CN106518222A - Viscosity reducing method for freezing method nitrophosphate neutralized slurry - Google Patents
Viscosity reducing method for freezing method nitrophosphate neutralized slurry Download PDFInfo
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- CN106518222A CN106518222A CN201610949066.4A CN201610949066A CN106518222A CN 106518222 A CN106518222 A CN 106518222A CN 201610949066 A CN201610949066 A CN 201610949066A CN 106518222 A CN106518222 A CN 106518222A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B3/00—Fertilisers based essentially on di-calcium phosphate
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Abstract
The invention discloses a viscosity reducing method for freezing method nitrophosphate neutralized slurry. According to the viscosity reducing method, on the basis of the freezing method nitrophosphate technological process, a resin exchange procedure is added for removing metal ions of calcium, magnesium, aluminum and iron in defluorinated mother liquor, and the purpose of reducing the viscosity of the neutralized mother liquor slurry is achieved. Through the method, the viscosity of the neutralized slurry is reduced, the cost is low, operation is simple, secondary pollution is avoided, obtained products are good in physical and chemical property, high in water solubility and wide in application range and meet the integration demand of water and fertilizer.
Description
Technical field
The present invention relates to a kind of production method of high-concentration water-soluble nitrophosphate fertilizer, particularly one kind utilizes low-grade phosphate ore
The viscosity reducing process of production high-concentration water-soluble nitrophosphate fertilizer neutralize slip.
Technical background
Phosphate Fertilizer Nitrate with Frozen Method production technology is a kind of with nitric acid, phosphorus ore and ammonia as raw material, is produced after chilled crystallization
The production technology of nitrophosphate fertilizer, such as Jing Hongjian, Chen Mingliang, Chen Jingyu etc. Phosphate Fertilizer Nitrate with Frozen Method production technology [M]. north
Capital：Chemical Industry Press, 2002, its production procedure includes phosphorus ore acid hydrolysis, acid non-soluble substance precipitate and separate, freezing and crystallizing, nitric acid
Calcium filtration, mother liquid ammonia neutralization, neutralize slip evaporation, biaxial granulation, drying and cooling technique, while for effective process by-product
Calcium nitrate, also has the cement plant of calcium nitrate treatment process and digestion side-product.Nitrophosphate fertilizer obtained by this kind of production technology
As a kind of high-concentration phosphate compound fertilizerses, because of its good physical property and agricultural effect, and it is widely used in cereal crops and economy
Crop production, is liked in agricultural production deeply.But recently as the continuous decline of phosphorus ore grade, calcium ferrum magnalium etc. in phosphorus ore
The content of metal constantly rises so that slip can occur a series of liquid phase chemistry with ammonia anti-when through neutralization step
Should, substantial amounts of spawn is generated, and is caused steeply rising for neutralize slip viscosity, very big difficulty is brought to neutralization operation, very
The stage that cannot be operated may be extremely reached, is caused system to be forced to stop, the requirement of high-tower granulation can not be met.So not only
Great economic loss can be brought, substantial amounts of manpower and materials are consumed for cleaning equipment, and can directly influence nitrophosphate fertilizer
Normal production and product quality.Therefore increasing people begin to focus on neutralize phosphoric acid change and affect because
Element, such as existing report [Pan Peihua. the reason for affecting neutralize slip viscosity simply analyses [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 slip viscosity after impact of the metal ions such as aluminum to neutralize slip viscosity, and removal, but there is no so far
It is a kind of to remove the metal ions such as Ca, Mg and Fe aluminum and reduce the open source literature report of phosphoric acid.
The content of the invention
The invention solves the problems that concrete technical problems be how to eliminate Ca, Mg and Fe aluminum metal ion pair neutralize slip in phosphorus ore
The impact of viscosity, its objective is to provide a kind of viscosity reducing process of Phosphate Fertilizer Nitrate with Frozen Method neutralize slip.
