CN113582776A - Garlic sulfur coating compound fertilizer and preparation method thereof - Google Patents
Garlic sulfur coating compound fertilizer and preparation method thereof Download PDFInfo
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- CN113582776A CN113582776A CN202110902479.8A CN202110902479A CN113582776A CN 113582776 A CN113582776 A CN 113582776A CN 202110902479 A CN202110902479 A CN 202110902479A CN 113582776 A CN113582776 A CN 113582776A
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- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05B—PHOSPHATIC FERTILISERS
- C05B17/00—Other phosphatic fertilisers, e.g. soft rock phosphates, bone meal
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- 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
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- 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
- C05G3/60—Biocides or preservatives, e.g. disinfectants, pesticides or herbicides; Pest repellants or attractants
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- 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
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- 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
- C05G5/30—Layered or coated, e.g. dust-preventing coatings
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- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention relates to a garlic sulfur coating compound fertilizer, which belongs to the technical field of fertilizer preparation and comprises the following raw materials: nitro compound fertilizer, slow release pesticide, phosphoric acid, urea, potassium magnesium phosphate fertilizer, zinc sulfate, manganese sulfate, ammonium molybdate and ferrous sulfate; heating phosphoric acid and urea at 60-70 ℃ to form urea phosphate molten slurry, adding potassium magnesium phosphate fertilizer, zinc sulfate, manganese sulfate, ammonium molybdate and ferrous sulfate, stirring and mixing, spraying into a granulator for granulation, spraying liquid sulfur on the surface of granules through a high-pressure spray head after granulation, and drying to obtain a component A; stirring and mixing the component A, the nitro-compound fertilizer and the slow-release insecticide to obtain the garlic-sulfur coated compound fertilizer, wherein the nitrogen, phosphorus and potassium nutrients are reasonably proportioned, and trace elements are added to ensure that the garlic can meet the requirements and does not cause fertilizer damage; the sulfur coating plays a role in slowly releasing nutrients, improves the utilization rate of the fertilizer compared with the common fertilizer, and plays a role in reducing weight and enhancing efficiency.
Description
Technical Field
The invention belongs to the technical field of fertilizer preparation, and particularly relates to a garlic sulfur coated compound fertilizer and a preparation method thereof.
Background
Garlic has been used as a natural bactericide since ancient times and is called "natural antibiotic". The garlic can be eaten raw, and has high nutritive value and obvious physiological effect. Can also be further processed into series of products, such as health food, cosmetics, feed additive, etc.
At present, garlic planting faces a plurality of problems, such as soil hardening, nutrient deficiency, fertilizer damage, continuous cropping, serious pest and disease damage and the like. The disease and insect pest problem is fatal, leaf blight easily occurs in garlic planting, the leaf blight mainly damages garlic leaves, the disease starts from leaf tips or other parts of the leaves, the leaves are initially in a small white circular point shape, then the irregular or elliptic gray-white or gray-brown disease spots are enlarged, black mildew-shaped substances grow on the upper parts, the diseased leaves are all withered when the disease is serious, a plurality of black granules are scattered on the disease, and the whole plant does not have bolt when the disease is serious. The main causes of the disease are that the germs are lost in the soil or overwinter on the garlic bulbs along with the disease residues by hypha or ascospore, the ascospore causes primary infection in the next year under proper conditions, and the disease part grows conidium for secondary infection. The occurrence of these problems not only affects the yield and quality of garlic, but also poses a threat to soil health. The garlic has long growth period, inconvenient later-stage additional fertilization and large labor cost in the whole growth process.
Therefore, the technical problem to be solved at present is to provide the garlic sulfur coated compound fertilizer with sterilization and weight gaining functions.
Disclosure of Invention
The invention aims to provide a garlic sulfur coating compound fertilizer and a preparation method thereof, which are used for solving the technical problems in the background technology.
