CN113197213B - Sulfoxaden dry suspending agent and preparation method thereof - Google Patents
Sulfoxaden dry suspending agent and preparation method thereof Download PDFInfo
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- CN113197213B CN113197213B CN202110319560.3A CN202110319560A CN113197213B CN 113197213 B CN113197213 B CN 113197213B CN 202110319560 A CN202110319560 A CN 202110319560A CN 113197213 B CN113197213 B CN 113197213B
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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
- A01N43/80—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 1,2
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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
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- Agronomy & Crop Science (AREA)
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Abstract
The invention provides a sufonazole dry suspending agent and a preparation method thereof, the dry suspending agent comprises active components of sufonazole, polycarboxylate, bentonite, disintegrant and dispersant, the active components, the polycarboxylate, the bentonite, the disintegrant, the dispersant and water are uniformly mixed in the preparation process, after mixing, the active components, the polycarboxylate, the bentonite, the disintegrant, the dispersant and the water are sanded and dispersed to prepare suspension liquid with solid particles with the particle size of less than 10 mu m, then the obtained suspension liquid is subjected to spray drying granulation, the spray dried particles are collected, and the dry suspending agent is obtained after screening. The sulfonepyraflufen-ethyl dry suspending agent prepared by the method has good prevention and control effect and stable physical and chemical properties, and is not easy to decompose and deteriorate to cause phytotoxicity; the suspension rate reaches more than 98 percent, only one-time dispersion is needed in the using process, the disintegration time is within 10s, and the using process is simple; the flowability is good, the wall is not adhered after pouring, and the secondary pollution cannot be formed after the pouring is left in the packaging container.
Description
Technical Field
The invention belongs to the technical field of pesticide herbicides, and particularly relates to an isoxazole herbicide sulfonylpyraflufen-ethyl dry suspending agent and a preparation method thereof.
Background
Pyraflufen (Pyroxasulfone) is an isoxazole herbicide developed by japan combinatorial chemistry, and exerts its medicinal effect by inhibiting very long chain fatty acid elongation synthase (VLCFAE) by a herbicide belonging to the genus pyraflufen. Since the development success, the variety is widely regarded and highly evaluated. The combination chemistry and lharamical company signed an authorization for sulfonepyrazazole with basf, allowing us and canada to sell such products for crops such as corn, soybean, and sunflower. At present, the formulation of the sulfonylpyraflufen herbicide is 40% of suspending agent and 40% of water dispersible granules, but the sulfonylpyraflufen suspending agent is easy to decompose and delaminate, has poor stability and inconvenient use, and reduces the weeding efficiency; the water dispersible granule of the sulfuryl pyraflufen-ethyl needs to be dispersed for the second time in the using process, and the fineness of the dispersed particles is thicker and basically about 40 mu m; the disintegration time is long, generally about 60 s; the suspending agent is low, generally not higher than 85%, the weeding effect is poor, the using process is complicated, and the weeding efficiency is reduced.
Disclosure of Invention
The invention aims to provide an isoxazole herbicide, namely a pyriftalid dry suspending agent, which has good control effect, stable physical and chemical properties and difficult decomposition and deterioration on the basis of the prior art; the finished product is granular solid, has good fluidity, does not stick to the wall after being poured, and cannot remain in a packaging container to form secondary pollution.
The invention also aims to provide a preparation method of the sulfuryl pyraflufen-ethyl dry suspending agent.
The technical scheme of the invention is as follows:
the preparation process of the dry suspending agent comprises the steps of uniformly mixing the active component, the polycarboxylate, the bentonite, the disintegrating agent, the dispersing agent and water, carrying out sand grinding and dispersing after mixing to prepare suspension liquid with solid particles with the particle size of less than 10 mu m, carrying out spray drying and granulation on the obtained suspension liquid, collecting the particles after spray drying, and screening to obtain the dry suspending agent.
Wherein the dry suspending agent comprises the following components in parts by weight: 25-50 parts of pyraflufen-ethyl, 2-5 parts of polycarboxylate, 37-64 parts of bentonite, 2-5 parts of disintegrant and 3-6 parts of dispersant; wherein the disintegrant is sodium carboxymethyl starch, polyvidone or their combination; the dispersant is one or more of p-methoxyl fatty amide benzene sulfonic acid sodium salt, lignosulfonate, butyl naphthalene sodium sulfonate, castor oil polyoxyethylene ether or lauryl sodium sulfate.
