CN109805016A - A kind of Herbicidal combinations of the secondary monooctyl ester containing fluroxypramide - Google Patents
A kind of Herbicidal combinations of the secondary monooctyl ester containing fluroxypramide Download PDFInfo
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Abstract
The invention discloses a kind of synergistic herbicidal pesticide composites, using 2- (the fluoro- 2- pyridine acyloxy of 6-)-N- (4- fluorophenyl)-N- (1- Methylethyl) thioacetamide (TAM-5) and the secondary monooctyl ester of fluroxypramide as effective component, it is collectively constituted with acceptable auxiliary element in pesticide, wherein TAM-5 and the secondary monooctyl ester weight ratio of fluroxypramide are that 1:1 to 1:5 has best synergistic effect.Synergistic effect is formed after two kinds of combination of active principles, and can expand degrass spectrum, while without antagonism, crop safety is improved.Synergistic herbicidal pesticide composite can effectively prevent and kill off annual gramineae weed and broadleaf weeds, it can inhibit part perennial weeds again, especially suitable for the field weeding of the industrial crops such as wheat paddock, Soybean Field, barley field, corn field and grape, tomato, capsicum, potato, pimento, eggplant, semen viciae fabae etc. vegetable farm herbicide, herbicidal effect is significantly improved, while to industrial crops and vegetable safety.
Description
Technical field
The present invention relates to a kind of weeding class composition pesticides, especially for being suitable for wheat, barley, corn, grape, fruit
Prevent and kill off broadleaf weeds in the ground such as garden, pasture, forest land, lawn.
Background technique
Fluroxypramide (also known as are as follows: fluroxypramide acid) is a kind of inner sucting conduction type postemergence weed control of Dow Chemical Company exploitation
Agent has good prevent and kill off to a variety of annual or perennial broadleaf weed in wheat, barley, wheat, corn field and orchard etc.
Effect.Fluroxypramide molecular formula C7H5Cl2FN2O3, molecular weight 255.03, No. CAS: 69377-81-7, structural formula is as shown in Equation 1.
Its Full Name in English 2- (4-amino-3,5-dichloro-6-fluoropyridin-2-yloxy) acetic acid, English letter
Claim Fluroxypyr.Fluroxypramide Chinese chemical name is known as the fluoro- 2- pyridine fluoroacetic acid of the chloro- 6- of 4- amino -3,5- bis-, and Chinese is also known as
Fluroxypyr.Sterling is white crystalline body, odorless, 232~233 DEG C of fusing point, vapour pressure 1.26 × 10-3Pa (25 DEG C),
PKa value is 2.94.Its dissolubility are as follows: be soluble in acetone, chloroform, methylene chloride isopolarity solvent and medium polar solvent；Non-
Solubility is lower in polar solvent (petroleum ether, n-hexane etc.)；(91mg/L not soluble in water；25℃).It is more stable under room temperature, it can
To stablize storage 2 years.Its fluroxypramide methyl ester derivation (the two fluoro- 2- pyridine fluoroacetic acid methyl esters of chloro- 6- of 4- amino -3,5-) is crystal
(56~57 DEG C of fusing point), fluroxypramide ethyl ester derivative (the fluoro- 2- pyridine fluoroacetic acid ethyl ester of the chloro- 6- of 4- amino -3,5- bis-) be compared with
For viscous liquid.Fluroxypramide belongs to pyridine fluoroacetic acid class herbicide, has uptake and translocation effect, belongs to typical hormone-type and remove
Careless agent.It is used after seedling, the reaction of classical hormones class herbicide occurs in sensitive crop.It is wider using optimum period on cereal crop,
It can be used for the ground such as wheat, barley, corn, grape and orchard, pasture, forest farm and prevent and kill off broadleaf weeds, such as clearvers, field bindweed, shepherd's purse
The weeds such as dish, herba stellariae mediae, volume stem amaranth, purslane.
The secondary monooctyl ester molecular formula C of fluroxypramide15H21Cl2FN2O3, molecular weight 367.25, No. CAS: 81406-37-3, structural formula is such as
Shown in formula 2.Its Full Name in English octan-2-yl 2- (4-amino-3,5-dichloro-6- fluoropyridin-2-
Yloxy) acetate, English abbreviation Fluroxypyr 1-methylheptyl ester.The secondary monooctyl ester Chinese chemical name of fluroxypramide
The referred to as fluoro- 2- pyridine fluoroacetic acid -1- methylheptyl ester of the chloro- 6- of 4- amino -3,5- bis-, Chinese are also known as fluroxypyr -1-
Methylheptyl ester.Sterling is white crystalline body, odorless, 56~57 DEG C of fusing point.Pesticide original medicine content is generally 95-98%, has
Soap scent.Acetone (62 g/L, 25 DEG C), methanol (250 g/L, 25 DEG C), methylene chloride (426 g/L, 25 DEG C) can be dissolved in
Etc. various polarities organic solvent, (saturated concentration is about 0.9ppm in 25 DEG C of water) not soluble in water, octanol is with water partition coefficient
6140:1.Since strong acidity (pKa value 2.94) is presented in fluroxypramide, it is being easy to cause other to have with the mutual timing of other herbicides
Imitate the decomposition of component, thus when being used as composition it is usually used be fluroxypramide acid Zhong Xin ester derivant it is (usually simple
The referred to as secondary monooctyl ester of fluroxypramide.Although in fact, the secondary monooctyl ester of the fluroxypramide used on surface, the fluroxypramide substantially used,
Because the secondary monooctyl ester of fluroxypramide be absorbed by plants it is internal, by metabolic degradation be fluroxypramide, to achieve the effect that weeding).Fluorine grass
The secondary monooctyl ester of cigarette is inner sucting conduction type herbicide after seedling, is absorbed by plants quickly after medicine, so that sensitive plant classical hormones class is occurred and removes
The reaction of careless agent, plant deformity, distortion.Temperature on the final effect of herbicide without influence, but influence its drug effect performance speed
Generally when temperature is lower, drug effect performance is slower, stops growing after can making dunsiekte, but not dead immediately, and temperature is stood after increasing
It is i.e. dead quickly.Broadleaf weeds, such as pig are prevented and kill off suitable for wheat, barley, corn, grape, orchard, pasture, forest land, lawn and other places
Calamity, volume stem smartweed, purslane, black nightshade, herba stellariae mediae, field bindweed, knotweed, amaranth etc. are brought disaster to, it is invalid to gramineae weed.Fluroxypramide contains as one kind
Efficient, less toxic, the low-residual herbicide of fluorine, are the developing ways of current new herbicides.Since it has in stubble and rear stubble
Plant height safety；Working life is wide, and drug effect is fast, and dosage is low；Miscibilty is good, mixed with a variety of gramineous weed weedicides to increase
Degrass spectrum and raising preventive effect.Resistance of rainwater washing against ability is strong, applies effect latter hour rainy the advantages that not influencing drug effect.Fluroxypramide
Secondary monooctyl ester raw medicine toxicity is smaller, rat acute: LD50=2400mg/kg(rat oral), the acute LD of little white rabbit50>5000mg/kg
(rabbit is percutaneous), rat suck LD50>296mg/m3(rat sucks 4 hours).Currently, the secondary monooctyl ester single dose of fluroxypramide is made with every liter
Agent is sold containing the missible oil (trade name: keeping it grand) of 200 grams of secondary monooctyl esters of fluroxypramide (equivalent acid is 139 grams of fluroxypramide acid at equivalent),
Fluroxypramide Zhong Xin ester content usually will not be too high in missible oil, this is because the limitation of its solubility.The secondary monooctyl ester of fluroxypramide also often with
Other herbicides form mixture and use: can be mixed with the secondary monooctyl ester of fluroxypramide, Brominal, 2,4-D butyl ester, 2- first -4- chlorine etc..Corn
Commeline communis, field bindweed, purslane, small japanese bearbind etc. are prevented and kill off in field, per acre with 20% fluroxypramide missible oil 70-100mL.Wheat paddock is used per acre
20% fluroxypramide missible oil 50-100mL.20% fluroxypramide missible oil 80-150mL is used in vineyard, orchard, pasture per acre.Insecticide spraying time:
It is miscellaneous: the 2-4 leaf phase.It is spraying with liquid volume 15-30kg per acre.
