CN113693078A - Herbicide containing anilofos, preparation method and application thereof - Google Patents
Herbicide containing anilofos, preparation method and application thereof Download PDFInfo
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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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds
- A01N57/14—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-oxygen bonds or phosphorus-to-sulfur bonds containing aromatic radicals
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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
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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
- A01N41/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom
- A01N41/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom containing a sulfur-to-oxygen double bond
- A01N41/10—Sulfones; Sulfoxides
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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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
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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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/26—Oxidation products of dithiocarbamic acid derivatives, e.g. thiuram sulfides
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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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
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Abstract
The invention discloses a herbicide containing anilofos, a preparation method and application thereof, belonging to the technical field of herbicides, wherein the preparation method comprises the steps of preparing a kernel substance, wrapping the kernel, preparing an outer-wrapping herbicide, and preparing the herbicide containing anilofos; the preparation method comprises the steps of preparing an inner core substance, uniformly mixing a difenoconazole technical substance, a thiram technical substance, sodium dodecyl sulfate, polyethylene glycol 4000, volcanic rock powder and zwitterionic polyacrylamide to obtain a raw material mixture, and then placing the raw material mixture into a liquid nitrogen ball milling tank to perform liquid nitrogen ball milling to obtain the inner core substance; the anilofos-containing herbicide prepared by the invention can reduce phytotoxicity when the anilofos-containing herbicide is used, improve the compounding effect, and meanwhile, the anilofos herbicide prepared by the invention also has bactericidal performance and can reduce the propagation and growth of bacteria when the anilofos herbicide is used.
Description
Technical Field
The invention relates to a herbicide containing anilofos, a preparation method and application thereof, belonging to the technical field of herbicides.
Background
The anilofos belongs to an organic phosphorus selective systemic conduction herbicide, is absorbed by young buds and underground stems of plants to inhibit cell fission and extension, so that new leaves of weeds are not easy to draw out, the growth stops, and the weeds are withered finally, and the effect on the germinated weeds is the best; has poor effect on grown weeds. The growth of the weeds is stopped after the weeds are applied, the leaves are dark green and sometimes decolored, the leaves are shortened and thick, the leaves are easy to break, the heart leaves are not easy to draw out, and finally the whole plants die. Although the control effect is good, the control range is limited, and only barnyard grass and cyperaceae weeds in a 3-leaf period can be controlled, and the control effect on old weeds is poor.
In order to expand the control range of anilofos, a compounding mode is usually adopted, anilofos is mixed with other herbicides or insecticides, so that the weed control spectrum is expanded, the dosage is reduced, the production cost is reduced, the pesticide residue is reduced, and the safety to crops is improved, but when the anilofos is mixed with other herbicides, the compound is improper, the phytotoxicity is easy to occur and the use effect is easy to be influenced, the existing compounding technology is immature, and when more than two kinds of pesticides are compounded, the compounding effect is easy to be influenced; in addition, the anilofos increases the tolerance of bacteria to antibiotics when in use, thereby causing the increase of bacteria, but the anilofos cannot be used in combination with a bactericide, so that the anilofos can cause the mass propagation and growth of bacteria when in use.
Patent CN109769852A discloses a herbicide composition containing anilofos, cyhalofop-butyl and benzobicyclon, which has a synergistic effect, wherein the active ingredients in the herbicide composition are anilofos, cyhalofop-butyl and benzobicyclon, and the mass ratio of the three components is 1-50: 1-30:5-25, more preferably 1-25:5-30:5-25, most preferably 10-25:5-30: 5-20; the patent has the following defects: the herbicide composition, when applied, increases the tolerance of bacteria to antibiotics, thereby causing an increase in bacteria.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the anilofos-containing herbicide, the preparation method and the application thereof, so that the phytotoxicity when the anilofos-containing herbicide is used can be reduced, the compounding effect is improved, and meanwhile, the prepared anilofos herbicide also has bactericidal performance and can reduce the propagation and growth of bacteria when in use.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a herbicide containing anilofos is prepared by taking difenoconazole and thiram as kernel substances, and coating the kernel substances with anilofos, bensulfuron methyl and benzobicylon as external herbicide;
the inner core material comprises the following components in parts by weight: 12-13 parts of difenoconazole technical material and 14-16 parts of thiram technical material;
the outsourcing herbicide comprises the following components in parts by weight: 10-15 parts of anilofos technical, 40-45 parts of bensulfuron methyl technical and 25-30 parts of benzobicylon technical.
