CN104230429A - Powdered water-soluble NPK composite fertilizer and preparation method thereof - Google Patents

Powdered water-soluble NPK composite fertilizer and preparation method thereof Download PDF

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Publication number
CN104230429A
CN104230429A CN201310242997.7A CN201310242997A CN104230429A CN 104230429 A CN104230429 A CN 104230429A CN 201310242997 A CN201310242997 A CN 201310242997A CN 104230429 A CN104230429 A CN 104230429A
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composite fertilizer
phosphoric acid
ammonium
soluble
preparation
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CN201310242997.7A
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张运森
褚红艳
王欣欣
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Shenzhen Batian Ecotypic Engineering Co Ltd
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Shenzhen Batian Ecotypic Engineering Co Ltd
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Abstract

The invention is applicable to the technical field of fertilizers and provides a powdered water-soluble NPK composite fertilizer and a preparation method thereof. The preparation method of the powdered water-soluble NPK composite fertilizer comprises the following steps: concentrating phosphoric acid by furnace process, introducing ammonia gas to react to generate a part of polyphosphate, performing spray-drying, screening and mixing with at least one of nitrogen salt and sylvite to obtain the powdered water-soluble NPK composite fertilizer. The powdered water-soluble composite fertilizer contains elements N and K as well as polyphosphate, and when the element P is measured in a form of P2O5 and the element K is measured in the form of K2O and the total mass of the composite fertilizer is 100%, the mass percentage of P2O5 is greater than or equal to 15%, and the mass percentage of the polyphosphate is greater than or equal 5% of the total mass of total phosphate. By adopting the powdered water-soluble NPK composite fertilizer, the problem that a water-soluble fertilizer is short in fertilizer efficiency period and not easy to transport and the problem that a composite fertilizer containing ammonium polyphosphate is complex in process are effectively solved.

Description

A kind of pulverulent water-soluble NPK composite fertilizer and preparation method thereof
Technical field
The invention belongs to technical field of fertilizers, particularly relate to a kind of pulverulent water-soluble NPK composite fertilizer and preparation method thereof.
Background technology
Water soluble fertilizer is a kind of emerging fertilizer, and relative to conventional fertilizers, Water soluble fertilizer has the following advantages: completely water-soluble, quick-acting is strong, is beneficial to plant absorption and makes full use of; Fertilization mode variation, can carry out spraying, drip irrigation, soil irrigation, soilless culture and foliage-spray etc.But, due to Water soluble fertilizer in soil very easily dissolve cause run off, ageing poor, can not preserve for a long time in soil, therefore Effects of Fertilization Frequency is higher.In recent years, the application of ammonium polyphosphate in fertilizer is subject to the attention of domestic people gradually.Easily run off to solve Water soluble fertilizer, the problem of poor in timeliness, mainly at present adopt the method for adding ammonium polyphosphate, but be mainly liquid fertilizer containing the fertilizer of ammonium polyphosphate.And liquid fertilizer is comparatively large by region limitations affect, be applicable to using nearby, transport at a distance, storage cost are higher, are difficult to universal utilization.
Summary of the invention
An object of the embodiment of the present invention is to provide a kind of pulverulent water-soluble composite fertilizer, is intended to the poor in timeliness solving current Water soluble fertilizer, Liquid Fertilizer not easily transports, stores the problems such as inconvenience.
Another object of the embodiment of the present invention is the preparation method providing a kind of pulverulent water-soluble composite fertilizer, is intended to solve the problem that inconvenient, the existing ammonium polyphosphate compound fertilizer technology of liquid fertilizer transport is complicated, cost is high.
In order to realize the object of foregoing invention, technical scheme of the present invention is as follows:
A kind of pulverulent water-soluble NPK composite fertilizer, containing N, K element, described composite fertilizer is also containing poly-phosphate, and P element is with P 2o 5meter, K element is with K 2o counts, in the total mass of compound manure for 100%, and wherein N, P 2o 5, K 2mass percentage>=45% of the total amount of O, described P 2o 5mass percentage>=15%, described poly-phosphate accounts for mass percentage>=5% of total phosphate total amount.
