CN108378057A - A kind of rice weeding composition of Han metamifops - Google Patents
A kind of rice weeding composition of Han metamifops Download PDFInfo
- Publication number
- CN108378057A CN108378057A CN201810256372.9A CN201810256372A CN108378057A CN 108378057 A CN108378057 A CN 108378057A CN 201810256372 A CN201810256372 A CN 201810256372A CN 108378057 A CN108378057 A CN 108378057A
- Authority
- CN
- China
- Prior art keywords
- reaction
- acid
- metamifops
- preparation
- weeding composition
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- 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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
-
- 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
- A01N39/00—Biocides, pest repellants or attractants, or plant growth regulators containing aryloxy- or arylthio-aliphatic or cycloaliphatic compounds, containing the group or, e.g. phenoxyethylamine, phenylthio-acetonitrile, phenoxyacetone
- A01N39/02—Aryloxy-carboxylic acids; Derivatives thereof
- A01N39/04—Aryloxy-acetic acids; Derivatives thereof
-
- 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
- A01N43/34—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
- A01N43/42—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 condensed with carbocyclic 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
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/74—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,3
- A01N43/76—1,3-Oxazoles; Hydrogenated 1,3-oxazoles
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- General Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a kind of preparation methods of the rice weeding composition of Han metamifops, including prepare kettle and filtering, metering, packaging and storage after grinding, sand mill fine grinding, sampling analysis, qualification is mixed；Preparation method is scientific and reasonable, easy to operate, convenient for improving production efficiency, production cost is low, there is environment friendly and pollution-free metamifops efficient, low toxicity, environmental protection, cyhalofop-butyl can preferably remove barnyard grass, the grassy weeds such as moleplant seed simultaneously, only carry out cauline leaf sprinkling and low toxicity, there is special efficacy to the malignant weed rhizome of nutgrass flatsedge, and part broad leaved weed can be prevented and kill off, it is very environmentally friendly.
Description
Technical field
The present invention relates to medical compounds field, specially a kind of rice weeding composition of Han metamifops.
Background technology
Widely distributed weeds have 30000 kinds in the whole world, different degrees of harm are caused to crop for about 1800 kinds every year, often
Crop production reduction is up to 9.7% year caused by Weed infestation, and herbicide refers to that weeds can be made thoroughly or selectively to occur is withered
Medicament, also known as herbicide, to eliminate or inhibit a substance of plant growth.Common herbicide kind is organic compound
It is miscellaneous to can be widely used for the ground such as prevention farmland, orchard, floral nursery, grassland and bare place, railway line, river, reservoir, warehouse for object
The noxious plants such as grass, miscellaneous filling, miscellaneous tree.Many weeds are efficiently controlled using herbicide in the last hundred years, but chemical agent is big
Amount using also having caused a series of problem, the appearance, soil pollution of such as herbicide-resistant weeds plant, the degeneration of water quality,
And the harm etc. to non-weeds biology, it is unfavorable for carrying out weeding.
Invention content
The present invention provides a kind of rice weeding composition of Han metamifops, and preparation method is scientific and reasonable, easy to operate, just
In improving production efficiency, production cost is low, while environment friendly and pollution-free , metamifops have efficient, low toxicity, environmental protection, cyanogen fluorine grass
Ester can preferably remove barnyard grass, and the grassy weeds such as moleplant seed only carry out cauline leaf sprinkling and low toxicity, to the malignant weed rhizome of nutgrass flatsedge
There is special efficacy, and part broad leaved weed can be prevented and kill off, it is very environmentally friendly, it can effectively solve the problems in above-mentioned background technology.
To achieve the above object, the present invention provides the following technical solutions：A kind of rice weeding combination of Han metamifops
Object, formula You metamifops, cyhalofop-butyl, bispyribac-sodium, dichloro quinolinic acid, halosulfuronmethyl, chlorine fluorine are than fluoroacetic acid, by certain
Ratio mixing composition, the formula are made of the raw material of following parts by weight：10-15 parts of metamifop, cyhalofop-butyl 10-15
Part, 5-8 parts of bispyribac-sodium, 5-10 parts of dichloro quinolinic acid, 5-8 parts of halosulfuronmethyl, chlorine fluorine are than fluoroacetic acid 5-10 parts.
