CN117623825B - Preparation method and application of stable fertilizer - Google Patents
Preparation method and application of stable fertilizer Download PDFInfo
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- CN117623825B CN117623825B CN202311710354.0A CN202311710354A CN117623825B CN 117623825 B CN117623825 B CN 117623825B CN 202311710354 A CN202311710354 A CN 202311710354A CN 117623825 B CN117623825 B CN 117623825B
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- urea
- melamine
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- 239000003337 fertilizer Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 112
- 239000004202 carbamide Substances 0.000 claims abstract description 112
- 238000000576 coating method Methods 0.000 claims abstract description 41
- 239000011248 coating agent Substances 0.000 claims abstract description 39
- 239000002601 urease inhibitor Substances 0.000 claims abstract description 15
- 239000003112 inhibitor Substances 0.000 claims abstract description 14
- 229940090496 Urease inhibitor Drugs 0.000 claims abstract description 13
- 239000002367 phosphate rock Substances 0.000 claims abstract description 9
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000440 bentonite Substances 0.000 claims abstract description 4
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 4
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000463 material Substances 0.000 claims description 65
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 51
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- 238000005507 spraying Methods 0.000 claims description 36
- 238000006243 chemical reaction Methods 0.000 claims description 33
- 239000008367 deionised water Substances 0.000 claims description 32
- 229910021641 deionized water Inorganic materials 0.000 claims description 32
- 239000000203 mixture Substances 0.000 claims description 32
- CKYUSAVHVQKPBQ-UHFFFAOYSA-N 2-n,2-n-bis(ethenyl)-1,3,5-triazine-2,4,6-triamine Chemical compound NC1=NC(N)=NC(N(C=C)C=C)=N1 CKYUSAVHVQKPBQ-UHFFFAOYSA-N 0.000 claims description 27
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 26
- 239000002245 particle Substances 0.000 claims description 25
- 239000011230 binding agent Substances 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 22
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 14
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 14
- 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 claims description 12
- 239000004021 humic acid Substances 0.000 claims description 12
- ROHTVIURAJBDES-UHFFFAOYSA-N 2-n,2-n-bis(prop-2-enyl)-1,3,5-triazine-2,4,6-triamine Chemical compound NC1=NC(N)=NC(N(CC=C)CC=C)=N1 ROHTVIURAJBDES-UHFFFAOYSA-N 0.000 claims description 11
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 11
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 11
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 11
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 11
- 239000003431 cross linking reagent Substances 0.000 claims description 11
- 239000003999 initiator Substances 0.000 claims description 11
- 239000012188 paraffin wax Substances 0.000 claims description 11
- DZSVIVLGBJKQAP-UHFFFAOYSA-N 1-(2-methyl-5-propan-2-ylcyclohex-2-en-1-yl)propan-1-one Chemical compound CCC(=O)C1CC(C(C)C)CC=C1C DZSVIVLGBJKQAP-UHFFFAOYSA-N 0.000 claims description 10
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 10
- 229920002866 paraformaldehyde Polymers 0.000 claims description 10
- PLPFTLXIQQYOMW-UHFFFAOYSA-N 5-chlorobenzene-1,3-dicarboxylic acid Chemical compound OC(=O)C1=CC(Cl)=CC(C(O)=O)=C1 PLPFTLXIQQYOMW-UHFFFAOYSA-N 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 239000005457 ice water Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 230000003472 neutralizing effect Effects 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000007873 sieving Methods 0.000 claims description 9
- 229920000536 2-Acrylamido-2-methylpropane sulfonic acid Polymers 0.000 claims description 4
- XHZPRMZZQOIPDS-UHFFFAOYSA-N 2-Methyl-2-[(1-oxo-2-propenyl)amino]-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(C)(C)NC(=O)C=C XHZPRMZZQOIPDS-UHFFFAOYSA-N 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 21
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 11
- 239000002250 absorbent Substances 0.000 abstract description 4
- 230000002745 absorbent Effects 0.000 abstract description 4
- 229920005989 resin Polymers 0.000 abstract description 4
- 239000011347 resin Substances 0.000 abstract description 4
- 239000011162 core material Substances 0.000 abstract 1
- 239000008187 granular material Substances 0.000 description 55
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 14
- 239000002689 soil Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 10
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 7
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 7
- 239000003822 epoxy resin Substances 0.000 description 7
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 description 7
- 229920000647 polyepoxide Polymers 0.000 description 7
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 4
- 239000000618 nitrogen fertilizer Substances 0.000 description 4
- 108010046334 Urease Proteins 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 230000002401 inhibitory effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- JJERWOHJLOFBPM-UHFFFAOYSA-N prop-1-ene;1,3,5-triazine-2,4,6-triamine Chemical compound CC=C.NC1=NC(N)=NC(N)=N1 JJERWOHJLOFBPM-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 230000001546 nitrifying effect Effects 0.000 description 2
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 2
- 235000015097 nutrients Nutrition 0.000 description 2
- 235000016709 nutrition Nutrition 0.000 description 2
- 230000035764 nutrition Effects 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 241001453382 Nitrosomonadales Species 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 150000002894 organic compounds Chemical group 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
- Fertilizers (AREA)
Abstract
The invention relates to the technical field of fertilizers and discloses a preparation method and application of a stable fertilizer. Finally, urea is taken as a core, phosphorite or bentonite, a urease inhibitor and a nitrification inhibitor are taken as inner coatings, and a super absorbent resin is taken as an outer coating, so that the prepared stable fertilizer has excellent water retention and slow release effects and nitrogen element utilization rate.
