CN116178075B - High-efficiency urea-based compound fertilizer and preparation method thereof - Google Patents
High-efficiency urea-based compound fertilizer and preparation method thereof Download PDFInfo
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- CN116178075B CN116178075B CN202310259520.3A CN202310259520A CN116178075B CN 116178075 B CN116178075 B CN 116178075B CN 202310259520 A CN202310259520 A CN 202310259520A CN 116178075 B CN116178075 B CN 116178075B
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- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 239000004202 carbamide Substances 0.000 title claims abstract description 88
- 239000003337 fertilizer Substances 0.000 title claims abstract description 66
- 150000001875 compounds Chemical class 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229920000858 Cyclodextrin Polymers 0.000 claims abstract description 45
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 238000010438 heat treatment Methods 0.000 claims abstract description 39
- 239000000654 additive Substances 0.000 claims abstract description 38
- 230000000996 additive effect Effects 0.000 claims abstract description 38
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 31
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000000843 powder Substances 0.000 claims abstract description 31
- 239000010455 vermiculite Substances 0.000 claims abstract description 31
- 235000019354 vermiculite Nutrition 0.000 claims abstract description 31
- 229910052902 vermiculite Inorganic materials 0.000 claims abstract description 31
- 239000010457 zeolite Substances 0.000 claims abstract description 31
- 239000001116 FEMA 4028 Substances 0.000 claims abstract description 29
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims abstract description 29
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims abstract description 29
- 229960004853 betadex Drugs 0.000 claims abstract description 29
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000002156 mixing Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 23
- LFVGISIMTYGQHF-UHFFFAOYSA-N ammonium dihydrogen phosphate Chemical compound [NH4+].OP(O)([O-])=O LFVGISIMTYGQHF-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910000387 ammonium dihydrogen phosphate Inorganic materials 0.000 claims abstract description 23
- 235000019837 monoammonium phosphate Nutrition 0.000 claims abstract description 23
- 239000006012 monoammonium phosphate Substances 0.000 claims abstract description 23
- HFHDHCJBZVLPGP-UHFFFAOYSA-N schardinger α-dextrin Chemical compound O1C(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC(C(O)C2O)C(CO)OC2OC(C(C2O)O)C(CO)OC2OC2C(O)C(O)C1OC2CO HFHDHCJBZVLPGP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000006185 dispersion Substances 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 15
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 15
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 15
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 15
- 239000008117 stearic acid Substances 0.000 claims abstract description 15
- PUVAFTRIIUSGLK-UHFFFAOYSA-M trimethyl(oxiran-2-ylmethyl)azanium;chloride Chemical compound [Cl-].C[N+](C)(C)CC1CO1 PUVAFTRIIUSGLK-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 14
- 238000012216 screening Methods 0.000 claims abstract description 10
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000002686 phosphate fertilizer Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- SSBRSHIQIANGKS-UHFFFAOYSA-N [amino(hydroxy)methylidene]azanium;hydrogen sulfate Chemical compound NC(N)=O.OS(O)(=O)=O SSBRSHIQIANGKS-UHFFFAOYSA-N 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 3
- 238000004176 ammonification Methods 0.000 description 3
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 3
- 229910052939 potassium sulfate Inorganic materials 0.000 description 3
- 235000011151 potassium sulphates Nutrition 0.000 description 3
- 210000002700 urine Anatomy 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- MZILPZDBVFUXMY-UHFFFAOYSA-N [O-][N+]([S])=O Chemical compound [O-][N+]([S])=O MZILPZDBVFUXMY-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Chemical group 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- WZLMXYBCAZZIRQ-UHFFFAOYSA-N [N].[P].[K] Chemical compound [N].[P].[K] WZLMXYBCAZZIRQ-UHFFFAOYSA-N 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 230000004720 fertilization Effects 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002372 labelling Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 230000004083 survival effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B7/00—Fertilisers based essentially on alkali or ammonium orthophosphates
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/30—Anti-agglomerating additives; Anti-solidifying additives
