CN103004766B - Fomesafen soluble powder - Google Patents
Fomesafen soluble powder Download PDFInfo
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- CN103004766B CN103004766B CN201210540390.2A CN201210540390A CN103004766B CN 103004766 B CN103004766 B CN 103004766B CN 201210540390 A CN201210540390 A CN 201210540390A CN 103004766 B CN103004766 B CN 103004766B
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Abstract
The invention relates to the field of pesticide preparations and particularly relates to fomesafen soluble powder. The fomesafen soluble powder is prepared from 32-99 parts by weight of fomesafen solid-state salt, 0.2-30 parts by weight of an accessory ingredient and 0.8-70 parts by weight of soluble filler. The soluble powder is solid-state, so that the soluble powder can be packaged by using water-soluble films; and the soluble powder has the advantages of convenience for use, safety, environmental friendliness, low cost and the like and cannot be matched by the existing preparations such as fomesafen 25% water aqua, 12.8% missible oil, 20% missible oil, 20% micro-emulsion and 30% micro-emulsion. The prepared soluble powder has no harm to the environment, is safe to crops and also has the advantages of low package cost and low transportation cost. Moreover, the impurity content in the fomesafen solid-state salt prepared by the preparation method of the fomesafen solid-state salt disclosed by the invention is very low, so that the pesticide effect is prominently enhanced.
Description
Technical field
The present invention relates to field of pesticide preparation, particularly a kind of fomesafen soluble powder.
Background technology
Fomesafen (Fomesafen), chemical name: 5-(2-chloro-trifluoromethyl phenoxy)-N-methylsulfonyl-2-nitrobenzamide.Appearance off-white pulverulent solids, fusing point 218-221 DEG C, vapour pressure <0.1mpa (50 DEG C).The solvability of dissolubility in water depends on the size of pH value, 50mg/L (pH7), and pHl-2 is then less than 1mg/L; Acetone 300g/L; Carrene 10g/L: dimethylbenzene 1.9g/L; Methyl alcohol 20g/L; Acid ph value is about 2.7 (20 DEG C), can generate water soluble salt.Fomesafen structural formula is such as formula shown in I, and fomesafen sodium salt structural formula is such as formula shown in II, and fomesafen sylvite structural formula is such as formula III:
Fomesafen is a kind of diphenyl ether herbicide with high selectivity, be mainly used in preventing and kill off broad leaved weed and the rhizome of nutgrass flatsedge between soybean, Peanut Fields, also certain preventive effect is had to grassy weed, can be absorbed by weeds root leaf, make its rapid withered and yellow death. there is efficient, low toxicity, to features such as crop safeties, extensively welcome by peasant user.
On Vehicles Collected from Market the preparation of fomesafen mainly 25%, 250g/l aqua, that has registered in addition also has 12.8% missible oil, 20% missible oil, 20% microemulsion, 30% microemulsion.Missible oil uses a large amount of organic solvent, there is environmental pollution, easily generation poisoning and stores and transports uneasy congruent shortcoming.Microemulsion existence and stability problem, easily occur the problems such as flocculation, condensation and layering bleed, production cost is high.Fomesafen aqua restricted levels system, because the unstable easily crystallization of fomesafen saline solution, lower content is easy crystallization just, but fomesafen is mainly used in the weeding of northern China Soybean Field, low temperature storing and transporting is easily endured cold crystallization, so fomesafen can only make the aqua of lower content, otherwise easily crystallization impact uses and drug effect.
Above preparation is liquid preparation, and active constituent content is all lower, and production storage and transport cost is comparatively large, and in processing in the former medicine of fomesafen with impurity can affect drug effect, harm environment.
Summary of the invention
In view of this, the invention provides a kind of fomesafen soluble powder.This fomesafen soluble powder is safe from harm to environment, and to Crop securify, and packing cost is low, and cost of transportation is low.
In order to realize foregoing invention object, the invention provides following technical scheme:
The invention provides a kind of fomesafen soluble powder, be made up of the raw material of following weight portion:
Fomesafen solid salt 32 ~ 99 weight portion
Auxiliary agent 0.2 ~ 30 weight portion
Soluble filler 0.8 ~ 66 weight portion.
