CN115886019A - Dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl ester and preparation method and application thereof - Google Patents
Dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl ester and preparation method and application thereof Download PDFInfo
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- CN115886019A CN115886019A CN202211305132.6A CN202211305132A CN115886019A CN 115886019 A CN115886019 A CN 115886019A CN 202211305132 A CN202211305132 A CN 202211305132A CN 115886019 A CN115886019 A CN 115886019A
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- Prior art keywords
- ethyl
- methoxone
- pyrazosulfuron
- isooctyl
- percent
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- BGNQYGRXEXDAIQ-UHFFFAOYSA-N Pyrazosulfuron-ethyl Chemical group C1=NN(C)C(S(=O)(=O)NC(=O)NC=2N=C(OC)C=C(OC)N=2)=C1C(=O)OCC BGNQYGRXEXDAIQ-UHFFFAOYSA-N 0.000 title claims abstract description 89
- 239000000375 suspending agent Substances 0.000 title claims abstract description 52
- -1 methoxone isooctyl ester Chemical class 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000003921 oil Substances 0.000 claims abstract description 60
- 239000003381 stabilizer Substances 0.000 claims abstract description 32
- 239000002199 base oil Substances 0.000 claims abstract description 31
- 241000196324 Embryophyta Species 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 239000007787 solid Substances 0.000 claims abstract description 12
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 11
- 239000002270 dispersing agent Substances 0.000 claims abstract description 9
- 239000002562 thickening agent Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 26
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 25
- 239000000203 mixture Substances 0.000 claims description 20
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 16
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 125000005456 glyceride group Chemical group 0.000 claims description 14
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical group CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 14
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 14
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 11
- 239000012053 oil suspension Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- NGFPWHGISWUQOI-UHFFFAOYSA-N 2-sec-butylphenol Chemical group CCC(C)C1=CC=CC=C1O NGFPWHGISWUQOI-UHFFFAOYSA-N 0.000 claims description 6
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- NFIDBGJMFKNGGQ-UHFFFAOYSA-N isopropylmethylphenol Natural products CC(C)CC1=CC=CC=C1O NFIDBGJMFKNGGQ-UHFFFAOYSA-N 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 229920005682 EO-PO block copolymer Polymers 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 239000004359 castor oil Substances 0.000 claims description 5
- 235000019438 castor oil Nutrition 0.000 claims description 5
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 5
- 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 claims description 5
- 238000010008 shearing Methods 0.000 claims description 5
- 238000010902 jet-milling Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- 150000002191 fatty alcohols Chemical class 0.000 claims description 3
- 229920005646 polycarboxylate Polymers 0.000 claims description 3
- 230000035485 pulse pressure Effects 0.000 claims description 3
- 239000004576 sand Substances 0.000 claims description 3
- ZORQXIQZAOLNGE-UHFFFAOYSA-N 1,1-difluorocyclohexane Chemical compound FC1(F)CCCCC1 ZORQXIQZAOLNGE-UHFFFAOYSA-N 0.000 claims description 2
- TVFWYUWNQVRQRG-UHFFFAOYSA-N 2,3,4-tris(2-phenylethenyl)phenol Chemical compound C=1C=CC=CC=1C=CC1=C(C=CC=2C=CC=CC=2)C(O)=CC=C1C=CC1=CC=CC=C1 TVFWYUWNQVRQRG-UHFFFAOYSA-N 0.000 claims description 2
- 239000000440 bentonite Substances 0.000 claims description 2
- 229910000278 bentonite Inorganic materials 0.000 claims description 2
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims description 2
- OOCMUZJPDXYRFD-UHFFFAOYSA-L calcium;2-dodecylbenzenesulfonate Chemical compound [Ca+2].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O.CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O OOCMUZJPDXYRFD-UHFFFAOYSA-L 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 2
- 239000000194 fatty acid Substances 0.000 claims description 2
- 229930195729 fatty acid Natural products 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000011347 resin Substances 0.000 claims description 2
- 229920005989 resin Polymers 0.000 claims description 2
- 239000001593 sorbitan monooleate Substances 0.000 claims description 2
- 229940035049 sorbitan monooleate Drugs 0.000 claims description 2
- 235000011069 sorbitan monooleate Nutrition 0.000 claims description 2
- 238000005507 spraying Methods 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 32
- 230000002363 herbicidal effect Effects 0.000 abstract description 11
- 239000004009 herbicide Substances 0.000 abstract description 10
- 239000005574 MCPA Substances 0.000 abstract description 4
- WHKUVVPPKQRRBV-UHFFFAOYSA-N Trasan Chemical compound CC1=CC(Cl)=CC=C1OCC(O)=O WHKUVVPPKQRRBV-UHFFFAOYSA-N 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 235000019198 oils Nutrition 0.000 description 45
- 239000002253 acid Substances 0.000 description 14
- 239000000575 pesticide Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 241000234646 Cyperaceae Species 0.000 description 9
- 241000209094 Oryza Species 0.000 description 9
- 235000007164 Oryza sativa Nutrition 0.000 description 9
- 239000003814 drug Substances 0.000 description 9
- 238000010899 nucleation Methods 0.000 description 9
- 235000009566 rice Nutrition 0.000 description 9
- QYDYPVFESGNLHU-UHFFFAOYSA-N elaidic acid methyl ester Natural products CCCCCCCCC=CCCCCCCCC(=O)OC QYDYPVFESGNLHU-UHFFFAOYSA-N 0.000 description 8
- QYDYPVFESGNLHU-KHPPLWFESA-N methyl oleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC QYDYPVFESGNLHU-KHPPLWFESA-N 0.000 description 8
- 229940073769 methyl oleate Drugs 0.000 description 8
- 235000012424 soybean oil Nutrition 0.000 description 8
- 239000003549 soybean oil Substances 0.000 description 8
