WO2022142861A1 - Method for preparing high-solubility nitrogen-phosphorus water-soluble fertilizer - Google Patents
Method for preparing high-solubility nitrogen-phosphorus water-soluble fertilizer Download PDFInfo
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- WO2022142861A1 WO2022142861A1 PCT/CN2021/132242 CN2021132242W WO2022142861A1 WO 2022142861 A1 WO2022142861 A1 WO 2022142861A1 CN 2021132242 W CN2021132242 W CN 2021132242W WO 2022142861 A1 WO2022142861 A1 WO 2022142861A1
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- WO
- WIPO (PCT)
- Prior art keywords
- phosphorus
- phosphoric acid
- soluble fertilizer
- nitrogen
- water
- Prior art date
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- 239000003337 fertilizer Substances 0.000 title claims abstract description 69
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 29
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 128
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 64
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 61
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000011574 phosphorus Substances 0.000 claims abstract description 53
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 53
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- 238000003756 stirring Methods 0.000 claims abstract description 34
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000004202 carbamide Substances 0.000 claims abstract description 24
- 239000002002 slurry Substances 0.000 claims abstract description 24
- 239000011343 solid material Substances 0.000 claims abstract description 24
- 239000012066 reaction slurry Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims description 71
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 46
- 229910052757 nitrogen Inorganic materials 0.000 claims description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000002360 preparation method Methods 0.000 claims description 11
- 239000002994 raw material Substances 0.000 claims description 11
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 9
- 239000011575 calcium Substances 0.000 claims description 9
- 229960005069 calcium Drugs 0.000 claims description 9
- 229910052791 calcium Inorganic materials 0.000 claims description 9
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 8
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 8
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 8
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 claims description 8
- 239000011777 magnesium Substances 0.000 claims description 8
- 229910052749 magnesium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 229910052742 iron Inorganic materials 0.000 claims description 7
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 7
- -1 iron-magnesium-aluminum-calcium Chemical compound 0.000 claims description 6
- MHJAJDCZWVHCPF-UHFFFAOYSA-L dimagnesium phosphate Chemical compound [Mg+2].OP([O-])([O-])=O MHJAJDCZWVHCPF-UHFFFAOYSA-L 0.000 claims description 5
- 229910000395 dimagnesium phosphate Inorganic materials 0.000 claims description 5
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 5
- 239000000347 magnesium hydroxide Substances 0.000 claims description 5
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 5
- 239000000395 magnesium oxide Substances 0.000 claims description 5
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 5
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 claims description 5
- 229910000157 magnesium phosphate Inorganic materials 0.000 claims description 5
- 239000004137 magnesium phosphate Substances 0.000 claims description 5
- 229960002261 magnesium phosphate Drugs 0.000 claims description 5
- 235000010994 magnesium phosphates Nutrition 0.000 claims description 5
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 5
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 5
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical group [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 5
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 4
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 4
- 239000011790 ferrous sulphate Substances 0.000 claims description 4
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 4
- 235000014413 iron hydroxide Nutrition 0.000 claims description 4
- 229910000398 iron phosphate Inorganic materials 0.000 claims description 4
- WBJZTOZJJYAKHQ-UHFFFAOYSA-K iron(3+) phosphate Chemical compound [Fe+3].[O-]P([O-])([O-])=O WBJZTOZJJYAKHQ-UHFFFAOYSA-K 0.000 claims description 4
- 229910021506 iron(II) hydroxide Inorganic materials 0.000 claims description 4
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 4
- 238000000638 solvent extraction Methods 0.000 claims description 4
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 claims description 3
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 claims description 3
- 229940062672 calcium dihydrogen phosphate Drugs 0.000 claims description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- FUFJGUQYACFECW-UHFFFAOYSA-L calcium hydrogenphosphate Chemical compound [Ca+2].OP([O-])([O-])=O FUFJGUQYACFECW-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 235000011116 calcium hydroxide Nutrition 0.000 claims description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000292 calcium oxide Substances 0.000 claims description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 claims description 3
- 235000012255 calcium oxide Nutrition 0.000 claims description 3
- 229910000389 calcium phosphate Inorganic materials 0.000 claims description 3
- 235000019700 dicalcium phosphate Nutrition 0.000 claims description 3
- 235000019691 monocalcium phosphate Nutrition 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 239000006227 byproduct Substances 0.000 claims description 2
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims 1
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 6
- 230000008569 process Effects 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 description 76
- 238000005273 aeration Methods 0.000 description 19
- 230000007246 mechanism Effects 0.000 description 11
- 238000005457 optimization Methods 0.000 description 10
- 230000009471 action Effects 0.000 description 7
- 230000000903 blocking effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 229910000358 iron sulfate Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000004114 Ammonium polyphosphate Substances 0.000 description 2
- DZHMRSPXDUUJER-UHFFFAOYSA-N [amino(hydroxy)methylidene]azanium;dihydrogen phosphate Chemical compound NC(N)=O.OP(O)(O)=O DZHMRSPXDUUJER-UHFFFAOYSA-N 0.000 description 2
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 2
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 description 2
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 2
- 229920001276 ammonium polyphosphate Polymers 0.000 description 2
- 206010006514 bruxism Diseases 0.000 description 2
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 2
- 229910000388 diammonium phosphate Inorganic materials 0.000 description 2
- 235000019838 diammonium phosphate Nutrition 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000009434 installation Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000019837 monoammonium phosphate Nutrition 0.000 description 2
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000783 alginic acid Substances 0.000 description 1
- 235000010443 alginic acid Nutrition 0.000 description 1
- 229960001126 alginic acid Drugs 0.000 description 1
- 229920000615 alginic acid Polymers 0.000 description 1
- 150000004781 alginic acids Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000004720 fertilization Effects 0.000 description 1
- 239000004021 humic acid Substances 0.000 description 1
- 235000006180 nutrition needs Nutrition 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B9/00—Fertilisers based essentially on phosphates or double phosphates of magnesium
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
-
- 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
Definitions
- the invention relates to the technical field of preparation of a water-soluble fertilizer, in particular to a preparation method of a high-solubility nitrogen-phosphorus water-soluble fertilizer.
- Water-soluble fertilizer refers to compound fertilizers containing nitrogen, phosphorus, potassium, calcium, magnesium, trace elements, amino acids, humic acid, alginic acid, etc. that can be completely dissolved in water. It is a quick-acting fertilizer with good water solubility and no residue. It can be completely dissolved in water and can be directly absorbed and utilized by the roots and leaves of crops.
- the effective absorption rate of the fertilizer is more than double that of ordinary chemical fertilizers, and the fertilizer effect is fast, which can meet the nutritional needs of high-yield crops during the rapid growth period, and the fertilization operation is almost free of labor, which greatly saves labor costs.
- solubility of common nitrogen and phosphorus water-soluble fertilizers is generally about 20-180 grams per 100 grams of water, and water-soluble fertilizers with high solubility are more affected by "water and fertilizer integration". "The modern agriculture welcomes, therefore, how to quickly prepare high solubility nitrogen and phosphorus water-soluble fertilizer is a technical problem we need to solve.
- the purpose of the present invention is to provide a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, which is used for rapidly preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, and has the advantage of a simple process.
- the technical scheme adopted in the present invention is:
- a method for preparing a high solubility nitrogen and phosphorus water-soluble fertilizer comprising the following steps:
- Step 1 Add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 70 to 135 ° C for 60 to 180 minutes to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 10% to 50%. %;
- Step 2 Add the reaction slurry into the solidifier, control the temperature of the slurry material at 150-220 °C, and dry and solidify the slurry into a solid material for 30-90 minutes, and control the polymerization rate of phosphorus in the solid material dried and solidified to be 85. % ⁇ 99%;
- Step 3 The solid material is cooled to 40-70° C. from the solidifier and then crushed to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
- the curing agent is magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium hydrogen phosphate, magnesium phosphate, iron sulfate, ferrous sulfate, iron phosphate, iron oxide, iron hydroxide, ferrous hydroxide, One or more of aluminum sulfate, aluminum phosphate, aluminum oxide, aluminum hydroxide, calcium oxide, calcium hydroxide, calcium dihydrogen phosphate, and calcium hydrogen phosphate.
- the added amount of the curing agent is the mass ratio of the iron, magnesium, aluminum, and calcium elements in the curing agent to the mass ratio of P 2 O 5 in the phosphoric acid .
- the phosphoric acid and the curing agent can be replaced by raffinate phosphoric acid purifying by-products by wet-process phosphoric acid solvent extraction
- the P 2 O 5 mass percentage concentration of the raffinate phosphoric acid is 40% to 50%
- the raffinate phosphoric acid contains
- the mass of iron, magnesium, aluminum, and calcium elements is 4% to 10% of the mass of P 2 O 5 contained in the raffinate phosphoric acid.
- the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
- step 3 the nitrogen content of the powder and granular nitrogen and phosphorus water-soluble fertilizer is 12%-18%, the P2O5 content is 55 %-64%, and the solubility is 300-500g/100g water.
- the present invention has the following beneficial effects:
- the present invention prepares high-solubility nitrogen-phosphorus water-soluble fertilizer through phosphoric acid, urea, curing agent and polymerization aid, prepares reaction slurry by heating and stirring, and then solidifies and dries the reaction slurry and crushes it to obtain high-solubility nitrogen-phosphorus fertilizer
- the water-soluble fertilizer has a simple preparation process and can achieve the purpose of rapid preparation of a high-solubility nitrogen-phosphorus water-soluble fertilizer.
- the solubility of the high solubility nitrogen and phosphorus water-soluble fertilizer is 300-500g/100g water, which is much higher than that of common nitrogen and phosphorus water-soluble fertilizers on the market (such as ammonium dihydrogen phosphate, diammonium hydrogen phosphate, urea phosphate, ammonium polyphosphate, etc.). Solubility, water-soluble fertilizers with high solubility are more popular in modern agriculture with "water and fertilizer integration".
- FIG. 1 is a schematic diagram of the overall structure of the reactor according to the present invention.
- FIG. 2 is an enlarged schematic diagram of a part of A in FIG. 1 of the present invention.
