CN105519524A - A herbicide composition containing l-alpha-terpineol and preparations thereof - Google Patents

A herbicide composition containing l-alpha-terpineol and preparations thereof Download PDF

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CN105519524A
CN105519524A CN201511020431.5A CN201511020431A CN105519524A CN 105519524 A CN105519524 A CN 105519524A CN 201511020431 A CN201511020431 A CN 201511020431A CN 105519524 A CN105519524 A CN 105519524A
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terpineol
weight portion
sodium
diuron
sulfonate
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CN105519524B (en
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韦茂春
赖开平
黄科林
易芬远
方峰
叶一强
马就庆
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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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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/24Biocides, 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 ingredients to enhance the sticking of the active ingredients
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N39/00Biocides, pest repellants or attractants, or plant growth regulators containing aryloxy- or arylthio-aliphatic or cycloaliphatic compounds, containing the group or, e.g. phenoxyethylamine, phenylthio-acetonitrile, phenoxyacetone
    • A01N39/02Aryloxy-carboxylic acids; Derivatives thereof
    • A01N39/04Aryloxy-acetic acids; Derivatives thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/661,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms
    • A01N43/681,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms with two or three nitrogen atoms directly attached to ring carbon atoms
    • A01N43/70Diamino—1,3,5—triazines with only one oxygen, sulfur or halogen atom or only one cyano, thiocyano (—SCN), cyanato (—OCN) or azido (—N3) group directly attached to a ring carbon atom
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N47/00Biocides, 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
    • A01N47/08Biocides, 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
    • A01N47/28Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/30Derivatives containing the group >N—CO—N aryl or >N—CS—N—aryl

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Agronomy & Crop Science (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

A herbicide composition containing l-alpha-terpineol is disclosed. The composition comprises a synergist a and a herbicide active component b, wherein the synergist is the l-alpha-terpineol, and the herbicide active component is one of 2-methyl-4-chlorophenoxyacetic acid, ametryn and diuron or is a mixture prepared from more than one of the 2-methyl-4-chlorophenoxyacetic acid, the ametryn and the diuron. The composition reduces the using amount of herbicides in unit area and improves weeding effects of herbicides for sugarcane fields and safety to sugarcane, thus reducing the herbicide using cost. The composition can be prepared into wettable powder, water dispersible granules, emulsifiable solutions or dispersible oil suspensions, and can be used for control of annual weeds in sugarcane fields.

Description

A kind of herbicidal composition containing levogyrate alpha-terpineol and preparation thereof
Technical field
The present invention relates to technical field of pesticide, be specifically related to a kind of herbicidal composition containing levogyrate alpha-terpineol and its preparation method and application.
Background technology
Levogyrate alpha-terpineol (English common name α-(L)-Terpineol), it is a kind of chemical products (patent No.: ZL03178548.4 of being synthesized by Chemical Industry Inst., Guangxi Zhuang Autonomous Region, title: the preparation method of levogyrate alpha-terpineol), itself there is good moistening, adhesion, infiltration capacity.Guangxi Chemical Inst. has carried out large quantity research to its biologically active and range of application so far from 2003, specifically see published Chinese patent, such as: ZL200910114473.3, containing microbicide compositions and the production method thereof of Difenoconazole and levogyrate alpha-terpineol; ZL200910114624.5, the beta-cypermethrin pesticide composition containing L-terpineol synergist; ZL201010525128.1, containing microbicide compositions and the production method thereof of Tebuconazole and levogyrate alpha-terpineol.Demonstrate levogyrate alpha-terpineol and all have certain synergistic effect to insecticide and bactericide.
In sugarcane production process, weeds are one of principal elements affecting its quality and yield.Weeds in sugarcane field is of a great variety, and applied chemistry weed killer herbicide effectively can not only prevent and kill off weeds in sugarcane field, can also time and labour saving, enhances productivity.The weed killer herbicide that current registration is used for sugarcane field is formulated primarily of one or several active ingredients such as 2 first 4 chlorine, ametryn, diuron, hexazinone, atrazine, Brominals, and wherein the mixture preparation of 2 first 4 chlorine sodium and ametryn effectively can prevent and kill off sugarcane field major part weeds.Application number is that patent of invention " a kind of weed killer herbicide preventing and treating weeds in sugarcane field " its active ingredient of 200610053858.X is diuron, 2 first 4 chlorine sodium and ametryn are applicable to sugarcane field and prevent and kill off annual gramineous weed and broad leaved weed more than 50 ~ 60 is planted; Application number be 201210397471.1 application for a patent for invention " a kind of sugarcane field specific complex weed killer herbicide " be for main active with methoxone, diuron, ametryn, more than 90% is reached to annual single broadleaf weed control efficiency, and soil sealing process can be got after using, suppress the sprouting of later stage weeds, to sugarcane safety, can grow up by effective guarantee sugarcane health.