A process for preparing the herbicide containing anilofos includes preparing kernel substance, wrapping the kernel substance, preparing coated herbicide, and preparing the herbicide containing anilofos.
The preparation method comprises the steps of uniformly mixing difenoconazole technical raw material, thiram technical raw material, sodium dodecyl sulfate, polyethylene glycol 4000, volcanic powder and zwitter-ion polyacrylamide to obtain a raw material mixture, then placing the raw material mixture into a liquid nitrogen ball milling tank to carry out liquid nitrogen ball milling, adding alumina balls with the diameter of 3-5mm into the liquid nitrogen ball milling tank, controlling the volume of liquid nitrogen to be 65-70% of the volume of the liquid nitrogen ball milling tank, controlling the ball milling rotation speed during liquid nitrogen ball milling to be 160-type 180rpm, ball milling time to be 3-4h, and controlling the ball-to-material ratio to be (5-7): and 1, finishing ball milling by using liquid nitrogen to obtain a kernel substance.
The raw materials in the step of preparing the inner core material comprise the following components in parts by weight: 12-13 parts of difenoconazole technical material, 14-16 parts of thiram technical material, 10-12 parts of sodium dodecyl sulfate, 13-15 parts of sodium dodecyl sulfate, 3-5 parts of polyethylene glycol 4000, 7-10 parts of volcanic rock powder and 2-5 parts of zwitterionic polyacrylamide.
The inner core is wrapped, the inner core substance is added into deionized water, then tetramethylolphosphonium chloride, 10% by mass of sodium hydroxide aqueous solution, ferric chloride, acrylic acid and polyvinyl alcohol are added, then ultrasonic vibration is carried out at 70-80 ℃, the ultrasonic vibration frequency is controlled to be 20-30kHz, the ultrasonic vibration amplitude is 5-8 mu m, the ultrasonic vibration time is 30-40min, the inner core liquid is obtained after the ultrasonic vibration is finished, vacuum spray drying is carried out on the inner core liquid, and the wrapped inner core is obtained after the vacuum spray is finished.
The vacuum degree in the vacuum spray drying process is 0.05-0.07MPa, the atomization pressure is 0.3-0.5MPa, the feeding temperature is 70-75 ℃, the feeding amount is 750mL/h, and the air inlet temperature is 110-120 ℃.
The raw materials in the step of wrapping the inner core comprise the following components in parts by weight: 10-12 parts of core material, 50-60 parts of absolute ethyl alcohol, 2-5 parts of tetrakis (hydroxymethyl) phosphonium chloride, 7-10 parts of 10% sodium hydroxide aqueous solution by mass fraction, 3-5 parts of ferric chloride, 1-3 parts of acrylic acid and 3-4 parts of polyvinyl alcohol.
The preparation method of the externally-coated herbicide comprises the steps of placing anilofos technical, bensulfuron methyl technical, benzobicylon technical, alkyl ketene dimer and calcium lignosulfonate at a temperature of-5 ℃ to-2 ℃ for low-temperature grinding until the particle size is 30-40 mu m, then raising the temperature to 25-30 ℃, adding zeolite powder, tween 80, polyethylene glycol 2000, polyethylene glycol 6000, guar gum and sodium alginate, uniformly mixing, introducing into a jet mill, and crushing to 10-20 mu m to obtain the externally-coated herbicide.