- FIG. 3 is an enlarged schematic diagram of a part of B in FIG. 1 of the present invention.
- the present embodiment discloses a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps:
- Step 1 add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 70° C. for 60 minutes to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 10%;
- Step 2 adding the reaction slurry into the solidifier, controlling the temperature of the slurry material at 150°C, drying the slurry for 30 minutes and solidifying it into a solid material, and controlling the polymerization rate of phosphorus in the solid material dried and solidified to be 85%;
- Step 3 The solid material is cooled to 40°C and then crushed from the solidifier to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
- the curing agent is a mixture of magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium hydrogen phosphate, magnesium phosphate and iron sulfate.
- the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
- step 3 the nitrogen content of the powder and granular nitrogen and phosphorus water-soluble fertilizer is 18%, the P 2 O 5 content is 55%, and the solubility is 300g/100g water.
- the present invention prepares high-solubility nitrogen-phosphorus water-soluble fertilizer through phosphoric acid, urea, curing agent and polymerization aid, prepares reaction slurry by heating and stirring, and then solidifies and dries the reaction slurry and crushes it to obtain high-solubility nitrogen-phosphorus fertilizer
- the water-soluble fertilizer has a simple preparation process and can achieve the purpose of rapid preparation of a high-solubility nitrogen-phosphorus water-soluble fertilizer.
- the present embodiment discloses a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps:
- Step 1 add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 100° C. for 90 minutes to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 35%;
- Step 2 adding the reaction slurry into the solidifier, controlling the temperature of the slurry material to be 180°C, drying the slurry for 60 minutes and solidifying it into a solid material, and controlling the polymerization rate of phosphorus in the solid material dried and solidified to be 95%;
- Step 3 The solid material is cooled to 50°C and then crushed from the solidifier to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
- the curing agent is magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium hydrogen phosphate, magnesium phosphate, iron sulfate, ferrous sulfate, iron phosphate, iron oxide, iron hydroxide, ferrous hydroxide, Aluminum sulfate, aluminum phosphate, aluminum oxide, aluminum hydroxide, calcium oxide, calcium hydroxide, calcium dihydrogen phosphate or calcium hydrogen phosphate, in this embodiment, the curing agent is aluminum hydroxide.
- the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
- step 3 the nitrogen content of the powdered and granular nitrogen and phosphorus water-soluble fertilizer is 16 %, the P2O5 content is 60%, and the solubility is 400g/100g water.
- the present embodiment discloses a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps:
- Step 1 add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 135 ° C for 180 min to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 50%;
- Step 2 adding the reaction slurry into the solidifier, controlling the temperature of the slurry material at 220°C, drying the slurry for 90 minutes and solidifying it into a solid material, and controlling the polymerization rate of phosphorus in the solid material dried and solidified to be 99%;
- Step 3 The solid material is cooled to 70°C from the solidifier and then crushed to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
- the curing agent is magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium hydrogen phosphate, magnesium phosphate, iron sulfate, ferrous sulfate, iron phosphate, iron oxide, iron hydroxide, ferrous hydroxide, A mixture of aluminum sulfate.
- the polymerization aid in step 1 is the powdery and granular nitrogen-phosphorus water-soluble fertilizer obtained in step 3, and the addition of the polymerization aid is the mass ratio of the mass of the polymerization aid to P 2 O 5 in phosphoric acid.
- M 2 : P 2 O 5 0.10, wherein M 2 is the mass of the polymerization aid added.
- the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
- step 3 the nitrogen content of the powdered and granular nitrogen and phosphorus water-soluble fertilizer is 12 %, the P2O5 content is 64%, and the solubility is 500g/100g water.
- the present embodiment discloses a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps:
- Step 1 add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 70° C. for 60 minutes to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 10%;
- Step 2 adding the reaction slurry into the solidifier, controlling the temperature of the slurry material at 150°C, drying the slurry for 30 minutes and solidifying it into a solid material, and controlling the polymerization rate of phosphorus in the solid material dried and solidified to be 85%;
- Step 3 The solid material is cooled to 40°C and then crushed from the solidifier to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
- the added phosphoric acid and curing agent are raffinate phosphoric acid purified by wet-process phosphoric acid solvent extraction method
- the P 2 O 5 mass percentage concentration of the raffinate phosphoric acid is 40%
- the raffinate phosphoric acid contains
- the quality of iron, magnesium, aluminum, and calcium elements is 4% of the mass of P 2 O 5 contained in the raffinate phosphoric acid
- the raw material ratio of the raffinate phosphoric acid and urea is the mass of P 2 O 5 in the raffinate phosphoric acid and the quality of N in the urea.
- the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
- step 3 the nitrogen content of the powder and granular nitrogen and phosphorus water-soluble fertilizer is 18%, the P 2 O 5 content is 55%, and the solubility is 300g/100g water.
- the present embodiment discloses a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps:
- Step 1 add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 135 ° C for 180 min to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 50%;
- Step 2 adding the reaction slurry into the solidifier, controlling the temperature of the slurry material at 220°C, drying the slurry for 90 minutes and solidifying it into a solid material, and controlling the polymerization rate of phosphorus in the solid material dried and solidified to be 99%;
- Step 3 The solid material is cooled to 70°C after the solidified material is crushed to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
- the added phosphoric acid and curing agent are raffinate phosphoric acid purified by wet-process phosphoric acid solvent extraction method
- the P 2 O 5 mass percentage concentration of the raffinate phosphoric acid is 50%
- the raffinate phosphoric acid contains
- the quality of iron, magnesium, aluminum, and calcium elements is 10% of the quality of P 2 O 5 contained in the raffinate phosphoric acid
- the raw material ratio of the raffinate phosphoric acid and urea is the quality of P 2 O 5 in the raffinate phosphoric acid and N in the urea.
- the polymerization aid in step 1 is the powdery and granular nitrogen-phosphorus water-soluble fertilizer obtained in step 3, and the addition of the polymerization aid is the mass ratio of the mass of the polymerization aid to P 2 O 5 in phosphoric acid.
- M 2 : P 2 O 5 0.10, wherein M 2 is the mass of the polymerization aid added.
- the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
- step 3 the nitrogen content of the powdered and granular nitrogen and phosphorus water-soluble fertilizer is 12 %, the P2O5 content is 64%, and the solubility is 500g/100g water.
- the stirring step in step 1 the most critical step in the preparation of high-solubility nitrogen and phosphorus water-soluble fertilizer is the stirring step in step 1. If the stirring is performed in step 1, the uneven stirring will lead to poor mixing of raw materials, making subsequent production difficult. It is stable and affects the preparation of high-solubility nitrogen-phosphorus water-soluble fertilizer; therefore, the applicant has improved the reactor for preparing high-solubility nitrogen-phosphorus water-soluble fertilizer, so that the raw materials can be fully dissolved and mixed to ensure the preparation of high-solubility nitrogen and phosphorus water-soluble fertilizer.
- step 1 a reactor of the following structure is used to agitate the raw materials:
- the reactor includes a reactor body 1 having a tank-like structure, a grinding assembly 2 and a stirring assembly 3 installed in the reactor body 1; the upper end of the reactor body 1 is provided with a feeding port 4, and the lower end is provided with There is a discharge port 5, and the discharge port 5 is provided with a discharge valve 6;
- the grinding assembly 2 includes a grinding motor 7, a grinding shaft 8 and a grinding mechanism 9, the grinding shaft 8 is rotatably mounted on the reactor body 1, and the upper end of the grinding shaft 8 is connected with the grinding motor 7 installed on the reactor body 1 through the transmission mechanism 10,
- the grinding mechanism 9 is arranged at the lower end of the grinding shaft 8, and the interior of the grinding shaft 8 is hollow;
- the stirring assembly 3 includes a stirring motor 11, a stirring shaft 12 and a stirring rod 13.
- the stirring shaft 12 is rotatably installed in the grinding shaft 8, and the axis line of the grinding shaft 8 is collinear with that of the stirring shaft 12; the upper end of the grinding shaft 8 extends After exiting the stirring shaft 12, it is connected to the stirring motor 11.
- the materials are stirred by the stirring component 3 to speed up the dissolving efficiency of the materials, so that the materials can be mixed evenly;
- the ground accumulated material will flow back into the reactor body 1;
- the material component 14 it is transported to the grinding mechanism 9, and the large-particle materials can be ground at the grinding component 2, and the large-particle materials are ground and thinned, and the dissolution of the materials is accelerated; this can not only allow the materials to be fully dissolved, It makes the mixing of materials more uniform. First, it can prevent undissolved materials from blocking the discharge port 5 of the reactor body 1.
- the addition of the grinding process can make the material dissolve faster and reduce the stirring time; at the same time, the material is uniformly mixed during the grinding process.
- the grinding mechanism 9 includes an upper grinding disc assembly 15 and a lower grinding disc assembly 16;
- the upper grinding disc assembly 15 includes an upper grinding disc 17, the upper grinding disc 17 is provided with a collection groove 18 having a hemispherical structure, and the lower end of the upper grinding disc 17 is provided with a first grinding tooth; the collecting groove 18 and the lower end of the upper grinding disc 17 There are several guide channels 19 between them, and the upper grinding disc 17 is fixedly installed on the grinding shaft 8;
- the lower grinding assembly 2 includes a base 20 and a lower grinding disc 21.
- the base 20 is fixedly installed in the reactor body 1 through a support frame 30, a positioning protrusion 22 is provided in the middle of the base 20, and a mounting hole 23 is provided in the middle of the lower grinding disc 21.
- An extension portion 24 is provided, a second grinding tooth is provided on the upper end surface of the lower grinding disc 21, the lower grinding disc 21 is slidably mounted on the base 20 through the positioning protrusion 22 and the mounting hole 23, and a limiting portion 25 is provided on the extending portion 24,
- the stirring shaft 12 passes through the base 20;
- a limiting component 26 is arranged to prevent the lower grinding disc 21 from rotating, and a strong spring 27 is arranged between the lower grinding disc 21 and the base 20 .
