CN108496983A - A kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides - Google Patents
A kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides Download PDFInfo
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- CN108496983A CN108496983A CN201810564023.3A CN201810564023A CN108496983A CN 108496983 A CN108496983 A CN 108496983A CN 201810564023 A CN201810564023 A CN 201810564023A CN 108496983 A CN108496983 A CN 108496983A
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- mefenacet
- pyrazosulfuron
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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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
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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
- A01N25/34—Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
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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
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/74—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,3
- A01N43/78—1,3-Thiazoles; Hydrogenated 1,3-thiazoles
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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
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
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- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
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Abstract
The application belongs to field of pesticide preparation, specially a kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides, active ingredient in the effervescent agent is pyrazosulfuron, mefenacet and three azole amides, the percentage that the Sulfometuron Methyl, mefenacet and three azole amides account for effervescent agent weight is respectively 15,10 75,7 50.
Description
Technical field
The application belongs to field of pesticide preparation, specially a kind of to contain pyrazosulfuron, mefenacet and three azole amides
Effervescent formulation.
Technical background
Currently, the common formulations of pesticide mainly have 3 kinds of wet powder, missible oil, aqua dosage forms, wherein wettable powder is thin
Degree and suspensibility are poor, and complex preparation is few, causes many areas that need to prevent and kill off grassy weed and broad leaved weed respectively, both time-consuming
Take medicine again；And not only drug effect is relatively low for this backward dosage form, also easily polluted agricultural land environment, and missible oil and aqua are due to for liquid
Difficulty during transport will necessarily be increased and preserved.
Pesticide effervescence agent is a kind of developed recently more rapid solid-state novel form, and pesticide effervescence agent is by effervescent agent and each
Constituent solid particles or powder mixing, via being granulated or suppressing, pesticide effervescence agent thermoplastic polymer can be disintegrated rapidly after entering water,
Active ingredient is uniformly spread, and after pesticide activity component contacts target, plays the active function of weeding, desinsection, sterilization etc.,
With the features such as easy to operate, time saving and energy saving and efficient.
Invention content
A kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides, it is effective in the effervescent agent
Ingredient is pyrazosulfuron, mefenacet and three azole amides, and the Sulfometuron Methyl, mefenacet and three azole amides account for effervesce
The percentage of agent weight is respectively 1-5,10-75,7-50.
The effervescent formulation is sustained-release and controlled release effervescent formulation；Preferably, the sustained-release and controlled release effervescent formulation is sustained-release and controlled release
Granulae effervescentes or sustained-release and controlled release effervescent tablet.
The effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides includes the original of following portions by weight
Material：1-5 parts of pyrazosulfuron, 10-75 parts of mefenacet, 7-50 parts of three azole amide, isophorone diisocyanate (IPDI)
0.5-10 parts, ethylenediamine 0.5-2 points, 0.5-1 parts of antifoaming agent, 25-30 parts of effervescent agent, 3-8 parts of adhesive, 1-6 parts of wetting agent, the
One 5-10 parts of dispersant, 5-10 parts of the second dispersant, 10-50 parts of 150# solvent naphthas, 10-20 parts of emulsifier.
Contain 2 parts of pyrazosulfuron, 15 parts of mefenacet, three 8 parts of azole amides in the effervescent agent.
The antifoaming agent is dimethyl silicone polymer, polyoxypropylene ethylene oxide glycerin ether, benzyl carbinol oleate, phenylacetic acid
It is one or more in bay alcohol ester.
Described adhesive is the mixture of substance A and ethyl alcohol, and the mass ratio of the substance A and ethyl alcohol is 1:3, the substance
A be polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose or Arabic gum in one kind or
It is a variety of.
The effervescent agent includes acid constituents and alkaline constituents, and the weight ratio of the acid constituents and alkaline constituents is 1：1, the acid group
It is divided into one or more in tartaric acid, citric acid, citric acid, succinic acid, cholic acid, deoxycholic aicd；The alkaline constituents is carbonic acid
It is one or more in sodium, sodium bicarbonate, saleratus, potassium carbonate.
First dispersant is sodium lignin sulfonate or polycarboxylate.
