CN105475273A - Compound missible oil containing oxadiargyl, oxyfluorfen and pretilachlor and preparation method thereof - Google Patents

Compound missible oil containing oxadiargyl, oxyfluorfen and pretilachlor and preparation method thereof Download PDF

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Publication number
CN105475273A
CN105475273A CN201510997698.3A CN201510997698A CN105475273A CN 105475273 A CN105475273 A CN 105475273A CN 201510997698 A CN201510997698 A CN 201510997698A CN 105475273 A CN105475273 A CN 105475273A
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China
Prior art keywords
oxyfluorfen
parts
pretilachlor
oxadiargyl
evil humulone
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Pending
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CN201510997698.3A
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Chinese (zh)
Inventor
毛堂富
徐长才
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ANHUI MEILAND AGRICULTURAL DEVELOPMENT Co Ltd
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ANHUI MEILAND AGRICULTURAL DEVELOPMENT Co Ltd
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Priority to CN201510997698.3A priority Critical patent/CN105475273A/en
Publication of CN105475273A publication Critical patent/CN105475273A/en
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N33/00Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
    • A01N33/16Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
    • A01N33/18Nitro compounds
    • A01N33/20Nitro compounds containing oxygen or sulfur attached to the carbon skeleton containing the nitro group
    • A01N33/22Nitro compounds containing oxygen or sulfur attached to the carbon skeleton containing the nitro group having at least one oxygen or sulfur atom and at least one nitro group directly attached to the same aromatic ring system
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/18Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
    • A01N37/26Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof containing the group; Thio analogues thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72Biocides, 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
    • A01N43/82Biocides, 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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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention relates to compound missible oil containing oxadiargyl, oxyfluorfen and pretilachlor and a preparation method thereof and relates to the technical field of prevention and treatment of weeds of paddy fields. The compound missible oil is prepared from 3 parts of oxadiargyl, 16 parts of oxyfluorfen, 20 parts of pretilachlor, 6 parts of tristyrylphenol ethoxylates, 3 parts of ethoxylated distyrylphenol formaldehyde condensate, 9 parts of calcium dodecyl benzene sulfonate and 43 parts of xylene. The preparation method comprises the following steps: adding oxadiargyl, oxyfluorfen and pretilachlor to xylene and stirring until all the components are dissolved; then adding the residual raw materials, and stirring and mixing uniformly with a reaction kettle; sampling and analyzing the content; after the raw materials are qualified, standing, filtering, packaging, and sampling and analyzing the content again; and storing after the product is qualified. The compounded compound missible oil containing oxadiargyl, oxyfluorfen and pretilachlor, with the concentration of 39%, is used by mixing oxadiargyl, oxyfluorfen and pretilachlor at the ratio of 3 to 16 to 20, and has an obvious synergistic effect range; and preparations, which are mixed at other ratios, cannot reach the obvious synergistic effect range.

Description

A kind of Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream and preparation method thereof
Technical field
The present invention relates to rice field weed control technical field, specifically relate to a kind of Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream and preparation method thereof.
Background technology
At present, the existing Herbicidal combinations for rice field weed control, such as Chinese patent " CN104823987A " discloses one " containing triazole acyl grass amine and the Herbicidal combinations of Bing Que Evil humulone ", wherein effective active composition is triazole acyl grass amine and Bing Que Evil humulone, and both proportionings are 10:1 ~ 1:10.Separately have Chinese patent " CN103975934A " to disclose one " Herbicidal combinations containing Bing Que Evil humulone ", wherein effective active composition is Bing Que Evil humulone, the third careless amine and penoxsuam, and the proportioning of three is 1 ~ 50:1 ~ 80:1 ~ 40.
Inventor verifies through long term test, and this above-mentioned several Herbicidal combinations mainly exists following defect:
1), by several concrete proportioning disclosed in above-mentioned several Herbicidal combinations test, find cannot play good control efficiency to paddy field barnyard grass, Monochoria vaginalis, mexicana and difformed galingale herb.
