CN105519524B - A kind of herbicidal composition and its preparation containing levogyrate alpha-terpineol - Google Patents

A kind of herbicidal composition and its preparation containing levogyrate alpha-terpineol Download PDF

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CN105519524B
CN105519524B CN201511020431.5A CN201511020431A CN105519524B CN 105519524 B CN105519524 B CN 105519524B CN 201511020431 A CN201511020431 A CN 201511020431A CN 105519524 B CN105519524 B CN 105519524B
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sodium
terpineol
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sulfonate
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CN105519524A (en
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韦茂春
赖开平
黄科林
易芬远
方峰
叶强
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)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a kind of herbicidal compositions containing left-handed α terpinols, it is made of wherein synergist a and herbicidal active component b, the synergist is left-handed α terpinols, and the herbicidal active component is one or more kinds of compounding compositions in 2 first, 4 chlorine, ametryn and diuron.The composition can reduce unit area herbicide dosage, sugarcane field herbicidal herbicidal effect and the safety to sugarcane be improved, to reduce drug cost.The composition can be configured to the annual grassy weeds of wettable powder, water dispersible granules, missible oil or dispersible oil-suspending agent for preventing and kill off sugarcane field.

Description

A kind of herbicidal composition and its preparation containing levogyrate alpha-terpineol
Technical field
The present invention relates to technical field of pesticide, and in particular to a kind of herbicidal composition and its system containing levogyrate alpha-terpineol Preparation Method and application.
Background technology
Levogyrate alpha-terpineol (English common name α-(L)-Terpineol), is by Chemical Industry Inst., Guangxi Zhuang Autonomous Region A kind of chemical products (patent No. of synthesis:ZL03178548.4, title:The preparation method of levogyrate alpha-terpineol), itself has Good moistening, adhesion, penetrating power.Guangxi Chemical Inst. so far carried out its bioactivity and application range from 2003 Numerous studies, are specifically shown in published Chinese patent, such as:ZL200910114473.3 contains difenoconazole and left-handed α- The microbicide compositions and its production method of terpinol;ZL200910114624.5 contains the efficient of L-terpineol synergist Cypermethrin insecticide composition;ZL201010525128.1, microbicide compositions containing Tebuconazole and levogyrate alpha-terpineol and Its production method.Show that levogyrate alpha-terpineol has certain synergistic effect to insecticide and fungicide.
During sugarcane production, weeds are one of the principal elements for influencing its quality and yield.Weeds in sugarcane field type is numerous More, applied chemistry herbicide can not only effectively prevent and kill off weeds in sugarcane field, moreover it is possible to which production efficiency is improved in time and labour saving.Registration at present Herbicide for sugarcane field is mainly one or several by 2 first, 4 chlorine, ametryn, diuron, hexazinone, atrazine, Brominal etc. Active ingredient is formulated, wherein the mixture preparation of 2 first, 4 chlorine sodium and ametryn can effectively prevent and kill off sugarcane field major part weeds.Application Number be 200610053858.X patent of invention《A kind of herbicide of prevention weeds in sugarcane field》Its active ingredient is diuron, 2 first 4 Chlorine sodium and ametryn prevents and kill off annual gramineous weed suitable for sugarcane field and broad leaved weed more than 50~60 is planted;Application No. is 201210397471.1 application for a patent for invention《A kind of sugarcane field specific complex herbicide》It is with dimethyl tetrachloride, diuron, green bristlegrass It is main active only to go out, and to annual single broadleaf weed control effect up to 90% or more, and can get soil after applying Sealing process inhibits the sprouting of later stage weeds, can the growth of effective guarantee sugarcane health to sugarcane safety.
With the popularization and application of herbicide, the mixture preparation only containing 2 first, 4 chlorine sodium and two active ingredient of ametryn is also not The weeds such as Bermuda grass, Rottboellia exaltata L. F, Egyptian grass can be prevented and kill off, it is also not ideal enough to the control effect of aged lady's-grass, and contain diuron The mixture herbicide of composition is not only able to prevent the weeds such as Bermuda grass, Rottboellia exaltata L. F, Egyptian grass well, moreover it is possible to significantly improve green bristlegrass It goes out only to the control effect of sugarcane field main weeds lady's-grass.
Two or more herbicide mixtures have the advantages that single dose is incomparable in all various aspects, and effect is main It is increasing action target site, expands herbicide controlling spectrum, extend the optimum period for applying fertilizer, reduce residual activity, reduce poisoning, improves weeding effect Fruit delays and controls the generation of Weed Resistance.
