CN114176088A - Azoxystrobin dry suspending agent and preparation method thereof - Google Patents
Azoxystrobin dry suspending agent and preparation method thereof Download PDFInfo
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- CN114176088A CN114176088A CN202111471142.2A CN202111471142A CN114176088A CN 114176088 A CN114176088 A CN 114176088A CN 202111471142 A CN202111471142 A CN 202111471142A CN 114176088 A CN114176088 A CN 114176088A
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- Prior art keywords
- azoxystrobin
- suspending agent
- dry suspending
- agent
- lignin
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- 239000005730 Azoxystrobin Substances 0.000 title claims abstract description 62
- WFDXOXNFNRHQEC-GHRIWEEISA-N azoxystrobin Chemical compound CO\C=C(\C(=O)OC)C1=CC=CC=C1OC1=CC(OC=2C(=CC=CC=2)C#N)=NC=N1 WFDXOXNFNRHQEC-GHRIWEEISA-N 0.000 title claims abstract description 62
- 239000000375 suspending agent Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000008186 active pharmaceutical agent Substances 0.000 claims abstract description 31
- 239000002270 dispersing agent Substances 0.000 claims abstract description 28
- 239000007787 solid Substances 0.000 claims abstract description 18
- 239000000080 wetting agent Substances 0.000 claims abstract description 17
- 125000000129 anionic group Chemical group 0.000 claims abstract description 16
- 229920005610 lignin Polymers 0.000 claims abstract description 14
- 229920005552 sodium lignosulfonate Polymers 0.000 claims abstract description 13
- 239000000945 filler Substances 0.000 claims abstract description 10
- 239000000575 pesticide Substances 0.000 claims abstract description 10
- 229920005551 calcium lignosulfonate Polymers 0.000 claims abstract description 6
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims description 19
- 239000002002 slurry Substances 0.000 claims description 14
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims description 8
- 238000001694 spray drying Methods 0.000 claims description 8
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000004576 sand Substances 0.000 claims description 6
- 238000010008 shearing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 5
- 239000011575 calcium Substances 0.000 claims description 5
- 239000011324 bead Substances 0.000 claims description 3
- UDHMTPILEWBIQI-UHFFFAOYSA-N butyl naphthalene-1-sulfonate;sodium Chemical compound [Na].C1=CC=C2C(S(=O)(=O)OCCCC)=CC=CC2=C1 UDHMTPILEWBIQI-UHFFFAOYSA-N 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- 238000005469 granulation Methods 0.000 claims description 3
- 230000003179 granulation Effects 0.000 claims description 3
- 230000002572 peristaltic effect Effects 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- 239000007921 spray Substances 0.000 claims description 3
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Inorganic materials [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 2
- 239000003814 drug Substances 0.000 abstract description 8
- 229940079593 drug Drugs 0.000 abstract description 8
- 239000004480 active ingredient Substances 0.000 abstract description 3
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 27
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- 238000011282 treatment Methods 0.000 description 7
- 201000010099 disease Diseases 0.000 description 6
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 6
- 239000005995 Aluminium silicate Substances 0.000 description 5
- 235000012211 aluminium silicate Nutrition 0.000 description 5
- 230000000857 drug effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000008187 granular material Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000009736 wetting Methods 0.000 description 4
- 241000207199 Citrus Species 0.000 description 3
- JIJAYWGYIDJVJI-UHFFFAOYSA-N butyl naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S(=O)(=O)OCCCC)=CC=CC2=C1 JIJAYWGYIDJVJI-UHFFFAOYSA-N 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- 235000020971 citrus fruits Nutrition 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 239000003899 bactericide agent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000004359 castor oil Substances 0.000 description 2
- 235000019438 castor oil Nutrition 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 2
- 239000008233 hard water Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000003090 pesticide formulation Substances 0.000 description 2
- 229920005646 polycarboxylate Polymers 0.000 description 2
- 229940051841 polyoxyethylene ether Drugs 0.000 description 2
- 229920000056 polyoxyethylene ether Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000010159 Duncan test Methods 0.000 description 1
