CN105248436A - Dispersible oil suspending agent of quinclorac, cyhalofop-butyl and penoxsulam composite herbicide and preparation method of dispersible oil suspending agent - Google Patents
Dispersible oil suspending agent of quinclorac, cyhalofop-butyl and penoxsulam composite herbicide and preparation method of dispersible oil suspending agent Download PDFInfo
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- CN105248436A CN105248436A CN201510726709.4A CN201510726709A CN105248436A CN 105248436 A CN105248436 A CN 105248436A CN 201510726709 A CN201510726709 A CN 201510726709A CN 105248436 A CN105248436 A CN 105248436A
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- cyhalofop
- butyl
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- quinolinic acid
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Abstract
The invention relates to the technical field of pesticide compounding, in particular to a dispersible oil suspending agent of a quinclorac, cyhalofop-butyl and penoxsulam composite herbicide and a preparation method of the dispersible oil suspending agent. The composite pesticide comprises the following raw materials and auxiliary materials in parts by weight: 10 parts of quinclorac, 7 parts of cyhalofop-butyl, 3 parts of penoxsulam, 3 parts of dispersion agents, 5 parts of wetting agents, 0.5 part of thickening agents, 0.3 part of preservatives, 0.5 part of defoaming agents and 71.7 parts of de-ionized water. The preparation method of the dispersible oil suspending agent of the composite pesticide comprises the following steps of extracting each raw and auxiliary material into a preparation kettle to be mixed and uniformly stirred; performing primary milling by a colloid mill; performing fine milling by a sand mill; performing filtering; controlling the suspension rate to be higher than or equal to 90 percent and the 75mum test sieve passing rate to be higher than or equal to 98 percent; after the sampling analysis qualification, performing metering, packaging and warehouse entering.
Description
Technical field
The present invention relates to technical field of pesticide combination, what be specifically related to a kind of dichloro quinolinic acid, cyhalofop-butyl and penoxsuam compound herbicide dispersibles oil-suspending agent and preparation method thereof.
Background technology
There is weed killer herbicide several frequently seen as follows in the market:
Dichloro quinolinic acid (quinclorac) is the new selective seedling post processing weed killer herbicide of BASF Aktiengesellschaft's exploitation, belong to hormone-type quinoline beautiful jade shuttle acids medicament, it is herbicide for paddy field after bud before bud, be mainly used in the barnyard grass in water prevention rice field and part broad leaved weeds, special efficacy is had to 4-6 leaf phase barnyard grass, have that consumption is few, the longevity of residure is long, use the advantages such as optimum period is wide, can Bidirectional Conduction in plant corpus, by site absorption such as seed, root, plumular axis, leaves, occur after process that leaf curling is out of shape, color reddens intensification, and 2-4 week whole strain dye grass is dead.Very popular since emerging, become rapidly be most widely used in paddy field one of except barnyard grass agent, but, the reason such as to use due to this medicine and administrated method is incorrect cause barnyard grass for years and the resistance of dichloro quinolinic acid strengthened.
Cyhalofop-butyl (cyhalofop-butyl) Chinese commodity are called a thousand pieces of gold, it is the fragrant phenoxy phenoxy propionic acid weed killer herbicide developed by The Dow Agrosciences, LLC., also be unique a kind of kind paddy rice to tight security in this type of weed killer herbicide, belong to acetyl-CoA carboxylase (ACCase) inhibitor, for Uptake and translocation weed killer herbicide, conduct in plant corpus after being absorbed by blade and leaf sheath, be absorbed into weeds Mortality Ratio from cyhalofop-butyl comparatively slow, generally need 1-3 week.Be mainly used in preventing and kill off important grassy weed, cyhalofop-butyl is efficient to moleplant seed, has certain preventive effect, also can prevent and kill off lady's-grass, Paspalum distichum, green foxtail, eleusine indica, amur foxtail etc. to low age barnyard grass, to sedge weed and broad leaved weed invalid.