The performance of sugarcane field herbicidal function and effect is in addition to compatibility, the environment between herbicide chemical composition, each chemical composition The phase such as condition, insecticide-applying way is outside the Pass, also closely related with the selection of builder.Builder is by increasing herbicide in plant The hold-up on surface extends the residence time and improves the penetration capacity to plant epidermis, to improve the bioactivity of herbicide, Dosage is reduced, cost is reduced, improves its compatibility with environment.2 first of levogyrate alpha-terpineol pair, 4 chlorine sodium, ametryn and enemy's grass The synergistic effect of grand equal herbicides there is no pertinent literature to report.
Invention content
The object of the present invention is to provide a kind of herbicidal compositions containing levogyrate alpha-terpineol, to reduce unit area weeding Agent dosage improves herbicide herbicidal effect and the safety to crop, to reduce drug cost.
The herbicidal composition containing levogyrate alpha-terpineol of the present invention includes the raw material composition of following parts by weight: Synergist 1-90 parts by weight, herbicidal active component 1-90 parts by weight;
Wherein, it is described by synergist be levogyrate alpha-terpineol, the herbicidal active component be 2 first, 4 chlorine, ametryn and One or more kinds of compounding compositions in diuron.
Preferably, synergist 2-10 parts by weight, herbicidal active component 90-100 parts by weight.
Solid pharmaceutical preparation is made with auxiliary material cooperation in the herbicidal composition, and the auxiliary material includes:1-30 parts by weight are filled out Material, the functional auxiliary material of 1-30 parts by weight;The functional auxiliary material includes one in surfactant, binder and disintegrant Kind or more than one mixing.
The surfactant be 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- naphthalenesulfonateformaldehyde formaldehydes are poly- Close object sodium salt, calcium lignosulfonate, polyethers ichthyodin, alkanolamide sodium sulfonate of ethoxylated, di-2-ethylhexylphosphine oxide methyl naphthalene sulfonic acid One or more kinds of combinations in sodium, phenethyl phenol polyethenoxy ether, polycarboxylic acid salt's macromolecule dispersing agent;
The binder is starch sulfate, polyvinylpyrrolidone or polyvinyl alcohol;
The disintegrant is anhydrous sodium sulfate, urea, ammonium sulfate or diammonium hydrogen phosphate.
The filler is one in precipitated calcium carbonate, white carbon, talcum powder, kaolin, bentonite or attapulgite Kind or more than one combinations.
Liquid preparation is made with auxiliary material cooperation in the herbicidal composition, and the auxiliary material includes:0-50 parts by weight it is molten Agent, the thickening of the surfactant of 1-30 parts by weight, the antifoaming agent of 0-5 parts by weight, the antifreezing agent of 0-5 parts by weight, 0-5 parts by weight Agent.
The solvent is n,N-Dimethylformamide, N-Methyl pyrrolidone, cyclohexanone, dichloromethane, mineral oil, is planted One or more kinds of combinations in object oil or vegetable oil esters compound;
The surfactant is calcium dodecyl benzene sulfonate, ethoxylated dodecyl alcohol, sodium lignin sulfonate, poly- carboxylic Barbiturates macromolecule dispersing agent, sodium laureth sulfate, polyoxyethylene fatty alkyl ether sulfonate, dodecyl sulphate calcium, 12 Sodium alkyl sulfate, dodecyl sodium sulfate, calcium lignosulfonate, polyethers ichthyodin, alkanolamide sodium sulfonate of ethoxylated, fat One or more kinds of combinations in fat alcohol polyoxyethylene ether, phenethyl phenol polyethenoxy ether;
The antifoaming agent is polypropylene glycerol aether or polyether-modified silicon;
The antifreezing agent is ethylene glycol, sorbierite or glycerine;
The thickener is alumina silicate, xanthans or dispersed silica.
The herbicidal composition can be applied in prevention sugarcane field annual gramineous weed, broad leaved weed and nutgrass flatsedge On section weeds.
The present invention has following remarkable result compared with existing 2 first, 4 chlorine, ametryn and diuron mixture preparation:
(1) levogyrate alpha-terpineol is added, not only maintains the plurality of advantages of former herbicide, but also make each component in mixture It is reduced using concentration in the case where activity is not lost, is increased to the activity of mixture.
(2) levogyrate alpha-terpineol has powerful infiltration, Zhan Zhe, wetting power, can increase by 2 first, 4 chlorine sodium, ametryn, enemy Careless grand adherency and absorption on plant, and then the utilization rate of these herbicides is improved, reduce usage amount, reduces because of weeding Agent is excessively used and the risk that makes crop by poisoning.
(3) herbicidal composition provided by the present invention improves weeding speed, reduces the bad climates such as low temperature, rainfall Influence to drug effect.