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/40—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting fertiliser dosage or release rate; for affecting solubility
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/80—Soil conditioners
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G3/00—Mixtures of one or more fertilisers with additives not having a specially fertilising activity
- C05G3/90—Mixtures of one or more fertilisers with additives not having a specially fertilising activity for affecting the nitrification of ammonium compounds or urea in the soil
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05G—MIXTURES OF FERTILISERS COVERED INDIVIDUALLY BY DIFFERENT SUBCLASSES OF CLASS C05; MIXTURES OF ONE OR MORE FERTILISERS WITH MATERIALS NOT HAVING A SPECIFIC FERTILISING ACTIVITY, e.g. PESTICIDES, SOIL-CONDITIONERS, WETTING AGENTS; FERTILISERS CHARACTERISED BY THEIR FORM
- C05G5/00—Fertilisers characterised by their form
- C05G5/10—Solid or semi-solid fertilisers, e.g. powders
- C05G5/12—Granules or flakes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
- Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Pest Control & Pesticides (AREA)
- Soil Sciences (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a high-efficiency urea-based compound fertilizer and a preparation method thereof, relating to the technical field of compound fertilizers, and comprising the following steps: s1, preparing a modified additive: mixing, roasting and crushing zeolite powder, diatomite and vermiculite; adding beta-cyclodextrin into water, heating, stirring and dissolving to form cyclodextrin dispersion liquid; adding the roasting material into cyclodextrin dispersion liquid, continuously adding polyethylene glycol and 2, 3-epoxypropyl trimethyl ammonium chloride, stirring and heating; continuously adding stearic acid and octadecylamine, and heating to obtain a modified additive; s2, mixing urea, sulfuric acid, liquid ammonia, monoammonium phosphate and diamine phosphate for reaction to obtain a reaction solution; and S3, uniformly mixing the modified additive in the step S14 with the reaction liquid in the step S2, granulating, drying, cooling and screening to obtain the urea-based compound fertilizer. The invention has the beneficial effects that the modified additive is mixed with urea, phosphate fertilizer and the like, so that the caking of the compound fertilizer is reduced, and the long-acting and slow release of the fertilizer is realized.
Description
Technical Field
The invention relates to the technical field of compound fertilizers, in particular to a high-efficiency urea-based compound fertilizer and a preparation method thereof.
Background
With the continuous adjustment of the agricultural industry structure, the economic crops occupy larger proportion in the agricultural production, so that the requirements of the market on fertilizer production are also higher. On the other hand, the compound fertilizer industry in China has been rapidly developed in recent years, the market competition is increasingly strong, and whether high-quality and high-efficiency compound fertilizer products can be produced is a key factor related to the survival and development of enterprises. In a sense, the competition of the domestic compound fertilizer industry is competition of quality and cost at present.
The compound fertilizer refers to a chemical fertilizer containing three elements of nitrogen, phosphorus and potassium or only any two of the three elements; the fertilizer is mainly divided into sulfur-based, chlor-based, urine-based, nitro-sulfur-based and the like according to the nutrient proportion, wherein the sulfur-based compound fertilizer is a compound fertilizer prepared from potassium sulfate as a source of potassium element, the chlor-based compound fertilizer is a compound fertilizer prepared from potassium element in the form of potassium chloride, the urine-based compound fertilizer is a compound fertilizer prepared from nitrogen element in the compound fertilizer in the form of urea, the nitro-sulfur-based compound fertilizer is a compound fertilizer prepared from ammonium nitrate, the potassium element is prepared from potassium sulfate as a source of potassium element, or dechlorinated potassium chloride ions are removed.
The urea-based compound fertilizer is a high-concentration nitrogen-phosphorus-potassium multi-element compound fertilizer prepared by using urea as a nitrogen source and basic fertilizers such as ammonium chloride, potassium sulfate, heavy calcium, ammonium phosphate and the like as raw materials and carrying out secondary processing, and common production methods include an extrusion method, a granule method, a slurry method, a melt method and the like.