According to above-mentioned technical proposal, the preparation method of the cyhalofop-butyl is 1）Etherification reaction：It is organic molten to aprotic
Acid binding agent, organic base and phase transfer catalyst are added in agent, is then added portionwise（R）-2-（4- hydroxyphenoxies）Propionic acid, then add
Enter 3,4- difluorobenzonilyiles, be heated to 60~90 DEG C, insulation reaction 2~4 hours removes solvent, be down to room temperature, adds after reaction
Water dissolution is adjusted with acid pH to 3~5, stirring, and solid is precipitated, and filtering obtains intermediate（R）-2-[4-（2- fluorine-4-nitriles）-
Phenoxy group]-propionic acid；Wherein,（R）-2-（4- hydroxyphenoxies）The molar ratio of propionic acid and 3,4- difluorobenzonilyiles is 1:1~1.5；Institute
The acid binding agent stated is inorganic base,
2）Dehydration esterification：By step 1）The intermediate of acquisition（R）-2-[4-（2- fluorine-4-nitriles）Phenoxy group]-propionic acid and positive fourth
Reaction vessel is added in alcohol, dehydrated solvent and bronsted acid catalyst, is heated to reflux, water is divided to be separated to anhydrous, reaction terminates, and obtains
Reaction solution is washed to neutrality by reaction solution, and removing solvent obtains cyhalofop-butyl；The dehydrated solvent refers to water-immiscible
Alkanes or ketone non-proton organic solvent.
According to above-mentioned technical proposal, the preparation method of the halosulfuronmethyl includes step a and step b；The step a
For：Built-in reaction dissolvent in reaction vessel puts into the chloro- 1- methyl -5- sulfoamidos -4- pyrazole carboxylic acid first of 3- into reaction vessel
Then catalyst is added in ester and diphenyl carbonate, compound III is obtained after reaction；The step b is：Built-in reaction in reaction vessel
Solvent takes in compounds Ⅳ and step a in gained compound III input reaction vessel, up to halosulfuronmethyl after reaction.
According to above-mentioned technical proposal, the preparation method of the dichloro quinolinic acid is that 450mL first is first added in reaction bulb
Dichloro quinolinic acid wet product is added in alcohol with stirring（Folding hundred）It is small to keep the temperature 2 under reflux for 250g and 45g sodium hydroxides, temperature rising reflux
When, vacuum distillation steams methanol, when steaming 350~400ml of methanol, stops distillation, pours out material, the crystallisation by cooling in disk,
After placing 24 hours, drying obtains dichloroquinoline acid sodium-salt 325.8g, mass content 82.0%, yield 98.7%.
A kind of preparation method of the rice weeding composition of Han metamifops, includes the following steps：Kettle mixing is prepared to stir
It filters, measure, pack and is put in storage after mixing grinding, sand mill fine grinding, sampling analysis, qualification.
According to above-mentioned technical proposal, the sampling analysis is acquired by liquid collector and prepares kettle inner liquid medicine, and is sent to inspection
Analysis room is tested to test analysis.
According to above-mentioned technical proposal, the packaging is carried out by packing machine.
Compared with prior art, beneficial effects of the present invention：Preparation method is scientific and reasonable, easy to operate, convenient for improving production
Efficiency, production cost is low, while environment friendly and pollution-free , metamifops have efficient, low toxicity, environmental protection, and cyhalofop-butyl can be preferable
Barnyard grass is removed, the grassy weeds such as moleplant seed only carry out cauline leaf sprinkling and low toxicity, have special efficacy to the malignant weed rhizome of nutgrass flatsedge, and
Part broad leaved weed can be prevented and kill off, it is very environmentally friendly.
Description of the drawings
Attached drawing is used to provide further understanding of the present invention, and a part for constitution instruction, the reality with the present invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.
In the accompanying drawings：
Fig. 1 is the preparation flow figure of the present invention.
Specific implementation mode
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1：As shown in Figure 1, the present invention provides a kind of rice weeding composition of Han metamifops, formula You Evil
Azole amide, cyhalofop-butyl, bispyribac-sodium, dichloro quinolinic acid, halosulfuronmethyl, chlorine fluorine are mixed in a certain ratio group than fluoroacetic acid
At formula is made of the raw material of following parts by weight：10 parts of metamifop, 10 parts of cyhalofop-butyl, 5 parts of bispyribac-sodium, dichloroquinoline
5 parts of acid, 5 parts of halosulfuronmethyl, chlorine fluorine are than 5 parts of fluoroacetic acid.
