CN115553292A - Environment-friendly processing method of agricultural herbicide - Google Patents
Environment-friendly processing method of agricultural herbicide Download PDFInfo
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- CN115553292A CN115553292A CN202211298644.4A CN202211298644A CN115553292A CN 115553292 A CN115553292 A CN 115553292A CN 202211298644 A CN202211298644 A CN 202211298644A CN 115553292 A CN115553292 A CN 115553292A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
- A01N33/18—Nitro compounds
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P13/00—Herbicides; Algicides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/04—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C08G12/10—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with acyclic compounds having the moiety X=C(—N<)2 in which X is O, S or —N
- C08G12/12—Ureas; Thioureas
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- 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
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Abstract
The invention discloses an environment-friendly processing method of an agricultural herbicide, relates to the field of agriculture, and is used for solving the problems of improving the effective utilization rate of pesticides, reducing toxicity, reducing environmental pollution and the like; mixing distilled water, sodium hydroxide, urea and the intermediate 2 for reaction to obtain a capsule wall material; dissolving a herbicide trifluralin in benzene, adding a defoaming agent, a capsule wall material, an emulsifier, a dispersant, sodium chloride and hydrochloric acid, stirring, heating to solidify a capsule wall, adding sodium hydroxide and ice water, filtering, adding an antifreezing agent, a wetting dispersant and a thickener, and drying to form a micro-capsule preparation to obtain the agricultural herbicide; the environment-friendly processing method of the agricultural herbicide has the excellent characteristics of improving the effective utilization rate of the pesticide, avoiding the easy decomposition and loss of the herbicide, reducing the toxic phytotoxicity, reducing the environmental pollution and the like; the purposes of environmental protection, reduction of pesticide volatilization, frequency and prolongation of the effective period of the pesticide are achieved.
Description
Technical Field
The invention relates to the field of agriculture, in particular to an environment-friendly processing method of an agricultural herbicide.
Background
With the development of economy and science, the problem of environmental pollution is increasingly aggravated, wherein improper use of pesticides becomes one of the main causes of environmental pollution; the pesticide is an important means for crop yield conservation, and due to the fact that the pesticide is used in a large amount and is not applied scientifically and reasonably, the problems that input cost of farmers is increased, pesticide residues exceed standards, crops are prone to phytotoxicity and large pollution to the environment occur, harm to health of a pesticide applicator and phytotoxicity to the crops are caused during pesticide application, active ingredients of the pesticide can be directly exposed in air, rainwater and soil after the pesticide is applied, the pesticide is prone to volatilization and decomposition, and meanwhile harm is caused to beneficial organisms; the environment is seriously polluted due to the large amount of pesticides used and the improper pesticide application method, and the cost of farmers is increased, wherein the environment-friendly and lasting pesticide becomes a key research object.
The existing pesticide formulations, such as powder, aqueous emulsion, suspending agent and the like, have short lasting period, can weed only by increasing the application amount and the application frequency, and have a plurality of defects, such as the water aqua of the herbicide is easy to volatilize and causes pollution and toxicity to rivers and other organisms; the short duration increases the application frequency and the application amount, increases the toxicity risk to the applicator, and increases the pesticide residue in the soil; the formulations such as emulsion in water suspending agent are easy to mix unevenly, and are easy to delaminate and precipitate after long storage time; when the herbicide is sprayed, the herbicide is difficult to control, is not uniformly distributed, and influences the concentration of the herbicide on the surface of weeds, so an environment-friendly processing method of the agricultural herbicide is needed to solve the problems.