Second dispersant is 2- naphthalene sulfonic acid formaldehyde polymers sodium salt, the aromatic compound sodium salt of sulfonation, alkyl naphthalene
Sodium sulfate salt, diisooctyl succinate sodium sulfonate or maleic acid-acrylic acid copolymer sodium salt weigh one or more.
The wetting agent is pull open powder, lauryl sodium sulfate, aliphatic alcohol sulfate, diisooctyl succinate sodium sulfonate
In any one or more.
The preparation method of effervescent formulation, is as follows：
(1) oil phase is formed
Pyrazosulfuron, mefenacet and three azole amides are mixed with 150# solvent naphthas, emulsifier input dispersion machine
Uniformly, it is sanded subsequently into sand mill, until grain size D90≤5.0 μm of material, are added isophorone diisocyanate, stir
30-40min is mixed, oil phase is formed；
(2) water phase is formed
The mass ratio of addition water and the first dispersant in cutter, water and the first dispersant is 3:1, after being completely dissolved,
PH ranging from 5.0-6.0 are adjusted, water phase is formed；
(3) encystation
Ethylenediamine is diluted with water, the volume ratio of ethylenediamine and water is 1：2, antifoaming agent is added, mixture A is obtained；It will
Oil phase is added in water phase, high speed shear 30min, and rotating speed is that 2300-2600 turns/min, and grain size is sheared to 3-12 microns, is obtained
Mixture B；Then, mixture A is added dropwise in mixture B, rate of addition 50kg/min, after being added dropwise to complete, 800 turns/min
3h is stirred, micro-capsule is formed；
(4) then micro-capsule is sent into and is flowed by a diameter of 4 μm of strainer filtering by the microcapsule suspension for forming step (3)
Change bed to be dried, drying temperature control forms loose granular micro-capsule at 50-60 DEG C；
(5) air-flow crushing
By the second dispersant, wetting agent, effervescent agent mixing, air-flow crushing is then crossed, obtains the object of fineness of materials≤25 μm
Material；
(6) rotating granulation
By the material input rotary pelleting machine that step (4) obtains granular micro-capsule and step (5) obtains, in 1500 turns/min
Under conditions of be uniformly mixed, add adhesive, mix 10 minutes under conditions of 1500 turns/min, complete be granulated, mistake 12 mesh
Mesh screen obtains micro-capsule effervescence granular；
(7) it shapes；
Under the conditions of 50-80 DEG C, the microcapsule granule obtained to step (6) is dried so that and moisture is less than 1%,
Up to the sustained-release and controlled release granulae effervescentes containing pyrazosulfuron, mefenacet and three azole amides；
(8) microcapsule granule that step (6) obtains is poured into tablet press machine and carries out tabletting, the ambient humidity of drying, tabletting is 25-
30%, drying is so that moisture is less than 1% to get the sustained release control containing pyrazosulfuron, mefenacet and three azole amides
Release effervescent tablet.
The usage amount of the effervescent agent is 560-750g/ mus.
Compared with the prior art, the present invention has the following advantages：
The broad-leaved and nutgrass flatsedge that barnyard grass and later stage are unearthed after turning green for rice transplanting, need the weeding of a closed for second time
Combination, the pyrazosulfuron and three azole amides of triazolineone and the mefenacet of amides of this patent sulfonylurea
Ternary herbicidal active component compounds the secondary generation rice field intractable weed in rice field such as Echinochloa, abnormal shape after prevention transplanting is turned green by science
The annual grassy weeds such as nutgrass flatsedge and Procumbent Falsepimpernel, the perennial weeds such as firefly Lin and Herba Cyperi Glomerati have excellent preventive effect.
This patent uses three kinds of different activities herbicidal constituents, action target diversification to have pole to rice field resistant weed drug effect
It is big to be promoted, while the effervescent agent convenient for application is used, a dispenser, quickness and high efficiency solves the problems, such as rice field closed for second time weeding.
