CN107027774B - A kind of ternary weeding composition containing Pendimethalin - Google Patents
A kind of ternary weeding composition containing Pendimethalin Download PDFInfo
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- CN107027774B CN107027774B CN201710440048.8A CN201710440048A CN107027774B CN 107027774 B CN107027774 B CN 107027774B CN 201710440048 A CN201710440048 A CN 201710440048A CN 107027774 B CN107027774 B CN 107027774B
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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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
- A01N33/18—Nitro compounds
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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
- A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
- A01N43/40—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
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- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
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- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
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- General Health & Medical Sciences (AREA)
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Abstract
The present invention relates to a kind of ternary weeding composition, for the Herbicidal combinations comprising Pendimethalin, flufenacet and diflufenican as active constituent, the weight ratio of three is 35:3‑5:1‑2.Further, the present invention is configured to microcapsule suspension suspending agent by selecting specific oil-soluble capsule material.Synergistic effect is presented compared to unitary single dose, binary built composition with the ternary weeding composition of special ratios in the present invention, and application is strong in production practices；The microcapsule suspension suspending agent of the present invention has good quick-release, slow release effect in performance, forms homogeneous suspension system, is used for closing weeding, more saving of work and time before broadcasting rear seedling；Particularly, microcapsule suspension suspending agent of the invention is especially made with specific preparation method, stability, especially heat storage stability and low-temperature stability are excellent due to having selected specific oiliness capsule material.
Description
Technical field
The present invention relates to herbicide field, more particularly to a kind of complex herbicidal composition, and in particular to one kind includes diformazan
Penta pleasure spirit, flufenacet and diflufenican ternary weeding composition.
Technical background
Pendimethalin is also known as amine and disappears grass or pendimethalin, is the phenyl amines weeding succeeded in developing by American Cyanamid Company
Agent.Pendimethalin is a kind of outstanding dry crop selective herbicide, can effectively prevent and kill off annual gramineae and certain one
Year life broad leaved weed, is widely used in a variety of works such as corn and soybean, peanut, cotton, direct-seeding dry rice, potato, tobacco, vegetables
Object prevents the weeds such as barnyard grass, lady's-grass, green bristlegrass, annual bluegrass, lamb's-quarters, the amaranth in field；Since Pendimethalin has good weeding
Hypotoxicities selective and to people, animal, Pendimethalin is the 3rd big herbicide of the world at present, and sales volume is only second to natural disposition of going out
Herbicide glyphosate, paraquat are the maximum selective herbicides of sales volume in the world.However chronic administration single dose, study table
Bright, a variety of weeds gradually produce resistance, therefore more and more research steering research Pendimethalins and other activity of weeding
The combination of ingredient reduces resistance while continuing to play Pendimethalin drug effect, especially common with other active constituents
Reach synergistic effect.
The more prior arts report the complex composition that Pendimethalin is combined with other active components, such as
200780039986.1 disclosing the Herbicidal combinations of Pendimethalin and flumioxazin；201380066614,3 disclose two
First penta find pleasure in spirit and diflufenican Herbicidal combinations；201510391390.4 disclosing removing for Pendimethalin and flufenacet
Careless composition, 201210011440.8 disclose the Herbicidal combinations etc. of Pendimethalin and pyrithiobac-sodium；About including two
First penta find pleasure in spirit ternary weeding composition, only disclosed in 201310300099.2 in the prior art comprising pendimethalin,
The ternary recompounded composite of three kinds of active constituents of Oxyfluorfen and Evil humulones, the ternary composition is in prevention peanut weeds in field
When have synergistic effect.
However the existing binary comprising Pendimethalin active constituent, ternary weeding composition still have resistance and ask
Topic, and the activity after combination is still not high enough.
Invention content
The purpose of the present invention is to provide a kind of ternary weeding composition including Pendimethalin, the composition, which removes, to be prolonged
Outside the resistance of slow Pendimethalin, there is good synergistic effect, obtained Herbicidal combinations weeding effect between active constituent
Fruit is notable；Further, when the ternary composition is configured to preparation, micro-capsule is configured to using specific adjuvant and is hanged
Floating-suspending agent, it is time saving and energy saving when obtained microcapsules is used to close weeding, while can achieve the effect that quick-release and sustained release.
To achieve the purpose of the present invention, the present invention provides a kind of ternary weeding composition, which is characterized in that the weeding group
Object is closed comprising Pendimethalin, flufenacet and diflufenican as active constituent, the weight ratio of three is 3-5:3-5:1-
2。
It is highly preferred that the weight ratio of three is 4-5:3-4:1；More preferably 5:3:1.
