CN104230448A - Method for preparing N-P-K (Nitrogen-Phosphorus-Potassium) compound fertilizer by using hydrochloric acid to decompose phosphorite acidified solution - Google Patents
Method for preparing N-P-K (Nitrogen-Phosphorus-Potassium) compound fertilizer by using hydrochloric acid to decompose phosphorite acidified solution Download PDFInfo
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Abstract
The invention discloses a method for preparing an N-P-K (Nitrogen-Phosphorus-Potassium) compound fertilizer by using a hydrochloric acid to decompose a phosphorite acidified solution, relates to a production method of a compound fertilizer, and particularly a method of decomposing phosphorite through industrial by-product hydrochloric acid. The specific technical process provided by the invention comprises: a, phosphorite acidifying; b, defluorination and decalcification of acidified solution; c, ammoniation; d, concentration; and e, adding potassium to pellet to obtain a chlorine-contianing N-P-K compound fertilizer. According to the method provided by the invention, hydrochloric acid can be consumed on a large scale, and the difficult problem of being difficult to use the industrial by-product hydrochloric acid can be effectively solved; furthermore, compared with sulfuric acid, a way of decomposing the phosphorite by hydrochloric acid has the advantages of being fast to react, high in decomposition ratio, wide in range of application of phosphorite raw material, low in cost and the like; in addition, the abundant phosphate rock resources with middle or low grade can be fully utilized in China, the total nutrient of the obtained N-P-K compound fertilizer is not less than 40%, and the N-P-K compound fertilizer can be served as a basic fertilizer for chlorine sensitive crops, therefore the N-P-K compound fertilizer huge in market potential and good in economic benefit.
Description
Technical field
The present invention relates to a kind of production method of composite fertilizer, particularly one utilizes industrial by-product decomposing phosphate rock by chlorhydric acid, and the acid hydrolysis solution obtained is for the preparation of the method for N-P-K composite fertilizer.
Background technology
There is abundant phosphate rock resource in China, reserves are only second to Morocco, occupy second place of the world, but compared with world's concerned countries, it has larger gap in ore quality, washability and Rock Phosphate (72Min BPL) exploitation etc., wherein can be relatively low for the Rock Phosphate (72Min BPL) basic unit price of processing and utilization, only have 40.54 hundred million tons, P
2o
5the rich ore that massfraction is greater than 30% only has 11.08 hundred million tons, and national Rock Phosphate (72Min BPL) P
2o
5average mass fraction only has 17%.In recent years, along with the excessive use of abundant ore source, now increasingly exhausted, how effective exploitation, utilize Mid-and low-grade phosphate rock resources to become particularly important for the Sustainable development of China's sulphur dioxide of phosphor chemical industry.
The hydrochloric acid of industrial production by-product is used for decomposing phosphate rock by the present invention, and the acid hydrolysis solution obtained is through defluorinate, decalcification, and logical ammonia neutralization, adds potassium, granulation produces chloride N-P-K composite fertilizer.The present invention can consume industrial by-product hydrochloric acid on a large scale, and the chloride N-P-K complex fertilizer product added value obtained is high, and economic benefit is good, has important reality and economic implications to effectively utilizing industrial by-product hydrochloric acid and domestic abundant Mid-and low-grade phosphate rock resources.
About the correlative study of decomposing phosphate rock by chlorhydric acid, research history existing very long both at home and abroad, because there is the problem of calcium chloride and phosphoric acid separation difficulty in this route, generally be divided into two lines: one is utilize decomposing phosphate rock by chlorhydric acid, with an organic solvent phosphoric acid by wet process is extracted, and then through back extraction, evaporation, concentrated obtain purification of phosphoric acid and reclaim organic solvent, there is the shortcomings such as flow process complexity, investment is large, energy consumption is high in this route; Two is utilize decomposing phosphate rock by chlorhydric acid to produce secondary calcium phosphate, normally adopt in lime slurry or calcium carbonate and acid hydrolysis solution, calcium in acid hydrolysis solution is separated out with the form of secondary calcium phosphate, although this technique flow process is simple, be convenient to control, but also there is a large amount of calcium chloride solutions to be wasted, the problems such as economy is not high.Instant invention overcomes the drawback that above-mentioned operational path exists, with ammonium sulfate as the calcium ion in heavy calcium agent precipitation acid hydrolysis solution, by-product high purity gypsum, the ammonia that ammonium sulfate is brought into enters the finished product, and ammonia does not devalue; Whole process discharge refuse is few, with environmental friendliness; Added value of product is high, can more economical, effectively utilize industrial by-product hydrochloric acid and domestic abundant Mid-and low-grade phosphate rock resources.