- the mixed liquid with undissolved materials will enter the collecting tank 18 under the action of the circulating feeding component 14, and then flow through the material guiding channel 19 and then enter the upper grinding disc 17 and the lower grinding plate 17.
- the grinding area formed between the discs 21 is ground; during grinding, the upper grinding disc 17 rotates, and the lower grinding disc 21 will not rotate under the action of the limiting component 26; in this way, the undissolved material can be mixed. Liquid grinding.
- the limiting component 26 includes a limiting column 28 provided on the lower grinding disc 21 and a limiting hole 29 provided on the base 20 that can cooperate with the limiting column 28, and each limiting component 26 is provided with a
- the strong spring 27 is sleeved on the limit post 28 , the upper end of the strong spring 27 is in contact with the lower grinding disc 21 , and the lower end is in contact with the base 20 .
- the lower grinding disc 21 can be placed to rotate to affect the grinding effect; and the provided strong spring 27 can push the lower grinding disc 21 against the upper grinding disc 17.
- the dissolved particles are larger, and can also achieve normal grinding; at the same time, under the action of the strong spring 27, the grinding effect of the material can be further improved.
- the limiting portion 25 is an annular limiting plate screwed on the extension portion 24 ;
- the end of the support frame 30 is provided with a connecting seat 31
- the reactor body 1 is provided with a mounting seat 42
- the connecting seat 31 and the mounting seat 42 are connected by bolts, which facilitates the installation of the base 20 .
- the included angle between the axis line of the material guide channel 19 and the axis line of the upper grinding disc 17 is 45°.
- the inclined material guide channel 19 can make the undissolved material mixture enter the upper grinding disc 17 and the lower grinding disc 21 more conveniently.
- the discharge valve 6 is a two-way valve
- the circulating feeding component 14 includes a material pipe 32 and a material pump 33.
- One end of the two-way valve of the material pipe 32 is connected to one of the outlet ends, and the other end extends into the reactor body 1, and the material
- the discharge end of the pipe 32 is located above the collecting tank 18 , and the material pump 33 is installed on the material pipe 32 .
- the undissolved large granular materials will accumulate at the bottom of the reactor body 1, and the undissolved materials can be sent to the grinding mechanism 9 through the action of the material pump 33; the two-way valve also Able to achieve the purpose of cutting.
- an aeration device 34 is also installed on the reactor body 1, and the aeration device 34 includes a filter 35, a fan 36 and an aeration plate 37.
- the filter 35 and the fan 36 are installed on the reactor body 1, and the aeration plate 37 is installed in the reactor body 1 and is located under the stirring assembly 3.
- the aeration plate 37 is provided with a number of aeration holes 38, and the aeration plate 37 passes through.
- the pipeline is connected with the fan 36 , the fan 36 is connected with the filter 35 , and the filter 35 is communicated with the reactor body 1 ;
- the material can be disturbed by the pumped air when the material is stirred, so as to further improve the mixing effect of the material.
- each aeration hole 38 is provided with an aeration nozzle 40 , a material blocking cap 41 is provided above the outlet of the aeration nozzle 40 , and the material blocking cap 41 is connected to the aeration nozzle 40 .
- the provided aeration plate 37 can also play a blocking role, reducing the influence of the stirring component 3 on the materials deposited at the bottom of the reactor body 1 during stirring, and facilitating the circulation of the materials deposited by the feeding component 14. Sent to the grinding mechanism 9.
- the edge of the upper grinding disc 17 is provided with a baffle plate 43 inclined in the axial direction of the upper grinding disc 17, so that after the material enters the collecting tank 18, under the action of the centrifugal force of the upper grinding disc 17, The material can be effectively placed to splash, so that it can better enter the material guide channel 19 .
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Abstract
Disclosed is a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps: step 1: adding phosphoric acid, urea, a curing agent and a polymerization aid into a reactor, stirring the reaction at 70-135 °C for 60-180 minutes to obtain a reaction slurry, and controlling the polymerization rate of phosphorus in the slurry to be 10%-50%; step 2: adding the reaction slurry into a curing device, controlling the temperature of the slurry at 150-220 °C, drying and curing the slurry for 30-90 minutes to obtain a solid material, and controlling the polymerization rate of phosphorus in the dried and cured solid material to be 85%-99%; and step 3: removing the solid material from the curing device and cooling same to 40-70 °C, and then crushing same, so as to obtain a powdery high-solubility nitrogen-phosphorus water-soluble fertilizer. The method is used for quickly preparing the high-solubility nitrogen-phosphorus water-soluble fertilizer, and has the advantage of simple process.
Description
本发明涉及一种水溶肥制备技术领域，具体涉及一种高溶解度氮磷水溶肥制备方法。The invention relates to the technical field of preparation of a water-soluble fertilizer, in particular to a preparation method of a high-solubility nitrogen-phosphorus water-soluble fertilizer.
水溶肥是指能够完全溶解于水的含氮、磷、钾、钙、镁、微量元素、氨基酸、腐植酸、海藻酸等复合型肥料，从形态分有固体水溶肥和液体水溶肥两种，它是一种速效性肥料，水溶性好、无残渣，可以完全溶解于水中，能被作物的根系和叶面直接吸收利用，采用水肥同施，以水带肥，实现了水肥一体化，它的有效吸收率高出普通化肥一倍多，而且肥效快，可解决高产作物快速生长期的营养需求，而施肥作业几乎可以不用人工，大大节约了人力成本。Water-soluble fertilizer refers to compound fertilizers containing nitrogen, phosphorus, potassium, calcium, magnesium, trace elements, amino acids, humic acid, alginic acid, etc. that can be completely dissolved in water. It is a quick-acting fertilizer with good water solubility and no residue. It can be completely dissolved in water and can be directly absorbed and utilized by the roots and leaves of crops. The effective absorption rate of the fertilizer is more than double that of ordinary chemical fertilizers, and the fertilizer effect is fast, which can meet the nutritional needs of high-yield crops during the rapid growth period, and the fertilization operation is almost free of labor, which greatly saves labor costs.
常见氮磷水溶肥(如磷酸二氢铵、磷酸氢二铵、磷酸脲、聚磷酸铵等)的溶解度普遍在约20-180克/100克水，高溶解度的水溶肥更受“水肥一体化”的现代农业欢迎，因此，如何快速制备高溶解度的氮磷水溶肥是我们需要解决的技术问题。The solubility of common nitrogen and phosphorus water-soluble fertilizers (such as ammonium dihydrogen phosphate, diammonium hydrogen phosphate, urea phosphate, ammonium polyphosphate, etc.) is generally about 20-180 grams per 100 grams of water, and water-soluble fertilizers with high solubility are more affected by "water and fertilizer integration". "The modern agriculture welcomes, therefore, how to quickly prepare high solubility nitrogen and phosphorus water-soluble fertilizer is a technical problem we need to solve.
发明内容SUMMARY OF THE INVENTION
本发明的目的在于提供一种高溶解度氮磷水溶肥制备方法，其用于快速制备高溶解度氮磷水溶肥，具有工艺简单的优点。The purpose of the present invention is to provide a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, which is used for rapidly preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, and has the advantage of a simple process.
为解决上述技术问题，本发明所采用的技术方案是：For solving the above-mentioned technical problems, the technical scheme adopted in the present invention is:
一种高溶解度氮磷水溶肥制备方法，包括如下步骤：A method for preparing a high solubility nitrogen and phosphorus water-soluble fertilizer, comprising the following steps:
步骤1：将磷酸、尿素、固化剂、助聚剂加入反应器中，在70～135℃ 下搅拌反应60～180min，得到反应料浆，控制料浆物料中磷的聚合率在10％～50％；Step 1: Add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 70 to 135 ° C for 60 to 180 minutes to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 10% to 50%. %;
步骤2：将反应料浆加入到固化器中，控制料浆物料温度在150～220℃，经30～90min料浆干燥固化成固体物料，控制干燥固化成的固体物料中磷的聚合率在85％～99％；Step 2: Add the reaction slurry into the solidifier, control the temperature of the slurry material at 150-220 °C, and dry and solidify the slurry into a solid material for 30-90 minutes, and control the polymerization rate of phosphorus in the solid material dried and solidified to be 85. %～99%;
步骤3：固体物料出固化器冷却至40～70℃后破碎，得到粉粒状氮磷水溶肥。Step 3: The solid material is cooled to 40-70° C. from the solidifier and then crushed to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
其中，在步骤1中，磷酸的P
2O
5质量百分比浓度为40％～50％，并且所述的磷酸与尿素的原料配比为磷酸中P
2O
5与尿素中N的质量比为P
2O
5：N＝2.6～3.5。
Wherein, in step 1, the P 2 O 5 mass percentage concentration of phosphoric acid is 40% to 50%, and the raw material ratio of the phosphoric acid and urea is that the mass ratio of P 2 O 5 in phosphoric acid to N in urea is P 2 O 5 : N=2.6 to 3.5.
进一步限定，在步骤1中，固化剂为氧化镁、氢氧化镁、硫酸镁、磷酸氢镁、磷酸镁，硫酸铁、硫酸亚铁、磷酸铁、氧化铁、氢氧化铁、氢氧化亚铁、硫酸铝、磷酸铝、氧化铝、氢氧化铝、氧化钙、氢氧化钙、磷酸二氢钙、磷酸氢钙中的一种或几种。Further limiting, in step 1, the curing agent is magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium hydrogen phosphate, magnesium phosphate, iron sulfate, ferrous sulfate, iron phosphate, iron oxide, iron hydroxide, ferrous hydroxide, One or more of aluminum sulfate, aluminum phosphate, aluminum oxide, aluminum hydroxide, calcium oxide, calcium hydroxide, calcium dihydrogen phosphate, and calcium hydrogen phosphate.