Penoxsuam (penoxsulam) Chinese commodity are called rice outstanding person, with weed killer herbicide after the seedling developed by The Dow Agrosciences, LLC., it is triazolopyrimidine sulfonamide weed killer herbicide, works by suppressing acetolactate synthestase (ALS).For current rice field broad-spectrum herbicide, it is inner-adsorption conduction-type herbicide, through cauline leaf, young shoot and Root Absorption, conduct to meristematic tissue by xylem and phloem, suppress plant strain growth, make growing point chlorosis, after process, the bud mutation of 7-14 zenith is red, downright bad, and 2-4 week plant is dead.Effectively can prevent and kill off barnyard grass, annual sedge weed, and effective to numerous broad leaved weed, the lasting period reaches 30-60 days, a drug energy basic controlling full season Weed infestation, but use cost is higher, and invalid to moleplant seed weeds.
Therefore existing weed killer herbicide weeding category is single, good effect can not be had to multiple careless class.
Summary of the invention
For the problems referred to above, the invention provides a kind of cost low, a kind of dichloro quinolinic acid of good herbicidal effect, cyhalofop-butyl and a penoxsuam compound herbicide can be had to polytype weeds simultaneously dispersible oil-suspending agent.
To achieve the above object of the invention, a kind of dichloro quinolinic acid of the present invention, cyhalofop-butyl and penoxsuam compound herbicide dispersible oil-suspending agent, comprise the raw material of following weight portion:
Dichloro quinolinic acid 10, cyhalofop-butyl 7, penoxsuam 3.
Further, the auxiliary material of following weight portion is also comprised:
Dispersant 3, wetting agent 5, thickener 0.5, preservative 0.3, defoamer 0.5, anhydrate ion 71.7.
Further, described dispersant is fatty alcohol-polyoxyethylene ether.
Further, described wetting agent is phenethyl phenol APEO.
Further, described thickener xanthans.
Further, described preservative is Sodium Benzoate.
Further, described weed killer herbicide is suspending agent.
To achieve the above object of the invention, the present invention prepares the method dispersibling oil-suspending agent of above-mentioned a kind of dichloro quinolinic acid, cyhalofop-butyl and penoxsuam compound herbicide, comprise raw and auxiliary material suction preparation still mixing and stirring, just grind through colloid mill, then through sand mill fine grinding, filter, and control suspensibility >=90%, 75 μm of testing sieve percent of pass >=98%, after sample analysis is qualified, metering, packaging, warehouse-in.
Beneficial effect:
Compared with existing correlation technique, the present invention has following beneficial effect:
Dichloro quinolinic acid prepared by the present invention, cyhalofop-butyl and penoxsuam compound herbicide dispersible oil-suspending agent, dichloro quinolinic acid, cyhalofop-butyl and penoxsuam are carried out rational mixture, have and expand control of weeds spectrum, to grassy weed, sedge weed and broad leaved weed, all there is good control efficiency; Reduce dosage and spraying times, reduce cost accounting; And three kinds of pharmacy effect mechanism there are differences, composite use is conducive to the development overcoming or delay herbicide resistance, all has positive role to aspects such as shift of weed communities.
The oil-suspending agent that dispersibles of dichloro quinolinic acid prepared by the present invention, cyhalofop-butyl and penoxsuam compound herbicide all meets technical standard of enterprise requirement in suspensibility, persistent foamability, wet screening test etc. and heat storage stability etc.
The preparation method dispersibling oil-suspending agent of dichloro quinolinic acid prepared by the present invention, cyhalofop-butyl and penoxsuam compound herbicide, preparation technology is comparatively easy, is easy to suitability for industrialized production.
Embodiment
The present invention will be further described below.
A kind of dichloro quinolinic acid of the present invention, cyhalofop-butyl and penoxsuam compound herbicide dispersible oil-suspending agent, comprise following raw material: dichloro quinolinic acid, cyhalofop-butyl, penoxsuam.
Other titles of dichloro quinolinic acid, cyhalofop-butyl, penoxsuam, structural formula and basic materialization parameter are as follows:
(1) dichloro quinolinic acid
ISO adopted name: quinclorac
CIPAC digital code: 493
CAS registration number: 84087-01-4
The chloro-8-Quinoline Carboxylic Acid of chemical name: 3,7-bis-
Structural formula:
Empirical formula: C
10h
5cl
2nO
2
Relative molecular mass: 242.1
Biologically active: weeding
Fusing point: 274 DEG C
Vapour pressure (20 DEG C): < 0.01mpa
Solvability: dissolubility 0.065mg/kg in water, is slightly soluble in acetone, ethanol, ethyl acetate etc.
