CN103518771A - Herbicide composition containing glyphosate, MCPA (2-methyl-4-chloro-phenoxyacetic acid) and carfentrazone-ethyl - Google Patents

Herbicide composition containing glyphosate, MCPA (2-methyl-4-chloro-phenoxyacetic acid) and carfentrazone-ethyl Download PDF

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CN103518771A
CN103518771A CN201310491482.0A CN201310491482A CN103518771A CN 103518771 A CN103518771 A CN 103518771A CN 201310491482 A CN201310491482 A CN 201310491482A CN 103518771 A CN103518771 A CN 103518771A
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salt
glyphosate
chlorine
azoles humulone
herbicidal composition
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赖开平
韦少平
叶一强
李致宝
张丽娟
韦茂春
易芬远
方峰
梁子宁
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GUANGXI SANJING CHEMICAL TECHNOLOGY Co Ltd
Guangxi Research Institute of Chemical Industry
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GUANGXI SANJING CHEMICAL TECHNOLOGY Co Ltd
Guangxi Research Institute of Chemical Industry
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Abstract

The invention discloses a herbicide composition containing glyphosate, MCPA (2-methyl-4-chloro-phenoxyacetic acid) and carfentrazone-ethyl. The herbicide composition is characterized in that the pesticide active ingredients of the composition are glyphosate or salts thereof, MCPA or salts or esters thereof and carfentrazone-ethyl; based on the herbicide composition, the weight percent of the pesticide active ingredients is 31.1-85%, wherein the weight percent of the glyphosate or salts thereof is 30-70%, the weight percent of the MCPA or salts or esters thereof is 1-30%, the weight percent of the carfentrazone-ethyl is 0.1-20% and the balance is non-pesticide ingredients. The dosage forms of the herbicide composition are wettable powder, water dispersible granules, soluble powder, soluble granules, aqueous solutions, emulsion in water and microemulsion. The composition has the advantages that after compounding, the herbicide composition has obvious synergistic effects, expands the weed control spectrum, increases the weed control speed, obviously reduces the usage amount and numbers of use of herbicides and can be applied to controlling imperata cylindrica, Bidens pilosa, dicranopteris dichotoma, eleusine indica, erigeron canadensis and other weeds in arable lands and non-arable lands.

Description

Herbicidal composition containing glyphosate, 2 first 4 chlorine and azoles humulone
Technical field
The invention belongs to agricultural herbicide technical field, relate to particularly a kind of herbicidal composition, particularly take the herbicidal composition that glyphosate or its salt, 2 first 4 chlorine or its salt or its ester and azoles humulone be active ingredient, this herbicidal composition can be applied to prevent and treat the weeds such as cogongrass Imperata cylindrica, bidens pilosa Bidens pilosa, iron awn winnow basket Dicranopteris dichotoma, eleusine indica Eleusine indica, Horseweed Herb Erigeron canadensis.
Technical background
Glyphosate claims that again agriculture reaches, glyphosate, english common name glyphosate, CA registration number: 1071-83-6, chemical name N-(phosphoric acid methyl) glycine.Molecular formula C 3h 8nO 5p, molecular weight 169.09.It is a kind of organic phosphates weed killer herbicide, also be the inner-adsorption conduction-type herbicide that cauline leaf absorbs, the main interior enol acetonyl shikimene phosphate synthase of object that suppresses, thereby suppress shikimene to the conversion of phenyl alanine, cruel propylhomoserin and tryptophan, make synthetic being interfered of protein cause plant dead, can be used for preventing and kill off monocotyledon weed and part broad leaved weed.Because glyphosate is real, be a kind of acid, and the solvability in water is little, so glyphosate is generally processed to solvability is larger in water sodium salt, sylvite, ammonium salt, isopropyl amine salt, dimethylamine salt, trimethyl sulfosalt etc., but weed killer herbicide characteristic is identical with glyphosate.
2 first 4 chlorine claim again virtue rice large, hundred wealthy clean, english common name: MCPA, and CA registration number: 94-74-6, chemical name is 2-methyl-4-tomatotone.Molecular formula C 9h 9cLO 3, molecular weight 200.45.For hormone herbicide, there is stronger interior suction conductivity.Its mechanism of action is suppress metabolism of nucleic acid and protein on plant top synthetic, growing point is stopped growing, not tensible of young leaflet tablet, normally carrying out of inhibited photosynthesis, be transmitted to the medicament of plant bottom, make the nucleic acid of plant stem tissue and the synthetic increase of protein, promote abnormal cell division, the tip of a root expands, and loses absorbing capacity, cause the distortion of stem stalk, deformity, screen casing stops up, and phloem destroys, and organic matter transportation is obstructed, thereby destroy the normal viability of plant, finally cause plant dead.Because 2 first 4 chlorine are real, be a kind of acid, and the solvability in water is little, so 2 first 4 chlorine are generally processed to solvability is larger in water isopropyl amine salt, dimethylamine salt, sylvite, sodium salt, ammonium salt etc., but weed killer herbicide characteristic is identical with 2 first 4 chloric acid.
Azoles humulone spirit, triazolone grass ester, the carfentrazone of going out of expressing one's gratification again, English common name carfentrazone-ethyl, chemical name is: the chloro-5-[4-of the chloro-3-{2-of ethyl-2-(difluoromethyl)-4,5-dihydro-3-methyl-5-oxygen-1H-1,2,4-triazol-1-yl]-4-fluorophenyl } ethyl propionate, its CA registration number: 128639-02-1, molecular formula C 15h 14c 12f 3n 3o 3, molecular weight 412.2, is a kind of triazolineone weed killer herbicide, it has good low temperature resistant and resistance of rainwater washing against effect, can suppress the accumulation that proporphyrinogen oxidase causes poisonous intermediate, make blade withered, dead rapidly, can be used for preventing and kill off broad leaved weed and nutgrass flatsedge.
