CN106332874A - Pinoxaden and fluroxypr-mepthyl compound emulsifiable concentrate and preparation method thereof - Google Patents
Pinoxaden and fluroxypr-mepthyl compound emulsifiable concentrate and preparation method thereof Download PDFInfo
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- CN106332874A CN106332874A CN201610723528.0A CN201610723528A CN106332874A CN 106332874 A CN106332874 A CN 106332874A CN 201610723528 A CN201610723528 A CN 201610723528A CN 106332874 A CN106332874 A CN 106332874A
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- Prior art keywords
- pinoxaden
- fluroxypr
- mepthyl
- fluroxypyr
- monooctyl ester
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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
- A01N25/00—Biocides, 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
- A01N25/02—Biocides, 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
-
- 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
-
- 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
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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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)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention provides a pinoxaden and fluroxypr-mepthyl compound emulsifiable concentrate and a preparation method thereof, and relates to the technical field of prevention and control of annual weeds in wheat fields. According to the present invention, 100 parts of the pinoxaden and fluroxypr-mepthyl compound emulsifiable concentrate is prepared at least from 5 parts of pinoxaden, 20 parts of fluroxypr-mepthyl, 7.5 parts of tristyrylphenol polyoxyethylene ether, 7.5 parts of distyrylphenol formaldehyde condensation compound polyoxyethylene ether, 15 parts of calcium dodecylbenzenesulfonate, and the balance of xylene; pinoxaden and fluroxypr-mepthyl are added to xylene, stirring is performed until both materials are dissolved, the remaining raw materials are added, uniform stirring and mixing are performed through a reaction kettle, sampling is performed and the content is analyzed, standing is performed after the qualified standard is achieved, filtration and packaging are performed, sampling is performed again and the content is analyzed, and warehousing is performed after the qualified standard is achieved; and the obvious synergistic effect can be provided when the 25% pinoxaden and fluroxypr-mepthyl compound emulsifiable concentrate is subjected to mixing use according to the ratio of 1:4 while the obvious synergistic effect cannot be achieved with the other preparations being subjected to the mixing use according to a certain ratio.
Description
Technical field
The present invention relates to wheat paddock annual grassy weeds Prevention Technique field, it is specifically related to a kind of pinoxaden and chlorine fluorine pyrrole
Fluoroacetic acid different monooctyl ester compounded cream and preparation method thereof.
Background technology
At present, the existing Herbicidal combinations for preventing and treating wheat paddock annual grassy weeds, such as Chinese patent cn
103461344 a disclose a kind of " Wheat field weeding composition ", and active ingredient is pyribenzoxim, azoles humulone, chlorine fluorine pyrrole oxygen
Acetic acid, pyribenzoxim percentage by weight in the composition is 1%～20%, azoles humulone percentage by weight in the composition
It is 1%～50% for 1%～20%, fluroxypyr percentage by weight in the composition, remaining is insecticides adjuvant.Separately have
Chinese patent cn 104521997 a discloses a kind of " Wheat field weeding composition ", and active ingredient is florasulam, chlorine ammonia
Pyridine acid (or its esters compound), phenoxy carboxylic acid herbicides, wherein phenoxy carboxylic acid herbicides are selected from MCPA,MCP,methoxone, diformazan
The different monooctyl ester of tetrachloro sodium, MCPA,MCP,methoxone, 2,4- drip, 2,4- d butyl ester, 2,4- drip one of different monooctyl ester.
Inventor verifies through long term test, and this above-mentioned several Herbicidal combinations is primarily present following defect:
1), by testing to concrete proportionings several disclosed in above-mentioned several Herbicidal combinations, find to wheat paddock one
The year preventing and treating of raw weeds cannot play good prevention effect.
2), it is directed to several formulations disclosed in above-mentioned several Herbicidal combinations, find all to exist difference through verification experimental verification
The defect of problem.For example, wettable powder easily causes product to bond, and is difficult dispersion in water and suspends, or blocking shower nozzle, in spray
In day with fog, the phenomenon such as reason precipitation, causes to spray irregular.
3), compound problem, by virulence test, heat are carried out to concrete proportionings several disclosed in above-mentioned several Herbicidal combinations
Storage stability test and mixture co-toxicity coefficient measure and find, are all unable to reach obvious synergistic effect.
Content of the invention
An object of the present invention is to provide a kind of pinoxaden and fluroxypyr different monooctyl ester compounded cream, this breast
Oil is reasonable in design, good to the prevention effect of wheat paddock annual grassy weeds, and can achieve that pinoxaden and fluroxypyr are different pungent
The notable synergistic effect that ester compounds.
For achieving the above object, present invention employs technical scheme below:
A kind of pinoxaden and fluroxypyr different monooctyl ester compounded cream, are at least made up of the component of following weight portion:
Pinoxaden belongs to neophyl pyrazolines herbicide, and the mechanism of action is acetylcoenzyme a carboxylase (acc) inhibitor.
