CN108812653A - It is a kind of to contain pyrazosulfuron, pretilachlor and effervescent formulation of furans sulphur humulone and preparation method thereof - Google Patents
It is a kind of to contain pyrazosulfuron, pretilachlor and effervescent formulation of furans sulphur humulone and preparation method thereof Download PDFInfo
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- CN108812653A CN108812653A CN201810563982.3A CN201810563982A CN108812653A CN 108812653 A CN108812653 A CN 108812653A CN 201810563982 A CN201810563982 A CN 201810563982A CN 108812653 A CN108812653 A CN 108812653A
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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
- A01N25/12—Powders or granules
- A01N25/14—Powders or granules wettable
-
- 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
-
- 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
- A01N37/18—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 the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
- A01N37/22—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 the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides
-
- 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
- A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
- A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
- A01N43/06—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings
- A01N43/08—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom five-membered rings with oxygen as the ring hetero atom
-
- 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
Abstract
It is specially a kind of to contain pyrazosulfuron, pretilachlor and effervescent formulation of furans sulphur humulone and preparation method thereof the invention belongs to pesticide field.The effervescent formulation its effective component pyrazosulfuron, pretilachlor, the weight ratio of furans sulphur humulone are：1-5：10-75：1-15.The present invention uses three kinds of different activities herbicidal constituents, and action target diversification can solve resistant weed, and to Security of rice height, herbicide spectrum width is high to weeds in paddy field preventive effect, has both quick-acting and lasting effect.Simultaneously using the effervescent agent convenient for application, it can directly spread fertilizer over the fields, save labor, it is primary to be administered, quickly and efficiently solve the problems, such as rice field closed for second time weeding.
Description
Technical field
The invention belongs to pesticide field, specially a kind of effervesce system containing pyrazosulfuron, pretilachlor and furans sulphur humulone
Agent and preparation method thereof.
Background technique
Paddy field weeding is a great problem of Rice Cropping, and chemical weed control is the main means of current control weeds.In recent years,
Since some herbicide kind large area use, already leads to many weeds and produce drug resistance.It is removed since chemistry is used for a long time
Careless method causes weeds in paddy field population to be changed, angustifolia arrowhead herb, Monochoria korsakowii, needle spikesedge herb, firefly Lin, flat stalk Fischer grass, barnyard grass etc. at
For malignant weed or main weeds population, they belong to the difficult weeds in paddy field removed of comparison.Due to a variety of weeds in rice field
Grass phase is complicated, many kinds of, and has complicated resistance, and herbicide in the prior art not can effectively solve weeds in paddy field,
Herbicidal effect is bad, can show defect in a certain respect.
It buys a variety of single doses oneself according to oneself " hobby " mostly in the weeding of rice main producing region peasant household to use with, because single dose is general
Produced by different manufacturing enterprises, the mixed often proportion in scene is not scientific, single dose combination is not scientific cause weeding drug effect difference or because
It matches the drug effects such as unreasonable and Adverse drug events takes place frequently；On the other hand, main paddy field weeding dosage form is mostly missible oil, wettable powder at present
Deng these dosage forms cannot be directly administered, and application is taken a lot of work laborious.
Pyrazosulfuron belongs to sulfonylurea herbicide, is selective inner-adsorption conduction-type herbicide, is mainly inhaled by root system
It receives, is shifted rapidly in weeds plant body, inhibit growth, weeds are gradually dead.Rice can decompose the medicament, several to paddy growth
Do not influence.Efficacy stability, it is highly-safe, the lasting period 25~35 days.Can prevent and kill off annual and perennial broadleaf weed and
Sedge weed, such as anisotropic nutgrass flatsedge, Herba Cyperi Glomerati, firefly Lin, Monochoria vaginalis, Chinese celery, mexicana, angustifolia arrowhead herb, bog pondweed, green duckweed, Eclipta prostrata.
It is invalid to barnyard grass, semen euphorbiae.
Pretilachlor is that have highly selective paddy field herbicides special.To rice safety, broad weed-killing spectrum.Weed seed exists
Medicament is absorbed in germination process, root absorption is poor.It can only make soil treatment before bud.For soil treatment, rice field barnyard grass can be prevented and kill off
Grass, difformed galingale herb, needle spikesedge herb, Monochoria vaginalis, alisma canaliculatum etc..It is poor to wet slotting rice selective when singly applying.
Furans sulphur humulone category three ketones herbicide is 4- medical midbodies of para (ortho)-hydroxybenzoic acetone acid dual oxide enzyme (HPPD) inhibitor, can press down
Indispensable pigment synthesis in plant growth processed is absorbed by root, stem, young shoot, leaf and is conducted rapidly.HPPD is most heavy at present
One of herbicide action target wanted.Furans sulphur humulone mainly passes through blade face and root absorption, and xylem and bast to
It pushes up and is conducted to base, be distributed in entire plant.Weeds are after by medicine, blade face albefaction, then separate living tissue necrosis.