- 235000010446 mineral oil Nutrition 0.000 description 7
- 239000002480 mineral oil Substances 0.000 description 7
- 239000003513 alkali Substances 0.000 description 6
- 230000015556 catabolic process Effects 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 238000009472 formulation Methods 0.000 description 6
- 239000000725 suspension Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 235000015112 vegetable and seed oil Nutrition 0.000 description 6
- 239000008158 vegetable oil Substances 0.000 description 6
- 238000009333 weeding Methods 0.000 description 6
- 150000007530 organic bases Chemical class 0.000 description 5
- 230000000087 stabilizing effect Effects 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 238000005338 heat storage Methods 0.000 description 4
- 230000001965 increasing effect Effects 0.000 description 4
- GHBFNMLVSPCDGN-UHFFFAOYSA-N rac-1-monooctanoylglycerol Chemical compound CCCCCCCC(=O)OCC(O)CO GHBFNMLVSPCDGN-UHFFFAOYSA-N 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- PDIYKJRLQHHRAG-UHFFFAOYSA-N 6-methylheptyl 2-(4-chloro-2-methylphenoxy)acetate Chemical compound CC(C)CCCCCOC(=O)COC1=CC=C(Cl)C=C1C PDIYKJRLQHHRAG-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000005564 Halosulfuron methyl Substances 0.000 description 3
- FMGZEUWROYGLAY-UHFFFAOYSA-N Halosulfuron-methyl Chemical group ClC1=NN(C)C(S(=O)(=O)NC(=O)NC=2N=C(OC)C=C(OC)N=2)=C1C(=O)OC FMGZEUWROYGLAY-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000004480 active ingredient Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003153 chemical reaction reagent Substances 0.000 description 3
- 235000005687 corn oil Nutrition 0.000 description 3
- 239000002285 corn oil Substances 0.000 description 3
- GHVNFZFCNZKVNT-UHFFFAOYSA-M decanoate Chemical compound CCCCCCCCCC([O-])=O GHVNFZFCNZKVNT-UHFFFAOYSA-M 0.000 description 3
- UAOMVDZJSHZZME-UHFFFAOYSA-N diisopropylamine Chemical compound CC(C)NC(C)C UAOMVDZJSHZZME-UHFFFAOYSA-N 0.000 description 3
- AMFGTOFWMRQMEM-UHFFFAOYSA-N triazophos Chemical compound N1=C(OP(=S)(OCC)OCC)N=CN1C1=CC=CC=C1 AMFGTOFWMRQMEM-UHFFFAOYSA-N 0.000 description 3
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000004945 emulsification Methods 0.000 description 2
- 229940080812 glyceryl caprate Drugs 0.000 description 2
- 229940087068 glyceryl caprylate Drugs 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000003801 milling Methods 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
- LCPDWSOZIOUXRV-UHFFFAOYSA-N phenoxyacetic acid Chemical compound OC(=O)COC1=CC=CC=C1 LCPDWSOZIOUXRV-UHFFFAOYSA-N 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 159000000000 sodium salts Chemical class 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 2
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 2
- LKUNXBRZDFMZOK-GFCCVEGCSA-N Capric acid monoglyceride Natural products CCCCCCCCCC(=O)OC[C@H](O)CO LKUNXBRZDFMZOK-GFCCVEGCSA-N 0.000 description 1
- 239000005558 Fluroxypyr Substances 0.000 description 1
- 235000019482 Palm oil Nutrition 0.000 description 1
- 231100000674 Phytotoxicity Toxicity 0.000 description 1
- 240000004713 Pisum sativum Species 0.000 description 1
- 235000010582 Pisum sativum Nutrition 0.000 description 1
- 241000209504 Poaceae Species 0.000 description 1
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 240000006394 Sorghum bicolor Species 0.000 description 1
- 235000011684 Sorghum saccharatum Nutrition 0.000 description 1
- 229940100389 Sulfonylurea Drugs 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 244000098338 Triticum aestivum Species 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- SMLHHBQGIJMAIM-UHFFFAOYSA-N calcium;2-dodecylbenzenesulfonic acid Chemical compound [Ca].CCCCCCCCCCCCC1=CC=CC=C1S(O)(=O)=O SMLHHBQGIJMAIM-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004033 diameter control Methods 0.000 description 1
- 229940043279 diisopropylamine Drugs 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 238000007336 electrophilic substitution reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000009313 farming Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- MEFQWPUMEMWTJP-UHFFFAOYSA-N fluroxypyr Chemical compound NC1=C(Cl)C(F)=NC(OCC(O)=O)=C1Cl MEFQWPUMEMWTJP-UHFFFAOYSA-N 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000013350 formula milk Nutrition 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- TTWJBBZEZQICBI-UHFFFAOYSA-N metoclopramide Chemical compound CCN(CC)CCNC(=O)C1=CC(Cl)=C(N)C=C1OC TTWJBBZEZQICBI-UHFFFAOYSA-N 0.000 description 1
- 229960004503 metoclopramide Drugs 0.000 description 1
- 239000002540 palm oil Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- STAPBGVGYWCRTF-UHFFFAOYSA-M sodium;2-(4-chloro-2-methylphenoxy)acetate Chemical compound [Na+].CC1=CC(Cl)=CC=C1OCC([O-])=O STAPBGVGYWCRTF-UHFFFAOYSA-M 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- YROXIXLRRCOBKF-UHFFFAOYSA-N sulfonylurea Chemical class OC(=N)N=S(=O)=O YROXIXLRRCOBKF-UHFFFAOYSA-N 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009885 systemic effect Effects 0.000 description 1
- LADGBHLMCUINGV-UHFFFAOYSA-N tricaprin Chemical compound CCCCCCCCCC(=O)OCC(OC(=O)CCCCCCCCC)COC(=O)CCCCCCCCC LADGBHLMCUINGV-UHFFFAOYSA-N 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to a herbicide, in particular to a dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl ester, a preparation method and application thereof, wherein the dispersible oil suspending agent comprises the following components in percentage by mass: 1 to 12 percent of pyrazosulfuron-ethyl, 1 to 60 percent of dimethyl-tetrachloro-isooctyl ester, 8 to 25 percent of emulsifier, 0.1 to 6 percent of dispersant, 0.1 to 5 percent of thickener, 0.1 to 5 percent of solid stabilizer, 0.1 to 5 percent of liquid stabilizer and 100 percent of carrier oil phase. Compared with the prior art, the dispersible oil suspending agent containing pyrazosulfuron-ethyl and MCPA is environment-friendly, good in stability, high in farmland weed control effect, simple and convenient in preparation method and easy for industrial mass production.
