CN105145591A - Compound suspension concentrate containing pretilachlor, clomazone and oxadiargyl and preparation method and application of compound suspension concentrate - Google Patents
Compound suspension concentrate containing pretilachlor, clomazone and oxadiargyl and preparation method and application of compound suspension concentrate Download PDFInfo
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Abstract
The invention discloses compound suspension concentrate containing pretilachlor, clomazone and oxadiargyl and a preparation method and application of the compound suspension concentrate. The compound suspension concentrate, 100% in total, is prepared from 15-60% of pretilachlor, 5-25% of clomazone, 5-20% of oxadiargyl, 1-15% of emulsifying agent, 0.1-6% of dispersing agent, 0-10 % of thickening agent, 1-10% of antifreezing agent, 0.1-2% of defoaming agent, 0.1-3% of preservative and the balance water. All the components have different effects and characteristics and are suitable for a paddy field at the same time after being compounded, weeds can not easily have resistance to drug, the components can be complementary in advantage, the weed killing range is enlarged, paddy is safe, no side effects exist, high safety is achieved for afterreap crops, acting sites are increased, the drug resistance of weeds can be easily overcome and delayed, and an important means for comprehensively preventing and treating weeds in field is achieved. The prepared suspension concentrate is constant in pH value and viscosity, and the grain size is not prone to increase. The suspension concentrate is high in soil affinity, the pesticide effect is improved, field consumption is lowered, production and use cost is reduced, and pesticide residuals and environment pollution are reduced.
Description
Technical field
The present invention relates to a kind of farm weeding preparation, in particular a kind of contain the third careless amine, clomazone and oxadiargyl composite suspoemulsion, preparation method and application.
Background technology
Aqueous suspension emulsion is one or more water-insoluble agricultural chemicals liquid actives (or low melting point pesticide activity component mixture in a solvent) and another kind of or several water-insoluble pesticidal solid active component, take water as medium, rely on surfactant to be processed into a kind of liquid preparation of stable outstanding newborn dispersion.It has the advantage of suspending agent and aqueous emulsion, and as avoided emulsifiable concentrates for agricultural chemicals and wettable powder because organic solvent and dust are to the pollution of environment and operator and murder by poisoning, storing safety, has higher biologically active etc.Because aqueous suspension emulsion is a three-phase mixture, and there is dynamics and thermodynamic phase simultaneously, therefore easily occur the problems such as pH value or viscosity can not keep constant, particle diameter increase.Hang at known water in addition in some surfactants used in emulsion, such as alkylphenol polyoxyethylene, it is not entirely satisfactory in ecology and toxicity, therefore needs substitute.Suspended emulsion good stability provided by the invention, mixed surfactant used is environmental protection and safety.
Third careless amine is selectivity preemergence herbicide, cell division inhibitor.Weeds absorb medicament by middle hypocotyl and coleoptile, and interferencing protein synthesizes, and also have remote-effects to the photosynthesis of weeds and respiration.Generally by soil treatment, prevent and kill off the weeds such as paddy field barnyard grass, duck leaf grass, difformed galingale herb, Brittle Falsepimpernel Herb, needle spikesedge herb, kind algae, firefly Lin, poor to perennial weed preventive effect.
Clomazone is Yi Zhong oxazole class selectivity preemergence herbicide, also after can doing bud, weedicide uses, absorbed by root, bud, affect carotin and chlorophyllous biosynthesis, thus cause plant dead by suppressing photosynthesis of plant, be mainly used in preventing and kill off annual gramineous weed and part broad leaved weed, Soybean Field and south rice field have broad application prospects northeastward.