Using the herbicidal active compounds of these three different role mechanism, developing one kind, can effectively to solve current rice field a variety of
Weeds complexity resistance, and the Recompounded pesticide with high activity of weeding, have great importance.
Technical solution
To solve above-mentioned the problems of the prior art, this patent selects suitable herbicidal active component according to weeds situation；
Appropriate proportioning has been selected according to weed population quantity；Effervesce dosage form is selected according to property easy to use, convenient for directly spreading fertilizer over the fields.This hair
Bright to disclose a kind of Herbicidal combinations and its preparation method and application, specific technical solution is as follows：
A kind of effervescent formulation containing pyrazosulfuron, pretilachlor and furans sulphur humulone, effective component pyrazosulfuron, the third grass
Amine, furans sulphur humulone weight ratio be：1-5：10-75：1-15.
Preferably, the weight ratio of the pyrazosulfuron, pretilachlor, furans sulphur humulone is：3:15:6.
Preferably, the effervescent formulation is granulae effervescentes or effervescent tablet.
Preferably, comprising the following components in parts by weight：1-5 parts of pyrazosulfuron, 10-75 parts of pretilachlor, furans sulphur humulone
1-15 parts, 5-10 parts of dispersing agent, 1-6 parts of wetting agent, 15-50 parts of effervescent agent, 3-8 parts of adhesive, 0.5-1.5 parts of excipient, cream
8-20 parts of agent, 10-25 parts of adsorbent.
Preferably, the dispersing agent is sodium lignin sulfonate, polycarboxylate, 2- naphthalene sulfonic acid formaldehyde polymer sodium salt, sulphur
One of the aromatic compound sodium salt of change, alkyl naphthalene sodium sulfate salt, maleic acid-acrylic acid copolymer sodium salt or a variety of groups
It closes；The wetting agent is pull open powder, in lauryl sodium sulfate, aliphatic alcohol sulfate, diisooctyl succinate sodium sulfonate
One or more combinations；Described adhesive be polyvinyl alcohol, polyvinylpyrrolidone, polyethylene glycol, carboxymethyl cellulose, Ah
The mixture of one of primary glue or a variety of combinations and ethyl alcohol is drawn, mixed weight ratio is 1:3, the excipient is talcum
Powder, the emulsifier are the combination of calcium dodecyl benzene sulfonate, phenethyl phenol polyethenoxy ether, and its ratio be 1:0.9, the suction
Attached dose is one of precipitated silica, gas-phase silica, diatomite, magnesium stearate, kaolin, zeolite powder or a variety of groups
It closes；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 constituents is
One of tartaric acid, citric acid, citric acid, succinic acid, cholic acid, deoxycholic aicd or a variety of combinations；The alkaline constituents is carbon
One of sour potassium sodium carbonate, sodium bicarbonate, saleratus or a variety of combinations.
Preferably, the effervescent formulation, comprises the following components in parts by weight：2 parts of pyrazosulfuron, 15 parts of pretilachlor,
2 parts of furans sulphur humulone, 5 parts of dispersing agent, 2 parts of wetting agent, 40 parts of effervescent agent, 9.5 parts of adhesive, 0.5 part of excipient, emulsifier 6
Part, 20 parts of adsorbent.
The invention also discloses the preparation method of above-mentioned effervescent formulation, specific technical solution is as follows：
The preparation method of any of the above-described effervescent formulation, the effervescent formulation are effervescent tablet, including following technique
Step：
(1) weighing material；
(2) air-flow crushing：Dispersing agent, wetting agent, pyrazosulfuron, furans sulphur humulone investment mixing machine are uniformly mixed, so
Air-flow crushing is crossed afterwards to final material fineness≤25 μm；
(3) preparation of pretilachlor missible oil：Reaction in reaction kettle is added in pretilachlor and emulsifier and obtains pretilachlor missible oil, it is standby
With；
(4) rotating granulation：Baiting valve is closed, adds an adsorbent into rotary pelleting machine, then pretilachlor missible oil is added,
Rotation is uniformly mixed；The material that step 2 prepares is added, effervescent agent rotation is uniformly mixed, and adds adhesive, and rotation is shredded,
Baiting valve is opened after the completion of being granulated, will make particle releasing, 12 mesh screens is crossed or vibrating screen sifts out larger particles, is obtained uniform
Granulae effervescentes；
(5) it dries：Step 4 gained wet granular is dry by drying machine, control dryer entrance mouth humidity 20% with
Under, drying temperature is not higher than 60 DEG C in drying course, drying to particle moisture content<0.5%, it is spare；
(6) tabletting：Particle dried obtained by step 5, excipient investment mixing machine are uniformly mixed, tabletting is subsequently poured into
Machine carries out tabletting；
(7) it packs.
