CN103222461A - Environment-friendly mixed solvent used for pyrethroid pesticide preparation - Google Patents

Environment-friendly mixed solvent used for pyrethroid pesticide preparation Download PDF

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CN103222461A
CN103222461A CN2013101903203A CN201310190320A CN103222461A CN 103222461 A CN103222461 A CN 103222461A CN 2013101903203 A CN2013101903203 A CN 2013101903203A CN 201310190320 A CN201310190320 A CN 201310190320A CN 103222461 A CN103222461 A CN 103222461A
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dimethyl carbonate
white oil
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solvent
mixed solvent
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CN103222461B (en
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安峰明
苏安安
卢瑞
李现玲
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Guangxi Tianyuan Biochemical Co Ltd
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Guangxi Tianyuan Biochemical Co Ltd
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Abstract

The invention discloses an environment-friendly mixed solvent used for a pyrethroid pesticide preparation. The mixed solvent is composed of dimethyl carbonate and white oil, wherein mass percent of dimethyl carbonate is 0.5-60%, the mass percent of white oil is 0.5-40%, and the rest parts are other components of the pesticide preparation. The mixed solvent is used in a pyrethroid pesticide, dissolubility of a pyrethroid active ingredient in the mixed solvent system is high, stability is good, and the mixed solvent has the advantages of safety, environmental friendliness, low cost and wide application. The mixed solvent is the best choice for substituting a solvent of the conventional pesticide preparation, such as methyl alcohol, dimethyl benzene and N,N-dimethylformamide. Dosage forms applicable to the pyrethroid pesticide can be missible oil, emulsion in water and microemulsion.

Description

A kind of environmental protection mixed solvent that is used for the pyrethrin pesticide preparation
Technical field
The present invention relates to the pesticide solvent technical field, be specifically related to a kind of environmental protection mixed solvent that is used for the pyrethrin pesticide preparation.
Background technology
Mainly with methyl alcohol, dimethylbenzene and N, organic solvents such as dinethylformamide are as solvent in the present pyrethrin pesticide preparation processing, and the extensive application of these organic solvents has brought problems.At first, organic solvent is in the application process of pesticidal preparations product, and is bigger residual to all having in control crop and the environment, caused significant threat for agricultural production safety and Environmental security.Secondly, utilize organic solvent methyl alcohol, dimethylbenzene, toluene, benzene to produce Pesticidal products as solvent, in production, transportation, there are a large amount of security risks, solvent not only causes health threat to the workman in the production application process, simultaneously also lower because of the flash-point of this kind solvent, volatility has caused inflammable, explosive and the many problems of storage such as loss is big soon.Once more, use the pyrethrin pesticide preparation of conventional solvent preparation, product through the time storage process in the active component resolution ratio easily exceed standard, resolution ratio can reach 10~15% in general 12~24 months, particularly water base chemical preparation comprises that aqueous emulsion and microemulsion resolution ratio are up to 20~40%.And industry standard generally required 2 years to store resolution ratio less than≤5%.At last, along with the development of society, the raising of agricultural production awareness of safety, country puts into effect relevant policy, the use of the organic solvent in the Pesticidal products is controlled, thereby the selection of guiding pesticide solvent develops to direction green, environmental protection.
Dimethyl carbonate is a kind of water white fine solvent, 90.1 ℃ of boiling points, and 4 ℃ of fusing points, slightly fragrance is one of important downstream product of methyl alcohol, has safety, toxicity is little, pollution is few, is regarded as " green " chemical products.This solvent is slightly soluble in water, can be with arbitrary proportion and immiscible organic solvents such as alcohol, ketone, ester, non-corrosiveness.2000, DMC belonged to nontoxic or little chemical product that poisons by the registration of European chemical management board.Through the inquiry of patent prior art as can be known, patent " a kind of is the Affirm (Merck Co.) microemulsion of solvent with the dimethyl carbonate " (application number: 201210300394.3) reported the correlative study of using dimethyl carbonate preparation Affirm (Merck Co.) microemulsion.But different pesticide activity component solvability require different, the solubility property of solvent disperses to play key effect to the dissolving of former medicine, so the present invention is by dimethyl carbonate and white oil synergy, the soluble end of dimethyl carbonate and white oil is enlarged, to satisfy the dissolubility requirement of different pesticide activity components.
White oil is a kind of colourless, odorless, tasteless viscous liquid, generally is made up of alkane and the cycloalkane of relative molecular weight 300-400, has chemical stability and photostability.Report about the dissolvant white oil aspect has " farm chemical emulsion preparation " (patent No.: 200710117977.1) at present.This patent report single use white oil substitute dimethylbenzene as the farm chemical emulsion preparation solvent, but use the former drug effect fruit of white oil dissolving chrysanthemum ester class unsatisfactory during pesticidal preparations research and development test, white oil is applicable to that other pesticide active ingredient soluble end except chrysanthemum ester class is narrower, simultaneously this patent do not illustrate yet pyrethrin pesticide with white oil as the stability indicator in the cream preparation system of solvent.
Summary of the invention
The purpose of this invention is to provide a kind of environmental protection mixed solvent that is used for the pyrethrin pesticide preparation; with the alternative methyl alcohol of this mixed solvent, dimethylbenzene and N; organic solvents such as dinethylformamide solve the with an organic solvent existing variety of issue of present pyrethrin pesticide.This mixed solvent and pesticide active ingredient compatibility are good, and dissolving power is strong, and is applied widely, and pyrethrin pesticide composition ageing stability is good, environmentally friendly in this dicyandiamide solution.
Above-mentioned purpose of the present invention is achieved by the following technical solution: a kind of environmental protection mixed solvent that is used for the pyrethrin pesticide preparation, form by dimethyl carbonate and white oil, and wherein each component shared mass percent in preparation is: dimethyl carbonate 0.5-60%; White oil 0.5-40%.
In the present invention, unless specified otherwise is arranged, described percentage is mass percent.And dimethyl carbonate and white oil shared mass percent sum in preparation is not 100%.
As preferably, among the present invention, be used for the preferred 10-40% of dimethyl carbonate of the mixed solvent of pyrethrin pesticide system; The preferred 5-30% of white oil.
The environmental protection mixed solvent that is used for the pyrethrin pesticide preparation described in the typical example in the present invention preferably comprises draws together dimethyl carbonate 0.5%, white oil 9.5%.
In another embodiment of the present invention, the described environmental protection mixed solvent that is used for the pyrethrin pesticide preparation preferably comprises dimethyl carbonate 10%, white oil 40%.
In another embodiment of the present invention, the described environmental protection mixed solvent that is used for the pyrethrin pesticide preparation preferably comprises dimethyl carbonate 20%, white oil 30%.
In another embodiment of the present invention, the described environmental protection mixed solvent that is used for the pyrethrin pesticide preparation preferably comprises dimethyl carbonate 40%, white oil 27%.
In another embodiment of the present invention, the described environmental protection mixed solvent that is used for the pyrethrin pesticide preparation preferably comprises dimethyl carbonate 9.5%, white oil 0.5%.
In another embodiment of the present invention, the described environmental protection mixed solvent that is used for the pyrethrin pesticide preparation preferably comprises dimethyl carbonate 5%, white oil 5%.