Cause aliphatic acid biosynthesis block, make cell division stopping cell membrane destructurized containing fat, lead to weeds dead.In having
Suction conductibility is mainly used in barley field and prevents and kill off annual gramineous weed, through toxicity test and field control effectiveness test, result
Show there is good preventive effect to barley field annual gramineous weed such as wild oat, green bristlegrass, barnyard grass etc..To crop safety,
In resistance crop body, make it grand can lose toxicity in conjunction with conjugates.Degradable in soil, the half-life is shorter, will not be to rear
Stubble crop causes poisoning.
The different monooctyl ester of fluroxypyr belongs to inner sucting conduction type after seedling cauline leaf process herbicide, is inhaled by weeds quickly after dispenser
Receive, and be transmitted to each position of complete stool, make plant deformity, distortion, finally dead.This product mainly prevents and kill off the annual broad-leaved of winter wheat field
Weeds, such as clearvers, volume stem smartweed, purslane, Amaranthus retroflexus, black nightshade, chickweed, field bindweed, common vetch, water peanut, Descurainia sophia etc..
The pinoxaden of the present invention and fluroxypyr different monooctyl ester compounded cream, its advantage shows:
1), the missible oil of present invention preparation is all obvious at aspects such as stability of emulsion, low-temperature stability and heat storage stabilities
Better than the product prepared by other proportionings.
2), pass through experimental verification, pinoxaden monooctyl ester different with fluroxypyr is with 1:4 proportioning mixed compounded 25%
When pinoxaden and fluroxypyr different monooctyl ester compounded cream, notable synergistic sphere of action can be played, and other proportioning is mixed
Preparation, is all unable to reach notable synergistic sphere of action.Meanwhile, the actual toxicity of different ratio is not with theoretical toxicity
Strengthen and lifted, between actual toxicity and theoretical toxicity, have no regular change.
Another object of the present invention is to providing a kind of pinoxaden and the system of fluroxypyr different monooctyl ester compounded cream
Preparation Method, pinoxaden and the different monooctyl ester of fluroxypyr is added stirring in dimethylbenzene to treat all to dissolve, is subsequently adding triphen
Vinyl benzene phenol polyethenoxy ether, diphenylethyllene phenol formaldehyde condensation products APEO and calcium dodecyl benzene sulfonate simultaneously lead to
Cross reactor to be uniformly mixed, sample analysis content, qualified rear standing, filtration, packaging, again sample analysis content, qualified
After put in storage.
The pinoxaden of the present invention and the preparation method of fluroxypyr different monooctyl ester compounded cream, preparation technology is more simple
Just it is easy to industrialized production.
Specific embodiment
Below with reference to embodiment, the present invention is described in detail.But, embodiment content is only to this
Bright example and explanation, affiliated those skilled in the art do various repairing to described specific embodiment
Change or supplement or using similar mode substitute, without departing from invention design or surmount defined in the claims
Scope, all should belong to protection scope of the present invention.
First, the preparation of pinoxaden and fluroxypyr different monooctyl ester compounded cream, and the breast prepared by each embodiment
The testing result of all technical of oil, heat storage stability result of the test.
Embodiment 1
25% pinoxaden and fluroxypyr different monooctyl ester compounded cream, each component and its weight portion are as follows:
| Composition | Weight portion |
| Pinoxaden | 5 |
| The different monooctyl ester of fluroxypyr | 20 |
| Tristyrylphenol polyoxyethylene ether | 7.5 |
| Diphenylethyllene phenol formaldehyde condensation products APEO | 7.5 |
| Calcium dodecyl benzene sulfonate | 15 |
| Dimethylbenzene | 45 |
Preparation method: pinoxaden and the different monooctyl ester of fluroxypyr are added stirring in dimethylbenzene to treat all to dissolve, so
Add tristyrylphenol polyoxyethylene ether, diphenylethyllene phenol formaldehyde condensation products APEO and detergent alkylate afterwards
Sulfoacid calcium is simultaneously uniformly mixed by reactor, sample analysis content, qualified rear standing, filtration, packaging, again sample analysis
Content, warehousing after passing.
Embodiment 2
24% pinoxaden and fluroxypyr different monooctyl ester compounded cream, each component and its weight portion are as follows:
| Composition | Weight portion |
| Pinoxaden | 5 |
| The different monooctyl ester of fluroxypyr | 19 |
| Tristyrylphenol polyoxyethylene ether | 7.5 |
| Diphenylethyllene phenol formaldehyde condensation products APEO | 7.5 |
| Calcium dodecyl benzene sulfonate | 15 |
| Dimethylbenzene | 46 |
Preparation method is with embodiment 1.