The secondary monooctyl ester structural formula of fluroxypramide is relative complex, therefore its synthesis route is more, is mainly the following synthesis
Technique.The first is alkylation process (bibliography: United States Patent (USP), patent name: Herbicidal use of
Aminohalopyridyloxy acid and derivatives thereof, inventor Stanley D. Megregor
Deng: US:4110104,1978-08-29): this method is by the chloro- 6- fluorine pyridine -2- phenol potassium of 4- amino -3,5- bis- and monoxone Zhong Xin
Ester is directly etherified and obtains product.Pyridine obtains penta chloropyridine through superchlorination for starting material, by fluorination, ammonification, three steps of hydrolysis
Reaction obtains the chloro- 6- fluorine pyridine -2- phenol potassium of important intermediate 4- amino -3,5- two.Meanwhile monoxone and sec-octyl alcohol are urged in sulfuric acid
Change lower esterification and obtains another secondary monooctyl ester of intermediate monoxone.Then the chloro- 6- fluorine pyrrole of intermediate 4- amino -3,5- two
Pyridine -2- phenol potassium and the secondary monooctyl ester of intermediate monoxone, which are directly etherified, obtains the secondary monooctyl ester of product fluroxypramide.The advantages of this route is route
Simply.This synthesis technology committed step etherification procedure, yield is not high, and purity is lower, purifies relative difficulty；Second is transesterification
Method (bibliography: United States Patent (USP), patent name: Preparation of higher alkylesters of
Carboxylicacids, inventor Lan R. Kings etc.: US:5214150,1993-05-25): this method is fluroxypramide methyl esters
Ester exchange reaction, which is carried out, with sec-octyl alcohol obtains product.Pyridine obtains penta chloropyridine through superchlorination for starting material, by fluorination, ammonia
Change, hydrolysis three-step reaction obtains the chloro- 6- fluorine pyridine -2- phenol potassium of important intermediate 4- amino -3,5- two.Intermediate 4- amino-
The chloro- 6- fluorine pyridine -2- phenol potassium of 3,5- bis- and methyl chloroacetate carry out condensation reaction and obtain intermediate fluroxypramide methyl esters.Intermediate fluorine
Careless cigarette methyl esters and sec-octyl alcohol carry out ester exchange reaction and obtain the secondary monooctyl ester of product fluroxypramide.The advantages of this route be product purity compared with
It is good, it purifies relatively easy.The disadvantage is that temperature reaches 160 DEG C in ester exchange reaction, and system needs to depressurize, to equipment requirement
Higher, overall operation is also more complicated than alkylation process.The third is alcoholic extract hydroxyl group carboxylic acid ester process (bibliography: United States Patent (USP), proprietary term
Claim: Aminohalopyridyloxy acid and derivativesthereof, inventor Stanley D. Megregor
Deng: US:3761486,1973-9-25): this method is 4- amino -3,5- bis- chloro- 2, and 6- difluoro pyridine and the secondary monooctyl ester of hydroxyacetic acid are straight
It taps into row reaction and obtains product.Pyridine obtains penta chloropyridine through superchlorination for starting material, obtains by fluorination, ammonification two-step reaction
To the chloro- 2,6- difluoro pyridine of intermediate 4- amino -3,5- two.The chloro- 2,6- difluoro pyridine of intermediate 4- amino -3,5- two and hydroxyl
The secondary monooctyl ester of guanidine-acetic acid carries out condensation reaction and obtains the secondary monooctyl ester of fluroxypramide.The advantages of this route is that synthesis step is short, easy to operate.It lacks
Point is that condensation reaction yield is not high, and product purity is lower, it is most important that raw material hydroxyl sec-octyl acetate is expensive (than current
The secondary monooctyl ester price of fluroxypramide is higher by by about one time on the market), there is presently no industrial values.4th kind is methyl sulfone intermediate method
(bibliography: United States Patent (USP), patent name: Optically active phenoxypropionic acid
Derivatives, inventor Koichi. Moriya etc.: US:4596599,1986-6-24): this method is 4- amino -3,5- bis-
Chloro- 6- fluorine pyridine -2- methyl sulfone is directly reacted to obtain product with the secondary monooctyl ester of hydroxyacetic acid.Pyridine is starting material through superchlorination
Penta chloropyridine is obtained, obtains chloro- 2, the 6- difluoro pyridine of intermediate 4- amino -3,5- bis- by fluorination, ammonification two-step reaction.In this
The chloro- 2,6- difluoro pyridine of mesosome 4- amino -3,5- two and chloro ethyl mercaptan are condensed to yield 4- amino -3,5- under sodium methoxide catalyzed
The two chloro- fluoro- 2- methylsulfanyl pyridine intermediates of 6-, the bis- fluoro- 2- methylsulfanyl pyridine of chloro- 6- of intermediate 4- amino -3,5- use dioxygen
Water, which further aoxidizes, obtains the chloro- 6- fluorine pyridine -2- methyl sulfone of intermediate 4- amino -3,5- two.Intermediate 4- amino -3,5- two is chloro-
6- fluorine pyridine -2- methyl sulfone and the secondary monooctyl ester of hydroxyacetic acid carry out condensation reaction and obtain the secondary monooctyl ester of fluroxypramide.The advantages of this route is tool
There is stronger originality, the original synthetic route of patent can be evaded.The disadvantage is that reaction step is tediously long, condensation reaction yield is not high, produces
Product purity is lower, most important defect be also will use expensive raw material hydroxyl sec-octyl acetate (the secondary monooctyl ester of hydroxyacetic acid,
Than the secondary monooctyl ester price of fluroxypramide is higher by by about one time on the market at present), while the sodium methoxide, highly concentrated that also use price relatively high
Hydrogen peroxide is spent, therefore the route only only has research significance at present, there are no industrial values.5th kind is sodium methoxide method (ginseng
Examine document: the synthetic method of Cheng Xia, New Herbicides fluroxypramide summarize [J], Xi'an Petroleum University's journal (natural science edition),
1990,21 (3): 27-29): this method be the two fluoro- 2- methoxypyridine of chloro- 6- of 4- amino -3,5- and the secondary monooctyl ester of monoxone directly into
Row condensation reaction obtains product.Pyridine obtains penta chloropyridine through superchlorination for starting material, obtains by fluorination, ammonification two-step reaction
To the chloro- 2,6- difluoro pyridine of intermediate 4- amino 3,5- bis-.The chloro- 2,6- difluoro pyridine of intermediate 4- amino 3,5- bis- and methanol
Sodium reacts to obtain the fluoro- 2- methoxypyridine intermediate of the chloro- 6- of 4- amino -3,5- bis-, and the chloro- 6- of intermediate 4- amino -3,5- bis- is fluoro-
2- methoxypyridine and the secondary monooctyl ester of monoxone carry out condensation reaction and obtain the secondary monooctyl ester of fluroxypramide.The advantages of this route is synthesis step
It is short.The disadvantage is that condensation reaction yield is very low, product purity is not also high, therefore the route synthesis cost is higher.
Wheat cultivated area over the years in China's is the 22% ~ 30% of the whole nation cultivation ground gross area, cultivated area be even more reach 4.2 ~
5.5 hundred million mu.Weeds in wheat paddock are divided into broadleaf weed and monocotyledon weed.Broadleaf weed is called broadleaf weeds.Soybean,
Peanut belongs to dicotyledon, and broadleaf weed is similar to soybean, peanut, and also there are two cotyledons when emergence.It is single as corn
Only one cotyledon of cotyledon weeds.Both types weeds are widely different to the sensitivity of herbicide.It turns green to jointing, wheat
The common broadleaf weed of Tanaka has Descurainia sophia, Herba Galii Teneri, herba stellariae mediae, shepherd's purse, conical silene herb, corn gromwell, sandwort, wartwort etc..It broadcasts
Ma wormwood artemisia also known as wheat wormwood artemisia, Descurainia sophia germination and emergence before the winter belong to winter annual weeds.This is the Descurainia sophia of strain.Descurainia sophia is in wheat harvest
Preceding seed is mature.Shepherd's purse is also winter annual weeds.It emerges after wheat cultivation.Continued growth after wheat is turned green, and bolting is bloomed, and is arrived
Seed is mature before wheat harvest.Herba Galii Teneri is called drawing and draws rattan, glues stickweed, and snake shell grass belongs to winter annual weeds.Conical silene herb is called rice watt
Tank, this is the conical silene herb of period of seedling establishment, arrives wheat booting period, and conical silene herb starts to bloom.Wheat weeds when wheat is turned green be goose not
Food.The corn gromwell grown in wheatland, belongs to Boraginaceae.It also blooms in wheat booting period.Wheat is turned green the list common to jointing
Cotyledon weeds have: amur foxtail, wild avena sativa etc..Common cornfield gramineae weed has wild avena sativa, amur foxtail, barnyard grass, herba setariae viridis, hard
Grass, herba digitariae, herba eleusines indicae etc..The herbicide that common wheatland prevents and kill off gramineae weed has galloping horse, diclofop-methyl, suffer, oat fear, kills
Careless pellet, molinate, Avadex, blueness Yan Ling, difenzoquat etc..Common wheatland broadleaf weeds has purslane, clearvers, field thistle (thorn
Youngster's dish), it is shepherd's purse, rice crock, sowthistle, humulus grass (drawing is uprooted plants after their edible portions have been harvested), Siberian cocklebur, Descurainia sophia, garden sorrel, leaf knotweed, field bindweed, Amaranthus retroflexus, recessed
Head amaranth, ivy glorybind, sonchus oleraceus etc..The herbicide for preventing and kill off broadleaf weeds for wheatland has 2,4- d butyl ester, dimethyl tetrachloride, benzene to reach
Pine, tribenuron-methyl, dicamba, metsulfuron-methyl, green sulphur is grand, fluroxypyr, symetryne, Brominal, ioxynil etc..National wheat paddock
Cultivated area is big, weeds huge number, and same kind is used for a long time or same veriety is all easy to produce resistance, it is therefore desirable to
Herbicide kind does not stop to weed out the old and bring forth the new.
