CN110352975A - A kind of Synergistic herbicide compositions of wheat paddock containing isoproturon - Google Patents
A kind of Synergistic herbicide compositions of wheat paddock containing isoproturon Download PDFInfo
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- CN110352975A CN110352975A CN201910627209.3A CN201910627209A CN110352975A CN 110352975 A CN110352975 A CN 110352975A CN 201910627209 A CN201910627209 A CN 201910627209A CN 110352975 A CN110352975 A CN 110352975A
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/82—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/30—Derivatives containing the group >N—CO—N aryl or >N—CS—N—aryl
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Abstract
The invention discloses a kind of synergistic herbicidal pesticide composites, with N- (5- tert-butyl -1,3,4- thiadiazoles -2- bases)-N'- (2,6- difluoro pyridine -4- base)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidines (TDCA-10) and isoproturon are that acceptable auxiliary element collectively constitutes in effective component, with pesticide, wherein the permission weight ratio of TDCA-10 and isoproturon is 50:1 to 1:50 in Herbicidal combinations of the present invention, and better ratio is 10:1 to 1:10.By indoor pot experiment and field efficacy experiment, synergistic effect is formed after showing two kinds of combination of active principles, and degrass spectrum can be expanded, while without antagonism, crop safety is improved.
Description
Technical field
The present invention relates to a kind of weeding class composition pesticides, especially for wheat paddock, Soybean Field and tomato, capsicum,
The vegetable farm herbicides such as potato, nursery leek, pimento, eggplant, semen viciae fabae, pea, onion.
Background technique
China is one of yield wheat big country, the world, and wheat yield is sure to occupy the first in the world for many years.However China's weeds of wheat
It is numerous, it is easy to influence wheat yield and quality.The main weeds of wheat paddock have Descurainia sophia, barnyard grass, wild avena sativa, willow leaf thorn smartweed, acid
Mould leaf knotweed, volume stem smartweed, Chenopodiaceae, Amaranthus retroflexus, Siberian cocklebur, bur beggar-ticks, dayflower, weasel hemp nettle, artemisia, sowthistle, field thistle, setose thistle, acid
Mould etc..China's wheat field herbicide passes through years of researches, has had very more kinds to occur, has mainly had: 69g/L essence oxazole
Diclofop-methyl EW, 69 grams per liter fenoxapropPethyls+safener, 3% mesosulfuron WP, 3.6% iodosulfuron-methyl-sodium methyl two
The grand WDG(0.6:3 of sulphur), the grand WDG(5:1.25 of the phonetic methiodide of 6.25% acyl), 70% flucarbazone WDG, 75% tribenuron-methyl DF, 50 grams/
Rise pinoxaden alkynes oxalic acid EC(2.5:2.5), 480 grams per liter dicamba AS, 15% alkynes oxalic acid WP, 20% fluroxypyr
EC, 58g/ rise double phonetic sulphur SC(25:33 of fluorine azoles), 559g/ rise florasulam 2,4-D isobutyl ester SC(0.6:45.3), 7.5%
Pyroxsulam WDG, the different monooctyl ester SC of 43% florasulam dimethyl tetrachloride, 15% couple of fluorine fluroxypyr SC(0.5:14.5).
Although can be used for wheat field herbicide kind at present, it is enough, part herbicide kind still has phytotoxicity, or
There is resistance after a period of use in the more quality herbicide of person, it is therefore necessary to the new and effective wheat paddock weeding of continual exploitation
Agent.
China is also one of Chan Mian big country, the world, wherein being main production cotton with provinces and regions such as Shandong, Ji, Henan, Soviet Union, Hubei Province, new, Anhui
Area.Weed in cotton field mainly has 24 sections about more than 60, wherein with the herba digitariae in gramineae weed, herba eleusines indicae, semen euphorbiae, non-irrigated barnyard grass, dog
It is maximum that density occurs for tail grass, Paspalum distichum, Bermuda grass etc.；Broadleaf weeds with Eclipta prostrata, Amaranthus retroflexus, argy wormwood, chenopodium glaucum linn, Acalypha-austratis-L,
Based on piemarker etc.；Sedge weed is based on the rhizome of nutgrass flatsedge.In Yellow River basin cotton region, with the rise of temperature, cotton after sowing cotton seed
A variety of weeds start rudiment successively in field, until mid or late May field formed first emergence peak, at this time with herba setariae viridis, herba digitariae,
Based on non-irrigated barnyard grass, Chenopodiaceae etc., with rainfall and pour water later it may also occur that primary small germination peak；To July, with arriving for rainy season
Come, the weeds such as rhizome of nutgrass flatsedge are largely unearthed, and second germination peak is formed, and at the same time, the weeds that early period is unearthed enter growth most
The flower phase, thus easily cotton is caused seriously to cause harm.China cotton field is widely distributed, and different cotton region weed communities and dominant population have
Institute is different.Yangtze river basin cotton region has a moderate climate with heavy rainfall, is suitable for weed growth, dominant weed is with herba digitariae, herba eleusines indicae and rhizoma cyperi
Based on son.North china to like to form based on cool resistance to early weeds various weed communities, common weed mainly have herba digitariae, Bermuda grass,
Dish etc. is a variety of.Since the herbicide kind of single type is used for a long time, the variation of farmland weed population and the succession of community accelerate, certain
Secondary weeds are increasingly becoming main weeds, and intractable weed harm is got worse, and increase chemical weed control difficulty.China cotton field chemistry
Weeding there are the problem of be that method of administration is improper first.The distribution of China cotton field is wide, the generation of planted in different ecological areas weeds and applies weeding
Primary and secondary wants the succession of herbaceous of weeds still to lack further investigation after agent, and not formed formula of targetedly preventing and kill off is to the section of numerous cotton growers
Deficiency is educated in general education, the not perfectly flat weighing apparatus of various regions application technology level, because selecting medicament and administration time, dosage method etc. in practice
Improper often result in phytotoxicity.Late, fundamental research is weaker, cotton field chemical weed control product for China cotton field chemical weed control starting
It is kind less, it carries out in a deep going way and more effectively applies there is an urgent need to research.These factors need cotton field herbicide continuous
Release that effect is more preferable, the wider array of new varieties of degrass spectrum.
