CN117776811A - Compound fertilizer for chelating medium trace elements with humic acid and preparation method thereof - Google Patents
Compound fertilizer for chelating medium trace elements with humic acid and preparation method thereof Download PDFInfo
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- CN117776811A CN117776811A CN202311507859.7A CN202311507859A CN117776811A CN 117776811 A CN117776811 A CN 117776811A CN 202311507859 A CN202311507859 A CN 202311507859A CN 117776811 A CN117776811 A CN 117776811A
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- compound fertilizer
- sulfate
- potassium
- potassium fulvate
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- 239000003337 fertilizer Substances 0.000 title claims abstract description 222
- 150000001875 compounds Chemical class 0.000 title claims abstract description 125
- 239000011573 trace mineral Substances 0.000 title claims abstract description 87
- 235000013619 trace mineral Nutrition 0.000 title claims abstract description 87
- 239000004021 humic acid Substances 0.000 title claims abstract description 71
- 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 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 96
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 92
- 239000011591 potassium Substances 0.000 claims abstract description 92
- WZISDKTXHMETKG-UHFFFAOYSA-H dimagnesium;dipotassium;trisulfate Chemical compound [Mg+2].[Mg+2].[K+].[K+].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O WZISDKTXHMETKG-UHFFFAOYSA-H 0.000 claims abstract description 56
- 239000013522 chelant Substances 0.000 claims abstract description 52
- 239000013067 intermediate product Substances 0.000 claims abstract description 42
- 238000000576 coating method Methods 0.000 claims abstract description 41
- 239000011248 coating agent Substances 0.000 claims abstract description 40
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000004202 carbamide Substances 0.000 claims abstract description 37
- 238000002156 mixing Methods 0.000 claims abstract description 35
- 229910000365 copper sulfate Inorganic materials 0.000 claims abstract description 34
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims abstract description 34
- 239000011790 ferrous sulphate Substances 0.000 claims abstract description 34
- 235000003891 ferrous sulphate Nutrition 0.000 claims abstract description 34
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims abstract description 34
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims abstract description 34
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 34
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 34
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 34
- 229940099596 manganese sulfate Drugs 0.000 claims abstract description 30
- 239000011702 manganese sulphate Substances 0.000 claims abstract description 30
- 235000007079 manganese sulphate Nutrition 0.000 claims abstract description 30
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims abstract description 30
- 238000001035 drying Methods 0.000 claims abstract description 28
- YYRMJZQKEFZXMX-UHFFFAOYSA-L calcium bis(dihydrogenphosphate) Chemical compound [Ca+2].OP(O)([O-])=O.OP(O)([O-])=O YYRMJZQKEFZXMX-UHFFFAOYSA-L 0.000 claims abstract description 26
- 229910000389 calcium phosphate Inorganic materials 0.000 claims abstract description 26
- 235000019691 monocalcium phosphate Nutrition 0.000 claims abstract description 26
- 238000012216 screening Methods 0.000 claims abstract description 24
- 229960000355 copper sulfate Drugs 0.000 claims abstract description 14
- 229960001781 ferrous sulfate Drugs 0.000 claims abstract description 14
- YYRMJZQKEFZXMX-UHFFFAOYSA-N calcium;phosphoric acid Chemical compound [Ca+2].OP(O)(O)=O.OP(O)(O)=O YYRMJZQKEFZXMX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002426 superphosphate Substances 0.000 claims abstract description 8
- 239000011230 binding agent Substances 0.000 claims description 52
- 239000002245 particle Substances 0.000 claims description 36
- 239000002994 raw material Substances 0.000 claims description 26
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 18
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 18
- YDEXUEFDPVHGHE-GGMCWBHBSA-L disodium;(2r)-3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Na+].[Na+].COC1=CC=CC(C[C@H](CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O YDEXUEFDPVHGHE-GGMCWBHBSA-L 0.000 claims description 17
- 239000007787 solid Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 238000005507 spraying Methods 0.000 claims description 10
- 230000035484 reaction time Effects 0.000 claims description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 2
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 2
- 229940072033 potash Drugs 0.000 claims description 2
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 2
- 235000015320 potassium carbonate Nutrition 0.000 claims description 2
- 235000015097 nutrients Nutrition 0.000 abstract description 19
- 239000000047 product Substances 0.000 abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 7
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 7
- 239000002689 soil Substances 0.000 abstract description 7
- 230000007547 defect Effects 0.000 abstract description 2
- 238000003860 storage Methods 0.000 abstract description 2
- 238000001125 extrusion Methods 0.000 description 24
- -1 humic acid compound Chemical class 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 20
- 238000005469 granulation Methods 0.000 description 14
- 230000003179 granulation Effects 0.000 description 14
- 238000007873 sieving Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000011161 development Methods 0.000 description 5
- 230000018109 developmental process Effects 0.000 description 5
- 239000008187 granular material Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 238000005054 agglomeration Methods 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 238000013270 controlled release Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000011777 magnesium Substances 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 230000004720 fertilization Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 2
- 229910001950 potassium oxide Inorganic materials 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- WZLMXYBCAZZIRQ-UHFFFAOYSA-N [N].[P].[K] Chemical compound [N].[P].[K] WZLMXYBCAZZIRQ-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000009920 chelation Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000005515 coenzyme Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 230000008638 plant developmental process Effects 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000029058 respiratory gaseous exchange Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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- Fertilizers (AREA)
Abstract
The invention belongs to the technical field of fertilizers, and relates to a preparation method of a compound fertilizer for chelating trace elements in humic acid, which comprises the following steps: step one, mixing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate with water, and reacting to obtain a potassium fulvate microelement chelate intermediate product; mixing a potassium magnesium sulfate fertilizer, urea and calcium superphosphate with the potassium fulvate microelement chelate intermediate product, reacting, granulating, drying and screening to obtain a primary compound fertilizer; and thirdly, performing outer coating treatment on the primary compound fertilizer, drying and screening to obtain the fertilizer. The invention combines potassium magnesium sulfate fertilizer, urea, superphosphate, potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and the like, provides N, P, K macroelements and medium trace elements, can relieve the defect of lack of the medium trace elements in the existing soil, balances the nutrient elements of the soil, improves the crop yield, has high strength and good sphericity of the product, and is convenient for storage and transportation.