Disclosure of Invention
In order to overcome the problems of the background art, the invention aims to provide an environment-friendly processing method of an agricultural herbicide, which comprises the following steps: mixing distilled water, urea and the intermediate 2, adding sodium hydroxide to adjust the pH value to 8.3-8.5, and stirring and reacting at 68-75 ℃ to obtain a capsule wall material; dissolving herbicide trifluralin in benzene, adding a defoaming agent, stirring for 20-30min, adding a capsule wall material, then adding an emulsifier and a dispersant, stirring, and adding hydrochloric acid to adjust the pH value to 1.9-2.8; reacting for 3.5-4.5h, gradually reducing the rotating speed to 170-200r/min, adding sodium chloride, gradually heating to 65 ℃ to solidify the capsule wall, reacting for 1-2h, adding sodium hydroxide to adjust the pH value to be neutral, then adding ice water, filtering, adding an antifreezing agent, a wetting dispersant and a thickening agent, and drying to form a microcapsule preparation to obtain the agricultural herbicide; the microcapsule herbicide solves the problems of environmental pollution and harm to the health of a pesticide applicator of the existing agricultural herbicide.
The purpose of the invention can be realized by the following technical scheme:
a chemical processing method of an agricultural environment-friendly herbicide comprises the following steps:
a1: adding hydrobromic acid and 2-amino-4-methylpyridine into a four-neck flask, stirring, cooling to-16-13 ℃ after the 2-amino-4-methylpyridine is completely dissolved, dropwise adding liquid bromine, controlling the dropwise adding rate to be 0.5-1mL/min, and controlling the temperature in the dropwise adding process to be-15 to-10 ℃; stirring for 90-120min after the dropwise addition is finished, dropwise adding a sodium nitrite solution, stirring for 25-35min, heating to 10-15 ℃, stirring for 40-50min, cooling to-20 to-15 ℃, dropwise adding a sodium hydroxide solution, and controlling the temperature to be lower than-15 to-10 ℃ in the dropwise adding process; heating to 18-20 deg.C, stirring for 50-60min, extracting with toluene, mixing organic phases, washing with water, drying, and concentrating to obtain intermediate 1;
the reaction process is as follows:
a2: adding the intermediate 1, N-bromosuccinimide and benzoyl peroxide into a four-neck flask, taking petroleum ether as a solvent, stirring and dissolving, heating to 60-70 ℃, keeping the temperature for 24-30h, after the reaction is finished, filtering, heating and refluxing the crude product and a saturated sodium bicarbonate solution for 2-2.5h, cooling, adding the reaction product into an ice hydrochloric acid aqueous solution while stirring, standing and layering, extracting an upper layer of liquid with diethyl ether, combining an extraction liquid and a lower layer of liquid, washing with distilled water for 1-2 times, washing with a hydrochloric acid solution for 2-3 times and with a sodium hydroxide solution for 3-5 times, washing with distilled water to be neutral, drying with anhydrous magnesium sulfate, standing for 22-24h, performing vacuum filtration, performing rotary evaporation on a filtrate to remove the solvent and the extraction liquid, and refluxing the evaporation product with anhydrous ethanol for 4-6 times to obtain an intermediate 2;
the reaction process is as follows:
a3: mixing distilled water, urea and the intermediate 2, reacting for 1h, adding sodium hydroxide to adjust the pH value to 8.3, reacting for 1-1.5h at the stirring speed of 100-150r/min at the temperature of 68-75 ℃, and after the reaction is finished, performing rotary evaporation on a reaction product to remove the solvent and cooling to 23-25 ℃ to obtain a capsule wall material;
the reaction process is as follows:
a4: dissolving the original drug of the herbicide trifluralin in benzene, adding a defoaming agent, stirring for 20-30min at 45-50 ℃ and the rotating speed of 700-900r/min, adding the capsule wall material after the mixture is uniform, adding an emulsifying agent and a dispersing agent, and stirring for 20-30min at the rotating speed of 1200-1500r/min to form stable emulsion; then reducing the rotating speed to 700-800r/min, and adding hydrochloric acid in batches in 60min to adjust the pH value of the system to 1.9-2.8; reacting for 3.5-4.5h, gradually reducing the rotating speed to 170-200r/min, adding sodium chloride, gradually heating to 65 ℃ to solidify the capsule wall, adding sodium hydroxide to adjust the pH value to be neutral after the reaction is finished, then adding ice water, filtering, adding an antifreezing agent, a wetting dispersant and a thickening agent, and drying to form a microcapsule preparation to obtain the agricultural herbicide.