Specific implementation mode
The measurement of 1 co-toxicity coefficient of embodiment
Colby methods are to evaluate herbicide mixture effect quickly practical method, are especially suitable for evaluation herbicide controlling spectrum complementary type
The mixed measurement of the synergy type of herbicide, the reasonability clearly matched, and two or more herbicides can also be applied should
Method is evaluated.This method measures single dose and mixture and applies the relative weights of rear target weeds (test group accounts for control group first
Weight percent), then the theoretical relative weight of mixture is calculated by the actual measurement preventive effect of single dose, by the actual measurement preventive effect of itself and mixture
It compares to evaluate synergy type.The calculation formula of theoretical relative weight is：
E0=X*Y*Z ... n/100(n-1)
Wherein X indicates herbicide A1Dosage is P1When weeds relative weight；Y indicates herbicide A2Dosage is P2When it is miscellaneous
The relative weight of grass；E0Indicate herbicide A1+A2+A3+ ...+An dosages are (P1+P2+…+Pn) when weeds theoretical relative weight；
E indicates herbicide A1+A2+A3+ ...+An dosages are (P1+P2+…+Pn) practical application when weeds relative weight.
If E0-E>10%, then it is synergistic effect；- 10%<E0-E<10%, then it is summation action；E0-E<- 10%, then for
Antagonism.
Inventor is by a large amount of screening test, to the different ratio of pyrazosulfuron, mefenacet and three azole amides
A large amount of efficiency test has been carried out, has been found in specific ratio range, obtained Herbicidal combinations have synergistic effect, right
Resistant weed such as barnyard grass, firefly Lin, cyperus iria etc. has excellent preventive effect.With the horizontal orthogonal test of following three factor four
Data are illustrated.
The mixed relative weight of 1 pyrazosulfuron of table, mefenacet and three azole amides
As seen from the above table, mixed by A, B, C ternary designed in three factor level orthogonal tests, within the scope of aforementioned proportion,
Theoretical value and the difference of measured value illustrate that three is mixed and show as synergistic function, and absolutely mostly between 5.35-26.99
The mixed ratio of number is synergistic effect (E0-E>10%).When three's ratio range is in (2):(10-30):When (7-21), three's synergy
Effect is apparent, the most preferably proportioning as pyrazosulfuron, mefenacet and three azole amides.
Embodiment 2
Effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides includes the raw material of following portions by weight：
1 part of pyrazosulfuron, 10 parts of mefenacet, 7 parts of three azole amide, 0.5 part of isophorone diisocyanate (IPDI), ethylenediamine
0.5 point, 0.5 part of antifoaming agent, 25 parts of effervescent agent, 3 parts of adhesive, 1 part of wetting agent, 5 parts of the first dispersant, the second dispersant 5-
Part, 10 parts of 150# solvent naphthas, 10 parts of emulsifier；
The antifoaming agent is Laurate alcohol ester phenylacetate；
Described adhesive is the mixture of substance A and ethyl alcohol, and the mass ratio of the substance A and ethyl alcohol is 1:3, the substance
A is the mixture of polyvinyl alcohol and Arabic gum, and the mass ratio of the polyvinyl alcohol and Arabic gum is 3:4；
The effervescent agent includes acid constituents and alkaline constituents, and the weight ratio of the acid constituents and alkaline constituents is 1：1, the acid group
It is divided into the mixture of citric acid and cholic acid, the mass ratio of the citric acid and cholic acid is 3:1；The alkaline constituents is sodium bicarbonate；
First dispersant is sodium lignin sulfonate；
Second dispersant is 2- naphthalene sulfonic acid formaldehyde polymer sodium salts；
The wetting agent is the mixture of pull open powder and lauryl sodium sulfate, the pull open powder and dodecyl sulphate
The mass ratio of sodium is 1:1；
The preparation method of effervescent formulation, is as follows：
(1) oil phase is formed
Pyrazosulfuron, mefenacet and three azole amides are mixed with 150# solvent naphthas, emulsifier input dispersion machine
Uniformly, it is sanded subsequently into sand mill, until grain size D90≤5.0 μm of material, are added isophorone diisocyanate, stir
30-40min is mixed, oil phase is formed；