Description
Technical Field
The invention belongs to the technical field of fertilizers, and particularly relates to a compound fertilizer for chelating medium trace elements with humic acid and a preparation method thereof.
Background
The growth and development of crops need to absorb various nutrients, and the nutrient elements determine the yield and quality of the crops. The nitrogen, phosphorus and potassium fertilizer is largely and even excessively input for a long time in agricultural production, but the systematic supply of medium and trace element nutrients is neglected, so that the proportion of the nutrient elements in the soil is unbalanced, the yield of crops is difficult to improve even if other nutrient components are continuously added, and the yield and quality of agricultural products are influenced.
The medium elements mainly comprise calcium, magnesium, sulfur and the like, and refer to nutrient elements which are required to be lower than nitrogen, phosphorus and potassium and higher than other elements in the plant growth and development process, and the content of the medium elements in the plant is about 0.1-0.5%. The microelements mainly comprise zinc, copper, iron and the like, and the necessary nutrient elements are equally important in crops no matter how much and are irreplaceable. The medium trace elements are mostly components of "enzymes" or "coenzymes" in plants for promoting photosynthesis, respiration, substance conversion, and the like. When a certain medium trace element in the soil for providing plant nutrient elements is insufficient, the yield of crops is reduced, the quality is reduced, and even particles are not harvested when serious. In this case, the application of the medium trace element fertilizer tends to achieve a very remarkable income-increasing effect.
The medium trace element fertilizer has obvious effects in improving crop yield, improving crop quality and improving crop resistance, and has wide development prospect and market opportunity. After the agricultural rural chemical fertilizer zero-growth action scheme is proposed, great opportunity is brought to the development of the medium and trace element fertilizer industry. In recent years, the development speed of China medium trace element fertilizer enterprises is rapid, medium trace element fertilizer products registered by the enterprises show blowout type increase, but the development faces more small fertilizer enterprises and smaller scale. From the world, the developed European and American countries have gone out of N, P, K macroelement fertilizer era and enter a precise and balanced fertilization stage. However, at present, the domestic nitrogen-phosphorus-potassium ternary compound fertilizer is still the mainstream of production and consumption, and the medium trace element fertilizer is not enough to use. For a long time, the supplement of medium trace elements to soil is ignored due to the excessive and unreasonable use of the N, P, K large fertilizer.
Disclosure of Invention
The purpose of the application is to provide a humic acid chelated medium trace element compound fertilizer and a preparation method thereof, so as to at least solve one of the problems of unbalanced nutrient element proportion, insufficient strength and sphericity of a coated fertilizer product, inconvenience in transportation and the like in the prior art.
In order to achieve the above purpose, the invention adopts the following technical scheme:
a preparation method of a compound fertilizer for chelating trace elements in humic acid comprises the following steps:
step one, mixing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate with a certain amount of water, and reacting for a certain time at a certain temperature to obtain a potassium fulvate microelement chelate intermediate product;
mixing the potassium magnesium sulfate fertilizer, urea and calcium superphosphate with the potassium fulvate microelement chelate intermediate product according to a certain proportion, reacting for a certain time at a certain temperature, and then granulating, drying and screening to obtain a primary compound fertilizer;
and thirdly, performing outer coating treatment on the primary compound fertilizer, drying and screening to obtain the humic acid chelated medium trace element compound fertilizer.
In the preparation method of the compound fertilizer, as a preferred embodiment, in the first step, the compound fertilizer comprises the following raw material components in percentage by weight: 60-80% of potassium fulvate, 5-10% of ferrous sulfate, 5-10% of copper sulfate, 5-10% of zinc sulfate and 5-10% of manganese sulfate; further preferably, the potassium fulvate may be 70-80%, the ferrous sulfate may be 5-8%, the copper sulfate may be 5-8%, the zinc sulfate may be 5-8%, and the manganese sulfate may be 5-8%.
In the preparation method of the compound fertilizer, as a preferred implementation manner, in the first step, the reaction temperature is 50-70 ℃ and the reaction time is 1-2 h; further preferably, the reaction temperature is 60 to 70 ℃ and the reaction time is 1.5 to 2 hours.
In the above-mentioned method for producing a compound fertilizer, as a preferred embodiment, in the first step, the mass ratio of the added water to the solid is (10 to 20): 100; further preferably (10 to 15): 100.
in the preparation method of the compound fertilizer, as a preferred embodiment, in the second step, the compound fertilizer comprises the following raw material components in percentage by weight: 10-30% of potassium magnesium sulfate fertilizer, 15-35% of urea, 30-40% of superphosphate and 20-30% of potassium fulvate microelement chelate intermediate product; further preferably, the potassium magnesium sulfate fertilizer accounts for 10 to 20 percent, the urea accounts for 25 to 35 percent, the calcium superphosphate accounts for 30 to 35 percent, and the potassium fulvate microelement chelate intermediate product accounts for 20 to 25 percent.
In the preparation method of the compound fertilizer, as a preferred implementation manner, in the second step, the reaction temperature is normal temperature, and the reaction time is 20-40min.
In the preparation method of the compound fertilizer, as a preferred implementation manner, in the second step, the particle size of the primary compound fertilizer obtained by granulation, drying and screening is less than or equal to 3.35mm; further preferably, the particle size of the primary compound fertilizer is 1.75-3.35 mm.