The raw materials for preparing the external herbicide comprise the following components in parts by weight: 10-15 parts of anilofos technical, 40-45 parts of bensulfuron methyl technical, 25-30 parts of benzobicylon technical, 10-15 parts of alkyl ketene dimer, 12-15 parts of calcium lignosulfonate, 80-90 parts of zeolite powder, 5-10 parts of tween 80, 15-20 parts of polyethylene glycol 2000, 5-10 parts of polyethylene glycol 6000, 30-40 parts of guar gum and 40-50 parts of sodium alginate.
The preparation method comprises the steps of preparing the herbicide containing anilofos, placing the wrapped inner core into a granulator, wrapping the wrapped inner core with the outer herbicide, and controlling the mass ratio of the wrapped inner core to the outer herbicide to be 1: 5-6, and obtaining the herbicide containing anilofos after the coating is finished.
The application of the herbicide containing anilofos in rice is characterized in that the herbicide containing anilofos and water are mixed according to a mass ratio of 1: 300 to obtain herbicide aqueous solution, and then uniformly spraying the herbicide aqueous solution to the paddy field, wherein the dosage of the herbicide aqueous solution per mu is 600 g.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the herbicide containing anilofos, disclosed by the invention, through adding the alkyl ketene dimer and the calcium lignosulfonate in the step of preparing the external herbicide and grinding the raw materials at low temperature, three kinds of herbicides can be reasonably compounded, the problems that the compounding effect of more than two kinds of herbicides is not ideal and the effect of anilofos on controlling more than 3 leaves of barnyard grass is poor are solved, and the control effect of the compounded herbicide when the compounded herbicide is used for controlling more than 3 leaves of barnyard grass is 86.9% -89.2%;
(2) according to the herbicide containing anilofos, provided by the invention, the tetrakis hydroxymethyl phosphonium chloride and the polyvinyl alcohol are added in the step of coating the kernel, and the guar gum and the sodium alginate are added in the step of preparing the outer herbicide, so that the total control effect on weeds in rice can be improved, and the total control effect is improved to 97.3% -98.2%;
(3) the invention has the advantages that the prepared herbicide containing anilofos is prepared by adding tetrakis hydroxymethyl phosphonium chloride and polyvinyl alcohol in the step of wrapping the inner core and adding guar gum and sodium alginate in the step of preparing the outer-wrapped herbicide, the tetrakis hydroxymethyl phosphonium chloride and the polyvinyl alcohol can play a good role in wrapping and slowly releasing the bactericide, the guar gum and the sodium alginate can wrap the herbicide while slowly releasing, the influence of the herbicide and the bactericidal effect is avoided, when in use, the herbicide firstly plays a role in weeding, then the bactericidal substance in the inner core can be slowly released in soil, thereby realizing the compounding of the bactericide and the herbicide, improving the bactericidal effect of the herbicide and the bactericidal property, avoiding the occurrence of a large amount of variation, propagation and growth of bacteria after the herbicide is used, under the condition of not additionally using the bactericide after the herbicide is used, the survival rate of the rice after one month and two months can reach 100 percent;
(4) according to the herbicide containing anilofos, provided by the invention, the tetrakis hydroxymethyl phosphonium chloride and the polyvinyl alcohol are added in the step of coating the inner core, and the guar gum and the sodium alginate are added in the step of preparing the outer herbicide, so that the bactericide and the herbicide can be compounded, the weeding effect of the herbicide is improved, the bactericidal property is improved, and the control efficiency reaches 82.3% -84.8% after the herbicide is used for 10 days when the herbicide is used for preventing and treating rice sheath blight.
Detailed Description
In order to more clearly understand the technical features, objects, and effects of the present invention, specific embodiments of the present invention will now be described.