Oxadiargyl system proporphyrinogen oxidase inhibitor is before a kind of diazolones seedling and early stage herbicide after seedling.Young shoot before and after mainly being emerged by some susceptible weeds is contacted with seedling and absorbs and work, and is a kind of contact killing type weed killer herbicide, mainly absorbs in the contact of weeds germination and emergence and works.Be mainly used in paddy field weed-killer, also effective to the peanut, cotton, sugarcane etc. of dry land; Barnyard grass, moleplant seed, ditch millet, difformed galingale herb, Monochoria vaginalis, mexicana, globe daisy alkali grass, Sagittaria pygmaea etc. are prevented and kill off for rice field.Also can be used for preventing and kill off crop annual gramineous weed and the broad leaved weeds such as cotton, soybean, sunflower, peanut, potato, sugarcane, celery, fruit tree.To looking for section, Li Ke, Euphorbiaceae, Zui Jiangcao section, optically-active section weeds have good preventive effect.
On Agriculture Field control of weeds, often there is defect in various degree in the weed killer herbicide kind containing single-activity component, as weeds after continuous administration easily develop immunity to drugs, herbicide spectrum is narrow, using repeatedly can weighting ring environment pollution, and residue of pesticide extend.Different cultivars composition carries out composite, is the modal method of control Herbicide-resistant weeds.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of contain the third careless amine, clomazone and oxadiargyl composite suspoemulsion, preparation method and application, open up the novel form of herbicide for paddy field application.
The present invention is achieved by the following technical solutions: the present invention by weight, comprise following component, third careless amine 15 ~ 60%, clomazone 5 ~ 25%, oxadiargyl 5 ~ 20%, emulsifier 1 ~ 15%, dispersant 0.1 ~ 6%, thickener 0 ~ 10%, antifreezing agent 1 ~ 10%, defoamer 0.1 ~ 2%, preservative 0.1 ~ 3%, water complements to 100%.
Described emulsifier be selected from AEO series fatty alcohol-polyoxyethylene ether, alkylphenol-polyethenoxy polyethers and sulphate thereof or phosphate, NP series polyoxyethylene nonylphenol ether, thermally coupled distillation columns, phenethyl phenol polyoxyethylene phosphonate, aliphatic alcohol polyoxyvinethene phosphate, styryl phenol polyethenoxy polyethenoxy ether, this dish SPAN, soil temperature TWEEN in one or more.
Described dispersant be selected from lignosulfonates, alkylaryl sulfonate, alkylsulfonate naphthalenesulfonate formaldehyde condensation compound, phosphate ester salt, polycarboxylate, macromolecule EO-PO block polyether, BY series castor oil polyoxyethylene ether in one or more.
Described thickener be selected from sodium cellulose glycolate, polyvinyl alcohol, aluminium-magnesium silicate, white carbon, xanthans, bentonite one or more.
Described antifreezing agent be selected from ethylene glycol, urea, propane diols, glycerine, sodium chloride one or more.
Described defoamer is selected from C
8-C
10one or more in fatty alcohol, silicone based, ester-ether type compound.
Described preservative be selected from Sodium Benzoate, Kathon CG, methenamine, formaldehyde one or more.
Contain a preparation method for the composite suspoemulsion of the third careless amine, clomazone and oxadiargyl, comprise the following steps:
(1) Bing Que Evil humulone suspending agent is prepared
(11) first shear in oxadiargyl, suspension aid, surfactant, preservative, antifreezing agent and water input reactor;
(12) the material grinding will sheared again, grinding limit, limit adds and has weighed defoamer;
(13) finally add load weighted thickener, continue to shear;
(2) the third careless amine, clomazone oil phase is prepared;
First add the third careless amine, clomazone, then add emulsifier and mix, obtained mixing oil phase;
(3) the third careless amine, clomazone and oxadiargyl suspoemulsion is prepared;
Bing Que Evil humulone suspending agent obtained to oil phase obtained for step (2), step (1), water are added to shear in still successively and is uniformly dispersed, shear the suspension emulsion that obtained average grain diameter is less than 3 microns.
Described shear time 5 ~ 10 minutes, rotating speed is 2950rmp.
A kind of application of composite suspoemulsion as herbicide for paddy field containing the third careless amine, clomazone and oxadiargyl.
