CN116616304A - Azolyl ether and tebuconazole suspending agent and preparation method thereof - Google Patents
Azolyl ether and tebuconazole suspending agent and preparation method thereof Download PDFInfo
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- CN116616304A CN116616304A CN202310489112.7A CN202310489112A CN116616304A CN 116616304 A CN116616304 A CN 116616304A CN 202310489112 A CN202310489112 A CN 202310489112A CN 116616304 A CN116616304 A CN 116616304A
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- tebuconazole
- pyraclostrobin
- suspending agent
- polydimethylsiloxane
- urea
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- PXMNMQRDXWABCY-UHFFFAOYSA-N 1-(4-chlorophenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol Chemical compound C1=NC=NN1CC(O)(C(C)(C)C)CCC1=CC=C(Cl)C=C1 PXMNMQRDXWABCY-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000005839 Tebuconazole Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000375 suspending agent Substances 0.000 title claims description 24
- IEUQLXVHBHEVSJ-UHFFFAOYSA-N 2-(1h-pyrrol-2-yloxy)-1h-pyrrole Chemical compound C=1C=CNC=1OC1=CC=CN1 IEUQLXVHBHEVSJ-UHFFFAOYSA-N 0.000 title 1
- 239000005869 Pyraclostrobin Substances 0.000 claims abstract description 39
- HZRSNVGNWUDEFX-UHFFFAOYSA-N pyraclostrobin Chemical compound COC(=O)N(OC)C1=CC=CC=C1COC1=NN(C=2C=CC(Cl)=CC=2)C=C1 HZRSNVGNWUDEFX-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000003814 drug Substances 0.000 claims abstract description 28
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 22
- SNAAJJQQZSMGQD-UHFFFAOYSA-N aluminum magnesium Chemical compound [Mg].[Al] SNAAJJQQZSMGQD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000004202 carbamide Substances 0.000 claims abstract description 22
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 22
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 22
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 claims abstract description 22
- 235000010234 sodium benzoate Nutrition 0.000 claims abstract description 22
- 239000004299 sodium benzoate Substances 0.000 claims abstract description 22
- 239000000230 xanthan gum Substances 0.000 claims abstract description 22
- 229920001285 xanthan gum Polymers 0.000 claims abstract description 22
- 229940082509 xanthan gum Drugs 0.000 claims abstract description 22
- 235000010493 xanthan gum Nutrition 0.000 claims abstract description 22
- 229940079593 drug Drugs 0.000 claims abstract description 17
- 239000000725 suspension Substances 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims description 44
- 239000004576 sand Substances 0.000 claims description 39
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 38
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 37
- 239000007788 liquid Substances 0.000 claims description 30
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 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 17
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 17
- 239000000126 substance Substances 0.000 claims description 17
- 239000006185 dispersion Substances 0.000 claims description 15
- VAYGXNSJCAHWJZ-UHFFFAOYSA-N dimethyl sulfate Chemical compound COS(=O)(=O)OC VAYGXNSJCAHWJZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000003801 milling Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims 3
- KWKXNDCHNDYVRT-UHFFFAOYSA-N dodecylbenzene Chemical compound CCCCCCCCCCCCC1=CC=CC=C1 KWKXNDCHNDYVRT-UHFFFAOYSA-N 0.000 claims 3
- 239000011734 sodium Substances 0.000 claims 3
- 229910052708 sodium Inorganic materials 0.000 claims 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 claims 3
- 241000209140 Triticum Species 0.000 abstract description 20
- 235000021307 Triticum Nutrition 0.000 abstract description 20
- 206010039509 Scab Diseases 0.000 abstract description 7
- 241001465754 Metazoa Species 0.000 abstract description 3
- 239000010902 straw Substances 0.000 abstract description 3
- 239000000575 pesticide Substances 0.000 abstract description 2
- MZSDGDXXBZSFTG-UHFFFAOYSA-M sodium;benzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1 MZSDGDXXBZSFTG-UHFFFAOYSA-M 0.000 abstract 1