The purpose of the invention can be realized by the following technical scheme:
the garlic sulfur coating compound fertilizer comprises the following raw materials in parts by weight: 20-30 parts of nitro compound fertilizer, 1-3 parts of slow-release insecticide, 5-10 parts of phosphoric acid, 2-3 parts of urea, 1 part of potassium magnesium phosphate fertilizer, 0.2 part of zinc sulfate, 0.1 part of manganese sulfate, 0.1 part of ammonium molybdate and 0.1 part of ferrous sulfate;
the garlic sulfur coating compound fertilizer is prepared by the following steps:
firstly, heating phosphoric acid and urea at 60-70 ℃ by using a melting tank to form urea phosphate molten slurry, then adding a potassium magnesium phosphate fertilizer, zinc sulfate, manganese sulfate, ammonium molybdate and ferrous sulfate, stirring at the rotation speed of 100-;
and secondly, adding the component A, the nitro-compound fertilizer and the slow-release insecticide into a stirring tank, and stirring and mixing for 30-60min under the condition that the rotating speed is 200-300r/min to obtain the garlic sulfur coated compound fertilizer.
Further, the slow release insecticide is prepared by the following steps:
step S11, adding chlorantraniliprole and DMF into a reaction kettle, adding potassium permanganate and hydrochloric acid solution with mass fraction of 17%, heating to 65-68 ℃, stirring for reaction for 4-5h, cooling to room temperature to obtain an intermediate 1, using chlorantraniliprole as a bottom material, and obtaining the intermediate 1 through oxidation of acidic potassium permanganate, wherein the dosage ratio of the chlorantraniliprole to the DMF to the potassium permanganate to the hydrochloric acid solution is 0.8-1.2 g: 25-28 mL: 0.1 g: 3-5 mL;
the reaction process is as follows:
step S12, adding 4-aminobenzaldehyde, 2- (bromomethyl) acrylic acid, THF and deionized water into a round-bottom flask, stirring for 3min, adding indium powder, magnetically stirring, tracking by TLC, adding a hydrochloric acid solution, stirring for 3-6h after the aldehyde raw material point disappears, extracting with ethyl acetate, drying with anhydrous sodium sulfate, filtering, decompressing and steaming to obtain an intermediate 2, and obtaining an intermediate 2 by using 4-aminobenzaldehyde and 2- (bromomethyl) acrylic acid as substrates through reduction reaction and condensation reaction, wherein the dosage ratio of the 4-aminobenzaldehyde, the 2- (bromomethyl) acrylic acid, the THF, the deionized water, the indium powder and the hydrochloric acid solution is 1 mmol: 1.0-1.2 mmol: 5mL of: 5-8 mL: 1.1 mmol: 2-4mL, wherein the concentration of the hydrochloric acid solution is 6 mol/L;
the reaction process is as follows:
s13, taking the intermediate 1, triethylamine and tetrahydrofuran, magnetically stirring in a three-neck flask, adding the intermediate 2 at 0 ℃, then adding 4-dimethylaminopyridine, adding N, N' -dicyclohexylcarbodiimide after reaction liquid is clarified, heating to 25 ℃, reacting for 3 hours, concentrating the reaction liquid under reduced pressure to 1/3 of volume, then adding ethyl acetate for extraction, and removing ethyl acetate through reduced pressure distillation of extract liquid to obtain an intermediate 3; taking the intermediate 1 and the intermediate 2 as raw materials, and carrying out an amide reaction to obtain an intermediate 3, wherein the dosage ratio of the intermediate 1, triethylamine, tetrahydrofuran, the intermediate 2, 4-dimethylaminopyridine and N, N' -dicyclohexylcarbodiimide is 50 mmol: 3.2-3.8 mL: 38-41 mL: 50 mmol: 0.2-0.3 g: 0.3-0.5 g;
the reaction process is as follows:
step S14, adding bentonite and water into a reactor, ultrasonically dispersing for 20-25min at the frequency of 30-50kHz to obtain a suspension, then adding octadecyl trimethyl ammonium chloride, stirring for 4h at the rotating speed of 150r/min under the condition of a water bath at the temperature of 60 ℃, centrifuging for 15min at the rotating speed of 3000r/min, washing precipitates with deionized water until no precipitate is generated by detection of a silver nitrate solution, and finally drying to constant weight at the temperature of 65 ℃ to obtain modified bentonite, wherein the dosage ratio of the bentonite, the water and the octadecyl trimethyl ammonium chloride is 1 g: 50mL of: 0.28-0.35 g;
step S15, stirring and mixing the intermediate 3 and methanol to obtain a solution a, adding modified bentonite and water into a round-bottom flask, performing ultrasonic dispersion at the frequency of 48kHz for 15-20min, dropwise adding the solution a into the round-bottom flask, after dropwise adding, stirring and reacting at the room temperature at the rotation speed of 200-300r/min for 4-6h, after reaction, performing vacuum filtration, washing a filter cake with deionized water for 3-5 times, and finally drying in a 65 ℃ oven to constant weight to obtain the slow-release insecticide, wherein the dosage ratio of the intermediate 3 to the methanol is 1 g: 8.5-9.6mL, and the dosage ratio of the solution a, the modified bentonite and the water is 3.7-4.5 mL: 2 g: 18-22 mL.