2), for several formulations disclosed in above-mentioned several Herbicidal combinations, find through verification experimental verification the defect that all there is different problem.Such as, the wetting powder made easily causes product to bond, not easily dispersion suspension in water, or blocking shower nozzle, the phenomenon such as reason precipitation in sprayer, cause spray irregular, easily make crop local produce poisoning, its main cause is that the selection of auxiliary agent and filler all exists different defects.
3), composite problem, by several concrete proportioning disclosed in above-mentioned several Herbicidal combinations carry out virulence test, heat storage stability test and co-toxicity coefficient measure find, all cannot reach obvious synergistic effect.
Summary of the invention
An object of the present invention is to provide a kind of Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream, this missible oil is reasonable in design, good to the control efficiency of paddy field barnyard grass, Monochoria vaginalis, mexicana and difformed galingale herb, and the notable synergistic effect of Bing Que Evil humulone, Oxyfluorfen and the third careless amine can be realized.
For achieving the above object, present invention employs following technical scheme:
A kind of Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream, be made up of the component of following weight portion:
Third alkynes Evil humulone is a kind of novel oxadiazole nitrogen-containing hetero lopps weed killer herbicide, broad leaved weed is prevented and kill off before being mainly used in the seedlings such as paddy rice, potato, sunflower, vegetables, beet, orchard, the weeds such as mexicana, duckweed, the water silk floss of algae, little najas marina in annual and perennial barnyard grass gramineous, the difformed galingale herb of sedge family, needle spikesedge herb, broadleaved herb can also be prevented and kill off, in addition also can kill and wound and suppress firefly Lin, convexutricle sedge herb, Monochoria korsakowii, rhizoma alismatis, arrowhead and pondweed etc.This kind is used for agent for removing grass in paddy field, residually in paddy rice lowly ensures that China's rice outlet residue of pesticide do not exceed standard, and improves China's rice competitive advantage in world markets.So the exploitation of oxadiargyl will produce great economic benefit and social benefit.
Oxyfluorfen is contact killing type weed killer herbicide, plays herbicide effect when there being light.Enter in plant corpus mainly through coleoptile, mesocotyl, less through root absorption, and have denier upwards to be transported by root to enter leaf portion.Before bud and after bud, application effect is best in early days, comparatively wide to the weeds herbicidal spectrum of seed germination, can prevent and kill off broad leaved weed, nutgrass flatsedge and barnyard grass, but only have inhibitory action to perennial weed.In paddy field, apply after in water layer in 24 hours, be deposited in soil table, water-soluble extremely low, mobility is less, is adsorbed in very soon in 0 ~ 3 centimetre of topsoil, not easily moves vertically downward after dispenser, become carbonic acid gas by the microbial decomposition in soil in three weeks, in soil, the half life period is about 30 days.
Third careless amine is that selectivity sprouts pretreating reagent, and by plant hypocotyl, mesocotyl and coleoptile absorb, and root slightly absorbs, and direct interference weeds body internal protein synthesizes, and has remote-effects to photosynthetic and respiration.Be injured the distortion of weeds seedling, primary leaf difficulty is stretched out, and leaf look deepens green, and growth stops, until dead.Paddy rice has stronger capacity of decomposition to the third careless amine, thus has certain selectivity.
Bing Que Evil humulone of the present invention, Oxyfluorfen and the third careless amine compounded cream, its beneficial effect shows:
1) missible oil that, prepared by the present invention is all obviously better than the product prepared by other proportionings in stability of emulsion, low-temperature stability and heat storage stability etc.
2), verify by experiment Bing Que Evil humulone, Oxyfluorfen and the third careless amine with 3:16:20 proportioning mixed composite 39% time Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream, notable synergistic sphere of action can be played, and the preparation that other proportioning is mixed, all cannot reach notable synergistic sphere of action.Meanwhile, the actual toxicity of different ratio does not promote along with the enhancing of theoretical toxicity, there is no regular change between actual toxicity and theoretical toxicity.