- DHXVGJBLRPWPCS-UHFFFAOYSA-N Tetrahydropyran Chemical compound C1CCOCC1 DHXVGJBLRPWPCS-UHFFFAOYSA-N 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000003640 drug residue Substances 0.000 description 2
- 235000013312 flour Nutrition 0.000 description 2
- 230000035784 germination Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000004546 suspension concentrate Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 208000004770 Fusariosis Diseases 0.000 description 1
- 206010051919 Fusarium infection Diseases 0.000 description 1
- 240000005926 Hamelia patens Species 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 231100000570 acute poisoning Toxicity 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- LINOMUASTDIRTM-QGRHZQQGSA-N deoxynivalenol Chemical compound C([C@@]12[C@@]3(C[C@@H](O)[C@H]1O[C@@H]1C=C(C([C@@H](O)[C@@]13CO)=O)C)C)O2 LINOMUASTDIRTM-QGRHZQQGSA-N 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000001076 estrogenic effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000003053 toxin Substances 0.000 description 1
- 231100000765 toxin Toxicity 0.000 description 1
- 108700012359 toxins Proteins 0.000 description 1
- LINOMUASTDIRTM-UHFFFAOYSA-N vomitoxin hydrate Natural products OCC12C(O)C(=O)C(C)=CC1OC1C(O)CC2(C)C11CO1 LINOMUASTDIRTM-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/24—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing the groups, or; Thio analogues thereof
-
- 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
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
- A01N43/647—Triazoles; Hydrogenated triazoles
- A01N43/653—1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P3/00—Fungicides
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- 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
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- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Environmental Sciences (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Pest Control & Pesticides (AREA)
- Zoology (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
本发明公开了一种唑醚、戊唑醇悬浮剂及制备方法，涉及农药技术领域，所述悬浮剂由吡唑醚菌酯原药、戊唑醇原药、morwet D‑425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素以及水制备而得；重量比为1.00～1.06:3.010～3.126:0.3～0.7:0.1～0.4:0.024～0.051:0.11～0.21:0.01～0.04:0.02～0.05:0.3～0.6，余量为水；该悬浮剂能够有效的对小麦赤霉病进行防治，并且施加后，药物在小麦中的残留量极低，秸秆和小麦在后续被人畜食用时不存在安全隐患，安全间隔期适中。The invention discloses a pyraclostrobin and tebuconazole suspension and a preparation method thereof, and relates to the technical field of pesticides. Sodium phenylsulfonate, xanthan gum, magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane, urea and water; the weight ratio is 1.00～1.06:3.010～3.126:0.3～0.7:0.1～ 0.4: 0.024～0.051: 0.11～0.21: 0.01～0.04: 0.02～0.05: 0.3～0.6, the balance is water; the suspension can effectively prevent and treat wheat scab, and after application, the drug in wheat The residual amount is extremely low, and there is no potential safety hazard when the straw and wheat are subsequently eaten by humans and animals, and the safety interval is moderate.
Description
技术领域technical field
本发明涉及农药技术领域，具体为一种唑醚、戊唑醇悬浮剂及制备方法。The invention relates to the technical field of pesticides, in particular to a suspending agent of azole ether and tebuconazole and a preparation method thereof.
背景技术Background technique
小麦赤霉病又称烂穗病、麦秸枯、烂麦头、红麦头、红头瘴，是由多种镰刀菌侵染所引起的、发生在小麦上的病害。从苗期到穗期均可发生，引起苗腐、茎基腐、秆腐和穗腐，以穗腐危害最大。湿度大时，病部均可见粉红色霉层。小麦受害后千综合粒重降低，发芽率下降，发芽势减弱，出粉率低，面粉质量差，色泽灰暗，商品价值降低。病麦含有致呕毒素和类雌性激素述等毒素，人畜食后可引起急性中毒。Wheat head blight, also known as ear rot, wheat straw withered, rotten wheat head, red wheat head, and red head miasma, is a disease that occurs on wheat caused by a variety of Fusarium infection. It can occur from the seedling stage to the ear stage, causing seedling rot, stem base rot, stalk rot and ear rot, and ear rot is the most harmful. When the humidity is high, a pink mold layer can be seen on the diseased part. After the wheat is damaged, the comprehensive grain weight decreases, the germination rate decreases, the germination potential weakens, the flour extraction rate is low, the flour quality is poor, the color is dark, and the commodity value decreases. Sick wheat contains toxins such as vomitoxin and estrogen-like hormones, which can cause acute poisoning after eating by humans and animals.