In another embodiment of the present invention, the described environmental protection mixed solvent that is used for the pyrethrin pesticide preparation preferably comprises dimethyl carbonate 13%, white oil 12%.
In another embodiment of the present invention, the described environmental protection mixed solvent that is used for the pyrethrin pesticide preparation preferably comprises dimethyl carbonate 30%, white oil 20%.
In another embodiment of the present invention, the described environmental protection mixed solvent that is used for the pyrethrin pesticide preparation preferably comprises dimethyl carbonate 60%, white oil 20%.
The environmental protection mixed solvent that is used for the pyrethrin pesticide preparation of the present invention can mix with pesticide active ingredient, emulsifying dispersant.
Preferably, described pesticide activity component is selected from cypermethrin, beta-cypermethrin, gamma cyhalothrin, decis, sumicidin, cyfluthrin or Biphenthrin pesticidal preparations.
Described emulsifying dispersant is selected from one or more in fatty alcohol-polyoxyethylene ether, polycarboxylate, alkylaryl polyoxyethylene polyoxypropylene ether, nonyl phenol polyethenoxy ether, nonyl phenol polyethenoxy ether phosphate, calcium dodecyl benzene sulfonate, phenethyl phenol polyethenoxy sodium sulphate or the alkylphenol polyoxyethylene.
The formulation that the environmental protection mixed solvent that is used for the pyrethrin pesticide preparation of the present invention can be used for processing is missible oil, aqueous emulsion and microemulsion.
Compared with prior art, the present invention has following beneficial effect fruit:
1, solubility property significantly improves.This mixed solvent has greatly improved the solubility property to the former medicine of chrysanthemum ester class, as pesticide solvent, solubility property can improve 8 times, is example with the beta-cypermethrin with respect to single white oil of using, when list dissolved beta-cypermethrin with white oil, need white oil: beta-cypermethrin 〉=24:1 solubilized was complete; And when adopting this mixed solvent to dissolve, only need: mixed solvent: beta-cypermethrin 〉=3:1 is that dissolvable agents is complete, has solved singly with the low defective of white oil formulated product content, and the pyrethrin pesticide stability of formulation is better in this dicyandiamide solution.
2, safety environmental protection again.Adopt high dimethyl carbonate of flash-point and white oil as pesticide solvent, the dimethyl carbonate flash-point: 21.7 ℃ (opening), white oil flash-point: 164-223 ℃ (opening), the two mixes flash-point, and is nonflammable explosive.These two solvent toxicity are low, and are little to environmental influence, to producing and user's safety.
3, cost is low.The present invention adopts dimethyl carbonate and white oil to prepare pyrethrin pesticide as solvent, and at present, the dimethylbenzene price is 9000-1000 unit/ton, and the dimethyl carbonate price is 6000 yuan/ton, and the white oil price is 8000 yuan/ton.Utilize dimethyl carbonate and white oil to substitute dimethylbenzene, can save cost effectively.
4, synergy is remarkable.The present invention adopts dimethyl carbonate and white oil to prepare pyrethrin pesticide as solvent, can obviously improve the preventive effect of pyrethrin pesticide preparation pest control.
In addition, mixed solvent is not only big than the solvability that white oil list is used, and active ingredient pyrethrin pesticide good stability in this mixed solvent system.Simultaneously, this mixed solvent is good to the target crop safety; Low to environmental toxicity, pollute little; Use cost is low, the significant advantage of synergy, more meets the demand of social development.
Embodiment
The present invention is described further according to following embodiment, and what those skilled in the art can understand is that following embodiment only plays explanation to the present invention.Under the prerequisite that does not deviate from invention spirit, to any improvement that the present invention did with substitute all within protection domain of the present invention.
Preparation embodiment
Used reagent and medicine are commercially available conventional products among the embodiment.In following examples
The preceding content of resolution ratio computing formula: resolution ratio %=(storage-Re storage or normal temperature storage back content)/the preceding content of storage * 100%
Relative density (g/ml, 20 ℃) is measured: measure general rule with reference to GB/T 4472-1984 chemical products density, relative density
The assay method of solvability: (under the normal temperature, 25 ℃) adopts the gram number with the pyrethrin pesticide that can dissolve in the 100g solvent and the state that reaches capacity to calculate.The computing formula of solvability is: the saturated gram number/100g of the former medicine of solvability=dissolving.
Acidity (%) is measured: with reference to GB/T 28135-2011 agricultural chemicals acid (alkali) degree assay method
Flash-point (remaining silent) is measured: with reference to NYT1860.11-2010 agricultural chemicals physical and chemical property determining test guide rule the 11st part
Determination of moisture: GB1600-2001 agricultural chemicals moisture determination.
The preceding content of storage is that sample prepares to carry out the content that (54 ± 2 ℃) store 14 days former medicines that detect, and storage back content is that sample carries out the content that (54 ± 2 ℃) storage detected former medicine in 14 days.Heat storage test: storage temperature (54 ± 2) ℃, stored 14 days.
Embodiment 1:
Solvent samples 1: take by weighing dimethyl carbonate 5kg, white oil 95kg respectively, stir then and promptly get the mixed solvent that 100kg originally executes example.
3% high performance aqueous emulsion of cypermethrin (sample 1)
Each constituent mass percentage in the prescription: the former medicine of 95% beta-cypermethrin: 3%, solvent samples 1 10%, fatty alcohol-polyoxyethylene ether 3%, polycarboxylate 2%, ethylene glycol 3%, defoamer 0.05%, water complement to 100%.
Beta-cypermethrin in the top example is also replaceable to be the formulation products of cypermethrin, gamma cyhalothrin, decis, sumicidin, cyfluthrin and Biphenthrin.
3% high performance aqueous emulsion of cypermethrin (control sample 1)
Each constituent mass percentage in the prescription: the former medicine of 95% beta-cypermethrin: 3%, dimethylbenzene 10%, fatty alcohol-polyoxyethylene ether 3%, polycarboxylate 2%, ethylene glycol 3%, defoamer 0.05%, water complement to 100%.
Above sample, store simultaneously preceding Determination on content, normal temperature through the time stability test and heat storage test, heat storage sample design temperature in baking oven is 54 ± 2 ℃ and places 14 days, normal temperature sample and place 12,18 and 24 months respectively.Adopt high performance liquid chromatography to store preceding sample, heat storage sample and the normal temperature of different periods through the time storage sample in the content of beta-cypermethrin measure, and calculate its resolution ratio, measurement result sees Table 1, and the test data in the table is all to get result of the test mean value more than 10 times.
The stability test result of active component in table 1 3% high performance aqueous emulsion of cypermethrin
Figure 2013101903203100002DEST_PATH_IMAGE001
Show that from last watch test result sample 1 is promptly with dimethyl carbonate 0.5%, white oil 9.5% is a dicyandiamide solution, and it is the comparative sample 1 of solvent that the ageing stability of sample 1 is far superior to 10% dimethylbenzene.
All other technical indicators of table 2 sample 1
Figure 2013101903203100002DEST_PATH_IMAGE002
Table 3 solvent samples 1 and white oil, dimethyl carbonate and dimethylbenzene contrast the result pyrethrin pesticide solvability and stability test thereof.
