CN106472511A - A kind of synthesis technique of fluoroglycofen-ethyl active compound - Google Patents
A kind of synthesis technique of fluoroglycofen-ethyl active compound Download PDFInfo
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- CN106472511A CN106472511A CN201610781385.9A CN201610781385A CN106472511A CN 106472511 A CN106472511 A CN 106472511A CN 201610781385 A CN201610781385 A CN 201610781385A CN 106472511 A CN106472511 A CN 106472511A
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- fluoroglycofen
- ethyl
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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
- A01N37/00—Biocides, 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
- A01N37/44—Biocides, 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 at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
- A01N37/48—Nitro-carboxylic 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
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- 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)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of synthesis technique of fluoroglycofen-ethyl active compound, including following raw material：Ethyl acetate：5 13 parts；Acifluorfen：20 43 parts；Emulsifying agent：10 15 parts；Methyl oleate：15 19 parts；Piece alkali：38 parts；N,N'-dimethyl-.gamma..gamma.'-dipyridylium：7 10 parts；Phenyl phenol polyoxyethyl ether：8 15 parts；Deionized water：30 50 parts.The present invention by merging ethyl acetate, acifluorfen, emulsifying agent, methyl oleate, piece alkali, N,N'-dimethyl-.gamma..gamma.'-dipyridylium, phenyl phenol polyoxyethyl ether and deionized water by certain ratio, serve chemical reaction, reach dissolving to get up the saving time, drug effect is fast, efficiency high, herbicide can directly volatilize after being absorbed by weeds effect, and weeds are thoroughly killed, and the work giving people brings conveniently.
Description
Technical field
The present invention relates to agricultural herbicide fluoroglycofen-ethyl new synthesis technology field, specially a kind of fluoroglycofen-ethyl active compound
Synthesis technique.
Background technology
Herbicide refers to make weeds that withered medicament thoroughly or selectively occurs, also known as herbicide, in order to eliminating or
One class material of suppression plant growing.Sodium chlorate therein, Borax, arsenate and trichloroacetic acid are for any kind of plant all
Play the role of withered, its effect is affected by herbicide, plant and environmental condition three factor.It is divided into go out natural disposition and selection by effect
Property herbicide, selective herbicide particularly nitrophenol, chlorophenol or carbamic derivant majority is all effective.The world removes
Careless agent development is gradually steady, main development efficiently, the kind of low toxicity, wide spectrum and low consumption, the little disposable place of environmental pollution
Reason agent is increasingly becoming main flow.
Fluoroglycofen-ethyl belongs to diphenyl ether herbicide, and fluoroglycofen-ethyl is one kind of herbicide, and fluoroglycofen-ethyl belongs to hexichol
Ether-derivative herbicides, is that protoporphyrin aoxidizes mould inhibitor, existing herbicide is poorly soluble, and dissolving gets up to lose time, and drug effect is slow,
Efficiency is low, after herbicide is absorbed by weeds, only just plays effect under illumination condition, not thorough to killing of weeds, gives people
Work bring inconvenience.
Content of the invention
It is an object of the invention to provide a kind of synthesis technique of fluoroglycofen-ethyl active compound, there is efficiency high and diffluent
Advantage, to solve the problems, such as that efficiency is low and not readily dissolves.
For achieving the above object, the present invention provides following technical scheme：A kind of synthesis technique of fluoroglycofen-ethyl active compound, bag
Include following raw material：
Ethyl acetate：5-13 part；
Acifluorfen：20-43 part；
Emulsifying agent：10-15 part；
Methyl oleate：15-19 part；
Piece alkali：3-8 part；
N,N'-dimethyl-.gamma..gamma.'-dipyridylium：7-10 part；
Phenyl phenol polyoxyethyl ether：8-15 part；
Deionized water：30-50 part.
Preferably, fluoroglycofen-ethyl active compound includes following raw material:
Ethyl acetate：12 parts；
Acifluorfen：28 parts；
Emulsifying agent：12 parts；
Methyl oleate：17 parts；
Piece alkali：5 parts；
N,N'-dimethyl-.gamma..gamma.'-dipyridylium：10 parts；
Phenyl phenol polyoxyethyl ether：12 parts；
Deionized water：30-50 part.