Description
Technical Field
The invention relates to a herbicide, in particular to a dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl ester, and a preparation method and application thereof.
Background
Pyrazosulfuron-ethyl is a sulfonylurea high-activity systemic selective ALS herbicide, and is suitable for preventing and killing annual or perennial broadleaf weeds, cyperaceae and partial gramineous weeds in rice seedling fields, direct seeding fields, transplanting fields and seedling throwing fields. The methoxone is a phenoxyacetic acid selective hormone herbicide, is easy to be absorbed by roots and leaves, and is mainly used for preventing and killing various annual and perennial broadleaf weeds after seedling in rice, wheat, peas, lawns and non-farming areas. Methoxone itself is an acid, with very low solubility in water, and is typically produced as an ester or salt. The commercial forms are generally dimethyl tetrachloroisooctyl and dimethyl tetrachloro sodium salt, wherein the dimethyl tetrachloro sodium salt has poor low temperature resistance and is easy to cause phytotoxicity at low temperature; the safety and the weeding activity of the methoxone isooctyl ester are higher than those of methoxone sodium salt. The reasonable compounding of the pyrazosulfuron-ethyl and the methoxone isooctyl ester can expand the weeding spectrum and improve the weeding activity of the agent.
The currently marketed raw pesticide of the MCPA often contains a certain amount of free acid, and the content of the free acid in enterprise standard for producing the raw pesticide is generally required to be less than or equal to 1.5 percent through inquiry. Although the content of free acid in the raw methoxone isooctyl ester is controlled, the residual free acid has great influence on the chemical stability of pyrazosulfuron-ethyl, which can cause the content degradation. In addition, the residual free acid content of different batches of raw methoxone isooctyl ester produced by different enterprises, even the same enterprise, fluctuates. The formula is not favorable for developing a stable pyrazosulfuron-ethyl and methoxone isooctyl ester dispersible oil suspending agent formula. In order to neutralize free acid, it is common practice to add organic bases, such as triethanolamine and diisopropylamine, to the dispersible oil suspension formulation, although the free acid can be neutralized, the viscosity of the system is inevitably increased, and the dispersibility of the product in water is poor, the fluidity is poor and even the problem of bottom formation occurs. Meanwhile, practice proves that the organic base can accelerate and promote the degradation of pyrazosulfuron-ethyl in the dispersible oil suspending agent.
In addition, in the development of the traditional dispersible oil suspending agent formula, vegetable oil, mineral oil and the like such as methyl oleate, soybean oil, rapeseed oil, corn oil, palm oil and the like are generally adopted as the carrier oil phase. However, the methyl oleate in the market has uneven quality, and components such as methanol and water are easy to remain in the production and synthesis process, which can further cause the pyrazosulfuron-ethyl to degrade; meanwhile, vegetable oil such as methyl oleate, soybean oil and the like contains unsaturated fatty acid, and is easy to rot and rancidity when stored at room temperature, which is one of unstable factors of the system product and also easily causes the degradation of pyrazosulfuron-ethyl, even the product is pasted and solidified. One of the difficulties with mineral oil systems today is the difficulty in emulsification. It is therefore necessary to screen for a more suitable carrier oil phase.
The research on the herbicide has been more, for example, an organic inhibition type rice herbicide is related in patent document CN113519543A, a gramineae lawn compound herbicide is related in patent document CN1939129A, and a sorghum field herbicide is related in patent document CN104396985A, but the compound of pyrazosulfuron-ethyl and methoxone isooctyl, corresponding dispersible oil suspending agents and preparation methods thereof are not mentioned in the three documents. Although the CN112244035A relates to a herbicidal composition containing halosulfuron-methyl, fluroxypyr and methoxone and mentions that the related dosage form contains dispersible oil suspending agent, the formulation adopted in the patent document is the combination of halosulfuron-methyl, which has great limitations in the application range and application method, and no solution is given about the specific formulation of dispersible oil suspending agent or the problems encountered in the process of developing the formulation, and it is difficult to be used as the basis for improving the combination of halosulfuron-methyl and methoxone isooctyl.