Description
Technical Field
The invention relates to the technical field of fertilizers, in particular to a preparation method and application of a stable fertilizer.
Background
The agricultural is a national agricultural science, the agriculture is the basis of national economy, and is the basic material condition for social development, wherein chemical fertilizers and water resources are the important material basis for developing modern agriculture. Because urea has the characteristics of high nitrogen content and small influence on soil quality in the fertilizer field, the urea becomes one of the main nitrogenous fertilizers in the world, but because most of nitrogen elements and phosphorus elements have higher water solubility, most of the nitrogen elements and phosphorus elements are lost to the surrounding environment along with water when the urea is applied to the soil, and the urea is subjected to two processes of hydrolysis and nitration conversion when being applied to the soil and dispersed into various forms, and the small part of the urea is absorbed and utilized by plants, and the large part of the urea is lost in the air or flows through the ground surface, so that the waste of the nitrogenous fertilizer is caused, the utilization rate of the urea is lower, so that the loss and decomposition of the nitrogen elements are reduced, and the increase of the utilization rate of the nitrogen elements in the fertilizer is the key point of the current research of losing weight and enhancing efficiency.
The super absorbent resin is a novel functional polymer material, can absorb water which is hundreds to thousands of times heavier than the super absorbent resin, has the characteristics of high water absorption rate, good water retention property and the like, can be recycled, and is widely applied to the fields of agriculture, gardens, medical sanitation, buildings, petroleum and the like.
Urease is a nickel lazy non-oxidation reductase, which can accelerate the hydrolysis speed of urea, but can reduce the absorption of nitrogen fertilizer by plants and harm to environment and agriculture due to the faster reaction speed. The urease inhibitor is a compound or element with an inhibiting effect on the urease activity, can inhibit the ammonia production reaction of urea, reduce the volatilization loss of ammonia and improve the nitrogen fertilizer utilization rate.
The nitrification inhibitor is an organic or inorganic compound capable of inhibiting the activity of ammonia oxidizing bacteria and nitrifying bacteria, thereby inhibiting the conversion of ammonium nitrogen into nitrifying nitrogen, and prolonging the residence time of the ammonium nitrogen in soil so as to enable plants to absorb and utilize more nitrogen.
For example, the patent with the publication number of CN102976863B discloses a water-retaining slow-release fertilizer, which is prepared by uniformly mixing a slow-release fertilizer, a water-retaining agent, humic acid and the like, and has the characteristics of low cost and simple and convenient application, but the utilization rate of nitrogen is not improved.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a preparation method and application of the stable fertilizer, and the stable fertilizer prepared by the preparation method not only has excellent water retention and slow release effects, but also has higher nitrogen element utilization rate.
A method for preparing a stable fertilizer, the method comprising:
(1) In an ice-water bath, adding 30-40% sodium hydroxide solution into acrylic acid, stirring and neutralizing to adjust the pH to 5-6, adding octacarboxyl divinyl melamine, 2-acrylamido-2-methylpropanesulfonic acid, humic acid and carboxymethyl cellulose into the mixture, stirring uniformly, adding an initiator and a cross-linking agent, heating to 55-70 ℃, reacting for 3-6 hours, drying and crushing after the reaction is finished, and obtaining the coating material.
