CN105707071B - A kind of pesticidal preparations wetting agent and preparation method thereof and the application in pesticidal preparations - Google Patents
A kind of pesticidal preparations wetting agent and preparation method thereof and the application in pesticidal preparations Download PDFInfo
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- CN105707071B CN105707071B CN201610038828.5A CN201610038828A CN105707071B CN 105707071 B CN105707071 B CN 105707071B CN 201610038828 A CN201610038828 A CN 201610038828A CN 105707071 B CN105707071 B CN 105707071B
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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
- A01N25/30—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 characterised by the surfactants
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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
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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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
- A01N37/36—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 singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
- A01N37/38—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 singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
- A01N37/40—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 singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system having at least one carboxylic group or a thio analogue, or a derivative thereof, and one oxygen or sulfur atom attached to the same aromatic ring system
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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
- 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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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C231/00—Preparation of carboxylic acid amides
- C07C231/02—Preparation of carboxylic acid amides from carboxylic acids or from esters, anhydrides, or halides thereof by reaction with ammonia or amines
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/02—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of sulfonic acids or halides thereof
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
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Abstract
The present invention relates to a kind of insecticides adjuvants, and in particular to a kind of pesticidal preparations wetting agent and preparation method thereof and its application in pesticidal preparations.The preparation method of the pesticidal preparations wetting agent, includes the following steps：Salicylic acid and potassium hydroxide are added in the reactor, triethylene tetramine is added dropwise later, obtains intermediate monoamides, adds dehydrogenation rosin acid in the reactor and obtains intermediate asymmetry bisamide by series reaction；Intermediate asymmetry bisamide and butanone are added in reactor, propane sultone is added dropwise, filters and is simultaneously repeatedly washed with butanone, and recrystallize, in the ethanol solution of alkali and white solid is precipitated, after suction filtration, is dried in vacuo to obtain pesticidal preparations wetting agent.The beneficial effects of the present invention are：Pesticidal preparations wetting agent provided by the invention is asymmetry, bisamide, disulfonate structure, has preferable surface-active, compound property and wettability, improves the absorptivity of pesticide.
Description
Technical field
The present invention relates to a kind of insecticides adjuvants, and in particular to a kind of pesticidal preparations wetting agent and preparation method thereof and its in agriculture
Application in medicine preparation.
Background technology
People have found that many plants, weeds and pest are not easy to be soaked by water and liquid very early, are not easy to adhere to and withhold, are
Because their epidermises are often covered with one layer of hydrophobic wax coat, and composition, shape, thickness are different, same plant different growing stages
Different parts situation is also different, directly affects pesticide supplying effect.Researcher find wax main component be long-chain aliphatic acid,
Alcohol, aldehyde, ester etc. also have other such as cyclic terpene, phenols, sterol even carrotene ingredient in certain plants epicutile wax.
Pesticide wetting agent is to refer to reduce liquid-solid interfacial tension, increases drug containing liquid and (is planted to the process object surface of solids
Object, pest and other) contact, can soak or can accelerate the substance of wet processes.In order to give full play to drug effect, select
Soak the strong wetting and penetrating agent of penetration, it is clear that be very important.Common wetting agent is mainly in pesticidal preparations at present
K12, JFC, NP-10, fast T, azone, organosilicon etc., certain natural products such as lignosulfonates, Tea Saponin etc. are also preferable
Wetting agent.Due to the effect of wetting agent, drug dispersion can be made to increase, preparation stability increases, to be conducive to releasing for drug
It puts, permeate and absorbs, greatly enhance drug effect.But it is not yet reported for the asymmetric Gemini anionic wetting agent of pesticidal preparations design
Road.
Dehydrogenation rosin acid is to be extracted by rosin and obtained, and rosin is a kind of resourceful, reproducible natural resources, it has
The rigid structure of the tricyclic diterpene of strong-hydrophobicity will connect the dehydrogenation rosin acid of strong hydrophilicity group (such as amido bond, sulfonate)
It is introduced into Gemini surface active agent, has not only met surfactant " raw material greenization " requirement, but also provide for its higher value application
New thinking.
Salicylic acid is a kind of small molecule aldehydes matter being widely present in plant, is phenylalanine metabolic pathway
Intermediate product belongs to the derivative of cinnamic acid.Participate in the transpiration of plant, seed is sprouted, is bloomed, is solid, stomata closing, heat production etc.