Specific implementation mode
It is further illustrated the present invention below by embodiment.It should be understood that the embodiment of the present invention is for illustrating The present invention is rather than limiting the invention.The simple modifications that essence according to the present invention carries out the present invention belong to the present invention Claimed range.Percentage is weight percentage in following embodiment.
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.It is by recipe requirements, raw material, various auxiliary agents and filler etc. is fully mixed It closes, wettable powder is obtained after micronizer crushes.
Embodiment 2
Levogyrate alpha-terpineol 10kg, ametryn 70kg, sodium laureth sulfate 5kg, calcium lignosulfonate 5kg, white carbon 10kg.Raw material, various auxiliary agents and filler etc. are fully mixed in batch mixer by formula rate, air-flow powder is added after mixing It is crushed to fineness in broken machine and reaches 325 mesh, obtains wettable 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.Raw material, various auxiliary agents and filler etc. are filled by formula rate Divide and mixed in batch mixer, being crushed to fineness in addition airslide disintegrating mill after mixing reaches 325 mesh, obtains wettable powder Agent.
Embodiment 4
Levogyrate alpha-terpineol 4kg, 2 first 4 chlorine sodium 10kg, ametryn 40kg, di-2-ethylhexylphosphine oxide bitter edible plant sodium sulfonate 4kg, sulfomethylated lignin Sour sodium 4kg, kaolin complement to 100kg.First kaolin and levogyrate alpha-terpineol are added in batch mixer and are uniformly mixed, then by 2 4 chlorine sodium of first, ametryn, diuron, sodium methylene bis-naphthalene sulfonate and sodium lignin sulfonate are sequentially added in batch mixer and are sufficiently mixed, It is crushed to fineness in material addition airslide disintegrating mill after mixing and reaches 325 mesh, obtains 50kg composite wettable powders.
Embodiment 5
Levogyrate alpha-terpineol 6kg, 2 first 4 chlorine sodium 8kg, diuron 52kg, dispersing agent MF 10kg, hard charcoal Black 24kg.First white carbon and levogyrate alpha-terpineol are added in batch mixer and are uniformly mixed, then 2 first, 4 chlorine sodium, ametryn, enemy is careless Grand, dispersing agent MF is sequentially added in batch mixer and is sufficiently mixed, and air-flow crushing is added in material after mixing It is crushed to fineness in machine and reaches 325 mesh, obtains wettable powder.
Embodiment 6
Levogyrate alpha-terpineol 7kg, ametryn 40g, diuron 30g, dodecyl sulphate calcium 5kg, calcium lignosulfonate 5kg, talcum powder 13kg.By recipe requirements, raw material, various auxiliary agents and filler etc. are sufficiently mixed, crushed by micronizer Obtain wettable powder afterwards.
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 are sequentially added in mixing machine, are uniformly mixed, then with air-flow powder Broken machine crushes, until active ingredient grain size is less than 45 μm;Obtain wettable 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.It is by formula rate that raw material, various auxiliary agents and filler etc. is abundant It is mixed in batch mixer, being crushed to fineness in addition airslide disintegrating mill after mixing reaches 325 mesh, obtains wettable 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 by bentonite and left-handed α-pine tar Alcohol is added in batch mixer and is uniformly mixed, then by ametryn, alkanolamide sodium sulfonate of ethoxylated, fatty alcohol polyoxyethylene ether sulphur Sour sodium, which sequentially adds in batch mixer, to be sufficiently mixed, and being crushed to fineness in material addition airslide disintegrating mill after mixing reaches 325 mesh, then the material after crushing is added in batch mixer and is mixed 1 hour, form certain density premix.Starch sulfate With water by weight 1:2 are uniformly mixed, and are fully gelatinized at 80 DEG C.Premix is added together with the starch sulfate after gelatinization Water dispersible granules are made in Squeezinggranulator, 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, binder polyvinylpyrrolidone 2kg, anhydrous sodium sulfate 1kg, white carbon 5kg are uniformly mixed in mixing machine, through ultra micro Airslide disintegrating mill is ground into powder, obtains -800 targeted fine powder of 700 mesh;Gained fine powder is mixed with the addition of the aqueous solution of binder It is uniformly mixed in device, is granulated with Squeezinggranulator, dried to get to water dispersible granules at 50 DEG C -100 DEG C.
Embodiment 11
Levogyrate alpha-terpineol 3kg, 2 first 4 chlorine sodium 15kg, ametryn 40kg, polycarboxylic acid salt macromolecule dispersing agent 5kg, benzene Ethyl phenol polyethenoxy ether 5kg, polyvinyl alcohol 3kg, white carbon 29kg.Above-mentioned substance is uniformly mixed, grinds, penetrate into suitable quantity of water And be granulated, up to water dispersible granules after drying.