The invention has the beneficial effects that:
the invention uses nitro compound fertilizer, slow release pesticide, phosphoric acid, urea and phosphoric acidThe garlic-sulfur coated compound fertilizer is prepared by taking potash magnesium fertilizer, zinc sulfate, manganese sulfate, ammonium molybdate and ferrous sulfate as raw materials, wherein the nitrogen, phosphorus and potassium nutrients are reasonably proportioned, and trace elements are added to ensure that the garlic can meet the requirements and does not cause fertilizer damage; the sulfur coating plays a role in slowly releasing nutrients, improves the utilization rate of the fertilizer compared with the common fertilizer, and plays a role in reducing weight and enhancing efficiency; the nitro compound fertilizer contains 'dinitrogen' (nitrate nitrogen and ammonium nitrogen), can be directly absorbed by garlic without secondary conversion, the ammonium nitrogen in the nitro compound fertilizer can be stored by soil, the fertilizer supply time is prolonged, the subsequent growth nutrition of the garlic is sufficient, the trace element zinc can improve the stress resistance and participate in the photosynthesis, the yield of the garlic is improved, the molybdenum element can participate in the photosynthesis, the respiration and the synthesis process of organic phosphorus-containing compounds of plants, the fertilizer has stronger nitrogen fixation, the fertilizer is supplemented into the nutrition requirement of the garlic, the growth quality of the garlic can be effectively improved, the compound fertilizer can also play a role in preventing soil insects, alleviating plant diseases and insect pests and reducing the pesticide investment, the chlorine insect benzamide is firstly used as a base material, the methyl on the benzene ring is oxidized into carboxyl through the oxidation of acid potassium permanganate, obtaining an intermediate 1, further synthesizing an intermediate 2 containing terminal amino and a cyclic lactone structure by taking 4-aminobenzaldehyde and 2- (bromomethyl) acrylic acid as raw materials, further carrying out an amide reaction between the intermediate 1 and the intermediate 2 to obtain an intermediate 3, introducing octadecyl trimethyl ammonium chloride into interlayer of montmorillonite to prepare organic bentonite by utilizing the exchange capacity of the bentonite and external inorganic or organic cations, entering the volume effect of quaternary ammonium salt ions between wafer layers, increasing the interlayer spacing of the wafer, effectively improving the interlayer microenvironment of the montmorillonite, improving the hydrophobicity and the adsorbability of organic matters, and loading the intermediate 3 by utilizing the modified bentonite to obtain the slow-release insecticide, wherein chlorantraniliprole can be combined with ryanodyne receptors of insects to induce the insects to release Ca stored in cells2 +The intermediate 3 has an unsaturated C ═ C double bond outside the cyclic lactone structure and can be used as an electrophilic group and a member of an active enzyme in a living bodyThe essential groups have Michael addition reaction, so that the structures of the active parts are changed, the activity is lost, and the antibacterial effect is exerted, therefore, the slow-release pesticide not only has the insecticidal effect, but also has the antibacterial effect, and the safety of the garlic growth environment can be effectively ensured by adding the slow-release pesticide into the compound fertilizer, and the quality and the yield of the garlic are further improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The slow release insecticide is prepared by the following steps:
step S11, adding 0.8g of chlorantraniliprole and 25mL of DMF (dimethyl formamide) into a reaction kettle, adding 0.1g of potassium permanganate and 3mL of hydrochloric acid solution with the mass fraction of 17%, heating to 65 ℃, stirring for reaction for 4 hours, and cooling to room temperature to obtain an intermediate 1;
