CN114467951A - High-stability herbicide for paddy fields and preparation method thereof - Google Patents

High-stability herbicide for paddy fields and preparation method thereof Download PDF

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Publication number
CN114467951A
CN114467951A CN202210136760.XA CN202210136760A CN114467951A CN 114467951 A CN114467951 A CN 114467951A CN 202210136760 A CN202210136760 A CN 202210136760A CN 114467951 A CN114467951 A CN 114467951A
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herbicide
methyl
paddy field
stability
water
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赵殿生
李梁
付永利
李金娟
刘品志
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Huafeng Crop Technology Heilongjiang Co ltd
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Huafeng Crop Technology Heilongjiang Co ltd
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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
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
    • 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
    • A01N25/02—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 containing liquids as carriers, diluents or solvents
    • A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • 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
    • A01N25/08—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 containing solids as carriers or diluents
    • 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
    • A01N25/30—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 characterised by the surfactants
    • 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
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
    • A01N37/22—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides
    • 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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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a high-stability herbicide for a paddy field, which comprises the following components in percentage by mass: 10-15% of pyriminobac-methyl, 10-12% of pretilachlor, 4-9% of bensulfuron-methyl, 5-8% of inorganic salt, 0.2-0.5% of sodium dodecyl benzene sulfonate, 0.5-2.5% of fulvic acid, 0.5-1.5% of dispersant, 0.2-0.8% of antifreeze agent, 1-4% of hydrotalcite-like carrier, 0.4-1.2% of thickening agent, 0.5-1% of binder, 10-15% of water and the balance of oily solvent, wherein the sum of the mass percentages of the components is 100%. Also discloses a preparation method of the herbicide. The pyriminobac-methyl, the pretilachlor and the bensulfuron methyl are taken as active components, and after compounding, the drug resistance of weeds is slowed down through the synergistic effect among different active components; in addition, the stability of the herbicide is improved by adding the antifreeze agent, the thickening agent and the dispersing agent, and various performance indexes in the period of validity are ensured to meet the requirements.

Description

High-stability herbicide for paddy fields and preparation method thereof
Technical Field
The invention belongs to the technical field of agricultural medicine preparation processes, and particularly relates to a high-stability herbicide for a paddy field and a preparation method of the herbicide for the paddy field.
Background
Weeds in the rice field compete for fertilizer, light and space with rice, so that poor growth of the rice and reduction of yield and quality become one of main factors influencing rice production. In recent years, the difficulty of weed control has been increasing with the change of weed phase in rice fields. At present, the types of weeds in rice fields are nearly 40, and gramineous weeds with high occurrence frequency include barnyard grass, moleplant seeds, paspalum distichum, Leersia hexandra, weedy rice and pseudooryzae; the Cyperaceae weeds include shaped Cyperus rotundus, rhizoma Sparganii, Fluoritum (tuber and seed reproduction), Cyperus rotundus, Scirpus planiculmis, and herba Salsolae Collinae; the broad-leaved weeds comprise amaranth, eclipta prostrata, monochoria vaginalis, stranguria japonica, jie-weed, short arrowhead and alternanthera philoxeroides. Wherein the weeds such as the paddy rice, the barnyard grass, the moleplant seed, the amaranth, the carp intestine and the like become main weeds seriously harmful to the production of the paddy rice. Chemical control is time-saving and labor-saving, and is widely used due to its fast action, good effect, convenient use and no regional seasonal restriction.