According to above-mentioned technical proposal, the preparation method of cyhalofop-butyl is 1）Etherification reaction：Into non-proton organic solvent
Acid binding agent, organic base and phase transfer catalyst is added, is then added portionwise（R）-2-（4- hydroxyphenoxies）Propionic acid adds 3,
4- difluorobenzonilyiles, are heated to 60~90 DEG C, and insulation reaction 2~4 hours removes solvent, be down to room temperature, adds water-soluble after reaction
Solution, is adjusted with acid pH to 3~5, stirs, and solid is precipitated, and filtering obtains intermediate（R）-2-[4-（2- fluorine-4-nitriles）Benzene oxygen
Base]-propionic acid；Wherein,（R）-2-（4- hydroxyphenoxies）The molar ratio of propionic acid and 3,4- difluorobenzonilyiles is 1:1~1.5；Tie up acid
Agent is inorganic base；
2）Dehydration esterification：By step 1）The intermediate of acquisition（R）-2-[4-（2- fluorine-4-nitriles）Phenoxy group]-propionic acid and positive fourth
Reaction vessel is added in alcohol, dehydrated solvent and bronsted acid catalyst, is heated to reflux, water is divided to be separated to anhydrous, reaction terminates, and obtains
Reaction solution is washed to neutrality by reaction solution, and removing solvent obtains cyhalofop-butyl；Dehydrated solvent refer to water-immiscible alkane
Class or ketone non-proton organic solvent.
According to above-mentioned technical proposal, the preparation method of halosulfuronmethyl includes step a and step b；Step a is：Reaction is held
Built-in reaction dissolvent in device puts into the chloro- 1- methyl -5- sulfoamidos -4- pyrazole carboxylic acids methyl esters of 3- and carbonic acid into reaction vessel
Then catalyst is added in diphenyl ester, compound III is obtained after reaction；Step b is：Built-in reaction dissolvent, takes chemical combination in reaction vessel
In object IV and step a in gained compound III input reaction vessel, up to halosulfuronmethyl after reaction.
According to above-mentioned technical proposal, the preparation method of dichloro quinolinic acid is that 450mL methanol is first added in reaction bulb, in
It is added with stirring dichloro quinolinic acid wet product（Folding hundred）250g and 45g sodium hydroxides, temperature rising reflux keep the temperature 2 hours under reflux, subtract
Pressure distillation, steams methanol, when steaming 350~400ml of methanol, stops distillation, pours out material, and the crystallisation by cooling in disk is placed
After 24 hours, drying obtains dichloroquinoline acid sodium-salt 325.8g, mass content 82.0%, yield 98.7%.
A kind of preparation method of the rice weeding composition of Han metamifops, includes the following steps：Kettle mixing is prepared to stir
It filters, measure, pack and is put in storage after mixing grinding, sand mill fine grinding, sampling analysis, qualification.
According to above-mentioned technical proposal, sampling analysis is acquired by liquid collector and prepares kettle inner liquid medicine, and is sent to inspection point
It tests analysis analysis room.
According to above-mentioned technical proposal, packaging is carried out by packing machine.
Embodiment 2：As shown in Figure 1, the present invention provides a kind of rice weeding composition of Han metamifops, formula You Evil
Azole amide, cyhalofop-butyl, bispyribac-sodium, dichloro quinolinic acid, halosulfuronmethyl, chlorine fluorine are mixed in a certain ratio group than fluoroacetic acid
At formula is made of the raw material of following parts by weight：13 parts of metamifop, 13 parts of cyhalofop-butyl, 7 parts of bispyribac-sodium, dichloroquinoline
8 parts of acid, 7 parts of halosulfuronmethyl, chlorine fluorine are than 7 parts of fluoroacetic acid.