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 by levogyrate alpha-terpineol, 2 first, 4 chlorine sodium, enemy's grass Grand, alkanolamide sodium sulfonate of ethoxylated, sodium lignin sulfonate, urea, kaolin are added in mixing machine and are uniformly mixed, and pass through Airslide disintegrating mill crushes to obtain female powder, by female powder with 2% binder polyvinyl alcohol it is uniform, be then granulated, dry, sieving Obtain water dispersible granules.
Embodiment 13
Levogyrate alpha-terpineol 5kg, ametryn 60kg, diuron 15kg, calcium dodecyl benzene sulfonate 6kg, 2- naphthalene sulfonic acids first Aldehyde polymer sodium salt 4kg, ammonium sulfate 5kg, starch sulfate 2kg, diatomite 3.First diatomite and levogyrate alpha-terpineol are added It is uniformly mixed in batch mixer, then by ametryn, diuron, calcium dodecyl benzene sulfonate, 2- naphthalene sulfonic acid formaldehyde polymers sodium salt, sulphur Sour ammonium, which sequentially adds in batch mixer, to be sufficiently mixed, and being crushed to fineness in material addition micro jet after mixing reaches To 600 mesh, then the material after crushing is added in batch mixer and is mixed 1 hour, forms certain density premix.Sulfuric ester is formed sediment Powder is with water by weight 1:2 are uniformly mixed, and are fully gelatinized at 80 DEG C.Premix is added together with the starch sulfate after gelatinization Enter and water dispersible granules are made in Squeezinggranulator, after drying, cooling, screening, inspection, carries out finished product packing.
Embodiment 14
Levogyrate alpha-terpineol 4kg, 2 first 4 chlorine sodium 12kg, ametryn 48kg, diuron 15kg, polycarboxylate family macromolecule point Powder 5kg, sodium laureth sulfate 3kg, diammonium hydrogen phosphate 10kg, white carbon 3kg.After mixture is sufficiently mixed uniformly, carry out Ultra micro air-flow crushing obtains 750 mesh fine powders, then suitable water is added in gained fine powder in kneader and is mediated, and is made through squash type Grain machine is granulated, in fluidizing fluid-bed at 50 DEG C drying to get to water dispersible granules.
Embodiment 15
Levogyrate alpha-terpineol 10kg, ametryn 30kg, calcium dodecyl benzene sulfonate 3kg, ethoxylated dodecyl alcohol 6kg, Ethylene glycol 2kg, n,N-Dimethylformamide 49kg.By levogyrate alpha-terpineol, ametryn, calcium dodecyl benzene sulfonate, laruyl alcohol Polyoxyethylene ether, ethylene glycol sequentially add stirring in n,N-Dimethylformamide and obtain missible oil to equal liquid phase.
Embodiment 16
Levogyrate alpha-terpineol 12kg, diuron 30kg, calcium dodecyl benzene sulfonate 2kg, alkane ethyl phenol polyethenoxy ether 8kg, N-Methyl pyrrolidone 48kg.By levogyrate alpha-terpineol, diuron, calcium dodecyl benzene sulfonate, alkane ethyl phenol polyoxy second Alkene ether sequentially adds stirring in N-Methyl pyrrolidone and obtains missible oil to equal liquid phase.
Embodiment 17
2 first 4 chlorine sodium 5kg, ametryn 20kg, diuron 15kg, levogyrate alpha-terpineol 8kg, polycarboxylate family macromolecule point Powder 6kg, xanthans 0.1kg, soybean oil 10kg, methyl oleate supply 36kg.Reaction kettle is added in soybean oil and methyl oleate After start stirring, put into 2 first, 4 chlorine sodium, ametryn, diuron, levogyrate alpha-terpineol, polycarboxylic acid salt's macromolecule dispersing agent successively Xanthans is added into sand mill after stirring evenly to be ground, until grain size is to being made dispersible oil-suspending agent 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, antifoaming agent polypropylene glycerol aether 0.3kg, soybean oil 42kg.By 2 4 chlorine sodium of first, ametryn, diuron, levogyrate alpha-terpineol, soybean oil and calcium dodecyl benzene sulfonate, phenethyl phenol polyoxyethylene Ether is put into togerther progress level-one sand milling in sand mill, two level and three-level sanding is carried out after filtering respectively again, until active compound is uniform Dispersion is crushed to until colloidal particle size is 5 μm or less, and it is that can be made into and can divide that antifoaming agent polypropylene glycerol aether and ethylene glycol, which is added, Dissipate oil-suspending agent.