其中，所述固化剂的加入量为固化剂中铁镁铝钙元素质量与磷酸中P
2O
5的质量比为M
1：P
2O
5＝0.04～0.10，其中M
1为固化剂中铁镁铝钙元素质量总和；
Wherein , the added amount of the curing agent is the mass ratio of the iron, magnesium, aluminum, and calcium elements in the curing agent to the mass ratio of P 2 O 5 in the phosphoric acid . The sum of the mass of calcium elements;
其中，步骤1中的所述助聚剂为步骤3所得到的粉粒状氮磷水溶肥，所述的助聚剂的加入量为助聚剂质量与磷酸中P
2O
5的质量比为M
2：P
2O
5＝0.04～0.10，其中M
2为助聚剂加入质量。
Wherein, the described polymerization aid in step 1 is the powdery granular nitrogen-phosphorus water-soluble fertilizer obtained in step 3, and the added amount of described polymerization aid is the mass ratio of the mass of the polymerization aid to P 2 O 5 in phosphoric acid, which is M 2 : P 2 O 5 =0.04-0.10, wherein M 2 is the mass of the polymerization aid added.
其中，所述的磷酸及固化剂可以用湿法磷酸溶剂萃取法净化副产的萃余磷酸代替，该萃余磷酸的P
2O
5质量百分比浓度为40％～50％，该萃余磷酸含有的铁镁铝钙元素质量是该萃余磷酸含有的P
2O
5质量的4％～10％。
Wherein, the phosphoric acid and the curing agent can be replaced by raffinate phosphoric acid purifying by-products by wet-process phosphoric acid solvent extraction, the P 2 O 5 mass percentage concentration of the raffinate phosphoric acid is 40% to 50%, and the raffinate phosphoric acid contains The mass of iron, magnesium, aluminum, and calcium elements is 4% to 10% of the mass of P 2 O 5 contained in the raffinate phosphoric acid.
进一步优化，步骤1和步骤2中，所述磷的聚合率为物料中有效磷含量与正磷酸盐含量的差值同有效磷含量的比值。Further optimization, in steps 1 and 2, the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
其中，步骤3中，所述粉粒状氮磷水溶肥的氮含量为12％～18％，P
2O
5含量为55％～64％，溶解度为300～500g/100g水。
Wherein, in step 3, the nitrogen content of the powder and granular nitrogen and phosphorus water-soluble fertilizer is 12%-18%, the P2O5 content is 55 %-64%, and the solubility is 300-500g/100g water.
与现有技术相比，本发明具有以下有益效果：Compared with the prior art, the present invention has the following beneficial effects:
本发明通过磷酸、尿素、固化剂、助聚剂来制备高溶解度氮磷水溶肥，通过加温搅拌来制取反应料浆，然后将反应料浆固化干燥后破碎即可制得高溶解度氮磷水溶肥，其制备工艺简单，能够实现高溶解度氮磷水溶肥快速制备的目的。The present invention prepares high-solubility nitrogen-phosphorus water-soluble fertilizer through phosphoric acid, urea, curing agent and polymerization aid, prepares reaction slurry by heating and stirring, and then solidifies and dries the reaction slurry and crushes it to obtain high-solubility nitrogen-phosphorus fertilizer The water-soluble fertilizer has a simple preparation process and can achieve the purpose of rapid preparation of a high-solubility nitrogen-phosphorus water-soluble fertilizer.
同时，该高溶解度氮磷水溶肥的溶解度为300～500g/100g水，远高于市场上常见氮磷水溶肥(如磷酸二氢铵、磷酸氢二铵、磷酸脲、聚磷酸铵等)的溶解度，高溶解度的水溶肥更受“水肥一体化”的现代农业欢迎。At the same time, the solubility of the high solubility nitrogen and phosphorus water-soluble fertilizer is 300-500g/100g water, which is much higher than that of common nitrogen and phosphorus water-soluble fertilizers on the market (such as ammonium dihydrogen phosphate, diammonium hydrogen phosphate, urea phosphate, ammonium polyphosphate, etc.). Solubility, water-soluble fertilizers with high solubility are more popular in modern agriculture with "water and fertilizer integration".
为了更清楚地说明本发明实施方式的技术方案，下面将对实施方式中所需要使用的附图作简单地介绍，应当理解，以下附图仅示出了本发明的某些实施例，因此不应被看作是对范围的限定，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他相关的附图。In order to illustrate the technical solutions of the embodiments of the present invention more clearly, the following briefly introduces the accompanying drawings used in the embodiments. It should be understood that the following drawings only show some embodiments of the present invention, and therefore do not It should be regarded as a limitation of the scope, and for those of ordinary skill in the art, other related drawings can also be obtained according to these drawings without any creative effort.
图1为本发明所述反应器的整体结构示意图。FIG. 1 is a schematic diagram of the overall structure of the reactor according to the present invention.
图2为本发明图1中A处局部放大示意图。FIG. 2 is an enlarged schematic diagram of a part of A in FIG. 1 of the present invention.
图3为本发明图1中B处局部放大示意图。FIG. 3 is an enlarged schematic diagram of a part of B in FIG. 1 of the present invention.
附图标记：1-反应器本体，2-研磨组件，3-搅拌组件，4-进料口，5-出料口，6-出料阀，7-研磨电机，8-研磨轴，9-研磨机构，10-传动 机构，11-搅拌电机，12-搅拌轴，13-搅拌杆，14-循环给料组件，15-上研磨盘组件,16-下研磨盘组件,17-上研磨盘,18-集料槽,19-导料通道,20-底座,21-下研磨盘,22-定位凸起，23-安装孔，24-延伸部，25-限位部，26-限位组件，27-强力弹簧，28-限位柱，29-限位孔，30-支撑架，31-连接座，32-料管，33-料泵，34-曝气装置，35-过滤器，36-风机，37-曝气盘，38-曝气孔，39-单向电磁阀，40-曝气喷嘴，41-挡料帽，42-安装座。Reference numerals: 1-reactor body, 2-grinding assembly, 3-stirring assembly, 4-feeding port, 5-feeding port, 6-feeding valve, 7-grinding motor, 8-grinding shaft, 9- Grinding mechanism, 10-transmission mechanism, 11-stirring motor, 12-stirring shaft, 13-stirring rod, 14-circulating feeding component, 15-upper grinding disc component, 16-lower grinding disc component, 17-upper grinding disc, 18-collection chute, 19-material guide channel, 20-base, 21-lower grinding disc, 22-positioning protrusion, 23-installation hole, 24-extension part, 25-limiting part, 26-limiting component, 27-Strong spring, 28-Limiting column, 29-Limiting hole, 30-Support frame, 31-Connecting seat, 32-Material pipe, 33-Material pump, 34-Aeration device, 35-Filter, 36- Fan, 37-aeration plate, 38-aeration hole, 39-one-way solenoid valve, 40-aeration nozzle, 41-blocking cap, 42-mounting seat.
下面结合实施例对本发明作进一步的描述，所描述的实施例仅仅是本发明一部分实施例，并不是全部的实施例。基于本发明中的实施例，本领域的普通技术人员在没有做出创造性劳动前提下所获得的其他所用实施例，都属于本发明的保护范围。The present invention will be further described below with reference to the embodiments, and the described embodiments are only a part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, other used embodiments obtained by persons of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
实施例一Example 1
本实施例公开了一种高溶解度氮磷水溶肥制备方法，包括如下步骤：The present embodiment discloses a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps:
步骤1：将磷酸、尿素、固化剂、助聚剂加入反应器中，在70℃下搅拌反应60min，得到反应料浆，控制料浆物料中磷的聚合率在10％；Step 1: add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 70° C. for 60 minutes to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 10%;
步骤2：将反应料浆加入到固化器中，控制料浆物料温度在150℃，经30min料浆干燥固化成固体物料，控制干燥固化成的固体物料中磷的聚合率在85％；Step 2: adding the reaction slurry into the solidifier, controlling the temperature of the slurry material at 150°C, drying the slurry for 30 minutes and solidifying it into a solid material, and controlling the polymerization rate of phosphorus in the solid material dried and solidified to be 85%;
步骤3：固体物料出固化器冷却至40℃后破碎，得到粉粒状氮磷水溶肥。Step 3: The solid material is cooled to 40°C and then crushed from the solidifier to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
其中，在步骤1中，磷酸的P
2O
5质量百分比浓度为40％，并且所述的磷酸与尿素的原料配比为磷酸中P
2O
5与尿素中N的质量比为P
2O
5： N＝2.6。
Wherein, in step 1, the P 2 O 5 mass percentage concentration of phosphoric acid is 40%, and the raw material ratio of the phosphoric acid and urea is that the mass ratio of P 2 O 5 in phosphoric acid to N in urea is P 2 O 5 : N=2.6.
进一步限定，在步骤1中，固化剂为氧化镁、氢氧化镁、硫酸镁、磷酸氢镁、磷酸镁及硫酸铁的混合物。Further limited, in step 1, the curing agent is a mixture of magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium hydrogen phosphate, magnesium phosphate and iron sulfate.
其中，所述固化剂的加入量为固化剂中铁镁铝钙元素质量与磷酸中P
2O
5的质量比为M
1：P
2O
5＝0.04，其中M
1为固化剂中铁镁铝钙元素质量总和；
Wherein, the added amount of the curing agent is that the mass ratio of iron-magnesium-aluminum-calcium elements in the curing agent to P 2 O 5 in the phosphoric acid is M 1 : P 2 O 5 =0.04, wherein M 1 is the iron, magnesium, aluminum, and calcium elements in the curing agent. mass sum;
进一步限定，步骤1中的所述助聚剂为步骤3所得到的粉粒状氮磷水溶肥，所述的助聚剂的加入量为助聚剂质量与磷酸中P
2O
5的质量比为M
2：P
2O
5＝0.04，其中M
2为助聚剂加入质量。
Further limit, the described polymerization aid in step 1 is the powdery granular nitrogen-phosphorus water-soluble fertilizer obtained in step 3, and the added amount of described polymerization aid is the mass ratio of the mass of the polymerization aid to P 2 O 5 in phosphoric acid: M 2 : P 2 O 5 =0.04, wherein M 2 is the mass of the polymerization aid added.