The weed killer herbicide that Chinese patent discloses some glyphosates, 2 first 4 chlorine or azoles humulone and become with other compound combination, for example: 200910063612.4, gram Weeding water agent of making without track and 2 first 4 chlorine sodium binary builts and preparation method thereof; 201110327315.3, a kind of Herbicidal combinations containing ethoxysulfuron and 2 first 4 chlorine sodium; 201310083527.0, a kind of oil-suspending agent that dispersibles containing florasulam and the different monooctyl ester of 2 first 4 chlorine; 201010605083.9, a kind of herbicidal composition containing benzene azoles humulone, fluthiacet and 2 first 4 chlorine sodium; 201110394725.X, a kind of Wheat field weeding composition and preparation thereof; 201210318528.4, a kind of Herbicidal combinations containing hexazinone and phenoxy carboxylic acid; 200910034319.5,200910034319.5, azoles humulone cyhalofop-butyl dichloro quinolinic acid complex weedicide; 201110157619.X, a kind of Herbicidal combinations containing azoles humulone and Brominal; 201110158872.7, a kind of Herbicidal combinations containing azoles humulone and Flumetsulam; 201110160825.6, a kind of Herbicidal combinations containing azoles humulone; 200810173590.2, a kind of combinations of herbicides; 200910243683.2, herbicidal composition; 200910222125.8, effectiveness-enhanced glyphosate weeding combination etc.Shown that the weed killer herbicide that glyphosate, 2 first 4 chlorine or azoles humulone and they become with other compound combination has good herbicide effect and is applied in agricultural.In the prior art, patent documentation CN101784194A discloses glyphosate and the composite Herbicidal combinations of MCPA, although also mentioned when using together with other weed killer herbicide, can be by described composition and other one or more weed killer herbicide preparations, and enumerate out hundreds of kind weed killer herbicide, but it also reckons without compatibility after composite and the antagonism of appearance, and its synergy, expand the DeGrain of herbicide spectrum, herbicidal effect needs further to be improved.In addition, patent documentation CN102657218A discloses 2 first 4 chlorine isopropyl amine salts and the composite composition of glyphosate isopropyl amine salt, and it is complementary mentioning the two, but itself and not mentioned the two and azoles humulone is composite, also and reckon without the mixed ratio etc. of the antagonism of compatibility, synergy mixed ratio and appearance after ternary built.Patent documentation CN102771508A discloses the combination of glyphosate isopropyl amine salt, 2 first 4 chlorine sodium salts and fluroxypyr, and equally also not mentioned azoles humulone is composite.In sum, with research and the application of glyphosate, 2 first 4 chlorine and these 3 kinds of mixture of herbicides of azoles humulone, have no open source literature report at present.
Cogongrass, bidens pilosa, iron awn winnow basket, eleusine indica, Horseweed Herb etc. are weeds common in various crop field, forest land and uncultivated area, use separately glyphosate, 2 first 4 chlorine or azoles humulone effectively not to prevent and kill off these weeds, want to obtain desirable preventive effect and can only strengthen formulation rate simultaneously.Yet by strengthen dosage reach preventive effect will certainly increase the weight of weed killer herbicide residual, cause the poisoning of crop increased to cost accounting simultaneously.And, use separately in actual applications the weeding speed of glyphosate slow, and be subject to the impact of the bad climates such as low temperature, rainfall and limited the performance of drug effect.In addition, use for a long time single weed killer herbicide to tend to cause the generation of herbicide resistance, and then reduce the preventive effect of weed killer herbicide.
Different weed killer herbicides carries out the composite herbicide that can expand and composes, and adopt the mixture of herbicides that the mode of action is different and demonstrate synergistic effect, be mixture to the inhibitory action of weed growth the desired value higher than each component independent role in mixture, make weeds be difficult to eliminate the impact of different weed killer herbicides on its metabolic pathway, and then delay the generation of herbicide resistance, being the target of exploitation mixture of herbicides preparation, is also to alleviate environmental pollution, reduces the effective means of herbicide residue.We are through screening, discovery is by glyphosate, 2 first 4 chlorine and azoles humulone is composite can realize above-mentioned advantage, herbicide combination product containing mentioned component also has broad weed-killing spectrum, the fireballing feature of herbicide, thereby there is the advantages such as impact that drug effect is not subject to the bad climates such as low temperature, rainfall, be the fine herbicide of the weeds chemical controls such as cogongrass, bidens pilosa, iron awn winnow basket, eleusine indica, Horseweed Herb.
Summary of the invention
The invention provides a kind of glyphosate, 2 first 4 chlorine and the composite weed killer herbicide of azoles humulone, between this weed killer herbicide active ingredient, there is synergistic function, can also widen herbicide spectrum, improve herbicide speed, form efficient a, wide spectrum, weed killer herbicide kind that use cost is low.This weed killer herbicide not only can be prevented and kill off all weeds that glyphosate, 2 first 4 chlorine and azoles humulone single dose can be prevented and kill off, the weeds such as cogongrass that independent use glyphosate, 2 first 4 chlorine or azoles humulone can not finely prevent and kill off, bidens pilosa, iron awn winnow basket, eleusine indica, Horseweed Herb be can also prevent and kill off, forest land, the disposable chemical weed control of uncultivated area realized.
Technical scheme of the present invention is as follows:
2, containing the herbicidal composition of glyphosate, 2 first 4 chlorine and azoles humulone, it is characterized in that: this herbicidal composition is comprised of pesticide active ingredient and non-farm chemical ingredients, the weight percentage of pesticide active ingredient is 31.1%~85%, and surplus is non-farm chemical ingredients; Described pesticide active ingredient is glyphosate or its salt, 2 first 4 chlorine or its salt or its ester and azoles humulone; Wherein:
The parts by weight of glyphosate or its salt are: 30~70 parts;
The parts by weight of 2 first 4 chlorine or its salt or its ester: 1~30 part;
The parts by weight of azoles humulone are: 0.1~20 part.
Described glyphosate is N-(phosphonomethyl) glycine, and its salt has organic salt and mineral salt, and its organic salt selects white ethanolamine salt, triisopropanolamine salt, triethylamine salt, isopropyl amine salt, dimethylamine salt, and its mineral salt are sylvite, sodium salt, ammonium salt.