In order to solve the above 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 is to give birth to Phosphate Fertilizer Nitrate with Frozen Method
Neutralization mother solution Jing resins exchange operations during product, controlling reaction temperature, response time and reaction environment remove neutralization female
Calcium and magnesium ferro-aluminum metal ion in liquid, reduces slip viscosity；
The resins exchange operation follow these steps to carry out：
1）Resin absorption
Neutralization mother solution is inserted into a diameter of 1000 mm by top-feed mouth, potassium type resin layer height is that the resin of 2000 mm is handed over
Change in tower, be 2-6 BV/h using the calcium in the potassium ion in resin and mother solution, magnesium, aluminum and iron ion in mother liquid flow rate, temperature
For 30-60 DEG C, pH value is to react 2-4 hours under conditions of 4-6, carries out ion exchange, calcium, magnesium, aluminum in mother solution 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 mouth
Enter neutralization step；
2）Resin regeneration
After resin exchange tower adsorption saturation, the neutralization mother solution discharging opening of the neutralization mother solution charge door at top and its bottom is closed
Close, while potassium nitrate solution is passed in resin exchange tower by the regeneration charge door of resins exchange tower bottom, to adsorption saturation
Potassium type resin afterwards is 10-20% in nitric acid potassium concn；0.7-0.9 times for phosphorus ore quality of the consumption of potassium nitrate；Temperature is 10-
3-6 hours are reacted under conditions of 40 DEG C, the calcium of potassium type resin absorption, magnesium, ferrum and aluminium ion are cemented out by potassium ion and is formed
Regenerated liquid, a portion is back in resin exchange tower as returning charge reacts to potassium type resin, and another part is sent to nitre
Sour ammonium calcium production process；Exist without calcium, magnesium, ferrum and aluminum plasma in liquid to be regenerated, close regenerated liquid and import and export, open neutralization female
Liquid charge door, circulates the resin absorption operation in previous step.
Wherein, the resin exchange tower is provided with three, and wherein one master one secondary is standby.
Realize a kind of viscosity reducing process of Phosphate Fertilizer Nitrate with Frozen Method neutralize slip that the invention described above is provided, its central scope
It is by the neutralization mother solution Jing resins exchange operations in Phosphate Fertilizer Nitrate with Frozen Method production process, the original being exchanged with each other using interionic
Reason, by controlling reaction temperature, response time and the reaction environment of operation, to remove the gold such as the calcium and magnesium ferro-aluminum in neutralization mother solution
Category ion, so that reduce the purpose of slip viscosity.
Compared with prior art, major advantage with good effect is：One is that to make use of resins exchange method to eliminate de-
Calcium and magnesium ferro-aluminum metal ion in fluorine mother solution, reduces the viscosity of slip, reduce follow-up neutralization step produce load and
Difficulty, low cost are simple to operate；Two is that increased resins exchange production process method is simple, relatively independent, have a style of one's own, very
Easily technological transformation is realized on existing Phosphate Fertilizer Nitrate with Frozen Method device；Three is the potassium type tree utilized in resins exchange operation
Fat, both ensure that the removal to calcium and magnesium ferro-aluminum plasma in slip, and it was necessary to introduce crop growth in neutralize slip
Potassium ion, so that improve fertilizer and the utilization scope of product；Four be gained after resins exchange neutralize slip viscosity it is little, it is miscellaneous
Matter is few, and water solublity is strong, and with the nitrophosphate fertilizer product good physical and chemical of its neutralized gained, wide accommodation can facilitate crop
Punching is applied, drip irrigation, topdress, soilless culture etc., meet the demand of water-fertilizer integral.
Description of the drawings
Fig. 1 is the integrated artistic schematic flow sheet of this viscosity reducing process.
Fig. 2 is the resins exchange schematic flow sheet 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 change table figure of mother solution viscosity.
In figure：1 phosphorus ore；2- nitric acid；3 acidolysis reactions；4 precipitate and separate；5- acid non-soluble substances；6 freezing and crystallizings；
7 nitre calcium are filtered；8 calcium nitrates；9 mother solutions；10 potassium nitrate；11 mother solution defluorinates；12- solid-liquid separation；13 hexafluosilicic acid
Potassium；14 resins exchange；15 nitric acid；16 mother solutions are neutralized；17 nitric acid；18 ammonias；19 slips evaporate；20 make
Grain；21 are dried, cooling；22 water solublity nitrophosphate fertilizers；23 resin regeneration liquid；24 nitre calcium are converted.
Specific embodiment
Below the specific embodiment of the present invention is made further instructions.
