CN105707071A - Wetting agent for pesticide preparations, method for preparing wetting agent and application of wetting agent to pesticide preparations - Google Patents
Wetting agent for pesticide preparations, method for preparing wetting agent and application of wetting agent to pesticide preparations Download PDFInfo
- Publication number
- CN105707071A CN105707071A CN201610038828.5A CN201610038828A CN105707071A CN 105707071 A CN105707071 A CN 105707071A CN 201610038828 A CN201610038828 A CN 201610038828A CN 105707071 A CN105707071 A CN 105707071A
- Authority
- CN
- China
- Prior art keywords
- wetting agent
- reactor
- pesticidal preparations
- butanone
- preparation
- 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.)
- Granted
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
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Environmental Sciences (AREA)
- Dentistry (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Plant Pathology (AREA)
- Pest Control & Pesticides (AREA)
- Agronomy & Crop Science (AREA)
- Toxicology (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a pesticide adjuvant, in particular to a wetting agent for pesticide preparations, a method for preparing the wetting agent and application of the wetting agent to the pesticide preparations. The method for preparing the wetting agent for the pesticide preparations includes steps of adding salicylic acid and potassium hydroxide into a reactor, then adding triethylene tetramine into the reactor drop by drop to obtain intermediate monoamide, adding dehydroabietic acid into the reactor and carrying out a series of reaction to obtain intermediate asymmetric bisamides; adding the intermediate asymmetric bisamides and butanone into the reactor, adding propane suhone into the reactor drop by drop, carrying out suction filtration, repeatedly washing substances in the reactor by the aid of butanone, re-crystallizing the substances, neutralizing the substances by the aid of ethanol solution of alkali, separating white solid from the substances, carrying out suction filtration and drying the white solid under the vacuum condition to obtain the wetting agent for the pesticide preparations. The wetting agent, the method and the application have the advantages that the wetting agent for the pesticide preparations is of an asymmetric structure with the bisamides and bis-sulfonate and is excellent in surface activity, compound property and wetting property, and the pesticide absorption rate can be increased.
Description
Technical field
The present invention relates to a kind of insecticides adjuvant, be specifically related to a kind of pesticidal preparations wetting agent and preparation method thereof and its application in pesticidal preparations.
Background technology
People find very early, many plants, weeds and insect are not easily by water and medicinal liquid moistening, not easily adhere to and hold and stay, it is because they epidermises and is often covered with one layer of hydrophobic wax coat, and form, shape, thickness different, same plant different growing stages different parts situation is also different, directly affects pesticide supplying effect.Researcher find waxiness be mainly composed of the fatty acid of long-chain, alcohol, aldehyde, ester etc., in certain plants epicutile wax also have other such as compositions such as cyclic terpene, phenols, sterin even carotene.
Pesticide wetting agent refers to reduce liquid-solid interfacial tension, increases the contact to processing the object surface of solids (plant, insect and other) of the pastille liquid so that it is can moistening or can accelerate the material of wet processes.In order to give full play to drug effect, the wetting and penetrating agent that selective wetting penetration is strong, it is clear that be very important.Wetting agent conventional in current pesticidal preparations is mainly K12, JFC, NP-10, fast T, azone, organosilicon etc., and some natural product such as lignosulfonates, tea saponin etc. are also good wetting agent.Due to the effect of wetting agent, drug dispersion can being made to increase, preparation stability increases, thus being conducive to the release of medicine, infiltration and absorption, greatly strengthens drug effect.But the asymmetric Gemini anionic wetting agent for pesticidal preparations design is not yet reported.
Dehydrogenation rosin acid is to be extracted by Colophonium and obtain, Colophonium is a kind of aboundresources, reproducible natural resources, it has the rigid structure of the tricyclic diterpene of strong-hydrophobicity, the dehydrogenation rosin acid that will connect strong hydrophilicity group (such as amido link, sulfonate etc.) introduces in Gemini surface active agent, both meet surfactant " raw material greenization " requirement, provide new thinking for its higher value application again.