For the purposes of the present invention, the parameters of spray drying during the spray drying granulation are as follows: the air inlet temperature is 100-120 ℃, the air outlet temperature is 50-70 ℃, and the feeding speed is controlled to keep the moisture in the discharged product within 1.5 percent during spray drying.
In a preferred scheme, the sulfuryl pyraflufen-ethyl dry suspending agent provided by the invention comprises the following components in parts by weight: 25 parts of sulfonepyraflufen-ethyl, 2 parts of polycarboxylate, 64 parts of bentonite, 3 parts of lignosulfonate, 3 parts of sodium carboxymethyl starch and 3 parts of sodium p-methoxy fatty amido benzene sulfonate.
In a preferred scheme, the sulfuryl pyraflufen-ethyl dry suspending agent provided by the invention comprises the following components in parts by weight: 40 parts of sulfonepyraflufen-ethyl, 5 parts of polycarboxylate, 47 parts of bentonite, 5 parts of povidone and 3 parts of sodium butylnaphthalene sulfonate.
In a preferred scheme, the sulfuryl pyraflufen-ethyl dry suspending agent provided by the invention comprises the following components in parts by weight: 50 parts of pyraflufen-ethyl, 5 parts of polycarboxylate, 37 parts of bentonite, 5 parts of castor oil polyoxyethylene ether, 2 parts of sodium carboxymethyl starch and 1 part of sodium dodecyl sulfate.
The invention also provides a preparation method of the sulfuryl pyraflufen-ethyl dry suspending agent, which comprises the following steps:
(1) uniformly mixing an active component, polycarboxylate, bentonite, a disintegrating agent, a dispersing agent and water, and performing sand grinding dispersion in the mixing process to prepare a suspension, wherein the particle size of solid particles in the suspension is less than 10 mu m;
(2) carrying out spray drying granulation on the suspension obtained in the step (1), and collecting spray-dried particles;
(3) and (3) screening the particles obtained in the step (2) to obtain spherical uniform particles.
In a preferred embodiment, in step (1), the mixture is subjected to sand milling dispersion during mixing to prepare a suspension, wherein the particle size of solid particles in the suspension is 3-5 μm.
In the step (2), the spray drying parameters in the spray drying granulation are as follows: the air inlet temperature is 100-120 ℃, the air outlet temperature is 50-70 ℃, and the feeding speed is controlled to keep the moisture in the discharged product within 1.5 percent during spray drying.
In a preferred embodiment, in step (3), after sieving, spherical uniform particles having a particle size of 20 to 100 mesh, preferably 50 to 80 mesh, are obtained.
Further, in the step (1), preparing a suspension by sanding and dispersing by using a sand mill; in the step (2), a cyclone separator and a bag-type dust collector are adopted to collect the spray-dried particles.
The preparation method of the pyriflufen-sodium dry suspending agent comprises the following more detailed steps:
(1) uniformly mixing an active component, polycarboxylate, bentonite, a disintegrating agent, a dispersing agent and water in a shearing kettle, and after mixing, performing sand grinding and dispersing to prepare a suspension of solid particles with the particle size of less than 10 mu m;
(2) pumping the suspension obtained in the step (1) into a spray granulation tower for spray drying granulation, and collecting spray-dried particles through a cyclone separator and a bag-type dust collector; in spray drying granulation, the parameters of spray drying are as follows: the air inlet temperature is 100-120 ℃, the air outlet temperature is 50-70 ℃, and the feeding speed is controlled to keep the moisture in the discharged product within 1.5 percent during spray drying.
(3) Screening the particles obtained in the step (2) to obtain spherical uniform particles with the particle size of 20-100 meshes, preferably 50-80 meshes.