Along with applying of weed killer herbicide, mixture preparation only containing 2 first 4 chlorine sodium and ametryn two active ingredients can't prevent and kill off the weeds such as Bermuda grass, Rottboellia exaltata L. F, Egyptian grass, also not ideal enough to the control efficiency of aged lady's-grass, and the mixture herbicide containing diuron composition, not only can be good at the weeds such as control Bermuda grass, Rottboellia exaltata L. F, Egyptian grass, the control efficiency of ametryn to sugarcane field main weeds lady's-grass can also be significantly improved.
Two or more herbicide mixtures, in the advantage that all many-sides have single dose incomparable, it acts on mainly increasing action target site, expand herbicide spectrum, extend the optimum period for applying fertilizer, reduce residual activity, reduce poisoning, improve herbicidal effect, delay and control the generation of Weed Resistance.
The performance of sugarcane field herbicidal action effect except with the compatibility, environmental condition, insecticide-applying way etc. between weed killer herbicide chemical composition, each chemical composition mutually outside the Pass, also closely relevant with selecting of builder.Builder by increase weed killer herbicide plant surface hold-up, extend the holdup time and improve penetration capacity to plant epidermis, thus improve the biologically active of weed killer herbicide, reduce dosage, reduce costs, improve the compatibility of itself and environment.The synergistic effect of levogyrate alpha-terpineol to weed killer herbicides such as 2 first 4 chlorine sodium, ametryn and diuron there is no pertinent literature report.
Summary of the invention
The object of this invention is to provide a kind of herbicidal composition containing levogyrate alpha-terpineol, to reduce unit are weed killer herbicide using dosage, improve weed killer herbicide herbicidal effect and the safety to crop, thus reduce drug cost.
The described herbicidal composition containing levogyrate alpha-terpineol of the present invention, comprises the raw material composition of following weight portion: synergist 1-90 weight portion, herbicidal active component 1-90 weight portion;
Wherein, described is levogyrate alpha-terpineol by synergist, and described herbicidal active component is one or more the composite compositions in 2 first 4 chlorine, ametryn and diuron.
Preferably, synergist 2-10 weight portion, herbicidal active component 90-100 weight portion.
Described herbicidal composition, coordinates with auxiliary material and makes solid pharmaceutical preparation, and described auxiliary material comprises: the filler of 1-30 weight portion, the functional auxiliary material of 1-30 weight portion; Described functional auxiliary material comprises one or more mixing in surfactant, binding agent and disintegrant.
Described surfactant is sodium lignin sulfonate, sodium laureth sulfate, polyoxyethylene fatty alkyl ether sulfonate, dodecyl sulphate calcium, lauryl sodium sulfate, dodecyl sodium sulfate, calcium dodecyl benzene sulfonate, 2-naphthalene sulfonic acid formaldehyde polymer sodium salt, calcium lignosulfonate, polyethers ichthyodin, alkanolamide sodium sulfonate of ethoxylated, dispersing agent MF, phenethyl phenol polyethenoxy ether, one or more combination in polycarboxylic acid salt's macromolecule dispersing agent,
Described binding agent is starch sulfate, polyvinylpyrrolidone or polyvinyl alcohol;
Described disintegrant is for being anhydrous sodium sulfate, urea, ammonium sulfate or diammonium hydrogen phosphate.
Described filler is precipitated calcium carbonate, one or more combinations in white carbon, talcum powder, kaolin, bentonite or attapulgite.
Described herbicidal composition, coordinates with auxiliary material and makes liquid preparation, and described auxiliary material comprises: the defoamer of the solvent of 0-50 weight portion, the surfactant of 1-30 weight portion, 0-5 weight portion, the antifreezing agent of 0-5 weight portion, the thickener of 0-5 weight portion.
Described solvent is DMF, 1-METHYLPYRROLIDONE, cyclohexanone, carrene, mineral oil, one or more the combination in vegetable oil or vegetable oil esters compound;
Described surfactant is one or more the combination in calcium dodecyl benzene sulfonate, ethoxylated dodecyl alcohol, sodium lignin sulfonate, polycarboxylic acid salt's macromolecule dispersing agent, sodium laureth sulfate, polyoxyethylene fatty alkyl ether sulfonate, dodecyl sulphate calcium, lauryl sodium sulfate, dodecyl sodium sulfate, calcium lignosulfonate, polyethers ichthyodin, alkanolamide sodium sulfonate of ethoxylated, fatty alcohol-polyoxyethylene ether, phenethyl phenol polyethenoxy ether;
Described defoamer is polypropylene glycerol aether or polyether-modified silicon;
Described antifreezing agent is ethylene glycol, sorbierite or glycerine;
Described thickener is alumina silicate, xanthans or dispersed silica.
