CN116730781A - Stable ammonium polyphosphate fertilizer and preparation method and application thereof - Google Patents
Stable ammonium polyphosphate fertilizer and preparation method and application thereof Download PDFInfo
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- 229920001276 ammonium polyphosphate Polymers 0.000 title claims abstract description 77
- 239000004114 Ammonium polyphosphate Substances 0.000 title claims abstract description 68
- 235000019826 ammonium polyphosphate Nutrition 0.000 title claims abstract description 68
- 239000003337 fertilizer Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000011343 solid material Substances 0.000 claims abstract description 30
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 28
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 25
- 239000003112 inhibitor Substances 0.000 claims abstract description 24
- 239000011344 liquid material Substances 0.000 claims abstract description 18
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000004202 carbamide Substances 0.000 claims abstract description 10
- 238000006482 condensation reaction Methods 0.000 claims abstract description 9
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 12
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 6
- LXKCHCXZBPLTAE-UHFFFAOYSA-N 3,4-dimethyl-1H-pyrazole phosphate Chemical compound OP(O)(O)=O.CC1=CNN=C1C LXKCHCXZBPLTAE-UHFFFAOYSA-N 0.000 claims description 4
- 125000003118 aryl group Chemical group 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000419 plant extract Substances 0.000 claims description 4
- 239000000618 nitrogen fertilizer Substances 0.000 claims description 3
- 239000002686 phosphate fertilizer Substances 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 14
- 239000000203 mixture Substances 0.000 abstract description 9
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 8
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 4
- 238000002386 leaching Methods 0.000 abstract description 3
- 235000015097 nutrients Nutrition 0.000 abstract description 3
- 229910002651 NO3 Inorganic materials 0.000 abstract description 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract description 2
- 229910021529 ammonia Inorganic materials 0.000 abstract description 2
- 239000003673 groundwater Substances 0.000 abstract description 2
- 235000015816 nutrient absorption Nutrition 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 13
- 239000000047 product Substances 0.000 description 13
- 238000004519 manufacturing process Methods 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- 239000002689 soil Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 6
- 239000011574 phosphorus Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 5
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 description 4
- 238000004806 packaging method and process Methods 0.000 description 4
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 3
- 229920000388 Polyphosphate Polymers 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 3
- 230000007935 neutral effect Effects 0.000 description 3
- 238000006384 oligomerization reaction Methods 0.000 description 3
- 239000001205 polyphosphate Substances 0.000 description 3
- 235000011176 polyphosphates Nutrition 0.000 description 3
- 235000019832 sodium triphosphate Nutrition 0.000 description 3
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 3
- NPBVQXIMTZKSBA-UHFFFAOYSA-N Chavibetol Natural products COC1=CC=C(CC=C)C=C1O NPBVQXIMTZKSBA-UHFFFAOYSA-N 0.000 description 2
- 239000005770 Eugenol Substances 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- UVMRYBDEERADNV-UHFFFAOYSA-N Pseudoeugenol Natural products COC1=CC(C(C)=C)=CC=C1O UVMRYBDEERADNV-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- XPPKVPWEQAFLFU-UHFFFAOYSA-J diphosphate(4-) Chemical compound [O-]P([O-])(=O)OP([O-])([O-])=O XPPKVPWEQAFLFU-UHFFFAOYSA-J 0.000 description 2
- 235000011180 diphosphates Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229960002217 eugenol Drugs 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- -1 polyethylene Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000011573 trace mineral Substances 0.000 description 2
- 235000013619 trace mineral Nutrition 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229920001971 elastomer Polymers 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000004720 fertilization Effects 0.000 description 1
- 239000011094 fiberboard Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002366 mineral element Substances 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B17/00—Other phosphatic fertilisers, e.g. soft rock phosphates, bone meal
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/10—Solid or semi-solid fertilisers, e.g. powders
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
- Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Soil Sciences (AREA)
- Fertilizers (AREA)
Abstract
The application relates to the technical field of ammonium polyphosphate preparation, in particular to a stable ammonium polyphosphate fertilizer, a preparation method and application thereof. The application firstly adopts phosphoric acid and urea to carry out condensation reaction to obtain a homogeneous liquid material, then carries out polymerization reaction on the liquid material to obtain a solid material, and then blends the solid material with a nitrification inhibitor to obtain the stable ammonium polyphosphate fertilizer. The application provides a brand-new preparation method of ammonium polyphosphate fertilizer, which can blend the prepared ammonium polyphosphate with a nitrification inhibitor, combine the stability in the process, control the release characteristic of nitrogen nutrient by using the nitrification inhibitor, and simultaneously be consistent with the nutrient absorption rule of crops, so as to produce the stable ammonium polyphosphate fertilizer, enable the ammonium polyphosphate fertilizer to inhibit ammonia volatilization and nitrate leaching to a certain extent, and further reduce the pollution to the environment and groundwater.
