CN112314615A - Preparation method of water dispersible granules of herbicide - Google Patents
Preparation method of water dispersible granules of herbicide Download PDFInfo
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- CN112314615A CN112314615A CN202011164012.XA CN202011164012A CN112314615A CN 112314615 A CN112314615 A CN 112314615A CN 202011164012 A CN202011164012 A CN 202011164012A CN 112314615 A CN112314615 A CN 112314615A
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- carfentrazone
- ethyl
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- 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
- A01N25/12—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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a preparation method of 36% carfentrazone-ethyl tribenuron-methyl water dispersible granules, which comprise the following components: carfentrazone-ethyl, benzenesulfonic acid, kaolin, a mixture of alkyl naphthalene sulfonate and an anionic wetting agent, sodium lignosulfonate, sodium sulfate corn starch; wherein carfentrazone-ethyl and benzenesulfonic acid are raw medicinal components, kaolin is a carrier, a mixture EFW of alkyl naphthalene sulfonate and an anionic wetting agent is a wetting agent, sodium lignosulfonate is a dispersing agent, sodium sulfate is a disintegrating agent, and corn starch is a filler. The mixed components are pulverized by adopting airflow to 12-20 mu m. Then the multi-spiral compound mixer customized by the invention is used for uniform mixing, kneading, granulating, drying and screening. And (5) packaging after inspection. The invention improves the uniformity of the powder particle size distribution, reduces the recovery rate, lowers the production cost, reduces the average particle size of the powder, reduces the using amount of the wetting agent and obviously improves the content of effective components.
Description
Technical Field
The invention relates to the technical field of herbicide pesticides, in particular to a preparation method of water dispersible granules of a herbicide.
Background
Carfentrazone-ethyl, also known as clomazone-ethyl and carfentrazone-ethyl, is a viscous yellow liquid, and is a contact-type selective weeding light plant chlorophyll biosynthesis process, and carfentrazone-ethyl inhibits the activity of protoporphyrinogen oxidase to cause the accumulation of toxic intermediates, thereby destroying the cell membrane of weeds, and leading the leaves to be rapidly dried and dead. The herbicide is mainly used for preventing and killing broad-leaved weeds and sedge weeds in crop fields of wheat, barley, rice, corn and the like. Tribenuron-methyl is also named as giant star and broad-leaved weed, is a white solid, is a selective systemic conduction type herbicide, can be absorbed by the roots and leaves of weeds, and is conducted in plants. Tribenuron-methyl inhibits the activity of acetolactate synthase in plants, thereby affecting the biosynthesis of branched-chain amino acids. After the plants are damaged, the plants show that growing points are necrotic, veins are dark green, the growth is severely inhibited, the plants are dwarfed, and finally the whole plants die. The herbicide is mainly used for preventing and killing broadleaf weeds in wheat crop fields. The two effective components have different action mechanisms, and after being mixed, the weeding effect is improved, and the occurrence and the development of drug resistance are delayed.
The water dispersible granule is a new pesticide formulation developed in the 80 th of the 20 th century, has the advantages of solid preparation (granule and wettable powder) and liquid preparation (suspending agent), and is rapidly developed due to the organic solvent, no dust, and convenient packaging, transportation and use. As an important development direction of novel pesticide ring dosage forms, water dispersible granules become main dosage forms of pesticides at home and abroad in recent years. The main problem of the existing water dispersible granule production is that wettable powder needs to be prepared in the processing process, and due to the limitation of the grinding fineness and the mixing process, the effective components of the wettable powder are not uniform, and the content of the effective components of part of the product is difficult to be greater than the nominal content, so that the exertion of the drug effect of the finally obtained water dispersible granule product in the use process is influenced.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of carfentrazone-ethyl tribenuron-methyl water dispersible granules.
