CN105967164A - Method for preparing high-polymerization-ratio water-soluble ammonium polyphosphate - Google Patents
Method for preparing high-polymerization-ratio water-soluble ammonium polyphosphate Download PDFInfo
- Publication number
- CN105967164A CN105967164A CN201610479295.4A CN201610479295A CN105967164A CN 105967164 A CN105967164 A CN 105967164A CN 201610479295 A CN201610479295 A CN 201610479295A CN 105967164 A CN105967164 A CN 105967164A
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- water
- polymerization
- ammonium polyphosphate
- ammonium phosphate
- carbamide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/38—Condensed phosphates
- C01B25/40—Polyphosphates
- C01B25/405—Polyphosphates of ammonium
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
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- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a method for preparing high-polymerization-ratio water-soluble ammonium polyphosphate, wherein monoammonium phosphate and urea at the molar ratio of (0.8-1.8):1 are added into a reaction kettle, stirred and heated, the temperature of the materials is controlled to 110-180 DEG C, and a condensation reaction is performed to produce high-polymerization-ratio water-soluble ammonium polyphosphate powder. The material used in the method can be ammonium phosphate produced from a wet-process phosphoric acid with high impurity content, a produced powdery solid product of ammonium polyphosphate has a very high polymerization ratio, and the polymerized phosphorus content accounts for more than 95% of the total phosphorus content. The produced powdery solid product of ammonium polyphosphate is excellent in water solubility, the weight of water-insoluble matters is less than 0.1%, the product can be applied in the fields of liquid fertilizers or other fertilizers, and the development of Chinese modern agriculture is greatly promoted.
Description
Technical field
The invention belongs to chemical fertilizer field, be specifically related to a kind of method preparing high aggregate rate water-soluble poly ammonium phosphate.
Background technology
APP is also known as ammonium polyphosphate or polycondensation ammonium phosphate (being called for short APP), and APP is a kind of polyphosphoric acid containing N and P
Salt, by its degree of polymerization can be divided into oligomeric, in poly-and high poly-three kinds, its degree of polymerization more highly-water-soluble is the least, on the contrary then water solublity
The biggest.Can be divided into crystalline and amorphous by its structure, crystalline state APP is long chain water-insoluble salt.
During beginning, APP produces as fire retardant, and APP is nonpoisonous and tasteless, does not produce etchant gas, moisture absorption
Property little, heat stability is high, is the non-halogen fire retardant of a kind of function admirable.Typically have two kinds of production methods: one be use phosphoric acid-
Carbamide thermal polymerization, another kind is the carbamide thermal polymerization method of ammonium phosphate, and polymerization temperature is about 205-300 DEG C.Prepared by these two kinds of methods
The APP degree of polymerization is higher, it is impossible to use as water soluble fertilizer.
Later, APP had progressed into the production of Chemical Mixed Fertilizer and liquid fertilizer, particularly had obtained extensively should in developed country
With.Early 1970s, the U.S. develops with commodity phosphoric acid by wet process (54%P2O5, mass fraction) and produce APP basis
Liquid fertilizer, namely becomes peroxophosphoric acid by wet-process phosphoric acid concentration, reacts with ammonia in tubular reactor, generates high-concentration polyphosphoric acid
Ammonium, adds water cooling and generates the liquid fertilizer product that grade is 10-34-0.Basis liquid fertilizer can produce liquid compound with nitrogen solution, potash fertilizer etc.
Fertile.
It is generally believed that the APP as Fertilizer application should be that short chain is the most water-soluble, but APP prepared by existing method
The degree of polymerization is higher, water solublity is relatively low, and aggregate rate is relatively low, is not suitable for agricultural.
Summary of the invention
It is an object of the present invention to provide a kind of method preparing high aggregate rate water-soluble poly ammonium phosphate, reduce the degree of polymerization of APP,
Improve aggregate rate and the water solublity of APP, make APP be suitable for agricultural.
The technical scheme is that a kind of method preparing high aggregate rate water-soluble poly ammonium phosphate, by raw material MAP and urine
Element (0.8-1.8) 1 in molar ratio joins in reactor, stirs, heats, and controls temperature of charge 110-180 DEG C, molten state
Material start solidification, formed powdery solid, after having reacted, cooling discharging, obtain high aggregate rate water-soluble poly ammonium phosphate.
Further, the mol ratio of MAP and carbamide is (1.1-1.3) 1, controls temperature of charge and is 140-170 DEG C.