China is one of Chan Mian big country, the world, wherein with provinces and regions such as Shandong, Ji, Henan, Soviet Union, Hubei Province, new, Anhui for main cotton growing 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 tail
It is maximum that density occurs for grass, Paspalum distichum, Bermuda grass etc.；Broadleaf weeds is with Eclipta prostrata, Amaranthus retroflexus, argy wormwood, chenopodium glaucum linn, Acalypha-austratis-L, piemarker
Based on fiber crops etc.；Sedge weed is based on the rhizome of nutgrass flatsedge.In Yellow River basin cotton region, with the rise of temperature, cotton field after sowing cotton seed
A variety of weeds start rudiment successively, until mid or late May forms first emergence peak in field, at this time with herba setariae viridis, herba digitariae, drought
Based on barnyard grass, Chenopodiaceae etc., with rainfall and pour water later it may also occur that primary small germination peak；To July, with the arrival in rainy season,
The weeds such as the 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 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 are not
Together.Yangtze river basin cotton region has a moderate climate with heavy rainfall, is suitable for weed growth, and dominant weed is with herba digitariae, herba eleusines indicae and the rhizome of nutgrass flatsedge
It is main.To like to form various weed communities based on cool resistance to early weeds, common weed mainly has herba digitariae, Bermuda grass, dish etc. for North china
It 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.The chemical weed control of China cotton field
There are the problem of be that method of administration is improper first.The distribution of China cotton field is wide, after the generation of planted in different ecological areas weeds and spraying herbicide
Primary and secondary wants the succession of herbaceous of weeds still to lack further investigation, not formed targetedly to prevent and kill off the section's general education being formulated to numerous cotton growers
Educate deficiency, the not perfectly flat weighing apparatus of various regions application technology level, because selecting medicament and administration time, dosage method etc. no in practice
When often resulting in phytotoxicity.The chemical weed control of China cotton field starting late, fundamental research is weaker, cotton field chemical weed control kind compared with
It is few, it carries out in a deep going way and more effectively applies there is an urgent need to research.These factors all make cotton field herbicide need constantly to release
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.
Soybean Field common weed is just like three-coloured amaranth, knotweed, Chenopodiaceae, black nightshade, Siberian cocklebur, barnyard grass, herba setariae viridis, herba digitariae, broomcorn millet etc..Sugarcane field is normal
See that weeds there are the annual grassy weeds such as the rhizome of nutgrass flatsedge, herba digitariae, herba eleusines indicae, bald barnyard, bidens pilosa, Bermuda grass.Corn field is common miscellaneous
Not only there are also perennial weeds for raw weeds one year in grass, but also these weeds have multiple out of grass, and difficulty of prevention and cure is big.Agriculture at present
Phytotoxicity easily occurs for most-often used glyphosate, glufosinate-ammonium, the secondary monooctyl ester of fluroxypramide, Bi Kecao etc. in industry production.Simultaneously before major part
Height is required to the careless age of weeds when stating Common Herbicides application, beyond a certain range of careless age, herbicidal effect is substantially reduced.Grass is sweet
Phosphine, glufosinate-ammonium class herbicide are more only applicable to bare place weeding.Meanwhile weeds chemical herbicide will be generated it is different degrees of
Resistance.These factors, all making herbicide need constantly to release, effect is more preferable, the wider array of new varieties of degrass spectrum.
Chinese patent (application number CN2013100125604, January 15 2013 date of application, Granted publication date 2014
On November 19) in report the general formula of the artificial Xihua Univ of patent application (inventor Yang Weiqing, Ma Menglin etc.) be TAM's
(formula 3, X indicates halogen in formula 3 for the disubstituted thioacetyl amine compound of 2- pyridine acyloxy-N- and its synthetic method；Y is indicated
Halogen；Z indicates branched alkyl).Chinese patent (application number CN2013100201913, January 21 2013 date of application, authorization
Date of declaration September in 2014 3 days) in report the artificial Xihua Univ of patent application (inventor Yang Weiqing, Zhang Yuanyuan etc.) right
General formula is that the novel synthesis of the disubstituted thioacetyl amine compound of 2- pyridine acyloxy-N- of TAM is reported, the new side
Method uses ester-interchange method to the synthesis of target product, obtains very good effect.Chinese patent (application number CN2013100201928, Shen
Please January 21 2013 date, March 26 2014 Granted publication date) in report the artificial Xihua Univ of patent application (hair
Bright artificial Yang Weiqing, Zhang Yuanyuan etc.) general formula be TAM the disubstituted thioacetyl amine compound of 2- pyridine acyloxy-N- make
For the purposes of herbicide, it is mainly used for preventing and kill off broadleaf weeds and gramineae weed in farmland.In the compound that general formula is TAM
TAM-5(formula 4) activity of weeding is best, annual gramineae weed and broadleaf weeds can be effectively prevented and kill off, but it is more to part
Year, raw weeds can only play limited inhibitory effect, and degrass spectrum is not extensive enough.In addition, the TAM-1 in the compound that general formula is TAM
(formula 5) activity of weeding is also preferable, is only second to TAM-5, can also effectively prevent and kill off annual gramineae weed and broadleaf weeds, equally
Limited inhibitory effect can only be played to part perennial weeds, degrass spectrum is not extensive enough.Meanwhile the life of TAM-5 and TAM-1
Produce cost for most of herbicide kinds currently on the market, slightly higher, economically consider, also it is necessary to
Interworking use is carried out with other effective herbicides.
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 efficient, the safe weeding pesticide composition of part perennial weeds can be inhibited, can be used for wheat, barley, corn,
Prevent and kill off broadleaf weeds in the ground such as grape, orchard, pasture, forest land, lawn.Although aforementioned Chinese patent (CN 2013100201928, Shen
Please January 21 2013 date, March 26 2014 Granted publication date) in report general formula be TAM 2- pyridine acyl-oxygen
The disubstituted thioacetyl amine compound of base-N- is mainly used for the excellent of broadleaf weeds and gramineae weed in farmland as herbicide
Good purposes.But this kind of thioacetyl amine compound is prepared into preparation exclusive use and still has that degrass spectrum is not wide enough, unit
Dispenser cost is higher, requires the defects of high to certain weeds careless age.These defects are reduced to a certain extent in other words in order to overcome,
In initial experimentation We conducted TAM-5 respectively with imazethapyr, metosulam, atrazine, Diflufenican, spy
Nearly 40 kinds of the secondary monooctyl ester of fourth benzthiazuron, flufenacet, pyrithiobac-sodium, fluroxypramide etc. can prevent and kill off broadleaf weeds and gramineae weed
Herbicide kind is combined a large amount of screening experiments of (combination including three kinds of herbicide components).Finally, we pass through largely
Indoor and field experiment and further Economic Evaluation, have found TAM-5 and combine with the Herbicidal synergistic of the secondary monooctyl ester of fluroxypramide
Object.It has surprisingly been found that the Synergistic herbicide compositions are used for wheat, barley, corn, grape, orchard, pasture, forest land, lawn
Etc. ground prevent and kill off broadleaf weeds, not only herbicidal effect is good, has notable synergistic effect, and does not have visible medicine to industrial crops
Evil.
Herbicidal combinations of the present invention are 2- (the fluoro- 2- pyridine acyloxy of 6-)-N- (4- fluorophenyl)-N- (1- with Chinese
Methylethyl) [English name is (N- (4-fluorophenyl)-N-isopropylthiocarbamoyl) to thioacetamide
Hereinafter referred to as TAM-5 in the methyl-6-fluoropyrid- ine-2-carboxylate(present invention), structural formula such as formula 4
It is shown；And with Chinese be the two fluoro- 2- pyridine fluoroacetic acid -1- methylheptyl ester of chloro- 6- of 4- amino -3,5- (present invention in
The secondary monooctyl ester of fluroxypramide is referred to as using its Chinese) (English name is Octan-2-yl 2- (4-amino-3,5-dichloro-6-
Fluoropyridin-2-yloxy) acetate, English abbreviation Fluroxypyr 1-methylheptyl ester), structure
Formula is as shown in Equation 2；The present invention is using the compound of TAM-5 and the secondary monooctyl ester of fluroxypramide as effective component (two kinds of effective component), with agriculture
Acceptable auxiliary element collectively constitutes in medicine.