In addition, the farmlands such as Soybean Field, sugarcane field, corn field, Rapeseed Field, tea place and bare place weeding equally have it is numerous miscellaneous
Grass.By taking common soybean weeds as an example, soybean weeds can be divided into three categories in the sense that preventing and kill off, i.e. annual gramineae
Weeds, annual broadleaf weed and perennial weeds.Soybean Field annual gramineous weed mainly has barnyard grass, herba setariae viridis, golden dog
Tail grass, wild broomcorn millet, herba digitariae, wild avena sativa etc..Soybean Field annual broadleaf weed mainly has Amaranthus retroflexus, Siberian cocklebur, black nightshade (black star), iron
Three-coloured amaranth, Chenopodiaceae (Chenopodium album), bog marshcress herb, piemarker, water spine pin, willow leaf thorn smartweed, herba stellariae mediae, wolf tail grass (ghost fork), salsola collina, elscholtiza (open country Soviet Union
Son), purslane, pale persicaria, dayflower (orchid dish), Semen Cuscutae etc..Soybean Field perennial weeds mainly has sowthistle, meadow pine
(section bone grass), field thistle (field thistle), setose thistle (cottonsedge-like thistle herb), reed, alkali grass etc..From in recent years, in most of China
Area is all presented a kind of trend, dayflower, wolf tail grass, pale persicaria, Siberian cocklebur, black nightshade, bog marshcress herb, piemarker, sowthistle, field thistle, big
The broadleaf weeds such as Ji have gradually replaced the gramineae weeds such as barnyard grass, wild avena sativa, herba setariae viridis and have become Soybean Field main weeds.It is small
Ji, sowthistle, dayflower are more known as Soybean Field " three dishes ", become the difficult point that soybean weeds are prevented and kill off.Soybean Field chemistry removes
Careless agent usage mode is generally taken and broadcasts preceding or soil treatment before seedling sowing and stem and leaf treatment after seedling two ways.Before broadcasting or after broadcasting
It is management of weeds the advantages of soil treatment before seedling in the budding period and before causing damages, herbicidal effect is more stable, dispenser cost
It is relatively low, even if management of weeds is bad compared with fruit, can also be remedied after seedling.Disadvantage: first is that pH value, by soil types, organic
Matter content is affected, and is not suitable for when soil excessively glues weight, the content of organic matter is excessively high or pH value does not meet certain medicament using soil
Earth processing；Second is that some herbicides such as metribuzin, 2,4-D butyl ester etc. are also easy to produce in sand soil, low-lying land due to the leaching of medicament
Phytotoxicity；Third is that be affected by meteorological condition, especially spring arid, wind is big and abnormal low temperature or high temperature can all influence weeding effect
Fruit.The advantages of stem and leaf treatment after seedling be influenced by soil types, the content of organic matter, soil moisture it is smaller, can be according to being unearthed
The suitable herbicide with strong points of weeds type selection.Disadvantage: first is that in drought, air humidity is small and weed growth is slow
Herbicidal effect is bad in the case where slow；Second is that some medicaments are also easy to produce phytotoxicity under the conditions of too high or too low for temperature；Third is that after seedling
Cauline leaf process must just can be carried out when most of weeds are unearthed and have the leaf area of certain adhering liquid medicine, at this time soybean early period
Growth is influenced by crop smothering, causes the underproduction.Therefore, Soybean Field chemical weed control is generally based on soil treatment, after seedling at cauline leaf
Supplemented by reason., radix biggish plot more to weeds type needs to carry out secondary chemical weed control.Therefore Soybean Field chemical weed control,
It flexibly to be grasped in implementation process, particular problem concrete analysis.Due to, soil property difference in all parts of the country is larger, and climate difference is significant,
Increase the difficulty of soybean field weeding.
(denomination of invention: application number CN2015100098343, January 9 2015 date of application contain three nitrogen to Chinese patent
1,2,3- thiadiazoles -5- formamidine the compound of heterocycle and synthesis) in report the artificial Xihua Univ (inventor of patent application
The town Wang Hui, Liu Ping, Yang Wei are clear etc.) general formula be TDCA the polysubstituted -1,2,3- thiadiazoles -5- formamidine compound of N- and its conjunction
At method (formula 1).Chinese patent reports patent in (application number CN2015100237806, January 19 2015 date of application)
Apply for the polysubstituted -1,2,3- thiadiazoles -5- of N- that artificial Xihua Univ (inventor Liu Ping, Yang Wei clear etc.) mutual-through type is TDCA
The novel synthesis of formamidine compound is reported that the new method uses the synthesis of target product and is first cyclized, finally upper first
The method of base obtains fine experiment effect.Chinese patent (application number CN2015103042053, June 9 2015 date of application
Day, denomination of invention: cyclization method synthesize polynitrogen heterocycle thiadiazoles -5- formamidine compound) in report the artificial Xihua of patent application
University's (inventor Yang Weiqing, Liu Ping etc.) mutual-through type is the polysubstituted -1,2,3- thiadiazoles -5- formamidine compound of N- of TDCA
Novel synthesis reported that the new method is to the synthesis of target product using first upper methyl, and the method being finally cyclized, this is new
The easy preparation of synthetic method high income, catalyst, catalyst is cheap, phosphorus-containing wastewater is few, to more environment-friendly.Chinese patent
(application number CN2015100238141, January 19 2015 date of application, denomination of invention: 1 containing three azacyclo-s, 2,3- thiophenes
Diazole -5- formamidine new herbicides) in report the artificial Xihua Univ of patent application (inventor Zhang Yan, Liu Ping, Yang Weiqing
Deng) general formula be TDCA N- polysubstituted -1, purposes of 2, the 3- thiadiazoles -5- formamidine compounds as herbicide, main use
Broadleaf weeds and gramineae weed are prevented and kill off in farmland.General formula be TDCA compound in TDCA-10(formula 2), TDCA-6(formula
3), TDCA-13(formula 4) there is good activity of weeding, annual gramineae weed and broadleaf weeds can be effectively prevented and kill off, but
It is that limited inhibitory effect can only be played to part perennial weeds, degrass spectrum is not extensive enough.Therefore general formula is the chemical combination of TDCA
Object so as to further expansion degrass spectrum, and reduces use cost it is necessary to use with other mixture of herbicides.
Isoproturon is initially to be developed by French Rhone-Poulenc company in the beginning of the seventies in last century, Full Name in English N, N-
Dime- thyl-N-[4- (1-methylethyl) phenyl] urea, English abbreviation Isoproturon, experiment code name are
LS69-1299.Isoproturon Chinese chemical name is known as N, N- dimethyl-N-(4- isopropyl phenyl) urea, molecular formula C12H18N2O,
CAS 34123-59-6, structural formula are as shown in Equation 5.Isoproturon raw medicine appearance is white powdery solids, fusing point 158-159
DEG C, under the conditions of 25 DEG C, it is not dissolved in water (0.07 g/L, 25 DEG C), methanol (56 g/L, 25 DEG C), acetone (82 g/ can be dissolved in
L, 25 DEG C), a variety of organic polar solvents such as methylene chloride (63 g/L, 25 DEG C).But solubility is smaller in low polar solvent: benzene
(6 g/L, 25 DEG C), n-hexane (0.2 g/L, 25 DEG C).
Isoproturon can prevent and kill off Chenopodiaceae as inner sucting conduction type processing soil treatment agent and cauline leaf process agent, annual bluegrass, and herba digitariae etc. 1 year
Raw weeds, to crop safety.After plant root absorbs isoproturon inorganic agent, transporting is simultaneously accumulated in blade, inhibits photosynthesis,
Cause weeds withered.Isoproturon system phenyl ureagroup herbicides are the inhibitor of photosynthesis electron transmission, are interfered photosynthetic
It carries out, oxygen and carbon dioxide cannot be released under light illumination, organic matter, which generates, to be stopped, and susceptible weeds are withered because of starvation.Isoproturon
Different from other hormone like herbicides, light reception intensity does not influence the environment of generation effect, or even at a fairly low temperature still
Effectively.This feature of isoproturon is actually also a double-edged sword, it is easy to generate jelly to plant there is also a significant drawback
Evil phenomenon: especially sensitive to wheat, there are jelly phytotoxicity, (isoproturon can reduce the freezing tolerance of wheat, meet serious frostbite after application
It is easy to happen jelly phytotoxicity, phytotoxicity degree increases with the increase of formulation rate, and the dosage for controlling isoproturon advantageously reduces jelly phytotoxicity
Risk), when especially application phase temperature is low, applies isoproturon and want and pay attention to warming up head application in cold tail, guarantee 1 week left side after application
The right side does not occur daily minimal tcmperature in 2 DEG C of weather below.Isoproturon is to spring wheat field annual grassy weeds significant effect and to crop
Safety.Isoproturon can prevent and kill off annual grassy weeds, such as herba digitariae, Chenopodiaceae, annual bluegrass, amur foxtail, be mainly used for wheat paddock, Soybean Field and
The vegetable farm herbicides such as tomato, capsicum, potato, nursery leek, pimento, eggplant, semen viciae fabae, pea, onion.Isoproturon has soil concurrently
Closing and cauline leaf process effect, degrass spectrum is also wider, can prevent and kill off the weeds such as hard grass, Wang grass, annual bluegrass, amur foxtail, wild avena sativa, special
Be not to have certain complementation with clodinafop-propargyl better than clodinafop-propargyl to the preventive effects of the weeds such as annual bluegrass, before weeds are unearthed and
Weeds Seedling Stage optimum period, suitable moisture in the soil medication are generally per acre with 125 grams of 50% isoproturon wettable powder.There is also one for isoproturon
A feature, half-life period is longer, has researcher once to carry out half-life experiments with laboratory loamy soil, and measurement isoproturon half-life period is
20 days, and the comparative experiments under similarity condition shows that the half-life period of 2,4- drop and atrazine is respectively 3 days and 36 days.Isoproturon
Toxicity is smaller, and effect on environment is not significant.Acute toxicity: LD50=3350mg/kg(mouse oral)；LD50=3600 mg/kg(are big
Mouse is oral), while any stimulation is not generated to test animal skin and mucous membrane.Subacute toxicity: with 400ppm concentration
Food is fed with rat 3 months, without any symptom, and is more than 2 weeks observation periods also without any symptom of discovery；It is fed with dog 3
The concentration that toxicity is not presented for a month is no more than 100ppm.In addition, isoproturon is to aquatic animal, there are certain risks: to trout and catfish
Fish belongs to low toxicity.