step S12, adding 1mmol of 4-aminobenzaldehyde, 1.0mmol of 2- (bromomethyl) acrylic acid, 5mL of THF and 5mL of deionized water into a round-bottom flask, stirring for 3min, adding 1.1mmol of indium powder, magnetically stirring, tracking by TLC, adding 2mL of hydrochloric acid solution with the concentration of 6mol/L, stirring for 3h after the aldehyde raw material point disappears, extracting with ethyl acetate, drying with anhydrous sodium sulfate, filtering, and performing reduced pressure rotary evaporation to obtain an intermediate 2;
step S13, taking 50mmol of intermediate 1, 3.2mL of triethylamine and 38mL of tetrahydrofuran, magnetically stirring in a three-neck flask, adding 50mmol of intermediate 2 at 0 ℃, then adding 0.2g of 4-dimethylaminopyridine, adding 0.2g of N, N' -dicyclohexylcarbodiimide after reaction liquid is clarified, heating to 25 ℃, reacting for 3 hours, concentrating the reaction liquid under reduced pressure to 1/3 of volume, then adding ethyl acetate for extraction, and removing ethyl acetate by distilling extract liquid under reduced pressure to obtain an intermediate 3;
step S14, adding 1g of bentonite and 50mL of water into a reactor, performing ultrasonic dispersion for 20min at the frequency of 30kHz to obtain a suspension, then adding 0.28g of octadecyl trimethyl ammonium chloride, stirring for 4h at the rotating speed of 150r/min under the water bath condition of 60 ℃, then centrifuging for 15min at the rotating speed of 3000r/min, washing the precipitate with deionized water until no precipitate is generated by detection of a silver nitrate solution, and finally drying at the temperature of 65 ℃ to constant weight to obtain modified bentonite;
step S15, stirring and mixing 1g of intermediate 3 and 8.5mL of methanol to obtain a solution a, adding 2g of modified bentonite and 18mL of water into a round-bottom flask, performing ultrasonic dispersion at the frequency of 48kHz for 15min, dropwise adding 3.7mL of the solution a into the round-bottom flask, stirring and reacting at the rotating speed of 200r/min for 4h at room temperature after dropwise adding, performing vacuum filtration after reaction, washing a filter cake with deionized water for 3 times, and finally drying in a 65 ℃ oven to constant weight to obtain the slow-release pesticide.
Example 2
The slow release insecticide is prepared by the following steps:
step S11, adding 1.0g of chlorantraniliprole and 26mL of DMF (dimethyl formamide) into a reaction kettle, adding 0.1g of potassium permanganate and 4mL of hydrochloric acid solution with the mass fraction of 17%, heating to 67 ℃, stirring for reacting for 4.5h, and cooling to room temperature to obtain an intermediate 1;
step S12, adding 1mmol of 4-aminobenzaldehyde, 1.1mmol of 2- (bromomethyl) acrylic acid, 5mL of THF and 7mL of deionized water into a round-bottom flask, stirring for 3min, adding 1.1mmol of indium powder, magnetically stirring, tracking by TLC, adding 3mL of hydrochloric acid solution with the concentration of 6mol/L, stirring for 4h, extracting with ethyl acetate, drying with anhydrous sodium sulfate, filtering, and performing reduced pressure rotary evaporation to obtain an intermediate 2;
step S13, taking 50mmol of intermediate 1, 3.5mL of triethylamine and 40mL of tetrahydrofuran, magnetically stirring in a three-neck flask, adding 50mmol of intermediate 2 at 0 ℃, then adding 0.25g of 4-dimethylaminopyridine, adding 0.25g of N, N' -dicyclohexylcarbodiimide after reaction liquid is clarified, heating to 25 ℃, reacting for 3 hours, concentrating the reaction liquid under reduced pressure to 1/3 of volume, then adding ethyl acetate for extraction, and removing ethyl acetate by distilling extract liquid under reduced pressure to obtain an intermediate 3;