Because the urea-based compound fertilizer contains a large number of O, N, H atoms, hydrogen bond chains are more easily formed with H 2 O molecules, and the intermolecular force of the hydrogen bond chains promotes the mutual adhesion of the urea-based compound fertilizers; and urea itself has stronger hygroscopicity and is easy to form a lattice compound, so that the urea-based compound fertilizer is easy to absorb moisture in preparation and storage to generate caking and pulverization, and the fertilizer after caking can lead to cracking in the storage and transportation processes on one hand, and can easily lead to blocking of a spray head in the fertilization process on the other hand, so that the application is influenced.
Disclosure of Invention
The invention aims to at least solve one of the technical problems in the prior art and provides a high-efficiency urea-based compound fertilizer and a preparation method thereof.
The technical scheme of the invention is as follows:
the first aspect of the invention provides a preparation method of a high-efficiency urea-based compound fertilizer, which comprises the following steps:
s1, preparing a modified additive:
S11, mixing zeolite powder, diatomite and vermiculite, roasting, and crushing to 1000-1500 meshes to obtain a roasting material;
s12, adding beta-cyclodextrin into water, heating to 60-80 ℃, and stirring and dissolving to form cyclodextrin dispersion liquid;
S13, adding the roasting material in the step S11 into the cyclodextrin dispersion liquid in the step S12, continuously adding polyethylene glycol and 2, 3-epoxypropyl trimethyl ammonium chloride, stirring, and heating at 60-70 ℃ for 2-4 h;
S14, continuously adding stearic acid and octadecylamine, and heating at 30-40 ℃ for 1-2 h to obtain a modified additive;
s2, mixing urea, sulfuric acid, liquid ammonia, monoammonium phosphate and diamine phosphate for reaction to obtain a reaction solution;
And S3, uniformly mixing the modified additive in the step S14 with the reaction liquid in the step S2, granulating, drying, cooling and screening to obtain the urea-based compound fertilizer.
Preferably, in the step S11, the roasting is performed, firstly, the temperature is raised to 200-280 ℃ at the speed of 1-3 ℃/min, the heat is preserved for 1-2 hours, then the temperature is raised to 400-500 ℃ at the speed of 1-3 ℃/min, the heat is preserved for 1-2 hours, and finally, the temperature is raised to 800-900 ℃ at the speed of 3-5 ℃/min, and the heat is preserved for 1-2 hours.
Preferably, in the steps S11 and S12, the mass ratio of the zeolite powder, the diatomite, the vermiculite and the beta-cyclodextrin is 1-2:1-2:1:1.
Preferably, in the step S13, the addition amount of polyethylene glycol is 1-2 times of the mass of beta-cyclodextrin, and the addition amount of 2, 3-epoxypropyl trimethyl ammonium chloride is 0.3-0.7 times of the mass of beta-cyclodextrin.
Preferably, in the step S14, the addition amount of the stearic acid is 3-5% of the total mass of the zeolite powder, the diatomite and the vermiculite, and the addition amount of the octadecylamine is 6-8% of the total mass of the zeolite powder, the diatomite and the vermiculite.
Preferably, in step S2, urea, sulfuric acid and water are added into a reactor to react, then liquid ammonia is continuously added to react, and finally monoammonium phosphate and diamine phosphate are added to react, so as to obtain a reaction solution.
Preferably, in the step S2, the mass ratio of urea to sulfuric acid to water is 2-4:1-2:0.1-0.2; the addition of the liquid ammonia is 0.4 to 0.6 times of the mass of the urea, the addition of the monoammonium phosphate is 1 to 1.2 times of the mass of the urea, and the addition of the diamine phosphate is 0.8 to 1 time of the mass of the urea respectively.
Preferably, in step S3, the addition amount of the modifying additive is 5-10% of the mass of urea, and the granulating temperature is 60-70 ℃.