It is more to its synthesising process research although isoproturon structural formula is relatively easy, according to using the primary raw material can be with
It is roughly divided into following five kinds of synthesis technologies.Process one (and initial synthesis technology, phosgene technique): with cumic aldehyde
Amine is that starting material and phosgene react generation intermediate 4- cumene isocyanic acid, intermediate 4- cumene isocyanic acid into
One step and dimethylamine carry out condensation reaction and obtain isoproturon, and due to the use of hypertoxic phosgene, production process is absolutely unsafe, this method
It has basically been eliminated at present；Process two (urea technique): being starting material and urea in strong acid (salt using cumidine
Acid) under the conditions of carry out reaction generate intermediate 4- isopropyl phenyl urea, intermediate 4- isopropyl phenyl urea further with dimethylamine
It carries out condensation reaction and obtains isoproturon, due to the use of a large amount of concentrated hydrochloric acids, production process is larger to equipment corrosion, while concentrated hydrochloric acid
It finally neutralizes and generates a large amount of inorganic salts solid sodium chlorides；Process three (N- replaces three chloroethene phthalein amine techniques): with p-isopropyl
Aniline is that starting material carries out reacting generation intermediate p-isopropyl tribromo-acetyl aniline with trichloro-acetic chloride in anhydrous conditions,
Intermediate p-isopropyl tribromo-acetyl aniline further with dimethylamine in DMSO as solvent, it is sodium hydroxide catalyzed in inorganic strong alkali
Under the conditions of, it carries out condensation reaction and obtains isoproturon, since dimethyl alum is expensive, only applied in laboratory research；Work
Process four (triphosgene, and the improvement to initial optical self-encoding technique): using cumidine as starting material with
Triphosgene (BTC) carry out reaction generate intermediate 4- cumene isocyanic acid, intermediate 4- cumene isocyanic acid further with
Dimethylamine carries out condensation reaction and obtains isoproturon, and due to the phosgene without using severe toxicity, production process safety is significantly improved, the party
Method has become the main synthesizing mean of isoproturon at present；This method has a distinguishing feature: being easy to generate diaryl urea
By-product can inhibit the generation of the by-product in production process very well using anti-dripping method.(the methylchloroformate work of process five
Skill): react with methylchloroformate generating intermediate cumidine formic acid first as starting material using cumidine
Ester, intermediate cumidine methyl formate further carries out condensation reaction with dimethylamine and obtains isoproturon, due to not using
The phosgene (and comparatively safe triphosgene) of severe toxicity, while also without isocyanate intermediate process, this method is in safety
Property aspect have very big advantage, therefore after completely solving cost and quality problem, which has biggish potential answer
Use feasibility.Therefore, because it is undesirable to there is the weeds effect big to careless age in isoproturon single variety preparation use process, and hold
The problems such as phytotoxicity easily is generated to diversified economy crop, therefore isoproturon can be used in compounding, so as to further expansion degrass spectrum.
Summary of the invention
For above situation, the present invention will report that one kind can effectively prevent and kill off annual gramineae weed and broad-leaved is miscellaneous
Grass, and can inhibit efficient, the safe weeding pesticide composition of part perennial weeds can be used for wheat paddock, Cotton Fields, big
The farmlands such as beans field, sugarcane field, corn field, Rapeseed Field and bare place weeding.Especially it is used for wheat paddock weeding.Although aforementioned China
Patent (application number CN2015100238141, January 19 2015 date of application, denomination of invention: 1 containing three azacyclo-s, 2,
3- thiadiazoles -5- formamidine new herbicides) in report the artificial Xihua Univ of patent application (inventor Zhang Yan, Liu Ping, poplar
Dimension is clear etc.) general formula be purposes of polysubstituted -1,2, the 3- thiadiazoles -5- formamidine compound of N- of TDCA as herbicide, lead
It is used to prevent and kill off broadleaf weeds and gramineae weed in farmland.But this kind of formamidine compound is prepared into preparation and is used alone still
There are degrass spectrums not enough extensively, unit dispenser cost is higher, requires the defects of high to certain weeds careless ages.In order to overcome in other words one
Determine to reduce these defects in degree, in initial experimentation We conducted TDCA respectively with atrazine, terbufos benzthiazuron,
Nearly 40 kinds of flufenacet, nicosulfuron, clodinafop-propargyl etc. the herbicide kinds that can prevent and kill off broadleaf weeds and gramineae weed carry out
Combine a large amount of screening experiments of (combination including three kinds of herbicide components).Finally, we pass through a large amount of indoor and field experiments
And further Economic Evaluation, have found the Synergistic herbicide compositions of TDCA and isoproturon.It has surprisingly been found that the increasing
It imitates Herbicidal combinations and is used for wheat paddock selective herbicidal, not only herbicidal effect is good, has notable synergistic effect, and make to economy
Object wheat does not have any phytotoxicity.
Herbicidal combinations of the present invention are N- (5- tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,6- bis- with Chinese
Fluorine pyridin-4-yl)-N, [English name is N- (5-tert-butyl-1,3,4- to 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidine
thiadiazol-2-yl)-N'- (2,6-difluoropyridin-4-yl)-N,4-dimethyl-1,2,3-
thiadiazole-5-carboxamidine；Structural formula is as shown in Equation 2, the present invention in hereinafter referred to as TDCA-10] compound
With isoproturon (Chinese N, N- dimethyl-N-(4- isopropyl phenyl) urea；English name is N, N-dime- thyl-N
ʹ-[4-(1-methylethyl)phenyl] urea；English abbreviation Isoproturon；It is referred to as in the present invention using its Chinese
Isoproturon, structural formula are as shown in Equation 5) it is that acceptable auxiliary element collectively constitutes in effective component, with pesticide；The present invention removes
The permission weight ratio of TDCA-10 and isoproturon is 50:1 to 1:50 in careless composition, and better ratio is 10:1 to 1:10.
Herbicidal combinations of the present invention can with Chinese for N- (5- tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,
6- dichloropyridine -4- base)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidine, structural formula is as shown in Equation 3；It is following in the present invention
Abbreviation TDCA-6] compound and isoproturon (Chinese N, N- dimethyl-N-(4- isopropyl phenyl) urea；English name
For N, N-dime- thyl-N-[4- (1-methylethyl) phenyl] urea；English abbreviation Isoproturon；The present invention
Middle to be referred to as isoproturon using its Chinese, structural formula is as shown in Equation 5) be in effective component, with pesticide acceptable auxiliary at
Divide and collectively constitutes；The permission weight ratio of TDCA-6 and isoproturon is 50:1 to 1:50 in Herbicidal combinations of the present invention, preferably
Ratio is 10:1 to 1:10.
Herbicidal combinations of the present invention can with Chinese for N- (5- tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,
6- dibromo pyridine -4- base)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidine, structural formula is as shown in Equation 4；It is following in the present invention
Abbreviation TDCA-13] compound and isoproturon (Chinese N, N- dimethyl-N-(4- isopropyl phenyl) urea；English name
Referred to as N, N-dime- thyl-N-[4- (1-methylethyl) phenyl] urea；English abbreviation Isoproturon；This hair
It is bright middle as shown in Equation 5 using its Chinese referred to as isoproturon, structural formula) it is acceptable auxiliary in effective component, with pesticide
Ingredient collectively constitutes；The permission weight ratio of TDCA-13 and isoproturon is 50:1 to 1:50 in Herbicidal combinations of the present invention, more preferably
Ratio be 10:1 to 1:10.