And a kind of preparation method of pulverulent water-soluble NPK composite fertilizer, comprises the following steps:
Mix after Phosphoric Acid Concentration with ammonia, obtain the mixture slip of phosphoric acid one ammonium and ammonium polyphosphate through thermal response;
Described slip is carried out atomization drying, screening processes the mixture powder obtaining phosphoric acid one ammonium and ammonium polyphosphate;
Carry out mixing treatment by after the material screening containing N, K element with described mixture powder, obtain the pulverulent water-soluble NPK composite fertilizer containing ammonium polyphosphate, wherein said mixture powder accounts for percent mass mark >=30% of finished product.
The water-soluble composite fertilizer of powdery containing ammonium polyphosphate that the embodiment of the present invention provides, good water solubility, nutrient content are high, and wherein, poly-phosphate accounts for mass percentage >=5% of total phosphate total amount, and the fertilizer efficiency time is long, and purity is high.The preparation method of the pulverulent water-soluble composite fertilizer containing ammonium polyphosphate that the embodiment of the present invention provides is with short production cycle, technique is simply controlled.
Accompanying drawing explanation
Fig. 1 is the technological process of production sketch of the pulverulent water-soluble composite fertilizer that the embodiment of the present invention provides.
Embodiment
In order to make the technical problem to be solved in the present invention, technical scheme and beneficial effect clearly understand, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiments provide a kind of preparation method of pulverulent water-soluble NPK composite fertilizer, comprise the following steps:
S01. mix after Phosphoric Acid Concentration with ammonia, obtain the mixture slip of phosphoric acid one ammonium and ammonium polyphosphate through thermal response;
S02. described slip is carried out atomization drying, screening processes the mixture powder obtaining phosphoric acid one ammonium and ammonium polyphosphate;
S03. carry out mixing treatment by after the material screening containing N, K element with described mixture powder, obtain the pulverulent water-soluble NPK composite fertilizer containing ammonium polyphosphate, wherein said mixture powder accounts for percent mass mark >=30% of finished product.
Particularly, as preferred embodiment, in described step S01 after Phosphoric Acid Concentration and ammonia blending means be phosphoric acid after concentration evaporator is concentrated, the ammonia mixing post-heating pumping into reactor He pass into.Wherein, the preferred thermal phosphoric acid of described phosphoric acid, mass percent >=50%, phosphoric acid quality percentage ratio >=85% after concentrated, described reactor is unrestricted, and the embodiment of the present invention preferably uses tubular reactor.
Thermal response described in above-mentioned steps S01, due to the volatile escape of ammonia, therefore in order to make up the ammonia loss vapored away, adds excess of ammonia gas at reactor.As concrete preferred embodiment, NH during charging in reactor 3with P 2o 5mol ratio is (1.0-1.8): 1.As concrete preferred embodiment, after concentrated in tubular reactor during charging, the flow of phosphoric acid is 5-12t/h; The flow of ammonia is 0.7-1.6t/h.
In above-mentioned steps S01, obtained the mixture slip of phosphoric acid one ammonium and ammonium polyphosphate by thermal response.The ammonium polyphosphate of to be the polymerization degree the be 3-8 of ammonium polyphosphate described in the embodiment of the present invention.Because poly-phosphate directly can not be absorbed by plant, but the ammonium phosphate salt that slowly hydrolysis, gradually release directly can be absorbed by plant in soil.Therefore, ammonium polyphosphate, as poly-phosphate composition main in composite fertilizer described in the embodiment of the present invention, is the important component effectively solving the short problem of composite fertilizer's fertilizer efficiency period.And the temperature and time of thermal response described in the embodiment of the present invention is larger to the content influence of ammonium polyphosphate in reaction product.Therefore the poly-phosphate fertilizer of different content is produced by controlling thermal response temperature and time.Repeatedly study discovery through contriver, when thermal response temperature is 180 DEG C-280 DEG C, the content being obtained by reacting ammonium polyphosphate is higher.