In conclusion, although the herbicide formed by reasonably compounding pyrazosulfuron-ethyl and methoxone isooctyl can expand the weeding spectrum and improve the weeding activity of the herbicide; however, the problem of pyrazosulfuron-ethyl stability is solved, and related formulas are only reported in few researches, so that the invention provides a dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl to fill the gap in the aspect.
Disclosure of Invention
The invention aims to solve at least one of the problems and provide a dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl and a preparation method and application thereof.
The purpose of the invention is realized by the following technical scheme:
the invention discloses a dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl, which comprises the following components in percentage by mass:
1 to 12 percent of pyrazosulfuron-ethyl, 1 to 60 percent of dimethyl-tetrachloro-isooctyl ester, 8 to 25 percent of emulsifier, 0.1 to 6 percent of dispersant, 0.1 to 5 percent of thickener, 0.1 to 5 percent of solid stabilizer, 0.1 to 5 percent of liquid stabilizer and 100 percent of carrier oil phase.
Preferably, the mass ratio of the pyrazosulfuron-ethyl to the methoxone isooctyl ester is 1.
Pyrazosulfuron-ethyl (pyrazosulfuron-ethyl), CAS accession number [93697-74-6], chemical structural formula is:
MCPA-isooctyl ester (MCPA-isooctyl), CAS number [26544-20-7], and chemical structural formula as follows:
the weight sum of the pyrazosulfuron-ethyl and the methoxone isooctyl in the oil suspending agent accounts for 1-72 percent of the total weight of the pesticide preparation.
Preferably, the first and second electrodes are formed of a metal,
the emulsifier is one or more of calcium dodecyl benzene sulfonate, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, tristyrylphenol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, sorbitan monooleate polyoxyethylene ether, sorbitan fatty acid ester and EO-PO block copolymer;
the dispersing agent is one or more of alkylphenol polyoxyethylene phosphate, castor oil polyoxyethylene phosphate, polycarboxylate and EO-PO block copolymer;
the thickening agent is one or two of organic bentonite and white carbon black;
the solid stabilizer is one or two of sodium dodecyl benzene sulfonate and anhydrous sodium carbonate;
the liquid stabilizer is o-sec-butylphenol;
the carrier oil phase is caprylic/capric glyceride or a mixture of solvent oil S-200 and caprylic/capric glyceride.
It is further preferred that the first and second liquid crystal display panels,
the emulsifier is one or a mixture of any more of dodecyl benzene sulfonic acid calcium (no water and alcohol system), alkylphenol ethoxylates OP-4, OP-7 and OP-10, fatty alcohol polyoxyethylene ether AEO-3, castor oil polyoxyethylene ether EL-10, EL-20, BY-125 and EO-PO block copolymer ethan 992 and ethan NS-500LQ mixed in any proportion;
the dispersant is one or a mixture OF any several OF polycarboxylate SP-OF3472B, atlox 4912 and Atlox 4914 mixed in any proportion.
Preferably, the solid stabilizer is a mixture of sodium dodecyl benzene sulfonate and anhydrous sodium carbonate, wherein the mass ratio of the sodium dodecyl benzene sulfonate to the anhydrous sodium carbonate is = 1.
Preferably, the mass ratio of the solid stabilizer to the liquid stabilizer is = 4.
Preferably, when the content of the tetrachloro isooctyl ester is less than 30%, the carrier oil phase is caprylic capric glyceride; when the content of the tetrachloro-isooctyl ester is more than or equal to 30 percent, the carrier oil phase is a mixture of solvent oil S-200 and caprylic/capric glyceride.
The second aspect of the invention discloses a method for preparing any one of the dispersible oil suspending agents containing pyrazosulfuron-ethyl and methoxone isooctyl, which comprises the following steps:
s1: the pyrazosulfuron-ethyl and the solid-state stabilizer are stirred and mixed according to the formula proportion, then the mixture is subjected to airflow grinding to obtain the particle size D90 of less than or equal to 18 mu m, and the ground materials are stirred and mixed again;
s2: adding an emulsifier and a liquid stabilizer into a part of carrier oil phase according to a formula ratio, and stirring until the emulsifier and the liquid stabilizer are uniformly mixed;
s3: adding the dimethyl tetrachloro isooctyl ester into the solution obtained in the step S2, and continuously stirring until the mixture is uniformly mixed;
s4: adding a thickening agent and the mixed material obtained in the step S1 into the mixed liquid obtained in the step S3, and shearing until the mixed material is uniformly mixed;
s5: sanding the sheared material in the step S4 until the particle size D90 is less than or equal to 5 mu m;
s6: and (5) adding a dispersing agent and the residual carrier oil phase into the material subjected to sanding in the step S5, and shearing until the materials are uniformly mixed to obtain the dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl ester.
Preferably, the first and second electrodes are formed of a metal,
in the step S1, the stirring and mixing time is 30min; the crushing pressure of the jet milling is 0.78-0.8 MPa, the pulse pressure is 0.4-0.5 MPa, the frequency of the grading wheel is 42Hz, and the feeding frequency is 3-5 Hz;
in the step S2, part of the carrier oil phase accounts for 70-90% of the formula amount of the carrier oil phase;
in the step S5, the sanding is carried out in a horizontal sand mill by adopting three-stage series connection, and the material temperature in the sanding process is less than or equal to 30 ℃.
The third aspect of the invention discloses an application of the dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl in preventing and killing farmland weeds.