At present, a common herbicide is an organic compound, for example, Chinese patent (application number: 201910349960.1, publication number: CN110024788A) discloses a bicyclosulfuron-compounded herbicide for paddy fields, which comprises bicyclosulfuron-methyl, pretilachlor, bispyribac-sodium, an auxiliary agent and a carrier, the compound herbicide is adopted, the defect that the weeding effect of the bicyclosulfuron-methyl on broadleaf weeds is poor is overcome, the herbicide is wide in weed control range and low in dosage, but the weeding speed is slow, and the weeding speed is not easy to degrade. Chinese patent (application number: 201710284574.X, publication number: CN106973918A) discloses a herbicide composition containing oxaziclomefone and propisochlor and application thereof, wherein the herbicide composition comprises oxaziclomefone and propisochlor, the control effect of the herbicide composition is superior to the activity of the herbicide composition when the herbicide composition is used alone, the generation of weed resistance is slowed down, and the herbicide composition is safe for crops; however, the herbicide has a single active component, cannot meet the requirement of weeding in the whole growth process of rice, and the active component is easy to lose effectiveness and poor in stability.
Disclosure of Invention
The invention aims to provide a high-stability herbicide for paddy fields, which has a synergistic effect on weed control and improves the weed removal efficiency.
The invention also aims to provide a preparation method of the herbicide for the paddy field with high stability.
The technical scheme adopted by the invention is that the high-stability herbicide for the paddy field comprises the following components in percentage by mass: 10-15% of pyriminobac-methyl, 10-12% of pretilachlor, 4-9% of bensulfuron-methyl, 5-8% of inorganic salt, 0.2-0.5% of sodium dodecyl benzene sulfonate, 0.5-2.5% of fulvic acid, 0.5-1.5% of dispersant, 0.2-0.8% of antifreeze agent, 1-4% of solid hydrotalcite-like carrier, 0.4-1.2% of thickening agent, 0.5-1% of binder, 10-15% of water and the balance of oily solvent, wherein the sum of the mass percentages of the components is 100%.
The present invention is also characterized in that,
the inorganic salt is one or two of magnesium sulfate, potassium nitrate, potassium chloride and ferrous sulfate.
The dispersant is any one of sodium lignosulfonate, calcium lignosulfonate and magnesium lignosulfonate; the antifreeze is any one of ethylene glycol, glycerol and propylene glycol.
The thickener is one or more of hydroxyethyl cellulose, sodium polyacrylate and polyvinylpyrrolidone.
The binder is any one of modified corn starch, polyacrylate and alkylaryl polyoxyethylene ether.
The oily solvent is one or more of dimethyl phthalate, methyl oleate and xylene.
The invention adopts another technical scheme that a preparation method of the herbicide for the high-stability paddy field is implemented according to the following steps:
step 1, preparing a solid hydrotalcite-like carrier;
step 2, mixing inorganic salt, a solid hydrotalcite-like carrier and water, uniformly stirring, adding fulvic acid, stirring, and standing for 1-2 hours to obtain a uniform water phase;
step 3, mixing pyriminobac-methyl, pretilachlor, bensulfuron-methyl, sodium dodecyl benzene sulfonate and an oily solvent, then adding a thickening agent and a binder at the temperature of 60-70 ℃ for stirring reaction, wherein the reaction temperature is 100-130 ℃, the reaction time is 30-50 min, then adding an antifreeze agent and a dispersant, and stirring for 20-35 min to obtain a uniform oil phase;
and 4, mixing and dispersing the oil phase and the water phase to obtain the high-stability herbicide for the paddy field.
The present invention is also characterized in that,
in the step 1, the method specifically comprises the following steps: adding Cu (NO)3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2Mixing the O and water uniformly to obtain a mixed salt solution; respectively dripping NaOH solution and mixed salt solution on Na2CO3Controlling the titration speed in the solution, controlling the pH value of the solution to be between 9 and 10, heating the mixed solution to 60 to 65 ℃ after the titration is finished, stirring and aging, cooling, washing the solution to be neutral by using deionized water, drying, grinding and sieving to obtain the hydrotalcite-like compound.
Cu(NO3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2The mass ratio of O to water is 1-2: 2-3: 0.04-0.12: 50-100.
The titration time is 1-2.5 h; the aging time is 5-8 h; when sieving, a sieve of 80-100 meshes is adopted.
