CN105432606B - Composition containing benziothiazolinone and preparing method thereof - Google Patents

Composition containing benziothiazolinone and preparing method thereof Download PDF

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Publication number
CN105432606B
CN105432606B CN201510881173.3A CN201510881173A CN105432606B CN 105432606 B CN105432606 B CN 105432606B CN 201510881173 A CN201510881173 A CN 201510881173A CN 105432606 B CN105432606 B CN 105432606B
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China
Prior art keywords
benziothiazolinone
microemulsion
composition containing
preparing method
wettable powder
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CN201510881173.3A
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CN105432606A (en
Inventor
王鹏
吴泽和
崔继承
段新新
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HUATE WESTERN SHAANXI SCIENCE AND TECHNOLOGY INDUSTRIAL Co Ltd
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HUATE WESTERN SHAANXI SCIENCE AND TECHNOLOGY INDUSTRIAL Co Ltd
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Priority to CN201611078467.3A priority Critical patent/CN106818723A/en
Priority to CN201510881173.3A priority patent/CN105432606B/en
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, 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
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72Biocides, 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
    • A01N43/80Biocides, 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 one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2

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

Abstract

The invention relates to a composition containing benziothiazolinone and a preparing method thereof. The composition is microemulsion with benziothiazolinone as the active material. The microemulsion contains benziothiazolinone, an emulgator, an organic solvent, a cosolvent, an antifreezing agent, a penetrant and softened water. A benziothiazolinone microemulsion (ME) and benziothiazolinone wettable powder (WP) indoor toxicity contrast test proves that the efficacy of the ME is obviously higher than that of the WP.

