CN114249610A - Preparation process and device of ammonium potassium polyphosphate containing chelated medium and trace elements - Google Patents
Preparation process and device of ammonium potassium polyphosphate containing chelated medium and trace elements Download PDFInfo
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- CN114249610A CN114249610A CN202111659226.9A CN202111659226A CN114249610A CN 114249610 A CN114249610 A CN 114249610A CN 202111659226 A CN202111659226 A CN 202111659226A CN 114249610 A CN114249610 A CN 114249610A
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- trace elements
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- potassium
- ammonium
- phosphoric acid
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- 239000011573 trace mineral Substances 0.000 title claims abstract description 73
- 235000013619 trace mineral Nutrition 0.000 title claims abstract description 70
- FQLQNUZHYYPPBT-UHFFFAOYSA-N potassium;azane Chemical compound N.[K+] FQLQNUZHYYPPBT-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 235000019828 potassium polyphosphate Nutrition 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 51
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 150
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 70
- 239000000463 material Substances 0.000 claims abstract description 68
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 67
- 239000011343 solid material Substances 0.000 claims abstract description 67
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 50
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000011574 phosphorus Substances 0.000 claims abstract description 49
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 48
- 239000004202 carbamide Substances 0.000 claims abstract description 48
- 239000002002 slurry Substances 0.000 claims abstract description 48
- 238000003756 stirring Methods 0.000 claims abstract description 46
- 239000012066 reaction slurry Substances 0.000 claims abstract description 44
- 238000001816 cooling Methods 0.000 claims abstract description 42
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000011591 potassium Substances 0.000 claims abstract description 29
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000000654 additive Substances 0.000 claims abstract description 13
- 230000000996 additive effect Effects 0.000 claims abstract description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 230000008569 process Effects 0.000 claims abstract description 11
- 239000003337 fertilizer Substances 0.000 claims description 53
- 239000011777 magnesium Substances 0.000 claims description 35
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 33
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 32
- 235000011151 potassium sulphates Nutrition 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 29
- 239000000126 substance Substances 0.000 claims description 23
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical class [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 22
- DLYUQMMRRRQYAE-UHFFFAOYSA-N tetraphosphorus decaoxide Chemical compound O1P(O2)(=O)OP3(=O)OP1(=O)OP2(=O)O3 DLYUQMMRRRQYAE-UHFFFAOYSA-N 0.000 claims description 18
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 16
- 239000011575 calcium Chemical class 0.000 claims description 16
- 229910052749 magnesium Inorganic materials 0.000 claims description 12
- 239000010949 copper Chemical class 0.000 claims description 11
- 239000011572 manganese Chemical class 0.000 claims description 11
- 239000011701 zinc Chemical class 0.000 claims description 11
- 229910052791 calcium Inorganic materials 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 10
- 229910052748 manganese Inorganic materials 0.000 claims description 10
- 229910052750 molybdenum Chemical class 0.000 claims description 10
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 10
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical class [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 9
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical class [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 9
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical class [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 9
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical class [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical class [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 9
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical class [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 9
- 239000011733 molybdenum Chemical class 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 239000001103 potassium chloride Substances 0.000 claims description 8
- 235000011164 potassium chloride Nutrition 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 229910000402 monopotassium phosphate Inorganic materials 0.000 claims description 6
- 235000019796 monopotassium phosphate Nutrition 0.000 claims description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 6
- 238000007711 solidification Methods 0.000 claims description 6
- 230000008023 solidification Effects 0.000 claims description 6
- PJNZPQUBCPKICU-UHFFFAOYSA-N phosphoric acid;potassium Chemical compound [K].OP(O)(O)=O PJNZPQUBCPKICU-UHFFFAOYSA-N 0.000 claims description 5
- 239000004323 potassium nitrate Substances 0.000 claims description 5
- 235000010333 potassium nitrate Nutrition 0.000 claims description 5
- 239000013522 chelant Substances 0.000 claims description 4
- 229910017053 inorganic salt Inorganic materials 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 3
- 239000002367 phosphate rock Substances 0.000 claims description 3
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 24
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 22
- 235000015097 nutrients Nutrition 0.000 abstract description 15
- 235000011007 phosphoric acid Nutrition 0.000 description 63
- 239000000047 product Substances 0.000 description 43
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 42
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 21
- 235000019341 magnesium sulphate Nutrition 0.000 description 21
- 239000002994 raw material Substances 0.000 description 17
- 239000004114 Ammonium polyphosphate Substances 0.000 description 9
- 235000019826 ammonium polyphosphate Nutrition 0.000 description 9
- 229920001276 ammonium polyphosphate Polymers 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 7
- 238000004519 manufacturing process Methods 0.000 description 7
- 239000002689 soil Substances 0.000 description 7
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 6
- ZCCIPPOKBCJFDN-UHFFFAOYSA-N calcium nitrate Chemical compound [Ca+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ZCCIPPOKBCJFDN-UHFFFAOYSA-N 0.000 description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 5
- 230000000712 assembly Effects 0.000 description 5
- 238000000429 assembly Methods 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 3
- 239000001110 calcium chloride Substances 0.000 description 3
- 229910001628 calcium chloride Inorganic materials 0.000 description 3
- 229910000365 copper sulfate Inorganic materials 0.000 description 3
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 description 3
- 239000011790 ferrous sulphate Substances 0.000 description 3
- 235000003891 ferrous sulphate Nutrition 0.000 description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 3
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 description 3
- 229940099596 manganese sulfate Drugs 0.000 description 3
- 239000011702 manganese sulphate Substances 0.000 description 3
- 235000007079 manganese sulphate Nutrition 0.000 description 3
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 3
- 239000011684 sodium molybdate Substances 0.000 description 3
- 235000015393 sodium molybdate Nutrition 0.000 description 3
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 description 3