Salicylic acid is a kind of small molecule aldehydes matter being widely present in plant, is the intermediate product of phenylalanine metabolic pathway, belongs to the derivant of cinnamic acid.The transpiration of involved in plant, seed germination, bloom, solid, stomatal closure, the multiple physiological and biochemical procedure such as heat production；Induction plant produces salt disease-resistant, anti-, the multiple physiological character such as cold-resistant, may also participate in plant cell mitochondrion cyanide-resistant respiration and non-phosphorylating approach, improves jasmonic metaboilic level in plant.
Potassium is formed without stable compound in plant, and exists in ionic condition, not yet finds any Organic substance containing potassium so far in plant.It can promote photosynthesis, improve the assimilation ratio of carbon dioxide, promote the transport of photosynthate, promote the synthesis of protein, participate in Premeabilisation of cells adjustment effect, when in cell, potassium concentration is higher, the osmotic potential of its water suction also increases therewith, and promotes that cell absorbs moisture from the external world, thus pressure potential can be caused again to change, cell water-filling is made to expand, regulate stomatal movement, the activity of kinase, promote metabolism of organic acids, strengthen stress resistance of plant, and Na, Ca, N, S are also the necessary nutrients of plant growing.
Summary of the invention
The technical problem to be solved is: for the deficiencies in the prior art, it is provided that a kind of green, environmental protection, efficient pesticidal preparations wetting agent and preparation method thereof, and the application that this wetting agent is in pesticidal preparations.
In order to solve above-mentioned technical problem, the technical solution used in the present invention is: providing a kind of pesticidal preparations wetting agent, its structural formula is:
Wherein M is Ca2+、Na+、NH4 +Or K+。
Another technical scheme of the present invention is the preparation method providing a kind of pesticidal preparations wetting agent, comprises the following steps:
(1) salicylic acid and potassium hydroxide are added in the reactor, open stirring, it is warmed up to 90 DEG C under nitrogen protection, triethylene tetramine is slowly dripped in reactor, dropwised in 1 hour, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, obtain intermediate monoamides, add dehydrogenation rosin acid in the reactor, open stirring, it is warmed up to 90 DEG C under nitrogen protection, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, with 150# solvent naphtha and butanone mixed solvent recrystallization 3 times, the volume ratio 1:1 of described 150# solvent naphtha and butanone is, remove by-product, the vacuum drying oven of 60 DEG C dries to constant weight, obtain white powder and the asymmetric bisamide of intermediate；
(2) the asymmetric bisamide of intermediate step (1) prepared and butanone add in reactor, it is warming up to backflow, and be stirred vigorously, add 150# solvent naphtha until solution is clarified, now at a reflux temperature, propane sultone is slowly dripped to reactor, reaction 24h is continued after 0.5h dropwises, system is cooled to 25-30 degree, sucking filtration also repeatedly washs with butanone, obtain white solid powder, then dehydrated alcohol recrystallization is used 3 times, again (can be as required with alkali, use different cationic alkali to be made into and comprise Different Nutrient Elements, containing Na, Ca, K, NH4Pesticidal preparations wetting agent salt) alcoholic solution in and precipitate out white solid, after sucking filtration, 60 DEG C of vacuum drying ovens obtain ideal product and pesticidal preparations wetting agent after dry 24h.
The reaction equation of above-mentioned prepared intermediate monoamides is:
The reaction equation of above-mentioned prepared intermediate double amide is:
The reaction equation of the pesticidal preparations wetting agent of the above-mentioned asymmetric double type of prepared product is:
Preferably, in the preparation method of above-mentioned pesticidal preparations wetting agent, potassium hydroxide in described step (1) presses 1.5% interpolation of salicylic acid mass percent, the mol ratio of salicylic acid and triethylene tetramine is 1.0:1.0-1.3, and the mol ratio of described intermediate monoamides 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 and the mol ratio of propane sultone in described step (2) are 1.0:2.0-2.3.
Preferably, in the preparation method of above-mentioned pesticidal preparations wetting agent, in described step (2), alkali is: sodium hydroxide, potassium hydroxide, triethanolamine or lime water.
Another technical scheme provided by the invention is: the application in preparing pesticidal preparations of the above-mentioned pesticidal preparations wetting agent.
Another technical scheme provided by the invention is: provide a kind of emamectin benzoate missible oil preparation, component including following percetage by weight forms: the emamectin benzoate of 2.3%, the etoh solvent of 10%, the emulsifying agent agriculture breast 600# of 8%, the above-mentioned gained pesticidal preparations wetting agent of 2%, the stabilizer BHT of 1%, residuals weight is 150# solvent naphtha.
