CN102334499B - Application of isothiocyanate compound in preparing agricultural herbicide for controlling farmland weeds and lawn weeds - Google Patents
Application of isothiocyanate compound in preparing agricultural herbicide for controlling farmland weeds and lawn weeds Download PDFInfo
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Abstract
The invention provides applications of an isothiocyanate compound in preparing agricultural herbicide for controlling farmland weeds and lawn weeds. The isothiocyanate compound can be a single dose or a compound agent, and can be prepared into soluble liquid, emulsion in water, greese, creaming agent, and the like. The agricultural herbicide disclosed herein has the advantages of high activity towards weeds, and small dosage, and is economic, safe and practical.
Description
Technical field
The present invention relates to the application in control farmland weed and turf weed of agricultural chemicals single dose and built agent.Specifically, relate to Cruciferae Armoracia and brassica plant source compound or derivatives thereof---isosulfocyanate compound is as single dose or the built agent of weed killer herbicide controlling weeds.
Background technology
Because weeds and crops strive fertilizer, win honour for, strive space, the serious output that affects crops and quality.And some weeds is the vector of diseases and pests of agronomic crop or the place that pad volt is survived the winter, and encourages spreading and propagation of damage by disease and insect.Therefore,, for guaranteeing crops good harvest, weeding runs through from being seeded into the whole process of results.Viewing and admiring weeds in lawn not only affects attractive in appearancely, also hinders the growth of turfgrass, therefore also needs weeding.
Along with the development of China's lawn cause, the requirement of landscaping also improves day by day, weeds prevent and kill off an important step that becomes Lawn management process.In those early years, the preventing and kill off of weeds generally be take manually as main, and artificial weeding is wasted time and energy, and efficiency is low.Along with popularizing of science and technology, the application of weed killer herbicide agricultural chemicals is more and more general.Weed killer herbicide agricultural chemicals is artificial synthetic, in order to eliminate or to control weed growth, cover crop and the chemical substance of viewing and admiring lawn.Weed killer herbicide has quick, efficient, economic feature, it can increase substantially labor productivity, be to realize the requisite advanced technology of agricultural modernization, become the important leverage of stable and high agricultural yields, the improvement tool of existing cropping system is of great significance.
At present, the method for controlling weeds is mainly by chemical control method.Chemical control method is by using chemical pesticide, with medical instruments dispenser, with instant effect, efficiency is high, using method is easy, has unique application advantage.But use in a large number chemical pesticide to damage ecotope, residue of pesticide, often can work the mischief to the biology of non-target.Measure of biotic control has environmental friendliness, to the natural beneficial organism feature such as safely, is the new approaches that control of weeds need be sought to deal with problems.
Isothiocyanates (being called for short ITCs) compounds is extensively present in the plant of Cruciferae, and especially rape genus and Armoracia plant quantum of output are more considerable.In different plants, the kind of contained isosulfocyanate compound is different, wherein in majority of plant, contain allyl group isosulfocyanate and (be called for short AITC, lower same), methylisothiocyanate ester, ethyl isothiocyanate, isopentene group isothiocyanates, PITC, BITC, 1-phenylethyl isothiocyanates, 2-phenylethyl isothiocyanates.
Once several product formulation formulas that are respectively used to soil, grain, textile and tobacco warehouse that to have proposed to take allyl group isosulfocyanate in CN101133739A be main active, and the fumigating method very easily to user is provided, also indicated concrete use object and the dosage of AITC as Pesticidal products.
The four kinds of common weeds of take are controlling object, the inventor has carried out single compound bioactivity screening and compound screening seriatim to various concrete isosulfocyanate compounds, find that one group of (totally ten six kinds) isothiocyanates has good preventive effect to four kinds of different weeds respectively, two or more ITCs combination can produce synergistic effect.
The complex preparation of a kind of isothiocyanates single dose and two or more isothiocyanates is had no to open report and applies for a patent as weed killer herbicide.
Summary of the invention
The object of this invention is to provide the application of one group of isosulfocyanate compound in the agricultural herbicide for the preparation of control farmland weed and turf weed.
In order to realize the object of the invention, the invention provides the application of one group of isosulfocyanate compound in the agricultural herbicide for the preparation of control farmland weed and turf weed.
Isosulfocyanate compound of the present invention is BITC, ethyl isothiocyanate, 1-phenylethyl isothiocyanates, 2-phenylethyl isothiocyanates, isopentene group isothiocyanates, allyl group isosulfocyanate, PITC, methylisothiocyanate ester, 1-methyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates, 1-methyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates, 1-methyl-3-methyl mercapto-4-cyano pyrazole-5-aminopropan isothiocyanates, 1-methyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates, 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates, 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates, 1-phenyl-3-methyl mercapto-4-cyano pyrazole-5-aminopropan isothiocyanates or 1-phenyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates etc.
Described weeds are barnyard grass, butch clover, orchardgrass grass, cyperus iria, alternanthera philoxeroides, lady's-grass, kitchen garden, green foxtail, Siberian cocklebur etc.
The single dose that isosulfocyanate compound of the present invention can be prepared respectively, or use with the composite built agent of BITC (or allyl group isosulfocyanate) and other isothiocyanates difference.
Inventor has passed through a large amount of tests, prepare methylisothiocyanate ester (A), ethyl isothiocyanate (B), allyl group isosulfocyanate (C), isopentene group isothiocyanates (D), PITC (E), BITC (F), 1-phenylethyl isothiocyanates (G), 2-phenylethyl isothiocyanates (H), p-methylphenyl isothiocyanates (I), 1-methyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates (J), 1-methyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates (K), 1-methyl-3-methyl mercapto-4-cyano pyrazole-5-aminopropan isothiocyanates (L), 1-methyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates (M), 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates (N), 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates (O), 1-phenyl-3-methyl mercapto-4-cyano pyrazole-5-aminopropan isothiocyanates (P), the isosulfocyanate compounds such as 1-phenyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates (Q), and respectively to barnyard grass, butch clover, orchardgrass grass, cyperus iria, alternanthera philoxeroides etc. have carried out screening active ingredients.
Former medicine involved in the present invention and extraction mother liquor are all commercially available, such as Le Liji bio tech ltd, Wuhan.