Described herbicidal composition can be applicable on control sugarcane field annual gramineous weed, broad leaved weed and sedge weed.
The present invention compares with diuron mixture preparation with existing 2 first 4 chlorine, ametryn, has following remarkable result:
(1) add levogyrate alpha-terpineol, not only maintain the plurality of advantages of former weed killer herbicide, but also each component working concentration when activity is not lost in mixture is reduced, thus the activity of mixture is increased.
(2) levogyrate alpha-terpineol has powerful infiltration, Zhan Zhe, wetting power, the adhesion on plant of 2 first 4 chlorine sodium, ametryn, diuron and absorption can be increased, and then improve the availability of these weed killer herbicides, decrease usage amount, reduce and make crop be subject to the risk of poisoning because of the excessive use of weed killer herbicide.
(3) herbicidal composition provided by the present invention improves weeding speed, reduces the impact of the bad climate such as low temperature, rainfall on drug effect.
Embodiment
The present invention is further illustrated below by embodiment.It should be understood that embodiments of the invention are for illustration of the present invention instead of limitation of the present invention.Essence according to the present invention all belongs to the scope of protection of present invention to the simple modifications that the present invention carries out.In following examples, percentage is all weight percentage.
Embodiment 1
Levogyrate alpha-terpineol 5kg, 2 first 4 chlorine sodium 56kg, lauryl sodium sulfate 3kg, 2-alkyl naphthalene sulfonic acid first condensation product sodium salt 5kg, sodium lignin sulfonate 6kg, precipitated calcium carbonate 25kg.By recipe requirements, by the fully mixing such as raw material, various auxiliary agent and filler, after micronizer is pulverized, namely obtain wetting powder.
Embodiment 2
Levogyrate alpha-terpineol 10kg, ametryn 70kg, sodium laureth sulfate 5kg, calcium lignosulfonate 5kg, white carbon 10kg.By formula rate, raw material, various auxiliary agent and filler etc. are fully mixed in batch mixer, add after mixing in airslide disintegrating mill and be crushed to fineness and reach 325 orders, obtain wetting powder.
Embodiment 3
Levogyrate alpha-terpineol 8kg, diuron 80kg, polyoxyethylene fatty alkyl ether sulfonate 2kg, dodecyl sodium sulfate 3kg, polyoxyethylene fatty alkyl ether sulfonate 2kg, attapulgite 5kg.By formula rate, raw material, various auxiliary agent and filler etc. are fully mixed in batch mixer, add after mixing in airslide disintegrating mill and be crushed to fineness and reach 325 orders, obtain wetting powder.
Embodiment 4
Levogyrate alpha-terpineol 4kg, 2 first 4 chlorine sodium 10kg, ametryn 40kg, di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate 4kg, sodium lignin sulfonate 4kg, kaolin complements to 100kg.First kaolin and levogyrate alpha-terpineol are added in batch mixer and mix, again 2 first 4 chlorine sodium, ametryn, diuron, sodium methylene bis-naphthalene sulfonate and sodium lignin sulfonate are added in batch mixer successively and fully mix, material after mixing adds in airslide disintegrating mill and is crushed to fineness and reaches 325 orders, obtains 50kg composite wettable powder.
Embodiment 5
Levogyrate alpha-terpineol 6kg, 2 first 4 chlorine sodium 8kg, diuron 52kg, dispersing agent MF 10kg, white carbon 24kg.First white carbon and levogyrate alpha-terpineol are added in batch mixer and mix, again 2 first 4 chlorine sodium, ametryn, diuron, dispersing agent MF are added in batch mixer successively and fully mix, material after mixing adds in airslide disintegrating mill and is crushed to fineness and reaches 325 orders, obtains wetting powder.
Embodiment 6
Levogyrate alpha-terpineol 7kg, ametryn 40g, diuron 30g, dodecyl sulphate calcium 5kg, calcium lignosulfonate 5kg, talcum powder 13kg.By recipe requirements, by the fully mixing such as raw material, various auxiliary agent and filler, after micronizer is pulverized, namely obtain wetting powder.
Embodiment 7
Levogyrate alpha-terpineol 10kg, 2 first 4 chlorine sodium 10kg, ametryn 40kg, diuron 23kg, dodecyl sodium sulfate 3kg, sodium lignin sulfonate 5kg, White Carbon black 2kg and diatomite 1kg adds in mixer successively, mix, then pulverize with airslide disintegrating mill, be less than 45 μm to active ingredient particle diameter; Obtain wetting powder.
Embodiment 8
Levogyrate alpha-terpineol 3kg, 2 first 4 chlorine sodium 12kg, ametryn 48kg, diuron 20kg, calcium dodecyl benzene sulfonate 5kg, sodium lignin sulfonate 5kg, bentonite 1kg, white carbon 6kg.By formula rate, raw material, various auxiliary agent and filler etc. are fully mixed in batch mixer, add after mixing in airslide disintegrating mill and be crushed to fineness and reach 325 orders, obtain wetting powder.