- 229960001763 zinc sulfate Drugs 0.000 description 3
- 239000004254 Ammonium phosphate Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- KYAXVUURGCWDJW-UHFFFAOYSA-N [K].P(=O)(O)(O)[O-].[NH4+] Chemical compound [K].P(=O)(O)(O)[O-].[NH4+] KYAXVUURGCWDJW-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 235000019289 ammonium phosphates Nutrition 0.000 description 2
- 150000003863 ammonium salts Chemical class 0.000 description 2
- INQZXVMNJLSCGI-UHFFFAOYSA-M azanium;potassium;hydrogen phosphate Chemical compound [NH4+].[K+].OP([O-])([O-])=O INQZXVMNJLSCGI-UHFFFAOYSA-M 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000004720 fertilization Effects 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 238000003973 irrigation Methods 0.000 description 2
- 230000002262 irrigation Effects 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000618 nitrogen fertilizer Substances 0.000 description 2
- 239000002686 phosphate fertilizer Substances 0.000 description 2
- 229920000137 polyphosphoric acid Polymers 0.000 description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 2
- 239000011644 potassium salts of orthophosphoric acid Substances 0.000 description 2
- 235000019858 potassium salts of orthophosphoric acid Nutrition 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 2
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229920000388 Polyphosphate Polymers 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910021538 borax Inorganic materials 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 235000011180 diphosphates Nutrition 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000012851 eutrophication Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 230000035558 fertility Effects 0.000 description 1
- 239000005431 greenhouse gas Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 235000021048 nutrient requirements Nutrition 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 235000021317 phosphate Nutrition 0.000 description 1
- 230000008979 phosphorus utilization Effects 0.000 description 1
- 239000001205 polyphosphate Substances 0.000 description 1
- 235000011176 polyphosphates Nutrition 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
- 235000011181 potassium carbonates Nutrition 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- 235000011009 potassium phosphates Nutrition 0.000 description 1
- 239000004328 sodium tetraborate Substances 0.000 description 1
- 235000010339 sodium tetraborate Nutrition 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 230000005068 transpiration Effects 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a preparation process and a device of ammonium potassium polyphosphate containing chelated medium and trace elements, wherein the preparation process comprises the following steps: step 1: adding phosphoric acid, urea, potassium and a medium trace element additive into a reactor, and stirring and reacting at 60-90 ℃ for 10-60 min to obtain reaction slurry; step 2: adding the reaction slurry obtained in the step (1) into a polymerization curing device with the absolute pressure of 1-70Kpa, controlling the temperature of the slurry material to be 140-220 ℃, and drying and curing the slurry into a solid material after 20-90 min; and step 3: and cooling the solid material to 30-80 ℃ and then crushing the solid material. The device is mainly used for preparing ammonium potassium polyphosphate containing chelated medium and trace elements. The ammonium potassium polyphosphate prepared by the process simultaneously contains three major elements of nitrogen, phosphorus and potassium and various medium and trace elements, can comprehensively meet the requirements of different crops on nutrients, and has good water solubility under the condition of chelating the medium and trace elements and having the three major element nutrients of nitrogen, phosphorus and potassium.
Description
Technical Field
The invention relates to the technical field of preparation of potassium ammonium polyphosphate, in particular to a preparation process of potassium ammonium polyphosphate containing chelated medium and trace elements; in addition, the invention also relates to a preparation device of ammonium potassium polyphosphate containing chelated medium and trace elements.
Background
Chemical fertilizers are important materials in agricultural production and are important means for ensuring the yield of crops. Under the requirement of ensuring the normal fertilizer demand of crops, how to improve the utilization efficiency of the fertilizer is related to not only the stable yield and high yield of grains but also the environmental protection. The general utilization rate of the solid fertilizer is low, the utilization rate of the solid nitrogen fertilizer is 20-50%, the utilization rate of the solid phosphate fertilizer is 10-25%, and the utilization rate of the solid potassium fertilizer is 40-70%. The important reason for the low utilization rate of the solid fertilizer is that when the fertilizer is applied to soil and the soil has little moisture, the fertilizer is adsorbed by the soil and is difficult to reach the root of crops, the nitrogen fertilizer is decomposed, part of decomposed products are discharged into the atmosphere and are one of sources of greenhouse gases, and the part of the soil, phosphate fertilizer and potassium fertilizer are easy to enter underground water to cause eutrophication in a water system. This not only wastes a large amount of fertilizer, but also creates a validation environmental problem.
A water and fertilizer integrated fertilization mode represented by drip irrigation and spray irrigation is an important means for improving the utilization rate of fertilizer, and the development of high-quality and high-concentration liquid fertilizer is the basis of water and fertilizer integrated development. The liquid fertilizer is prepared by dissolving or dispersing nutrients required by crops in water and preparing the nutrients into a liquid form. Various nutrients absorbed by crops are absorbed through roots and leaf surfaces, wherein a root system is the most important absorption mode, all nutrients are absorbed and conducted by the roots, and water is required to be used as a medium. The existence of moisture can obviously improve the utilization rate of the fertilizer, and can reach more than 90 percent, because the fertilizer is uniformly distributed in the soil along with the moisture in a small quantity of multiple fertilization modes through the integration of water and fertilizer, the fertilizer in the soil moves along with the water through the transpiration effect of the leaf surfaces of the crops, and most of the nutrients are absorbed by the crops.
The water-soluble fertilizer has the characteristics of high nutrient utilization rate in agricultural application, obvious effects of saving expenses and increasing yield, convenient and rapid application, convenient proportion preparation and the like, and is widely used abroad. The compound water-soluble fertilizer with major elements has comprehensive main nutrients of nitrogen, phosphorus and potassium, so that compounding links are reduced during application, and time and labor are saved. Compared with orthophosphate, the polymeric phosphorus nutrient in the fertilizer is not easy to be fixed by soil, and the polymeric phosphorus is slow-release and long-acting. The water-soluble fertilizer contains chelated medium and trace elements, which is helpful for crop growth and improves the quality and yield of agricultural products, thereby achieving the effect of increasing yield and harvest. The water-soluble fertilizer containing three major elements of nitrogen, polymeric phosphorus and potassium and a plurality of chelated medium and trace elements meets the requirement of the development trend of modern agriculture of 'water and fertilizer integration'.