In the preparation method of the compound fertilizer, as a preferred embodiment, in the third step, the raw materials used for the outer coating treatment comprise a primary compound fertilizer, a potassium magnesium sulfate fertilizer and a binder solution; the mass ratio of the binder is 10: polyvinyl alcohol and sodium lignin sulfonate of (4-10), the concentration of the binder solution is 0.5-2%; the mass ratio of the primary compound fertilizer to the potassium magnesium sulfate fertilizer to the binder is 100: (15-30): (1-3); further preferably, the binder has a mass ratio of 10: polyvinyl alcohol and sodium lignin sulfonate of (6-8), wherein the concentration of the binder solution is 1-1.5%, and the mass ratio of the primary compound fertilizer to the potassium magnesium sulfate fertilizer to the binder is 100: (20-25): (1-2).
In the preparation method of the compound fertilizer, as a preferred implementation manner, in the third step, the potassium magnesium sulfate fertilizer is slowly added, the binder solution is added in a spraying way, and the adding time is 5-20 min; further preferably, the addition time is 10 to 15 minutes.
In the preparation method of the compound fertilizer, as a preferred implementation manner, in the third step, the coating time is calculated from the end of the addition, and the coating time is 5-40 min; further preferably, the coating time may be 20 to 30 minutes.
A compound fertilizer of humic acid chelated medium trace elements is prepared by the preparation method.
Compared with the prior art, the scheme of the application has the following beneficial effects:
(1) The invention combines the potassium magnesium sulfate fertilizer, urea, superphosphate, potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and the like according to a certain proportion to obtain the humic acid chelated medium trace element compound fertilizer, wherein the compound fertilizer is rich in the medium trace elements such as Ca, mg, S, fe, cu, zn, mn and the like, can provide N, P, K macroelements and simultaneously provide the medium trace elements, can alleviate the defect of lack of the medium trace elements in the soil at present, balance the soil nutrient elements and improve the crop yield.
(2) The invention combines the potassium magnesium sulfate fertilizer, urea, superphosphate, potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and the like according to a certain proportion to obtain the humic acid chelated medium trace element compound fertilizer, wherein the total nutrient (N+P) in the fertilizer 2 O 5 +K 2 The mass fraction of the O) is more than or equal to 25%, the total humic acid content is more than or equal to 6%, the activated humic acid content is more than or equal to 3%, and the requirement of the humic acid compound fertilizer (HG/T5046-2016) on the low-concentration humic acid compound fertilizer is met.
(4) The invention has poor granulating effect of potassium magnesium sulfate fertilizer, potassium fulvate, calcium superphosphate, ferrous sulfate, copper sulfate and zinc sulfate, can improve the granulating effect of urea after being added, improves the sphericity of particles, and can react with the calcium superphosphate, accelerate the nutrient conversion of the urea, reduce the loss caused by the conversion of the urea into ammonia in the fertilization process, thereby improving the utilization rate of the fertilizer. Furthermore, a small amount of water can be generated in the reaction process of urea and superphosphate, so that the sphericity of the granules can be effectively improved, and the granulating effect is improved. After extrusion granulation, the compound polyvinyl alcohol and sodium lignin sulfonate are adopted as binders for outer coating, so that the coating has good bonding effect, the sphericity of a coated product is high, the granularity qualification rate is relatively high, the agglomeration phenomenon in the coating process is not obvious, meanwhile, the interaction of polyvinyl alcohol, sodium lignin sulfonate and urea in the compound fertilizer can improve the coating effect, greatly enhance the strength and sphericity of the product, facilitate storage and transportation, facilitate the control of solubility and play a role in slow release.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a flowchart of a preparation method of a humic acid chelated medium trace element compound fertilizer, which is provided by the embodiment of the invention.
Detailed Description
The technical scheme of the invention is clearly and completely described below with reference to the accompanying drawings, and as shown in fig. 1, the preferred embodiment of the compound fertilizer for chelating trace elements in humic acid and the preparation method thereof provided by the invention is as follows, and comprises the following steps:
(1) Respectively crushing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate, and uniformly mixing; gradually adding a certain amount of water for mixing, and reacting for 1-2 hours at the temperature of 50-70 ℃ to obtain a potassium fulvate trace element chelate intermediate product;
(2) Adding potassium magnesium sulfate fertilizer, urea and calcium superphosphate into a potassium fulvate trace element chelate intermediate product according to a certain proportion, reacting for 20-40min at normal temperature, then carrying out extrusion granulation in an extrusion granulator, drying at 100-130 ℃, and screening to obtain a primary compound fertilizer;
(3) Mixing polyvinyl alcohol with sodium lignin sulfonate and water to obtain a binder solution, placing the primary compound fertilizer into a disc granulator, slowly adding a potassium magnesium sulfate fertilizer, spraying the binder solution on the surface, performing outer coating treatment, drying at 100-130 ℃, and sieving with a 5-mesh sieve (with the aperture of about 4 mm) to obtain the humic acid chelated medium trace element compound fertilizer.
Preferably, in the step (1), the raw material comprises the following raw material components in percentage by weight: 60-80% of potassium fulvate, 5-10% of ferrous sulfate, 5-10% of copper sulfate, 5-10% of zinc sulfate and 5-10% of manganese sulfate; further preferably, the potassium fulvate may be 70-80%, the ferrous sulfate may be 5-8%, the copper sulfate may be 5-8%, the zinc sulfate may be 5-8%, and the manganese sulfate may be 5-8%.
Preferably, in the step (1), the reaction temperature is 60-70 ℃ and the reaction time is 1.5-2 h.
Preferably, in the step (1), the mass ratio of the added water to the solid is (10 to 20): 100. further preferably, in the step (1), the mass ratio of the added water to the solid is (10 to 15): 100. if the water addition amount is too small, the ball is not easy to be formed, the powder is easy to be pulverized, and if the water addition amount is too large, the ball is easy to be agglomerated.
Preferably, in the step (2), the components in parts by weight are as follows: 10-30% of potassium magnesium sulfate fertilizer, 15-35% of urea, 30-40% of calcium superphosphate and 20-30% of potassium fulvate microelement chelate intermediate product; further preferably, the potassium magnesium sulfate fertilizer accounts for 10 to 20 percent, the urea accounts for 25 to 35 percent, the calcium superphosphate accounts for 30 to 35 percent, and the potassium fulvate microelement chelate intermediate product accounts for 20 to 25 percent.