Herbicidal combinations of the present invention can be to have with any two kinds in TDCA-10, TDCA-6, TDCA-13 and isoproturon
Acceptable auxiliary element collectively constitutes in effect ingredient, with pesticide.Herbicidal combinations of the present invention can be with TDCA-10, TDCA-
6, the mixture of tri- kinds of TDCA-13 of arbitrary proportion is assisted with acceptable in isoproturon composition effective component, with pesticide again
Ingredient collectively constitutes.
Acceptable auxiliary element in described pesticide, including used in pesticide at present, unfavorable shadow will not be generated
Loud all kinds of common solvents and/or inert filler and/or surfactant and/or preservative and/or antifreezing agent and/or agglomeration resistance
Agent and/or defoaming agent and/or cosolvent and/or the corresponding adding ingredient such as stabilizer and/or thickener, and can be according to being produced
Dosage form do corresponding selection or adjustment.
Agrochemical formulations generally comprise the Herbicidal combinations of the present invention of 0.1-99 weight %, especially 2-90 weight %.?
Herbicidal combinations concentration is in wettable powder (WP), such as the rest part in 10-90 weight %, 100 weight % is by routinely making
Agent auxiliary element composition.Herbicidal combinations concentration is in suspending agent (SC), such as 1-90 weight %, preferably 5-75 weight %, 100
Rest part in weight % is made of conventional formulation auxiliary element.Herbicidal combinations concentration is in suspoemulsion (SE), such as 1-
90 weight %, preferably 5-75 weight %, the rest part in 100 weight % are made of conventional formulation auxiliary element.In water dispersant
(WDG) Herbicidal combinations concentration is in, such as 1-95 weight %, preferably 10-70 weight %, and the rest part in 100 weight % is by normal
Regulation agent auxiliary element composition.The preparation of other powder types includes 1-40 weight % reactive compound, and preferably 5-20 weight % is living
Property compound, the rest part in 100 weight % are made of conventional formulation auxiliary element.
Herbicidal combinations of the present invention are needed according to different uses or application Huan Jing ∕ condition, raw by current conventional pesticide
TDCA-10 in the Herbicidal combinations and isoproturon effective component and corresponding auxiliary element are sufficiently mixed by production mode for raw material,
It is prepared into various forms of available corresponding dosage forms.Possible dosage form includes: microcapsule formulations, wettable powder, moisture
Powder, suspending agent, aqueous emulsion, suspoemulsion, microcapsule formulations etc..Such as several typical common dosage forms and preparation can be with:
Microcapsule formulations (CJ), which refer to, forms " core-shell structure copolymer " structure small container using natural or synthesis high molecular material, by pesticide
It coats wherein, and the formulations of pesticide in water that suspend.Micro-capsule suspension appearance is a thick working fluid, with aqueous emulsion
And aqueous suspension agent is similar.With micro- sem observation, its shape of microcapsules is spherical in shape, rugby shape, grain or other shapes.Microcapsules
Diameter is generally at 3-30 microns.Small rice grain and mung bean grain size are about as much as with the observation of 400 power microscopes.Due to microcapsules agriculture
Medical instrument has the features such as lasting period is long, toxicity is low, safe ready, just becomes a developing direction of pesticides new formulation.Microcapsules
Customary preparation methods have complex coacervation, Simple coacervation, interfacial polymerization, situ aggregation method, orifice-coagulating bath method etc..It is several recently
There is some novel processing steps, such as molecular inclusion, microchannel emulsification method, supercritical fluid quick expansion method, ferment again in year
Female microcapsule method, self-assembled multilayer film method.Microcapsules often have sodium alginate, chitosan, gelatin, porous-starch etc. with wall material.?
Complex coacervation is most popular method in above-mentioned microcapsule preparation method.Complex coacervation preparation principle is with two kinds with opposite charges
Substance make embedded object, core material disperses wherein, to change change pH values, temperature or solution concentration, due to the effect between charge, make two kinds
Wall material solubility declines and is condensed into microcapsules precipitation.A kind of positively charged colloidal solution and another negatively charged colloid
Solution mutually mixes, and since the interaction between xenogenesis charge forms compound polyelectrolyte and separates, and is deposited on capsule-core week
It encloses and obtains microcapsules.Complex coacervation is often capsule material with gelatin, Arabic gum.Gelatin is protein, in aqueous solution, strand
It is upper to contain-NH2With-COOH and its accordingly dissociate group-NH3 +With-COO-, but contain-NH3 +With-COO-How much is ion, by medium
The influence of pH value.For gelatin solution in pH 4.0 or so, positive charge is most.Arabic gum is polysaccharide, in aqueous solution, point
Contain-COOH and-COO in subchain-, there is negative electrical charge.Therefore in gelatin and Arabic gum mixed aqueous solutions, pH is adjusted about
When being 4.0, gelatin and Arabic gum form compound because charged phase neutralizes instead, and solubility reduces, and are condensed into from system
Capsule is precipitated.Curing agent formaldehyde is added, formaldehyde and gelatin generate the condensation reaction of amine aldehyde, and gelatin molecule is cross-linked into reticular structure, protects
The shape for holding micro-capsule becomes irreversible micro-capsule；Add 2% NaOH to adjust medium pH 8 ~ 9, is conducive to amine aldehyde condensation reaction progress
Completely.
Suspending agent (SC) i.e. agricultural chemicals suspension agent (SC) is water insoluble solids pesticide or not mixed liquid pesticidal in water or oil
Dispersion.When preparation, with water or oil for decentralized medium, by TDCA-10 of the present invention and isoproturon composition and auxiliary element
(such as thickener, stabilizer, Ricinate, antifreezing agent, pH adjusting agent, defoaming agent) is made through soybean dietary fiber (grinding)
?.Wherein Ricinate is phosphate polyethers, alkylnaphthalene sulfonate, alkylbenzene sulfonate, aliphatic alcohol sulfate, alkyl bromide
Change ammonium, alkyl ammomium chloride, crown ether, quaternary alkylphosphonium salt, alkyl polyoxyethylene base ether sulfate, lignosulfonates, lignin, carboxymethyl
One of cellulose, sodium carboxymethylcellulose, azone, thiophene ketone are several；Thickener and stabilizer are polyvinyl alcohol, condensation
One of phosphate, xanthan gum, aluminum magnesium silicate etc. are several；Antifreezing agent be sodium chloride, urea, ammonium sulfate, ethylene glycol,
One of glycerol etc. is several；PH adjusting agent is potassium dihydrogen phosphate, dipotassium hydrogen phosphate, citric acid, sodium carbonate, potassium carbonate etc.
One of or it is several.Organosilicon is commonly used as defoaming agent and foam inhibitor.
Suspoemulsion (SE) the i.e. hybrid dispersions of the insoluble pesticide of water in water, one such effective component is in suspension
State, other effective components are in emulsion state.It can be by the present composition and corresponding emulsion, wet point when being prepared when preparation
The auxiliary elements such as powder, thickener, stabilizer, antifreezing agent, pH adjusting agent, defoaming agent, conventionally, through wet process Ultramicro-powder
It is broken to be mixed to prepare.Wherein emulsifier is alkyl phenol polyoxyethylene ether class (agriculture breast 100#), alkylbenzene sulfonate (agriculture breast 500#), benzene
Ethyl phenol polyethenoxy ether class (agriculture breast 600#), alkyl phenol or aralkyl phenol polyethenoxy ether formaldehyde condensation species (Nongru-700 #)
Deng one of or it is several.Wherein Ricinate is lignosulfonates, lignin, phosphate polyethers, carboxymethyl fibre
Tie up element, sodium carboxymethylcellulose, crown ether, alkylnaphthalene sulfonate, alkylbenzene sulfonate, aliphatic alcohol sulfate, alkyl ammonium halide, season
One of phosphonium salt, alkyl polyoxyethylene base ether sulfate, azone, thiophene ketone are several；Thickener and stabilizer are polyethylene
One of alcohol, condensed phosphate, xanthan gum, aluminum magnesium silicate etc. are several；Antifreezing agent be sodium chloride, urea, ammonium sulfate,
One of ethylene glycol, glycerol etc. are several；PH adjusting agent be potassium dihydrogen phosphate, dipotassium hydrogen phosphate, citric acid, sodium carbonate,
One of potassium carbonate etc. is several.Organosilicon is commonly used as defoaming agent and foam inhibitor.