The second aspect of the invention provides a high-efficiency urea-based compound fertilizer, which is characterized in that the urea-based compound fertilizer is prepared by the method of any one of claims 1-8.
The invention has at least one of the following beneficial effects:
1. According to the invention, the modified additive is prepared, and the modified additive is mixed with urea, phosphate fertilizer and the like, so that the caking of the compound fertilizer is reduced, specifically, zeolite powder, diatomite and vermiculite can be adhered to the surfaces of fertilizer particles to form a barrier for crystal connection among the particles, so that the purpose of inhibiting the caking of the fertilizer is achieved. In addition, the zeolite powder, the diatomite and the vermiculite can play a role in slow release of fertilizer efficiency, realize long-acting and slow release of the fertilizer, play a role in improving soil and reducing loss of nutrient elements, and the modified cyclodextrin can be combined with the fertilizer, so that the slow release effect can be further improved.
2. The invention firstly reacts urea with sulfuric acid and water to generate urea sulfate; continuously adding liquid ammonia, and carrying out primary ammonification reaction on urea sulfate and urea sulfate to generate ammonia sulfate; finally, monoammonium phosphate and diamine phosphate are added for secondary ammoniation reaction; because urea reacts with sulfuric acid and water to generate urea sulfate, and the primary ammonification reaction and the secondary ammonification reaction are exothermic reactions, the urea is not required to be heated to be in a molten state, and the energy consumption is reduced; and a large amount of reaction heat is generated through the reaction, so that the viscosity of the material can be increased, and the pelletization rate is facilitated.
Detailed Description
The present invention will be described in further detail with reference to the following specific examples, but the present invention is not limited to the following specific examples.
Example 1
The preparation method of the high-efficiency urea-based compound fertilizer comprises the following steps:
s1, preparing a modified additive:
S11, mixing zeolite powder, diatomite and vermiculite, roasting, heating to 200 ℃ at a speed of 1 ℃/min, preserving heat for 2 hours, heating to 400 ℃ at a speed of 1 ℃/min, preserving heat for 2 hours, heating to 800 ℃ at a speed of 3 ℃/min, preserving heat for 2 hours, and crushing to 1000-1500 meshes to obtain a roasting material;
S12, adding beta-cyclodextrin into water, heating to 60 ℃, and stirring and dissolving to form cyclodextrin dispersion liquid;
s13, adding the roasting material in the step S11 into the cyclodextrin dispersion liquid in the step S12, continuously adding polyethylene glycol and 2, 3-epoxypropyl trimethyl ammonium chloride, stirring, and heating at 60 ℃ for 4 hours;
s14, continuously adding stearic acid and octadecylamine, and heating at 30 ℃ for 2 hours to obtain a modified additive;
wherein the mass ratio of the zeolite powder, the diatomite, the vermiculite and the beta-cyclodextrin is 1:1:1:1.
The addition amount of polyethylene glycol is 1 time of the mass of beta-cyclodextrin, and the addition amount of 2, 3-epoxypropyl trimethyl ammonium chloride is 0.3 time of the mass of beta-cyclodextrin.
The addition amount of stearic acid is 3% of the total mass of zeolite powder, diatomite and vermiculite, and the addition amount of octadecylamine is 6% of the total mass of zeolite powder, diatomite and vermiculite.
S2, mixing urea, sulfuric acid, liquid ammonia, monoammonium phosphate and diamine phosphate for reaction to obtain a reaction solution; specifically, urea, sulfuric acid and water are added into a reactor for reaction, then liquid ammonia is continuously added for reaction, and finally monoammonium phosphate and diamine phosphate are added for reaction, so that a reaction liquid is obtained.
Wherein the mass ratio of urea to sulfuric acid to water is 2:1:0.1; the addition of the liquid ammonia is 0.4 times of the mass of the urea, the addition of the monoammonium phosphate is 1 time of the mass of the urea, and the addition of the diamine phosphate is 0.8 to 1 time of the mass of the urea respectively.