A variety of physiological and biochemical procedures；It induces plant to generate a variety of physiological characters such as disease-resistant, salt resistance, cold-resistant, may also participate in plant cell line
Plastochondria cyanide-resistant respiration and non-phosphorylating approach improve jasmonic metaboilic level in plant.
Potassium does not form stable compound in plant, and exists in ionic condition, is not yet sent out in plant so far
What incumbent organic matter containing potassium.It can promote photosynthesis, improve the assimilability of carbon dioxide, promote the fortune of photosynthate
It is defeated, promote the synthesis of protein, participates in Premeabilisation of cells adjustment effect, when intracellular potassium concentration is higher, the infiltration of water suction
Gesture also increases therewith, and cell is promoted to absorb moisture from the external world, to pressure potential be caused to change again, cell water-filling is made to expand,
Stomatal movement is adjusted, the activity of kinase promotes metabolism of organic acids, enhances stress resistance of plant, and Na, Ca, N, S are also plant life
Long necessary nutrient.
Invention content
The technical problem to be solved by the present invention is to：In view of the deficiencies of the prior art, it provides a kind of green, environmentally friendly, efficient
The application in pesticidal preparations of pesticidal preparations wetting agent and preparation method thereof and the wetting agent.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：A kind of pesticidal preparations wetting agent is provided,
Structural formula is：
Wherein M is Ca2+、Na+、NH4 +Or K+。
Another technical solution of the present invention is to provide a kind of preparation method of pesticidal preparations wetting agent, is included the following steps：
(1) salicylic acid and potassium hydroxide are added in the reactor, opens stirring, is warming up to 90 DEG C under nitrogen protection, to
Triethylene tetramine is slowly added dropwise in reactor, is added dropwise in 1 hour, 6h is then reacted under 150-160 DEG C of constant temperature, it is cooling
To 25-30 degree, intermediate monoamides is obtained, adds dehydrogenation rosin acid in the reactor, stirring is opened, rises under nitrogen protection
Then temperature reacts 6h to 90 DEG C under 150-160 DEG C of constant temperature, be cooled to 25-30 degree, with 150# solvent naphthas and butanone mixed solvent
Recrystallization 3 times, the volume ratio 1 of the 150# solvent naphthas and butanone:1 is, removes by-product, is dried in 60 DEG C of vacuum drying chamber
To constant weight, white powder i.e. intermediate asymmetry bisamide is obtained；
(2) intermediate asymmetry bisamide made from step (1) and butanone are added in reactor, are warming up to reflux, and
It is vigorously stirred, adds 150# solvent naphthas until solution clarification, at this time at a reflux temperature, propane sulphur is slowly added dropwise to reactor
Lactone, the reaction was continued after 0.5h is added dropwise for 24 hours, and system is cooled to 25-30 degree, filters and is repeatedly washed with butanone, is obtained
White solid powder, then with absolute ethyl alcohol recrystallize 3 times, then with alkali (can be as needed, the alkali using different cations is matched
At comprising Different Nutrient Elements, contain Na, Ca, K, NH4Pesticidal preparations wetting agent salt) ethanol solution in and that white is precipitated is solid
Body, after suction filtration, in 60 DEG C of vacuum drying chambers drying obtain ideal product i.e. pesticidal preparations wetting agent afterwards for 24 hours.
The reaction equation of above-mentioned obtained intermediate monoamides is：
The reaction equation of above-mentioned obtained intermediate double amide is：
The reaction equation of the pesticidal preparations wetting agent of above-mentioned obtained product asymmetry double type is：
Preferably, in the preparation method of above-mentioned pesticidal preparations wetting agent, the potassium hydroxide in the step (1) presses bigcatkin willow
The molar ratio of 1.5% addition of sour mass percent, salicylic acid and triethylene tetramine is 1.0:1.0-1.3, the intermediate list
The molar ratio of amide and dehydrogenation rosin acid is 1.0:1.0-1.1.
Preferably, in the preparation method of above-mentioned pesticidal preparations wetting agent, asymmetric bisamide in the step (2) and
The molar ratio of propane sultone is 1.0:2.0-2.3.
Preferably, in the preparation method of above-mentioned pesticidal preparations wetting agent, alkali is in the step (2)：Sodium hydroxide, hydrogen
Potassium oxide, triethanolamine or limewash.