Description
Technical Field
The application relates to the technical field of ammonium polyphosphate preparation, in particular to a stable ammonium polyphosphate fertilizer, a preparation method and application thereof.
Background
Ammonium polyphosphate is a polyphosphate containing N and P, abbreviated APP. The polymerization degree can be divided into 3 types of oligomerization, medium polymerization and high polymerization according to the polymerization degree, and when the polymerization degree is below 20, the polymerization degree is called oligomerization and is water-soluble; the polymerization degree of 50 or more is called high polymerization and can be used as a flame retardant. In the 80 s, the oligomeric water-soluble APP is mainly applied to flame retardant materials such as paper, wood and the like, and the high-polymerization-degree ammonium polyphosphate is widely applied to intumescent fireproof coatings, polyethylene, polypropylene, polyurethane, epoxy resin, rubber products, fiber boards, dry powder extinguishing agents and the like, so that the oligomeric water-soluble APP is a safe and efficient nitrogen-phosphorus non-halogen smoke abatement flame retardant.
Agricultural ammonium polyphosphate (APP, ammonium polyphosphate) is a low-N high-P polyphosphate, the pH value is near neutral, and the chemical general formula is (NH) 4 ) n +2P n O 3n+1 . APP can be classified into oligomerization, medium polymerization and high polymerization according to the degree of polymerization, and the higher the degree of polymerization, the smaller the water solubility, generally when n<20 is water-soluble, n>20 is water insoluble, and APP is used as a novel fertilizer which enters the fertilizer field at present and is often used as a basic phosphate fertilizer for preparing high-concentration liquid compound fertilizer. The solid ammonium polyphosphate product is generally composed of 20-30% orthophosphate, 40-50% pyrophosphate (P) 2 O 7 4- ) 10-15% tripolyphosphate (P) 3 O 10 5- ) 3-5% of tetramer and polyphosphate above tetramer; liquid ammonium polyphosphate products generally contain higher amounts of tripolyphosphate and phosphate ions than granular products, but the composition varies, typically ranging from 30-40% orthophosphate, 50-55% pyrophosphate, and a portion of the tripolyphosphate and tetrapolyphosphate. The proportion of the liquid APP commonly used in foreign countries is as follows: 8-24-0, 10-34-0, 11-37-0, 11-44-0,8-28-0, etc., and the solid is 18-58-0. APP has recently come into the field of liquid fertilizer production.
APP agricultural ammonium polyphosphate is an important phosphorus raw material for developing water-soluble fertilizer, and has the following advantages: (1) The content of phosphorus nutrient is high, the pH value is 6.5-7.5 and is close to neutral, the use safety coefficient of crops is high, and the activity of mineral elements is good. (2) The solubility is large, the solubility is more than or equal to 150 g/100 g of water, and the liquid fertilizer with higher phosphorus content can be prepared; the crystallization temperature is lower, and the production and the use are convenient. (3) The chelating effect on metal ions can prevent metal impurities in the solution from forming precipitates, and trace elements are added into the liquid fertilizer, so that the high-concentration high-quality liquid fertilizer can be prepared; the phosphorus is not easily fixed by metal ions such as iron, calcium and the like in the soil, but can form a soluble complex with invalid trace elements in the soil to be absorbed and utilized by plants. (4) Although not directly absorbed by plants in the soil, the fertilizer can be slowly hydrolyzed into orthophosphate in the soil and then utilized by the plants, thus being a slow-dissolving long-acting fertilizer. (5) can be made into foliar fertilizer for foliar application of crops; the agricultural ammonium polyphosphate is used as fertilizer, the application amount can be 3 times higher than that of orthophosphate, but leaves cannot be burnt, and the neutral solution can be maintained on the leaves for several days without being evaporated to dryness or salted out. (6) The heavy metal content is low, the heavy metal in the soil can be passivated, the soil is improved, and the method is safe and environment-friendly.