According to above-mentioned technical proposal, the preparation method of cyhalofop-butyl is 1）Etherification reaction：Into non-proton organic solvent
Acid binding agent, organic base and phase transfer catalyst is added, is then added portionwise（R）-2-（4- hydroxyphenoxies）Propionic acid adds 3,
4- difluorobenzonilyiles, are heated to 60~90 DEG C, and insulation reaction 2~4 hours removes solvent, be down to room temperature, adds water-soluble after reaction
Solution, is adjusted with acid pH to 3~5, stirs, and solid is precipitated, and filtering obtains intermediate（R）-2-[4-（2- fluorine-4-nitriles）Benzene oxygen
Base]-propionic acid；Wherein,（R）-2-（4- hydroxyphenoxies）The molar ratio of propionic acid and 3,4- difluorobenzonilyiles is 1:1~1.5；Tie up acid
Agent is inorganic base；
2）Dehydration esterification：By step 1）The intermediate of acquisition（R）-2-[4-（2- fluorine-4-nitriles）Phenoxy group]-propionic acid and positive fourth
Reaction vessel is added in alcohol, dehydrated solvent and bronsted acid catalyst, is heated to reflux, water is divided to be separated to anhydrous, reaction terminates, and obtains
Reaction solution is washed to neutrality by reaction solution, and removing solvent obtains cyhalofop-butyl；Dehydrated solvent refer to water-immiscible alkane
Class or ketone non-proton organic solvent.
According to above-mentioned technical proposal, the preparation method of halosulfuronmethyl includes step a and step b；Step a is：Reaction is held
Built-in reaction dissolvent in device puts into the chloro- 1- methyl -5- sulfoamidos -4- pyrazole carboxylic acids methyl esters of 3- and carbonic acid into reaction vessel
Then catalyst is added in diphenyl ester, compound III is obtained after reaction；Step b is：Built-in reaction dissolvent, takes chemical combination in reaction vessel
In object IV and step a in gained compound III input reaction vessel, up to halosulfuronmethyl after reaction.
According to above-mentioned technical proposal, the preparation method of dichloro quinolinic acid is that 450mL methanol is first added in reaction bulb, in
It is added with stirring dichloro quinolinic acid wet product（Folding hundred）250g and 45g sodium hydroxides, temperature rising reflux keep the temperature 2 hours under reflux, subtract
Pressure distillation, steams methanol, when steaming 350~400ml of methanol, stops distillation, pours out material, and the crystallisation by cooling in disk is placed
After 24 hours, drying obtains dichloroquinoline acid sodium-salt 325.8g, mass content 82.0%, yield 98.7%.
A kind of preparation method of the rice weeding composition of Han metamifops, includes the following steps：Kettle mixing is prepared to stir
It filters, measure, pack and is put in storage after mixing grinding, sand mill fine grinding, sampling analysis, qualification.
According to above-mentioned technical proposal, sampling analysis is acquired by liquid collector and prepares kettle inner liquid medicine, and is sent to inspection point
It tests analysis analysis room.
According to above-mentioned technical proposal, packaging is carried out by packing machine.
Embodiment 3：As shown in Figure 1, the present invention provides a kind of rice weeding composition of Han metamifops, formula You Evil
Azole amide, cyhalofop-butyl, bispyribac-sodium, dichloro quinolinic acid, halosulfuronmethyl, chlorine fluorine are mixed in a certain ratio group than fluoroacetic acid
At formula is made of the raw material of following parts by weight：15 parts of metamifop, 15 parts of cyhalofop-butyl, 8 parts of bispyribac-sodium, dichloroquinoline
10 parts of acid, 8 parts of halosulfuronmethyl, chlorine fluorine are than 10 parts of fluoroacetic acid.
According to above-mentioned technical proposal, the preparation method of cyhalofop-butyl is 1）Etherification reaction：Into non-proton organic solvent
Acid binding agent, organic base and phase transfer catalyst is added, is then added portionwise（R）-2-（4- hydroxyphenoxies）Propionic acid adds 3,
4- difluorobenzonilyiles, are heated to 60~90 DEG C, and insulation reaction 2~4 hours removes solvent, be down to room temperature, adds water-soluble after reaction
Solution, is adjusted with acid pH to 3~5, stirs, and solid is precipitated, and filtering obtains intermediate（R）-2-[4-（2- fluorine-4-nitriles）Benzene oxygen
Base]-propionic acid；Wherein,（R）-2-（4- hydroxyphenoxies）The molar ratio of propionic acid and 3,4- difluorobenzonilyiles is 1:1~1.5；Tie up acid
Agent is inorganic base；
2）Dehydration esterification：By step 1）The intermediate of acquisition（R）-2-[4-（2- fluorine-4-nitriles）Phenoxy group]-propionic acid and positive fourth
Reaction vessel is added in alcohol, dehydrated solvent and bronsted acid catalyst, is heated to reflux, water is divided to be separated to anhydrous, reaction terminates, and obtains
Reaction solution is washed to neutrality by reaction solution, and removing solvent obtains cyhalofop-butyl；Dehydrated solvent refer to water-immiscible alkane
Class or ketone non-proton organic solvent.