Another technical solution provided by the invention is：Above-mentioned pesticidal preparations wetting agent answering in preparing pesticidal preparations
With.
Another technical solution provided by the invention is：A kind of emamectin benzoate missible oil preparation, including following weight percent are provided
Group be grouped as：2.3% emamectin benzoate, 10% etoh solvent, 8% emulsifier agriculture breast 600#, 2% above-mentioned gained pesticide
Preparation wetting agent, 1% stabilizer BHT, remaining weight are 150# solvent naphthas.
The beneficial effects of the present invention are：Pesticidal preparations wetting agent provided by the invention is asymmetry, bisamide, disulfonic acid
Salt structure has preferable surface-active, compound property and wettability.
Pesticidal preparations wetting agent of the present invention introduces amide groups, is conducive to the biodegradation of the substance, reduces environmental pollution；Agriculture
Due to the asymmetry of its structure in medicine preparation wetting agent, its excellent wetting permeability is assigned；Pesticidal preparations soak agent molecule
Middle introducing abietyl and salicyl can accelerate cuticula of the active compound by target, and have extremely strong wetting permeability, improve
The absorptivity of pesticide；
Pesticidal preparations wetting agent molecule of the present invention can be made into different salt as needed, if Na, Ca, K are plant lifes
Long necessary nutrient not only promotes the photosynthesis of plant, but also improves the resistance of plant.It is special due to its structure
Property, pesticidal preparations wetting agent is strong at micella ability, cmc values are low, reduces the efficient, with other surfaces activating agent of surface tension
Compatibility is good.
The synthesis changeability of pesticidal preparations wetting agent molecular structure prepared by the present invention is strong, good surface activity, wetting, infiltration
Power is splendid, and surface tension is low.Pesticidal preparations wetting agent preparation method of the present invention is simple, it is easy to operate and be easy to purification, separation；It is former
Expect that source is wide and environmentally friendly, production cost is low, three-waste free pollution.
Specific implementation mode
To explain the technical content, the achieved purpose and the effect of the present invention in detail, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is：The pesticidal preparations wetting agent of the present invention is assigned due to the asymmetry of its structure
Give its excellent wetting permeability；And abietyl and salicyl are introduced in the molecule, cutin of the active compound by target can be accelerated
Layer, and there is extremely strong wetting permeability, improve the absorptivity of pesticide.
Embodiment 1
20.7 grams of salicylic acids and catalyst are added in the 250ml four-hole boiling flasks equipped with condenser pipe, thermometer and blender
Potassium hydroxide (is added) by salicylic acid quality 1.5%, is opened stirring, is warming up to 90 DEG C under nitrogen protection, slow into reactor
Slowly 24.1 grams of triethylene tetramines are added dropwise, is added dropwise in 1 hour, then reacts 6h under 150-160 DEG C of constant temperature, be cooled to
25-30 degree, obtains intermediate monoamides, adds 45 grams of dehydrogenation rosin acids in the reactor, opens stirring, under nitrogen protection
90 DEG C are warming up to, then reacts 6h under 150-160 DEG C of constant temperature, is cooled to 25-30 degree, it is molten with 150# solvent naphthas and butanone mixing
Agent (volume ratio 1:1) it recrystallizes 3 times, removes by-product, dry to constant weight in 60 DEG C of vacuum drying chamber, obtain white powder i.e.
Intermediate asymmetry bisamide of the purity 95% or more.
In the 250ml four-hole boiling flasks equipped with reflux condensing tube, blender, constant pressure funnel and thermometer, in addition
16.5 grams and 60 milliliters butanone solutions of mesosome asymmetry bisamide are warming up to reflux, and are vigorously stirred, and add 150# solvent naphthas
Until solution is clarified, at this time at a reflux temperature, 7.3 grams of propane sultones is slowly added dropwise to reactor, are added dropwise in 0.5h
The reaction was continued afterwards for 24 hours, and system is cooled to 25-30 degree, filters and is repeatedly washed with butanone, obtains white solid matter, then use
Absolute ethyl alcohol recrystallizes 3 times, then in the ethanol solution of sodium hydroxide and precipitation white solid, 60 DEG C of vacuum drying chambers after suction filtration
Middle drying obtains ideal product i.e. pesticidal preparations wetting agent afterwards for 24 hours, and (it is soaked for the pesticidal preparations of the nutrient containing Na
Agent).Pesticidal preparations wetting agent analysis indexes are as follows obtained by the present embodiment：(0.1% aqueous solution) surface tension 28.41mN/m；It oozes
Saturating power (canvas sedimentation) 36 seconds.
