WO2008151513A1 - Concentré de suspension de thiodiazole de zn et sa préparation - Google Patents

Concentré de suspension de thiodiazole de zn et sa préparation Download PDF

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Publication number
WO2008151513A1
WO2008151513A1 PCT/CN2008/001100 CN2008001100W WO2008151513A1 WO 2008151513 A1 WO2008151513 A1 WO 2008151513A1 CN 2008001100 W CN2008001100 W CN 2008001100W WO 2008151513 A1 WO2008151513 A1 WO 2008151513A1
Authority
WO
WIPO (PCT)
Prior art keywords
zinc
thiazole
agent
sodium
suspending agent
Prior art date
Application number
PCT/CN2008/001100
Other languages
English (en)
Chinese (zh)
Inventor
Fanglin Wei
Guonian Zhu
Qunhui Xu
Zhenyuan Xu
Danqian Xu
Jingui Dai
Xianming Tong
Original Assignee
Zhejiang Xinnong Chemical Co., Ltd.
The Institute Of Pesticide And Environmental Toxicology, Zhejiang University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Zhejiang Xinnong Chemical Co., Ltd., The Institute Of Pesticide And Environmental Toxicology, Zhejiang University filed Critical Zhejiang Xinnong Chemical Co., Ltd.
Priority to BRPI0811361-0A2A priority Critical patent/BRPI0811361A2/pt
Priority to AU2008261509A priority patent/AU2008261509C1/en
Publication of WO2008151513A1 publication Critical patent/WO2008151513A1/fr
Priority to EG2009121791A priority patent/EG26147A/en

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D285/00—Heterocyclic compounds containing rings having nitrogen and sulfur atoms as the only ring hetero atoms, not provided for by groups C07D275/00 - C07D283/00
    • C07D285/01—Five-membered rings
    • C07D285/02—Thiadiazoles; Hydrogenated thiadiazoles
    • C07D285/04—Thiadiazoles; Hydrogenated thiadiazoles not condensed with other rings
    • C07D285/12—1,3,4-Thiadiazoles; Hydrogenated 1,3,4-thiadiazoles
    • C07D285/125—1,3,4-Thiadiazoles; Hydrogenated 1,3,4-thiadiazoles with oxygen, sulfur or nitrogen atoms, directly attached to ring carbon atoms, the nitrogen atoms not forming part of a nitro radical
    • 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
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/82—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms

Definitions

  • the invention relates to a bactericide, in particular to a thiazole zinc suspension agent and a preparation method thereof.
  • Background technique :
  • An aqueous suspension concentrate also known as an aqueous suspension, a suspension, or a suspension concentrate, is a solid raw drug that is insoluble or poorly soluble in water by means of a dispersant, a wetting agent, etc.
  • a pesticide dosage form that uses an input energy dispersed in water to form a uniform and stable suspension system is an important type of agent representing the development direction of modern pesticide preparation technology.
  • Suspending agents are mainly composed of pesticides, wetting agents, dispersing agents, thickeners, antifreeze agents, preservatives, pH adjusters, defoamers and water.
  • the suspending agent Since the dispersing medium is water, the suspending agent has the characteristics of low cost, safety in production, storage, transportation and use, and can be mixed with water in any proportion, is not affected by water quality and temperature, and is convenient to use. Compared with the pesticide formulation with organic solvent as the medium, it has the advantages of less environmental impact and lighter phytotoxicity; compared with the wettable powder, it has the advantages of no dust pollution and convenient use.
  • Zn Thiodiazole bis(2-amino-1,3,4-thiadiazole-5-thiol) zinc, which is a new innovation developed by Zhejiang Xinnong Chemical Co., Ltd.
  • Pesticide is a new generation of high-efficiency, low-toxic organic zinc agricultural fungicide for controlling bacterial diseases of crops, and has obtained national invention patent (ZL00132119.6).
  • the development of zinc thiazole into a suspension will make this self-created new pesticide a highly efficient, safe and economical green pesticide preparation, laying the foundation for a good market prospect.
  • Thiazole zinc can effectively prevent bacterial diseases such as bacterial blight, bacterial stripe disease and citrus canker.
  • Rice bacterial blight often occurs in Zhejiang, Jiangxi, Guangdong, Guangxi, Sichuan, Hunan, Hubei, Hainan, Yunnan, Guizhou, Anhui, Jiangsu and other provinces (regions), with an annual area of more than 90 million mu; bacterial stripe disease It often occurs in Zhejiang, Jiangxi, Fujian, Guangdong, Guangxi, Hunan, Hainan, Yunnan and other provinces (districts), with an annual occurrence of 7,000-80 million mu; citrus canker disease occurs in Zhejiang, Fujian, Jiangxi, Guangdong, Guangxi, Sichuan and Yunnan provinces (districts) have an annual area of more than 10 million mu.
  • suspending agents involves many disciplines such as pesticide chemistry, pesticide formulation, physical chemistry, chemical machinery, etc.
  • the research and preparation techniques are more complicated.
  • Suspension agents have emerged in the 1970s, but due to the development of technologies such as grinding machinery and surfactants, the scale of their promotion is still difficult to compare with bulk formulations such as emulsifiable concentrates and wettable powders.
  • the currently developed varieties, especially the domestically produced suspension products have poor physical stability, delamination and sedimentation during storage, and it is difficult to uniformly disperse the active ingredients of the pesticides, and even the agglomerates cannot be poured out of the package, which is not easy in water. Dispersion and low suspension rate seriously affect the promotion and use of suspension agent, a new pesticide formulation, in agricultural production.
  • the present invention aims to solve the above-mentioned technical problems, and provides a highly effective and drug-resistant control of rice bacterial blight, which can avoid dust pollution, reduce production cost, and has better physical stability, dispersibility, and suspension rate.
  • Bacterial diseases such as bacterial stripe disease and citrus canker, thiazole zinc suspension agent and preparation method thereof.
  • the present invention provides a zinc thiazole suspension containing 5-60% by weight of the active ingredient thiazole zinc.
  • weight percentage is further included as follows: wetter 2-8%, dispersant 2-5%, thickener 0-3%, antifreeze 0-5%, preservative 0-0.5%, defoaming Agent 0-0.5% and water balance.
  • the wetting agent is selected from the group consisting of EO/PO block polyether, fatty alcohol polyoxyethylene ether, fatty alcohol ethoxylate, tallow ethoxylated amine salt, alkylnaphthalene sulfonate, fatty alcohol polyoxyethylene Ether sulfate, acyl glutamate.
  • the dispersing agent is selected from the group consisting of sodium naphthalenesulfonic acid condensate, sodium phenolsulfonic acid condensate, and methylnaphthalenesulfonic acid Sodium formaldehyde condensate, sodium lignosulfonate, sodium methylene dinaphthalene sulfonate, sodium homopolymer of sodium acrylate, high molecular polycarboxylate, sodium dioctyl sulfosuccinate, EO/PO block Ether, maleic acid-acrylic acid copolymer sodium salt.
  • the thickening agent is selected from the group consisting of xanthan gum, magnesium aluminum silicate, sodium carboxymethylcellulose, sodium starch phosphate, sodium starch octenyl succinate, polyvinyl alcohol.
  • the antifreeze is selected from the group consisting of ethylene glycol, propylene glycol, glycerol, isopropanol, and urea.
  • the preservative is selected from the group consisting of formaldehyde, phenyl salicylate, butyl p-hydroxybenzoate, and potassium sorbate.
  • the antifoaming agent is selected from the group consisting of silicone defoamers and polyether defoamers.
  • the water is deionized water or distilled water.
  • the invention further provides a preparation method of a zinc thiazole suspension agent, which adopts the following process steps: the raw materials are weighed according to the foregoing weight ratio, and the raw materials are sanded and filtered to remove the sanding medium or homogenized by a high pressure homogenizer to obtain Thiazole zinc suspending agent.
  • the raw material is sanded in a sand mill for 30-120 minutes, and the thiazole zinc suspension is obtained after filtering and removing the sanding medium.