Preferably, the preparation method of fluoroglycofen-ethyl active compound comprises the following steps:
S1, take out the acifluorfen of 20-43 part, the emulsifying agent of 10-15 part, the methyl oleate of 15-19 part, 3-8 part
Piece alkali, the ethyl acetate of the N,N'-dimethyl-.gamma..gamma.'-dipyridylium of 7-10 part, the phenyl phenol polyoxyethyl ether of 8-15 part and 5-13 part are put in container and are carried out
Polishing；
S2, the deionized water of certain component is heated, be heated to 25-30 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stirring with
Heating, during controlling reaction temperature 70-80 DEG C, carries out precipitation, cleaning, filter pressing and air-dried obtains fluoroglycofen after reaction 3-4 hour
Ether active compound.
Preferably, fluoroglycofen-ethyl active compound has used sanding apparatus in polishing, and sanding apparatus are medicinal material pulverizer.
Preferably, fluoroglycofen-ethyl active compound preparation after the completion of can in the woods, vegetable garden, orchard, garden, and peach tree, willow,
Chinese cabbage, Herba Spinaciae and Caulis Sacchari sinensis, prior to seeding, after planting or the mid-term of plant growing and later stage are diluted except roguing to it
Grass, the growth of crops is sprayed in protection.
Compared with prior art, the invention has the advantages that：
1st, the present invention passes through ethyl acetate, acifluorfen, emulsifying agent, methyl oleate, piece alkali, N,N'-dimethyl-.gamma..gamma.'-dipyridylium, phenyl phenol
Polyoxyethyl ether and deionized water are merged by certain ratio, serve chemical reaction, have reached dissolving and have got up to save
Make an appointment, drug effect is fast, efficiency high, herbicide can directly volatilize after being absorbed by weeds effect, weeds are thoroughly killed, gives people
Work brings conveniently.
2nd, the present invention, strong applicability, it is easy to promote the use of.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical solution of the present invention is clearly and completely described it is clear that being retouched
The embodiment stated is only a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, this
The every other embodiment that field those of ordinary skill is obtained under the premise of not making creative work, broadly falls into the present invention
The scope of protection.
Embodiment one
A kind of synthesis technique of fluoroglycofen-ethyl active compound comprises the following steps：
S1, take out the acifluorfen of 20-43 part, the emulsifying agent of 10-15 part, the methyl oleate of 15-19 part, 3-8 part
Piece alkali, the ethyl acetate of the N,N'-dimethyl-.gamma..gamma.'-dipyridylium of 7-10 part, the phenyl phenol polyoxyethyl ether of 8-15 part and 5-13 part are put in container and are carried out
Pulverize；
S2, the deionized water of certain component is heated, be heated to 25-30 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stirring with
Heating, during controlling reaction temperature 70-80 DEG C, carries out precipitation, cleaning, filter pressing and air-dried obtains fluoroglycofen after reaction 3-4 hour
Ether active compound.
Embodiment two
A kind of synthesis technique of fluoroglycofen-ethyl active compound comprises the following steps：
S1, take out 21 parts acifluorfen, 11 parts of emulsifying agent, 16 parts of methyl oleate, 4 parts of piece alkali, the hundred of 7 parts
Careless withered, 8 parts of phenyl phenol polyoxyethyl ether and 5 parts of ethyl acetate are put in container and are pulverized；
S2, the deionized water of certain component is heated, be heated to 25 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stirring with
Heating, during 70 DEG C of controlling reaction temperature, reaction carries out precipitation, cleaning, filter pressing after 3 hours and air-dried to obtain fluoroglycofen-ethyl former
Medicine.
Embodiment three
A kind of synthesis technique of fluoroglycofen-ethyl active compound comprises the following steps：
S1, take out 22 parts acifluorfen, 12 parts of emulsifying agent, 16 parts of methyl oleate, 4 parts of piece alkali, the hundred of 8 parts
Careless withered, 9 parts of phenyl phenol polyoxyethyl ether and 6 parts of ethyl acetate are put in container and are pulverized；
S2, the deionized water of certain component is heated, be heated to 25 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stirring with
Heating, during 71 DEG C of controlling reaction temperature, reaction carries out precipitation, cleaning, filter pressing after 3.1 hours and air-dried to obtain fluoroglycofen-ethyl former
Medicine.