Embodiment 2
20.7 grams of salicylic acids and catalyst are added in the 250ml four-hole boiling flasks equipped with condenser pipe, thermometer and blender
Potassium hydroxide (is added) by salicylic acid quality 1.5%, is opened stirring, is warming up to 90 DEG C under nitrogen protection, slow into reactor
Slowly 24.1 grams of triethylene tetramines are added dropwise, is added dropwise in 1 hour, then reacts 6h under 150-160 DEG C of constant temperature, be cooled to
25-30 degree, obtains intermediate monoamides, adds 45 grams of dehydrogenation rosin acids in the reactor, opens stirring, under nitrogen protection
90 DEG C are warming up to, then reacts 6h under 150-160 DEG C of constant temperature, is cooled to 25-30 degree, it is molten with 150# solvent naphthas and butanone mixing
Agent (volume ratio 1:1) it recrystallizes 3 times, removes by-product, dry to constant weight in 60 DEG C of vacuum drying chamber, obtain white powder i.e.
Intermediate asymmetry bisamide of the purity 95% or more.
In the 250ml four-hole boiling flasks equipped with reflux condensing tube, blender, constant pressure funnel and thermometer, in addition
16.5 grams and 60 milliliters butanone solutions of mesosome asymmetry bisamide are warming up to reflux, and are vigorously stirred, and add 150# solvent naphthas
Until solution is clarified, at this time at a reflux temperature, 7.3 grams of propane sultones is slowly added dropwise to reactor, are added dropwise in 0.5h
The reaction was continued afterwards for 24 hours, and system is cooled to 25-30 degree, filters and is repeatedly washed with butanone, obtains white solid matter, then use
Absolute ethyl alcohol recrystallizes 3 times, then in the ethanol solution of potassium hydroxide and precipitation white solid, 60 DEG C of vacuum drying chambers after suction filtration
Middle drying obtains ideal product i.e. pesticidal preparations wetting agent afterwards for 24 hours (it is the pesticidal preparations wetting agent of the nutrient containing K).
Pesticidal preparations wetting agent analysis indexes are as follows obtained by the present embodiment：(0.1% aqueous solution) surface tension 29.36mN/m；Penetration
(canvas sedimentation) 28 seconds.
Embodiment 3
20.7 grams of salicylic acids and catalyst are added in the 250ml four-hole boiling flasks equipped with condenser pipe, thermometer and blender
Potassium hydroxide (is added) by salicylic acid quality 1.5%, is opened stirring, is warming up to 90 DEG C under nitrogen protection, slow into reactor
Slowly 24.1 grams of triethylene tetramines are added dropwise, is added dropwise in 1 hour, then reacts 6h under 150-160 DEG C of constant temperature, be cooled to
25-30 degree, obtains intermediate monoamides, adds 45 grams of dehydrogenation rosin acids in the reactor, opens stirring, under nitrogen protection
90 DEG C are warming up to, then reacts 6h under 150-160 DEG C of constant temperature, is cooled to 25-30 degree, it is molten with 150# solvent naphthas and butanone mixing
Agent (volume ratio 1:1) it recrystallizes 3 times, removes by-product, dry to constant weight in 60 DEG C of vacuum drying chamber, obtain white powder i.e.
Intermediate asymmetry bisamide of the purity 95% or more.
In the 250ml four-hole boiling flasks equipped with reflux condensing tube, blender, constant pressure funnel and thermometer, in addition
16.5 grams and 60 milliliters butanone solutions of mesosome asymmetry bisamide are warming up to reflux, and are vigorously stirred, and add 150# solvent naphthas
Until solution is clarified, at this time at a reflux temperature, 7.3 grams of propane sultones is slowly added dropwise to reactor, are added dropwise in 0.5h
The reaction was continued afterwards for 24 hours, and system is cooled to 25-30 degree, filters and is repeatedly washed with butanone, obtains white solid matter, then use
Absolute ethyl alcohol recrystallizes 3 times, then in triethanolamine ethanol solution and precipitation white solid, after suction filtration in 60 DEG C of vacuum drying chambers
Drying obtains ideal product i.e. pesticidal preparations wetting agent afterwards for 24 hours, and (it is containing NH4 +The pesticidal preparations wetting agent of nutrient).