Preferably, the farmland weeds are paddy field weeds, and an application method of spraying stem leaves is adopted, but other application technologies applied in agriculture can be adopted according to needs to be used for different farmland weeds.
Compared with the prior art, the invention has the following beneficial effects:
practice proves that the chemical stability of the pyrazosulfuron-ethyl is poor in the oil suspending agent compounded by the pyrazosulfuron-ethyl and the methoxone isooctyl, but the chemical stability of the pyrazosulfuron-ethyl is good in the dispersible oil suspending agent containing the pyrazosulfuron-ethyl and the methoxone isooctyl obtained by the formula scheme of the invention, the decomposition rate of the pyrazosulfuron-ethyl in heat storage tests (54 ℃ and 65 ℃ and 14 d) is lower than 5%, and the pyrazosulfuron-ethyl is benefited by:
1) According to physicochemical properties, the pyrazosulfuron-ethyl is easy to degrade when meeting water and alcohol, and all raw materials selected in the formula components are systems without water and alcohol, so that a good stable environment is created for the pyrazosulfuron-ethyl.
2) The stabilizer combination provided by the invention is one of the keys of pyrazosulfuron-ethyl stability. According to the existing research, a certain amount of free acid is often contained in the raw methoxone isooctyl ester, the pH value of the free acid is generally between 3.0 and 5.0, pyrazosulfuron-ethyl can be degraded in the environment, and the addition of organic base to neutralize the free acid can increase the viscosity of the system easily, so that the product has poor water dispersibility, poor fluidity and even the problem of bottom coagulation. Meanwhile, practice proves that the organic base can promote the degradation of pyrazosulfuron-ethyl in the dispersible oil suspending agent. One of the functions of the anhydrous sodium carbonate in the solid stabilizer is to replace organic alkali and neutralize residual free acid in the raw pesticide of the MCPA, and meanwhile, the viscosity of the dispersible oil suspending agent product cannot be additionally increased; the anhydrous sodium carbonate has another function of being a pH regulator of a system, and the pH value of the dispersible oil suspending agent containing the pyrazosulfuron-ethyl and the methoxone isooctyl ester can be controlled between 6.5 and 8.0. Based on the stabilizer anhydrous sodium carbonate, anhydrous sodium carbonate and twelve sodium carbonate are adoptedThe combination of sodium alkyl benzene sulfonate and o-sec-butylphenol has good stabilizing effect on pyrazosulfuron-ethyl. The possible reason is that under the microenvironment, the product contains trace moisture and H in water molecules + The water-soluble polymer is used as an electrophilic reagent to attack an aromatic ring on the sodium dodecyl benzene sulfonate to generate electrophilic substitution reaction, so that the moisture content is reduced, and the adverse effect of moisture on the pyrazosulfuron-ethyl is further reduced; and o-sec-butylphenol has an antioxidant action. The combination of the anhydrous sodium carbonate, the sodium dodecyl benzene sulfonate and the o-sec-butylphenol stabilizer plays a role in synergistic stabilization.
3) The carrier oil phase caprylic capric glyceride provided by the invention is also an important factor for the stability of pyrazosulfuron-ethyl. According to the existing research, the defects that the oil phase of the traditional dispersible oil suspending agent carrier is 1) easy to cause pyrazosulfuron-ethyl degradation, 2) the unsaturated fatty acid is easy to rot and rancidity when stored at room temperature, and 3) the mineral oil system is difficult to emulsify exist in the product system.
Compared with the traditional vegetable oil and mineral oil such as carrier oil phase methyl oleate, soybean oil and corn oil, the pyrazosulfuron-ethyl and methoxone isooctyl-containing dispersible oil suspending agent obtained by using the caprylic capric triglyceride as the carrier oil phase has relatively better weeding effect, and the reason may be that:
1) According to the principle of similarity and compatibility, the compatibility of the caprylic-capric glyceride and the target weed leaves is stronger, and the medicament can penetrate through the wax layer of the leaves more easily, so that the absorption rate of the medicament by the weeds is improved.
2) The caprylic capric glyceride has certain emulsification stabilizing function, is easier to emulsify compared with vegetable oil such as soybean oil and mineral oil, has smaller emulsified particle size after being diluted by water, and is beneficial to the absorption of liquid medicine in the impurity removing process.
3) The caprylic capric glyceride has good film forming and moisture retention performances, the retention time of the liquid medicine sprayed to the leaves is longer, and the drug effect is effectively guaranteed.
4) The caprylic capric acid glyceride can be absorbed by leaves, and has effect in promoting plant metabolism, thereby increasing the absorption of the leaves to the medicinal preparation.
5) Compared with vegetable oil such as methyl oleate, soybean oil and the like, the caprylic/capric glyceride has better low-temperature performance, still has good fluidity and transparency at the low temperature of minus 10 ℃, is more convenient to use, and is particularly used in northern areas.
In addition, at present, the caprylin-caprin is not found in application reports of pesticide dispersible oil suspending agents, and is mainly used in food, cosmetics and pharmaceutical industries. Therefore, the glyceryl caprylate and caprate serving as the carrier oil phase is innovatively applied to the formula of the dispersible oil suspending agent containing the pyrazosulfuron-ethyl and the methoxone isooctyl ester, unpredictably plays three roles of stabilizing the pyrazosulfuron-ethyl, carrying the oil phase and enhancing the effect, and is an excellent substitute for the traditional carrier oil phase of vegetable oil such as methyl oleate, soybean oil and corn oil and mineral oil.