The synthetic route of its substituted pyrazolecarboxylic aminopropan isothiocyanates is as follows:
Wherein, the preparation process of substituted pyrazolecarboxylic aminopropan isothiocyanates: the first step, acetonitrile is solvent, 0 ℃ of stirring reaction 4 hours, rate of charge NCCH
2r
1: CS
2: KOH=1: 1: 2, R
1representative-CN or-COOEt; Second step, drains the compound obtaining 1, is transferred to reaction vessel, adds appropriate water and methyl alcohol mixed solvent, drips the PhCH of 2 times of amounts
2cl or dimethyl suflfate, at 50 ℃ of stirring reactions, after 4 hours, after precipitation, ethyl alcohol recrystallization obtains compound 2; The 3rd step, take ethanol as solvent, adds compound 2, stirs, and at 25 ℃, drips R
2nHNH
2(R
2represent CH
3-or Ph-), 80 ℃ reflux 5 hours after, precipitation, isopropyl alcohol recrystallization obtains compound 3; The 4th step, is transferred to reaction vessel by compound 3 use DMF, then adds equimolar KOH, drips equimolarly 1 at 25 ℃, and 3-dibromopropane, drips and finish, and reacts after 6 hours, is warming up to 45 ℃, then adds equimolar NaN
3, then react after 4 hours, precipitation obtains compound 5, with THF, compound 5 is transferred in reaction vessel again, adds equimolar PhP
3, at room temperature drip equimolar CS
2, reacting after 5 hours, decompression distillation precipitation, then obtains crystal 6 with the pure crystallization of ethyl acetate.
Find after deliberation: independent fats isothiocyanates, independent aromatics isothiocyanates are on the impact of four kinds of weeds not obvious, and the isothiocyanates single dose of being combined with isothiocyanate group by pyrazole ring is stronger to the biologically active of these four kinds of weeds.In addition, the built agent by fats isothiocyanates and aromatics isothiocyanates binary combination also presents good activity of weeding to four kinds of weeds.
By the screening of single dose and complex preparation, discovery is with 1-methyl-3-methyl mercapto-4-cyano pyrazole-5-aminopropan isothiocyanates (L), 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates (N), or N, F, L, F, the activity of weeding of the binary built composition of N, C or C, L is more excellent.
Carry out in addition composite test and find that BITC (or allyl group isosulfocyanate) and other isothiocyanates are composite, all remarkable compared with single dose synergy, and reduced the usage amount of single dose, more friendly to environment, to person poultry safety, can form a kind of more preferably biogenic fumigant.
The composite weight ratio of described BITC (or allyl group isosulfocyanate) and other isothiocyanates is 1: 9～9: 1, and being preferably is 1: 4～4: 1.
Wherein, preferably other isothiocyanates are BITC, ethyl isothiocyanate, allyl group isosulfocyanate, PITC, 2-phenylethyl isothiocyanates, 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates, 1-phenyl-3-methyl mercapto-4-cyano pyrazole-5-aminopropan isothiocyanates, methylisothiocyanate ester etc.
The present invention can make pesticidal preparations well known in the art by isothiocyanates single dose and BITC (or allyl group isosulfocyanate) with other isothiocyanates built agents, such as soluble liquid, aqueous emulsion, finish, emulsifiable concentrate etc.According to different application occasion, can be made into different dosage form.
Wherein, when described single dose is made to finish, each component and weight percentage are:
Isosulfocyanate compound 1～16%,
Antioxidant 0.1～2%,
Solvent 10～85%,
Vegetable oil polishing to 100%.
Described antioxidant is Vitamin C acids material or gallic acid pentyl ester.
Described solvent is toluene, dimethylbenzene, ethyl acetate, Ethyl formate or cyclohexanone etc.
Described vegetable oil is thick rapeseed oil, castor oil, cotton oil or thick soya-bean oil etc.
Its preparation process is: first antioxidant is dropped in the isosulfocyanate compound quantitatively taking and fully mixed thoroughly; The vegetable oil and the solvent that accurate quantitative analysis are taken fully mix again; Finally above-mentioned two kinds of solution are mixed in preparing tank and continue and stir 1～3 hour.
The component of described aqueous emulsion and weight percentage are:
Isosulfocyanate compound 1～20%,
Emulsifier 4～28%,
Ascorbic acid 0.1～2%,
Solvent 10～30%,
Water polishing to 100%.
Wherein, described emulsifier is T4103 (production is changed very much in Nanjing), No. 500,602 (above two kinds of emulsifier are Zhong Mountain petrochemical iy produced), OP-10, Well201, Well205, M30 (above four kinds of emulsifier are Fujian Weir Chemical Manufacture); Described solvent is ethyl acetate or cyclohexanone.
Its preparation process is: first ascorbic acid is dropped in the isosulfocyanate compound quantitatively taking and fully mixed thoroughly; Emulsifier and solvent that accurate quantitative analysis is taken fully mix; Finally above-mentioned two kinds of solution are continued in preparing tank to stir 1～3 hour.
The component of described soluble liquid and weight percentage are:
Isosulfocyanate compound 1～20%,
Emulsifier 2～30%,
Ascorbic acid 1～10%,
Solvent polishing to 100%.
Described emulsifier is T4103 (production is changed very much in Nanjing), emulsifier No. 10, No. 500,602 (above three kinds is Zhong Mountain petrochemical iy produced), OP-10, Well201, Well205, M30 (above four kinds is Fujian Weir Chemical Manufacture); Described solvent is methyl alcohol, Ethyl formate, ethyl acetate, ethanol, dimethylbenzene or line oil, wherein take mixed solvent as good, and dimethylbenzene and a line oil are 1: 1 (V/V), and methyl alcohol and ethanol are 1: 1 (V/V).
Its preparation process is: first ascorbic acid is dropped in the isosulfocyanate compound quantitatively taking and fully mixed thoroughly; Agricultural emulsifier and solvent that accurate quantitative analysis is taken fully mix; Finally above-mentioned two kinds of solution are continued in preparing tank to stir 1～3 hour.
Described emulsifiable concentrate component and weight percentage are:
Isosulfocyanate compound: 1～40%,
Antioxidant: 0.1～2.5%,
Pesticide use emulsifier: 5～20%,
With mixed solvent, mend to 100%; Described emulsifier is one or more in agriculture breast 100#, TX-10, No. 500,602, OP500, OP10, Tween 80 or agriculture breast 600#, and described mixed solvent is the two or more mixing in toluene, dimethylbenzene, ethyl acetate or a line oil.