为了对小麦赤霉病进行防治，本领域的技术人员提出了唑醚、戊唑醇悬浮剂及制备方法。In order to prevent and treat wheat scab, those skilled in the art have proposed fenazole ether, tebuconazole suspending agent and preparation method.
发明内容Contents of the invention
针对现有技术的不足，本发明提供了一种唑醚、戊唑醇悬浮剂及制备方法，能够有效防治小麦赤霉病。Aiming at the deficiencies of the prior art, the present invention provides a suspending agent of azole ether and tebuconazole and a preparation method thereof, which can effectively prevent and treat wheat head blight.
为实现以上目的，本发明提供了一种唑醚、戊唑醇悬浮剂，所述悬浮剂由吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素以及水制备而得；In order to achieve the above object, the present invention provides a kind of azole ether, tebuconazole suspending agent, described suspending agent is made of pyraclostrobin former medicine, tebuconazole former medicine, morwet D-425, dodecylbenzenesulfonate sodium phosphate, xanthan gum, magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane, urea and water;
吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素的重量比为1.00～1.06:3.010～3.126:0.3～0.7:0.1～0.4:0.024～0.051:0.11～0.21:0.01～0.04:0.02～0.05:0.3～0.6，余量为水。Pyraclostrobin technical, tebuconazole technical, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane, urea The weight ratio is 1.00～1.06:3.010～3.126:0.3～0.7:0.1～0.4:0.024～0.051:0.11～0.21:0.01～0.04:0.02～0.05:0.3～0.6, and the balance is water.
进一步的，所述吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素的重量比为1.00:3.010:0.3:0.1:0.024:0.11:0.01:0.02:0.3，余量为水。Further, the pyraclostrobin original drug, tebuconazole original drug, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane The weight ratio of oxane to urea is 1.00:3.010:0.3:0.1:0.024:0.11:0.01:0.02:0.3, and the balance is water.
进一步的，所述吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素的重量比为1.02:3.093:0.5:0.2:0.035:0.16:0.02:0.04:0.5，余量为水。Further, the pyraclostrobin original drug, tebuconazole original drug, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane The weight ratio of oxane to urea is 1.02:3.093:0.5:0.2:0.035:0.16:0.02:0.04:0.5, and the balance is water.
进一步的，所述吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素的重量比为1.06:3.126:0.7:0.4:0.051:0.21:0.04:0.05:0.6，余量为水。Further, the pyraclostrobin original drug, tebuconazole original drug, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane The weight ratio of oxane to urea is 1.06:3.126:0.7:0.4:0.051:0.21:0.04:0.05:0.6, and the balance is water.
进一步的，所述吡唑醚菌酯原药中，Further, in the original drug of pyraclostrobin,
吡唑醚菌酯质量分数≥97.5％；Mass fraction of pyraclostrobin ≥97.5%;
硫酸二甲酯质量分数≤3mg/kg；Dimethyl sulfate mass fraction ≤3mg/kg;
水分质量分数≤0.5％；Moisture mass fraction ≤ 0.5%;
丙酮不溶物质量分数≤0.2％；Acetone insoluble matter fraction ≤ 0.2%;
PH范围5.0～8.0。The pH range is 5.0-8.0.
进一步的，所述戊唑醇原药中，Further, in the original drug of tebuconazole,
戊唑醇质量分数≥96.0％；Tebuconazole mass fraction ≥ 96.0%;
水分质量分数≤0.5％；Moisture mass fraction ≤ 0.5%;
丙酮不溶物质量分数≤0.2％；Acetone insoluble matter fraction ≤ 0.2%;
PH范围6.0～9.0。The pH range is 6.0-9.0.