As concrete preferred embodiment, in this step S01, when thermal response prepares the mixture slip of phosphoric acid one ammonium and ammonium polyphosphate, generating portion may contain the steam of said mixture simultaneously, now need the mixture slip obtained to be separated with steam, be separated preferred vapour separator and be separated.Dropped in slurry vessel by slip after being separated, the steam separated, after water washing, flow to recycle again in reactor.Adopt water to carry out washing and recycling to steam, the water soluble component on the one hand in steam is recycled, and can improve the overall yield of thermal response, on the other hand, water can reuse in the reactor, reduces production cost.
In above-mentioned steps S02, in order to obtain drying, uniform mixture powder, need to carry out atomization drying process to the mixture slip of above-mentioned phosphoric acid one ammonium obtained in S01 and ammonium polyphosphate.Its detailed process is: slip carries out atomization process by spray-drying tower, forms drop, increases moisture evaporation area.Drop slip forms mixture powder after warm air drying, falls at the bottom of spray-drying tower.The mixture slip of phosphoric acid one ammonium and ammonium polyphosphate can obtain the mixture powder of uniform drying fast through spraying dry.Wherein, in spray-drying process, the mixture slip of phosphoric acid one ammonium and ammonium polyphosphate can polymerization reaction take place further, thus improves the content of poly-phosphate, extends the fertilizer efficiency period of fertilizer.Repeatedly study discovery through contriver, when the temperature of warm air drying process is 200-300 DEG C, spray-dired efficiency is high, effective, simultaneously can provide a good temperature environment for phosphatic polymerization.
During spray drying treatment, tower top can produce the tail gas containing dust, and containing the phosphoric acid salt dust that a large amount of particle diameter is tiny in tail gas, account for the 1-3% of phosphoric acid salt total amount, dust content is 1.5-3g/m 3.In order to improve productive rate, avoid polluting surrounding enviroment, the embodiment of the present invention is by tail gas after cyclonic separator is separated, and recovery part be bonded in phosphate powder, gas fraction carries out entering air after dust removal process through sack cleaner simultaneously.
The mixture powder of phosphoric acid one ammonium obtained after spray-dried and ammonium polyphosphate is carried out cooling, sieving process, the mixture powder of screening particle diameter≤20 object phosphoric acid one ammonium and ammonium polyphosphate.Mixture particle diameter being greater than 20 object phosphoric acid one ammoniums and ammonium polyphosphate, as returning charge, adds slurry vessel with phosphoric acid one ammonium in step S02, again carries out mist projection granulating after melting together with the mixture slip of ammonium polyphosphate.
In described step S03, in order to the described raw material containing N, K element is mixed with mixture powder, need the raw material containing N, K element to carry out screening process before mixing, filter out size≤20 object raw material.Particle diameter is greater than 20 object raw materials as returning charge, returning charge mixes after fragmentation again, screening, and wherein, described mixture powder accounts for percent mass mark >=30% of finished product.Of course it is to be understood that natural needed to carry out break process before screening if containing the raw material of N, K element for time block.In addition, what meet other different-grain diameter specifications of Different Crop demand in this area contains ammonium polyphosphate composite fertilizer and preparation method thereof, also in protection scope of the present invention.
In step S03, the described raw material containing N, K element is the raw material containing at least one in nitrogen salt and at least one in sylvite.Wherein said nitrogen salt is at least one in ammonium nitrate, ammonium sulfate, urea, is more preferably ammonium nitrate; Described sylvite is at least one in potassium sulfate, Repone K.As preferred embodiment, described nitrogen salt and sylvite are at least one at least one in ammonium nitrate or ammonium sulfate or urea and potassium sulfate or Repone K.Of course it is to be understood that in this area other phosphoric acid salt, nitrogen salt, sylvite and the ratio of mixture thereof that can be used for preparing the above-mentioned powdery composite fertilizer containing ammonium polyphosphate, also within protection scope of the present invention.
