CN1269138A - Formula high-efficiency colloidal suspending agent of cypermethrin and its preparation - Google Patents

Formula high-efficiency colloidal suspending agent of cypermethrin and its preparation Download PDF

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Publication number
CN1269138A
CN1269138A CN 99103571 CN99103571A CN1269138A CN 1269138 A CN1269138 A CN 1269138A CN 99103571 CN99103571 CN 99103571 CN 99103571 A CN99103571 A CN 99103571A CN 1269138 A CN1269138 A CN 1269138A
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cypermethrin
suspending agent
efficiency
triethanolamine
colloidal suspending
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孙振宝
房志宏
王兰萍
舒国欣
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CHAOYANG LONGHUA PESTICIDE PLANT BEIJING
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CHAOYANG LONGHUA PESTICIDE PLANT BEIJING
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Abstract

A high-effective cypermethrin colloidal suspending agent is formed from high-effective cypermethrin, acrylic crosslinked polymer, triethanolamine, nonyl phenol polyethanoxy ether, propanetriol, di-(octyl-amino-ethyl) glycine hydrochloride, powder type silicon oil defoaming agent and deionized water, and its preparation process includes the following steps: thermally dissolving high-effective cypermethrin in propanetriol and phenol polyethanoxy ether, adding water and uniformly mixing, high-speed shearing, grinding and mixing under a pressure of 200-400 kg, adding other components and using triethanolamine to make neutralization and stirring so as to obtain the invented product.