另外，本发明还提出了一种唑醚、戊唑醇悬浮剂的制备方法，包括：In addition, the present invention also proposes a preparation method of azole ether and tebuconazole suspending agent, comprising:
S1、将制备所述悬浮剂的原料按照所述重量比进行计量；S1. Metering the raw materials for preparing the suspending agent according to the weight ratio;
S2、依次向高剪切分散机中加入吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素以及水，得到分散液；S2. Add pyraclostrobin technical substance, tebuconazole technical substance, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, magnesium aluminum silicate and sodium benzoate to the high shear disperser in sequence , polydimethylsiloxane, urea and water to obtain a dispersion;
S3、将分散液加入至砂磨机A中，进行粗研磨，得到粗砂磨液；S3, adding the dispersion liquid to the sand mill A, and performing coarse grinding to obtain a coarse sand grinding liquid;
S4、将粗砂磨液加入至砂磨机B中，进行细研磨，得到细研磨液；S4, adding the coarse grinding liquid to the sand mill B, and performing fine grinding to obtain a fine grinding liquid;
S5、对细研磨液的细度进行检测，合格品灌装、入库。S5. Detect the fineness of the fine abrasive liquid, and fill and store qualified products.
进一步的，所述S2中，高剪切分散机的转速为2800转/分钟，分散时间为20分钟。Further, in S2, the rotational speed of the high-shear disperser is 2800 rpm, and the dispersion time is 20 minutes.
进一步的，所述S3中，砂磨机A的进料速度为300～350kg/h，研磨主轴的转速为20～30转/分钟，砂磨温度＜35℃；Further, in said S3, the feed rate of the sand mill A is 300-350 kg/h, the rotational speed of the grinding spindle is 20-30 rpm, and the sanding temperature is <35°C;
所述S4中，砂磨机B的进料速度为150～200kg/h，研磨主轴的转速为30～40转/分钟，砂磨温度＜35℃。In S4, the feed rate of the sand mill B is 150-200 kg/h, the rotational speed of the grinding spindle is 30-40 rpm, and the sand-milling temperature is <35°C.
进一步的，所述S5中，对于不合格的细研磨液，回到S4的砂磨机B中继续研磨，直至检测合格。Further, in said S5, for the unqualified fine grinding liquid, return to the sand mill B of S4 and continue grinding until the detection is qualified.
本发明提供了一种唑醚、戊唑醇悬浮剂及制备方法。与现有技术相比具备以下有益效果：The invention provides an azole ether and tebuconazole suspending agent and a preparation method. Compared with the prior art, it has the following beneficial effects:
能够有效的对小麦赤霉病进行防治，并且施加后，药物在小麦中的残留量极低，秸秆和小麦在后续被人畜食用时不存在安全隐患，安全间隔期适中。It can effectively prevent and control wheat scab, and after application, the drug residue in wheat is extremely low, and there is no potential safety hazard when straw and wheat are subsequently eaten by humans and animals, and the safety interval is moderate.
具体实施方式Detailed ways
下面，通过具体实施例对本发明的技术方案进行详细说明，但是应该明确提出这些实施例用于举例说明，但是不解释为限制本发明的范围。In the following, the technical solution of the present invention will be described in detail through specific examples, but these examples should be clearly set forth for illustration, but should not be construed as limiting the scope of the present invention.
实施例1Example 1
一种唑醚、戊唑醇悬浮剂，由如下重量比制得：吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素的重量比为1.00:3.010:0.3:0.1:0.024:0.11:0.01:0.02:0.3，余量为水；A suspending agent of azole ether and tebuconazole is prepared by the following weight ratio: pyraclostrobin technical substance, tebuconazole technical substance, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, The weight ratio of magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane, and urea is 1.00:3.010:0.3:0.1:0.024:0.11:0.01:0.02:0.3, and the balance is water;
其中，在吡唑醚菌酯原药中，Among them, in pyraclostrobin active drug,
吡唑醚菌酯质量分数为97.5％；The mass fraction of pyraclostrobin is 97.5%;
硫酸二甲酯质量分数为1.8mg/kg；The mass fraction of dimethyl sulfate is 1.8mg/kg;
水分质量分数为0.5％；Moisture mass fraction is 0.5%;
丙酮不溶物质量分数为0.2％；Acetone insoluble matter fraction is 0.2%;
PH为5.0。The pH is 5.0.