Preferably, in the step (2), the particle size of the primary compound fertilizer obtained by granulating, drying and sieving is less than or equal to 3.35mm. Further preferably, in the step (2), the particle size of the primary compound fertilizer obtained by granulating, drying and sieving is 1.75-3.35 mm.
Preferably, in the step (3), the mass ratio of the primary compound fertilizer, the potash magnesium sulphate fertilizer and the binder used for the outer coating treatment is 100: (15-30): (1-3), wherein the binder comprises polyvinyl alcohol and sodium lignin sulfonate, and the mass ratio of the polyvinyl alcohol to the sodium lignin sulfonate is 10: (4-10), wherein the concentration of the binder solution is 0.5-2%. Further preferably, in the step (3), the mass ratio of the primary compound fertilizer, the potassium magnesium sulfate fertilizer and the binder is 100: (20-25): (1-2), wherein the mass ratio of polyvinyl alcohol to sodium lignin sulfonate in the binder is 10: (6-8), wherein the concentration of the binder solution is 1-1.5%.
Preferably, in the step (3), the potassium magnesium sulfate fertilizer is added slowly to prevent agglomeration, and the binder solution is added by spraying for 5-20 min. Further preferably, the addition time is 10 to 15 minutes.
Preferably, in the step (3), the coating time is calculated from the end of the addition of the potassium magnesium sulfate fertilizer and the binder solution, and the coating time is 5-40 min. Further preferably, the coating time may be 20 to 30 minutes.
The following examples are given to illustrate the present invention in further detail, but the scope of the present invention is not limited to the following examples.
The examples do not identify specific experimental procedures or conditions, which may be followed by procedures or conditions that are routine procedures described in the literature in this field.
The reagents and starting materials used in the examples were the same as those commercially available except as otherwise indicated. The potassium fulvate is mineral source potassium fulvate, wherein the mass fraction of the mineral source potassium fulvate is 50% based on dry basis, and the potassium oxide (K 2 The mass fraction of O) is 10%; potassium oxide (K) in the used potassium magnesium sulfate fertilizer 2 O) is 30% by mass, magnesium (Mg) is 7% by mass, and sulfur (S) is 18% by mass; the mass fraction of available phosphorus in the used calcium superphosphate is 18%; the mass fraction of total nitrogen in the urea is 45%; the average degree of polymerization of the polyvinyl alcohol used was 1750.+ -.50.
Example 1
The embodiment provides a compound fertilizer for chelating medium trace elements by humic acid, as shown in figure 1, and the preparation method comprises the following steps:
(1) Preparing a potassium fulvate trace element chelate intermediate: respectively crushing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate, and then uniformly mixing; gradually adding a certain amount of water for mixing, and reacting for 2 hours at the temperature of 60 ℃ to obtain a potassium fulvate trace element chelate intermediate product; wherein, the potassium fulvate accounts for 70 percent, the ferrous sulfate accounts for 7 percent, the copper sulfate accounts for 8 percent, the zinc sulfate accounts for 8 percent, and the manganese sulfate accounts for 7 percent; the mass ratio of the added water to the solid was 15:100.
(2) Preparing a primary compound fertilizer: adding potassium magnesium sulfate fertilizer, urea and calcium superphosphate into a potassium fulvate trace element chelate intermediate product according to a certain proportion, reacting for 30min at normal temperature, performing extrusion granulation in an extrusion granulator, drying in a 105 ℃ oven, and screening to obtain a primary compound fertilizer; wherein, the potassium magnesium sulfate fertilizer accounts for 10 percent, the urea accounts for 35 percent, the calcium superphosphate accounts for 30 percent, and the potassium fulvate microelement chelate intermediate product accounts for 25 percent; the particle size diameter of the primary compound fertilizer is less than or equal to 3.35mm.
(3) Coating: mixing polyvinyl alcohol and sodium lignin sulfonate with the mass ratio of 1:1 as a binder and water to obtain a binder solution with the concentration of 1%; placing the primary compound fertilizer into a disc granulator, slowly adding a potassium magnesium sulfate fertilizer, and spraying a binder solution on the surface of the fertilizer, and coating, wherein the mass ratio of the primary compound fertilizer to the potassium magnesium sulfate fertilizer to the binder is 100:20:2, adding the raw materials for 15min, and coating for 30min after the raw materials are added; and then drying at 105 ℃ and sieving with a 5-mesh sieve to obtain the humic acid chelated medium trace element compound fertilizer.
The humic acid chelated medium trace element compound fertilizer prepared in the example is tested according to the regulations of humic acid compound fertilizer (HG/T5046-2016). The total nutrient (N+P) in the humic acid chelated medium trace element compound fertilizer prepared by the embodiment is measured 2 O 5 +K 2 25.58% by mass of O), wherein the mass fraction of N is 12.51%, P 2 O 5 Is 4.28% by mass, K 2 The mass fraction of O is 8.79%; total humic acid content 6.95% and activated humic acid content 4.43%; the standard sieve screening test shows that the mass percentage content of the particles with the granularity diameter of 1-4.75 mm is 91.2%; meets the requirement of the humic acid compound fertilizer (HG/T5046-2016) on the low-concentration humic acid compound fertilizer.
The average crushing pressure of the particles was 58N as measured by an automatic particle strength tester.
Example 2
The embodiment provides a compound fertilizer for chelating medium trace elements by humic acid, as shown in figure 1, and the preparation method comprises the following steps:
(1) Preparing a potassium fulvate trace element chelate intermediate: respectively crushing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate, and then uniformly mixing; gradually adding a certain amount of water for mixing, and reacting for 1.5 hours at the temperature of 50 ℃ to obtain a potassium fulvate trace element chelate intermediate product; wherein the potassium fulvate accounts for 70 percent, the ferrous sulfate accounts for 7 percent, the copper sulfate accounts for 8 percent, the zinc sulfate accounts for 8 percent, and the manganese sulfate accounts for 7 percent; the mass ratio of the added water to the solid is 10:100.
