CN108552183B - Suspended seed coating agent of difenapyr and its application - Google Patents
Suspended seed coating agent of difenapyr and its application Download PDFInfo
- Publication number
- CN108552183B CN108552183B CN201810241669.8A CN201810241669A CN108552183B CN 108552183 B CN108552183 B CN 108552183B CN 201810241669 A CN201810241669 A CN 201810241669A CN 108552183 B CN108552183 B CN 108552183B
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- agent
- seed coating
- suspension seed
- parts
- mefenpyr
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- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 235000010489 acacia gum Nutrition 0.000 description 1
- 239000000205 acacia gum Substances 0.000 description 1
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229940023476 agar Drugs 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229920005550 ammonium lignosulfonate Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000440 bentonite Substances 0.000 description 1
- 229910000278 bentonite Inorganic materials 0.000 description 1
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 description 1
- 229940077388 benzenesulfonate Drugs 0.000 description 1
- DMSMPAJRVJJAGA-UHFFFAOYSA-N benzo[d]isothiazol-3-one Chemical compound C1=CC=C2C(=O)NSC2=C1 DMSMPAJRVJJAGA-UHFFFAOYSA-N 0.000 description 1
- 229920005551 calcium lignosulfonate Polymers 0.000 description 1
- RYAGRZNBULDMBW-UHFFFAOYSA-L calcium;3-(2-hydroxy-3-methoxyphenyl)-2-[2-methoxy-4-(3-sulfonatopropyl)phenoxy]propane-1-sulfonate Chemical compound [Ca+2].COC1=CC=CC(CC(CS([O-])(=O)=O)OC=2C(=CC(CCCS([O-])(=O)=O)=CC=2)OC)=C1O RYAGRZNBULDMBW-UHFFFAOYSA-L 0.000 description 1
- 235000013877 carbamide Nutrition 0.000 description 1
- 239000001768 carboxy methyl cellulose Substances 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- CWFOCCVIPCEQCK-UHFFFAOYSA-N chlorfenapyr Chemical compound BrC1=C(C(F)(F)F)N(COCC)C(C=2C=CC(Cl)=CC=2)=C1C#N CWFOCCVIPCEQCK-UHFFFAOYSA-N 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 229910052570 clay Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- RZHBMYQXKIDANM-UHFFFAOYSA-N dioctyl butanedioate;sodium Chemical compound [Na].CCCCCCCCOC(=O)CCC(=O)OCCCCCCCC RZHBMYQXKIDANM-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- ISXSFOPKZQZDAO-UHFFFAOYSA-N formaldehyde;sodium Chemical compound [Na].O=C ISXSFOPKZQZDAO-UHFFFAOYSA-N 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 244000230342 green foxtail Species 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 239000008233 hard water Substances 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 239000001863 hydroxypropyl cellulose Substances 0.000 description 1
- 235000010977 hydroxypropyl cellulose Nutrition 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000010413 mother solution Substances 0.000 description 1
- 229920000847 nonoxynol Polymers 0.000 description 1
- QGLWBTPVKHMVHM-UHFFFAOYSA-N octadec-9-en-1-amine Chemical compound CCCCCCCCC=CCCCCCCCCN QGLWBTPVKHMVHM-UHFFFAOYSA-N 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- WKSAUQYGYAYLPV-UHFFFAOYSA-N pyrimethamine Chemical compound CCC1=NC(N)=NC(N)=C1C1=CC=C(Cl)C=C1 WKSAUQYGYAYLPV-UHFFFAOYSA-N 0.000 description 1
- 229960000611 pyrimethamine Drugs 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- QEVHRUUCFGRFIF-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C(C5=CC=C(OC)C=C5N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 QEVHRUUCFGRFIF-MDEJGZGSSA-N 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000007226 seed germination Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 1
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- RUQIYMSRQQCKIK-UHFFFAOYSA-M sodium;2,3-di(propan-2-yl)naphthalene-1-sulfonate Chemical compound [Na+].C1=CC=C2C(S([O-])(=O)=O)=C(C(C)C)C(C(C)C)=CC2=C1 RUQIYMSRQQCKIK-UHFFFAOYSA-M 0.000 description 1
- HLPHHOLZSKWDAK-UHFFFAOYSA-M sodium;formaldehyde;naphthalene-1-sulfonate Chemical compound [Na+].O=C.C1=CC=C2C(S(=O)(=O)[O-])=CC=CC2=C1 HLPHHOLZSKWDAK-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 239000011345 viscous material Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/50—1,3-Diazoles; Hydrogenated 1,3-diazoles
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01C—PLANTING; SOWING; FERTILISING
- A01C1/00—Apparatus, or methods of use thereof, for testing or treating seed, roots, or the like, prior to sowing or planting
- A01C1/06—Coating or dressing seed
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Environmental Sciences (AREA)
- Dentistry (AREA)
- Plant Pathology (AREA)
- Pest Control & Pesticides (AREA)
- Engineering & Computer Science (AREA)
- Agronomy & Crop Science (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Soil Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
本发明涉及一种吡唑解草酯悬浮种衣剂及其应用。所述吡唑解草酯悬浮种衣剂包括如下重量份的组分:吡唑解草酯5~80份,润湿剂0.1~10份,分散剂0.1~10份,增稠剂0.1~5份,成膜剂1~5份,防冻剂0.1~10份,消泡剂0.1~5份,警示剂0.1~5份,防腐剂0.1~5份,去离子水余量。本发明所述吡唑解草酯悬浮种衣剂符合悬浮种衣剂质量标准,采用本发明提供的吡唑解草酯悬浮种衣剂进行种子处理,配合除草剂喷雾,相对于现有的吡唑解草酯与除草剂混合喷雾技术,可以显著提高作物对除草剂的耐药性,提高除草剂对杂草防治效果,减少除草剂用量。The present invention relates to a suspension seed coating of pyraclostrobin and its application. The fenflu-fen-prop-prop suspension seed coating agent comprises the following components in parts by weight: 5-80 parts of fen-diflufen-ethyl, 0.1-10 parts of wetting agent, 0.1-10 parts of dispersant, and 0.1-5 parts of thickener 1 to 5 parts of film-forming agent, 0.1 to 10 parts of antifreeze, 0.1 to 5 parts of defoamer, 0.1 to 5 parts of warning agent, 0.1 to 5 parts of preservative, and the balance of deionized water. The pyriflufen-ethyl suspension seed coating agent of the present invention complies with the quality standard of the suspension seed coating agent, and the pyrifenapyr suspension seed coating agent provided by the present invention is used for seed treatment, and the herbicide spray is combined. The mixed spraying technology of carzapyr and herbicides can significantly improve the resistance of crops to herbicides, improve the control effect of herbicides on weeds, and reduce the dosage of herbicides.
Description
技术领域technical field
本发明涉及农药技术领域,具体地,涉及一种吡唑解草酯悬浮种衣剂及其应用。The invention relates to the technical field of pesticides, in particular, to a suspension seed coating of pyrfenapyr and its application.
背景技术Background technique
据报道,我国麦田草害发生面积占种植面积的55%以上,严重危害面积占28%,平均产量损失达15%,其中,节节麦等麦田禾本科杂草,近年来发生面积迅速扩大,造成小麦严重减产甚至绝收。同时,随着我国劳动力成本的不断提高,利用除草剂控制麦田杂草危害已经成为小麦生产的必需措施。但是,节节麦等麦田禾本科杂草由于与小麦亲缘关系相近,除草剂难以在小麦和禾本科杂草之间获得较高的选择性,导致可用于防治麦田禾本科杂草的除草剂严重缺乏。目前我国可以较为有效地防治节节麦的除草剂仅有甲基二磺隆,但是甲基二磺隆对小麦药害风险较高,容易产生药害,所以通常在甲基二磺隆制剂中加入安全剂吡唑解草酯,采用二者混合喷雾的方式,以保护小麦,提高小麦对甲基二磺隆的耐药性而对野燕麦等杂草没有影响。According to reports, the occurrence area of weeds in wheat fields in my country accounts for more than 55% of the planting area, the serious damage area accounts for 28%, and the average yield loss is 15%. This has resulted in a serious reduction in wheat production or even no harvest. At the same time, with the continuous increase of labor costs in my country, the use of herbicides to control weeds in wheat fields has become a necessary measure for wheat production. However, due to the close kinship with wheat, it is difficult for herbicides to obtain high selectivity between wheat and grass weeds, resulting in serious herbicides that can be used to control grass weeds in wheat fields. lack. At present, the only herbicide that can effectively prevent and control the wheat in my country is metsulfuron-methyl, but metsulfuron-methyl has a high risk of phytotoxicity to wheat and is prone to phytotoxicity, so it is usually used in metsulfuron-methyl preparations. The safener pyraclosulfate was added, and the two mixed sprays were used to protect wheat and improve the resistance of wheat to metsulfuron without affecting weeds such as wild oats.
然而,申请人通过研究发现,吡唑解草酯作为安全剂与除草剂混合喷雾使用过程中存在以下问题:(1)虽然吡唑解草酯对野燕麦等杂草没有影响,但对节节麦等杂草有保护作用,能够提高其对除草剂的耐药性,使除草剂对节节麦等杂草防效降低,并最终导致除草剂用量大幅增加。(2)化合物可以被植物吸收的部位以及在植物体内的传导方向有很强的特异性,例如乙嘧酚及其类似物茎叶喷雾可以有效防治苹果白粉病,但是从根部施药时则无效。目前吡唑解草酯的使用方式是添加到除草剂制剂中,茎叶喷雾,通过茎叶吸收而发挥作用的,而关于吡唑解草酯用于作物其它施药部位是否有活性及其作用效果尚未见报道。(3)吡唑解草酯原药熔点50~52℃,属于低熔点原药。低熔点原药制成悬浮剂后容易出现分层、固化、悬浮率下降的问题。However, the applicant found through research that the following problems existed in the process of mixing and spraying of fenflufen-ethyl as a safener and herbicide: (1) Although fenflufen-ethyl has no effect on weeds such as wild oats, it has no effect on the Weeds such as wheat have a protective effect, which can improve their resistance to herbicides, reduce the control effect of herbicides on weeds such as Jiejie, and ultimately lead to a substantial increase in the dosage of herbicides. (2) The part where the compound can be absorbed by the plant and the direction of conduction in the plant has a strong specificity. For example, pyrimethamine and its analogs can effectively prevent and control apple powdery mildew by stem and leaf spray, but it is ineffective when applied from the root. . At present, the use of pyrafenpyr is added to herbicide formulations, sprayed on stems and leaves, and absorbed by stems and leaves, and whether pyrazin is active in other application parts of crops and its effect The effect has not yet been reported. (3) The melting point of pyraclostrobin is 50~52℃, which belongs to low melting point. After the low-melting technical drug is made into a suspension agent, the problems of delamination, solidification and suspension rate decrease are prone to occur.
发明内容SUMMARY OF THE INVENTION
为了解决上述技术问题,本发明提供一种吡唑解草酯悬浮种衣剂,其不仅提高了小麦对除草剂的耐药性,同时还能够提高除草剂对节节麦等杂草的防治效果,减少除草剂用量。此外,所述悬浮种衣剂还具有稳定性好的特点。In order to solve the above-mentioned technical problems, the present invention provides a suspension seed coating of pyraclostrofen-ethyl, which not only improves the resistance of wheat to herbicides, but also can improve the control effect of herbicides on weeds such as juniper. , reduce the dosage of herbicides. In addition, the suspended seed coating agent also has the characteristics of good stability.