The no test data of "-" expression in the table.
Last table data show that 1 pair of chrysanthemum ester of solvent samples class active component has fine solubility, and dissolving chrysanthemum ester class active component ability is suitable with dimethylbenzene, is better than dimethyl carbonate.Use 3% high performance aqueous emulsion of cypermethrin of solvent samples 1 preparation and be better than dimethylbenzene or dimethyl carbonate sample as solvent with the stability of content chrysanthemum ester class aqueous emulsion, and it is single poor owing to solubility property with white oil, with solvent samples 1 same amount situation under, promptly add 10% white oil owing to can't dissolve chrysanthemum ester active component in the prescription, so can't prepare 3% high performance aqueous emulsion of cypermethrin.
3% high performance aqueous emulsion of cypermethrin (control sample 1) carries out the biologically active drug effect relatively with 3% high performance aqueous emulsion of cypermethrin (sample 1), test period in June, 2012, test site: suburbs, Liuzhou, active ingredient usage amount: 9.4g/ hectare, occupation mode: convert water spray, controlling object: wild cabbage-cabbage caterpillar, result of the test is as shown in the table.
The computing formula of control efficiency: insect population insect population number * 100 before rate (%)=(medicine before insect population number-medicine after insect population number)/medicine of going down.
Preventive effect (%)=(the chemicals treatment district insect population rate of going down-blank district insect population go down rate)/(100-blank district insect population go down rate) * 100.
Table 4 3% high performance aqueous emulsion of cypermethrin (control sample 1) is prevented and treated cabbage caterpillar drug effect table as a result with 3% high performance aqueous emulsion of cypermethrin (sample 1)
Figure 2013101903203100002DEST_PATH_IMAGE004
As can be seen from the table sample 1 comparison in the same old way product 1 control efficiency cabbage pieris effect better or quite.
Above-mentioned table 1~4 show, the sample that is better than dimethylbenzene or dimethyl carbonate preparation with 3% high performance aqueous emulsion of cypermethrin (sample 1) and other chrysanthemum ester class aqueous emulsion ageing stabilities of solvent samples 1 preparation, the ability and the dimethylbenzene of solvent samples 1 dissolving chrysanthemum ester class are equal to or slightly better, and are better than dimethyl carbonate and white oil.Biological activity determination shows that 3% high performance aqueous emulsion of cypermethrin (sample 1) control cabbage pieris drug effect and control sample 1 are quite or better.In sum, it is feasible that solvent samples 1 alternative dimethylbenzene is applied to chrysanthemum ester class aqueous emulsion, and its solvent cost is low, and toxicity is low.
Embodiment 2:
Solvent samples 2: take by weighing dimethyl carbonate 20kg, white oil 80kg respectively, stir then and promptly get the solvent compositions that 100kg originally executes example.
2.5% Biphenthrin microemulsion (sample 2)
Each constituent mass percentage in the prescription: the former medicine of 95% Biphenthrin: 2.5%, solvent samples 50%(is equivalent to add dimethyl carbonate 10%, white oil 40% in this product), alkylaryl polyoxyethylene polyoxypropylene ether 8%, polycarboxylate 7%, calcium dodecyl benzene sulfonate 2%, ethylene glycol 3%, defoamer 0.05%, water complements to 100%.
Biphenthrin in the top example is also replaceable to be the formulation products of beta-cypermethrin, cypermethrin, gamma cyhalothrin, decis, sumicidin and cyfluthrin.
2.5% Biphenthrin microemulsion (control sample 2)
Each constituent mass percentage in the prescription: the former medicine of 95% Biphenthrin: 2.5%, dimethylbenzene 40%, and methyl alcohol 10%, alkylaryl polyoxyethylene polyoxypropylene ether 8%, polycarboxylate 7%, calcium dodecyl benzene sulfonate 2%, ethylene glycol 3%, defoamer 0.05%, water complement to 100%.
Above sample is store test of preceding assay, normal temperature ageing stability and heat storage test simultaneously, and heat storage sample design temperature in baking oven is 54 ± 2 ℃ and places 14 days, normal temperature sample and place 12,18 and 24 months respectively.Adopt gas chromatography to store preceding sample, heat storage sample and the normal temperature of different periods through the time storage sample in the content of Biphenthrin measure, and calculate its resolution ratio, measurement result sees Table 5, Test data in the table is all to get result of the test mean value more than 10 times.
The stability test result of active component in the table 5 2.5% Biphenthrin microemulsion
Figure 2013101903203100002DEST_PATH_IMAGE005
Above-mentioned result of the test shows that sample 2 is promptly with dimethyl carbonate 10%, and the dicyandiamide solution of white oil 40%, the ageing stability of sample 2 are better than with dimethylbenzene 40%, and methyl alcohol 10% is the sample of solvent.
All other technical indicators of table 6 sample 2
Figure 2013101903203100002DEST_PATH_IMAGE006
Table 7 sample 2 and white oil, dimethyl carbonate and dimethylbenzene contrast the result pyrethrin pesticide solvability and stability test thereof.
Figure 2013101903203100002DEST_PATH_IMAGE007
The no test data of "-" expression in the table.
Last table data show that 2 pairs of chrysanthemum esters of solvent samples class active component has fine solubility, and the ability and the dimethylbenzene of dissolving chrysanthemum ester class active component are suitable, and are better than dimethyl carbonate.The stability of chrysanthemum ester class active component in solvent samples 2 systems also is better than the stability in dimethylbenzene or dimethyl carbonate system, and it is single poor owing to solubility property with white oil, with solvent samples 1 same amount situation under, promptly add 50% white oil in the prescription because can't the lytic activity component, can't prepare 2.5% Biphenthrin microemulsion.
2.5% Biphenthrin microemulsion (control sample 2) carries out the biologically active drug effect relatively with 2.5% Biphenthrin microemulsion (sample 2), test period in June, 2012, test site: Fujian Anxi County, active ingredient usage amount: 37.5g/ hectare, occupation mode: convert water spray, controlling object: tea tree-tea lesser leafhopper, result of the test such as following table.
The computing formula of control efficiency: insect population insect population number * 100 before rate (%)=(medicine before insect population number-medicine after insect population number)/medicine of going down
Preventive effect (%)=(the chemicals treatment district insect population rate of going down-blank district insect population go down rate)/(100-blank district insect population go down rate) * 100.
The drug effect of table 8 2.5% Biphenthrin microemulsion (control sample 2) and 2.5% Biphenthrin microemulsion (sample 2) control tea lesser leafhopper is table as a result
Figure 2013101903203100002DEST_PATH_IMAGE008
As can be seen from the above table, sample 2 comparison in the same old way product 2 control tea tree-tea lesser leafhoppers effect better or quite.
Above-mentioned table 5~8 show, 2.5% Biphenthrin microemulsion of solvent-applied sample 2 preparations and other chrysanthemum ester class microemulsion ageing stabilities are better than the sample of dimethylbenzene or dimethyl carbonate preparation in the implementation column 2, solvent samples 2 dissolving chrysanthemum ester class abilities and dimethylbenzene are equal to or slightly better, and are better than dimethyl carbonate and white oil.2.5% Biphenthrin microemulsion control tea tree-tea lesser leafhopper drug effect that biological activity determination shows solvent samples 2 and dimethylbenzene preparation quite or better.In sum, it is feasible that solvent samples 2 alternative dimethylbenzene are applied to chrysanthemum ester class aqueous emulsion, and its solvent cost is low, and toxicity is low.
