CN113729011A - Glyphosate soluble granule and production method thereof - Google Patents
Glyphosate soluble granule and production method thereof Download PDFInfo
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- CN113729011A CN113729011A CN202110870720.3A CN202110870720A CN113729011A CN 113729011 A CN113729011 A CN 113729011A CN 202110870720 A CN202110870720 A CN 202110870720A CN 113729011 A CN113729011 A CN 113729011A
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- Prior art keywords
- glyphosate
- weight
- coating layer
- soluble granule
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- 239000008187 granular material Substances 0.000 title claims abstract description 45
- 239000005562 Glyphosate Substances 0.000 title claims abstract description 36
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 229940097068 glyphosate Drugs 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000011247 coating layer Substances 0.000 claims abstract description 36
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- PDYXIVPKOMYDOK-UHFFFAOYSA-N Glyphosate-monoammonium Chemical compound [NH4+].OC(=O)CNCP(O)([O-])=O PDYXIVPKOMYDOK-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000000546 pharmaceutical excipient Substances 0.000 claims abstract description 16
- AMUTYVGRCVFCCD-UHFFFAOYSA-N 5,6-diaminopyridine-3-carboxylic acid Chemical compound NC1=CC(C(O)=O)=CN=C1N AMUTYVGRCVFCCD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229920002472 Starch Polymers 0.000 claims abstract description 13
- 239000008107 starch Substances 0.000 claims abstract description 13
- 235000019698 starch Nutrition 0.000 claims abstract description 13
- 229920000609 methyl cellulose Polymers 0.000 claims abstract description 12
- 239000001923 methylcellulose Substances 0.000 claims abstract description 12
- 239000002131 composite material Substances 0.000 claims abstract description 11
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims abstract description 7
- 239000000741 silica gel Substances 0.000 claims abstract description 6
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 6
- 238000001125 extrusion Methods 0.000 claims abstract description 4
- 238000005469 granulation Methods 0.000 claims abstract description 4
- 230000003179 granulation Effects 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 239000007884 disintegrant Substances 0.000 claims abstract description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 13
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 13
- 235000010981 methylcellulose Nutrition 0.000 claims description 11
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 10
- 239000011248 coating agent Substances 0.000 claims description 10
- 238000000576 coating method Methods 0.000 claims description 10
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 9
- 239000011790 ferrous sulphate Substances 0.000 claims description 9
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 9
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 9
- 235000019270 ammonium chloride Nutrition 0.000 claims description 8
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 7
- 229920000881 Modified starch Polymers 0.000 claims description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 7
- -1 amide ammonium chloride Chemical class 0.000 claims description 7
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 7
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 7
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 7
- 239000011736 potassium bicarbonate Substances 0.000 claims description 7
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 7
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 7
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 7
- 229910052710 silicon Inorganic materials 0.000 claims description 7
- 239000010703 silicon Substances 0.000 claims description 7
- 235000013162 Cocos nucifera Nutrition 0.000 claims description 6
- 244000060011 Cocos nucifera Species 0.000 claims description 6
- 239000000377 silicon dioxide Substances 0.000 claims description 6
- 239000004964 aerogel Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 229940010514 ammonium ferrous sulfate Drugs 0.000 claims description 3
- 239000006255 coating slurry Substances 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 9
- 239000000575 pesticide Substances 0.000 abstract description 5
- 230000000052 comparative effect Effects 0.000 description 12
- 241000196324 Embryophyta Species 0.000 description 10
- 238000012360 testing method Methods 0.000 description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 6
- 150000001412 amines Chemical class 0.000 description 4
- 239000003760 tallow Substances 0.000 description 4
- 229920000877 Melamine resin Polymers 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000002363 herbicidal effect Effects 0.000 description 3
- 239000004009 herbicide Substances 0.000 description 3
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 235000017557 sodium bicarbonate Nutrition 0.000 description 3
