CN1879478A - Benfuracard micro-emulsion - Google Patents
Benfuracard micro-emulsion Download PDFInfo
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- CN1879478A CN1879478A CN 200510078417 CN200510078417A CN1879478A CN 1879478 A CN1879478 A CN 1879478A CN 200510078417 CN200510078417 CN 200510078417 CN 200510078417 A CN200510078417 A CN 200510078417A CN 1879478 A CN1879478 A CN 1879478A
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- phosphoric acid
- acid ester
- benfuracard micro
- phosphate
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Abstract
The invention relates to a microemulsion and process for preparation, wherein the microemulsion comprises (by weight ratio): (1) 1-25% of benfuracarb, (2) 1-20% of at least one phosphoric acid ester type anionic surface active agent as emulsion agent and dispersing agent, (3) 1-20% of at least one non-ionic surface active agent as emulsion agent and dispersing agent, (4) 1-10% of at least one epoxy compound as stabilizing agent, (5) 1-20% of at least one of the alcohols as co-emulsifying agent, (6) balancing water.
Description
Technical field
The present invention relates to a kind of agricultural chemical insecticide Benfuracard micro-emulsion and preparation method thereof.
Background technology
Microemulsion is the external eighties of an a kind of environmentally friendly novel form newly developed, belong to a kind of of aqueous emulsion, it is medium with water, act on water-fast effective active component by dispersion, emulsification etc., by homogenize technology, it is dispersed in the water, forms the thermodynamic stable system of oil-in-water type.Disperse phase is liquid-drop diameter≤0.1um after homogenize, so appearance transparent, physics, chemical stability are good, and is strong to plant and insect tissue cell permeability, the preventive effect height, and its accumulating and result of use all are better than old formulation kinds such as missible oil, granule, pulvis.
Benfuracard micro (benfuracarb) is a kind of new and effective, broad spectrum activity, the systemic insecticide of Japanese Otsuka Kagaku K.K. (OtsukrChemicals Co.Ltd.) exploitation, is the low derivative that poisons of carbofuran.Have interior suction, tag and stomach poison function, be used to prevent and treat rice water weevil, thrips, borer, the iron wire worm, cotten aphid, the corn may-bug, onion fly, diamond-back moth, codling moth, chi Qu etc. make processing soil treatment agent and can prevent and treat soil insect and blade face insect.
The present invention finds by further investigation, adopt the emulsification-dispersion-stabilising system of phosphoric acid ester anion surfactant-non-ionic surface active agent-co-emulsifier-epoxychloropropane, can make the Benfuracard micro-emulsion of physicochemical property excellence, this microemulsion has that emulsion property is stable, the transparency temperature wide ranges, resolution ratio is low and the excellent reliable advantage of drug effect, has good market prospects.
Summary of the invention
The purpose of this invention is to provide a kind of Benfuracard micro-emulsion with good stability, the Benfuracard micro cream preparation that replaces highly toxic carbofuran agricultural chemicals and easily environment is polluted, reduce the toxicity of product, increase safety in utilization, can produce good economic benefits and social benefit.
Below narrate the main contents of invention:
Microemulsion of the present invention comprises by weight
1) 1-25% Benfuracard micro;
2) at least a phosphoric acid ester anion surfactant of 1-20% as emulsification, dispersant;
3) at least a non-ionic surface active agent of 1-20% as emulsification, dispersant;
4) at least a epoxy compounds of 1-10% as stabilizing agent;
5) at least a alcohols of 1-20% as co-emulsifier;
6) water complements to 100%.
Microemulsion is a kind of with the environmentally friendly pesticidal preparations of water as solvent, and it should have the transparency temperature scope of good heat storage stability, water dilution stability and broad.Benfuracard micro is owing to be that the key problem in technology of this invention and difficulty just are how to determine rational prescription to acid, to heat, hydrolabil agricultural chemicals, the one, reduce the hydrolysis of Benfuracard micro, and the resolution ratio of control active ingredient is no more than 5%; The 2nd, the stability of maintenance product micro emulsion avoids product to produce muddiness or layering between storage period.
The present inventor discovers by intensive, adopt the emulsification-dispersion-stabilising system of phosphoric acid ester anion surfactant-non-ionic surface active agent-co-emulsifier-epoxy compounds, can make the Benfuracard micro-emulsion of physicochemical property excellence.