Embodiment 3:
Solvent samples 3: take by weighing dimethyl carbonate 40kg, white oil 60kg respectively, stir then and promptly get the solvent compositions that 100kg originally executes example.
5% deltamethrin milk oil (sample 3)
Each constituent mass percentage in the prescription: 95% deltamethrin original medicine: 5%, solvent samples 50%(is equivalent to add dimethyl carbonate 20%, white oil 30% in this product), polyoxyethylene nonylphenol ether 6%, calcium dodecyl benzene sulfonate 4%, methyl oleate complement to 100%.
Decis in the top example is also replaceable to be the formulation products of beta-cypermethrin, cypermethrin, gamma cyhalothrin, sumicidin, cyfluthrin and Biphenthrin.
5% deltamethrin milk oil (control sample 3)
Each constituent mass percentage in the prescription: 95% deltamethrin original medicine: 5%, dimethylbenzene 50%, polyoxyethylene nonylphenol ether 6%, calcium dodecyl benzene sulfonate 4%, methyl alcohol complement to 100%.
Above sample is store test of preceding assay, normal temperature ageing stability and heat storage test simultaneously, and heat storage sample design temperature in baking oven is 54 ± 2 ℃ and places 14 days, normal temperature sample and place 12,18 and 24 months respectively.With reference to HG2801-1996 adopt gas chromatography to store preceding sample, heat storage sample and the normal temperature of different periods through the time storage sample in the content of decis measure, and calculate its resolution ratio, measurement result sees Table 9, Test data in the table is all to get result of the test mean value more than 10 times.
The stability test result of active component in table 9 5% deltamethrin milk oil
Figure 2013101903203100002DEST_PATH_IMAGE009
Above-mentioned result of the test shows that sample 3 is promptly with dimethyl carbonate 20%, and the dicyandiamide solution of white oil 30%, the ageing stability of sample 3 are better than with dimethylbenzene 50%, and methyl alcohol is supplied the sample into solvent.
Other technical indicator of table 10 sample 3
Figure 2013101903203100002DEST_PATH_IMAGE010
Table 11 solvent samples 3 and white oil, dimethyl carbonate and dimethylbenzene contrast the result pyrethrin pesticide solvability and stability test thereof.
Figure 2013101903203100002DEST_PATH_IMAGE011
The no test data of "-" expression in the table.
Last table data show that 3 pairs of each quasi-chrysanthemum ester class active components of solvent samples have fine solubility, and lytic activity component ability and dimethylbenzene are suitable, are better than dimethyl carbonate.Use 5% deltamethrin milk oil of solvent samples 3 preparations and be better than dimethylbenzene or dimethyl carbonate sample as solvent with content chrysanthemum ester class aqueous emulsion stability, and it is single poor owing to solubility property with white oil, with solvent samples 3 same amount situations under, promptly add 50% white oil in the prescription because can't the lytic activity component, can't prepare 5% deltamethrin milk oil.
5% deltamethrin milk oil (control sample 3) carries out the biologically active drug effect relatively with 5% deltamethrin milk oil (sample 3), test period in June, 2012, test site: suburb, county, Yongning, Guangxi, active ingredient usage amount: 18g/ hectare, occupation mode: convert water spray, controlling object: Chinese cabbage-cabbage caterpillar, result of the test such as following table.
The computing formula of control efficiency: the computing formula of control efficiency: insect population insect population number * 100 before rate (%)=(medicine before insect population number-medicine after insect population number)/medicine of going down
Preventive effect (%)=(the chemicals treatment district insect population rate of going down-blank district insect population go down rate)/(100-blank district insect population go down rate) * 100.
Table 12 5% deltamethrin milk oil (control sample 3) compares with 5% deltamethrin milk oil (sample 3) drug effect
Figure 2013101903203100002DEST_PATH_IMAGE012
As can be seen from the above table, sample 3 is better or suitable with control sample 3 control Chinese cabbage-cabbage caterpillars.
Above-mentioned table 9~12 show, 5% decis of solvent-applied sample 3 preparations and other chrysanthemum ester class missible oil ageing stabilities are better than the sample of dimethylbenzene or dimethyl carbonate preparation in the implementation column 3, solvent samples 3 dissolving chrysanthemum ester class abilities and dimethylbenzene are equal to or slightly better, and are better than dimethyl carbonate or white oil.5% deltamethrin milk oil control Chinese cabbage-cabbage caterpillar drug effect that biological activity determination shows solvent samples 3 and dimethylbenzene preparation quite or better.In sum, it is feasible that solvent samples 3 alternative dimethylbenzene are applied to chrysanthemum ester class aqueous emulsion, and its solvent cost is low, and toxicity is low.
Embodiment 4:
Solvent samples 4: take by weighing dimethyl carbonate 59.7kg, white oil 40.3kg respectively, stir then and promptly get the solvent compositions that 100kg originally executes example.
5% fenvalerate missible oil (sample 4)
Each constituent mass percentage in the prescription: 95% sumicidin: 5%, solvent samples 67%(is equivalent to add dimethyl carbonate 40%, white oil 27% in this product), alkylaryl polyoxyethylene polyoxypropylene ether 4%,, phenethyl phenol polyethenoxy sodium sulphate 6%, methyl oleate complements to 100%.
Sumicidin in the top example is also replaceable to be the formulation products of beta-cypermethrin, cypermethrin, gamma cyhalothrin, decis, cyfluthrin and Biphenthrin.
5% fenvalerate missible oil (control sample 4)
Each constituent mass percentage in the prescription: 95% sumicidin: 5%, dimethylbenzene 67%, alkylaryl polyoxyethylene polyoxypropylene ether 4%,, phenethyl phenol polyethenoxy sodium sulphate 6%, methyl oleate complements to 100%.
Above sample is store test of preceding assay, normal temperature ageing stability and heat storage test simultaneously, and heat storage sample design temperature in baking oven is 54 ± 2 ℃ and places 14 days, normal temperature sample and place 12,18 and 24 months respectively.Adopt gas chromatography to store preceding sample, heat storage sample and the normal temperature of different periods through the time storage sample in the content of sumicidin measure, and calculate its resolution ratio, measurement result sees Table 13, and the test data in the table is all to get result of the test mean value more than 10 times.
The stability test result of active component in table 13 5% fenvalerate missible oil
Figure 2013101903203100002DEST_PATH_IMAGE013
Above-mentioned result of the test shows that sample 4 is promptly with dimethyl carbonate 40%, and the dicyandiamide solution of white oil 27%, the ageing stability of sample 4 are better than with dimethylbenzene 67%, and methyl oleate is supplied the sample into solvent.
All other technical indicators of table 14 sample 4
Figure 2013101903203100002DEST_PATH_IMAGE014
Table 15 solvent samples 4 contrasts the result pyrethrin pesticide solvability and stability test thereof with white oil, dimethyl carbonate and dimethylbenzene.
Figure 2013101903203100002DEST_PATH_IMAGE015
The no test data of "-" expression in the table.