Embodiment 19
2 first 4 chlorine sodium 5kg, ametryn 20kg, diuron 12kg, levogyrate alpha-terpineol 9kg, sodium lignin sulfonate 3kg, fat Fat alcohol polyoxyethylene ether 3kg, phenethyl phenol polyethenoxy ether 4kg, xanthans 0.5kg, sorbierite 0.5kg, rapeseed oil are supplied 44kg.Sodium lignin sulfonate, fatty alcohol polyoxyethylene ether, phenethyl phenol polyethenoxy ether, xanthan are sequentially added in rapeseed oil Glue, sorbierite, mixing, stirring, 2 first, 4 chlorine sodium, green bristlegrass are added with stirring in 1500~10000 revs/min of rotating speed of high-speed shearing machine It goes out after net, diuron, levogyrate alpha-terpineol, shears 10~40 minutes, then until being ground to grain size less than 5 μm through sand mill, i.e., Dispersible oil-suspending agent is made.
Embodiment 20
Levogyrate alpha-terpineol 1kg, 2 first 4 chlorine 30kg, ametryn 35kg, diuron 25kg, calcium dodecyl benzene sulfonate 2kg, Ethoxylated dodecyl alcohol 1kg, n,N-Dimethylformamide 7kg.By levogyrate alpha-terpineol, ametryn, dodecyl benzene sulfonic acid Calcium, ethoxylated dodecyl alcohol sequentially add stirring in n,N-Dimethylformamide and obtain missible oil to equal liquid phase.
Embodiment 21
Levogyrate alpha-terpineol 90kg, ametryn 1kg, phenethyl phenol polyethenoxy ether 3kg, dodecyl sodium sulfate 2kg are recessed Convex stick soil 4kg.Above-mentioned substance is uniformly mixed, is ground, dispersible oil-suspending agent is obtained.
(levogyrate alpha-terpineol is compounded with 2 first, 4 chlorine sodium, ametryn or diuron to bidens pilosa embodiment 22 respectively Indoor virulence)
By indoor biometrics, the synergy feelings after 4 chlorine sodium of levogyrate alpha-terpineol and 2 first, ametryn or diuron compounding are specified Condition surveys object using 4 leaf phase bidens pilosas (Bidens pilosa) as raw, selects and do not applied herbicide soil, pH6.8, It after soil is air-dried sieving, is packed into the plastic flowerpot (having pallet) of diameter 32cm, deep 20cm, it is consistent that 15 plants of stalwartnesses is planted per basin 4 leaf phase seedling for test.It is accurate with reference to the experiment of NY/T1155.4-2006 farm-chemical indoor determinations using cauline leaf spray-on process Then the 4th part of herbicide:Active determination test cauline leaf spray-on process is tested, and often handles 4 repetitions, often repeatedly 15 plants of plants. Levogyrate alpha-terpineol, 2 first, 4 chlorine sodium, ametryn, diuron are made into required 5 series concentration gradients, by experimental design list Cauline leaf spraying treatment is carried out to three leaf Bidens bipinnatas after mixing solely or with levogyrate alpha-terpineol, if clear water compares and be free of left-handed α-pine tar Alcohol processing control.
Synegism evaluation is carried out according to co-toxicity coefficient, calculation formula is:
ATI=(S/M) * 100
In formula:ATI-mixture surveys toxicity index;S-standard herbicide ED50;The ED of M-mixture50
TTI=TIA × PA+TIB × PB
In formula:TTI-mixtures theoretical toxicity index;TIA-A medicament toxicity index;Percentage of PA-A medicaments in mixture Content;TIB-B medicament toxicity index;Percentage composition of PB-B medicaments in mixture.
CTC=(ATI/TTI) * 100
In formula:CTC-co-toxicity coefficient;ATI-mixture surveys toxicity index;TTI-mixtures theoretical toxicity index.
Synegism evaluation is carried out according to co-toxicity coefficient, if co-toxicity coefficient >=120 are synergistic effect, if>120 co-toxicity coefficients >80 be summation action, if co-toxicity coefficient≤80 are antagonism.
Test result is shown in Table 1.1,1.2,1.3.