Example example 9
Levogyrate alpha-terpineol 10kg, ametryn 60kg, polyethers ichthyodin 4kg, alkanolamide sodium sulfonate of ethoxylated 2kg, polyoxyethylene fatty alkyl ether sulfonate 2kg, starch sulfate 2kg, bentonite 20kg.First bentonite and levogyrate alpha-terpineol are added in batch mixer and mix, again ametryn, alkanolamide sodium sulfonate of ethoxylated, polyoxyethylene fatty alkyl ether sulfonate are added in batch mixer successively and fully mix, material after mixing adds in airslide disintegrating mill and is crushed to fineness and reaches 325 orders, again the material after pulverizing is added in batch mixer and mix 1 hour, form certain density premix.Starch sulfate is mixed by weight 1:2 with water, abundant gelatinization at 80 DEG C.Premix is added in Squeezinggranulator together with the starch sulfate after gelatinization and makes water dispersible granules, after drying, cooling, screening, inspection, carry out finished product packing.
Embodiment 10
Levogyrate alpha-terpineol 6kg, diuron 70kg, lauryl sodium sulfate 8kg, 2-naphthalene sulfonic acid formaldehyde polymer sodium salt 8kg, binding agent polyvinylpyrrolidone 2kg, anhydrous sodium sulfate 1kg, white carbon 5kg mix in mixer, be ground into powder through micro jet, obtain 700 order-800 object fine powders; Gained fine powder is added in blender with the aqueous solution of binding agent and mixes, carry out granulation with Squeezinggranulator, dry at 50 DEG C-100 DEG C, namely obtain water dispersible granules.
Embodiment 11
Levogyrate alpha-terpineol 3kg, 2 first 4 chlorine sodium 15kg, ametryn 40kg, polycarboxylic acid salt's macromolecule dispersing agent 5kg, phenethyl phenol polyethenoxy ether 5kg, polyvinyl alcohol 3kg, white carbon 29kg.By above-mentioned substance Homogeneous phase mixing, grinding, infiltration suitable quantity of water granulation, after drying, namely obtain water dispersible granules.
Embodiment 12
Levogyrate alpha-terpineol 5kg, 2 first 4 chlorine sodium 10kg, diuron 55kg, alkanolamide sodium sulfonate of ethoxylated 4kg, sodium lignin sulfonate 6kg, urea 15kg, polyvinyl alcohol 2kg, kaolin 3kg.First levogyrate alpha-terpineol, 2 first 4 chlorine sodium, diuron, alkanolamide sodium sulfonate of ethoxylated, sodium lignin sulfonate, urea, kaolin are added in mixer and mix, pulverize through airslide disintegrating mill and obtain female powder, by female powder with 2% binding agent polyvinyl alcohol mix evenly, then granulation, dry, sieve and obtain water dispersible granules.
Embodiment 13
Levogyrate alpha-terpineol 5kg, ametryn 60kg, diuron 15kg, calcium dodecyl benzene sulfonate 6kg, 2-naphthalene sulfonic acid formaldehyde polymer sodium salt 4kg, ammonium sulfate 5kg, starch sulfate 2kg, diatomite 3.First diatomite and levogyrate alpha-terpineol are added in batch mixer and mix, again ametryn, diuron, calcium dodecyl benzene sulfonate, 2-naphthalene sulfonic acid formaldehyde polymer sodium salt, ammonium sulfate are added in batch mixer successively and fully mixes, material after mixing adds in micro jet and is crushed to fineness and reaches 600 orders, again the material after pulverizing is added in batch mixer and mix 1 hour, form certain density premix.Starch sulfate is mixed by weight 1:2 with water, abundant gelatinization at 80 DEG C.Premix is added in Squeezinggranulator together with the starch sulfate after gelatinization and makes water dispersible granules, after drying, cooling, screening, inspection, carry out finished product packing.
Embodiment 14
Levogyrate alpha-terpineol 4kg, 2 first 4 chlorine sodium 12kg, ametryn 48kg, diuron 15kg, polycarboxylic acid salt's macromolecule dispersing agent 5kg, sodium laureth sulfate 3kg, diammonium hydrogen phosphate 10kg, white carbon 3kg.After mixture fully mixes, carry out ultra micro air-flow crushing, obtain 750 order fine powders, then gained fine powder is added in kneader appropriate water and mediate, through squash type granulator granulation, dry at 50 DEG C in fluidizing fluid-bed, namely obtain water dispersible granules.