Wherein, US3911086 discloses a method for preparing ammonium potassium polyphosphate with average polymerization degree more than 50, the raw materials are ammonium orthophosphate, ammonium dipolyphosphate, ammonium tripolyphosphate, ammonium tetrapolyphosphate, long-chain polyphosphoric acid, potassium dihydrogen phosphate, potassium carbonate and potassium chloride, and the product is prepared by reacting for 1-16h under the conditions of 200-400 ℃ and introducing ammonia gas. The literature (Journal of agricultural and Food Chemistry (1979),27(3),612-15) discloses that by mixing ammonium and potassium phosphates together, heating to 250 ℃ and 300 ℃ and reacting for 3-16h with ammonia gas, the phosphorus content of the product is higher, but the water-soluble phosphorus content reaches 27% of the total phosphorus content. The ammonium potassium polyphosphate prepared by using the ammonium salt and the potassium salt of orthophosphoric acid or oligomeric phosphoric acid has large polymerization degree and poor water solubility.
The application numbers are: CN201410836414.8, publication number: invention of CN105800583BThe patent discloses oligomeric potassium ammonium phosphate and preparation and application thereof. Taking ammonium salt and potassium salt of orthophosphoric acid as raw materials, reacting in the presence of a condensing agent and auxiliary materials containing nitrogen and potassium nutrients to obtain oligomeric ammonium potassium phosphate with the average polymerization degree of 2-20; wherein, N is P in potassium ammonium phosphate oligomer2O5:K2The mass portion ratio of O is (1-30): (2-45): 1-50. The oligomeric ammonium potassium phosphate is used for preparing fertilizers. The main raw materials adopted by the preparation method are orthophosphate, and compared with the main raw materials of orthophosphoric acid, polyphosphoric acid and phosphorus pentoxide in the existing method, the preparation method has the characteristics of cheap raw materials and low production cost. Meanwhile, the adopted condensing agent can promote the conversion of phosphate radicals in orthophosphate into polyphosphate radicals and provide a raw material of nitrogen nutrients. The phosphorus element of the method selects ammonium phosphate as a raw material, the cost is high, and the obtained product does not contain chelated medium and trace elements.
The application numbers are: CN201410060534.3, publication number: the invention patent of CN103787726B discloses an ammonium polyphosphate water-soluble fertilizer and a preparation method thereof. Adding phosphoric acid, urea, potassium sulfate, zinc chloride, copper chloride, borax and auxiliary materials into a reaction kettle, mixing and dissolving in the kettle, then adding phosphorus pentoxide and stirring uniformly; heating the reaction kettle to 185 ℃ under stirring, reacting for 30-45 minutes, and then heating to 200 ℃ and 205 ℃ for reacting for 1.5-2 hours; and after the reaction is finished, reducing the temperature in the reaction kettle to room temperature, and absorbing ammonia gas generated by the reaction by using a dilute phosphoric acid solution to obtain the catalyst. The ammonium polyphosphate-potassium sulfate water-soluble fertilizer prepared by the invention has the characteristics of good water solubility, low impurity content and high effective content of nitrogen, phosphorus and potassium, and the preparation method has the advantages of simplicity, practicability, low production cost and the like. The method uses high-concentration phosphoric acid and phosphorus pentoxide, and has high raw material requirement and high raw material cost.
Disclosure of Invention
The invention aims to provide a process for preparing ammonium potassium polyphosphate containing chelated medium and trace elements, wherein the ammonium potassium polyphosphate prepared by the process simultaneously contains three major elements of nitrogen, phosphorus and potassium and a plurality of medium and trace elements, can comprehensively meet the requirements of different crops on nutrients, and has good water solubility under the condition of chelating the medium and trace elements and having the three major elements of nitrogen, phosphorus and potassium.
In addition, the invention also discloses a device for preparing the ammonium potassium polyphosphate containing the chelated medium and trace elements, which is mainly used for preparing the ammonium potassium polyphosphate containing the chelated medium and trace elements.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation process of ammonium potassium polyphosphate containing chelated medium and trace elements comprises the following steps:
step 1: adding phosphoric acid, urea, potassium and a medium trace element additive into a reactor, and stirring and reacting at 60-90 ℃ for 10-60 min to obtain reaction slurry;
step 2: adding the reaction slurry obtained in the step (1) into a polymerization curing device with the absolute pressure of 1-70Kpa, controlling the temperature of the slurry material to be 140-220 ℃, drying and curing the slurry into a solid material after 20-90 min, and controlling the polymerization rate of phosphorus in the solid material obtained by drying and curing to be 80-94%;
and step 3: cooling the solid material to 30-80 ℃, and then crushing to obtain a chelated medium-trace element-containing ammonium potassium polyphosphate water-soluble fertilizer;
wherein,
the phosphoric acid, urea and potassium in the step 1, and P contained in the phosphoric acid, urea and potassium respectively2O5、N、K2The ratio of O is P2O5：N：K2O＝1：0.45-0.65：0.2-1；
The medium trace element additive in the step 1 is one or more of metal inorganic salts of magnesium, calcium, iron, zinc, copper, manganese and molybdenum;
the medium trace element additive in the step 1 contains medium trace elements of magnesium, calcium, iron, zinc, copper, manganese and molybdenum, wherein the medium trace elements are M and P in phosphoric acid in terms of element mass2O5In a ratio of M: p2O5＝0.01-0.15：1；
And 2, the polymerization rate of the phosphorus is the ratio of the difference value of the effective phosphorus content and the orthophosphate content in the material to the effective phosphorus content.
Wherein, the potassium in the step 1 is one or more of potassium sulfate, potassium chloride, potassium nitrate and potassium dihydrogen phosphate.
Further optimized, the metal inorganic salt is one or more of sulfate, nitrate or chloride.
Further limiting, the average polymerization degree of phosphorus of the ammonium potassium polyphosphate containing the chelated medium trace elements in the step 3 is 2-5.
In one possible design, the water insoluble content of the chelated medium trace element-containing potassium ammonium polyphosphate described in step 3 is no more than 0.5%.
Wherein P of phosphoric acid described in step 12O5The mass fraction is 24-56%.
Further optimization, when the phosphoric acid in the step 1 is wet process phosphoric acid, the trace elements in magnesium, calcium, iron, zinc, copper, manganese and molybdenum are counted as N by the mass of the elements, and P in the phosphoric acid2O5The ratio of (A) to (B) is N: p2O50.01-0.15: when 1, the dosage of the medium trace element additive can be zero.
Wherein, the wet process phosphoric acid is prepared by decomposing phosphorite with sulfuric acid.