Different from the traditional preparation method of dispersible oil suspending agent, the preparation method of the invention carries out jet milling on pyrazosulfuron-ethyl original drug, solid stabilizer sodium dodecyl benzene sulfonate and anhydrous sodium carbonate in advance, and has the advantages that:
1) Because the compatibility of the sodium dodecyl benzene sulfonate and the anhydrous sodium carbonate with the carrier oil phase is poor, although the anhydrous sodium carbonate replaces organic alkali to solve one of the technical problems of the invention, the problems of non-fine sanding, uneven particle distribution and the like easily occur when the anhydrous sodium carbonate is directly sanded together with other materials in the practical application in the formula, so that the stability and the repeatability among product batches are poor. In the preparation method, the air flow crushing is carried out in advance, and the sodium dodecyl benzene sulfonate and the anhydrous sodium carbonate particles are pulverized in advance, so that the sodium dodecyl benzene sulfonate and the anhydrous sodium carbonate particles are more easily and uniformly distributed in a dispersible oil suspending agent system, and meanwhile, the problem of low sanding efficiency is solved.
2) The sodium dodecyl benzene sulfonate has the function of a wetting agent besides the function of a stabilizer, and is subjected to air flow crushing together with the pyrazosulfuron-ethyl technical product, so that the crushing efficiency of the pyrazosulfuron-ethyl is improved.
3) Because the original pesticide of the metoclopramide is oily liquid, the original pesticide of the pyrazosulfuron-ethyl is crushed in advance, and the sanding efficiency of the whole system is improved.
In view of the above, it is desirable to provide,
1) According to the invention, anhydrous sodium carbonate is selected to replace organic alkali to neutralize free acid in the raw methoxone isooctyl ester, so that the problems of poor dispersibility in water, poor fluidity and even bottom formation of the product caused by the increase of the viscosity of the system due to the addition of the organic alkali to neutralize the free acid are solved, and the adverse effect of the organic alkali on pyrazosulfuron-ethyl in the system is avoided.
2) The glyceryl caprylate and caprate serving as the carrier oil phase is innovatively introduced into the pesticide dispersible oil suspending agent for application, and the pyrazosulfuron-ethyl and MCPA dispersible oil suspending agent provided by the invention has the triple effects of stabilizing the pyrazosulfuron-ethyl, carrying the oil phase and remarkably increasing the effect.
3) According to the preparation method, the pyrazosulfuron-ethyl original medicine, the stabilizer sodium dodecyl benzene sulfonate and the anhydrous sodium carbonate are subjected to airflow crushing in advance, so that the problems of uneven distribution and low sanding efficiency of the stabilizer sodium dodecyl benzene sulfonate and the anhydrous sodium carbonate in a product system are effectively solved, and the stability and repeatability of the quality among batches of the product are ensured.
4) The dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl ester provided by the invention is environment-friendly, good in stability and high in effect of preventing farmland weeds.
5) The preparation method provided by the invention is simple and convenient in process and easy to industrialize.
Detailed Description
The present invention is described in detail below with reference to specific examples, but the present invention is not limited thereto in any way.
In the following examples, unless otherwise specified, commercially available reagents that can be routinely obtained by those skilled in the art may be used as the reagents used, and the methods used may be those conventionally used in the art. And, all percentages are by mass unless otherwise indicated.
Example 1
The preparation method of the dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl (formula shown in table 1) comprises the following steps:
1) Putting pyrazosulfuron-ethyl original drug and a solid stabilizer (sodium dodecyl benzene sulfonate and anhydrous sodium carbonate) into a mixing kettle according to a formula ratio, and stirring for 30 minutes; starting a freeze dryer, an air compressor and a 600 type jet mill in sequence, adjusting the milling pressure to be within the range of 0.75-0.8 MPa, the pulse pressure to be within the range of 0.4-0.5 MPa, the frequency of a grading wheel to be 42Hz, slowly adding the mixed materials at the feeding frequency of 3-5 Hz for jet milling, and controlling the milling particle size to be D90 to be less than or equal to 18 mu m; and (3) putting the crushed materials into a mixer for mixing, and stirring for 30 minutes to obtain the materials for later use.
2) Adding an emulsifier and a liquid stabilizer o-sec-butylphenol into a reaction kettle filled with a quantitative carrier oil phase according to a formula ratio, and opening a stirring device to stir for 5 minutes until the materials are uniformly mixed; wherein the adding amount of the carrier oil phase added in the step is controlled to be 70-90% of the total amount of the carrier oil phase.
3) Adding the raw material of the dimethyl tetrachloro isooctyl ester into the mixture obtained in the step 2), and continuously stirring for 10 minutes until the materials are uniformly mixed.
4) Adding the thickening agent and the materials prepared in the step 1) into the step 3), and cutting for 15-25 minutes until the materials are uniformly mixed.
5) Transfer to horizontal sand mill with the material of misce bene in the above-mentioned 4) and carry out the sanding (tertiary series connection, material temperature is less than or equal to 30 ℃ during the sanding), particle diameter control range behind the material sanding: d90 is less than or equal to 5 mu m (the dispersion medium is the corresponding carrier oil phase during detection).
6) Transferring the sanded material to a transfer kettle, adding a dispersing agent and the balance of a carrier oil phase, shearing for 20 minutes until the materials are uniformly mixed, and detecting and subpackaging to obtain the dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl.
Examples 2 to 6
The procedure was as in example 1, and the formulations of the examples are shown in Table 1.