step S14, adding 1g of bentonite and 50mL of water into a reactor, performing ultrasonic dispersion for 23min at the frequency of 40kHz to obtain a suspension, then adding 0.30g of octadecyl trimethyl ammonium chloride, stirring for 4h at the rotation speed of 150r/min under the water bath condition of 60 ℃, then centrifuging for 15min at the rotation speed of 3000r/min, washing the precipitate with deionized water until no precipitate is generated by detection of a silver nitrate solution, and finally drying at the temperature of 65 ℃ to constant weight to obtain modified bentonite;
step S15, stirring and mixing 1g of intermediate 3 and 8.8mL of methanol to obtain a solution a, adding 2g of modified bentonite and 20mL of water into a round-bottom flask, performing ultrasonic dispersion at the frequency of 48kHz for 18min, dropwise adding 4.0mL of the solution a into the round-bottom flask, stirring and reacting at the rotating speed of 250r/min for 5h at room temperature after dropwise adding, performing vacuum filtration after reaction, washing a filter cake with deionized water for 4 times, and finally drying in a 65 ℃ oven to constant weight to obtain the slow-release pesticide.
Example 3
The slow release insecticide is prepared by the following steps:
step S11, adding 1.2g of chlorantraniliprole and 28mL of DMF (dimethyl formamide) into a reaction kettle, adding 0.1g of potassium permanganate and 5mL of hydrochloric acid solution with the mass fraction of 17%, heating to 68 ℃, stirring for reaction for 5 hours, and cooling to room temperature to obtain an intermediate 1;
step S12, adding 1mmol of 4-aminobenzaldehyde, 1.2mmol of 2- (bromomethyl) acrylic acid, 5mL of THF and 8mL of deionized water into a round-bottom flask, stirring for 3min, adding 1.1mmol of indium powder, magnetically stirring, tracking by TLC, adding 4mL of hydrochloric acid solution with the concentration of 6mol/L, stirring for 6h, extracting with ethyl acetate, drying with anhydrous sodium sulfate, filtering, and performing reduced pressure rotary evaporation to obtain an intermediate 2;
step S13, taking 50mmol of intermediate 1, 3.8mL of triethylamine and 41mL of tetrahydrofuran, magnetically stirring in a three-neck flask, adding 50mmol of intermediate 2 at 0 ℃, then adding 0.3g of 4-dimethylaminopyridine, adding 0.3g of N, N' -dicyclohexylcarbodiimide after reaction liquid is clarified, heating to 25 ℃, reacting for 3 hours, concentrating the reaction liquid under reduced pressure to 1/3 of volume, then adding ethyl acetate for extraction, and removing ethyl acetate by distilling extract liquid under reduced pressure to obtain an intermediate 3;
step S14, adding 1g of bentonite and 50mL of water into a reactor, performing ultrasonic dispersion for 25min at the frequency of 50kHz to obtain a suspension, then adding 0.35g of octadecyl trimethyl ammonium chloride, stirring for 4h at the rotation speed of 150r/min under the water bath condition of 60 ℃, then centrifuging for 15min at the rotation speed of 3000r/min, washing the precipitate with deionized water until no precipitate is generated by detection of a silver nitrate solution, and finally drying at the temperature of 65 ℃ to constant weight to obtain modified bentonite;
step S15, stirring and mixing 1g of intermediate 3 and 9.6mL of methanol to obtain a solution a, adding 2g of modified bentonite and 22mL of water into a round-bottom flask, performing ultrasonic dispersion at the frequency of 48kHz for 20min, dropwise adding 4.5mL of the solution a into the round-bottom flask, stirring and reacting at the rotating speed of 300r/min for 6h at room temperature after dropwise adding, performing vacuum filtration after the reaction is finished, washing a filter cake with deionized water for 5 times, and finally drying in a 65 ℃ oven to constant weight to obtain the slow-release pesticide.