The invention has the beneficial effects that the pyriminobac-methyl, the pretilachlor and the bensulfuron methyl are taken as the compounded active components, and the usage amount of the drug can be reduced, the drug resistance of weeds can be slowed down and the safety to crops is high through the synergistic effect among different active components after the compounding; in addition, by adding the antifreeze agent, the thickening agent and the dispersing agent, the stability of the herbicide is improved, the active components are kept for long-term storage, and various performance indexes in the period of validity are ensured to meet the requirements.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
The invention relates to a high-stability herbicide for a paddy field, which comprises the following components in percentage by mass: 10-15% of pyriminobac-methyl, 10-12% of pretilachlor, 4-9% of bensulfuron-methyl, 5-8% of inorganic salt, 0.2-0.5% of sodium dodecyl benzene sulfonate, 0.5-2.5% of fulvic acid, 0.5-1.5% of dispersant, 0.2-0.8% of antifreeze agent, 1-4% of solid hydrotalcite-like carrier, 0.4-1.2% of thickening agent, 0.5-1% of binder, 10-15% of water and the balance of oily solvent, wherein the sum of the mass percentages of the components is 100%.
The inorganic salt is one or the combination of magnesium sulfate, potassium nitrate, potassium chloride and ferrous sulfate;
the dispersant is any one of sodium lignosulfonate, calcium lignosulfonate and magnesium lignosulfonate;
the antifreeze is any one of ethylene glycol, glycerol and propylene glycol;
the thickener is one or more of hydroxyethyl cellulose, sodium polyacrylate and polyvinylpyrrolidone;
the binder is any one of modified corn starch, polyacrylate and alkylaryl polyoxyethylene ether;
the oily solvent is any one or more of dimethyl phthalate, methyl oleate and xylene;
the invention relates to a preparation method of a herbicide for a high-stability paddy field, which is implemented according to the following steps:
step 1, preparing a solid hydrotalcite-like carrier;
adding Cu (NO)3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2Mixing the O and water uniformly to obtain a mixed salt solution; respectively dripping NaOH solution and mixed salt solution on Na2CO3Controlling the titration speed in the solution, controlling the pH value of the solution to be between 9 and 10, heating the mixed solution to 60 to 65 ℃ after the titration is finished, stirring and aging, cooling, washing the solution to be neutral by using deionized water, drying, grinding and sieving to obtain the final productObtaining the hydrotalcite-like compound.
Cu(NO3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2The mass ratio of O to water is 1-2: 2-3: 0.04-0.12: 50-100 parts of;
the titration time is 1-2.5 h; the aging time is 5-8 h; when sieving, a sieve with 80-100 meshes is adopted;
step 2, mixing inorganic salt, a solid hydrotalcite-like carrier and water, uniformly stirring, adding fulvic acid, stirring, and standing for 1-2 hours to obtain a uniform water phase;
step 3, mixing pyriminobac-methyl, pretilachlor, bensulfuron-methyl, sodium dodecyl benzene sulfonate and an oily solvent, then adding a thickening agent and a binder at the temperature of 60-70 ℃ for stirring reaction, wherein the reaction temperature is 100-130 ℃, the reaction time is 30-50 min, then adding an antifreeze agent and a dispersant, and stirring for 20-35 min to obtain a uniform oil phase;
and 4, mixing and dispersing the oil phase and the water phase to obtain the high-stability herbicide for the paddy field.
According to the high-stability herbicide for the paddy field, the pyriminobac-methyl, the pretilachlor and the bensulfuron methyl are used as the compounded active components, so that the herbicide has a synergistic effect on weed control and improves the weeding effect; the fulvic acid is added to promote the growth of plants, particularly the opening degree of leaf pores of crops can be properly controlled, transpiration is reduced, the drought resistance is important, the stress resistance can be improved, the yield is increased, the quality is improved, and the fulvic acid has a synergistic effect when being mixed with the active components; the solid hydrotalcite-like carrier is added, so that the active ingredients in the herbicide can be well adsorbed, and the slow release effect is achieved; by adding the antifreeze agent, the thickening agent and the dispersing agent, the stability of the herbicide is improved, the active components are kept for long-term storage, and various performance indexes in the period of validity are ensured to meet the requirements. In addition, the herbicide has better control effect than the effect of each component when used alone, has wide weeding range, has control effect on barnyard grass, broadleaf weeds and nutgrass flatsedge, and has effect on perennial weeds, stubborn weeds and sulfonylurea-resistant weeds.