In the prior art, the agricultural ammonium polyphosphate base liquid fertilizer is often mixed with a nitrogen solution and a potassium fertilizer to produce a liquid compound fertilizer, and the ammonium polyphosphate serving as a main component cannot be realized; at present, enterprises for producing agricultural ammonium polyphosphate fertilizers are few in China, the traditional ammonium polyphosphate production method is relatively complex in process, and the reasons are that the properties, the compositions and the production methods of the ammonium polyphosphate fertilizers are controversial, so that the product quality, the quantity and the application range are quite different.
Disclosure of Invention
Aiming at the defects in the prior art, the application provides a stable ammonium polyphosphate fertilizer, and a preparation method and application thereof. The application provides a brand-new preparation method of ammonium polyphosphate fertilizer, which can blend the prepared ammonium polyphosphate with a nitrification inhibitor, combine the stability in the process, control the release characteristic of nitrogen nutrient by using the nitrification inhibitor, and simultaneously be consistent with the nutrient absorption rule of crops, so as to produce the stable ammonium polyphosphate fertilizer, enable the ammonium polyphosphate fertilizer to inhibit ammonia volatilization and nitrate leaching to a certain extent, and further reduce the pollution to the environment and groundwater.
In order to achieve the above purpose, the technical scheme of the application is as follows:
a preparation method of a stable ammonium polyphosphate fertilizer comprises the following steps:
s1, mixing phosphoric acid and urea, and then performing condensation reaction to obtain a homogeneous liquid material;
s2, carrying out polymerization reaction on the liquid material in the step S1 to obtain a solid material, wherein the solid material is synthesized ammonium polyphosphate;
s3, cooling the solid material obtained in the step S2 to 30-50 ℃, blending with the nitrification inhibitor, and crushing to obtain the stable ammonium polyphosphate fertilizer.
Preferably, the condensation reaction conditions in the step S1 are as follows: condensation reaction is carried out for 15-40min at 50-120 ℃.
Preferably, in the step S1, the mass percentage of phosphoric acid is 65-75%, the mass percentage of urea is 25-35%, and the sum of the mass percentages is 100%.
Preferably, the polymerization conditions in the step S2 are as follows: the liquid material is placed in a tubular reactor and polymerized at 150-250 ℃ for 50-150min.
Preferably, the nitrification inhibitor in the step S3 is one or more selected from dicyandiamide, thiourea, 3, 4-dimethylpyrazole phosphate and aromatic plant extract eugenol.
Preferably, the mass ratio of the solid material to the nitrification inhibitor in the step S3 is 0.1-2:100.
the application also protects the stable ammonium polyphosphate fertilizer prepared by the preparation method, and the polymerization degree of ammonium polyphosphate in the stable ammonium polyphosphate fertilizer is less than 20.
The application also protects the application of the stable ammonium polyphosphate fertilizer in preparing nitrogen fertilizer and phosphorus fertilizer.
Compared with the prior art, the application has the beneficial effects that:
1. the application adopts the synergistic technology of the nitrogen high-efficiency inhibitor to control the form and the process of the conversion of nitrogen in soil, reduce the leaching loss of nitrogen and improve the utilization efficiency of nitrogen fertilizer. The application combines with fertilization organically to achieve the aim of synergy, on one hand, the application can ensure that the stable ammonium polyphosphate is produced for the growth of crops, on the other hand, the method is simple and easy to implement, and the production process parameters are easy to control.
2. The preparation method of the stable ammonium polyphosphate is simple and is convenient for mass production. The method comprises the following steps: firstly, carrying out condensation reaction on phosphoric acid and urea to obtain a homogeneous liquid material, and then, carrying out polymerization reaction on the liquid material to obtain a solid material, wherein the solid material is ammonium polyphosphate, and the preparation principle of the application is as follows:
condensation reaction: (NH) 2 ) 2 CO+H 3 PO 4 →(NH 2 ) 2 CO·H 3 PO 4 ;
Polymerization reaction:
(n-1)CO(NH 2 ) 2 +nH 3 PO 4 →(NH 4 ) (n+2) P n O (3n+1) +(n-4)NH 3 +(n-1)CO 2 。
3. compared with the traditional ammonium polyphosphate preparation method, the production equipment and the process are simple, and are favorable for continuous production.