(2) Sieving urea particles to obtain urea particles with the diameter of 1-3mm, adding the urea particles into a disc granulator, spraying organic binder with the mass fraction of 40-60% on the surfaces of the urea particles until a layer of binder solution appears on the surfaces, adding slow-release materials, urease inhibitors and nitrification inhibitors which are sieved by a sieve with the diameter of 0.1-0.4mm into the urea particles, rotating the slow-release materials until the slow-release materials wrap the urea on the surfaces of the urea particles, spraying heated and melted paraffin into the slow-release materials to obtain coated urea, spraying the organic binder, finally spraying coating material powder into the coated urea particles until the coating material is fully wrapped on the surfaces of the fertilizer, and drying to obtain the stable fertilizer.
Preferably, in the step (1), the mass ratio of the acrylic acid to the octacarboxyl divinyl melamine to the 2-acrylamido-2-methylpropanesulfonic acid to the humic acid to the carboxymethyl cellulose to the initiator to the cross-linking agent is 100:30-50:5-10:10-15:20-30:0.4-0.6:0.1-0.3.
Preferably, in the step (2), the mass ratio of urea, slow-release material, urease inhibitor, nitrification inhibitor paraffin and coating material is 100:20-30:1-3:0.5-2:3-6:2-10.
Preferably, in the step (2), the slow release material is one of bentonite and phosphorite.
Preferably, in the step (1), the preparation method of the octacarboxyl divinyl melamine comprises the following steps:
S1, adding N, N-diallyl melamine and paraformaldehyde into deionized water at 60-75 ℃, adding 10% sodium hydroxide solution into the deionized water to adjust the pH to 8-9, stirring and dispersing, reacting for 40-80min, decompressing and distilling after the reaction is finished, washing with deionized water, filtering and drying to obtain an intermediate 1.
S2, adding the intermediate 1, 5-chloroisophthalic acid into deionized water at 20-35 ℃, stirring and dispersing, adding triethylamine into the mixture, stirring and reacting for 10-24 hours, filtering and drying after the reaction is finished to obtain the octacarboxyl divinyl melamine.
Preferably, in the step S1, the molar ratio of the N, N-diallyl melamine to the paraformaldehyde is 1:4-6.
Preferably, in the step S2, the molar ratio of the intermediate 1, the 5-chloroisophthalic acid and the triethylamine is 1:4-5.2:4.5-5.5.
The invention utilizes N, N-diallyl melamine to sequentially carry out hydroxylation reaction and substitution reaction to obtain octacarboxyl divinyl melamine with novel structure, and then initiates copolymerization and crosslinking with acrylic acid, octacarboxyl divinyl melamine, 2-acrylamide-2-methylpropanesulfonic acid and the like to obtain the coating material. Finally, urea is used as a core, a slow-release material, a urease inhibitor and a nitrification inhibitor are used as inner coatings, and a super absorbent resin is used as an outer coating, so that the fertilizer with water retention and slow release is prepared.
The octacarboxyl divinyl melamine prepared by the invention contains more carboxyl groups, can generate hydrogen bonds with water molecules, has excellent water absorption performance, and can be copolymerized and crosslinked with acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid and the like, wherein the octacarboxyl divinyl melamine contains more carboxyl groups, sulfonic acid groups and the like and has good adsorption effect on the water molecules, so that the prepared coating material has excellent water absorption and retention performances.
When the octacarboxyl divinyl melamine prepared by the method is copolymerized with acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid and the like, a larger cross-linked network structure can be formed, more cross-linked sites are contained, when the octacarboxyl divinyl melamine is impacted, the stress suffered by one molecular chain can be dispersed into other molecular chains through the cross-linked sites, and when one molecular chain breaks, the other molecular chains can play a role in reinforcement, so that the octacarboxyl divinyl melamine has excellent mechanical properties, and the problem that the coating is easy to fall off is solved.
When the fertilizer is applied to the soil, the coating material on the outer layer of the fertilizer particles absorbs water and swells to be converted into gel, water molecules gradually permeate into the inner core, urea in the fertilizer begins to dissolve, and dissolved nutrient elements begin to be gradually released into the soil environment through the outer layer coating in the exchange of dynamic water, so that nutrition is provided for plants. The urease inhibitor used in the invention can inhibit the activity of soil urease, reduce the speed of converting amide organic nitrogen into inorganic ammonium nitrogen, thereby reducing the volatilization and nitrification of ammonium nitrogen fertilizer.