Description

Formula high-efficiency colloidal suspending agent of cypermethrin and preparation technology
The present invention relates to formula high-efficiency colloidal suspending agent of cypermethrin and preparation technology.
Beta-cypermethrin, English name are High effect cypermethrin, and chemical name is: 2, and 2-dimethyl-3-(2, the 2-dichloroethylene) cyclopropane-carboxylic acid-alpha-cyano-(3-phenoxy group) benzyl ester, chemical structural formula is:
Figure A9910357100031
Beta-cypermethrin is a white crystals, and fusing point is 60 ℃~65 ℃, is insoluble in water, is soluble in acetone and aromatic hydrocarbons organic solvent.It has good tagging and stomach poison function to insect, has obtained using widely in agricultural and sanitary insect pest control at present.This medicine has been realized suitability for industrialized production in units such as China Tianjin insecticide factories.Its preparation has missible oil, wetting powder and suspending agent to come out.
Because beta-cypermethrin toxicity is bigger, the oral LD of rat acute 50Be 640mg/Kg, skin and mucous membrane are had certain excitant.
The present invention adds beta-cypermethrin compositions such as acrylic crosslinking polymer, under high pressure fully shear, grind, mix and make colloidal suspending agent, reduced the excitant of beta-cypermethrin, the delay insecticidal effect that has kept simultaneously it again makes it more to be applicable to the application in the control of sanitary insect pests such as mosquito, fly and cockroach.Other components in the prescription: acrylic crosslinking polymer (Carbopol, carbomer, Beijing Daily-use Chenmical Inst.) is a kind of water-soluble resin, is white powder.Consumption is about 0.5%, and to being that particulate in the suspension of medium just has good suspending ability with water, homogeneity can be good, and stability is also good, and storage life is long, and antibiotic property is strong, owing to avirulence, is used widely in daily chemical products.Before with the triethanolamine neutralization, the aqueous solution of carbomer has good flowability, therefore is easy to mix with other components, but with after the triethanolamine neutralization, mobile just the reduction widely, thereby show carbomer to atomic obvious suspending effect.Glycerine in the prescription except the antifreezing agent as colloidal suspending agent, because it is a polyhydroxy-alcohol compounds, to the suspending agent of carbomer as colloidal suspending agent, can play good stabilization simultaneously.Component two in the prescription-(octyl group amino-ethyl) glycine hydrochloride (octicin solution, Shandong Province's Qingzhou City Organic Chemical Plant) is a kind of good antimildew and antibacterial agent, and is not only effective but also toxicity is extremely low.Owing to wherein contain certain surfactant, the particulate in water had certain peptizaiton.Polyoxyethylene nonylphenol ether in the prescription (NP-40, Beijing treasure dragon chemical plant) is a kind of good emulsifier, can reduce the surface tension of water, helps the dispersion of particulate in water.Add very a spot of powder-type silicon oil foam killer (the carefree water-loss reducer in Beijing Co., Ltd) in the prescription, can significantly reduce the foam that produces because of high-speed stirred, therefore can guarantee the effect of under high pressure grinding, mixing better
The preparation technology of this colloidal suspending agent is: with commercially available content is 96% beta-cypermethrin, tentatively pulverizes, crosses 60 mesh sieves, to remove wherein foreign material.Be heated to about 80 ℃ with polyoxyethylene nonylphenol ether (NP-40) and glycerine then, make it to dissolve fully evenly, mix with the powder-type silicon oil foam killer again, under agitation add in the deionized water, start and spare the matter grinder, above-mentioned mixed liquor is added in the feed hopper gradually, and elder generation is mixed under normal pressure, regulating system pressure to 180-200 kilogram carries out abundant mixing and emulsifying gradually again.Take out this emulsification mixed liquor and be added to gradually in the hopper, regulating system pressure to the 380-400 kilogram, carry out high pressure and shear ground and mixed, promptly obtain the beta-cypermethrin mother liquor.In the container of cleaning, add deionized water, under slowly stirring, gradually the acrylic crosslinking polymer pressed powder be added in the water, place 4 hours from last, make the abundant swelling of acrylic crosslinking polymer, with the above-mentioned beta-cypermethrin mother liquor and two that makes--(octyl group amino-ethyl) glycine hydrochloride, under agitation be added in the solution of acrylic crosslinking polymer, mix.Triethanolamine is added gradually, continue fully to mix, promptly obtain high-efficiency colloidal suspending agent of cypermethrin.Take a sample, analyze with high performance liquid chromatograph.Recording insecticidal active ingredient beta-cypermethrin content is 5%.What 5 μ m such as little what of 99% grain diameter in the colloid, suspensibility is more than 80%.PH value about 7.This colloidal suspending agent is measured through Tianjin chemicals toxicological detection, the oral LD of its male rat 50Be 2130-6890mg/kg, and the oral LD of female rats 50Be 5620-12100mg/kg, through skin LD 50Big what 2000mg/kg.This colloidal suspending agent has been carried out killing the evaluation of pesticide effectiveness of mosquitos and flies and cockroach respectively by Tianjin health Centre for Disease Control and Beijing Sanitary and Antiepidemic Station.
The examination worm: Culex pipiens pallens (CULEX PIPIENS PALLENS), do not suck blood, the female adult mosquito of 2~3 ages in days sprouts wings; Housefly (MUSCA DOMESTICA VICINA), back adult on the 2nd~3 sprouts wings; Groton bug (BLATTELLA GERMANICA), 2 the week age adult.Method of testing: (1) mosquitos and flies: medicament is pressed dispenser dosage 50a.i.mg/M 2Be coated on equably on glass plate, paint plank, the lime plate face, and 0 day after the dispenser and 50 ℃ ± 1 ℃ baking 1 week (being equivalent to deposit half a year under the normal temperature) two Time Slot mosquitos and flies is carried out efficacy testing.Test method is carried out according to GB GB 13917.1-92.(2) cockroach: medicament is pressed dispenser dosage 83.33a.i.mg/M 2Be coated on equably on paint plank, the cement board surface, and toasted for 1 week (being equivalent to deposit half a year under the normal temperature) two Time Slot at 0 day after the dispenser and 50C+1C cockroach is carried out the evaluation of pesticide effectiveness, test method is carried out according to GB 13917.1-92.Every kind of panel triplicate of above-mentioned test is also obtained corresponding KT 50And 24 hours lethality (%), the cockroach test also requires 48,72 hours lethality (%).Test result sees Table 1, table 2.
Table 1 tries worm plate face KT to effect (50a.i.mg/M2) time of mosquitos and flies on different panels 50(on-lower limit) Min KT 95Min 24 hours lethality (%) 0 day mosquito glass 10.41 (9.06-11.96) 18.83 98.33
Housefly glass 4.41 (3.96-4.90) 8.82 100.00 bakings 1 all mosquito plates 10.49 (9.41-11.72) 25.67 96.67
30 minutes rate of knockdown of 13.97 100.000 days mosquito oil of housefly 4.42 (3.53-6.40) are 41.67% 96.67
30 minutes rate of knockdown of housefly lacquer 4.41 (4.03-4.84) 7.96 100.00 baking 1 all mosquito plates are 0% 95.00
30 minutes rate of knockdown of 13.79 100.000 days mosquito stone of housefly 6.46 (5.49-7.45) are 26.67% 96.67
30 minutes rate of knockdown of housefly ash 4.95 (3.96-6.18) 20.94 100.00 baking 1 all mosquito plates are 0% 86.67
Housefly 7.23 (6.22-8.41) 16.11 100.00
Table 2 tries worm plate face KT to effect (83.33a.i.mg/M) time of cockroach on different panels 50(on--lower limit) Min KT 95Min hour lethality (%)
24 48 720 days cockroach paint 7.78, (7.04-8.95) 12.29 60.00 96.67 96.67 bakings, 1 all cockroach plates 9.87, (6.68-9.89) 33.57 13.33 26.67 86.670 days cockroach cement 8.25, (7.32-9.31) 14.34 26.67 70.00 90.00 bakings, 1 all cockroach plates 16.93, (14.45-19.82) 34.96 13.33 26.67 80.00
Above-mentioned detection shows: this colloidal suspending agent dispenser dosage and detection method, be according to " agriculture chemical registration hygienic insecticide indoor harmacological effect estimates " and in GB 17322.1-1998 standard-required estimate.Three kinds of different plate faces when 1 week (being equivalent to deposit half a year under the room temperature), all greater than 70%, meet hygienic insecticide A grade standard to 24 hours lethality of mosquitos and flies 50 ℃ ± 1 ℃ baking.When two kinds of different plate faces toasted for 1 week (being equivalent to deposit half a year under the room temperature), 72 hours lethality of cockroach all greater than 70%, are also met hygienic insecticide A grade standard.Different plates is faced mosquitos and flies and cockroach all has good lethal effect.This medicine efficiency time is long, can be used for indoor delay and sprays the control sanitary insect pest.
In sum, by the high-efficiency colloidal suspending agent of cypermethrin that preparation technology of the present invention makes, prescription is reasonable, production technology advanced person, reliable product quality.It is the very desirable hygienic biocide durative action preparation in hotel, restaurant, family and other public places.
Embodiment 1
Form the colloidal suspending agent prescription with following component and percentage by weight:
1) beta-cypermethrin 5%;
2) polyoxyethylene nonylphenol ether (NP-40) 3%;
3) glycerine 5%;
4) two-(octyl group amino-ethyl) glycine hydrochlorides 0.5%;
5) acrylic crosslinking polymer (Carbopol) 0.3%
6) triethanolamine 0.3%;
7) the powder-type silicon oil foam killer 0.01%;
8) deionized water to 100%.Embodiment 2
Prepare colloidal suspending agent by following technology: after beta-cypermethrin was pulverized 60 mesh sieves, with polyoxyethylene nonylphenol ether, glycerine thermosol, mix being added in the deionized water again with defoamer, adjusting homogenizer system pressure to 180~200 kilograms carries out abundant mixing and emulsifying.Slowly pressure is transferred to 380~400 kilograms, is carried out high pressure again and shear, grind, mix, be added to stirring and evenly mixing in the acrylic crosslinking polymer aqueous solution mother liquid obtained, neutralizing with triethanolamine promptly obtains high-efficiency colloidal suspending agent of cypermethrin.