Example 1
A preparation method of a herbicide containing anilofos comprises the following specific steps:
1. preparing an inner core material: uniformly mixing a difenoconazole technical material, a thiram technical material, sodium dodecyl sulfate, polyethylene glycol 4000, volcanic rock powder and zwitterionic polyacrylamide to obtain a raw material mixture, then placing the raw material mixture into a liquid nitrogen ball milling tank for liquid nitrogen ball milling, adding alumina balls with the diameter of 3mm into the liquid nitrogen ball milling tank, controlling the volume of liquid nitrogen to be 65% of the volume of the liquid nitrogen ball milling tank, controlling the ball milling rotation speed during liquid nitrogen ball milling to be 160rpm, and controlling the ball milling time to be 3h, wherein the ball-to-material ratio is 5: 1, obtaining a kernel substance after liquid nitrogen ball milling is finished;
the raw materials in the step of preparing the inner core material comprise the following components in parts by weight: 12 parts of difenoconazole technical material, 14 parts of thiram technical material, 10 parts of sodium dodecyl sulfate, 13 parts of sodium dodecyl sulfate, 3 parts of polyethylene glycol 4000, 7 parts of volcanic rock powder and 2 parts of zwitterionic polyacrylamide.
2. Wrapping the inner core: adding core materials into deionized water, adding tetramethylolphosphonium chloride, 10% by mass of sodium hydroxide aqueous solution, ferric chloride, acrylic acid and polyvinyl alcohol, then carrying out ultrasonic vibration at 70 ℃, controlling the ultrasonic vibration frequency to be 20kHz, the ultrasonic vibration amplitude to be 5 microns, the ultrasonic vibration time to be 30min, obtaining core liquid after the ultrasonic vibration is finished, carrying out vacuum spray drying on the core liquid, controlling the vacuum degree in the vacuum spray drying process to be 0.05MPa, the atomizing pressure to be 0.3MPa, the feeding temperature to be 70 ℃, the feeding amount to be 700mL/h, the air inlet temperature to be 110 ℃, and obtaining the wrapped core after the vacuum spray is finished;
the raw materials in the step of wrapping the inner core comprise the following components in parts by weight: 10 parts of inner core material, 50 parts of absolute ethyl alcohol, 2 parts of tetrakis (hydroxymethyl) phosphonium chloride, 7 parts of sodium hydroxide aqueous solution with the mass fraction of 10%, 3 parts of ferric chloride, 1 part of acrylic acid and 3 parts of polyvinyl alcohol.
3. Preparing an external herbicide: carrying out low-temperature grinding on anilofos technical, bensulfuron methyl technical, benzobicyclon technical, alkyl ketene dimer and calcium lignosulfonate at the temperature of-5 ℃ until the particle size is 30 mu m, raising the temperature to 25 ℃, adding zeolite powder, tween 80, polyethylene glycol 2000, polyethylene glycol 6000, guar gum and sodium alginate, uniformly mixing, introducing into a jet mill, and crushing to 10 mu m to obtain an externally-coated herbicide;
the raw materials for preparing the external herbicide comprise the following components in parts by weight: 10 parts of anilofos technical, 40 parts of bensulfuron methyl technical, 25 parts of benzobicyclon technical, 10 parts of alkyl ketene dimer, 12 parts of calcium lignosulphonate, 80 parts of zeolite powder, 5 parts of tween 80, 15 parts of polyethylene glycol 2000, 5 parts of polyethylene glycol 6000, 30 parts of guar gum and 40 parts of sodium alginate.
4. Preparation of anilofos-containing herbicides: placing the wrapped inner core into a granulator, wrapping the wrapped inner core by using an outsourcing herbicide, and controlling the mass ratio of the wrapped inner core to the outsourcing herbicide to be 1: and 5, obtaining the herbicide containing anilofos after the coating is finished.
Example 2
A preparation method of a herbicide containing anilofos comprises the following specific steps:
1. preparing an inner core material: uniformly mixing a difenoconazole technical material, a thiram technical material, sodium dodecyl sulfate, polyethylene glycol 4000, volcanic rock powder and zwitterionic polyacrylamide to obtain a raw material mixture, then placing the raw material mixture into a liquid nitrogen ball milling tank for liquid nitrogen ball milling, adding alumina balls with the diameter of 4mm into the liquid nitrogen ball milling tank, controlling the volume of liquid nitrogen to be 67% of the volume of the liquid nitrogen ball milling tank, controlling the ball milling rotation speed during the liquid nitrogen ball milling to be 170rpm, and controlling the ball milling time to be 3.5h, wherein the ball-to-material ratio is 6: 1, obtaining a kernel substance after liquid nitrogen ball milling is finished;
the raw materials in the step of preparing the inner core material comprise the following components in parts by weight: 12 parts of difenoconazole technical material, 15 parts of thiram technical material, 11 parts of sodium dodecyl sulfate, 14 parts of sodium dodecyl sulfate, 4 parts of polyethylene glycol 4000, 8 parts of volcanic rock powder and 3 parts of zwitterionic polyacrylamide.