Last table data show that 4 pairs of each quasi-chrysanthemum ester class active components of solvent samples have fine solubility, and lytic activity component ability and dimethylbenzene are suitable, are better than dimethyl carbonate.Use 5% fenvalerate missible oil of solvent samples 4 preparations and be better than dimethylbenzene and dimethyl carbonate sample as solvent with content chrysanthemum ester class aqueous emulsion stability, and it is single poor owing to solubility property with white oil, with solvent samples 3 same amount situations under, promptly add 67% white oil in the prescription because can't the lytic activity component, can't prepare 5% fenvalerate missible oil.
5% fenvalerate missible oil (control sample 4) carries out the biologically active drug effect relatively with 5% fenvalerate missible oil (sample 4), test period in June, 2012, test site: Zhuhai City, Guangdong Province sluice gate county, active ingredient usage amount: 40g/ hectare, occupation mode: convert water spray, controlling object: soybean-aphid, result of the test such as following table 16.
The computing formula of control efficiency: insect population insect population number * 100 before rate (%)=(medicine before insect population number-medicine after insect population number)/medicine of going down.
Preventive effect (%)=(the chemicals treatment district insect population rate of going down-blank district insect population go down rate)/(100-blank district insect population go down rate) * 100
Table 16 5% fenvalerate missible oil (control sample 4) and 5% sumicidin (sample 4) are to control soybean aphid drug effect result
As can be seen from the above table, sample 4 comparison in the same old way product 4 control soybean aphids effect better or quite.
Above-mentioned table 14~16 show, 5% deltamethrin milk oil of solvent-applied sample 4 preparations and other chrysanthemum ester class missible oil ageing stabilities are better than the sample of dimethylbenzene or dimethyl carbonate preparation in the implementation column 4, solvent samples 4 dissolving chrysanthemum ester class abilities and dimethylbenzene are equal to or slightly better, and are better than dimethyl carbonate or white oil.5% deltamethrin milk oil control soybean-aphid drug effect that biological activity determination shows solvent samples 4 and dimethylbenzene preparation quite or better.In sum, it is feasible that solvent samples 4 alternative dimethylbenzene are applied to chrysanthemum ester class aqueous emulsion, and its solvent cost is low, and toxicity is low.
Embodiment 5:
Solvent samples 5: take by weighing dimethyl carbonate 95kg, white oil 5kg respectively, stir then and promptly get the solvent compositions that 100kg originally executes example.
2.5% cyfluthrin aqueous emulsion (sample 5)
Each constituent mass percentage in the prescription: the former medicine of 95% cyfluthrin: 2.5%, solvent samples 10%(is equivalent to add dimethyl carbonate 9.5%, white oil 0.5% in this product), fatty alcohol-polyoxyethylene ether 3%, polycarboxylate 2%, ethylene glycol 3%, defoamer 0.05%, water complement to 100%.
Cyfluthrin in the top example is also replaceable to be the formulation products of beta-cypermethrin, cypermethrin, gamma cyhalothrin, decis, sumicidin and Biphenthrin.
2.5% cyfluthrin aqueous emulsion (control sample 5)
Each constituent mass percentage in the prescription: the former medicine of 95% cyfluthrin: 2.5%, dimethylbenzene 10%, fatty alcohol-polyoxyethylene ether 3%, polycarboxylate 2%, ethylene glycol 3%, defoamer 0.05%, water complement to 100%.
Above sample is store test of preceding assay, normal temperature ageing stability and heat storage test simultaneously, and heat storage sample design temperature in baking oven is 54 ± 2 ℃ and places 14 days, normal temperature sample and place 12,18 and 24 months respectively.Adopt high performance liquid chromatography to store preceding sample, heat storage sample and the normal temperature of different periods through the time storage sample in the content of cyfluthrin measure, and calculate its resolution ratio, measurement result sees Table 17, and the test data in the table is all to get result of the test mean value more than 10 times.
The stability test result of active component in the table 17 2.5% cyfluthrin aqueous emulsion
Figure 2013101903203100002DEST_PATH_IMAGE017
Above-mentioned result of the test shows that sample 5 is promptly with dimethyl carbonate 9.5%, and it is the sample of solvent that the dicyandiamide solution of white oil 0.5%, the ageing stability of sample 5 are better than with dimethylbenzene 10%.
All other technical indicators of table 18 sample 5
Figure 2013101903203100002DEST_PATH_IMAGE018
Table 19 solvent samples 5 contrasts the result pyrethrin pesticide solvability and stability test thereof with white oil, dimethyl carbonate, dimethylbenzene.
Figure 2013101903203100002DEST_PATH_IMAGE019
The no test data of "-" expression in the table.
Last table data show that 5 pairs of each quasi-chrysanthemum ester class active components of solvent samples have fine solubility, and lytic activity component ability and dimethylbenzene are suitable, are better than dimethyl carbonate.Use 2.5% cyfluthrin aqueous emulsion of solvent samples 5 preparations and be better than dimethylbenzene or dimethyl carbonate sample as solvent with content chrysanthemum ester class aqueous emulsion stability, and it is single poor owing to solubility property with white oil, with solvent samples 5 same amount situations under, promptly add 10% white oil in the prescription because can't the lytic activity component, can't prepare 2.5% cyfluthrin aqueous emulsion.
2.5% cyfluthrin aqueous emulsion (control sample 5) carries out the biologically active drug effect relatively with 2.5% cyfluthrin aqueous emulsion (sample 5), test period in June, 2012, test site: heart country fair town, Nanning City field of vegetables, active ingredient usage amount: 20g/ hectare, occupation mode: convert water spray, controlling object: wild cabbage-cabbage caterpillar, result of the test such as following table 20.
The computing formula of control efficiency: insect population insect population number * 100 before rate (%)=(medicine before insect population number-medicine after insect population number)/medicine of going down.
Preventive effect (%)=(the chemicals treatment district insect population rate of going down-blank district insect population go down rate)/(100-blank district insect population go down rate) * 100.
Table 20 2.5% cyfluthrin aqueous emulsion (control sample 5) and 2.5% cyfluthrin aqueous emulsion (sample 5) drug effect comparative result.
Figure 2013101903203100002DEST_PATH_IMAGE021
As can be seen from the above table, sample 5 comparison in the same old way product 5 control wild cabbage-cabbage caterpillars effect better or quite.
Above-mentioned table 17~20 show, 2.5% cyfluthrin aqueous emulsion of solvent-applied sample 5 preparations and other chrysanthemum ester class aqueous emulsion ageing stabilities are better than the sample of dimethylbenzene or dimethyl carbonate preparation in the implementation column 5, solvent samples 5 dissolving chrysanthemum ester class abilities and dimethylbenzene are equal to or slightly better, and are better than dimethyl carbonate and white oil.2.5% cyfluthrin aqueous emulsion control wild cabbage-cabbage caterpillar drug effect that biological activity determination shows solvent samples 5 and dimethylbenzene preparation quite or better.In sum, it is feasible that solvent samples 5 alternative dimethylbenzene are applied to chrysanthemum ester class aqueous emulsion, and its solvent cost is low, and toxicity is low.
Embodiment 6:
Solvent samples 6: take by weighing dimethyl carbonate 50kg, white oil 50kg respectively, stir then and promptly get the solvent compositions that 100kg originally executes example.