2 described first 4 chlorine are 2-methyl-4-tomatotone, and its salt has organic salt and mineral salt, and its organic salt is selected from isopropyl amine salt, dimethylamine salt, and its mineral salt are sylvite, sodium salt, ammonium salt, and its ester is ethyl butyrate, sulfo-ethyl ester, second thioesters, different monooctyl ester.
Described composition comprises wetting powder, water dispersible granules, solvable fecula agent, soluble granula, aqua, aqueous emulsion, the microemulsion of being made by pesticide active ingredient and non-farm chemical ingredients.
Described non-farm chemical ingredients refers to one or more in filler in pesticidal preparations meaning, adhesive, surfactant, defoamer, antifreezing agent, solvent, thickener, cosolvent.The filler that is applicable to preparation herbicidal composition of the present invention is any filler that is generally used for preparing weed killer herbicide.Such as ammonium sulfate, diatomite, bentonite, kaolin, attapulgite, clay, white carbon, precipitated calcium carbonate and talcum powder etc.Meanwhile, the mixture of different fillers is also suitable for.
The adhesive that is applicable to preparation herbicidal composition of the present invention is any adhesive that is generally used for preparing weed killer herbicide.Such as at least one of cellulose and modifier, starch and modifier thereof, gelatin, polyvinyl alcohol, gum Arabic and sodium silicate etc.
The surfactant that is applicable to preparation herbicidal composition of the present invention is any surfactant that is generally used for preparing weed killer herbicide.Sodium lignin sulfonate for example, sodium methylene bis-naphthalene sulfonate, calcium lignosulfonate, polyethers ichthyodin, fatty alcohol-polyoxyethylene ether sodium sulfonate, alkanolamide sodium sulfonate of ethoxylated, calcium dodecyl benzene sulfonate, alkyl poly glucoside, lauryl sodium sulfate, lauryl alcohol sodium sulphate, dodecyl sulphate calcium, neopelex, sodium butylnaphthalenesulfonate, alkylaryl polyoxyethylene polyoxypropylene ether, phenethyl phenol polyethenoxy ether, dibenzyl xenyl APEO, at least one of fatty alcohol-polyoxyethylene ether and alkylphenol polyoxyethylene etc.
The defoamer that is applicable to preparation herbicidal composition of the present invention is any defoamer that is generally used for preparing weed killer herbicide.Such as at least one of isooctanol, silicone emulsion and polypropylene glycerol aether etc.
The antifreezing agent that is applicable to preparation herbicidal composition of the present invention is any antifreezing agent that is generally used for preparing weed killer herbicide.Such as at least one of ethylene glycol, propane diols, glycerine, sorbierite and urea etc.
The solvent that is applicable to preparation herbicidal composition of the present invention is any solvent that is generally used for preparing weed killer herbicide.Such as at least one of toluene, dimethylbenzene, acetone, cyclohexanone, methyl alcohol, ethanol, carrene, chloroform and purified water etc.
The thickener that is applicable to preparation herbicidal composition of the present invention is any thickener that is generally used for preparing weed killer herbicide.Such as at least one of polyvinyl alcohol, methyl hydroxyethylcellulose, ethylhydroxyethylcellulose, xanthans and alumina silicate etc.
The cosolvent that is applicable to preparation herbicidal composition of the present invention is any cosolvent that is generally used for preparing weed killer herbicide.Such as at least one of oleic acid glyceryl ester, ethylene glycol, polyethylene glycol, propane diols, glycerine and n-butanol etc.
Described herbicidal composition is for the annual and perennial weeds of preventing and kill off forest land and uncultivated area, such as can prevent and kill off plough and uncultivated area in the weeds such as cogongrass, bidens pilosa, iron awn winnow basket, eleusine indica, Horseweed Herb.
The present invention has following remarkable result:
(1) the present invention is increased the activity of mixture after composite, has obvious synergistic effect, has significantly reduced usage amount and the access times of weed killer herbicide, reduces costs.
(2) the present invention has expanded herbicide spectrum after composite, can prevent and treat multiple weeds simultaneously.
(3) the present invention makes weeds be difficult to eliminate the impact of the different weed killer herbicide of mechanism of action on its metabolic pathway after composite, delays in weeds that pesticide resistance is individual to be produced.
(4) herbicidal composition provided by the present invention has improved weeding speed, has reduced the impacts of bad climate on drug effect such as low temperature, rainfall.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, the present invention describes with following specific embodiment, but the present invention is limited to absolutely not these examples.The following stated is only the good embodiment of the present invention, only for explaining the present invention, can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that all any modifications of making within the spirit and principles in the present invention, be equal to replacement and improvement etc., within all should being included in protection scope of the present invention.
If do not specialize, the conventional means that in embodiment, technological means used is well known to those skilled in the art.
Embodiment 1 (32.1% glyphosate 2 first 4 chlorazol humulone wetting powders):
Percentage composition by weight, glyphosate potassium (in glyphosate) 30%, 2 first 4 chlorine sodium (take 2 first 4 chlorine) 2%, azoles humulone 0.1%, dodecyl sulphate calcium 3%, sodium lignin sulfonate 7%, sodium methylene bis-naphthalene sulfonate 2%, surplus are precipitated calcium carbonate.
According to conventional pesticide preparation processing technology, according to above-mentioned formula, glyphosate, 2 first 4 chlorine, azoles humulone, dodecyl sulphate calcium, sodium lignin sulfonate, sodium methylene bis-naphthalene sulfonate, precipitated calcium carbonate are added successively in batch mixer and fully mixed, material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, obtains active constituent content and be 32.1% composite wettable powder.
Embodiment 2 (65% glyphosate 2 first 4 chlorazol humulone wetting powders):
Percentage composition by weight, ammonium glyphosate (in glyphosate) 45%, 2 first 4 chlorine sylvite (take 2 first 4 chlorine) 10%, azoles humulone 15%, lauryl sodium sulfate 2%, sodium lignin sulfonate 3%, lauryl alcohol sodium sulphate 1%, surplus are precipitated calcium carbonate.