A kind of viscosity reducing process of above-mentioned the provided Phosphate Fertilizer Nitrate with Frozen Method neutralize slip of the present invention is provided, be
On the basis of the technological process of existing Phosphate Fertilizer Nitrate with Frozen Method production, in solid-liquid separation 12 with mother solution and 16 two operations
Between have additional resins exchange 14, accompanying drawing 3 is shown in its technological process.Nitric acid 2 and phosphorus ore 1 are carried out in being stoichiometrically added to acidolysis groove
Acidolysis reaction 3, the 5 Jing precipitate and separate 4 of acid non-soluble substance in acid hydrolysis solution are separated, then by the acidolysis of detached acid non-soluble substance 5
Liquid sends into freezing and crystallizing 6, and the calcium nitrate 8 after chilled crystallization is separated out from acid hydrolysis solution and filters 7 into calcium nitrate carries out solid-liquid
Separate, gained liquid is mother solution 9；Mother solution 9 wanted 11 operation of Jing mother solutions defluorinate and mother solution solid-liquid before resins exchange 14 is gone to
12 operations are separated, the mother solution 9 for filtering 7 from calcium nitrate is sent in mother solution defluorinate groove, mother solution is carried out by adding potassium nitrate 10
Defluorinate, makes the hexafluosilicic acid ion in mother solution 9 generate potassium fluosilicate 13 with potassium ion reaction and crystallizes, by solid-liquid separation 12 by fluorine silicon
Sour potassium 13 discharges system, sends in resins exchange 14 with mother solution in gained defluorinate, will using the ion exchanging function of potassium type resin
The potassium ion of calcium, magnesium, ferrum, aluminium ion and resin in mother solution is exchanged, and wherein eliminates calcium, magnesium, ferrum, aluminum ions neutralize slip
It is sent in mother solution and 16 operations, adds ammonia 18 and ammonium nitrate 17 pairs female according to the technique of Phosphate Fertilizer Nitrate with Frozen Method in N-process
Liquid is neutralized 16, evaporation 19, pelletize 20, is dried cooling 21, and so as to obtain NPK nitrophosphate fertilizers, we are to tree in the process
Change of the Ester exchange method to the mother solution viscosity in N-process after the clearance and removal metal ion of each metal ion species
It is determined.In addition the potassium type resin of adsorption saturation then carries out 23 operation of resin regeneration, with potassium nitrate to adsorption saturation after
Potassium type resin is rinsed and soaks, and cements out and to form regenerated liquid the calcium of resin absorption, magnesium, ferrum, aluminium ion potassium ion
23 are sent to nitre calcium converts 24 operations.
Further illustrate 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)3
Amount to 2.5%, other impurities；The concentration of nitric acid 2 is 58%.
Nitric acid 2 and phosphorus ore 1 stoichiometrically 1.2：1 be added to acidolysis groove in carry out acidolysis reaction 3, it is sour insoluble in acid hydrolysis solution
5 Jing precipitate and separate 4 of thing is separated, and the acid hydrolysis solution for being completely separated acid non-soluble substance 5 is sent into freezing and crystallizing 6 then, chilled
Crystallization calcium nitrate 8 is separated out from acid hydrolysis solution and filters 7 into calcium nitrate carries out solid-liquid separation, and gained liquid is mother solution 9, then
Mother solution 9 is sent in mother solution defluorinate groove 11, mother solution defluorinate is carried out by adding potassium nitrate 10, is made the hexafluosilicic acid ion in mother solution 9
Potassium fluosilicate crystallization 13 is generated with potassium ion reaction, process reaction condition is reaction temperature 10-50 DEG C, and the response time, 0.5-1 was little
When, the mol ratio of the addition of potassium nitrate according to potassium nitrate with hexafluosilicic acid is：KNO3/H2SiF6=2-4, wherein potassium fluosilicate Jing are solid
Liquid discharges system after separating 12, and then sends in resins exchange 14 with mother solution in defluorinate, using the ion exchange work(of potassium type resin
The potassium ion of the calcium in mother solution, magnesium, ferrum, aluminium ion and resin can be exchanged, it is 40 DEG C that process reaction condition is temperature, during reaction
Between 3 hours, pH value is 5,4 BV/h of mother liquid flow rate；Wherein eliminate calcium, magnesium, ferrum, aluminum ions neutralize slip to be sent in mother solution
With 16 operations, ammonia 18 and ammonium nitrate 17 is added to be neutralized mother solution according to the technique of Phosphate Fertilizer Nitrate with Frozen Method in N-process
16th, evaporation 19, pelletize 20, dry cooling 21, so as to obtain nitrophosphate fertilizer, the addition and phosphorus ore of ammonia wherein in neutralization step
Mass ratio is 0.10-0.18, and addition and the phosphorus ore quality ratio of ammonium nitrate are 0.05-0.70；We are to resin in the process
Exchange process to the mother solution after the clearance and removal metal ion of each metal ion species, enter by the change of viscosity in N-process
Go measure, as a result see attached list Fig. 3.In addition the potassium type resin of adsorption saturation then carries out 23 operation of resin regeneration, with potassium nitrate pair
Potassium type resin after adsorption saturation is rinsed and soaks, and the calcium of potassium type resin absorption, magnesium, ferrum, aluminium ion are put with potassium ion
Swap out to form regenerated liquid 23, be sent to nitre calcium and convert 24 operations.Step for regeneration reaction condition be nitric acid potassium concn 10%, potassium nitrate
Consumption be 0.8 times of phosphorus ore quality, 20 DEG C of temperature, 4 hours response time.
Embodiment 2
The quality index of the phosphorus ore 1 of the present embodiment is different from embodiment one, and quality index is：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%.