The complete technical scheme of the invention comprises the following steps:
a preparation method of 36% carfentrazone-ethyl tribenuron-methyl water dispersible granules comprises the following components: carfentrazone-ethyl, benzenesulfonic acid, kaolin, a mixture of alkyl naphthalene sulfonate and an anionic wetting agent, sodium lignosulfonate, sodium sulfate corn starch; wherein carfentrazone-ethyl and benzenesulfonic acid are raw medicinal components, kaolin is a carrier, a mixture EFW of alkyl naphthalene sulfonate and an anionic wetting agent is a wetting agent, sodium lignosulfonate is a dispersing agent, sodium sulfate is a disintegrating agent, and corn starch is a filler.
The method comprises the following steps:
(1) weighing raw material components with required content, mixing carfentrazone-ethyl, a carrier and a filler to realize adsorption to obtain a component A, and mixing tribenuron-methyl, a wetting agent, a dispersing agent and a disintegrating agent to obtain a component B;
(2) adding the component A and the component B into a double-helix conical mixer for preliminary pre-mixing to obtain a pre-mixture;
(3) crushing the mixture obtained in the step (2) by adopting airflow to obtain a crushed mixture, wherein the crushed mixture is 12-20 microns;
(4) adding the crushed mixture into a customized multi-spiral composite mixer for uniform mixing to obtain a rear mixture, namely wet powder;
(5) kneading the mixture in a kneader;
(6) feeding the kneaded product into a granulator for extrusion granulation;
(7) drying the product after the granulator in a fluidized bed dryer;
(8) screening the dried granules;
(9) and packaging after the inspection is qualified.
Drawings
FIG. 1 is a process flow of the preparation method of carfentrazone-ethyl tribenuron-methyl water dispersible granules disclosed by the invention.
FIG. 2 is a schematic diagram of a multi-helix hybrid mixer.
In the figure: 1-a first cylinder; 2-a second cylinder; 3, a connecting port; 4, supporting frames; 5 — a first inlet; 6-a second inlet; 7-main motor; 8, an auxiliary motor; 9-rotating arm; 10-a first screw rod; 11-a second screw rod; 12-a third screw rod; 13-a base; 14-discharge hole.
Detailed Description
The technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only illustrative and are not intended to limit the present application.
The implementation of the technical solution of the present invention is obtained, in part, based on the previous research result "36% carfentrazone-ethyl tribenuron-methyl water dispersible granule" (world pesticide, vol 36, No. 4, 2014, 8 months) of the present applicant, and further development and research of the preparation process are performed.
As shown in FIG. 1, the preparation process of the invention comprises the following steps:
(10) weighing raw material components with required content, mixing carfentrazone-ethyl, a carrier and a filler to realize adsorption to obtain a component A, and mixing tribenuron-methyl, a wetting agent, a dispersing agent and a disintegrating agent to obtain a component B.
(11) And adding the component A and the component B into a double-helix conical mixer for preliminary premixing to obtain a premixed material.
(12) And (3) crushing the mixture obtained in the step (2) by adopting airflow to obtain a crushed mixture, wherein the crushed mixture is crushed to 12-20 microns.
(13) The pulverized mixture is added into a multi-screw compound mixer customized by the invention for uniform mixing to obtain a post-mixture, namely wettable powder.
(14) The latter mixture is kneaded in a kneader.
(15) And (4) feeding the kneaded product into a granulator for extrusion granulation.
(16) The product after the granulator was dried in a fluid bed dryer.
(17) And screening the dried granules.
(18) And packaging after the inspection is qualified.
Each step is described in detail below:
the invention discloses carfentrazone-ethyl tribenuron-methyl water dispersible granules which comprise the following components: carfentrazone-ethyl, benzene sulfonic acid, kaolin, a mixture of alkyl naphthalene sulfonate and an anionic wetting agent, sodium lignosulfonate, sodium sulfate corn starch. Wherein carfentrazone-ethyl and benzenesulfonic acid are raw medicinal components, kaolin is a carrier, a mixture EFW of alkyl naphthalene sulfonate and an anionic wetting agent is a wetting agent, sodium lignosulfonate is a dispersing agent, sodium sulfate is a disintegrating agent, and corn starch is a filler.