Herbicidal combinations of the present invention are other than the compound of above-mentioned TAM-5 and the secondary monooctyl ester composition composition of fluroxypramide, simultaneously
It also is 2- (6- Chloro-2-Pyridyle acyloxy)-N- (4- fluorophenyl)-N- (1- Methylethyl) thioacetamide [English with Chinese
Literary fame is known as (N- (4-fluorophenyl)-N-isopropylthiocarbamoyl) methyl-6-chloropyrid-
Hereinafter referred to as TAM-1 in the ine-2-carboxylate(present invention), structural formula is as shown in Equation 5；It and with Chinese is 4-
The fluoro- 2- pyridine fluoroacetic acid -1- methylheptyl ester of the chloro- 6- of amino -3,5- two is (secondary using its Chinese referred to as fluroxypramide in the present invention
Monooctyl ester) (English name is Octan-2-yl 2- (4-amino-3,5-dichloro-6- fluoropyridin-2-yloxy)
Acetate, English abbreviation Fluroxypyr 1-methylheptyl ester), structural formula is as shown in Equation 2；The present invention is with TAM-
The 1 secondary monooctyl ester of compound and fluroxypramide is effective component (two kinds of effective component), total with acceptable auxiliary element in pesticide
With composition.
Herbicidal combinations of the present invention in addition to the compound and fluroxypramide of above-mentioned TAM-5 secondary monooctyl ester composition Herbicidal combinations,
The secondary monooctyl ester of the compound and fluroxypramide of TAM-1 forms Herbicidal combination beyond the region of objective existence, while the present invention is with the compound of TAM-1, TAM-5
Three groups of compound and the secondary monooctyl ester of fluroxypramide are divided into effective component (three kinds of effective component), in pesticide acceptable auxiliary at
Divide and collectively constitutes.
The permission weight ratio of TAM-5 and the secondary monooctyl ester of fluroxypramide is 100:1 to 1:100 in Herbicidal combinations of the present invention, excellent
Selecting ratio is 5:1 to 1:20, optimal proportion 1:1 to 1:5.
The permission weight ratio of TAM-1 and the secondary monooctyl ester of fluroxypramide is 100:1 to 1:100 in Herbicidal combinations of the present invention, excellent
Selecting ratio is 5:1 to 1:20, optimal proportion 1:1 to 1:5.
The permission weight ratio of TAM-5, TAM-1 and the secondary monooctyl ester of fluroxypramide is 100 in three component Herbicidal combinations of the invention:
1:1 to 1:1:100 is preferably in a proportion of 1:1:1 to 1:1:10.
Herbicidal combinations of the present invention can be used for the field weeding of the industrial crops such as wheat paddock, Soybean Field, barley field, corn field,
It can be used for grape, tomato, capsicum, potato, nursery leek, pimento, eggplant, semen viciae fabae, pea, onion etc. dish simultaneously
Field weeding.
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
TAM-5 in the Herbicidal combinations and the secondary monooctyl ester effective component of fluroxypramide and corresponding auxiliary element are that raw material is abundant by production mode
Mixing, is prepared into various forms of available corresponding dosage forms.Possible dosage form includes: aqueous emulsion, microcapsule formulations, wettable
Property pulvis, water dispersant, suspending agent, suspoemulsion, microcapsule formulations etc..Such as several typical common dosage forms and preparation can be with:
Aqueous emulsion (EW), the raw medicine liquid or raw medicine for being insoluble in water are dissolved in the resulting liquid dispersion of organic solvent not soluble in water
The liquid preparation that Yu Shuizhong is formed.When preparation can by described active drug ingredient and including solvent, emulsifier, co-emulsifier,
Auxiliary element including antifreeze, defoaming agent, antimicrobial, pH adjusting agent, density adjuster, thickener etc., through high shear
Emulsification is made.Solvent therein can choose in pesticide in benzene class, ketone or the alcohols equal solvent such as common toluene, dimethylbenzene
It is one or more of;Emulsifier can choose such as above-mentioned ethoxylated alkyl ether, ethoxyquin alkyl phenylate, alkylbenzene sulfonate, ring
Oxidative ethane-propylene oxide block copolymer, alkyl phenol polyglycol ether, polyoxyethylene fatty acid ester, sorbitan alkyl ester, polyoxy
One or more of the poly- alkane alkene polyamine of alkane alkene, amides etc.;Co-emulsifier can choose such as butanol, isobutanol, dodecanol-
1, one or more of alkanes alcohols such as tetradecanol -1, octadecanol -1;Antifreeze can choose such as above-mentioned sodium chloride,
Urea, ammonium sulfate, ethylene glycol, one or more of polyalcohols such as 1,2- propylene glycol;Thickener and stabilizer also can choose
One or more of such as above-mentioned xanthan gum (XG), polyvinyl alcohol (PVA), aluminum magnesium silicate, and use when necessary
Auxiliary agents such as pH adjusting agent and defoaming agent etc..
Microcapsule formulations (CJ), which refer to, forms " core-shell structure copolymer " structure small container using natural or synthesis high molecular material, will
Pesticide coats wherein, and the formulations of pesticide in water that suspend.Micro-capsule suspension appearance is a thick working fluid, with water
Emulsion and aqueous suspension agent are similar.With micro- sem observation, its shape of microcapsules is spherical in shape, rugby shape, grain or other shapes.It is micro-
Capsule 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 micro- glue
Capsule pesticide has the characteristics that the lasting period is long, toxicity is low, safe ready, just becomes a developing direction of pesticides new formulation.Micro- glue
The customary preparation methods of capsule have complex coacervation, Simple coacervation, interfacial polymerization, situ aggregation method, orifice-coagulating bath method etc..Most
Occur some novel processing steps, such as molecular inclusion, microchannel emulsification method, supercritical fluid quick expansion again in recent years
Method, yeast microcapsule method, self-assembled multilayer film method.Microcapsules often have sodium alginate, chitosan, gelatin, porous-starch with wall material
Deng.Complex coacervation is most popular method in above-mentioned microcapsule preparation method.Complex coacervation preparation principle is with two kinds with phase
The substance of counter charges makees embedded object, and core material disperses wherein, to change change pH values, temperature or solution concentration, due to the effect between charge,
Make two kinds of wall material solubility declines and is condensed into microcapsules precipitation.A kind of positively charged colloidal solution and another kind are negatively charged
Colloidal solution mutually mix, since the interaction between xenogenesis charge forms compound polyelectrolyte and separate, be deposited on
Microcapsules are obtained around capsule-core.Complex coacervation is often capsule material with gelatin, Arabic gum.Gelatin is protein, in aqueous solution,
Contain-NH on strand2With-COOH and its accordingly dissociate group-NH3 +With-COO-, but contain-NH3 +With-COO-Ion is how much,
It is influenced by PH values.For gelatin solution in pH 4.0 or so, positive charge is most.Arabic gum is polysaccharide, water-soluble
In liquid ,-COOH and-COO is contained on strand-, there is negative electrical charge.Therefore in gelatin and Arabic gum mixed aqueous solutions,
PH is adjusted when being about 4.0, gelatin and Arabic gum form compound because charged phase neutralizes instead, solubility reduction, from system
Middle cohesion encystation is precipitated.Curing agent formaldehyde is added, formaldehyde and gelatin generate the condensation reaction of amine aldehyde, and gelatin molecule crosslinking reticulates
Structure keeps the shape of micro-capsule, becomes irreversible micro-capsule；Add 2% NaOH to adjust medium pH 8 ~ 9, it is anti-to be conducive to the condensation of amine aldehyde
It should carry out 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 TAM-5 of the present invention and the secondary monooctyl ester composition of fluroxypramide and auxiliary
Ingredient (such as thickener, stabilizer, Ricinate, antifreezing agent, pH adjusting agent, defoaming agent) is through soybean dietary fiber (grinding)
It is made.Wherein Ricinate is phosphate polyethers, alkylnaphthalene sulfonate, alkylbenzene sulfonate, aliphatic alcohol sulfate, alkyl
Ammonium bromide, alkyl ammomium chloride, crown ether, quaternary alkylphosphonium salt, alkyl polyoxyethylene base ether sulfate, lignosulfonates, lignin, carboxylic first
One of base cellulose, sodium carboxymethylcellulose, azone, thiophene ketone are several；Thickener and stabilizer are polyvinyl alcohol, contracting
Close one of phosphate, xanthan gum, aluminum magnesium silicate etc. or several；Antifreezing agent is sodium chloride, urea, ammonium sulfate, second two
One of alcohol, glycerol etc. are several；PH adjusting agent is potassium dihydrogen phosphate, dipotassium hydrogen phosphate, citric acid, sodium carbonate, carbonic acid
One of potassium etc. 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 the secondary monooctyl ester of TAM-5 and fluroxypramide of the present invention, then be added diatomite, clay, precipitated calcium carbonate,
The common diluent such as white carbon black or inert substance add other common auxiliary elements, such as alkylnaphthalene sulfonate, alkyl benzene sulphonate
Salt, aliphatic alcohol sulfate, alkyl bromination ammonium, alkyl ammomium chloride, quaternary alkylphosphonium salt, alkyl polyoxyethylene base ether sulfate, sulfomethylated lignin
One of hydrochlorate, lignin, carboxymethyl cellulose, sodium carboxymethylcellulose, azone, thiophene ketone are several, and common steady
Determine 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 secondary monooctyl ester water dispersible granules (WDG) of the Herbicidal combinations TAM-5 fluroxypramide of embodiment 1:30%
60 grams of TAM-5, the secondary monooctyl ester of 240 grams of fluroxypramides, 20 grams of dispersing agent D909S, 35 grams of lignin, 45 grams of acrylic acid are weighed respectively
Minor matters polymer, 35 grams of dodecyl sodium sulfates, 25 grams of polyethylene glycol, 40 grams of 600C suspension aids, 500 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 drying to obtain
Water dispersible granules.