在戊唑醇原药中，In the original drug of tebuconazole,
戊唑醇质量分数为99.3％；Tebuconazole mass fraction is 99.3%;
水分质量分数为0.5％；Moisture mass fraction is 0.5%;
丙酮不溶物质量分数为0.2％；Acetone insoluble matter fraction is 0.2%;
PH为6.0。The pH is 6.0.
上述唑醚、戊唑醇悬浮剂的制备方法，包括：The preparation method of above-mentioned azole ether, tebuconazole suspending agent, comprises:
S1、将吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素、水按照所述重量比进行计量；S1, pyraclostrobin technical, tebuconazole technical, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane , urea, and water are metered according to the weight ratio;
S2、依次向高剪切分散机中加入吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素以及水，得到分散液，高剪切分散机的转速为2800转/分钟，分散时间为20分钟；S2. Add pyraclostrobin technical substance, tebuconazole technical substance, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, magnesium aluminum silicate and sodium benzoate to the high shear disperser in sequence , polydimethylsiloxane, urea and water to obtain a dispersion, the speed of the high-shear disperser is 2800 rpm, and the dispersion time is 20 minutes;
S3、将分散液加入至砂磨机A中，进行粗研磨，得到粗砂磨液，砂磨机A的进料速度为300kg/h，研磨主轴的转速为20转/分钟，砂磨温度＜35℃，防止物料膏化；S3. Add the dispersion liquid to the sand mill A for rough grinding to obtain a coarse sand grinding liquid. The feed rate of the sand mill A is 300kg/h, the rotating speed of the grinding spindle is 20 rpm, and the sand mill temperature < 35 ℃, to prevent the material from creaming;
S4、将粗砂磨液加入至砂磨机B中，进行细研磨，得到细研磨液，砂磨机B的进料速度为150kg/h，研磨主轴的转速为30转/分钟，砂磨温度＜35℃，防止物料膏化；S4, adding the coarse sand grinding liquid into the sand mill B, and finely grinding to obtain the fine grinding liquid, the feeding speed of the sand mill B is 150kg/h, the rotating speed of the grinding spindle is 30 revs/min, and the sand grinding temperature <35°C, prevent material from creaming;
S5、对细研磨液的细度进行检测，合格品灌装、入库，对于不合格的细研磨液，回到S4的砂磨机B中继续研磨，直至检测合格。S5. Detect the fineness of the fine abrasive liquid, fill and store qualified products, and return to the sand mill B in S4 to continue grinding for unqualified fine abrasive liquid until it passes the test.
实施例2Example 2
一种唑醚、戊唑醇悬浮剂，由如下重量比制得：吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素的重量比为1.02:3.093:0.5:0.2:0.035:0.16:0.02:0.04:0.5，余量为水。A suspending agent of azole ether and tebuconazole is prepared by the following weight ratio: pyraclostrobin technical substance, tebuconazole technical substance, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, The weight ratio of magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane and urea is 1.02:3.093:0.5:0.2:0.035:0.16:0.02:0.04:0.5, and the balance is water.
其中，在吡唑醚菌酯原药中，Among them, in pyraclostrobin active drug,
吡唑醚菌酯质量分数为98.3％；The mass fraction of pyraclostrobin is 98.3%;
硫酸二甲酯质量分数为1.2mg/kg；The mass fraction of dimethyl sulfate is 1.2mg/kg;
水分质量分数为0.3％；Moisture mass fraction is 0.3%;
丙酮不溶物质量分数为0.2％；Acetone insoluble matter fraction is 0.2%;
PH为6.5。The pH is 6.5.