According to above-mentioned formula, glyphosate, 2 first 4 chlorine, azoles humulone, lauryl sodium sulfate, sodium lignin sulfonate, lauryl alcohol sodium sulphate, precipitated calcium carbonate are added successively in batch mixer and fully mixed, material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, obtains active constituent content and be 65% composite wettable powder.
Embodiment 3 (66% glyphosate 2 first 4 chlorazol humulone wetting powders):
Percentage composition by weight, sodium glyphosate (in glyphosate) 35.8%, 2 first 4 chlorine sodium salts (take 2 first 4 chlorine) 30%, azoles humulone 0.2%, lauryl sodium sulfate 5%, calcium lignosulfonate 3%, sodium butylnaphthalenesulfonate 2%, surplus are kaolin.
According to conventional pesticide preparation processing technology, according to above-mentioned formula, glyphosate, 2 first 4 chlorine, azoles humulone, lauryl sodium sulfate, sodium lignin sulfonate, sodium butylnaphthalenesulfonate, kaolin are added successively in batch mixer and fully mixed, material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, obtains active constituent content and be 66% composite wettable powder.
Embodiment 4 (72% glyphosate 2 first 4 chlorazol humulone wetting powders):
Percentage composition by weight, ammonium glyphosate (in glyphosate) 52%, 2 first 4 chlorine sodium salts (in 2 first 4 chlorine) 15%, azoles humulone 5%, fatty alcohol-polyoxyethylene ether sodium sulfonate 3%, calcium lignosulfonate 2%, surplus is attapulgite.
According to above-mentioned formula by glyphosate, 2 first 4 chlorine, azoles humulone, fatty alcohol-polyoxyethylene ether sodium sulfonate, calcium lignosulfonate, attapulgite adds successively in batch mixer and fully mixes, material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, obtains active constituent content and be 72% composite wettable powder.
Embodiment 5 (73% glyphosate 2 first 4 chlorazol humulone wetting powders):
Percentage composition by weight, sodium glyphosate (in glyphosate) 38%, 2 first 4 chlorine sodium salts (take 2 first 4 chlorine) 30%, azoles humulone 5%, polyethers ichthyodin 2%, neopelex 6%, surplus are white carbon.
According to above-mentioned formula, glyphosate, 2 first 4 chlorine, azoles humulone, polyethers ichthyodin, neopelex, white carbon are added successively in batch mixer and fully mixed, material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, obtains active constituent content and be 73% composite wettable powder.
Embodiment 6 (77% glyphosate 2 first 4 chlorazol humulone wetting powders):
Percentage composition by weight, glyphosate glyphosate potassium (in glyphosate) 32%, 2 first 4 chlorine sodium salts (take 2 first 4 chlorine) 25%, azoles humulone 20%, polyethers ichthyodin 2%, neopelex 4%, surplus are white carbon.
According to above-mentioned formula by glyphosate, 2 first 4 chlorine, azoles humulone,, polyethers ichthyodin, neopelex, white carbon add successively in batch mixer and fully mix, material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, obtains active constituent content and be 77% composite wettable powder.
Embodiment 7 (80% glyphosate 2 first 4 chlorazol humulone wetting powders):
Percentage composition by weight, ammonium glyphosate (in glyphosate) 68%, 2 first 4 chlorine sodium salts (in 2 first 4 chlorine) 6%, azoles humulone 6%, fatty alcohol-polyoxyethylene ether sodium sulfonate 1%, neopelex 2%, surplus is attapulgite.
According to above-mentioned formula by glyphosate, 2 first 4 chlorine, azoles humulone, fatty alcohol-polyoxyethylene ether sodium sulfonate, neopelex, attapulgite adds successively in batch mixer and fully mixes, material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, obtains active constituent content and be 80% composite wettable powder.
Embodiment 8 (42% glyphosate 2 first 4 chlorazol humulone water dispersible granules):
Percentage composition by weight, sodium glyphosate (in glyphosate) 35%, 2 first 4 chlorine sylvite (in 2 first 4 chlorine) 5%, azoles humulone 2%, calcium lignosulfonate 2%, alkanolamide sodium sulfonate of ethoxylated 2%, fatty alcohol-polyoxyethylene ether sodium sulfonate 1%, gelatin 6%, surplus is bentonite.
First bentonite and azoles humulone are added in batch mixer and mixed, again glyphosate, 2 first 4 chlorine, calcium lignosulfonate, alkanolamide sodium sulfonate of ethoxylated, fatty alcohol-polyoxyethylene ether sodium sulfonate are added successively in batch mixer and fully mix, material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, again the material after pulverizing is added in batch mixer and mixed 1 hour, form certain density premix.Gelatin and appropriate water-soluble solution, by premix with together with gelatin after dissolving, add that in Squeezinggranulator, to make content be 42% composition water dispersible granules, after drying, cooling, screening, check, carry out finished product packing.
Embodiment 9 (70% glyphosate 2 first 4 chlorazol humulone water dispersible granules):
Percentage composition by weight, sodium glyphosate (in glyphosate) 40%, 2 first 4 chlorine sodium salts (in 2 first 4 chlorine) 20%, azoles humulone 20%, alkanolamide sodium sulfonate of ethoxylated 3%, sodium lignin sulfonate 2%, gum Arabic 5%, ammonium sulfate 4%, surplus is talcum powder.
First ammonium sulfate, talcum powder and azoles humulone are added in batch mixer and mixed, again glyphosate, 2 first 4 chlorine, alkanolamide sodium sulfonate of ethoxylated, sodium lignin sulfonate are added successively in batch mixer and fully mix, material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, again the material after pulverizing is added in batch mixer and mixed 1 hour, form certain density premix.Gum Arabic and appropriate water-soluble solution, by premix with together with gum Arabic after dissolving, add that in Squeezinggranulator, to make content be 70% composition water dispersible granules, after drying, cooling, screening, check, carry out finished product packing.