The coated material prepared by the invention has hydrogen bond association with urea, so that the coated material can absorb urea, and when the content of urea in the external environment is low, the urea can be slowly released into the environment, so that the coated material has slow release effect besides the water absorption and water retention effects. The stable fertilizer prepared by the invention has excellent water retention, slow release effect and nitrogen element utilization rate.
Drawings
FIG. 1 is a route to octacarboxyl divinyl melamine.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) At 60 ℃, 20mmol of N, N-diallyl melamine and 100mmol of paraformaldehyde are added into deionized water, 10% sodium hydroxide solution is added into the deionized water to adjust the pH to 8.5, the mixture is stirred and dispersed, the reaction is carried out for 60min, and after the reaction is finished, the mixture is distilled under reduced pressure, washed by deionized water, filtered and dried to obtain an intermediate 1.
(2) At 25 ℃, 10mmol of intermediate 1 and 52mmol of 5-chloroisophthalic acid are added into deionized water, stirred and dispersed, 50mmol of triethylamine is added into the mixture, the mixture is stirred and reacted for 12 hours, and after the reaction is finished, the mixture is filtered and dried to obtain octacarboxyl divinyl melamine.
(3) In an ice-water bath, adding 35% sodium hydroxide solution into 20g of acrylic acid, stirring and neutralizing to adjust the pH to 6, adding 6g of octacarboxyl divinyl melamine, 1g of 2-acrylamide-2-methylpropanesulfonic acid, 3g of humic acid and 5g of carboxymethyl cellulose, stirring uniformly, adding 0.12g of potassium persulfate initiator and 0.05g of N, N-methylenebisacrylamide crosslinking agent, heating to 65 ℃, reacting for 6 hours, drying and crushing after the reaction is finished, and obtaining the coating material.
(4) Sieving urea granules to obtain urea granules with the diameter of 2mm, adding 200g of urea granules into a disc granulator, spraying an epoxy resin E-44 organic binder with the mass fraction of 50% on the surfaces of the urea granules until a layer of binding liquid appears on the surfaces, adding 50g of phosphorite slow-release material which is sieved by a 0.1mm sieve, 2g of urease inhibitor hydroquinone and 4g of nitrification inhibitor dicyandiamide into the urea granules, rotating the urea granules until the slow-release material wraps the urea granules, spraying 10g of heated and melted paraffin into the urea granules to obtain coated urea, spraying an organic binder, finally spraying 4g of coating material powder into the urea granules until the coating material is fully wrapped on the surfaces of the fertilizers, and drying to obtain the stable fertilizer.
Example 2
(1) At 75 ℃, 20mmol of N, N-diallyl melamine and 80mmol of paraformaldehyde are added into deionized water, 10% sodium hydroxide solution is added into the deionized water to adjust the pH to 9, the mixture is stirred and dispersed for reaction for 40min, and after the reaction is finished, the mixture is distilled under reduced pressure, washed by deionized water, filtered and dried to obtain an intermediate 1.
(2) At 35 ℃, 10mmol of intermediate 1 and 40mmol of 5-chloroisophthalic acid are added into deionized water, stirred and dispersed, 50mmol of triethylamine is added into the mixture, the mixture is stirred and reacted for 24 hours, and after the reaction is finished, the mixture is filtered and dried to obtain octacarboxyl divinyl melamine.
(3) In an ice-water bath, adding 32% sodium hydroxide solution into 20g of acrylic acid, stirring and neutralizing to adjust the pH to 6, adding 7g of octacarboxyl divinyl melamine, 2g of 2-acrylamide-2-methylpropanesulfonic acid, 2g of humic acid and 6g of carboxymethyl cellulose, stirring uniformly, adding 0.12g of potassium persulfate initiator and 0.02g of N, N-methylene bisacrylamide cross-linking agent, heating to 70 ℃, reacting for 3 hours, drying and crushing after the reaction is finished, and obtaining the coating material.