Drawings
FIG. 1 is a flow chart illustrating the operation of embodiments 1-4 of the present application;
figure 2 is an XRD pattern of the solid material obtained in example 1 of the application.
Detailed Description
The following detailed description of specific embodiments of the application is, but it should be understood that the application is not limited to specific embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the application without making any inventive effort, are intended to be within the scope of the application. The experimental methods described in the examples of the present application are conventional methods unless otherwise specified.
Example 1
A preparation method of stable ammonium polyphosphate comprises the following steps:
step 1, adding phosphoric acid and urea into a mixer together, and then reacting for 15min at 60 ℃ to obtain a homogeneous liquid material;
wherein the mass percentage of phosphoric acid is 65%;
step 2, transferring the liquid material in the step 1 into a tubular polymerizer, carrying out polymerization reaction for 30min at 150 ℃ to obtain a solid material, and then cooling to 30 ℃;
step 3, connecting the tail end of the tubular polymerizer in the step 2 with a crushing device, and crushing the solid material and the nitrification inhibitor together after the solid material leaves the tubular polymerizer and enters the crushing device to obtain a powdery material;
wherein the nitrification inhibitor is a mixture of dicyandiamide and aromatic plant extract, and the mass ratio of dicyandiamide to aromatic plant extract eugenol is 1:1; the mass ratio of the solid material to the nitrification inhibitor is 2:100;
step 4, directly packaging the powdery material in the step 3 to obtain a water-soluble solid ammonium polyphosphate product;
and preparing the powdery material and water according to a proportion to obtain a liquid ammonium polyphosphate product.
Example 2
A preparation method of stable ammonium polyphosphate comprises the following steps:
step 1, adding phosphoric acid and urea into a mixer together, and then reacting for 20min at 70 ℃ to obtain a homogeneous liquid material;
wherein the mass percentage of phosphoric acid is 68%;
step 2, transferring the liquid material in the step 1 into a tubular polymerizer, carrying out polymerization reaction at 200 ℃ for 50min to obtain a solid material, and then cooling to 40 ℃;
step 3, connecting the tail end of the tubular polymerizer in the step 2 with a crushing device, and crushing the solid material and the nitrification inhibitor together after the solid material leaves the tubular polymerizer and enters the crushing device to obtain a powdery material;
wherein the nitrification inhibitor is a mixture of dicyandiamide and thiourea, and the mass ratio of the dicyandiamide to the thiourea is 1:1.5; the mass ratio of the solid material to the nitrification inhibitor is 1.5:100;
step 4, directly packaging the powdery material in the step 3 to obtain a water-soluble solid ammonium polyphosphate product;
and preparing the powdery material and water according to a proportion to obtain a liquid ammonium polyphosphate product.
Example 3
A preparation method of stable ammonium polyphosphate comprises the following steps:
step 1, adding phosphoric acid and urea into a mixer together, and then reacting for 15min at 80 ℃ to obtain a homogeneous liquid material;
wherein the mass percentage of phosphoric acid is 75%;
step 2, transferring the liquid material in the step 1 into a tubular polymerizer, carrying out polymerization reaction at 180 ℃ for 60min to obtain a solid material, and then cooling to 50 ℃;
step 3, connecting the tail end of the tubular polymerizer in the step 2 with a crushing device, and crushing the solid material and the nitrification inhibitor together after the solid material leaves the tubular polymerizer and enters the crushing device to obtain a powdery material;
wherein the nitrification inhibitor is a mixture of dicyandiamide and thiourea, and the mass ratio of the dicyandiamide to the thiourea is 1:2; the mass ratio of the solid material to the nitrification inhibitor is 1.8:100;
step 4, directly packaging the powdery material in the step 3 to obtain a water-soluble solid ammonium polyphosphate product;
and preparing the powdery material and water according to a proportion to obtain a liquid ammonium polyphosphate product.