Summary of the invention
The object of the invention is to the defect overcoming prior art, provide a kind of hydrochloric acid of industrial production by-product that utilizes as acid hydrolysis solution decomposing phosphate rock, and market potential is huge, added value is high, and effluent discharge is few, with environmental friendliness; Phosphorus, nitrogen recovery high decomposing phosphate rock by chlorhydric acid acid hydrolysis solution prepare the method for N-P-K composite fertilizer.
Decomposing phosphate rock by chlorhydric acid acid hydrolysis solution of the present invention prepares the method for N-P-K composite fertilizer, be achieved in that industrial by-product hydrochloric acid as acid hydrolysis solution decomposing phosphate rock, the acid hydrolysis solution obtained is through defluorinate, decalcification, solid-liquid separation, phosphorous, the nitrogen solution that obtain lead to ammonia neutralization, concentrate, add potassium granulation and produce chloride N-P-K composite fertilizer, concrete grammar is as follows:
A. adopt industrial by-product hydrochloric acid to be used for decomposing phosphate rock as acid hydrolysis solution, phosphorus ore raw material is mid low grade phosphate rock and phosphorus concentrate;
B. acid hydrolysis solution defluorinate after decomposing phosphate rock step a obtained, the solid residue of separating acid insolubles obtains defluorinate acid hydrolysis solution;
C. the defluorinate acid hydrolysis solution obtained by step b adds ammonium sulfate with precipitated calcium ion, crystallization control condition, and what filter generation is solid gypsum, and filtrate is decalcification acid hydrolysis solution;
D. the decalcification acid hydrolysis solution obtained by step c leads to ammonia neutralization, concentrated, adds potassium, granulation produces chloride N-P-K composite fertilizer and solid gypsum;
E. solid gypsum steps d obtained obtains high purity gypsum product through washing, drying treatment;
In step a, phosphorus ore globule size is 1 ~ 5mm, phosphorus ore P
2o
5massfraction is 15% ~ 30%.
In step a, the weight fraction of hydrochloric acid is 20 ~ 35%; Hydrochloric acid consumption is 100 ~ 105% of theoretical amount, temperature of reaction 15 ~ 50 DEG C, reaction times 0.5 ~ 2.0h.
In step b, defluorinating agent is the one in sodium sulfate, sodium-chlor, potassium sulfate, Repone K; Consumption is 50 ~ 80% of theoretical amount; Temperature of reaction is 30 ~ 50 DEG C, and the reaction times is 1.0 ~ 2.5h.
Ammonium sulfate in step c is ammoniumsulphate soln, and its massfraction is 20 ~ 40%, and consumption is sulfate radical and calcium ion mol ratio 0.9-1.2:1 in defluorinate acid hydrolysis solution, and temperature of reaction is 30-60 DEG C, and the reaction times is 1.0-4.0h;
Ammonia used with ammonification in steps d is liquefied ammonia, and potash fertilizer raw material is Repone K.
In steps d, ammonification ammonia used is liquefied ammonia, and neutralization reaction terminal pH is 3.8 ~ 4.2, degree of neutralization 1.0-1.2.
In step e, the condition of vacuum evaporation is temperature 60-80 DEG C, pressure 0.04 ~ 0.08MPa.
In step g, the finished product chloride N-P-K composite fertilizer is granular or powdery.
Method provided by the invention can obtain the water-soluble chloride composite fertilizer of the middle and high concentration meeting CNS (GB15063-2001), and high density refers to total nutrient (N+P
2o
5+ K
2o) content>=40%, water-soluble phosphorus accounts for available phosphorus percentage>=70%; Middle concentration refers to total nutrient (N+P
2o
5+ K
2o) content>=30%, water-soluble phosphorus accounts for available phosphorus percentage>=50%, and product can be used as avoids chlorine farm crop base fertilizer, and market potential is huge, and added value is high; Present method effluent discharge is few, with environmental friendliness; Phosphorus, nitrogen recovery are high, economically can utilize the hydrochloric acid of industrial by-product and domestic abundant Mid-and low-grade phosphate rock resources.