Comparative example 1
Step S11, adding 1g of bentonite and 50mL of water into a reactor, performing ultrasonic dispersion for 25min at the frequency of 50kHz to obtain a suspension, then adding 0.35g of octadecyl trimethyl ammonium chloride, stirring for 4h at the rotation speed of 150r/min under the water bath condition of 60 ℃, then centrifuging for 15min at the rotation speed of 3000r/min, washing the precipitate with deionized water until no precipitate is generated by detection of a silver nitrate solution, and finally drying at the temperature of 65 ℃ to constant weight to obtain modified bentonite;
step S12, stirring and mixing 1g of chlorantraniliprole and 9.6mL of methanol to obtain a solution a, adding 2g of modified bentonite and 22mL of water into a round-bottom flask, performing ultrasonic dispersion at the frequency of 48kHz for 20min, dropwise adding 4.5mL of the solution a into the round-bottom flask, stirring and reacting at the rotating speed of 300r/min for 6h at room temperature after dropwise adding, performing vacuum filtration after the reaction is finished, washing a filter cake for 5 times by using deionized water, and finally drying in a 65 ℃ oven to constant weight to obtain the slow-release pesticide.
Example 4
The garlic sulfur coating compound fertilizer comprises the following raw materials in parts by weight: 20 parts of nitro compound fertilizer, 1 part of slow-release insecticide of example 1, 5 parts of phosphoric acid, 2 parts of urea, 1 part of potassium magnesium phosphate fertilizer, 0.2 part of zinc sulfate, 0.1 part of manganese sulfate, 0.1 part of ammonium molybdate and 0.1 part of ferrous sulfate;
the garlic sulfur coating compound fertilizer is prepared by the following steps:
firstly, heating phosphoric acid and urea at 60 ℃ by using a melting tank to form urea phosphate molten slurry, then adding a potassium magnesium phosphate fertilizer, zinc sulfate, manganese sulfate, ammonium molybdate and ferrous sulfate, stirring for 20min at a rotating speed of 100r/min to obtain suspension molten slurry, quickly spraying the suspension molten slurry into a granulator for granulation, spraying liquid sulfur on the surfaces of granules through a high-pressure spray nozzle after granulation is formed, and drying at room temperature to obtain a component A;
and secondly, adding the component A, the nitro compound fertilizer and the slow-release insecticide into a stirring tank, and stirring and mixing for 30min under the condition of the rotating speed of 200r/min to obtain the garlic sulfur coated compound fertilizer.
Example 5
The garlic sulfur coating compound fertilizer comprises the following raw materials in parts by weight: 25 parts of nitro compound fertilizer, 2 parts of slow-release insecticide of example 2, 8 parts of phosphoric acid, 2.5 parts of urea, 1 part of potassium magnesium phosphate fertilizer, 0.2 part of zinc sulfate, 0.1 part of manganese sulfate, 0.1 part of ammonium molybdate and 0.1 part of ferrous sulfate;
the garlic sulfur coating compound fertilizer is prepared by the following steps:
firstly, heating phosphoric acid and urea at 65 ℃ by using a melting tank to form urea phosphate molten slurry, then adding a potassium magnesium phosphate fertilizer, zinc sulfate, manganese sulfate, ammonium molybdate and ferrous sulfate, stirring for 30min at a rotation speed of 150r/min to obtain suspension molten slurry, quickly spraying the suspension molten slurry into a granulator for granulation, spraying liquid sulfur on the surfaces of granules through a high-pressure spray nozzle after granulation is formed, and drying at room temperature to obtain a component A;
and secondly, adding the component A, the nitro compound fertilizer and the slow-release insecticide into a stirring tank, and stirring and mixing for 40min under the condition of the rotating speed of 250r/min to obtain the garlic sulfur coated compound fertilizer.