By adopting the technical scheme of the invention, the advantages are as follows:
the provided sulpirenoconazole dry suspending agent has good prevention and control effect and stable physical and chemical properties, and is not easy to decompose and deteriorate to cause phytotoxicity; the suspension rate reaches more than 98 percent, only one-time dispersion is needed in the using process, the disintegration time is within 10s, and the using process is simple. In addition, the dry suspending agent is granular solid, has good fluidity, does not stick to the wall after being poured, and cannot remain in a packaging container to form secondary pollution.
Detailed Description
The present invention will be further illustrated by the following examples, but these examples are not intended to limit the present invention in any way.
Example 1: the 25% sulfuryl pyraflufen-ethyl dry suspending agent comprises the following components in parts by weight:
the preparation method comprises the following steps:
(1) uniformly mixing the pyraflufen-ethyl, the polycarboxylate, the lignosulfonate, the p-methoxy fatty amide benzene sulfonate, the bentonite and water in a shearing kettle, and grinding and dispersing the mixture to prepare suspension liquid, wherein the particle size of solid particles in the suspension liquid is 3-5 mu m.
(2) Pumping the suspension obtained in the step (1) into a spray granulation tower for spray drying granulation, and collecting spray-dried particles through a cyclone separator and a bag-type dust collector; in spray drying granulation, the parameters of spray drying are as follows: the air inlet temperature is 100-120 ℃, the air outlet temperature is 50-70 ℃, and the feeding speed is controlled to keep the moisture in the discharged product within 1.5 percent during spray drying.
(3) And (3) screening the particles obtained in the step (2) to obtain spherical uniform particles with the particle size of 50-80 meshes.
Example 2: the 40% pyraflufen-ethyl dry suspending agent comprises the following components in parts by weight:
the preparation method comprises the following steps:
(1) uniformly mixing the sulfonepyraclonil, polycarboxylate, povidone, sodium butylnaphthalene sulfonate, bentonite and water in a shearing kettle, and grinding and dispersing the mixture to prepare suspension, wherein the particle size of solid particles in the suspension is 3-5 mu m.
(2) Pumping the suspension obtained in the step (1) into a spray granulation tower for spray drying granulation, and collecting spray-dried particles through a cyclone separator and a bag-type dust collector; in spray drying granulation, the parameters of spray drying are as follows: the air inlet temperature is 100-120 ℃, the air outlet temperature is 50-70 ℃, and the feeding speed is controlled to keep the moisture in the discharged product within 1.5 percent during spray drying.
(3) And (3) screening the particles obtained in the step (2) to obtain spherical uniform particles with the particle size of 50-80 meshes.
Example 3: the 50% sulfuryl pyraflufen-ethyl dry suspending agent comprises the following components in parts by weight:
the preparation method comprises the following steps:
(1) the preparation method comprises the following steps of uniformly mixing the sulfuryl pyraflufen-ethyl, the polycarboxylate, the castor oil polyoxyethylene ether, the sodium dodecyl sulfate, the sodium carboxymethyl starch, the bentonite and water in a shearing kettle, and grinding and dispersing the mixture to prepare a suspension, wherein the particle size of solid particles in the suspension is 3-5 mu m.
(2) Pumping the suspension obtained in the step (1) into a spray granulation tower for spray drying granulation, and collecting spray-dried particles through a cyclone separator and a bag-type dust collector; in spray drying granulation, the parameters of spray drying are as follows: the air inlet temperature is 100-120 ℃, the air outlet temperature is 50-70 ℃, and the feeding speed is controlled to keep the moisture in the discharged product within 1.5 percent during spray drying.
(3) And (3) screening the particles obtained in the step (2) to obtain spherical uniform particles with the particle size of 50-80 meshes. Comparative example 1: the 40% sulfonepyraflufen-ethyl water dispersible granule comprises the following components in parts by weight: different preparation methods
The preparation method comprises the following steps:
crushing and mixing active components of the sufonazole and an auxiliary agent (polycarboxylate, polyvidone, sodium butylnaphthalene sulfonate and bentonite) for 20 minutes, putting the obtained mixture into a double-helix mixer (I), crushing the mixture by a jet mill while mixing to reach the particle size of more than 800 meshes, collecting the mixture by a cyclone separator and a bag-type dust remover, and finally mixing the mixture again in a double-helix mixer (II) to obtain uniform powder with the particle size of 30-70 mu m. Accurately weighing quantitative powder in a rolling ball granulator, spraying water, sieving to obtain wet granules of 20-100 meshes, drying, sieving to obtain uniform spherical granules of 20-100 meshes, metering, and packaging.