Example IV
A kind of synthesis technique of fluoroglycofen-ethyl active compound comprises the following steps：
S1, take out 23 parts acifluorfen, 13 parts of emulsifying agent, 16 parts of methyl oleate, 4 parts of piece alkali, the hundred of 8 parts
Careless withered, 9 parts of phenyl phenol polyoxyethyl ether and 6 parts of ethyl acetate are put in container and are pulverized；
S2, the deionized water of certain component is heated, be heated to 26 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stirring with
Heating, during 72 DEG C of controlling reaction temperature, reaction carries out precipitation, cleaning, filter pressing after 3.1 hours and air-dried to obtain fluoroglycofen-ethyl former
Medicine.
Embodiment five
A kind of synthesis technique of fluoroglycofen-ethyl active compound comprises the following steps：
S1, take out 24 parts acifluorfen, 13 parts of emulsifying agent, 16 parts of methyl oleate, 4 parts of piece alkali, the hundred of 8 parts
Careless withered, 9 parts of phenyl phenol polyoxyethyl ether and 6 parts of ethyl acetate are put in container and are pulverized；
S2, the deionized water of certain component is heated, be heated to 26 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stirring with
Heating, during 72 DEG C of controlling reaction temperature, reaction carries out precipitation, cleaning, filter pressing after 3.1 hours and air-dried to obtain fluoroglycofen-ethyl former
Medicine.
Embodiment six
A kind of synthesis technique of fluoroglycofen-ethyl active compound comprises the following steps：
S1, take out 25 parts acifluorfen, 14 parts of emulsifying agent, 16 parts of methyl oleate, 4 parts of piece alkali, the hundred of 8 parts
Careless withered, 9 parts of phenyl phenol polyoxyethyl ether and 6 parts of ethyl acetate are put in container and are pulverized；
S2, the deionized water of certain component is heated, be heated to 26 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stirring with
Heating, during 72 DEG C of controlling reaction temperature, reaction carries out precipitation, cleaning, filter pressing after 3.1 hours and air-dried to obtain fluoroglycofen-ethyl former
Medicine.
Embodiment seven
A kind of synthesis technique of fluoroglycofen-ethyl active compound comprises the following steps：
S1, take out 30 parts acifluorfen, 14 parts of emulsifying agent, 17 parts of methyl oleate, 4 parts of piece alkali, the hundred of 8 parts
Careless withered, 9 parts of phenyl phenol polyoxyethyl ether and 6 parts of ethyl acetate are put in container and are pulverized；
S2, the deionized water of certain component is heated, be heated to 27 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stirring with
Heating, during 73 DEG C of controlling reaction temperature, reaction carries out precipitation, cleaning, filter pressing after 3.3 hours and air-dried to obtain fluoroglycofen-ethyl former
Medicine.
Embodiment eight
A kind of synthesis technique of fluoroglycofen-ethyl active compound comprises the following steps：
S1, take out 35 parts acifluorfen, 14 parts of emulsifying agent, 18 parts of methyl oleate, 6 parts of piece alkali, the hundred of 9 parts
Careless withered, 13 parts of phenyl phenol polyoxyethyl ether and 10 parts of ethyl acetate are put in container and are pulverized；
S2, the deionized water of certain component is heated, be heated to 29 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stirring with
Heating, during 78 DEG C of controlling reaction temperature, reaction carries out precipitation, cleaning, filter pressing after 3.5 hours and air-dried to obtain fluoroglycofen-ethyl former
Medicine.
Embodiment nine
A kind of synthesis technique of fluoroglycofen-ethyl active compound comprises the following steps：
S1, take out 40 parts acifluorfen, 15 parts of emulsifying agent, 18 parts of methyl oleate, 7 parts of piece alkali, the hundred of 9 parts
Careless withered, 14 parts of phenyl phenol polyoxyethyl ether and 12 parts of ethyl acetate are put in container and are pulverized；
S2, the deionized water of certain component is heated, be heated to 29 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stirring with
Heating, during 79 DEG C of controlling reaction temperature, reaction carries out precipitation, cleaning, filter pressing after 3.8 hours and air-dried to obtain fluoroglycofen-ethyl former
Medicine.