其中，步骤1和步骤2中，所述磷的聚合率为物料中有效磷含量与正磷酸盐含量的差值同有效磷含量的比值。Wherein, in step 1 and step 2, the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
进一步优化，步骤3中，所述粉粒状氮磷水溶肥的氮含量为18％，P
2O
5含量为55％，溶解度为300g/100g水。
Further optimization, in step 3, the nitrogen content of the powder and granular nitrogen and phosphorus water-soluble fertilizer is 18%, the P 2 O 5 content is 55%, and the solubility is 300g/100g water.
本发明通过磷酸、尿素、固化剂、助聚剂来制备高溶解度氮磷水溶肥，通过加温搅拌来制取反应料浆，然后将反应料浆固化干燥后破碎即可制得高溶解度氮磷水溶肥，其制备工艺简单，能够实现高溶解度氮磷水溶肥快速制备的目的。The present invention prepares high-solubility nitrogen-phosphorus water-soluble fertilizer through phosphoric acid, urea, curing agent and polymerization aid, prepares reaction slurry by heating and stirring, and then solidifies and dries the reaction slurry and crushes it to obtain high-solubility nitrogen-phosphorus fertilizer The water-soluble fertilizer has a simple preparation process and can achieve the purpose of rapid preparation of a high-solubility nitrogen-phosphorus water-soluble fertilizer.
实施例二 Embodiment 2
本实施例公开了一种高溶解度氮磷水溶肥制备方法，包括如下步骤：The present embodiment discloses a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps:
步骤1：将磷酸、尿素、固化剂、助聚剂加入反应器中，在100℃下搅拌反应90min，得到反应料浆，控制料浆物料中磷的聚合率在35％；Step 1: add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 100° C. for 90 minutes to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 35%;
步骤2：将反应料浆加入到固化器中，控制料浆物料温度在180℃，经60min料浆干燥固化成固体物料，控制干燥固化成的固体物料中磷的聚合率在95％；Step 2: adding the reaction slurry into the solidifier, controlling the temperature of the slurry material to be 180°C, drying the slurry for 60 minutes and solidifying it into a solid material, and controlling the polymerization rate of phosphorus in the solid material dried and solidified to be 95%;
步骤3：固体物料出固化器冷却至50℃后破碎，得到粉粒状氮磷水溶肥。Step 3: The solid material is cooled to 50°C and then crushed from the solidifier to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
其中，在步骤1中，磷酸的P
2O
5质量百分比浓度为45％，并且所述的磷酸与尿素的原料配比为磷酸中P
2O
5与尿素中N的质量比为P
2O
5：N＝3。
Wherein, in step 1, the P 2 O 5 mass percentage concentration of phosphoric acid is 45%, and the raw material ratio of the phosphoric acid and urea is that the mass ratio of P 2 O 5 in phosphoric acid to N in urea is P 2 O 5 : N=3.
进一步限定，在步骤1中，固化剂为氧化镁、氢氧化镁、硫酸镁、磷酸氢镁、磷酸镁，硫酸铁、硫酸亚铁、磷酸铁、氧化铁、氢氧化铁、氢氧化亚铁、硫酸铝、磷酸铝、氧化铝、氢氧化铝、氧化钙、氢氧化钙、磷酸二氢钙或磷酸氢钙，在本实施例中，固化剂为氢氧化铝。Further limiting, in step 1, the curing agent is magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium hydrogen phosphate, magnesium phosphate, iron sulfate, ferrous sulfate, iron phosphate, iron oxide, iron hydroxide, ferrous hydroxide, Aluminum sulfate, aluminum phosphate, aluminum oxide, aluminum hydroxide, calcium oxide, calcium hydroxide, calcium dihydrogen phosphate or calcium hydrogen phosphate, in this embodiment, the curing agent is aluminum hydroxide.
其中，所述固化剂的加入量为固化剂中铁镁铝钙元素质量与磷酸中P
2O
5的质量比为M
1：P
2O
5＝0.06，其中M
1为固化剂中铁镁铝钙元素质量总和；
Wherein, the added amount of the curing agent is that the mass ratio of the iron-magnesium-aluminum-calcium element in the curing agent to the P 2 O 5 in the phosphoric acid is M 1 : P 2 O 5 =0.06, wherein M 1 is the iron-magnesium-aluminum-calcium element in the curing agent mass sum;
进一步限定，步骤1中的所述助聚剂为步骤3所得到的粉粒状氮磷水溶肥，所述的助聚剂的加入量为助聚剂质量与磷酸中P
2O
5的质量比为M
2：P
2O
5＝0.06，其中M
2为助聚剂加入质量。
Further limit, the described polymerization aid in step 1 is the powdery granular nitrogen-phosphorus water-soluble fertilizer obtained in step 3, and the added amount of described polymerization aid is the mass ratio of the mass of the polymerization aid to P 2 O 5 in phosphoric acid: M 2 : P 2 O 5 =0.06, wherein M 2 is the mass of the polymerization aid added.
其中，步骤1和步骤2中，所述磷的聚合率为物料中有效磷含量与正磷酸盐含量的差值同有效磷含量的比值。Wherein, in step 1 and step 2, the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
进一步优化，步骤3中，所述粉粒状氮磷水溶肥的氮含量为16％，P
2O
5含量为60％，溶解度为400g/100g水。
Further optimization, in step 3, the nitrogen content of the powdered and granular nitrogen and phosphorus water-soluble fertilizer is 16 %, the P2O5 content is 60%, and the solubility is 400g/100g water.
实施例三 Embodiment 3
本实施例公开了一种高溶解度氮磷水溶肥制备方法，包括如下步骤：The present embodiment discloses a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps:
步骤1：将磷酸、尿素、固化剂、助聚剂加入反应器中，在135℃下搅拌反应180min，得到反应料浆，控制料浆物料中磷的聚合率在50％；Step 1: add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 135 ° C for 180 min to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 50%;
步骤2：将反应料浆加入到固化器中，控制料浆物料温度在220℃，经90min料浆干燥固化成固体物料，控制干燥固化成的固体物料中磷的 聚合率在99％；Step 2: adding the reaction slurry into the solidifier, controlling the temperature of the slurry material at 220°C, drying the slurry for 90 minutes and solidifying it into a solid material, and controlling the polymerization rate of phosphorus in the solid material dried and solidified to be 99%;
步骤3：固体物料出固化器冷却至70℃后破碎，得到粉粒状氮磷水溶肥。Step 3: The solid material is cooled to 70°C from the solidifier and then crushed to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
其中，在步骤1中，磷酸的P
2O
5质量百分比浓度为50％，并且所述的磷酸与尿素的原料配比为磷酸中P
2O
5与尿素中N的质量比为P
2O
5：N＝3.5。
Wherein, in step 1, the P 2 O 5 mass percentage concentration of phosphoric acid is 50%, and the raw material ratio of the phosphoric acid and urea is that the mass ratio of P 2 O 5 in phosphoric acid to N in urea is P 2 O 5 : N=3.5.
进一步限定，在步骤1中，固化剂为氧化镁、氢氧化镁、硫酸镁、磷酸氢镁、磷酸镁，硫酸铁、硫酸亚铁、磷酸铁、氧化铁、氢氧化铁、氢氧化亚铁、硫酸铝的混合物。Further limiting, in step 1, the curing agent is magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium hydrogen phosphate, magnesium phosphate, iron sulfate, ferrous sulfate, iron phosphate, iron oxide, iron hydroxide, ferrous hydroxide, A mixture of aluminum sulfate.
其中，所述固化剂的加入量为固化剂中铁镁铝钙元素质量与磷酸中P
2O
5的质量比为M
1：P
2O
5＝0.10，其中M
1为固化剂中铁镁铝钙元素质量总和；
Wherein, the added amount of the curing agent is that the mass ratio of iron-magnesium-aluminum-calcium element in the curing agent to P 2 O 5 in the phosphoric acid is M 1 : P 2 O 5 =0.10, wherein M 1 is the iron-magnesium-aluminum-calcium element in the curing agent mass sum;
进一步限定，步骤1中的所述助聚剂为步骤3所得到的粉粒状氮磷水溶肥，所述的助聚剂的加入量为助聚剂质量与磷酸中P
2O
5的质量比为M
2：P
2O
5＝0.10，其中M
2为助聚剂加入质量。
It is further limited that the polymerization aid in step 1 is the powdery and granular nitrogen-phosphorus water-soluble fertilizer obtained in step 3, and the addition of the polymerization aid is the mass ratio of the mass of the polymerization aid to P 2 O 5 in phosphoric acid. M 2 : P 2 O 5 =0.10, wherein M 2 is the mass of the polymerization aid added.
其中，步骤1和步骤2中，所述磷的聚合率为物料中有效磷含量与正磷酸盐含量的差值同有效磷含量的比值。Wherein, in step 1 and step 2, the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
进一步优化，步骤3中，所述粉粒状氮磷水溶肥的氮含量为12％，P
2O
5含量为64％，溶解度为500g/100g水。
Further optimization, in step 3, the nitrogen content of the powdered and granular nitrogen and phosphorus water-soluble fertilizer is 12 %, the P2O5 content is 64%, and the solubility is 500g/100g water.
实施例四Embodiment 4
本实施例公开了一种高溶解度氮磷水溶肥制备方法，包括如下步骤：The present embodiment discloses a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps:
步骤1：将磷酸、尿素、固化剂、助聚剂加入反应器中，在70℃下搅拌反应60min，得到反应料浆，控制料浆物料中磷的聚合率在10％；Step 1: add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 70° C. for 60 minutes to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 10%;
步骤2：将反应料浆加入到固化器中，控制料浆物料温度在150℃， 经30min料浆干燥固化成固体物料，控制干燥固化成的固体物料中磷的聚合率在85％；Step 2: adding the reaction slurry into the solidifier, controlling the temperature of the slurry material at 150°C, drying the slurry for 30 minutes and solidifying it into a solid material, and controlling the polymerization rate of phosphorus in the solid material dried and solidified to be 85%;
步骤3：固体物料出固化器冷却至40℃后破碎，得到粉粒状氮磷水溶肥。Step 3: The solid material is cooled to 40°C and then crushed from the solidifier to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
其中，在步骤1中，加入的磷酸及固化剂为用湿法磷酸溶剂萃取法净化副产的萃余磷酸，该萃余磷酸的P
2O
5质量百分比浓度为40％，该萃余磷酸含有的铁镁铝钙元素质量是该萃余磷酸含有的P
2O
5质量的4％，所述的萃余磷酸与尿素的原料配比为萃余磷酸中P
2O
5与尿素中N的质量比为P
2O
5：N＝2.6。
Wherein, in step 1, the added phosphoric acid and curing agent are raffinate phosphoric acid purified by wet-process phosphoric acid solvent extraction method, the P 2 O 5 mass percentage concentration of the raffinate phosphoric acid is 40%, and the raffinate phosphoric acid contains The quality of iron, magnesium, aluminum, and calcium elements is 4% of the mass of P 2 O 5 contained in the raffinate phosphoric acid, and the raw material ratio of the raffinate phosphoric acid and urea is the mass of P 2 O 5 in the raffinate phosphoric acid and the quality of N in the urea. The ratio was P 2 O 5 :N=2.6.