本发明是采用如下技术方案实现的。The present invention is realized by adopting the following technical solutions.
一种吡唑解草酯悬浮种衣剂,包括如下重量份的组分:A kind of pyraclostrofen suspension seed coating agent, comprising the following components by weight:
吡唑解草酯5~80份,5 to 80 parts of difenapyr,
润湿剂0.1~10份,Wetting agent 0.1 to 10 parts,
分散剂0.1~10份,0.1 to 10 parts of dispersant,
增稠剂0.1~5份,Thickener 0.1 to 5 parts,
成膜剂1~5份,1 to 5 parts of film-forming agent,
防冻剂0.1~10份,Antifreeze 0.1 to 10 parts,
消泡剂0.1~5份,0.1 to 5 parts of defoamer,
警示剂0.1~5份,Warning agent 0.1 to 5 copies,
防腐剂0.1~5份,Preservatives 0.1 to 5 parts,
去离子水余量。Deionized water balance.
优选地,所述吡唑解草酯悬浮种衣剂包括如下重量份的组分:Preferably, the pyraclostrofen suspension seed coating agent comprises the following components in parts by weight:
吡唑解草酯10~50份,10 to 50 parts of difenapyr,
润湿剂1~7份,1 to 7 parts of wetting agent,
分散剂1~7份,1 to 7 parts of dispersant,
增稠剂0.1~3份,Thickener 0.1 to 3 parts,
成膜剂1~3份,1 to 3 parts of film-forming agent,
防冻剂1~5份,1 to 5 parts of antifreeze,
消泡剂0.5~3份,0.5 to 3 parts of defoamer,
警示剂0.1~2份,Warning agent 0.1 to 2 copies,
防腐剂0.5~3份,Preservatives 0.5 to 3 parts,
去离子水余量。Deionized water balance.
更优选地,所述吡唑解草酯悬浮种衣剂由如下重量计的组分组成:吡唑解草酯30%、润湿剂4%、分散剂5%、增稠剂1.1%、成膜剂2%、防冻剂2%、消泡剂1.5%、警示剂0.5%、防腐剂1%、去离子水补足余量。More preferably, the fenflu-fen-prop-prop suspension seed coating is composed of the following components by weight: fenflufen-ethyl 30%, wetting agent 4%, dispersing agent 5%, thickening agent 1.1%, Film agent 2%, antifreeze agent 2%, defoamer 1.5%, warning agent 0.5%, preservative 1%, deionized water to make up the balance.
所述吡唑解草酯悬浮种衣剂中,所述的润湿剂可以是苯乙烯基酚聚氧乙烯聚氧丙烯醚、烷基酚甲醛树脂聚氧乙烯醚、苄基二甲基酚聚氧乙烯醚、壬基酚聚氧乙烯醚、辛基酚聚氧乙烯醚、9-十八烯胺、蓖麻油聚氧乙烯醚、拉开粉(二异丁基萘磺酸钠)、十二烷基苯磺酸钠、月桂醇硫酸钠、二辛基丁二酸酯磺酸钠、二异丙基萘磺酸钠、十三醇聚氧乙烯醚中的一种或多种;优选地,所述的润湿剂可以是烷基酚甲醛树脂聚氧乙烯醚、壬基酚聚氧乙烯醚、蓖麻油聚氧乙烯醚中的一种或多种;更优选地,所述润湿剂是烷基酚甲醛树脂聚氧乙烯醚。In the pyrazolyl-methyl suspension seed coating agent, the wetting agent can be styryl phenol polyoxyethylene polyoxypropylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, benzyl dimethylphenol polyoxyethylene Oxyethylene ether, nonylphenol polyoxyethylene ether, octylphenol polyoxyethylene ether, 9-octadecenamine, castor oil polyoxyethylene ether, pulling powder (sodium diisobutylnaphthalene sulfonate), dodecyl One or more of sodium alkyl benzene sulfonate, sodium lauryl sulfate, sodium dioctyl succinate sulfonate, sodium diisopropyl naphthalene sulfonate, tridecyl polyoxyethylene ether; preferably, The wetting agent can be one or more of alkylphenol formaldehyde resin polyoxyethylene ether, nonylphenol polyoxyethylene ether, castor oil polyoxyethylene ether; more preferably, the wetting agent is Alkylphenol formaldehyde resin polyoxyethylene ether.
所述分散剂可以是木质素磺酸钠、木质素磺酸钙、木质素磺酸铵、NNO(萘磺酸钠甲醛缩合物)、NO(二丁基萘磺酸钠甲醛缩合物)、扩散剂MF(甲基萘磺酸钠甲醛缩合物)、拉开粉(二异丁基萘磺酸钠)、脂肪醇环氧乙烷加成物磷酸盐、烷基酚聚氧乙烯基醚磷酸盐、SOPA(烷基酚聚氧乙烯基醚甲醛缩合物硫酸盐)、聚氧乙烯聚氧丙烯醚嵌段共聚物、烷基酚聚氧乙烯基磷酸酯、阿拉伯胶、卵磷脂、羧甲基纤维素、聚乙烯醇、聚乙烯吡咯烷酮、聚乙二醇中的一种或多种;优选地,所述分散剂可以是:木质素磺酸钠、NNO、聚氧乙烯聚氧丙烯醚嵌段共聚物、烷基酚聚氧乙烯基磷酸酯、聚乙烯吡咯烷酮中的一种或多种;更优选地,所述分散剂是NNO和/或聚氧乙烯聚氧丙烯醚嵌段共聚物。The dispersing agent can be sodium lignosulfonate, calcium lignosulfonate, ammonium lignosulfonate, NNO (sodium naphthalene sulfonate formaldehyde condensate), NO (dibutylnaphthalene sulfonate sodium formaldehyde condensate), diffusion Agent MF (sodium methylnaphthalene sulfonate formaldehyde condensate), pull powder (sodium diisobutylnaphthalene sulfonate), fatty alcohol ethylene oxide adduct phosphate, alkylphenol polyoxyethylene ether phosphate , SOPA (alkylphenol polyoxyethylene ether formaldehyde condensate sulfate), polyoxyethylene polyoxypropylene ether block copolymer, alkylphenol polyoxyethylene phosphate, gum arabic, lecithin, carboxymethyl fiber One or more of polyvinyl alcohol, polyvinyl pyrrolidone, polyethylene glycol; preferably, the dispersing agent can be: sodium lignosulfonate, NNO, polyoxyethylene polyoxypropylene ether block copolymer One or more of polyoxyethylene phosphate, alkylphenol polyoxyethylene phosphate, and polyvinylpyrrolidone; more preferably, the dispersant is NNO and/or polyoxyethylene polyoxypropylene ether block copolymer.
所述增稠剂可以是石膏、黏土、硅酸铝镁、水玻璃、羧甲基淀粉钠、可溶性淀粉、羧甲基纤维素钠、海藻酸钠、琼脂、黄原胶、羟乙基纤维素、膨润土中的一种或多种;优选地,所述增稠剂可以是硅酸铝镁、黄原胶、海藻酸钠、羟乙基纤维素中的一种或多种;更优选地,所述增稠剂是硅酸铝镁和/或黄原胶。The thickener can be gypsum, clay, magnesium aluminum silicate, water glass, sodium carboxymethyl starch, soluble starch, sodium carboxymethyl cellulose, sodium alginate, agar, xanthan gum, hydroxyethyl cellulose , one or more of bentonite; preferably, the thickener can be one or more of aluminum magnesium silicate, xanthan gum, sodium alginate, hydroxyethyl cellulose; more preferably, The thickener is magnesium aluminum silicate and/or xanthan gum.
所述成膜剂可以是海藻酸钠、琼脂、聚乙烯醇、聚乙二醇、聚醋酸乙烯酯、聚丙烯酰胺、聚乙烯醋酸酯、聚乙烯吡咯烷酮、聚(甲基)丙烯酸衍生物、多元醇聚合物、乙基纤维素、轻丙基纤维素、聚醋酸内酯、聚丙烯酰胺中的一种或多种;优选地,所述成膜剂可以是聚乙烯醇、聚乙二醇、聚丙烯酰胺中的一种或多种;更优选地,所述成膜剂是聚乙二醇。The film-forming agent can be sodium alginate, agar, polyvinyl alcohol, polyethylene glycol, polyvinyl acetate, polyacrylamide, polyvinyl acetate, polyvinylpyrrolidone, poly(meth)acrylic acid derivatives, polyvinyl One or more of alcohol polymer, ethyl cellulose, hydroxypropyl cellulose, polyacetolactone, polyacrylamide; preferably, the film-forming agent can be polyvinyl alcohol, polyethylene glycol, one or more of polyacrylamides; more preferably, the film former is polyethylene glycol.
所述防冻剂可以是乙二醇、丙二醇、丙三醇、尿素、甘油、甘油-乙醚双甘醇、甲基丙撑双甘醇中的一种或多种;优选地,所述防冻剂可以是乙二醇、丙三醇、尿素中的一种或多种;更优选地,所述防冻剂是尿素。The antifreeze can be one or more of ethylene glycol, propylene glycol, glycerol, urea, glycerin, glycerol-diethyl ether diethylene glycol, and methyl propylene diethylene glycol; preferably, the antifreeze can be is one or more of ethylene glycol, glycerol, and urea; more preferably, the antifreeze is urea.
所述消泡剂可以是异辛醇、异戊醇、硬脂酸、月桂酸中的一种或多种;优选地,所述消泡剂是异辛醇。The defoamer can be one or more of isooctyl alcohol, isoamyl alcohol, stearic acid, and lauric acid; preferably, the defoamer is isooctanol.
所述警示剂可以是酸性大红、碱性玫瑰精、若达明2B中的一种或多种;优选地,所述警示剂是碱性玫瑰精。The warning agent can be one or more of Scarlet Scarlet, Rhodamine, Rhodamine 2B; preferably, the warning agent is Rhodamine.
所述防腐剂可以是甲醛、水杨酸钠、苯甲酸钠、1,2-苯并噻唑啉-3-酮、2-羟基联苯、山梨酸、苯甲酸、苯甲醛、对羟基苯甲醛、对羟基苯甲酯、异噻唑啉酮(卡松)中的一种或多种;优选地,所述防腐剂是异噻唑啉酮。The preservative can be formaldehyde, sodium salicylate, sodium benzoate, 1,2-benzothiazolin-3-one, 2-hydroxybiphenyl, sorbic acid, benzoic acid, benzaldehyde, p-hydroxybenzaldehyde, p-hydroxybenzaldehyde One or more of methyl hydroxybenzoate and isothiazolinone (casone); preferably, the preservative is isothiazolinone.
本发明所用的各种原料和试剂均为市售,可以容易地获得。例如吡唑解草酯原药可以购自江苏天容集团股份有限公司,烷基酚甲醛树脂聚氧乙烯醚(农乳700号)购自河北燕诚化学助剂有限公司,NNO购自广州市创琞化工科技有限公司,聚氧乙烯聚氧丙烯醚嵌段共聚物(聚醚F-68)购自桑达化工(南通)有限公司等。Various raw materials and reagents used in the present invention are commercially available and can be easily obtained. For example, the original drug of pyraclostrobin can be purchased from Jiangsu Tianrong Group Co., Ltd., alkylphenol formaldehyde resin polyoxyethylene ether (Nongru No. 700) can be purchased from Hebei Yancheng Chemical Auxiliary Co., Ltd., and NNO can be purchased from Guangzhou City Chuangyu Chemical Technology Co., Ltd., polyoxyethylene polyoxypropylene ether block copolymer (polyether F-68) was purchased from Sunda Chemical (Nantong) Co., Ltd., etc.