The secondary monooctyl ester water dispersible granules (WDG) of the Herbicidal combinations TAM-1 fluroxypramide of embodiment 2:30%
60 grams of TAM-1, the secondary monooctyl ester of 240 grams of fluroxypramides, 30 grams of dispersing agent D909S, 30 grams of lignin, 40 grams of acrylic acid are weighed respectively
Minor matters polymer, 50 grams of dodecyl sodium sulfates, 60 grams of polyethylene glycol, 30 grams of 600C suspension aids, 460 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 drying to obtain
Water dispersible granules.
The secondary monooctyl ester TAM-5 water dispersible granules (WDG) of the Herbicidal combinations fluroxypramide of embodiment 3:30%
200 grams of TAM-5, the secondary monooctyl ester of 100 grams of fluroxypramides, 30 grams of dispersing agent D909S, 45 grams of lignin, 45 grams of propylene are weighed respectively
Sour minor matters polymer, 40 grams of dodecyl sodium sulfates, 35 grams of polyethylene glycol, 25 grams of 600C suspension aids, 480 grams of bentonites, it is standby
With；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 dry
Up to water dispersible granules.
The secondary monooctyl ester TAM-5 water dispersible granules (WDG) of the Herbicidal combinations fluroxypramide of embodiment 4:40%
350 grams of TAM-5, the secondary monooctyl ester of 50 grams of fluroxypramides, 30 grams of dispersing agent D909S, 20 grams of lignin, 30 grams of acrylic acid are weighed respectively
Minor matters polymer, 45 grams of dodecyl sodium sulfates, 55 grams of polyethylene glycol, 30 grams of 600C suspension aids, 390 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 drying to obtain
Water dispersible granules.
The secondary monooctyl ester TAM-5 suspending agent (SC) of the Herbicidal combinations fluroxypramide of embodiment 5:30%
100 grams of TAM-5, the secondary monooctyl ester of 200 grams of fluroxypramides, 25 grams of neopelexes, 45 grams of polyethylene glycol, 35 are weighed respectively
Gram lignosulfonates calcium, 30 grams, 35 grams sodium carboxymethylcelluloses of tetrabutylammonium bromide, 30 grams of aluminum magnesium silicates, 500 grams of water, it is standby
With.Each material is sequentially added in reaction kettle, just dispersion is carried out using high-speed shearing machine, is then ground in sand mill effectively
Grain diameter of components is at 2~5 μm.
The secondary monooctyl ester TAM-5 suspending agent (SC) of the Herbicidal combinations fluroxypramide of embodiment 6:20%
The secondary monooctyl ester of 180 grams of fluroxypramides, 20 grams of TAM-5,50 grams of polyethylene glycol, 40 grams of aluminum magnesium silicates, 35 grams of lignin are weighed respectively
Sulfonate calcium, 30 grams, 40 grams sodium carboxymethylcelluloses of tetrabutylammonium bromide, 35 grams of neopelexes, 570 grams of water, it is standby
With.Each material is sequentially added in reaction kettle, just dispersion is carried out using high-speed shearing machine, is then ground in sand mill effectively
Grain diameter of components is at 2~5 μm.
The secondary monooctyl ester TAM-5 suspending agent (SC) of the Herbicidal combinations fluroxypramide of embodiment 7:30%
100 grams of TAM-5, the secondary monooctyl ester of 200 grams of fluroxypramides, 40 grams of neopelexes, 25 grams of lignin sulfonic acids are weighed respectively
Salt calcium, 35 grams, 30 grams sodium carboxymethylcelluloses of tetrabutylammonium bromide, 30 grams of aluminum magnesium silicates, 80 grams of polyethylene glycol, 460 grams of water, it is standby
With.Each material is sequentially added in reaction kettle, just dispersion is carried out using high-speed shearing machine, is then ground in sand mill effectively
Grain diameter of components is at 2~5 μm.
The secondary monooctyl ester TAM-1 suspending agent (SC) of the Herbicidal combinations fluroxypramide of embodiment 8:30%
The secondary monooctyl ester of 80 grams of fluroxypramides, 220 grams of TAM-1,65 grams of polyethylene glycol, 25 grams of sodium carboxymethylcelluloses, 30 grams are weighed respectively
Lignosulfonates calcium, 35 grams, 20 grams aluminum magnesium silicates of tetrabutylammonium bromide, 25 grams of neopelexes, 500 grams of water, it is standby
With.Each material is sequentially added in reaction kettle, just dispersion is carried out using high-speed shearing machine, is then ground in sand mill effectively
Grain diameter of components is at 2~5 μm.
The secondary monooctyl ester TAM-1 suspending agent (SC) of the Herbicidal combinations fluroxypramide of embodiment 9:30%
The secondary monooctyl ester of 180 grams of fluroxypramides, 120 grams of TAM-1,45 grams of polyethylene glycol, 30 grams of lignosulfonates calcium, 35 grams are weighed respectively
Neopelex, 35 grams, 30 grams sodium carboxymethylcelluloses of tetrabutylammonium bromide, 25 grams of aluminum magnesium silicates, 500 grams of water, it is standby
With.Each material is sequentially added in reaction kettle, just dispersion is carried out using high-speed shearing machine, is then ground in sand mill effectively
Grain diameter of components is at 2~5 μm.
The secondary monooctyl ester TAM-1 suspending agent (SC) of the Herbicidal combinations fluroxypramide of embodiment 10:20%
The secondary monooctyl ester of 190 grams of fluroxypramides, 10 grams of TAM-1,50 grams of polyethylene glycol, 40 grams of lignosulfonates calcium, 30 grams are weighed respectively
Sodium carboxymethylcellulose, 35 grams, 40 grams aluminum magnesium silicates of tetrabutylammonium bromide, 35 grams of neopelexes, 570 grams of water, it is standby
With.Each material is sequentially added in reaction kettle, just dispersion is carried out using high-speed shearing machine, is then ground in sand mill effectively
Grain diameter of components is at 2~5 μm.
The secondary monooctyl ester TAM-1 suspending agent (SC) of the Herbicidal combinations fluroxypramide of embodiment 11:20%
Weigh respectively the secondary monooctyl ester of 50 grams of fluroxypramides, 150 grams of TAM-1,55 grams of lignosulfonates calcium, 30 grams of tetrabutylammonium bromide,
30 grams of sodium carboxymethylcelluloses, 40 grams of aluminum magnesium silicates, 35 grams of neopelexes, 60 grams of polyethylene glycol, 550 grams of water, it is standby
With.Each material is sequentially added in reaction kettle, just dispersion is carried out using high-speed shearing machine, is then ground in sand mill effectively
Grain diameter of components is at 2~5 μm.
The secondary monooctyl ester TAM-1 suspending agent (SC) of the Herbicidal combinations fluroxypramide of embodiment 12:30%
The secondary monooctyl ester of 280 grams of fluroxypramides, 20 grams of TAM-1,40 grams of neopelexes, 25 grams of lignosulfonates are weighed respectively
Calcium, 20 grams, 30 grams sodium carboxymethylcelluloses of tetrabutylammonium bromide, 25 grams of aluminum magnesium silicates, 80 grams of polyethylene glycol, 480 grams of water, it is standby
With.Each material is sequentially added in reaction kettle, just dispersion is carried out using high-speed shearing machine, is then ground in sand mill effectively
Grain diameter of components is at 2~5 μm.