The preparation method of any of the above-described effervescent formulation, the effervescent formulation are granulae effervescentes, including following technique
Step：
(1) weighing material；
(2) air-flow crushing：Dispersing agent, wetting agent, pyrazosulfuron, furans sulphur humulone investment mixing machine are uniformly mixed, so
Air-flow crushing is crossed afterwards to final material fineness≤25 μm；
(3) preparation of pretilachlor missible oil：Reaction in reaction kettle is added in pretilachlor and emulsifier and obtains pretilachlor missible oil, it is standby
With；
(4) rotating granulation：Baiting valve is closed, adds an adsorbent into rotary pelleting machine, then pretilachlor missible oil is added,
Rotation is uniformly mixed；The material that step 2 prepares is added, effervescent agent rotation is uniformly mixed, and adds adhesive, and rotation is shredded,
Baiting valve is opened after the completion of being granulated, will make particle releasing, crosses 12 mesh screens or, obtaining uniform granulae effervescentes；
(5) it dries：Step 4 gained wet granular is dry by drying machine, control dryer entrance mouth humidity 20% with
Under, drying temperature is not higher than 60 DEG C in drying course, drying to particle moisture content<0.5%, it is spare；
(6) it packs.
Beneficial effect
Pyrazosulfuron is acetolactate synthestase (ALS) inhibitor, and pretilachlor is fatty acid synthetic inhibitor, hinders white matter
Synthesis, furans sulphur humulone are HPPD inhibitor, and three plays drug effect in weed germination phase and seedling early stage.In view of paddy field
Hygrothermal environment, weed seed meets the environmental condition for being suitble to sprout after site preparation, and focus mostly on the sprouting in 7-15 days after transplanting, applies at this time
On the one hand three different effective components of the mechanism of action expand degrass spectrum, on the other hand realize miscellaneous to the resistance of different loci
Grass is disposably prevented and kill off, and is saved labor, efficient low-consume.This patent is the combination of the herbicidal active compounds of three kinds of different role mechanism,
It is that a kind of pair of rice field malignant weed for solving the current a variety of weeds complexity resistances in rice field and screening meticulously has high activity of weeding
Composition, have extremely strong prevention and control ability to angustifolia arrowhead herb, firefly Lin, Monochoria korsakowii, needle spikesedge herb, barnyard grass, nutgrass flatsedge etc..Effervescent formulation can be straight
It connects and spreads fertilizer over the fields, easy to use, application is convenient.Belong to the Herbicidal combination and formulation development of high effect.
This patent has notable synergistic effect, 1+ after selecting three kinds of completely not identical mechanism of action herbicidal active component compoundings
1+1 > 3, which especially prevents and kill off resistance angustifolia arrowhead herb, firefly Lin, Monochoria korsakowii, needle spikesedge herb, barnyard grass, nutgrass flatsedge etc. to difficulty, very good effect,
In addition this patent be ternary effervescent agent can rice field change traditional pesticide-clay mixture method combine a drug solve rice field it is big absolutely
Number grass family, broad-leaved, nutgrass flatsedge problem.The present invention can solve China future rice field resistant weed, while can fast be administered completely
For agricultural production practice.
This patent uses three kinds of different activities herbicidal constituents, and action target diversification can solve resistant weed, and right
Security of rice is high, herbicide spectrum width, high to weeds in paddy field preventive effect, has both quick-acting and lasting effect.Simultaneously using convenient for application
Effervescent agent can directly spread fertilizer over the fields, save labor, primary to be administered, and quickly and efficiently solve the problems, such as rice field closed for second time weeding.
Specific embodiment
The invention will now be further described with reference to specific embodiments, the advantages and features of the present invention will be with description and
It is apparent.But examples are merely exemplary, and it is not intended to limit the scope of the present invention in any way.Those skilled in the art answer
It should be appreciated that without departing from the spirit and scope of the invention can details to technical solution of the present invention and form repair
Change or replace, but these modifications and replacement are fallen within the protection scope of the present invention.All chemical groups used in the present invention
It is commercially available for dividing.
Embodiment 1
A kind of Herbicidal combinations effervescent tablet, effective component are pyrazosulfuron, pretilachlor, furans sulphur humulone, the bubble
Preparation is risen to comprise the following components in parts by weight：1 part of pyrazosulfuron, 10 parts of pretilachlor, 1 part of furans sulphur humulone, 5 parts of dispersing agent, profit
1 part of humectant, 15 parts of effervescent agent, 3 parts of adhesive, 0.5 part of excipient, 8 parts of emulsifier, 10 parts of adsorbent.