Comparative example 2: the 40% sulfonepyraflufen-ethyl water dispersible granule comprises the following components in parts by weight:
the preparation method comprises the following steps:
(1) uniformly mixing the sulfonepyraflufen-ethyl, the polycarboxylate, the sodium carboxymethylcellulose, the fatty alcohol-polyoxyethylene ether, the bentonite and the water in a shearing kettle, and after mixing, performing sand grinding dispersion to prepare a suspension, wherein the particle size of solid particles in the suspension is 3-5 mu m.
(2) Pumping the suspension obtained in the step (1) into a spray granulation tower for spray drying granulation, and collecting spray-dried particles through a cyclone separator and a bag-type dust collector; in spray drying granulation, the parameters of spray drying are as follows: the air inlet temperature is 100-120 ℃, the air outlet temperature is 50-70 ℃, and the feeding speed is controlled to keep the moisture in the discharged product within 1.5 percent during spray drying.
(3) And (3) screening the particles obtained in the step (2) to obtain spherical uniform particles with the particle size of 50-80 meshes. Comparative example 3: the 40% sulfonepyrazoxazole water suspending agent comprises the following components in parts by weight: components and methods of preparation
The preparation method comprises the following steps:
mixing and dispersing the sulfonepyraclonil, the additives (polycarboxylate, sodium butylnaphthalene sulfonate, povidone, bentonite, glycol and xanthan gum) and water in a shearing kettle according to a formula ratio for 20 minutes, then throwing the obtained mixture into a sand mill for sand milling to obtain a suspension, detecting, measuring and packaging the suspension, wherein the particle size of solid particles in the suspension is 3-5 mu m.
Effect data:
the dry suspension of the sulfurmeprazole prepared in the example (25%, 40% and 50%), the water dispersible granule of the sulfurmeprazole prepared in the comparative example 1 and the comparative example 2 (40%) and the water suspension of the sulfurmeprazole prepared in the comparative example 3 (40%) were tested for herbicidal effect on wheat, and the specific test results are shown in table 1.
TABLE 1 herbicidal Effect data
As can be seen from Table 1, the dry suspending agent prepared in the examples of the present invention has a weeding effect higher than that of the water suspending agent and the water dispersible granule prepared in the comparative examples by about 6-7% in gramineae and about 10% in broadleaf weeds.
The content stability tests were performed on the dry suspension of pyraflufen-ethyl prepared in example (25%, 40% and 50%) and the aqueous suspension of pyraflufen-ethyl prepared in comparative example 3 (40%), and the specific test results are shown in table 2.
Table 2 content stability test data
As can be seen from Table 2, the dry suspensions prepared in the examples of the present invention are superior in thermal stability and storage stability to the aqueous suspensions prepared in the comparative examples.
The dry suspension agent of the sulfurous pyraflufen prepared in the example (25%, 40% and 50%) and the water dispersible granule of the sulfurous pyraflufen prepared in the comparative example 1 and the comparative example 2 (40%) are subjected to a disintegration time test, and the specific test results are shown in table 3.
Table 3 disintegration time test data
As can be seen from Table 3, the dry suspension prepared in the examples of the present invention has a faster disintegration rate than the water dispersible granule prepared in the comparative example, and the disintegration effect is not affected even when stored at 54 ℃ and 70 ℃ for one or two years. The dry suspending agent prepared in the embodiment of the invention does not need to be repeatedly stirred in the using process, and is more convenient to use.
The suspension rate test was performed on the dry suspension agent of sulfurous pyraflufen prepared in example (25%, 40% and 50%) and the water dispersible granule of sulfurous pyraflufen prepared in comparative example 1 and comparative example 2 (40%), and the specific test results are shown in table 4.