(2) Preparing a primary compound fertilizer: adding potassium magnesium sulfate fertilizer, urea and calcium superphosphate into a potassium fulvate trace element chelate intermediate product according to a certain proportion, reacting for 30min at normal temperature, performing extrusion granulation in an extrusion granulator, drying in a 105 ℃ oven, and screening to obtain a primary compound fertilizer; wherein, the proportion of the potassium magnesium sulfate fertilizer is 10%, the proportion of the urea is 30%, the proportion of the calcium superphosphate is 35%, and the proportion of the potassium fulvate microelement chelate intermediate product is 25%; the particle size diameter of the primary compound fertilizer is less than or equal to 3.35mm.
(3) Coating: mixing polyvinyl alcohol and sodium lignin sulfonate with the mass ratio of 10:8 as a binder and water to obtain a binder solution with the concentration of 1.5%; placing the primary compound fertilizer into a disc granulator, slowly adding a potassium magnesium sulfate fertilizer, and spraying a binder solution on the surface of the fertilizer, and coating, wherein the mass ratio of the primary compound fertilizer to the potassium magnesium sulfate fertilizer to the binder is 100:25:1, adding raw materials for 15min, and coating for 30min after the raw materials are added; and then drying at 105 ℃ and sieving with a 5-mesh sieve to obtain the humic acid chelated medium trace element compound fertilizer.
The humic acid chelated medium trace element compound fertilizer prepared in the example is tested according to the regulations of humic acid compound fertilizer (HG/T5046-2016). The total nutrient (N+P) in the humic acid chelated medium trace element compound fertilizer prepared by the embodiment is measured 2 O 5 +K 2 25.33% by mass of O), wherein the mass fraction of N is 11.58%, P 2 O 5 Is 4.12% by mass, K 2 The mass fraction of O is 9.63%; total humic acid content 6.59%, activated humic acid content 4.13%; through standard sieve screening test, the mass percentage content of the particles with the granularity diameter of 1-4.75 mm is 90.6%; meets the requirement of the humic acid compound fertilizer (HG/T5046-2016) on the low-concentration humic acid compound fertilizer. The average crushing resistance of the particles was measured by an automatic particle strength tester and found to be 51N.
Example 3
The embodiment provides a compound fertilizer for chelating medium trace elements by humic acid, as shown in figure 1, and the preparation method comprises the following steps:
(1) Preparing a potassium fulvate trace element chelate intermediate: respectively crushing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate, and then uniformly mixing; gradually adding a certain amount of water for mixing, and reacting for 2 hours at the temperature of 60 ℃ to obtain a potassium fulvate trace element chelate intermediate product; wherein, the potassium fulvate accounts for 80 percent, the ferrous sulfate accounts for 5 percent, the copper sulfate accounts for 5 percent, the zinc sulfate accounts for 5 percent, and the manganese sulfate accounts for 5 percent; the mass ratio of the added water to the solid was 15:100.
(2) Preparing a primary compound fertilizer: adding potassium magnesium sulfate fertilizer, urea and calcium superphosphate into a potassium fulvate trace element chelate intermediate product according to a certain proportion, reacting for 40min at normal temperature, then carrying out extrusion granulation in an extrusion granulator, drying in a drying oven at 105 ℃, and screening to obtain a primary compound fertilizer; wherein, the proportion of the potassium magnesium sulfate fertilizer is 10%, the proportion of the urea is 35%, the proportion of the calcium superphosphate is 35%, and the proportion of the potassium fulvate microelement chelate intermediate product is 20%; the particle size of the primary compound fertilizer is 1.75-3.35 mm.
(3) Coating: mixing polyvinyl alcohol and sodium lignin sulfonate with the mass ratio of 10:8 as a binder with water to obtain a binder solution with the concentration of 1.5%, placing the primary compound fertilizer into a disc granulator, slowly adding a potassium magnesium sulfate fertilizer, spraying the binder solution on the surface of the primary compound fertilizer, and coating, wherein the mass ratio of the primary compound fertilizer to the potassium magnesium sulfate fertilizer to the binder is 100:25:2, adding the raw materials for 10min, and coating for 30min after the raw materials are added; and then drying at 105 ℃, and sieving with a 5-mesh sieve to obtain the humic acid chelated medium trace element compound fertilizer with slow and controlled release.
The humic acid chelated medium trace element compound fertilizer prepared in the example is tested according to the regulations of humic acid compound fertilizer (HG/T5046-2016). The total nutrient (N+P) in the humic acid chelated medium trace element compound fertilizer prepared by the embodiment is measured 2 O 5 +K 2 The mass fraction of O) is 25.75%,wherein the mass fraction of N is 12.11%, P 2 O 5 Is 4.55% by mass, K 2 The mass fraction of O is 9.09%; total humic acid content 6.09%, activated humic acid content 3.69%; through standard sieve screening test, the mass percentage content of the particles with the granularity diameter of 1-4.75 mm is 93.6%; meets the requirement of the humic acid compound fertilizer (HG/T5046-2016) on the low-concentration humic acid compound fertilizer. The average crushing resistance of the particles was 64N as measured by an automatic particle strength tester.
Example 4
The embodiment provides a compound fertilizer for chelating medium trace elements by humic acid, as shown in figure 1, and the preparation method comprises the following steps:
(1) Preparing a potassium fulvate trace element chelate intermediate: respectively crushing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate, and then uniformly mixing; gradually adding a certain amount of water for mixing, and reacting for 2 hours at 50 ℃ to obtain a potassium fulvate trace element chelate intermediate product; 80 percent of potassium fulvate, 5 percent of ferrous sulfate, 5 percent of copper sulfate, 5 percent of zinc sulfate and 5 percent of manganese sulfate; the mass ratio of the added water to the solid was 15:100.