And S3, uniformly mixing the modified additive in the step S14 with the reaction liquid in the step S2, granulating, drying, cooling and screening, wherein the addition amount of the modified additive is 5% of the mass of urea, and the granulating temperature is 60 ℃ to obtain the urea-based compound fertilizer.
Example 2
The preparation method of the high-efficiency urea-based compound fertilizer comprises the following steps:
s1, preparing a modified additive:
S11, mixing zeolite powder, diatomite and vermiculite, roasting, heating to 220 ℃ at a speed of 2 ℃/min, preserving heat for 2 hours, heating to 420 ℃ at a speed of 2 ℃/min, preserving heat for 1-2 hours, heating to 820 ℃ at a speed of 4 ℃/min, preserving heat for 2 hours, and crushing to 1000-1500 meshes to obtain a roasting material;
s12, adding beta-cyclodextrin into water, heating to 65 ℃, and stirring and dissolving to form cyclodextrin dispersion liquid;
S13, adding the roasting material in the step S11 into the cyclodextrin dispersion liquid in the step S12, continuously adding polyethylene glycol and 2, 3-epoxypropyl trimethyl ammonium chloride, stirring, and heating at 62 ℃ for 3.5h;
S14, continuously adding stearic acid and octadecylamine, and heating at 32 ℃ for 2 hours to obtain a modified additive;
wherein the mass ratio of the zeolite powder, the diatomite, the vermiculite and the beta-cyclodextrin is 1.5:1:1:1.
The addition amount of polyethylene glycol is 1.2 times of the mass of beta-cyclodextrin, and the addition amount of 2, 3-epoxypropyl trimethyl ammonium chloride is 0.4 times of the mass of beta-cyclodextrin.
The addition amount of stearic acid is 3.5% of the total mass of zeolite powder, diatomite and vermiculite, and the addition amount of octadecylamine is 6.5% of the total mass of zeolite powder, diatomite and vermiculite.
S2, mixing urea, sulfuric acid, liquid ammonia, monoammonium phosphate and diamine phosphate for reaction to obtain a reaction solution; specifically, urea, sulfuric acid and water are added into a reactor for reaction, then liquid ammonia is continuously added for reaction, and finally monoammonium phosphate and diamine phosphate are added for reaction, so that a reaction liquid is obtained.
Wherein the mass ratio of urea to sulfuric acid to water is 2.5:1.2:0.12; the addition amount of the liquid ammonia is 0.45 times of the mass of the urea, the addition amount of the monoammonium phosphate is 1.05 times of the mass of the urea, and the addition amount of the diamine phosphate is 0.85 times of the mass of the urea respectively.
And S3, uniformly mixing the modified additive in the step S14 with the reaction liquid in the step S2, granulating, drying, cooling and screening, wherein the addition amount of the modified additive is 6% of the mass of urea, and the granulating temperature is 62 ℃ to obtain the urea-based compound fertilizer.
Example 3
The preparation method of the high-efficiency urea-based compound fertilizer comprises the following steps:
s1, preparing a modified additive:
S11, mixing zeolite powder, diatomite and vermiculite, roasting, heating to 240 ℃ at a speed of 2 ℃/min, preserving heat for 1.5 hours, heating to 450 ℃ at a speed of 2 ℃/min, preserving heat for 1.5 hours, heating to 850 ℃ at a speed of 4 ℃/min, preserving heat for 1.5 hours, and crushing to 1000-1500 meshes to obtain a roasting material;
S12, adding beta-cyclodextrin into water, heating to 70 ℃, and stirring and dissolving to form cyclodextrin dispersion liquid;
S13, adding the roasting material in the step S11 into the cyclodextrin dispersion liquid in the step S12, continuously adding polyethylene glycol and 2, 3-epoxypropyl trimethyl ammonium chloride, stirring, and heating at 65 ℃ for 3 hours;
S14, continuously adding stearic acid and octadecylamine, and heating at 35 ℃ for 1.5 hours to obtain a modified additive;
wherein the mass ratio of the zeolite powder, the diatomite, the vermiculite and the beta-cyclodextrin is 1:1.5:1:1.