本发明所述的吡唑解草酯悬浮种衣剂可采用本领域常规悬浮种衣剂制备方法制得。The pyraclostrofen suspension seed coating agent of the present invention can be prepared by adopting the conventional preparation method of the suspension seed coating agent in the art.
在本发明中,所述吡唑解草酯悬浮种衣剂的制备方法,包括:In the present invention, the preparation method of the pyrfenapyr suspending seed coating comprises:
将各种组分过筛(如320目),与去离子水按比例混合,高速搅拌预分散30min,控制体系在45℃以下,除杂,即得。优选采用砂磨机砂磨,砂磨介质为锆珠,介质系数为1,砂磨2.5h,砂磨温度控制在45℃以下。The various components are sieved (such as 320 mesh), mixed with deionized water in proportion, pre-dispersed with high-speed stirring for 30 minutes, and the system is controlled below 45°C, and impurities are removed. It is preferable to use a sand mill for sanding, the sanding medium is zirconium beads, the medium coefficient is 1, the sanding is 2.5 hours, and the sanding temperature is controlled below 45 °C.
本发明还提供所述吡唑解草酯悬浮种衣剂在防治麦田杂草中的应用。具体为:利用所述吡唑解草酯悬浮种衣剂对小麦种子进行包衣处理。The present invention also provides application of the pyraclostrofen suspension seed coating agent in preventing and controlling weeds in wheat fields. Specifically, the wheat seeds are coated by using the pyraclostrofen suspension seed coating agent.
本发明所述的麦田杂草以禾本科杂草、阔叶杂草、莎草科杂草为主。优选地,所述的麦田杂草选自节节麦、雀麦、无芒雀麦、看麦娘、日本看麦娘、早熟禾、菵草、硬草、棒头草、多花黑麦草、毒麦、蜡烛草、山羊草、圆柱山羊草、播娘蒿、荠菜、麦家公、麦瓶草、藜、打碗花、莎草等中的一种或几种。更优选地,所述的麦田杂草为节节麦和/或播娘蒿。The wheat field weeds described in the present invention are mainly grass weeds, broadleaf weeds and sedge weeds. Preferably, the weeds in the wheat field are selected from the group consisting of sclerotium, brome, brome, ryegrass, japonica, bluegrass, serratia, hard grass, club grass, multiflora ryegrass, One or more of barley, candle grass, goat grass, cylindrical goat grass, sagebrush, shepherd's purse, maijiagong, wheat bottle grass, quinoa, bowl flower, sedge, etc. More preferably, the weeds in the wheat field are S. japonica and/or Artemisia annua.
在具体应用时,所述吡唑解草酯悬浮种衣剂的有效成分用量为1-2000g/100kg种子。优选地,所述吡唑解草酯悬浮种衣剂的用量为10-1000g/100kg种子。更优选地,所述吡唑解草酯悬浮种衣剂的用量为20-500g/100kg种子。In a specific application, the active ingredient dosage of the pyriflufen-ethyl suspended seed coating agent is 1-2000g/100kg of seeds. Preferably, the dosage of the pyrfenapyr suspending seed coating agent is 10-1000g/100kg of seeds. More preferably, the dosage of the pyriflufen-ethyl suspension seed coating agent is 20-500g/100kg of seeds.
在具体应用时,所述吡唑解草酯悬浮种衣剂的用量为1.875-3750g/hm2;优选地,所述吡唑解草酯悬浮种衣剂的用量为18.75-1875g/hm2;进一步优选地,所述吡唑解草酯悬浮种衣剂的用量为37.5–937.5g/hm2;更优选地,所述吡唑解草酯悬浮种衣剂的用量45-375g/hm2。In the specific application, the consumption of the fenflu-fen-prop-prop suspension seed coating agent is 1.875-3750g/hm 2 ; preferably, the consumption of the fenflufen-ethyl suspended seed coating agent is 18.75-1875g/hm 2 ; Further preferably, the dosage of the fenflu-fen-prop-prop suspension seed coating agent is 37.5-937.5 g/hm 2 ; more preferably, the dosage of the fenflu-fen-ethyl suspended seed coating agent is 45-375 g/hm 2 .
在具体应用时,所述吡唑解草酯悬浮种衣剂与甲基二磺隆配合使用,如先用所述吡唑解草酯悬浮种衣剂对种子包衣处理,再喷施甲基二磺隆,可取得更好的效果;优选地,所述吡唑解草酯悬浮种衣剂的用量为1.875-3750g/hm2;进一步优选地,所述吡唑解草酯悬浮种衣剂的用量为18.75-1875g/hm2;更进一步优选地,所述吡唑解草酯悬浮种衣剂的用量为37.5–937.5g/hm2;更优选地,所述吡唑解草酯悬浮种衣剂的用量45-375g/hm2;所述甲基二磺隆的用量以8-20g/hm2为宜。In the specific application, the pyriflufen-ethyl suspension seed coating agent is used in combination with methyldisulfuron, for example, the seeds are coated with the pyriflufen-ethyl suspension seed coating agent, and then the methyl disulfonic acid is sprayed. It can achieve better effect; preferably, the consumption of the fenflu-fen-ethyl suspension seed coating agent is 1.875-3750g/hm 2 ; further preferably, the consumption of the fenflufen-ethyl suspended seed coating agent It is 18.75-1875g/hm 2 ; more preferably, the dosage of the fenflu-fen-ethyl suspension seed coating agent is 37.5-937.5g/hm 2 ; more preferably, the fenflufen-ethyl suspended seed coating agent The dosage is 45-375 g/hm 2 ; the dosage of the methyldisulfuron is preferably 8-20 g/hm 2 .
本发明具有以下积极有益效果:The present invention has the following positive beneficial effects:
1、本发明所述吡唑解草酯悬浮种衣剂配合除草剂用于防治麦田杂草,通过对小麦种子的包衣处理,避免吡唑解草酯对节节麦等杂草的保护,可显著提高除草剂对节节麦等杂草的防治效果,减少除草剂的用量。1. The pyrazin suspension seed coating agent of the present invention is used in conjunction with herbicides to prevent and treat weeds in wheat fields, and by the coating treatment of wheat seeds, the protection of pyrazin-fen-ethyl to weeds such as Jiejie is avoided, It can significantly improve the control effect of herbicides on weeds such as Jiejie, and reduce the dosage of herbicides.
2、本发明通过大量的筛选和研究,制备出了质量合格的吡唑解草酯悬浮种衣剂,解决了吡唑解草酯悬浮剂剂型容易出现分层、固化、悬浮率下降的问题;2. The present invention has prepared a quality-qualified fenflu-fen-ethyl suspension seed coating through a large number of screenings and researches, and solved the problems that the fen-flufen-ethyl suspension agent is prone to delamination, solidification, and a drop in the suspension rate;
3、本发明所述吡唑解草酯悬浮种衣剂配合除草剂防治麦田杂草,可显著提高小麦对除草剂的耐药性,减轻除草剂药害;3. The suspension seed coating of pyraclostrobin of the present invention is combined with herbicides to control weeds in wheat fields, which can significantly improve the resistance of wheat to herbicides and reduce the phytotoxicity of herbicides;
具体实施方式Detailed ways
以下实施例用于说明本发明,但不用来限制本发明的范围。The following examples are intended to illustrate the present invention, but not to limit the scope of the present invention.
实施例中未注明具体技术或条件者,按照本领域内的文献所描述的技术或条件,或者按照产品说明书进行。If no specific technique or condition is indicated in the examples, the technique or condition described in the literature in the field or the product specification is used.
所用试剂或仪器未注明生产厂商者,均为可通过正规渠道商购买得到的常规产品。The reagents or instruments used without the manufacturer's indication are conventional products that can be purchased through regular channels.
如无特别说明,本发明所有实施例及实验例中的百分含量均指重量百分含量。Unless otherwise specified, the percentages in all the examples and experimental examples of the present invention refer to weight percentages.
实施例1 30%吡唑解草酯悬浮种衣剂Example 1 30% mezafen-prop-prop-prop suspension seed coating
以质量百分数计,配方如下:In terms of mass percentage, the formula is as follows:
吡唑解草酯30%、烷基酚甲醛树脂聚氧乙烯醚4%、NNO 2%、聚氧乙烯聚氧丙烯醚嵌段共聚物3%、硅酸铝镁1%、黄原胶0.1%、聚乙二醇2%、尿素2%、异辛醇1.5%、玫瑰精0.5%、异噻唑啉酮1%、去离子水补足余量。Meafenpyr 30%, Alkylphenol Formaldehyde Resin Polyoxyethylene Ether 4%, NNO 2%, Polyoxyethylene Polyoxypropylene Ether Block Copolymer 3%, Aluminum Magnesium Silicate 1%, Xanthan Gum 0.1% , polyethylene glycol 2%, urea 2%, isooctanol 1.5%, rose essence 0.5%, isothiazolinone 1%, deionized water to make up the balance.
实施例2 10%吡唑解草酯悬浮种衣剂Example 2 10% Mezafenapyr Suspension Seed Coating Agent
以质量百分数计,配方如下:In terms of mass percentage, the formula is as follows:
吡唑解草酯10%、壬基酚聚氧乙烯醚2%、NNO 1%、烷基酚聚氧乙烯基磷酸酯1%、硅酸铝镁0.5%、羟乙基纤维素0.1%、聚乙烯醇3%、乙二醇5%、异戊醇1%、酸性大红1%、山梨酸1.5%、去离子水补足余量。Meafenpyr 10%, Nonylphenol Ethoxylate 2%, NNO 1%, Alkylphenol Polyoxyethylene Phosphate 1%, Aluminum Magnesium Silicate 0.5%, Hydroxyethyl Cellulose 0.1%, Polyurethane Vinyl alcohol 3%, ethylene glycol 5%, isoamyl alcohol 1%, acid scarlet 1%, sorbic acid 1.5%, deionized water make up the balance.
实施例3 40%吡唑解草酯悬浮种衣剂Example 3 40% pyraclostrofen suspension seed coating
以质量百分数计,配方如下:In terms of mass percentage, the formula is as follows:
吡唑解草酯40%、蓖麻油聚氧乙烯醚8%、木质素磺酸钠4%、烷基酚聚氧乙烯基磷酸酯5%、海藻酸钠2%、聚丙烯酰胺3%、丙三醇3%、月桂酸2%、若明达2B 2%、苯甲酸2%、去离子水补足余量。Meafenpyr ethyl 40%, castor oil polyoxyethylene ether 8%, sodium lignosulfonate 4%, alkylphenol polyoxyethylene phosphate 5%, sodium alginate 2%, polyacrylamide 3%, propylene Triol 3%, lauric acid 2%, Ruominda 2B 2%, benzoic acid 2%, deionized water make up the balance.
效果试验1:Effect test 1:
本发明还提供了一系列助剂对比试验,用于验证本发明实施例1所述吡唑解草酯悬浮种衣剂中各助剂具体选择的显著效果。The present invention also provides a series of adjuvant comparative tests, which are used to verify the remarkable effect of the specific selection of each adjuvant in the pyrazin-carbofen suspension seed coating agent described in Example 1 of the present invention.