- 208000031888 Mycoses Diseases 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- ABUGVBRDFWGJRD-CHOYNLESSA-N [9-[(2r,3r,4s,5r)-3,4-dihydroxy-5-methyloxolan-2-yl]-2-(2,4-dinitrophenyl)sulfanylpurin-6-yl] [hydroxy(phosphonooxy)phosphoryl] hydrogen phosphate Chemical compound O[C@@H]1[C@H](O)[C@@H](C)O[C@H]1N1C2=NC(SC=3C(=CC(=CC=3)[N+]([O-])=O)[N+]([O-])=O)=NC(OP(O)(=O)OP(O)(=O)OP(O)(O)=O)=C2N=C1 ABUGVBRDFWGJRD-CHOYNLESSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- OCKWRSQKDJOGNJ-UHFFFAOYSA-L dipotassium;[2,3,4-tris(2-phenylethenyl)phenyl] phosphate Chemical class [K+].[K+].C=1C=CC=CC=1C=CC1=C(C=CC=2C=CC=CC=2)C(OP([O-])(=O)[O-])=CC=C1C=CC1=CC=CC=C1 OCKWRSQKDJOGNJ-UHFFFAOYSA-L 0.000 description 1
- 239000007884 disintegrant Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 229920003063 hydroxymethyl cellulose Polymers 0.000 description 1
- 229940031574 hydroxymethyl cellulose Drugs 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- PSZYNBSKGUBXEH-UHFFFAOYSA-M naphthalene-1-sulfonate Chemical group C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 PSZYNBSKGUBXEH-UHFFFAOYSA-M 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 230000002085 persistent effect Effects 0.000 description 1
- -1 polyoxyethylene Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- LGORLCOUTMVEAC-UHFFFAOYSA-M sodium;2-nonylphenolate Chemical compound [Na+].CCCCCCCCCC1=CC=CC=C1[O-] LGORLCOUTMVEAC-UHFFFAOYSA-M 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 239000004546 suspension concentrate Substances 0.000 description 1
- 230000002459 sustained effect Effects 0.000 description 1
- 238000013268 sustained release Methods 0.000 description 1
- 239000012730 sustained-release form Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
-
- 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
- A01N25/30—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
Abstract
The invention relates to an azoxystrobin dry suspending agent and a preparation method thereof, belonging to the technical field of pesticide preparation. The azoxystrobin dry suspending agent comprises the following components in percentage by mass: 40-60% of azoxystrobin technical, 4-10% of solid wetting agent, 7-20% of lignin, 1-5% of anionic dispersing agent and the balance of filler, wherein the balance is added to 100%; the lignin is sodium lignosulfonate and/or calcium lignosulfonate; the anionic dispersant is GY-DS 1287. The GY-DS 1287 dispersing agent and the anionic solid wetting agent used in the azoxystrobin dry suspending agent have good compatibility with active ingredients of raw medicines, have good water-entering self-dispersibility, and simultaneously have synergistic effect with lignin, thereby avoiding the problem that the dry suspending agent is not easy to disintegrate and disperse.
Description
Technical Field
The invention relates to the technical field of pesticide preparation, and particularly provides an azoxystrobin dry suspending agent and a preparation method thereof.
Background
With the environmental and ecological challenges faced by traditional pesticide formulations, the development of environmentally compatible pesticides is a necessary trend and is also a requirement for the sustainable development of the environment and pesticides and the development of the pesticides themselves. The dry suspending agent is a particle pesticide formulation product, which is a new generation product that is obviously superior to other formulations in all aspects of content, package, process, cost, quality stability and using technology after the suspending agent. The dry suspending agent has the advantages of quick disintegration, fine dispersion, high suspension rate, quick formation of stable suspension when meeting water, no precipitation, no caking, no blockage of a spray head during use and the like.
The dry suspending agent mainly comprises a dispersing agent, a wetting agent, a defoaming agent, a pH regulator, a filler and the like, and has the main properties: effective content, disintegration, dispersibility, suspension rate, persistent foaming property, pH value, normal temperature storage stability and the like. The disintegration, the dispersibility and the suspension rate directly influence the drug effect, and the dispersing agent plays an important role in the drug effect. In the same formulation, the use of different dispersant types can obviously affect the performance of the preparation, and if the dispersant is incompatible with the pesticide active ingredient, the problems of unstable performance, caking, incapability of disintegrating, reduction of suspension rate and the like of the granule preparation can be caused, so that the drug effect is affected, and the importance of the dispersant is seen.