Described built agent is made finish, and each component and weight percentage are:
BITC (or allyl group isosulfocyanate) 1～60%,
Other isothiocyanates 0.25～20%,
Antioxidant 0.1～2%,
Solvent 10～85%,
Vegetable oil polishing to 100%;
Described antioxidant is Vitamin C acids material or gallic acid pentyl ester; Described solvent is toluene, dimethylbenzene, ethyl acetate or cyclohexanone; Described vegetable oil is thick rapeseed oil, castor oil, cotton oil or thick soya-bean oil.
Described built agent is made aqueous emulsion, and each component and weight percentage are:
BITC (or allyl group isosulfocyanate) 1～20%,
Other isothiocyanates 0.25～10%,
Emulsifier 4～28%,
Ascorbic acid 0.1～2%,
Solvent 10～30%,
Water polishing to 100%; Wherein, described emulsifier is T4103 (production is changed very much in Nanjing), No. 500,602 (above two kinds of emulsifier are Zhong Mountain petrochemical iy produced), OP-10, Well201, Well205, M30 (above four kinds of emulsifier are Fujian Weir Chemical Manufacture); Described solvent is ethyl acetate or cyclohexanone.
Described built agent is made soluble liquid, and each component and weight percentage are:
BITC (or allyl group isosulfocyanate) 1～20%,
Other isothiocyanates 0.2～20%,
Emulsifier 2～30%,
Ascorbic acid 1～10%,
Solvent polishing to 100%; Wherein emulsifier is T4103 (production is changed very much in Nanjing), No. 500,602 (above two kinds is Zhong Mountain petrochemical iy produced), OP-10, Well201, Well205, M30 (above four kinds is Fujian Weir Chemical Manufacture); Described solvent is Ethyl formate, ethyl acetate, methyl alcohol, ethanol, benzene or line oil.
Described built agent is made emulsifiable concentrate, and each component and weight percentage are:
BITC (or allyl group isosulfocyanate) 1～20%,
Other isothiocyanates 1～20%,
Antioxidant: 0.1～2.5%,
Pesticide use emulsifier: 5～20%,
With mixed solvent, mend to 100%; Described emulsifier is one or more in agriculture breast 100#, TX-10, No. 500,602, OP500, OP10, Tween 80 or agriculture breast 600#, and described mixed solvent is the two or more mixing in toluene, dimethylbenzene, ethyl acetate or a line oil.
Above production process is all completed by machine in confined conditions, avoid personnel directly to contact liquid.
Isosulfocyanate compound of the present invention is made control of weeds single dose or built agent, can adopt the mode of spraying or soil treatment to implement.
Isosulfocyanate compound of the present invention can be used for preventing and treating farmland or turf weed, and high to weeds activity, consumption is few, and economic security is applicable.
Embodiment
Following examples are used for illustrating the present invention, but are not used for limiting the scope of the invention.
The production of embodiment 1 20% BITC soluble liquid " swep " P1
Accurate quantitative analysis takes 10.64 kilograms of the former medicines of 94% BITC, at 0.2M
3in blend tank, fully mix.Accurately take 0.5 kilogram, ascorbic acid, in 5 kilograms of input blend tanks of emulsifier T4103, also again fully mix.In blend tank, accurately drop into 5.125 kilograms of Ethyl formates and 28.735 kilograms of ethyl acetate again, in blend tank, fully mix.Continue to stir 1 hour.Preparation obtains 50kg " swep " soluble liquid P1 product.
Sampling analysis, in P1 product, the content of BITC accounts for 20.02%.In product is distributed into, scribble in the aluminium pot of barrier material, 5 kilograms, every tank, amounts to 10 tanks.Hermetically sealed can mouth, the labelled content that is is " swep " P1 product of 20%.
Embodiment 2 10%1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates emulsifiable concentrate " swep " P2 produce
Accurate quantitative analysis takes 10.2 kilograms of the former medicines of 98%1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates (N), at 2M
3in blend tank, fully mix.Accurately take 10 kilograms, ascorbic acid, drop in blend tank (1) and again fully mix.In blend tank, accurately drop into 10 kilograms of ethyl acetate, 10 kilograms of castor oil again, Well205 3kg, No. 10 1kg of emulsifier, OP-10 2.5kg, remainder dimethylbenzene polishing fully mixes in blend tank.Continue to stir 1 hour.Preparation obtains 50kg containing " swep " emulsifiable concentrate P2 semi-finished product of 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates (N) 10%.
Sampling analysis, wherein the content of 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates (N) is 9.99%.In product is distributed into, scribble in the aluminium pot of barrier material, 5 kilograms, every tank, amounts to 10 tanks.Hermetically sealed can mouth, the labelled content that is is " swep " P2 emulsifiable concentrate product of 10%.
Embodiment 3 8%1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates " swep " aqueous emulsion P3 produce
Accurate quantitative analysis takes 81.6 kilograms of the former medicines of 98%1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates (O), adds 2M
3in blend tank.Accurately take 18.4 kilograms, ascorbic acid, drop in blend tank and again fully mix.In blend tank, accurately drop into 900 kilograms of ethyl acetate again, in blend tank, fully mix.Continue to stir 1 hour.Preparation obtains the aqua product of 1000KG 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates (L).
Sampling analysis, wherein the content of 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates (L) is 8%.In product is distributed into, scribble in the aluminium pot of barrier material, 5 kilograms, every tank, amounts to 200 tanks.Hermetically sealed can mouth, the labelled content that is is 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates (L) aqua product of 8%.
Embodiment 4 16% allyl group isosulfocyanate " swep " finish P4 produce
Accurate quantitative analysis takes 8.51 kilograms of the former medicines of 94% allyl group isosulfocyanate, at 2M
3in blend tank, fully mix.Accurately take 0.5 kilogram, ascorbic acid, drop in blend tank and again fully mix.In blend tank, accurately drop into 18.52 kilograms of Ethyl formates and 22.47 kilograms of cotton oils again, in blend tank, fully mix.Continue to stir 1 hour.Preparation obtains 50kg " swep " finish P4 product.
Sampling analysis, wherein the content of allyl group isosulfocyanate is 16.02%.In product is distributed into, scribble in the aluminium pot of barrier material, 5 kilograms, every tank, amounts to 10 tanks.Hermetically sealed can mouth, the labelled content that is is " swep " P4 finish product of 20%.
