CN101444205A - High-lythidathion content oil emulsion and preparation method thereof - Google Patents
High-lythidathion content oil emulsion and preparation method thereof Download PDFInfo
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- CN101444205A CN101444205A CNA2008102496063A CN200810249606A CN101444205A CN 101444205 A CN101444205 A CN 101444205A CN A2008102496063 A CNA2008102496063 A CN A2008102496063A CN 200810249606 A CN200810249606 A CN 200810249606A CN 101444205 A CN101444205 A CN 101444205A
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Abstract
The invention discloses a high-lythidathion content oil emulsion and a preparation method thereof. The oil emulsion is prepared from (wt%) lythidathion 50-90, oil 0-22, assistants 0-5, solvent 4-20, emulsifying agent 1-12, stabilizer 0.01-1, and essence 0.01-0.1. The oil emulsion has the advantages of good stability, lasting drug action, low environmental pollution, simple and reasonable preparation method, and low production cost.
Description
Technical field
Invention relates to prescription of a kind of high-lythidathion content oil emulsion and preparation method thereof, belongs to field of agrochemicals.Belong to formulations of pesticide manufacture field.
Background technology
Add a large amount of toluene, dimethylbenzene equal solvent in traditional missible oil, increased the inflammable and explosive danger of links such as pesticide producing, storing on the one hand; Increased pollution on the other hand, had a strong impact on existent environment of people environment.
Lythidathion is Japanese Shi Yuan company in June, 1985 stating Patent (clear 60-104096), a kind of novelty of putting on market in 1992, efficient, wide spectrum, the nematocide of safety and the agricultural chemicals that kills soil insect, nematode and soil insect to tobacco, peanut, soybean, citrus, vegetables have extraordinary preventive and therapeutic effect, China obtains one of only several nematocides of registration on vegetables, be specially adapted to the production of pollution-free vegetable.Lythidathion has tags and new and effective, the low toxicity nematode killing agent of interior suction conductive performance, can effectively prevent in the nematode invaded plants body and kills nematode in the invaded plants body, and the lasting period can reach 2～3 months, and application effect is not influenced by soil condition.
On January 1st, 2007 rose, China completely forbids 5 kinds of high-toxic pesticides such as acephatemet, lythidathion should be one of important alternative kind, but the formulation of lythidathion only has granule (10% lythidathion GR at present, People's Republic of China (PRC) agriculture chemical registration card number: LS20020026), and the granular preparation instability of lythidathion, easily decompose, therefore, be subjected to bigger restriction when being applied to agricultural production, far can not satisfy the demand in market.
Summary of the invention
The technical deficiency of formulation at existing lythidathion the invention provides a kind of high-lythidathion content oil emulsion and preparation method thereof, and its technical scheme of taking is:
This missible oil is formulated by following raw materials by weight percent: lythidathion 50%-90%; Oil 0%-22%; Auxiliary agent 0%-5%; Solvent 4%-20%; Emulsifier 1%-12%; Stabilizing agent 0.01%-1%; Essence 0.01%-0.1%.
Selected lythidathion is that content is greater than 92% (wt%) lythidathion crude oil.
Selected oil is at least a in rapeseed oil or cottonseed oil or castor oil or palm oil or soybean oil or turpentine oil or kerosene or diesel oil or esterification rapeseed oil or esterification cottonseed oil or esterification castor oil or esterification palm oil or esterification soybean oil or esterification tung oil or ethyl ester rapeseed oil or ethyl ester cottonseed oil or ethyl ester castor oil or ethyl ester palm oil or ethyl ester soybean oil or the ethyl ester tung oil.
Selected auxiliary agent is at least a in hydroxypropyl methylcellulose or HEMC or gelatin or sodium alginate or the chitin.
Selected solvent is at least a in dimethylbenzene or toluene or ethyl acetate or acetone or the methyl alcohol.
Selected emulsifier is at least a in the block polymer of the oxirane of alkylphenol polyoxyethylene or fatty alcohol and expoxy propane or aliphatic alcohol polyoxyvinethene phosphate (or salt) or alkylphenol polyoxyethylene phosphate (or salt) or sucrose glyceride (Sucroglycerids) or alkyl polyglycoside (APG) or aliphatic acid polyethenoxy ether or polyalcohol APEO or calcium dodecyl benzene sulfonate or succinate monoester sodium sulfonate or fluorine-containing surfactant or the organic silicon surfactant.