The beneficial effects of the present invention is: pesticidal preparations wetting agent provided by the invention is asymmetric, bisamide, disulfonate structure, has good surface activity, compound property and wettability.
Pesticidal preparations wetting agent of the present invention introduces amide groups, is conducive to the biodegradation of this material, reduces environmental pollution；Due to the unsymmetry of its structure in pesticidal preparations wetting agent, give the wetting permeability of its excellence；Pesticidal preparations wetting agent molecule introduces abietyl and salicyl, it is possible to accelerate the former medicine horny layer by target, and there is extremely strong wetting permeability, improve the absorbance of pesticide；
Pesticidal preparations wetting agent molecule of the present invention can be made into different salt as required, is all the necessary nutrient of plant growing such as Na, Ca, K, not only promotes the photosynthesis of plant, and improves the resistance of plant.Due to the particularity of its structure, pesticidal preparations wetting agent becomes that micelle ability is strong, cmc value is low, the compatibility that reduces capillary efficiency height and other surfactants is good.
The synthesis transmutability of pesticidal preparations wetting agent molecular structure prepared by the present invention is strong, good surface activity, and moistening, penetration are splendid, and surface tension is low.Pesticidal preparations wetting agent preparation method of the present invention is simple, easy and simple to handle and be prone to purify, separate；Raw material sources are wide and environmental protection, and production cost is low, three-waste free pollution.
Detailed description of the invention
By describing the technology contents of the present invention in detail, being realized purpose and effect, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is in that: the pesticidal preparations wetting agent of the present invention, due to the unsymmetry of its structure, gives the wetting permeability of its excellence；And introduce abietyl and salicyl in the molecule, it is possible to accelerate the former medicine horny layer by target, and there is extremely strong wetting permeability, improve the absorbance of pesticide.
Embodiment 1
Equipped with condensing tube, the 250ml four-hole boiling flask of thermometer and agitator adds 20.7 grams of salicylic acid and catalyst potassium hydroxide (adding by salicylic acid quality 1.5%), open stirring, it is warmed up to 90 DEG C under nitrogen protection, 24.1 grams of triethylene tetramines are slowly dripped in reactor, dropwised in 1 hour, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, obtain intermediate monoamides, add 45 grams of dehydrogenation rosin acid in the reactor, open stirring, it is warmed up to 90 DEG C under nitrogen protection, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, with 150# solvent naphtha and butanone mixed solvent (volume ratio 1:1) recrystallization 3 times, remove by-product, the vacuum drying oven of 60 DEG C dries to constant weight, obtain white powder and the purity asymmetric bisamide of the intermediate more than 95%.
Equipped with reflux condensing tube, agitator, in the 250ml four-hole boiling flask of constant pressure funnel and thermometer, add 16.5 grams and 60 milliliters butanone solutions of the asymmetric bisamide of intermediate and be warming up to backflow, and be stirred vigorously, add 150# solvent naphtha until solution is clarified, now at a reflux temperature, 7.3 grams of propane sultone are slowly dripped to reactor, reaction 24h is continued after 0.5h dropwises, system is cooled to 25-30 degree, sucking filtration also repeatedly washs with butanone, obtain white solid matter, then dehydrated alcohol recrystallization is used 3 times, use again in the alcoholic solution of sodium hydroxide and precipitate out white solid, after sucking filtration, 60 DEG C of vacuum drying ovens obtain ideal product and pesticidal preparations wetting agent (it is the pesticidal preparations wetting agent containing Na nutrient) after dry 24h.The present embodiment gained pesticidal preparations wetting agent analysis indexes is as follows: (0.1% aqueous solution) surface tension 28.41mN/m；Penetration (canvas sedimentation) 36 seconds.