(4) Sieving urea granules to obtain urea granules with the diameter of 3mm, adding 200g of urea granules into a disc granulator, spraying epoxy resin E-44 organic binder with the mass fraction of 60% on the surfaces of the urea granules until a layer of binder solution appears on the surfaces, adding 60g of phosphorite slow-release material which is sieved by a 0.1mm sieve, 4g of urease inhibitor hydroquinone and 1g of nitrification inhibitor dicyandiamide into the urea granules, rotating the urea granules until the slow-release material wraps the surfaces of the urea granules, spraying 12g of heated and melted paraffin into the urea granules to obtain coated urea, spraying organic binder, finally spraying 8g of coating material powder into the urea granules until the coating material is fully wrapped on the surfaces of the fertilizer, and drying to obtain the stable fertilizer.
Example 3
(1) At 75 ℃, 20mmol of N, N-diallyl melamine and 90mmol of paraformaldehyde are added into deionized water, 10% sodium hydroxide solution is added into the deionized water to adjust the pH to 9, the mixture is stirred and dispersed for reaction for 80min, and after the reaction is finished, the mixture is distilled under reduced pressure, washed by deionized water, filtered and dried to obtain an intermediate 1.
(2) At 30 ℃, 10mmol of intermediate 1 and 50mmol of 5-chloroisophthalic acid are added into deionized water, stirred and dispersed, 48mmol of triethylamine is added into the mixture, the mixture is stirred and reacted for 20 hours, and after the reaction is finished, the mixture is filtered and dried to obtain octacarboxyl divinyl melamine.
(3) In an ice-water bath, adding 40% sodium hydroxide solution into 20g of acrylic acid, stirring and neutralizing to adjust the pH to 6, adding 8g of octacarboxyl divinyl melamine, 1.5g of 2-acrylamide-2-methylpropanesulfonic acid, 3g of humic acid and 4.5g of carboxymethyl cellulose, stirring uniformly, adding 0.09g of potassium persulfate initiator and 0.05g of N, N-methylenebisacrylamide crosslinking agent, heating to 60 ℃, reacting for 4 hours, drying and crushing after the reaction is finished, and obtaining the coating material.
(4) Sieving urea granules to obtain urea granules with the diameter of 2mm, adding 200g of urea granules into a disc granulator, spraying epoxy resin E-44 organic binder with the mass fraction of 60% on the surfaces of the urea granules until a layer of binder solution appears on the surfaces, adding 40g of phosphorite slow-release material which is sieved by a 0.3mm sieve, 6g of urease inhibitor hydroquinone and 2g of nitrification inhibitor dicyandiamide into the urea granules, rotating the urea granules until the slow-release material wraps the surfaces of the urea granules, spraying 12g of heated and melted paraffin into the urea granules to obtain coated urea, spraying organic binder, finally spraying 12g of coating material powder into the coated urea granules until the coated material is fully wrapped on the surfaces of the fertilizer, and drying to obtain the stable fertilizer.
Example 4
(1) At 70 ℃, 20mmol of N, N-diallyl melamine and 90mmol of paraformaldehyde are added into deionized water, 10% sodium hydroxide solution is added into the deionized water to adjust the pH to 9, the mixture is stirred and dispersed for reaction for 70min, and after the reaction is finished, the mixture is distilled under reduced pressure, washed by deionized water, filtered and dried to obtain an intermediate 1.
(2) At 30 ℃, 10mmol of intermediate 1 and 52mmol of 5-chloroisophthalic acid are added into deionized water, stirred and dispersed, 50mmol of triethylamine is added into the mixture, the mixture is stirred and reacted for 18 hours, and after the reaction is finished, the mixture is filtered and dried to obtain octacarboxyl divinyl melamine.
(3) In an ice-water bath, adding 40% sodium hydroxide solution into 20g of acrylic acid, stirring and neutralizing to adjust the pH to 5, adding 9g of octacarboxyl divinyl melamine, 1.8g of 2-acrylamide-2-methylpropanesulfonic acid, 2.5g of humic acid and 4.5g of carboxymethyl cellulose, stirring uniformly, adding 0.12g of potassium persulfate initiator and 0.05g of N, N-methylene bisacrylamide crosslinking agent, heating to 60 ℃, reacting for 6 hours, drying and crushing after the reaction is finished, and obtaining the coating material.