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 description 2
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- JXOHGGNKMLTUBP-HSUXUTPPSA-N shikimic acid Chemical compound O[C@@H]1CC(C(O)=O)=C[C@@H](O)[C@H]1O JXOHGGNKMLTUBP-HSUXUTPPSA-N 0.000 description 2
- JXOHGGNKMLTUBP-JKUQZMGJSA-N shikimic acid Natural products O[C@@H]1CC(C(O)=O)=C[C@H](O)[C@@H]1O JXOHGGNKMLTUBP-JKUQZMGJSA-N 0.000 description 2
- 230000009885 systemic effect Effects 0.000 description 2
- 238000004260 weight control Methods 0.000 description 2
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 description 1
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- 235000015759 Artemisia selengensis Nutrition 0.000 description 1
- 241001168877 Artemisia selengensis Species 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 239000004471 Glycine Substances 0.000 description 1
- COLNVLDHVKWLRT-QMMMGPOBSA-N L-phenylalanine Chemical compound OC(=O)[C@@H](N)CC1=CC=CC=C1 COLNVLDHVKWLRT-QMMMGPOBSA-N 0.000 description 1
- QIVBCDIJIAJPQS-VIFPVBQESA-N L-tryptophane Chemical compound C1=CC=C2C(C[C@H](N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-VIFPVBQESA-N 0.000 description 1
- OUYCCCASQSFEME-QMMMGPOBSA-N L-tyrosine Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-QMMMGPOBSA-N 0.000 description 1
- 102000003960 Ligases Human genes 0.000 description 1
- 108090000364 Ligases Proteins 0.000 description 1
- 241000209510 Liliopsida Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004965 Silica aerogel Substances 0.000 description 1
- QIVBCDIJIAJPQS-UHFFFAOYSA-N Tryptophan Natural products C1=CC=C2C(CC(N)C(O)=O)=CNC2=C1 QIVBCDIJIAJPQS-UHFFFAOYSA-N 0.000 description 1
- MBHRHUJRKGNOKX-UHFFFAOYSA-N [(4,6-diamino-1,3,5-triazin-2-yl)amino]methanol Chemical compound NC1=NC(N)=NC(NCO)=N1 MBHRHUJRKGNOKX-UHFFFAOYSA-N 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- MRUAUOIMASANKQ-UHFFFAOYSA-N cocamidopropyl betaine Chemical compound CCCCCCCCCCCC(=O)NCCC[N+](C)(C)CC([O-])=O MRUAUOIMASANKQ-UHFFFAOYSA-N 0.000 description 1
- 229940073507 cocamidopropyl betaine Drugs 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 150000002085 enols Chemical class 0.000 description 1
- 241001233957 eudicotyledons Species 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229910001448 ferrous ion Inorganic materials 0.000 description 1
- 229930182470 glycoside Natural products 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000007721 medicinal effect Effects 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- CAAULPUQFIIOTL-UHFFFAOYSA-N methyl dihydrogen phosphate Chemical compound COP(O)(O)=O CAAULPUQFIIOTL-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- COLNVLDHVKWLRT-UHFFFAOYSA-N phenylalanine Natural products OC(=O)C(N)CC1=CC=CC=C1 COLNVLDHVKWLRT-UHFFFAOYSA-N 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910000073 phosphorus hydride Inorganic materials 0.000 description 1
- 230000005080 plant death Effects 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 229910021487 silica fume Inorganic materials 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 235000012222 talc Nutrition 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 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
- 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
- A01N25/26—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 in coated particulate form
-
- 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
- A01N57/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
- A01N57/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds
- A01N57/20—Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds containing acyclic or cycloaliphatic radicals
Landscapes
- 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 application belongs to the field of pesticides, and relates to a glyphosate soluble granule which comprises an easily disintegrating agent and consists of ammonium glyphosate, a synergist, an excipient and a composite disintegrant; the coating layer is coated outside the easily-disintegrating body; the compound disintegrating agent consists of talcum powder, CMS and superfine silica gel powder; the coating layer consists of methylcellulose, starch and isooctyl palmitate. The preparation method of the glyphosate soluble granule comprises the following steps of grinding the ammonium glyphosate with a set amount and the composite disintegrating agent with a set amount to 5-50 mu m; uniformly mixing the obtained mixture with a set amount of synergist and a set amount of excipient, and performing dry extrusion granulation to obtain an easily-disintegrated body; the obtained easily disintegrable body is wrapped with a coating layer. The soluble granule which can be stably stored and can be rapidly disintegrated in water is formed by the coating layer and the easily disintegrated body, so that the purpose of improving the control effect is achieved, and the soluble granule is environment-friendly.