In the composition, carfentrazone-ethyl and benzenesulfonic acid are raw medicinal components, the effective content of the carfentrazone-ethyl and benzenesulfonic acid is a key index of the product, and the carfentrazone-ethyl and benzenesulfonic acid are respectively divided into 22% of carfentrazone-ethyl and 14% of benzenesulfonic acid based on the previous research results. In the selection of the carrier, in order to ensure complete adsorption and granulation, the carrier content was determined to be 40% according to the previous research results. On the basis, through further research, the dispersibility, the suspensibility and the disintegration of the product are important factors directly influencing the use and the effect of the product in the use process, and in order to ensure that the water dispersible granules are well dispersed in water without precipitation, are fully wetted and can be quickly disintegrated to achieve a good use effect, the factors need to be comprehensively considered in a synergistic manner, and meanwhile, the production cost is also considered. Researches show that if the particle size of the airflow mixed product after airflow crushing is greatly reduced, the suspension rate after disintegration can be obviously improved, so that the particle size of the crushed mixture after airflow crushing is reduced to 12-20 mu m from the existing particle size of more than 35 mu m, the suspension rate in use is obviously improved, and the quality of the product is improved. But at the same time the corresponding amounts of wetting agent, dispersing agent and disintegrating agent need to be designed correspondingly. Through analysis and experiments on various parameters, according to different particle sizes of products after jet milling, the following use modes are set for determination:
d is defined when the particle size of the jet-milled product is 12 μm 012 μm, particle size P of the granulated water dispersible granule00.75mm, amount of dispersant d 010% of wetting agent L 03% of disintegrant0The content was 2.4%. The particle size of the jet-milled product herein was 12 μm, which means that the D95 particle size of the product was 12 μm, as follows.
When the product after jet milling has a particle size D1(greater than D)0) Particle size of the granule
Amount of dispersant used
Thus ensuring that finer comminuted mixture is not agglomeratedRelatively more dispersant is used for polymerization. Meanwhile, in order to ensure the disintegration time, the particle size of the granules prepared by finely crushing the mixture is smaller, the surface area is correspondingly increased, and the disintegration efficiency is improved. The particle size of the granules needs to be reduced properly, and more dispersing agent needs to be adopted because the particle size is fine and easy to agglomerate, but the dosage of the dispersing agent is 10 percent at most and 7 percent at most.
The overall components of the carfentrazone-ethyl tribenuron-methyl water dispersible granule component are defined as follows: 22% of carfentrazone-ethyl, 14% of benzenesulfonic acid, 40% of kaolin, EFW3% of a mixture of alkyl naphthalene sulfonate and an anionic wetting agent, 7-10% of sodium lignosulfonate, 2.4% of sodium sulfate and the balance of corn starch.
The innovation of the present invention in the preparation process with respect to step 4 is explained below. Because the original drug needs to be prepared into wettable powder in advance, as shown in steps 1-4 of the preparation method, the inventor finds that two problems often occur in the preparation of the wettable powder, firstly, the particle size of the product obtained after airflow pulverization in step (3) is often distributed unevenly, and the product needs to be sieved and recycled frequently, so that the production cost is increased, or the suspension rate and the dispersibility of the final water dispersible granule product are unstable. The other problem is that after the jet milling, the prior art generally adopts a double-helix conical mixer which is the same as the primary mixing for mixing, and after the mixing is finished, although the local components of the powder are relatively uniform, the condition of uneven content of the whole effective components often occurs, so that the problems of product use and quality occur, and the unqualified phenomenon is easily generated in part of production batches.
In order to solve the technical problems, the inventor analyzes the reasons for the problems, and finds that the reason for uneven particle size after jet milling is that the water content of the raw materials of different manufacturers and batches is different due to the used filler or carrier, and meanwhile, the raw materials are likely to be agglomerated due to the absorption of more water during transportation and long-term storage, and the particle size of the partially agglomerated filler or carrier is still larger after the subsequent jet milling, so that more coarse powder is remained after sieving and needs to be recovered. The second problem arises because the double helix conical mixer currently used cannot achieve sufficient uniform mixing and needs improvement.