TABLE 1 formulations for examples 1-6
The dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl ester obtained in examples 1-6 was tested for suspension rate, pourability, wet sieve test, persistent foamability, low temperature stability, thermal storage stability and other properties, and the test data are shown in table 2 (in the table, raw drug A refers to pyrazosulfuron-ethyl, raw drug B refers to methoxone isooctyl ester);
wherein, the first and the second end of the pipe are connected with each other,
the content of active ingredients is as follows: measuring by HPLC;
suspension percentage: according to GB/T14825-2006;
pH value: according to GB/T1601-1993;
moisture content: proceeding according to GB/T1600-2021;
fineness determination method (i.e. wet sieve test): performed according to GB/T16150-1995;
dispersion stability: reference GB 28155-2011;
pourability: according to GB/T31737-2015;
and (3) durable foaming property: according to GB/T28137-2011;
heat storage stability: according to GB/T19136-2021;
low-temperature stability: the method is carried out according to GB/T19137-2003.
Table 2 results of performance test of examples 1 to 6
Note: in the table, the raw pesticide A refers to pyrazosulfuron-ethyl, and the raw pesticide B refers to methoxone isooctyl ester.
As can be seen from Table 2, the dispersible oil suspension agent products containing pyrazosulfuron-ethyl and methoxone isooctyl prepared in examples 1-6 have excellent dispersibility, suspension rate, pourability, wet sieve test, persistent foamability, cold storage stability (-5 ℃) and heat storage stability (65 ℃ and 54 ℃) and the like, wherein the products have good heat storage stability, do not cream and bottom, have good fluidity, and have degradation rates of pyrazosulfuron-ethyl and methoxone isooctyl lower than 5%. It can be seen that the preparation processes of examples 1 to 6 are simple and convenient, and are easy for industrial production.
The 16% pyrazosulfuron-ethyl and methoxone isooctyl dispersible oil suspension prepared in the example 1 is applied to direct seeding paddy fields for preventing and killing annual broadleaf and cyperaceae weeds, the dosage of the effective components is 240-350 g/hectare, the control effect of the whole plant in 15 days is 86.49-90.37%, the control effect of the whole plant in 30 days is 88.77-92.45%, and the control effect of the whole fresh weight in 30 days is 91.22-94.88%, so that the suspension is safe for paddy rice.
The 18% pyrazosulfuron-ethyl and methoxone isooctyl dispersible oil suspension prepared in the example 2 is applied to direct seeding paddy fields for preventing and killing annual broadleaf and cyperaceae weeds, the dosage of the effective components is 240-350 g/hectare, the control effect of the whole plant in 15 days is 87.55-91.14%, the control effect of the whole plant in 30 days is 89.96-93.08%, and the control effect of the whole fresh weight in 30 days is 92.42-95.67%, so that the oil suspension is safe for paddy rice.
The 55% pyrazosulfuron-ethyl and methoxone isooctyl dispersible oil suspension prepared in the embodiment 3 is applied to a direct seeding paddy field for controlling annual broadleaf and cyperaceae weeds, the dosage of the active ingredients is 240-350 g/hectare, the control effect of the whole plant in 15 days is 87.95-91.22%, the control effect of the whole plant in 30 days is 90.12-93.96%, and the control effect of the whole fresh weight in 30 days is 92.65-96.02%, so that the suspension is safe for paddy rice.
The 42 percent pyrazosulfuron-ethyl and methoxone isooctyl dispersible oil suspension prepared in the embodiment 4 is applied to direct seeding paddy fields for preventing and killing annual broadleaf and cyperaceae weeds, the dosage of the effective components is 240 to 350 g/hectare, the control effect of the whole plant in 15 days is 86.55 to 90.13 percent, the control effect of the whole plant in 30 days is 88.46 to 92.24 percent, and the control effect of the whole fresh weight in 30 days is 91.07 to 94.46 percent, thus being safe for paddy rice.
The 64% pyrazosulfuron-ethyl-methoxone isooctyl dispersible oil suspension prepared in the example 5 is applied to direct seeding paddy fields for preventing and killing annual broadleaf and cyperaceae weeds, the dosage of the effective components is 240-350 g/hectare, the control effect of the whole plant in 15 days is 87.00-90.69%, the control effect of the whole plant in 30 days is 88.92-92.66%, and the control effect of the whole fresh weight in 30 days is 92.32-95.05%, so that the suspension is safe for paddy rice.
The 72 percent pyrazosulfuron-ethyl and methoxone isooctyl dispersible oil suspending agent prepared in the embodiment 6 is applied to a direct seeding paddy field to control annual broadleaf and cyperaceae weeds, the dosage of the active ingredients is 240 to 350 g/hectare, the control effect of the whole plant in 15 days is 87.16 to 90.05 percent, the control effect of the whole plant in 30 days is 89.00 to 92.75 percent, and the control effect of the whole fresh weight in 30 days is 91.69 to 94.94 percent, so that the dispersible oil suspending agent is safe for paddy rice.
Therefore, the dispersible oil suspension containing pyrazosulfuron-ethyl and methoxone isooctyl prepared by the invention has good effect of preventing and killing annual broadleaf and cyperaceae weeds when being applied to direct-seeding paddy fields, and is safe for paddy.