The dispersing agent is sodium lignin sulfonate；The wetting agent is pull open powder, diisooctyl succinate sodium sulfonate
Combination, described adhesive are the mixture of polyvinyl alcohol and ethyl alcohol, and mixed weight ratio is 1:3, the excipient is talcum powder,
The emulsifier is calcium dodecyl benzene sulfonate.
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 combination of citric acid, citric acid；The alkaline constituents is the combination of sodium bicarbonate, sodium carbonate.The solvent is ethyl alcohol.
The preparation method of above-mentioned Herbicidal combinations effervescent tablet, comprises the following steps that：
(1) weighing material；
(2) air-flow crushing：Dispersing agent, wetting agent, pyrazosulfuron, furans sulphur humulone investment mixing machine are uniformly mixed, so
Air-flow crushing is crossed afterwards to final material fineness≤25 μm；
(3) preparation of pretilachlor missible oil：Reaction in reaction kettle is added in pretilachlor and emulsifier and obtains pretilachlor missible oil, it is standby
With；
(4) rotating granulation：Baiting valve is closed, adds an adsorbent into rotary pelleting machine, then pretilachlor missible oil is added,
Rotation is uniformly mixed；The material that step 2 prepares is added, effervescent agent rotation is uniformly mixed, and adds adhesive, and rotation is shredded,
Baiting valve is opened after the completion of being granulated, will make particle releasing, 12 mesh screens is crossed or vibrating screen sifts out larger particles, is obtained uniform
Granulae effervescentes；
(5) it dries：Step 4 gained wet granular is dry by drying machine, control dryer entrance mouth humidity 20% with
Under, drying temperature is not higher than 60 DEG C in drying course, drying to particle moisture content<0.5%, it is spare；
(6) tabletting：Particle dried obtained by step 5, excipient investment mixing machine are uniformly mixed, tabletting is subsequently poured into
Machine carries out tabletting；Mixed material, which all needs to extrude, avoids the material stock moisture absorption；Tablet first is adjusted with manually before each tabletting of tablet press machine
Size, grammes per square metre, open electronic tabletting again after meeting the requirements, directly open and electronic be possible to push up bad punching pin；Ambient humidity controls when tabletting
30% hereinafter, extrude tablet answer rapid vacuum to pack, prevent in air the moisture absorption lead to the bag that rises；In tableting processes, if gone out
It is rough that existing sticking phenomenon leads to extrude tablet, can shut down cleaning, and when cleaning is necessary to switch off power supply, forbids out to stretch when electronic tabletting
Hand samples in tablet press machine, and tableting process terminates, and cuts off the power, and in time cleans out tablet press machine, especially by upper and lower punching pin
Viscous material is cleaned out, and otherwise can be difficult to clear up after the moisture absorption；
(7) it packs.
Embodiment 2
A kind of Herbicidal combinations effervescent, effective component be pyrazosulfuron, pretilachlor, furans sulphur humulone, it is described
Effervescent tablet comprises the following components in parts by weight：5 parts of pyrazosulfuron, 75 parts of pretilachlor, 15 parts of furans sulphur humulone, dispersing agent 10
Part, 6 parts of wetting agent, 50 parts of effervescent agent, 8 parts of adhesive, 1.5 parts of excipient, 20 parts of emulsifier, 25 parts of adsorbent.
Preferably, the dispersing agent is 2- naphthalene sulfonic acid formaldehyde polymer sodium salt, alkyl naphthalene sodium sulfate salt, maleic acid-
Combination in acrylic copolymer sodium salt；The wetting agent is the combination of lauryl sodium sulfate, aliphatic alcohol sulfate；It is described
Adhesive is the mixture of carboxymethyl cellulose and ethyl alcohol, mixed proportion 1:3, the excipient is talcum powder, the emulsification
Agent is phenethyl phenol polyethenoxy ether, and the adsorbent is white carbon black, diatomite, kaolin, the combination in zeolite powder.
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 combination of citric acid, cholic acid；The alkaline constituents is the combination of sodium carbonate, saleratus.