The TAM-5 wettable powder (WP) of embodiment 13:30%
300 grams of TAM-5,35 grams of lignosulfonates calcium, 45 grams of sodium carboxymethylcelluloses, 70 grams of aluminum magnesium silicates, 40 are weighed respectively
Gram neopelex, 15 grams of tetrabutylammonium bromide, 480 grams of kaolin, 25 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 secondary monooctyl ester TAM-5(7:1 of Herbicidal combinations fluroxypramide of embodiment 14:40%) wettable powder (WP)
The secondary monooctyl ester of 350 grams of fluroxypramides, 50 grams of TAM-5,25 grams, 50 grams lignosulfonates calcium of pull powder Bx, 40 grams are weighed respectively
Sodium carboxymethylcellulose, 35 grams of aluminum magnesium silicates, 40 grams of neopelexes, 30 grams of tetrabutylammonium bromide, 380 grams of kaolinites
Soil, it is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester TAM-5 wettable powder (WP) of the Herbicidal combinations fluroxypramide of embodiment 15:40%
The secondary monooctyl ester of 100 grams of fluroxypramides, 300 grams of TAM-5, pull powder Bx 20 grams, 40 grams lignosulfonates calcium, 40 are weighed respectively
Gram sodium carboxymethylcellulose, 30 grams of aluminum magnesium silicates, 30 grams of neopelexes, 20 grams of tetrabutylammonium bromide, 420 grams of kaolinites
Soil, it is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester TAM-5 wettable powder (WP) of the Herbicidal combinations fluroxypramide of embodiment 16:25%
Weigh respectively the secondary monooctyl ester of 150 grams of fluroxypramides, 100 grams of TAM-5,35 grams of tetrabutylammonium bromide, 30 grams 35 grams of pull powder Bx
Lignosulfonates calcium, 35 grams of sodium carboxymethylcelluloses, 50 grams of aluminum magnesium silicates, 35 grams of neopelexes, 530 grams of kaolinites
Soil, it is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester TAM-5 wettable powder (WP) of the Herbicidal combinations fluroxypramide of embodiment 17:20%
The secondary monooctyl ester of 50 grams of fluroxypramides, 150 grams of TAM-5,50 grams of aluminum magnesium silicates, 50 grams of neopelexes, 40 are weighed respectively
Gram lignosulfonates calcium, 50 grams of sodium carboxymethylcelluloses, 20 grams of tetrabutylammonium bromide, 560 grams of kaolin, pull powder Bx 30
Gram, it is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester TAM-5 wettable powder (WP) of the Herbicidal combinations fluroxypramide of embodiment 18:25%
The secondary monooctyl ester of 200 grams of fluroxypramides, 50 grams of TAM-5,45 grams of lignosulfonates calcium, 45 grams of carboxymethyl celluloses are weighed respectively
Sodium, 40 grams of aluminum magnesium silicates, 45 grams of neopelexes, 40 grams of tetrabutylammonium bromide, 510 grams of kaolin, pull powder Bx 25
Gram, it is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester TAM-5 wettable powder (WP) of the Herbicidal combinations fluroxypramide of embodiment 19:50%
The secondary monooctyl ester of 450 grams of fluroxypramides, 50 grams of TAM-5,30 grams of lignosulfonates calcium, 25 grams of carboxymethyl celluloses are weighed respectively
Sodium, 30 grams of aluminum magnesium silicates, 30 grams of neopelexes, 25 grams of tetrabutylammonium bromide, 340 grams of kaolin, pull powder Bx 15
Gram, it is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester TAM-1 wettable powder (WP) of the Herbicidal combinations fluroxypramide of embodiment 20:25%
The secondary monooctyl ester of 180 grams of fluroxypramides, 70 grams of TAM-1,35 grams of tetrabutylammonium bromide, 40 grams of aluminum magnesium silicates, 35 grams of wood are weighed respectively
Mahogany sulfonate calcium, 40 grams of sodium carboxymethylcelluloses, 35 grams of neopelexes, 540 grams of kaolin, pull powder Bx 25
Gram, it is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester TAM-1 wettable powder (WP) of the Herbicidal combinations fluroxypramide of embodiment 21:20%
The secondary monooctyl ester of 50 grams of fluroxypramides, 150 grams of TAM-1,50 grams of neopelexes, 50 grams of aluminum magnesium silicates, 40 are weighed respectively
Gram lignosulfonates calcium, 50 grams of sodium carboxymethylcelluloses, 20 grams of tetrabutylammonium bromide, 560 grams of kaolin, pull powder Bx 30
Gram, it is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester TAM-1 wettable powder (WP) of the Herbicidal combinations fluroxypramide of embodiment 22:25%
The secondary monooctyl ester of 200 grams of fluroxypramides, 50 grams of TAM-1,45 grams of lignosulfonates calcium, 45 grams of carboxymethyl celluloses are weighed respectively
Sodium, 40 grams of aluminum magnesium silicates, 35 grams of neopelexes, 30 grams of tetrabutylammonium bromide, 530 grams of kaolin, pull powder Bx 25
Gram, it is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester TAM-5 water dispersible granules (WDG) of the Herbicidal combinations fluroxypramide of embodiment 23:40%
Weigh respectively the secondary monooctyl ester of 300 grams of fluroxypramides, 100 grams of TAM-5,50 grams of dodecyl sodium sulfates, 30 grams of 600C suspension aids,
45 grams of polyethylene glycol, 45 grams of acrylic acid minor matters polymer, 40 grams of lignin, 390 grams of bentonites, it is spare；Each material is successively added
Enter in reaction kettle, be uniformly mixed, then ground in sand mill, suitable quantity of water is added, is granulated, is drying to obtain water dispersible granules.
The secondary monooctyl ester TAM-5 water dispersible granules (WDG) of the Herbicidal combinations fluroxypramide of embodiment 24:50%
200 grams of TAM-5, the secondary monooctyl ester of 300 grams of fluroxypramides, 50 grams of lignin, 40 grams of acrylic acid minor matters polymer, 30 grams are weighed respectively
Dodecyl sodium sulfate, 40 grams of polyethylene glycol, 30 grams of 600C suspension aids, 310 grams of bentonites, it is spare；Each material is successively added
Enter in reaction kettle, be uniformly mixed, then ground in sand mill, suitable quantity of water is added, is granulated, is drying to obtain water dispersible granules.
The secondary monooctyl ester TAM-5TAM-1 water dispersible granules (WDG) of the Herbicidal combinations fluroxypramide of embodiment 25:30%
It is poly- that the secondary monooctyl ester of 200 grams of fluroxypramides, 50 grams of TAM-5,50 grams of TAM-1,50 grams of lignin, 50 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, 500 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 secondary monooctyl ester TAM-5TAM-1 water dispersible granules (WDG) of the Herbicidal combinations fluroxypramide of embodiment 26:30%
The secondary monooctyl ester of 260 grams of fluroxypramides, 20 grams of TAM-5,20 grams of TAM-1,50 grams of polyethylene glycol, 60 grams of dodecyl sulphurs are weighed respectively
Sour sodium, 30 grams of lignin, 20 grams of acrylic acid minor matters polymer, 30 grams of 600C suspension aids, 510 grams of bentonites, 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 secondary monooctyl ester wettable powder (WP) of the fluroxypramide of embodiment 27:40%
The secondary monooctyl ester of 400 grams of fluroxypramides, 35 grams, 40 grams lignosulfonates calcium of pull powder Bx, 40 grams of carboxymethyl celluloses are weighed respectively
Plain sodium, 20 grams of aluminum magnesium silicates, 20 grams of neopelexes, 25 grams of tetrabutylammonium bromide, 420 grams of kaolin, it is spare；System
It is standby: each material to be sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester aqueous suspension agent (SC) of the fluroxypramide of embodiment 28:20%
The secondary monooctyl ester of 200 grams of fluroxypramides, 70 grams of lignosulfonates calcium, 60 grams of sodium carboxymethylcelluloses, 30 grams of silicic acid are weighed respectively
Magnalium, 50 grams of neopelexes, 70 grams of polyethylene glycol, 520 grams of water, it is spare；Each material is sequentially added in reaction kettle,
Just dispersion is carried out using high-speed shearing machine, effective component partial size is then ground in sand mill at 2~5 μm.
The reactive compound TAM-5 aqueous suspension agent (SC) of embodiment 29:30%
The secondary monooctyl ester of 300 grams of fluroxypramides, 25 grams of defoaming agent tributyl phosphates, 40 grams of lignosulfonates calcium, 35 grams of carboxylics are weighed respectively
Sodium carboxymethylcellulose pyce, 35 grams of aluminum magnesium silicates, 45 grams of neopelexes, 60 grams of polyethylene glycol, 460 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 TAM-1 wettable powder (WP) of embodiment 30:30%
300 grams of TAM-1,45 grams of lignosulfonates calcium, 25 grams of tetrabutylammonium bromide, 35 grams of carboxymethyl celluloses are weighed respectively
45 grams, 485 grams sodium, 30 grams of aluminum magnesium silicates, 35 grams of neopelexes, pull powder Bx 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 secondary monooctyl ester TAM-1 wettable powder (WP) of the Herbicidal combinations fluroxypramide of embodiment 31:40%
The secondary monooctyl ester of 300 grams of fluroxypramides, 100 grams of TAM-1,40 grams of lignosulfonates calcium, 40 grams of carboxymethyl celluloses are weighed respectively
Sodium, 30 grams of aluminum magnesium silicates, 30 grams of neopelexes, 30 grams of tetrabutylammonium bromide, 400 grams of kaolin, pull powder Bx 30
Gram, it is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester TAM-1 water dispersible granules (WDG) of the Herbicidal combinations fluroxypramide of embodiment 32:30%
250 grams of TAM-1, the secondary monooctyl ester of 50 grams of fluroxypramides, 50 grams of lignin, 40 grams of acrylic acid minor matters polymer, 40 grams are weighed respectively
Dodecyl sodium sulfate, 40 grams of polyethylene glycol, 30 grams of 600C suspension aids, 500 grams of bentonites, it is spare；Each material is successively added
Enter in reaction kettle, be uniformly mixed, then ground in sand mill, suitable quantity of water is added, is granulated, is drying to obtain water dispersible granules.