In order to solve the problems, the filler and the carrier are firstly dried before primary mixing, so that the water content is reduced to a certain degree, researches and findings show that the water content of the filler is reduced to be below 2 percent, the water content of the carrier is reduced to be below 3.5 percent, the rotating speed and the mixing time of the double-helix conical mixer are properly increased in the primary mixing process, the uneven particle size distribution of a crushed product is greatly improved after air flow crushing, the recovery condition after sieving is reduced, and the production cost is reduced. In view of the second problem, the double-helix conical mixer adopted at present is improved, and a multi-helix composite mixer is obtained, the structure of which is shown in figure 2,
including the urceolus, this urceolus is including the first barrel of traditional back taper 1 that is located upper portion and the cylindricality second barrel 2 that is located its below, through connector 3 intercommunication between first barrel 1 and the second barrel 2, is equipped with support frame 4 on the first barrel 1. Be equipped with first entry 5 and second entry 6 on the first barrel 1, can add single raw materials through solitary entry, also can add different raw materials respectively through two entries, make the device can use when preliminary mixing, also can use when the secondary mixes, expanded the service function of the device. The main motor 7 is arranged above the first barrel 1, the auxiliary motor 8 is arranged on the base 13 below the second barrel, the main motor 7 is connected with the rotating arm 9 in the first barrel 1, the two sides of the rotating arm 9 are respectively connected with the first screw rod 10 and the second screw rod 11, the first screw rod 10 and the second screw rod 11 are the same as the structure of a traditional double-helix conical mixer, and are asymmetrically designed and different in length, and the upper surfaces of the first screw rod 10 and the second screw rod 11 are respectively provided with a screw blade to stir and mix raw materials. The auxiliary motor is connected with a third screw rod 12 in the second cylinder 2, a propeller blade is arranged on the third screw rod, and the radius of the propeller blade on the third screw rod is larger than that of the connecting port 3.
During stirring, the crushed product after airflow crushing is added from the first inlet above, then the first screw rod 10 and the second screw rod 11 revolve around the central shaft of the first cylinder under the rotation action of the rotating arm while performing self-transmission around the axes of the first screw rod and the second screw rod 11, so as to mix the powder, and analysis shows that although the first screw rod 10 and the second screw rod 11 can perform compound motions such as shearing, lifting and the like on the powder, due to the shape of the cylinder, a blind zone which is still insufficiently mixed is generated near the center above the cylinder, so that the blind zone becomes mixed, the powder in the part and the powder components near the screw rods generate difference, and the final product components are not uniform enough, therefore, the second cylinder is arranged below the first cylinder, the powder mixed above enters the second cylinder for secondary mixing, and the radius of the screw blade on the third screw rod is designed to be larger than the connecting port 3 and slightly smaller than the inner diameter of the second cylinder, all the powder can be fully mixed. Through carrying out experimental analysis to the mixing arrangement who newly develops, to the particle size mixing of particle size about 800 ~ 1250 meshes, make the propeller blade diameter on the third hob be about 1.2 times of connector internal diameter, and the rotational speed of third hob is about 1.8 ~ 2.0 times of first, two hob rotational speeds, can show the homogeneity that improves the final product, consequently design adoption this parameter, the powder that finishes mixing gets into the kneader and kneads after sending out from the discharge gate of second barrel one side.
The invention obtains another innovation point that the fineness of the powder after the air flow grinding is obviously improved, the particle size of the existing main wettable powder product is mainly about 400 meshes, and the particle size is more than 35 mu m, because the smaller the particle size of the air flow grinding is, the larger the non-uniformity of the particle size distribution is, the more the powder is left after sieving, according to the prior test, when the particle size of the powder is reduced from 400 meshes to 600 meshes, the sieving amount after the grinding is reduced to 74-80%, and the individual batch is even below 70%. And the powder left by the screen is mixed with the filler additive, so that the components are difficult to determine, and the powder cannot be reused as a raw material, thereby causing great waste and increasing the production cost. After the kaolin and the corn starch are dried, the method provided by the invention increases the current powder from 400 meshes to 800-1250 meshes, reduces the particle size from the current more than 35 mu m to 12-20 mu m, and ensures that the sieving amount is more than or equal to 95%. The ultrafine powder agent obviously improves the suspension rate in use, reduces the using amount of a wetting agent and a disintegrating agent, and obviously improves the content of effective components.