1.1 levogyrate alpha-terpineol of table and 2 first, 4 chlorine sodium compound the co-toxicity coefficient inhibited to bidens pilosa fresh weight
1.2 levogyrate alpha-terpineol of table compounds the co-toxicity coefficient inhibited to bidens pilosa fresh weight with ametryn
1.3 levogyrate alpha-terpineol of table compounds the co-toxicity coefficient inhibited to bidens pilosa fresh weight with diuron
It is right after ametryn or diuron are mixed with levogyrate alpha-terpineol respectively from table 1,2,3 as can be seen that 2 first, 4 chlorine sodium The ED of bidens pilosa50Value is respectively 225,380,410, and co-toxicity coefficient is respectively 144.65,141.45,143.88, greatly In 120, show 2 first, 4 chlorine sodium, ametryn or diuron is mixed with levogyrate alpha-terpineol shows different degrees of synergy and make With.Embodiment 23
For the synergy situation of 2 first of clear levogyrate alpha-terpineol pair, 4 chlorine sodium, ametryn and diuron ternary built herbicide, First have to find the optimum proportioning of 2 first, 4 chlorine sodium, ametryn and diuron three's mixture according to bioassay for herbicide method, so Afterwards according to optimum proportioning, levogyrate alpha-terpineol is introduced, determines that levogyrate alpha-terpineol matches the best synergy of ternary built herbicide Than.With the lady's-grass (Digitaria sanguinalis), the bidens pilosa of 3 leaf phases (Bidens pilosa), 4 leaves of 3 leaf phases The rhizome of nutgrass flatsedge (Cyperu rotundus) of phase surveys object as raw, and herbicide soil, pH6.8, by soil wind were not applied in selection It after dry sieving, is packed into the plastic flowerpot (having pallet) of diameter 32cm, deep 20cm, the 5 consistent leaf phases of 15 plants of stalwartnesses is planted per basin Seedling is for test.Using cauline leaf spray-on process, with reference to NY/T1155.4-2006 farm-chemical indoor determination test rule herbicides 4th part:Active determination test cauline leaf spray-on process is tested, and 4 repetitions is often handled, often repeatedly 15 plants of plants, if not drug containing Agent processing is blank control.Data statistical analysis method is with reference to NY/T 1155.7-2006 farm-chemical indoor determination test rules The 7th part of herbicide:Colby methods in the synergy measurement of mixture, calculate each mixture combinatorial theory survival rate E0It is worth, is real Difference (the E of border survival rate E values and theoretical value and actual value0-E)。E0-E>10% is synergistic effect;E0-E<- 10% is antagonism Effect;E0- E values are addition between ± 10%.
The practical weeds survival rate E of single dose and each mixture is calculated according to formula (1):
The theoretical weeds survival rate E of mixture0It is calculated by formula (2):
In formula:
The weeds survival rate of A-herbicide 1
The weeds survival rate of B-herbicide 2
The weeds survival rate of C-herbicide 3
The weeds survival rate of N-herbicide N
N-is the kind quantity of mixture herbicide
The three kinds of effect criterions shown after herbicide mixture:E0-E>10% is synergistic effect;E0-E<- 10% is Antagonism;E0- E values are addition between ± 10%.
Calculate its result such as the following table 2.
The joint toxicity measuring (Colby methods) of 2.2 first of table, 4 chlorine sodium and ametryn and diuron mixture to weeds
According to table 2 as a result, 2 first, 4 chlorine sodium in low dosage (150g a.i./hm2), ametryn is in high dose (600g a.i./hm2) under, diuron high and low dose (300,450g a.i./hm2) use the apparent synergistic effect of performance, E0-E with> 10.9.Best mixed ratio ranging from 150:600:300~150:600:450, i.e., 1:4:2~1:4:3.It is mixed to consider ternary The formulation technique and product cost of preparaton, using 2 first, 4 chlorine sodium:Ametryn:Diuron=1:4:2.3 ratio mixture, Determine that ternary herbicide optimum formula is 73%2 first, 4 chlorine sodium ametryn diuron (10+40+23).
On the basis of above-mentioned ternary Herbicidal composition screens, by 2 first, 4 chlorine sodium:Ametryn:Diuron=10:40:23 make It for an entirety, then is compounded with levogyrate alpha-terpineol, is surveyed using the eleusine indica (Eleusine indica) of 3 leaf phases as raw Target specifies the control effect to eleusine indica after mixture, using cauline leaf spray-on process, with reference in NY/T1155.4-2006 pesticides room The 4th part of bioassay test criterion herbicide:Active determination test cauline leaf spray-on process is tested, and often handles 4 repetitions, often 15 plants of plants are repeated, if it is blank control not apply chemicals treatment.Concrete outcome such as table 3.
3 levogyrate alpha-terpineol of table and first go out diuron (10+40+23) mixture to the control effect of eleusine indica
It can be seen that the levogyrate alpha-terpineol that the present invention is added can obviously increase 73% first from the above-mentioned test of pesticide effectiveness Diuron (10+40+23) mixture go out to the control effect of eleusine indica, the several ratios of levogyrate alpha-terpineol are gone out with 73% first The control effect of diuron (10+40+23) mixture mixture is all higher than 93%.And wherein with levogyrate alpha-terpineol:First is gone out enemy Grass it is grand=10:Control effect when 73 is most apparent, reaches 98.28%.