Embodiment 15
Levogyrate alpha-terpineol 10kg, ametryn 30kg, calcium dodecyl benzene sulfonate 3kg, ethoxylated dodecyl alcohol 6kg, ethylene glycol 2kg, DMF 49kg.By levogyrate alpha-terpineol, ametryn, calcium dodecyl benzene sulfonate, ethoxylated dodecyl alcohol, ethylene glycol, add successively in DMF and be stirred to equal liquid phase, obtain missible oil.
Embodiment 16
Levogyrate alpha-terpineol 12kg, diuron 30kg, calcium dodecyl benzene sulfonate 2kg, alkane ethyl phenol APEO 8kg, 1-METHYLPYRROLIDONE 48kg.By levogyrate alpha-terpineol, diuron, calcium dodecyl benzene sulfonate, alkane ethyl phenol APEO, add successively in 1-METHYLPYRROLIDONE and be stirred to equal liquid phase, obtain missible oil.
Embodiment 17
2 first 4 chlorine sodium 5kg, ametryn 20kg, diuron 15kg, levogyrate alpha-terpineol 8kg, polycarboxylic acid salt's macromolecule dispersing agent 6kg, xanthans 0.1kg, soybean oil 10kg, methyl oleate supplies 36kg.Stirring is started after soybean oil and methyl oleate are added reactor, drop into 2 first 4 chlorine sodium successively, ametryn, diuron, levogyrate alpha-terpineol, polycarboxylic acid salt's macromolecule dispersing agent stir and add xanthans in backward sand mill and grind, until particle diameter dispersibles oil-suspending agent to making within 5 μm.
Embodiment 18
2 first 4 chlorine sodium 5kg, ametryn 20kg, diuron 10kg, levogyrate alpha-terpineol 10kg, calcium dodecyl benzene sulfonate 4kg, phenethyl phenol polyethenoxy ether 4kg, ethylene glycol 5kg, defoamer polypropylene glycerol aether 0.3kg, soybean oil 42kg.2 first 4 chlorine sodium, ametryn, diuron, levogyrate alpha-terpineol, soybean oil are put into sand mill and carried out one-level sand milling together with calcium dodecyl benzene sulfonate, phenethyl phenol polyethenoxy ether, secondary and three grades of sand millings are carried out again respectively after filtration, until by dispersed for former medicine, be crushed to colloidal particle size be below 5 μm till, add defoamer polypropylene glycerol aether and ethylene glycol and namely can be made into and dispersible oil-suspending agent.
Embodiment 19
2 first 4 chlorine sodium 5kg, ametryn 20kg, diuron 12kg, levogyrate alpha-terpineol 9kg, sodium lignin sulfonate 3kg, fatty alcohol-polyoxyethylene ether 3kg, phenethyl phenol polyethenoxy ether 4kg, xanthans 0.5kg, sorbierite 0.5kg, 44kg supplied by rapeseed oil.Sodium lignin sulfonate, fatty alcohol-polyoxyethylene ether, phenethyl phenol polyethenoxy ether, xanthans, sorbierite is added successively in rapeseed oil, mixing, stirring, add 2 first 4 chlorine sodium, ametryn, diuron, levogyrate alpha-terpineol under the rotating speed of high-speed shearing machine 1500 ~ 10000 revs/min stirs after, shear 10 ~ 40 minutes, being ground to particle diameter through sand mill is again less than till 5 μm, namely obtains and dispersibles oil-suspending agent.
Embodiment 20
Levogyrate alpha-terpineol 1kg, 2 first 4 chlorine 30kg, ametryn 35kg, diuron 25kg, calcium dodecyl benzene sulfonate 2kg, ethoxylated dodecyl alcohol 1kg, DMF 7kg.By levogyrate alpha-terpineol, ametryn, calcium dodecyl benzene sulfonate, ethoxylated dodecyl alcohol, add successively in DMF and be stirred to equal liquid phase, obtain missible oil.
Embodiment 21
Levogyrate alpha-terpineol 90kg, ametryn 1kg, phenethyl phenol polyethenoxy ether 3kg, dodecyl sodium sulfate 2kg, attapulgite 4kg.By above-mentioned substance Homogeneous phase mixing, grinding, namely obtain and dispersible oil-suspending agent.
Embodiment 22 (levogyrate alpha-terpineol respectively with 2 first 4 chlorine sodium, ametryn or the composite indoor virulence to bidens pilosa of diuron)
Pass through indoor biometrics, specify levogyrate alpha-terpineol and 2 first 4 chlorine sodium, ametryn or diuron composite after synergy situation, object is surveyed as raw using 4 leaf phases bidens pilosa (Bidenspilosa), select and do not use weed killer herbicide soil, pH6.8, after air-dry for soil sieving, loads diameter 32cm, in the plastic flowerpot (having pallet) of dark 20cm, every basin plant 15 strains healthy and strong consistent 4 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, and often processes 4 times and repeats, often repeat 15 strain plants.Levogyrate alpha-terpineol, 2 first 4 chlorine sodium, ametryn, diuron are made into 5 required series concentration gradients, separately or after mix with levogyrate alpha-terpineol cauline leaf spraying process is carried out to three leaf Bidens bipinnatas by experimental scheme, if clear water contrast and not contrasting containing levogyrate alpha-terpineol process.Co-toxicity coefficient is calculated according to Sun-Johnson method, synegism evaluation is carried out, if co-toxicity coefficient >120 is synergistic effect, if 120 >=co-toxicity coefficient >80 is summation action according to co-toxicity coefficient, if co-toxicity coefficient≤80 are antagonism, computing formula is:
Result of the test is in table 1.