According to above-mentioned technical proposal, the preparation method of halosulfuronmethyl includes step a and step b；Step a is：Reaction is held
Built-in reaction dissolvent in device puts into the chloro- 1- methyl -5- sulfoamidos -4- pyrazole carboxylic acids methyl esters of 3- and carbonic acid into reaction vessel
Then catalyst is added in diphenyl ester, compound III is obtained after reaction；Step b is：Built-in reaction dissolvent, takes chemical combination in reaction vessel
In object IV and step a in gained compound III input reaction vessel, up to halosulfuronmethyl after reaction.
According to above-mentioned technical proposal, the preparation method of dichloro quinolinic acid is that 450mL methanol is first added in reaction bulb, in
It is added with stirring dichloro quinolinic acid wet product（Folding hundred）250g and 45g sodium hydroxides, temperature rising reflux keep the temperature 2 hours under reflux, subtract
Pressure distillation, steams methanol, when steaming 350~400ml of methanol, stops distillation, pours out material, and the crystallisation by cooling in disk is placed
After 24 hours, drying obtains dichloroquinoline acid sodium-salt 325.8g, mass content 82.0%, yield 98.7%.
A kind of preparation method of the rice weeding composition of Han metamifops, includes the following steps：Kettle mixing is prepared to stir
It filters, measure, pack and is put in storage after mixing grinding, sand mill fine grinding, sampling analysis, qualification.
According to above-mentioned technical proposal, sampling analysis is acquired by liquid collector and prepares kettle inner liquid medicine, and is sent to inspection point
It tests analysis analysis room.
According to above-mentioned technical proposal, packaging is carried out by packing machine.
Based on above-mentioned, it is an advantage of the current invention that preparation method is scientific and reasonable, it is easy to operate, it is raw convenient for improving production efficiency
Produce it is at low cost, while environment friendly and pollution-free , metamifops have efficiently, low toxicity, environmental protection, cyhalofop-butyl can preferably remove barnyard grass
Grass, the grassy weeds such as moleplant seed only carry out cauline leaf sprinkling and low toxicity, have special efficacy to the malignant weed rhizome of nutgrass flatsedge, and can prevent and kill off
Part broad leaved weed, it is very environmentally friendly.
Finally it should be noted that：The foregoing is merely the preferred embodiments of the present invention, are not intended to restrict the invention, to the greatest extent
Present invention has been described in detail with reference to the aforementioned embodiments for pipe, for those skilled in the art, still can be with
Technical scheme described in the above embodiments is modified or equivalent replacement of some of the technical features.It is all
Within the spirit and principles in the present invention, any modification, equivalent replacement, improvement and so on should be included in the guarantor of the present invention
Within the scope of shield.
Claims (7)
1. a kind of rice weeding composition of Han metamifops, it is characterised in that：Be formulated You metamifops, cyhalofop-butyl,
Bispyribac-sodium, dichloro quinolinic acid, halosulfuronmethyl, chlorine fluorine are mixed in a certain ratio composition, the formula is by following heavy than fluoroacetic acid
The raw material of amount part is made：10-15 parts of metamifop, 10-15 parts of cyhalofop-butyl, 5-8 parts of bispyribac-sodium, dichloro quinolinic acid 5-10
Part, 5-8 parts of halosulfuronmethyl, chlorine fluorine are than fluoroacetic acid 5-10 parts.