Claims (3)

1. formula high-efficiency colloidal suspending agent of cypermethrin and preparation technology is characterized in that forming (weight %) by following ingredients:
1) beta-cypermethrin 5%;
2) polyoxyethylene nonylphenol ether (NP-40) 3%;
3) glycerine 5%;
4) two-(octyl group amino-ethyl) glycine hydrochlorides 0.5%;
5) acrylic crosslinking polymer (Carbopol) 0.3%;
6) triethanolamine 0.3%;
7) the powder-type silicon oil foam killer 0.01%;
8) deionized water to 100%.
2. by described formula high-efficiency colloidal suspending agent of cypermethrin of claim 1 and preparation technology, it is characterized in that: with acrylic crosslinking polymer (Carbopol) as suspending agent, with in the triethanolamine with after promptly form colloidal suspension and play the suspending effect.
3. by described formula high-efficiency colloidal suspending agent of cypermethrin of claim 1 and preparation technology, it is characterized in that: preparation technology is: the beta-cypermethrin thermosol is in polyoxyethylene nonylphenol ether (NP-40) and glycerine, mix and add defoamer then with deionized water, under 200~400 kilograms of pressure, shear, grind, mix in the homogenizer high speed, after adding all the other components, promptly with the triethanolamine neutralization.
CN 99103571 1999-04-05 1999-04-05 Formula high-efficiency colloidal suspending agent of cypermethrin and its preparation Pending CN1269138A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101919382A (en) * 2010-06-28 2010-12-22 浙江特菱杀虫药业有限公司 Water aqua type aerial fog pesticide and preparation method thereof
WO2011083485A1 (en) * 2010-01-08 2011-07-14 Tagros Chemicals India Limited Insect management compositions for use on natural and synthetic materials and surfaces
CN106732169A (en) * 2016-12-30 2017-05-31 武汉科技大学 A kind of silicon carbide micro-powder dispersant with rust inhibition
CN106942264A (en) * 2017-03-15 2017-07-14 合肥华创现代农业科技有限公司 A kind of aqueous emulsion of phosphate compounding comprising effective cypermethrin and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011083485A1 (en) * 2010-01-08 2011-07-14 Tagros Chemicals India Limited Insect management compositions for use on natural and synthetic materials and surfaces
CN101919382A (en) * 2010-06-28 2010-12-22 浙江特菱杀虫药业有限公司 Water aqua type aerial fog pesticide and preparation method thereof
CN106732169A (en) * 2016-12-30 2017-05-31 武汉科技大学 A kind of silicon carbide micro-powder dispersant with rust inhibition
CN106942264A (en) * 2017-03-15 2017-07-14 合肥华创现代农业科技有限公司 A kind of aqueous emulsion of phosphate compounding comprising effective cypermethrin and preparation method thereof

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