Water dispersible granules (WDG) can fater disintegration in water, and can be uniformly dispersed in formation higher suspension dispersion in water
A kind of granular preparation of system.The present composition and auxiliary element one can be reinstated to air-flow smashing or ultra-fine grinding when preparation,
Wettable powder is made, this is dry method；The present composition, auxiliary agent, adjuvant etc. are ground in sand mill using water as medium
Mill, is made suspending agent, and then re-dry is granulated, this is wet process.
Wettable powder (WP), i.e., solid powder preparation that in water can be evenly dispersed.It, can be according to conventional side when preparation
Formula is firstly added the composition of TDCA-10 and isoproturon of the present invention, and diatomite, clay, precipitated calcium carbonate, hard charcoal is then added
The common diluent such as black or inert substance add other common auxiliary elements, as alkylnaphthalene sulfonate, alkylbenzene sulfonate,
Aliphatic alcohol sulfate, alkyl bromination ammonium, alkyl ammomium chloride, quaternary alkylphosphonium salt, alkyl polyoxyethylene base ether sulfate, lignin sulfonic acid
One of salt, lignin, carboxymethyl cellulose, sodium carboxymethylcellulose, azone, thiophene ketone are several, and common stabilization
The complementary auxiliary component such as agent, foam inhibitor, anticaking agent.
It should be noted that specific dosage form mentioned above is the representative dosage form that the present composition can be prepared, enumerate not
It is limited to these above-mentioned dosage forms.
Concrete mode by the following examples is again described in further detail above content of the invention.But it does not answer
This range for being interpreted as the above-mentioned theme of the present invention is only limitted to example below by this.The above-mentioned technical idea feelings of the present invention are not being departed from
Under condition, the various replacements or change made according to ordinary skill knowledge and customary means, should all include of the invention
In range.Each material composition ratio is weight % in embodiment.
Specific embodiment:
The Herbicidal combinations TDCA-10 isoproturon wettable powder (WP) of embodiment 1:50%
100 grams of TDCA-10,400 grams of isoproturons, 35 grams, 35 grams lignosulfonates calcium of pull powder Bx, 35 grams of carboxylics are weighed respectively
Sodium carboxymethylcellulose pyce, 30 grams of aluminum magnesium silicates, 35 grams of neopelexes, 20 grams of tetrabutylammonium bromide, 310 grams of kaolin,
It is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The Herbicidal combinations TDCA-10 isoproturon wettable powder (WP) of embodiment 2:50%
400 grams of TDCA-10,100 grams of isoproturons, 30 grams of lignosulfonates calcium, 30 grams of sodium carboxymethylcelluloses, 35 are weighed respectively
Gram aluminum magnesium silicate, 40 grams of neopelexes, 20 grams of tetrabutylammonium bromide, 330 grams of kaolin, 15 grams of pull powder Bx, it is standby
With；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The TDCA-10 wettable powder (WP) of embodiment 3:30%
Weigh respectively 300 grams of TDCA-10,25 grams, 30 grams lignosulfonates calcium of pull powder Bx, 35 grams of sodium carboxymethylcelluloses,
35 grams of aluminum magnesium silicates, 35 grams of neopelexes, 20 grams of tetrabutylammonium bromide, 560 grams of kaolin, it is spare；Preparation: will be each
Material sequentially adds in reaction kettle, and stirring mixes them thoroughly, and is crushed to 5~20 μm.
The Herbicidal combinations TAM-5 isoproturon wettable powder (WP) of embodiment 4:40%
200 grams of TDCA-10,200 grams of isoproturons, 35 grams of lignosulfonates calcium, 35 grams of sodium carboxymethylcelluloses, 25 are weighed respectively
Gram aluminum magnesium silicate, 18 grams of neopelexes, 22 grams of tetrabutylammonium bromide, 440 grams of kaolin, 25 grams of pull powder Bx, it is standby
With；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The Herbicidal combinations TDCA-10 isoproturon wettable powder (WP) of embodiment 5:40%
100 grams of TDCA-10,300 grams of isoproturons, 25 grams of lignosulfonates calcium, 35 grams of sodium carboxymethylcelluloses, 40 are weighed respectively
Gram aluminum magnesium silicate, 30 grams of neopelexes, 25 grams of tetrabutylammonium bromide, 430 grams of kaolin, 15 grams of pull powder Bx, it is standby
With；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The Herbicidal combinations TDCA-10 isoproturon wettable powder (WP) of embodiment 6:50%
250 grams of TDCA-10,250 grams of isoproturons, 45 grams of lignosulfonates calcium, 45 grams of sodium carboxymethylcelluloses, 30 are weighed respectively
Gram aluminum magnesium silicate, 25 grams of neopelexes, 25 grams of tetrabutylammonium bromide, 320 grams of kaolin, 10 grams of pull powder Bx, it is standby
With；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The Herbicidal combinations TDCA-10 isoproturon wettable powder (WP) of embodiment 7:50%
50 grams of TDCA-10,450 grams of isoproturons, 30 grams of lignosulfonates calcium, 30 grams of sodium carboxymethylcelluloses, 40 are weighed respectively
Gram aluminum magnesium silicate, 30 grams of neopelexes, 20 grams of tetrabutylammonium bromide, 330 grams of kaolin, 20 grams of pull powder Bx, it is standby
With；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The Herbicidal combinations TDCA-10 isoproturon wettable powder (WP) of embodiment 8:50%
450 grams of TDCA-10,50 grams of isoproturons, 45 grams of lignosulfonates calcium, 45 grams of sodium carboxymethylcelluloses, 30 are weighed respectively
Gram aluminum magnesium silicate, 20 grams of neopelexes, 20 grams of tetrabutylammonium bromide, 320 grams of kaolin, 20 grams of pull powder Bx, it is standby
With；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The Herbicidal combinations TDCA-10 isoproturon suspending agent (SC) of embodiment 9:30%
200 grams of TDCA-10,100 grams of isoproturons, 30 grams of lignosulfonates calcium, 30 grams, 30 grams of tetrabutylammonium bromide are weighed respectively
Sodium carboxymethylcellulose, 30 grams of aluminum magnesium silicates, 20 grams of neopelexes, 50 grams of polyethylene glycol, 510 grams of water, it is spare.It will
Each material sequentially adds in reaction kettle, carries out just dispersion using high-speed shearing machine, effective component is then ground in sand mill
Partial size is at 2~5 μm.
The Herbicidal combinations TDCA-10 isoproturon suspending agent (SC) of embodiment 10:30%
150 grams of TDCA-10,150 grams of isoproturons, 30 grams of lignosulfonates calcium, 20 grams, 20 grams of tetrabutylammonium bromide are weighed respectively
Sodium carboxymethylcellulose, 30 grams of aluminum magnesium silicates, 20 grams of neopelexes, 60 grams of polyethylene glycol, 520 grams of water, it is spare.It will
Each material sequentially adds in reaction kettle, carries out just dispersion using high-speed shearing machine, effective component is then ground in sand mill
Partial size is at 2~5 μm.
The Herbicidal combinations TDCA-10 isoproturon suspending agent (SC) of embodiment 11:30%
100 grams of TDCA-10,200 grams of isoproturons, 30 grams of lignosulfonates calcium, 30 grams, 20 grams of tetrabutylammonium bromide are weighed respectively
Sodium carboxymethylcellulose, 40 grams of aluminum magnesium silicates, 20 grams of neopelexes, 50 grams of polyethylene glycol, 510 grams of water, it is spare.It will
Each material sequentially adds in reaction kettle, carries out just dispersion using high-speed shearing machine, effective component is then ground in sand mill
Partial size is at 2~5 μm.