The preparation device of the ammonium potassium polyphosphate containing the chelated medium trace elements has the following structure, and comprises a stirring device for stirring materials, a polymerization solidifying device connected with the stirring device and used for solidifying the materials, and a cooling device and a crushing device for cooling and crushing the solidified materials;
the polymerization curing device comprises a cylinder body, a distributing device arranged in the cylinder body and used for being connected with the stirring device, a belt feeding component arranged in the cylinder body and used for conveying cured materials, a cutter arranged at the tail end of the belt feeding component, a heating component arranged in the cylinder body and a vacuum suction component communicated with the interior of the cylinder body;
the distributing device is positioned above the end part of the belt feeding assembly; the spiral feeding assembly is arranged below the discharge end of the belt feeding assembly, the discharge end of the spiral feeding assembly is connected with the cooling device, and the crushing device is connected with the cooling device.
In some preferred embodiments, the belt feeding assemblies are provided with a plurality of belt feeding assemblies, the belt feeding assemblies are arranged in a staggered mode from top to bottom, materials on the previous belt feeding assembly can fall on the next belt feeding assembly, and each belt feeding assembly corresponds to one cutter.
Further optimize, the cutter on the belt feeding component positioned at the lowest position comprises a first cutter and a second cutter, the first cutter and the second cutter are obliquely arranged above the belt feeding component, and a material channel is formed between the first cutter and the second cutter.
Wherein, belt feeding subassembly is including rotating two rods that set up in the barrel, and the suit is changeing the belt on the rod to and change and be connected driving motor between the rod with one of them.
Wherein, heating element includes first hot plate and second hot plate, and first hot plate is located the top of belt, and forms heating channel with the top surface of belt, and the second hot plate setting is between belt top surface and bottom surface, and each heating element all corresponds a belt feeding assembly.
Further limited, the first heating plate and the second heating plate are heat exchange plates or carbon fiber heating plates.
Further optimize, the vacuum suction assembly includes the connector of setting on the barrel and with the vacuum pump that the connector links to each other.
The spiral feeding assembly comprises a feeding barrel, a rotating shaft, a driving motor and a material guide hopper, the rotating shaft is rotatably installed on the feeding barrel, spiral stirring blades are arranged on the rotating shaft, the material guide hopper is arranged on the feeding barrel, the driving motor is connected with the rotating shaft, a discharge hole is formed in the feeding barrel, and the discharge hole is connected with a cooling device.
In some embodiments, a support frame is disposed on the tub.
Wherein, the end part of the heating channel is provided with a fan, and the fan is just opposite to the heating channel.
Compared with the prior art, the invention has the following beneficial effects:
the invention adds the raw materials into a reactor, and stirs at 60-90 ℃,solidifying and drying the obtained slurry under the absolute pressure vacuum condition, and finally crushing a solidified and cooled product to obtain the ammonium polyphosphate potassium water-soluble fertilizer containing the chelated medium and trace elements; by reacting the phosphoric acid, urea and potassium described in step 1 with P contained therein respectively2O5、N、K2The ratio of O is P2O5：N：K2O is 1: 0.45-0.65: 0.2-1, the product prepared by the raw materials of the components in the proportion can be better solidified into a product, the water solubility of the product can be ensured to reach the standard, the product has the capability of adding and chelating other medium and trace elements, the fertility and the quality of the ammonium potassium polyphosphate can be effectively improved, and the ammonium potassium polyphosphate has the chelated medium and trace elements; during the curing reaction, the polymerization rate range of the slurry from the curing reaction to proper phosphorus is strictly controlled, the capability of generating water-soluble chelate by combining metal ions in the raw materials can be further improved, the water-insoluble substance of the product is not more than 0.5 percent, and the agricultural use requirement of the water-soluble fertilizer is met; in addition, the invention also discloses a device for preparing the ammonium potassium polyphosphate containing the chelated medium and trace elements, which is mainly used for preparing the ammonium potassium polyphosphate containing the chelated medium and trace elements and has the advantages of simple structure, good curing and drying effect and high speed.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is a block diagram of the overall process of the preparation process of the present invention.
Fig. 2 is a schematic view of the overall structure of the apparatus according to the second embodiment of the present invention.
Fig. 3 is a schematic view of the overall structure of the device according to the third embodiment of the present invention.
Fig. 4 is a schematic diagram illustrating a positional relationship between the first cutter and the second cutter in the third embodiment of the present invention.
Reference numerals:
1-a polymerization solidification device, 2-a cooling device, 3-a crushing device, 4-a barrel, 5-a distributor, 6-a belt feeding component, 7-a cutter, 8-a heating component, 9-a vacuum suction component, 10-a spiral feeding component, 11-a packaging machine, 12-a rotating rod, 13-a belt, 14-a first heating plate, 15-a second heating plate, 16-a heating channel, 17-a connector, 18-a vacuum pump, 19-a feeding barrel, 20-a rotating shaft, 21-a guide hopper, 22-a spiral stirring blade, 23-a first cutter, 24-a second cutter and 25-a fan.
Detailed Description
The present invention will be further described with reference to the following examples, which are intended to illustrate only some, but not all, of the embodiments of the present invention. Based on the embodiments of the present invention, other embodiments used by those skilled in the art without any creative effort belong to the protection scope of the present invention.
Example one
Referring to fig. 1, the present example discloses a preparation process of ammonium potassium polyphosphate containing chelated medium trace elements, which comprises the following steps:
step 1: adding phosphoric acid, urea, potassium and a medium trace element additive into a reactor, and stirring and reacting at 60-90 ℃ for 10-60 min to obtain reaction slurry;
when stirring, the stirrer is made of carbon steel lining polytetrafluoroethylene material, the jacket of the stirring equipment is insulated, and the heat source of the jacket can be steam, hot water and heat conducting oil, so that the stirring effect is improved;
step 2: adding the reaction slurry obtained in the step (1) into a polymerization curing device with the absolute pressure of 1-70Kpa, controlling the temperature of the slurry material to be 140-220 ℃, drying and curing the slurry into a solid material after 20-90 min, and controlling the polymerization rate of phosphorus in the solid material obtained by drying and curing to be 80-94%; in a vacuum environment, the slurry reaction polymerization curing time can be greatly shortened, and the productivity of the device is improved.