Embodiment 10 (60% glyphosate 2 first 4 chlorazol humulone water dispersible granules):
Percentage composition by weight, ammonium glyphosate (in glyphosate) 30%, 2 first 4 chlorine sodium salts (in 2 first 4 chlorine) 25%, azoles humulone 5%, calcium lignosulfonate 2%, polyethers ichthyodin 3%, sodium silicate 5%, surplus is diatomite.
First diatomite and azoles humulone are added in batch mixer and mixed, again glyphosate, 2 first 4 chlorine, calcium lignosulfonate, polyethers ichthyodin are added successively in batch mixer and fully mix, material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, again the material after pulverizing is added in batch mixer and mixed 1 hour, form certain density premix.Sodium silicate is dissolved, premix is added together with after sodium silicate after dissolving in Squeezinggranulator, to make content be 60% composition water dispersible granules, after drying, cooling, screening, check, carry out finished product packing.
Embodiment 11 (80% glyphosate 2 first 4 chlorazol humulone water dispersible granules):
Percentage composition by weight, ammonium glyphosate (in glyphosate) 60%, 2 first 4 chlorine sodium salts (in 2 first 4 chlorine) 10%, azoles humulone 10%, calcium lignosulfonate 1%, polyethers ichthyodin 3%, carboxymethyl cellulose 6%, surplus is diatomite.
First diatomite and azoles humulone are added in batch mixer and mixed, again glyphosate, 2 first 4 chlorine, calcium lignosulfonate, polyethers ichthyodin are added successively in batch mixer and fully mix, material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, again the material after pulverizing is added in batch mixer and mixed 1 hour, form certain density premix.Appropriate water-soluble solution for carboxymethyl cellulose, premix is added together with after carboxymethyl cellulose after dissolving in Squeezinggranulator, to make content be 80% composition water dispersible granules, after drying, cooling, screening, check, carry out finished product packing.
Embodiment 12 (32.1% glyphosate 2 first 4 chlorazol humulone aquas):
Percentage composition by weight, ammonium glyphosate (in glyphosate) 30%, 2 first 4 oronain salt (in 2 first 4 chlorine) 2%, azoles humulone 0.1%, calcium dodecyl benzene sulfonate 2%, alkylphenol polyoxyethylene 6%, ethanol 5%, n-butanol 0.5%, surplus is purified water.
According to conventional pesticide preparation processing technology, by formula ratio, add successively glyphosate, 2 first 4 chlorine, azoles humulone, calcium dodecyl benzene sulfonate, alkylphenol polyoxyethylene, ethanol, n-butanol and water, in stirred tank, be uniformly mixed, through detecting, packing, make 32.1% glyphosate 2 first 4 chlorazol humulone aquas.
Embodiment 13 (35.5% glyphosate 2 first 4 chlorazol humulone aquas):
Percentage composition by weight, glyphosate dimethylamine salt (in glyphosate) 30%, 2 first 4 chlorine isopropyl amine salts (in 2 first 4 chlorine) 5%, azoles humulone 0.5%, calcium dodecyl benzene sulfonate 4%, fatty alcohol-polyoxyethylene ether 4%, methyl alcohol 5%, surplus is purified water.
According to conventional pesticide preparation processing technology, by formula ratio, add successively glyphosate, 2 first 4 chlorine, azoles humulone, calcium dodecyl benzene sulfonate, fatty alcohol-polyoxyethylene ether, first alcohol and water, in stirred tank, be uniformly mixed, through detecting, packing, make 35.5% glyphosate 2 first 4 chlorazol humulone aquas.
Embodiment 14 (36% glyphosate 2 first 4 chlorazol humulone aquas):
Percentage composition by weight, glyphosate isopropyl amine salt (in glyphosate) 30%, 2 first 4 chlorine dimethylamine salts (in 2 first 4 chlorine) 5%, azoles humulone 1%, calcium dodecyl benzene sulfonate 3%, alkyl poly glucoside 5%, methyl alcohol 5%, ethylene glycol 0.5%, surplus is purified water.
According to conventional pesticide preparation processing technology, by formula ratio, add successively glyphosate, 2 first 4 chlorine, azoles humulone, calcium dodecyl benzene sulfonate, alkyl poly glucoside, methyl alcohol, ethylene glycol and water, in stirred tank, be uniformly mixed, through detecting, packing, make 36% glyphosate 2 first 4 chlorazol humulone aquas.
Embodiment 15 (35% glyphosate 2 first 4 chlorazol humulone aqueous emulsions):
Percentage composition by weight, glyphosate ethanolamine salt (in glyphosate) 30%, the different monooctyl ester of 2 first 4 chlorine (in 2 first 4 chlorine) 4%, azoles humulone 1%, calcium dodecyl benzene sulfonate 4%, phenethyl phenol polyethenoxy ether 4%, toluene 8%, silicone emulsion 0.6%, polypropylene glycerol aether 0.4%, glycerine 1%, methyl hydroxyethylcellulose 0.2%, xanthans 0.3%, surplus is purified water.
By azoles humulone, calcium dodecyl benzene sulfonate, phenethyl phenol polyethenoxy ether, toluene abundant stirring and dissolving in container, be mixed with the oil phase of homogeneous.Glyphosate, 2 first 4 chlorine, silicone emulsion, polypropylene glycerol aether, glycerine, methyl hydroxyethylcellulose, xanthans and water are uniformly mixed in container, are mixed with the water of homogeneous.Under normal temperature and homogenizer (rotating speed is 4000~5000r/min) high speed shear condition, oil phase is slowly added in the water of formula ratio, after adding, continue to maintain above-mentioned rotating speed cutting 40min, obtain active constituent content and be 35% composition aqueous emulsion.
Embodiment 16 (36% glyphosate 2 first 4 chlorazol humulone aqueous emulsions):
Percentage composition by weight, glyphosate triisopropanolamine salt (in glyphosate) 30%, Thistrol ethyl ester (in 2 first 4 chlorine) 3%, azoles humulone 3%, calcium dodecyl benzene sulfonate 4%, dibenzyl xenyl APEO 4%, dimethylbenzene 8%, silicone emulsion 0.6%, isooctanol 0.1%, glycerine 0.5%, sorbierite 0.5%, ethylhydroxyethylcellulose 0.1%, polyvinyl alcohol 0.2%, alumina silicate 0.1%, surplus is purified water.