The preparation method of above-mentioned Herbicidal combinations effervescent, comprises the following steps that：
(1) weighing material；
(2) air-flow crushing：Dispersing agent, wetting agent, pyrazosulfuron, furans sulphur humulone investment mixing machine are uniformly mixed, so
Air-flow crushing, final material fineness≤25 μm are crossed afterwards；
(3) preparation of pretilachlor missible oil：Reaction in reaction kettle is added in pretilachlor and emulsifier and obtains pretilachlor missible oil, it is standby
With；
(4) rotating granulation：Baiting valve is closed, is added an adsorbent into rotary pelleting machine, hermetic seal is opened, starts low speed rotation
Turn, low speed chopping, pretilachlor missible oil is at the uniform velocity added, control accelerates；It adds and starts high speed rotation 5 minutes, closed after being adjusted to low speed
Rotation is closed, hermetic seal, observation of uncapping are closed, until uniformly then this process is completed without particle；The material that step 2 prepares is added, bubble
It rises agent rotation to be uniformly mixed, adds adhesive, rotation, chopping open baiting valve after the completion of being granulated, particle releasing will have been made,
It crosses 12 mesh screens or vibrating screen sifts out larger particles, obtain uniform effervescence granular；
(5) it dries：Step 4 gained wet granular is dry to particle moisture content by drying machine<0.5%, it is spare, control drying
Machine air inlet humidity is 20% hereinafter, drying temperature is not higher than 60 DEG C in drying course；
(6) it packs.
Embodiment 3
A kind of Herbicidal combinations effervescent tablet, effective component are pyrazosulfuron, pretilachlor, furans sulphur humulone, the bubble
Effervescent tablet comprises the following components in parts by weight：3 parts of pyrazosulfuron, 15 parts of pretilachlor, 6 parts of furans sulphur humulone, 7 parts of dispersing agent, profit
4 parts of humectant, 30 parts of effervescent agent, 5 parts of adhesive, 1 part of excipient, 12 parts of emulsifier, 20 parts of adsorbent.
The dispersing agent is diisooctyl succinate sodium sulfonate；The wetting agent is aliphatic alcohol sulfate, succinic acid two
The combination of different dioctyl sodium sulfosuccinate, described adhesive are the mixture of polyvinylpyrrolidone and ethyl alcohol, mixed proportion 1:3, institute
Stating excipient is talcum powder, and the emulsifier is calcium dodecyl benzene sulfonate, and the adsorbent is zeolite powder.
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 combination of citric acid, cholic acid；The alkaline constituents is the combination of sodium carbonate, sodium bicarbonate.
The preparation method of above-mentioned Herbicidal combinations effervescent tablet, comprises the following steps that：
(1) weighing material；
(2) air-flow crushing：Dispersing agent, wetting agent, pyrazosulfuron, furans sulphur humulone investment mixing machine are uniformly mixed, so
Air-flow crushing is crossed afterwards to final material fineness≤25 μm；
(3) preparation of pretilachlor missible oil：Reaction in reaction kettle is added in pretilachlor and emulsifier and obtains pretilachlor missible oil, it is standby
With；
(4) rotating granulation：Baiting valve is closed, adds an adsorbent into rotary pelleting machine, then pretilachlor missible oil is added,
Rotation is uniformly mixed；The material that step 2 prepares is added, effervescent agent rotation is uniformly mixed, and adds adhesive, and rotation is shredded,
Baiting valve is opened after the completion of being granulated, will make particle releasing, 12 mesh screens is crossed or vibrating screen sifts out larger particles, is obtained uniform
Granulae effervescentes；
(5) it dries：Step 4 gained wet granular is dry by drying machine, control dryer entrance mouth humidity 20% with
Under, drying temperature is not higher than 60 DEG C in drying course, drying to particle moisture content<0.5%, it is spare；
(6) tabletting：Particle dried obtained by step 5, excipient investment mixing machine are uniformly mixed, tabletting is subsequently poured into
Machine carries out tabletting；Mixed material, which all needs to extrude, avoids the material stock moisture absorption；Tablet first is adjusted with manually before each tabletting of tablet press machine
Size, grammes per square metre, open electronic tabletting again after meeting the requirements, directly open and electronic be possible to push up bad punching pin；Ambient humidity controls when tabletting
30% hereinafter, extrude tablet answer rapid vacuum to pack, prevent in air the moisture absorption lead to the bag that rises；In tableting processes, if gone out
It is rough that existing sticking phenomenon leads to extrude tablet, can shut down cleaning, and when cleaning is necessary to switch off power supply, forbids out to stretch when electronic tabletting
Hand samples in tablet press machine, and tableting process terminates, and cuts off the power, and in time cleans out tablet press machine, especially by upper and lower punching pin
Viscous material is cleaned out, and otherwise can be difficult to clear up after the moisture absorption；
(7) it packs.
Embodiment 4
A kind of Herbicidal combinations effervescent tablet, effective component are pyrazosulfuron, pretilachlor, furans sulphur humulone, the bubble
Effervescent tablet comprises the following components in parts by weight：2 parts of pyrazosulfuron, 15 parts of pretilachlor, 2 parts of furans sulphur humulone, 5 parts of dispersing agent, profit
2 parts of humectant, 40 parts of effervescent agent, 9.5 parts of adhesive, 0.5 part of excipient, 6 parts of emulsifier, 20 parts of adsorbent.