1、润湿剂、分散剂对比试验1. Comparative test of wetting agent and dispersing agent
(1)润湿剂、分散剂初筛(1) Primary screening of wetting agents and dispersing agents
采用流点法进行润湿剂、分散剂初筛。先用水溶解润湿剂或分散剂,将其定容制成质量分数为5%的水溶液,再准确称取2.0000g已预粉碎的吡唑解草酯原药于20mL试管中,称量试管质量;逐滴滴加5%的润湿剂或分散剂水溶液,加几滴便用超声波进行混合,当粘稠物刚刚可以沿试管壁下滑时,再称其质量,其前后质量差(m)即为所滴加的润湿剂或分散剂溶液的质量,该润湿、分散剂对吡唑解草酯的流点即可用m除以原药的质量表示,流点越小表明润湿、分散效果越好。同一润湿、分散剂分别进行测试3次,取平均值。The wetting agent and dispersing agent were initially screened by the flow point method. First dissolve the wetting agent or dispersing agent with water, make it into an aqueous solution with a mass fraction of 5%, and then accurately weigh 2.0000g of the pre-crushed pyraclostrobin in a 20mL test tube, and weigh the mass of the test tube. ; Add 5% aqueous solution of wetting agent or dispersing agent drop by drop, add a few drops and mix with ultrasonic waves, when the viscous substance can just slide down the test tube wall, weigh it again, the quality difference before and after (m) That is, the quality of the dripping wetting agent or dispersing agent solution, the flow point of the wetting and dispersing agent to pyriflufen-ethyl can be expressed by m divided by the quality of the original drug, the smaller the flow point is, the wetting, The better the dispersion effect. The same wetting and dispersing agent were tested 3 times respectively, and the average value was taken.
表1吡唑解草酯悬浮种衣剂润湿剂、分散剂初筛结果(流点法)Table 1 The results of preliminary screening of the wetting agent and dispersing agent of pyraclostrobin suspended seed coating agent (flow point method)
润湿剂、分散剂初筛结果见表1。选择流点较小(小于1.00)的润湿剂蓖麻油聚氧乙烯醚、壬基酚聚氧乙烯醚、烷基酚甲醛树脂聚氧乙烯醚和分散剂NNO、聚氧乙烯聚氧丙烯醚嵌段共聚物、聚乙烯吡咯烷酮、木质素磺酸钠、烷基酚聚氧乙烯基磷酸酯进行进一步试验。The results of the initial screening of wetting agents and dispersing agents are shown in Table 1. Select the wetting agent castor oil polyoxyethylene ether, nonylphenol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether and dispersant NNO, polyoxyethylene polyoxypropylene ether embedded with smaller flow point (less than 1.00). Block copolymer, polyvinylpyrrolidone, sodium lignosulfonate, alkylphenol polyoxyethylene phosphate were further tested.
(2)润湿剂、分散剂种类筛选(2) Screening of wetting agents and dispersing agents
采用尝试法对初筛出的润湿剂、分散剂进行进一步筛选,确定具体种类。将初筛出的润湿剂和分散剂以不同方式组合后与30g吡唑解草酯(折百)混合,加水至100g,以锆珠为介质,介质系数为1,砂磨2.5h,砂磨温度控制在45℃以下,制得30%吡唑解草酯悬浮液。分别以悬浮率、粘度及分散性为指标确定润湿剂及分散剂的种类。The wetting and dispersing agents initially screened were further screened by trial method to determine the specific types. The wetting agent and dispersing agent that were initially screened were combined in different ways, mixed with 30 g of pyrafenacet (Zhebai), water was added to 100 g, zirconium beads were used as the medium, the medium coefficient was 1, and the sand was milled for 2.5 hours. The grinding temperature is controlled below 45° C. to obtain a 30% pyriflufen-ethyl suspension. The types of wetting agents and dispersing agents were determined with the suspension rate, viscosity and dispersibility as indicators respectively.
分散性测定采用目测分级法:于100mL量筒中,装入99.5mL标准硬水,用移液枪取0.5mL待测悬浮液样品,从距离量筒水面5cm处滴入水中,观察其分散状况。按其分散的好坏分为8级。The dispersibility was measured by the visual classification method: put 99.5mL of standard hard water in a 100mL graduated cylinder, use a pipette to take a 0.5mL sample of the suspension to be tested, drop it into the water from a distance of 5cm from the water surface of the graduated cylinder, and observe its dispersion status. It is divided into 8 grades according to the quality of its dispersion.
1级:在水中不能自动分散,呈团块状快速下沉至底部,无浑浊液出现;Level 1: It cannot automatically disperse in water, and it quickly sinks to the bottom in the form of a lump, and no turbid liquid appears;
2级:在水中不能自动分散,呈团块状下沉,下沉速度稍减慢,有浑浊液出现,最终全部样品沉底;Level 2: It cannot automatically disperse in water, sinks in a clump shape, the sinking speed slows down slightly, a turbid liquid appears, and finally all the samples sink to the bottom;
3级:在水中不能自动分散,有明显浑浊液出现,部分样品呈团状下沉到底部;Level 3: It cannot be automatically dispersed in water, there is obvious turbid liquid, and some samples sink to the bottom in a lump;
4级:在水中能自动分散,呈团、颗粒团缓慢下降,量筒有1/3的浑浊液出现,部分样品沉到底部;Level 4: It can automatically disperse in water, form agglomerates, and the particles slowly descend, 1/3 of the turbid liquid appears in the graduated cylinder, and some samples sink to the bottom;
5级:在水中自动分散,呈云雾团缓慢下降,量筒有1/2的浑浊液出现,部分样品沉到底部;Level 5: Automatically disperse in water, slowly descending as a cloudy mass, 1/2 of the turbid liquid appears in the graduated cylinder, and some samples sink to the bottom;
6级:在水中自动分散,呈云雾团缓慢下降,量筒有3/4的浑浊液出现,少部分样品沉到底部;Level 6: Automatically disperse in water, slowly descending as a cloudy mass, 3/4 of the turbid liquid appears in the graduated cylinder, and a small part of the sample sinks to the bottom;
7级:在水中呈云雾状自动分散,无明显颗粒团缓慢下降,浑浊液迅速扩散;Level 7: Automatically disperse in the form of a cloud and mist in the water, no obvious particle clusters fall slowly, and the turbid liquid diffuses rapidly;
8级:在水中呈云雾状自动分散,浑浊液迅速形成。Grade 8: It will automatically disperse in the form of a cloud and mist in the water, and the turbid liquid will form rapidly.
表2吡唑解草酯悬浮种衣剂润湿剂、分散剂种类筛选结果(尝试法)Table 2 Screening results of the types of wetting agent and dispersing agent of pyraclostrofen suspension seed coating agent (trial method)
润湿剂、分散剂种类筛选结果表明:润湿剂为壬基酚聚氧乙烯醚、烷基酚甲醛树脂聚氧乙烯醚、蓖麻油聚氧乙烯醚,分散剂为NNO、聚氧乙烯聚氧丙烯醚嵌段共聚物、烷基酚聚氧乙烯基磷酸酯时,悬浮率高(90.4~92.8%),分散性好(7~8级),粘度适中(303~377mPs·s),所得悬浮液质量较好。其中,润湿剂为烷基酚甲醛树脂聚氧乙烯醚,分散剂为NNO和聚氧乙烯聚氧丙烯醚嵌段共聚物时所得悬浮液质量最好,分散性8级,粘度适中(332mPs·s),悬浮率92.4%,是本发明优选地,因此,以烷基酚甲醛树脂聚氧乙烯醚为润湿剂,NNO和聚氧乙烯聚氧丙烯醚嵌段共聚物为分散剂进行下一步试验。The screening results of wetting agents and dispersing agents show that the wetting agents are nonylphenol polyoxyethylene ether, alkylphenol formaldehyde resin polyoxyethylene ether, castor oil polyoxyethylene ether, and the dispersing agents are NNO, polyoxyethylene polyoxyethylene In the case of propylene ether block copolymer and alkylphenol polyoxyethylene phosphate ester, the suspension rate is high (90.4-92.8%), the dispersibility is good (7-8 grades), and the viscosity is moderate (303-377mPs s), and the obtained suspension Liquid quality is good. Among them, when the wetting agent is alkylphenol formaldehyde resin polyoxyethylene ether, and the dispersing agent is NNO and polyoxyethylene polyoxypropylene ether block copolymer, the obtained suspension has the best quality, the dispersibility is 8 grades, and the viscosity is moderate (332mPs· s), the suspension rate is 92.4%, which is the preferred choice of the present invention. Therefore, the next step is carried out with the alkylphenol formaldehyde resin polyoxyethylene ether as the wetting agent and NNO and the polyoxyethylene polyoxypropylene ether block copolymer as the dispersing agent. test.
(3)分散剂配比筛选(3) Screening of dispersant ratio
采用尝试法对筛选出的分散剂进行进一步筛选,确定使用比例。将NNO和聚氧乙烯聚氧丙烯醚嵌段共聚物按照不同比例混合,与4g润湿剂烷基酚甲醛树脂聚氧乙烯醚、30g吡唑解草酯(折百)混合,加水至100g,以锆珠为介质,介质系数为1,砂磨2.5h,砂磨温度控制在45℃以下,制得30%吡唑解草酯悬浮液。分别以悬浮率、粘度及分散性为指标确定分散剂的最佳配比。The screened dispersants were further screened by trial method to determine the usage ratio. Mix NNO and polyoxyethylene polyoxypropylene ether block copolymer according to different proportions, mix with 4g wetting agent alkylphenol formaldehyde resin polyoxyethylene ether, 30g pyraclostrobin (100%), add water to 100g, Using zirconium beads as the medium, the medium coefficient is 1, sanding for 2.5 hours, and the sanding temperature is controlled below 45°C, to prepare a 30% pyraclostrobin suspension. The optimum ratio of dispersant was determined by taking the suspension rate, viscosity and dispersibility as indicators.
表3吡唑解草酯悬浮种衣剂分散剂配比筛选结果(尝试法)Table 3 Screening results (trial method) of dispersant ratio of pyraclostrofen suspension seed coating agent
分散剂配比筛选结果表明:NNO和聚氧乙烯聚氧丙烯醚嵌段共聚物配比为1:2、1:3、2:3、2:4、2:5、2:6时,悬浮率高(90.3%~93.4%),分散性好(7~8级),粘度适中(251~362mPs·s),所得悬浮液质量较好。其中,NNO和聚氧乙烯聚氧丙烯醚嵌段共聚物配比为2:3时所得悬浮液质量最好,分散性8级,粘度适中(340mPs·s),悬浮率93.4%,是本发明优选的方案,因此,以NNO:聚氧乙烯聚氧丙烯醚嵌段共聚物=2:3为分散剂进行下一步试验。The screening results of dispersant ratio show that: when the ratio of NNO and polyoxyethylene polyoxypropylene ether block copolymer is 1:2, 1:3, 2:3, 2:4, 2:5, 2:6, the suspension High rate (90.3%-93.4%), good dispersibility (7-8 grades), moderate viscosity (251-362 mPs·s), and the obtained suspension is of good quality. Among them, when the ratio of NNO and polyoxyethylene polyoxypropylene ether block copolymer is 2:3, the quality of the suspension obtained is the best, the dispersibility is 8 grades, the viscosity is moderate (340mPs·s), and the suspension rate is 93.4%, which is the invention of the present invention. The preferred solution, therefore, takes NNO: polyoxyethylene polyoxypropylene ether block copolymer=2:3 as the dispersant to carry out the next test.