Example 1
The invention relates to a high-stability herbicide for a paddy field, which comprises the following components in percentage by mass: 10% of pyriminobac-methyl, 10% of pretilachlor, 9% of bensulfuron-methyl, 5% of inorganic salt, 0.2% of sodium dodecyl benzene sulfonate, 2% of fulvic acid, 1% of dispersant, 0.2% of antifreeze agent, 1% of solid hydrotalcite-like carrier, 0.4% of thickener, 0.5% of binder, 15% of water and the balance of oily solvent, wherein the sum of the mass percentages of the components is 100%.
The inorganic salt is magnesium sulfate; the dispersant is sodium lignosulfonate; the antifreeze agent is ethylene glycol; the thickening agent is prepared from the following components in percentage by mass of 1: 2, hydroxyethyl cellulose and sodium polyacrylate; the binder is modified corn starch;
the oily solvent is dimethyl phthalate and methyl oleate with the volume ratio of 2: 1;
a preparation method of a herbicide for a high-stability paddy field is implemented according to the following steps:
step 1, preparing a solid hydrotalcite-like carrier;
adding Cu (NO)3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2Mixing the O and water uniformly to obtain a mixed salt solution; respectively dripping NaOH solution and mixed salt solution on Na2CO3Controlling the titration speed in the solution, controlling the pH value of the solution to be 9, heating the mixed solution to 60 ℃ after the titration is finished, stirring and aging, cooling, washing the solution to be neutral by using deionized water, drying, grinding and sieving to obtain the hydrotalcite-like compound.
Cu(NO3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2The mass ratio of O to water is 1: 2: 0.04: 50;
the titration time is 2 h; the aging time is 6 h; when sieving, a 80-mesh sieve is adopted;
step 2, mixing inorganic salt, a solid hydrotalcite-like carrier and water, uniformly stirring, adding fulvic acid, stirring, and standing for 1h to obtain a uniform water phase;
step 3, mixing pyriminobac-methyl, pretilachlor, bensulfuron-methyl, sodium dodecyl benzene sulfonate and an oily solvent, then adding a thickening agent and a binder at the temperature of 60 ℃ for stirring reaction, wherein the reaction temperature is 100 ℃, the reaction time is 30min, then adding an antifreeze agent and a dispersant, and stirring for 35min to obtain a uniform oil phase;
and 4, mixing and dispersing the oil phase and the water phase to obtain the high-stability herbicide for the paddy field.
Example 2
The invention relates to a high-stability herbicide for a paddy field, which comprises the following components in percentage by mass: the composition comprises, by mass, 12% of pyriminobac-methyl, 10% of pretilachlor, 8% of bensulfuron-methyl, 6% of inorganic salt, 0.2% of sodium dodecyl benzene sulfonate, 1.5% of fulvic acid, 0.5% of dispersant, 0.5% of antifreeze agent, 2.5% of solid hydrotalcite-like carrier, 1% of thickener, 1% of binder, 12% of water and the balance of oily solvent, wherein the sum of the mass percentages of the components is 100%.
The inorganic salt is prepared from the following components in a mass ratio of 1:1, potassium nitrate and ferrous sulfate; the dispersant is calcium lignosulfonate; the antifreeze agent is glycerol; the thickening agent is hydroxyethyl cellulose adhesive which is polyacrylate;
the oily solvent is dimethyl phthalate and xylene with the volume ratio of 1: 1.5;
a preparation method of a herbicide for a high-stability paddy field is implemented according to the following steps:
step 1, preparing a solid hydrotalcite-like carrier;
adding Cu (NO)3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2Mixing the O and water uniformly to obtain a mixed salt solution; respectively dripping NaOH solution and mixed salt solution on Na2CO3And controlling the titration speed in the solution, controlling the pH value of the solution to be 9.5, heating the mixed solution to 64 ℃ after titration is completed, stirring and aging, cooling, washing the solution to be neutral by using deionized water, drying, grinding and sieving to obtain the hydrotalcite-like compound.