Pesticidal preparations wetting agent analysis indexes are as follows obtained by the present embodiment：(0.1% aqueous solution) surface tension 29.86mN/m；Penetration
(canvas sedimentation) 42 seconds.
Embodiment 4
20.7 grams of salicylic acids and catalyst are added in the 250ml four-hole boiling flasks equipped with condenser pipe, thermometer and blender
Potassium hydroxide (is added) by salicylic acid quality 1.5%, is opened stirring, is warming up to 90 DEG C under nitrogen protection, slow into reactor
Slowly 24.1 grams of triethylene tetramines are added dropwise, is added dropwise in 1 hour, then reacts 6h under 150-160 DEG C of constant temperature, be cooled to
25-30 degree, obtains intermediate monoamides, adds 45 grams of dehydrogenation rosin acids in the reactor, opens stirring, under nitrogen protection
90 DEG C are warming up to, then reacts 6h under 150-160 DEG C of constant temperature, is cooled to 25-30 degree, it is molten with 150# solvent naphthas and butanone mixing
Agent (volume ratio 1:1) it recrystallizes 3 times, removes by-product, dry to constant weight in 60 DEG C of vacuum drying chamber, obtain white powder i.e.
Intermediate asymmetry bisamide of the purity 95% or more.
In the 250ml four-hole boiling flasks equipped with reflux condensing tube, blender, constant pressure funnel and thermometer, in addition
16.5 grams and 60 milliliters butanone solutions of mesosome asymmetry bisamide are warming up to reflux, and are vigorously stirred, and add 150# solvent naphthas
Until solution is clarified, at this time at a reflux temperature, 7.3 grams of propane sultones is slowly added dropwise to reactor, are added dropwise in 0.5h
The reaction was continued afterwards for 24 hours, and system is cooled to 25-30 degree, filters and is repeatedly washed with butanone, obtains white solid matter, then use
Absolute ethyl alcohol recrystallizes 3 times, then in lime hydrous ethanol solution and white solid being precipitated, dry in 60 DEG C of vacuum drying chambers after suction filtration
It is dry to obtain ideal product i.e. pesticidal preparations wetting agent afterwards for 24 hours (it is the pesticidal preparations wetting agent of the nutrient containing Ca).This
Pesticidal preparations wetting agent analysis indexes are as follows obtained by embodiment：(0.1% aqueous solution) surface tension 28.29mN/m；Penetration (sail
Cloth settles) 32 seconds.
Embodiment 5
20.7 grams of salicylic acids and catalyst are added in the 250ml four-hole boiling flasks equipped with condenser pipe, thermometer and blender
Potassium hydroxide (is added) by salicylic acid quality 1.5%, is opened stirring, is warming up to 90 DEG C under nitrogen protection, slow into reactor
Slowly 28.51 grams of triethylene tetramines are added dropwise, is added dropwise in 1 hour, then reacts 6h under 150-160 DEG C of constant temperature, be cooled to
25-30 degree, obtains intermediate monoamides, adds 49.6 grams of dehydrogenation rosin acids in the reactor, stirring is opened, in nitrogen protection
Under be warming up to 90 DEG C, then react 6h under 150-160 DEG C of constant temperature, be cooled to 25-30 degree, mixed with 150# solvent naphthas and butanone
Solvent (volume ratio 1:1) it recrystallizes 3 times, removes by-product, dry to constant weight in 60 DEG C of vacuum drying chamber, obtain white powder
That is intermediate asymmetry bisamide of the purity 95% or more.
In the 250ml four-hole boiling flasks equipped with reflux condensing tube, blender, constant pressure funnel and thermometer, in addition
16.5 grams and 60 milliliters butanone solutions of mesosome asymmetry bisamide are warming up to reflux, and are vigorously stirred, and add 150# solvent naphthas
Until solution is clarified, at this time at a reflux temperature, 8.4 grams of propane sultones is slowly added dropwise to reactor, are added dropwise in 0.5h
The reaction was continued afterwards for 24 hours, and system is cooled to 25-30 degree, filters and is repeatedly washed with butanone, obtains white solid matter, then use
Absolute ethyl alcohol recrystallizes 3 times, then in sodium hydroxide ethanol solution and precipitation white solid, after suction filtration in 60 DEG C of vacuum drying chambers
It is dry to obtain ideal product i.e. pesticidal preparations wetting agent afterwards for 24 hours (it is the pesticidal preparations wetting agent of the nutrient containing Na).