Another object of the present invention is to the preparation method that a kind of Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream are provided, Bing Que Evil humulone, Oxyfluorfen and the third careless amine are added in dimethylbenzene to stir and treat whole dissolving, then add tristyrylphenol polyoxyethylene ether, diphenylethyllene phenol formaldehyde condensation products APEO and calcium dodecyl benzene sulfonate and be uniformly mixed by reactor, sample analysis content, qualifiedly to leave standstill afterwards, filter, packaging, sample analysis content again, warehousing after passing.
The preparation method of Bing Que Evil humulone of the present invention, Oxyfluorfen and the third careless amine compounded cream, preparation technology is comparatively easy, is easy to suitability for industrialized production.
Embodiment
Below with reference to embodiment, the present invention is described in detail.But; embodiment content is only citing made for the present invention and explanation; affiliated those skilled in the art make various amendment to described specific embodiment or supplement or adopt similar mode to substitute; only otherwise depart from the design of invention or surmount this scope as defined in the claims, protection scope of the present invention all should be belonged to.
One, the preparation of Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream, and testing result, the heat storage stability result of the test of all technical of missible oil prepared by each embodiment.
Embodiment 1
39% Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream, each component and weight portion as follows:
Composition Weight portion
Bing Que Evil humulone 3
Oxyfluorfen 16
Third careless amine 20
Tristyrylphenol polyoxyethylene ether 6
Diphenylethyllene phenol formaldehyde condensation products APEO 3
Calcium dodecyl benzene sulfonate 9
Dimethylbenzene 43
Preparation method: Bing Que Evil humulone, Oxyfluorfen and the third careless amine are added in dimethylbenzene to stir and treat whole dissolving, then add tristyrylphenol polyoxyethylene ether, diphenylethyllene phenol formaldehyde condensation products APEO and calcium dodecyl benzene sulfonate and be uniformly mixed by reactor, sample analysis content, qualifiedly to leave standstill afterwards, filter, packaging, sample analysis content again, warehousing after passing.
Embodiment 2
39.5% Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream, each component and weight portion as follows:
Preparation method is with embodiment 1.
Embodiment 3
38.5% Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream, each component and weight portion as follows:
Composition Weight portion
Bing Que Evil humulone 2.5
Oxyfluorfen 16
Third careless amine 20
Tristyrylphenol polyoxyethylene ether 6
Diphenylethyllene phenol formaldehyde condensation products APEO 3 3 -->
Calcium dodecyl benzene sulfonate 9
Dimethylbenzene 43.5
Preparation method is with embodiment 1.
Embodiment 4
38% Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream, each component and weight portion as follows:
Composition Weight portion
Bing Que Evil humulone 3
Oxyfluorfen 15.5
Third careless amine 19.5
Tristyrylphenol polyoxyethylene ether 6
Diphenylethyllene phenol formaldehyde condensation products APEO 3
Calcium dodecyl benzene sulfonate 9
Dimethylbenzene 44
Preparation method is with embodiment 1.
Embodiment 5
40% Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream, each component and weight portion as follows:
Preparation method is with embodiment 1.
Bing Que Evil humulone prepared by embodiment 1 ~ 5, Oxyfluorfen and the third careless amine compounded cream, the testing result of product all technical is as shown in table 1, and product heat storage stability result of the test is as shown in table 2.
The testing result of a table 15 embodiment preparing product all technical
A table 25 embodiment preparing product heat storage stability result of the test
Can be found out by table 1 and 2, product prepared by embodiment 1 is all obviously better than the product prepared by other proportionings in stability of emulsion, low-temperature stability and heat storage stability etc.