The dispersing agent is sodium lignin sulfonate；The wetting agent is that pull open powder, aliphatic alcohol sulfate, succinic acid two are different
The combination of dioctyl sodium sulfosuccinate, described adhesive are that the mixture mixed proportion of polyvinylpyrrolidone and ethyl alcohol is 1:3, mixing
Weight ratio is 1:3, the excipient is talcum powder, and the emulsifier is calcium dodecyl benzene sulfonate, and the adsorbent is zeolite
Powder.
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 combination of citric acid, cholic acid；The alkaline constituents is the combination of sodium carbonate, sodium bicarbonate.
The preparation method of above-mentioned Herbicidal combinations effervescent tablet, comprises the following steps that：
(1) weighing material；
(2) air-flow crushing：Dispersing agent, wetting agent, pyrazosulfuron, furans sulphur humulone investment mixing machine are uniformly mixed, so
Air-flow crushing is crossed afterwards to final material fineness≤25 μm；
(3) preparation of pretilachlor missible oil：Reaction in reaction kettle is added in pretilachlor and emulsifier and obtains pretilachlor missible oil, it is standby
With；
(4) rotating granulation：Baiting valve is closed, adds an adsorbent into rotary pelleting machine, then pretilachlor missible oil is added,
Rotation is uniformly mixed；The material that step 2 prepares is added, effervescent agent rotation is uniformly mixed, and adds adhesive, and rotation is shredded,
Baiting valve is opened after the completion of being granulated, will make particle releasing, 12 mesh screens is crossed or vibrating screen sifts out larger particles, is obtained uniform
Granulae effervescentes；
(5) it dries：Step 4 gained wet granular is dry by drying machine, control dryer entrance mouth humidity 20% with
Under, drying temperature is not higher than 60 DEG C in drying course, drying to particle moisture content<0.5%, it is spare；
(6) tabletting：Particle dried obtained by step 5, excipient investment mixing machine are uniformly mixed, tabletting is subsequently poured into
Machine carries out tabletting；Mixed material, which all needs to extrude, avoids the material stock moisture absorption；Tablet first is adjusted with manually before each tabletting of tablet press machine
Size, grammes per square metre, open electronic tabletting again after meeting the requirements, directly open and electronic be possible to push up bad punching pin；Ambient humidity controls when tabletting
30% hereinafter, extrude tablet answer rapid vacuum to pack, prevent in air the moisture absorption lead to the bag that rises；In tableting processes, if gone out
It is rough that existing sticking phenomenon leads to extrude tablet, can shut down cleaning, and when cleaning is necessary to switch off power supply, forbids out to stretch when electronic tabletting
Hand samples in tablet press machine, and tableting process terminates, and cuts off the power, and in time cleans out tablet press machine, especially by upper and lower punching pin
Viscous material is cleaned out, and otherwise can be difficult to clear up after the moisture absorption；
(7) it packs.
The evaluation of 1 mixed effect of experimental example
Referring to synergy measuring method Colby method evaluation the using with the present invention relates to ternary composition of herbicide mixture
Effect.
Calculation formula is：
If E0For the theoretical preventive effect of single dose A, B, C after mixed；
A, B, C are respectively the actual measurement preventive effect of herbicide A, B, C under certain dosage；
If E is actual measurement preventive effect, calculation formula is：
If E is significantly less than E0, then it is synergistic effect；E and E0It is close, then it is summation action；E is significantly greater than E0, then it is antagonism
Effect.
Inventor carries out the different ratio of pyrazosulfuron, pretilachlor and furans sulphur humulone by a large amount of screening test
A large amount of efficiency test finds that in specific ratio range, obtained Herbicidal combinations have synergistic effect, antagonism
Weeds such as angustifolia arrowhead herb, firefly Lin, needle spikesedge herb etc. have excellent preventive effect.With the horizontal orthogonal experiment data of following three factor four
It is illustrated.
1 pyrazosulfuron of table, pretilachlor and furans sulphur humulone respectively match mixed effect
As seen from the above table, mixed by A, B, C ternary designed in the test of three factors, four horizontal quadrature, practical preventive effect is respectively less than
Theoretical preventive effect, i.e., it is each to match mixed more normal single dose respectively using with synergistic effect.When three's ratio range is at (1-5):
(15-75):When (1-15), three shows synergistic function, wherein 2:(15-55):Synergistic effect is significant when (1-15) range,
And A:B:C is 2:15:When 2, E-E0Value is equal to -22.77, and synergistic effect is most strong, as pyrazosulfuron, pretilachlor and furans sulphur grass
The most preferably proportion of ketone.