In other embodiments of the present invention, a kind of fomesafen soluble powder provided by the invention is made up of the raw material of following weight portion:
Fomesafen solid salt 75 ~ 99 weight portion
Auxiliary agent 0.2 ~ 10 weight portion
Soluble filler 0.8 ~ 23 weight portion.
As preferably, fomesafen solid salt is fomesafen sodium or fomesafen potassium.
As preferably, in fomesafen solid salt, the percentage composition of fomesafen is at least 99%.
In order to give full play to the drug effect of active ingredient, ensureing the quality of soluble powder and easy to use, when producing soluble powder, appropriate auxiliary agent can be added.In fomesafen soluble powder provided by the invention, auxiliary agent is nonionic surface active agent and/or ionic surfactant.
As preferably, nonionic surface active agent is a kind of or both the above mixtures in alkylaryl polyoxyethylene ether, aliphatic alcohol polyethenoxy base ether or polyoxyethylene carboxylate.
As preferably, ionic surfactant is anionic surfactant, preferred, anionic surfactant is a kind of or both the above mixtures in alkylbenzenesulfonate, alpha-alkene sulfonate, alkylsulfonate, alpha-sulfo monocarboxylate, fatty acid sulfoalkyl ester, sulphosuccinates, alkyl glyceryl ether sulfonate, alkylnaphthalene sulfonate, lignosulfonates, alkyl phosphoric acid list dibasic acid esters salt, fatty alcohol-polyoxyethylene ether phosphate mono-ester/diester salt, fatty alcohol sulfate salt or secondary alkyl sulphate salt.
In order to ensure soluble powder mobility, storage and stability, soluble filler can be added.In fomesafen soluble powder provided by the invention, soluble filler is sodium sulphate, sodium bicarbonate, natrium carbonicum calcinatum, Anhydrous potassium carbonate, saleratus, ammonium sulfate, sodium chloride, potassium chloride, soluble starch, calcium bicarbonate, pulls open a kind of in powder or urea or both above mixtures.
As preferably, the preparation method of fomesafen solid salt be fomesafen add alkali (as sodium hydroxide or potassium hydroxide) make salting liquid, decrease temperature crystalline, filtration, drying after and get final product;
Crystallization comprises the first crystallization and the second crystallization;
The temperature of the first crystallization is 10 ~ 25 DEG C, and the time of the first crystallization is 4 ~ 8h;
The temperature of the second crystallization is-5 ~ 0 DEG C, and the time of the second crystallization is 2 ~ 6h;
Drying comprises first dry, the second dry and the 3rd drying;
The temperature of the first drying is 20 ~ 30 DEG C, and the time of the first drying is 2 ~ 4h;
The temperature of the second drying is 40 ~ 50 DEG C, and the time of the first drying is 1 ~ 2h;
The temperature of the 3rd drying is 80 ~ 100 DEG C, and the time of the first drying is 1 ~ 2h.
The purity of the fomesafen solid salt obtained by said method is higher, and percentage composition can up to more than 99%.
The invention provides a kind of fomesafen soluble powder, be made up of the soluble filler of the fomesafen solid salt of 32 ~ 99 weight portions, the auxiliary agent of 0.2 ~ 30 weight portion and 0.8 ~ 70 weight portion.Because obtained soluble powder is solid-state, water soluble film can be adopted to pack, having the plurality of advantages such as easy to use, safe, environmental protection, cost are low, is that existing preparation is incomparable at present for fomesafen 25% aqua, 12.8% missible oil, 20% missible oil, 20% microemulsion, 30% microemulsion etc.The soluble powder made, is safe from harm to environment, and to Crop securify, and packing cost is low, and cost of transportation is low.In addition, in the fomesafen solid salt that the preparation method of fomesafen solid salt provided by the invention obtains, impurity content is extremely low, can significantly improve drug effect.
Embodiment
The invention discloses a kind of fomesafen soluble powder, those skilled in the art can use for reference present disclosure, and suitable improving technique parameter realizes.Special needs to be pointed out is, all similar replacements and change apparent to those skilled in the art, they are all deemed to be included in the present invention.Method of the present invention and application are described by preferred embodiment, related personnel obviously can not depart from content of the present invention, spirit and scope methods and applications as herein described are changed or suitably change with combination, realize and apply the technology of the present invention.