(2) water phase is formed
The mass ratio of addition water and the first dispersant in cutter, water and the first dispersant is 3:1, after being completely dissolved,
PH ranging from 5.0-6.0 are adjusted, water phase is formed；
(3) encystation
Ethylenediamine is diluted with water, the volume ratio of ethylenediamine and water is 1：2, antifoaming agent is added, mixture A is obtained；It will
Oil phase is added in water phase, high speed shear 30min, and rotating speed is that 2300-2600 turns/min, and grain size is sheared to 3-12 microns, is obtained
Mixture B；Then, mixture A is added dropwise in mixture B, rate of addition 50kg/min, after being added dropwise to complete, 800 turns/min
3h is stirred, micro-capsule is formed；
(4) then micro-capsule is sent into and is flowed by a diameter of 4 μm of strainer filtering by the microcapsule suspension for forming step (3)
Change bed to be dried, drying temperature control forms loose granular micro-capsule at 50-60 DEG C；
(5) air-flow crushing
By the second dispersant, wetting agent, effervescent agent mixing, air-flow crushing is then crossed, obtains the object of fineness of materials≤25 μm
Material；
(6) rotating granulation
By the material input rotary pelleting machine that step (4) obtains granular micro-capsule and step (5) obtains, in 1500 turns/min
Under conditions of be uniformly mixed, add adhesive, mix 10 minutes under conditions of 1500 turns/min, complete be granulated, mistake 12 mesh
Mesh screen obtains micro-capsule effervescence granular；
(7) it shapes；
Under the conditions of 50-80 DEG C, the microcapsule granule obtained to step (6) is dried so that and moisture is less than 1%,
Up to the sustained-release and controlled release granulae effervescentes containing pyrazosulfuron, mefenacet and three azole amides；
(8) microcapsule granule that step (6) obtains is poured into tablet press machine and carries out tabletting, the ambient humidity of drying, tabletting is 25-
30%, drying is so that moisture is less than 1% to get the sustained release control containing pyrazosulfuron, mefenacet and three azole amides
Release effervescent tablet.
Embodiment 3
The effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides includes the original of following portions by weight
Material：5 parts of pyrazosulfuron, 75 parts of mefenacet, 50 parts of three azole amide, 10 parts of isophorone diisocyanate (IPDI), second
Diamines 2 divides, 1 part of antifoaming agent, 30 parts of effervescent agent, 8 parts of adhesive, 6 parts of wetting agent, 10 parts of the first dispersant, the second dispersant 10
Part, 50 parts of 150# solvent naphthas, 20 parts of emulsifier；
The antifoaming agent is the mixture of benzyl carbinol oleate and Laurate alcohol ester phenylacetate, the benzyl carbinol oleate and benzene
The mass ratio of acetic acid bay alcohol ester is 2:1；
Described adhesive is the mixture of substance A and ethyl alcohol, and the mass ratio of the substance A and ethyl alcohol is 1:3, the substance
A is polyethylene glycol；
The effervescent agent includes acid constituents and alkaline constituents, and the weight ratio of the acid constituents and alkaline constituents is 1：1, the acid group
The mass ratio of the mixture being divided into succinic acid, cholic acid and deoxycholic aicd, the succinic acid, cholic acid and deoxycholic aicd is 3:2:5；
The alkaline constituents is sodium carbonate and the mass ratio with the mixture in potassium carbonate, the sodium carbonate and with potassium carbonate is 1:4；
First dispersant is sodium lignin sulfonate；
Second dispersant is 2- naphthalene sulfonic acid formaldehyde polymer sodium salts；
The wetting agent be lauryl sodium sulfate and diisooctyl succinate sodium sulfonate in mixture, described 12
The mass ratio of sodium alkyl sulfate and diisooctyl succinate sodium sulfonate is 3:1；
The preparation method of effervescent formulation, is as follows：
(1) oil phase is formed
Pyrazosulfuron, mefenacet and three azole amides are mixed with 150# solvent naphthas, emulsifier input dispersion machine
Uniformly, it is sanded subsequently into sand mill, until grain size D90≤5.0 μm of material, are added isophorone diisocyanate, stir
30-40min is mixed, oil phase is formed；
(2) water phase is formed
The mass ratio of addition water and the first dispersant in cutter, water and the first dispersant is 3:1, after being completely dissolved,