2. a kind of rice weeding composition of Han metamifops according to claim 1, it is characterised in that：The cyanogen fluorine
The preparation method of careless ester is 1）Etherification reaction：Acid binding agent, organic base and phase transfer catalysis (PTC) are added into non-proton organic solvent
Then agent is added portionwise（R）-2-（4- hydroxyphenoxies）Propionic acid adds 3,4- difluorobenzonilyiles, is heated to 60~90 DEG C, protects
Temperature reaction 2~4 hours, removes solvent, is down to room temperature, be dissolved in water, be adjusted with acid pH to 3~5 after reaction, stirs, analysis
Go out solid, filters, obtain intermediate（R）-2-[4-（2- fluorine-4-nitriles）Phenoxy group]-propionic acid；Wherein,（R）-2-（4- hydroxyls
Phenoxy group）The molar ratio of propionic acid and 3,4- difluorobenzonilyiles is 1:1~1.5；The acid binding agent is inorganic base；2）Dehydration esterification：
By step 1）The intermediate of acquisition（R）-2-[4-（2- fluorine-4-nitriles）Phenoxy group]-propionic acid and n-butanol, dehydrated solvent and
Reaction vessel is added in bronsted acid catalyst, is heated to reflux, water is divided to be separated to anhydrous, reaction terminates, and obtains reaction solution, by reaction solution
It is washed to neutrality, removing solvent obtains cyhalofop-butyl；The dehydrated solvent refers to that water-immiscible alkanes or ketone are non-
Protic organic solvent.
3. a kind of rice weeding composition of Han metamifops according to claim 1, it is characterised in that：The chlorine pyrrole
The preparation method of Sulfometuron Methyl includes step a and step b；The step a is：Built-in reaction dissolvent in reaction vessel holds to reaction
The chloro- 1- methyl -5- sulfoamidos -4- pyrazole carboxylic acids methyl esters of 3- and diphenyl carbonate are put into device, catalyst is then added, and are reacted
Compound III is obtained afterwards；The step b is：Built-in reaction dissolvent in reaction vessel takes gained compound in compounds Ⅳ and step a
In III input reaction vessel, up to halosulfuronmethyl after reaction.
4. a kind of rice weeding composition of Han metamifops according to claim 1, it is characterised in that：The dichloro
The preparation method of quinolinic acid is that 450mL methanol is first added in reaction bulb, and dichloro quinolinic acid wet product is added with stirring（Folding hundred）
250g and 45g sodium hydroxides, temperature rising reflux keep the temperature 2 hours under reflux, and vacuum distillation steams methanol, when steaming methanol 350
When~400ml, stop distillation, pour out material, the crystallisation by cooling in disk, after placing 24 hours, drying obtains dichloro quinolinic acid sodium
Salt 325.8g, mass content 82.0%, yield 98.7%.
5. a kind of preparation method of the rice weeding composition of Han metamifops, it is characterised in that：Include the following steps：It prepares
Filtering, metering, packaging and storage after grinding, sand mill fine grinding, sampling analysis, qualification is mixed in kettle.
6. according to a kind of preparation method of the rice weeding composition of Han metamifops of claim 5, it is characterised in that：It is described
Sampling analysis is acquired by liquid collector and prepares kettle inner liquid medicine, and is sent to check analysis room and is tested analysis.
7. according to a kind of preparation method of the rice weeding composition of Han metamifops of claim 5, it is characterised in that：It is described
Packaging is carried out by packing machine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810256372.9A CN108378057A (en) | 2018-03-27 | 2018-03-27 | A kind of rice weeding composition of Han metamifops |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810256372.9A CN108378057A (en) | 2018-03-27 | 2018-03-27 | A kind of rice weeding composition of Han metamifops |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108378057A true CN108378057A (en) | 2018-08-10 |
Family
ID=63072375