The addition amount of polyethylene glycol is 1.5 times of the mass of beta-cyclodextrin, and the addition amount of 2, 3-epoxypropyl trimethyl ammonium chloride is 0.5 times of the mass of beta-cyclodextrin.
The addition amount of stearic acid is 4% of the total mass of zeolite powder, diatomite and vermiculite, and the addition amount of octadecylamine is 7% of the total mass of zeolite powder, diatomite and vermiculite.
S2, mixing urea, sulfuric acid, liquid ammonia, monoammonium phosphate and diamine phosphate for reaction to obtain a reaction solution; specifically, urea, sulfuric acid and water are added into a reactor for reaction, then liquid ammonia is continuously added for reaction, and finally monoammonium phosphate and diamine phosphate are added for reaction, so that a reaction liquid is obtained.
Wherein the mass ratio of urea to sulfuric acid to water is 3:1.5:0.15; the addition amount of the liquid ammonia is 0.5 times of the mass of the urea, the addition amount of the monoammonium phosphate is 1.1 times of the mass of the urea, and the addition amount of the diamine phosphate is 0.9 times of the mass of the urea respectively.
And S3, uniformly mixing the modified additive in the step S14 with the reaction liquid in the step S2, granulating, drying, cooling and screening, wherein the addition amount of the modified additive is 7% of the mass of urea, and the granulating temperature is 65 ℃ to obtain the urea-based compound fertilizer.
Example 4
The preparation method of the high-efficiency urea-based compound fertilizer comprises the following steps:
s1, preparing a modified additive:
S11, mixing zeolite powder, diatomite and vermiculite, roasting, heating to 260 ℃ at a speed of 2 ℃/min, preserving heat for 1.5 hours, heating to 450 ℃ at a speed of 2 ℃/min, preserving heat for 1.5 hours, heating to 850 ℃ at a speed of 4 ℃/min, preserving heat for 1.5 hours, and crushing to 1000-1500 meshes to obtain a roasting material;
S12, adding beta-cyclodextrin into water, heating to 70 ℃, and stirring and dissolving to form cyclodextrin dispersion liquid;
s13, adding the roasting material in the step S11 into the cyclodextrin dispersion liquid in the step S12, continuously adding polyethylene glycol and 2, 3-epoxypropyl trimethyl ammonium chloride, stirring, and heating at 68 ℃ for 3 hours;
S14, continuously adding stearic acid and octadecylamine, and heating at 35 ℃ for 1.5 hours to obtain a modified additive;
wherein the mass ratio of the zeolite powder, the diatomite, the vermiculite and the beta-cyclodextrin is 2:1:1:1.
The addition amount of polyethylene glycol is 2 times of the mass of beta-cyclodextrin, and the addition amount of 2, 3-epoxypropyl trimethyl ammonium chloride is 0.6 times of the mass of beta-cyclodextrin.
The addition amount of stearic acid is 4.5% of the total mass of zeolite powder, diatomite and vermiculite, and the addition amount of octadecylamine is 7.5% of the total mass of zeolite powder, diatomite and vermiculite.
S2, mixing urea, sulfuric acid, liquid ammonia, monoammonium phosphate and diamine phosphate for reaction to obtain a reaction solution; specifically, urea, sulfuric acid and water are added into a reactor for reaction, then liquid ammonia is continuously added for reaction, and finally monoammonium phosphate and diamine phosphate are added for reaction, so that a reaction liquid is obtained.
Wherein the mass ratio of urea to sulfuric acid to water is 3.5:1.8:0.15; the addition amount of the liquid ammonia is 0.55 times of the mass of the urea, the addition amount of the monoammonium phosphate is 1.15 times of the mass of the urea, and the addition amount of the diamine phosphate is 0.95 times of the mass of the urea respectively.