In the present invention, the phosphoric acid ester anion surfactant is selected from alkyl phosphate class, polyoxyethylene carboxylate phosphoric acid ester, alkyl polyoxyethylene ether phosphate or alkyl polyethenoxy ether phosphoric acid ester, alkylphenol polyoxyethylene phosphoric acid ester, aralkyl phenol polyethenoxy ether phosphoric acid ester.Alkyl phosphate class such as alkyl phosphate triethanolamine; Polyoxyethylene carboxylate phosphoric acid ester such as linoleic acid polyoxyethylene ester phosphate, linolenic acid polyoxyethylene ester phosphate, castor oil acid polyoxyethylene ester phosphate etc.; Alkyl polyoxyethylene ether phosphoric acid ester such as iso-octyl alcohol polyoxyethylene ether phosphate, ethoxylated dodecyl alcohol phosphate, polyoxyethylene octadecanol phosphate, Brij phosphate etc.; Alkylphenol polyoxyethylene phosphoric acid ester such as octyl group polyoxyethylene ether phosphate, polyoxyethylene nonylphenol ether phosphate, binonylphenol polyoxyethylene ether phosphate, dodecylphenol polyoxyethylene ether phosphate, tetradecylphenol polyoxyethylene ether phosphate and cetyl phenol polyethenoxy ether phosphate or aralkyl phenol polyethenoxy ether phosphoric acid ester such as phenethyl phenol polyethenoxy ether phosphate or its alkali metal salt or amine salt.Preferred phosphoric acid ester anion surfactant can be wherein a kind of, also can be its mixture.The EO value of the phosphoric acid ester anion surfactant that is fit to is generally 2-20 according to the difference of the type of selected phosphate, is preferably 4-16.Serve as preferred with phosphoric acid ester anion surfactants such as NP-12 phosphate, NP-10 phosphate, TX-10 phosphate, 601 phosphates, 602 phosphates, 603 phosphates, MC-470F especially wherein.
The non-ionic surface active agent that is fit to is selected from alkylphenol polyoxyethylene class, alkylphenol-polyethenoxy polyethenoxy ether, benzylphenol polyethylene glycol oxide ethers, fatty alcohol polyethenoxy ether class, phenethyl phenol polyethenoxy polyoxypropylene ethers, fatty acid ethylene oxide adduct, castor oil ethylene oxide adduct, alkylphenol polyoxyethylene formaldehyde condensation products, aryl phenol polyoxyethylene formaldehyde condensation products or aralkyl phenol polyethenoxy ether formaldehyde condensation products.Selected non-ionic surface active agent can be wherein a kind of, also can be its mixture.Serve as preferred with the newborn 600# of farming, 700#, 1600#, NP-10, NP-12, TX-10,120#, 130#, 140#, non-ionic surface active agents such as 33#, 34# especially wherein.
The stabilizing agent that is fit to is selected from epoxy compounds, preferred epoxychloropropane.
For the present invention, adoptable epoxy compounds stabilizing agent dosage is generally 1-10%, is preferably 2-6%.
The co-emulsifier that is fit to is selected from butanols or isobutanol, and consumption is generally 1-20%, is preferably 5-16%.
For improving the low-temperature storage stability of microemulsion of the present invention, also can add the antifreezing agent of 1-10% by weight in the prescription.The antifreezing agent that is fit to is selected from urea, C
2-C
4The combination of one or both of lower aliphatic alcohols.C
2-C
4Lower aliphatic alcohols can be ethanol, ethylene glycol, polyethylene glycol, propyl alcohol, isopropyl alcohol, propane diols, glycerine or the tert-butyl alcohol, and preferred urea, glycerine or ethylene glycol are as antifreezing agent.
This microemulsion can prepare in a known manner, for example adopt oil phase to join direct emulsion process, phase conversion method (antiphase method), soluble oils method, the second emulsifying method of water, referring to " formulations of pesticide process technology " (second edition), the 406-407 page or leaf, Liu Bulin, Chemical Industry Press, in October, 1998.The preferred phase conversion method that adopts prepares in the embodiment of the invention, organic matter component in the prescriptions such as active constituent Benfuracard micro in the prescription and emulsifier fully is mixed into the oil phase of homogeneous transparent, under agitation slowly add distilled water or deionized water, form WO emulsion, again through heated and stirred, make it rapid phase inversion and become oil-in-water type, be chilled to room temperature and make it to reach balance, can make stable O/W type microemulsion after filtration.But, then should adopt other method for making if the oil phase amount is excessive in the component.
The physicochemical property of Benfuracard micro-emulsion of the present invention is:
Outward appearance: light brown transparency liquid;
Stability of emulsion: with the water-reducible emulsion-stabilizing of any ratio;
Heat storage stability: store 2 all outward appearances down at 54 ℃ and keep transparent homogeneous phase, resolution ratio≤5%;
Cold storage stability: in 0～-10 ℃ of refrigerator, stored 24 hours, place in the room temperature and can recover pellucidity;
Transparency temperature scope: 0～60 ℃;
Ageing stability: can stablize under the normal temperature and store more than 2 years.