The present invention has the following advantages compared to existing technology: each component action character of the present invention is different, compositely be applicable to paddy field afterwards simultaneously, weeds are not easy to develop immunity to drugs, and can have complementary advantages, and expand herbicide scope, to rice safety, have no side effect, good to succession crop safety, action site increases, being conducive to the generation overcoming and delay herbicide resistance, is the important means of integrated control weeds in field.The present invention is environmentally-friendly water-based agent type, has and produces storage and the advantage such as use safety, environmental pollution is little, product cost is low, easy packaging, not easily occur the problems such as pH value or viscosity can not keep constant, particle diameter increase.The affinity of the present invention and soil is strong, and drug effect improves, and field rate declines, and reduces production and use cost, reduces residue of pesticide and environmental pollution.
Embodiment
Elaborate to embodiments of the invention below, the present embodiment is implemented under premised on technical solution of the present invention, give detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
32% the third careless amine, clomazone and oxadiargyl suspoemulsions
(1) 30% Bing Que Evil humulone SC is prepared
Component | Percentage by weight |
Oxadiargyl | 30.0% |
Fatty alcohol-polyoxyethylene ether | 7.0% |
Lignosulfonates | 4.0% |
Ethylene glycol | 6.0% |
White carbon | 4.0% |
Organic silicone defoamer | 0.5% |
Formaldehyde | 1.0% |
Water | Complementary |
According to above-mentioned given formula, first former for oxadiargyl medicine, emulsifier fatty alcohol-polyoxyethylene ether, dispersant lignosulfonates, preservative formaldehyde, antifreeze glycol and water are dropped in reactor and shear; The material grinding will sheared again, grinding limit, limit adds and has weighed organic silicone defoamer; Finally add load weighted thickener white carbon, continue to shear.
(2) the third careless amine, clomazone oil phase is prepared
Component | Percentage by weight |
Third careless amine | 64.3% |
Clomazone | 25.7% |
Phenethyl phenol polyoxyethylene phosphonate | 10.0% |
According to above-mentioned given formula, first add the third careless amine, clomazone, then add emulsifier phenethyl phenol polyoxyethylene phosphonate, be uniformly mixed formation oil phase.
(3) the 32% the third careless amine, clomazone and oxadiargyl SE are prepared
Component | Percentage by weight |
30% Bing Que Evil humulone SC | 13.3% |
Third careless amine, clomazone oil phase | 31.1% |
Water | Complementary |
Under high shear, 30% Bing Que Evil humulone SC is added to by a certain percentage in the 90% the third careless amine, clomazone emulsion, add the water of surplus again, carry out high shear, shear time 5-10 minute (rotating speed is 2950rmp), control average grain diameter and be less than 3 microns, obtain the 32% the third careless amine, clomazone and oxadiargyl SE.
Embodiment 2
33% the third careless amine, clomazone and oxadiargyl suspoemulsions
(1) 30% Bing Que Evil humulone SC is prepared
Component | Percentage by weight |
Oxadiargyl | 30.0% |
Styrylphenol polyoxyethylene ether phosphate | 6.0% |
Polycarboxylate | 3.0% |
Aluminium-magnesium silicate | 5.0% |
Propane diols | 6.0% |
Organic silicone defoamer | 0.5% |
Methenamine | 0.8% |
Water | Complementary |
Preparation method is identical with embodiment 1.
(2) the third careless amine, clomazone oil phase is prepared
Component | Percentage by weight |
Third careless amine | 62.1% |
Clomazone | 27.9% |
Alkylphenol-polyethenoxy polyethers | 10.0% |
Preparation method is identical with embodiment 1.
(3) the 33% the third careless amine, clomazone and oxadiargyl SE are prepared
Component | Percentage by weight |
30% Bing Que Evil humulone SC | 13.3% |
Third careless amine, clomazone oil phase | 32.2% |
Water | Complementary |
Preparation method is identical with embodiment 1.