The secondary monooctyl ester TAM-5 microcapsule formulations (CJ) of the Herbicidal combinations fluroxypramide of embodiment 33:8%
The secondary monooctyl ester of 50 grams of fluroxypramides, 30 grams of TAM-5,45 grams of gelatin, 35 grams of poly-aspartates, 20 grams of Tween-60s, 80 are weighed respectively
Gram Arabic gum, 20 grams of polyethylene glycol, 65 gram of 20% formalin, 10% acetum are appropriate, and (titer is i.e. by preparation process
Titration operation determine 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 48 DEG C of -50 DEG C of heat preservations are spare in stirring.(2) I
The preparation of primary sol solution: being added appropriate distilled water in reaction unit, Arabic gum powder is added, is heated to 80 DEG C, is gently mixed
Make to dissolve, 80 DEG C of heat preservations are spare.(3) preparation of TAM-5 and the secondary monooctyl ester effective component emulsion of fluroxypramide: TAM-5, fluroxypramide is secondary
Monooctyl ester, Tween-60, polyethylene glycol, above-mentioned preparation gumwater, be placed in tissue mashing machine, emulsify 40 seconds to get
Emulsion.(4) it mixes: under the conditions of 50~55 DEG C, above-mentioned poly-aspartate and gelatin mixed solution is added, being gently mixed makes to mix
Uniformly.(5) preparation of micro-capsule: under constant stirring, being added dropwise 10% acetum in Xiang Qianshu mixed liquor, adjust pH to 3.8~
4.0；(6) solidification of micro-capsule: under constant stirring, about 30 DEG C of distilled water being added in micro-capsule liquid, will contain micro-capsule liquid from 50~
It removes, is stirred continuously, natural cooling in 55 DEG C of water-baths, when temperature drops to 32~35 DEG C, ice cube is added, continue stirring to temperature
For 10 DEG C hereinafter, 20% formalin is added, continue 15~25min of stirring, then uses its pH 8~9 of 20%NaOH solution tune, continuation
20~30min is stirred, observation stands and settles to micro-capsule until being precipitated.(7) it the filtering and drying of micro-capsule: has been settled to micro-capsule
Entirely, it is removed by filtration supernatant, micro-capsule distillation is washed to formaldehydeless taste, centrifugation, drying.
The secondary monooctyl ester TAM-5 microcapsule formulations (CJ) of the Herbicidal combinations fluroxypramide of embodiment 34:10%
The secondary monooctyl ester of 66.7 grams of fluroxypramides, 33.3 grams of TAM-5,50 grams of gelatin, 40 grams of poly-aspartates, 20 grams of tweens-are weighed respectively
60, (titer was i.e. by preparing in right amount for 90 grams of Arabic gums, 30 grams of polyethylene glycol, 70 gram of 20% formalin, 10% acetum
Titration operation in journey determines usage amount, similarly hereinafter), 20% NaOH solution (titer), distilled water complementary to 1000 grams, it is spare；
The completely identical embodiment 33 of preparation step.
The secondary monooctyl ester TAM-1 microcapsule formulations (CJ) of the Herbicidal combinations fluroxypramide of embodiment 35:8%
The secondary monooctyl ester of 50 grams of fluroxypramides, 30 grams of TAM-1,45 grams of gelatin, 35 grams of poly-aspartates, 20 grams of Tween-60s, 80 are weighed respectively
Gram Arabic gum, 20 grams of polyethylene glycol, 65 gram of 20% formalin, 10% acetum are appropriate, and (titer is i.e. by preparation process
Titration operation determine usage amount, similarly hereinafter), 20% NaOH solution (titer), distilled water complementary to 1000 grams, it is spare；Preparation
The completely identical embodiment 33 of step.
The secondary monooctyl ester TAM-1 microcapsule formulations (CJ) of the Herbicidal combinations fluroxypramide of embodiment 36:10%
The secondary monooctyl ester of 60 grams of fluroxypramides, 40 grams of TAM-1,35 grams of gelatin, 50 grams of poly-aspartates, 20 grams of Tween-60s, 85 are weighed respectively
Gram Arabic gum, 20 grams of polyethylene glycol, 65 gram of 20% formalin, 10% acetum are appropriate, and (titer is i.e. by preparation process
Titration operation determine usage amount, similarly hereinafter), 20% NaOH solution (titer), distilled water complementary to 1000 grams, it is spare；Preparation
The completely identical embodiment 33 of step.
The secondary monooctyl ester aqueous emulsion (EW) of the fluroxypramide of embodiment 37:30%
The secondary monooctyl ester of 300 grams of fluroxypramides, 40 grams of emulsifier op-4s, 120 grams of trimethylbenzenes, 40 grams of ethylene glycol, 40 grams of epoxies are weighed respectively
Oxide-propylene oxide block copolymer, 460 grams of water, it is spare；Preparation: raw medicine, emulsifier, solvent, co-emulsifier are mixed and is made into
Uniform oil phase, water, antifreeze are mixed and are made into uniform water phase, under high shear agitation, oil are mutually poured into water phase, sufficiently
Even mixing.
The TAM-5 aqueous emulsion (EW) of embodiment 38:40%
400 grams of TAM-5,150 grams of trimethylbenzenes, 30 grams of ethylene glycol, 30 grams of epoxy ethane-epoxy propane block copolymerizations are weighed respectively
Object, 20 grams of emulsifier op-4s, 370 grams of water, it is spare；Preparation: raw medicine, emulsifier, solvent, co-emulsifier are mixed and are made into uniform oil
Water, antifreeze are mixed and are made into uniform water phase by phase, under high shear agitation, oil are mutually poured into water phase, full and uniform mixing
?.
The TAM-5 wettable powder (WP) of embodiment 39:45%
450 grams of TAM-5,35 grams of lignosulfonates calcium, pull powder Bx 20 grams, 35 grams sodium carboxymethylcelluloses, 40 are weighed respectively
Gram aluminum magnesium silicate, 30 grams of neopelexes, 20 grams of tetrabutylammonium bromide, 410 grams of kaolin, it is spare；Preparation: by each object
Material sequentially adds in reaction kettle, and stirring mixes them thoroughly, and is crushed to 5~20 μm.
The secondary monooctyl ester suspending agent (SC) of the Herbicidal combinations TAM-5 fluroxypramide of embodiment 40:30%
Weigh respectively 100 grams of TAM-5, the secondary monooctyl ester of 200 grams of fluroxypramides, 40 grams of lignosulfonates calcium, 40 grams of tetrabutylammonium bromide,
35 grams of sodium carboxymethylcelluloses, 35 grams of aluminum magnesium silicates, 30 grams of neopelexes, 50 grams of polyethylene glycol, 470 grams of water, it is standby
With.Each material is sequentially added in reaction kettle, just dispersion is carried out using high-speed shearing machine, is then ground in sand mill effectively
Grain diameter of components is at 2~5 μm.
The secondary monooctyl ester wettable powder (WP) of the Herbicidal combinations TAM-5 fluroxypramide of embodiment 41:50%
The secondary monooctyl ester of 100 grams of fluroxypramides, 400 grams of TAM-5,30 grams of lignosulfonates calcium, 30 grams of carboxymethyl celluloses are weighed respectively
Sodium, 35 grams of aluminum magnesium silicates, 35 grams of neopelexes, 20 grams of tetrabutylammonium bromide, 330 grams of kaolin, pull powder Bx 20
Gram, it is spare；Preparation: each material is sequentially added in reaction kettle, stirring mixes them thoroughly, and is crushed to 5~20 μm.
By following experiment it can be shown that above-mentioned Herbicidal combinations of the invention: the compound and fluroxypramide Zhong Xin of TAM-5
Ester forms Herbicidal combinations, the compound of TAM-1 and the secondary monooctyl ester composition Herbicidal combinations of fluroxypramide, the change of the invention with TAM-1
It closes three groups of object, the compound of TAM-5 and the secondary monooctyl ester of fluroxypramide and is divided into effective component (three kinds of effective component), 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
The secondary monooctyl ester of Herbicidal combinations TAM-5 fluroxypramide
30% reactive compound (TAM-5) wettable powder (WP) (being prepared according to the embodiment of the present invention 13), 20% fluroxypramide
To gramineae weed and broadleaf weeds (herba digitariae after secondary monooctyl ester aqueous suspension agent (SC) (being prepared according to the embodiment of the present invention 28) and compounding
Careless 1-3 leaf phase, black nightshade 1-2 leaf phase) indoor virulence experimental result, as shown in table 1.