Physicochemical property and give birth to survey the result and show, Benfuracard micro-emulsion of the present invention have that emulsion property is stable, the transparency temperature wide ranges, resolution ratio is low and the excellent reliable advantage of drug effect.The successful preparation of Benfuracard micro-emulsion can improve the safety of production, storing and use effectively, and can significantly reduce the pollution to environment, so said preparation has positive society and Significance for Environment.
This microemulsion has following five advantages: (1) flash-point height, do not fire and do not explode, production, storing and safe in utilization; (2) use no or little organic solvent, environmental pollution is little, and the producer and user's murder by poisoning is greatly alleviated, and helps the improvement of eco-environmental quality; (3) water is matrix, and aboundresources is inexpensive, and product cost is low, and packing easily; (4) the sprinkling stink is lighter, and chemical injury of crops and fruit tree fruit drop phenomenon are obviously reduced; (5) particle of microemulsion emulsion is ultra tiny, and is littler than common missible oil particle, and plant and insect cell are had excellent permeability, the absorption ratio height, so drug effect just may take place in low dosage.
Embodiment
The present invention is specifically described with the following example, but the present invention is not limited only to this several examples.
Embodiment 1:5% Benfuracard micro-emulsion
Benfuracard micro 5%
Epoxychloropropane 2%
Butanols 5%
Phenethyl phenol polyethenoxy ether (600#) 5%
Polyoxyethylene nonylphenol ether phosphoric acid ester sodium (NP-12 phosphate) 8%
Glycerine 5%
Water to 100%
Load weighted Benfuracard micro, epoxychloropropane, butanols, phenethyl phenol polyethenoxy ether (603#), polyoxyethylene nonylphenol ether phosphoric acid ester sodium (NP-12 phosphate) drop in the homogenizer respectively and stir in advance, slowly add the water that is dissolved with glycerine then, the strong mixing and homogenize, promptly make 5% Benfuracard micro-emulsion.
Embodiment 2:10% Benfuracard micro-emulsion
Benfuracard micro 10%
Epoxychloropropane 2%
Isobutanol 10%
Polyoxyethylene nonylphenol ether (NP-10) 7%
Ethoxylated dodecyl alcohol phosphoric acid ester sodium (MC-470F) 15%
Polyethylene glycol (200) 4%
Water to 100%
Load weighted Benfuracard micro, epoxychloropropane, isobutanol, polyoxyethylene nonylphenol ether (NP-10), ethoxylated dodecyl alcohol phosphoric acid ester sodium (MC-470F) drop in the homogenizer respectively and stir in advance, slowly add the water that is dissolved with polyethylene glycol then, the strong mixing and homogenize, promptly make 10% Benfuracard micro-emulsion.
Embodiment 3:15% Benfuracard micro-emulsion
Benfuracard micro 15%
Epoxychloropropane 5%
Phenethyl phenol polyethenoxy ether (600#) 10%
Polyoxyethylene nonylphenol ether phosphate amine salt (NP-10 phosphate) 10%
Isobutanol 16%
Urea 5%
Water to 100%
Load weighted Benfuracard micro, epoxychloropropane, isobutanol, phenethyl phenol polyethenoxy ether (600#), polyoxyethylene nonylphenol ether phosphate amine salt (NP-10 phosphate) drop in the homogenizer respectively and stir in advance, slowly add the water that is dissolved with urea then, the strong mixing and homogenize, promptly make 15% Benfuracard micro-emulsion.
Embodiment 4:20% Benfuracard micro-emulsion
Benfuracard micro 20%
Epoxychloropropane 3%
Castor oil ethylene oxide adduct (140#) 10%
Phenethyl phenol polyethenoxy ether phosphate amine salt (602 phosphate) 15%
Butanols 16%
Urea 2%
Ethylene glycol 3%
Water to 100%
Load weighted Benfuracard micro, epoxychloropropane, butanols in advance dropped in the homogenizer respectively stir, slowly add the water that is dissolved with urea, ethylene glycol, castor oil ethylene oxide adduct (140#), phenethyl phenol polyethenoxy ether phosphate amine salt (602 phosphate) then, the strong mixing and homogenize, promptly make 20% Benfuracard micro-emulsion.
Below be the Toxicity Determination data of 15% Benfuracard micro-emulsion of example 3 to aphis craccivora:
| The medicament title | Concentration (ppm) | Total borer population (head) | Dead borer population (head) | Percentage correction (%) | LC 50/LC 90 (ppm) | 95% confidence interval |
| 15% Benfuracard micro-emulsion | 5 3.5 2.45 1.715 1.2005 0.84035 0.588245 | 256 259 172 247 226 247 230 | 256 237 127 117 55 24 6 | 100.0 91.5 73.8 47.4 24.3 9.7 2.6 | 1.7581 3.4257 | 1.6798～1.8401 3.1703～3.7559 |
| 20% Benfuracard micro missible oil | 5 3.5 2.45 1.715 1.2005 0.84035 0.588245 | 255 214 228 186 253 242 270 | 255 190 160 76 44 24 7 | 100.0 88.8 70.2 40.9 17.4 9.9 2.6 | 1.8990 3.7170 | 1.8119～1.9948 3.4106～4.1216 |
| CK | 291 | 4 | 1.4 |
As can be known from the table data: Benfuracard micro-emulsion is followed with the cream preparation of content and is compared, and not only has the advantage of producing storing safety, environmental pollution minimizing, also has the insecticidal activity advantage higher than cream preparation.