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810256372.9A Withdrawn CN108378057A (en) | 2018-03-27 | 2018-03-27 | A kind of rice weeding composition of Han metamifops |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108378057A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109287649A (en) * | 2018-11-01 | 2019-02-01 | 安徽远景作物保护有限公司 | A kind of Herbicidal combinations and its application containing dichloro quinolinic acid |
| CN109452299A (en) * | 2018-11-19 | 2019-03-12 | 安徽远景作物保护有限公司 | A kind of Herbicidal composition for rice field and its application |
| CN109479891A (en) * | 2018-11-13 | 2019-03-19 | 安徽远景作物保护有限公司 | A kind of Herbicidal combinations and its application containing halosulfuronmethyl |
| CN109651140A (en) * | 2018-12-12 | 2019-04-19 | 江苏中旗科技股份有限公司 | A kind of synthetic method of cyhalofop-butyl active compound |
| CN110003051A (en) * | 2019-05-06 | 2019-07-12 | 湖南速博生物技术有限公司 | A kind of preparation method of cyhalofop-butyl standard items |
Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101965837A (en) * | 2010-09-17 | 2011-02-09 | 北京颖新泰康国际贸易有限公司 | Herbicide composition and application thereof |
| CN102113503A (en) * | 2010-12-30 | 2011-07-06 | 苏州富美实植物保护剂有限公司 | Herbicide composite used in paddy field |
| CN102342280A (en) * | 2011-10-26 | 2012-02-08 | 中化蓝天集团有限公司 | Active composition for preventing and eliminating resistant weeds in paddy field and weedicide thereof |
| CN102796043A (en) * | 2012-06-13 | 2012-11-28 | 江苏绿利来股份有限公司 | Method for preparing quinclorac hydrochloride |
| CN104585205A (en) * | 2014-12-24 | 2015-05-06 | 广东中迅农科股份有限公司 | Herbicide composition containing metamifop, cyhalofop-butyl and halosulfuron-methyl |
| CN105330649A (en) * | 2015-12-09 | 2016-02-17 | 安徽久易农业股份有限公司 | Preparation method of hingosulfuron-methyl |
| CN105601538A (en) * | 2016-02-02 | 2016-05-25 | 江苏丰山集团股份有限公司 | Preparation method of cyhalofop-butyl |
| CN106035350A (en) * | 2016-05-27 | 2016-10-26 | 创新美兰（合肥）股份有限公司 | Cyhalofop-butyl, metamifop and bentazone compounded dispersible oil suspended agent and preparation method thereof |
| CN106376577A (en) * | 2016-10-26 | 2017-02-08 | 广东中迅农科股份有限公司 | Weeding composition containing metamifop |
| CN106472519A (en) * | 2016-09-28 | 2017-03-08 | 安徽众邦生物工程有限公司 | A kind of rice direct seeding field ternary weeding composition containing cyhalofop-butyl |
| CN107232211A (en) * | 2017-07-14 | 2017-10-10 | 安徽金农康农药检测有限公司 | A kind of penoxsuam is He metamifop compounds dispersible oil-suspending agent and preparation method thereof |
| CN108403886A (en) * | 2018-05-10 | 2018-08-17 | 无锡市人民医院 | A kind of Chinese medicine surgery anesthesia agent production method |
-
2018
- 2018-03-27 CN CN201810256372.9A patent/CN108378057A/en not_active Withdrawn
Patent Citations (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101965837A (en) * | 2010-09-17 | 2011-02-09 | 北京颖新泰康国际贸易有限公司 | Herbicide composition and application thereof |
| CN102113503A (en) * | 2010-12-30 | 2011-07-06 | 苏州富美实植物保护剂有限公司 | Herbicide composite used in paddy field |
| CN102342280A (en) * | 2011-10-26 | 2012-02-08 | 中化蓝天集团有限公司 | Active composition for preventing and eliminating resistant weeds in paddy field and weedicide thereof |
| CN102796043A (en) * | 2012-06-13 | 2012-11-28 | 江苏绿利来股份有限公司 | Method for preparing quinclorac hydrochloride |
| CN104585205A (en) * | 2014-12-24 | 2015-05-06 | 广东中迅农科股份有限公司 | Herbicide composition containing metamifop, cyhalofop-butyl and halosulfuron-methyl |
| CN105330649A (en) * | 2015-12-09 | 2016-02-17 | 安徽久易农业股份有限公司 | Preparation method of hingosulfuron-methyl |
| CN105601538A (en) * | 2016-02-02 | 2016-05-25 | 江苏丰山集团股份有限公司 | Preparation method of cyhalofop-butyl |
| CN106035350A (en) * | 2016-05-27 | 2016-10-26 | 创新美兰（合肥）股份有限公司 | Cyhalofop-butyl, metamifop and bentazone compounded dispersible oil suspended agent and preparation method thereof |
| CN106472519A (en) * | 2016-09-28 | 2017-03-08 | 安徽众邦生物工程有限公司 | A kind of rice direct seeding field ternary weeding composition containing cyhalofop-butyl |