Stability: stable under light, heat and weak acid, weak base condition.
(2) cyhalofop-butyl
ISO adopted name: cyhalofop-butyl
CIPAC digital code: 596
CAS accession number: 122008-85-9
Chemical name: (R)-2-[4 (4-cyano group-2-fluorophenoxy) phenoxy group]-butyl propionate
Structural formula:
Empirical formula: C
20h
20fNO
4
Relative molecular mass: 357.4
Biologically active: weeding
Density (20 DEG C): 1.2375g/cm3
Fusing point: 48-49 DEG C
Vapour pressure (20 DEG C): 1.2 × 10-6Pa
Solvability: be dissolved in most of organic solvent: acetonitrile 57.3%, methyl alcohol 37.3%, acetone 60.7%, chloroform 59.4%, water insoluble.
Stability (25 DEG C): good, heat storage resolution ratio is less than 5%.
(3) penoxsuam
ISO adopted name: penoxsulam
CAS accession number: 219714-96-2
Chemical name: 3-(2,2-difluoroethoxy)-N-(5,8-dimethoxy-[1,2,4] triazol [1,5-C] pyrimidine-2-base)-α, α, α-fluoroform phenyl-2-sulfonamide
Structural formula:
Empirical formula: C
16h
14f
5n
5o
5s
Relative molecular mass: 483.7
Biologically active: weeding
Density (20 DEG C): 1.61g/mL
Fusing point: 212 DEG C
Vapour pressure (20 DEG C): 2.49 × 10-14Pa
Solvability (mg/L, 19 DEG C): water 5.7 (pH5), 410 (pH7), 1460 (pH9).
Stability: stable in the water of pH5-9.
The toxicological information of above raw material:
Dichloro quinolinic acid: rat acute per os LD
50for 2680mg/kg, rat acute is through skin LD
50> 2000mg/kg, Acute inhalation LC
50(4h) > 5.2mg/L, fish, honeybee are nontoxic, belong to low toxicity herbicide.
Cyhalofop-butyl: rat acute per os LD
50> 5000mg/kg, rat acute is through skin LD
50> 2000mg/kg.Non-stimulated to skin, there is minimal irritation to eyes, without carcinogenic, teratogenesis, mutagenesis, belong to low toxicity herbicide.
Penoxsuam: rat acute per os LD
50> 5000mg/kg, rabbit is acute through skin LD
50> 5000mg/kg, rat acute sucks LC
50(4h) > 3.5mg/L, has pole minimal irritation to eyes and skin.
Carry out weeding comparative examples below by way of several dissimilar weeds, the present invention is described further.
By type of cutting weeds: barnyard grass Echinochloacrusgalli (L.) Beauv., Monochoria vaginalis Monochoriavaginalis (Burm.f.) PreslexKunth., cyperus iria Cyperusiria (L.), difformed galingale herb Cyperusdifformis (L.).
Weeds embodiment condition of culture:
Test soil organic matter content is 2%, pH6.9, the air-dry loam that permeability is good;
Temperature 26 ± 0.5 DEG C, humidity 75 ± 5%, L: D=14: 10;
Weed seed to be soaked seed 24h through vernalization.
Embodiment medicament
Penoxsuam (penoxsulam) former medicine, content: 98%; Cyhalofop-butyl (cyhalofop-butyl) former medicine, content: 95%; Dichloro quinolinic acid (quincforac) former medicine, content: 96%.
Medicament is prepared
Above-mentioned single dose and mixture, respectively with the mother liquor preparing high concentration after acetone solution, are diluted to series mass concentration (see table 1) with the 0.1% POLYSORBATE 80 aqueous solution by the former medicine of penoxsuam, cyhalofop-butyl and dichloro quinolinic acid.