Preferably, the mol ratio of MAP and carbamide is 1.2 1, and controlling temperature of charge is 160 DEG C.
Further, raw material MAP is the MAP that phosphoric acid by wet process prepares, and its N content is 9%-11%, P2O5Content
For 44%-55%.
High aggregate rate water-soluble poly ammonium phosphate finished product degree of polymerization distribution scope obtained by the method for the present invention is 2-5, average degree of polymerization
Being 3.5, for short chain APP, water solublity is high.
Compared with prior art the invention have the advantages that
1, the water-soluble poly ammonium phosphate that present invention MAP, carbamide are produced, the APP powdery solid produced produces
Product aggregate rate is the highest, and the phosphorus content of its polymeric form accounts for total phosphorus content more than 95%.
2, the water-soluble poly ammonium phosphate that present invention MAP, carbamide are produced, the APP powdery solid produced produces
Product water solublity is the highest, and the weight of water-insoluble contained by it is less than 0.1%, can be used for liquid fertilizer or other fertilizer field, can be greatly
The big development promoting China's modern agriculture.
3, raw material MAP selected by the present invention is the MAP that phosphoric acid by wet process prepares, and its N content is 9%-11%, P2O5
Content is 44%-55%, it is possible to be substantially reduced production cost.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is further explained, will be described the preferred forms of the present invention.
Embodiment 1
In special equipment, pour 230Kg MAP and 120Kg carbamide into, open stirring, close special equipment caping, and rise
Temperature, rises to 200 DEG C at temperature of charge, and mixture constantly occurs condensation reaction, releases ammonia, carbon dioxide and steam,
After reaction 90min, finally give APP powdery solid product 250Kg.
Embodiment 2
In special equipment, pour 230Kg MAP and 120Kg carbamide into, open stirring, close special equipment caping, and rise
Temperature, rises to 180 DEG C at temperature of charge, and mixture constantly occurs condensation reaction, releases ammonia, carbon dioxide and steam,
After reaction 120min, finally give APP powdery solid product 261Kg.
Embodiment 3
In special equipment, pour 92Kg MAP and 60Kg carbamide into, open stirring, close special equipment caping, and heat up,
Rising to 160 DEG C at temperature of charge, constantly there is condensation reaction in mixture, releases ammonia, carbon dioxide and steam, reaction
After 150min, finally give APP powdery solid product 117Kg.
Embodiment 4
In special equipment, pour 69Kg MAP and 60Kg carbamide into, open stirring, close special equipment caping, and heat up,
Rising to 160 DEG C at temperature of charge, constantly there is condensation reaction in mixture, releases ammonia, carbon dioxide and steam, reaction
After 150min, finally give thick APP 101Kg.
Embodiment 5
In special equipment, pour 207Kg MAP and 60Kg carbamide into, open stirring, close special equipment caping, and rise
Temperature, rises to 140 DEG C at temperature of charge, and mixture constantly occurs condensation reaction, releases ammonia, carbon dioxide and steam,
After reaction 180min, finally give APP powdery solid product 225Kg.
Embodiment 6
In special equipment, pour 230Kg MAP and 60Kg carbamide into, open stirring, close special equipment caping, and rise
Temperature, rises to 140 DEG C at temperature of charge, and mixture constantly occurs condensation reaction, releases ammonia, carbon dioxide and steam,
And finally give block APP solid product 239Kg.
Embodiment 7
In special equipment, pour 207Kg MAP and 60Kg carbamide into, open stirring, close special equipment caping, and rise
Temperature, rises to 110 DEG C at temperature of charge, and mixture constantly occurs condensation reaction, releases ammonia, carbon dioxide and steam,
And finally give powdery APP solid product 246Kg.
Table 1: different case study on implementation results contrast
| Nitrogen content/% | P2O5 content/% | Water-insoluble/% | Aggregate rate/% | Product Status | |
| Embodiment 1 | 20 | 46 | 7.8 | 99 | Block |
| Embodiment 2 | 23 | 44 | 0.07 | 98 | Powdery |
| Embodiment 3 | 29 | 39 | 0.05 | 98 | Powdery |
| Embodiment 4 | 32 | 34 | 1.3 | 93 | Thick |
| Embodiment 5 | 20 | 46 | 0.06 | 96 | Powdery |
| Embodiment 6 | 19 | 48 | 0.6 | 67 | Block |
| Embodiment 7 | 21 | 42 | 0.09 | 95 | Powdery |
Found out by table 1, when the mol ratio of MAP and carbamide is (0.8-1.8) 1, (real when reaction temperature is 110-180 DEG C
Execute example 2, embodiment 3, embodiment 5 and embodiment 7), the APP product obtained is all in powdery, and its aggregate rate is minimum to be reached
To 95%, up to 98%, water-insoluble maximum is only 0.09%.Its performance fully meets the needs of agricultural fertilizer.