5% gamma cyhalothrin aqueous emulsion (sample 6)
Each constituent mass percentage in the prescription: the former medicine of 95% gamma cyhalothrin: 5%, solvent samples 10%(is equivalent to add dimethyl carbonate 5%, white oil 5% in this product), alkylphenol polyoxyethylene 3%, nonyl phenol polyethenoxy ether phosphate 2%, glycerine 3%, defoamer 0.05%, water complement to 100%.
Gamma cyhalothrin in the top example is also replaceable to be the formulation products of beta-cypermethrin, cypermethrin, decis, sumicidin, cyfluthrin and Biphenthrin.
5% gamma cyhalothrin aqueous emulsion (control sample 6)
Each constituent mass percentage in the prescription: the former medicine of 95% gamma cyhalothrin: 5%, dimethylbenzene 10%, and alkylphenol polyoxyethylene 3%, nonyl phenol polyethenoxy ether phosphate 2%, glycerine 3%, defoamer 0.05%, water complement to 100%.
Above sample is store test of preceding assay, normal temperature ageing stability and heat storage test simultaneously, and heat storage sample design temperature in baking oven is 54 ± 2 ℃ and places 14 days, normal temperature sample and place 12,18 and 24 months respectively.Adopt high performance liquid chromatography to store preceding sample, heat storage sample and the normal temperature of different periods through the time storage sample in the content of gamma cyhalothrin measure, and calculate its resolution ratio, measurement result sees Table 21, and the test data in the table is all to get result of the test mean value more than 10 times.
The stability test result of active component in the table 21 5% gamma cyhalothrin aqueous emulsion
。Above-mentioned result of the test shows that sample 6 is promptly with dimethyl carbonate 5%, and it is the sample of solvent that the dicyandiamide solution of white oil 5%, the ageing stability of sample 6 are better than with dimethylbenzene 10%.
All other technical indicators of table 22 sample 6
Table 23 solvent samples 6 contrasts the result pyrethrin pesticide solvability and stability test thereof with white oil, dimethyl carbonate, dimethylbenzene.
Figure 2013101903203100002DEST_PATH_IMAGE024
The no test data of "-" expression in the table.
Last table data show that 6 pairs of each quasi-chrysanthemum ester class active components of solvent samples have fine solubility, and lytic activity component ability and dimethylbenzene are suitable, are better than dimethyl carbonate.Use 5% gamma cyhalothrin aqueous emulsion of solvent samples 6 preparations and be better than dimethylbenzene or dimethyl carbonate sample as solvent with content chrysanthemum ester class aqueous emulsion stability, and it is single poor owing to solubility property with white oil, with solvent samples 6 same amount situations under, promptly add 10% white oil in the prescription because can't the lytic activity component, can't prepare 5% gamma cyhalothrin aqueous emulsion.
5% gamma cyhalothrin aqueous emulsion (control sample 6) carries out the biologically active drug effect relatively with 5% gamma cyhalothrin aqueous emulsion (sample 6), test period in June, 2012, test site: Anxi County suburb, Fujian, active ingredient usage amount: 27g/ hectare, occupation mode: convert water spray, controlling object: tea tree-tea lesser leafhopper, result of the test such as following table 24.
The computing formula of control efficiency: insect population insect population number * 100 before rate (%)=(medicine before insect population number-medicine after insect population number)/medicine of going down.
Preventive effect (%)=(the chemicals treatment district insect population rate of going down-blank district insect population go down rate)/(100-blank district insect population go down rate) * 100.
Table 24 5% gamma cyhalothrin aqueous emulsion (control sample 6) compares with 5% gamma cyhalothrin aqueous emulsion (sample 6) drug effect result
Figure 2013101903203100002DEST_PATH_IMAGE025
As can be seen from the above table, sample 6 comparison in the same old way product 6 control tea tree-tea lesser leafhoppers effect better or quite.
Above-mentioned table 21~24 show, 5% gamma cyhalothrin aqueous emulsion of solvent-applied sample 6 preparations and other chrysanthemum ester class aqueous emulsion ageing stabilities are better than the sample of dimethylbenzene or dimethyl carbonate preparation in the implementation column 6, solvent samples 6 dissolving chrysanthemum ester class abilities and dimethylbenzene are equal to or slightly better, and are better than dimethyl carbonate and white oil.5% gamma cyhalothrin aqueous emulsion control tea tree-tea lesser leafhopper drug effect that biological activity determination shows solvent samples 6 and dimethylbenzene preparation quite or better.In sum, it is feasible that solvent samples 6 alternative dimethylbenzene are applied to chrysanthemum ester class aqueous emulsion, and its solvent cost is low, and toxicity is low.
Embodiment 7:
Solvent samples 7: take by weighing dimethyl carbonate 52kg, white oil 48kg respectively, stir then and promptly get the solvent compositions that 100kg originally executes example.
10% cypermethrin microemulsion (sample 7)
Each constituent mass percentage in the prescription: 95% cypermethrin technical material: 10%, solvent samples 25%(is equivalent to add dimethyl carbonate 13% in this product, white oil 12%), fatty alcohol-polyoxyethylene ether 6%, dodecyl benzoic acid calcium 4%, castor oil polyoxyethylene ether 5%, isopropyl alcohol 3%, defoamer 0.05%, water complement to 100%.
Cypermethrin in the top example is also replaceable to be the formulation products of beta-cypermethrin, gamma cyhalothrin, decis, sumicidin, cyfluthrin and Biphenthrin.
10% cypermethrin microemulsion (control sample 7)
Each constituent mass percentage in the prescription: 95% cypermethrin technical material: 10%, dimethylbenzene 25%(is equivalent to add dimethyl carbonate 13% in this product, white oil 12%), fatty alcohol-polyoxyethylene ether 6%, dodecyl benzoic acid calcium 4%, castor oil polyoxyethylene ether 5%, isopropyl alcohol 3%, defoamer 0.05%, water complement to 100%.
Above sample is store test of preceding assay, normal temperature ageing stability and heat storage test simultaneously, and heat storage sample design temperature in baking oven is 54 ± 2 ℃ and places 14 days, normal temperature sample and place 12,18 and 24 months respectively.Adopt gas chromatography to store preceding sample, heat storage sample and the normal temperature of different periods through the time storage sample in the content of cypermethrin measure, and calculate its resolution ratio, measurement result sees Table 25, and the test data in the table is all to get result of the test mean value more than 10 times.
The stability test result of active component in the table 25 10% cypermethrin microemulsion
Above-mentioned result of the test shows that sample 7 is promptly with dimethyl carbonate 13%, and white oil 12% is a dicyandiamide solution, and it is the sample of solvent that the ageing stability of sample 7 is better than with dimethylbenzene 25%.
All other technical indicators of table 26 sample 7
Figure 2013101903203100002DEST_PATH_IMAGE027
Table 27 solvent samples 7 contrasts the result pyrethrin pesticide solvability and stability test thereof with white oil, dimethylbenzene.
Figure 2013101903203100002DEST_PATH_IMAGE028
The no test data of "-" expression in the table.