PH ranging from 5.0-6.0 are adjusted, water phase is formed；
(3) encystation
Ethylenediamine is diluted with water, the volume ratio of ethylenediamine and water is 1：2, antifoaming agent is added, mixture A is obtained；It will
Oil phase is added in water phase, high speed shear 30min, and rotating speed is that 2300-2600 turns/min, and grain size is sheared to 3-12 microns, is obtained
Mixture B；Then, mixture A is added dropwise in mixture B, rate of addition 50kg/min, after being added dropwise to complete, 800 turns/min
3h is stirred, micro-capsule is formed；
(4) then micro-capsule is sent into and is flowed by a diameter of 4 μm of strainer filtering by the microcapsule suspension for forming step (3)
Change bed to be dried, drying temperature control forms loose granular micro-capsule at 50-60 DEG C；
(5) air-flow crushing
By the second dispersant, wetting agent, effervescent agent mixing, air-flow crushing is then crossed, obtains the object of fineness of materials≤25 μm
Material；
(6) rotating granulation
By the material input rotary pelleting machine that step (4) obtains granular micro-capsule and step (5) obtains, in 1500 turns/min
Under conditions of be uniformly mixed, add adhesive, mix 10 minutes under conditions of 1500 turns/min, complete be granulated, mistake 12 mesh
Mesh screen obtains micro-capsule effervescence granular；
(7) it shapes；
Under the conditions of 50-80 DEG C, the microcapsule granule obtained to step (6) is dried so that and moisture is less than 1%,
Up to the sustained-release and controlled release granulae effervescentes containing pyrazosulfuron, mefenacet and three azole amides；
(8) microcapsule granule that step (6) obtains is poured into tablet press machine and carries out tabletting, the ambient humidity of drying, tabletting is 25-
30%, drying is so that moisture is less than 1% to get the sustained release control containing pyrazosulfuron, mefenacet and three azole amides
Release effervescent tablet.
Embodiment 4
The effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides includes the original of following portions by weight
Material：2 parts of pyrazosulfuron, 15 parts of mefenacet, 8 parts of three azole amide, isophorone diisocyanate (red skin IPDI6 parts, second
1.5 parts of diamines, 0.8 part of antifoaming agent, 28 parts of effervescent agent, 6 parts of adhesive, 4 parts of wetting agent, 7 parts of the first dispersant, the second dispersant
8 parts, 25 parts of 150# solvent naphthas, 15 parts of emulsifier；
The antifoaming agent be dimethyl silicone polymer and benzyl carbinol oleate mixture, the dimethyl silicone polymer and
The mass ratio of benzyl carbinol oleate is 5:1；
Described adhesive is the mixture of substance A and ethyl alcohol, and the mass ratio of the substance A and ethyl alcohol is 1:3, the substance
A is carboxymethyl cellulose or Arabic gum；
The effervescent agent includes acid constituents and alkaline constituents, and the weight ratio of the acid constituents and alkaline constituents is 1：1, the acid group
It is divided into the mixture of tartaric acid and succinic acid, the mass ratio of the tartaric acid and succinic acid is 1:5；The alkaline constituents is bicarbonate
The mass ratio of the mixture of sodium and potassium carbonate, the sodium bicarbonate and potassium carbonate is 1:1；
First dispersant is sodium lignin sulfonate；
Second dispersant is the mixture of 2- naphthalene sulfonic acid formaldehyde polymers sodium salt and diisooctyl succinate sodium sulfonate,
The mass ratio of the 2- naphthalene sulfonic acid formaldehyde polymers sodium salt and diisooctyl succinate sodium sulfonate is 1:1；
The wetting agent is lauryl sodium sulfate；
The preparation method of effervescent formulation, is as follows：
(1) oil phase is formed
Pyrazosulfuron, mefenacet and three azole amides are mixed with 150# solvent naphthas, emulsifier input dispersion machine
Uniformly, it is sanded subsequently into sand mill, until grain size D90≤5.0 μm of material, are added isophorone diisocyanate, stir
30-40min is mixed, oil phase is formed；
(2) water phase is formed
The mass ratio of addition water and the first dispersant in cutter, water and the first dispersant is 3:1, after being completely dissolved,
PH ranging from 5.0-6.0 are adjusted, water phase is formed；