Two, toxicological information
Bing Que Evil humulone: rat acute per os LD 50> 5000mg/kg, rat acute is through skin LD 50> 2000mg/kg, rat acute sucks LC 50(4h) > 5.16mg/L, non-stimulated to family's skin, there is minimal irritation to rabbit eyes, guinea pig skin is stimulated without sensitization, belong to lower toxicity.
Oxyfluorfen: rat acute per os LD 50> 5000mg/kg, rabbit is acute through skin LD 50> 10000mg/kg.
Third careless amine: rat acute per os LD 50for 6099mg/kg, rat acute is through skin LD 50> 3100mg/kg.
Three, the indoor biological activity (virulence) of Bing Que Evil humulone, Oxyfluorfen and the third careless amine compounded cream measures.
1 test objective
Pot experiment method method is adopted to determine Bing Que Evil humulone, Oxyfluorfen and the third careless amine biologically active to barnyard grass, Monochoria vaginalis, mexicana and difformed galingale herb, and adopt the synergy type of Cobly method evaluation three mixture, for rationally mixed and in producing the proportioning of three is selected to provide scientific basis.
2 experimental conditions
2.1 for examination material
Barnyard grass [Echinochloacrusgalli (L.) Beauv.]: Seed storage is collected in field, Anhui Meilan Agricultural Development Co., Ltd. laboratory;
Monochoria vaginalis [Monochoriavaginalis (Burm.f.) PreslexKunth]: Seed storage is collected in field, Anhui Meilan Agricultural Development Co., Ltd. laboratory;
Mexicana [Rotalaindica (Willd.) Koehne]: Seed storage is collected in field, Anhui Meilan Agricultural Development Co., Ltd. laboratory;
Difformed galingale herb [cyperusdifformisl.]: Seed storage is collected in field, Anhui Meilan Agricultural Development Co., Ltd. laboratory.
2.2 test medicine
96% Bing Que Evil humulone (Oxadiargyl) former medicine, Anhui Meilan Agricultural Development Co., Ltd. provides;
95% Oxyfluorfen (oxyfluorfen) former medicine, Anhui Meilan Agricultural Development Co., Ltd. provides;
97% the third careless amine (pretilachlor) former medicines, Anhui Meilan Agricultural Development Co., Ltd. provides.
2.3 test proportioning process
Design according to embodiment 1-5 proportioning.
2.4 processing mode
2.4.1 medicament is to the activity test of barnyard grass
After barnyard grass seed presoaking and germinating, point is sowed at the sectional area 0.25m that earth is housed 2basin in, every basin broadcasts 100, is cultured to barnyard grass 1 leaf 1 heart stage to process in greenhouse.Spray liquid with the accurate laboratory spray tower of POTTER, spouting liquid, for often to process 50ml, keeps ground moistening after medicine, and establishes clear water blank.Often process repetition 4 times, within after medicine 20 days, take each process barnyard grass acrial part fresh weight, the inhibition percentage and the remaining barnyard grass that calculate each process aerial growth are the percentage contrasted, and use the synergy type to barnyard grass with Gobly method evaluation three.The actual preventive effect of mixe herbicide calculates as follows:
E 0=A × B × C × ... N/100 (N-1)(this test is ternary built, therefore E 0=A × B × C/10000)
In formula: A is the Weed-control effect of weed killer herbicide 1;
B is the Weed-control effect of weed killer herbicide 2;
C is the Weed-control effect of weed killer herbicide 3;
N is mixed weed killer herbicide kind quantity;
E 0for the Weed-control effect+weed killer herbicide n Weed-control effect of the Weed-control effect+weed killer herbicide 3 of the Weed-control effect+weed killer herbicide 2 of weed killer herbicide 1;
E 1for the actual preventive effect of mixe herbicide, E is observation (100-E 1).
E-E 0>10% is synergistic effect; E-E0<-10% is antagonism; E-E0 value between theoretical value ± 10% be addition.