Embodiment 24 (different temperatures influences experiment to containing levogyrate alpha-terpineol effect of herbicides)
By indoor biometrics, specifies levogyrate alpha-terpineol and 73% first goes out after diuron compounding temperature to its drug effect It influences, is test target with barnyard grass (Echinochloa crusgalli), with reference to NY/T1155.4-2006 pesticide indoor biologicals Measure test rule herbicide part 1:Activity test culture dish is tested.After barnyard grass seed presoaking and germinating, life is selected It is every 20, ware in 9cm culture dishes, the unified pendulum upwards of plumule that long consistent seed, which is uniformly placed on and is covered with the internal diameter of two layers of filter paper, It puts, is separately added into 73% containing 10% levogyrate alpha-terpineol of 100,50,25,12.5,6.25,3.125 and 1.5625mg/L First is gone out diuron herbicide liquid 9ml, and comparison medicament is to be not added with 73% first of levogyrate alpha-terpineol to go out diuron, empty White control plus distilled water.Often handle 3 repetitions.Will culture dish move into plant incubator in, be respectively set 5 temperature 10,15, 20, it 25 and 30 DEG C, is cultivated 7 days in the case where humidity is 75% dark condition, measurement bud is long, calculates inhibiting rate, and DPS softwares is used in combination to return Analysis formulates dose response standard curve, seeks EC50Value, compares otherness between treatment of different temperature.In 1.5625-100mg/L agent It measures in range, the herbicide containing levogyrate alpha-terpineol is in different temperatures environment to the EC of barnyard grass50Value is shown in Table 4.
4 different temperatures of table on 73% first containing 10% levogyrate alpha-terpineol go out diuron herbicidal activity influence
From table 4, it can be seen that temperature influences the herbicide activity of weeding containing levogyrate alpha-terpineol, there is no the orders of magnitude Difference, EC at each temperature50Value difference is different less.On the whole, 73% first containing 10% levogyrate alpha-terpineol is gone out diuron Herbicide is higher than comparison medicament in 10-15 DEG C of activity of low temperature.
(different time rainfall goes out diuron WP to 73% first containing 10% levogyrate alpha-terpineol to embodiment 25 after processing The influence of effect of herbicides)
Selection barnyard grass (Echinochloa crusgalli), which is made a living, surveys target, waits for that barnyard grass grew for 4 leaf phases, singling is spare.In Auto spraying tower (pressure 0.2MPa, dose 75mL/m2, spray time 30s) and spraying treatment.Dispenser dosage be 1250g.a.i./ hm2If two processing:1. processing is that 73% first containing 10% levogyrate alpha-terpineol is gone out diuron WP, 2. processing is control 73% first of medicament is gone out diuron WP, and is set blank control and do not washed away control, and 3 repetitions are often handled.After dispenser respectively at L, 2,3,6 and 12h simulates nature rain drop erosion with the rainfall simulator for being equivalent to precipitation 30mm to each processing.Processing is placed on It is grown in greenhouse, the reaction symptom of plant after routine observation processing, 15 days observation test results.
5 different time of table washes away after processing to the histamine result (%) of barnyard grass
The serious browning young leaves deformity atrophy of base of the plant, vein is observed after processing.Different time manages disease everywhere in drenching with rain Shape is almost the same.15 days after processing, comprehensive inhibiting rate the results are shown in Table 5, and data are shown in table, 1. processing contains 10% left-handed α-pine tar 73% first of alcohol go out diuron WP different times wash away processing have 85% or more high activity, difference is unknown between processing It is aobvious.As it can be seen that after dispenser rainfall to 73% first containing 10% levogyrate alpha-terpineol go out diuron WP activity of weeding it is not bright Development ring, than 73% first of comparison medicament go out diuron WP activity it is high.Rainfall is to containing 10% levogyrate alpha-terpineol after dispenser 73% first diuron WP drug effects of going out influence little, there is 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, reference in Nanning City's Wuming County Pesticide field efficacy medicine test criterion (one) herbicide is prevented sugarcane field weed GB/T 17980.49-2000 and is carried out.It tests knot Fruit such as table 6:
Control effect of the 6 19 invention examples of table to sugarcane field weed
Note:Comparison medicament is the 4 chlorine soluble powder of sodium agent of commercially available 56%2 first, 80% ametryn wettable powder and 80% enemy The grand wettable powder of grass, April 10, spray, investigated hybrid strain preventive effect, preventive effect (%)=(CK number of weeds-medication weeds April 30 Number)/CK number of weeds × 100%.
It can go out from upper table, comparable in dosage, the present invention is better than comparison medicine to the preventive effect of weeds The effect of agent.