The concrete operations technical process of above-mentioned pulverulent water-soluble NPK composite fertilizer preparation method is shown in shown in accompanying drawing 1.
The preparation method of the pulverulent water-soluble NPK composite fertilizer that the embodiment of the present invention provides, after concentrated, pass into ammonia gas react by thermal phosphoric acid and generate a part of poly-phosphate, technique is simply controlled, with low cost, adjust the relative content of poly-phosphate by temperature and time when regulating thermal response and drying, thus extend the fertilizer efficiency period of composite fertilizer.
Correspondingly, the embodiment of the present invention additionally provides a kind of pulverulent water-soluble NPK composite fertilizer, and containing N, K element, in addition, described composite fertilizer is also containing poly-phosphate, and P element is with P 2o 5meter, K element is with K 2o counts, in the total mass of compound manure for 100%, and wherein N, P 2o 5, K 2mass percentage>=45% of the total amount of O, described P 2o 5mass percentage>=15%, described poly-phosphate accounts for mass percentage>=5% of total phosphate total amount.
In described pulverulent water-soluble NPK composite fertilizer, feed compositions is nitrogen, phosphorus and potassium.In above-mentioned composite fertilizer, each composition can carry out adjustment according to the fertile specification of different composite and carry out satisfied different need of production, but, be 100%, N, P in the total mass of compound manure 2o 5, K 2mass percentage>=45% of the total amount of O, P 2o 5mass percent>=15%.
In described pulverulent water-soluble NPK composite fertilizer, in order to obtain the sizeable powdered fertilizer of uniform particle sizes, surface-area and quality, the particle diameter of above-mentioned water-soluble NPK composite fertilizer is preferably≤20 orders.
Above-mentioned pulverulent water-soluble NPK composite fertilizer can but not only adopt the preparation method of pulverulent water-soluble NPK composite fertilizer mentioned above to be prepared.
Containing poly-phosphate in above-mentioned pulverulent water-soluble NPK composite fertilizer.Described poly-phosphate comprises the poly-phosphate that the micro-complexing of ammonium polyphosphate and phosphoric acid salt and other is polymerized.The slow hydrolysis of poly-phosphate can extend the nitrogenous fertilizer time limit of composite fertilizer on the one hand effectively, on the other hand, when the amount of application increase of poly-phosphate even reaches common phosphatic 4 times, its orthophosphoric acid salt concentration that slowly hydrolysis discharges also is not enough to cause plant leaf surface to be burnt, thus the nitrogenous fertilizer preventing single-dose application from too much causing burns seedling, also can avoid the groundwater pollution phenomenon that excessive use of fertilizer causes.Described poly-phosphate accounts for total water-soluble phosphoric acid salts contg and can regulate according to different plant, the demand of different growing stages to nitrogenous fertilizer, but mass percent needs >=5%.
The pulverulent water-soluble NPK composite fertilizer that the embodiment of the present invention provides is solid composite fertilizer, and this composite fertilizer's good water solubility, nutrient content are high, fertilizer efficiency period limit for length, purity are high, and is convenient to transport and stores.
Embodiment one: nitre sulfenyl 15-15-15 composite fertilizer
Thermal phosphoric acid is after concentration evaporator is concentrated, and pass into Hybrid Heating in tubular reactor with the ammonia of the flow of the flow of 10t/h and 0.9t/h, temperature of reaction is 180 DEG C-280 DEG C, is obtained by reacting slip and the steam of monoammonium phosphate and ammonium polyphosphate simultaneously;
Slip after separate vapour, returning charge are passed in slurry vessel, then by slip by spray-drying tower, after atomization, slip drop and hot blast cross, and fall at the bottom of tower after drying, then cold front heavy rain, screening at the bottom of tower, obtain phosphate powder.
Solid material, after crusher in crushing, screening, enters mixing machine with ammonium nitrate 15.1t/h flow, potassium sulfate with the flow of 11.6t/h and mixes with above-mentioned phosphate powder, be then packaged to be compound manure.