Embodiment 3
23% pinoxaden and fluroxypyr different monooctyl ester compounded cream, each component and its weight portion are as follows:
Preparation method is with embodiment 1.
Embodiment 4
26% pinoxaden and fluroxypyr different monooctyl ester compounded cream, each component and its weight portion are as follows:
| Composition | Weight portion |
| Pinoxaden | 6 |
| The different monooctyl ester of fluroxypyr | 20 |
| Tristyrylphenol polyoxyethylene ether | 7.5 |
| Diphenylethyllene phenol formaldehyde condensation products APEO | 7.5 |
| Calcium dodecyl benzene sulfonate | 15 |
| Dimethylbenzene | 44 |
Preparation method is with embodiment 1.
Embodiment 5
27% pinoxaden and fluroxypyr different monooctyl ester compounded cream, each component and its weight portion are as follows:
| Composition | Weight portion |
| Pinoxaden | 6 |
| The different monooctyl ester of fluroxypyr | 21 |
| Tristyrylphenol polyoxyethylene ether | 7.5 |
| Diphenylethyllene phenol formaldehyde condensation products APEO | 7.5 |
| Calcium dodecyl benzene sulfonate | 15 |
| Dimethylbenzene | 43 |
Preparation method is with embodiment 1.
Embodiment 6
25% pinoxaden and fluroxypyr different monooctyl ester compounded cream, each component and its weight portion are as follows:
Preparation method: pinoxaden and the different monooctyl ester of fluroxypyr are added stirring in dimethylbenzene to treat all to dissolve, so
Add Aucubin, tristyrylphenol polyoxyethylene ether, diphenylethyllene phenol formaldehyde condensation products APEO afterwards
Be uniformly mixed with calcium dodecyl benzene sulfonate and by reactor, sample analysis content, qualified after standing, filter, packaging,
Sample analysis content again, warehousing after passing.
Pinoxaden prepared by embodiment 1～6 and fluroxypyr different monooctyl ester compounded cream, product items technology refers to
As shown in table 1, product heat storage stability result of the test is as shown in table 2 for target testing result.
16 embodiments of table prepare the testing result of product all technical
26 embodiments of table prepare product heat storage stability result of the test
By table 1 and 2 as can be seen that the product of embodiment 1 and 6 preparation is in stability of emulsion, low-temperature stability and warm
The aspects such as storage stability are significantly better than that the product prepared by other proportionings.
2nd, toxicological information
The different monooctyl ester of fluroxypyr: rat acute ld50For 2405mg/kg, rabbit acute percutaneous ld50>5000mg/
Kg, rat acute sucks 4 (hour) ld50>296mg/l.
Pinoxaden: rat acute ld50> 5000mg/kg, acute percutaneous ld50> 2000mg/kg, Acute inhalation
(4h): male rat lc50=4.63mg/l, female rats lc50=6.24mg/l.
3rd, indoor biological activity (virulence) of pinoxaden and fluroxypyr different monooctyl ester compounded cream measures.
1 test objective
The life to grass, amur foxtail of pinoxaden and the different monooctyl ester of fluroxypyr is determined using pot experiment method method
Thing activity, selects to provide scientific basis for the proportioning in both rationally mixed and production.
2 experimental conditions
2.1 material to be tested
Grass: Seed storage is collected in Anhui Meilan Agricultural Development Co., Ltd. laboratory field；
Amur foxtail: Seed storage is collected in Anhui Meilan Agricultural Development Co., Ltd. laboratory field.
2.2 test medicine
Pinoxaden active compound, Anhui Meilan Agricultural Development Co., Ltd. provides；
Fluroxypyr different monooctyl ester active compound, Anhui Meilan Agricultural Development Co., Ltd. provides.
2.3 test proportionings are processed
It is designed according to embodiment 1-6 proportioning.
2.4 processing mode
2.4.1 medicament is to careless activity test
After grass seed presoaking and germinating, point is sowed at the sectional area 0.25m equipped with soil2Basin in, every basin broadcasts 100, greenhouse
Inside cultivate and processed to careless 1 leaf 1 heart stage.Spray liquid with potter precision laboratory spray tower, spouting liquid is often to process
50ml, keeps ground moistening after medicine, and sets clear water blank.Often process and be repeated 4 times, weigh each treating meadow within 20 days after medicine
Upper part fresh weight, calculates each inhibition percentage processing aerial growth and remaining grass for the percentage of comparison, uses
Gowing method is evaluated the two and is used with to careless synergy type.The actual preventive effect of mixe herbicide calculates as follows:
e0=x+y (100-x)/100
In formula: x is fluroxypyr different monooctyl ester consumption is to careless fresh weight preventive effect during p；
Y is to careless fresh weight preventive effect for pinoxaden consumption for q；
e0It is to be right to careless fresh weight preventive effect+pinoxaden consumption for q during p for fluroxypyr different monooctyl ester consumption
The fresh weight preventive effect of grass；
E is the actual preventive effect of mixe herbicide.
e-e0＞ 10% is synergistic effect；e-e0＜ -10% is antagonism；e-e0Value is to add between theoretical value ± 10%
One-tenth acts on.