As a further scheme of the invention: the dosage ratio of the 2-amino-4-methylpyridine to the liquid bromine in the step A1 is 0.1mol:0.25-0.3mol, wherein the mass fraction of the sodium hydroxide solution is 10%, the mass fraction of the hydrobromic acid is 48%, and the mass fraction of the sodium nitrite solution is 8%.
As a further scheme of the invention: the dosage ratio of the intermediate 1, the N-bromosuccinimide, the benzoyl peroxide, the diethyl ether and the petroleum ether in the step A2 is 0.1mol:0.25-0.3mol:0.02-0.05mol:200mL of: 150mL, wherein the mass fraction of the ice hydrochloric acid aqueous solution is 5-10%, and the mass fraction of the sodium hydroxide solution is 10%.
As a further scheme of the invention: the dosage ratio of the distilled water, the urea and the intermediate 2 in the step A3 is 100-120mL:0.1mol:30-35g.
As a further scheme of the invention: the defoaming agent in the step A4 is a silicon polyether defoaming agent DF-2692, and the mass fraction is 0.1-0.3%; the emulsifier is styrene-maleic anhydride copolymerized sodium salt, and the using amount of the emulsifier is 1.5-2.5g; the dispersant is sodium polyacrylate with the mass fraction of 1.5-2%; the benzene amount is 6% of the total amount of the microcapsule preparation; the mass fraction of the hydrochloric acid is 2 percent, and the mass fraction of the sodium chloride is 0.3-0.4 percent; the antifreezing agent is glycol, and the dosage of the antifreezing agent is 3 percent of the total amount of the microcapsule preparation; the dispersant is sodium polyacrylate, and the dosage of the dispersant is 1.5-2% of the total amount of the microcapsule preparation; the thickening agent is xanthan gum and aluminum magnesium silicate, and the amount of the thickening agent is 0.15% of the total amount of the microcapsule preparation.
The invention has the beneficial effects that:
according to the environment-friendly processing method of the herbicide, distilled water, sodium hydroxide, urea and an intermediate 2 are mixed and reacted to obtain a capsule wall material; dissolving the herbicide trifluralin in benzene, adding a defoaming agent, a capsule wall material, an emulsifier, a dispersant and hydrochloric acid, stirring, then adding sodium chloride, heating to solidify the capsule wall, adding sodium hydroxide and ice water, filtering, adding an antifreezing agent, a wetting dispersant and a thickening agent, and drying to form a microcapsule preparation, thereby obtaining the agricultural herbicide. The microcapsule preparation improves the effective utilization rate of the herbicide, and avoids easy decomposition and easy loss of the herbicide; the toxicity and the phytotoxicity of the herbicide are reduced, and the herbicide has the excellent characteristics of reducing environmental pollution and the like; the purposes of environmental protection, reduction of the volatilization and use frequency of the pesticide and prolongation of the lasting period of the pesticide are achieved.
Preparing a capsule wall material in the environment-friendly processing process of a herbicide, and carrying out substitution reaction on amino of 2-amino-4-methylpyridine and bromine atoms in liquid bromine under the alkaline condition of 2-mercaptopyridine and bromoethanol to obtain an intermediate 1; adding 2-amino-4-methylpyridine, N-bromosuccinimide and benzoyl peroxide into a four-neck flask, stirring, taking petroleum ether as a solvent, filtering after the reaction is finished, refluxing, cooling, extracting with diethyl ether, washing, drying, standing, then carrying out vacuum filtration, carrying out rotary evaporation on the filtrate to remove the solvent and extract liquor, and refluxing to obtain an intermediate 2; mixing distilled water, urea and the intermediate 2, reacting for 1-2h, adding sodium hydroxide, stirring and reacting for 1-1.5h, after the reaction is finished, rotationally evaporating a reaction product to remove a solvent to obtain a capsule wall material, wherein the capsule wall material is semitransparent, weak acid and weak base resistant, good in insulating property, excellent in wear resistance, low in cost, good in compactness, high in core material content, high in heat stability temperature and good in mechanical property, and simultaneously adding styrene-maleic anhydride sodium copolymer and sodium polyacrylate as an emulsifier and a dispersant to adjust the particle size of the microcapsule and the viscosity of a system, so that the particle size distribution is more uniform; the added sodium chloride increases the drug loading capacity of the microcapsule, improves the appearance of the surface of the microcapsule, makes the surface of the microcapsule smoother and tighter, increases the ionic strength in the solution and plays a role of a stabilizer; the microcapsule preparation solves the problems of agglomeration, adhesion, rough and unstable surface, low yield and the like of common microcapsules.