Cu(NO3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2The mass ratio of O to water is 1: 3: 0.08: 80;
the titration time is 2.5 h; the aging time is 8 h; when sieving, a 100-mesh sieve is adopted;
step 2, mixing inorganic salt, a solid hydrotalcite-like carrier and water, uniformly stirring, adding fulvic acid, stirring, and standing for 1-2 hours to obtain a uniform water phase;
step 3, mixing pyriminobac-methyl, pretilachlor, bensulfuron-methyl, sodium dodecyl benzene sulfonate and an oily solvent, then adding a thickening agent and a binder at the temperature of 65 ℃ for stirring reaction, wherein the reaction temperature is 120 ℃, the reaction time is 45min, then adding an antifreeze agent and a dispersant, and stirring for 25min to obtain a uniform oil phase;
and 4, mixing and dispersing the oil phase and the water phase to obtain the high-stability herbicide for the paddy field.
Example 3
The invention relates to a high-stability herbicide for a paddy field, which comprises the following components in percentage by mass: the composition comprises, by weight, 15% of pyriminobac-methyl, 11% of pretilachlor, 5% of bensulfuron-methyl, 7% of inorganic salt, 0.5% of sodium dodecyl benzene sulfonate, 2% of fulvic acid, 1.2% of a dispersant, 0.6% of an antifreeze agent, 3% of a solid hydrotalcite-like carrier, 1% of a thickener, 0.8% of a binder, 10% of water and the balance of an oily solvent; the sum of the mass percentages of the components is 100 percent.
The inorganic salt is potassium chloride; the dispersant is magnesium lignosulfonate; the antifreeze agent is propylene glycol; the thickening agent comprises sodium polyacrylate and polyvinylpyrrolidone in a mass ratio of 2: 1; the binder is alkylaryl polyoxyethylene ether;
the oily solvent is methyl oleate and xylene with the volume ratio of 2: 1;
the invention relates to a preparation method of a herbicide for a high-stability paddy field, which is implemented according to the following steps:
step 1, preparing a solid hydrotalcite-like carrier;
mixing Cu(NO3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2Mixing the O and water uniformly to obtain a mixed salt solution; respectively dripping NaOH solution and mixed salt solution on Na2CO3Controlling the titration speed in the solution, controlling the pH value of the solution to be 9, heating the mixed solution to 60-65 ℃ after titration, stirring and aging, cooling, washing the solution to be neutral by using deionized water, drying, grinding and sieving to obtain the hydrotalcite-like compound.
Cu(NO3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2The mass ratio of O to water is 1: 2: 0.1: 70;
the titration time is 1.5 h; the aging time is 6 h; when sieving, a 80-mesh sieve is adopted;
step 2, mixing inorganic salt, a solid hydrotalcite-like carrier and water, uniformly stirring, adding fulvic acid, stirring, and standing for 1h to obtain a uniform water phase;
step 3, mixing pyriminobac-methyl, pretilachlor, bensulfuron-methyl, sodium dodecyl benzene sulfonate and an oily solvent, then adding a thickening agent and a binder at the temperature of 60 ℃ for stirring reaction, wherein the reaction temperature is 100 ℃, the reaction time is 50min, then adding an antifreeze agent and a dispersant, and stirring for 35min to obtain a uniform oil phase;
and 4, mixing and dispersing the oil phase and the water phase to obtain the high-stability herbicide for the paddy field.