Example 6
The garlic sulfur coating compound fertilizer comprises the following raw materials in parts by weight: 30 parts of nitro compound fertilizer, 3 parts of slow-release insecticide of example 3, 10 parts of phosphoric acid, 3 parts of urea, 1 part of potassium magnesium phosphate fertilizer, 0.2 part of zinc sulfate, 0.1 part of manganese sulfate, 0.1 part of ammonium molybdate and 0.1 part of ferrous sulfate;
the garlic sulfur coating compound fertilizer is prepared by the following steps:
firstly, heating phosphoric acid and urea at 70 ℃ by using a melting tank to form urea phosphate molten slurry, then adding a potassium magnesium phosphate fertilizer, zinc sulfate, manganese sulfate, ammonium molybdate and ferrous sulfate, stirring for 40min at a rotation speed of 200r/min to obtain suspension molten slurry, quickly spraying the suspension molten slurry into a granulator for granulation, spraying liquid sulfur on the surfaces of granules through a high-pressure spray nozzle after granulation is formed, and drying at room temperature to obtain a component A;
and secondly, adding the component A, the nitro compound fertilizer and the slow-release insecticide into a stirring tank, and stirring and mixing for 60min under the condition of the rotating speed of 300r/min to obtain the garlic sulfur coated compound fertilizer.
Comparative example 2
The slow-release insecticide in the embodiment 4 is replaced by the slow-release insecticide in the proportion 1, and the rest of raw materials and the preparation process are unchanged.
Comparative example 3
The nitro compound fertilizer in example 5 was removed, and the remaining raw materials and preparation process were unchanged.
Comparative example 4
The slow release insecticide of example 6 was removed and the remaining raw materials and preparation process were unchanged.
Comparative example 5
The comparative example is a compound fertilizer special for garlic sold by Zhengzhou Epida agricultural science and technology limited.
The compound fertilizers of examples 4-6 and comparative examples 2-5 were subjected to performance tests, which were as follows:
selecting a variety Jinxiang white-skin garlic, applying 120 kilograms of compound fertilizer to each mu of garlic, scattering the fertilizer on the surface of soil at one time, combining soil preparation, turning over and burying soil, uniformly mixing the soil and the fertilizer, then sowing garlic seeds, sowing the garlic seeds 4cm below the soil, and applying fertilizer once without topdressing.
Blank group: applying 120 kg of potassium sulfate ternary compound fertilizer per mu, applying basal application before sowing, long leaf flourishing period and bulb expanding period according to the proportion of 5: 2: three administrations were carried out at 3 min.
Other management conditions are consistent.
The application results of the compound fertilizers of examples 4 to 6 and comparative examples 2 to 5 are shown in the following table:
| item | Average garlic circumference/cm | Average yield per kg per mu | Efficiency of increase in production% |
| Example 4 | 27 | 1149 | 14.9 |
| Example 5 | 28 | 1156 | 15.6 |
| Example 6 | 27 | 1141 | 14.1 |
| Comparative example 2 | 20 | 1105 | 10.5 |
| Comparative example 3 | 21 | 1021 | 2.1 |
| Comparative example 4 | 17 | 1089 | 8.9 |
| Comparative example 5 | 19 | 1112 | 11.2 |
| Blank group | 15 | 1000 | 0 |
As can be seen from the above table, the compound fertilizers of examples 4-6 are superior to comparative examples 2-5 in the garlic bulb growth and garlic acre yield increase test processes, and the compound fertilizers prepared by the invention can effectively promote the garlic growth and increase the garlic yield.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. The garlic sulfur coating compound fertilizer is characterized by comprising the following raw materials in parts by weight: 20-30 parts of nitro compound fertilizer, 1-3 parts of slow-release insecticide, 5-10 parts of phosphoric acid, 2-3 parts of urea, 1 part of potassium magnesium phosphate fertilizer, 0.2 part of zinc sulfate, 0.1 part of manganese sulfate, 0.1 part of ammonium molybdate and 0.1 part of ferrous sulfate;