Table 1 levogyrate alpha-terpineol and 2 first 4 chlorine sodium, ametryn or the composite co-toxicity coefficient that bidens pilosa fresh weight is suppressed of diuron
As can be seen from Table 1,2 first 4 chlorine sodium, after ametryn or diuron are mixed with levogyrate alpha-terpineol respectively, to the ED of bidens pilosa fresh weight inhibition 50value value is respectively 225,380,410, and its co-toxicity coefficient is respectively 133.3,131.6,134.1, is all greater than 120, shows 2 first 4 chlorine sodium, ametryn or the diuron synergistic effect that all show in various degree mixed with levogyrate alpha-terpineol.
Embodiment 23
For clear and definite levogyrate alpha-terpineol is to the synergy situation of 2 first 4 chlorine sodium, ametryn and diuron ternary built weed killer herbicide, first the optimum proportioning of 2 first 4 chlorine sodium, ametryn and diuron three mixture will be found according to bioassay for herbicide method, then according to optimum proportioning, introduce levogyrate alpha-terpineol, determine the best synergy proportioning of levogyrate alpha-terpineol to ternary built weed killer herbicide.Object is surveyed as raw using the lady's-grass (Digitariasanguinalis) of 3 leaf phases, the bidens pilosa of 3 leaf phases (Bidenspilosa), the rhizome of nutgrass flatsedge of 4 leaf phases (Cyperurotundus), select and do not use weed killer herbicide soil, pH6.8, after air-dry for soil sieving, load diameter 32cm, in the plastic flowerpot (having pallet) of dark 20cm, every basin plant 15 strains healthy and strong consistent 5 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, and often processes 4 times and repeats, often repeat 15 strain plants, if be not 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 in the synergy mensuration of mixture, calculates each mixture combinatorial theory survival rate E 0difference (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 actual weeds survival rate E of single dose and each mixture calculates according to formula (1):
The theoretical weeds survival rate E of mixture 0calculate by formula (2):
E 0 = A &times; B &times; C &times; ... N 100 ( n - 1 ) ... ( 2 )
In formula:
The weeds survival rate of A-weed killer herbicide 1
The weeds survival rate of B-weed killer herbicide 2
The weeds survival rate of C-weed killer herbicide 3
The weeds survival rate of N-weed killer herbicide N
N-be the kind quantity of mixture herbicide
Three kinds of effect criterion: the E shown after herbicide mixture 0-E>10% is synergistic effect; E 0-E<-10% is antagonism; E 0-E value is addition between ± 10%.
Calculate its result as following table 2.
Table 2.2 first 4 chlorine sodium and ametryn and diuron mixture are to the joint toxicity measuring (Colby method) of weeds
According to the result of table 2,2 first 4 chlorine sodium are at low dosage (150ga.i./hm 2), ametryn is at high dose (600ga.i./hm 2) under, diuron high and low dose (300,450ga.i./hm 2) the obvious synergistic effect of mixed performance, E0-E>10.9.Best mixed ratio scope is 150:600:300 ~ 150:600:450, i.e. 1:4:2 ~ 1:4:3.Consider formulation technique and the product cost of Ternary preparation, adopt 2 first 4 chlorine sodium: ametryn: the ratio mixture of diuron=1:4:2.3, determine that ternary weed killer herbicide optimum formula is 73%2 first 4 chlorine sodium ametryn diuron (10+40+23).
On the basis of above-mentioned ternary Herbicidal composition screening, by 2 first 4 chlorine sodium: ametryn: diuron=10:40:23 integrally, carry out composite with levogyrate alpha-terpineol again, target is surveyed as raw using the eleusine indica (Eleusineindica) of 3 leaf phases, specify the control efficiency to eleusine indica after mixture, 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, often process and repeat for 4 times, often repeat 15 strain plants, if not dispenser agent is treated to blank.Concrete outcome is as table 3.
Table 3 levogyrate alpha-terpineol and first go out diuron (10+40+23) mixture to the control efficiency of eleusine indica
Can find out that levogyrate alpha-terpineol that the present invention adds obviously can increase by 73% first and go out the agent of diuron (10+40+23) mixture to the control efficiency of eleusine indica from the above-mentioned test of pesticide effectiveness, the go out control efficiency of diuron (10+40+23) mixture mixture of the several ratio of levogyrate alpha-terpineol and 73% first is all greater than 93%.And wherein with levogyrate alpha-terpineol: first go out diuron=10:73 time control efficiency the most obvious, reach 98.28%.