2、增稠剂对比试验2. Thickener comparison test
采用经验法进行增稠剂筛选。将不同增稠剂与润湿剂烷基酚甲醛树脂聚氧乙烯醚4g、分散剂NNO 2g、聚氧乙烯聚氧丙烯醚嵌段共聚物3g、吡唑解草酯30g(折百)混合,加水至100g,以锆珠为介质,介质系数为1,砂磨2.5h,砂磨温度控制在45℃以下,制得30%吡唑解草酯悬浮液。分别以粘度、悬浮率及热贮稳定性为指标确定增稠剂种类。Thickener screening was carried out empirically. Mix different thickeners with wetting agent alkylphenol formaldehyde resin polyoxyethylene ether 4g, dispersant NNO 2g, polyoxyethylene polyoxypropylene ether block copolymer 3g, and pyrafenacet 30g (100%), Add water to 100 g, use zirconium beads as the medium, the medium coefficient is 1, sand mill for 2.5 hours, and control the sand milling temperature below 45° C. to obtain a 30% pyrazin-carbofen suspension. The types of thickeners were determined with viscosity, suspension rate and thermal storage stability as indicators.
表4吡唑解草酯悬浮种衣剂增稠剂筛选结果Table 4 Screening results of pyraclostrofen suspension seed coating thickener thickener
增稠剂筛选结果表明:增稠剂为硅酸铝镁、海藻酸钠、黄原胶、羟乙基纤维素时,悬浮率高(89.5%~97.8%),粘度适中(242~506mPs·s),热贮稳定性较好,所得悬浮液质量较好(表4)。其中,硅酸铝镁和黄原胶配比为1:0.1时所得悬浮液质量最好,悬浮率97.3%,粘度适中(325mPs·s),热贮稳定,是本发明优选的方案,因此,以硅酸铝镁和黄原胶(质量比1:0.1)为增稠剂进行下一步试验。The screening results of thickeners show that when the thickeners are aluminum magnesium silicate, sodium alginate, xanthan gum and hydroxyethyl cellulose, the suspension rate is high (89.5%-97.8%) and the viscosity is moderate (242-506mPs·s). ), the heat storage stability is better, and the quality of the obtained suspension is better (Table 4). Among them, when the ratio of magnesium aluminum silicate and xanthan gum is 1:0.1, the quality of the obtained suspension is the best, the suspension rate is 97.3%, the viscosity is moderate (325mPs s), and the thermal storage is stable, which is the preferred solution of the present invention. Therefore, The next experiment was carried out with magnesium aluminum silicate and xanthan gum (mass ratio 1:0.1) as thickeners.
3、润湿剂、分散剂、增稠剂用量的对比试验3. Comparative test of the dosage of wetting agent, dispersing agent and thickening agent
通过正交试验明确润湿剂、分散剂、增稠剂之间的相互作用,确定最终用量。将润湿剂(烷基酚甲醛树脂聚氧乙烯醚)、分散剂(NNO:聚氧乙烯聚氧丙烯醚嵌段共聚物=2:3)、增稠剂(硅酸铝镁:黄原胶=1:0.1)以不同用量分别与吡唑解草酯30g(折百)混合,加水至100g,以锆珠为介质,介质系数为1,砂磨2.5h,砂磨温度控制在45℃以下,制得30%吡唑解草酯悬浮液。以悬浮率为指标确定润湿剂、分散剂、增稠剂用量。The interaction between the wetting agent, dispersing agent and thickening agent was clarified by orthogonal test, and the final dosage was determined. Wetting agent (alkylphenol formaldehyde resin polyoxyethylene ether), dispersing agent (NNO: polyoxyethylene polyoxypropylene ether block copolymer = 2:3), thickener (aluminum magnesium silicate: xanthan gum) =1:0.1) Mix with 30g (100%) of pyraclostrobin in different dosages, add water to 100g, use zirconium beads as the medium, the medium coefficient is 1, sand for 2.5h, and the sanding temperature is controlled below 45 ℃ , to obtain a 30% suspension of diflufenapyr. Determine the dosage of wetting agent, dispersing agent and thickening agent according to the index of suspension rate.
表5吡唑解草酯悬浮种衣剂润湿剂、分散剂、增稠剂用量筛选结果Table 5 Screening results of the dosage of pyraclostrofen suspension seed coating agent wetting agent, dispersing agent and thickening agent
注:润湿剂为烷基酚甲醛树脂聚氧乙烯醚,分散剂为NNO:聚氧乙烯聚氧丙烯醚嵌段共聚物=2:3,增稠剂为硅酸铝镁:黄原胶=1:0.1。Note: Wetting agent is alkylphenol formaldehyde resin polyoxyethylene ether, dispersant is NNO: polyoxyethylene polyoxypropylene ether block copolymer = 2:3, thickener is aluminum magnesium silicate: xanthan gum = 1:0.1.
润湿剂、分散剂、增稠剂用量筛选结果表明:润湿剂、分散剂、增稠剂用量为4%+5%+1.1%、5%+5%+0.1%、3%+5%+0.5%、5%+4%+1.1%、3%+4%+0.1%、4%+4%+0.5%、5%+6%+0.5%时,悬浮率较高(90.0%~98.3%),所得悬浮液质量较好(表5)。其中,润湿剂(烷基酚甲醛树脂聚氧乙烯醚)4%、分散剂(NNO:聚氧乙烯聚氧丙烯醚嵌段共聚物=2:3)5%、增稠剂(硅酸铝镁:黄原胶=1:0.1)1.1%时所得悬浮液质量最好,悬浮率98.3%,是本发明优选的方案,因此,以烷基酚甲醛树脂聚氧乙烯醚4%为润湿剂,NNO 2%+聚氧乙烯聚氧丙烯醚嵌段共聚物3%为分散剂,硅酸铝镁1%+黄原胶0.1%为增稠剂进行下一步试验。The screening results of the dosage of wetting agent, dispersing agent and thickening agent show that the dosage of wetting agent, dispersing agent and thickening agent is 4%+5%+1.1%, 5%+5%+0.1%, 3%+5% +0.5%, 5%+4%+1.1%, 3%+4%+0.1%, 4%+4%+0.5%, 5%+6%+0.5%, the suspension rate is high (90.0%~98.3 %), the quality of the obtained suspension was better (Table 5). Among them, wetting agent (alkylphenol formaldehyde resin polyoxyethylene ether) 4%, dispersant (NNO: polyoxyethylene polyoxypropylene ether block copolymer = 2:3) 5%, thickener (aluminum silicate) Magnesium: xanthan gum=1:0.1) 1.1% of the obtained suspension has the best quality, and the suspension rate is 98.3%, which is the preferred solution of the present invention. Therefore, 4% of alkylphenol formaldehyde resin polyoxyethylene ether is used as the wetting agent , NNO 2% + polyoxyethylene polyoxypropylene ether block copolymer 3% as dispersant, aluminum magnesium silicate 1% + xanthan gum 0.1% as thickener for the next test.
4、成膜剂种类及用量的对比试验4. Comparison test of types and dosages of film formers
采用经验法进行成膜剂种类及用量筛选。将不同成膜剂与润湿剂烷基酚甲醛树脂聚氧乙烯醚4g、分散剂NNO 2g、聚氧乙烯聚氧丙烯醚嵌段共聚物3g、增稠剂硅酸铝镁1g、黄原胶0.1g、吡唑解草酯30g(折百)混合,加水至100g,以锆珠为介质,介质系数为1,砂磨2.5h,砂磨温度控制在45℃以下,制得30%吡唑解草酯悬浮液。用移液枪吸取1mL制得的悬浮液加入到培养皿中,加入小麦种子50g,加盖均匀摇晃5min,打开盖子,将包衣种子平展开,使其成膜,观察种子表面,记录成膜时间(所有种子表面的种衣剂均固化成膜需要的时间)并测定包衣均匀度和脱落率。The types and dosages of film-forming agents were screened by empirical method. Different film formers and wetting agents, alkylphenol formaldehyde resin polyoxyethylene ether 4g, dispersant NNO 2g, polyoxyethylene polyoxypropylene ether block copolymer 3g, thickener aluminum magnesium silicate 1g, xanthan gum Mix 0.1g and 30g (folded) of difenapyr, add water to 100g, use zirconium beads as the medium, the medium coefficient is 1, sand mill for 2.5h, and control the sand mill temperature below 45°C to obtain 30% pyrazole chlorfenapyr suspension. Pipette 1 mL of the prepared suspension into a petri dish, add 50 g of wheat seeds, cover and shake for 5 minutes, open the lid, spread the coated seeds flat to form a film, observe the surface of the seeds, and record the film formation time (the time it takes for the seed coating on all seed surfaces to cure into a film) and measure the coating uniformity and shedding rate.
表6吡唑解草酯悬浮种衣剂成膜剂种类及用量筛选结果Table 6 Screening results of the types and dosages of the film-forming agent of pyraclostrofen suspension seed coating agent
成膜剂种类及用量筛选结果表明:聚乙烯醇用量3%~5%、聚乙二醇用量2%~4%、聚丙烯酰胺用量3%~4%时,包衣均匀度高(90.6%~95.7%),脱落率低(0.2%~6.6%),成膜时间短(3~6min),成膜效果好(表6)。其中,聚乙二醇用量2%时均匀度95.7%、脱落率3.4%、成膜时间5min,且用量少,成本低,是本发明优选的方案,因此,以聚乙二醇2%为成膜剂进行下一步试验。The screening results of the type and dosage of film-forming agents show that when the dosage of polyvinyl alcohol is 3% to 5%, the dosage of polyethylene glycol is 2% to 4%, and the dosage of polyacrylamide is 3% to 4%, the coating uniformity is high (90.6%). ~95.7%), low shedding rate (0.2%~6.6%), short film forming time (3~6min), and good film forming effect (Table 6). Among them, when the polyethylene glycol dosage is 2%, the uniformity is 95.7%, the shedding rate is 3.4%, and the film forming time is 5 minutes, and the dosage is small and the cost is low, which is the preferred solution of the present invention. Therefore, 2% polyethylene glycol is used as the The film-forming agent was tested in the next step.
5、防冻剂种类及用量的对比试验5. Comparative test of antifreeze type and dosage
采用经验法进行防冻剂种类及用量筛选。将不同防冻剂与润湿剂烷基酚甲醛树脂聚氧乙烯醚4g、分散剂NNO 2g、聚氧乙烯聚氧丙烯醚嵌段共聚物3g、增稠剂硅酸铝镁1g、黄原胶0.1g、成膜剂聚乙二醇2g、吡唑解草酯30g(折百)混合,加水至100g,以锆珠为介质,介质系数为1,砂磨2.5h,砂磨温度控制在45℃以下,制得30%吡唑解草酯悬浮液。将制得的悬浮液在0±1℃下放置7d,7d后恢复至室温,测定粘度、悬浮率、筛析。The type and amount of antifreeze were screened by empirical method. Different antifreeze and wetting agent alkylphenol formaldehyde resin polyoxyethylene ether 4g, dispersant NNO 2g, polyoxyethylene polyoxypropylene ether block copolymer 3g, thickener aluminum magnesium silicate 1g, xanthan gum 0.1g g. Mix 2 g of polyethylene glycol as a film-forming agent, and 30 g of pyrfenapyr (100%), add water to 100 g, use zirconium beads as the medium, the medium coefficient is 1, sand for 2.5 hours, and the sanding temperature is controlled at 45 ° C In the following, a 30% suspension of diflufenapyr was prepared. The prepared suspension was placed at 0±1°C for 7 days, and returned to room temperature after 7 days, and the viscosity, suspension rate and sieve analysis were measured.