Example 4
The invention relates to a high-stability herbicide for a paddy field, which comprises the following components in percentage by mass: the composition comprises, by weight, 15% of pyriminobac-methyl, 12% of pretilachlor, 9% of bensulfuron-methyl, 8% of an inorganic salt, 0.2% of sodium dodecyl benzene sulfonate, 0.5% of fulvic acid, 0.5% of a dispersant, 0.2% of an antifreeze agent, 4% of a solid hydrotalcite-like carrier, 0.4% of a thickener, 0.5% of a binder, 10% of water and the balance of an oily solvent; the sum of the mass percentages of the components is 100 percent.
The inorganic salt is potassium chloride; the dispersant is magnesium lignosulfonate; the antifreeze agent is glycerol; the thickening agent is prepared from the following components in percentage by mass of 1: 1.2 of hydroxyethyl cellulose and polyvinyl pyrrolidine; the binder is modified corn starch; the oily solvent is dimethylbenzene;
the invention relates to a preparation method of a herbicide for a high-stability paddy field, which is implemented according to the following steps:
step 1, preparing a solid hydrotalcite-like carrier;
adding Cu (NO)3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2Mixing the O and water uniformly to obtain a mixed salt solution; respectively dripping NaOH solution and mixed salt solution on Na2CO3And controlling the titration speed in the solution, controlling the pH value of the solution to be 10, heating the mixed solution to 65 ℃ after titration, stirring and aging, cooling, washing the solution to be neutral by using deionized water, drying, grinding and sieving to obtain the hydrotalcite-like compound.
Cu(NO3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2The mass ratio of O to water is 2: 3: 0.04: 100;
the titration time is 2.5 h; the aging time is 8 h; when sieving, a 100-mesh sieve is adopted;
step 2, mixing inorganic salt, a solid hydrotalcite-like carrier and water, uniformly stirring, adding fulvic acid, stirring, and standing for 1h to obtain a uniform water phase;
step 3, mixing pyriminobac-methyl, pretilachlor, bensulfuron-methyl, sodium dodecyl benzene sulfonate and an oily solvent, then adding a thickening agent and a binder at the temperature of 60 ℃ for stirring reaction, wherein the reaction temperature is 130 ℃, the reaction time is 30min, then adding an antifreeze agent and a dispersant, and stirring for 20min to obtain a uniform oil phase;
and 4, mixing and dispersing the oil phase and the water phase to obtain the high-stability herbicide for the paddy field.
TABLE 1 comparison of the herbicidal Effect of the herbicides for paddy fields according to the present invention and commercially available herbicides
Figure BDA0003504693690000111
Figure BDA0003504693690000121
Comparing the weeding effects of the herbicides for paddy fields prepared in examples 1 to 4 of the present invention with those of the existing commercially available herbicides, as shown in table 1, it can be seen from the table that the weeding effects of the herbicides of the present invention and the commercially available herbicides are low and the difference between the weeding efficiencies of the herbicides is not large when the herbicides are applied for 3 days, but the weeding efficiency of the herbicides of the present invention is remarkably high for sedge, leaf-tip weeds and broadleaf weeds when the herbicides are applied for 10 days, which indicates that the herbicides of the present invention can obtain a high weeding effect due to the combined action of multiple mechanisms and a wide weeding range.

Claims (10)

1. The high-stability herbicide for the paddy field is characterized by comprising the following components in percentage by mass: 10-15% of pyriminobac-methyl, 10-12% of pretilachlor, 4-9% of bensulfuron-methyl, 5-8% of inorganic salt, 0.2-0.5% of sodium dodecyl benzene sulfonate, 0.5-2.5% of fulvic acid, 0.5-1.5% of dispersant, 0.2-0.8% of antifreeze agent, 1-4% of solid hydrotalcite-like carrier, 0.4-1.2% of thickening agent, 0.5-1% of binder, 10-15% of water and the balance of oily solvent, wherein the sum of the mass percentages of the components is 100%.
2. A highly stable herbicide for paddy field as claimed in claim 1, wherein said inorganic salt is one or two of magnesium sulfate, potassium nitrate, potassium chloride and ferrous sulfate.