The production of embodiment 5 12% allyl group isosulfocyanates and 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates built agent finish synergy " swep " emulsifiable concentrate P5 of 1.3%
Accurately take approximately 12.75 kilograms of the former medicines of AITC of 94% content, 1.44 kilograms of the former medicines of 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates of content 90%, 1 kilogram, ascorbic acid stirs three in blend tank.In blend tank, quantitatively add 10 kilograms of emulsifier TX-10 again, 5 kilograms of T4103,17.5 kilograms of thick cottonseed oils, supplement ethyl acetate to 100kg, and limit edged stirs, and after all material adds, continues to stir 1 hour with agitator.
In sample examination product, containing the amount of AITC, be 11.98%, methylisothiocyanate ester content is 1.30%, finally obtains active princlple total content and be 2 tons of " swep " emulsifiable concentrate products of 13.3%, product with 500ml glass bottle bottle sealing with embodiment 1.
Embodiment 6 1% BITCs and 7%1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates built agent synergy " swep " soluble liquid P6 produce
Accurate quantitative analysis takes 20%AITC and extracts 77.8 kilograms of the former medicines that 50 kilograms, mother liquor and 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanate content are 90%.Two kinds of active liquids are fully mixed in blend tank (1).Accurately take again 15 kilograms, ascorbic acid, drop in blend tank (1) and again fully mix.In blend tank (2), add 40 kilograms of agricultural emulsifier NO．600s, No. 10 120 kgs of emulsifier, after mixing, add again 712.2 kilograms, ethyl acetate, fully mix.872.2 kilograms of materials in blend tank (2) are all moved in allotment (1) by pipeline, after hermetically sealed can mouth, start agitator and stir 1 hour.Preparation obtains 1000 kilograms of soluble liquid products.
In sampling analysis product, the content of AITC is 1.01%, 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanate content is 6.99%, be hermetically sealed can mouth, the labelled content that is is 8% built agent product synergy " swep " soluble liquid P6 product.Product is distributed in the plastic bottle of dual obstruct to every bottled medicine 500mL.
The production of embodiment 7 2% BITCs and 8% 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates built agent soluble liquid synergy " swep " P7
Accurately take 21.28 kilograms of the former medicines of AITC of 94% content, 89 kilograms of the former medicines that content is 90%, 20 kilograms, ascorbic acid stirs three in blend tank.In blend tank, quantitatively add 100 kilograms of agricultural emulsifier Well201 again, 180 kilograms of cyclohexanone, 180 kilograms of castor oil, add 409.72 kilograms, water, and limit edged stirs, and after all material adds, continues to stir 1 hour with agitator.
Amount containing AITC in sample examination product is 2%; 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanate content is 8%; finally obtain active princlple total content and be 1 ton of " swep " P7 product of 10%, product with 500mL glass bottle bottle sealing with embodiment 1.
The production of embodiment 8 20% allyl group isosulfocyanate soluble liquid " swep " P8
Accurately take 10.64 kilograms of 94% allyl group isosulfocyanate crude oil, 0.5 kilogram, ascorbic acid, 4.5 kilograms of emulsifier well201, drop in blend tank, fully mix.Again to accurately dropping into methyl alcohol in blend tank: ethanol=1: 34.36 kilograms of 1 mixed solvents, in blend tank, fully mix and continue stirring 1 hour, obtain 50kg " swep " P8 product.
Sampling analysis, in P8 product, the content of allyl group isosulfocyanate is 19.98%.Product is distributed in aforementioned aluminium pot, 1 liter, every tank, totally 52 tanks, sealing paste label is final products.
The production of embodiment 9 40%1-phenyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates emulsifiable concentrate " swep " P9
Accurately take 22.2 kilograms of 90% the former medicines of 1-phenyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates; 3 kilograms of No. 500, emulsifier, OP-103 kilogram, 10 kilograms of castor oil, 25.65 kilograms of dimethylbenzene, 0.5 kilogram, ascorbic acid; drop into 200L blend tank and fully mix and continue stirring 1 hour, obtain 50 kilograms of " swep " P9 products.
Sampling analysis, in product, the content of 1-phenyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates is 39.9%.The bilayer that product is distributed into 1000ml intercepts in plastic bottle, and sealing paste label becomes the finished product of " swep " P9.
The production of amino isothiocyanates emulsifiable concentrate " swep " P10 of embodiment 10 12%1-phenyl-3-methyl mercapto-4-cyano pyrazoles-5-
Accurately take 6.65 kilograms of the amino isothiocyanates of 1-phenyl-3-methyl mercapto-4-cyano pyrazole of 90.5%-5-, 3 kilograms of No. 10,3 kilograms, No. 500,0.5 kilogram, ascorbic acid, emulsifier, emulsifier, 12 kilograms of rapeseed oils, 15 kilograms of dimethylbenzene, 10.15 kilograms of methyl alcohol, input 200L allotment is whole to be mixed and continues stirring 1 hour, obtains 50 kilograms of " swep " P10 products.
Sampling Detection, contains the amino isothiocyanates 11.96% of 1-phenyl-3-methyl mercapto-4-cyano pyrazole-5-in product.By embodiment 9 packing labeling, become final products.
Embodiment 11 20%1-methyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates emulsifiable concentrates (swep P11) are produced
Accurately take 10.55 kilograms of the former medicines of 1-methyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates (content is 95%), 0.5 kilogram, ascorbic acid, 4 kilograms of emulsifier " 602 ", 3 kilograms of well205, dimethylbenzene and line oil (1: 1, v/v) 32.0 kilograms, drop in 200L blend tank, fully stir evenly, obtain 50 kilograms of " swep " P11 products.
Sampling Detection, contains 1-methyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates 20.0% in product.By embodiment 9 packing, label and become " swep " P11 finished product.
Embodiment 12 10%1-methyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates and 10% benzyl RBITC built agents (missible oil), " swep " P12 produces.
Accurately take 5.2 kilograms of 1-methyl-3-benzylthio-4-ethoxycarbonyl former medicines of pyrazoles-5-aminopropan isothiocyanates (content 96%), 5.32 kilograms of the former medicines of BITC (content 94%), 0.5 kilogram, ascorbic acid, the mixed solvent of 4 kilograms of No. 500, emulsifier, 3 kilograms of M30,1 kilogram of OP-10, dimethylbenzene and a line oil (1: 1, v/v) polishing to 100% by weight, drop in blend tank and stir, obtain 50 kilograms of " swep " P12 semi-finished product.
Sampling Detection, in product, 1-methyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanate content is 10.10%, BITC content is 10.05%.Product becomes finished product by embodiment 9 packing.