Azoxystrobin is a broad-spectrum and high-efficiency bactericide. The azoxystrobin has the characteristics of good systemic conductivity, strong permeability, long lasting period and the like. Has the functions of protecting, treating and eradicating almost all fungal diseases, has various use modes, and not only can be used for spraying stem leaves, but also can be used for treating seeds and soil. More than 400 preparations are registered in the pesticide verification institute in China, and the preparation is also a bactericide variety which is most registered. The azoxystrobin dry suspending agent has wider application, but the existing azoxystrobin dry suspending agent has the problems of difficult dispersion in water, slow disintegration, low suspension rate and the like.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides an azoxystrobin dry suspending agent and a preparation method thereof, wherein a dispersing agent used in the azoxystrobin dry suspending agent is a modified anionic high-molecular surfactant, specifically GY-DS 1287, which is widely available and good in compatibility with raw medicines, has good water-entering self-dispersibility, avoids the problem of difficult disintegration and dispersion, and has no dead particles.
In order to solve the technical problems, the invention provides the following technical scheme:
on one hand, the invention provides an azoxystrobin dry suspending agent, which comprises the following components in percentage by mass: 40-60% of azoxystrobin technical, 4-10% of solid wetting agent, 7-20% of lignin, 1-5% of anionic dispersing agent and the balance of filler, wherein the balance is added to 100%; the lignin is sodium lignosulfonate and/or calcium lignosulfonate; the anionic dispersant is GY-DS 1287.
Preferably, the azoxystrobin dry suspending agent consists of the following components in percentage by mass: 45-55% of azoxystrobin technical, 5-8% of solid wetting agent, 10-20% of lignin, 1-5% of anionic dispersing agent and the balance of filler are added to make up to 100%.
Preferably, the solid wetting agent is one or more of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate and sodium butyl naphthalene sulfonate.
Further, the filler is one or more of kaolin, light calcium and barium sulfate.
On the other hand, the invention also provides a preparation method of the azoxystrobin dry suspending agent, which comprises the following steps:
step 1: pouring the anionic dispersant, the solid wetting agent, the lignin and the filler into a shearing kettle filled with water, shearing and stirring uniformly, and then adding the azoxystrobin raw pesticide and stirring uniformly to form slurry;
step 2: sucking the slurry into a primary sand mill and a secondary sand mill for sanding in sequence;
and step 3: and pressing the sanded slurry into a pressure type spray drying granulator, a centrifugal spray dryer or a fluidized bed spray drying granulator through a peristaltic pump for spray drying granulation.
Preferably, in the step 1, the solid content in the slurry is 20-40%. In the step 2, the sanding medium is pickaxe beads with the diameter of 0.3-1.6 mm.
Compared with the prior art, the invention has the following beneficial effects:
(1) the azoxystrobin dry suspending agent material is subjected to sanding, the particle size of slurry is less than or equal to 5 mu m, the dispersion in water is good, the suspension performance is good, and the precipitation and layering are not easy to occur;
(2) the invention utilizes the synergistic effect of GY-DS 1287 dispersant and anionic solid wetting agent, has better wettability and dispersibility, and the prepared azoxystrobin dry suspending agent has the advantages of good dispersibility in water, quick wetting and the like;
(3) the azoxystrobin dry suspending agent is compounded with an anionic solid wetting agent and lignin by a GY-DS 1287 dispersant, so that the problems of non-fine disintegration, poor dispersion and easy generation of dead granules of the preparation are solved.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments.
The reagents and materials used in the examples and comparative examples were commercially available unless otherwise specified. Wherein the anionic dispersant is GY-DS 1287 of Beijing Guangyuan agricultural chemistry Limited liability company.
The invention provides an azoxystrobin dry suspending agent and a preparation method thereof, and the specific embodiment is as follows.
Example 1
The azoxystrobin dry suspending agent comprises the following components in percentage by mass: 50% of azoxystrobin technical product, 3% of Guangyuan Yinong GY-DS 1287, 8% of sodium dodecyl sulfate, 7% of sodium lignosulfonate and 32% of kaolin.