The present invention can consume hydrochloric acid on a large scale, efficiently solve the difficult problem that industrial by-product hydrochloric acid is difficult to utilize, decomposing phosphate rock by chlorhydric acid and sulfuric acid phase ratio, have be swift in response, rate of decomposition is high, phosphorus ore raw material is applied widely, low cost and other advantages, can make full use of the Mid-and low-grade phosphate rock resources of China's abundant accordingly, products obtained therefrom nitrogen-phosphorus-potassium compound fertilizer total nutrient >=40%, can be used as and avoid chlorine farm crop base fertilizer, its market potential is huge, and economic benefit is good.
Accompanying drawing explanation
Fig. 1 is schematic flow sheet of the present invention.
Embodiment
Be described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings.Described embodiment, only for explaining the present invention, and can not be interpreted as limitation of the present invention.
Below in conjunction with embodiment, the present invention is described further, but be not limited to embodiment.
Embodiment 1
A. by P
2o
5content is the ground phosphate rock that 26.84% Rock Phosphate (72Min BPL) is broken for globule size 1mm, washing lotion when being filtered with acidolysis section acid non-soluble substance by industrial by-product hydrochloric acid mixes, be mixed with the hydrochloric acid soln that weight fraction is 25%, above-mentioned hydrochloric acid soln is added acidolysis groove under agitation and ground phosphate rock carries out acidolysis reaction, hydrochloric acid consumption is 100% of theoretical amount, temperature of reaction is 40 DEG C, and the reaction times is 2.0h;
B. under agitation, in step a acidolysis gained slip, add anhydrous sodium sulphate carry out defluorination reaction, its consumption is 60% of theoretical amount, and temperature of reaction is 40 DEG C, and the reaction times is 2.0h, then filters slip, and filtrate is the acid hydrolysis solution through defluorinate process;
C. under agitation, in step b filtration gained filtrate, add weight fraction is that 25% ammoniumsulphate soln carries out heavy calcium reaction, ammonium sulfate consumption is sulfate radical and calcium ion mol ratio 1.0 in acid hydrolysis solution, temperature of reaction is 40 DEG C, reaction times is 2.5h, removes gypsum by solid-liquid separation, and liquid phase is the acid hydrolysis solution after decalcification, gained gypsum 100g wash water/100g gypsum, washing, under 100 DEG C of conditions drying can obtain high purity gypsum product;
D. step c gained acid hydrolysis solution is carried out logical ammonia neutralization, control neutralization reaction terminal pH4.0, degree of neutralization 1.12;
E. by steps d neutralization reaction gained slip in temperature 70 C, under pressure 0.055MPa condition, carry out vacuum evaporation, removing free-water wherein;
F. add Repone K toward step e evaporation concentration gained slip, the nitrogen in adjustment nutrient, phosphorus, potassium proportioning are 17-19-6;
G. step f gained slip is carried out concentrating, granulation, final generation produces chloride N-P-K composite fertilizer.
Embodiment 2
A. by P
2o
5content is the ground phosphate rock that 23.82% Rock Phosphate (72Min BPL) is broken for globule size 5mm, washing lotion when being filtered with acidolysis section acid non-soluble substance by industrial by-product hydrochloric acid mixes, be mixed with the hydrochloric acid soln that weight fraction is 18%, above-mentioned hydrochloric acid soln is added acidolysis groove under agitation and ground phosphate rock carries out acidolysis reaction, hydrochloric acid consumption is 105% of theoretical amount, temperature of reaction is 30 DEG C, and the reaction times is 1.0h;
B. under agitation, in step a acidolysis gained slip, add potassium sulfate carry out defluorination reaction, its consumption is 80% of theoretical amount, and temperature of reaction is 30 DEG C, and the reaction times is 1.0h, then filters slip, and filtrate is the acid hydrolysis solution through defluorinate process;
C. under agitation, in step b filtration gained filtrate, add weight fraction is that 30% ammoniumsulphate soln carries out heavy calcium reaction, ammonium sulfate consumption is sulfate radical and calcium ion mol ratio 1.10 in acid hydrolysis solution, temperature of reaction is 30 DEG C, reaction times is 3.0h, removes gypsum by solid-liquid separation, and liquid phase is the acid hydrolysis solution after decalcification, gained gypsum 150g wash water/100g gypsum, washing, under 90 DEG C of conditions drying can obtain gypsum product;
D. step c gained acid hydrolysis solution is carried out logical ammonia neutralization, control neutralization reaction terminal pH4.2, degree of neutralization 1.18;
E. by steps d neutralization reaction gained slip in temperature 60 C, under pressure 0.07MPa condition, carry out vacuum evaporation, removing free-water wherein;
F. add Repone K toward step e evaporation concentration gained slip, the nitrogen in adjustment nutrient, phosphorus, potassium proportioning are 16-18-6;
G. step f gained slip is carried out concentrating, granulation, final generation produces chloride N-P-K composite fertilizer.