Embodiment 13 10% allyl group isosulfocyanates add the production of the different sulphur chlorate of 5%1-methyl-3-methyl mercapto-4-cyano pyrazole-5-aminopropan compounded cream agent (" swep " P13)
Accurately take 5.32 kilograms, the former powder of allyl group isosulfocyanate (content 94%), 2.75 kilograms of 1-methyl-3-methyl mercapto-4-former medicines of the different sulphur chlorate of cyano pyrazole-5-aminopropan (content 91%), 0.5 kilogram, ascorbic acid, 4 kilograms of No. 500, emulsifier, OP-104 kilogram, dimethylbenzene 33.43. kilogram.Raw material is dropped in 200L blend tank, stir, obtain 50 kilograms of the semi-finished product of " swep " P13.
Sampling Detection, contains allyl group isosulfocyanate 10.07% in " swep " P13 product, contains the different sulphur chlorate 4.98% of 1-methyl-3-methyl mercapto-4-cyano pyrazole-5-aminopropan.Press embodiment 9 bottling labeling, become " swep " P13 finished product.
Embodiment 14 10%1-methyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates add the production of the composite finish of 6% methylisothiocyanate ester (" swep " P14)
Accurately take 5.56 kilograms of 1-methyl-3-methyl mercapto-4-ethoxycarbonyl former medicines of pyrazoles-5-aminopropan isothiocyanates (content 90%); 3.30 kilograms of the former medicines of methylisothiocyanate ester (91% content); 0.5 kilogram of gallic acid pentyl ester; 3 kilograms, ethyl acetate; 37.64 kilograms of thick rapeseed oils; drop in 200L blend tank and stir, obtain 50 kilograms of " swep " P14 semi-finished product.
In product, content detection result is 1-methyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates 10.03%, methylisothiocyanate ester 5.99%.By embodiment 9 packing, obtain " swep " P14 finished product.
The production of the 1-phenylethyl isothiocyanates of embodiment 15 10% and 2.5% allyl group isosulfocyanate compounded cream agent " swep " P15
Accurately take 5.27 kilograms of the former medicines of 1-phenylethyl isothiocyanates (content 95%), 1.33 kilograms of the former medicines of allyl group isosulfocyanate (content 94%), 0.5 kilogram of gallic acid pentyl ester, 4.5 kilograms of emulsifier well205,3.5 kilograms of OP-10,12.5 kilograms, ethyl acetate, 22.4 kilograms of methyl alcohol, drop into blend tank after stirring " swep " P15 semi-finished product, this example is prepared 50 kilograms of " swep " P15 semi-finished product.
In sampling Detection product, the content of two kinds of effective ingredients is: 1-phenylethyl isothiocyanates 9.97%, allyl group isosulfocyanate 2.51%.By embodiment 9 packings, be " swep " P15 finished product.
The production of the 2-phenylethyl isothiocyanates emulsifiable concentrate (" swep " P16) of embodiment 16 25%
Accurately take 13.45 kilograms of the former medicines (content 93%) of 2-phenylethyl isothiocyanates, 0.5 kilogram, ascorbic acid, 4 kilograms of No. 500, emulsifier, 2 kilograms of OP-10,10 kilograms, ethyl acetate, 20.05 kilograms of dimethylbenzene, drop into blend tank, stir, obtain 50 kilograms of " swep " P16 semi-finished product.
Sampling Detection, in product, 2-phenylethyl isothiocyanate content is 25.06%.By embodiment 9, be distributed into the double-deck plastic bottle that intercepts of 500ml, be " swep " P16 product.Embodiment 1715% ethyl isothiocyanate adds 5% BITC compounded cream (" swep " P17)
Accurately take 7.90 kilograms of the former medicines of ethyl isothiocyanate (content 95%), 2.66 kilograms of the former medicines of BITC (content 94%), 0.5 kilogram, ascorbic acid, 5 kilograms of No. 10, emulsifier, 5 kilograms of OP-10,10 kilograms of dimethylbenzene, 18.94 kilograms of methyl alcohol, drop in 200L blend tank, stir, become effective component content and be " swep " P17 semi-finished product of 20%.
After testing, in product, contain ethyl isothiocyanate 15.02%, BITC 5.00%.Product is pressed embodiment 16 packing, becomes the finished product of " swep " P17.
Embodiment 18 10% PITCs add 2% BITC compounded cream (" swep " P18)
Accurately take 5.22 kilograms of the former medicines of PITC (content 96%), 1.07 kilograms of the former medicines of BITC (content 94%), 0.5 kilogram of gallic acid pentyl ester, well2055 kilogram, 5 kilograms of OP-10, mixed solvent (dimethylbenzene: line oil=1: 1v/v) 33.21 kilograms, obtain 50 kilograms of " swep " P18 semi-finished product after input blend tank fully mixes.
Two kinds of effective component contents in product are respectively after testing: PITC 10.10%, BITC 2.03%.Product is packaged into product P 18 by embodiment 16.
Embodiment 19 2.5% BITCs add 15% methylisothiocyanate ester soluble liquid (" swep " P19)
Accurately take 1.33 kilograms of the former medicines of BITC (content 94%), methylisothiocyanate 7.5kg, add emulsifier T41035kg, methyl alcohol and alcohol mixed solvent (1: 1v/v) 36.17 kilograms, drop into blend tank, stir, obtain " swep " P19 semi-finished product that 50 kilograms of total effective ingredients are 17.5%.
Product is through sampling Detection, and wherein effective component content is: BITC 2.51%, methylisothiocyanate ester 15.04%.The bilayer that is sub-packed in 500ml intercepts in plastic bottle and labeling, becomes " swep " P19 finished product.
Embodiment 20 20% isopentene group isothiocyanates add 4% allyl group isosulfocyanate missible oil (" swep " P20)
Accurately take 10.42 kilograms of the former medicines of isopentene group isothiocyanates (content 96%), 2.13 kilograms of the former medicines of allyl group isosulfocyanate (content 94%), 0.5 kilogram, ascorbic acid, 8 kilograms of No. 500, emulsifier, the mixed solvent (1: 1v/v) 22.95 kilograms that dimethylbenzene and line oil form, 6 kilograms of castor oil, drop in 200 liter blend tanks and continue to stir 1 hour, obtain " swep " P20 semi-finished product that 50 kilograms of total effective component contents are 24%.
Product content testing result is: isopentene group isothiocyanates 19.97%, allyl group isosulfocyanate 4.09%.With the Aluminum Bottle packing that is coated with barrier layer in 500ml, become " swep " P20 finished product.