Finally carry out nitrogen content, phosphorus content and granule strength to composite fertilizer to measure, record composite fertilizer's nitrogen content 15%, containing Vanadium Pentoxide in FLAKES amount 15%, be 15% containing potassium oxide amount, poly-phosphate content is 15%.
Embodiment two: nitre sulfenyl 10-20-20
Identical with the step of embodiment one, wherein concentrated rear phosphoric acid flow is 12t/h; The flow of ammonia is 1t/h.
To in mixing machine during reinforcing body raw material in step (3): potassium sulfate adds with the flow of 14.1t/h, and ammonium nitrate adds with the flow of 9.76t/h.
Finally carry out nitrogen content, phosphorus content and granule strength to composite fertilizer to measure, record composite fertilizer's nitrogen content 10%, containing Vanadium Pentoxide in FLAKES amount 20%, be 20% containing potassium oxide amount, poly-phosphate content is 15%.
Embodiment three: nitre chloro 15-15-15
Identical with the step of embodiment one, wherein concentrated rear phosphoric acid flow is 8t/h; The flow of ammonia is 0.8t/h.
To in mixing machine during reinforcing body raw material in step (3): Repone K adds with the flow of 8.2t/h, and ammonium nitrate adds with the flow of 15t/h.
Finally carry out nitrogen content, phosphorus content and granule strength to composite fertilizer to measure, record composite fertilizer's nitrogen content 10%, containing Vanadium Pentoxide in FLAKES amount 15%, be 15% containing potassium oxide amount, poly-phosphate content is 25%.
In embodiment one to three, the mensuration of composite fertilizer's phosphorus content adopts the method for the GB8573-2010 mensuration of available phosphorus content " in the composite fertilizer ", the mensuration of nitrogen content adopts GB8572-2010 " mensuration of determination of total nitrogen in compound fertilizer ", and poly-phosphate content adopts GB9984-2004 " phosphoric acid salt that industrial tripoly phosphate sodium STPP ion exchange column chromatography method separation determination is multi-form ".
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (9)

1. a preparation method for pulverulent water-soluble NPK composite fertilizer, comprises the following steps:
Mix after Phosphoric Acid Concentration with ammonia, obtain the mixture slip of phosphoric acid one ammonium and ammonium polyphosphate through thermal response;
Described slip is carried out atomization drying, screening processes the mixture powder obtaining phosphoric acid one ammonium and ammonium polyphosphate;
Carry out mixing treatment by after the material screening containing N, K element with described mixture powder, obtain the pulverulent water-soluble NPK composite fertilizer containing ammonium polyphosphate, wherein said mixture powder accounts for percent mass mark >=30% of finished product.
2. the preparation method of pulverulent water-soluble NPK composite fertilizer as claimed in claim 1, is characterized in that: described concentrated rear phosphoric acid carries out mixing with the flow of 5-12t/h, ammonia with the flow of 0.7-1.6t/h and carries out thermal response.
3. the preparation method of pulverulent water-soluble NPK composite fertilizer as claimed in claim 1 or 2, is characterized in that: in the mixture slip step preparing phosphoric acid one ammonium and ammonium polyphosphate, and described concentrated rear phosphoric acid is with P 2o 5meter, described ammonia and P 2o 5mol ratio be (1.0-1.8): 1.
4. the preparation method of pulverulent water-soluble NPK composite fertilizer as claimed in claim 1, is characterized in that: in the mixture slip step preparing phosphoric acid one ammonium and ammonium polyphosphate, described thermal response temperature is 180-280 DEG C.
5. the preparation method containing pulverulent water-soluble NPK composite fertilizer as claimed in claim 1, is characterized in that: in the step of mixture powder preparing phosphoric acid one ammonium and ammonium polyphosphate, the temperature of described atomization drying process is 200-300 DEG C.