Embodiment 24 (different temperatures is tested containing the impact of levogyrate alpha-terpineol effect of herbicides)
Pass through indoor biometrics, specify levogyrate alpha-terpineol and 73% first goes out the composite rear temperature of diuron to the impact of its drug effect, with barnyard grass (Echinochloacrusgalli) for test target, with reference to NY/T1155.4-2006 farm-chemical indoor determination test rule weed killer herbicide part 1: activity test culture dish is tested.After barnyard grass seed presoaking and germinating, selecting the consistent seed of growth, to be evenly placed on the internal diameter being covered with two metafiltration paper be in 9cm culture dish, 20, every ware, plumule is unified upwards to be put, add 100,50,25,12.5,6.25,3.125 and the going out diuron weed killer herbicide liquid 9ml containing 73% first of 10% levogyrate alpha-terpineol of 1.5625mg/L respectively, contrast medicament is that 73% first not adding levogyrate alpha-terpineol is gone out diuron, blank adding distil water.Often process and repeat for 3 times.Culture dish is moved in plant incubator, 5 temperature 10,15,20,25 and 30 DEG C are set respectively, be cultivate 7 days under the dark condition of 75% in humidity, measure bud long, calculate inhibiting rate, and with the regression analysis of DPS software, formulate dose response calibration curve, ask ED 50value, compares otherness between treatment of different temperature.In 1.5625-100mg/L dosage range, containing the weed killer herbicide of levogyrate alpha-terpineol in different temperatures environment to the ED of barnyard grass 50value is in table 4.
Table 4 different temperatures is on diuron herbicidal activity impact of going out containing 73% first of 10% levogyrate alpha-terpineol
As can be seen from Table 4, there is not the difference of the order of magnitude to the weed killer herbicide activity of weeding impact containing levogyrate alpha-terpineol in temperature, ED at each temperature 50value difference is not quite different.On the whole, high at low temperature 10-15 DEG C of specific activity contrast medicament containing 73% first of the 10% levogyrate alpha-terpineol diuron weed killer herbicide that goes out.
Embodiment 25 (after process different time rainfall 73% first containing 10% levogyrate alpha-terpineol is gone out the impact of diuron WP effect of herbicides)
Select barnyard grass (Echinochloacrusgalli) to make a living survey target, treat that barnyard grass grew for 4 leaf phases, determine strain for subsequent use.In auto spraying tower (pressure 0.2MPa, dose 75mL/m 2, spray time 30s) and spraying process.Dispenser dosage is 1250g.a.i./hm 2if two process: 1. process is the diuron WP that goes out containing 73% first of 10% levogyrate alpha-terpineol, process 2. for contrast medicament 73% first is gone out diuron WP, and is established blank and is not washed away contrast, often processes 3 repetitions.After dispenser respectively at l, 2,3,6 and 12h with being equivalent to the rainfall simulator of precipitation 30mm to the rain drop erosion of each process simulating nature.Process is placed in greenhouse and grows, the reaction symptom of plant after routine observation process, 15 days viewing test results.
Table 5 different time washes away the suppression result (%) to barnyard grass after process
Base of the plant, serious brownization of vein is observed after process. the atrophy of young leaves deformity.Each process symptom that different time is drenched with rain is basically identical.Process latter 15 days, comprehensive inhibiting rate the results are shown in Table 5, data display in table, and 1. process washes away containing 73% first of the 10% levogyrate alpha-terpineol diuron WP different time that goes out the high activity that process all has more than 85%, and between process, difference is not obvious.Visible, after dispenser, the activity of weeding of rainfall to the diuron WP that goes out containing 73% first of 10% levogyrate alpha-terpineol does not have a significant effect, higher than the go out activity of diuron WP of contrast medicament 73% first.After dispenser, rainfall goes out the impact of diuron WP drug effect not quite to 73% first containing 10% levogyrate alpha-terpineol, has certain ability to resist splash erosion.
Inventive embodiments Field information situation:
In April, 2013, we carried out the weeding field control effectiveness test of a sugarcane field at Nanning City's Wuming County, carried out with reference to pesticide field efficacy medicine test criterion (one) weed killer herbicide control sugarcane field weeds GB/T17980.49-2000.Its result of the test is as table 6:
A table 619 invention example is to the control efficiency of sugarcane field weeds
Note: contrast medicament is commercially available 56%2 first 4 chlorine soluble powder of sodium agent, 80% ametryn wetting powder and 80% diuron wetting powder, spray in April 10 medicine, investigation on April 30 hybrid strain preventive effect, preventive effect (%)=(CK number of weeds-medication number of weeds)/CK number of weeds × 100%.