Embodiment processing method
Cauline leaf spray-on process is adopted to measure penoxsuam, cyhalofop-butyl and dichloro quinolinic acid single dose and the composite virulence to barnyard grass, Monochoria vaginalis, cyperus iria and difformed galingale herb thereof.Test paddy field soil is loaded on 4/5 place of Φ 15cm basin alms bowl, then adopts top pouring, make the complete moistening saturation state of soil.By pretreated for trying weed seed uniform broadcasting in soil surface, hot-house culture is moved into after earthing about 0.5cm, regular moisturizing ensures weeds normal growth, after weeds emerge, thinning is to the strain of every basin 15, when weeds grow to the 2-3 leaf phase, reagent agent is adopted metered dose tower directed spraying process, often process 4 times and repeat, and establish the dilution of the 0.1% POLYSORBATE 80 aqueous solution not containing medicament not make blank.After medicine, 2d adds water and makes to keep water layer 2-3cm in alms bowl, and process is raised and observed under being placed on temperature (26 ± 0.5) DEG C, relative moisture (75 ± 5) %, photoperiod L: D=(14: 10) h.
After process, 21d investigates 1 time, adopts absolute value investigation method record weeds fresh weight.
According to investigation result, be calculated as follows the fresh weight inhibition of each process, unit is percentage (%).
In formula: R is fresh weight inhibition, X
0for contrast weeds fresh weight, X
1for process weeds fresh weight.
Statistical analysis
Adopt Cloby method to test to the activity of weeding after mixed, formula is E
0=XYZ/100, E
0the theoretical weeds survival rate of weed killer herbicide (A+B+C) when representing that consumption is (O+P+Q), the weeds survival rate of weed killer herbicide A when X represents that consumption is O, the weeds survival rate of weed killer herbicide B when Y represents that consumption is P, the weeds survival rate of weed killer herbicide C when Z represents that consumption is Q; E represents the actual weeds survival rate of each process.
By Colby method, work as E
0-E > 10% is synergistic effect; Work as E
0-E <-10% is antagonism; Work as E
0-E value is addition between ± 10%.
Embodiment contrast one, the activity of weeding of penoxsuam, cyhalofop-butyl different ratio mixed with dichloro quinolinic acid:
Penoxsuam, cyhalofop-butyl and each single dose of dichloro quinolinic acid and mixed different ratio thereof are to the activity of weeding (table 1) of barnyard grass, Monochoria vaginalis, cyperus iria and difformed galingale herb
The activity of weeding of table 1 penoxsuam, cyhalofop-butyl different ratio mixed with dichloro quinolinic acid
Embodiment contrast two, the co-toxicity effect contrast of different ratio,
Penoxsuam, cyhalofop-butyl different ratio mixed with dichloro quinolinic acid is to the co-toxicity effect (showing 2-table 5) supplying to try weeds to adopt Colby method to judge.
Table 2 penoxsuam, cyhalofop-butyl and dichloro quinolinic acid different ratio are to the co-toxicity effect of barnyard grass
Table 3 penoxsuam, cyhalofop-butyl and dichloro quinolinic acid different ratio are to the co-toxicity effect of Monochoria vaginalis
Table 4 penoxsuam, cyhalofop-butyl and difluoro-quinoline acid different ratio is to the co-toxicity effect of cyperus iria
Table 5 penoxsuam, cyhalofop-butyl and dichloro quinolinic acid different ratio are to the co-toxicity effect of difformed galingale herb
Known by contrasting above, penoxsuam, cyhalofop-butyl and dichloro quinolinic acid three kinds of pharmacy effect mechanism there are differences, and composite use is conducive to the development overcoming or delay herbicide resistance, expand herbicidal spectrum, improve control efficiency.Result of the test shows: three kinds of single doses and complex preparation thereof all have good control effects to for examination weeds, the co-toxicity of mixture shows as addition, wherein, when penoxsuam, cyhalofop-butyl and dichloro quinolinic acid effective ingredient consumption ratio are 6: 14: 20 proportioning, (3: 7: 10) are active best.
Dispersible oil-suspending agent preparation method
Raw and auxiliary material by following weight portion: dichloro quinolinic acid 10, cyhalofop-butyl 7, penoxsuam 3, dispersant 3, wetting agent 5, thickener 0.5, preservative 0.3, defoamer 0.5, ion 71.7 suction of anhydrating preparation still mixing and stirring, just grind through colloid mill, again through sand mill fine grinding, filter, and control suspensibility >=90%, 75 μm of testing sieve percent of pass >=98%, after sample analysis is qualified, metering, packaging.Gained dispersibles oil-suspending agent and all meet technical standard of enterprise requirement (table 6) in suspensibility, persistent foamability, wet screening test etc. and heat storage stability etc.