Last table data show that 7 pairs of each quasi-chrysanthemum ester class active components of solvent samples have fine solubility, and lytic activity component ability and dimethylbenzene are suitable, are better than dimethyl carbonate.Use 10% cypermethrin microemulsion of solvent samples 7 preparations and be better than dimethylbenzene or dimethyl carbonate sample as solvent with content chrysanthemum ester class aqueous emulsion stability, and it is single poor owing to solubility property with white oil, with solvent samples 7 same amount situations under, promptly add 25% white oil in the prescription because can't the lytic activity component, can't prepare 10% cypermethrin microemulsion.
10% aqueous emulsion of cypermethrin (control sample 7) carries out the biologically active drug effect relatively with 10% aqueous emulsion of cypermethrin (sample 7), test period in June, 2012, test site: Guiping County, Guigang, Guangxi, active ingredient usage amount: 50g/ hectare, occupation mode: convert water spray, controlling object: wild cabbage-cabbage caterpillar, result of the test such as following table 28.
The computing formula of control efficiency: insect population insect population number * 100 before rate (%)=(medicine before insect population number-medicine after insect population number)/medicine of going down.
Preventive effect (%)=(the chemicals treatment district insect population rate of going down-blank district insect population go down rate)/(100-blank district insect population go down rate) * 100.
Table 28 10% aqueous emulsion of cypermethrin (control sample 7) compares with 10% aqueous emulsion of cypermethrin (sample 7) drug effect
Figure 2013101903203100002DEST_PATH_IMAGE029
As can be seen from the above table, sample 7 comparison in the same old way product 7 control wild cabbage-cabbage caterpillars effect better or quite.
Above-mentioned table 25~28 show, 10% aqueous emulsion of cypermethrin of solvent-applied sample 7 preparations and other chrysanthemum ester class aqueous emulsion ageing stabilities are better than the sample of dimethylbenzene and dimethyl carbonate preparation in the implementation column 7, solvent samples 7 dissolving chrysanthemum ester class abilities and dimethylbenzene are equal to or slightly better, and are better than dimethyl carbonate and white oil.10% aqueous emulsion of cypermethrin control wild cabbage-cabbage caterpillar drug effect that biological activity determination shows solvent samples 7 and dimethylbenzene preparation quite or better.In sum, it is feasible that solvent samples 7 alternative dimethylbenzene are applied to chrysanthemum ester class aqueous emulsion, and its solvent cost is low, and toxicity is low.
Embodiment 8:
Solvent samples 8: take by weighing dimethyl carbonate 60kg, white oil 40kg respectively, stir then and promptly get the solvent compositions that 100kg originally executes example.
4.5% r (sample 8)
Each constituent mass percentage in the prescription: the former medicine of 95% beta-cypermethrin: 4.5%, solvent samples 50%(is equivalent to add dimethyl carbonate 30%, white oil 20% in this product), fatty alcohol-polyoxyethylene ether 5%, calcium dodecyl benzene sulfonate 5%, methyl oleate supply.
Beta-cypermethrin in the top example is also replaceable to be the formulation products of cyfluthrin, gamma cyhalothrin, decis, sumicidin and Biphenthrin.
4.5% r (control sample 8)
Each constituent mass percentage in the prescription: the former medicine of 95% beta-cypermethrin: 4.5%, dimethylbenzene 50%, fatty alcohol-polyoxyethylene ether 5%, calcium dodecyl benzene sulfonate 5%, methyl alcohol are supplied.
Above sample is store test of preceding assay, normal temperature ageing stability and heat storage test simultaneously, and heat storage sample design temperature in baking oven is 54 ± 2 ℃ and places 14 days, normal temperature sample and place 12,18 and 24 months respectively.With reference to rower HG3631-1999 adopt high performance liquid chromatography to store preceding sample, heat storage sample and the normal temperature of different periods through the time storage sample in the content of beta-cypermethrin measure, and calculate its resolution ratio, measurement result sees Table 29, and the test data in the table is all to get result of the test mean value more than 10 times.
The stability test result of active component in table 29 4.5% r
Figure 2013101903203100002DEST_PATH_IMAGE030
Above-mentioned result of the test shows that sample 8 is promptly with dimethyl carbonate 30%, and it is the sample of solvent that the dicyandiamide solution of white oil 20%, the ageing stability of sample 8 are better than with dimethylbenzene 50%.
All other technical indicators of table 30 sample 8
Figure 2013101903203100002DEST_PATH_IMAGE031
Table 31 sample 8 contrasts the result pyrethrin pesticide solvability and stability test thereof with white oil, dimethyl carbonate and dimethylbenzene.
The no test data of "-" expression in the table.
Last table data show that 8 pairs of each quasi-chrysanthemum ester class active components of solvent samples have fine solubility, and lytic activity component ability and dimethylbenzene are suitable, are better than dimethyl carbonate.Use 4.5% r of solvent samples 8 preparations and be better than dimethylbenzene or dimethyl carbonate sample as solvent with content chrysanthemum ester class aqueous emulsion stability, and it is single poor owing to solubility property with white oil, with solvent samples 8 same amount situations under, promptly add 50% white oil in the prescription because can't the lytic activity component, can't prepare 4.5% r.
4.5% r (control sample 8) and 4.5% r (sample 8) carry out the biologically active drug effect relatively, test period in June, 2012, test site: Yunnan Province's mountain of papers, active ingredient usage amount: 20g/hectare, occupation mode: convert water spray, controlling object: tobacco-oriental tobacco budworm, result of the test such as following table.
The computing formula of control efficiency: insect population insect population number * 100 before rate (%)=(medicine before insect population number-medicine after insect population number)/medicine of going down.
Preventive effect (%)=(the chemicals treatment district insect population rate of going down-blank district insect population go down rate)/(100-blank district insect population go down rate) * 100.
Table 32 4.5% r (control sample 8) and 4.5% r (sample 8) drug effect are relatively
As can be seen from the above table, sample 8 comparison in the same old way product 8 control tobacco-oriental tobacco budworms effect better or quite.
Above-mentioned table 29~32 show, 4.5% r of solvent-applied sample 8 preparations and other chrysanthemum ester class missible oil ageing stabilities are better than the sample of dimethylbenzene or dimethyl carbonate preparation in the implementation column 8, solvent samples 8 dissolving chrysanthemum ester class abilities and dimethylbenzene are equal to or slightly better, and are better than dimethyl carbonate and white oil.4.5% r control tobacco-oriental tobacco budworm drug effect that biological activity determination shows solvent samples 8 and dimethylbenzene preparation quite or better.In sum, it is feasible that solvent samples 8 alternative dimethylbenzene are applied to chrysanthemum ester class missible oil, and its solvent cost is low, and toxicity is low.
Embodiment 9:
Solvent samples 9: take by weighing dimethyl carbonate 75kg, white oil 25kg respectively, stir then and promptly get the solvent compositions that 100kg originally executes example.
2.5% efficient cyhalothrin emulsifiable concentrate (sample 9)
Each constituent mass percentage in the prescription: the former medicine of 95% gamma cyhalothrin: 2.5%, solvent samples 80%(is equivalent to add dimethyl carbonate 60%, white oil 20% in this product), polyoxyethylene nonylphenol ether 5%, calcium dodecyl benzene sulfonate 3%, methyl oleate complement to 100%.