Embodiment 21 10% BITCs add 3% p-methylphenyl isothiocyanates compounded cream agent (" swep " P21)
Accurately take 5.32 kilograms of the former medicines of BITC (content 94%), 1.57 kilograms of the former medicines of p-methylphenyl isothiocyanates (content 96%), 0.5 kilogram, ascorbic acid, 5 kilograms of No. 10, emulsifier, No. OP-10 3 kilograms, 5 kilograms, ethyl acetate, 5 kilograms of dimethylbenzene, 24.61 kilograms of methyl alcohol, drop into blend tank, continue to stir 1 hour, obtain 50 kilograms of " swep " P21 semi-finished product.
Product sampling Detection, two kinds of active ingredient content in " swep " P21 are BITC 10.02%, p-methylphenyl isothiocyanates 3.00%.With bilayer, intercept plastic bottle and be packed as 500ml/ bottle, obtain active ingredient total content and be " swep " P21 product of 13%.
The production of embodiment 22 1% allyl group isosulfocyanates and 10% the composite aqueous emulsion of PITC " swep " P22
Accurately take AITC content and be about 100 kilograms, 10% plant extract mother liquor, 108.7 kilograms of the former medicines of PITC content 92%, 20 kilograms, ascorbic acid stirs three in blend tank.In blend tank, quantitatively add agricultural emulsifier Well201120 kilogram again, 200 kilograms of cyclohexanone, 180 kilograms of castor oil, add 271.3 kilograms, water, and limit edged stirs, and after all material adds, continues to stir 1 hour with agitator.
In sample examination product, containing the amount of AITC, be 1.01%, PITC content is 10.0%, finally obtains active princlple total content and be 1 ton of " swep " P22 product of 11.01%, product with 500mL glass bottle bottle sealing with embodiment 16.
Experimental example 1
In booth vegetable ground, Wuhan Le Liji company proving ground, choose the field of three long-term growing vegetables, every field 100m
2.Adopt the mode of trench digging dispenser, every 1m, open a ditch, the 20% allyl group isosulfocyanate soluble liquid (P1) that directly uses embodiment 1 to produce, consumption is 125ml.Use 20% napropamide missible oil to make medicament contrast, every 100m
2consumption is 100ml.Two kinds of processing spray earthing, add water, spread immediately thick film, and after airtight 14 days, spacious gas four days, checks after two months the strain number of weeds, and add up its preventive effect.Result shows, fumigates and processes the wildness again that soil can significantly reduce weeds, and preventive effect reaches 80% left and right.
The field test results that table 1 " swep " P1 prevents and kill off upland weeds
Experimental example 2
There is the aquatic weeds such as a large amount of barnyard grasses, water peanut, nutgrass flatsedge, dayflower in farmland, Jiangxia District township, Hubei, so that hazard rice is produced.Spray formulated " swep " P2 by embodiment 2, contrast medicament adopts 10% Bentazon aqua, adopts random small plot experiment, and result is as follows.Each community 25m
2，Mei investigates community 5 points, and investigation area is 1m
2.In the paddy rice 4-6 leaf phase, spray medicine, can not cause poisoning to paddy rice.30 days investigation pesticide supplying effects after medicine, when P2 medicament is used 100g/ mu, preventive effect reaches 60-70%, is significantly higher than 10% Bentazon aqua.
The field test results that table 2 " swep " P2 prevents and kill off farmland weed
Experimental example 3
Farm, Dongxihu District, Wuhan City, Hubei Province, water peanut grows in a large number, chooses a uniform field of growth, is divided into 1m
2experimental plot, each processes four repetitions, carries out randomized block experiment.Spray according to 8% " swep " aqueous emulsion P3 that implements 3 configurations, every mu of consumption 120g, dilutes 1000 times.Contrast medicament adopts the phonetic semi-annular jade pendant mamaplasty of 20% fluorine oil formulation, and blank is clear water contrast, and after medicine, 30 days statisticses are as follows.
The field test results that table 3 " swep " P3 prevents and kill off water peanut
Result shows, 8%L " swep " aqueous emulsion P3 is being used 120g/ mu, and successful is better than the grand 120g/ mu of the phonetic semi-annular jade pendant of 20% fluorine.
Experimental example 4
Farm, Yichang City, Hubei Province corn field, spring is weedy.Spray formulated " swep " P1,2,3,8,9,10,11,16 by embodiment 1,2,3,8,9,10,11,16, contrast medicament is used 30% gyphosate solution, adopts random small plot experiment, divides each community 4m
2，Mei investigates community 4 points, and investigation area is 0.25m
2.Result is as follows, and the preventive effect of medicament P2 contrasts higher than medicament, and the preventive effect of medicament P8 significantly contrasts lower than medicament.
The field test results that table 4 " swep " single dose series is prevented and kill off corn ground weed
Experimental example 5
In booth base, Dongxihu District, Wuhan, Hubei, choose the luxuriant soil block of weeds in former years, harvesting crops is complete, weeds are all sliced off, before seedling, carry out soil treatment, blank, athomin single dose, " grass go out spirit " P5 are set, 200 times of " swep " P5 dilutions of then embodiment 5 being produced, in each cave, add 300ml, cover nylon film, after stifling 14d, spacious gas 5d.Add up after two months the weeds weight of three fields, athomin single dose, chemicals treatment group, preventive effect is only 80%, 92% respectively, compound drug contrasts, single dose AITC has improved 12%.
Experimental example 6
Cheng Ningshi farm, Hubei Province corn field, weedy.Spray formulated " swep " P6 by embodiment 6, contrast medicament adopts " swep " P6 medicament of pressing embodiment 2 preparations, adopts random small plot experiment, and result is as follows.Divide each community 64m
2，Mei investigates community 4 points, and investigation area is 1m
2.In the corn 3-5 leaf phase, spray medicine, can not cause poisoning to corn.30 days investigation pesticide supplying effects after medicine, when P6 medicament is used 100g/ mu, preventive effect reaches 90%, is significantly higher than single dose.
The field test results that corn ground weed is prevented and kill off in the composite system of table 5 " swep " P6 and single dose agent
Experimental example 7
In 20 mu of soybeans of suburb township, Chengdu, Sichuan a slice, many weeds that growing, adopt random small plot experiment, and result is as follows.Divide each community 64m
2，Mei investigates community 4 points, and investigation area is 1m
2.Fresh weight efficiency test for soybeans weeds, during dispenser, soybean is the 4-5 leaf phase, weeds 2-3 leaf phase dispenser sprays by medicaments such as formulated " swep " P2 of embodiment 7, " swep " P6, " swep " P7,20% Brominal missible oil, 50% atrazine wetting powders, and after medicine, investigation in 32 days is to weeds fresh weight preventive effect.After medicine, 30 days investigation pesticide supplying effects, when P7 pharmacy control efficacy is the highest, reach the object of eliminating weeds substantially, and reduce the consumption of single dose.