Can go out from upper table, when using dosage is suitable, the preventive effect of the present invention to weeds is better than the effect contrasting medicament.
The Economic and Efficiency Analysis that the present invention applies in sugarcane field
In May, 2014, we carried out the weeding test of pesticide effectiveness at Si Tang town, Xingning District, Nanning City sugarcane field, and test method is carried out with reference to pesticide field efficacy medicine test criterion (one) weed killer herbicide control sugarcane field weeds GB/T17980.49-2000.Its result of the test is as following table 7.
The application economic benefits comparison of table 7 the present invention in the sugarcane field of mixed raw Bermuda grass
Note: spray in May 4 medicine, investigation on June 4 hybrid strain preventive effect, every mu of spray liquid medicine 45 kilograms.Preventive effect (%)=(the remaining weeds weight in CK weeds weight-medication district)/CK weeds weight × 100%.
Can go out from upper table, the preventive effect of the embodiment of the present invention to weeds is better than the effect of ametryn single dose, and the cost of use weed killer herbicide is cheaper, herbicide spectrum is wider, to the malignant weed Bermuda grass of sugarcane field, there is very excellent preventive effect, and embodiment of the present invention weeding speed is faster, economic benefit is obvious.

Claims (8)

1., containing a herbicidal composition for levogyrate alpha-terpineol, it is characterized in that the raw material composition comprising following weight portion: synergist 1-90 weight portion, herbicidal active component 1-90 weight portion;
Wherein, described synergist is levogyrate alpha-terpineol, and described herbicidal active component is one or more the composite compositions in 2 first 4 chlorine, ametryn and diuron.
2. herbicidal composition according to claim 1, is characterized in that the raw material composition comprising following weight portion: synergist 2-10 weight portion, herbicidal active component 90-100 weight portion.
3. herbicidal composition according to claim 1 and 2, coordinates with auxiliary material and makes solid pharmaceutical preparation, it is characterized in that, described auxiliary material comprises: the filler of 1-30 weight portion, the functional auxiliary material of 1-30 weight portion; Described functional auxiliary material comprises one or more mixing in surfactant, binding agent and disintegrant.
4. herbicidal composition according to claim 3, is characterized in that:
Described surfactant is sodium lignin sulfonate, sodium laureth sulfate, polyoxyethylene fatty alkyl ether sulfonate, dodecyl sulphate calcium, lauryl sodium sulfate, dodecyl sodium sulfate, calcium dodecyl benzene sulfonate, 2-naphthalene sulfonic acid formaldehyde polymer sodium salt, calcium lignosulfonate, polyethers ichthyodin, alkanolamide sodium sulfonate of ethoxylated, dispersing agent MF, phenethyl phenol polyethenoxy ether, one or more combination in polycarboxylic acid salt's macromolecule dispersing agent,
Described binding agent is starch sulfate, polyvinylpyrrolidone or polyvinyl alcohol;
Described disintegrant is for being anhydrous sodium sulfate, urea, ammonium sulfate or diammonium hydrogen phosphate.
5. herbicidal composition according to claim 3, is characterized in that: described filler is precipitated calcium carbonate, one or more combinations in white carbon, talcum powder, kaolin, bentonite or attapulgite.
6. herbicidal composition according to claim 1 and 2, coordinate with auxiliary material and make liquid preparation, it is characterized in that, described auxiliary material comprises: the defoamer of the solvent of 0-50 weight portion, the surfactant of 1-30 weight portion, 0-5 weight portion, the antifreezing agent of 0-5 weight portion, the thickener of 0-5 weight portion.
7. herbicidal composition according to claim 6, is characterized in that:
Described solvent is DMF, 1-METHYLPYRROLIDONE, cyclohexanone, carrene, mineral oil, one or more the combination in vegetable oil or vegetable oil esters compound;
Described surfactant is one or more the combination in calcium dodecyl benzene sulfonate, ethoxylated dodecyl alcohol, sodium lignin sulfonate, polycarboxylic acid salt's macromolecule dispersing agent, sodium laureth sulfate, polyoxyethylene fatty alkyl ether sulfonate, dodecyl sulphate calcium, lauryl sodium sulfate, dodecyl sodium sulfate, calcium lignosulfonate, polyethers ichthyodin, alkanolamide sodium sulfonate of ethoxylated, fatty alcohol-polyoxyethylene ether, phenethyl phenol polyethenoxy ether;
Described defoamer is polypropylene glycerol aether or polyether-modified silicon;
Described antifreezing agent is ethylene glycol, sorbierite or glycerine;
Described thickener is alumina silicate, xanthans or dispersed silica.
8. the purposes of the herbicidal composition of claim 1-7 described in any one on control sugarcane field annual gramineous weed, broad leaved weed and sedge weed.
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