(2) Preparing a primary compound fertilizer: adding potassium magnesium sulfate fertilizer, urea and calcium superphosphate into a potassium fulvate trace element chelate intermediate product according to a certain proportion, reacting for 30min at normal temperature, performing extrusion granulation in an extrusion granulator, drying in a 105 ℃ oven, and screening to obtain a primary compound fertilizer; 10% of potassium magnesium sulfate fertilizer, 35% of urea, 35% of calcium superphosphate and 20% of potassium fulvate microelement chelate intermediate product; the particle size of the primary compound fertilizer is 1.75-3.35 mm.
(3) Coating: mixing polyvinyl alcohol and sodium lignin sulfonate with the mass ratio of 10:8 as a binder with water to obtain a binder solution with the concentration of 1%, placing the primary compound fertilizer into a disc granulator, slowly adding a potassium magnesium sulfate fertilizer, spraying the binder solution on the surface of the primary compound fertilizer, and coating, wherein the mass ratio of the primary compound fertilizer to the potassium magnesium sulfate fertilizer to the binder is 100:20:2, adding the raw materials for 15min, and coating for 30min after the raw materials are added; and then drying at 105 ℃, and sieving with a 5-mesh sieve to obtain the humic acid chelated medium trace element compound fertilizer with slow and controlled release.
The humic acid chelated medium trace element compound fertilizer prepared in the example is tested according to the regulations of humic acid compound fertilizer (HG/T5046-2016). The total nutrient (N+P) in the humic acid chelated medium trace element compound fertilizer prepared by the embodiment is measured 2 O 5 +K 2 25.66% by mass of O), wherein the mass fraction of N is 12.45%, P 2 O 5 Is 5.09% by mass, K 2 The mass fraction of O is 8.12%; total humic acid content 6.36% and activated humic acid content 4.45%; through standard sieve screening test, the mass percentage content of the particles with the granularity diameter of 1-4.75 mm is 92.1%; meets the requirement of the humic acid compound fertilizer (HG/T5046-2016) on the low-concentration humic acid compound fertilizer. The average crushing resistance of the particles was 55N as measured by an automatic particle strength tester.
Comparative example 1
The comparative example provides a compound fertilizer for chelating trace elements in humic acid, as shown in figure 1, and the preparation method comprises the following steps:
(1) Preparing a potassium fulvate trace element chelate intermediate: respectively crushing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate, and then uniformly mixing; gradually adding a certain amount of water for mixing, and reacting for 2 hours at the temperature of 60 ℃ to obtain a potassium fulvate trace element chelate intermediate product; wherein, the potassium fulvate accounts for 80 percent, the ferrous sulfate accounts for 5 percent, the copper sulfate accounts for 5 percent, the zinc sulfate accounts for 5 percent, and the manganese sulfate accounts for 5 percent; the mass ratio of the added water to the solid was 30:100.
(2) Preparing a primary compound fertilizer: adding potassium magnesium sulfate fertilizer, urea and calcium superphosphate into a potassium fulvate trace element chelate intermediate product according to a certain proportion, reacting for 30min at normal temperature, performing extrusion granulation in an extrusion granulator, drying in a 105 ℃ oven, and screening to obtain a primary compound fertilizer; 15% of potassium magnesium sulfate fertilizer, 35% of urea, 35% of calcium superphosphate and 15% of potassium fulvate microelement chelate intermediate product; the particle size of the primary compound fertilizer is 1.75-3.35 mm.
(3) Coating: mixing polyvinyl alcohol and sodium lignin sulfonate with the mass ratio of 10:8 as a binder with water to obtain a binder solution with the concentration of 1%, placing the primary compound fertilizer into a disc granulator, slowly adding a potassium magnesium sulfate fertilizer, spraying the binder solution on the surface of the primary compound fertilizer, and coating, wherein the mass ratio of the primary compound fertilizer to the potassium magnesium sulfate fertilizer to the binder is 100:20:2, adding the raw materials for 15min, and coating for 30min after the raw materials are added; and then drying at 105 ℃, and sieving with a 5-mesh sieve to obtain the humic acid chelated medium trace element compound fertilizer with slow and controlled release.
In the step (1) of the comparative example, the content of the potassium fulvate is reduced, the total humic acid content is only 4.81 percent, and the requirement of the humic acid compound fertilizer with low concentration in the humic acid compound fertilizer (HG/T5046-2016) is not met. In addition, the mass ratio of the water added to the solid in the step (1) of this comparative example was 30:100, the excessive addition of water under the condition can cause agglomeration of particles, and after extrusion granulation, a part of particles are agglomerated together, so that screening in the step (2) is difficult, and a part of particles collapse, do not form balls and are unfavorable for the next coating.
Comparative example 2
The comparative example provides a compound fertilizer for chelating trace elements in humic acid, as shown in figure 1, and the preparation method comprises the following steps:
(1) Preparing a potassium fulvate trace element chelate intermediate: respectively crushing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate, and then uniformly mixing; gradually adding a certain amount of water for mixing, and reacting for 2 hours at 50 ℃ to obtain a potassium fulvate trace element chelate intermediate product; 80 percent of potassium fulvate, 5 percent of ferrous sulfate, 5 percent of copper sulfate, 5 percent of zinc sulfate and 5 percent of manganese sulfate; the mass ratio of the added water to the solid was 15:100.
(2) Preparing a primary compound fertilizer: adding potassium magnesium sulfate fertilizer, urea and calcium superphosphate into a potassium fulvate trace element chelate intermediate product according to a certain proportion, reacting for 30min at normal temperature, performing extrusion granulation in an extrusion granulator, drying in a 105 ℃ oven, and screening to obtain a primary compound fertilizer; 10% of potassium magnesium sulfate fertilizer, 35% of urea, 35% of calcium superphosphate and 20% of potassium fulvate microelement chelate intermediate product; the particle size of the primary compound fertilizer is 1.75-3.35 mm.