(4) Sieving urea particles to obtain urea particles with the diameter of 1mm, adding 200g of urea particles into a disc granulator, spraying an epoxy resin E-44 organic binder with the mass fraction of 50% on the surfaces of the urea particles until a layer of binder solution appears on the surfaces, adding 60g of bentonite slow-release material which is sieved by a 0.2mm sieve, 5g of urease inhibitor hydroquinone and 4g of nitrification inhibitor dicyandiamide into the urea particles, rotating the mixture until the slow-release material wraps the urea particles, spraying 10g of heated and melted paraffin into the urea particles to obtain coated urea, spraying an organic binder, finally spraying 16g of coating material powder into the urea particles until the coating material is fully wrapped on the surfaces of the fertilizers, and drying to obtain the stable fertilizer.
Example 5
(1) At 65 ℃,20 mmol of N, N-diallyl melamine and 110mmol of paraformaldehyde are added into deionized water, 10% sodium hydroxide solution is added into the deionized water to adjust the pH to 9, the mixture is stirred and dispersed for reaction for 80min, and after the reaction is finished, the mixture is distilled under reduced pressure, washed by deionized water, filtered and dried to obtain an intermediate 1.
(2) At 35 ℃, 10mmol of intermediate 1 and 45mmol of 5-chloroisophthalic acid are added into deionized water, stirred and dispersed, 48mmol of triethylamine is added into the mixture, stirred and reacted for 24 hours, and after the reaction is finished, the mixture is filtered and dried to obtain octacarboxyl divinyl melamine.
(3) In an ice-water bath, adding 36% sodium hydroxide solution into 20g of acrylic acid, stirring and neutralizing to adjust the pH to 6, adding 10g of octacarboxyl divinyl melamine, 2g of 2-acrylamide-2-methylpropanesulfonic acid, 2g of humic acid and 5g of carboxymethyl cellulose, stirring uniformly, adding 0.1g of potassium persulfate initiator and 0.06g of N, N-methylene bisacrylamide cross-linking agent, heating to 70 ℃, reacting for 5 hours, drying and crushing after the reaction is finished, and obtaining the coating material.
(4) Sieving urea granules to obtain urea granules with the diameter of 1mm, adding 200g of urea granules into a disc granulator, spraying an epoxy resin E-44 organic binder with the mass fraction of 50% on the surfaces of the urea granules until a layer of binder solution appears on the surfaces, adding 50g of phosphorite slow-release material which is sieved by a 0.4mm sieve, 6g of urease inhibitor hydroquinone and 1g of nitrification inhibitor dicyandiamide into the urea granules, rotating the urea granules until the slow-release material wraps the urea granules, spraying 8g of heated and melted paraffin into the urea granules to obtain coated urea, spraying an organic binder, finally spraying 20g of coating material powder into the urea granules until the coating material is fully wrapped on the surfaces of the fertilizers, and drying to obtain the stable fertilizer.
Comparative example 1
(1) At 60 ℃, 20mmol of N, N-diallyl melamine and 100mmol of paraformaldehyde are added into deionized water, 10% sodium hydroxide solution is added into the deionized water to adjust the pH to 8.5, the mixture is stirred and dispersed, the reaction is carried out for 60min, and after the reaction is finished, the mixture is distilled under reduced pressure, washed by deionized water, filtered and dried to obtain an intermediate 1.
(2) In an ice-water bath, adding 35% sodium hydroxide solution into 20g of acrylic acid, stirring and neutralizing to adjust the pH to 6, adding 6g of intermediate 1, 1g of 2-acrylamido-2-methylpropanesulfonic acid, 3g of humic acid and 5g of carboxymethyl cellulose into the mixture, stirring uniformly, adding 0.12g of potassium persulfate initiator and 0.05g of N, N-methylenebisacrylamide cross-linking agent, heating to 65 ℃, reacting for 6h, drying and crushing to obtain the coating material.
(3) Sieving urea granules to obtain urea granules with the diameter of 2mm, adding 200g of urea granules into a disc granulator, spraying an epoxy resin E-44 organic binder with the mass fraction of 50% on the surfaces of the urea granules until a layer of binding liquid appears on the surfaces, adding 50g of phosphorite slow-release material which is sieved by a 0.1mm sieve, 2g of urease inhibitor hydroquinone and 4g of nitrification inhibitor dicyandiamide into the urea granules, rotating the urea granules until the slow-release material wraps the urea granules, spraying 10g of heated and melted paraffin into the urea granules to obtain coated urea, spraying an organic binder, finally spraying 4g of coating material powder into the urea granules until the coating material is fully wrapped on the surfaces of the fertilizers, and drying to obtain the stable fertilizer.