3. The herbicide as claimed in claim 1, wherein the dispersant is any one of sodium lignosulfonate, calcium lignosulfonate and magnesium lignosulfonate; the antifreeze is any one of ethylene glycol, glycerol and propylene glycol.
4. A highly stable herbicide for paddy field as claimed in claim 1, wherein said thickener is any one or more of hydroxyethyl cellulose, sodium polyacrylate, polyvinylpyrrolidone.
5. A highly stable herbicide for paddy field as claimed in claim 1, wherein said binder is any one of modified corn starch, polyacrylate, alkylaryl polyoxyethylene ether.
6. The herbicide as claimed in claim 1, wherein the oily solvent is one or more selected from dimethyl phthalate, methyl oleate and xylene.
7. A preparation method of a herbicide for a high-stability paddy field is characterized by comprising the following steps:
step 1, preparing a solid hydrotalcite-like carrier;
step 2, mixing inorganic salt, a solid hydrotalcite-like carrier and water, uniformly stirring, adding fulvic acid, stirring, and standing for 1-2 hours to obtain a uniform water phase;
step 3, mixing pyriminobac-methyl, pretilachlor, bensulfuron methyl, sodium dodecyl benzene sulfonate and an oily solvent, then adding a thickening agent and a binder at the temperature of 60-70 ℃ for stirring reaction, wherein the reaction temperature is 100-130 ℃, the reaction time is 30-50 min, then adding an antifreeze agent and a dispersant, and stirring for 20-35 min to obtain a uniform oil phase;
and 4, mixing and dispersing the oil phase and the water phase to obtain the high-stability herbicide for the paddy field.
8. The method for preparing a herbicide for high stability paddy field as claimed in claim 7, wherein in the step 1, the following steps are specifically performed: mixing Cu (NO3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2Mixing the O and water uniformly to obtain a mixed salt solution; respectively dripping NaOH solution and mixed salt solution on Na2CO3Controlling the titration speed in the solution, controlling the pH value of the solution to be between 9 and 10, heating the mixed solution to 60 to 65 ℃ after the titration is finished, stirring and aging, cooling, washing the solution to be neutral by using deionized water, drying, grinding and sieving to obtain the hydrotalcite-like compound.
9. The process for preparing a herbicide for paddy field of claim 8 wherein Cu (NO) is Cu3)2·3H2O、Al(NO3)3·9H2O、Co(NO3)2·6H2The mass ratio of O to water is 1-2: 2-3: 0.04-0.12: 50-100.
10. The method for preparing a herbicide for paddy field of high stability as claimed in claim 8, wherein the titration time is 1-2.5 h; the aging time is 5-8 h; when sieving, a sieve of 80-100 meshes is adopted.
CN202210136760.XA 2022-02-15 2022-02-15 High-stability herbicide for paddy fields and preparation method thereof Pending CN114467951A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107333788A (en) * 2017-08-04 2017-11-10 安徽圣丰生化有限公司 A kind of herbicidal composition and application containing pretilachlor, KIH 6127 and pyrazosulfuron
WO2018058904A1 (en) * 2016-09-30 2018-04-05 江苏清原农冠杂草防治有限公司 Herbicide composition with enhanced effectiveness and application thereof
CN113133453A (en) * 2021-04-08 2021-07-20 中土化工（安徽）有限公司 Weeding composition containing pretilachlor, pyriminobac-methyl and bensulfuron methyl

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018058904A1 (en) * 2016-09-30 2018-04-05 江苏清原农冠杂草防治有限公司 Herbicide composition with enhanced effectiveness and application thereof
CN107333788A (en) * 2017-08-04 2017-11-10 安徽圣丰生化有限公司 A kind of herbicidal composition and application containing pretilachlor, KIH 6127 and pyrazosulfuron
CN113133453A (en) * 2021-04-08 2021-07-20 中土化工（安徽）有限公司 Weeding composition containing pretilachlor, pyriminobac-methyl and bensulfuron methyl

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