The Economic and Efficiency Analysis that the present invention applies in sugarcane field
In May, 2014, we were in the Nanning City Xingning District towns the Si Tang sugarcane field progress weeding test of pesticide effectiveness, test method ginseng It is carried out according to pesticide field efficacy medicine test criterion (one) herbicide prevention sugarcane field weed GB/T 17980.49-2000.It tests knot Fruit such as the following table 7.
7 present invention of table applies economic benefits comparison in the sugarcane field of mixed raw Bermuda grass
Note:May 4 sprayed, and June 4 investigated hybrid strain preventive effect, and spray 45 kilograms of water per acre.Preventive effect (%)=(CK weeds weight Amount-medication area remaining weeds weight)/CK weeds weight × 100%.
It can go out from upper table, the embodiment of the present invention is better than the preventive effect of weeds the effect of ametryn single dose, and uses The cost of herbicide is less expensive, herbicide controlling spectrum is wider, has very excellent preventive effect to the malignant weed Bermuda grass of sugarcane field, And weeding of embodiment of the present invention speed is faster, economic benefit is apparent.

Claims (8)

1. a kind of herbicidal composition containing levogyrate alpha-terpineol, it is characterised in that the raw material composition including following parts by weight:Increase Imitate agent 1-90 parts by weight, herbicidal active component 1-90 parts by weight;
Wherein, the synergist is levogyrate alpha-terpineol, and the herbicidal active component is 2 first, 4 chlorine, ametryn and diuron In one or more kinds of compounding compositions.
2. herbicidal composition according to claim 1, it is characterised in that the raw material composition including following parts by weight:Synergy Agent 2-10 parts by weight, herbicidal active component 90-100 parts by weight.
3. solid pharmaceutical preparation is made with auxiliary material cooperation, which is characterized in that institute in herbicidal composition according to claim 1 or 2 Stating auxiliary material includes:The filler of 1-30 parts by weight, the functional auxiliary material of 1-30 parts by weight;The functional auxiliary material includes surface One or more kinds of mixing in activating agent, binder and disintegrant.
4. herbicidal composition according to claim 3, it is characterised in that:
The surfactant is sodium lignin sulfonate, sodium laureth sulfate, polyoxyethylene fatty alkyl ether sulfonate, 12 Alkylsurfuric acid calcium, lauryl sodium sulfate, dodecyl sodium sulfate, calcium dodecyl benzene sulfonate, 2- naphthalene sulfonic acid formaldehyde polymers Sodium salt, calcium lignosulfonate, polyethers ichthyodin, alkanolamide sodium sulfonate of ethoxylated, dispersing agent MF, benzene One or more kinds of combinations in ethyl phenol polyethenoxy ether, polycarboxylic acid salt's macromolecule dispersing agent;
The binder is starch sulfate, polyvinylpyrrolidone or polyvinyl alcohol;
The disintegrant is anhydrous sodium sulfate, urea, ammonium sulfate or diammonium hydrogen phosphate.
5. herbicidal composition according to claim 3, it is characterised in that:The filler is precipitated calcium carbonate, hard charcoal One or more kinds of combinations in black, talcum powder, kaolin, bentonite or attapulgite.
6. liquid preparation is made with auxiliary material cooperation, which is characterized in that institute in herbicidal composition according to claim 1 or 2 Stating auxiliary material includes:The solvent of 0-50 parts by weight, the surfactant of 1-30 parts by weight, the antifoaming agent of 0-5 parts by weight, 0-5 weight The antifreezing agent of part, the thickener of 0-5 parts by weight.
7. herbicidal composition according to claim 6, it is characterised in that:
The solvent is n,N-Dimethylformamide, N-Methyl pyrrolidone, cyclohexanone, dichloromethane, mineral oil, vegetable oil Or one or more kinds of combinations in vegetable oil esters compound;
The surfactant is calcium dodecyl benzene sulfonate, ethoxylated dodecyl alcohol, sodium lignin sulfonate, polycarboxylate Family macromolecule dispersant, sodium laureth sulfate, polyoxyethylene fatty alkyl ether sulfonate, dodecyl sulphate calcium, dodecyl Sodium sulphate, dodecyl sodium sulfate, calcium lignosulfonate, polyethers ichthyodin, alkanolamide sodium sulfonate of ethoxylated, fatty alcohol One or more kinds of combinations in polyoxyethylene ether, phenethyl phenol polyethenoxy ether;
The antifoaming agent is polypropylene glycerol aether or polyether-modified silicon;
The antifreezing agent is ethylene glycol, sorbierite or glycerine;
The thickener is alumina silicate, xanthans or dispersed silica.
8. the herbicidal composition described in claim 1-7 any one is in prevention sugarcane field annual gramineous weed, broad-leaved Purposes on weeds and sedge weed.
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