Selected stabilizing agent is the organic base compounds, be n-butylamine or sec-butylamine or tert-butylamine or di-n-butylamine or di-sec-butylamine or tri-n-butylamine or n-propylamine or isopropylamine or di-n-propylamine or diisopropylamine or Tri-n-Propylamine or monoethyl amine or diethylamine or triethylamine or 1.4-butanediamine or 1.3-propane diamine or N, at least a in N-diisopropylethylamine or monoethanolamine or diethanol amine or triethanolamine or fatty acid potassium or the sodium soap.
The preparation method of this missible oil is: following each raw material of weighing at first by weight percentage: lythidathion 50%-90%; Oil 0%-22%; Auxiliary agent 0%-5%; Solvent 4%-20%; Emulsifier 1%-12%; Stabilizing agent 0.01%-1%; Essence 0.01%-0.1%; Then oil and lythidathion crude oil are added and have in the mixing kettle of high-speed stirring apparatus, on one side stir and heat temperature raising to 50-70 ℃, add solvent and auxiliary agent on one side, add emulsifier then, and carry out strong agitation and be incubated 1-2h at 50-70 ℃; Cooling reduces temperature to normal temperature, adds stabilizing agent and essence while stirring, and after mixing, being transparent oily liquid promptly is finished product.
Also the various raw materials after weighing can be mixed in premixed device, and then mix in adding colloid mill or sand mill or homogenizer or the high-shear emulsifying equipment, being transparent oily liquid promptly is finished product.
This missible oil good stability, lasting medicine, environmental pollution is few, its preparation method advantages of simple, production cost is lower.The performance indications such as the table 1 of lythidathion missible oil of the present invention:
The performance indications of table 1 high-lythidathion content oil emulsion
| Project name | Index |
| Outward appearance | Brown or faint yellow oily transparency liquid does not have suspension or sediment |
| Lythidathion content/g/L | 50-90 |
| Density/g/L (20 ℃) | 978-1022 |
| Moisture/%≤ | 0.4 |
| The pH value | 4.9-9.0 |
| Stability of emulsion (200 times of standard hard water dilutions) | Qualified |
| Low-temperature stability | Qualified |
| Heat endurance | Qualified |
Embodiment
Below in conjunction with embodiment the present invention is described in detail:
Embodiment 1:
Rapeseed oil 220L and lythidathion crude oil 510L adding are had in the reactor of high-speed stirring apparatus, after unlatching is stirred and is mixed, add ethyl acetate solvent 210L and HEMC 25kg while stirring, stirring also is heated to 50 ℃, after HEMC dissolves fully and mixes, under strong agitation, add nonyl phenol polyoxyethylene polyoxypropylene ether 50kg in batches, 50 ℃ are incubated 2h down, reduce temperature to normal temperature, add 1.3-propane diamine 100g and lemon type essence 100g while stirring, after mixing, being the transparence oily liquids promptly is finished product.
The cold storage-stable of finished product adopts 0 ℃ of storage 7 days, and heat endurance adopts 54 ± 2 ℃ of storages 14 days, and stability of emulsion adopts 200 times of mensuration of standard hard water dilution, result such as table 2.
The test of table 2 stability of emulsion
50% lythidathion missible oil is prevented and treated the field control effectiveness test of tomato root-knot eelworm, according to GB/T17980.72-2004, pesticide field efficacy medicine test criterion (two) the 72nd part: insecticide control nonirrigated farmland soil insect, result of the test such as table 3.Contrast medicine 10% lythidathion granule is provided by Japanese Ishihara Sangyo Kaisha, Ltd..Result of the test shows, and is good to the control efficiency of tomato root-knot eelworm.
Table 3 lythidathion missible oil is to the control effect of 2 instar larvaes of root-knot nematode in the soil
50% lythidathion emulsion is prevented and treated the field control effectiveness test of garlic root maggot, according to GB/T17980.72-2004, pesticide field efficacy medicine test criterion (two) the 72nd part: insecticide control nonirrigated farmland soil insect, result of the test such as table 4.