Comparative examples 1 to 6
The anhydrous sodium carbonate in the formulas of the embodiments 1 to 6 is replaced by triethanolamine serving as an organic base, the other components and the use amount of the triethanolamine are kept unchanged, the corresponding pH value is controlled, and the detection proves that the decomposition rates of the pyrazosulfuron-ethyl in the dispersible oil suspending agent products containing the pyrazosulfuron-ethyl and the methoxone isooctyl prepared in the comparative examples 1 to 6 are all not qualified and are all more than 30%, and the phenomena of viscosity increase in different degrees or creaming and bottom forming in different degrees can occur. Therefore, in the formula of the oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl, the stabilizing effect of the anhydrous sodium carbonate is better than that of triethanolamine which is an organic alkali, and the prepared dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl has the advantages of good physical stability, no creaming and good fluidity.
Comparative examples 7 to 9
The glycerol caprylate and caprate components in the formula of the example 2 are respectively replaced by methyl oleate (comparative example 7), soybean oil (comparative example 8) and mineral oil (white oil No. 10) (comparative example 9), and the oil suspending agent with the new formula is applied to a direct seeding paddy field to control annual broadleaf weeds and cyperaceae weeds, and the field test results are as follows:
from the above data, it can be seen that the synergy of caprylic capric glyceride in the formula of the present invention is most significant compared with methyl oleate, soybean oil and 10# white oil.
The embodiments described above are intended to facilitate a person of ordinary skill in the art in understanding and using the invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make modifications and alterations without departing from the scope of the present invention.
Claims (10)
1. A dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl is characterized by comprising the following components in percentage by mass:
1 to 12 percent of pyrazosulfuron-ethyl, 1 to 60 percent of dimethyl-tetrachloro-isooctyl ester, 8 to 25 percent of emulsifier, 0.1 to 6 percent of dispersant, 0.1 to 5 percent of thickener, 0.1 to 5 percent of solid stabilizer, 0.1 to 5 percent of liquid stabilizer and 100 percent of carrier oil phase.
2. The dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl as claimed in claim 1, wherein the mass ratio of pyrazosulfuron-ethyl to methoxone isooctyl is 1.
3. The dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl ester according to claim 1,
the emulsifier is one or more of calcium dodecyl benzene sulfonate, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, tristyrylphenol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, sorbitan monooleate polyoxyethylene ether, sorbitan fatty acid ester and EO-PO block copolymer;
the dispersing agent is one or more of alkylphenol polyoxyethylene phosphate, castor oil polyoxyethylene phosphate, polycarboxylate and EO-PO block copolymer;
the thickening agent is one or two of organic bentonite and white carbon black;
the solid stabilizer is one or two of sodium dodecyl benzene sulfonate and anhydrous sodium carbonate;
the liquid stabilizer is o-sec-butylphenol;
the carrier oil phase is caprylic/capric glyceride or a mixture of solvent oil S-200 and caprylic/capric glyceride.
4. The dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl ester as claimed in claim 3, wherein the solid stabilizer is a mixture of sodium dodecylbenzene sulfonate and anhydrous sodium carbonate, wherein the mass ratio of sodium dodecylbenzene sulfonate to anhydrous sodium carbonate is = 1-4.
5. The dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl as claimed in claim 3, is characterized in that the mass ratio of the solid stabilizer to the liquid stabilizer is = 4.
6. The dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl as claimed in claim 3, wherein when the methoxone isooctyl content is less than 30%, the carrier oil phase is caprylic capric glyceride; when the content of the methoxone isooctyl ester is more than or equal to 30 percent, the carrier oil phase is a mixture of solvent oil S-200 and caprylic/capric glyceride.
7. A method for preparing the dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl as described in any one of claims 1 to 6, which comprises the following steps:
s1: the pyrazosulfuron-ethyl and the solid-state stabilizer are stirred and mixed according to the formula proportion, then the mixture is subjected to airflow grinding to obtain the particle size D90 of less than or equal to 18 mu m, and the ground materials are stirred and mixed again;
s2: adding the emulsifier and the liquid stabilizer into part of the carrier oil phase according to the formula proportion, and stirring until the emulsifier and the liquid stabilizer are uniformly mixed;
s3: adding the dimethyl tetrachloro isooctyl ester into the solution obtained in the step S2, and continuously stirring until the mixture is uniformly mixed;
s4: adding a thickening agent and the mixed material obtained in the step S1 into the mixed liquid obtained in the step S3, and shearing the mixed liquid until the mixed liquid is uniformly mixed;
s5: sanding the sheared material in the step S4 until the particle size D90 is less than or equal to 5 mu m;
s6: and (4) adding a dispersing agent and the residual carrier oil phase into the material subjected to sanding in the step (S5), and shearing until the materials are uniformly mixed to obtain the dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl ester.
8. The preparation method of the dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl ester as claimed in claim 7,
in the step S1, the stirring and mixing time is 30min; the crushing pressure of the jet milling is 0.78-0.8 MPa, the pulse pressure is 0.4-0.5 MPa, the frequency of the grading wheel is 42Hz, and the feeding frequency is 3-5 Hz;
in the step S2, part of the carrier oil phase accounts for 70-90% of the formula amount of the carrier oil phase;
in the step S5, the sanding is carried out in a horizontal sand mill by adopting three-stage series connection, and the material temperature in the sanding process is less than or equal to 30 ℃.
9. The use of the dispersible oil suspending agent containing pyrazosulfuron-ethyl and methoxone isooctyl as defined in any one of claims 1 to 6 for preventing and killing farmland weeds.
10. The application of the dispersible oil suspension concentrate containing pyrazosulfuron-ethyl and methoxone isooctyl as claimed in claim 9, wherein the farmland weeds are paddy field weeds, and the application method of stem and leaf spraying is adopted.
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