Embodiment 2
Equipped with condensing tube, the 250ml four-hole boiling flask of thermometer and agitator adds 20.7 grams of salicylic acid and catalyst potassium hydroxide (adding by salicylic acid quality 1.5%), open stirring, it is warmed up to 90 DEG C under nitrogen protection, 24.1 grams of triethylene tetramines are slowly dripped in reactor, dropwised in 1 hour, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, obtain intermediate monoamides, add 45 grams of dehydrogenation rosin acid in the reactor, open stirring, it is warmed up to 90 DEG C under nitrogen protection, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, with 150# solvent naphtha and butanone mixed solvent (volume ratio 1:1) recrystallization 3 times, remove by-product, the vacuum drying oven of 60 DEG C dries to constant weight, obtain white powder and the purity asymmetric bisamide of the intermediate more than 95%.
Equipped with reflux condensing tube, agitator, in the 250ml four-hole boiling flask of constant pressure funnel and thermometer, add 16.5 grams and 60 milliliters butanone solutions of the asymmetric bisamide of intermediate and be warming up to backflow, and be stirred vigorously, add 150# solvent naphtha until solution is clarified, now at a reflux temperature, 7.3 grams of propane sultone are slowly dripped to reactor, reaction 24h is continued after 0.5h dropwises, system is cooled to 25-30 degree, sucking filtration also repeatedly washs with butanone, obtain white solid matter, then dehydrated alcohol recrystallization is used 3 times, use again in the alcoholic solution of potassium hydroxide and precipitate out white solid, after sucking filtration, 60 DEG C of vacuum drying ovens obtain ideal product and pesticidal preparations wetting agent (it is the pesticidal preparations wetting agent containing K nutrient) after dry 24h.The present embodiment gained pesticidal preparations wetting agent analysis indexes is as follows: (0.1% aqueous solution) surface tension 29.36mN/m；Penetration (canvas sedimentation) 28 seconds.
Embodiment 3
Equipped with condensing tube, the 250ml four-hole boiling flask of thermometer and agitator adds 20.7 grams of salicylic acid and catalyst potassium hydroxide (adding by salicylic acid quality 1.5%), open stirring, it is warmed up to 90 DEG C under nitrogen protection, 24.1 grams of triethylene tetramines are slowly dripped in reactor, dropwised in 1 hour, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, obtain intermediate monoamides, add 45 grams of dehydrogenation rosin acid in the reactor, open stirring, it is warmed up to 90 DEG C under nitrogen protection, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, with 150# solvent naphtha and butanone mixed solvent (volume ratio 1:1) recrystallization 3 times, remove by-product, the vacuum drying oven of 60 DEG C dries to constant weight, obtain white powder and the purity asymmetric bisamide of the intermediate more than 95%.
Equipped with reflux condensing tube, agitator, in the 250ml four-hole boiling flask of constant pressure funnel and thermometer, add 16.5 grams and 60 milliliters butanone solutions of the asymmetric bisamide of intermediate and be warming up to backflow, and be stirred vigorously, add 150# solvent naphtha until solution is clarified, now at a reflux temperature, 7.3 grams of propane sultone are slowly dripped to reactor, reaction 24h is continued after 0.5h dropwises, system is cooled to 25-30 degree, sucking filtration also repeatedly washs with butanone, obtain white solid matter, then dehydrated alcohol recrystallization is used 3 times, use again in triethanolamine alcoholic solution and precipitate out white solid, (it is for containing NH to obtain ideal product and pesticidal preparations wetting agent after sucking filtration in 60 DEG C of vacuum drying ovens after dry 24h4 +The pesticidal preparations wetting agent of nutrient).The present embodiment gained pesticidal preparations wetting agent analysis indexes is as follows: (0.1% aqueous solution) surface tension 29.86mN/m；Penetration (canvas sedimentation) 42 seconds.
Embodiment 4
Equipped with condensing tube, the 250ml four-hole boiling flask of thermometer and agitator adds 20.7 grams of salicylic acid and catalyst potassium hydroxide (adding by salicylic acid quality 1.5%), open stirring, it is warmed up to 90 DEG C under nitrogen protection, 24.1 grams of triethylene tetramines are slowly dripped in reactor, dropwised in 1 hour, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, obtain intermediate monoamides, add 45 grams of dehydrogenation rosin acid in the reactor, open stirring, it is warmed up to 90 DEG C under nitrogen protection, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, with 150# solvent naphtha and butanone mixed solvent (volume ratio 1:1) recrystallization 3 times, remove by-product, the vacuum drying oven of 60 DEG C dries to constant weight, obtain white powder and the purity asymmetric bisamide of the intermediate more than 95%.