  • the process further comprises: putting the raw material into a high-shear homogenizing emulsifier for high-speed shearing for 20-30 minutes, then pumping it into the sanding machine, sanding for 30-90 minutes, or circulating sanding for 1-3 times, filtering After removing the sanding medium, the thiazole zinc suspension agent is obtained; or the unmilled shear material is pumped into the high pressure homogenizer to obtain the thiazole zinc suspension agent after high pressure homogenization.
  • the thiazole zinc is a solid substance, insoluble in water, and must be suspended in water by means of additives such as dispersing agents and wetting agents. However, the following factors may cause poor physical stability of the thiazole zinc suspending agent:
  • Ostwald ripening that is, in a broadly distributed polydisperse system, small particles will gradually dissolve and become smaller in the aqueous medium over time, while large-sized particles will gradually decrease. Become bigger
  • the thiazol zinc suspending agent can be prevented from coalescence during storage, the particle size and distribution of the dispersed particles remain unchanged, and the dispersed phase particles can be stably Suspended in a dispersion medium without sedimentation.
  • the thiazole zinc suspension gram preparation provided by the invention has the advantages of uniform milky white, good fluidity, good dispersibility, high suspension rate, good physical stability of cold and heat storage, and good physical stability after two years of storage.
  • the thiazole zinc suspension preparation prepared according to the method provided by the invention has uniform whiteness, easy flow, excellent dispersibility and a suspension ratio of >98%. After heat storage at 54 ⁇ 1 °C for two weeks, the decomposition rate of thiazole zinc was less than 5%, and the appearance of the preparation remained uniform after storage, and the suspension rate was >95%. Cold storage at 0 ⁇ 1 °C for 7 days The appearance of the preparation remained uniform and preferred fluidity. After two years of storage, the water separation rate is ⁇ 5%, the dispersion is good, and the suspension rate is >95%.
  • the invention provides a thiazole zinc suspension agent and a preparation method thereof, which have the following advantages compared with the prior art:
  • the green thiazole zinc suspending agent provided by the invention has no phytotoxicity after being tested on the peach tree, and the control effect is ideal to effectively solve the problem of preventing bacterial diseases on peach, plum, apricot and plum crops.
  • the blank used in the fungicide provides an effective control agent. It not only provides new pesticide varieties for effectively controlling bacterial diseases of rice, citrus, peach, plum and other crops, but also creates significant economic and social benefits, and is of great significance for adjusting the structure of pesticide products and promoting technological advancement in the industry.
  • the thiazole zinc suspension agent provided by the present invention and its details are described in detail below with reference to specific examples.
  • the present invention is intended to be illustrative of the present invention, and is not intended to limit the scope of the present invention. All modifications and variations based on the basic idea of the invention are intended to fall within the scope of the invention.
  • thiazole zinc 2.0% of alkylnaphthalene sulfonate, 1.3% of fatty alcohol polyoxyethylene ether sulfate, 1.0% of sodium phenolsulfonate condensate, 2.0% of methyl naphthalenesulfonate formaldehyde condensate, carboxymethyl Base cellulose sodium 2.0%, ethylene glycol 2.0%, butyl p-hydroxybenzoate 0.2%, silicone defoamer 0.1%, deionized water to 100%, put into high shear homogenizer high speed shear After cutting for 25 minutes, it was pumped to a sand mill for 90 minutes, and after filtration, a 20% thiazole zinc suspension was obtained.
  • thiazole zinc 4.0% of fatty alcohol ethyloxide, 1.0% of EO/PO block polyether, 4.0% of high molecular polycarboxylate, 0.2% of formaldehyde, 0.5% of polyvinyl alcohol, 2.0% of isopropanol, Deionized water was added to 100%, and it was put into a high shear homogenizer for high-speed shearing for 30 minutes, and then transferred to a sand mill. After circulating sanding for 1-3 times, 40% thiazole zinc suspension was obtained.
  • thiazole zinc 50.0% of thiazole zinc, 3.0% of fatty alcohol polyoxyethylene ether sulfate, 1.0% of tallow ethoxyamine salt, 2.0% of acyl glutamate, 3.0% of polycarboxylate, sodium sulfonate condensate 1.0% salt, 1.0% dioctyl sulfosuccinate sodium salt, 3.0% urea, 0.4% silicone defoamer, deionized water Add to 100%, put into a high shear homogenizer to shear at high speed for 20 minutes, and then homogenize with a high pressure homogenizer to obtain 50% thiazole zinc suspension.
  • thiazole zinc 3.0% of fatty alcohol ethoxylate, 1.0% of alkylnaphthalenesulfonate, 4.0% of fatty alcohol polyoxyethylene ether sulfate, 3.0% of sodium phenolsulfonate condensate, methylene dinaphthalene Sodium sulfonate 1.5%, sodium methylnaphthalene sulfonate formaldehyde condensate 0.5%, silicone defoamer 0.2%, distilled water added to 100%, put into a high shear homogenizer for high-speed shearing for 30 minutes, and then After homogenization with a high pressure homogenizer, 60% thiazole zinc suspension is obtained.
  • the thiazole zinc suspending agent provided by the invention has good adhesion, spreading and penetrating ability on the surface of the plant.
  • the indoor biological activity of the thiazole zinc suspension by Nanjing Agricultural University showed that the zinc thiazole suspension provided by the invention has good biological activity against rice bacterial blight, and the biological activity is better than that of the leaf blue double.
  • the thiazole suspension agent provided by the present invention has bacterial diseases such as citrus canker, rice bacterial blight, rice bacterial leaf streak and the like. Has a good control effect.
  • the zinc thiazole suspension agent provided by the invention has been proved to be a low-toxic pesticide by the test of Zhejiang Academy of Medical Sciences, and the results are shown in Table 6.
  • the thiazole zinc suspending agent provided by the invention is proved to be environmental biosafety by the Nanjing Institute of Environmental Sciences of the State Environmental Protection Administration. The results are shown in Table 7:

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  • Life Sciences & Earth Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical & Material Sciences (AREA)
  • Dentistry (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Plant Pathology (AREA)
  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

L'invention concerne un concentré de suspension de thiodiazole de Zn et sa préparation. Le concentré de suspension comprend de 5 à 60% de thiodiazole de Zn, de 2 à 8% d'agent de mouillage, de 2 à 5% de dispersant, de 0 à 3% d'agent épaississant, de 0 à 5% d'agent antigel, de 0 à 0,5% d'agent conservateur, de 0 à 0,5% d'agent antimousse et le reste d'eau. Le concentré de suspension peut être préparé par broyage avec un broyeur à sable, par homogénéisation par cisaillement à vitesse élevée combinée avec sablage, ou par homogénéisation par cisaillement à vitesse élevée combinée avec une homogénéisation par pression élevée. Le produit a un fort effet de lutte contre des maladies bactériennes, par exemple, la maladie bactérienne des feuilles du riz, les colonies bactériennes et le chancre bactérien des agrumes. Ses avantages comprennent une faible pollution environnementale, une faible toxicité; une propriété de formulation supérieure telle qu'aucune précipitation ou stratification lors d'un stockage à la température ambiante pendant deux ans, une longue durée de conservation, des propriétés non inflammables et sûres pour le stockage et le transport.
PCT/CN2008/001100 2007-06-08 2008-06-05 Concentré de suspension de thiodiazole de zn et sa préparation WO2008151513A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
BRPI0811361-0A2A BRPI0811361A2 (pt) 2007-06-08 2008-06-05 Suspenção concentrada de tiodiazol-zinco e seu método de preparação
AU2008261509A AU2008261509C1 (en) 2007-06-08 2008-06-05 Suspension concentrate of Zn thiodiazole and preparation thereof
EG2009121791A EG26147A (en) 2007-06-08 2009-12-08 Output of the suspended concentration of ZN thiodiazole and its preparation method