2.4.2 the activity test to amur foxtail for the medicament
After vernalization after amur foxtail seed-soaking, point is sowed at the sectional area 0.25m equipped with soil2Basin in, remaining same 2.4.1.
3 interpretations of result and discussion
The mixture of embodiment 1-6 totally 6 different compound proportions is to careless e-e0Value is followed successively by 22.20%, 1.65%,
3.35%, 2.35%, 2.60%, 23.25%；E-e to amur foxtail0Value is respectively 21.50%, 2.15%, 3.35%,
2.60%, 2.65%, 22.25%, thus illustrating that embodiment 1 belongs to respect to the synergy of the compound proportion of embodiment 2-5
In obvious addition synergistic effect, and the synergy of embodiment 2-5 substantially belongs to addition.Meanwhile, by the reality of embodiment 6
After testing as can be seen that with the addition of a small amount of Aucubin in compounded cream, pinoxaden and fluroxypyr can be made different
The compounding synergy of monooctyl ester is lifted further.
Claims (2)
1. a kind of pinoxaden and fluroxypyr different monooctyl ester compounded cream it is characterised in that: at least by following weight portion
Component is made:
2. a kind of method preparing pinoxaden as claimed in claim 1 and fluroxypyr different monooctyl ester compounded cream, it is special
Levy and be: pinoxaden and the different monooctyl ester of fluroxypyr are added stirring in dimethylbenzene to treat all to dissolve, is subsequently adding triphen
Vinyl benzene phenol polyethenoxy ether, diphenylethyllene phenol formaldehyde condensation products APEO and calcium dodecyl benzene sulfonate simultaneously lead to
Cross reactor to be uniformly mixed, sample analysis content, qualified rear standing, filtration, packaging, again sample analysis content, qualified
After put in storage.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610723528.0A CN106332874A (en) | 2016-08-25 | 2016-08-25 | Pinoxaden and fluroxypr-mepthyl compound emulsifiable concentrate and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610723528.0A CN106332874A (en) | 2016-08-25 | 2016-08-25 | Pinoxaden and fluroxypr-mepthyl compound emulsifiable concentrate and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106332874A true CN106332874A (en) | 2017-01-18 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610723528.0A Pending CN106332874A (en) | 2016-08-25 | 2016-08-25 | Pinoxaden and fluroxypr-mepthyl compound emulsifiable concentrate and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105707086A (en) * | 2016-04-13 | 2016-06-29 | 安徽美兰农业发展股份有限公司 | Clomazone and oxadiazon compound emulsifiable concentrate and preparation method thereof |
| WO2021036251A1 (en) * | 2019-08-27 | 2021-03-04 | 青岛清原化合物有限公司 | Herbicidal composition containing r-type pyridyloxy carboxylic acid derivatives and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101562978A (en) * | 2006-10-27 | 2009-10-21 | 先正达参股股份有限公司 | Herbicidal compositions |
| CN105557716A (en) * | 2016-02-04 | 2016-05-11 | 创新美兰（合肥）股份有限公司 | Pinoxaden and clodinafop-propargyl compound emulsifiable oil and preparation method thereof |
| CN105766975A (en) * | 2016-04-08 | 2016-07-20 | 江苏富田农化有限公司 | Herbicidal composite containing mesosulfuron-methyl, pinoxaden and fluroxypyr |
-
2016
- 2016-08-25 CN CN201610723528.0A patent/CN106332874A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101562978A (en) * | 2006-10-27 | 2009-10-21 | 先正达参股股份有限公司 | Herbicidal compositions |
| CN105557716A (en) * | 2016-02-04 | 2016-05-11 | 创新美兰（合肥）股份有限公司 | Pinoxaden and clodinafop-propargyl compound emulsifiable oil and preparation method thereof |
| CN105766975A (en) * | 2016-04-08 | 2016-07-20 | 江苏富田农化有限公司 | Herbicidal composite containing mesosulfuron-methyl, pinoxaden and fluroxypyr |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105707086A (en) * | 2016-04-13 | 2016-06-29 | 安徽美兰农业发展股份有限公司 | Clomazone and oxadiazon compound emulsifiable concentrate and preparation method thereof |
| WO2021036251A1 (en) * | 2019-08-27 | 2021-03-04 | 青岛清原化合物有限公司 | Herbicidal composition containing r-type pyridyloxy carboxylic acid derivatives and application thereof |
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Application publication date: 20170118 |