在戊唑醇原药中，In the original drug of tebuconazole,
戊唑醇质量分数为99.5％；Tebuconazole mass fraction is 99.5%;
水分质量分数为0.3％；Moisture mass fraction is 0.3%;
丙酮不溶物质量分数为0.2％；Acetone insoluble matter fraction is 0.2%;
PH为7.5。The pH is 7.5.
上述唑醚、戊唑醇悬浮剂的制备方法，包括：The preparation method of above-mentioned azole ether, tebuconazole suspending agent, comprises:
S1、将吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素、水按照所述重量比进行计量；S1, pyraclostrobin technical, tebuconazole technical, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane , urea, and water are metered according to the weight ratio;
S2、依次向高剪切分散机中加入吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素以及水，得到分散液，高剪切分散机的转速为2800转/分钟，分散时间为20分钟；S2. Add pyraclostrobin technical substance, tebuconazole technical substance, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, magnesium aluminum silicate and sodium benzoate to the high shear disperser in sequence , polydimethylsiloxane, urea and water to obtain a dispersion, the speed of the high-shear disperser is 2800 rpm, and the dispersion time is 20 minutes;
S3、将分散液加入至砂磨机A中，进行粗研磨，得到粗砂磨液，砂磨机A的进料速度为320kg/h，研磨主轴的转速为25转/分钟，砂磨温度＜35℃；S3. Add the dispersion liquid to the sand mill A for rough grinding to obtain a coarse sand grinding liquid. The feed rate of the sand mill A is 320kg/h, the rotating speed of the grinding spindle is 25 rpm, and the sand mill temperature < 35°C;
S4、将粗砂磨液加入至砂磨机B中，进行细研磨，得到细研磨液，砂磨机B的进料速度为180kg/h，研磨主轴的转速为35转/分钟，砂磨温度＜35℃；S4, adding the coarse sand grinding liquid to the sand mill B, and finely grinding to obtain the fine grinding liquid, the feeding speed of the sand mill B is 180kg/h, the rotating speed of the grinding spindle is 35 rpm, and the sand grinding temperature <35°C;
S5、对细研磨液的细度进行检测，合格品灌装、入库，对于不合格的细研磨液，回到S4的砂磨机B中继续研磨，直至检测合格。S5. Detect the fineness of the fine abrasive liquid, fill and store qualified products, and return to the sand mill B in S4 to continue grinding for unqualified fine abrasive liquid until it passes the test.
实施例3Example 3
一种唑醚、戊唑醇悬浮剂，由如下重量比制得：吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素的重量比为1.06:3.126:0.7:0.4:0.051:0.21:0.04:0.05:0.6，余量为水。A suspending agent of azole ether and tebuconazole is prepared by the following weight ratio: pyraclostrobin technical substance, tebuconazole technical substance, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, The weight ratio of magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane and urea is 1.06:3.126:0.7:0.4:0.051:0.21:0.04:0.05:0.6, and the balance is water.
其中，在吡唑醚菌酯原药中，Among them, in pyraclostrobin active drug,
吡唑醚菌酯质量分数为99.7％；The mass fraction of pyraclostrobin is 99.7%;
硫酸二甲酯质量分数为0.1mg/kg；The mass fraction of dimethyl sulfate is 0.1mg/kg;
水分质量分数为0.1％；Moisture mass fraction is 0.1%;
丙酮不溶物质量分数为0.1％；Acetone insoluble matter fraction is 0.1%;
PH为8.0。The pH is 8.0.
在戊唑醇原药中，In the original drug of tebuconazole,
戊唑醇质量分数为99.7％；Tebuconazole mass fraction is 99.7%;
水分质量分数为0.2％；Moisture mass fraction is 0.2%;
丙酮不溶物质量分数为0.1％；Acetone insoluble matter fraction is 0.1%;
PH为9.0。The pH is 9.0.