Description

Composition containing benziothiazolinone and preparation method thereof
Background technology
The invention belongs to formulations of pesticide field, it is related to pesticide new product benziothiazolinone microemulsion and preparation method thereof.
Background technology
Benziothiazolinone(Benziothiazolinone)Belong to isothiazole heterocyclic compound, be a kind of efficiently, low toxicity, broad spectrum activity kill Microbial inoculum, its mechanism of action is:With bacterium, the anion binding of the surface of cell membrane of mould or react with sulfydryl, destroy protein With the synthesis system of cell membrane, thus suppressing bacterium, mould breeding, interference pathogen cell metabolism so as to physiologic derangement, Lead to pathogen dead.The benziothiazolinone of Shaanxi Xida Huate Science & Technology Industrial Co., Ltd.'s development and production obtains agriculture radical for 2008 Family's agricultural chemicals formal registration, and wide popularization and application.This compound has good preventing and treating effect to bacterium, fungus-caused corps diseases Really, and fool proof to crops.At present, the formulation of benziothiazolinone generally pulvis, wettable powder, suspending agent, moisture dissipates Granula.
Content of the invention
It is an object of the invention to provide a kind of composition containing benziothiazolinone, to provide a kind of novel form to benziothiazolinone.For this reason, The present invention employs the following technical solutions:
Composition containing benziothiazolinone is it is characterised in that it is the microemulsion with benziothiazolinone as active material.
Further, 2-8% containing benziothiazolinone in described combination, by mass percentage.
Further, described microemulsion comprises following component and content range, by mass percentage:
Benziothiazolinone 2-8%;
Organic solvent 15-30%;
Cosolvent 6-15%;
Emulsifying agent 10-25%;
Antifreezing agent 3-5%;
Bleeding agent 1-3%;
Softened water complements to 100%.
Further, in described microemulsion, emulsifying agent is selected from nonionic surfactant and anion surfactant One or more, nonionic surfactant is selected from APES, APES phosphate, alkyl phenol APEO formaldehyde condensation products, benzylbiphenyl phenol polyethenoxy ether;Anion surfactant be selected from alkylbenzenesulfonate, C8- 20 sodium alkyl sulfates, styrene polyoxyethylene ether ammonium sulfate salt;It is preferably nonionic surfactant and anionic surface The mixture of activating agent.
Further, in described microemulsion, organic solvent is selected from water miscible cyclohexanone, cyclohexanol, dimethylformamide; Cosolvent is selected from water miscible methyl alcohol, ethanol, isopropanol.
Further, in described microemulsion, antifreezing agent is selected from ethylene glycol, propane diols, glycerine;Bleeding agent is selected from laruyl alcohol Ether sodium sulfate, JFC, sodium lignin sulfonate.
The processing technology of microemulsion:First in the dissolution kettle with agitating device, benziothiazolinone is dissolved in organic solvent and helps In the mixed liquor of solvent, this solution is put in the emulsifying kettle with high shear machine, then sequentially adds antifreezing agent, bleeding agent, breast Agent after softening water, to 100%, start high-shear impeller stirring 30-50 minute, be obtained meet mark Cui benziothiazolinone micro- Emulsion, through carrying out after the assay was approved packing, putting in storage.
The benziothiazolinone microemulsion that the present invention provides(M i c r o e m u l s i o n)It is with water as matrix, few use Organic solvent(As far as possible without benzene class organic solvent)Environmental protection type agricultural chemical novel formulation.Using physicochemical liquid-liquid dispersion system The polymolecularity emulsion that theoretical and method is prepared, its oil, globule particle diameter are 10-100nm.
The experiment proved that, the drug effect 10%-30% higher than missible oil of benziothiazolinone microemulsion of the present invention, with wettable powder phase Relatively, drug effect improves significantly, belongs to efficient, low and stains, stores and transports safe benziothiazolinone novel form.
Specific embodiment
Embodiment prepared by benziothiazolinone microemulsion
Present invention following examples illustrate, but do not limit the present invention.
Preparation embodiment one:3% benziothiazolinone microemulsion
Benziothiazolinone 3%
Cyclohexanone 20%
Ethanol 9%
APES 8%
Sodium alkyl benzene sulfonate 7%
Ethylene glycol 5%
JFC 2%
Softened water complements to 100%
First in the dissolution kettle with agitating device, benziothiazolinone is dissolved in cyclohexanone and the mixed liquor of ethanol, then will This solution is put in the emulsifying kettle with high shear machine, sequentially adds ethylene glycol, JFC, APES, alkyl benzene sulphonate Sodium and softened water, start high-shear impeller stirring 30-50 minute, are obtained and meet standard 3% benziothiazolinone microemulsion, through inspection Test qualified after carry out packing, put in storage.
Benziothiazolinone microemulsion manufactured in the present embodiment is taken to carry out physicochemical property test, result is as follows:
Outward appearance:As clear as crystal single-phase liquid;
Transparency temperature region:- 5 spend to more than 60 degree;
Low-temperature stability:Occur without layering under -5 degree within 2 weeks, crystallization;
Thermodynamic stability:?(54=2)Lower 2 weeks active ingredient resolution ratios of degree are less than 3%;
Stability of emulsion:Water-reducible emulsion-stabilizing in any proportion;
Ageing stability:Stable under normal temperature.
Preparation embodiment two:8% benziothiazolinone microemulsion
Benziothiazolinone 8%
Cyclohexanone 15%
Ring alcohol 10%
Dimethylformamide 15%
APES phosphate 12%
Lauryl sodium sulfate 8%
Propane diols 5%
Sodium laureth sulfate 3%
Softened water complements to 100%
First in the dissolution kettle with agitating device, benziothiazolinone is dissolved in cyclohexanone, ring alcohol and dimethylformamide In mixed liquor, then this solution is put in the mixing emulsifying kettle with high shear machine, sequentially add addition propane diols, lauryl alcohol Sodium sulphate, APES phosphate, lauryl sodium sulfate and softened water, start high-shear impeller stirring 30- 50 minutes, standard compliant 8% benziothiazolinone microemulsion is obtained, through carrying out after the assay was approved packing, putting in storage.
Benziothiazolinone microemulsion manufactured in the present embodiment is taken to carry out physicochemical property test, result is as follows:
Outward appearance:As clear as crystal single-phase liquid;
Transparency temperature region:- 5 spend to more than 60 degree;
Low-temperature stability:Occur without layering under -5 degree within 2 weeks, crystallization;
Thermodynamic stability:?(54=2)Lower 2 weeks active ingredient resolution ratios of degree are less than 3%;
Stability of emulsion:Water-reducible emulsion-stabilizing in any proportion;
Ageing stability:Stable under normal temperature.
Benziothiazolinone microemulsion indoor biometricses embodiment
Test is carried out with reference to < agricultural chemicals room bioassay test criterion bactericide >.
Calculate mycelial growth inhibition rate by mycelium morphology factor test measurements, then calculated by virulence regression equation y=a+bX Go out the EC of every kind of medicament50, relative virus force index is calculated according to Wadlcy method simultaneously.
Raw embodiment one 3% benziothiazolinone microemulsion of surveying, to cucumber bacterial angular leaf spot Toxicity Determination, the results are shown in Table 1, wherein WP represents wettable powder, and ME represents microemulsion
Table 1 3% benziothiazolinone microemulsion is to cucumber bacterial angular leaf spot Toxicity Determination
Reagent agent Virulence regression equation y=a+bX EC50(Mg/L) Coefficient correlation Relative virus force index
3% benziothiazolinone WP Y=3.371+1.424X 0.716 0.9930
3% benziothiazolinone ME Y=3.309+1.535X 0.375 0.9973 1.91
It is stronger that table 1 result shows that benziothiazolinone microemulsion and benziothiazolinone wettable powder all have to cucumber bacterial angular leaf spot germ Inhibitory activity, its toxicity index microemulsion is 1.91 times of wettable powder, and microemulsion drug effect is substantially better than wettable powder.
Raw embodiment 2 3% benziothiazolinone microemulsion of surveying, to pear scab Toxicity Determination, the results are shown in Table 2
Table 2 3% benziothiazolinone microemulsion is to scab Toxicity Determination
Reagent agent Virulence regression equation y=a+bX EC50(Mg/L) Coefficient correlation Relative virus force index
3% benziothiazolinone WP Y=4.227+0.638X 0.487 0.9792
3% benziothiazolinone ME Y=4.498+0.500X 0.272 0.9842 1.79
Table 2 result shows that benziothiazolinone microemulsion and benziothiazolinone wettable powder all have to pear scab germ and lives compared with high inhibition Property, its toxicity index microemulsion is 1.79 times of wettable powder, and microemulsion drug effect is substantially better than wettable powder.