进一步限定，步骤1中的所述助聚剂为步骤3所得到的粉粒状氮磷水溶肥，所述的助聚剂的加入量为助聚剂质量与磷酸中P
2O
5的质量比为M
2：P
2O
5＝0.04，其中M
2为助聚剂加入质量。
Further limit, the described polymerization aid in step 1 is the powdery granular nitrogen-phosphorus water-soluble fertilizer obtained in step 3, and the added amount of described polymerization aid is the mass ratio of the mass of the polymerization aid to P 2 O 5 in phosphoric acid: M 2 : P 2 O 5 =0.04, wherein M 2 is the mass of the polymerization aid added.
其中，步骤1和步骤2中，所述磷的聚合率为物料中有效磷含量与正磷酸盐含量的差值同有效磷含量的比值。Wherein, in step 1 and step 2, the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
进一步优化，步骤3中，所述粉粒状氮磷水溶肥的氮含量为18％，P
2O
5含量为55％，溶解度为300g/100g水。
Further optimization, in step 3, the nitrogen content of the powder and granular nitrogen and phosphorus water-soluble fertilizer is 18%, the P 2 O 5 content is 55%, and the solubility is 300g/100g water.
实施例五 Embodiment 5
本实施例公开了一种高溶解度氮磷水溶肥制备方法，包括如下步骤：The present embodiment discloses a method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps:
步骤1：将磷酸、尿素、固化剂、助聚剂加入反应器中，在135℃下搅拌反应180min，得到反应料浆，控制料浆物料中磷的聚合率在50％；Step 1: add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 135 ° C for 180 min to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 50%;
步骤2：将反应料浆加入到固化器中，控制料浆物料温度在220℃，经90min料浆干燥固化成固体物料，控制干燥固化成的固体物料中磷的聚合率在99％；Step 2: adding the reaction slurry into the solidifier, controlling the temperature of the slurry material at 220°C, drying the slurry for 90 minutes and solidifying it into a solid material, and controlling the polymerization rate of phosphorus in the solid material dried and solidified to be 99%;
步骤3：固体物料出固化器冷却至70℃后破碎，得到粉粒状氮磷水 溶肥。Step 3: The solid material is cooled to 70°C after the solidified material is crushed to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
其中，在步骤1中，加入的磷酸及固化剂为用湿法磷酸溶剂萃取法净化副产的萃余磷酸，该萃余磷酸的P
2O
5质量百分比浓度为50％，该萃余磷酸含有的铁镁铝钙元素质量是该萃余磷酸含有的P
2O
5质量的10％，所述的萃余磷酸与尿素的原料配比为萃余磷酸中P
2O
5与尿素中N的质量比为P
2O
5：N＝3.5。
Wherein, in step 1, the added phosphoric acid and curing agent are raffinate phosphoric acid purified by wet-process phosphoric acid solvent extraction method, the P 2 O 5 mass percentage concentration of the raffinate phosphoric acid is 50%, and the raffinate phosphoric acid contains The quality of iron, magnesium, aluminum, and calcium elements is 10% of the quality of P 2 O 5 contained in the raffinate phosphoric acid, and the raw material ratio of the raffinate phosphoric acid and urea is the quality of P 2 O 5 in the raffinate phosphoric acid and N in the urea. The ratio was P 2 O 5 :N=3.5.
进一步限定，步骤1中的所述助聚剂为步骤3所得到的粉粒状氮磷水溶肥，所述的助聚剂的加入量为助聚剂质量与磷酸中P
2O
5的质量比为M
2：P
2O
5＝0.10，其中M
2为助聚剂加入质量。
It is further limited that the polymerization aid in step 1 is the powdery and granular nitrogen-phosphorus water-soluble fertilizer obtained in step 3, and the addition of the polymerization aid is the mass ratio of the mass of the polymerization aid to P 2 O 5 in phosphoric acid. M 2 : P 2 O 5 =0.10, wherein M 2 is the mass of the polymerization aid added.
其中，步骤1和步骤2中，所述磷的聚合率为物料中有效磷含量与正磷酸盐含量的差值同有效磷含量的比值。Wherein, in step 1 and step 2, the polymerization rate of phosphorus is the ratio of the difference between the content of available phosphorus and the content of orthophosphate in the material to the content of available phosphorus.
进一步优化，步骤3中，所述粉粒状氮磷水溶肥的氮含量为12％，P
2O
5含量为64％，溶解度为500g/100g水。
Further optimization, in step 3, the nitrogen content of the powdered and granular nitrogen and phosphorus water-soluble fertilizer is 12 %, the P2O5 content is 64%, and the solubility is 500g/100g water.
实施例六Embodiment 6
在实际的制备中发现，制备高溶解度氮磷水溶肥非常关键的步骤为在步骤1中的搅拌步骤，若在步骤1中进行搅拌时，搅拌不均匀会导致原料混合差，使得后续的生产不稳定，影响高溶解度氮磷水溶肥的制备；因此，申请人对制备高溶解度氮磷水溶肥的反应器进行了改进，以使得原料能够充分溶解混合，保证高溶解度氮磷水溶肥的制备。In the actual preparation, it is found that the most critical step in the preparation of high-solubility nitrogen and phosphorus water-soluble fertilizer is the stirring step in step 1. If the stirring is performed in step 1, the uneven stirring will lead to poor mixing of raw materials, making subsequent production difficult. It is stable and affects the preparation of high-solubility nitrogen-phosphorus water-soluble fertilizer; therefore, the applicant has improved the reactor for preparing high-solubility nitrogen-phosphorus water-soluble fertilizer, so that the raw materials can be fully dissolved and mixed to ensure the preparation of high-solubility nitrogen and phosphorus water-soluble fertilizer.
在步骤1中使用下述结构的反应器来对原料进行搅拌：In step 1, a reactor of the following structure is used to agitate the raw materials:
参看图1-图3；反应器包括呈罐状结构的反应器本体1、安装在反应器本体1内的研磨组件2和搅拌组件3；反应器本体1上端设置有进料口4，下端设置有出料口5，出料口5设置有出料阀6；1-3; the reactor includes a reactor body 1 having a tank-like structure, a grinding assembly 2 and a stirring assembly 3 installed in the reactor body 1; the upper end of the reactor body 1 is provided with a feeding port 4, and the lower end is provided with There is a discharge port 5, and the discharge port 5 is provided with a discharge valve 6;
研磨组件2包括研磨电机7、研磨轴8和研磨机构9，研磨轴8转动安装在反应器本体1上，研磨轴8上端与安装在反应器本体1上的研 磨电机7通过传动机构10连接，研磨机构9设置在研磨轴8的下端，研磨轴8内部中空；The grinding assembly 2 includes a grinding motor 7, a grinding shaft 8 and a grinding mechanism 9, the grinding shaft 8 is rotatably mounted on the reactor body 1, and the upper end of the grinding shaft 8 is connected with the grinding motor 7 installed on the reactor body 1 through the transmission mechanism 10, The grinding mechanism 9 is arranged at the lower end of the grinding shaft 8, and the interior of the grinding shaft 8 is hollow;
搅拌组件3包括搅拌电机11、搅拌轴12和搅拌杆13，搅拌轴12转动安装在研磨轴8内，研磨轴8的轴心线与搅拌轴12的轴心线共线；研磨轴8上端延伸出搅拌轴12后与搅拌电机11连接，所述搅拌杆13有多个且固定安装在搅拌轴12上；反应器本体1上还设置有循环给料组件14，循环给料组件14用于将反应器本体1底部的积料抽取至研磨机构9处研磨后，研磨后的积料将反流回反应器本体1内。The stirring assembly 3 includes a stirring motor 11, a stirring shaft 12 and a stirring rod 13. The stirring shaft 12 is rotatably installed in the grinding shaft 8, and the axis line of the grinding shaft 8 is collinear with that of the stirring shaft 12; the upper end of the grinding shaft 8 extends After exiting the stirring shaft 12, it is connected to the stirring motor 11. There are a plurality of the stirring rods 13 and are fixedly installed on the stirring shaft 12; After the accumulated material at the bottom of the reactor body 1 is extracted to the grinding mechanism 9 for grinding, the ground accumulated material will flow back into the reactor body 1 .