2. Wrapping the inner core: adding core materials into deionized water, adding tetramethylolphosphonium chloride, 10% by mass of sodium hydroxide aqueous solution, ferric chloride, acrylic acid and polyvinyl alcohol, then carrying out ultrasonic vibration at 75 ℃, controlling the ultrasonic vibration frequency to be 25kHz, the ultrasonic vibration amplitude to be 7 microns, the ultrasonic vibration time to be 35min, obtaining core liquid after the ultrasonic vibration is finished, carrying out vacuum spray drying on the core liquid, controlling the vacuum degree in the vacuum spray drying process to be 0.06MPa, the atomizing pressure to be 0.4MPa, the feeding temperature to be 72 ℃, the feeding amount to be 720mL/h, the air inlet temperature to be 115 ℃, and obtaining the wrapped core after the vacuum spray is finished;
the raw materials in the step of wrapping the inner core comprise the following components in parts by weight: 11 parts of inner core material, 55 parts of absolute ethyl alcohol, 3 parts of tetrakis (hydroxymethyl) phosphonium chloride, 8 parts of 10 mass percent sodium hydroxide aqueous solution, 4 parts of ferric chloride, 2 parts of acrylic acid and 3 parts of polyvinyl alcohol.
3. Preparing an external herbicide: carrying out low-temperature grinding on anilofos technical, bensulfuron methyl technical, benzobicyclon technical, alkyl ketene dimer and calcium lignosulfonate at the temperature of-4 ℃ until the particle size is 35 mu m, raising the temperature to 27 ℃, adding zeolite powder, tween 80, polyethylene glycol 2000, polyethylene glycol 6000, guar gum and sodium alginate, uniformly mixing, introducing into a jet mill, and crushing to 15 mu m to obtain an externally-coated herbicide;
the raw materials for preparing the external herbicide comprise the following components in parts by weight: 12 parts of anilofos technical, 42 parts of bensulfuron methyl technical, 27 parts of benzobicyclon technical, 12 parts of alkyl ketene dimer, 13 parts of calcium lignosulfonate, 85 parts of zeolite powder, 7 parts of tween 80, 17 parts of polyethylene glycol 2000, 8 parts of polyethylene glycol 6000, 35 parts of guar gum and 45 parts of sodium alginate.
4. Preparation of anilofos-containing herbicides: placing the wrapped inner core into a granulator, wrapping the wrapped inner core by using an outsourcing herbicide, and controlling the mass ratio of the wrapped inner core to the outsourcing herbicide to be 1: 5.5, obtaining the herbicide containing anilofos after the coating is finished.
Example 3
A preparation method of a herbicide containing anilofos comprises the following specific steps:
1. preparing an inner core material: uniformly mixing a difenoconazole technical material, a thiram technical material, sodium dodecyl sulfate, polyethylene glycol 4000, volcanic rock powder and zwitterionic polyacrylamide to obtain a raw material mixture, then placing the raw material mixture into a liquid nitrogen ball milling tank for liquid nitrogen ball milling, adding alumina balls with the diameter of 5mm into the liquid nitrogen ball milling tank, controlling the volume of liquid nitrogen to be 70% of the volume of the liquid nitrogen ball milling tank, controlling the ball milling rotation speed during liquid nitrogen ball milling to be 180rpm, and controlling the ball milling time to be 4h, wherein the ball-to-material ratio is 7: 1, obtaining a kernel substance after liquid nitrogen ball milling is finished;
the raw materials in the step of preparing the inner core material comprise the following components in parts by weight: 13 parts of a benzene ether epoxiconazole technical material, 16 parts of a thiram technical material, 12 parts of sodium dodecyl sulfate, 15 parts of sodium dodecyl sulfate, 5 parts of polyethylene glycol 4000, 10 parts of volcanic rock powder and 5 parts of zwitterionic polyacrylamide.