2 field experiment of experimental example
Effervescent formulation prepared by 1-4 of the embodiment of the present invention is referring to " National Standard of the People's Republic of China's pesticide field medicine
Imitate test rule (one) " field efficacy and safety testing are designed, it is mixed with mefenacet field with clear furans sulphur humulone
Effect.Specific test operation is as follows：
Test medicine：The effervescent formulation of embodiment 1-4 preparation；
Comparison medicament 1：10% pyrazosulfuron wettable powder；
Comparison medicament 2：30% pretilachlor missible oil；
Comparison medicament 3：27% fluorine ketone sulphur grass amine furans sulphur humulone (9+18) suspending agent；
Pilot survey object：Medicament is investigated to the preventive effect of weeds and total careless preventive effect, investigates the safety of medicine ensuing crop.
Experimental field be selected from Heilungkiang advance township transplanting rice field, field main weeds be prevention and treatment angustifolia arrowhead herb, firefly Lin, Monochoria korsakowii,
Needle spikesedge herb, barnyard grass, nutgrass flatsedge etc..
Spraying time：Rice transplanting turn green after 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 using it is spraying,
Pesticide-clay mixture or the fertile method application of poison.Water layer 3-5cm when application is retained 5-7 days, avoids water layer from flooding rice seedling lobus cardiacus, thereafter conventional tube
Reason.Local farming method is pressed in field management.
Quarter Design：The random district's groups arrangement of cell, 30 square metres of every cell, 4 repetitions.
Preventive effect investigation：Absolute-value scheme, every cell randomly choose at 4 points, and 0.25 square metre every is sampled, statistics weeds strain
Number calculates strain preventive effect (E1)。
CK0To be administered preceding number of weeds, CK1For number of weeds after application；Pt0Number of weeds before being administered for treatment region, Pt1For processing
Number of weeds after area's application.
Crop investigation：Observing medicament, whether there is or not phytotoxicity to crop, record the type and extent of phytotoxicity.Investigate medicine after 30d plant height,
The indexs such as tiller number, fresh weight.
Test result is as shown in table 2：
30d preventive effect after each weeds medicine of table 2
From the above data, composition dosage of the present invention is in 200-300ga.i./ha to local paddy field
Key resistance weeds needle spikesedge herb, lustrous and transparent Lin, angustifolia arrowhead herb total careless preventive effect up to 94% or more, and three kinds of active constituents are used alone
Total careless preventive effect of finished product control formulation is below 85%.Although comparison medicament 3, which is used alone, can reach 84.3% preventive effect, use
Medicine cost is higher than effervescent formulation of the present invention, and high production cost is unfavorable for peasant's increasing both production and income.
Chemical injury of crops reaction is observed after medicine：The present invention relates to each dosage processing of medicament to be showed no obvious symptom of chemical damage, leaf color
Normally, growing way is good.30 days after medicine, crop tiller number, strain fresh weight are investigated, specific data are shown in Table 3.
30d crop pattern index 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 (200ga.i./ha), each index value of times amount (400ga.i./ha) processing and blank control difference are not
Significantly.Comparison medicament inhibits paddy growth to a certain extent.To sum up, the present invention relates to compositions under recommended dose to for trying water
Rice safety, does not make significant difference to growth.
Claims (10)
1. a kind of effervescent formulation containing pyrazosulfuron, pretilachlor and furans sulphur humulone, which is characterized in that its effective component pyrrole is phonetic
Sulphur is grand, pretilachlor, the weight ratio of furans sulphur humulone are：1-5：10-75：1-15.
2. effervescent formulation according to claim 1, which is characterized in that the pyrazosulfuron, pretilachlor, furans sulphur humulone
Weight ratio is 3:15:6.
3. effervescent formulation according to claim 1, which is characterized in that the effervescent formulation is granulae effervescentes or effervescent tablet
Agent.
4. effervescent formulation according to claim 1, which is characterized in that comprise the following components in parts by weight：Pyrazosulfuron 1-5
Part, 10-75 parts of pretilachlor, 1-15 parts of furans sulphur humulone, 5-10 parts of dispersing agent, 1-6 parts of wetting agent, 15-50 parts of effervescent agent, bonding
3-8 parts of agent, 0.5-1.5 parts of excipient, 8-20 parts of emulsifier, 10-25 parts of adsorbent.