Table 4 lythidathion emulsion is to the control effect of garlic root maggot 2 instar larvaes
Embodiment 2:
Castor oil 200L and lythidathion crude oil 705L adding are had in the reactor of high-speed stirring apparatus, after unlatching is stirred and is mixed, add xylene solvent 90L and hydroxypropyl methylcellulose 10kg while stirring, stirring also is heated to 70 ℃, after hydroxypropyl methylcellulose dissolves fully and mixes, carrying out under the intensively stirred condition, add the oxirane of laruyl alcohol and the block polymer 90kg of expoxy propane in batches, 70 ℃ of constant temperature also keep 1h, reduce temperature to normal temperature, add diethanol amine 400g and lemon type essence 500g while stirring.After mixing, being the transparence oily liquids promptly is finished product.
The cold storage-stable of finished product adopts 0 ℃ of storage 7 days, and heat endurance adopts 54 ± 2 ℃ of storages 14 days, and stability of emulsion adopts 200 times of mensuration of standard hard water dilution, result such as table 5.
The test of table 5 stability of emulsion
Embodiment 3:
Take by weighing palm oil 50L, lythidathion crude oil 820L, gelatin 45kg, mixed solvent respectively and be dimethylbenzene and methyl alcohol (volume ratio 1:1) 100L, sucrose glyceride 90kg, ethylenediamine 1kg, lemon type essence 100g, add in the premixed device and carry out premixed, and then add colloid mill and mix, being the transparence oily liquids promptly is finished product.
The cold storage-stable of finished product adopts 0 ℃ of storage 7 days, and heat endurance adopts 54 ± 2 ℃ of storages 14 days, and stability of emulsion adopts 200 times of mensuration of standard hard water dilution, result such as table 6.
The test of table 6 stability of emulsion
Embodiment 4:
Take by weighing soybean oil 20L, lythidathion crude oil 940L, sodium alginate 5kg, mixed solvent respectively and be dimethylbenzene and methyl alcohol (volume ratio 2:1) 50L, calcium dodecyl benzene sulfonate 50kg, nonyl phenol polyoxyethylene polyoxypropylene ether 20kg, tri-n-butylamine 10kg, lemon type essence 100g, add in the premixed device and carry out premixed, and then add homogenizer and mix, being the transparence oily liquids promptly is finished product.
The cold storage-stable of finished product adopts 0 ℃ of storage 7 days, and heat endurance adopts 54 ± 2 ℃ of storages 14 days, and stability of emulsion adopts 200 times of mensuration of standard hard water dilution, result such as table 7.
The test of table 7 stability of emulsion
Embodiment 5:
Take by weighing the oxirane of turpentine oil 20L, esterification soybean oil 30L, lythidathion crude oil 850L, solvent acetone 150L, lauric acid APEO 16kg, laruyl alcohol and block polymer 10kg, tert-butylamine 500g, the lemon type essence 200g of expoxy propane respectively, add in the premixed device and carry out premixed, and then mix in the adding high-shear emulsion machine, being the transparence oily liquids promptly is finished product.
The cold storage-stable of finished product adopts 0 ℃ of storage 7 days, and heat endurance adopts 54 ± 2 ℃ of storages 14 days, and stability of emulsion adopts 200 times of mensuration of standard hard water dilution, result such as table 8.
The test of table 8 stability of emulsion
Embodiment 6:
Take by weighing lythidathion crude oil 900L, chitin 1kg, solvent acetone 100L, methyl alcohol 80L, fluorine-containing surfactant (LH-31) 10kg, fatty acid potassium 1kg, lemon type essence 300g respectively, add in the premixed device and carry out premixed, and then mix in the adding sand mill, being the transparence oily liquids promptly is finished product.
The cold storage-stable of finished product adopts 0 ℃ of storage 7 days, and heat endurance adopts 54 ± 2 ℃ of storages 14 days, and stability of emulsion adopts 200 times of mensuration of standard hard water dilution, result such as table 9.
The test of table 9 stability of emulsion
Embodiment 7:
Take by weighing diesel oil 20L, lythidathion crude oil 940L, solvent xylene 80L, polyoxyethylene trisiloxanes (silwell-77) 50kg, sodium soap 1kg, lemon type essence 100g respectively, add in the premixed device and carry out premixed, and then mix in the adding high-shear emulsion machine, being the transparence oily liquids promptly is finished product.The cold storage-stable of finished product adopts 0 ℃ of storage 7 days, and heat endurance adopts 54 ± 2 ℃ of storages 14 days, and stability of emulsion adopts 200 times of mensuration of standard hard water dilution, result such as table 10.