Embodiment 3
A. by P
2o
5content is the ground phosphate rock that 20.35% Rock Phosphate (72Min BPL) is broken for globule size 3mm, washing lotion when being filtered with acidolysis section acid non-soluble substance by industrial by-product hydrochloric acid mixes, be mixed with the hydrochloric acid soln that weight fraction is 20%, above-mentioned hydrochloric acid soln is added acidolysis groove under agitation and ground phosphate rock carries out acidolysis reaction, hydrochloric acid consumption is 103% of theoretical amount, temperature of reaction is 45 DEG C, and the reaction times is 1.5h;
B. under agitation, in step a acidolysis gained slip, add sodium-chlor carry out defluorination reaction, its consumption is 70% of theoretical amount, and temperature of reaction is 45 DEG C, and the reaction times is 1.5h, then filters slip, and filtrate is the acid hydrolysis solution through defluorinate process;
C. under agitation, in step b filtration gained filtrate, add weight fraction is that 35% ammoniumsulphate soln carries out heavy calcium reaction, ammonium sulfate consumption is sulfate radical and calcium ion mol ratio 1.20 in acid hydrolysis solution, temperature of reaction is 60 DEG C, reaction times is 2.0h, removes gypsum by solid-liquid separation, and liquid phase is the acid hydrolysis solution after decalcification, gained gypsum 120g wash water/100g gypsum, washing, under 105 DEG C of conditions drying can obtain gypsum product;
D. step c gained acid hydrolysis solution is carried out logical ammonia neutralization, control neutralization reaction terminal pH3.8, degree of neutralization 1.07;
E. by steps d neutralization reaction gained slip in temperature 80 DEG C, under pressure 0.045MPa condition, carry out vacuum evaporation, removing free-water wherein;
F. add Repone K toward step e evaporation concentration gained slip, the nitrogen in adjustment nutrient, phosphorus, potassium proportioning are 14-16-10;
G. step f gained slip is carried out concentrating, granulation, final generation produces chloride N-P-K composite fertilizer.
Claims (8)
1. decomposing phosphate rock by chlorhydric acid acid hydrolysis solution prepares a method for N-P-K composite fertilizer, it is characterized in that, comprises the following steps:
A. adopt industrial by-product hydrochloric acid to be used for decomposing phosphate rock as acid hydrolysis solution, phosphorus ore raw material is mid low grade phosphate rock and phosphorus concentrate;
B. acid hydrolysis solution defluorinate after decomposing phosphate rock step a obtained, the solid residue of separating acid insolubles obtains defluorinate acid hydrolysis solution;
C. the defluorinate acid hydrolysis solution obtained by step b adds ammonium sulfate with precipitated calcium ion, crystallization control condition, and what filter generation is solid gypsum, and filtrate is decalcification acid hydrolysis solution;
D. the decalcification acid hydrolysis solution obtained by step c leads to ammonia neutralization, concentrated, adds potassium, granulation produces chloride N-P-K composite fertilizer and solid gypsum;
E. solid gypsum steps d obtained obtains high purity gypsum product through washing, drying treatment.
2. a kind of decomposing phosphate rock by chlorhydric acid acid hydrolysis solution according to claim 1 prepares the method for N-P-K composite fertilizer, it is characterized in that: in step a, phosphorus ore globule size is 1 ~ 5mm, phosphorus ore P
2o
5content is 15% ~ 30%.
3. a kind of decomposing phosphate rock by chlorhydric acid acid hydrolysis solution according to claim 1 prepares the method for N-P-K composite fertilizer, it is characterized in that: in step a, the weight fraction of hydrochloric acid is 20 ~ 35%; Hydrochloric acid consumption is 100 ~ 105% of theoretical amount, temperature of reaction 15 ~ 50 DEG C, reaction times 0.5 ~ 2.0h.
4. a kind of decomposing phosphate rock by chlorhydric acid acid hydrolysis solution according to claim 1 prepares the method for N-P-K composite fertilizer, it is characterized in that: in step b, defluorinating agent is the one in sodium sulfate, sodium-chlor, potassium sulfate, Repone K; Consumption is 50 ~ 80% of theoretical amount; Temperature of reaction is 30 ~ 50 DEG C, and the reaction times is 1.0 ~ 2.5h.