Embodiment described above only have expressed the detailed description of the invention of the application, and it describes more concrete and in detail, but can not be because of
This and be interpreted as the restriction to the application protection domain.It should be pointed out that, for the person of ordinary skill of the art,
On the premise of conceiving without departing from technical scheme, it is also possible to making some deformation and improvement, these broadly fall into the guarantor of the application
Protect scope.
Claims (4)
1. the method preparing high aggregate rate water-soluble poly ammonium phosphate, it is characterised in that raw material MAP and carbamide are massaged
You join in reactor than (0.8-1.8) 1, stir, heat, and control temperature of charge 110-180 DEG C, the material of molten state
Start solidification, form powdery solid, after having reacted, cooling discharging, obtain high aggregate rate water-soluble poly ammonium phosphate.
A kind of method preparing high aggregate rate water-soluble poly ammonium phosphate the most according to claim 1, it is characterised in that phosphoric acid
The mol ratio of one ammonium and carbamide is (1.1-1.3) 1, and control temperature of charge is 140-170.
A kind of method preparing high aggregate rate water-soluble poly ammonium phosphate the most according to claim 1, it is characterised in that phosphoric acid
The mol ratio of one ammonium and carbamide is 1.2 1, and controlling temperature of charge is 160.
4., according to a kind of method that can prepare high aggregate rate water-soluble poly ammonium phosphate described in any one of claim 1-3, it is special
Levying and be, raw material MAP is the MAP that phosphoric acid by wet process prepares, and its N content is 9%-11%, P2O5Content is
44%-55%.
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| CN201610479295.4A CN105967164A (en) | 2016-06-27 | 2016-06-27 | Method for preparing high-polymerization-ratio water-soluble ammonium polyphosphate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107827515A (en) * | 2017-10-31 | 2018-03-23 | 上海化工研究院有限公司 | A kind of production method and device of hollow granular water soluble fertilizer |
| CN108383097A (en) * | 2018-05-15 | 2018-08-10 | 佳瑞科（武汉）国际贸易有限公司 | A method of utilizing extraction Wet-process Phosphoric Acid Production water solubility ammonium polyphosphate |
| CN113321562A (en) * | 2021-06-10 | 2021-08-31 | 山东农业大学 | Chemically synthesized water-soluble fertilizer special for apples in full bearing period and preparation method thereof |
| CN114249610A (en) * | 2021-12-30 | 2022-03-29 | 瓮福达州化工有限责任公司 | Preparation process and device of ammonium potassium polyphosphate containing chelated medium and trace elements |
| CN114478076A (en) * | 2022-01-18 | 2022-05-13 | 贵州川恒化工股份有限公司 | Preparation method of zinc-rich phosphorus-nitrogen type liquid fertilizer stock solution |
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| US4687651A (en) * | 1985-10-15 | 1987-08-18 | Thermal Science, Inc. | Method for producing ammonium polyphosphate |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107827515A (en) * | 2017-10-31 | 2018-03-23 | 上海化工研究院有限公司 | A kind of production method and device of hollow granular water soluble fertilizer |
| CN108383097A (en) * | 2018-05-15 | 2018-08-10 | 佳瑞科（武汉）国际贸易有限公司 | A method of utilizing extraction Wet-process Phosphoric Acid Production water solubility ammonium polyphosphate |
| CN113321562A (en) * | 2021-06-10 | 2021-08-31 | 山东农业大学 | Chemically synthesized water-soluble fertilizer special for apples in full bearing period and preparation method thereof |
| CN114249610A (en) * | 2021-12-30 | 2022-03-29 | 瓮福达州化工有限责任公司 | Preparation process and device of ammonium potassium polyphosphate containing chelated medium and trace elements |
| CN114478076A (en) * | 2022-01-18 | 2022-05-13 | 贵州川恒化工股份有限公司 | Preparation method of zinc-rich phosphorus-nitrogen type liquid fertilizer stock solution |
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Application publication date: 20160928 |