The test of table 10 stability of emulsion
Embodiment 8:
Esterification castor oil 50L and lythidathion crude oil 820L adding are had in the reactor of high-speed stirring apparatus, after unlatching is stirred and is mixed, add solvent toluene 80L and methyl alcohol 50L, hydroxypropyl methylcellulose 20kg, stirring also is heated to 70 ℃, after hydroxypropyl methylcellulose dissolves fully and mixes, carrying out under the intensively stirred condition, add the oxirane of laruyl alcohol and the block polymer 120kg of expoxy propane in batches, 65 ℃ of constant temperature also keep 1.5h, reduce temperature to normal temperature, add n-propylamine 1kg and lemon type essence 300g while stirring, after mixing, being the transparence oily liquids promptly is finished product.
The cold storage-stable of finished product adopts 0 ℃ of storage 7 days, and heat endurance adopts 54 ± 2 ℃ of storages 14 days, and stability of emulsion adopts 200 times of mensuration of standard hard water dilution, result such as table 11.
The test of table 11 stability of emulsion
Embodiment 9:
Take by weighing ethyl ester tung oil 150L, lythidathion crude oil 705L, gelatin 10kg, alkylphenol polyoxyethylene phosphate 90kg, sucrose glyceride 30kg, N respectively, N-diisopropylethylamine 1kg, lemon type essence 1kg, add in the premixed device and carry out premixed, and then mill in the adding sand mill evenly, being the transparence oily liquids promptly is finished product.
The cold storage-stable of finished product adopts 0 ℃ of storage 7 days, and heat endurance adopts 54 ± 2 ℃ of storages 14 days, and stability of emulsion adopts 200 times of mensuration of standard hard water dilution, result such as table 12.
The test of table 12 stability of emulsion
Claims (9)
1, a kind of high-lythidathion content oil emulsion is characterized in that this missible oil is formulated by following raw materials by weight percent: lythidathion 50%-90%; Oil 0%-22%; Auxiliary agent 0%-5%; Solvent 4%-20%; Emulsifier 1%-12%; Stabilizing agent 0.01%-1%; Essence 0.01%-0.1%.
2, a kind of high-lythidathion content oil emulsion according to claim 1 is characterized in that: described lythidathion is that content is greater than 92% (wt%) lythidathion crude oil.
3, a kind of high-lythidathion content oil emulsion according to claim 1 is characterized in that: described oil is at least a in rapeseed oil or cottonseed oil or castor oil or palm oil or soybean oil or turpentine oil or kerosene or diesel oil or esterification rapeseed oil or esterification cottonseed oil or esterification castor oil or esterification palm oil or esterification soybean oil or esterification tung oil or ethyl ester rapeseed oil or ethyl ester cottonseed oil or ethyl ester castor oil or ethyl ester palm oil or ethyl ester soybean oil or the ethyl ester tung oil.
4, a kind of high-lythidathion content oil emulsion according to claim 1 is characterized in that: described auxiliary agent is at least a in hydroxypropyl methylcellulose or HEMC or gelatin or sodium alginate or the chitin.
5, a kind of high-lythidathion content oil emulsion according to claim 1 is characterized in that: described solvent is at least a in dimethylbenzene or toluene or ethyl acetate or acetone or the methyl alcohol.
6, a kind of high-lythidathion content oil emulsion according to claim 1 is characterized in that: described emulsifier is at least a in the block polymer of the oxirane of alkylphenol polyoxyethylene or fatty alcohol and expoxy propane or aliphatic alcohol polyoxyvinethene phosphate (or salt) or alkylphenol polyoxyethylene phosphate (or salt) or sucrose glyceride (Sucroglycerids) or alkyl polyglycoside (APG) or aliphatic acid polyethenoxy ether or polyalcohol APEO or calcium dodecyl benzene sulfonate or succinate monoester sodium sulfonate or fluorine-containing surfactant or the organic silicon surfactant.
7, a kind of high-lythidathion content oil emulsion according to claim 1, it is characterized in that: stabilizing agent is the organic base compounds, be n-butylamine or sec-butylamine or tert-butylamine or di-n-butylamine or di-sec-butylamine or tri-n-butylamine or n-propylamine or isopropylamine or di-n-propylamine or diisopropylamine or Tri-n-Propylamine or monoethyl amine or diethylamine or triethylamine or 1.4-butanediamine or 1.3-propane diamine or N, at least a in N-diisopropylethylamine or monoethanolamine or diethanol amine or triethanolamine or fatty acid potassium or the sodium soap.