表7吡唑解草酯悬浮种衣剂防冻剂种类及用量筛选结果Table 7 Screening results of the types and dosages of antifreeze agents for pyraclostrofen suspension seed coating
防冻剂种类及用量筛选结果表明:乙二醇4%~5%、丙三醇4%~5%、尿素2%~5%时,经冷贮试验后悬浮率高(91.2%~96.4%),筛析高(99.0%~99.9%),粘度适中(表7)。其中,尿素用量2%时,经低温贮存后粘度适中(373mPs·s),悬浮率94.9%,筛析99.7%,且用量少,成本低,是本发明优选的方案,因此,以尿素2%为防冻剂进行下一步试验。The screening results of the type and dosage of antifreeze show that: when ethylene glycol is 4%-5%, glycerol 4%-5%, and urea is 2%-5%, the suspension rate is high (91.2%-96.4%) after the cold storage test. , high sieve separation (99.0% ~ 99.9%), moderate viscosity (Table 7). Wherein, when the amount of urea is 2%, the viscosity is moderate (373mPs·s) after storage at low temperature, the suspension rate is 94.9%, the sieving rate is 99.7%, and the amount is small and the cost is low, which is the preferred solution of the present invention. Therefore, urea 2 % is the antifreeze agent for the next test.
6、消泡剂种类及用量的对比试验6. Comparative test of type and dosage of defoamer
采用经验法进行消泡剂种类及用量筛选。将不同消泡剂与润湿剂烷基酚甲醛树脂聚氧乙烯醚4g、分散剂NNO 2g、聚氧乙烯聚氧丙烯醚嵌段共聚物3g、增稠剂硅酸铝镁1g、黄原胶0.1g、成膜剂聚乙二醇2g、防冻剂尿素2g、吡唑解草酯30g(折百)混合,加水至100g,以锆珠为介质,介质系数为1,砂磨2.5h,砂磨温度控制在45℃以下,制成30%吡唑解草酯悬浮液,观察制备过程及产品中的气泡数量。The type and dosage of defoamer were screened by empirical method. Different defoamer and wetting agent alkylphenol formaldehyde resin polyoxyethylene ether 4g, dispersant NNO 2g, polyoxyethylene polyoxypropylene ether block copolymer 3g, thickener aluminum magnesium silicate 1g, xanthan gum 0.1g, 2g film-forming agent polyethylene glycol, 2g antifreeze urea, and 30g pyraclostrobin (100%), add water to 100g, use zirconium beads as medium, medium coefficient is 1, sand for 2.5h, sand The grinding temperature was controlled below 45° C. to prepare a 30% pyrafenox suspension, and the preparation process and the number of air bubbles in the product were observed.
表8吡唑解草酯悬浮种衣剂消泡剂种类及用量筛选结果Table 8 Screening results of the types and dosages of defoaming agents of pyraclostrofen suspension for seed coating
消泡剂种类及用量筛选结果表明:异辛醇用量1.0%~2.5%时制备过程及产品中气泡较少(表8)。其中,异辛醇用量1.5%时,制备过程中及产品没有明显气泡,且用量少,成本低,是本发明优选的方案,因此,以异辛醇1.5%为消泡剂进行下一步试验。The screening results of the type and dosage of defoamer show that: when the dosage of isooctanol is 1.0% to 2.5%, there are less bubbles in the preparation process and product (Table 8). Among them, when the amount of isooctyl alcohol is 1.5%, there are no obvious bubbles in the preparation process and the product, and the amount is small and the cost is low, which is the preferred solution of the present invention. Therefore, the next step test is carried out with 1.5% isooctanol as the defoaming agent. .
实施例4 30%吡唑解草酯悬浮种衣剂的制备方法Example 4 The preparation method of 30% diflufenapyr suspension seed coating
实施例1所述30%吡唑解草酯悬浮种衣剂由如下方法制得:The 30% diflufenapyr suspension seed coating described in Example 1 is prepared by the following method:
将各种固体成分过320目筛,将吡唑解草酯原药、烷基酚甲醛树脂聚氧乙烯醚、NNO、聚氧乙烯聚氧丙烯醚嵌段共聚物、硅酸铝镁、黄原胶、聚乙二醇、尿素、异辛醇、玫瑰精、异噻唑啉酮、去离子水按比例加入砂磨机中,高速搅拌预分散30min,加入砂磨介质锆珠(介质系数为1),砂磨2.5h,砂磨温度控制在45℃以下,经过滤去掉砂磨介质及杂质。Pass various solid components through a 320-mesh sieve, and sieve the pyrazole hydrochloride, alkylphenol formaldehyde resin polyoxyethylene ether, NNO, polyoxyethylene polyoxypropylene ether block copolymer, aluminum magnesium silicate, xanthogen Glue, polyethylene glycol, urea, isooctanol, rose essence, isothiazolinone, and deionized water are added to the sand mill in proportion, and pre-dispersed at high speed for 30 minutes, and then add sand grinding medium zirconium beads (media coefficient is 1) , Sanding for 2.5h, the sanding temperature is controlled below 45 ℃, and the sanding medium and impurities are removed by filtration.
效果验证2 30%吡唑解草酯悬浮种衣剂的质量检测Effect Verification 2 Quality Inspection of 30% Mezafenapyr Suspended Seed Coating Agent
按照实施例1所述的30%吡唑解草酯悬浮种衣剂配方制备5批次样品。Five batches of samples were prepared according to the formulation of 30% diflufenapyr suspension seed coating described in Example 1.
30%吡唑解草酯悬浮种衣剂质量指标参照NY 621—2002,具体为:The quality index of 30% pyraclostrobin suspended seed coating refers to NY 621-2002, specifically:
1、外观:应为可流动的均匀悬浮液,长期存放可有少量沉淀或分层,但置于室温下用手摇动应能恢复原状,不应有结块;1. Appearance: It should be a flowable and uniform suspension, there may be a small amount of precipitation or stratification in long-term storage, but it should be able to restore to its original state when shaken by hand at room temperature, and there should be no agglomeration;
2、有效成分含量≥标明含量;2. The content of active ingredients ≥ the indicated content;
3、pH值:5.0~7.0;3. pH value: 5.0~7.0;
4、悬浮率≥90%;4. Suspension rate ≥ 90%;
5、筛析(通过44μm试验筛)≥99%;5. Sieve analysis (passing 44μm test sieve) ≥ 99%;
6、粘度范围(25℃):100~600mPa·s;6. Viscosity range (25℃): 100~600mPa·s;
7、成膜性:合格;7. Film formation: qualified;
8、包衣均匀度≥90%;8. Coating uniformity ≥90%;
9、包衣脱落率≤8%;9. The coating shedding rate is less than or equal to 8%;
10、低温稳定性:合格;10. Low temperature stability: qualified;
11、热贮稳定性:合格。11. Thermal storage stability: qualified.
有效成分含量测定采用高效液相色谱法,Hypersil C18色谱柱,进样体积5.0μL;柱温35℃;流动相:V(乙腈):V(水)=25:75,流速1.0mL/min;经孔径0.45μm的滤膜过滤,于超声波浴槽中超声脱气15min;检测波长273nm;保留时间约7.24min。pH值测定按照GB/T1601—1993进行。筛析测定按照GB/T 16150—1995进行。悬浮率、粘度范围、成膜性、包衣均匀度、包衣脱落率、低温稳定性、热贮稳定性测定按照NY 621—2002进行。The content of active ingredients was determined by high performance liquid chromatography, Hypersil C18 chromatographic column, injection volume 5.0 μL; column temperature 35 °C; mobile phase: V (acetonitrile): V (water) = 25:75, flow rate 1.0 mL/min; Filtered through a filter membrane with a pore size of 0.45 μm, and ultrasonically degassed in an ultrasonic bath for 15 minutes; the detection wavelength was 273 nm; the retention time was about 7.24 minutes. The pH value was measured according to GB/T1601-1993. The sieve analysis was carried out in accordance with GB/T 16150-1995. Suspension rate, viscosity range, film-forming property, coating uniformity, coating shedding rate, low temperature stability, and thermal storage stability were measured in accordance with NY 621-2002.
30%吡唑解草酯悬浮种衣剂的质量检测结果表明,5批次样品各项质量检测结果均为合格,表明该配方及制备方法可行(表9)。The quality inspection results of the 30% pyrimethacrylate suspended seed coating showed that all the quality inspection results of the 5 batches of samples were qualified, indicating that the formula and preparation method were feasible (Table 9).
表9 30%吡唑解草酯悬浮种衣剂质量检测结果Table 9 Quality test results of 30% pyraclostrofen suspension seed coating
效果验证3 30%吡唑解草酯悬浮种衣剂对种子安全性测定Effect verification 3. Determination of the safety of 30% mezafen-prop-prop-prop suspension seed coating on seeds
吡唑解草酯用量47.1g/hm2即有很好的效果,因此,以47.1g/hm2为正常用量,试验中分别按照正常用量的1、2、4、6、8、10倍进行种子处理,以明确对种子的安全性。将所制备的30%吡唑解草酯悬浮种衣剂按比例稀释后,按照用量47.1、94.2、188.4、282.6、376.8、471.0g/hm2分别对小麦(品种:济麦22)种子进行包衣,药种比(种衣剂药液质量:种子质量)为1:50,以清水处理为对照。47.1g/hm 2 of difenapyr has a good effect. Therefore, taking 47.1g/hm 2 as the normal dosage, the tests were carried out according to 1, 2, 4, 6, 8, and 10 times of the normal dosage, respectively. Seed treatment to clarify the safety of seeds. After diluting the prepared 30% diflufenapyr suspension seed coating agent in proportion, the seeds of wheat (variety: Jimai 22) were packaged according to the dosage of 47.1, 94.2, 188.4, 282.6, 376.8 and 471.0 g /hm2 respectively. The ratio of coating to drug species (the quality of the seed coating agent liquid: the quality of the seeds) was 1:50, and the water treatment was used as the control.
通过室内试验测定30%吡唑解草酯悬浮种衣剂对种子室内发芽势和室内发芽率的影响:将种子等距离排列在润湿的滤纸上,于20℃恒温培养箱中培养,每天观察发芽情况并及时补充水分,分别于第4天时统计并计算室内发芽势,于第12天时测定室内发芽率。设4个重复,每个重复50粒。Determination of the effect of 30% pyriflufen-ethyl suspended seed coating agent on the indoor germination potential and indoor germination rate of seeds by indoor test: Arrange the seeds equidistantly on the moistened filter paper, cultivate in a constant temperature incubator at 20 °C, and observe every day. The germination situation and timely supplement of water were counted and calculated on the 4th day, and the indoor germination rate was measured on the 12th day. Set 4 repetitions, each with 50 capsules.
通过田间试验测定30%吡唑解草酯悬浮种衣剂对种子田间发芽率的影响:田间整地后人工开沟播种,播种后7d、15d分别调查出苗数,计算出苗率。设4个重复,每个重复200粒。The effect of 30% pyrazin suspension seed coating on seed germination rate was determined by field test: artificially ditch sowing after field preparation, investigate the number of seedlings 7d and 15d after sowing, and calculate the germination rate. Set 4 repetitions, each with 200 capsules.
表10 30%吡唑解草酯悬浮种衣剂对小麦种子安全性Table 10 The safety of 30% pyrazin-flu-fen suspension seed coating on wheat seeds
30%吡唑解草酯悬浮种衣剂对种子安全性测定结果表明,正常用量10倍处理对小麦有一定药害,可以降低小麦发芽势和发芽率;正常用量1~8倍处理,对小麦安全。表明本发明制备的30%吡唑解草酯悬浮种衣剂对种子安全(表10)。The results of 30% pyraclostrobin suspended seed coating on seeds showed that the treatment of 10 times the normal dosage had certain phytotoxicity to wheat and could reduce the germination potential and germination rate of wheat; Safety. It is shown that the 30% mezafenapyr suspension seed coating prepared by the present invention is safe for seeds (Table 10).