Equipped with reflux condensing tube, agitator, in the 250ml four-hole boiling flask of constant pressure funnel and thermometer, add 16.5 grams and 60 milliliters butanone solutions of the asymmetric bisamide of intermediate and be warming up to backflow, and be stirred vigorously, add 150# solvent naphtha until solution is clarified, now at a reflux temperature, 7.3 grams of propane sultone are slowly dripped to reactor, reaction 24h is continued after 0.5h dropwises, system is cooled to 25-30 degree, sucking filtration also repeatedly washs with butanone, obtain white solid matter, then dehydrated alcohol recrystallization is used 3 times, use again in lime water alcoholic solution and precipitate out white solid, after sucking filtration, 60 DEG C of vacuum drying ovens obtain ideal product and pesticidal preparations wetting agent (it is the pesticidal preparations wetting agent containing Ca nutrient) after dry 24h.The present embodiment gained pesticidal preparations wetting agent analysis indexes is as follows: (0.1% aqueous solution) surface tension 28.29mN/m；Penetration (canvas sedimentation) 32 seconds.
Embodiment 5
Equipped with condensing tube, the 250ml four-hole boiling flask of thermometer and agitator adds 20.7 grams of salicylic acid and catalyst potassium hydroxide (adding by salicylic acid quality 1.5%), open stirring, it is warmed up to 90 DEG C under nitrogen protection, 28.51 grams of triethylene tetramines are slowly dripped in reactor, dropwised in 1 hour, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, obtain intermediate monoamides, add 49.6 grams of dehydrogenation rosin acid in the reactor, open stirring, it is warmed up to 90 DEG C under nitrogen protection, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, with 150# solvent naphtha and butanone mixed solvent (volume ratio 1:1) recrystallization 3 times, remove by-product, the vacuum drying oven of 60 DEG C dries to constant weight, obtain white powder and the purity asymmetric bisamide of the intermediate more than 95%.
Equipped with reflux condensing tube, agitator, in the 250ml four-hole boiling flask of constant pressure funnel and thermometer, add 16.5 grams and 60 milliliters butanone solutions of the asymmetric bisamide of intermediate and be warming up to backflow, and be stirred vigorously, add 150# solvent naphtha until solution is clarified, now at a reflux temperature, 8.4 grams of propane sultone are slowly dripped to reactor, reaction 24h is continued after 0.5h dropwises, system is cooled to 25-30 degree, sucking filtration also repeatedly washs with butanone, obtain white solid matter, then dehydrated alcohol recrystallization is used 3 times, use again in sodium hydroxide alcoholic solution and precipitate out white solid, after sucking filtration, 60 DEG C of vacuum drying ovens obtain ideal product and pesticidal preparations wetting agent (it is the pesticidal preparations wetting agent containing Na nutrient) after dry 24h.The present embodiment gained pesticidal preparations wetting agent analysis indexes is as follows: (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, it component including following percetage by weight and content:
Above-mentioned 2.3% emamectin benzoate missible oil preparation performance: outward appearance: homogeneous phase transparent liquid；Emamectin benzoate mass fraction: 2.3%；PH value: 5.0-7.0；Stability of emulsion (200 times) stability: qualified；Low-temperature stability: qualified；Heat storage stability (54 ± 2 DEG C, 14d) resolution ratio: less than 2%；Surface tension (0.1% aqueous solution): 31.97mN/m；Penetration (0.2% aqueous solution, canvas settles): 45S.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalents utilizing description of the present invention to make, or directly or indirectly it is used in relevant technical field, all in like manner include in the scope of patent protection of the present invention.