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 embodiment is a preparation method of a capsule wall material, which comprises the following steps:
a1: adding hydrobromic acid with the mass fraction of 48% and 0.1mol of 2-amino-4-methylpyridine into a four-neck flask, stirring, cooling to-16 ℃ after the 2-amino-4-methylpyridine is completely dissolved, dropwise adding 0.25mol of liquid bromine, controlling the dropwise adding rate to be 0.5mL/min, and controlling the temperature in the dropwise adding process to be-15 ℃; stirring for 90min after the dropwise addition is finished, dropwise adding a sodium nitrite solution with the mass fraction of 8%, stirring for 25min, heating to 10 ℃, stirring for 40min, cooling to-20 ℃, dropwise adding a sodium hydroxide solution with the mass fraction of 10%, and controlling the temperature to be lower than-15 ℃ in the dropwise addition process; heating to 18 ℃ and stirring for 50min, extracting with toluene, combining organic phases, washing with water, drying, and concentrating to obtain an intermediate 1;
a2: adding 0.1mol of intermediate 1, 0.3mol of N-bromosuccinimide and 0.02mol of benzoyl peroxide into a four-neck flask, using petroleum ether as a solvent, stirring and dissolving, heating to 60 ℃, preserving heat for 24 hours, filtering after the reaction is finished, heating and refluxing a crude product and a saturated sodium bicarbonate solution for 2 hours, cooling, adding a reaction product into an ice hydrochloric acid aqueous solution while stirring, standing and layering, extracting an upper layer of liquid by using diethyl ether, combining an extraction liquid and a lower layer of liquid, washing 1 time by using distilled water, washing 2 times by using a hydrochloric acid solution and 3 times by using a sodium hydroxide solution, washing the mixture to be neutral by using distilled water, drying the mixture by using anhydrous magnesium sulfate, standing for 22 hours, performing vacuum filtration, performing rotary evaporation on a filtrate to remove the solvent and the extraction liquid, and refluxing the evaporation product by using anhydrous ethanol for 4 times to obtain an intermediate 2;
a3: mixing distilled water, urea and the intermediate 2, reacting for 1h, adding sodium hydroxide to adjust the pH value to 8.3, reacting for 1h at 68 ℃ with stirring speed of 100r/min, and after the reaction is finished, performing rotary evaporation on the reaction product to remove the solvent and cooling to 23 ℃ to obtain the capsule wall material.