| CN106376577A (en) * | 2016-10-26 | 2017-02-08 | 广东中迅农科股份有限公司 | Weeding composition containing metamifop |
| CN107232211A (en) * | 2017-07-14 | 2017-10-10 | 安徽金农康农药检测有限公司 | A kind of penoxsuam is He metamifop compounds dispersible oil-suspending agent and preparation method thereof |
| CN108403886A (en) * | 2018-05-10 | 2018-08-17 | 无锡市人民医院 | A kind of Chinese medicine surgery anesthesia agent production method |
Non-Patent Citations (3)
| Title |
|---|
| 刘广文等: "《现代农药剂型加工技术》", 31 January 2013, 化学工业出版社 * |
| 时春喜等: "《农药使用技术手册》", 31 January 2009, 金盾出版社 * |
| 郭玉人等: "《农药安全使用手册》", 30 September 2009, 上海科学技术出版社 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109287649A (en) * | 2018-11-01 | 2019-02-01 | 安徽远景作物保护有限公司 | A kind of Herbicidal combinations and its application containing dichloro quinolinic acid |
| CN109479891A (en) * | 2018-11-13 | 2019-03-19 | 安徽远景作物保护有限公司 | A kind of Herbicidal combinations and its application containing halosulfuronmethyl |
| CN109452299A (en) * | 2018-11-19 | 2019-03-12 | 安徽远景作物保护有限公司 | A kind of Herbicidal composition for rice field and its application |
| CN109452299B (en) * | 2018-11-19 | 2022-01-28 | 安徽远景作物保护有限公司 | Paddy field weeding composition and application thereof |
| CN109651140A (en) * | 2018-12-12 | 2019-04-19 | 江苏中旗科技股份有限公司 | A kind of synthetic method of cyhalofop-butyl active compound |
| CN110003051A (en) * | 2019-05-06 | 2019-07-12 | 湖南速博生物技术有限公司 | A kind of preparation method of cyhalofop-butyl standard items |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108378057A (en) | A kind of rice weeding composition of Han metamifops | |
| CN101449675B (en) | Preparation method of herbicide methylated vegetable oil adjuvants | |
| AU2017258911A1 (en) | Aqueous adjuvant-compositions | |
| CN108378043A (en) | A kind of herbicidal composition of Han metamifops and dichloro quinolinic acid | |
| CN105613500A (en) | Plant-growth regulator composition | |
| CN108271796A (en) | A kind of herbicidal composition of penoxsuam and KIH 6127 | |
| CN109362744A (en) | A kind of herbicidal composition containing metamifop and dichloro quinolinic acid | |
| CN110692642A (en) | Dispersible oil suspending agent containing metamifop and quinclorac | |
| CN114213426A (en) | Application of fructus crataegi extract and its compound in preparing herbicide | |
| CA3146587C (en) | Use of dihydroporphin derived from chlorophyll as plant growth regulator | |
| JPS6150922B2 (en) | ||
| CN107467061A (en) | A kind of L glufosinate-ammoniumaqua aquas and preparation method thereof | |
| CN101496515A (en) | Butralin wettable powder | |
| CN109287647A (en) | A kind of herbicide and preparation method thereof containing halosulfuronmethyl | |
| CN107912451A (en) | Herbicide and preparation method using lilac leaf extract as active ingredient | |
| CN109287638A (en) | A kind of rice weeding composition containing metamifop | |
| CN108569973A (en) | A kind of double hydrogen jasmonics（Dialkyl amido）Ester compounds or its salt | |
| CN109221193A (en) | A kind of herbicidal composition and preparation method thereof containing pinoxaden | |
| CN110003270B (en) | Glyphosate dicationic ionic liquid compound and preparation method and application thereof | |
| CN108402063A (en) | A kind of herbicide containing halosulfuronmethyl | |
| CN107212018A (en) | A kind of composition pesticide of suitable drip irrigation | |
| CN102469778A (en) | Cocoalkylpolyamine alkoxylates as agents for high strength herbicide compositions | |
| EP3922620A1 (en) | Process for obtaining a liquid fertilizer for leaves and a liquid fertilizer composition for leaves | |
| CN108271797A (en) | A kind of herbicidal composition and preparation method thereof containing penoxsuam | |
| CN106083780B (en) | N- (2,3- Dihydrobenzofuranes -7- epoxides) alkanol and its preparation method and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WW01 | Invention patent application withdrawn after publication | ||
| WW01 | Invention patent application withdrawn after publication |
Application publication date: 20180810 |