Table 6 dichloro quinolinic acid, cyhalofop-butyl and penoxsuam compound herbicide dispersible oil-suspending agent item controlled index
Using method
The effective dose dispersibling oil-suspending agent water prevention rice field annual weed of dichloro quinolinic acid, cyhalofop-butyl and penoxsuam compound herbicide is 90-210 gram/ha, and application method is cauline leaf spraying.
Environmental influence
Birds acute oral toxicity (LD
50): LD
50for 1330mg/Kg.bw, low toxicity
Fish acute toxicity (LD
50or TLM): LC
50for 10.30mg/L, low toxicity
Water flea class acute toxicity: EC
50for 2.54mg/L, poisoning
Acute Toxicity of Algae silkworm (LD
50or microgram/silkworm): EC
50for 7.58mg/L, low toxicity
Honeybee acute oral toxicity (LD
50or microgram/honeybee) natural enemy and beneficial organism (LD
50): LC
50> 2000mg/L
Bee Acute exposure toxicity: LD
50(48h) > 100.0ug/ honeybee, low toxicity
Natural enemy oophagous trichogrammae class acute toxicity: safety coefficient is 114, low-risk
Silkworm class acute toxicity: LC
50for 1140mg/L, low toxicity
Earthworm acute toxicity: LC
50> 100mg/Kg dry ground, low toxicity
The present invention be should be understood that; above-described embodiment; further detailed description has been carried out to object of the present invention, technical scheme and beneficial effect; these are only embodiments of the invention; be not intended to limit the present invention, every within spiritual principles of the present invention, done any amendment, equivalent replacement, improvement etc.; all should be included within protection scope of the present invention, the protection domain that protection scope of the present invention should define with claim is as the criterion.
Claims (8)
1. dichloro quinolinic acid, cyhalofop-butyl and penoxsuam compound herbicide dispersible an oil-suspending agent, it is characterized in that, comprise the raw material of following weight portion:
Dichloro quinolinic acid 10, cyhalofop-butyl 7, penoxsuam 3.
2. a kind of dichloro quinolinic acid according to claim 1, cyhalofop-butyl and penoxsuam compound herbicide dispersible oil-suspending agent, it is characterized in that, also comprise the auxiliary material of following weight portion:
Dispersant 3, wetting agent 5, thickener 0.5, preservative 0.3, defoamer 0.5, anhydrate ion 71.7.
3. a kind of dichloro quinolinic acid according to claim 2, cyhalofop-butyl and penoxsuam compound herbicide dispersible oil-suspending agent, it is characterized in that, described dispersant is fatty alcohol-polyoxyethylene ether.
4. a kind of dichloro quinolinic acid according to claim 2, cyhalofop-butyl and penoxsuam compound herbicide dispersible oil-suspending agent, it is characterized in that, described wetting agent is phenethyl phenol APEO.
5. a kind of dichloro quinolinic acid according to claim 2, cyhalofop-butyl and penoxsuam compound herbicide dispersible oil-suspending agent, it is characterized in that, described thickener is xanthans.
6. a kind of dichloro quinolinic acid according to claim 2, cyhalofop-butyl and penoxsuam compound herbicide dispersible oil-suspending agent, it is characterized in that, described preservative is Sodium Benzoate.
7. a kind of dichloro quinolinic acid according to claim 1, cyhalofop-butyl and penoxsuam compound herbicide dispersible oil-suspending agent, it is characterized in that, described compound herbicide formulation is for dispersibling oil-suspending agent.
8. prepare the method dispersibling oil-suspending agent of claim 1 to 7 arbitrary described a kind of dichloro quinolinic acid, cyhalofop-butyl and penoxsuam compound herbicide for one kind, it is characterized in that, comprise raw and auxiliary material suction preparation still mixing and stirring, just grind through colloid mill, then through sand mill fine grinding, filter, and control suspensibility >=90%, 75 μm of testing sieve percent of pass >=98%, after sample analysis is qualified, metering, packaging, warehouse-in.
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Cited By (1)
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