In actual use, after the solid material is solidified, in the cooling and crushing stage, the relative humidity in the environment is not more than 40%, preferably 30-40%, so that the cooling and crushing effects are ensured, and the quality of the product is prevented from being reduced after water absorption;
it is noted that, during the crushing operation, the particle size of the crushed material is 0.15-1mm, which can ensure better dissolution when in use;
and step 3: cooling the solid material to 30-80 ℃, and then crushing to obtain a chelated medium-trace element-containing ammonium potassium polyphosphate water-soluble fertilizer;
wherein,
the phosphoric acid, urea and potassium in the step 1, and P contained in the phosphoric acid, urea and potassium respectively2O5、N、K2The ratio of O is P2O5：N：K2O is 1: 0.45-0.65: 0.2 to 1; in the actual preparation process, the applicant surprisingly found that the component ratio is controlled at P2O5：N：K2O is 1: 0.45-0.65: 0.2-1, the product has shorter time in the curing stage, and simultaneously, the water solubility of the product is better under the component proportion, and simultaneously, the product has better capability of adding and chelating other medium and trace elements. More importantly, the product prepared from the raw materials of the components in the proportion can be solidified into a solid product, can reach the water solubility standard, and has the capability of adding and chelating other medium and trace elements; the adjustment of the proportion of the phosphoric acid, the urea and the potassium can adjust the proportion of the product nutrients and adapt to the requirements of different crops in different periods.
The medium trace element additive in the step 1 is one or more of metal inorganic salts of magnesium, calcium, iron, zinc, copper, manganese and molybdenum; the metal inorganic salt includes but not limited to magnesium sulfate, calcium nitrate, ferrous sulfate, zinc sulfate, calcium chloride, magnesium chloride, copper sulfate, manganese sulfate, sodium molybdate, etc.;
the medium trace element additive in the step 1 contains medium trace elements of magnesium, calcium, iron, zinc, copper, manganese and molybdenum, wherein the medium trace elements are M and P in phosphoric acid in terms of element mass2O5In a ratio of M: p2O50.01-0.15: 1, the water-soluble fertilizer can be ensured while the product contains a proper amount of medium and trace elements for agricultural applicationThe water solubility of the material product reaches the standard.
And 2, the polymerization rate of the phosphorus is the ratio of the difference value of the effective phosphorus content and the orthophosphate content in the material to the effective phosphorus content.
Wherein, the potassium in the step 1 is one or more of potassium sulfate, potassium chloride, potassium nitrate and potassium dihydrogen phosphate.
Wherein, the metal inorganic salt is one or more of sulfate, nitrate or chloride.
In some preferred embodiments, the ammonium potassium polyphosphate containing chelated medium trace elements described in step 3 has a phosphorus average degree of polymerization of 2 to 5; the average polymerization degree is controlled to be 2-5, so that the solubility of the ammonium potassium polyphosphate is high, and liquid ammonium polyphosphate fertilizers with various proportions can be prepared; the chelating ability is strong, and the chelate can be combined with metal ions in raw materials to generate a water-soluble chelate; the slow release and phosphorus utilization rate is high, the product polymerization degree is low, the hydrolysis period is proper, and the hydrolysis release rate can be more suitable for the requirements of plants on nutrients in different growth stages.
Wherein the content of the water-insoluble substance of the ammonium potassium polyphosphate containing the chelated medium trace elements in the step 3 is not more than 0.5 percent.
In some possible designs, P of the phosphoric acid described in step 12O5The mass fraction is 24-56%. The invention has wider requirement on raw materials, and can be more suitable for the actual production situation of phosphoric acid, namely P of phosphoric acid2O5The mass fraction of 24-56% is the main range of commercial grade phosphoric acid raw material, is easily available and has low cost.
In some embodiments, when the phosphoric acid in step 1 is wet process phosphoric acid, the phosphoric acid contains trace elements of magnesium, calcium, iron, zinc, copper, manganese and molybdenum, wherein the trace elements are N in terms of element mass, and P in the phosphoric acid2O5The ratio of (A) to (B) is N: p2O50.01-0.15: when 1, the dosage of the medium trace element additive can be zero.
Wherein, the wet process phosphoric acid is prepared by decomposing phosphorite with sulfuric acid.
The product prepared by the method contains three major elements of nitrogen, phosphorus and potassium and various medium and trace elements, can comprehensively meet the nutrient requirements of different crops, and can reach good water solubility, namely the water-insoluble substance reaches the standard, under the condition of chelating the medium and trace elements and having the three major elements of nitrogen, phosphorus and potassium.
Example two
Referring to fig. 1-4, this example discloses a device for preparing potassium ammonium polyphosphate containing trace elements in chelated state, comprising a stirring device for stirring materials, a polymerization solidifying device 1 connected with the stirring device for solidifying the materials, a cooling device 2 and a crushing device 3 for cooling and crushing the solidified materials,
the polymerization curing device 1 comprises a cylinder 4, a distributor 5 arranged in the cylinder 4 and connected with the stirring device, a belt feeding component 6 arranged in the cylinder 4 and used for conveying cured materials, a cutter 7 arranged at the tail end of the belt feeding component 6, a heating component 8 arranged in the cylinder 4 and a vacuum suction component 9 communicated with the inside of the cylinder 4;
wherein, the distributing device 5 is positioned above the end part of the belt feeding component 6; a spiral feeding component 10 is arranged below the discharge end of the belt feeding component 6, the discharge end of the spiral feeding component 10 is connected with the cooling device 2, and the crushing device 3 is connected with the cooling device 2.
The preparation device mainly comprises a stirring device, a polymerization solidification device 1, a cooling device 2 and a crushing device 3, wherein in actual use, raw materials are placed in the stirring device to be fully stirred, then slurry obtained after stirring is sent to the polymerization solidification device 1 to be polymerized and solidified, and solidified materials are dried, cooled in the cooling device 2 and crushed through the crushing device 3 to realize drying and solidification integrated operation;
after the materials enter the barrel 4, the materials are uniformly sprayed on a belt feeding assembly 6 through the arranged distributor 5, and the temperature in the barrel 4 is increased through the arranged heating assembly 8 so as to dry the materials; meanwhile, the vacuum suction assembly 9 is arranged to suck the water vapor in the drying device, so that the drying efficiency is improved; the material solidifies and the drying at the in-process that belt feeding unit 6 went up to remove, then scrapes the material after drying from belt feeding unit 6 through cutter 7 that sets up, drops on spiral feeding unit 10 simultaneously, sends the material to cooling module through spiral feeding unit 10 and cools off.