The preparation method of the azoxystrobin dry suspending agent comprises the following steps:
step 1: pouring 3kg of Guangyuan Yinong GY-DS 1287, 8kg of sodium dodecyl sulfate and 7kg of sodium lignosulfonate into a shearing kettle filled with 100kg of water, shearing and stirring uniformly, and then adding 50kg of azoxystrobin raw pesticide and stirring uniformly to form slurry;
step 2: sucking the slurry into a primary sand mill, sanding the slurry in a secondary sand mill in sequence, and repeatedly sanding until the particle size of the slurry is less than or equal to 5 microns; the sanding medium is a pickaxe bead with the diameter of 0.6 mm;
and step 3: and pressing the sanded slurry into a pressure type spray drying granulator through a peristaltic pump for spray drying granulation, wherein the inlet temperature of hot air is 100 ℃, and the exhaust temperature is 60 ℃.
Example 2
The azoxystrobin dry suspending agent comprises the following components in percentage by mass: 50% of azoxystrobin technical product, 3.3% of Guangyuan Yinong GY-DS 1287, 4% of sodium dodecyl sulfate, 4% of sodium dodecyl benzene sulfonate, 10% of sodium lignosulfonate and 28.7% of light calcium.
The preparation method is the same as example 1.
Example 3
The azoxystrobin dry suspending agent comprises the following components in percentage by mass: 50% of azoxystrobin technical product, 2% of Guangyuan Yinong GY-DS 1287, 5% of sodium dodecyl sulfate, 5% of sodium lignosulfonate, 10% of calcium lignosulfonate and 28% of barium sulfate.
The preparation method is the same as example 1.
Example 4
The azoxystrobin dry suspending agent comprises the following components in percentage by mass: 40% of azoxystrobin technical product, 1% of Guangyuan Yinong GY-DS 1287, 10% of butyl naphthalene sulfonate, 18% of calcium lignosulfonate and 31% of kaolin.
The preparation method is the same as example 1.
Example 5
The azoxystrobin dry suspending agent comprises the following components in percentage by mass: 40% of azoxystrobin technical product, 2% of Guangyuan Yinong GY-DS 1287, 4% of sodium dodecyl sulfate, 20% of sodium lignosulfonate and 34% of light calcium.
The preparation method is the same as example 1.
Example 6
The azoxystrobin dry suspending agent comprises the following components in percentage by mass: 45% of azoxystrobin technical product, 1% of Guangyuan Yinong GY-DS 1287, 10% of sodium dodecyl sulfate, 12% of sodium lignosulfonate, 16% of kaolin and 16% of light calcium.
The preparation method is the same as example 1.
Example 7
The azoxystrobin dry suspending agent comprises the following components in percentage by mass: 55% of azoxystrobin technical product, 4% of Guangyuan Yinong GY-DS 1287, 4% of sodium dodecyl sulfate, 4% of butyl naphthalene sulfonate, 15% of sodium lignosulfonate and 18% of kaolin.
The preparation method is the same as example 1.
Example 8
The azoxystrobin dry suspending agent comprises the following components in percentage by mass: 60% of azoxystrobin technical product, 5% of Guangyuan Yinong GY-DS 1287, 3% of sodium dodecyl sulfate, 3% of butyl naphthalene sulfonate, 10% of sodium lignosulfonate, 8% of calcium lignosulfonate and 11% of barium sulfate.
The preparation method is the same as example 1.
To further highlight the beneficial effects of the present invention, the following comparative examples were constructed, taking example 7 as an example, for reasons of space.
Comparative example 1
The same procedure as in example 7 was repeated except that the Guangyuan GY-DS 1287 was replaced with an equivalent amount of polycarboxylate (wherein the polycarboxylate was the Guangyuan GY-D07).
Comparative example 2
The same procedure as in example 7 was repeated except that Guangyong GnO-DS 1287 was replaced with an equivalent amount of ethoxylated potassium tristyrylphenol phosphate.
Comparative example 3
The Guangyuan Yinong GY-DS 1287 was replaced with naphthalene sulfonate, and the rest of the conditions were the same as in example 7.
Comparative example 4
The Guangyuan Yinong GY-DS 1287 was replaced with the same amount of sodium lignosulfonate under the same conditions as in example 7.