效果实验4室内生测实施例Example of Indoor Bioassay of Effect Experiment 4
本发明的室内生测实施例依据《农药室内生物测定试验准则除草剂第4部分:活性测定试验茎叶喷雾法(NY/T 1155.4—2006)》进行,通过室内生物测定,明确30%吡唑解草酯悬浮种衣剂的应用效果。试验方法如下:The indoor bioassay examples of the present invention are carried out according to the "Pesticide Indoor Bioassay Test Guidelines for Herbicides Part 4: Activity Determination Test Stem and Leaf Spray Method (NY/T 1155.4-2006)", and through the indoor bioassay, it is clear that 30% pyrazole The application effect of fenpropion suspension seed coating agent. The test method is as follows:
准确称取95%甲基二磺隆原药2.5263g,溶解于25mL N,N-二甲基甲酰胺,制成浓度为96g/L的甲基二磺隆母液。准确称取95.5%吡唑解草酯原药2.0942g,溶解于25mL丙酮,制成浓度为80g/L的吡唑解草酯母液。试验时,分别取适量甲基二磺隆母液、唑解草酯母液,以适量0.1%的土温80水溶液稀释,制成供试喷雾药液。Accurately weigh 2.5263 g of 95% methyldisulfuron-methyl and dissolve it in 25 mL of N,N-dimethylformamide to prepare a methyldisulfuron-methyl mother liquor with a concentration of 96 g/L. Accurately weigh 2.0942 g of the 95.5% diflufenapyr technical drug, dissolve it in 25 mL of acetone, and prepare a diflufenapyr mother solution with a concentration of 80 g/L. During the test, an appropriate amount of the mother liquor of metsulfuron-methyl and the mother liquor of carflufenacil were respectively diluted with an appropriate amount of 0.1% aqueous solution of Tween 80 to prepare the test spray liquid.
采用盆栽试验法,供试靶标为冬小麦(品种:济麦22)、节节麦、野燕麦、播娘蒿。在日光温室内,选择直径12cm、高11cm的塑料盆钵育苗,施药前定苗,每盆保留均匀一致的植株10株。供试小麦及杂草2~3叶期茎叶喷施除草剂甲基二磺隆或甲基二磺隆与吡唑解草酯的混配剂,每处理重复4次,药液量450L/hm2。种子包衣处理,播种前将30%吡唑解草酯悬浮种衣剂按比例稀释后,按照药种比(种衣剂药液质量:种子质量)1:50对小麦种子进行包衣后播种。药后14d,称量每盆植株鲜重,计算各处理对杂草的防效或对小麦的药害率E:The pot experiment method was adopted, and the test targets were winter wheat (variety: Jimai 22), Jiejiemai, wild oats, and Artemisia somnifera. In the solar greenhouse, choose plastic pots with a diameter of 12 cm and a height of 11 cm to raise seedlings, set the seedlings before spraying, and keep 10 uniform plants in each pot. The test wheat and weeds were sprayed with the herbicide mesulfuron-methyl or the mixture of mesulfuron-ethyl and pyraclostrofen at the 2-3 leaf stage of the tested wheat and weeds. Each treatment was repeated 4 times, and the liquid volume was 450L/ hm 2 . Seed coating treatment, before sowing, after diluting 30% pyraclostrofen suspension seed coating agent in proportion, coat the wheat seeds according to the ratio of drug to seed (quality of seed coating agent liquid: seed quality) 1:50 before sowing . 14 days after the treatment, the fresh weight of each pot was weighed, and the control effect of each treatment on weeds or the phytotoxicity rate E to wheat was calculated:
式中:E——对杂草的防效或对小麦的药害率In the formula: E——the control effect on weeds or the phytotoxicity rate on wheat
T——药剂处理组小麦或杂草地上部分鲜重;T——the fresh weight of the wheat or weeds in the chemical treatment group;
C——空白对照组小麦或杂草地上部分鲜重。C—the fresh weight of part of the wheat or weeds in the blank control group.
生测试验结果见表11。结果表明:甲基二磺隆用量15.7g/hm2,不使用吡唑解草酯时对小麦的药害率为27.84%,吡唑解草酯47.1g/hm2种子处理后,对小麦的药害率为-0.20%;甲基二磺隆用量11.2g/hm2,不使用吡唑解草酯时对小麦的药害率为19.35%,吡唑解草酯47.1g/hm2种子处理后,对小麦的药害率为-0.15%,表明在室内条件下,吡唑解草酯具有种子处理活性。The results of the bioassay test are shown in Table 11. The results showed that when the dosage of metsulfuron-methyl was 15.7g /hm 2 , the phytotoxicity rate to wheat was 27.84% without the use of pyriflufen-ethyl. The phytotoxicity rate was -0.20%; the dosage of metsulfuron-methyl was 11.2g/hm 2 , the phytotoxicity rate to wheat was 19.35% without the use of diflufenapyr, and the cyclofenapyr 47.1g/hm 2 seed treatment Afterwards, the phytotoxicity rate to wheat was -0.15%, which indicated that pyraclostrofen had seed treatment activity under indoor conditions.
甲基二磺隆用量15.7g/hm2,采用30%吡唑解草酯悬浮种衣剂包衣处理后,对节节麦的防效为99.59%,对播娘蒿的防效为85.36%,对小麦的药害率为-0.20%,对野燕麦的防效为94.08%;现有的吡唑解草酯与甲基二磺隆混合喷雾技术对节节麦的防效为90.48%,对播娘蒿的防效为76.66%,对小麦药害率为6.81%,对野燕麦的防效为93.15%。表明采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理可以明显提高甲基二磺隆对节节麦和播娘蒿的防效,同时显著降低对小麦的药害,对野燕麦的防效没有影响。The dosage of metsulfuron-methyl was 15.7g/hm 2 , and after coating treatment with 30% pyrazol-but-fen-propoxylate suspension seed coating, the control effect on J. , the phytotoxicity rate to wheat was -0.20%, and the control effect to wild oat was 94.08%; The control effect on Artemisia somnifera was 76.66%, the phytotoxicity rate on wheat was 6.81%, and the control effect on wild oats was 93.15%. It is shown that the use of the 30% pyrazin suspension seed coating agent provided by the present invention for seed treatment can significantly improve the control effect of methyldisulfuron on A. The control efficacy of wild oats was not affected.
另外,不使用吡唑解草酯时,对节节麦的防效为98.05%,对播娘蒿的防效为85.43%,对小麦药害率为27.84%,对野燕麦的防效为92.92%,表明为了保证对作物的安全性,甲基二磺隆必须配合吡唑解草酯使用,但现有技术吡唑解草酯与甲基二磺隆混合喷雾可以显著降低除草剂对杂草的防效,采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理不影响除草剂药效。In addition, when pyraclostrobin was not used, the control effect on A. japonicus was 98.05%, the control effect on Artemisia annua was 85.43%, the phytotoxicity rate on wheat was 27.84%, and the control effect on wild oat was 92.92%. %, indicating that in order to ensure the safety of crops, mesulfuron-methyl must be used in combination with mefenox-ethyl, but the prior art mixed spraying of mesulfuron-ethyl and mesulfuron-ethyl can significantly reduce the effect of herbicides on weeds. The control effect of the herbicide is not affected by the use of the 30% pyriflufen-ethyl suspension seed coating provided by the present invention for seed treatment.
甲基二磺隆用量11.2g/hm2,采用30%吡唑解草酯悬浮种衣剂包衣处理后,对节节麦的防效为95.07%,对播娘蒿的防效为85.39%,对小麦的药害率为-0.15%,对野燕麦的防效为83.25%;现有的吡唑解草酯与甲基二磺隆混合喷雾技术对节节麦的防效为80.86%,对播娘蒿的防效为56.67%,对小麦药害率为5.16%,对野燕麦的防效为81.74%。表明采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理可以明显提高甲基二磺隆对节节麦和播娘蒿的防效,同时显著降低对小麦的药害,对野燕麦的防效没有影响。另外,不使用吡唑解草酯时,对节节麦的防效为93.47%,对播娘蒿的防效为84.30%,对小麦药害率为19.35%,对野燕麦的防效为81.43%,表明为了保证对作物的安全性,甲基二磺隆必须配合吡唑解草酯使用,但现有技术吡唑解草酯与甲基二磺隆混合喷雾可以显著降低除草剂对杂草的防效,采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理不影响除草剂药效。The dosage of metsulfuron-methyl was 11.2 g/hm 2 , and after coating treatment with 30% pyraclostrofen suspension seed coating agent, the control effect on J. , the phytotoxicity rate to wheat was -0.15%, and the control effect to wild oat was 83.25%; The control effect on Artemisia somnifera was 56.67%, the phytotoxicity rate on wheat was 5.16%, and the control effect on wild oats was 81.74%. It is shown that the use of the 30% pyrazin suspension seed coating agent provided by the present invention for seed treatment can significantly improve the control effect of methyldisulfuron on A. The control efficacy of wild oats was not affected. In addition, when pyraclostrobin was not used, the control effect of fenugreek was 93.47%, the control effect of Artemisia annua was 84.30%, the phytotoxicity rate of wheat was 19.35%, and the control effect of wild oat was 81.43%. %, indicating that in order to ensure the safety of crops, mesulfuron-methyl must be used in combination with mefenox-ethyl, but the prior art mixed spraying of mesulfuron-ethyl and mesulfuron-ethyl can significantly reduce the effect of herbicides on weeds. The control effect of the herbicide is not affected by the use of the 30% pyriflufen-ethyl suspension seed coating provided by the present invention for seed treatment.
采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理后喷施甲基二磺隆,用量11.2g/hm2,对节节麦的防效为95.07%,对播娘蒿的防效为85.39%;现有技术甲基二磺隆用量15.7g/hm2,对节节麦的防效为90.48%,对播娘蒿的防效为76.66%;表明采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理后喷施甲基二磺隆,可以显著降低除草剂用量,提高除草剂对杂草防治效果。The 30% pyrazin suspension seed coating provided by the present invention is used for seed treatment and then sprayed with metsulfuron-methyl at a dosage of 11.2 g/hm 2 . The effect is 85.39%; the dosage of metsulfuron-methyl in the prior art is 15.7g/hm 2 , the control effect on Jiejie is 90.48%, and the control effect on Artemisia spp. After the seed treatment with mezafenpyr suspension seed coating, the application of metsulfuron-methyl can significantly reduce the dosage of herbicides and improve the control effect of herbicides on weeds.
采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理后喷施甲基二磺隆,用量15.7g/hm2,对小麦的药害率为-0.20%;现有技术甲基二磺隆用量11.2g/hm2,对小麦药害率为5.16%;表明采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理可以显著提高除草剂对作物的安全性。The 30% mezafenib suspended seed coating agent provided by the present invention is used for seed treatment and then sprayed with methyldisulfuron, the dosage is 15.7g/hm 2 , and the phytotoxicity rate to wheat is -0.20%; The dosage of Sulfuron-methyl is 11.2g/hm 2 , and the phytotoxicity rate to wheat is 5.16%; it shows that the 30% pyrazin suspension seed coating provided by the present invention can significantly improve the safety of the herbicide to crops.