5. effervescent formulation according to claim 4, it is characterised in that：The dispersing agent is sodium lignin sulfonate, polycarboxylic acids
Salt, 2- naphthalene sulfonic acid formaldehyde polymer sodium salt, the aromatic compound sodium salt of sulfonation, alkyl naphthalene sodium sulfate salt, maleic-acrylic acid
One of copolymer sodium salt or a variety of combinations；The wetting agent is pull open powder, lauryl sodium sulfate, fatty alcohol sulphuric acid
One of salt, diisooctyl succinate sodium sulfonate or a variety of combinations；Described adhesive is polyvinyl alcohol, polyvinylpyrrolidine
One of ketone, polyethylene glycol, carboxymethyl cellulose, Arabic gum or the mixture of a variety of combinations and ethyl alcohol, mixed weight
Amount is than being 1:3.
6. effervescent formulation according to claim 4, it is characterised in that：The excipient is talcum powder, and the emulsifier is
One of calcium dodecyl benzene sulfonate, phenethyl phenol polyethenoxy ether or a variety of combinations, the adsorbent are gas phase hard charcoal
One of black, diatomite, magnesium stearate, kaolin, zeolite powder or a variety of combinations.
7. effervescent formulation according to claim 4, it is characterised in that：The effervescent agent includes acid constituents and alkaline constituents, institute
The weight ratio for stating acid constituents and alkaline constituents is 1:1, the acid constituents is tartaric acid, citric acid, citric acid, succinic acid, cholic acid, goes
One of oxycholic acid or a variety of combinations；The alkaline constituents is one of potassium carbonate sodium carbonate, sodium bicarbonate, saleratus
Or a variety of combination.
8. effervescent formulation according to claim 1, which is characterized in that comprise the following components in parts by weight：Pyrazosulfuron 2
Part, 15 parts of pretilachlor, 2 parts of furans sulphur humulone, 5 parts of dispersing agent, 2 parts of wetting agent, 40 parts of effervescent agent, 9.5 parts of adhesive, excipient
0.5 part, 6 parts of emulsifier, 20 parts of adsorbent.
9. the preparation method of any effervescent formulation of claim 1-8, which is characterized in that
The effervescent formulation is effervescent tablet, is comprised the following steps that：
(1) weighing material；
(2) air-flow crushing：Dispersing agent, wetting agent, pyrazosulfuron, furans sulphur humulone investment mixing machine are uniformly mixed, then mistake
Air-flow crushing is to final material fineness≤25 μm；
(3) preparation of pretilachlor missible oil：Reaction in reaction kettle is added in pretilachlor and emulsifier and obtains pretilachlor missible oil, it is spare；
(4) rotating granulation：Baiting valve is closed, adds an adsorbent into rotary pelleting machine, then pretilachlor missible oil is added, is rotated
It is uniformly mixed；The material that step 2 prepares is added, effervescent agent rotation is uniformly mixed, and adds adhesive, and rotation, chopping are granulated
Baiting valve is opened after the completion, will make particle releasing, crosses 12 mesh screens or vibrating screen sifts out larger particles, obtain uniform effervesce
Particle；
(5) it dries：Step 4 gained wet granular is dry by drying machine, dryer entrance mouth humidity is controlled 20% hereinafter, drying
Drying temperature is not higher than 60 DEG C during dry, drying to particle moisture content<0.5%, it is spare；
(6) tabletting：Dried particle obtained by step 5, excipient investment mixing machine are uniformly mixed, be subsequently poured into tablet press machine into
Row tabletting；
(7) it packs.
10. the preparation method of any effervescent formulation of claim 1-8, which is characterized in that
The effervescent formulation is granulae effervescentes, is comprised the following steps that：
(1) weighing material；
(2) air-flow crushing：Dispersing agent, wetting agent, pyrazosulfuron, furans sulphur humulone investment mixing machine are uniformly mixed, then mistake
Air-flow crushing is to final material fineness≤25 μm；
(3) preparation of pretilachlor missible oil：Reaction in reaction kettle is added in pretilachlor and emulsifier and obtains pretilachlor missible oil, it is spare；
(4) rotating granulation：Baiting valve is closed, adds an adsorbent into rotary pelleting machine, then pretilachlor missible oil is added, is rotated
It is uniformly mixed；The material that step 2 prepares is added, effervescent agent rotation is uniformly mixed, and adds adhesive, and rotation, chopping are granulated
Baiting valve is opened after the completion, will make particle releasing, crosses 12 mesh screens or vibrating screen sifts out larger particles, obtain uniform effervesce
Particle；
(5) it dries：Step 4 gained wet granular is dry by drying machine, dryer entrance mouth humidity is controlled 20% hereinafter, drying
Drying temperature is not higher than 60 DEG C during dry, drying to particle moisture content<0.5%, it is spare；
(6) it packs.
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| CN109566619A (en) * | 2018-12-26 | 2019-04-05 | 北京颖泰嘉和生物科技股份有限公司 | A kind of herbicidal composition and its application |
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