Wherein, the discharge end of the crushing device 3 is connected with a packaging machine 11, and the product is packaged by the packaging machine 11 arranged, so that the aim of automatic production is fulfilled.
The belt feeding assembly 6 comprises two rotating rollers 12 rotatably arranged in the barrel 4, a belt 13 sleeved on the rotating rollers 12, and a driving motor connected between one of the rotating rollers 12; the rotating roller 12 can be driven to rotate by the arranged motor, so that the belt 13 moves.
Wherein, heating element 8 includes first hot plate 14 and second hot plate 15, and first hot plate 14 is located the top of belt 13, and forms heating channel 16 with the top surface of belt 13, and second hot plate 15 sets up between belt 13 top surface and bottom surface, and each heating element 8 all corresponds a belt feeding unit 6.
Through the first and second heating plates that set up, the material can be better heated, and the drying efficiency of the material is improved.
Wherein, the first heating plate and the second heating plate are heat exchange plates or carbon fiber heating plates.
The vacuum suction assembly 9 comprises a connector 17 arranged on the cylinder 4 and a vacuum pump 18 connected with the connector 17; the vacuum pump 18 arranged can not only pump out the water vapor in the cylinder 4 to reduce the internal humidity, but also reduce the vacuum degree in the cylinder 4, thereby effectively improving the production efficiency, reducing the energy consumption, effectively reducing the load of the polymerization reactor and improving the production efficiency. Compared with the existing normal pressure preparation, the polymerization under vacuum can reduce energy consumption, increase product yield, improve product quality and improve product appearance and water solubility.
The spiral feeding assembly 10 comprises a feeding barrel 19, a rotating shaft 20, a driving motor and a material guide hopper 21, wherein the rotating shaft 20 is rotatably installed on the feeding barrel 19, a spiral stirring blade 22 is arranged on the rotating shaft 20, the material guide hopper 21 is arranged on feeding materials, the driving motor is connected with the rotating shaft 20, a discharging hole is formed in the feeding barrel 19, and the discharging hole is connected with the cooling device 2.
In some embodiments, a support frame is disposed on the tub.
EXAMPLE III
The embodiment is further optimized on the basis of the second embodiment, in the embodiment, the belt feeding assemblies 6 are provided with a plurality of belt feeding assemblies 6 which are sequentially arranged in a staggered manner from top to bottom, the material on the previous belt feeding assembly 6 can fall on the next belt feeding assembly 6, and each belt feeding assembly 6 corresponds to one cutter 7.
After the material is cut and scraped by the cutter 7, the material on the previous belt feeding component 6 can fall on the next belt feeding component 6, the running path of the material in the barrel 4 is prolonged, the curing and drying time is prolonged, and the curing and drying effects are improved.
In a possible design, the upper cutter 7 of the belt feeding assembly 6 positioned at the lowest position comprises a first cutter 23 and a second cutter 24, the first cutter 23 and the second cutter 24 are obliquely arranged above the belt feeding assembly 6, and a material channel is formed between the first cutter 23 and the second cutter 24.
Therefore, the first cutter 23 and the second cutter 24 can form an 'eight' shape, materials scraped off can be collected into a material channel conveniently, and the materials can fall off in a concentrated mode.
Further preferably, a fan 25 is arranged at the end part of the heating channel 16, and the fan 25 is over against the heating channel 16; the flow rate of air in the heating channel 16 is improved through the arranged fan 25, the evaporation efficiency is improved, and the drying efficiency is further improved.
In order to further understand the present invention for those skilled in the art, the following process will be further described with reference to specific preparation examples.
Preparation example 1
Phosphoric acid: p2O5The content is 24 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; magnesium sulfate: the Mg content is 20%.
Adding 600g of phosphoric acid, 139.6g of urea, 55.4g of potassium sulfate and 7.2g of magnesium sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 1Kpa, controlling the temperature of the slurry material at 220 ℃, and curing the slurry into a solid material after 20min, wherein the polymerization rate of phosphorus in the solid material is 88%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.02%. The product index is shown in the following table.
Preparation example 2
Phosphoric acid: p2O5The content is 24 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; magnesium sulfate: the Mg content is 20%.
Adding 600g of phosphoric acid, 139.6g of urea, 55.4g of potassium sulfate and 7.2g of magnesium sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 1Kpa, controlling the temperature of the slurry material at 140 ℃, and curing the slurry into a solid material after 90min, wherein the polymerization rate of phosphorus in the solid material is 85%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.05%. The product index is shown in the following table.
Preparation example 3
Phosphoric acid: p2O5The content is 24 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; magnesium sulfate: the Mg content is 20%.
Adding 600g of phosphoric acid, 139.6g of urea, 55.4g of potassium sulfate and 7.2g of magnesium sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 70Kpa, controlling the temperature of the slurry material at 220 ℃, and curing the slurry into a solid material after 20min, wherein the polymerization rate of phosphorus in the solid material is 90%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.02%. The product index is shown in the following table.
Preparation example 4
Phosphoric acid: p2O5The content is 24 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; magnesium sulfate: the Mg content is 20%.
Adding 600g of phosphoric acid, 201.7g of urea, 276.9g of potassium sulfate and 108g of magnesium sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 1Kpa, controlling the temperature of the slurry material at 140 ℃, and curing the slurry into a solid material after 20min, wherein the polymerization rate of phosphorus in the solid material is 80%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.5%. The product index is shown in the following table.
Preparation example 5
Phosphoric acid: p2O5The content is 56 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; magnesium sulfate: the Mg content is 20%.
Adding 600g of phosphoric acid, 325.8g of urea, 129.2g of potassium sulfate and 16.8g of magnesium sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 1Kpa, controlling the temperature of the slurry material at 140 ℃, and curing the slurry into a solid material after 20min, wherein the polymerization rate of phosphorus in the solid material is 82%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.3%. The product index is shown in the following table.
Preparation example 6
Phosphoric acid: p2O5The content is 56 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; magnesium sulfate: the Mg content is 20%.