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN200710106183.5 2007-06-08
CN2007101061835A CN101194611B (zh) 2007-06-08 2007-06-08 噻唑锌悬浮剂及其制备方法

Publications (1)

Publication Number Publication Date
WO2008151513A1 true WO2008151513A1 (fr) 2008-12-18

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Application Number Title Priority Date Filing Date
PCT/CN2008/001100 WO2008151513A1 (fr) 2007-06-08 2008-06-05 Concentré de suspension de thiodiazole de zn et sa préparation

Country Status (6)

Country Link
CN (1) CN101194611B (fr)
AU (1) AU2008261509C1 (fr)
BR (1) BRPI0811361A2 (fr)
EG (1) EG26147A (fr)
MY (1) MY157922A (fr)
WO (1) WO2008151513A1 (fr)

Cited By (2)

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CN102783480A (zh) * 2012-07-11 2012-11-21 广东中迅农科股份有限公司 一种苯噻菌胺水悬浮剂及其制备方法
CN104255716A (zh) * 2014-09-02 2015-01-07 浙江龙湾化工有限公司 一种噻菌铜水分散粒剂及其制备方法

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CN101953346B (zh) * 2010-09-15 2011-07-20 浙江新农化工股份有限公司 含噻唑锌的杀菌组合物
CN102524313A (zh) * 2012-01-30 2012-07-04 华南理工大学 氟虫双酰胺与天然除虫菊素复配悬浮剂及其制备方法
CN103070164A (zh) * 2013-02-26 2013-05-01 江苏省苏科农化有限责任公司 一种制备农药悬浮剂的新方法
CN103704221A (zh) * 2013-12-26 2014-04-09 浙江新农化工股份有限公司 一种提高植物产量和品质的方法
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CN105941427B (zh) * 2016-05-20 2018-07-17 南京华洲药业有限公司 一种含螺环菌胺和噻唑锌的杀菌组合物及其应用
CN106172497B (zh) * 2016-06-30 2018-10-30 江苏新农化工有限公司 含噻唑锌和亚磷酸盐的杀菌组合物及其制剂和应用
CN106508919A (zh) * 2016-09-14 2017-03-22 江苏新农化工有限公司 含噻唑锌和辛菌胺醋酸盐的组合物及其制剂和应用
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CN107417640B (zh) * 2017-02-22 2019-03-26 浙江大学 纳米噻唑锌的制备方法
CN109122699B (zh) * 2017-06-16 2021-02-02 浙江新农化工股份有限公司 一种包含噻唑锌颗粒的组合物及其制备方法
CN107372485A (zh) * 2017-07-27 2017-11-24 山东天农新材料发展有限公司 一种高压均质制备农药固体制剂的方法
CN108329281B (zh) * 2018-03-01 2019-09-10 江苏新农化工有限公司 一种优化的噻唑锌制备方法
CN108353914A (zh) * 2018-03-27 2018-08-03 蔡志浩 一种水稻病害防治药物
CN111406754B (zh) * 2020-04-28 2021-06-15 浙江禾本科技股份有限公司 一种噻螨酮水悬浮剂及其制备方法
CN114073250A (zh) * 2020-08-17 2022-02-22 浙江新农化工股份有限公司 一种包含纳米噻唑锌的悬浮剂及其制备方法
CN115812698A (zh) * 2022-08-17 2023-03-21 江苏艾津作物科技集团有限公司 一种用于杀软体动物的喷涂制剂及其制备方法和应用

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CN104255716A (zh) * 2014-09-02 2015-01-07 浙江龙湾化工有限公司 一种噻菌铜水分散粒剂及其制备方法

Also Published As

Publication number Publication date
EG26147A (en) 2013-03-27
AU2008261509C1 (en) 2012-11-01
AU2008261509B2 (en) 2012-03-15
CN101194611A (zh) 2008-06-11
CN101194611B (zh) 2010-06-02
AU2008261509A1 (en) 2008-12-18
MY157922A (en) 2016-08-15
BRPI0811361A2 (pt) 2014-09-30

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