Example 2:
the embodiment is a preparation method of a capsule wall material, which comprises the following steps:
a1: adding hydrobromic acid with the mass fraction of 48% and 0.1mol of 2-amino-4-methylpyridine into a four-neck flask, stirring, cooling to-13 ℃ after the 2-amino-4-methylpyridine is completely dissolved, dropwise adding 0.3mol of liquid bromine, controlling the dropwise adding rate to be 1mL/min, and controlling the temperature in the dropwise adding process to be-10 ℃; stirring for 120min after the dropwise addition is finished, then dropwise adding a sodium nitrite solution with the mass fraction of 8%, stirring for 35min, then heating to 15 ℃, stirring for 50min, then cooling to-15 ℃, dropwise adding a sodium hydroxide solution with the mass fraction of 10%, and controlling the temperature to be lower than-10 ℃ in the dropwise adding process; heating to 20 ℃ and stirring for 60min, extracting with toluene, combining organic phases, washing with water, drying, and concentrating to obtain an intermediate 1;
a2: adding 0.1mol of intermediate 1, 0.3mol of N-bromosuccinimide and 0.05mol of benzoyl peroxide into a four-neck flask, taking petroleum ether as a solvent, stirring for dissolving, heating to 70 ℃, preserving heat for 30 hours, filtering after the reaction is finished, heating and refluxing a crude product and a saturated sodium bicarbonate solution for 2.5 hours, cooling, adding a reaction product into an ice hydrochloric acid aqueous solution while stirring, standing for layering, extracting an upper layer liquid by using diethyl ether, combining an extraction liquid and a lower layer liquid, washing with distilled water for 2 times, washing with a hydrochloric acid solution for 3 times and washing with a sodium hydroxide solution for 5 times, washing with distilled water to be neutral, drying with anhydrous magnesium sulfate, standing for 24 hours, performing vacuum filtration, performing rotary evaporation on a filtrate to remove the solvent and the extraction liquid, and refluxing an evaporation product with anhydrous ethanol for 6 times to obtain an intermediate 2;
a3: mixing distilled water, urea and the intermediate 2, reacting for 2h, adding sodium hydroxide to adjust the pH to 8.5, reacting for 1.5h at 75 ℃ with stirring at a speed of 150r/min, and after the reaction is finished, performing rotary evaporation on the reaction product to remove the solvent and cooling to 25 ℃ to obtain a capsule wall material;
example 3:
the embodiment is a chemical processing method of an agricultural environment-friendly herbicide, which comprises the following steps:
the method comprises the following steps: dissolving a raw pesticide of herbicide trifluralin in 6% by mass in benzene, adding a silicon polyether defoamer DF-2692 with the mass fraction of 0.1%, stirring for 20min at 45 ℃ and the rotation speed of 700r/min, uniformly stirring, adding the capsule wall material from example 1, adding 1.5% by mass of styrene-maleic anhydride copolymerized sodium salt and 1.5% by mass of sodium polyacrylate, and stirring for 20min at the rotation speed of 1200r/min to form stable emulsion; then the rotating speed is reduced to 700r/min,
step two: adding 2% hydrochloric acid in batches in 60min to adjust the pH value of the system to 1.9; and reacting for 3.5 hours, gradually reducing the rotating speed to 170r/min, adding 0.3% of sodium chloride, gradually heating to 65 ℃ to solidify the capsule wall, wherein the solidification time is 100min, adding sodium hydroxide to adjust the pH value to be neutral after the reaction is finished, then adding ice water, filtering, adding 3% of glycol, 1.5% of sodium polyacrylate, 0.15% of xanthan gum and 0.15% of magnesium aluminum silicate by mass, and drying to form a microcapsule preparation to obtain the agricultural herbicide.
Example 4:
the embodiment is a chemical processing method of an agricultural environment-friendly herbicide, which comprises the following steps:
the method comprises the following steps: dissolving a raw pesticide of herbicide trifluralin in 6% by mass in benzene, adding 0.3% of silicon polyether defoamer DF-2692, stirring for 30min at 50 ℃ and at the rotation speed of 900r/min, adding the capsule wall material from example 2 after uniformly stirring, adding 2.5% by mass of styrene-maleic anhydride sodium copolymer and 2% by mass of sodium polyacrylate, and stirring for 30min at the rotation speed of 1500r/min to form stable emulsion; then the rotating speed is reduced to 800r/min,
step two: adding 2% hydrochloric acid in batches in 60min to adjust the pH value of the system to 2.8; and reacting for 4.5 hours, gradually reducing the rotating speed to 200r/min, adding 0.4% of sodium chloride, gradually heating to 65 ℃ to solidify the capsule wall, wherein the solidification time is 100min, adding sodium hydroxide to adjust the pH value to be neutral after the reaction is finished, then adding ice water, filtering, adding 3% of ethylene glycol, 2% of sodium polyacrylate, 0.15% of xanthan gum and 0.15% of aluminum magnesium silicate by mass, and drying to form a microcapsule preparation to obtain the agricultural herbicide.
Comparative example 1:
comparative example 1 differs from example 4 in that chitosan is used instead of the wall material.
Comparative example 2:
comparative example 2 differs from example 4 in that no sodium chloride was added.
The percent release and drug loading of trifluralin in the herbicides of the microcapsule formulations of examples 3 to 4 and comparative examples 1 to 2 were determined; adding 1g of the micro-capsule preparation of the trifluralin into an SPR-DT12A intelligent digital display tester to test the release amount of the trifluralin within 1 day at 25 ℃ and 200 r/min; adding 0.1g of trifluralin into 6mL of water, shaking for dispersion, measuring by using a WYL-1 type microcapsule suspending agent free release tester, extracting free components within 30min under the condition of 70r/min, and detecting results are shown in the following table:
| sample(s)Number of | Percentage of release | Drug loading |
| Example 3 | 30％ | 75％ |
| Example 4 | 35％ | 75％ |
| Comparative example 1 | 54％ | 55％ |
| Comparative example 2 | 52％ | 53％ |
With reference to the data, according to the embodiment and the comparative example 1, the capsule wall material of the invention has better wrapping property than chitosan, the stability of the microcapsule is stronger, and the slow release effect is better, and according to the comparative example 2, the addition of sodium chloride can improve the drug loading capacity of the microcapsule preparation, so that the environment-friendly processing method of the agricultural herbicide of the invention has excellent slow release effect and drug loading capacity performance, and is more environment-friendly.
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 it will be appreciated by those skilled in the art that various modifications, additions and substitutions can be made to the embodiments described without departing from the scope of the invention as defined in the appended claims.
Claims (6)
1. An environment-friendly processing method of agricultural herbicide is characterized by comprising the following steps:
the method comprises the following steps: mixing distilled water, urea and the intermediate 2, adding sodium hydroxide to adjust the pH value to 8.3-8.5, and stirring and reacting at 68-75 ℃ to obtain the capsule wall material.
Step two: dissolving the original drug of the herbicide trifluralin in benzene, adding a defoaming agent, stirring for 20-30min, adding a capsule wall material, then adding an emulsifying agent and a dispersing agent, stirring, and adding hydrochloric acid to adjust the pH value to 1.9-2.8; reacting for 3.5-4.5h, gradually reducing the rotating speed to 170-200r/min, adding sodium chloride, gradually heating to 65 ℃ to solidify the capsule wall, reacting for 1-2h, adding sodium hydroxide to adjust the pH value to be neutral, then adding ice water, filtering, adding an antifreezing agent, a wetting dispersant and a thickening agent, and drying to form a microcapsule preparation, thereby obtaining the agricultural herbicide.
2. The environment-friendly processing method of the agricultural herbicide as claimed in claim 1, wherein the preparation method of the capsule wall material is as follows:
a1: adding hydrobromic acid and 2-amino-4-methylpyridine into a four-neck flask, stirring, cooling to-16-13 ℃ after the 2-amino-4-methylpyridine is completely dissolved, dropwise adding liquid bromine, controlling the dropwise adding speed to be 0.5-1mL/min, and controlling the temperature in the dropwise adding process to be-15-10 ℃; stirring for 90-120min after the dropwise addition is finished, then dropwise adding a sodium nitrite solution, stirring for 25-35min, then heating to 10-15 ℃, stirring for 40-50min, then cooling to 20-15 ℃, dropwise adding a sodium hydroxide solution, and controlling the temperature to be lower than-15-10 ℃ in the dropwise adding process; heating to 18-20 deg.C, stirring for 50-60min, extracting with toluene, mixing organic phases, washing with water, drying, and concentrating to obtain intermediate 1;
a2: adding the intermediate 1, petroleum ether, N-bromosuccinimide and benzoyl peroxide into a four-neck flask, stirring and dissolving, heating to 60-70 ℃, preserving heat for 24-30h, filtering after the reaction is finished, heating and refluxing the crude product and a saturated sodium bicarbonate solution for 2-2.5h, cooling, adding the reaction product into an ice hydrochloric acid aqueous solution while stirring, standing and layering, extracting an upper layer liquid by using diethyl ether, combining an extraction liquid and a lower layer liquid, washing 1-2 times by using distilled water, washing 2-3 times by using a hydrochloric acid solution and 3-5 times by using a sodium hydroxide solution, washing to be neutral by using distilled water, drying by using anhydrous magnesium sulfate, standing for 22-24h, carrying out vacuum filtration, carrying out rotary evaporation on a filtrate to remove a solvent and the extraction liquid, and refluxing an evaporation product for 4-6 times by using anhydrous ethanol to obtain an intermediate 2;
a3: mixing distilled water, urea and the intermediate 2, reacting for 1-2h, adding sodium hydroxide to adjust the pH value to 8.3-8.5, reacting for 1-1.5h at the stirring speed of 100-150r/min at the temperature of 68-75 ℃, and after the reaction is finished, removing the solvent by rotary evaporation of the reaction product and cooling to 23-25 ℃ to obtain the capsule wall material.