The Herbicidal combinations TDCA-6 isoproturon suspending agent (SC) of embodiment 12:30%
100 grams of TDCA-6,200 grams of isoproturons, 35 grams of lignosulfonates calcium, 35 grams, 30 grams of tetrabutylammonium bromide are weighed respectively
Sodium carboxymethylcellulose, 20 grams of aluminum magnesium silicates, 20 grams of neopelexes, 50 grams of polyethylene glycol, 510 grams of water, it is spare.It will
Each material sequentially adds in reaction kettle, carries out just dispersion using high-speed shearing machine, effective component is then ground in sand mill
Partial size is at 2~5 μm.
The Herbicidal combinations TAM-9 isoproturon suspending agent (SC) of embodiment 13:30%
30 grams, 40 grams 100 grams of TAM-9,200 grams of isoproturons, 30 grams of lignosulfonates calcium, tetrabutylammonium bromide carboxylics are weighed respectively
Sodium carboxymethylcellulose pyce, 40 grams of aluminum magnesium silicates, 20 grams of neopelexes, 40 grams of polyethylene glycol, 500 grams of water, it is spare.It will be each
Material sequentially adds in reaction kettle, carries out just dispersion using high-speed shearing machine, effective component grain is then ground in sand mill
Diameter is at 2~5 μm.
The Herbicidal combinations TDCA-10 isoproturon suspending agent (SC) of embodiment 14:40%
200 grams of TDCA-10,200 grams of isoproturons, 20 grams of lignosulfonates calcium, 20 grams, 40 grams of tetrabutylammonium bromide are weighed respectively
Sodium carboxymethylcellulose, 40 grams of aluminum magnesium silicates, 30 grams of neopelexes, 50 grams of polyethylene glycol, 400 grams of water, it is spare.It will
Each material sequentially adds in reaction kettle, carries out just dispersion using high-speed shearing machine, effective component is then ground in sand mill
Partial size is at 2~5 μm.
The Herbicidal combinations TDCA-10 isoproturon suspending agent (SC) of embodiment 15:40%
100 grams of TDCA-10,300 grams of isoproturons, 30 grams of lignosulfonates calcium, 20 grams, 20 grams of tetrabutylammonium bromide are weighed respectively
Sodium carboxymethylcellulose, 30 grams of aluminum magnesium silicates, 40 grams of neopelexes, 70 grams of polyethylene glycol, 390 grams of water, it is spare.It will
Each material sequentially adds in reaction kettle, carries out just dispersion using high-speed shearing machine, effective component is then ground in sand mill
Partial size is at 2~5 μm.
The Herbicidal combinations TDCA-10 isoproturon suspending agent (SC) of embodiment 16:40%
300 grams of TDCA-10,100 grams of isoproturons, 30 grams of lignosulfonates calcium, 30 grams, 30 grams of tetrabutylammonium bromide are weighed respectively
Sodium carboxymethylcellulose, 30 grams of aluminum magnesium silicates, 20 grams of neopelexes, 50 grams of polyethylene glycol, 410 grams of water, it is spare.It will
Each material sequentially adds in reaction kettle, carries out just dispersion using high-speed shearing machine, effective component is then ground in sand mill
Partial size is at 2~5 μm.
The Herbicidal combinations TDCA-10 isoproturon suspending agent (SC) of embodiment 17:20%
100 grams of TDCA-10,100 grams of isoproturons, 20 grams of lignosulfonates calcium, 20 grams, 30 grams of tetrabutylammonium bromide are weighed respectively
Sodium carboxymethylcellulose, 30 grams of aluminum magnesium silicates, 40 grams of neopelexes, 60 grams of polyethylene glycol, 600 grams of water, it is spare.It will
Each material sequentially adds in reaction kettle, carries out just dispersion using high-speed shearing machine, effective component is then ground in sand mill
Partial size is at 2~5 μm.
The Herbicidal combinations TDCA-10 isoproturon suspending agent (SC) of embodiment 18:20%
50 grams of TDCA-10,150 grams of isoproturons, 30 grams of lignosulfonates calcium, 30 grams, 30 grams of tetrabutylammonium bromide are weighed respectively
Sodium carboxymethylcellulose, 30 grams of aluminum magnesium silicates, 20 grams of neopelexes, 50 grams of polyethylene glycol, 610 grams of water, it is spare.It will
Each material sequentially adds in reaction kettle, carries out just dispersion using high-speed shearing machine, effective component is then ground in sand mill
Partial size is at 2~5 μm.
The Herbicidal combinations TDCA-10 isoproturon suspending agent (SC) of embodiment 19:20%
150 grams of TDCA-10,50 grams of isoproturons, 30 grams of lignosulfonates calcium, 30 grams, 30 grams of tetrabutylammonium bromide are weighed respectively
Sodium carboxymethylcellulose, 30 grams of aluminum magnesium silicates, 20 grams of neopelexes, 50 grams of polyethylene glycol, 610 grams of water, it is spare.It will
Each material sequentially adds in reaction kettle, carries out just dispersion using high-speed shearing machine, effective component is then ground in sand mill
Partial size is at 2~5 μm.
The Herbicidal combinations TDCA-10 isoproturon microcapsule formulations (CJ) of embodiment 20:6%
Weigh respectively 30 grams of TDCA-10,30 grams of isoproturons, 40 grams of gelatin, 30 grams of poly-aspartates, 15 grams of Tween-60s, 60 grams Ah
Drawing primary glue, 15 grams of polyethylene glycol, 60 gram of 20% formalin, 10% acetum, (titer is i.e. by the drop in preparation process in right amount
Fixed operate determines usage amount, similarly hereinafter), 20% NaOH solution (titer), distilled water complementary to 1000 grams, it is spare；
It is prepared by preparation step (1) poly-aspartate and gelatin mixed solution: after gelatin is impregnated swelling with distillation appropriate amount of water, heating
Dissolution is heated to 50 DEG C, and poly-aspartate is added, and appropriate distilled water is added, and 50 DEG C of heat preservations are spare in stirring.(2) Arabic peptization
The preparation of liquid: being added appropriate distilled water in reaction unit, Arabic gum powder is added, is heated to 80 DEG C or so, being gently mixed makes
Dissolution, 80 DEG C of heat preservations are spare.(3) preparation of TDCA-10 and isoproturon effective component emulsion: by TDCA-10, isoproturon, tween-
60, polyethylene glycol, above-mentioned preparation gumwater, be placed in tissue mashing machine, emulsify 30 seconds to get emulsion.(4) it mixes
It closes: under the conditions of 50~55 DEG C, above-mentioned poly-aspartate and gelatin mixed solution is added, being gently mixed makes to be uniformly mixed.(5) micro-
The preparation of capsule: under constant stirring, 10% acetum is added dropwise in Xiang Qianshu mixed liquor, adjusts pH to 3.8~4.0；(6) micro-capsule
Solidification: under constant stirring, about 30 DEG C of distilled water is added in micro-capsule liquid, micro-capsule liquid will be contained and taken from 50~55 DEG C of water-baths
Under, be stirred continuously, natural cooling, when temperature drops to 32~35 DEG C, be added ice cube, continue stirring to temperature be 10 DEG C hereinafter,
20% formalin is added, continues 15~25min of stirring, then with its pH 8~9 of 20%NaOH solution tune, continue stirring 20~
30min, observation stand and settle to micro-capsule until being precipitated.(7) it the filtering and drying of micro-capsule: completely to micro-capsule sedimentation, crosses and filters out
Fall supernatant, micro-capsule distillation is washed to formaldehydeless taste, centrifugation, drying.