Nitric acid 2 and phosphorus ore 1 stoichiometrically 1.2：1 be added to acidolysis groove in carry out acidolysis reaction 3, it is sour insoluble in acid hydrolysis solution
5 Jing precipitate and separate 4 of thing is separated, and the acid hydrolysis solution for being completely separated acid non-soluble substance 5 is sent into freezing and crystallizing 6 then, chilled
Crystallization calcium nitrate 8 is separated out from acid hydrolysis solution and filters 7 into calcium nitrate carries out solid-liquid separation, and gained liquid is mother solution 9, then
Mother solution 9 is sent in mother solution defluorinate groove 11, mother solution defluorinate is carried out by adding potassium nitrate 10, is made the hexafluosilicic acid ion in mother solution 9
Potassium fluosilicate crystallization 13 is generated with potassium ion reaction, process reaction condition is reaction temperature 10-50 DEG C, and the response time, 0.5-1 was little
When, the mol ratio of the addition of potassium nitrate according to potassium nitrate with hexafluosilicic acid is：KNO3/H2SiF6=2-4, wherein potassium fluosilicate Jing are solid
Liquid discharges system after separating 12, and then sends in resins exchange 14 with mother solution in defluorinate, using the ion exchange work(of potassium type resin
The potassium ion of the calcium in mother solution, magnesium, ferrum, aluminium ion and resin can be exchanged, it is 30 DEG C that process reaction condition is temperature, during reaction
Between 2 hours, pH value is 4,5 BV/h of mother liquid flow rate；Wherein eliminate calcium, magnesium, ferrum, aluminum ions neutralize slip to be sent in mother solution
With 16 operations, ammonia 18 and ammonium nitrate 17 is added to be neutralized mother solution according to the technique of Phosphate Fertilizer Nitrate with Frozen Method in N-process
16th, evaporation 19, pelletize 20, dry cooling 21, so as to obtain nitrophosphate fertilizer, the addition and phosphorus ore of ammonia wherein in neutralization step
Mass ratio is 0.10-0.18, and addition and the phosphorus ore quality ratio of ammonium nitrate are 0.05-0.70；We are to resin in the process
Exchange process to the mother solution after the clearance and removal metal ion of each metal ion species, enter by the change of viscosity in N-process
Go measure, as a result see attached list Fig. 3.In addition the potassium type resin of adsorption saturation then carries out 23 operation of resin regeneration, with potassium nitrate pair
Potassium type resin after adsorption saturation is rinsed and soaks, and the calcium of potassium type resin absorption, magnesium, ferrum, aluminium ion are put with potassium ion
Swap out to form regenerated liquid 23, it is sent to nitre calcium and converts 24 operations.Step for regeneration process reaction condition be nitric acid potassium concn 20%, nitre
0.7 times for phosphorus ore quality of the consumption of sour potassium, 10 DEG C of temperature, 5 hours response time.
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
During neutralization mother solution Jing resins exchange operations, controlling reaction temperature, response time and reaction environment, remove neutralization mother solution
In calcium and magnesium ferro-aluminum metal ion, reduce slip viscosity；
The resins exchange operation follow these steps to carry out：
1）Resin absorption
Neutralization mother solution is inserted into a diameter of 1000 mm by top-feed mouth, potassium type resin layer height is that the resin of 2000 mm is handed over
Change in tower, be 2-6 BV/h using the calcium in the potassium ion in resin and mother solution, magnesium, aluminum and iron ion in mother liquid flow rate, temperature
For 30-60 DEG C, pH value is to react 2-4 hours under conditions of 4-6, carries out ion exchange, calcium, magnesium, aluminum in mother solution 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 mouth
Enter neutralization step；
2）Resin regeneration
After resin exchange tower adsorption saturation, the neutralization mother solution discharging opening of the neutralization mother solution charge door at top and its bottom is closed
Close, while potassium nitrate solution is passed in resin exchange tower by the regeneration charge door of resins exchange tower bottom, to adsorption saturation
Potassium type resin afterwards is 10-20% in nitric acid potassium concn；0.7-0.9 times for phosphorus ore quality of the consumption of potassium nitrate；Temperature is 10-
3-6 hours are reacted under conditions of 40 DEG C, the calcium of potassium type resin absorption, magnesium, ferrum and aluminium ion are cemented out by potassium ion and is formed
Regenerated liquid, a portion is back in resin exchange tower as returning charge reacts to potassium type resin, and another part is sent to nitre
Sour ammonium calcium production process；Exist without calcium, magnesium, ferrum and aluminum plasma in liquid to be regenerated, close regenerated liquid and import and export, open neutralization female
Liquid charge door, circulates the resin absorption operation in previous step.
2. viscosity reducing process according to claim 1, the resin exchange tower are provided with three, wherein one one pair one of master
It is standby.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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