Comparative example 2
(1) In an ice-water bath, adding 35% sodium hydroxide solution into 20g of acrylic acid, stirring and neutralizing to adjust the pH to 6, adding 6g of N, N-diene propylene melamine, 1g of 2-acrylamide-2-methylpropanesulfonic acid, 3g of humic acid and 5g of carboxymethyl cellulose, uniformly stirring, adding 0.12g of potassium persulfate initiator and 0.05g of N, N-methylene bisacrylamide cross-linking agent, heating to 65 ℃, reacting for 6h, drying and crushing after the reaction is finished, thus obtaining the coating material.
(2) Sieving urea granules to obtain urea granules with the diameter of 2mm, adding 200g of urea granules into a disc granulator, spraying an epoxy resin E-44 organic binder with the mass fraction of 50% on the surfaces of the urea granules until a layer of binding liquid appears on the surfaces, adding 50g of phosphorite slow-release material which is sieved by a 0.1mm sieve, 2g of urease inhibitor hydroquinone and 4g of nitrification inhibitor dicyandiamide into the urea granules, rotating the urea granules until the slow-release material wraps the urea granules, spraying 10g of heated and melted paraffin into the urea granules to obtain coated urea, spraying an organic binder, finally spraying 4g of coating material powder into the urea granules until the coating material is fully wrapped on the surfaces of the fertilizers, and drying to obtain the stable fertilizer.
200G of soil dried by a sieve with 0.2mm is placed in a beaker, 5g of stable fertilizer and deionized water capable of saturating a soil sample are added into the beaker, the mass of the beaker is weighed every 20 hours in a baking oven at 35 ℃, and the water retention rate is calculated. A= (m-m 0´/m0-m0´) ×100%, m is the total mass of soil and fertilizer (g) at each weighing, m 0´ is the total mass of dry soil and dry fertilizer (g), and m 0 is the total mass of fertilizer and soil (g) at which sufficient water absorption reaches saturation.
As is clear from the table, the water retention effect of examples 1 to 5 is better than that of comparative examples 1 to 2 because octacarboxyl divinyl melamine is contained in examples 1 to 5, only intermediate 1 is contained in comparative example 1, only N, N-diene propylene melamine is contained in comparative example 2, tetrahydroxy is contained in comparative example 1, diamino is contained in comparative example 2, and octacarboxyl groups are contained in examples 1 to 5, and the water absorption and water retention properties of comparative examples 1 to 2 are not the same as those of examples 1 to 5 in terms of quantity or capability, so that the fertilizer prepared by the present invention has excellent water retention properties.
According to GB/T23148-2009, a still water experiment is carried out, and the slow release performance of the fertilizer is tested.
Table 1: sustained release performance test of stable fertilizer
As is clear from the table, the slow release performance of examples 1 to 5 is better than that of comparative examples 1 to 2, because when the fertilizer is applied to the soil, the coating material of the outer layer of the fertilizer granule swells by absorbing water, turns into gel, water molecules gradually permeate into the inner core, urea therein starts to dissolve, and dissolved nutrient elements start to gradually release in the soil environment through the outer layer coating in the exchange of dynamic water, providing nutrition to plants. The coating material prepared by the method has good hydrogen bond association with urea, so that the coating material can adsorb the urea, and when the content of the urea in the external environment is low, the urea can be slowly released into the environment. Whereas comparative examples 1 and 2 were only intermediate 1 and N, N-diene propylene melamine, they had less adsorption effect on urea than examples 1-5.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (5)
1. The preparation method of the stable fertilizer is characterized by comprising the following steps:
(1) Adding 30-40% sodium hydroxide solution into acrylic acid in an ice water bath, stirring and neutralizing to adjust the pH to 5-6, adding octacarboxyl divinyl melamine, 2-acrylamide-2-methylpropanesulfonic acid, humic acid and carboxymethyl cellulose into the mixture, stirring uniformly, adding an initiator and a cross-linking agent, heating to 55-70 ℃, reacting for 3-6 hours, drying and crushing after the reaction is finished to obtain a coating material;