5. a kind of decomposing phosphate rock by chlorhydric acid acid hydrolysis solution according to claim 1 prepares the method for N-P-K composite fertilizer, it is characterized in that: the crystallization condition in step c for its massfraction be 20 ~ 40%, consumption is sulfate radical and calcium ion mol ratio 0.9-1.2:1 in defluorinate acid hydrolysis solution, temperature of reaction is 30-60 DEG C, and the reaction times is 1.0-4.0h.
6. a kind of decomposing phosphate rock by chlorhydric acid acid hydrolysis solution according to claim 1 prepares the method for N-P-K composite fertilizer, it is characterized in that: ammonia used with ammonification in steps d is liquefied ammonia, and potash fertilizer raw material is Repone K.
7. a kind of decomposing phosphate rock by chlorhydric acid acid hydrolysis solution according to claim 1 prepares the method for N-P-K composite fertilizer, it is characterized in that: the neutralization reaction terminal pH of steps d is 3.8 ~ 4.2, degree of neutralization 1.0-1.2.
8. a kind of decomposing phosphate rock by chlorhydric acid acid hydrolysis solution according to claim 1 prepares the method for N-P-K composite fertilizer, it is characterized in that: in step e, the condition of vacuum evaporation is temperature 60-80 DEG C, pressure 0.04 ~ 0.08MPa.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104555965A (en) * | 2015-02-11 | 2015-04-29 | 铜陵化学工业集团有限公司 | Method of combined production of multiple phosphates and phosphate fertilizer from low grade phosphate ore |
| CN105272385A (en) * | 2015-11-27 | 2016-01-27 | 宜昌鄂中化工有限公司 | Method for producing magnesium calcium chloride by utilizing phosphate tailing |
| CN105603215A (en) * | 2015-12-30 | 2016-05-25 | 武汉工程大学 | Method using extraction agent and hydrochloric acid acidolysis technology to efficiently leach K, Ca, Mg and P from P and K associated ore |
| CN108046864A (en) * | 2017-11-13 | 2018-05-18 | 兰小春 | Hydrochloric acid decomposes the method and device of low-grade phosphate ore production water soluble composite fertilizer |
| CN108975975A (en) * | 2017-05-31 | 2018-12-11 | 山东红日化工股份有限公司 | A kind of production method of decomposing phosphate rock by chlorhydric acid production amino compound fertilizer |
| CN112745160A (en) * | 2021-01-21 | 2021-05-04 | 瓮福（集团）有限责任公司 | Novel process for preparing NPK compound fertilizer by using phosphogypsum and potassium feldspar |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126742A (en) * | 2011-01-20 | 2011-07-20 | 山东金正大生态工程股份有限公司 | Method for producing chloride-based compound fertilizer and co-producing gypsum through decomposing phosphorite with hydrochloric acid |
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- 2014-10-16 CN CN201410547747.9A patent/CN104230448A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126742A (en) * | 2011-01-20 | 2011-07-20 | 山东金正大生态工程股份有限公司 | Method for producing chloride-based compound fertilizer and co-producing gypsum through decomposing phosphorite with hydrochloric acid |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104555965A (en) * | 2015-02-11 | 2015-04-29 | 铜陵化学工业集团有限公司 | Method of combined production of multiple phosphates and phosphate fertilizer from low grade phosphate ore |
| CN105272385A (en) * | 2015-11-27 | 2016-01-27 | 宜昌鄂中化工有限公司 | Method for producing magnesium calcium chloride by utilizing phosphate tailing |
| CN105603215A (en) * | 2015-12-30 | 2016-05-25 | 武汉工程大学 | Method using extraction agent and hydrochloric acid acidolysis technology to efficiently leach K, Ca, Mg and P from P and K associated ore |
| CN108975975A (en) * | 2017-05-31 | 2018-12-11 | 山东红日化工股份有限公司 | A kind of production method of decomposing phosphate rock by chlorhydric acid production amino compound fertilizer |
| CN108046864A (en) * | 2017-11-13 | 2018-05-18 | 兰小春 | Hydrochloric acid decomposes the method and device of low-grade phosphate ore production water soluble composite fertilizer |
| CN112745160A (en) * | 2021-01-21 | 2021-05-04 | 瓮福（集团）有限责任公司 | Novel process for preparing NPK compound fertilizer by using phosphogypsum and potassium feldspar |
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Application publication date: 20141224 |