By azoles humulone, calcium dodecyl benzene sulfonate, dibenzyl xenyl APEO, dimethylbenzene abundant stirring and dissolving in container, be mixed with the oil phase of homogeneous.Glyphosate, 2 first 4 chlorine, silicone emulsion, isooctanol, glycerine, sorbierite, ethylhydroxyethylcellulose, polyvinyl alcohol, alumina silicate and water are uniformly mixed in container, are mixed with the water of homogeneous.Under normal temperature and homogenizer (rotating speed is 4000~5000r/min) high speed shear condition, oil phase is slowly added in the water of formula ratio, after adding, continue to maintain above-mentioned rotating speed cutting 40min, obtain active constituent content and be 36% composition aqueous emulsion.Embodiment 17 (33% glyphosate 2 first 4 chlorazol humulone microemulsions):
Percentage composition by weight, glyphosate triethylamine salt (in glyphosate) 30%, 2 first 4 chlorine sulfo-ethyl esters (in 2 first 4 chlorine) 2.5%, azoles humulone 0.5%, dimethylbenzene 1%, methyl alcohol 5%, calcium dodecyl benzene sulfonate 1%, alkyl poly glucoside 2%, dibenzyl xenyl APEO 2%, propane diols 1%, polyethylene glycol 0.5%, n-butanol 1.5%, surplus is purified water.
By azoles humulone, dimethylbenzene, methyl alcohol, calcium dodecyl benzene sulfonate, alkyl poly glucoside, dibenzyl xenyl APEO, propane diols, polyethylene glycol, n-butanol abundant stirring and dissolving in container, be mixed with the oil phase of homogeneous.Glyphosate, 2 first 4 chlorine and water are uniformly mixed in container, are mixed with the water of homogeneous.After oil phase is slowly added in the water of formula ratio, mix and blend 1 hour, obtains active constituent content and is 33% composite microemulsion.
Embodiment 18 (35% glyphosate 2 first 4 chlorazol humulone microemulsions):
Percentage composition by weight, ammonium glyphosate (in glyphosate) 32%, 2 first 4 chloroethene thioesters (in 2 first 4 chlorine) 1%, azoles humulone 2%, chloroform 2%, ethanol 5%, calcium dodecyl benzene sulfonate 1%, fatty alcohol-polyoxyethylene ether 1%, alkylphenol polyoxyethylene 2%, ethylene glycol 1%, propane diols 0.5%, oleic acid glyceryl ester 0.5%, surplus is purified water.
By azoles humulone, chloroform, ethanol, calcium dodecyl benzene sulfonate, fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene, ethylene glycol, propane diols, oleic acid glyceryl ester abundant stirring and dissolving in container, be mixed with the oil phase of homogeneous.2 first 4 chlorine, glyphosate and water are uniformly mixed in container, are mixed with the water of homogeneous.After oil phase is slowly added in the water of formula ratio, mix and blend 1.5 hours, obtains active constituent content and is 35% composite microemulsion.
Embodiment 19 (37% glyphosate 2 first 4 chlorazol humulone soluble powders):
Percentage composition by weight, ammonium glyphosate (in glyphosate) 35%, 2 first 4 chlorine sodium salts (in 2 first 4 chlorine) 1.8%, azoles humulone 0.2%, methyl alcohol 4%, calcium dodecyl benzene sulfonate 0.3%, alkylphenol polyoxyethylene 0.2%, alkyl poly glucoside 4.5%, surplus is ammonium sulfate.
By azoles humulone, methyl alcohol, calcium dodecyl benzene sulfonate, alkylphenol polyoxyethylene abundant stirring and dissolving in container, be mixed with homogeneous liquid phase.Glyphosate, 2 first 4 chlorine, alkyl poly glucoside and ammonium sulfate are added successively in batch mixer fully and mixed, and the material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders, is mixed with the solid phase of homogeneous.After liquid phase is slowly added in the solid phase of formula ratio, mix and blend 1 hour, obtains active constituent content and is 37% composition soluble powder.
Embodiment 20 (55.8% glyphosate 2 first 4 chlorazol humulone soluble granulas):
Percentage composition by weight, ammonium glyphosate (in glyphosate) 30%, 2 first 4 chlorine sylvite (in 2 first 4 chlorine) 25%, azoles humulone 0.8%, ethanol 4%, calcium dodecyl benzene sulfonate 0.5%, alkylphenol polyoxyethylene 0.5%, sodium lignin sulfonate 4%, alkanolamide sodium sulfonate of ethoxylated 2%, starch sulfate 8%, surplus is sodium sulphate.
By azoles humulone, ethanol, calcium dodecyl benzene sulfonate, alkylphenol polyoxyethylene abundant stirring and dissolving in container, be mixed with homogeneous liquid phase.Glyphosate, 2 first 4 chlorine, sodium lignin sulfonate, alkanolamide sodium sulfonate of ethoxylated, sodium sulphate are added successively in batch mixer fully and mixed, and the material after mixing adds and in airslide disintegrating mill, is crushed to fineness and reaches 325 orders.After liquid phase is slowly added in the solid phase of formula ratio and is mixed 1 hour, form certain density premix.Starch sulfate is mixed to fully gelatinization at 80 ℃ by weight 1:2 with water.Premix is made to soluble granula with adding together with starch sulfate after gelatinization in Squeezinggranulator, after drying, cooling, screening, check, carry out finished product packing.
Embodiment 21 (glyphosate, 2 first 4 chlorine and the Toxicity Determination of triazolineone mixture of herbicides to bidens pilosa)
By indoor biometrics, define the synergy situation after glyphosate, 2 first 4 chlorine and triazolineone mixture of herbicides, wherein the kind of triazolineone weed killer herbicide has 1. azoles humulone; 2. amicarbazone (amicarbazone); 3. procarbazone (propoxycarbazone); 4. sulfentrazone (sulfentrazone); 5. azafenidin (azafenidin).