3. The environment-friendly processing method of an agricultural herbicide as claimed in claim 2, wherein the dosage ratio of the 2-amino-4-methylpyridine to the liquid bromine in the step A1 is 0.1mol:0.25-0.3mol, wherein the mass fraction of the sodium hydroxide solution is 10%, and the mass fraction of the hydrobromic acid is 48%. The mass fraction of the sodium nitrite solution is 8%.
4. The method for environmentally processing an agricultural herbicide as claimed in claim 2, wherein the amount ratio of the intermediate 1, the N-bromosuccinimide, the benzoyl peroxide, the diethyl ether and the petroleum ether in the step A2 is 0.1mol:0.25-0.3mol:0.02-0.05mol:200mL of: 150mL, wherein the mass fraction of the ice hydrochloric acid aqueous solution is 5-10%, the mass fraction of the sodium hydroxide solution is 10%, and the mass fraction of the hydrochloric acid solution is 5-10%.
5. The method for environmentally processing an agricultural herbicide as claimed in claim 2, wherein the ratio of the amount of the distilled water, the urea and the intermediate 2 in step A3 is 100-120mL:0.1mol:30-35g.
6. The environment-friendly processing method of the agricultural herbicide as claimed in claim 2, characterized by comprising the following steps:
the method comprises the following steps: mixing distilled water, urea and the intermediate 2, adding sodium hydroxide to adjust the pH value to 8.3-8.5, and stirring and reacting at 68-75 ℃ to obtain a capsule wall material;
step two: dissolving the original pesticide of the herbicide trifluralin in benzene, adding a defoaming agent, stirring for 20-30min, adding the capsule wall material, then adding an emulsifying agent and a dispersing agent, stirring, and adding hydrochloric acid to adjust the pH value to 1.9-2.8; reacting for 3.5-4.5h, gradually reducing the rotating speed to 170-200r/min, adding sodium chloride, gradually heating to 65 ℃ to solidify the capsule wall, reacting for 1-2h, adding sodium hydroxide to adjust the pH value to be neutral, then adding ice water, filtering, adding an antifreezing agent, a wetting dispersant and a thickening agent, and drying to form a microcapsule preparation, thereby obtaining the agricultural herbicide.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101010299A (en) * | 2004-06-15 | 2007-08-01 | 布里斯托尔-迈尔斯斯奎布公司 | Six-membered heterocycles useful as serine protease inhibitors |
| CN104782623A (en) * | 2015-03-25 | 2015-07-22 | 塔里木大学 | Trifluralin micro-capsule granule and preparation method thereof |
| CN115011047A (en) * | 2022-07-04 | 2022-09-06 | 广东裕泰实业有限公司 | Preparation method of antibacterial PVC packaging film |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101010299A (en) * | 2004-06-15 | 2007-08-01 | 布里斯托尔-迈尔斯斯奎布公司 | Six-membered heterocycles useful as serine protease inhibitors |
| CN104782623A (en) * | 2015-03-25 | 2015-07-22 | 塔里木大学 | Trifluralin micro-capsule granule and preparation method thereof |
| CN115011047A (en) * | 2022-07-04 | 2022-09-06 | 广东裕泰实业有限公司 | Preparation method of antibacterial PVC packaging film |
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