Claims (7)
1. a pesticidal preparations wetting agent, it is characterised in that its structural formula is:
Wherein M is Ca2+、Na+、NH4 +Or K+。
2. the preparation method of a pesticidal preparations wetting agent, it is characterised in that comprise the following steps:
(1) salicylic acid and potassium hydroxide are added in the reactor, open stirring, it is warmed up to 90 DEG C under nitrogen protection, triethylene tetramine is slowly dripped in reactor, dropwised in 1 hour, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, obtain intermediate monoamides, add dehydrogenation rosin acid in the reactor, open stirring, it is warmed up to 90 DEG C under nitrogen protection, then under 150-160 DEG C of constant temperature, react 6h, it is cooled to 25-30 degree, with 150# solvent naphtha and butanone mixed solvent recrystallization 3 times, the volume ratio 1:1 of described 150# solvent naphtha and butanone is, remove by-product, the vacuum drying oven of 60 DEG C dries to constant weight, obtain white powder and the asymmetric bisamide of intermediate；
(2) the asymmetric bisamide of intermediate step (1) prepared and butanone add in reactor, it is warming up to backflow, and be stirred vigorously, add 150# solvent naphtha until solution is clarified, now at a reflux temperature, propane sultone is slowly dripped to reactor, reaction 24h is continued after 0.5h dropwises, system is cooled to 25-30 degree, sucking filtration also repeatedly washs with butanone, obtain white solid powder, then dehydrated alcohol recrystallization is used 3 times, use again in the alcoholic solution of alkali and precipitate out white solid, after sucking filtration, 60 DEG C of vacuum drying ovens obtain ideal product and pesticidal preparations wetting agent after dry 24h.
3. the preparation method of pesticidal preparations wetting agent according to claim 2, it is characterized in that, potassium hydroxide in described step (1) presses 1.5% interpolation of salicylic acid mass percent, the mol ratio of salicylic acid and triethylene tetramine is 1.0:1.0-1.3, and the mol ratio of described 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, it is characterised in that asymmetric bisamide and the mol ratio of propane sultone in described step (2) are 1.0:2.0-2.3.
5. the preparation method of pesticidal preparations wetting agent according to claim 2, it is characterised in that in described step (2), alkali is: sodium hydroxide, potassium hydroxide, triethanolamine or lime water.
6. the pesticidal preparations wetting agent that the preparation method of pesticidal preparations wetting agent according to claim 2 prepares application in preparing pesticidal preparations.
7. an emamectin benzoate missible oil preparation, it is characterised in that include the component composition of following percetage by weight: the emamectin benzoate of 2.3%, the etoh solvent of 10%, the emulsifying agent agriculture breast 600# of 8%, pesticidal preparations wetting agent described in the claim 1 of 2%, the stabilizer BHT of 1%, residuals weight is 150# solvent naphtha.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610038828.5A CN105707071B (en) | 2016-01-21 | 2016-01-21 | A kind of pesticidal preparations wetting agent and preparation method thereof and the application in pesticidal preparations |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610038828.5A CN105707071B (en) | 2016-01-21 | 2016-01-21 | A kind of pesticidal preparations wetting agent and preparation method thereof and the application in pesticidal preparations |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105707071A true CN105707071A (en) | 2016-06-29 |
| CN105707071B CN105707071B (en) | 2018-09-18 |
Family
ID=56147547
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610038828.5A Active CN105707071B (en) | 2016-01-21 | 2016-01-21 | A kind of pesticidal preparations wetting agent and preparation method thereof and the application in pesticidal preparations |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105707071B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106283638A (en) * | 2016-08-11 | 2017-01-04 | 福建昆冈化学助剂科技有限公司 | A kind of weaving penetrating agent and preparation method thereof |
| CN106279243A (en) * | 2016-08-09 | 2017-01-04 | 威尔（福建）生物有限公司 | A kind of glufosinate-ammonium water preparation auxiliary agent compounding glyphosate and preparation method thereof |
| CN106268498A (en) * | 2016-08-16 | 2017-01-04 | 仇颖莹 | A kind of preparation method of high crystalline abietyl Gemini surface active agent |