Example 4
A preparation method of stable ammonium polyphosphate comprises the following steps:
step 1, adding phosphoric acid and urea into a mixer together, and then reacting for 15min at 100 ℃ to obtain a homogeneous liquid material;
wherein the mass percentage of phosphoric acid is 70%;
step 2, transferring the liquid material in the step 1 into a tubular polymerizer, carrying out polymerization reaction for 80min at 250 ℃ to obtain a solid material, and then cooling to 30 ℃;
step 3, connecting the tail end of the tubular polymerizer in the step 2 with a crushing device, and crushing the solid material and the nitrification inhibitor together after the solid material leaves the tubular polymerizer and enters the crushing device to obtain a powdery material;
wherein the nitrification inhibitor is a mixture of dicyandiamide and 3, 4-dimethylpyrazole phosphate, and the mass ratio of the dicyandiamide to the 3, 4-dimethylpyrazole phosphate is 1:0.3; the mass ratio of the solid material to the nitrification inhibitor is 1.2:100;
step 4, directly packaging the powdery material in the step 3 to obtain a water-soluble solid ammonium polyphosphate product;
and preparing the powdery material and water according to a proportion to obtain a liquid ammonium polyphosphate product.
The solid material prepared in example 1 was tested according to the standard HG/T5939-2021 of the chemical industry of the people's republic of China, and the test data obtained are shown in the following table:
project | Example 1 sample | Example 2 sample | Example 3 sample |
Available phosphorus (P) 2 O 5 )% | 52.2 | 54.5 | 53.2 |
Total nitrogen (N)% | 31.6 | 29.7 | 33.9 |
Moisture content% | 1.5 | 2.0 | 1.8 |
XRD tests are also carried out on the solid material prepared in the embodiment 1 of the application, as shown in figure 2, and the results of figure 2 show that the prepared ammonium polyphosphate has diffraction peaks near 16 degrees, is characteristic of the ammonium polyphosphate of type I, and does not have diffraction peaks near 20-23 degrees, so that the prepared ammonium polyphosphate is the ammonium polyphosphate of type I and does not contain the ammonium polyphosphate of type II.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present application without departing from the spirit or scope of the application. Thus, it is intended that the present application also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.
Claims (8)
1. The preparation method of the stable ammonium polyphosphate fertilizer is characterized by comprising the following steps of:
s1, mixing phosphoric acid and urea, and then performing condensation reaction to obtain a homogeneous liquid material;
s2, carrying out polymerization reaction on the liquid material in the step S1 to obtain a solid material;
s3, cooling the solid material obtained in the step S2 to 30-50 ℃, blending with the nitrification inhibitor, and crushing to obtain the stable ammonium polyphosphate fertilizer.
2. The method for preparing a stable ammonium polyphosphate fertilizer according to claim 1, wherein the condensation reaction conditions in the step S1 are as follows: condensation reaction is carried out for 15-40min at 50-120 ℃.
3. The method for preparing a stable ammonium polyphosphate fertilizer according to claim 1, wherein in the step S1, the mass percentage of phosphoric acid is 65-75%, the mass percentage of urea is 25-35%, and the sum of the mass percentages is 100%.
4. The method for preparing a stable ammonium polyphosphate fertilizer according to claim 1, wherein the polymerization conditions in the step S2 are as follows: the liquid material is placed in a tubular reactor and polymerized at 150-250 ℃ for 50-150min.
5. The method for preparing a stable ammonium polyphosphate fertilizer according to claim 1, wherein the nitrification inhibitor in the step S3 is selected from one or more of dicyandiamide, thiourea, 3, 4-dimethylpyrazole phosphate and aromatic plant extracts.
6. The method for preparing a stable ammonium polyphosphate fertilizer according to claim 1, wherein the mass ratio of the solid material to the nitrification inhibitor in the step S3 is 0.1-2:100.
7. a stable ammonium polyphosphate fertilizer prepared by the method of any one of claims 1-6, wherein the ammonium polyphosphate in the stable ammonium polyphosphate fertilizer has a degree of polymerization of < 20.
8. Use of the stable ammonium polyphosphate fertilizer of claim 7 in the preparation of a nitrogen fertilizer phosphate fertilizer.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN202310697905.8A CN116730781A (en) | 2023-06-13 | 2023-06-13 | Stable ammonium polyphosphate fertilizer and preparation method and application thereof |
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