Comparative example 5
The Guangyuan Yinong GY-DS 1287 was replaced with an equal amount of kaolin, and the rest of the conditions were the same as in example 7.
Comparative example 6
The Guangyuan Yinong GY-DS 1287 was replaced with the same amount of light calcium carbonate, and the rest of the conditions were the same as in example 7.
Comparative example 7
The conditions were the same as in example 7 except that the Guangyuan Yinong GY-DS 1287 was replaced with an equivalent amount of ammonium sulfate.
Comparative example 8
The Guangyuan Yinong GY-DS 1287 was replaced with the same amount of sodium nonylphenol polyoxyethylene ether succinate sulfonate, and the rest of the conditions were the same as those in example 7.
Comparative example 9
The Guangyuan Yinong GY-DS 1287 was replaced with the same amount of castor oil polyoxyethylene ether, and the rest of the conditions were the same as those in example 7.
Comparative example 10
The same procedure as in example 7 was repeated except that sodium lauryl sulfate and sodium butylnaphthalene sulfonate were replaced with the same amount of polyoxyethylene castor oil.
Comparative example 11
The sodium lignosulfonate was replaced with an equal amount of hydroxymethyl cellulose and the remaining conditions were the same as in example 7.
The dry suspending agents prepared in the above examples and comparative examples were subjected to the following performance tests.
1. Detection of wetting Properties
The determination method comprises the following steps: 500ml of water was added to a measuring cylinder, 1g of the azoxystrobin dry suspension of examples 1 to 8 and comparative examples 1 to 11 was placed in a weighing dish and poured into the measuring cylinder rapidly without shaking, and the time schedule for 99% of the samples to sink to the bottom of the cylinder was determined, and the results are shown in Table 1.
TABLE 1 results of measurement of wetting Properties
As can be seen from the detection data in Table 1, the azoxystrobin dry suspending agent prepared by the invention has good dispersibility and wettability. The use of the Guangyuan Yinong GY-DS 1287 dispersant in the formula improves the dispersibility and wettability of the preparation in water. After replacing the GY-DS 1287 dispersant with some dispersants conventional in the art (comparative examples 1 to 3 and comparative examples 8 to 9) or omitting the GY-DS 1287 dispersant (comparative examples 4 to 7), the dispersibility into water becomes poor and the time taken to sink to the bottom of the cylinder increases; the dry suspending agent prepared by replacing the solid wetting agent of the invention with a nonionic surfactant (comparative example 10) and replacing the lignin of the invention with a conventional disintegrant (comparative example 11) can be dispersed in water, but the time taken for the solid wetting agent to sink to the bottom of a cylinder is increased, which proves that the wetting property of the dry suspending agent is slightly deteriorated. This is because the specific type of GY-DS 1287 dispersant and solid wetting agent of the present invention has better wettability and dispersibility for azoxystrobin dry suspending agent.
2. Determination of disintegration Property
The determination method comprises the following steps: 250ml of standard hard water was added to the cylinder and 1g of the azoxystrobin dry suspension of examples 1-8 and comparative examples 1-11 was taken. Pouring into a measuring cylinder, taking the bottom of the measuring cylinder as the center, reversing up and down at the speed of 2 s/time, and recording the disintegration times when the granules are completely disintegrated. The results are shown in Table 2.
TABLE 2 results of disintegration measurement
As can be seen from the detection data in Table 2, compared with the comparative example, the azoxystrobin dry suspending agent provided by the invention solves the problems of non-fine disintegration and dead granules, and has better disintegration.
3. Determination of the suspension Rate
The test method comprises the following steps: 250ml of standard hard water was added to the cylinder and 1g of the azoxystrobin dry suspension of examples 1-8 and comparative examples 1-11 was taken. Pouring into a measuring cylinder, covering a plug, turning upside down at the speed of 2 s/time for 30 times by taking the bottom of the measuring cylinder as an axis, and standing for 30 minutes. 9/10 (i.e. 225ml) suspension of the contents was removed with a pipette within 10s-15s without shaking or picking up the sediment in the graduated cylinder. Suspension ratio W of effective component in sample1The test results are shown in the table3, respectively.