| CN112940625A (en) * | 2021-01-22 | 2021-06-11 | 仲恺农业工程学院 | Nano pesticide preparation based on biopolysaccharide grafted rosin and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101502772A (en) * | 2009-03-11 | 2009-08-12 | 中国林业科学研究院林产化学工业研究所 | Colophony-based sulphonate type gemini surfactant and method for preparing the same |
| CN102311368A (en) * | 2011-04-22 | 2012-01-11 | 扬州斯培德化工有限公司 | Twin-type wetting agent as well as preparation method and application thereof |
| CN103599729A (en) * | 2013-11-13 | 2014-02-26 | 中国林业科学研究院林产化学工业研究所 | Rosinyl quaternary ammonium salt dimeric surfactant as well as preparation method and application thereof |
-
2016
- 2016-01-21 CN CN201610038828.5A patent/CN105707071B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101502772A (en) * | 2009-03-11 | 2009-08-12 | 中国林业科学研究院林产化学工业研究所 | Colophony-based sulphonate type gemini surfactant and method for preparing the same |
| CN102311368A (en) * | 2011-04-22 | 2012-01-11 | 扬州斯培德化工有限公司 | Twin-type wetting agent as well as preparation method and application thereof |
| CN103599729A (en) * | 2013-11-13 | 2014-02-26 | 中国林业科学研究院林产化学工业研究所 | Rosinyl quaternary ammonium salt dimeric surfactant as well as preparation method and application thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106279243A (en) * | 2016-08-09 | 2017-01-04 | 威尔（福建）生物有限公司 | A kind of glufosinate-ammonium water preparation auxiliary agent compounding glyphosate and preparation method thereof |
| CN106283638A (en) * | 2016-08-11 | 2017-01-04 | 福建昆冈化学助剂科技有限公司 | A kind of weaving penetrating agent and preparation method thereof |
| CN106283638B (en) * | 2016-08-11 | 2018-07-24 | 福建昆冈化学助剂科技有限公司 | A kind of weaving bleeding agent and preparation method thereof |
| CN106268498A (en) * | 2016-08-16 | 2017-01-04 | 仇颖莹 | A kind of preparation method of high crystalline abietyl Gemini surface active agent |
| CN106268498B (en) * | 2016-08-16 | 2018-02-06 | 云南省玉溪市沁清化工有限公司 | A kind of preparation method of high crystalline abietyl Gemini surface active agent |
| CN112940625A (en) * | 2021-01-22 | 2021-06-11 | 仲恺农业工程学院 | Nano pesticide preparation based on biopolysaccharide grafted rosin and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105707071B (en) | 2018-09-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105707071A (en) | Wetting agent for pesticide preparations, method for preparing wetting agent and application of wetting agent to pesticide preparations | |
| CN105165852B (en) | A kind of botanical pesticide for desinsection | |
| CN115024326B (en) | Slow-release plant growth regulator and preparation method and application thereof | |
| CN108558507A (en) | A kind of composition and its application for improving fertilizer absorption rate | |
| CN118177208B (en) | High-quality bentazone powder and preparation method thereof | |
| CN108947654A (en) | Improve the compound nutritional regulator of the drought-enduring cold-resistant of cold-season turfgrass | |
| CN105850999B (en) | Preparation method and application of rosin-derived pesticide synergist | |
| CN102972413A (en) | Pyridalyl and flutenzine-containing insecticidal compound | |
| CN103450217B (en) | Thick hair Boreostereum vibrans thalline is preparing the application in Ginkgolide B | |
| CN102311368A (en) | Twin-type wetting agent as well as preparation method and application thereof | |
| CN106866533B (en) | Pyraclostrobin crystal form and preparation method thereof | |
| NO131117B (en) | ||
| CN103539733B (en) | A kind of preparation method of isoniazid para-aminosalicylate | |
| CN101648120B (en) | Amino acid type surfactant and preparation method and application thereof | |
| CN110240555A (en) | A kind of synthetic method of 1- isothiocyanic acid base -2- chloro-2-propene | |
| CN106316974A (en) | Production process of hymexazol technical material | |
| CN105948954A (en) | Production method for sugar alcohol chelated synergist | |
| CN112136824A (en) | Application of quassin compounds in preventing and treating plant fungal diseases | |
| CN110423162A (en) | A kind of liquid slow-release compound fertilizer and preparation method thereof | |
| CN106119305B (en) | A kind of preparation method of phenoxy propionic acid | |
| WO2001040141A1 (en) | A nutritive fertilizer used for spraying out of the roots of plants and its applying method | |
| CN112806369A (en) | High-content dicamba aqueous solution and preparation method thereof | |
| CN108689766A (en) | High potassium Multifunctional suspension type liquid fertilizer containing amino acid and preparation method thereof | |
| US20220127202A1 (en) | Process for obtaining a liquid foliar fertilizer and liquid foliar fertilizer composition | |
| CN101999406B (en) | Comprehensive improver for unsound grain rate and chalkiness of japonica rice |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |