AU2016101700B4 - Water soluble granule of glufosinate-ammonium - Google Patents
Water soluble granule of glufosinate-ammonium Download PDFInfo
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- AU2016101700B4 AU2016101700B4 AU2016101700A AU2016101700A AU2016101700B4 AU 2016101700 B4 AU2016101700 B4 AU 2016101700B4 AU 2016101700 A AU2016101700 A AU 2016101700A AU 2016101700 A AU2016101700 A AU 2016101700A AU 2016101700 B4 AU2016101700 B4 AU 2016101700B4
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- ammonium
- glufosinate
- water soluble
- soluble granule
- water
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- IAJOBQBIJHVGMQ-UHFFFAOYSA-N 2-amino-4-[hydroxy(methyl)phosphoryl]butanoic acid Chemical compound CP(O)(=O)CCC(N)C(O)=O IAJOBQBIJHVGMQ-UHFFFAOYSA-N 0.000 title claims abstract description 188
- 239000004549 water soluble granule Substances 0.000 title claims abstract description 83
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000004094 surface-active agent Substances 0.000 claims abstract description 27
- 239000002738 chelating agent Substances 0.000 claims abstract description 21
- 239000000203 mixture Substances 0.000 claims description 29
- -1 alkyl glycoside Chemical class 0.000 claims description 25
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 20
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 20
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 15
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 15
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 15
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims description 14
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 13
- 150000002191 fatty alcohols Chemical class 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 13
- 150000001412 amines Chemical class 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 229920005646 polycarboxylate Polymers 0.000 claims description 10
- GVKDLCPTYCLSQW-YFKNTREVSA-N C(\C=C/C(=O)OC(C)CCCCCC)(=O)OC(C)CCCCCC.[Na] Chemical compound C(\C=C/C(=O)OC(C)CCCCCC)(=O)OC(C)CCCCCC.[Na] GVKDLCPTYCLSQW-YFKNTREVSA-N 0.000 claims description 9
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 9
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 9
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims description 8
- 239000003760 tallow Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 7
- 238000005469 granulation Methods 0.000 claims description 6
- 230000003179 granulation Effects 0.000 claims description 6
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 claims description 6
- 229910052939 potassium sulfate Inorganic materials 0.000 claims description 6
- 235000011151 potassium sulphates Nutrition 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- JIJAYWGYIDJVJI-UHFFFAOYSA-N butyl naphthalene-1-sulfonate Chemical compound C1=CC=C2C(S(=O)(=O)OCCCC)=CC=CC2=C1 JIJAYWGYIDJVJI-UHFFFAOYSA-N 0.000 claims description 5
- ZPWVASYFFYYZEW-UHFFFAOYSA-L dipotassium hydrogen phosphate Chemical compound [K+].[K+].OP([O-])([O-])=O ZPWVASYFFYYZEW-UHFFFAOYSA-L 0.000 claims description 5
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims description 5
- PAWQVTBBRAZDMG-UHFFFAOYSA-N 2-(3-bromo-2-fluorophenyl)acetic acid Chemical compound OC(=O)CC1=CC=CC(Br)=C1F PAWQVTBBRAZDMG-UHFFFAOYSA-N 0.000 claims description 4
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 4
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- 235000019270 ammonium chloride Nutrition 0.000 claims description 4
- 229920001400 block copolymer Polymers 0.000 claims description 4
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 claims description 4
- 229910000388 diammonium phosphate Inorganic materials 0.000 claims description 4
- 235000019838 diammonium phosphate Nutrition 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 150000004665 fatty acids Chemical class 0.000 claims description 4
- 229910021485 fumed silica Inorganic materials 0.000 claims description 4
- 229930182470 glycoside Natural products 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 claims description 4
- 239000004323 potassium nitrate Substances 0.000 claims description 4
- 235000010333 potassium nitrate Nutrition 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 235000013877 carbamide Nutrition 0.000 claims description 3
- 235000002639 sodium chloride Nutrition 0.000 claims description 3
- 239000000575 pesticide Substances 0.000 abstract description 8
- 239000008233 hard water Substances 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 3
- 239000002671 adjuvant Substances 0.000 abstract description 2
- 239000004557 technical material Substances 0.000 description 46
- 239000008187 granular material Substances 0.000 description 22
- 238000004898 kneading Methods 0.000 description 18
- 238000012360 testing method Methods 0.000 description 9
- 230000002363 herbicidal effect Effects 0.000 description 7
- 239000004009 herbicide Substances 0.000 description 7
- 238000004090 dissolution Methods 0.000 description 6
- 102200108024 rs199473050 Human genes 0.000 description 5
- 241000196324 Embryophyta Species 0.000 description 4
- 241000737409 Dysphania multifida Species 0.000 description 3
- 241000219870 Trifolium subterraneum Species 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 230000009261 transgenic effect Effects 0.000 description 3
- 239000005562 Glyphosate Substances 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 102000005396 glutamine synthetase Human genes 0.000 description 2
- 108020002326 glutamine synthetase Proteins 0.000 description 2
- XDDAORKBJWWYJS-UHFFFAOYSA-N glyphosate Chemical compound OC(=O)CNCP(O)(O)=O XDDAORKBJWWYJS-UHFFFAOYSA-N 0.000 description 2
- 229940097068 glyphosate Drugs 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000002085 persistent effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 240000008620 Fagopyrum esculentum Species 0.000 description 1
- 235000009419 Fagopyrum esculentum Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012669 liquid formulation Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- FIKAKWIAUPDISJ-UHFFFAOYSA-L paraquat dichloride Chemical compound [Cl-].[Cl-].C1=C[N+](C)=CC=C1C1=CC=[N+](C)C=C1 FIKAKWIAUPDISJ-UHFFFAOYSA-L 0.000 description 1
- 238000003359 percent control normalization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- ACVYVLVWPXVTIT-UHFFFAOYSA-N phosphinic acid Chemical compound O[PH2]=O ACVYVLVWPXVTIT-UHFFFAOYSA-N 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- 230000005068 transpiration Effects 0.000 description 1
- 239000004552 water soluble powder Substances 0.000 description 1
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- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention provides a water soluble granule of glufosinate-ammonium, comprising glufosinate-ammonium, a surfactant and a carrier. Further, the water soluble granule of glufosinate-ammonium also comprises a chelator and a synergist. A glufosinate-ammonium pesticide which attains better solubility, dissolving stability, low foamability and good efficacy in high concentration of hard water, is obtained in the present invention by adjusting the type of auxiliaries of the water soluble granule of glufosinate-ammonium and using in combination with proper adjuvants, which enable the synergistic effect of various components. It is particularly suitable for countries and regions of higher water hardness.
Description
WATER SOLUBLE GRANULE OF GLUFOSINATE-AMMONIUM 2016101700 29 Aug 2016
Field of the invention [01] The present invention relates to the technical field of pesticides, and especially to a water soluble granule of glufosinate-ammonium.
Background of the invention [02] Gulfosinate-ammonium is an organophosphorus-based non-conductive sterilant herbicide using glutamine synthetase (GS) as the target enzyme. It belongs to the broad spectrum contact herbicide and has weak systemic action. Being different from glyphosate which kills the root, gulfosinate-ammonium kills the leaf first, and may be transmitted in the xylem of a plant by the transpiration of the plant. Its quick-acting property is between paraquat and glyphosate. Meanwhile, glufosinate-ammonium belongs to a hypophosphorous acid-based non-conductive sterilant herbicide which has high efficiency, low toxicity and is environmentally friendly. It is easy to degrade in soil, safe to crops, not easy to drift, wide in weed control spectrum, and has high activity, less dosage, small environmental pressure, and is a large tonnage pesticide variety in the world. However, environmental factors, such as light intensity, temperature and humidity, have great influences on the activity of glufosinate-ammonium.
[03] With the rapid development of transgenic techniques, plantation of transgenic herbicide-tolerant crops has been increasingly intensified in the recent years, and as a result, the use of tolerant herbicide has greatly increased. Being an excellent sterilant herbicide, glufosinate-ammonium is very suitable for a resistance gene. Almost all the staple crops have been encompassed by the commercially cultivated glufosinate-ammonium-tolerant crops, which are widely cultivated in North America, such as the US, and recently the cultivation promotion in some countries and regions of Europe, Australia and Asia makes the glufosinate-ammonium to be the world’s second largest transgenic crop-tolerant herbicide, therefore the market prospect of this product is very broad.
[04] At present, the formulations of glufosinate-ammonium on the market are mainly aqueous solution and soluble liquid, which have higher package and transportation costs, inconvenience on using and metering, and poorer efficacy, also crucially with many quality problems, such as flocculation, crystallization, storage-intolerance, easy decomposition, and the like. 1
Summary of the invention 2016101700 29 Aug 2016 [05] The technical problem solved by the present invention is providing a water soluble granule of glufosinate-ammonium. The water soluble granule of glufosinate-ammonium provided by the present application has characteristics of high solubility, excellent dissolution stability and high efficacy.
[06] In view of this, the present application provides a water soluble granule of glufosinate-ammonium, comprising glufosinate-ammonium, a surfactant and a carrier.
[07] Preferably, it further comprises a chelator and a synergist.
[08] Preferably, it comprises, by weight percentage, 5%~97% of glufosinate-ammonium, 1 %~20% of a surfactant and the balance of a carrier.
[09] Preferably, it comprises, by weight percentage, 5%~97% of glufosinate-ammonium, 1 %~20% of a surfactant, 1%~5% of a chelator, 0.1%~5% of a synergist and the balance of a carrier.
[10] Preferably, the content of glufosinate-ammonium is 10wt%~80wt%.
[11] Preferably, the content of glufosinate-ammonium is 20wt%~80wt%.
[12] Preferably, the content of the surfactant is 5wt%~15wt%.
[13] Preferably, it comprises, by weight percentage, 80% of glufosinate-ammonium, 5% of a surfactant and the balance of a carrier.
[14] Preferably, the content of the chelator is lwt%~3wt%.
[15] Preferably, the content of the synergist is 0.1wt%~3wt%.
[16] Preferably, it comprises, by weight percentage, 80% of glufosinate-ammonium, 12% of a surfactant, 1% of a chelator, 0.5% of a synergist and the balance of a carrier.
[17] Preferably, the surfactant is one or more selected from the group consisting of organosillicon polyether, tallow amine polyoxyethylene ether, alkyl glycoside, polyoxyethylene nonyl phenol, fatty amine polyoxyethylene ether, oxirane-epoxypropane block copolymer, alkylphenol polyoxyethylene polyoxypropylene ether, polycarboxylate, polyoxyethylene fatty acid, polyethylene glycol, methyloxirane, fatty alcohol sulfonate, fatty alcohol polyoxyethylene ether alkyl naphthalenesulfonic acid-formaldehyde condensate and sodium dodecyl sulfate; the carrier is one or more selected from the group consisting of ammonium sulfate, diammonium hydrogen phosphate, sodium sulfate, sodium chloride, urea, potassium nitrate, ammonium nitrate, ammonium chloride, dipotassium hydrogen phosphate, 2 fumed silica, potassium sulfate and sodium tripolyphosphate. 2016101700 29 Aug 2016 [18] Preferably, the chelator is one or more selected from the group consisting of ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetate, tetrasodium ethylenediaminetetraacetate and sodium tripolyphosphate; the synergist is one or more selected from the group consisting of butyl naphthalenesulfonate, fatty alcohol polyoxyethylene ether, alkyl fatty alcohol sulfonate and di-sec-octyl maleate sodium sulfonate.
[19] Preferably, the method for preparing the water soluble granule of glufosinate-ammonium is specifically: [20] mixing glufosinate-ammonium, a surfactant and a carrier to obtain a mixture; [21] mixing the mixture with water, then sequentially conducting extruding granulation and drying to obtain a water soluble granule of glufosinate-ammonium.
[22] Preferably, the method for preparing the water soluble granule of glufosinate-ammonium is specifically: [23] mixing glufosinate-ammonium, a surfactant, a chelator, a synergist and a carrier to obtain a mixture; [24] mixing the mixture with water, then sequentially conducting extruding granulation and drying to obtain a water soluble granule of glufosinate-ammonium.
[25] The present application provides a water soluble granule of glufosinate-ammonium comprising glufosinate-ammonium, a surfactant and a carrier, further, the water soluble granule of glufosinate-ammonium of the present application also comprises a chelator and a synergist. A glufosinate-ammonium pesticide which attains better solubility, dissolving stability, low foamability and good efficacy in high concentration of hard water, is obtained in the present invention by adjusting the type of auxiliaries of the water soluble granule of glufosinate-ammonium and using in combination with proper adjuvants, which enable the synergistic effect of various components. It is particularly suitable for countries and regions of higher water hardness.
Detailed description of the invention [26] In order to further understand the present invention, preferred embodiments of the present invention are described below in conjunction with examples, but it should be understood that these are described for further illustrating the characteristics and advantages of the present invention only, but not to limit the claims of the present invention. 3 [27] Examples of the present invention disclose a water soluble granule of glufosinate-ammonium comprising glufosinate-ammonium, a surfactant and a carrier. 2016101700 29 Aug 2016 [28] For better performance of the water soluble granule of glufosinate-ammonium, the water soluble granule of glufosinate-ammonium of the present invention also comprises a chelator and a synergist.
[29] In accordance with the present invention, the glufosinate-ammonium acts as the basic and key component of the water soluble granule of glufosinate-ammonium. Preferably, the content of the glufosinate-ammonium of the present invention is 5wt%~97wt%; in some examples, the content of the glufosinate-ammonium is preferably 10wt%~80wt%; in some examples, the content of the glufosinate-ammonium is preferably 20wt%~80wt%; in some examples, the content of the glufosinate-ammonium is preferably 55wt%~75wt%.
[30] The surfactant is one or more preferably selected from the group consisting of organosillicon polyether, tallow amine polyoxyethylene ether, alkyl glycoside, polyoxyethylene nonyl phenol, fatty amine polyoxyethylene ether, oxirane-epoxypropane block copolymer, alkylphenol polyoxyethylene polyoxypropylene ether, polycarboxylate, polyoxyethylene fatty acid, polyethylene glycol, methyloxirane, fatty alcohol sulfonate, fatty alcohol polyoxyethylene ether alkyl naphthalenesulfonic acid-formaldehyde condensate and sodium dodecyl sulfate; more preferably a combination of fatty alcohol sulfonate and polycarboxylate. The content of the surfactant is preferably lwt%~20wt%; in some examples, the content of the surfactant is preferably 2wt%~17wt%; in some examples, the content of the surfactant is preferably 5wt%~15wt%.
[31] The carrier, i.e. the filler of the water soluble granule of glufosinate-ammonium, of the present invention is one or more selected from the group consisting of ammonium sulfate, diammonium hydrogen phosphate, sodium sulfate, sodium chloride, urea, potassium nitrate, ammonium nitrate, ammonium chloride, dipotassium hydrogen phosphate, fumed silica, potassium sulfate and sodium tripolyphosphate. In examples, the carrier is preferably ammonium sulfate.
[32] As a preferred embodiment, the water soluble granule of glufosinate-ammonium, by weight percentage, comprises 5%~97% of glufosinate-ammonium, 1%~20% of a surfactant and the balance of a carrier.
[33] More preferably, the water soluble granule of glufosinate-ammonium, by weight percentage, comprises 80% of glufosinate-ammonium, 5% by weight of a surfactant and the balance of a carrier. 4 [34] When a chelator and a synergist are comprised in the water soluble granule of glufosinate-ammonium, the water soluble granule of glufosinate-ammonium, by weight percentage, comprises 5%~97% of glufosinate-ammonium, 1%~20% of a surfactant, 1%~5% of a chelator, 0.1%~5% of a synergist and the balance of a carrier. 2016101700 29 Aug 2016 [35] In the above described water soluble granule of glufosinate-ammonium, the preferred contents of the glufosinate-ammonium and the surfactant are the same as recorded above.
[36] The chelator mainly reduces the hardness of water, which enables the use of glufosinate-ammonium product in countries where the hardness of water is higher, such as Australia, without reduction of the performance of the product. The chelator is one or more preferably selected from the group consisting of ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetate, tetrasodium ethylenediaminetetraacetate and sodium tripolyphosphate. In an example, the chelator is more preferably selected from disodium ethylenediaminetetraacetate. Preferably, the content of the chelator is lwt%~5wt%; in some examples, the content of the chelator is preferably lwt%~3wt%.
[37] The synergist mainly plays a synergistic effect. Particularly, the addition of a synergist may improve the control effect of the present herbicide on target crops (weed), on the premise of having no influence on the performance of the product. The synergist of the present invention is one or more preferably selected from the group consisting of butyl naphthalenesulfonate, fatty alcohol polyoxyethylene ether, alkyl fatty alcohol sulfonate and di-sec-octyl maleate sodium sulfonate. In an example, the synergist is preferably di-sec-octyl maleate sodium sulfonate. In an example, the content of the synergist is preferably 0.1wt%~5wt%. In some examples, the content of the synergist is preferably 0.1wt%~3wt%.
[38] As a preferred embodiment, the water soluble granule of glufosinate-ammonium, by weight percentage, comprises 80% of glufosinate-ammonium, 12% of a surfactant, 1% of a chelator, 0.5% of a synergist and the balance of a carrier.
[39] There is no particular limit on the method for preparing the water soluble granule of glufosinate-ammonium in the present application, as long as it is prepared in accordance with a method known by those skilled in the art. For example, the method for preparing the water soluble granule of glufosinate-ammonium is specifically: mixing glufosinate-ammonium, a surfactant and a filler to obtain a first product, 5 or mixing glufosinate-ammonium, a surfactant, a chelator, a synergist and a filler to obtain a first product; 2016101700 29 Aug 2016 mixing the first product with water, then sequentially conducting extruding granulation and drying to obtain a water soluble granule of glufosinate-ammonium.
[40] In the above described process, the extruding granulation and the drying are technical means well-known by those skilled in the art, and there is no limit thereof in the present application.
[41] In the above described process, the mass of the water is 3%~6% of the mass in the first product, the temperature for the drying is preferably 40-90 °C.
[42] The water soluble granule of glufosinate-ammonium of the present invention is a solid granule, which solves the problems of the high transportation cost of pesticide, inconvenience on measuring, instability of liquid formulation and poor efficacy.
[43] The water soluble granule of glufosinate-ammonium provided by the present invention has excellent solubility, good stability of dissolution in high concentration of hard water, and has characteristics of low foamability, high efficacy; and the preparation method of the formulation is easy, the use thereof is convenient and overcomes the drawbacks of high package and transportation cost, inconvenience in using and measuring, poorer efficacy in the prior art, so that it is particularly suitable for countries and regions of higher water hardness.
[44] For further understanding of the present invention, the water soluble granule of glufosinate-ammonium provided by the present invention will be described in detail in conjunction with examples. However, the protection scope of the present invention are not limited by the following examples.
Example 1. Water soluble granule of 80% glufosinate-ammonium [45] 84.2 g of glufosinate-ammonium technical material, 5 g of Terwet®3780 (Hunstman, tallow amine polyoxyethylene ether) and 5 g of urea were mixed with 5.8 g of ammonium sulfate, then water of 3wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having glufosinate-ammonium in 80% mass fraction, yield 99.5%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material.
Example 2. Water soluble granule of 97% glufosinate-ammonium 6 [46] 97.4 g of glufosinate-ammonium technical material, 2 g of Terwet®3780 (Hunstman, tallow amine polyoxyethylene ether) and 0.2 g of urea were mixed with 0.4 g of ammonium sulfate, then water of 3.5wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having glufosinate-ammonium in 97% mass fraction, yield 99.2%; the glufosinate-ammonium technical material in the example was a 99.6% glufosinate-ammonium technical material. 2016101700 29 Aug 2016
Example 3. Water soluble granule of 75% glufosinate-ammonium [47] 78.9 g of the glufosinate-ammonium, 5 g of Terwet®3780 (Hunstman, tallow amine polyoxyethylene ether) and 5 g of urea were mixed with 11.1 g of ammonium sulfate, then water of 4wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having glufosinate-ammonium in 75% mass fraction, yield 99.3%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material.
Example 4. Water soluble granule of 55% glufosinate-ammonium [48] 57.9 g of glufosinate-ammonium, 5 g of Terwet®3780 (Hunstman, tallow amine polyoxyethylene ether) and 5 g of urea were mixed with 32.1 g of ammonium sulfate, then water of 4wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having glufosinate-ammonium in 55% mass fraction, yield 99.4%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material.
Example 5 Water soluble granule of 5% glufosinate-ammonium [49] 5 .27 g of glufosinate-ammonium, 5 g of Terwet®3780 (Hunstman, tallow amine polyoxyethylene ether) and 5 g of urea were mixed with 84.7 g of ammonium sulfate, then water of 5wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having glufosinate-ammonium in 5% mass fraction, yield 99.1%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material. 7
Example 6. Water soluble granule of 80% glufosinate-ammonium 2016101700 29 Aug 2016
[50] 84.2 g of glufosinate-ammonium technical material, 10 g of Geronol N70K (Solvay, fatty alcohol sulfonate), 2 g of TERSPERSE® 2700 (Hunstman, polycarboxylate), 1 g of disodium EDTA, 5 g of anhydrous Rapid Penetrant T (di-sec-octyl maleate sodium sulfonate) were mixed with 22.5 g of ammonium sulfate, then water of 3% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having glufosinate-ammonium in 80% mass fraction, yield 99.8%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material.
Example 7. Water soluble granule of 97% glufosinate-ammonium
[51] 97.4 g of glufosinate-ammonium technical material, 0.5 g of Geronol N70K (Solvay, fatty alcohol sulfonate), 0.5 g of TERSPERSE® 2700 (Hunstman, polycarboxylate), 0.5 g of disodium EDTA, 1 g of anhydrous Rapid Penetrant T (di-sec-octyl maleate sodium sulfonate) were mixed with 0.1 g of ammonium sulfate, then water of 4wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having glufosinate-ammonium in 97% mass fraction, yield 99.2%; the glufosinate-ammonium technical material in the example was a 99.6% glufosinate-ammonium technical material.
Example 8. Water soluble granule of 60% glufosinate-ammonium
[52] 63.2 g of glufosinate-ammonium technical material, 10 g of Geronol N70K (Solvay, fatty alcohol sulfonate), 2 g of TERSPERSE® 2700 (Hunstman, polycarboxylate), lg of disodium EDTA, 5 g of anhydrous Rapid Penetrant T (di-sec-octyl maleate sodium sulfonate) were mixed with 18.8 g of ammonium sulfate, then water of 3.5wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule of glufosinate-ammonium in 60% mass fraction, yield 99.3%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material.
Example 9. Water soluble granule of 30% glufosinate-ammonium 8
[53] 31.6 g of glufosinate-ammonium technical material, 10 g of Geronol N70K 2016101700 29 Aug 2016 (Solvay, fatty alcohol sulfonate), 2 g of TERSPERSE® 2700 (Hunstman, polycarboxylate), 1 g of disodium EDTA, 5 g of anhydrous Rapid Penetrant T (di-sec-octyl maleate sodium sulfonate) were mixed with 50.4 g of ammonium sulfate, then water of 4.5wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having glufosinate-ammonium in 30% mass fraction, yield 99.31%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material.
Example 10. Water soluble granule of 5% glufosinate-ammonium
[54] 5 .27 g of glufosinate-ammonium technical material, 10 g of Geronol N70K (Solvay, fatty alcohol sulfonate), 2 g of TERSPERSE® 2700 (Hunstman, polycarboxylate), 1 g of disodium EDTA, 5 g of anhydrous Rapid Penetrant T (di-sec-octyl maleate sodium sulfonate) were mixed with 76.7 g of ammonium sulfate, then water of 5wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule having glufosinate-ammonium in 5% mass fraction, yield 99.0%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material.
Example 11. Water soluble granule of 97% glufosinate-ammonium [55] 97.4 g of glufosinate-ammonium technical material, 1.5 g of alkyl glycoside, 0.5 g of oxirane-epoxypropane block copolymer were mixed with 0.6 g of sodium sulfate, then water of 3wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule of glufosinate-ammonium in 80% mass fraction, yield 99.2%; the glufosinate-ammonium technical material in the example was a 99.6% glufosinate-ammonium technical material.
Example 12. Water soluble granule of 5% glufosinate-ammonium [56] 5.27 g of glufosinate-ammonium, 15 g of fatty amine polyoxyethylene ether, 2 g of organosillicon polyether, 1.5 g of fumed silica were mixed with 76.3 g of potassium sulfate, then water of 5.8wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient 9 kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule of glufosinate-ammonium in 5% mass fraction, yield 99.2%; the glufosinate-ammonium technical material in the example was a 95% 2016101700 29 Aug 2016 glufosinate-ammonium technical material.
Example 13. Water soluble granule of 70% glufosinate-ammonium [57] 73.7 g of glufosinate-ammonium, 10 g of polycarboxylate, 5 g of sodium chloride were mixed with 11.3 g of diammonium hydrogen phosphate, then water of 4.5wt% of the total content of the above described components was added, then the mixture was put into in a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule of glufosinate-ammonium in 70% mass fraction, yield 99.3%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material.
Example 14. Water soluble granule of 50% glufosinate-ammonium [58] 52.6 g of glufosinate-ammonium, 8 g of fatty alcohol polyoxyethylene ether alkyl naphthalenesulfonic acid-formaldehyde condensate, 15 g of ammonium chloride were mixed with 24.4 g of potassium sulfate, then water of 4.5wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule of glufosinate-ammonium in 50% mass fraction, yield 99.1%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material.
Example 15. Water soluble granule of 97% glufosinate-ammonium [59] 97.4 g of glufosinate-ammonium technical material, 0.3 g of polyoxyethylene nonyl phenol, 0.7 g of alkylphenol polyoxyethylene polyoxypropylene ether, 0.4 g of tetrasodium EDTA, 1.1 g butyl naphthalenesulfonate were mixed with 0.1 g of ammonium sulfate, then water of 4.2wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule of glufosinate-ammonium in 97% mass fraction, yield 99.2%; the glufosinate-ammonium technical material in the example was a 99.6% glufosinate-ammonium technical material.
Example 16. Water soluble granule of 5% glufosinate-ammonium [60] 5.27 g of glufosinate-ammonium, 8 g of polyoxyethylene fatty acid, 5 g of to polyethylene glycol, 2 g of EDTA, 3 g of fatty alcohol polyoxyethylene ether, 30 g of potassium nitrate were mixed with 46.7 g of ammonium nitrate, then water of 5.5wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule of glufosinate-ammonium in 5% mass fraction, yield 99.3%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material. 2016101700 29 Aug 2016
Example 17. Water soluble granule of 60% glufosinate-ammonium [61] 63.2 g of glufosinate-ammonium, 20 g of methyloxirane, 4 g of sodium tripolyphosphate, 4 g of alkyl fatty alcohol sulfonate were mixed with 8.8 g of dipotassium hydrogen phosphate, then water of 3.8wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule of glufosinate-ammonium in 60% mass fraction, yield 99.2%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material.
Example 18. Water soluble granule of 20% glufosinate-ammonium [62] 21.1 g of glufosinate-ammonium, 15 g of sodium dodecyl sulfate, 3 g of tetrasodium EDTA, 7 g of butyl naphthalenesulfonate, 10 g of alkyl fatty alcohol sulfonate, 35 g of dipotassium hydrogen phosphate were mixed with 8.9 g of potassium sulfate, then water of 3.5wt% of the total content of the above described components was added, then the mixture was put into a 1 L kneader for sufficient kneading, extruded to granulate and dried, to obtain a finished product of water soluble granule of glufosinate-ammonium in 20% mass fraction, yield 99.2%; the glufosinate-ammonium technical material in the example was a 95% glufosinate-ammonium technical material.
[63] Conducting quality test on the water soluble granule of glufosinate-ammonium provided by examples 1~18 of the present invention, the test refers to methods provided in “Physical-Chemical method of Pesticide Technical Material and Formulation - CIPAC Handbook”, and the quality standard refers to “FAO pesticide standard setting and user manual” and “Guidelines on drafting specifications of water soluble powder pesticides”, specifically shown as table 1, the performance test results of the water soluble granule of glufosinate-ammonium of examples 1~ 18 is as shown table 2: 11 2016101700 29 Aug 2016
Table 1. Table of test method and standard for water soluble granule of glufo sinate- ammonium Test item Test method Standard Moisture % MT30.5 <3.0 PH MT75.3 5-8 Solubility and stability of dissolution MT179 5 min<1.0% 18 h<0.05% Persistent foamability MT47.2 <45 ml Storage stability MT46.3 54 °C + 2 °C 14d
Table 2. Data table of quality test results for the water soluble granule of glufo sinate- ammonium Test item Ex. No. 'v Moisture % pH Solubility and stability of dissolution Persistent foamability ml Storage stability Example 1 1.11 6.5 5 min 0.3% 18 h 0.02% 14 Qualified Example 2 1.26 6.8 5 min 0.6% 18 h 0.03% 16 Qualified Example 3 1.47 6.3 5 min 0.5% 18 h 0.03% 16 Qualified Example 4 1.24 6.7 5 min 0.6% 18 h 0.02% 15 Qualified Example 5 0.90 6.5 5 min 0.4% 18 h 0.01% 17 Qualified Example 6 1.10 6.8 5 min 0.1% 18 h 0.01% 8 Qualified Example 7 1.24 6.6 5 min 0.3% 18 h 0.01% 10 Qualified Example 8 1.38 6.4 5 min 0.2% 18 h 0.01% 11 Qualified 12 2016101700 29 Aug 2016
Example 9 1.29 6.5 5 min 0.2% 18 h 0.01% 12 Qualified Example 10 1.21 6.8 5 min 0.3% 18 h 0.01% 12 Qualified Example 11 1.28 6.6 5 min 0.8% 18 h 0.04% 20 Qualified Example 12 1.48 6.4 5 min 0.7% 18 h 0.05% 22 Qualified Example 13 1.59 6.5 5 min 0.7% 18 h 0.05% 21 Qualified Example 14 1.61 6.8 5 min 0.8% 18 h 0.04% 22 Qualified Example 15 1.58 6.6 5 min 0.5% 18 h 0.03% 18 Qualified Example 16 1.48 6.4 5 min 0.6% 18 h 0.03% 19 Qualified Example 17 1.51 6.6 5 min 0.5% 18 h 0.03% 20 Qualified Example 18 1.43 6.4 5 min 0.4% 18 h 0.04% 19 Qualified
Note: the water used for testing solubility and stability of dissolution is 3-fold D water, which has a hardness of 1026 mg/L, pH=6.0-7.0, Ca2+:Mg2+=4:l [64] As can be seen from table 2, the water soluble granule of glufosinate-ammonium of the present invention has better solubility and stability of dissolution, as well as lower foamability, in higher 3-fold D water hardness.
Example 19. Test for efficacy [65] The water soluble granules of glufosinate-ammonium of examples 1-18 were selected and used for the test for efficacy in New South Wales, Australia, fallow (formerly planted is buckwheat), mainly for controlling Subterranean clover {Trifolium subterraneum) and Scented goosefoot (Chenopodium multifidum), the above-described control objects were selected and used to conduct comparison of 13 2016101700 29 Aug 2016 efficacy, with a dosage of 2000 g a.i/ha.
Table 3. Data table of comparison of efficay employing the water soluble granules of glufosinate-ammonium of examples 1—18 (21 d after dosing) Examples Control of Subterranean clover, % Control of Scented goosefoot, % 1 96.8 97.1 2 93.2 94.5 3 94.2 95.4 4 95.0 95.9 5 94.7 94.9 6 98.8 100 7 96 96.2 8 96.3 96.8 9 95.8 96.1 10 95.1 96.2 11 82.3 83.2 12 84.0 84.5 13 83.8 84.9 14 83.7 84.5 15 85.7 86.5 16 86.0 87.0 17 86.6 87.2 18 86.9 87.4 Clear water as control 0 0 [66] As can be seen from table 3, the water soluble granules of glufosinate-ammonium of the present invention exhibit better control efficiency in test for efficacy in Australia which is a country with high concentration hard water, also exhibit different control efficiencies amongst different formulae and dosages, with a maximum of 98.8%.
[67] Illustrations of the above examples are used for assisting in understanding the method and core concept of the present invention only. It should be noted that, for an 14 ordinary skilled in the art, some improvements and modifications without departing from the principles of the present invention can be made to the present invention, which also fall within the protection scope of the claims of the present invention. 2016101700 29 Aug 2016 [68] The above described illustration of the disclosed examples enables those skilled in the art to achieve or use the present invention. Various modifications to these examples will be apparent to those skilled in the art, and the general principle defined herein can be implemented in other examples without departing from the spirit or scope of the present invention. Therefore, the present invention will not be limited by these examples as set forth herein, but will accord to the widest scope in accordance with the principles and novel features disclosed herein. 15
Claims (5)
1. A water soluble granule of glufosinate-ammonium, comprising: by weight percentage, 5%~97% of glufosinate-ammonium, 1%~20% of surfactant, 1%~5% of chelator, 0.1%~5% of synergist and the balance of a carrier; the chelator is one or more selected from the group consisting of ethylenediaminetetraacetic acid, disodium ethylenediaminetetraacetate, tetrasodium ethylenediaminetetraacetate and sodium tripolyphosphate; the synergist is one or more selected from the group consisting of butyl naphthalenesulfonate, fatty alcohol polyoxyethylene ether, alkyl fatty alcohol sulfonate and di-sec-octyl maleate sodium sulfonate.
2. The water soluble granule of glufosinate-ammonium according to claim 1, wherein the surfactant is one or more selected from the group consisting of organosillicon polyether, tallow amine polyoxyethylene ether, alkyl glycoside, polyoxyethylene nonyl phenol, fatty amine polyoxyethylene ether, oxirane-epoxypropane block copolymer, alkylphenol polyoxyethylene polyoxypropylene ether, polycarboxylate, polyoxyethylene fatty acid, polyethylene glycol, methyloxirane, fatty alcohol sulfonate, fatty alcohol polyoxyethylene ether alkyl naphthalenesulfonic acid-formaldehyde condensate and sodium dodecyl sulfate; the carrier is one or more selected from the group consisting of ammonium sulfate, diammonium hydrogen phosphate, sodium sulfate, sodium chloride, urea, potassium nitrate, ammonium nitrate, ammonium chloride, dipotassium hydrogen phosphate, fumed silica, potassium sulfate and sodium tripolyphosphate.
3. The water soluble granule of glufosinate-ammonium according to claim 1,wherein the content of the glufosinate-ammonium is 10wt%~80wt%.
4. The water soluble granule of glufosinate-ammonium according to claim 1, wherein a method for preparing the water soluble granule of glufosinate-ammonium is specifically: mixing glufosinate-ammonium, the surfactant and the carrier, to obtain a mixture; mixing the mixture with water, then sequentially conducting extruding granulation and drying, to obtain the water soluble granule of glufosinate-ammonium.
5. The water soluble granule of glufosinate-ammonium according to claim 1, wherein a method for preparing the water soluble granule of glufosinate-ammonium is specifically: mixing glufosinate-ammonium, the surfactant, the chelator, the synergist and the carrier, to obtain a mixture; mixing the mixture with water, then sequentially conducting extruding granulation and drying, to obtain the water soluble granule of glufosinate-ammonium.
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| CN113080199B (en) * | 2021-04-26 | 2022-01-11 | 南开沧州渤海新区绿色化工研究有限公司 | Synergistic composition of herbicide glufosinate |
| CN113262421A (en) * | 2021-06-08 | 2021-08-17 | 江苏乐尔环境科技股份有限公司 | Fly ash chelating agent capable of effectively inhibiting zinc leaching and preparation method thereof |
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| CN104412963A (en) * | 2013-08-29 | 2015-03-18 | 浙江新安化工集团股份有限公司 | Agricultural auxiliary agent, granules and preparation method of agricultural auxiliary agent and granules |
| CN105076199A (en) * | 2015-08-31 | 2015-11-25 | 江苏七洲绿色化工股份有限公司 | Weeding composition and preparation method thereof |
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| CN104412963A (en) * | 2013-08-29 | 2015-03-18 | 浙江新安化工集团股份有限公司 | Agricultural auxiliary agent, granules and preparation method of agricultural auxiliary agent and granules |
| CN105076199A (en) * | 2015-08-31 | 2015-11-25 | 江苏七洲绿色化工股份有限公司 | Weeding composition and preparation method thereof |
| CN105660688A (en) * | 2016-03-01 | 2016-06-15 | 江苏七洲绿色化工股份有限公司 | Soluble refined glufosinate ammonium preparation and preparation method thereof |
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