Further, the ternary weeding composition includes acceptable auxiliary agent in agriculture medication, and wherein active constituent accounts for
The 5-50 weight % of Herbicidal combinations.Preferably 20-40 weight %.
Further, the present invention is provided is configured to microcapsule suspension-suspendinagent agent by above-mentioned Herbicidal combinations, which is characterized in that
The Pendimethalin is configured to microcapsule suspending agent, and flufenacet and diflufenican are configured to suspending agent, wherein microcapsule diameter
It is 5-7 μm.
According to above-mentioned microcapsule suspension-suspendinagent agent, which is characterized in that it includes each components following by weight：
The cyst material is oiliness capsule material selected from the group below：Toluene di-isocyanate(TDI), methyl diphenylene diisocyanate
Or 4,4- methyl diphenylene diisocyanates.
The solvent is selected from petroleum ether, ethyl acetate, dichloromethane, chloroform, benzene or dimethylbenzene；The auxiliary agent is
Selected from dispersion moisture agent, emulsifier, thickener, antifreezing agent or antifoaming agent；The dispersion moisture agent is selected from detergent alkylate sulphur
Sour calcium, sodium methylene bis-naphthalene sulfonate, sodium lignin sulfonate, calcium lignosulfonate, aliphatic alcohol polyoxyvinethene phosphate, fatty alcohol
At least one of polyoxyethylene ether, lauryl sodium sulfate and diisobutyl naphthalene；The emulsifier is selected from benzene second
Alkenyl phenol polyethenoxy ether phosphate, Ben-zylphenol Polyoxyethyl Ether phosphate, anhydrous sorbitol tristearate, polyoxyethylene mountain
Six stearate of pears ether alcohol, cithrol, diethylene glycol monolaurate, Brij30, polyoxy second
At least one of alkene monopalmitate and anhydrous sorbitol APEO；The thickener is selected from aluminum magnesium silicate, xanthan
At least one of glue, polyvinyl alcohol, sodium alginate, guar gum, sodium carboxymethylcellulose, organobentonite and white carbon；It is described
Antifreezing agent is selected from least one of ethylene glycol, 1,2- propylene glycol, glycerine, urea, polyethylene glycol and sorbierite；It is described to disappear
Infusion is selected from least one of polyether antifoam agent, organic silicon defoamer and Siloxane-Oxyalkylene Copolymers antifoaming agent.
According to the preparation method of above-mentioned microcapsule suspension-suspendinagent agent, which is characterized in that described method includes following steps：
Step 1: Pendimethalin, solvent, cyst material and emulsifier are mixed, the first mixture is obtained；It again will dispersion
Wetting agent and antifoaming agent are mixed with water, then are mixed with first mixture, then shear, obtain first material；Wherein phase
For the Pendimethalin of 100 parts by weight, the dosage of dispersion moisture agent is 15-30 parts by weight, the dosage of antifoaming agent is
The dosage of 0.2-1.5 parts by weight, water is 150-240 parts by weight；
Step 2: flufenacet, diflufenican and water, dispersion moisture agent, antifoaming agent, antifreezing agent and thickener are mixed
Frosted processing is carried out afterwards, obtains second material；The dosage of flufenacet wherein relative to 100 parts by weight, water is 150-220
Part, the dosage of dispersion moisture agent be 15-30 parts by weight；The dosage of antifoaming agent is 0.2-1.8 parts by weight；
Step 3: the first material, second material are mixed, microcapsule suspension-suspendinagent agent is made.
Preferably, the step is a kind of, and the condition of shear treatment is 10000-13000 revs/min, and the time is 1-15 points
The temperature of clock, the heating is 35-68 DEG C, and the time is 1-4 hours.
Further, the present invention is provided above-mentioned ternary weeding composition and microcapsule suspension-suspendinagent agent for preventing and kill off broad-leaved
Weeds or grassy weed, especially for preventing and kill off amur foxtail, wild oat, little Mai Wang grass or clearvers.
It is explained about principle：Although the prior art have been disclosed for pendimethalin and flufenacet and pendimethalin and
The binary Herbicidal combinations of diflufenican, however binary and the mechanism of ternary effect differ greatly, not binary synergy, herein
On the basis of other components be added be formed by ternary with regard to certain synergy, the present inventor is had found by years of researches, when
By three kinds of active constituents, when especially combining at a specific ratio, synergistic effect compares single dose, compares binary combination effect
Significantly；In addition, for the ternary composition of the present invention is further configured to microcapsule suspension-suspendinagent agent, corresponding activity at
It is good with auxiliary agent compatibility to divide, and finally forms homogeneous suspension system together, is especially coated when using specific oiliness capsule material,
So that the stability of final preparation, especially heat storage stability and low-temperature stability have greatly improved.
Advantageous effect：
1, increasing is presented compared to unitary single dose, binary built composition with the ternary weeding composition of special ratios in the present invention
Effect acts on, and application is strong in production practices；
2, microcapsule suspension-suspendinagent agent of the invention has good quick-release, slow release effect in performance, forms homogeneous hang
Floating body system is used for closing weeding, more saving of work and time before broadcasting rear seedling；Particularly, microcapsule suspension-suspendinagent agent of the invention is due to choosing
Specific oiliness capsule material has been selected, has especially been made with specific preparation method, stability, especially heat storage stability and low temperature
Excellent in stability.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that described herein, specific examples are only used to explain the present invention, is not used to limit
The fixed present invention.
One, toxicity measures
The preparation method of test medicine is as follows：
Test medicine solution：The accurate Pendimethalin, flufenacet and diflufenican for weighing constant weight 95% is former
Medicine is dissolved with suitable methanol, is added in the clear water l containing 0.1% Tween 80 emulsifier, is stirred until homogeneous, that is, is configured to contain
There is the solution of certain active ingredient.Placebo solution：Add the water of the Tween 80 emulsifier of equivalent 0.1% with equivalent methanol.
Test method is as follows：Activity of the mixed rear medicament to amur foxtail, little Mai Wang grass is examined using gowing methods, in height
The soil of the polypots amount of setting of 7cm, diameter 10cm will uniformly be sowed in polypots for 20, seed for trying weeds, cover 0.5-
The thin sand and soil of 1cm thickness, is placed on room temperature (20 DEG C or so) day optical culture, and the above-mentioned a bulk solution prepared is compounded and is diluted to one
The liquid for determining concentration gradient carries out cauline leaf spraying treatment when weed growth is to the 3-5 leaf phases, each to handle per alms bowl spraying liquid 1ml
4 repetitions, are compared using blank solution.Test material is placed in culture, the growth feelings of routine observation weeds in room temperature after processing
Condition estimates the damage symptoms and growth inhibition situation of target weeds after 21 days, weigh strain fresh weight, calculates fresh weight inhibition rate
(%).
The synergy of ternary weeding composition evaluation method is as follows：
E0(%)=X*Y*Z/1002
E in formula0To be to the theoretical value for the percentage that weeds fresh weight inhibition rate is control, E after three kinds of active ingredient mixtures
After three kinds of active ingredient mixtures to weeds inhibiting rate be control percentage measured value, X be Pendimethalin at this dose
To the percentage that target weeds fresh weight inhibition rate is control, Y is flufenacet at this dose to target weeds fresh weight inhibition rate
For the percentage of control, Z is that diflufenican is at this dose the percentage compareed to target weeds fresh weight inhibition rate, when
E0-E be more than 10 when be synergistic effect, be less than 10 when be antagonism, between ± 10 when be addition.
The raw test of 1 Pendimethalin of table, flufenacet and diflufenican different ratio to amur foxtail activity of weeding
As a result
It is seen from the above data that Pendimethalin, flufenacet and diflufenican are multiple within the scope of application
It is excellent to the preventive effect of amur foxtail after matching, after three kinds of ingredient compoundings, there are significant synergistic effect, synergy coefficient to be all higher than 10,
Especially when the proportioning of three is 5:3:When 1, the two synergistic effect is optimal.And when three is with 3:6:2.5、4:6:2.5、5:6:
After 2.5 compoundings, three shows as antagonism.
Further, in order to compare the activity that ternary composition compares binary combination, applicant is by Pendimethalin, fluorine thiophene
Careless amine is according to 5:3 compoundings, are known as A1；It is configured to triple combination with third component diflufenican, carries out preventing and kill off amur foxtail
Determination of activity.
Evaluation of effect method evaluates herbicide mode of application according to gowing methods, and formula is as follows：
E0(%)=X+Y × (100-X)/100
C=E-E0
E in formula0For the theoretical preventive effect inhibited to weeds after two kinds of active ingredient mixtures, after E is two kinds of active ingredient mixtures
To the actual measurement preventive effect that weeds inhibit, X is A1 at this dose to the preventive effect of target weeds, Y be diflufenican at this dose
To the preventive effect of target weeds, C is that the synergy coefficient of mixture preparation works as C to evaluate the synergistic effect of two kinds of active ingredient
When more than 10 be synergistic effect, be less than 10 when be antagonism, between ± 10 when be addition.
Table 2：Ternary weeding composition of the present invention prevents and kill off the herbicide effect of amur foxtail
As can be seen from the above table, when A1 and diflufenican are with 8:When 1 proportioning, the two synergistic effect is most notable.
According to the above identical method, by Pendimethalin and diflufenican according to 5:1 compounding, is known as A2, with the
Three component flufenacets combine, and carry out the determination of activity for preventing and kill off amur foxtail.
Table 3：Ternary weeding composition of the present invention prevents and kill off the herbicide effect of amur foxtail
As can be seen from the above table, when A2 and flufenacet are with 80:When 40, synergistic effect is most notable.
According to the above identical method, by flufenacet and diflufenican according to 3:1 compounding, is known as A3, with third
Component Pendimethalin combines, and carries out the determination of activity for preventing and kill off amur foxtail.
Table 4：Ternary weeding composition of the present invention prevents and kill off the herbicide effect of amur foxtail
As can be seen from the above table, when A3 and Pendimethalin are with 40:When 50, synergistic effect is most notable.
In addition, according to the method described above, it is tested to wheat after Pendimethalin, flufenacet and diflufenican are compounded
Wang grass, wild oat and clearvers preventive effect, synergy coefficient is also all higher than 10, and opposite binary built composition two
Member, synergy coefficient are also all higher than 10.
Two, embodiment is prepared
Embodiment 1：By 100g Pendimethalins, 100g petroleum ethers, 15g toluene di-isocyanate(TDI)s and 20g styryl phenol
Polyoxyethylene ether phosphate mixes, and obtains the first mixture；Again by 20g calcium dodecyl benzene sulfonates and 1g organosilicons and 200g water
It mixes, then is mixed with first mixture, then shear, obtain first material；The condition of shear treatment be 12000 turns/
Minute, the time is 8 minutes, is warming up to 50 DEG C of insulation reactions 2 hours；By 60g flufenacets, 20g diflufenicans and 200g water,
Frosted processing is carried out after 20g calcium dodecyl benzene sulfonates, 1g organosilicons, 30g ethylene glycol and the mixing of 2g xanthans, obtains the second object
Material；The first material, second material are mixed, microcapsule suspension-suspendinagent agent is made.
Embodiment 2：In addition to cyst material is methyl diphenylene diisocyanate, remaining is the same as embodiment 1；
Embodiment 3：Except cyst material is 4,4- methyl diphenylene diisocyanates, remaining is the same as embodiment 1；
Embodiment 4：In addition to Pendimethalin is 60g, remaining is the same as embodiment 1；
Embodiment 5：In addition to flufenacet is 100g, remaining is the same as embodiment 1；
Embodiment 6：In addition to diflufenican is 40g, remaining is the same as embodiment 1.
Comparative example 1：In addition to cyst material is ethylenediamine, remaining is the same as embodiment 1；
Comparative example 2：In addition to cyst material is diethylene glycol, remaining is the same as embodiment 1；
Comparative example 3：In addition to cyst material is triethanolamine, remaining is the same as embodiment 1；
Comparative example 4：Except cyst material is outside 1,6-, six methylene phenylene diisocyanates, remaining is the same as embodiment 1；
Comparative example 5：In addition to cyst material is aliphatic triisocyanate, remaining is the same as embodiment 1.
Three, quantitative measurement embodiment
The microcapsule suspension-of the present invention that this testing example is used to be prepared in testing example 1-6 and comparative example 1-5 is outstanding
The heat storage stability and low-temperature stability of floating agent.
Heat storage stability is tested：Microcapsule suspension-suspendinagent agent in above-described embodiment and comparative example is fitted into container, is sealed
It is positioned over afterwards in the constant temperature oven of (54 ± 2) DEG C, observation is taken out after standing 14 days, according to GB/T14825-2006 standards, measure
Suspensibility the results are shown in Table 5.
Low-temperature stability measures：Microcapsule suspension-suspendinagent agent in above-described embodiment and comparative example is fitted into container, is sealed
Be placed in (0 ± 2) DEG C refrigerator, keep 1h, primary, each 15s is stirred at interval of 15min, observation appearance have it is unchanged,
(0 ± 2) DEG C continues to place 7 days, then takes out after being placed in and standing restore under room temperature, according to GB/T14825-2006 standards,
Suspensibility is measured, the results are shown in Table 5.
Mobile performance wherein about evaluation heat storage stability and low-temperature stability, is classified as follows：
1 grade of excellent flowability, no layering caking；
2 grades of mobility are substantially qualified, a small amount of layering caking；
3 grades of viscosity increase, a large amount of layering cakings.
Table 5
As can be seen from the above table, when cyst material is water-soluble cyst material, the stability of obtained preparation, especially
It is that low-temperature stability and heat storage stability are all poor, wherein when cyst material selects not this Applicant's Abstract graph specific oiliness cyst material,
Its stability is also than selecting specific cyst material poor worse；In addition, even if in the application active constituent amount ranges, it is real
Apply the preferred scope that example 1 is the application, the active constituent of the dosage and auxiliary agent have better compatibility (referring to embodiment 1,
Embodiment 4-6), corresponding stability is also more preferably.
A kind of ternary weeding composition containing Pendimethalin of the present invention is retouched by specific example
It states, those skilled in the art can use for reference the content of present invention, and the links such as appropriate feed change, process conditions are corresponding other to realize
Purpose, correlation change all without departing from present disclosure, and all similar substitutions and modifications are for those skilled in the art
For be it will be apparent that being considered as being included within the scope of the present invention.
Claims (5)
1. a kind of microcapsule suspension-suspendinagent agent of ternary weeding composition, which is characterized in that the Herbicidal combinations include diformazan penta
As active constituent, the Pendimethalin is configured to microcapsule suspending agent, flufenacet for happy spirit, flufenacet and diflufenican
It is configured to suspending agent with diflufenican, wherein microcapsule diameter is 5-7 μm；The microcapsule suspension-suspendinagent agent includes by weight
Following each component：
The cyst material is oiliness capsule material selected from the group below：Toluene di-isocyanate(TDI) or methyl diphenylene diisocyanate.
2. the preparation method of microcapsule suspension-suspendinagent agent according to claim 1, which is characterized in that the method includes such as
Lower step：
Step 1: Pendimethalin, solvent, cyst material and emulsifier are mixed, the first mixture is obtained；Again by dispersion moistening
Agent and antifoaming agent are mixed with water, then are mixed with first mixture, then shear, obtain first material；Wherein relative to
For the Pendimethalin of 100 parts by weight, the dosage of dispersion moisture agent is 15-30 parts by weight, the dosage of antifoaming agent is 0.2-1.5
The dosage of parts by weight, water is 150-240 parts by weight；
Step 2: flufenacet, diflufenican and water, dispersion moisture agent, antifoaming agent, antifreezing agent and thickener are mixed laggard
Row frosted is handled, and obtains second material；The dosage of flufenacet wherein relative to 100 parts by weight, water is 150-220 parts, divides
The dosage for dissipating wetting agent is 15-30 parts by weight；The dosage of antifoaming agent is 0.2-1.8 parts by weight；
Step 3: the first material, second material are mixed, microcapsule suspension-suspendinagent agent is made.
3. the preparation method of microcapsule suspension-suspendinagent agent according to claim 2, which is characterized in that in the step 1, cut
The condition for cutting processing is 10000-13000 revs/min, and the time is 1-15 minutes.
4. microcapsule suspension-suspendinagent agent according to claim 1 is used to prevent and kill off the purposes of broad leaved weed or grassy weed.
5. purposes according to claim 4, which is characterized in that the weeds are amur foxtail, wild oat, little Mai Wang grass or pig
Calamity calamity.
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| PT2515658T (en) * | 2009-12-17 | 2016-09-13 | Bayer Ip Gmbh | Herbicidal agents containing flufenacet |
| UA108372C2 (en) * | 2010-02-03 | 2015-04-27 | COMPOSITION OF PENDIMETHALINE Capsular SUSPENSION, METHOD OF ITS PREPARATION AND METHOD OF FIGHTING UNWANTED PLANTS | |
| RU2629663C2 (en) * | 2012-06-27 | 2017-08-31 | Байер Кропсайенс Аг | Herbicides containing flufenacet |
| CN104082324B (en) * | 2014-07-09 | 2016-08-24 | 联保作物科技有限公司 | A kind of Wheat field weeding composition and pharmaceutical preparation thereof |
| CN104904728A (en) * | 2015-07-02 | 2015-09-16 | 张家港市植保植检站 | Pesticide combination containing flufenacet and pendimethalin and appliance thereof |
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