Description
Technical Field
The invention belongs to the field of pesticides, relates to a herbicide, and particularly relates to a glyphosate soluble granule and a production method thereof.
Background
Glyphosate is also called N- (methyl phosphate) glycine and has a chemical formula of C3H8NO5P is an organic phosphine herbicide, and is a systemic conduction type broad-spectrum biocidal herbicide. By inhibiting enol pyruvyl shikimic acid phosphate synthetase in plants, the conversion of shikimic acid to phenylalanine, tyrosine and tryptophan is inhibited, so that the synthesis of protein is interfered to cause plant death. The glyphosate is known to have strong systemic conductivity, can be conducted to underground parts through stem leaves, can also be conducted among different tillers of the same plant, has strong destructive power on underground tissues of perennial deep-rooted weeds, and can reach the depth which can not be reached by common agricultural machinery. Glyphosate has control over plants of more than 40 families, including monocotyledons and dicotyledons. Annual and perennial, herbaceous and shrub, etc.
Chinese patent application publication No. CN110063339A discloses a glyphosate soluble granule, which consists of ammonium glyphosate, ammonium phosphate, water, a binder and a glyphosate synergist; the adhesive is prepared by the following method: (1) putting formaldehyde and melamine into a container according to the mass ratio of 1:2, slowly adding sodium bicarbonate into the container, and uniformly stirring the substances in the container by a stirring rod; (2) measuring the pH value by using a pH measuring instrument, stopping adding the sodium bicarbonate when the pH value reaches 8, heating the container, measuring the temperature by using a temperature measuring instrument, and stopping heating when the heating temperature reaches 90 ℃; (3) carrying out heat preservation treatment on the container by using a heat preservation tool, so that the temperature of the object in the container is continuously maintained at 80 ℃, and the heat preservation time is 30 minutes; (4) and slowly adding water into the container to make the object in the container viscous, and reducing the temperature to below 40 ℃ to finish the processing of the adhesive. The glyphosate synergist consists of alkyl glycoside, tallow amine polyoxyethylene ether, polypropylene glycol, sodium salt and cocamidopropyl betaine.
The technical scheme has a plurality of defects, for example, formaldehyde, melamine and sodium bicarbonate are adopted for preparing the adhesive, the melamine and the formaldehyde are condensed into hydroxymethyl melamine under the alkalescent condition to adhere the effective components and provide certain surface tension, but the disintegration and dispersion effects are poor; the glyphosate soluble granule contains a synergist of a tallow amine polyoxyethylene ether component, and although the tallow amine polyoxyethylene ether has good synergistic performance, the tallow amine polyoxyethylene ether is easy to cause harm to the environment and organisms.
Disclosure of Invention
The application aims to solve the problems and provide a glyphosate soluble granule;
in view of the above problems, it is another object of the present application to provide a method for preparing soluble glyphosate granules.
In order to achieve the purpose, the invention adopts the following technical scheme:
the present application creatively provides a glyphosate soluble granule comprising:
the easy disintegrating agent consists of glyphosate ammonium salt, a synergist, an excipient and a compound disintegrating agent;
the coating layer is coated outside the easily-disintegrating body;
the compound disintegrating agent consists of talcum powder, CMS and superfine silica gel powder;
the coating layer consists of methylcellulose, starch and isooctyl palmitate.
The soluble granule which can be stably stored and can be rapidly disintegrated in water is formed by the coating layer and the easily disintegrated body, so that the purpose of improving the control effect is achieved, and the soluble granule is environment-friendly.
The compound disintegrating agent has the capability of quick disintegration, can be dispersed and disintegrated in water in a very short time, improves the dispersing capability of soluble granules, ensures that the soluble granules are dispersed more uniformly and finely, shortens the disintegration time and improves the medicinal effect.
In the glyphosate soluble granule, the easily disintegrating agent consists of 75-90 parts by weight of ammonium glyphosate, 2-8 parts by weight of synergist, 2-13 parts by weight of excipient and 6-18 parts by weight of composite disintegrating agent.
Wherein the synergist comprises cocoanut amide ammonium chloride, ferrous sulfate and organic silicon polyoxyethylene ether in a weight ratio of 4-7:0.01-0.5: 1.
The synergist is prepared by compounding cocoanut amide ammonium chloride, ferrous sulfate and organic silicon polyoxyethylene ether, and can be expanded on the surface of a plant and quickly permeate and absorb. Thereby improving the drug effect of the soluble granules and improving the utilization rate.
Cocoamidoammonium chloride is cocoamidopropyl trimethyl ammonium chloride, and is used as a dispersing agent and can help soluble granules to be rapidly dispersed in liquid so as to enhance the permeability.
Ferrous ions in the ferrous sulfate can be combined with plants and absorbed, and the adhesion is improved.
The organic silicon polyoxyethylene ether has low surface tension, can be well spread on an oily surface, and is favorable for improving the utilization rate of pesticide.
Wherein the excipient comprises pregelatinized starch, potassium bicarbonate, microcrystalline cellulose and silicon dioxide aerogel in a weight ratio of 3-7:1-4:0.5-2: 0.5-1.
The excipient disclosed by the invention can endow the easily disintegrating agent with a fixed shape, has certain viscosity as a carrier and has the capability of quickly disintegrating in water, so that the synergist in the application can be formed as a soluble granule, can supplement each other when being mixed with a composite disintegrating agent, and can be quickly dispersed into uniform suspension in water.
In the glyphosate soluble granule, the weight ratio of the talcum powder to the CMS to the aerosil in the composite disintegrating agent is 1-5:2-8: 1-3.
Wherein CMS is sodium carboxymethyl starch.
In the glyphosate soluble granule, the coating layer consists of 0.1 to 0.5 weight part of methylcellulose, 0.1 to 0.5 weight part of starch and 0.2 to 0.8 weight part of isooctyl palmitate.
The coating layer is combined with methyl cellulose and starch through the isooctyl palmitate, has certain stability, can protect internal effective components after being stored for a long time, has certain polarity, and can be combined with water molecules in a large amount of water to enable the coating layer to break and release the internal easy-to-break body. And the isooctyl palmitate has good ductility and permeability, and can be combined with effective components in water, so that the combination effect of the effective components and plants is improved.
In the glyphosate soluble granule, the weight ratio of the easily disintegrating body to the coating layer is 60-100: 1.
The coating layer has a small coating thickness, and can be rapidly dispersed to achieve the effect of releasing the effective components.
A preparation method of the glyphosate soluble granule,
(1) grinding the ammonium glyphosate with a set amount and the composite disintegrating agent with a set amount together to 5-50 mu m;
(2) uniformly mixing the mixture obtained in the step (1) with a set amount of synergist and a set amount of excipient, and performing dry extrusion granulation to obtain an easily-disintegrated body;
(3) and (3) coating the easily-disintegrated body obtained in the step (2) with a coating layer.
In the preparation method of the glyphosate soluble granule, the particle size of the synergist is 5-100 mu m, and the particle size of the excipient is 50-100 mu m.
In the preparation method of the glyphosate soluble granule, the preparation method of the coating layer comprises the steps of mixing and grinding methylcellulose with a set amount and starch with a set amount to 5-50 mu m, adding isooctyl palmitate with a set amount, uniformly stirring to obtain instant coating slurry, and coating the easily-disintegrated body with a coating machine to form a coating layer, wherein the thickness of the coating layer is controlled to be less than 0.1 mm.
Detailed Description
Further illustrated by the following specific examples;
example 1
A glyphosate soluble granule comprises 100 parts by weight of easily disintegrating bodies and 1 part by weight of a coating layer, wherein the coating layer is coated outside the easily disintegrating bodies.
The easy-to-disintegrate body consists of 75 parts by weight of glyphosate ammonium salt, 4.5 parts by weight of cocoanut amide ammonium chloride, 0.5 part by weight of ferrous sulfate, 1 part by weight of organic silicon polyoxyethylene ether, 5 parts by weight of pregelatinized starch, 2 parts by weight of potassium bicarbonate, 1 part by weight of microcrystalline cellulose, 1 part by weight of silicon dioxide aerogel, 1 part by weight of talcum powder, 8 parts by weight of CMS and 1 part by weight of micropowder silica gel.
The coating layer was composed of 0.1 part by weight of methylcellulose, 0.1 part by weight of starch and 0.8 part by weight of isooctyl palmitate.