(3) Coating: mixing polyvinyl alcohol and sodium lignin sulfonate with the mass ratio of 10:8 as a binder with water to obtain a binder solution with the concentration of 3%, placing the primary compound fertilizer into a disc granulator, slowly adding a potassium magnesium sulfate fertilizer, spraying the binder solution on the surface of the primary compound fertilizer, and coating, wherein the mass ratio of the primary compound fertilizer to the potassium magnesium sulfate fertilizer to the binder is 100:20:2, adding the raw materials for 15min, and coating for 30min after the raw materials are added; and then drying at 105 ℃ and sieving with a 5-mesh sieve to obtain the humic acid chelated medium trace element compound fertilizer.
The comparative example step (1) and step (2) are consistent with example 4, and the concentration of polyvinyl alcohol and sodium lignin sulfonate is increased when step (3) is carried out, so that the viscosity of the binder is too high, the coating is too fast, the coating is uneven, and the agglomeration phenomenon exists; through the screening test of a standard sieve, the particles with the granularity of more than 4.75mm are increased, and the qualification rate of the particles with the granularity of 1-4.75 mm is reduced by only 46%.
Comparative example 3
This comparative example was intended to prepare a compound fertilizer of humic acid chelated medium trace elements, wherein step (1) and step (2) were the same as in example 4, but step (3) was not carried out.
(1) Preparing a potassium fulvate trace element chelate intermediate: respectively crushing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate, and then uniformly mixing; gradually adding a certain amount of water for mixing, and reacting for 2 hours at 50 ℃ to obtain a potassium fulvate trace element chelate intermediate product; 80 percent of potassium fulvate, 5 percent of ferrous sulfate, 5 percent of copper sulfate, 5 percent of zinc sulfate and 5 percent of manganese sulfate; the mass ratio of the added water to the solid was 15:100.
(2) Preparing a primary compound fertilizer: adding potassium magnesium sulfate fertilizer, urea and calcium superphosphate into a potassium fulvate trace element chelate intermediate product according to a certain proportion, reacting for 30min at normal temperature, performing extrusion granulation in an extrusion granulator, drying in a 105 ℃ oven, and screening to obtain a primary compound fertilizer with the particle size range of 1-4.75 mm; 10% of potassium magnesium sulfate fertilizer, 35% of urea, 35% of calcium superphosphate and 20% of potassium fulvate microelement chelate intermediate product.
The humic acid chelated medium trace element compound fertilizer prepared in the example is tested according to the regulations of humic acid compound fertilizer (HG/T5046-2016). The total nutrient (N+P) in the humic acid chelated medium trace element compound fertilizer prepared by the embodiment is measured 2 O 5 +K 2 25.83% by mass of O), wherein the mass fraction of N is 15.25%, P 2 O 5 Is 6.15% by mass, K 2 The mass fraction of O is 4.43%; total humic acid content 7.67%, activated humic acid content 5.12%; meets the requirement of the humic acid compound fertilizer (HG/T5046-2016) on the low-concentration humic acid compound fertilizer. The average crushing resistance of the granules was 41N, which was not significantly inferior to that of example 4, as measured by an automatic granule strength tester, and the granules were not spherical and irregular in shape.
Comparative example 4
The comparative example attempts to provide a compound fertilizer of humic acid chelated medium trace elements, and the preparation method comprises the following steps:
(1) Preparing a potassium fulvate trace element chelate intermediate: respectively crushing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate, and then uniformly mixing; gradually adding a certain amount of water for mixing, and reacting for 2 hours at 50 ℃ to obtain a potassium fulvate trace element chelate intermediate product; in the raw materials of the step, the proportion of potassium fulvate is 80%, the proportion of ferrous sulfate is 5%, the proportion of copper sulfate is 5%, the proportion of zinc sulfate is 5%, and the proportion of manganese sulfate is 5%; the mass ratio of the added water to the solid was 15:100.
(2) Preparing a primary compound fertilizer: adding potassium magnesium sulfate fertilizer into the potassium fulvate microelement chelate intermediate product according to a certain proportion, reacting for 30min at normal temperature, and then performing extrusion granulation in an extrusion granulator. And then drying in a 105 ℃ oven, and screening to obtain the primary compound fertilizer.
The comparative example is not added with urea and superphosphate, has poor particle cohesiveness, serious pulverization and unsuccessful pelleting.
Comparative example 5
The comparative example attempts to provide a compound fertilizer of humic acid chelated medium trace elements, and the preparation method comprises the following steps:
(1) Preparing a potassium fulvate trace element chelate intermediate: respectively crushing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate, and then uniformly mixing; gradually adding a certain amount of water for mixing, and reacting for 2 hours at 50 ℃ to obtain a potassium fulvate trace element chelate intermediate product; in the raw materials of the step, the proportion of potassium fulvate is 80%, the proportion of ferrous sulfate is 5%, the proportion of copper sulfate is 5%, the proportion of zinc sulfate is 5%, and the proportion of manganese sulfate is 5%; the mass ratio of the added water to the solid was 15:100.
(2) Preparing a primary compound fertilizer: adding potassium magnesium sulfate fertilizer and calcium superphosphate into the potassium fulvate microelement chelate intermediate product according to a certain proportion, reacting for 30min at normal temperature, and then performing extrusion granulation in an extrusion granulator. And then drying in a 105 ℃ oven, and screening to obtain the primary compound fertilizer.
The comparative example was not added with urea, the granule cohesiveness was poor, the pulverization was severe, and the pelletization was unsuccessful.
Comparative example 6
The comparative example attempts to provide a compound fertilizer of humic acid chelated medium trace elements, and the preparation method comprises the following steps:
(1) Preparing a potassium fulvate trace element chelate intermediate: respectively crushing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate, and then uniformly mixing; gradually adding a certain amount of water for mixing, and reacting for 2 hours at 50 ℃ to obtain a potassium fulvate trace element chelate intermediate product; 80 percent of potassium fulvate, 5 percent of ferrous sulfate, 5 percent of copper sulfate, 5 percent of zinc sulfate and 5 percent of manganese sulfate; the mass ratio of the added water to the solid was 15:100.
(2) Preparing a primary compound fertilizer: adding potassium magnesium sulfate fertilizer and urea into the potassium fulvate microelement chelate intermediate product according to a certain proportion, reacting for 30min at normal temperature, and then performing extrusion granulation in an extrusion granulator. Then drying in a baking oven at 105 ℃, and screening to obtain a primary compound fertilizer; in the raw materials of the step, the proportion of the potassium magnesium sulfate fertilizer is 30%, the proportion of the urea is 50%, and the proportion of the potassium fulvate microelement chelate intermediate product is 20%; the particle size of the primary compound fertilizer is 1.75-3.35 mm.
In this comparative example, no superphosphate was added, and the amount of fine particles during sieving was increased as compared with example 4. The average crushing resistance of the particles was 35N, lower than that of comparative example 3, as measured by an automatic particle strength tester.
According to the embodiment and the comparative example, the preparation method of the compound fertilizer with trace elements in humic acid chelation is provided, the prepared compound fertilizer meets the requirement of low-concentration humic acid compound fertilizer in humic acid compound fertilizer (HG/T5046-2016), the selected raw materials are common raw materials, the operation method is simple, the preparation equipment is conventional and easy to operate, the prepared compound fertilizer product has comprehensive nutrient elements, the product has the effect of slow and controlled release, the strength is high, and the requirement of long-distance transportation can be met.
In the present invention, unless otherwise understood in conjunction with the text, the expression "a/B" should be interpreted as any of the following three parallel cases: a, A is as follows; b, a step of preparing a composite material; a and B.
It is also to be noted that, in the present invention, the relative terms are to be construed as follows unless otherwise understood in conjunction with the entirety. Relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element.
While the invention has been disclosed by the foregoing description of specific embodiments thereof, it will be appreciated that those skilled in the art may devise various modifications, adaptations, or equivalents of the invention within the spirit and scope of the appended claims. Such modifications, improvements, or equivalents are intended to be included within the scope of this invention as claimed.
Claims (10)
1. The preparation method of the compound fertilizer for chelating the medium trace elements by humic acid is characterized by comprising the following steps:
step one, mixing potassium fulvate, ferrous sulfate, copper sulfate, zinc sulfate and manganese sulfate with a certain amount of water, and reacting for a certain time at a certain temperature to obtain a potassium fulvate microelement chelate intermediate product;
mixing the potassium magnesium sulfate fertilizer, urea and calcium superphosphate with the potassium fulvate microelement chelate intermediate product according to a certain proportion, reacting for a certain time at a certain temperature, granulating, drying and screening to obtain a primary compound fertilizer;
and thirdly, performing outer coating treatment on the primary compound fertilizer, drying and screening to obtain the humic acid chelated medium trace element compound fertilizer.
2. The preparation method according to claim 1, wherein in the first step, the preparation method comprises the following raw material components in percentage by weight: 60-80% of potassium fulvate, 5-10% of ferrous sulfate, 5-10% of copper sulfate, 5-10% of zinc sulfate and 5-10% of manganese sulfate; preferably, the potassium fulvate accounts for 70-80%, the ferrous sulfate accounts for 5-8%, the copper sulfate accounts for 5-8%, the zinc sulfate accounts for 5-8%, and the manganese sulfate accounts for 5-8%.
3. The preparation method according to claim 1 or 2, wherein in the first step, the reaction temperature is 50-70 ℃ and the reaction time is 1-2 h; preferably, in the first step, the reaction temperature is 60-70 ℃ and the reaction time is 1.5-2 h.
4. A method according to any one of claims 1 to 3, wherein in step one, the mass ratio of water added to solids is (10 to 20): 100; preferably (10 to 15): 100.
5. the preparation method according to any one of claims 1 to 4, wherein in the second step, the raw material components by weight percentage are as follows: 10-30% of potassium magnesium sulfate fertilizer, 15-35% of urea, 30-40% of superphosphate and 20-30% of potassium fulvate microelement chelate intermediate product; preferably, the potassium magnesium sulfate fertilizer accounts for 10-20%, the urea accounts for 25-35%, the calcium superphosphate accounts for 30-35%, and the potassium fulvate microelement chelate intermediate product accounts for 20-25%.
6. The method according to any one of claims 1 to 5, wherein in the second step, the reaction temperature is normal temperature and the reaction time is 20 to 40 minutes.
7. The method according to any one of claims 1 to 6, wherein in the second step, the primary compound fertilizer has a particle diameter of 3.35mm or less; preferably, the particle size of the primary compound fertilizer is 1.75-3.35 mm.
8. The method according to any one of claims 1 to 7, wherein in step three, the raw materials for the outer coating treatment include a primary compound fertilizer, a potash magnesium sulphate fertilizer and a binder solution; wherein the mass ratio of the binder is 10: polyvinyl alcohol and sodium lignin sulfonate of (4-10), wherein the concentration of the binder solution is 0.5-2%; the mass ratio of the primary compound fertilizer to the potassium magnesium sulfate fertilizer to the binder is 100: (15-30): (1-3);
preferably, the mass ratio of the binder is 10: polyvinyl alcohol and sodium lignin sulfonate of (6-8), wherein the concentration of the binder solution is 1-1.5%, and the mass ratio of the primary compound fertilizer to the potassium magnesium sulfate fertilizer to the binder is 100: (20-25): (1-2).
9. The preparation method of claim 8, wherein in the third step, the potassium magnesium sulfate fertilizer is added slowly, the binder solution is added by spraying, and the adding time is 5-20 min; preferably, the adding time is 10-15 min;
calculating coating time after the addition of the raw materials is finished, wherein the coating time is 5-40 min; preferably, the coating time is 20 to 30 minutes.
10. A compound fertilizer of humic acid chelated medium trace elements, prepared by the preparation method of any one of claims 1-9.
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