the slow-release insecticide is prepared by the following steps:
step S11, adding chlorantraniliprole and DMF into a reaction kettle, adding potassium permanganate and hydrochloric acid solution, heating to 65-68 ℃, stirring for reaction for 4-5h, and cooling to room temperature to obtain an intermediate 1;
step S12, adding 4-aminobenzaldehyde, 2- (bromomethyl) acrylic acid, THF and deionized water into a round-bottom flask, stirring for 3min, adding indium powder, magnetically stirring, tracking by TLC, adding a hydrochloric acid solution, stirring for 3-6h after the aldehyde raw material point disappears, extracting, drying, filtering, and carrying out reduced pressure rotary evaporation to obtain an intermediate 2;
step S13, taking the intermediate 1, triethylamine and tetrahydrofuran, magnetically stirring in a three-neck flask, adding the intermediate 2 at 0 ℃, then adding 4-dimethylaminopyridine, adding N, N' -dicyclohexylcarbodiimide after reaction liquid is clarified, heating to 25 ℃, reacting for 3 hours, concentrating the reaction liquid under reduced pressure, extracting, and distilling extract liquid under reduced pressure to obtain an intermediate 3;
step S14, adding bentonite and water into a reactor, performing ultrasonic dispersion for 20-25min to obtain a suspension, adding octadecyl trimethyl ammonium chloride, stirring for 4h under the water bath condition of 60 ℃, centrifuging for 15min, precipitating, washing and drying to obtain modified bentonite;
and step S15, stirring and mixing the intermediate 3 and methanol to obtain a solution a, adding the modified bentonite and water into a round-bottom flask, ultrasonically dispersing for 15-20min, dropwise adding the solution a, stirring and reacting for 4-6h at room temperature, carrying out vacuum filtration, washing a filter cake, and drying to obtain the slow-release pesticide.
2. The garlic sulfur-coated compound fertilizer as claimed in claim 1, wherein the dosage ratio of chlorantraniliprole, DMF, potassium permanganate and hydrochloric acid solution in step S11 is 0.8-1.2 g: 25-28 mL: 0.1 g: 3-5 mL.
3. The garlic sulfur-coated compound fertilizer as claimed in claim 1, wherein the amount ratio of 4-aminobenzaldehyde, 2- (bromomethyl) acrylic acid, THF, deionized water, indium powder and hydrochloric acid solution in step S12 is 1 mmol: 1.0-1.2 mmol: 5mL of: 5-8 mL: 1.1 mmol: 2-4mL, and the concentration of the hydrochloric acid solution is 6 mol/L.
4. The garlic sulfur-coated compound fertilizer as claimed in claim 1, wherein the ratio of the amount of intermediate 1, triethylamine, tetrahydrofuran, intermediate 2, 4-dimethylaminopyridine and N, N' -dicyclohexylcarbodiimide used in step S13 is 50 mmol: 3.2-3.8 mL: 38-41 mL: 50 mmol: 0.2-0.3 g: 0.3-0.5 g.
5. The garlic sulfur-coated compound fertilizer as claimed in claim 1, wherein the ratio of the bentonite to the water to the octadecyl trimethyl ammonium chloride in the step S14 is 1 g: 50mL of: 0.28-0.35 g.
6. The garlic sulfur-coated compound fertilizer as claimed in claim 1, wherein the ratio of the amount of the intermediate 3 to the amount of methanol in step S15 is 1 g: 8.5-9.6mL, and the dosage ratio of the solution a, the modified bentonite and the water is 3.7-4.5 mL: 2 g: 18-22 mL.
7. The preparation method of the garlic sulfur coating compound fertilizer as claimed in claim 1, characterized by comprising the following steps:
heating phosphoric acid and urea at 60-70 ℃ to form urea phosphate molten slurry, adding a potassium magnesium phosphate fertilizer, zinc sulfate, manganese sulfate, ammonium molybdate and ferrous sulfate, stirring for 20-40min to obtain suspension molten slurry, granulating the suspension molten slurry, spraying liquid sulfur on the surfaces of granules after granulation, and drying at room temperature to obtain a component A;
and secondly, adding the component A, the nitro compound fertilizer and the slow-release insecticide into a stirring tank, and stirring and mixing for 30-60min to obtain the garlic sulfur coated compound fertilizer.
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