The preparation method of the glyphosate soluble granule comprises the following steps:
(1) grinding the ammonium glyphosate with a set amount and the composite disintegrating agent with a set amount together to 5-50 mu m;
(2) uniformly mixing the mixture obtained in the step (1) with a set amount of synergist and a set amount of excipient, and performing dry extrusion granulation to obtain an easily-disintegrated body;
(3) mixing and grinding methylcellulose with a set amount and starch to 5-50 μm, adding isooctyl palmitate with a set amount, stirring to obtain instant coating slurry, and coating the easily-disintegrated body with a coating machine to obtain a coating layer with a thickness of less than 0.1 mm.
The particle size of the synergist is 5-100 μm, and the particle size of the excipient is 50-100 μm.
Example 2
A glyphosate soluble granule comprises 100 parts by weight of easily disintegrating bodies and 1 part by weight of a coating layer, wherein the coating layer is coated outside the easily disintegrating bodies.
The easy-to-disintegrate body consists of 80 parts by weight of glyphosate ammonium salt, 5.5 parts by weight of cocoanut amide ammonium chloride, 0.5 part by weight of ferrous sulfate, 1 part by weight of organic silicon polyoxyethylene ether, 3 parts by weight of pregelatinized starch, 1 part by weight of potassium bicarbonate, 0.5 part by weight of microcrystalline cellulose, 0.5 part by weight of silicon dioxide aerogel, 2 parts by weight of talcum powder, 5 parts by weight of CMS and 1 part by weight of micropowder silica gel.
The coating layer consisted of 0.2 parts by weight of methylcellulose, 0.2 parts by weight of starch and 0.6 parts by weight of isooctyl palmitate.
The preparation method of this example is the same as example 1.
Example 3
A glyphosate soluble granule comprises 100 parts by weight of easily disintegrating bodies and 1 part by weight of a coating layer, wherein the coating layer is coated outside the easily disintegrating bodies.
The easily disintegrating body consists of 90 parts by weight of glyphosate ammonium salt, 1.45 parts by weight of cocoanut amide ammonium chloride, 0.18 part by weight of ferrous sulfate, 0.36 part by weight of organic silicon polyoxyethylene ether, 1 part by weight of pregelatinized starch, 0.33 part by weight of potassium bicarbonate, 0.33 part by weight of microcrystalline cellulose, 0.33 part by weight of silicon dioxide aerogel, 2 parts by weight of talcum powder, 2 parts by weight of CMS and 2 parts by weight of micropowder silica gel.
The coating layer consisted of 0.2 parts by weight of methylcellulose, 0.1 parts by weight of starch and 0.7 parts by weight of isooctyl palmitate.
The preparation method of this example is the same as example 1.
Comparative example 1
This comparative example is essentially the same as example 1 except that no coating layer is included.
Comparative example 2
This comparative example is essentially the same as example 1 except that the easily disintegratable substance is composed of 75 parts by weight of ammonium glyphosate, 4.5 parts by weight of cocoamido ammonium chloride, 0.5 part by weight of ferrous sulfate, 1 part by weight of silicone polyoxyethylene ether, 11.25 parts by weight of pregelatinized starch, 4.5 parts by weight of potassium bicarbonate, and 2.25 parts by weight of microcrystalline cellulose.
Comparative example 3
This comparative example is essentially the same as example 1, except that the disintegratable mass consists of 75 parts by weight ammonium glyphosate, 5 parts by weight cocoamide ammonium chloride, 1 part by weight silicone polyoxyethylene ether, 5 parts by weight pregelatinized starch, 2 parts by weight potassium bicarbonate, 1 part by weight microcrystalline cellulose, 1 part by weight silica aerogel, 1 part by weight talc, 8 parts by weight CMS and 1 part by weight microsilica.
Application example 1
Granules were prepared by the methods of example 1, comparative example 2 and comparative example 3, respectively.
The soluble granule particles of example 1, comparative example 2 and comparative example 3 were formulated with water in a weight ratio of 1:30 as reagents 1-3, respectively.