上述唑醚、戊唑醇悬浮剂的制备方法，包括：The preparation method of above-mentioned azole ether, tebuconazole suspending agent, comprises:
S1、将吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素、水按照所述重量比进行计量；S1, pyraclostrobin technical, tebuconazole technical, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, magnesium aluminum silicate, sodium benzoate, polydimethylsiloxane , urea, and water are metered according to the weight ratio;
S2、依次向高剪切分散机中加入吡唑醚菌酯原药、戊唑醇原药、morwet D-425、十二烷基苯磺酸钠、黄原胶、硅酸镁铝、苯甲酸钠、聚二甲基硅氧烷、尿素以及水，得到分散液，高剪切分散机的转速为2800转/分钟，分散时间为20分钟；S2. Add pyraclostrobin technical substance, tebuconazole technical substance, morwet D-425, sodium dodecylbenzenesulfonate, xanthan gum, magnesium aluminum silicate and sodium benzoate to the high shear disperser in sequence , polydimethylsiloxane, urea and water to obtain a dispersion, the speed of the high-shear disperser is 2800 rpm, and the dispersion time is 20 minutes;
S3、将分散液加入至砂磨机A中，进行粗研磨，得到粗砂磨液，砂磨机A的进料速度为350kg/h，研磨主轴的转速为30转/分钟，砂磨温度＜35℃；S3. Add the dispersion liquid to the sand mill A for rough grinding to obtain a coarse sand grinding liquid. The feed rate of the sand mill A is 350kg/h, the rotating speed of the grinding spindle is 30 rpm, and the sand mill temperature < 35°C;
S4、将粗砂磨液加入至砂磨机B中，进行细研磨，得到细研磨液，砂磨机B的进料速度为200kg/h，研磨主轴的转速为40转/分钟，砂磨温度＜35℃；S4, adding the coarse sand grinding liquid into the sand mill B, and finely grinding to obtain the fine grinding liquid, the feeding speed of the sand mill B is 200kg/h, the rotating speed of the grinding spindle is 40 rpm, and the sand grinding temperature <35°C;
S5、对细研磨液的细度进行检测，合格品灌装、入库，对于不合格的细研磨液，回到S4的砂磨机B中继续研磨，直至检测合格。S5. Detect the fineness of the fine abrasive liquid, fill and store qualified products, and return to the sand mill B in S4 to continue grinding for unqualified fine abrasive liquid until it passes the test.
经过实施例1、2、3所制得的唑醚、戊唑醇悬浮剂，理化性质如下表所示：The physical and chemical properties of the azole ethers and tebuconazole suspensions prepared in Examples 1, 2, and 3 are shown in the following table:
药效试验结果Drug efficacy test results
我公司40％吡唑醚菌酯、戊唑醇悬浮剂，用于防治小麦赤霉病，推Our company's 40% pyraclostrobin and tebuconazole suspension concentrate are used to prevent and control wheat scab.
荐有效成分用药量120～150克/公顷。试验结果见下表：The recommended dosage of active ingredients is 120-150 g/ha. The test results are shown in the table below:
药物残留结果drug residue results
我公司产品40％吡唑醚菌酯·戊唑醇悬浮剂，用于防治小麦赤霉病，施药方法：喷雾，委托某研究所进行残留试验，该40％吡唑醚菌酯·戊唑醇悬浮剂在小麦上最大残留量为0.05mg/kg，40％吡唑醚菌酯·戊唑醇悬浮剂，防治小麦赤霉病，最高制剂用药量为25克/平亩，采用喷雾的方式于小麦赤霉病发病初期施药1次，安全间隔期可设定为28天。Our company's product 40% pyraclostrobin tebuconazole suspension concentrate is used to prevent and control wheat scab. Application method: spraying, and a research institute is entrusted to carry out the residue test. The 40% pyraclostrobin tebuconazole The maximum residual amount of alcohol suspension on wheat is 0.05mg/kg. 40% pyraclostrobin tebuconazole suspension can prevent and control wheat scab. Apply once at the early stage of wheat scab, and the safety interval can be set at 28 days.
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