The activity of weeding effect of 1 potted plant experiment of table
In 1 indoor pot experimental result column of table: being greater than calculated value to the activity of weeding observation of herba digitariae grass, the number in observation column
Synergy is indicated with " (+) " after value；Calculated value is greater than to the activity of weeding observation of black nightshade, is used after numerical value in observation column
" (+) " indicates synergy.1 indoor pot of table is the experimental results showed that (having analog result to herba digitariae grass and black nightshade), reactive compound
(TAM-5) after being compounded with fluroxypramide two kinds of ingredients of secondary monooctyl ester, than column range, (TAM-5 mass: fluroxypramide is monooctyl ester quality=1:1 secondary
~ 1:4) it is interior with notable synergistic effect.When TAM-5 mass is greater than the secondary monooctyl ester quality of fluroxypramide in Herbicidal combinations, we are in room
Synergy phenomenon (in table 1, being indicated after numerical value with " (-) " in observation column) is not found in interior experiment.Later, we were further
The ratio (TAM-5 mass: the secondary monooctyl ester quality of fluroxypramide=1:5,1:6,1:7,1:8,1:9,1:10) of the secondary monooctyl ester of fluroxypramide is improved,
It was found that working as TAM-5 mass: the ratio of the secondary monooctyl ester quality of fluroxypramide is 1:5, still has notable synergistic effect；The secondary monooctyl ester of fluroxypramide
After the ratio of quality is more than 1:5, synergistic effect is not significant, and more than synergistic effect is not found after 1:7, the partial data is not
It is listed in table 1.Brief summary: we are concluded that by indoor pot experiment than column range (TAM-5 mass: fluroxypramide Zhong Xin
Ester quality=1:1 ~ 1:5) in have notable synergistic effect, wherein when TAM-5 mass: the secondary monooctyl ester quality=1:3 ~ 1:4 of fluroxypramide it
Between reach optimum efficiency.Meanwhile we further carry out indoor pot experiment with TAM-1 substitution TAM-5 and obtain similar conclusion:
Than having notable synergistic effect in column range (TAM-1 mass: fluroxypramide is monooctyl ester quality=1:1 ~ 1:5 secondary), TAM-1 mass: fluorine grass
Reach optimum efficiency between the secondary monooctyl ester quality=1:3 ~ 1:4 of cigarette.
Two, the secondary monooctyl ester Herbicidal combinations field efficacy experiment of TAM-5 fluroxypramide
By taking Soybean Field as an example: in Soybean Field, big 1~3 leaf phase of bean seedlings tender shoots, 1~4 leaf phase of weeds, with 30% reactive compound
(TAM-5) wettable powder (WP) (being prepared according to the embodiment of the present invention 13), the 20% secondary monooctyl ester aqueous suspension agent (SC) of fluroxypramide
(according to the embodiment of the present invention 28 prepare) and 30% the secondary monooctyl ester water dispersible granules (WDG) of Herbicidal combinations TAM-5 fluroxypramide
(preparing according to the embodiment of the present invention 1) is to the effect experiment of soybean weeds.30 days investigation fresh weight preventive effects and 5% significant water after medicine
It is flat as shown in table 2.
Table 2 prevents and kill off the field test results of soybean weeds
The experimental result of table 2 shows, TAM-5 and the secondary monooctyl ester of fluroxypramide compounds (TAM-5 mass: fluorine grass in the present composition
The secondary monooctyl ester quality=1:4 of cigarette), in field experiment, notable synergistic effect is shown, and degrass spectrum can be expanded, while without antagonism
Effect improves crop safety, significantly improves herbicidal effect, reduce costs.By table 2 the experimental results showed that, by two kinds
The composite weedicide of single dose pharmaceutical composition, the preventive effect in 3 kinds of different weeds experiments is above the single-dose of full dosage respectively
Object further illustrates that TAM-5 can have significant synergistic effect after compounding with the secondary monooctyl ester of fluroxypramide, and without antagonism, to soybean
Safety.
Three, the secondary monooctyl ester Herbicidal combinations field efficacy experiment of TAM-1 fluroxypramide
By taking Soybean Field as an example (similar with the secondary monooctyl ester Herbicidal combinations field efficacy experiment condition of above-mentioned TAM-5 fluroxypramide):
In Soybean Field, big 1~3 leaf phase of bean seedlings tender shoots, 1~4 leaf phase of weeds, with 30% reactive compound (TAM-1) wettable powder
(WP) (preparing according to the embodiment of the present invention 30), the 20% secondary monooctyl ester aqueous suspension agent (SC) of fluroxypramide are (according to the embodiment of the present invention 28
Preparation) and 30% the secondary monooctyl ester water dispersible granules (WDG) of Herbicidal combinations TAM-1 fluroxypramide (according to the embodiment of the present invention 2 make
It is standby) to the effect experiment of soybean weeds.30 days investigation fresh weight preventive effects and 5% level of signifiance are as shown in table 3 after medicine.
Table 3 prevents and kill off the field test results of soybean weeds
The experimental result of table 3 shows, TAM-1 and the secondary monooctyl ester of fluroxypramide compounds (TAM-1 mass: fluorine grass in the present composition
The secondary monooctyl ester quality=1:4 of cigarette), in field experiment, certain synergistic effect is shown (with the secondary monooctyl ester weeding of TAM-5 fluroxypramide
Composition compares, and effect has certain gap), crop safety is improved, herbicidal effect is improved to a certain extent, reduces into
This.By table 2, table 3 the results showed that under 1, same dose, the herbicidal effect ratio TAM-5 effect of TAM-1 is slightly poor；2,TAM-
1 also has notable synergistic effect (although compared with the secondary monooctyl ester Herbicidal combinations of TAM-5 fluroxypramide with the secondary monooctyl ester compounding of fluroxypramide
Effect has certain gap).
Claims (9)
1. weeding pesticide composition, thio with 2- (the fluoro- 2- pyridine acyloxy of 6-)-N- (4- fluorophenyl)-N- (1- Methylethyl)
Acetamide (TAM-5) and the secondary monooctyl ester of fluroxypramide collectively constitute for acceptable auxiliary element in effective component, with pesticide, wherein
With 2- (the fluoro- 2- pyridine acyloxy of 6-)-N- (4- fluorophenyl)-N- (1- Methylethyl) thioacetamide (TAM-5) and fluroxypramide
Secondary monooctyl ester weight ratio is 100:1 to 1:100.
2. weeding pesticide composition as described in claim 1, it is characterized in that the effective component 2- (the fluoro- 2- pyridine acyl-oxygen of 6-
Base)-N- (4- fluorophenyl)-N- (1- Methylethyl) thioacetamide (TAM-5) and the secondary monooctyl ester weight ratio of fluroxypramide be 5:1 extremely
1:20。
3. weeding pesticide composition as described in claim 1, it is characterized in that the effective component 2- (the fluoro- 2- pyridine acyl-oxygen of 6-
Base)-N- (4- fluorophenyl)-N- (1- Methylethyl) thioacetamide (TAM-5) and the secondary monooctyl ester weight ratio of fluroxypramide be 1:1 extremely
1:5。
4. such as claim 1 herbicidal composition, by current conventional pesticide production method, be prepared into it is various forms of for
Wettable powder (WP), water dispersible granules (WDG), suspending agent (SC), the aqueous emulsion (EW), suspoemulsion (SE), microcapsules used
Any dosage form in the preparation formulations such as agent (CJ).
5. weeding pesticide composition as described in claim 1, it is characterized in that 2- (the fluoro- 2- pyridine acyloxy of 6-)-N- (4- fluorobenzene
Base)-N- (1- Methylethyl) thioacetamide (TAM-5) can be by compound 2- (the 6- chloro- 2- pyrrole similar with TAM-5 structure
Pyridine acyloxy)-N- (4- fluorophenyl)-N- (1- Methylethyl) thioacetamide (TAM-1) replacement.
6. weeding pesticide composition as described in claim 1, it is characterized in that 2- (the fluoro- 2- pyridine acyloxy of 6-)-N- (4- fluorobenzene
Base)-N- (1- Methylethyl) thioacetamide (TAM-5) can be by compound 2- (the 6- chloro- 2- pyrrole similar with TAM-5 structure
Pyridine acyloxy) partially replacement forms 2- (the fluoro- 2- of 6- to-N- (4- fluorophenyl)-N- (1- Methylethyl) thioacetamide (TAM-1)
Pyridine acyloxy)-N- (4- fluorophenyl)-N- (1- Methylethyl) thioacetamide (TAM-5), 2- (6- Chloro-2-Pyridyle acyl-oxygen
Base)-N- (4- fluorophenyl)-N- (1- Methylethyl) thioacetamide (TAM-1) and fluroxypramide secondary monooctyl ester composition be three components
Weeding pesticide composition.
7. weeding agricultural chemical compositions as described in claim 1, it is characterized in that being used for wheat paddock, Soybean Field, barley field, corn field
Equal industrial crops field weeding.
8. weeding agricultural chemical compositions as described in claim 1, it is characterized in that for grape, tomato, capsicum, potato, educating
Seedling leek, pimento, eggplant, semen viciae fabae, pea, onion etc. vegetable farm herbicide.
9. its composition is activating plants agent, agrochemical function using function such as claim 1 weeding agricultural chemical compositions
In this patent rights protection scope.
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| Title |
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| 张红刚: "高效除草剂氟草烟仲辛酯合成工艺研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
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