In fomesafen soluble powder provided by the invention, raw materials used medicine and auxiliary agent, soluble filler all can be buied by market.
Below in conjunction with embodiment, set forth the present invention further:
The preparation of embodiment 1 fomesafen soluble powder
By solid-state for fomesafen sylvite 99kg(content with 99% calculate), dodecyl sodium sulfate 0.2kg, natrium carbonicum calcinatum 0.8kg, mix and be crushed to 80-100 order, namely obtaining 90% fomesafen soluble powder (in fomesafen).
Use water dissolved dilution during use, water-insoluble is less than 0.5%.
The preparation method of fomesafen solid salt is the aqueous solution that fomesafen hydro-oxidation potassium makes salt, crystallization 4h under the condition of 10 DEG C, filter after crystallization 2h under the condition of-5 DEG C, dry 2h under the condition of 30 DEG C, then dry 1.2h under the condition of 46 DEG C, then under the condition of 90 DEG C after dry 1.5h and get final product.
The preparation of embodiment 2 fomesafen soluble powder
Solid-state for fomesafen sodium salt 95.5kg(content is calculated with 99%), sodium lignin sulfonate 1.5kg, natrium carbonicum calcinatum 3kg mix and be crushed to 80-100 order, obtains 90% fomesafen soluble powder (in fomesafen).Use water dissolved dilution during use, water-insoluble is less than 0.5%.
The preparation method of fomesafen solid salt is the aqueous solution that fomesafen hydro-oxidation sodium makes salt, crystallization 6h under the condition of 15 DEG C, filter after crystallization 4h under the condition of-3 DEG C, dry 4h under the condition of 20 DEG C, then dry 1.5h under the condition of 45 DEG C, then under the condition of 80 DEG C after dry 2h and get final product.
The preparation of embodiment 3 fomesafen soluble powder
Solid-state for fomesafen sodium salt 80kg(content is calculated with 99%), lauryl sodium sulfate 5kg, sodium sulphate 5kg, Anhydrous potassium carbonate 10kg mix and be crushed to 80-100 order, can obtain 75% fomesafen soluble powder (in fomesafen).Use water dissolved dilution during use, water-insoluble is less than 0.5%.
The preparation method of fomesafen solid salt is the aqueous solution that fomesafen hydro-oxidation sodium makes salt, crystallization 8h under the condition of 25 DEG C, filter after crystallization 6h under the condition of 0 DEG C, dry 3h under the condition of 25 DEG C, then dry 1.9h under the condition of 43 DEG C, then under the condition of 100 DEG C after dry 1h and get final product.
The preparation of embodiment 4 fomesafen soluble powder
Solid-state for fomesafen sylvite 50kg(content is calculated with 99%), calcium dodecyl benzene sulfonate 5kg, sodium lignin sulfonate 10kg, calcium bicarbonate 35kg mix and be crushed to 80-100 order, can obtain 45.5% fomesafen soluble powder (in fomesafen).Use water dissolved dilution during use, water-insoluble is less than 0.5%.
The preparation method of fomesafen solid salt is the aqueous solution that fomesafen hydro-oxidation potassium makes salt, crystallization 5h under the condition of 20 DEG C, filter after crystallization 5h under the condition of-2 DEG C, dry 2.5h under the condition of 28 DEG C, then dry 1.2h under the condition of 48 DEG C, then under the condition of 85 DEG C after dry 1.6h and get final product.
The preparation of embodiment 5 fomesafen soluble powder
Solid-state for fomesafen sodium salt 45kg(content is calculated with 99%), calcium dodecyl benzene sulfonate 5kg, sodium lignin sulfonate 10kg, calcium bicarbonate 40kg mix and be crushed to 80-100 order, can obtain 42% fomesafen soluble powder (in fomesafen).Use water dissolved dilution during use, water-insoluble is less than 0.5%.
The preparation method of fomesafen solid salt is the aqueous solution that fomesafen hydro-oxidation sodium makes salt, crystallization 7h under the condition of 23 DEG C, filter after crystallization 3h under the condition of-4 DEG C, dry 3.5h under the condition of 22 DEG C, then dry 1.5h under the condition of 45 DEG C, then under the condition of 95 DEG C after dry 1.2h and get final product.