Embodiment ten
A kind of synthesis technique of fluoroglycofen-ethyl active compound comprises the following steps：
S1, take out 43 parts acifluorfen, 15 parts of emulsifying agent, 19 parts of methyl oleate, 8 parts of piece alkali, 10 parts
N,N'-dimethyl-.gamma..gamma.'-dipyridylium, 15 parts of phenyl phenol polyoxyethyl ether and 13 parts of ethyl acetate are put in container and are pulverized；
S2, the deionized water of certain component is heated, be heated to 30 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stir
And heating, during 80 DEG C of controlling reaction temperature, reaction carries out precipitation, cleaning, filter pressing after 4 hours and air-dried to obtain fluoroglycofen-ethyl former
Medicine.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, permissible
Understand and can carry out multiple changes, modification, replacement to these embodiments without departing from the principles and spirit of the present invention
And modification, the scope of the present invention be defined by the appended.
Claims (5)
1. a kind of synthesis technique of fluoroglycofen-ethyl active compound it is characterised in that：Including following raw material：
Ethyl acetate：5-13 part；
Acifluorfen：20-43 part；
Emulsifying agent：10-15 part；
Methyl oleate：15-19 part；
Piece alkali：3-8 part；
N,N'-dimethyl-.gamma..gamma.'-dipyridylium：7-10 part；
Phenyl phenol polyoxyethyl ether：8-15 part；
Deionized water：30-50 part.
2. a kind of fluoroglycofen-ethyl active compound according to claim 1 synthesis technique it is characterised in that：Including following former
Material:
Ethyl acetate：12 parts；
Acifluorfen：28 parts；
Emulsifying agent：12 parts；
Methyl oleate：17 parts；
Piece alkali：5 parts；
N,N'-dimethyl-.gamma..gamma.'-dipyridylium：10 parts；
Phenyl phenol polyoxyethyl ether：12 parts；
Deionized water：35 parts.
3. a kind of fluoroglycofen-ethyl active compound according to claim 1 synthesis technique it is characterised in that：Its preparation method bag
Include following steps:
S1, take out the acifluorfen of 20-43 part, the emulsifying agent of 10-15 part, the methyl oleate of 15-19 part, the piece alkali of 3-8 part,
The ethyl acetate of the N,N'-dimethyl-.gamma..gamma.'-dipyridylium of 7-10 part, the phenyl phenol polyoxyethyl ether of 8-15 part and 5-13 part is put in container and is pulverized；
S2, the deionized water of certain component is heated, be heated to 25-30 DEG C；
S3, by heating after deionized water pour in container, be stirred with medicine container within, and continue stirring and add
Heat, during controlling reaction temperature 70-80 DEG C, carries out precipitation, cleaning, filter pressing and air-dried obtains fluoroglycofen-ethyl after reaction 3-4 hour
Active compound.
4. a kind of fluoroglycofen-ethyl active compound according to claim 1 synthesis technique it is characterised in that：Described pulverizing is used
Reducing mechanism, reducing mechanism is medicinal material pulverizer.
5. a kind of fluoroglycofen-ethyl active compound according to claim 1 synthesis technique it is characterised in that：Described raw material preparation
After the completion of can be in the woods, vegetable garden, orchard, garden, and peach tree, willow, Chinese cabbage, Herba Spinaciae and Caulis Sacchari sinensis, prior to seeding, after planting or
The mid-term of person's plant growing and later stage are diluted removing weeds to it, and the growth of crops is sprayed in protection.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108739819A (en) * | 2018-05-17 | 2018-11-06 | 赫章县山地高效农业科技有限公司 | A kind of tuber of pinellia field postemergence weed control agent composition and application method |
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| CN108739819A (en) * | 2018-05-17 | 2018-11-06 | 赫章县山地高效农业科技有限公司 | A kind of tuber of pinellia field postemergence weed control agent composition and application method |
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Application publication date: 20170308 |