Pesticidal preparations wetting agent analysis indexes are as follows obtained by the present embodiment：(0.1% aqueous solution) surface tension 27.36mN/m；Penetration
(canvas sedimentation) 29 seconds.
Embodiment 6
A kind of 2.3% emamectin benzoate missible oil preparation comprising the component and content of following weight percent：
Above-mentioned 2.3% emamectin benzoate missible oil preparation performance：Appearance：Homogeneous phase transparent liquid；Emamectin benzoate mass fraction：2.3%；pH
Value：5.0-7.0；Stability of emulsion (200 times) stability：It is qualified；Low-temperature stability：It is qualified；Heat storage stability (54 ± 2 DEG C,
14d) resolution ratio：Less than 2%；Surface tension (0.1% aqueous solution)：31.97mN/m；(0.2% aqueous solution, canvas are heavy for penetration
Drop)：45S.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair
Equivalents made by bright description are applied directly or indirectly in relevant technical field, are similarly included in this hair
In bright scope of patent protection.
Claims (7)
1. a kind of pesticidal preparations wetting agent, which is characterized in that its structural formula is：
Wherein M is Ca2+、Na+、NH4 +Or K+。
2. a kind of preparation method of pesticidal preparations wetting agent, which is characterized in that include the following steps：
(1) salicylic acid and potassium hydroxide are added in the reactor, opens stirring, 90 DEG C is warming up under nitrogen protection, to reaction
Triethylene tetramine is slowly added dropwise in device, is added dropwise in 1 hour, then reacts 6h under 150-160 DEG C of constant temperature, is cooled to
25-30 degree, obtains intermediate monoamides, adds dehydrogenation rosin acid in the reactor, opens stirring, heats up under nitrogen protection
To 90 DEG C, 6h then is reacted under 150-160 DEG C of constant temperature, is cooled to 25-30 degree, with 150# solvent naphthas and butanone mixed solvent weight
The volume ratio of crystallization 3 times, the 150# solvent naphthas and butanone is 1:1, by-product is removed, is dried in 60 DEG C of vacuum drying chamber
Constant weight obtains white powder i.e. intermediate asymmetry bisamide；
(2) intermediate asymmetry bisamide made from step (1) and butanone are added in reactor, are warming up to reflux, and acutely
Stirring adds 150# solvent naphthas until solution clarification, at this time at a reflux temperature, is slowly added dropwise to reactor in propane sulphur
Ester, the reaction was continued after 0.5h is added dropwise for 24 hours, and system is cooled to 25-30 degree, filters and is repeatedly washed with butanone, is obtained white
Then color solid powder is recrystallized 3 times with absolute ethyl alcohol, then in the ethanol solution of alkali and precipitation white solid, after suction filtration, 60
Drying obtains ideal product i.e. pesticidal preparations wetting agent afterwards for 24 hours in DEG C vacuum drying chamber.
3. the preparation method of pesticidal preparations wetting agent according to claim 2, which is characterized in that in the step (1)
Potassium hydroxide is added by the 1.5% of salicylic acid mass percent, and the molar ratio of salicylic acid and triethylene tetramine is 1.0:1.0-
1.3, the molar ratio of the intermediate monoamides and dehydrogenation rosin acid is 1.0:1.0-1.1.
4. the preparation method of pesticidal preparations wetting agent according to claim 2, which is characterized in that in the step (2)
The molar ratio of asymmetric bisamide and propane sultone is 1.0:2.0-2.3.
5. the preparation method of pesticidal preparations wetting agent according to claim 2, which is characterized in that alkali in the step (2)
For：Sodium hydroxide, potassium hydroxide, triethanolamine or limewash.
6. pesticidal preparations wetting agent made from the preparation method of pesticidal preparations wetting agent according to claim 2 is preparing agriculture
Application in medicine preparation.
7. a kind of emamectin benzoate missible oil preparation, which is characterized in that the group including following weight percent is grouped as：2.3% first dimension
Salt, 10% etoh solvent, 8% emulsifier agriculture breast 600#, pesticidal preparations wetting agent described in 2% claim 1,1%
Stabilizer BHT, remaining weight are 150# solvent naphthas.
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