Embodiment 3
34% the third careless amine, clomazone and oxadiargyl suspoemulsions
(1) 30% Bing Que Evil humulone SC is prepared
Component | Percentage by weight |
Oxadiargyl | 30.0% |
Soil temperature TWEEN | 7.0% |
Lignosulfonates | 4.5% |
Bentonite | 5.0% |
Glycerine | 6.0% |
Organic silicone defoamer | 0.6% |
Kathon CG | 0.5% |
Water | Complementary |
Preparation method is identical with embodiment 1.
(2) the third careless amine, clomazone oil phase is prepared
Component | Percentage by weight |
Third careless amine | 64.3% |
Clomazone | 25.7% |
Thermally coupled distillation columns | 10.0% |
Preparation method is identical with embodiment 1.
(3) the 34% the third careless amine, clomazone and oxadiargyl SE are prepared
Component | Percentage by weight |
30% Bing Que Evil humulone SC | 20.0% |
Third careless amine, clomazone oil phase | 31.1% |
Water | Complementary |
Preparation method is identical with embodiment 1.
Embodiment 4
48% the third careless amine, clomazone and oxadiargyl suspoemulsions
(1) 30% Bing Que Evil humulone SC is prepared
Component | Percentage by weight |
Oxadiargyl | 30.0% |
Aliphatic alcohol polyoxyvinethene phosphate | 4.0% |
Fatty alcohol-polyoxyethylene ether | 3.0% |
Alkylaryl sulfonate | 4.0% |
Xanthans | 4.0% |
Ethylene glycol | 4.0% |
Organic silicone defoamer | 0.6% |
Kathon CG | 0.4% |
Water | Complementary |
Preparation method is identical with embodiment 1.
(2) the third careless amine, clomazone oil phase is prepared
Component | Percentage by weight |
Third careless amine | 64.3% |
Clomazone | 25.7% |
Soil temperature TWEEN | 10.0% |
Preparation method is identical with embodiment 1.
(3) the 48% the third careless amine, clomazone and oxadiargyl SE are prepared
Component | Percentage by weight |
30% Bing Que Evil humulone SC | 20.0% |
90% the third careless amine, clomazone oil phases 90 | 46.7% |
Water | Complementary |
Preparation method is identical with embodiment 1.
Embodiment 5
45% the third careless amine, clomazone and oxadiargyl suspoemulsions
(1) 30% Bing Que Evil humulone SC is prepared
Component | Percentage by weight |
Oxadiargyl | 30.0% |
Aliphatic alcohol polyoxyvinethene phosphate | 7.0% |
BY series castor oil polyoxyethylene ether | 4.0% |
Sodium cellulose glycolate | 4.0% |
Propane diols | 5.0% |
Organic silicone defoamer | 0.6% |
Formaldehyde | 0.5% |
Water | Complementary |
Preparation method is identical with embodiment 1.
(2) the third careless amine, clomazone oil phase is prepared
Component | Percentage by weight |
Third careless amine | 69.2% |
Clomazone | 20.8% |
NP series polyoxyethylene nonylphenol ether | 10.0% |
Preparation method is identical with embodiment 1.
(3) the 45% the third careless amine, clomazone and oxadiargyl SE are prepared
Component | Percentage by weight |
30% Bing Que Evil humulone SC | 20.0% |
Third careless amine, clomazone oil phase | 43.3% |
Water | Complementary |
Preparation method is identical with embodiment 1.
One, testing result
Prepared by embodiment 1 ~ 5 third careless amine, clomazone and oxadiargyl suspoemulsion, the testing result of product all technical is as shown in table 1.
The testing result of table 1 embodiment 1 ~ 5 preparing product all technical
Two, Toxicity Determination
In order to effective water prevention rice field transplant field annual weed, select the third careless amine, clomazone and oxadiargyl compatibility, with paddy field transplant field annual weed for object, adopt spray-on process, both mensuration different ratio, to the indoor virulence of target weeds, screens optimum proportioning.
1, test
1.1 experiment targets
Barnyard grass, Monochoria vaginalis, cyperus iria, different in nature nutgrass flatsedge.Test seed collection is in great Yang town, Hefei City, Anhui Province.