(3) encystation
Ethylenediamine is diluted with water, the volume ratio of ethylenediamine and water is 1：2, antifoaming agent is added, mixture A is obtained；It will
Oil phase is added in water phase, high speed shear 30min, and rotating speed is that 2300-2600 turns/min, and grain size is sheared to 3-12 microns, is obtained
Mixture B；Then, mixture A is added dropwise in mixture B, rate of addition 50kg/min, after being added dropwise to complete, 800 turns/min
3h is stirred, micro-capsule is formed；
(4) then micro-capsule is sent into and is flowed by a diameter of 4 μm of strainer filtering by the microcapsule suspension for forming step (3)
Change bed to be dried, drying temperature control forms loose granular micro-capsule at 50-60 DEG C；
(5) air-flow crushing
By the second dispersant, wetting agent, effervescent agent mixing, air-flow crushing is then crossed, obtains the object of fineness of materials≤25 μm
Material；
(6) rotating granulation
By the material input rotary pelleting machine that step (4) obtains granular micro-capsule and step (5) obtains, in 1500 turns/min
Under conditions of be uniformly mixed, add adhesive, mix 10 minutes under conditions of 1500 turns/min, complete be granulated, mistake 12 mesh
Mesh screen obtains micro-capsule effervescence granular；
(7) it shapes；
Under the conditions of 50-80 DEG C, the microcapsule granule obtained to step (6) is dried so that and moisture is less than 1%,
Up to the sustained-release and controlled release granulae effervescentes containing pyrazosulfuron, mefenacet and three azole amides；
(8) microcapsule granule that step (6) obtains is poured into tablet press machine and carries out tabletting, the ambient humidity of drying, tabletting is 25-
30%, drying is so that moisture is less than 1% to get the sustained release control containing pyrazosulfuron, mefenacet and three azole amides
Release effervescent tablet.
The usage amount of effervescent agent described herein is 560-750ga.i./ha；Water contains in sustained-release and controlled release effervescent formulation
Amount is less than 1% (weight percent).
5 field experiment of embodiment
Effervescent formulation prepared by the embodiment of the present invention 2, embodiment 3 and embodiment 4 is with reference to " country of the People's Republic of China (PRC)
Standard pesticide field control effectiveness test criterion (one) " designs field efficacy and safety testing, with clear pyrazosulfuron, benzene thiophene acyl grass
The field mixed effect of amine, three azole amides.Specific test operation is as follows：
Test medicine：Effervescent formulation prepared by embodiment 2, embodiment 3 and embodiment 4；
Comparison medicament 1：10% pyrazosulfuron effervescent tablet；
Comparison medicament 2：50% mefenacet wettable powder；
Comparison medicament 3：25% 3 azole amide suspending agent；
Pilot survey object：Medicament is investigated to the preventive effect of weeds and total careless preventive effect, investigates medicine ensuing crop safety.Experimental field
Selected from Heilungkiang Mishan transplanting rice field, field main weeds are prevention angustifolia arrowhead herb, firefly Lin, Monochoria korsakowii, barnyard grass, nutgrass flatsedge etc..
Spraying time：After rice transplanting is turned green 3~7 days (after rice transplanting 10~20 days), field part weeds have emerged, mostly
In 2~4 leaf phases.
Application method and field management：The throwing of test medicine Direct Uniform is applied in the water layer of rice field, comparison medicament use spraying,
Pesticide-clay mixture or the fertile method dispenser of poison.Water layer 3-5cm when dispenser is retained 5-7 days, avoids water layer amnion rice seedling young leaves, thereafter conventional tube
Reason.Local farming method is pressed in field management.Quarter Design：The random district's groups arrangement of cell, per 30 square metres of cell, 4 repetitions.
Preventive effect is investigated：Absolute-value scheme randomly chooses per cell at 4 points, and 0.25 square metre every is sampled, statistics weeds strain
Number calculates strain preventive effect (E1)。
CK0For number of weeds before dispenser, CK1For number of weeds after dispenser；Pt0For number of weeds before treatment region dispenser, Pt1For processing
Number of weeds after area's dispenser.