2. Wrapping the inner core: adding core materials into deionized water, adding tetramethylolphosphonium chloride, 10% by mass of sodium hydroxide aqueous solution, ferric chloride, acrylic acid and polyvinyl alcohol, then carrying out ultrasonic vibration at 80 ℃, controlling the ultrasonic vibration frequency to be 30kHz, the ultrasonic vibration amplitude to be 8 microns, the ultrasonic vibration time to be 40min, obtaining core liquid after the ultrasonic vibration is finished, carrying out vacuum spray drying on the core liquid, controlling the vacuum degree in the vacuum spray drying process to be 0.07MPa, the atomizing pressure to be 0.5MPa, the feeding temperature to be 75 ℃, the feeding amount to be 750mL/h, the air inlet temperature to be 120 ℃, and obtaining the wrapped core after the vacuum spray is finished;
the raw materials in the step of wrapping the inner core comprise the following components in parts by weight: 12 parts of inner core material, 60 parts of absolute ethyl alcohol, 5 parts of tetrakis (hydroxymethyl) phosphonium chloride, 10 parts of 10 mass percent sodium hydroxide aqueous solution, 5 parts of ferric chloride, 3 parts of acrylic acid and 4 parts of polyvinyl alcohol.
3. Preparing an external herbicide: carrying out low-temperature grinding on anilofos technical, bensulfuron methyl technical, benzobicyclon technical, alkyl ketene dimer and calcium lignosulfonate at the temperature of-2 ℃ until the particle size is 40 mu m, raising the temperature to 30 ℃, adding zeolite powder, tween 80, polyethylene glycol 2000, polyethylene glycol 6000, guar gum and sodium alginate, uniformly mixing, introducing into a jet mill, and crushing to 20 mu m to obtain an outer herbicide;
the raw materials for preparing the external herbicide comprise the following components in parts by weight: 15 parts of anilofos technical, 45 parts of bensulfuron methyl technical, 30 parts of benzobicyclon technical, 15 parts of alkyl ketene dimer, 15 parts of calcium lignosulphonate, 90 parts of zeolite powder, 10 parts of tween 80, 20 parts of polyethylene glycol 2000, 10 parts of polyethylene glycol 6000, 40 parts of guar gum and 50 parts of sodium alginate.
4. Preparation of anilofos-containing herbicides: placing the wrapped inner core into a granulator, wrapping the wrapped inner core by using an outsourcing herbicide, and controlling the mass ratio of the wrapped inner core to the outsourcing herbicide to be 1: 6, obtaining the herbicide containing anilofos after the coating is finished.
Comparative example 1
The procedure for the preparation of anilofos-containing herbicides described in example 1 was followed with the following exceptions: in the step 2, no tetrakis (hydroxymethyl) phosphonium chloride and polyvinyl alcohol are added in the step of wrapping the inner core.
Comparative example 2
The procedure for the preparation of anilofos-containing herbicides described in example 1 was followed with the following exceptions: in the step 3 of preparing the external herbicide, alkyl ketene dimer and calcium lignosulfonate are not added, and anilofos raw pesticide is compounded with bensulfuron methyl, and the benzobicylon raw pesticide is ground at 25 ℃ until the particle size is 30 mu m.
Comparative example 3
The procedure for the preparation of anilofos-containing herbicides described in example 1 was followed with the following exceptions: in the step 3 of preparing the outsourcing herbicide, guar gum and sodium alginate are not added.
The examples 1 to 3 and the comparative examples 1 to 3 were each subjected to a test of efficacy, and the control effect on barnyard grass having 3 or more leaves was measured, and the test area was 1 mu each.