The Herbicidal combinations TDCA-10 isoproturon microcapsule formulations (CJ) of embodiment 21:6%
Weigh respectively 40 grams of TDCA-10,20 grams of isoproturons, 40 grams of gelatin, 30 grams of poly-aspartates, 15 grams of Tween-60s, 60 grams Ah
Drawing primary glue, 15 grams of polyethylene glycol, 60 gram of 20% formalin, 10% acetum, (titer is i.e. by the drop in preparation process in right amount
Fixed operate determines usage amount, similarly hereinafter), 20% NaOH solution (titer), distilled water complementary to 1000 grams, it is spare；
The completely identical embodiment 20 of preparation step.
The Herbicidal combinations TDCA-10 isoproturon water dispersible granules (WDG) of embodiment 22:60%
450 grams of TDCA-10,150 grams of isoproturons, 60 grams of lignin, 30 grams of acrylic acid minor matters polymer, 30 gram 12 are weighed respectively
Sodium alkyl sulfonate, 60 grams of polyethylene glycol, 30 grams of 600C suspension aids, 210 grams of bentonites, it is spare；Each material is sequentially added instead
It answers in kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, be granulated, be drying to obtain water dispersible granules.
The Herbicidal combinations TDCA-10 isoproturon water dispersible granules (WDG) of embodiment 23:50%
200 grams of TDCA-10,300 grams of isoproturons, 40 grams of lignin, 50 grams of acrylic acid minor matters polymer, 30 gram 12 are weighed respectively
Sodium alkyl sulfonate, 50 grams of polyethylene glycol, 30 grams of 600C suspension aids, 300 grams of bentonites, it is spare；Each material is sequentially added instead
It answers in kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, be granulated, be drying to obtain water dispersible granules.
The Herbicidal combinations TDCA-10TDCA-6 isoproturon water dispersible granules (WDG) of embodiment 24:30%
It is poly- that 100 grams of TDCA-10,100 grams of TDCA-6,100 grams of isoproturons, 30 grams of lignin, 40 grams of acrylic acid minor matters are weighed respectively
Object, 30 grams of dodecyl sodium sulfates, 40 grams of polyethylene glycol, 30 grams of 600C suspension aids, 530 grams of bentonites are closed, it is spare；By each object
Material sequentially adds in reaction kettle, is uniformly mixed, then grinds in sand mill, and suitable quantity of water is added, and is granulated, is drying to obtain water dispersion
Granula.
The Herbicidal combinations TDCA-10TDCA-13 isoproturon water dispersible granules (WDG) of embodiment 25:30%
It is poly- that 100 grams of TDCA-10,100 grams of TDCA-13,100 grams of isoproturons, 30 grams of lignin, 40 grams of acrylic acid minor matters are weighed respectively
Object, 30 grams of dodecyl sodium sulfates, 40 grams of polyethylene glycol, 30 grams of 600C suspension aids, 530 grams of bentonites are closed, it is spare；By each object
Material sequentially adds in reaction kettle, is uniformly mixed, then grinds in sand mill, and suitable quantity of water is added, and is granulated, is drying to obtain water dispersion
Granula.
The Herbicidal combinations TDCA-10TDCA-13 isoproturon water dispersible granules (WDG) of embodiment 26:50%
It is poly- that 250 grams of TDCA-10,50 grams of TDCA-13,200 grams of isoproturons, 50 grams of lignin, 50 grams of acrylic acid minor matters are weighed respectively
Object, 40 grams of dodecyl sodium sulfates, 60 grams of polyethylene glycol, 30 grams of 600C suspension aids, 270 grams of bentonites are closed, it is spare；By each object
Material sequentially adds in reaction kettle, is uniformly mixed, then grinds in sand mill, and suitable quantity of water is added, and is granulated, is drying to obtain water dispersion
Granula.
The Herbicidal combinations TDCA-10TDCA-6TDCA-13 isoproturon water dispersible granules of embodiment 27:30%
(WDG)
100 grams of TDCA-10,100 grams of TDCA-13,50 grams of TDCA-6,50 grams of isoproturons, 50 grams of lignin, 50 gram third are weighed respectively
Olefin(e) acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 60 grams of polyethylene glycol, 30 grams of 600C suspension aids, 470 grams of bentonites,
It is spare；Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated, is done
Dry water dispersible granules to obtain the final product.
The Herbicidal combinations TDCA-10TDCA-6TDCA-13 isoproturon water dispersible granules of embodiment 28:50%
(WDG)
250 grams of TDCA-10,50 grams of TDCA-13,50 grams of TDCA-6,150 grams of isoproturons, 50 grams of lignin, 50 gram third are weighed respectively
Olefin(e) acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 60 grams of polyethylene glycol, 30 grams of 600C suspension aids, 270 grams of bentonites,
It is spare；Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated, is done
Dry water dispersible granules to obtain the final product.
The Herbicidal combinations TDCA-10TDCA-6TDCA-13 isoproturon water dispersible granules of embodiment 29:60%
(WDG)
100 grams of TDCA-10,50 grams of TDCA-13,50 grams of TDCA-6,400 grams of isoproturons, 60 grams of lignin, 40 gram third are weighed respectively
Olefin(e) acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 50 grams of polyethylene glycol, 30 grams of 600C suspension aids, 180 grams of bentonites,
It is spare；Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated, is done
Dry water dispersible granules to obtain the final product.
The Herbicidal combinations TDCA-10TDCA-6TDCA-13 isoproturon water dispersible granules of embodiment 30:60%
(WDG)
100 grams of TDCA-10,100 grams of TDCA-13,100 grams of TDCA-6,300 grams of isoproturons, 60 grams of lignin, 40 grams are weighed respectively
Acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 50 grams of polyethylene glycol, 30 grams of 600C suspension aids, 180 grams of swellings
Soil, it is spare；Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
The Herbicidal combinations TDCA-10TDCA-6TDCA-13 isoproturon water dispersible granules of embodiment 31:60%
(WDG)
150 grams of TDCA-10,150 grams of TDCA-13,150 grams of TDCA-6,150 grams of isoproturons, 60 grams of lignin, 40 grams are weighed respectively
Acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 50 grams of polyethylene glycol, 30 grams of 600C suspension aids, 180 grams of swellings
Soil, it is spare；Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
The Herbicidal combinations TDCA-10 isoproturon water dispersible granules (WDG) of embodiment 32:30%
120 grams of TDCA-10,180 grams of isoproturons, 35 grams of lignin, 45 grams of acrylic acid minor matters polymer, 35 gram 12 are weighed respectively
Sodium alkyl sulfonate, 35 grams of polyethylene glycol, 40 grams of 600C suspension aids, 510 grams of bentonites, it is spare；Each material is sequentially added instead
It answers in kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, be granulated, be drying to obtain water dispersible granules.
The Herbicidal combinations TDCA-10TDCA-6TDCA-13 isoproturon water dispersible granules of embodiment 33:60%
(WDG)
50 grams of TDCA-10,50 grams of TDCA-13,50 grams of TDCA-6,450 grams of isoproturons, 60 grams of lignin, 40 gram third are weighed respectively
Olefin(e) acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 50 grams of polyethylene glycol, 30 grams of 600C suspension aids, 180 grams of bentonites,
It is spare；Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated, is done
Dry water dispersible granules to obtain the final product.
The Herbicidal combinations TDCA-6 isoproturon water dispersible granules (WDG) of embodiment 34:40%
250 grams of TDCA-6,150 grams of isoproturons, 60 grams of lignin, 50 grams of acrylic acid minor matters polymer, 40 gram 12 are weighed respectively
Sodium alkyl sulfonate, 60 grams of polyethylene glycol, 30 grams of 600C suspension aids, 360 grams of bentonites, it is spare；Each material is sequentially added instead
It answers in kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, be granulated, be drying to obtain water dispersible granules.
The Herbicidal combinations TDCA-13 isoproturon water dispersible granules (WDG) of embodiment 35:30%
200 grams of TAM-9,100 grams of isoproturons, 50 grams of lignin, 40 grams of acrylic acid minor matters polymer, 40 grams of dodecanes are weighed respectively
Base sodium sulfonate, 40 grams of polyethylene glycol, 30 grams of 600C suspension aids, 500 grams of bentonites, it is spare；Each material is sequentially added into reaction
It in kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, be granulated, be drying to obtain water dispersible granules.