Test result is as shown in table 2：
30d preventive effects after 2 each weeds medicine of table
By upper table data it is found that composition dosage of the present invention is in test medicine constant 560-750ga.i./ha
To the preventive effects of the main weeds such as the key resistance weeds barnyard grass of local rice terrace, cyperus iria, firefly Lin 90% or more, and it is single
Solely using the finished product of three kinds of active constituents always careless preventive effect all below 85%.And three kinds of herbicide mixtures, increase act on it is miscellaneous
The target site of grass, can effectively reduce the speed that weeds generate resistance, while three kinds of medicament applied onces, time and labour saving, efficiently,
Environmental protection.
Observation post administration chemical injury of crops reacts：The present invention relates to each dosage processing of medicament to be showed no apparent symptom of chemical damage, leaf color
Normally, growing way is good.30 days after medicine, investigation crop tiller number, strain fresh weight, specific data are shown in Table 3.
30d crop pattern indexs after 3 medicine of table
As seen from the above table, each chemicals treatment does not make significant difference to crop tiller number, fresh weight, plant height, through the significance of difference point
Analysis, test medicine constant (560ga.i./ha), each index value of times amount (1120ga.i./ha) processing and blank control difference are not
Significantly.Comparison medicament inhibits paddy growth when measuring again to a certain extent, however times amount processing is inevitable in actual production,
The risk that herbicide uses is increased, is unfavorable for stable yields and surely receives.To sum up, the present invention relates to compositions under recommended dose to for examination
Rice safety does not make significant difference to growth.
Claims (10)
1. a kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides, which is characterized in that the effervescent agent
In active ingredient be pyrazosulfuron, mefenacet and three azole amides, the Sulfometuron Methyl, mefenacet and triazole acyl grass
The percentage that amine accounts for effervescent agent weight is respectively 1-5,10-75,7-50.
2. a kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides as described in claim 1, special
Sign is that the effervescent formulation is sustained-release and controlled release effervescent formulation；Preferably, the sustained-release and controlled release effervescent formulation steeps for sustained-release and controlled release
Rise granula or sustained-release and controlled release effervescent tablet.
3. a kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides as described in claim 1, special
Sign is that the effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides includes the original of following portions by weight
Material：1-5 parts of pyrazosulfuron, 10-75 parts of mefenacet, 7-50 parts of three azole amide, isophorone diisocyanate（Red skin
IPDI）0.5-10 parts, ethylenediamine 0.5-2 points, 0.5-1 parts of antifoaming agent, 25-30 parts of effervescent agent, 3-8 parts of adhesive, wetting agent 1-6
Part, 5-10 parts of the first dispersant, 5-10 parts of the second dispersant, 10-50 parts of 150# solvent naphthas, 10-20 parts of emulsifier.
4. a kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides as claimed in claim 3, special
Sign is, 2 parts of pyrazosulfuron, 15 parts of mefenacet, three 8 parts of azole amides are contained in the effervescent agent.
5. a kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides as claimed in claim 3, special
Sign is that the antifoaming agent is dimethyl silicone polymer, polyoxypropylene ethylene oxide glycerin ether, benzyl carbinol oleate, phenylacetic acid
It is one or more in bay alcohol ester.
6. a kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides as claimed in claim 3, special
Sign is, described adhesive is the mixture of substance A and ethyl alcohol, and the mass ratio of the substance A and ethyl alcohol is 1:3, the substance A
For in polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, polyvinyl alcohol, carboxymethyl cellulose or Arabic gum one kind or
It is a variety of.
7. a kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides as claimed in claim 3, special
Sign is, the effervescent agent includes acid constituents and alkaline constituents, and the weight ratio of the acid constituents and alkaline constituents is 1：1, the acid group
It is divided into one or more in tartaric acid, citric acid, citric acid, succinic acid, cholic acid, deoxycholic aicd；The alkaline constituents is carbonic acid
It is one or more in sodium, sodium bicarbonate, saleratus, potassium carbonate.
8. a kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides as claimed in claim 3, special
Sign is that first dispersant is sodium lignin sulfonate or polycarboxylate.