Table 4 suspension test data
As can be seen from Table 4, the dry suspending agent prepared in the examples of the present invention has a higher suspension rate than the water dispersible granule prepared in the comparative example, and does not affect the suspending effect even when stored at 54 ℃ and 70 ℃ for one or two years. It is fully demonstrated that the dry suspending agent of the invention has better field efficacy than water dispersible granules.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: modifications of the technical solutions described in the foregoing embodiments are still possible, or some technical features may be equivalently replaced; and these modifications or substitutions do not depart from the spirit of the corresponding technical solutions of the embodiments of the present invention.
Claims (3)
1. The sulfuryl pyraflufen-ethyl dry suspending agent is characterized by comprising the following components in parts by weight:
40 parts of xaflufen;
5 parts of polycarboxylate;
5 parts of polyvidone;
3 parts of sodium butylnaphthalenesulfonate;
47 parts of bentonite;
60 parts of water;
the preparation method comprises the following steps:
(1) uniformly mixing the sulfonepyraclonil, polycarboxylate, povidone, sodium butylnaphthalene sulfonate, bentonite and water in a shearing kettle, and after mixing, performing sand grinding and dispersion to prepare suspension, wherein the particle size of solid particles in the suspension is 3-5 mu m;
(2) pumping the suspension obtained in the step (1) into a spray granulation tower for spray drying granulation, and collecting spray-dried particles through a cyclone separator and a bag-type dust collector; in spray drying granulation, the parameters of spray drying are as follows: the air inlet temperature is 100-120 ℃, the air outlet temperature is 50-70 ℃, and the feeding speed is controlled to keep the moisture in the discharged product within 1.5 percent during spray drying;
(3) and (3) screening the particles obtained in the step (2) to obtain spherical uniform particles with the particle size of 50-80 meshes.
2. The sulfuryl pyraflufen-ethyl dry suspending agent is characterized by comprising the following components in parts by weight:
25 parts of xaflufen;
2 parts of polycarboxylate;
3 parts of lignosulfonate;
3 parts of sodium carboxymethyl starch;
3 parts of sodium p-methoxylipoamide benzene sulfonate;
64 parts of bentonite;
60 parts of water;
the preparation method comprises the following steps:
(1) uniformly mixing the pyraflufen-ethyl, the polycarboxylate, the lignosulfonate, the sodium carboxymethyl starch, the sodium p-methoxyfatty amide benzene sulfonate, the bentonite and water in a shearing kettle, and grinding and dispersing the mixture to prepare suspension liquid, wherein the particle size of solid particles in the suspension liquid is 3-5 mu m;
(2) pumping the suspension obtained in the step (1) into a spray granulation tower for spray drying granulation, and collecting spray-dried particles through a cyclone separator and a bag-type dust collector; in spray drying granulation, the parameters of spray drying are as follows: the air inlet temperature is 100-120 ℃, the air outlet temperature is 50-70 ℃, and the feeding speed is controlled to keep the moisture in the discharged product within 1.5 percent during spray drying;
(3) and (3) screening the particles obtained in the step (2) to obtain spherical uniform particles with the particle size of 50-80 meshes.
3. The pyriftalid dry suspending agent is characterized by comprising the following components in parts by weight:
50 parts of pyraflufen-ethyl;
5 parts of castor oil polyoxyethylene ether;
5 parts of polycarboxylate;
1 part of sodium dodecyl sulfate;
2 parts of sodium carboxymethyl starch;
37 parts of bentonite;
60 parts of water;
the preparation method comprises the following steps:
(1) uniformly mixing the sulfonepyraflufen-ethyl, the polycarboxylate, the castor oil polyoxyethylene ether, the sodium dodecyl sulfate, the sodium carboxymethyl starch, the bentonite and the water in a shearing kettle, and sanding and dispersing the mixture to prepare a suspension, wherein the particle size of solid particles in the suspension is 3-5 mu m;
(2) pumping the suspension obtained in the step (1) into a spray granulation tower for spray drying granulation, and collecting spray-dried particles through a cyclone separator and a bag-type dust collector; in spray drying granulation, the parameters of spray drying are as follows: the air inlet temperature is 100-120 ℃, the air outlet temperature is 50-70 ℃, and the feeding speed is controlled to keep the moisture in the discharged product within 1.5 percent during spray drying;
(3) and (3) screening the particles obtained in the step (2) to obtain spherical uniform particles with the particle size of 50-80 meshes.
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