The test method comprises the following steps: the amount of barnyard grass of 3 leaves or more in each test rice was counted, and then the anilofos-containing herbicide of examples 1 to 3 and comparative examples 1 to 3 and water were mixed in a mass ratio of 1: 300 to obtain a herbicide aqueous solution, then adding the herbicide aqueous solution into a knapsack sprayer for uniform spraying, and during spraying, uniformly spraying the liquid medicine into the test rice to avoid the phenomena of missed spraying and multiple spraying, wherein the dosage of the herbicide aqueous solution per mu is 600 g.
After the test, the death condition of the barnyard grass with more than 3 leaves is observed after the medicine is applied for 10 days, the control effect is counted, and the test result is shown as follows:
the examples 1 to 3 and comparative examples 1 to 3 were each subjected to a rice efficacy test in an area of 1 mu each.
Test work: the rice needs good growth of rice seedlings, strong plants and no other plant diseases and insect pests.
Control target: barnyard grass, sedge grass, monochoria vaginalis, scripus triqueter, moleplant seed, eupatorium herb and the like.
The test method comprises the following steps: the anilofos-containing herbicide of examples 1 to 3 and comparative examples 1 to 3 and water were mixed in a mass ratio of 1: 300 to obtain a herbicide aqueous solution, then adding the herbicide aqueous solution into a knapsack sprayer for uniform spraying, and during spraying, uniformly spraying the liquid medicine into the test rice to avoid the phenomena of missed spraying and multiple spraying, wherein the dosage of the herbicide aqueous solution per mu is 600 g.
Observing the death condition of the weeds after 40 days of application after the test, and counting the total control effect; and observing the production condition of the rice after the application of the pesticide for one month and two months without additionally adding the bactericide to investigate whether the pesticide has phytotoxicity and bactericidal capacity on crops, wherein the test results are as follows:
the disease resistance tests of rice sheath blight disease were conducted on examples 1 to 3 and comparative examples 1 to 3, respectively, with test areas of 1 mu each, and the test methods were as follows:
the anilofos-containing herbicide of examples 1 to 3 and comparative examples 1 to 3 and water were mixed in a mass ratio of 1: 300, then adding the herbicide aqueous solution into a knapsack sprayer for uniform spraying, wherein during spraying, the liquid medicine is required to be uniformly sprayed into test rice infected with rice sheath blight, so that the phenomena of missing spraying and multiple spraying are avoided, the dosage of the herbicide aqueous solution per mu is 600g, the control effect after 10 days of pesticide application is counted, and the test results are as follows:
all percentages used in the present invention are mass percentages unless otherwise indicated.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The herbicide containing anilofos is characterized in that the difenoconazole and the thiram are used as kernel substances, and the anilofos, the bensulfuron methyl and the benzobicylon are used as external herbicides for external coating after the kernel substances are coated;
the inner core material comprises the following components in parts by weight: 12-13 parts of difenoconazole technical material and 14-16 parts of thiram technical material;
the outsourcing herbicide comprises the following components in parts by weight: 10-15 parts of anilofos technical, 40-45 parts of bensulfuron methyl technical and 25-30 parts of benzobicylon technical.
2. A preparation method of a herbicide containing anilofos is characterized by comprising the steps of preparing a kernel substance, wrapping the kernel substance, preparing an outer-wrapping herbicide and preparing the herbicide containing anilofos;
the preparation method comprises the steps of uniformly mixing difenoconazole technical raw material, thiram technical raw material, sodium dodecyl sulfate, polyethylene glycol 4000, volcanic powder and zwitter-ion polyacrylamide to obtain a raw material mixture, then placing the raw material mixture into a liquid nitrogen ball milling tank to carry out liquid nitrogen ball milling, adding alumina balls with the diameter of 3-5mm into the liquid nitrogen ball milling tank, controlling the volume of liquid nitrogen to be 65-70% of the volume of the liquid nitrogen ball milling tank, controlling the ball milling rotation speed during liquid nitrogen ball milling to be 160-type 180rpm, ball milling time to be 3-4h, and controlling the ball-to-material ratio to be (5-7): and 1, finishing ball milling by using liquid nitrogen to obtain a kernel substance.