表11 30%吡唑解草酯悬浮种衣剂种子处理对除草剂药效和药害的影响生测试验结果Table 11 Bioassay test results of the effect of 30% pyrazin suspension seed coating on the efficacy and phytotoxicity of herbicides
注:吡唑解草酯种子处理用量47.1g/hm2,播种量以187.5kg/hm2计,折合为25.12g/100kg种子,即a g/hm2折合(a/187.5×100)g/100kg种子。Note: The dosage of pyraclostrofen seed treatment is 47.1g/hm 2 , and the seeding rate is calculated as 187.5kg/hm 2 , which is equivalent to 25.12g/100kg seeds, that is, ag/hm 2 is equivalent to (a/187.5×100)g/100kg seed.
效果验证5田间药效试验实施例Effect Verification 5 Field Drug Efficacy Test Example
本发明的田间药效试验实施例依据《农药田间药效试验准则(一)除草剂防治麦类作物地杂草(GB/T 17980.41-2000)》进行,通过田间小区试验,验证室内生测试验结果。试验方法如下:The field efficacy test example of the present invention is carried out according to "Pesticide Field Efficacy Test Guidelines (1) Herbicide Controlling Weeds in Wheat Crops (GB/T 17980.41-2000)", and the indoor bioassay test is verified through field plot test result. The test method is as follows:
杂草2~3叶期茎叶喷雾处理,药液量450L/hm2,每处理重复4次,小区面积25m2,随机区组排列。药后30d调查,每小区随机抽取4个样点,每点1m2,分别调查小麦和每种杂草的鲜重,计算各处理对杂草的防效或对小麦的药害率E:The weeds were treated by spraying on stems and leaves at the 2-3 leaf stage, the liquid volume was 450L/hm 2 , each treatment was repeated 4 times, the plot area was 25 m 2 , and the cells were randomly arranged in blocks. 30 days after the treatment, 4 sampling points were randomly selected from each plot, each of 1 m 2 , and the fresh weights of wheat and each weed were investigated respectively, and the control effect of each treatment on weeds or the phytotoxicity rate E to wheat was calculated:
式中:E——对杂草的防效或对小麦的药害率In the formula: E——the control effect on weeds or the phytotoxicity rate on wheat
PT——药剂处理区小麦或杂草鲜重;PT - fresh weight of wheat or weeds in the chemical treatment area;
CK——空白对照区小麦或杂草鲜重。CK - fresh weight of wheat or weeds in blank control area.
试验在河北省邯郸市馆陶县寿山寺村进行,供试靶标为冬小麦(品种:济麦22)、节节麦、野燕麦、播娘蒿等,处理方法、各处理对杂草的防效及对小麦的药害率见表12。The test was carried out in Shoushansi Village, Guantao County, Handan City, Hebei Province. The targets for the test were winter wheat (variety: Jimai 22), Jiejie wheat, wild oats, Artemisia somnifera, etc. The treatment methods, the control effects of each treatment on weeds and The phytotoxicity rate to wheat is shown in Table 12.
田间药效试验结果表明:甲基二磺隆用量15.7g/hm2,不使用吡唑解草酯时对小麦的药害率为20.09%,吡唑解草酯47.1g/hm2种子处理后,对小麦的药害率为0.88%;甲基二磺隆用量11.2g/hm2,不使用吡唑解草酯时对小麦的药害率为18.28%,吡唑解草酯47.1g/hm2种子处理后,对小麦的药害率为0.24%,表明在田间条件下,吡唑解草酯具有种子处理活性。The results of the field efficacy test showed that: the dosage of metsulfuron-methyl was 15.7g/hm 2 , the phytotoxicity rate to wheat was 20.09% without the use of diflufenapyr, and 47.1g/hm 2 seeds were treated with diflufenapyr. , the phytotoxicity rate to wheat was 0.88%; the dosage of metsulfuron-methyl was 11.2g/hm 2 , the phytotoxicity rate to wheat was 18.28% when pyrafen-methyl was not used, 47.1g/hm After 2 seed treatments, the phytotoxicity rate to wheat was 0.24%, which indicated that pyraclostrobin had seed treatment activity under field conditions.
甲基二磺隆用量15.7g/hm2,采用30%吡唑解草酯悬浮种衣剂包衣处理后,对节节麦的防效为96.49%,对播娘蒿的防效为81.75%,对小麦的药害率为0.88%,对野燕麦的防效为91.86%;现有的吡唑解草酯与甲基二磺隆混合喷雾技术对节节麦的防效为87.55%,对播娘蒿的防效为71.21%,对小麦药害率为7.75%,对野燕麦的防效为91.21%。表明采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理可以明显提高甲基二磺隆对节节麦和播娘蒿的防效,同时显著降低对小麦的药害,对野燕麦的防效没有影响。另外,不使用吡唑解草酯时,对节节麦的防效为96.62%,对播娘蒿的防效为79.99%,对小麦药害率为20.09%,对野燕麦的防效为91.99%,表明为了保证对作物的安全性,甲基二磺隆必须配合吡唑解草酯使用,但现有技术吡唑解草酯与甲基二磺隆混合喷雾可以显著降低除草剂对杂草的防效,采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理不影响除草剂药效。The dosage of metsulfuron-methyl was 15.7g/hm 2 , and after coating treatment with 30% pyrazin-flu-methyl suspension seed coating agent, the control effect on J. , the phytotoxicity rate to wheat was 0.88%, and the control effect to wild oats was 91.86%; The control effect of Artemisia somnifera was 71.21%, the phytotoxicity rate to wheat was 7.75%, and the control effect to wild oats was 91.21%. It is shown that the use of the 30% pyrazin suspension seed coating agent provided by the present invention for seed treatment can significantly improve the control effect of methyldisulfuron on A. The control efficacy of wild oats was not affected. In addition, when pyraclostrochloride was not used, the control effect on A. japonicus was 96.62%, the control effect on Artemisia annua was 79.99%, the phytotoxicity rate on wheat was 20.09%, and the control effect on wild oat was 91.99%. %, indicating that in order to ensure the safety of crops, mesulfuron-methyl must be used in combination with mefenox-ethyl, but the prior art mixed spraying of mesulfuron-ethyl and mesulfuron-ethyl can significantly reduce the effect of herbicides on weeds. The control effect of the herbicide is not affected by the use of the 30% pyriflufen-ethyl suspension seed coating provided by the present invention for seed treatment.
甲基二磺隆用量11.2g/hm2,采用30%吡唑解草酯悬浮种衣剂包衣处理后,对节节麦的防效为91.82%,对播娘蒿的防效为80.93%,对小麦的药害率为0.24%,对野燕麦的防效为82.20%;现有的吡唑解草酯与甲基二磺隆混合喷雾技术对节节麦的防效为72.88%,对播娘蒿的防效为50.38%,对小麦药害率为6.56%,对野燕麦的防效为80.38%。表明采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理可以明显提高甲基二磺隆对节节麦和播娘蒿的防效,同时显著降低对小麦的药害,对野燕麦的防效没有影响。另外,不使用吡唑解草酯时,对节节麦的防效为91.75%,对播娘蒿的防效为79.26%,对小麦药害率为18.28%,对野燕麦的防效为81.26%,表明为了保证对作物的安全性,甲基二磺隆必须配合吡唑解草酯使用,但现有技术吡唑解草酯与甲基二磺隆混合喷雾可以显著降低除草剂对杂草的防效,采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理不影响除草剂药效。The dosage of metsulfuron-methyl was 11.2g/hm 2 , and after coating treatment with 30% pyraclostrofen suspension seed coating agent, the control effect on J. , the phytotoxicity rate to wheat was 0.24%, and the control effect to wild oat was 82.20%; The control effect of Artemisia sophorae was 50.38%, the phytotoxicity rate to wheat was 6.56%, and the control effect to wild oats was 80.38%. It is shown that the use of the 30% pyrazin suspension seed coating agent provided by the present invention for seed treatment can significantly improve the control effect of methyldisulfuron on A. The control efficacy of wild oats was not affected. In addition, when pyraclostrobin was not used, the control effect of fenugreek was 91.75%, the control effect of Artemisia annua was 79.26%, the phytotoxicity rate of wheat was 18.28%, and the control effect of wild oat was 81.26%. %, indicating that in order to ensure the safety of crops, mesulfuron-methyl must be used in combination with mefenox-ethyl, but the prior art mixed spraying of mesulfuron-ethyl and mesulfuron-ethyl can significantly reduce the effect of herbicides on weeds. The control effect of the herbicide is not affected by the use of the 30% pyriflufen-ethyl suspension seed coating provided by the present invention for seed treatment.
采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理后喷施甲基二磺隆,用量11.2g/hm2,对节节麦的防效为91.82%,对播娘蒿的防效为80.93%;现有技术甲基二磺隆用量15.7g/hm2,对节节麦的防效为87.55%,对播娘蒿的防效为71.21%;表明采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理后喷施甲基二磺隆,可以显著降低除草剂用量,提高除草剂对杂草防治效果。Using the 30% mezafenpyr suspension seed coating provided by the present invention to carry out seed treatment and then spraying metsulfuron-methyl at an dosage of 11.2 g/hm 2 , the control effect on A. The control effect is 80.93%; the dosage of metsulfuron-methyl in the prior art is 15.7g/hm 2 , the control effect on Jiejie is 87.55%, and the control effect on Artemisia spp. After the seed treatment with mezafenpyr suspension seed coating, the application of metsulfuron-methyl can significantly reduce the dosage of herbicides and improve the control effect of herbicides on weeds.
采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理后喷施甲基二磺隆,用量15.7g/hm2,对小麦的药害率为0.88%;现有技术甲基二磺隆用量11.2g/hm2,对小麦药害率为6.56%;表明采用本发明提供的30%吡唑解草酯悬浮种衣剂进行种子处理可以显著提高除草剂对作物的安全性。The 30% pyrazin suspension seed coating agent provided by the present invention is used for seed treatment and after spraying methyldisulfuron, the dosage is 15.7g/hm 2 , and the phytotoxicity rate to wheat is 0.88%; the prior art methyldisulfuron The phytotoxicity rate of wheat was 6.56% with the dosage of 11.2g/hm 2 , indicating that the use of the 30% pyraclostrofen suspension seed coating provided by the invention for seed treatment can significantly improve the safety of the herbicide to crops.
表12 30%吡唑解草酯悬浮种衣剂种子处理对除草剂药效和药害的影响田间试验结果Table 12 Field test results of the effects of 30% pyriflufen-ethyl suspension seed coating seed treatment on herbicide efficacy and phytotoxicity
注:吡唑解草酯种子处理用量47.1g/hm2,播种量以187.5kg/hm2计,折合为25.12g/100kg种子,即a g/hm2折合(a/187.5×100)g/100kg种子。Note: The dosage of pyraclostrofen seed treatment is 47.1g/hm 2 , and the seeding rate is calculated as 187.5kg/hm 2 , which is equivalent to 25.12g/100kg seeds, that is, ag/hm 2 is equivalent to (a/187.5×100)g/100kg seed.
虽然,上文中已经用一般性说明及具体实施方案对本发明作了详尽的描述,但在本发明基础上,可以对之作一些修改或改进,这对本领域技术人员而言是显而易见的。因此,在不偏离本发明精神的基础上所做的这些修改或改进,均属于本发明要求保护的范围。Although the present invention has been described in detail above with general description and specific embodiments, it is obvious to those skilled in the art that some modifications or improvements can be made on the basis of the present invention. Therefore, these modifications or improvements made without departing from the spirit of the present invention fall within the scope of the claimed protection of the present invention.
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