9. a kind of effervescent formulation containing pyrazosulfuron, mefenacet and three azole amides as claimed in claim 3, special
Sign is that second dispersant is 2- naphthalene sulfonic acid formaldehyde polymers sodium salt, the aromatic compound sodium salt of sulfonation, alkyl naphthalene sulphur
Acid sodium-salt, diisooctyl succinate sodium sulfonate or maleic acid-acrylic acid copolymer sodium salt weigh one or more；Preferably, institute
The wetting agent stated is any one in pull open powder, lauryl sodium sulfate, aliphatic alcohol sulfate, diisooctyl succinate sodium sulfonate
Kind is a variety of.
10. the preparation method of effervescent formulation as described in claim 1, which is characterized in that be as follows：
（1）Oil phase is formed
Pyrazosulfuron, mefenacet and three azole amides are uniformly mixed with 150# solvent naphthas, emulsifier input dispersion machine,
It is sanded subsequently into sand mill, until grain size D90≤5.0 μm of material, are added isophorone diisocyanate, stirs 30-
40min forms oil phase；
（2）Water phase is formed
The mass ratio of addition water and the first dispersant in cutter, water and the first dispersant is 3:1, after being completely dissolved, adjustment
PH ranging from 5.0-6.0 form water phase；
（3）Encystation
Ethylenediamine is diluted with water, the volume ratio of ethylenediamine and water is 1：2, antifoaming agent is added, mixture A is obtained；By oil phase
It is added in water phase, high speed shear 30min, rotating speed is that 2300-2600 turns/min, and grain size is sheared to 3-12 microns, must be mixed
Object B；Then, mixture A is added dropwise in mixture B, rate of addition 50kg/min, after being added dropwise to complete, 800 turns/min stirrings
3h forms micro-capsule；
（4）By step（3）Then micro-capsule is sent into fluid bed by the microcapsule suspension of formation by a diameter of 4 μm of strainer filtering
It is dried, drying temperature control forms loose granular micro-capsule at 50-60 DEG C；
（5）Air-flow crushing
By the second dispersant, wetting agent, effervescent agent mixing, air-flow crushing is then crossed, obtains the material of fineness of materials≤25 μm；
（6）Rotating granulation
By step（4）Obtain granular micro-capsule and step（5）The material of acquisition puts into rotary pelleting machine, in the item of 1500 turns/min
It is uniformly mixed under part, adds adhesive, mixed 10 minutes under conditions of 1500 turns/min, completed to be granulated, cross 12 mesh mesh screens,
Obtain micro-capsule effervescence granular；
（7）Forming；
Under the conditions of 50-80 DEG C, to step（6）The microcapsule granule of acquisition is dried so that moisture less than 1% to get containing
There are the sustained-release and controlled release granulae effervescentes of pyrazosulfuron, mefenacet and three azole amides；
（8）By step（6）The microcapsule granule of acquisition pours into tablet press machine and carries out tabletting, and the ambient humidity of drying, tabletting is 25-30%,
Drying is so that moisture is less than 1% to get the sustained-release and controlled release effervesce containing pyrazosulfuron, mefenacet and three azole amides
Tablet；Preferably, the usage amount of the effervescent agent is 500-750ga.i./ha.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102177906A (en) * | 2011-03-16 | 2011-09-14 | 广西壮族自治区化工研究院 | Herbicide effervescent tablets and preparation method thereof |
| CN107960420A (en) * | 2016-10-19 | 2018-04-27 | 大连广达农药有限责任公司 | A kind of composition pesticide for preventing and kill off transplanted rice field malignant weed and preparation method thereof |
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2018
- 2018-06-04 CN CN201810564023.3A patent/CN108496983A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102177906A (en) * | 2011-03-16 | 2011-09-14 | 广西壮族自治区化工研究院 | Herbicide effervescent tablets and preparation method thereof |
| CN107960420A (en) * | 2016-10-19 | 2018-04-27 | 大连广达农药有限责任公司 | A kind of composition pesticide for preventing and kill off transplanted rice field malignant weed and preparation method thereof |
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Application publication date: 20180907 |