Adding 600g of phosphoric acid, 325.8g of urea, 129.2g of potassium sulfate and 16.8g of magnesium sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 1Kpa, controlling the temperature of the slurry material at 220 ℃, and curing the slurry into a solid material after 90min, wherein the polymerization rate of phosphorus in the solid material is 94%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.02%. The product index is shown in the following table.
Preparation example 7
Phosphoric acid: p2O5The content is 56 percent; urea: the N content is 46.4%; potassium chloride: k2The O content is 62%; magnesium sulfate: the Mg content is 20%.
Adding 600g of phosphoric acid, 325.8g of urea, 108.4g of potassium chloride and 16.8g of magnesium sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 1Kpa, controlling the temperature of the slurry material at 220 ℃, and curing the slurry into a solid material after 90min, wherein the polymerization rate of phosphorus in the solid material is 94%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.02%. The product index is shown in the following table.
Preparation example 8
Phosphoric acid: p2O5The content is 56 percent; urea: the N content is 46.4%; potassium nitrate: k2The O content is 38.6 percent; magnesium sulfate: the Mg content is 20%.
Adding 600g of phosphoric acid, 325.8g of urea, 174.1g of potassium nitrate and 16.8g of magnesium sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 1Kpa, controlling the temperature of the slurry material at 220 ℃, and curing the slurry into a solid material after 90min, wherein the polymerization rate of phosphorus in the solid material is 94%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.03%. The product index is shown in the following table.
Preparation example 9
Phosphoric acid: p2O5The content is 56 percent; urea: the N content is 46.4%; potassium dihydrogen phosphate: k2The O content is 38.6 percent; magnesium sulfate: the Mg content is 20%.
Adding 600g of phosphoric acid, 325.8g of urea, 234.1g of monopotassium phosphate and 33.6g of magnesium sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 1Kpa, controlling the temperature of the slurry material at 220 ℃, and curing the slurry into a solid material after 90min, wherein the polymerization rate of phosphorus in the solid material is 92%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.05%. The product index is shown in the following table.
Preparation example 10
This example is the most preferred preparation, phosphoric acid: p2O5The content is 47 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; magnesium sulfate: mg containsThe amount is 20%.
Adding 600g of phosphoric acid, 273.5g of urea, 271.1g of potassium sulfate and 141g of magnesium sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 10Kpa, controlling the temperature of the slurry material at 160 ℃, and curing the slurry into a solid material after 60min, wherein the polymerization rate of phosphorus in the solid material is 88%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.40%. The product index is shown in the following table.
Preparation example 11
Phosphoric acid: p2O5The content is 47 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; calcium nitrate: the Ca content was 24.4%.
Adding 600g of phosphoric acid, 273.5g of urea, 271.1g of potassium sulfate and 111.6g of calcium nitrate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 10Kpa, controlling the temperature of the slurry material at 160 ℃, and curing the slurry into a solid material after 60min, wherein the polymerization rate of phosphorus in the solid material is 89%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing the chelated Ca element, wherein the content of the water-insoluble substance is 0.45%. The product index is shown in the following table.
Preparation example 12
Phosphoric acid: p2O5The content is 47 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; ferrous sulfate: the Fe content is 36.8%.
Adding 600g of phosphoric acid, 273.5g of urea, 271.1g of potassium sulfate and 13.8g of ferrous sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 10Kpa, controlling the temperature of the slurry material at 160 ℃, and curing the slurry into a solid material after 60min, wherein the polymerization rate of phosphorus in the solid material is 90%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing the chelated Fe element, wherein the content of the water-insoluble substance is 0.32%. The product index is shown in the following table.
Preparation example 13
Phosphoric acid: p2O5The content is 47 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; zinc sulfate: the Zn content is 39.8 percent.
Adding 600g of phosphoric acid, 273.5g of urea, 271.1g of potassium sulfate and 106.3g of zinc sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 10Kpa, controlling the temperature of the slurry material at 160 ℃, and curing the slurry into a solid material after 60min, wherein the polymerization rate of phosphorus in the solid material is 91%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Zn elements, wherein the content of water-insoluble substances is 0.35%. The product index is shown in the following table.
Preparation example 14
Phosphoric acid: p2O5The content is 47 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; calcium chloride: the Ca content is 36%.
Adding 600g of phosphoric acid, 273.5g of urea, 271.1g of potassium sulfate and 39.1g of calcium chloride into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 10Kpa, controlling the temperature of the slurry material at 160 ℃, and curing the slurry into a solid material after 60min, wherein the polymerization rate of phosphorus in the solid material is 91%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing the chelated Ca element, wherein the content of the water-insoluble substance is 0.45%. The product index is shown in the following table.
Preparation example 15
Phosphoric acid: p2O5The content is 47 percent; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%; magnesium chloride: the Mg content is 25 percent.
Adding 600g of phosphoric acid, 273.5g of urea, 271.1g of potassium sulfate and 111.5g of magnesium chloride into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 10Kpa, controlling the temperature of the slurry material at 160 ℃, and curing the slurry into a solid material after 60min, wherein the polymerization rate of phosphorus in the solid material is 91%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.5%. The product index is shown in the following table.
Preparation example 16
Phosphoric acid: p2O5The content is 47 percent; urea: the N content is 46.4%; potassium sulfate: 52% of K2O; copper sulfate: the Cu content is 39%; manganese sulfate: the Mn content is 36%; sodium molybdate: the Mo content is 46 percent.
Adding 600g of phosphoric acid, 273.5g of urea, 271.1g of potassium sulfate, 10g of copper sulfate, 10g of manganese sulfate and 2g of sodium molybdate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 10Kpa, controlling the temperature of the slurry material at 160 ℃, and curing the slurry into a solid material after 60min, wherein the polymerization rate of phosphorus in the solid material is 90%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium polyphosphate potassium water-soluble fertilizer containing chelated Cu, Mn and Mo elements, wherein the content of water-insoluble substances is 0.4%. The product index is shown in the following table.
Preparation example 17
Phosphoric acid (wet process phosphoric acid): p2O546% of Mg, 4.2% of Fe, 1.8% of Ca and 0.9% of Ca; urea: the N content is 46.4%; potassium sulfate: k2The O content is 52%.
