.10-0.18, and the additive amount and phosphorus ore quality ratio of ammonium nitrate are 0.05-0.70；We are to resin in the process
Exchange process to the mother liquor after the removal rates of each metal ion species and removal metal ion N-process medium viscosity variation into
It has gone measurement, has as a result seen attached list Fig. 3.Furthermore the potassium type resin of adsorption saturation then carries out 23 process of resin regeneration, with potassium nitrate pair
Potassium type resin after adsorption saturation is rinsed and impregnates, and the calcium of potassium type resin adsorption, magnesium, iron, aluminium ion are set with potassium ion
It swaps out to form regenerated liquid 23, it is sent to nitre calcium and converts 24 processes.Step for regeneration process reaction condition is nitric acid potassium concn 20%, nitre
The dosage of sour potassium is 0.7 times, 10 DEG C of temperature, the reaction time 5 hours of phosphorus ore quality.
Claims (2)
1. a kind of viscosity reducing process of Phosphate Fertilizer Nitrate with Frozen Method neutralize slip, the viscosity reducing process is to produce Phosphate Fertilizer Nitrate with Frozen Method
Neutralization mother liquor in the process controls reaction temperature, reaction time and reaction environment through resins exchange process, and removal neutralizes mother liquor
In calcium and magnesium ferro-aluminum metal ion, reduce slurry viscosity；
The resins exchange process follows these steps to carry out:
1) resin adsorption
It is 1000 mm that mother liquor, which will be neutralized, and be placed in diameter by top-feed mouth, and the resin that potassium type resin layer height is 2000 mm is handed over
Change in tower, using calcium, magnesium, aluminium and the iron ion in the potassium ion and mother liquor in resin mother liquid flow rate be 2-6 BV/h, temperature
Be 30-60 DEG C, pH value react 2-4 hours under conditions of being 4-6, progress ion exchange, calcium, magnesium, aluminium in mother liquor to be neutralized and
When iron ion removing rate respectively reaches 90%, 80%, 70% and 80%, neutralize slip is flowed out and is sent by resin exchange tower bottom discharge port
Enter neutralization step；
2) resin regeneration
After resin exchange tower adsorption saturation, the neutralization mother liquor discharge port for neutralizing mother liquor feed opening and its bottom at top is closed
It closes, while potassium nitrate solution being passed into resin exchange tower by the regeneration feed opening of resins exchange tower bottom, to adsorption saturation
Potassium type resin afterwards is 10-20% in nitric acid potassium concn；The dosage of potassium nitrate is 0.7-0.9 times of phosphorus ore quality；Temperature is 10-
It is reacted 3-6 hours under conditions of 40 DEG C, the calcium of potassium type resin adsorption, magnesium, iron and aluminium ion is cemented out by potassium ion and formed
Regenerated liquid, a portion is back in resin exchange tower as returning charge reacts potassium type resin, and another part is sent to nitre
Sour ammonium calcium production process；Exist in liquid to be regenerated without calcium, magnesium, iron and aluminium plasma, closes regenerated liquid inlet and outlet, it is female to open neutralization
Liquid feed opening recycles the resin adsorption process in previous step.
2. viscosity reducing process according to claim 1, the resin exchange tower is to be provided with three, wherein a main pair one
It is standby.
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| CN112624805A (en) * | 2021-01-06 | 2021-04-09 | 贵州芭田生态工程有限公司 | Method for reducing viscosity of nitric phosphate neutralized slurry and application |
| CN114455984A (en) * | 2022-02-14 | 2022-05-10 | 太原理工大学 | Production process for effectively inhibiting degradation of water-soluble phosphorus in nitrophosphate fertilizer neutralization slurry by freezing method |
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| CN101486595B (en) * | 2009-02-25 | 2011-03-30 | 天脊煤化工集团股份有限公司 | Technological process for producing high concentration nitric-phosphate fertilizer |
| CN102924128B (en) * | 2012-07-04 | 2014-09-10 | 天脊煤化工集团股份有限公司 | Neutralization apparatus for nitric phosphate fertilizer production mother liquid ammonia neutralization process |
| CN102731191B (en) * | 2012-07-04 | 2014-07-16 | 太原理工大学 | Neutralization process for ammonia in a mother liquor used for producing nitric acid phosphate fertilizer |
| CN103073344B (en) * | 2013-01-23 | 2014-10-15 | 天脊煤化工集团股份有限公司 | Production method for high-concentration defluorinate nitronitrogen phosphorus and potassium compound fertilizer |
| CN103288495A (en) * | 2013-05-16 | 2013-09-11 | 陈和平 | Method for carrying out stage treatment on reaction slurry |
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