6. the preparation method of pulverulent water-soluble NPK composite fertilizer as claimed in claim 1, is characterized in that: in the step of mixing treatment, and the described raw material containing N, K element comprises the raw material of at least one in nitrogenous salt and at least one in sylvite.
7. the preparation method of the pulverulent water-soluble NPK composite fertilizer as described in claim 1 or 6, is characterized in that: described nitrogen salt is at least one in ammonium nitrate, ammonium sulfate, urea; Described sylvite is at least one in potassium sulfate, Repone K.
8. the preparation method of pulverulent water-soluble NPK composite fertilizer as claimed in claim 1, is characterized in that: described concentrated after phosphoric acid quality percentage composition >=85%.
9. a pulverulent water-soluble NPK composite fertilizer, containing N, K element, is characterized in that: described composite fertilizer is also containing poly-phosphate, and P element is with P 2o 5meter, K element is with K 2o counts, in the total mass of compound manure for 100%, and wherein N, P 2o 5, K 2mass percentage>=45% of the total amount of O, described P 2o 5mass percentage>=15%, described poly-phosphate accounts for mass percentage>=5% of total phosphate total amount.
CN201310242997.7A 2013-06-18 2013-06-18 Powdered water-soluble NPK composite fertilizer and preparation method thereof Pending CN104230429A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105272477A (en) * 2015-11-17 2016-01-27 深圳市芭田生态工程股份有限公司 Water-soluble ammonium polyphosphate NPK compound fertilizer and preparation method thereof
CN105481582A (en) * 2015-12-31 2016-04-13 王丰登 Method for spray drying production of powdery multi-element water-soluble fertilizer
CN105669285A (en) * 2015-12-22 2016-06-15 南开大学 Preparation method for high-water-solubility ammonium polyphosphate-potassium sulfate fertilizer
CN105858704A (en) * 2015-04-01 2016-08-17 贵州芭田生态工程有限公司 A method of preparing a polyphosphate composite fertilizer through decomposing phosphate rock with nitric acid
CN108409394A (en) * 2018-04-27 2018-08-17 武汉工程大学 Complete water-soluble monoammonium phosphate or diammonium phosphate fertilizer and its preparation
CN114380632A (en) * 2020-10-22 2022-04-22 贵州芭田生态工程有限公司 NP and NPK fertilizer containing polyphosphate and water-soluble calcium and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1083916A (en) * 1964-03-30 1967-09-20 Armour & Co Improvements in or relating to ammonium phosphate and the production thereof
GB1598507A (en) * 1977-03-16 1981-09-23 Fertilizers & Chemicals Ltd Solid ammonium polyphosphate compositions and method for the manufacture thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1083916A (en) * 1964-03-30 1967-09-20 Armour & Co Improvements in or relating to ammonium phosphate and the production thereof
GB1598507A (en) * 1977-03-16 1981-09-23 Fertilizers & Chemicals Ltd Solid ammonium polyphosphate compositions and method for the manufacture thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105858704A (en) * 2015-04-01 2016-08-17 贵州芭田生态工程有限公司 A method of preparing a polyphosphate composite fertilizer through decomposing phosphate rock with nitric acid
CN105272477A (en) * 2015-11-17 2016-01-27 深圳市芭田生态工程股份有限公司 Water-soluble ammonium polyphosphate NPK compound fertilizer and preparation method thereof
CN105669285A (en) * 2015-12-22 2016-06-15 南开大学 Preparation method for high-water-solubility ammonium polyphosphate-potassium sulfate fertilizer
CN105481582A (en) * 2015-12-31 2016-04-13 王丰登 Method for spray drying production of powdery multi-element water-soluble fertilizer
CN108409394A (en) * 2018-04-27 2018-08-17 武汉工程大学 Complete water-soluble monoammonium phosphate or diammonium phosphate fertilizer and its preparation
CN114380632A (en) * 2020-10-22 2022-04-22 贵州芭田生态工程有限公司 NP and NPK fertilizer containing polyphosphate and water-soluble calcium and preparation method thereof

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Application publication date: 20141224