Above-described embodiment is through overtesting, and the weeds such as the cogongrass in preventing and kill off arable land and uncultivated area, bidens pilosa, iron awn winnow basket, eleusine indica, Horseweed Herb all have higher effect.
Using bidens pilosa as the raw object of surveying, select and do not use weed killer herbicide soil, pH6.8, by soil is air-dry sieve after, pack diameter 32cm into, in the plastic flowerpot (having pallet) of dark 20cm, every basin plant 15 strains healthy and strong consistent 2 the leaf phase seedling for test.Adopt cauline leaf spray-on process, with reference to NY/T1155.4-2006 farm-chemical indoor determination test rule weed killer herbicide the 4th part: active determination test cauline leaf spray-on process is tested, every processing repeats for 4 times, and every repetition 15 strain plants are not established and are treated to blank containing medicament.Data statistical analysis method is with reference to NY/T1155.7-2006 farm-chemical indoor determination test rule weed killer herbicide the 7th part: the Colby method of the synergy being mixed in measuring, calculates the combinatorial theory survival rate E that is respectively mixed 0poor (the E of value, actual survival rate E value and theoretical value and real value 0-E).E 0-E > 10% is synergistic effect; E 0-E <-10% is antagonism; E 0-E value is addition between ± 10%.
The results are shown in Table 1.
Table 1 glyphosate, 2 first 4 chlorine and the Toxicity Determination of triazolineone mixture of herbicides to bidens pilosa
Figure BSA0000096393210000111
Glyphosate, 2 first 4 chlorine and each proportioning of triazolineone herbicide combination product are to equal >-10% of the co-toxicity coefficient of bidens pilosa as seen from the table, there is not antagonism, illustrate that glyphosate, 2 first 4 chlorine and triazolineone mixture of herbicides are feasible.Under same dose and ratio, when glyphosate, 2 first 4 chlorine and azoles humulone are composite, each proportioning of mixture is to bidens pilosa survival rate difference (E 0-E) higher than other combination, illustrate that glyphosate, 2 first 4 chlorine and the synergistic effect of azoles humulone are apparently higher than glyphosate, 2 first 4 chlorine and other triazolineone combinations of herbicides.
Embodiment 22 (the composite Toxicity Determination to bidens pilosa of glyphosate, hormone herbicide and azoles humulone)
On the basis of embodiment 21, by indoor biometrics, define glyphosate, hormone herbicide and the azoles humulone synergy situation after composite, wherein the kind of hormone herbicide has 1. 2 first 4 chlorine; 2. 2,4-drip (2,4-D); 3. dicamba (dicamba); 4. dichloro quinolinic acid (quinclorac); 5. benazolin (benazolinethyl).Using bidens pilosa equally as the raw object of surveying, and test method and synegism evaluation, with embodiment 21, the results are shown in Table 2.
Table 2 glyphosate, 2 first 4 chlorine and the composite Toxicity Determination to bidens pilosa of hormone herbicide
Glyphosate, hormone herbicide and azoles humulone are composite as seen from the table, each proportioning of mixture is to equal >-10% of the co-toxicity coefficient of bidens pilosa, there is not antagonism, illustrate glyphosate, hormone herbicide and azoles humulone composite be feasible.Compare glyphosate, azoles humulone and the 2 first 4 chlorine survival rate difference (E of each proportioning of mixture to bidens pilosa when composite with other combination 0-E) higher than other, process, illustrate that the composite synergistic effect of glyphosate, azoles humulone and 2 first 4 chlorine is apparently higher than glyphosate, azoles humulone and the combination of other hormone herbicide.
Embodiment 23 (glyphosate and other broad spectrum weeding agent and 2 first 4 chlorine, the composite Toxicity Determination to bidens pilosa of azoles humulone)
By indoor biometrics, define glyphosate and other broad spectrum weeding agent and 2 first 4 chlorine, the azoles humulone synergy situation after composite, the kind of broad spectrum weeding agent has 1. glyphosate; 2. careless ammonium phosphine (glufosinate ammonium); 3. paraquat (paraquat); 4. hexazinone (hexazinone); 5. diuron (diuron); 6. Brominal (bromoxynil); 7. anilofos (dithiopyr); ; 8. ametryn (ametryn).Using bidens pilosa equally as the raw object of surveying, and test method and synegism evaluation, with embodiment 21, the results are shown in Table 3.
The agent of table 3 broad spectrum weeding, azoles humulone and the composite Toxicity Determination to bidens pilosa of 2 first 4 chlorine
Figure BSA0000096393210000131
When glyphosate and 2 first 4 chlorine, azoles humulone are composite as seen from the table, each proportioning of mixture is to bidens pilosa survival rate difference (E 0-E), higher than the combination of other broad spectrum weeding agent and 2 first 4 chlorine and azoles humulone, illustrate that glyphosate, 2 first 4 chlorine and the effect of azoles humulone compound synergic are the most obvious.
Embodiment 24 (containing glyphosate, 2 first 4 chlorine and the Toxicity Determination of azoles humulone herbicidal composition to weeds)
By indoor biometrics, define the composite rear synergy situation to multiple weeds of glyphosate, 2 first 4 chlorine and azoles humulone.According to the effective object of glyphosate, 2 first 4 chlorine and azoles humulone and product purposes from now on, using cogongrass, Horseweed Herb, iron awn winnow basket as the raw object of surveying, test method and synegism evaluation, with embodiment 21, the results are shown in Table 4.
Table 4 is containing glyphosate, 2 first 4 chlorine and the Toxicity Determination of azoles humulone herbicidal composition to weeds
The composite proportioning of respectively testing of glyphosate, 2 first 4 chlorine and azoles humulone all shows notable synergistic effect to cogongrass, Horseweed Herb, iron awn winnow basket as seen from the table, i.e. theoretical survival rate E 0the difference of value and actual survival rate E value is all greater than 10%.Therefore glyphosate, 2 first 4 chlorine and azoles humulone are composite is feasible.