Claims (2)

1. contain the composition of benziothiazolinone it is characterised in that it is the microemulsion with benziothiazolinone as active material;
Described microemulsion comprises following component and content range, by mass percentage:
2. contain the composition of benziothiazolinone it is characterised in that it is the microemulsion with benziothiazolinone as active material, described microemulsion bag Containing following component and content range, by mass percentage:
CN201510881173.3A 2015-12-04 2015-12-04 Composition containing benziothiazolinone and preparing method thereof Active CN105432606B (en)

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CN106305779A (en) * 2016-08-22 2017-01-11 陕西西大华特科技实业有限公司 Microbicide composition containing benziothiazolinone and copper hydroxide and applications thereof
CN107306972A (en) * 2017-06-13 2017-11-03 中国农业科学院植物保护研究所 Thymol and combinations thereof

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JPH02268199A (en) * 1989-04-07 1990-11-01 Ichikawa Gosei Kagaku Kk Novel cyclic peptide, its production, intermediate therefor and metal cluster complex
CN101669486B (en) * 2009-10-16 2012-06-06 深圳诺普信农化股份有限公司 Benzolkresoxim-methyl containing bactericide composition
CN102224818B (en) * 2011-04-22 2013-04-17 河北工程大学 Benziothiazolinone nanoemulsion and preparation method thereof
CN102763657B (en) * 2012-08-13 2014-09-17 江苏辉丰农化股份有限公司 Germicide composite with synergistic effect
CN103329921B (en) * 2013-06-09 2015-01-28 江苏辉丰农化股份有限公司 Benziothiazolinone-containing sterilization composite
CN104488906B (en) * 2014-12-18 2016-10-05 广西田园生化股份有限公司 A kind of containing methylsulfonyl bacterium azoles and the complex composition of benziothiazolinone and antibacterial

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