1.2 experimental instrument
Potter spray tower (BURCARD automatic type), electronic balance (sensibility reciprocal 0.1mg), artificial incubator (MGC-300H), Ф 15cm basin alms bowl, pipette, beaker, volumetric flask, writing brush, tweezers, scissors, glass bar, filter paper etc.
1.3 condition of culture
Test soil organic matter content is, PH6.9, the air-dry soil 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, and sowing date is on March 4th, 2015.
1.4 test medicine
The former medicine of third careless amine, content: 97% (Anhui Kelihua Chemical Co., Ltd. provides);
The former medicine of clomazone, content: 95% (Anhui Kelihua Chemical Co., Ltd.'s outsourcing);
The former medicine of Bing Que Evil humulone, content: 96% (Anhui Kelihua Chemical Co., Ltd. provides);
1.5 medicament preparations
Above-mentioned single dose and mixture, respectively with the mother liquor preparing high concentration after acetone solution, on the basis of preliminary experiment, are diluted to series mass concentration (see table 2) with the 0.1% Tween 80 aqueous solution by the third careless amine, clomazone and the former medicine of Bing Que Evil humulone.
2, test process
Cauline leaf spray-on process is adopted to measure the third careless amine, clomazone and oxadiargyl single dose and the composite virulence to barnyard grass, Monochoria vaginalis, broken leaf nutgrass flatsedge, 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.Evenly sow pretreated in soil surface for examination weed seed, 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% Tween 80 aqueous solution not containing medicament not make blank.Within after medicine 2 days, add water and make to keep water layer 2 ~ 3cm in alms bowl, process is raised and is observed under being placed on temperature (26 ± 0.5) DEG C, relative moisture (75 ± 5) %, photoperiod L:D=(14:10) h.
3, investigate: process investigation in latter 21 days once, adopt absolute value investigation method record weeds fresh weight.
4, computational methods
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.
5, statistical analysis
Adopt Cloby method to mixed E
0=XYZ/100
2, after herbicidal activity test, formula is 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 Cloby method, work as E
0-e > 10% is synergistic effect; Work as E
0-e <-10% is synergistic effect; Work as E
0-e ± 10% is synergistic effect.
6, discussion is analyzed
6.1 third careless amine, clomazones and each single dose of oxadiargyl and mixed different ratio thereof to the activity of weeding of barnyard grass, Monochoria vaginalis, broken leaf nutgrass flatsedge and difformed galingale herb in table 2.
The activity of weeding of table 2 third careless amine, clomazone and the mixed different ratio of Bing Que Evil humulone
The co-toxicity effect of 6.2 different ratio
Colby method is adopted to judge that the third careless amine, clomazone different ratio mixed with oxadiargyl is to providing the co-toxicity effect of weeds (see showing 3-table 6)
Table 3 third careless amine, clomazone and Bing Que Evil humulone different ratio are to the co-toxicity effect of barnyard grass
Table 4 third careless amine, clomazone and Bing Que Evil humulone different ratio are to the co-toxicity effect of Monochoria vaginalis
Table 5 third careless amine, clomazone and Bing Que Evil humulone different ratio are to the co-toxicity effect of cyperus iria
Table 6 third careless amine, clomazone and Bing Que Evil humulone different ratio are to the co-toxicity effect of difformed galingale herb
6.3 interpretations of result and discussion
Third careless amine, clomazone and oxadiargyl 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.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. the composite suspoemulsion containing the third careless amine, clomazone and oxadiargyl, it is characterized in that, by weight, comprise following component, third careless amine 15 ~ 60%, clomazone 5 ~ 25%, oxadiargyl 5 ~ 20%, emulsifier 1 ~ 15%, dispersant 0.1 ~ 6%, thickener 0 ~ 10%, antifreezing agent 1 ~ 10%, defoamer 0.1 ~ 2%, preservative 0.1 ~ 3%, water complements to 100%.