Gamma cyhalothrin in the top example is also replaceable to be the formulation products of beta-cypermethrin, cypermethrin, cyfluthrin, decis, sumicidin and cyfluthrin.
2.5% efficient cyhalothrin emulsifiable concentrate (control sample 9)
Each constituent mass percentage in the prescription: the former medicine of 95% gamma cyhalothrin: 2.5%, dimethylbenzene 80%, polyoxyethylene nonylphenol ether 5%, calcium dodecyl benzene sulfonate 3%, methyl alcohol complement to 100%.
Above sample is store test of preceding assay, normal temperature ageing stability and heat storage test simultaneously, and heat storage sample design temperature in baking oven is 54 ± 2 ℃ and places 14 days, normal temperature sample and place 12,18 and 24 months respectively.With high performance liquid chromatography to store preceding sample, heat storage sample and the normal temperature of different periods through the time storage sample in the content of gamma cyhalothrin measure, and calculate its resolution ratio, measurement result sees Table 33, and the test data in the table is all to get result of the test mean value more than 10 times.
The stability test result of active component in table 33 2.5% efficient cyhalothrin emulsifiable concentrate
Above-mentioned result of the test shows that sample 9 is promptly with dimethyl carbonate 60%, and it is the sample of solvent that the dicyandiamide solution of white oil 20%, the ageing stability of sample 9 are better than with dimethylbenzene 80%.
All other technical indicators of table 34 sample 9
Figure 2013101903203100002DEST_PATH_IMAGE035
Table 35 solvent samples 9 contrasts the result pyrethrin pesticide solvability and stability test thereof with white oil, dimethyl carbonate and dimethylbenzene.
Figure 2013101903203100002DEST_PATH_IMAGE036
The no test data of "-" expression in the table.
Last table data show that 9 pairs of each quasi-chrysanthemum ester class active components of solvent samples have fine solubility, and lytic activity component ability and dimethylbenzene are suitable, are better than dimethyl carbonate.Use 2.5% efficient cyhalothrin emulsifiable concentrate of solvent samples 9 preparations and be better than dimethylbenzene or dimethyl carbonate sample as solvent with content chrysanthemum ester class aqueous emulsion stability, and it is single poor owing to solubility property with white oil, with solvent samples 9 same amount situations under, promptly add 80% white oil in the prescription because can't the lytic activity component, can't prepare 2.5% efficient cyhalothrin emulsifiable concentrate.
2.5% efficient cyhalothrin emulsifiable concentrate (control sample 9) carries out the biologically active drug effect relatively with 2.5% efficient cyhalothrin emulsifiable concentrate (sample 9), test period in August, 2012, test site: heart Xu Zhen farmland, high and new technology industrial development zone, Nanning, active ingredient usage amount: 9.4g/ hectare, occupation mode: convert water spray, controlling object: wild cabbage-cabbage caterpillar, result of the test such as following table.
The computing formula of control efficiency: insect population insect population number * 100 before rate (%)=(medicine before insect population number-medicine after insect population number)/medicine of going down.
Preventive effect (%)=(the chemicals treatment district insect population rate of going down-blank district insect population go down rate)/(100-blank district insect population go down rate) * 100.
Table 36 2.5% efficient cyhalothrin emulsifiable concentrate (control sample 9) compares with 2.5% efficient cyhalothrin emulsifiable concentrate (sample 9) drug effect
Figure 2013101903203100002DEST_PATH_IMAGE037
As can be seen from the above table, sample 9 comparison in the same old way product 9 control cabbage pieris effect better or quite.
Above-mentioned table 33~36 show, 2.5% efficient cyhalothrin emulsifiable concentrate of solvent-applied sample 9 preparations and other chrysanthemum ester class missible oil ageing stabilities are better than the sample of dimethylbenzene or dimethyl carbonate preparation in the implementation column 9, solvent samples 9 dissolving chrysanthemum ester class abilities and dimethylbenzene are equal to or slightly better, and are better than dimethyl carbonate and white oil.2.5% efficient cyhalothrin emulsifiable concentrate control wild cabbage-cabbage caterpillar drug effect that biological activity determination shows solvent samples 9 and dimethylbenzene preparation quite or better.In sum, it is feasible that solvent samples 9 alternative dimethylbenzene are applied to chrysanthemum ester class aqueous emulsion, and its solvent cost is low, and toxicity is low.
In sum, dimethyl carbonate and white oil applied in any combination are very good in pyrethrin pesticide liquor preparation effect, solvability and dimethylbenzene, dimethyl carbonate, white oil list are with getting well or quite, and chrysanthemum ester class active component good stability in this mixed solvent system, solvent cost is low, toxicity is low, produces and uses safety, and is little to environmental influence.Be current instead of methanol, dimethylbenzene and N, dinethylformamide is the development trend of the solvent of conventional pesticide preparation.

Claims (9)

1. an environmental protection mixed solvent that is used for the pyrethrin pesticide preparation is characterized in that being made up of dimethyl carbonate and white oil, and wherein the mass percent of the shared preparation total amount of each component is:
Dimethyl carbonate 0.5-60%
White oil 0.5-40%.
2. the environmental protection mixed solvent that is used for the pyrethrin pesticide preparation according to claim 1 is characterized in that the preferred mass percentage of dimethyl carbonate and white oil is:
Dimethyl carbonate 10-40%
White oil 5-30%.
3. the environmental protection mixed solvent that is used for the pyrethrin pesticide preparation as claimed in claim 1 or 2 is characterized in that comprising dimethyl carbonate 0.5%, white oil 9.5%; Or dimethyl carbonate 10%, white oil 40%; Or dimethyl carbonate 20%, white oil 30%; Or dimethyl carbonate 40%, white oil 27%; Or dimethyl carbonate 9.5%, white oil 0.5%; Or dimethyl carbonate 5%, white oil 5%; Or dimethyl carbonate 13%, white oil 12%; Or dimethyl carbonate 30%, white oil 20%; Or dimethyl carbonate 60%, white oil 20%.
4. the using method of each described environmental protection mixed solvent of claim 1-3 is characterized in that: described environmental protection mixed solvent and pesticide activity component, the emulsifying dispersant that is used for the pyrethrin pesticide preparation mixed.
5. using method as claimed in claim 4 is characterized in that described pesticide activity component is selected from cypermethrin, beta-cypermethrin, gamma cyhalothrin, decis, sumicidin, cyfluthrin or Biphenthrin.
6. as claim 4 or 5 described usings method, it is characterized in that described emulsifying dispersant is selected from one or more in fatty alcohol-polyoxyethylene ether, polycarboxylate, alkylaryl polyoxyethylene polyoxypropylene ether, nonyl phenol polyethenoxy ether, nonyl phenol polyethenoxy ether phosphate, calcium dodecyl benzene sulfonate, phenethyl phenol polyethenoxy sodium sulphate, the alkylphenol polyoxyethylene.
7. pyrethrin pesticide preparation for preparing as using method as described in the claim 4-6.
8. pyrethrin pesticide preparation as claimed in claim 7, its formulation are missible oil, aqueous emulsion and microemulsion.
9. as the application of each described mixed solvent of claim 1-3 in preparation pyrethrin pesticide preparation.
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