Table 6 " swep " P7 prevents and kill off the field test results of soybeans weeds
Experimental example 8
Xiangfan City, Hubei Province farm soybeans, spray formulated " swep " P5, P6, P7, P12, P13, P14, P15, P17, P18, P19, P20, P21 by embodiment 5,6,7,12,13,14,15,17,18,19,20,21, contrast medicament is used 14.5% benazolin haloxyfop-r-methyl ethametsulfuron wetting powder, adopt random small plot experiment, divide each community 64m
2，Mei investigates community 4 points, and investigation area is 1m
2.Result is as follows, and the preventive effect of medicament P6 contrasts higher than medicament.
Table 7 " swep " built agent series is prevented and kill off the field test results of soybeans weeds
The stifling impact of processing suppressing weed seed germination of experimental example 9 compounds
In each container, add different compound drugs, make the amount of active ingredient and stifling volume of a container ratio be: 12.5 μ g/ml, airtight stifling.3 repetitions are established in each processing, and clear water contrast is set.Stifling processing after 7 days, opens wide container to place 4 days, then from each container, divides and gets 100 of seed samples as germination test.Germination rate experimental condition is 26 ± 1 ℃, keeps seed moistening, maintains germination condition 3-6 days, checks seed sprouting situation, calculates germination rate, and result of the test is in Table 8.
The result of the test of the stifling impact of the germination rate on weed seed of table 8 12.5 μ g/ml ITCs
Various seed is after the stifling processing of ITCs as can be seen from Table 8, and its germination rate has significant difference, but stifling concentration for the treatment of is had to strict boundary, and the germination rate of most of seed all can have obvious decline in one week.Allyl group isosulfocyanate fumigation activity is the highest, can under low concentration, suppress preferably the sprouting of seed.
The impact of experimental example 10 compounds on seed germination
Prepare 16 kinds of compounds and be mixed with the solution that concentration is 50 μ g/ml, take each seed 200g and be immersed in medicament, be immersed in medicament after seven days, take out 120 of each seed and make germination test, four repetitions are set, each processes 30.Germination rate experimental condition is 26 ± 1 ℃, keeps seed moistening, maintains germination condition 3-6 days, checks seed sprouting situation, calculates germination rate, and result of the test is in Table 9.
From the results shown in Table 9; suppressing the highest compound of suppressing weed seed germination activity is 1-phenyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates; secondly be 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates, BITC.
The ITCs of table 9 50 μ g/ml soaks the result of the test of the germination rate impact after weed seed
Experimental example 11 cauline leafs are processed
1) activity test to barnyard grass
Barnyard grass final singling after germination and emergence is processed to community 20 strains to each, and medicament is 1000 μ g/ml for examination concentration, adopts cauline leaf spray-on process to process.Each is processed and repeats 4 times, and establishes respectively clear water contrast and solvent control.The results are shown in Table 10, the mean value that in table, remaining strain number is 4 repetitions, remaining strain fresh weight is the strain mean value of remaining plant.
The activity test of ten kinds of compounds of table 10 to barnyard grass
* note: lowercase indicates 0.05 significant difference.
As shown in Table 10, under 1000mg/kg concentration, to barnyard grass, growth all has certain inhibitory action to 10 kinds of compounds, wherein the correction strain preventive effect of G and E reaches respectively 83.42% and 77.64%, the active N > L > O > K > Q > P > M > J > I > C of being of inhibition that barnyard grass is survived, and there is significant difference with solvent control, to the inhibitory action of barnyard grass fresh weight relatively a little less than, it suppresses active size is N > L > O > I > C > M > K > J > Q > P.
2) activity test to cyperus iria
Cyperus iria final singling after germination and emergence is processed to community 20 strains to each, and medicament is 1000mg/kg for examination concentration, adopts cauline leaf spray-on process to process.Each is processed and repeats 4 times, and establishes respectively solvent control and clear water contrast.The results are shown in Table 11, the mean value that in table, remaining strain number is 4 repetitions, remaining strain fresh weight is the mean value of remaining plant.
The activity test of ten kinds of compounds of table 11 to cyperus iria
* note: lowercase indicates 0.05 significant difference.
As shown in Table 11, under 1000mg/kg concentration, to cyperus iria, growth all has certain inhibitory action to 10 kinds of compounds, the active N > L > O > Q > M > P > K > I > J > C of being of inhibition that cyperus iria is survived, to the inhibitory action of cyperus iria fresh weight relatively a little less than, it suppresses active size is N > Q > O > L > P > J > K > C > M > I.
3) activity test to orchardgrass
Orchardgrass final singling after germination and emergence is processed to community 20 strains to each, and medicament is 1000mg/kg for examination concentration, adopts cauline leaf spray-on process to process.Each is processed and repeats 4 times, and establishes respectively solvent control and clear water contrast.The results are shown in Table 12, the mean value that in table, remaining strain number is 4 repetitions, remaining strain fresh weight is the mean value of remaining plant.
The activity test of ten kinds of compounds of table 12 to orchardgrass
* note: lowercase indicates 0.05 significant difference.
As shown in Table 12, under 1000mg/kg concentration, to orchardgrass grass, growth all has certain inhibitory action to 10 kinds of compounds, the active N > L > O > Q > M > P > K > I > C > J of being of inhibition that orchardgrass grass is survived, to the inhibitory action of orchardgrass grass fresh weight relatively a little less than, it suppresses active size is N > L > M > P > Q > O > K > I > J > C.
4) activity test of dialogue three leaves
Bai Sanye final singling after germination and emergence is processed to community 20 strains to each, and medicament is 500mg/kg for examination concentration, adopts cauline leaf spray-on process to process.Each is processed and repeats 4 times, and establishes respectively solvent control and clear water contrast.The results are shown in Table 13, the mean value that in table, remaining strain number is 4 repetitions, remaining strain fresh weight is the mean value of remaining plant.
The activity test of ten kinds of compound dialogue three leaves of table 13
* note: lowercase indicates 0.05 significant difference.