2. a kind of composite suspoemulsion containing the third careless amine, clomazone and oxadiargyl according to claim 1, it is characterized in that, described emulsifier be selected from AEO series fatty alcohol-polyoxyethylene ether, alkylphenol-polyethenoxy polyethers and sulphate thereof or phosphate, NP series polyoxyethylene nonylphenol ether, thermally coupled distillation columns, phenethyl phenol polyoxyethylene phosphonate, aliphatic alcohol polyoxyvinethene phosphate, styryl phenol polyethenoxy polyethenoxy ether, this dish SPAN, soil temperature TWEEN in one or more.
3. a kind of composite suspoemulsion containing the third careless amine, clomazone and oxadiargyl according to claim 1, it is characterized in that, described dispersant be selected from lignosulfonates, alkylaryl sulfonate, alkylsulfonate naphthalenesulfonate formaldehyde condensation compound, phosphate ester salt, polycarboxylate, macromolecule EO-PO block polyether, BY series castor oil polyoxyethylene ether in one or more.
4. a kind of composite suspoemulsion containing the third careless amine, clomazone and oxadiargyl according to claim 1, it is characterized in that, described thickener be selected from sodium cellulose glycolate, polyvinyl alcohol, aluminium-magnesium silicate, white carbon, xanthans, bentonite one or more.
5. a kind of composite suspoemulsion containing the third careless amine, clomazone and oxadiargyl according to claim 1, is characterized in that, described antifreezing agent be selected from ethylene glycol, urea, propane diols, glycerine, sodium chloride one or more.
6. a kind of composite suspoemulsion containing the third careless amine, clomazone and oxadiargyl according to claim 1, it is characterized in that, described defoamer is selected from C
8-C
10one or more in fatty alcohol, silicone based, ester-ether type compound.
7. a kind of composite suspoemulsion containing the third careless amine, clomazone and oxadiargyl according to claim 1, is characterized in that, described preservative be selected from Sodium Benzoate, Kathon CG, methenamine, formaldehyde one or more.
8. a kind of preparation method containing the composite suspoemulsion of the third careless amine, clomazone and oxadiargyl as described in claim 1 ~ 7, is characterized in that, comprise the following steps:
(1) Bing Que Evil humulone suspending agent is prepared
(11) first shear in oxadiargyl, suspension aid, surfactant, preservative, antifreezing agent and water input reactor;
(12) the material grinding will sheared again, grinding limit, limit adds and has weighed defoamer;
(13) finally add load weighted thickener, continue to shear;
(2) prepare the third careless amine, clomazone oil phase first adds the third careless amine, clomazone, then add emulsifier and mix, obtained mixing oil phase;
(3) the third careless amine, clomazone and oxadiargyl suspoemulsion is prepared
Bing Que Evil humulone suspending agent obtained to oil phase obtained for step (2), step (1), water are added to shear in still successively and is uniformly dispersed, shear the suspension emulsion that obtained average grain diameter is less than 3 microns.
9. a kind of preparation method containing the composite suspoemulsion of the third careless amine, clomazone and oxadiargyl according to claim 8, it is characterized in that, described shear time 5 ~ 10 minutes, rotating speed is 2950rmp.
10. a kind of application of composite suspoemulsion as herbicide for paddy field containing the third careless amine, clomazone and oxadiargyl as described in claim 1 ~ 7.
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CN113796376A (en) * | 2020-06-12 | 2021-12-17 | 沈阳中化农药化工研发有限公司 | Application of oleic alcohol ester surfactant |
WO2024150044A1 (en) * | 2023-01-12 | 2024-07-18 | Parijat Industries (India) Private Limited | An improved herbicide formulation and method of manufacturing the same |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN113796376A (en) * | 2020-06-12 | 2021-12-17 | 沈阳中化农药化工研发有限公司 | Application of oleic alcohol ester surfactant |
WO2024150044A1 (en) * | 2023-01-12 | 2024-07-18 | Parijat Industries (India) Private Limited | An improved herbicide formulation and method of manufacturing the same |
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Application publication date: 20151216 |