3. The method for preparing a anilofos-containing herbicide as claimed in claim 2, wherein the raw materials in the step of preparing the core material comprise, in parts by weight: 12-13 parts of difenoconazole technical material, 14-16 parts of thiram technical material, 10-12 parts of sodium dodecyl sulfate, 13-15 parts of sodium dodecyl sulfate, 3-5 parts of polyethylene glycol 4000, 7-10 parts of volcanic rock powder and 2-5 parts of zwitterionic polyacrylamide.
4. The method for preparing a anilofos-containing herbicide as claimed in claim 2, wherein the method comprises the steps of wrapping the core, adding the core material into deionized water, adding tetrakis hydroxymethyl phosphonium chloride, 10% by mass of an aqueous solution of sodium hydroxide, ferric chloride, acrylic acid and polyvinyl alcohol, performing ultrasonic vibration at 70-80 ℃, controlling the ultrasonic vibration frequency to be 20-30kHz, the ultrasonic vibration amplitude to be 5-8 μm, the ultrasonic vibration time to be 30-40min, obtaining a core liquid after the ultrasonic vibration is finished, performing vacuum spray drying on the core liquid, and obtaining the wrapped core after the vacuum spray is finished.
5. The method for preparing anilofos-containing herbicide as claimed in claim 4, wherein the vacuum degree in the vacuum spray drying process is 0.05-0.07MPa, the atomization pressure is 0.3-0.5MPa, the feeding temperature is 70-75 ℃, the feeding amount is 750mL/h, and the inlet temperature is 110-120 ℃.
6. The method for preparing a anilofos-containing herbicide as claimed in claim 4, wherein the raw materials in the step of coating the kernel comprise, in parts by weight: 10-12 parts of core material, 50-60 parts of absolute ethyl alcohol, 2-5 parts of tetrakis (hydroxymethyl) phosphonium chloride, 7-10 parts of 10% sodium hydroxide aqueous solution by mass fraction, 3-5 parts of ferric chloride, 1-3 parts of acrylic acid and 3-4 parts of polyvinyl alcohol.
7. The method for preparing the anilofos-containing herbicide as claimed in claim 2, wherein the preparation of the coated herbicide comprises grinding anilofos, bensulfuron methyl, benzobicyclon, alkyl ketene dimer and calcium lignosulfonate at a low temperature of-5 ℃ to-2 ℃ until the particle size is 30-40 μm, then raising the temperature to 25-30 ℃, adding zeolite powder, tween 80, polyethylene glycol 2000, polyethylene glycol 6000, guar gum and sodium alginate, mixing uniformly, and then introducing into a jet mill to be ground to 10-20 μm to obtain the coated herbicide.
8. The method for preparing anilofos-containing herbicides according to claim 7, wherein the raw materials for preparing the coated herbicide comprise, in parts by weight: 10-15 parts of anilofos technical, 40-45 parts of bensulfuron methyl technical, 25-30 parts of benzobicylon technical, 10-15 parts of alkyl ketene dimer, 12-15 parts of calcium lignosulfonate, 80-90 parts of zeolite powder, 5-10 parts of tween 80, 15-20 parts of polyethylene glycol 2000, 5-10 parts of polyethylene glycol 6000, 30-40 parts of guar gum and 40-50 parts of sodium alginate.
9. The method for preparing a anilofos-containing herbicide as claimed in claim 2, wherein the anilofos-containing herbicide is prepared by placing the coated core in a granulator, coating the coated core with the coated herbicide in a controlled mass ratio of the coated core to the coated herbicide of 1: 5-6, and obtaining the herbicide containing anilofos after the coating is finished.
10. The application of the anilofos-containing herbicide in rice is characterized in that the anilofos-containing herbicide and water are mixed according to a mass ratio of 1: 300 to obtain herbicide aqueous solution, and then uniformly spraying the herbicide aqueous solution to the paddy field, wherein the dosage of the herbicide aqueous solution per mu is 600 g.
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Application publication date: 20211126 |