这样，将原料投入反应器本体1内后，通过搅拌组件3对物料进行搅拌，加快物料的溶解效率，使得物料能够均匀的混合；由于设置有循环给料组件14，循环给料组件14用于将反应器本体1底部的积料抽取至研磨机构9处研磨后，研磨后的积料将反流回反应器本体1内；聚集在反应器本体1底部的大颗粒的物料将会在循环给料组件14的作用下运送至研磨机构9处，大颗粒的物料能够在研磨组件2处进行研磨，将大颗粒的物料研磨变细，加快物料的溶解；这样既可使得物料能够充分的溶解，使得物料的混合更加均匀，一是能够防止未溶解的物料将反应器本体1出料口5堵塞，二是保证了物料的充分溶解，物料混合更加均匀，保证后续生产的正常进行；三是通过研磨工艺的加入，能够使得物料的溶解速度更快，减少搅拌的时间；同时，在研磨的过程中也实现了对物料的均匀混合。In this way, after the raw materials are put into the reactor body 1, the materials are stirred by the stirring component 3 to speed up the dissolving efficiency of the materials, so that the materials can be mixed evenly; After the accumulated material at the bottom of the reactor body 1 is extracted to the grinding mechanism 9 for grinding, the ground accumulated material will flow back into the reactor body 1; Under the action of the material component 14, it is transported to the grinding mechanism 9, and the large-particle materials can be ground at the grinding component 2, and the large-particle materials are ground and thinned, and the dissolution of the materials is accelerated; this can not only allow the materials to be fully dissolved, It makes the mixing of materials more uniform. First, it can prevent undissolved materials from blocking the discharge port 5 of the reactor body 1. Second, it ensures that the materials are fully dissolved, and the materials are mixed more evenly, so as to ensure the normal progress of subsequent production; The addition of the grinding process can make the material dissolve faster and reduce the stirring time; at the same time, the material is uniformly mixed during the grinding process.
其中，研磨机构9包括上研磨盘组件15和下研磨盘组件16；Wherein, the grinding mechanism 9 includes an upper grinding disc assembly 15 and a lower grinding disc assembly 16;
上研磨盘组件15包括上研磨盘17，上研磨盘17上设置有呈半球形结构的集料槽18，上研磨盘17下端设置有第一研磨齿；集料槽18与上研磨盘17下端之间设置有若干导料通道19，上研磨盘17固定安装在研磨轴8上；The upper grinding disc assembly 15 includes an upper grinding disc 17, the upper grinding disc 17 is provided with a collection groove 18 having a hemispherical structure, and the lower end of the upper grinding disc 17 is provided with a first grinding tooth; the collecting groove 18 and the lower end of the upper grinding disc 17 There are several guide channels 19 between them, and the upper grinding disc 17 is fixedly installed on the grinding shaft 8;
下研磨组件2包括底座20和下研磨盘21，底座20通过支撑架30固定安装在反应器本体1内，底座20中部设置有定位凸起22，下研磨盘21中部设置有安装孔23，边缘设置有延伸部24，下研磨盘21上端面上设置有第二研磨齿，下研磨盘21通过定位凸起22及安装孔23滑动安装在底座20上，延伸部24上设置有限位部25，搅拌轴12穿过所述底座20；The lower grinding assembly 2 includes a base 20 and a lower grinding disc 21. The base 20 is fixedly installed in the reactor body 1 through a support frame 30, a positioning protrusion 22 is provided in the middle of the base 20, and a mounting hole 23 is provided in the middle of the lower grinding disc 21. An extension portion 24 is provided, a second grinding tooth is provided on the upper end surface of the lower grinding disc 21, the lower grinding disc 21 is slidably mounted on the base 20 through the positioning protrusion 22 and the mounting hole 23, and a limiting portion 25 is provided on the extending portion 24, The stirring shaft 12 passes through the base 20;
下研磨盘21与底座20之间设置有防止下研磨盘21转动的限位组件26，在下研磨盘21与底座20之间设置有强力弹簧27。Between the lower grinding disc 21 and the base 20 , a limiting component 26 is arranged to prevent the lower grinding disc 21 from rotating, and a strong spring 27 is arranged between the lower grinding disc 21 and the base 20 .
这样，在实际的使用中，带有未溶解的物料混合液将会在循环给料组件14的作用下进入集料槽18内，然后流经导料通道19后进入上研磨盘17与下研磨盘21之间形成的研磨区域进行研磨；在进行研磨的时候，上研磨盘17转动，下研磨盘21在限位组件26的作用下将不会转动；如此即可实现对未溶解的物料混合液的研磨。In this way, in actual use, the mixed liquid with undissolved materials will enter the collecting tank 18 under the action of the circulating feeding component 14, and then flow through the material guiding channel 19 and then enter the upper grinding disc 17 and the lower grinding plate 17. The grinding area formed between the discs 21 is ground; during grinding, the upper grinding disc 17 rotates, and the lower grinding disc 21 will not rotate under the action of the limiting component 26; in this way, the undissolved material can be mixed. Liquid grinding.
其中，限位组件26包括设置在下研磨盘21上的限位柱28和设置在底座20上能够与所述限位柱28配合的限位孔29，每一个限位组件26均配设一个所述强力弹簧27，强力弹簧27套在限位柱28上，强力弹簧27上端与下研磨盘21接触，下端与底座20接触。Wherein, the limiting component 26 includes a limiting column 28 provided on the lower grinding disc 21 and a limiting hole 29 provided on the base 20 that can cooperate with the limiting column 28, and each limiting component 26 is provided with a The strong spring 27 is sleeved on the limit post 28 , the upper end of the strong spring 27 is in contact with the lower grinding disc 21 , and the lower end is in contact with the base 20 .
这样，在限位柱28及限位孔29的作用下能够放置下研磨盘21发生转动而影响研磨效果；而设置的强力弹簧27能够将下研磨盘21顶在上研磨盘17上，若未溶解的颗粒较大，也能够实现正常研磨；同时，在强力弹簧27的作用下也能够进一步提高物料的研磨效果。In this way, under the action of the limiting column 28 and the limiting hole 29, the lower grinding disc 21 can be placed to rotate to affect the grinding effect; and the provided strong spring 27 can push the lower grinding disc 21 against the upper grinding disc 17. The dissolved particles are larger, and can also achieve normal grinding; at the same time, under the action of the strong spring 27, the grinding effect of the material can be further improved.
其中，限位部25为螺接在延伸部24上的环状限位板；限位部25能够起到限位的作用，放置下研磨盘21脱离底座20。Wherein, the limiting portion 25 is an annular limiting plate screwed on the extension portion 24 ;
进一步优化，支撑架30端部设置有连接座31，反应器本体1内设置有安装座42，连接座31与安装座42通过螺栓连接；便于实现底座20的安装。Further optimization, the end of the support frame 30 is provided with a connecting seat 31 , the reactor body 1 is provided with a mounting seat 42 , and the connecting seat 31 and the mounting seat 42 are connected by bolts, which facilitates the installation of the base 20 .
进一步优化，若干导料通道19倾斜设置在上研磨座上；进一步限定，导料通道19轴心线与上研磨盘17轴心线的夹角为40-50°。Further optimization, several material guide channels 19 are inclined on the upper grinding seat; further limited, the included angle between the axis line of the material guide channel 19 and the axis line of the upper grinding disc 17 is 40-50°.
在本实施例中，导料通道19轴心线与上研磨盘17轴心线的夹角为45°。In this embodiment, the included angle between the axis line of the material guide channel 19 and the axis line of the upper grinding disc 17 is 45°.
这样，在实际的使用中由于上研磨盘17在转动时会产生离心力，通过设置的倾斜的导料通道19，能够使得未溶解的物料混合液更方便的进入上研磨盘17与下研磨盘21之间的研磨区域；同时，也能够保证研磨后能够快速出料。In this way, in actual use, since the upper grinding disc 17 will generate centrifugal force when it rotates, the inclined material guide channel 19 provided can make the undissolved material mixture enter the upper grinding disc 17 and the lower grinding disc 21 more conveniently. The grinding area between them; at the same time, it can also ensure that the material can be discharged quickly after grinding.
其中，出料阀6为二通阀，循环给料组件14包括料管32和料泵33，料管32一端二通阀门其中一个出口端连接，另一端延伸进反应器本体1内，且料管32的出料端位于集料槽18上方，所述料泵33安装在料管32上。Among them, the discharge valve 6 is a two-way valve, and the circulating feeding component 14 includes a material pipe 32 and a material pump 33. One end of the two-way valve of the material pipe 32 is connected to one of the outlet ends, and the other end extends into the reactor body 1, and the material The discharge end of the pipe 32 is located above the collecting tank 18 , and the material pump 33 is installed on the material pipe 32 .
这样，在实际的使用中，未溶解的大颗粒状物料将会聚集在反应器本体1底部，通过料泵33的作用即可将未溶解的物料送至研磨机构9处；二通阀同时还能够实现下料的目的。In this way, in actual use, the undissolved large granular materials will accumulate at the bottom of the reactor body 1, and the undissolved materials can be sent to the grinding mechanism 9 through the action of the material pump 33; the two-way valve also Able to achieve the purpose of cutting.
实施例七 Embodiment 7
本实施例是在实施例四的基础上进一步优化，在本实施例中，反应器本体1上还安装有曝气装置34，曝气装置34包括过滤器35、风机36和曝气盘37，过滤器35、风机36安装在反应器本体1上，曝气盘37安装在反应器本体1内且位于搅拌组件3下方，曝气盘37上设置有若干曝气孔38，曝气盘37通过管道与风机36连接，风机36与过滤器35 连接，过滤器35与反应器本体1连通；在曝气盘37与风机36之间的管道上设置有单向电磁阀39。This embodiment is further optimized on the basis of Embodiment 4. In this embodiment, an aeration device 34 is also installed on the reactor body 1, and the aeration device 34 includes a filter 35, a fan 36 and an aeration plate 37. The filter 35 and the fan 36 are installed on the reactor body 1, and the aeration plate 37 is installed in the reactor body 1 and is located under the stirring assembly 3. The aeration plate 37 is provided with a number of aeration holes 38, and the aeration plate 37 passes through. The pipeline is connected with the fan 36 , the fan 36 is connected with the filter 35 , and the filter 35 is communicated with the reactor body 1 ;
这样，通过设置的曝气装置34能够在搅拌物料的时候，通过泵入的空气对物料进行扰动，进一步提高物料的混合效果。In this way, when the aeration device 34 is provided, the material can be disturbed by the pumped air when the material is stirred, so as to further improve the mixing effect of the material.
进一步优化，每一个曝气孔38处均设置有一曝气喷嘴40，曝气喷嘴40的出口上方设置有挡料帽41，挡料帽41连接在曝气喷嘴40上。Further optimization, each aeration hole 38 is provided with an aeration nozzle 40 , a material blocking cap 41 is provided above the outlet of the aeration nozzle 40 , and the material blocking cap 41 is connected to the aeration nozzle 40 .