(2) Sieving urea particles to obtain urea particles with the diameter of 1-3mm, adding the urea particles into a disc granulator, spraying organic binder with the mass fraction of 40-60% on the surfaces of the urea particles until a layer of binder solution appears on the surfaces, adding slow-release materials, urease inhibitors and nitrification inhibitors which are sieved by a sieve with the diameter of 0.1-0.4mm into the urea particles, rotating the urea particles until the slow-release materials wrap the surfaces of the urea particles, spraying heated and melted paraffin into the urea particles to obtain coated urea, spraying the organic binder, finally spraying coating material powder into the coated urea particles until the surfaces of the fertilizer are fully wrapped by the coating material, and drying to obtain stable fertilizer;
In the step (1), the mass ratio of the acrylic acid to the octacarboxyl divinyl melamine to the 2-acrylamido-2-methylpropanesulfonic acid to the humic acid to the carboxymethyl cellulose to the initiator to the cross-linking agent is 100:30-50:5-10:10-15:20-30:0.4-0.6:0.1-0.3;
in the step (2), the mass ratio of urea to slow-release material to urease inhibitor to nitrification inhibitor to paraffin to coating material is 100:20-30:1-3:0.5-2:3-6:2-10;
In the step (1), the preparation method of the octacarboxyl divinyl melamine comprises the following steps:
S1, adding N, N-diallyl melamine and paraformaldehyde into deionized water at 60-75 ℃, adding 10% sodium hydroxide solution into the deionized water to adjust the pH to 8-9, stirring and dispersing, reacting for 40-80min, decompressing and distilling after the reaction is finished, washing with deionized water, filtering and drying to obtain an intermediate 1;
S2, adding the intermediate 1 and 5-chloroisophthalic acid into deionized water, stirring and dispersing, adding triethylamine into the mixture, stirring and reacting, and after the reaction is finished, carrying out suction filtration and drying to obtain the octacarboxyl divinyl melamine.
2. The method for preparing a stable fertilizer according to claim 1, wherein in the step (2), the slow release material is one of bentonite and phosphorite.
3. The method for preparing a stable fertilizer according to claim 1, wherein in the step S1, the molar ratio of N, N-diallyl melamine to paraformaldehyde is 1:4-6.
4. The method for preparing the stable fertilizer according to claim 1, wherein in the step S2, the molar ratio of the intermediate 1, 5-chloroisophthalic acid and triethylamine is 1:4-5.2:4.5-5.5.
5. The method for preparing a stable fertilizer according to claim 1, wherein in the step S2, the stirring reaction time is 10-24 hours, and the stirring reaction temperature is 20-35 ℃.
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| CN102910991A (en) * | 2012-09-29 | 2013-02-06 | 湖北富邦科技股份有限公司 | Large-granule sustained-release ammonium chloride fertilizer, preparation method thereof and special granulating sustained-release material |
| CN104030838A (en) * | 2014-06-30 | 2014-09-10 | 成都新柯力化工科技有限公司 | Polymerized sustained-release compound fertilizer and preparation method thereof |
| WO2019153775A1 (en) * | 2018-02-09 | 2019-08-15 | 郑州高富肥料有限公司 | Sustained-release and controlled-release fertilizer having core-shell structure and preparation method therefor |
| CN110183274A (en) * | 2019-06-18 | 2019-08-30 | 吉林农业大学 | A kind of coated fertilizer and preparation method thereof with slow control-release function |
| CN110317098A (en) * | 2019-06-18 | 2019-10-11 | 苏州金螳螂园林绿化景观有限公司 | Soil organism nutrition supply technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102910991A (en) * | 2012-09-29 | 2013-02-06 | 湖北富邦科技股份有限公司 | Large-granule sustained-release ammonium chloride fertilizer, preparation method thereof and special granulating sustained-release material |
| CN104030838A (en) * | 2014-06-30 | 2014-09-10 | 成都新柯力化工科技有限公司 | Polymerized sustained-release compound fertilizer and preparation method thereof |
| WO2019153775A1 (en) * | 2018-02-09 | 2019-08-15 | 郑州高富肥料有限公司 | Sustained-release and controlled-release fertilizer having core-shell structure and preparation method therefor |
| CN110183274A (en) * | 2019-06-18 | 2019-08-30 | 吉林农业大学 | A kind of coated fertilizer and preparation method thereof with slow control-release function |
| CN110317098A (en) * | 2019-06-18 | 2019-10-11 | 苏州金螳螂园林绿化景观有限公司 | Soil organism nutrition supply technology |
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