The isoproturon wettable powder (WP) of embodiment 36:50%
500 grams of isoproturons, 30 grams of tetrabutylammonium bromide, 20 grams of lignosulfonates calcium, 40 grams of carboxymethyl celluloses are weighed respectively
Sodium, 40 grams of aluminum magnesium silicates, 30 grams of neopelexes, 320 grams of kaolin, 20 grams of pull powder Bx, it is spare；Preparation: will be each
Material sequentially adds in reaction kettle, and stirring mixes them thoroughly, and is crushed to 5~20 μm.
The isoproturon water dispersible granules (WDG) of embodiment 37:60%
600 grams of isoproturons, 30 grams of 600C suspension aids, 50 grams of polyethylene glycol, 50 grams of lignin, 30 grams of acrylic acid branches are weighed respectively
Polymer, 40 grams of dodecyl sodium sulfates, 200 grams of bentonites are saved, it is spare；Each material is sequentially added in reaction kettle, mixing is equal
It is even, it is then ground in sand mill, suitable quantity of water is added, be granulated, be drying to obtain water dispersible granules.
By following experiment it can be shown that two effective component TDCA-10 and isopropyl in above-mentioned Herbicidal combinations of the invention
Grand compounding can have apparent synergistic effect.
In the research of herbicide, activity of weeding after active compound is more than that each reactive compound is administered alone
Activity when, then show that there are synergistic effects.
The budget activity of the given combination of two kinds of herbicides can calculate it is following (bibliography: author Colby, S.R. etc.,
Periodical title " Weed ", 1 phase in 1967, P20-22)
When X=% amount of application be p kg/ha in the case where, herbicide A (reactive compound A) loss ratio,
And Y=% amount of application be q kg/ha in the case where, herbicide B (reactive compound B) loss ratio,
And E=% amount of application be p and q kg/ha in the case where, the speculative damage rate of herbicide A and B, then:
E=X+Y-X*Y/100
If actual damage value is more than calculated value, the activity of composition is super adduction, that is, shows synergy.
One, potted plant experiment
Herbicidal combinations TDCA-10 isoproturon
30% TDCA-10 wettable powder (WP) (being prepared according to the embodiment of the present invention 3), 50% isoproturon wettable powder
(WP) to gramineae weed and broadleaf weeds (herba digitariae grass 1-3 leaf phase, black nightshade after (preparing) and compound according to the embodiment of the present invention 36
The 2-4 leaf phase) indoor virulence experimental result, as shown in Table 1.
The activity of weeding effect of one potted plant experiment of table
1 indoor pot of table the experimental results showed that, after reactive compound (TDCA-10) is compounded with two kinds of ingredients of isoproturon, have it is bright
Aobvious synergistic effect.
Two, field efficacy is tested
By taking wheat paddock as an example: in wheat paddock, 1~2 leaf phase of wheat seedling tender shoots, 1~3 leaf phase of weeds, 30% TDCA-10 is wettable
Property pulvis (WP) (being prepared according to the embodiment of the present invention 3), 50% isoproturon wettable powder (WP) is (according to the embodiment of the present invention
36 preparation) and 30% Herbicidal combinations TDCA-10 isoproturon water dispersible granules (WDG) (according to the embodiment of the present invention 32 make
It is standby) to the effect experiment of weeds of wheat.4 weeks investigation fresh weight preventive effects and 5% level of signifiance are as shown in table 2 after medicine.
The field test results of 2 eliminating weed in wheat field of table
The experimental result of table 2 shows, TDCA-10 and isoproturon compound in the present composition, is capable of forming synergistic effect, and
And degrass spectrum can be expanded, while without antagonism, improving to crop safety, significantly improving herbicidal effect, reduce costs.By
Table 1, table 2 the experimental results showed that, by two kinds of single dose drugs (2:3) combine composite weedicide, respectively in 3 kinds of different weeds
Preventive effect in experiment is above the single dose drug of full dosage, further illustrates, TDCA-10 can have significantly after compounding with isoproturon
Synergistic effect, and without antagonism, to cotton safety.
Claims (9)
1. Herbicidal combinations, with N- (5- tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,6- difluoro pyridine -4- base)-N, 4-
Dimethyl -1,2,3- thiadiazoles -5- carbonamidine (abbreviation TDCA-10) and isoproturon are acceptable in effective component, with pesticide
Auxiliary element collectively constitutes, wherein N- (5- tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,6- difluoro pyridine -4- base)-N,
4- dimethyl -1,2,3- thiadiazoles -5- carbonamidine (TDCA-10) and isoproturon weight ratio are 200:1 to 1:200.
2. Herbicidal combinations as described in claim 1, it is characterized in that the effective component N- (5- tert-butyl -1,3,4- thiadiazoles -
2- yl)-N'- (2,6- difluoro pyridine -4- base)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidine (TDCA-10) and isoproturon
Weight ratio is 50:1 to 1:50.
3. weeding agricultural chemical compositions as described in claim 1, it is characterized in that effective component N- (5- tert-butyl -1,3, the 4-
Thiadiazoles -2- base)-N'- (2,6- difluoro pyridine -4- base)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidine (TDCA-10) and
Isoproturon weight ratio is 10:1 to 1:10.
4. such as claim 1 herbicidal composition, it is characterized in that being prepared into not similar shape by current conventional pesticide production method
In the preparation formulations such as the available water dispersible granules of formula, wettable powder, suspending agent, aqueous emulsion, suspoemulsion, microcapsule formulations
Any dosage form.
5. as in claim 1 herbicidal composition, it is characterized in that N- (5- tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,
6- difluoro pyridine -4- base)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidine (TDCA-10) can by with TDCA-10 structure class
As compound N-(5- tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,6- dichloropyridine -4- base)-N, dimethyl -1 4-,
2,3- thiadiazoles -5- carbonamidine (TDCA-6), N- (5- tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,6- dibromo pyridine -4-
Base)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidine (TDCA-13), N- (5- tert-butyl -1,3,4- thiadiazoles -2- base) -
N'- (pyridin-4-yl)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidine etc. replaces.
6. weeding agricultural chemical compositions as described in claim 1, it is characterized in that being used for Soybean Field, corn field, sugarcane field, rape
The farmlands such as field, tea place and bare place weeding.
7. weeding agricultural chemical compositions as described in claim 1, it is characterized in that can also be N- (5- tert-butyl -1,3,4- thiophene two
Azoles -2- base)-N'- (2,6- difluoro pyridine -4- base)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidine (TDCA-10), N- (5-
Tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,6- dichloropyridine -4- base)-N, 4- dimethyl -1,2,3- thiadiazoles -5- first
Amidine (TDCA-6), N- (5- tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,6- dibromo pyridine -4- base)-N, 4- dimethyl -
Any two kinds in 1,2,3- thiadiazoles -5- carbonamidine (TDCA-13) and isoproturon are acceptable in effective component, with pesticide
Auxiliary element collectively constitutes.
8. weeding agricultural chemical compositions as described in claim 1, it is characterized in that can also be N- (5- tert-butyl -1,3,4- thiophene two
Azoles -2- base)-N'- (2,6- difluoro pyridine -4- base)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidine (TDCA-10), N- (5-
Tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,6- dichloropyridine -4- base)-N, 4- dimethyl -1,2,3- thiadiazoles -5- first
Amidine (TDCA-6), N- (5- tert-butyl -1,3,4- thiadiazoles -2- base)-N'- (2,6- dibromo pyridine -4- base)-N, 4- dimethyl -
The mixture of the arbitrary proportion of 1,2,3- three kinds of thiadiazoles -5- carbonamidine (TDCA-13) forms effective component with isoproturon again, with agriculture
Acceptable auxiliary element collectively constitutes in medicine.
9. weeding agricultural chemical compositions as described in claim 1, it is characterized in that composition is for desinsection, mite killing purposes also in this hair
Within bright protection scope.
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