The above applications are only some embodiments of the present application. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept herein, and it is intended to cover all such modifications and variations as fall within the scope of the invention.
Claims (2)
1. A preparation method of 36% carfentrazone-ethyl tribenuron-methyl water dispersible granules is characterized in that the carfentrazone-ethyl tribenuron-methyl water dispersible granules comprise the following components: carfentrazone-ethyl, benzenesulfonic acid, kaolin, a mixture of alkyl naphthalene sulfonate and an anionic wetting agent, sodium lignosulfonate, sodium sulfate corn starch; wherein carfentrazone-ethyl and benzenesulfonic acid are raw medicine components, kaolin is a carrier, a mixture EFW of alkyl naphthalene sulfonate and an anionic wetting agent is a wetting agent, sodium lignosulfonate is a dispersing agent, sodium sulfate is a disintegrating agent, and corn starch is a filler;
the method comprises the following steps:
(1) weighing raw material components with required content, mixing carfentrazone-ethyl, a carrier and a filler to realize adsorption to obtain a component A, and mixing tribenuron-methyl, a wetting agent, a dispersing agent and a disintegrating agent to obtain a component B;
(2) adding the component A and the component B into a double-helix conical mixer for preliminary pre-mixing to obtain a pre-mixture;
(3) performing jet milling on the mixed mixture obtained in the step (2), and performing ultrafine milling to 12-20 microns to obtain a milled mixture;
(4) adding the crushed mixture into a customized multi-spiral composite mixer for uniform mixing to obtain a rear mixture, namely wet powder;
(5) kneading the mixture in a kneader;
(6) feeding the kneaded product into a granulator for extrusion granulation;
(7) drying the product after the granulator in a fluidized bed dryer;
(8) screening the dried granules;
(9) and packaging after the inspection is qualified.
2. The preparation method of 36% carfentrazone-ethyl tribenuron-methyl water dispersible granules according to claim 1, wherein the overall composition of the carfentrazone-ethyl tribenuron-methyl water dispersible granules is defined as follows: 22% of carfentrazone-ethyl, 14% of benzenesulfonic acid, 40% of kaolin, EFW3% of a mixture of alkyl naphthalene sulfonate and an anionic wetting agent, 7-10% of sodium lignosulfonate, 2.4% of sodium sulfate and the balance of corn starch.
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Citations (4)
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|---|---|---|---|---|
| CN102017973A (en) * | 2010-12-30 | 2011-04-20 | 苏州富美实植物保护剂有限公司 | Weeding composition for wheat field |
| CN102885049A (en) * | 2012-10-12 | 2013-01-23 | 河北亚光精细化工有限公司 | Bromo-3-chloro-5,5-dimethyhydantoin wettable powder and production method thereof |
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| CN208194263U (en) * | 2018-03-30 | 2018-12-07 | 安徽笃舜智能装备有限公司 | Ribbon mixer |
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2020
- 2020-10-27 CN CN202011164012.XA patent/CN112314615B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102017973A (en) * | 2010-12-30 | 2011-04-20 | 苏州富美实植物保护剂有限公司 | Weeding composition for wheat field |
| CN102885049A (en) * | 2012-10-12 | 2013-01-23 | 河北亚光精细化工有限公司 | Bromo-3-chloro-5,5-dimethyhydantoin wettable powder and production method thereof |
| CN107125256A (en) * | 2017-07-14 | 2017-09-05 | 安徽海日生物科技有限公司 | A kind of tribenuron-methyl and azoles humulone built wettable powder and preparation method thereof |
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