8, a kind of preparation method of a kind of high-lythidathion content oil emulsion as claimed in claim 1 is characterized in that: according to the described percentage by weight of claim 1 each raw material of weighing; Oil and lythidathion added have in the reactor of high-speed stirring apparatus, after mixing, on one side stir and heat temperature raising to 50-70 ℃, add auxiliary agent and solvent on one side, add emulsifier then, and carry out strong agitation and be incubated 1-2h down at 50-70 ℃; After temperature is reduced to normal temperature, add stabilizing agent and essence while stirring, after mixing, being transparent oily liquid promptly is finished product.
9, a kind of preparation method of a kind of high-lythidathion content oil emulsion as claimed in claim 1 is characterized in that: according to the described percentage by weight of claim 1 each raw material of weighing; Various raw materials are mixed in premixed device, and then mix in adding colloid mill or sand mill or homogenizer or the high-shear emulsifying equipment, being transparent oily liquid promptly is finished product.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102187861A (en) * | 2011-04-02 | 2011-09-21 | 河北三农农用化工有限公司 | Lythidathion effervescent tablets and method for preparing same |
| CN103120184A (en) * | 2012-06-01 | 2013-05-29 | 北京明德立达农业科技有限公司 | Fosthiazate pesticide composition and application thereof |
| CN107467016A (en) * | 2017-08-21 | 2017-12-15 | 山东华阳农药化工集团有限公司 | A kind of preparation method of ultra-low volume fosthiazate finish and its compound chrysanthemum ester type compound finish |
| CN108135159A (en) * | 2015-10-21 | 2018-06-08 | 巴斯夫欧洲公司 | Liquid pesticide compositions |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100736176B1 (en) * | 2004-09-24 | 2007-07-09 | 대한민국 | Nematicidal Compositions Containing Tartaric Acid |
| CN101180970A (en) * | 2007-12-03 | 2008-05-21 | 宋国春 | Hexaflumuron carbosulfan insecticidal composition |
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2008
- 2008-12-19 CN CN 200810249606 patent/CN101444205B/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102187861A (en) * | 2011-04-02 | 2011-09-21 | 河北三农农用化工有限公司 | Lythidathion effervescent tablets and method for preparing same |
| CN103120184A (en) * | 2012-06-01 | 2013-05-29 | 北京明德立达农业科技有限公司 | Fosthiazate pesticide composition and application thereof |
| CN108135159A (en) * | 2015-10-21 | 2018-06-08 | 巴斯夫欧洲公司 | Liquid pesticide compositions |
| CN107467016A (en) * | 2017-08-21 | 2017-12-15 | 山东华阳农药化工集团有限公司 | A kind of preparation method of ultra-low volume fosthiazate finish and its compound chrysanthemum ester type compound finish |
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Inventor after: Sun Jingwen Inventor after: Yan Xinhua Inventor after: Wang Fuwei Inventor after: Song Dongsheng Inventor after: Wang Fengzhi Inventor after: Liu Yufa Inventor after: Kong Bin Inventor after: Liu Ziyou Inventor after: Zhang Ruisheng Inventor after: Chen Yongping Inventor after: Liu Yingyan Inventor before: Song Dongsheng Inventor before: Liu Yufa Inventor before: Liu Ziyou Inventor before: Zhang Ruisheng Inventor before: Chen Yongping Inventor before: Liu Yingyan Inventor before: Yan Xinhua Inventor before: Wang Fuwei |
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Owner name: HUAYANG AGRICULTURAL CHEMICALS GROUP CO., LTD. SHA Free format text: FORMER OWNER: SHANDONG HUAYANG SCIENCE +. TECHNOLOGY CO., LTD. Effective date: 20121221 |
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Effective date of registration: 20121221 Address after: 271411 Ningyang County, Shandong province magnetic kiln town Patentee after: Huayang Agricultural Chemicals Group Co., Ltd. Shandong Prov. Address before: 271411 Shandong County of Ningyang Province town of magnetic kiln Patentee before: Shangdong Huayang Science &. Technology Co., Ltd. |