Adding 600g of phosphoric acid, 250g of urea and 150g of potassium sulfate into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 10Kpa, controlling the temperature of the slurry material at 160 ℃, and curing the slurry into a solid material after 60min, wherein the polymerization rate of phosphorus in the solid material is 91%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium polyphosphate potassium water-soluble fertilizer containing chelated Mg, Fe and Ca elements, wherein the content of water-insoluble substances is 0.4%. The product index is shown in the following table.
Preparation example 18
Phosphoric acid: p2O556 percent of Mg content and 0.56 percent of Mg content; urea: the N content is 46.4%; potassium chloride: k2The O content is 62%.
Adding 600g of phosphoric acid, 325.8g of urea and 129.2g of potassium chloride into a reactor, and stirring and reacting at 60 ℃ for 10 minutes to obtain reaction slurry; adding the reaction slurry into a polymerization curing device with the absolute pressure of 1Kpa, controlling the temperature of the slurry material at 170 ℃, and curing the slurry into a solid material after 50min, wherein the polymerization rate of phosphorus in the solid material is 91%; and cooling the solid material to 30 ℃, and crushing to obtain the ammonium potassium polyphosphate water-soluble fertilizer containing chelated Mg, wherein the content of water-insoluble substances is 0.2%. The product index is shown in the following table.
While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. Therefore, it is intended that the appended claims be interpreted as including preferred embodiments and all such alterations and modifications as fall within the scope of the invention. The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, it should be noted that any modifications, equivalents and improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation process of ammonium potassium polyphosphate containing chelated medium and trace elements is characterized by comprising the following steps:
step 1: adding phosphoric acid, urea, potassium and a medium trace element additive into a reactor, and stirring and reacting at 60-90 ℃ for 10-60 min to obtain reaction slurry;
step 2: adding the reaction slurry obtained in the step (1) into a polymerization curing device with the absolute pressure of 1-70Kpa, controlling the temperature of the slurry material to be 140-220 ℃, drying and curing the slurry into a solid material after 20-90 min, and controlling the polymerization rate of phosphorus in the solid material obtained by drying and curing to be 80-94%;
and step 3: cooling the solid material to 30-80 ℃, and then crushing to obtain a chelated medium-trace element-containing ammonium potassium polyphosphate water-soluble fertilizer;
wherein the phosphoric acid, urea and potassium in step 1 respectively contain P2O5、N、K2The ratio of O is P2O5：N：K2O＝1：0.45-0.65：0.2-1；
The medium trace element additive in the step 1 is one or more of metal inorganic salts of magnesium, calcium, iron, zinc, copper, manganese and molybdenum;
the medium trace element additive in the step 1 contains medium trace elements of magnesium, calcium, iron, zinc, copper, manganese and molybdenum, wherein the medium trace elements are M and P in phosphoric acid in terms of element mass2O5In a ratio of M: p2O5＝0.01-0.15：1；
And 2, the polymerization rate of the phosphorus is the ratio of the difference value of the effective phosphorus content and the orthophosphate content in the material to the effective phosphorus content.
2. The preparation process of the ammonium potassium polyphosphate containing the chelated medium and trace elements as claimed in claim 1, wherein: the potassium in the step 1 is one or more of potassium sulfate, potassium chloride, potassium nitrate and potassium dihydrogen phosphate.
3. The preparation process of the ammonium potassium polyphosphate containing the chelated medium and trace elements as claimed in claim 1, wherein: the metal inorganic salt is one or more of sulfate, nitrate or chloride.
4. The preparation process of the ammonium potassium polyphosphate containing the chelated medium and trace elements as claimed in claim 1, wherein: the average polymerization degree of phosphorus of the ammonium potassium polyphosphate containing the chelated medium trace elements in the step 3 is 2-5.
5. The preparation process of the ammonium potassium polyphosphate containing the chelated medium and trace elements as claimed in claim 1, wherein: the content of the water-insoluble substance of the ammonium potassium polyphosphate containing the chelated medium trace elements in the step 3 is not more than 0.5 percent.
6. The preparation process of the ammonium potassium polyphosphate containing the chelated medium and trace elements as claimed in claim 1, wherein: p of phosphoric acid described in step 12O5The mass fraction is 24-56%.
7. The preparation process of the ammonium potassium polyphosphate containing the chelated medium and trace elements as claimed in claim 1, wherein: when the phosphoric acid in the step 1 is wet process phosphoric acid, the mass of the trace elements in magnesium, calcium, iron, zinc, copper, manganese and molybdenum are N and P in the phosphoric acid2O5The ratio of (A) to (B) is N: p2O50.01-0.15: 1 hour, medium and microThe amount of the quantum element additive can be zero.
8. The preparation process of the ammonium potassium polyphosphate containing the chelated medium and trace elements as claimed in claim 1, wherein: the wet process phosphoric acid is prepared by decomposing phosphorite with sulfuric acid.
9. The utility model provides a contain microelement's in chelate state ammonium potassium polyphosphate preparation facilities which characterized in that: the device for preparing the ammonium potassium polyphosphate containing the chelated medium and trace elements is used for preparing the ammonium potassium polyphosphate containing the chelated medium and trace elements according to the ammonium potassium polyphosphate preparation process containing the chelated medium and trace elements in any one of claims 1 to 8;
the preparation device comprises a stirring device for stirring materials, a polymerization solidification device connected with the stirring device and used for solidifying the materials, and a cooling device and a crushing device for cooling and crushing the solidified materials, wherein the polymerization solidification device comprises a barrel, a distributor arranged in the barrel and used for being connected with the stirring device, a belt feeding assembly arranged in the barrel and used for conveying the solidified materials, a cutter arranged at the tail end of the belt feeding assembly, a heating assembly arranged in the barrel and a vacuum suction assembly communicated with the interior of the barrel;
the distributing device is positioned above the end part of the belt feeding assembly; the spiral feeding assembly is arranged below the discharge end of the belt feeding assembly, the discharge end of the spiral feeding assembly is connected with the cooling device, and the crushing device is connected with the cooling device.
10. The device for preparing the ammonium potassium polyphosphate containing the chelated medium and trace elements according to claim 1, is characterized in that: the belt feeding component is provided with a plurality of cutters, and the cutters are sequentially arranged from top to bottom in a staggered manner, the material on the previous belt feeding component can fall on the next belt feeding component, and each belt feeding component corresponds to one cutter.
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