2.4.2 medicament is to the activity test of Monochoria vaginalis
After Monochoria vaginalis seed-soaking, after vernalization, point is sowed at the sectional area 0.25m that earth is housed 2basin in, all the other same 2.4.1.
2.4.3 medicament is to the activity test of mexicana
After mexicana seed-soaking, after vernalization, point is sowed at the sectional area 0.25m that earth is housed 2basin in, all the other same 2.4.1.
2.4.4 medicament is to the activity test of difformed galingale herb
After difformed galingale herb seed-soaking, after vernalization, point is sowed at the sectional area 0.25m that earth is housed 2basin in, all the other same 2.4.1.
3 interpretations of result and discussion
The mixture of embodiment 1-5 totally 5 different compound proportions is to the E-E of barnyard grass 0value is followed successively by 22.25%, and 2.81%, 3.66%, 2.51%, 1.85%; To the E-E of Monochoria vaginalis 0value is respectively 21.38%, and 2.52%, 3.26%, 2.74%, 1.75%; To the E-E of mexicana 0value is respectively 21.27%, and 2.75%, 3.58%, 2.36%, 1.55%; To the E-E of difformed galingale herb 0value is respectively 23.65%, 4.07%, 5.12%, 4.73%, 3.79%, thus the synergy describing the compound proportion of embodiment 1 belongs to obvious addition synergistic effect, and the synergy of other embodiments belongs to addition substantially.

Claims (2)

1. the third alkynes Evil humulone, Oxyfluorfen and a third careless amine compounded cream, is characterized in that: be made up of the component of following weight portion:
2. prepare the method for the third alkynes Evil humulone, Oxyfluorfen and the third careless amine compounded cream as claimed in claim 1 for one kind, it is characterized in that: Bing Que Evil humulone, Oxyfluorfen and the third careless amine are added in dimethylbenzene to stir and treat whole dissolving, then add tristyrylphenol polyoxyethylene ether, diphenylethyllene phenol formaldehyde condensation products APEO and calcium dodecyl benzene sulfonate and be uniformly mixed by reactor, sample analysis content, qualifiedly to leave standstill afterwards, filter, packaging, sample analysis content again, warehousing after passing.
CN201510997698.3A 2015-12-24 2015-12-24 Compound missible oil containing oxadiargyl, oxyfluorfen and pretilachlor and preparation method thereof Pending CN105475273A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106508903A (en) * 2016-11-02 2017-03-22 吕春雷 Herbicide used for paddy rice and application and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09255511A (en) * 1996-03-26 1997-09-30 Rhone Poulenc Agrochim Herbicidal composition for paddy field
CN101926352A (en) * 2010-09-15 2010-12-29 合肥星宇化学有限责任公司 Weeding composition and weeding application thereof in rice paddy field
CN103262844A (en) * 2013-06-19 2013-08-28 北京燕化永乐农药有限公司 Paddy field weeding composition
CN104642369A (en) * 2015-02-09 2015-05-27 安徽海日农化有限公司 Prochloraz and isoprothiolane compound missible oil and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09255511A (en) * 1996-03-26 1997-09-30 Rhone Poulenc Agrochim Herbicidal composition for paddy field
CN101926352A (en) * 2010-09-15 2010-12-29 合肥星宇化学有限责任公司 Weeding composition and weeding application thereof in rice paddy field
CN103262844A (en) * 2013-06-19 2013-08-28 北京燕化永乐农药有限公司 Paddy field weeding composition
CN104642369A (en) * 2015-02-09 2015-05-27 安徽海日农化有限公司 Prochloraz and isoprothiolane compound missible oil and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106508903A (en) * 2016-11-02 2017-03-22 吕春雷 Herbicide used for paddy rice and application and preparation method thereof
CN106508903B (en) * 2016-11-02 2020-02-07 吕春雷 Herbicide for paddy field and application and preparation method thereof

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Application publication date: 20160413