TABLE 3 results of suspension ratio measurement
The suspension rate is high, and the azoxystrobin dry suspending agent needs a good dispersing agent to perform dispersing action to a certain extent, and the table 3 shows that the azoxystrobin dry suspending agent prepared by the invention has high suspension rate and good suspension effect.
4. Field efficacy test for citrus anthracnose
Due to space limitations, only the field trials of azoxystrobin dry suspension concentrate on citrus anthracnose in example 7 and comparative examples 1-11 were tested.
In the field test, 13 treatments of example 7 and comparative examples 1-11 are set, each treatment is repeated 4 times, and 52 treatment cells are set, 5 points are searched in each cell, and the statistical incidence and disease index of leaves and fruits are investigated. The disease indexes are investigated 4 times before the test period, the disease indexes are investigated 10 days after the test period, the test data adopts a Duncan test New redevelopment test method (DMRT), and the results are shown in Table 4.
TABLE 4 field test results of efficacy
The control effect calculation formula is as follows:
control effect (%) (disease index after drug treatment in control area-disease index after drug treatment in treatment area) x 100/disease index after drug treatment in control area.
As can be seen from the test results in Table 4, the azoxystrobin dry suspending agent has better drug effect; as can be seen from the data of the leaves 10d after the drug and the fruits 10d after the drug, compared with the comparative example, the dry suspending agent of the formula of the invention has better control effect than the dry suspending agent of other auxiliary agents, which shows that the dry suspending agent prepared by the invention has the advantages of fine disintegration and fine dispersion, has sustained drug effect and has sustained release function. The reason is that the dispersant is omitted and replaced in the comparative example, so that the dispersibility and wettability of the prepared dry suspending agent are poor, the disintegration is reduced, and the control effect on the anthracnose of the citrus is poor.
In conclusion, the GY-DS 1287 dispersing agent and the anionic solid wetting agent used in the azoxystrobin dry suspending agent have good compatibility with active ingredients of raw medicines, have good water-entering self-dispersibility, and simultaneously have synergistic effect with lignin, so that the problem that the dry suspending agent is not easy to disintegrate and disperse is avoided.
While the foregoing is directed to the preferred embodiment of the present invention, it will be understood by those skilled in the art that various changes and modifications may be made without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (7)
1. The azoxystrobin dry suspending agent is characterized by comprising the following components in percentage by mass: 40-60% of azoxystrobin technical, 4-10% of solid wetting agent, 7-20% of lignin, 1-5% of anionic dispersing agent and the balance of filler, wherein the balance is added to 100%; the lignin is sodium lignosulfonate and/or calcium lignosulfonate; the anionic dispersant is GY-DS 1287.
2. The azoxystrobin dry suspension agent according to claim 1, which is characterized by comprising the following components in percentage by mass: 45-55% of azoxystrobin technical, 5-8% of solid wetting agent, 10-20% of lignin, 1-5% of anionic dispersing agent and the balance of filler are added to make up to 100%.
3. The azoxystrobin dry suspension agent according to claim 1 or 2, wherein the solid wetting agent is one or more of sodium dodecylbenzene sulfonate, sodium dodecyl sulfate and sodium butylnaphthalene sulfonate.
4. The azoxystrobin dry suspension according to claim 3, wherein the filler is one or more of kaolin, light calcium and barium sulfate.
5. A method of preparing the azoxystrobin dry suspension of any one of claims 1-4, comprising:
step 1: pouring the anionic dispersant, the solid wetting agent, the lignin and the filler into a shearing kettle filled with water, shearing and stirring uniformly, and then adding the azoxystrobin raw pesticide and stirring uniformly to form slurry;
step 2: sucking the slurry into a primary sand mill and a secondary sand mill for sanding in sequence;
and step 3: and pressing the sanded slurry into a pressure type spray drying granulator, a centrifugal spray dryer or a fluidized bed spray drying granulator through a peristaltic pump for spray drying granulation.
6. The preparation method of the azoxystrobin dry suspending agent according to claim 5, wherein in the step 1, the solid content in the slurry is 20-40%.
7. The preparation method of the azoxystrobin dry suspending agent according to claim 5, wherein in the step 2, the sanding medium is pickaxel beads with the diameter of 0.3-1.6 mm.
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