And S3, uniformly mixing the modified additive in the step S14 with the reaction liquid in the step S2, granulating, drying, cooling and screening, wherein the addition amount of the modified additive is 8% of the mass of urea, and the granulating temperature is 68 ℃ to obtain the urea-based compound fertilizer.
Example 5
The preparation method of the high-efficiency urea-based compound fertilizer comprises the following steps:
s1, preparing a modified additive:
s11, mixing zeolite powder, diatomite and vermiculite, roasting, heating to 280 ℃ at a speed of 3 ℃/min, preserving heat for 1h, heating to 500 ℃ at a speed of 3 ℃/min, preserving heat for 1-2 h, heating to 900 ℃ at a speed of 5 ℃/min, preserving heat for 2h, and crushing to 1000-1500 meshes to obtain a roasting material;
s12, adding beta-cyclodextrin into water, heating to 80 ℃, and stirring and dissolving to form cyclodextrin dispersion liquid;
S13, adding the roasting material in the step S11 into the cyclodextrin dispersion liquid in the step S12, continuously adding polyethylene glycol and 2, 3-epoxypropyl trimethyl ammonium chloride, stirring, and heating at 70 ℃ for 2 hours;
s14, continuously adding stearic acid and octadecylamine, and heating at 40 ℃ for 1h to obtain a modified additive;
wherein the mass ratio of the zeolite powder, the diatomite, the vermiculite and the beta-cyclodextrin is 1:2:1:1.
The addition amount of polyethylene glycol is 2 times of the mass of beta-cyclodextrin, and the addition amount of 2, 3-epoxypropyl trimethyl ammonium chloride is 0.7 times of the mass of beta-cyclodextrin.
The addition amount of stearic acid is 5% of the total mass of zeolite powder, diatomite and vermiculite, and the addition amount of octadecylamine is 8% of the total mass of zeolite powder, diatomite and vermiculite.
S2, mixing urea, sulfuric acid, liquid ammonia, monoammonium phosphate and diamine phosphate for reaction to obtain a reaction solution; specifically, urea, sulfuric acid and water are added into a reactor for reaction, then liquid ammonia is continuously added for reaction, and finally monoammonium phosphate and diamine phosphate are added for reaction, so that a reaction liquid is obtained.
Wherein the mass ratio of urea to sulfuric acid to water is 4:2:0.2; the addition amount of the liquid ammonia is 0.6 times of the mass of the urea, the addition amount of the monoammonium phosphate is 1.2 times of the mass of the urea, and the addition amount of the diamine phosphate is 1 time of the mass of the urea respectively.
And S3, uniformly mixing the modified additive in the step S14 with the reaction liquid in the step S2, granulating, drying, cooling and screening, wherein the addition amount of the modified additive is 10% of the mass of urea, and the granulating temperature is 70 ℃ to obtain the urea-based compound fertilizer.
Comparative example 1
The difference from example 1 is that: and (3) directly granulating, drying, cooling and screening the reaction liquid in the step (S2) at the granulating temperature of 60 ℃ to obtain the urea-based compound fertilizer without adding the modifying additive, namely, without adding the modifying additive in the step (S1).