Setting 3 test zones, each test zone having an area of 20 square meters, the main weeds are herba Setariae viridis, Artemisia Selengensis, herba Humuli Scandentis, etc., respectively placing 1-3 reagents in 3 test zones at a ratio of 100g/667m2The pesticide application dosage is uniformly sprayed, the residual quantity of each test area is investigated and recorded 30d after the pesticide application, and the control effect is calculated as shown in the following tableThe following steps:
| plant control efficacy/%) | Fresh weight control Effect/%) | |
| Test zone 1 | 98.26 | 98.67 |
| Test zone 2 | 95.33 | 94.45 |
| Test zone 3 | 93.67 | 93.89 |
The results show that the compound disintegrating agent and the ferrous sulfate can improve the plant control effect and fresh weight control effect of the soluble granules.
Application example 2
Soluble granule particles were prepared by the methods of example 1 and comparative example 1, respectively. The heat storage stability test is carried out by adopting the test method specified in GB/T19136-2003, and the content of effective components before and after the test is tested, and the result is as follows:
| content of effective ingredient/%) | |
| Example 1 | 99.57 |
| Comparative example 1 | 98.65 |
The results show that the soluble granule particles with increased coating layer have better heat stability.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Although the terms disintegratable, ammonium glyphosate, synergist, excipient, composite disintegrant composition and coating are used more often herein, the possibility of using other terms is not excluded. These terms are used merely to more conveniently describe and explain the nature of the present invention and they are to be interpreted as any additional limitation which is not in accordance with the spirit of the present invention.
Claims (10)
1. A glyphosate soluble granule comprising:
the easy disintegrating agent consists of glyphosate ammonium salt, a synergist, an excipient and a compound disintegrating agent;
the coating layer is coated outside the easily-disintegrating body;
the compound disintegrating agent consists of talcum powder, CMS and superfine silica gel powder;
the coating layer consists of methylcellulose, starch and isooctyl palmitate.
2. The glyphosate soluble granule of claim 1, wherein:
the easily disintegrating tablet consists of 75-90 parts by weight of ammonium glyphosate, 2-8 parts by weight of synergist, 2-13 parts by weight of excipient and 6-18 parts by weight of composite disintegrant.
3. The glyphosate soluble granule of claim 1, wherein:
the coating layer consists of 0.1 to 0.5 weight part of methylcellulose, 0.1 to 0.5 weight part of starch and 0.2 to 0.8 weight part of isooctyl palmitate.
4. The glyphosate soluble granule of claim 1, wherein:
the weight ratio of the talcum powder to the CMS to the superfine silica powder in the composite disintegrating agent is 1-5:2-8: 1-3.
5. The glyphosate soluble granule of claim 1, wherein: the synergist comprises cocoanut oil amide ammonium chloride, ferrous sulfate and organic silicon polyoxyethylene ether in a weight ratio of 4-7:0.01-0.5: 1.
6. The glyphosate soluble granule of claim 1, wherein: the excipient comprises pregelatinized starch, potassium bicarbonate, microcrystalline cellulose and silicon dioxide aerogel in a weight ratio of 3-7:1-4:0.5-2: 0.5-1.
7. A glyphosate soluble granule as claimed in any one of claims 1 to 6, characterized in that: the weight ratio of the easily disintegrating body to the coating layer is 60-100: 1.
8. A process for the preparation of glyphosate soluble granules as claimed in any one of claims 1 to 7, characterized in that:
(1) grinding the ammonium glyphosate with a set amount and the composite disintegrating agent with a set amount together to 5-50 mu m;
(2) uniformly mixing the mixture obtained in the step (1) with a set amount of synergist and a set amount of excipient, and performing dry extrusion granulation to obtain an easily-disintegrated body;
(3) and (3) coating the easily-disintegrated body obtained in the step (2) with a coating layer.
9. The process for preparing glyphosate soluble granules of claim 8, wherein: the particle size of the synergist is 5-100 μm, and the particle size of the excipient is 50-100 μm.
10. The process for preparing glyphosate soluble granules of claim 8, wherein: the preparation method of the coating layer comprises the steps of mixing and grinding methyl cellulose and starch to 5-50 mu m, adding isooctyl palmitate to the mixture, uniformly stirring the mixture to obtain instant coating slurry, and coating the easily-disintegrated body with a coating machine to form a coating layer, wherein the thickness of the coating layer is controlled to be less than 0.1 mm.
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