Claims (5)
1. Benfuracard micro-emulsion, its composition includes by weight:
1) 1-25% Benfuracard micro;
2) at least a phosphoric acid ester anion surfactant of 1-20% as emulsification, dispersant;
3) at least a non-ionic surface active agent of 1-20% as emulsification, dispersant;
4) at least a epoxy compounds of 1-10% as stabilizing agent;
5) at least a alcohols of 1-20% as co-emulsifier;
6) water complements to 100%.
2. according to the described Benfuracard micro-emulsion of claim 1, it is characterized in that used phosphoric acid ester anion surfactant is selected from alkyl phosphate class, polyoxyethylene carboxylate phosphoric acid ester, alkyl polyoxyethylene ether phosphate or alkyl polyethenoxy ether phosphoric acid ester, alkylphenol polyoxyethylene phosphoric acid ester or aralkyl phenol polyethenoxy ether phosphoric acid ester or its alkali metal salt or amine salt; And its non-ionic surface active agent is selected from alkylphenol polyoxyethylene class, alkylphenol-polyethenoxy polyethenoxy ether, benzylphenol polyethenoxy ether class, fatty alcohol polyethenoxy ether class, phenethyl phenol polyethenoxy polyoxypropylene ethers, fatty acid ethylene oxide adduct, castor oil ethylene oxide adduct, alkylphenol polyoxyethylene formaldehyde condensation products, aryl phenol APEO formaldehyde condensation products or aralkyl phenol polyethenoxy ether formaldehyde condensation products; The stabilizing agent that is fit to is an epoxychloropropane, and used co-emulsifier is butanols or isobutanol.
3. according to the described Benfuracard micro-emulsion of claim 2, used phosphoric acid ester anion surfactant is NP-12 phosphate, NP-10 phosphate, TX-10 phosphate, 601 phosphates, 602 phosphates, 603 phosphates, MC-470F in it is characterized in that filling a prescription; Used non-ionic surface active agent is agricultural newborn 600#, 700#, 1600#, NP-10, NP-12, TX-10,120#, 130#, 140#, 33#, 34# in the prescription.
4. according to the described Benfuracard micro-emulsion of claim 1, also contain the antifreezing agent of 1-10% in it is characterized in that filling a prescription by weight.
5. according to the described Benfuracard micro-emulsion of claim 4, it is characterized in that used antifreezing agent is urea, C
2-C
4The combination of one or both of lower aliphatic alcohols.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100784170A CN100348103C (en) | 2005-06-13 | 2005-06-13 | Benfuracard micro-emulsion |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100784170A CN100348103C (en) | 2005-06-13 | 2005-06-13 | Benfuracard micro-emulsion |
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| CN1879478A true CN1879478A (en) | 2006-12-20 |
| CN100348103C CN100348103C (en) | 2007-11-14 |
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| CNB2005100784170A Expired - Fee Related CN100348103C (en) | 2005-06-13 | 2005-06-13 | Benfuracard micro-emulsion |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105409989A (en) * | 2015-11-30 | 2016-03-23 | 肇庆市真格生物科技有限公司 | Nematicidal composition containing fluensulfone and benfuracarb |
| CN106472498A (en) * | 2016-08-31 | 2017-03-08 | 湖南海利化工股份有限公司 | A kind of complex stabilizer for carbofuran derivant and preparation method and application |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1288972C (en) * | 2004-06-18 | 2006-12-13 | 浙江禾田化工有限公司 | Carbosulfan microemulsion |
-
2005
- 2005-06-13 CN CNB2005100784170A patent/CN100348103C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105409989A (en) * | 2015-11-30 | 2016-03-23 | 肇庆市真格生物科技有限公司 | Nematicidal composition containing fluensulfone and benfuracarb |
| CN106472498A (en) * | 2016-08-31 | 2017-03-08 | 湖南海利化工股份有限公司 | A kind of complex stabilizer for carbofuran derivant and preparation method and application |
| CN106472498B (en) * | 2016-08-31 | 2019-12-03 | 湖南海利化工股份有限公司 | A kind of compound stabilizer and the preparation method and application thereof for carbofuran derivative |
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| CN100348103C (en) | 2007-11-14 |
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