As shown in Table 13, under 1000mg/kg concentration, to orchardgrass grass, growth all has certain inhibitory action to 10 kinds of compounds, the active N > L > Q > O > M > P > K > I > J > C of being of inhibition that orchardgrass grass is survived, to the inhibitory action of orchardgrass grass fresh weight relatively a little less than, it suppresses active size is N > Q > L > P > O > M > K > I > J > C.
Experimental example 12 soil-fumigatings are processed
The blue or green sandstorm gathering is shone and a week gets rid of all weeds, and insulation, moisturizing, through after a period of time, then mix above-mentioned sand (absolute water content approximately 20%), and pack in flowerpot every basin 2kg into.50,125,250mg/kg (active ingredient and soil weight ratio) then, by following concentration gradient:, respectively complex preparation is imbedded to about 5cm place in basin, every basin is sown into 20mg barnyard grass seed, then pours into a small amount of clear water simultaneously.Finally, basin alms bowl and the sand of having executed medicine are sealed to 7d with plastic membrane of polyvinyl chloride, open wide after 4d, do not execute the blank that is treated to of any medicament simultaneously, each is processed and repeats 4 times.Statistics after 15 days, result is as follows.
Table 14 barnyard grass efficiency test result statistics
In notes table, N represents 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates, and A represents allyl group isosulfocyanate.
From the above results, can find out, the control efficiency of single dose AITC, 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates, when 125mg/kg processes, the average preventive effect of remaining plant reaches respectively 46%, 57%, the weight ratio of compound drug allyl group isosulfocyanate and N is 4: during 1125mg/kg, preventive effect can reach 78%, has significantly improved the control efficiency of AITC, has reduced the usage amount of AITC management of weeds.
Experimental example 5, cauline leaf spray complex treatment
From Hua Zhong Agriculture University's teaching practice farm, gather alternanthera philoxeroides seedling, choose the basically identical plant of size standby; On planting in each basin, quantity alternanthera philoxeroides seedling is about equally cultivated 20 days.BITC and two kinds of former medicines of compound of 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates are pressed (9: 1; 4: 1; 2: 1,1: 1,1: 2; 1: 4; 1: 9) ratio carries out the screening of best proportioning, and blank is set simultaneously, and during screening, each is processed 5 concentration gradients is set respectively; each concentration arranges three repetitions, the alternanthera philoxeroides of each reprocessing one basin growing way homogeneous.By measuring processed group alternanthera philoxeroides lethality, filter out synergy proportioning.
As can be seen from Table 15, when 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates: when the ratio of BITC is 4: 1, prevent and kill off the EC of alternanthera philoxeroides
50be 320 μ g/ml, CTC reaches 140, and synergy is remarkable, has reduced the consumption of compound N.
The composite alternanthera philoxeroides results from pot experiment test of preventing and kill off of two kinds of compounds of table 15
Note: in table, N represents 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates, and B represents BITC.
From Hua Zhong Agriculture University's teaching practice farm, gather alternanthera philoxeroides seedling, choose the basically identical plant of size standby; On planting in each basin, quantity alternanthera philoxeroides seedling is about equally cultivated 20 days.BITC and two kinds of former medicines of weed killer herbicide are pressed (9: 1,4: 1,2: 1,1: 1,1: 2,1: 4,1: 9) ratio carries out the screening of best proportioning, and blank is set simultaneously, and during screening, each is processed 5 concentration gradients is set respectively, each concentration arranges three repetitions, the alternanthera philoxeroides of each reprocessing one basin growing way homogeneous.By measuring processed group alternanthera philoxeroides lethality, filter out synergy proportioning.
As can be seen from Table 16, when 1-phenyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates: when the ratio of BITC is 4: 1, prevent and kill off the EC of alternanthera philoxeroides
50be 300 μ g/ml, CTC reaches 150, and synergy is remarkable, has reduced the consumption of compound N.
The composite alternanthera philoxeroides results from pot experiment test of preventing and kill off of two kinds of compounds of table 16
Note: in table " L " represent 1-phenyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates, " B " represents benzyl isothiocyanic acid.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements, all belong to the scope of protection of present invention without departing from theon the basis of the spirit of the present invention.
Claims (5)
1. the application of isosulfocyanate compound in the agricultural herbicide of preparation control farmland weed and turf weed, it is characterized in that, described isosulfocyanate compound is selected from 1-methyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates, 1-methyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates, 1-methyl-3-methyl mercapto-4-cyano pyrazole-5-aminopropan isothiocyanates, 1-methyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates, 1-phenyl-3-benzylthio-4-cyano pyrazole-5-aminopropan isothiocyanates, 1-phenyl-3-benzylthio-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates, 1-phenyl-3-methyl mercapto-4-cyano pyrazole-5-aminopropan isothiocyanates, one or more in 1-phenyl-3-methyl mercapto-4-ethoxycarbonyl pyrazoles-5-aminopropan isothiocyanates.
2. application according to claim 1, is characterized in that, the formulation of described agricultural herbicide is finish, aqueous emulsion, soluble liquid or emulsifiable concentrate.
3. application according to claim 2, is characterized in that, during described finish, each component and weight percentage are:
Isosulfocyanate compound 1～16%,
Antioxidant 0.1～2%,
Solvent 10～85%,
Vegetable oil polishing to 100%.
4. application according to claim 2, is characterized in that, during described aqueous emulsion, each component and weight percentage are:
Isosulfocyanate compound 1～20%,
Emulsifier 4～28%,
Ascorbic acid 0.1～2%,
Solvent 10～30%,
Water polishing to 100%.
5. application according to claim 2, is characterized in that, the component of described soluble liquid and weight percentage are:
Isosulfocyanate compound 1～20%,
Emulsifier 2～30%,
Ascorbic acid 1～10%, solvent polishing to 100%.
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Non-Patent Citations (3)
| Title |
|---|
| "Herbicidal activity of eight isothiocyanates on Texas panicum (Panicum texanum), large crabgrass (Digitaria sanguinalis), and sicklepod (Senna obtusifolia)";Jason K. Norsworthy等;《Weed Science》;20050731;第53卷(第4期);第515页摘要 * |
| Jason K. Norsworthy等."Herbicidal activity of eight isothiocyanates on Texas panicum (Panicum texanum), large crabgrass (Digitaria sanguinalis), and sicklepod (Senna obtusifolia)".《Weed Science》.2005,第53卷(第4期),第515页摘要. |
| JP昭6-1043192A 1986.03.01 |
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