Testing
The caking experiments were carried out on the urine-based compound fertilizer samples prepared in examples 1 to 5 and comparative example 1, respectively, and the specific operations are as follows:
Packaging the treated compound fertilizer samples in two layers by using a sample packaging bag, and labeling for grouping; then, placing the compound fertilizer into an accelerating agglomeration device, applying pressure to a compound fertilizer sample, placing the accelerating agglomeration device into a high-low temperature damp-heat test box, controlling the temperature to be 45-50 ℃ in daytime and the relative humidity to be 70-75%, and turning off a power supply at night to enable the room temperature and the indoor environment humidity to be the same; taking out samples after 5-7 d, respectively dropping three groups of samples from the front side and the back side of the 1m height for 1-2 times, unpacking, screening by a standard screen, and checking the anti-caking effect through the caking rate, wherein the caking rate is calculated according to the following formula:
caking ratio = caking compound fertilizer mass/compound fertilizer mass 100%
The results are shown in Table 1:
TABLE 1
| Caking Rate | |
| Example 1 | 3.2％ |
| Example 2 | 2.8％ |
| Example 3 | 2.3％ |
| Example 4 | 1.4％ |
| Example 5 | 1.9％ |
| Comparative example 1 | 38.5％ |
As can be seen from Table 1, examples 1 to 5 have a relatively low caking rate, and in particular example 4 has a caking rate of only 1.4%. As can be seen by comparing examples 1 to 5 with comparative example 1, the caking rates of examples 1 to 5 were much lower than comparative example 1 (no modifying additive was added), thus demonstrating that the present invention can reduce the caking rate of the compound fertilizer by adding the modifying additive.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (4)
1. The preparation method of the high-efficiency urea-based compound fertilizer is characterized by comprising the following steps of:
s1, preparing a modified additive:
S11, mixing zeolite powder, diatomite and vermiculite, roasting, and crushing to 1000-1500 meshes to obtain a roasted material; wherein the roasting is firstly heated to 200-280 ℃ at a speed of 1-3 ℃/min for heat preservation for 1-2 hours, then heated to 400-500 ℃ at a speed of 1-3 ℃/min for heat preservation for 1-2 hours, and finally heated to 800-900 ℃ at a speed of 3-5 ℃/min for heat preservation for 1-2 hours;
S12, adding beta-cyclodextrin into water, heating to 60-80 ℃, and stirring and dissolving to form cyclodextrin dispersion liquid; wherein the mass ratio of the zeolite powder to the diatomite to the vermiculite to the beta-cyclodextrin is 1-2:1-2:1:1;
S13, adding the roasting material in the step S11 into the cyclodextrin dispersion liquid in the step S12, continuously adding polyethylene glycol and 2, 3-epoxypropyl trimethyl ammonium chloride, stirring, and heating at 60-70 ℃ for 2-4 hours; wherein the addition amount of polyethylene glycol is 1-2 times of the mass of beta-cyclodextrin, and the addition amount of 2, 3-epoxypropyl trimethyl ammonium chloride is 0.3-0.7 times of the mass of beta-cyclodextrin;
S14, continuously adding stearic acid and octadecylamine, and heating at 30-40 ℃ for 1-2 hours to obtain a modified additive; the addition amount of stearic acid is 3-5% of the total mass of zeolite powder, diatomite and vermiculite, and the addition amount of octadecylamine is 6-8% of the total mass of zeolite powder, diatomite and vermiculite;
s2, mixing urea, sulfuric acid, liquid ammonia, monoammonium phosphate and diamine phosphate for reaction to obtain a reaction solution;
S3, uniformly mixing the modified additive in the step S14 with the reaction liquid in the step S2, granulating, drying, cooling and screening to obtain the urea-based compound fertilizer; the addition amount of the modifying additive is 5-10% of the mass of urea, and the granulating temperature is 60-70 ℃.
2. The method for preparing a high-efficiency urea-based compound fertilizer according to claim 1, wherein in the step S2, urea, sulfuric acid and water are added into a reactor for reaction, then liquid ammonia is continuously added for reaction, and finally monoammonium phosphate and diamine phosphate are added for reaction, so that a reaction solution is obtained.
3. The preparation method of the high-efficiency urea-based compound fertilizer according to claim 1, wherein in the step S2, the mass ratio of urea to sulfuric acid to water is 2-4:1-2:0.1-0.2; the addition amount of the liquid ammonia is 0.4-0.6 times of the mass of the urea, the addition amount of the monoammonium phosphate is 1-1.2 times of the mass of the urea, and the addition amount of the diamine phosphate is 0.8-1 time of the mass of the urea respectively.
4. A high-efficiency urea-based compound fertilizer, characterized in that it is prepared by the method of any one of claims 1-3.
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