能够有效的防止在加入物料的过程中，颗粒状物料落入曝气孔38内造成曝气盘37的堵塞。This can effectively prevent the blockage of the aeration plate 37 caused by the granular material falling into the aeration hole 38 during the process of adding the material.
更重要的是，通过设置的曝气盘37还能够起到阻挡的作用，减小搅拌组件3在搅拌时对反应器本体1底部沉积的物料的影响，便于循环给料组件14将沉积的物料送至研磨机构9处。More importantly, the provided aeration plate 37 can also play a blocking role, reducing the influence of the stirring component 3 on the materials deposited at the bottom of the reactor body 1 during stirring, and facilitating the circulation of the materials deposited by the feeding component 14. Sent to the grinding mechanism 9.
进一步优化，在实际的使用中，上研磨盘17边缘设置有上研磨盘17轴线方向倾斜的挡料板43，这样，物料进入集料槽18内后，在上研磨盘17离心力的作用下，能够有效的放置物料飞溅，能够使其更好的进入导料通道19。Further optimization, in actual use, the edge of the upper grinding disc 17 is provided with a baffle plate 43 inclined in the axial direction of the upper grinding disc 17, so that after the material enters the collecting tank 18, under the action of the centrifugal force of the upper grinding disc 17, The material can be effectively placed to splash, so that it can better enter the material guide channel 19 .
尽管已描述了本发明的优选实施例，但本领域内的技术人员一旦得知了基本创造性概念，则可对这些实施例作出另外的变更和修改。所以，所附权利要求意欲解释为包括优选实施例以及落入本发明范围的所有变更和修改。以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，应当指出的是，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。Although preferred embodiments of the present invention have been described, additional changes and modifications to these embodiments may occur to those skilled in the art once the basic inventive concepts are known. Therefore, the appended claims are intended to be construed to include the preferred embodiment and all changes and modifications that fall within the scope of the present invention. The above descriptions are only preferred embodiments of the present invention and are not intended to limit the present invention. It should be pointed out that any modifications, equivalent replacements and improvements made within the spirit and principles of the present invention shall include within the protection scope of the present invention.
Claims (8)
- 一种高溶解度氮磷水溶肥制备方法，其特征在于，包括如下步骤：A method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer, comprising the following steps:步骤1：将磷酸、尿素、固化剂、助聚剂加入反应器中，在70～135℃下搅拌反应60～180min，得到反应料浆，控制料浆物料中磷的聚合率在10％～50％；Step 1: Add phosphoric acid, urea, curing agent, and polymerization aid into the reactor, and stir and react at 70 to 135 ° C for 60 to 180 minutes to obtain a reaction slurry, and control the polymerization rate of phosphorus in the slurry material to be 10% to 50%. %;步骤2：将反应料浆加入到固化器中，控制料浆物料温度在150～220℃，经30～90min料浆干燥固化成固体物料，控制干燥固化成的固体物料中磷的聚合率在85％～99％；Step 2: Add the reaction slurry into the solidifier, control the temperature of the slurry material at 150-220 °C, and dry and solidify the slurry into a solid material for 30-90 minutes, and control the polymerization rate of phosphorus in the solid material dried and solidified to be 85. %～99%;步骤3：固体物料出固化器冷却至40～70℃后破碎，得到粉粒状氮磷水溶肥。Step 3: The solid material is cooled to 40-70° C. from the solidifier and then crushed to obtain a powdery nitrogen-phosphorus water-soluble fertilizer.
- 根据权利要求1所述的一种高溶解度氮磷水溶肥制备方法，其特征在于：在步骤1中，磷酸的P 2O 5质量百分比浓度为40％～50％，并且所述的磷酸与尿素的原料配比为磷酸中P 2O 5与尿素中N的质量比为P 2O 5：N＝2.6～3.5。 The method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer according to claim 1, wherein in step 1, the P 2 O 5 mass percentage concentration of phosphoric acid is 40% to 50%, and the phosphoric acid and urea The ratio of raw materials is that the mass ratio of P 2 O 5 in phosphoric acid to N in urea is P 2 O 5 : N=2.6～3.5.
- 根据权利要求1所述的一种高溶解度氮磷水溶肥制备方法，其特征在于：在步骤1中，固化剂为氧化镁、氢氧化镁、硫酸镁、磷酸氢镁、磷酸镁，硫酸铁、硫酸亚铁、磷酸铁、氧化铁、氢氧化铁、氢氧化亚铁、硫酸铝、磷酸铝、氧化铝、氢氧化铝、氧化钙、氢氧化钙、磷酸二氢钙、磷酸氢钙中的一种或几种。A method for preparing a high solubility nitrogen-phosphorus water-soluble fertilizer according to claim 1, characterized in that: in step 1, the curing agent is magnesium oxide, magnesium hydroxide, magnesium sulfate, magnesium hydrogen phosphate, magnesium phosphate, ferric sulfate, One of ferrous sulfate, iron phosphate, iron oxide, iron hydroxide, ferrous hydroxide, aluminum sulfate, aluminum phosphate, aluminum oxide, aluminum hydroxide, calcium oxide, calcium hydroxide, calcium dihydrogen phosphate, calcium hydrogen phosphate species or several.
- 根据权利要求1所述的一种高溶解度氮磷水溶肥制备方法，其特征在于：所述固化剂的加入量为固化剂中铁镁铝钙元素质量与磷酸中P 2O 5的质量比为M 1：P 2O 5＝0.04～0.10，其中M 1为固化剂中铁镁铝钙元素质量总和； A kind of high-solubility nitrogen-phosphorus water-soluble fertilizer preparation method according to claim 1, is characterized in that: the addition amount of described solidifying agent is that the mass ratio of iron-magnesium-aluminum-calcium element mass in the solidifying agent and P 2 O 5 in phosphoric acid is M 1 : P 2 O 5 =0.04～0.10, wherein M 1 is the total mass of iron, magnesium, aluminum, and calcium elements in the curing agent;
- 根据权利要求1所述的一种高溶解度氮磷水溶肥制备方法，其特征在于：步骤1中的所述助聚剂为步骤3所得到的粉粒状氮磷水溶肥，所述的助聚剂的加入量为助聚剂质量与磷酸中P 2O 5的质量比为M 2：P 2O 5＝0.04～0.10，其中M 2为助聚剂加入质量。 The method for preparing a high-solubility nitrogen and phosphorus water-soluble fertilizer according to claim 1, wherein the polymerization aid in step 1 is the powdery and granular nitrogen and phosphorus water-soluble fertilizer obtained in step 3, and the polymerization aid is The added amount is the mass ratio of the mass of the polymerization aid to the P 2 O 5 in the phosphoric acid, M 2 : P 2 O 5 =0.04-0.10, wherein M 2 is the mass of the polymerization aid added.
- 根据权利要求1所述的一种高溶解度氮磷水溶肥制备方法，其特征在于：所述的磷酸及固化剂为用湿法磷酸溶剂萃取法净化副产的萃余磷酸，该萃余磷 酸的P 2O 5质量百分比浓度为40％～50％，该萃余磷酸含有的铁镁铝钙元素质量是该萃余磷酸含有的P 2O 5质量的4％～10％。 The method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer according to claim 1, wherein the phosphoric acid and the curing agent are raffinate phosphoric acid purifying by-products by wet-process phosphoric acid solvent extraction. The mass percentage concentration of P 2 O 5 is 40% to 50%, and the mass of iron, magnesium, aluminum, and calcium elements contained in the raffinate phosphoric acid is 4% to 10% of the mass of P 2 O 5 contained in the raffinate phosphoric acid.
- 根据权利要求1所述的一种高溶解度氮磷水溶肥制备方法，其特征在于：步骤1和步骤2中，所述磷的聚合率为物料中有效磷含量与正磷酸盐含量的差值同有效磷含量的比值。The method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer according to claim 1, wherein in steps 1 and 2, the polymerization rate of the phosphorus is the same as the difference between the content of available phosphorus and the content of orthophosphate in the material. The ratio of available phosphorus content.
- 根据权利要求1所述的一种高溶解度氮磷水溶肥制备方法，其特征在于：步骤3中，所述粉粒状氮磷水溶肥的氮含量为12％～18％，P 2O 5含量为55％～64％，溶解度为300～500g/100g水。 The method for preparing a high-solubility nitrogen-phosphorus water-soluble fertilizer according to claim 1, wherein in step 3, the nitrogen content of the powdery and granular nitrogen-phosphorus water-soluble fertilizer is 12% to 18%, and the P 2 O 5 content is 55%～64%, the solubility is 300～500g/100g water.
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| 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 |
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| CN105621381A (en) * | 2015-12-28 | 2016-06-01 | 川恒生态科技有限公司 | Method for producing full water-soluble solid ammonium polyphosphate from phosphoric acid by wet process |
| CN106348271A (en) * | 2016-08-31 | 2017-01-25 | 广西越洋科技股份有限公司 | Production method for preparing ammonium polyphosphate from wet-process phosphoric acid serving as raw material |
| CN107176597A (en) * | 2017-06-30 | 2017-09-19 | 上海化工研究院有限公司 | A kind of continuous producing method of granular water-soluble poly ammonium phosphate |
| CN109437981A (en) * | 2018-12-27 | 2019-03-08 | 川恒生态科技有限公司 | Fertilizer triammonium polyphosphate and its production method containing microelement in metal |
| CN112624849A (en) * | 2020-12-28 | 2021-04-09 | 瓮福（集团）有限责任公司 | Preparation method of high-solubility nitrogen-phosphorus water-soluble fertilizer |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115430319A (en) * | 2022-08-15 | 2022-12-06 | 什邡市长丰化工有限公司 | Preparation method for entering water-based fertilizer without invalid impurities |
| CN116022757A (en) * | 2022-12-26 | 2023-04-28 | 中南大学 | Preparation method of battery-grade hydrated ferric phosphate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112624849B (en) | 2022-04-05 |
| CN112624849A (en) | 2021-04-09 |
| AU2021411535A1 (en) | 2023-03-09 |
| AU2021411535A8 (en) | 2023-03-16 |
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