Embodiment 25 (containing glyphosate, 2 first 4 chlorine and the field medicine effect test of azoles humulone herbicidal composition to weeds)
In August, 2012, in forest farm, east gate, Chongzuo City, Guangxi, prepared product is carried out to field medicine effect test, field advantage weeds are cogongrass, bidens pilosa, iron awn winnow basket, Horseweed Herb.Test medicine is the prepared product of embodiment 1~20, and contrast medicament is 30% gyphosate solution, 56%2 first 4 chlorine soluble powder of sodium agent, 40% azoles humulone water dispersible granules.The working concentration of test medicine, 30% gyphosate solution, 56%2 first 4 chlorine soluble powder of sodium agent is 1680g a.i./hm 2, the working concentration of 40% azoles humulone water dispersible granules is 36g a.i./hm 2(by Products Show dosage).Test and statistical method are with reference to GB-T17980.51-2000, and routine observation record, adopts absolute-value scheme to investigate, and the fresh weight preventive effect of investigating for the 42nd day of take is final result.Result of the test shows, the prepared product of embodiment 1~20 and 40% azoles humulone water dispersible granules are used latter 24 hours, and poisoning symptom just appears in part weeds, within the 4th day, just has weeds dead.And 30% gyphosate solution, 56%2 first 4 chlorine soluble powder of sodium agent 72 hours rear section weeds after using just start to occur poisoning symptom, within the 7th day, weeds occur dead, in quick-acting, the prepared product of embodiment 1~20 is better than 30% gyphosate solution and 56%2 first 4 chlorine soluble powder of sodium agent, suitable with 40% azoles humulone water dispersible granules.Fresh weight preventive effect was investigated in the 42nd day, result is as table 5.
Table 5 test medicine is to the field efficacy of weeds (fresh weight preventive effect) Chongzuo, Guangxi in 2012
Figure BSA0000096393210000151
Field medicine effect test result shows, containing glyphosate, 2 first 4 chlorine and azoles humulone herbicidal composition, each is processed the general control effect of weeds (fresh weight preventive effect) all over 80%, under same concentrations, embodiment 1~20 respectively processes drug effect and herbicide spectrum is all better than contrasting medicament 30% gyphosate solution and 56%2 first 4 chlorine soluble powder of sodium agent, is also better than 40% azoles humulone water dispersible granules under recommended dose.

Claims (6)

1. the herbicidal composition containing glyphosate, 2 first 4 chlorine and azoles humulone, it is characterized in that: this herbicidal composition is comprised of pesticide active ingredient and non-farm chemical ingredients, the weight percentage of pesticide active ingredient is 31.1%~85%, and surplus is non-farm chemical ingredients; Described pesticide active ingredient is glyphosate or its salt, 2 first 4 chlorine or its salt or its ester and azoles humulone; Wherein:
The parts by weight of glyphosate or its salt are: 30~70 parts;
The parts by weight of 2 first 4 chlorine or its salt or its ester: 1~30 part;
The parts by weight of azoles humulone are: 0.1~20 part.
2. the herbicidal composition containing glyphosate, 2 first 4 chlorine and azoles humulone according to claim 1; it is characterized in that; described glyphosate is N-(phosphonomethyl) glycine; its salt has organic salt and mineral salt; organic salt is ethanolamine salt, triisopropanolamine salt, triethylamine salt, isopropyl amine salt or dimethylamine salt, and mineral salt are sylvite, sodium salt or ammonium salt.
3. the herbicidal composition containing glyphosate, 2 first 4 chlorine and azoles humulone according to claim 1, it is characterized in that, 2 described first 4 chlorine are 2-methyl-4-tomatotone, its salt has organic salt and mineral salt, its organic salt is isopropyl amine salt or dimethylamine salt, its mineral salt are sylvite, sodium salt, ammonium salt, and its ester is that ethyl butyrate, sulfo-ethyl ester, second thioesters are different monooctyl ester.
4. the herbicidal composition containing glyphosate, 2 first 4 chlorine and azoles humulone according to claim 1, it is characterized in that, described non-farm chemical ingredients refers to the auxiliary agent in pesticidal preparations meaning, comprises one or more in filler, adhesive, surfactant, defoamer, antifreezing agent, solvent, thickener and cosolvent.
5. the herbicidal composition containing glyphosate, 2 first 4 chlorine and azoles humulone according to claim 1, is characterized in that: described herbicidal composition comprises wetting powder, water dispersible granules, soluble powder, soluble granula, aqua, aqueous emulsion and the microemulsion of being made by pesticide active ingredient and non-farm chemical ingredients.
6. the purposes of the herbicidal composition containing glyphosate, 2 first 4 chlorine and azoles humulone described in claim 1~5 any one, is characterized in that: the application aspect the annual and perennial weeds of this herbicidal composition in preventing and kill off forest land and uncultivated area.
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CN105410018A (en) * 2015-12-24 2016-03-23 安徽美兰农业发展股份有限公司 Ammonium glyphosate, chipton and clopyralid compound water agent and preparation method thereof
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CN103783051A (en) * 2014-02-26 2014-05-14 江苏富鼎化学有限公司 Composite herbicide containing florasulam, carfentrazone and agroxone
CN103783051B (en) * 2014-02-26 2016-01-27 江苏富鼎化学有限公司 A kind of mixed herbicide containing florasulam, azoles humulone and methoxone
CN104886126A (en) * 2015-06-05 2015-09-09 袁国防 Synergistic and sterilizing glyphosate herbicide composition
CN105410018A (en) * 2015-12-24 2016-03-23 安徽美兰农业发展股份有限公司 Ammonium glyphosate, chipton and clopyralid compound water agent and preparation method thereof
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CN106857516A (en) * 2017-02-16 2017-06-20 安徽海日农化有限公司 A kind of different monooctyl ester aqueous emulsion of chlorine of 2 first 4 and preparation method thereof

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