The preparation of embodiment 6 fomesafen soluble powder
By solid-state for fomesafen sylvite 32kg(content with 99% calculate), α-sodium allylsulfonate 30kg, soluble starch 38kg, mix and be crushed to 80-100 order, namely obtaining 29% fomesafen soluble powder (in fomesafen).
Use water dissolved dilution during use, water-insoluble is less than 0.5%.
The preparation method of fomesafen solid salt is the aqueous solution that fomesafen hydro-oxidation potassium makes salt, crystallization 6h under the condition of 18 DEG C, filter after crystallization 5h under the condition of-1 DEG C, dry 3.7h under the condition of 26 DEG C, then dry 1h under the condition of 50 DEG C, then under the condition of 88 DEG C after dry 1.7h and get final product.
The preparation of embodiment 7 fomesafen soluble powder
Solid-state for fomesafen sylvite 33kg(content is calculated with 99%), fatty alcohol-polyoxyethylene ether phosphate mono-ester/diester sodium 1kg, pull open powder 66kg, mix and be crushed to 80-100 order, namely obtaining 30% fomesafen soluble powder (in fomesafen).
Use water dissolved dilution during use, water-insoluble is less than 0.5%.
The preparation method of fomesafen solid salt is the aqueous solution that fomesafen hydro-oxidation potassium makes salt, crystallization 7h under the condition of 12 DEG C, filter after crystallization 4h under the condition of-2 DEG C, dry 2.8h under the condition of 24 DEG C, then dry 2h under the condition of 40 DEG C, then under the condition of 94 DEG C after dry 1.3h and get final product.
The preparation of embodiment 8 fomesafen soluble powder
By solid-state for fomesafen sylvite 67kg(content with 99% calculate), sodium lignin sulfonate 10kg, calcium bicarbonate 23kg, mix and be crushed to 80-100 order, namely obtaining 61% fomesafen soluble powder (in fomesafen).
Use water dissolved dilution during use, water-insoluble is less than 0.5%.
The preparation method of fomesafen solid salt is the aqueous solution that fomesafen hydro-oxidation potassium makes salt, crystallization 6h under the condition of 15 DEG C, filter after crystallization 5h under the condition of-5 DEG C, dry 3h under the condition of 25 DEG C, then dry 2h under the condition of 40 DEG C, then under the condition of 95 DEG C after dry 1.5h and get final product.
Embodiment 9 field control effectiveness test
The fomesafen soluble powder of embodiment 1-5 and 25% commercially available fomesafen aqua, 30% fomesafen microemulsion, 20% Fluosulfonamide oxalether cream are carried out the contrast controlling experiment of Soybean Field broad leaved weed, experimental condition, environment facies are same.Trial crops is: soybean (No. 43, Heihe); Test site is Heilongjiang Province, and experimental field soil property is black earth, and PH is 6.1, and the content of organic matter is about 6.67%, and front stubble is wheat; Field broad leaved weed is mainly: lamb's-quarters, acalypha copperleaf, dayflower, black nightshade; In large bean seedlings 2-3 leaf phase, broad leaved weed 2-5 leaf phase, cauline leaf process, artificial dispenser, adopts Shandong bodyguard's board WS-16 type manual sprayer, U.S. Teejet80015 type Fan spray head, an atomisation pressure 3-4 atmospheric pressure, spouting liquid 150 liters/hectare; Dispenser was fine for the same day, temperature 22.8 DEG C, south wind 2 grades, relative moisture 48%.15 days, the 30 days residual careless quantity of investigation after medicine, each community 3 point, often some 1m
2, fixed point investigation, calculating preventive effect of averaging.Repeat 4 times.
The remaining careless number of control efficiency %=(blank district careless number-treatment region alive) the remaining careless number of * 100/(blank district careless number-treatment region alive).
Table 1 Soybean Field broad leaved weed control efficiency
Security survey: observe after large bean seedlings, after each chemicals treatment, blade, the base of leaf of soybean have no significant change.Survey and produce result:
Table 2 soybean yields and quality
The large beans of each preparation process is heavy, 100-grain weight difference is little.
Interpretation of result: as can be seen from Table 1, in same consumption situation, the preventive effect of embodiment 1 to 5 chemicals treatment is apparently higher than contrast agents 25% fomesafen aqua, 30% fomesafen microemulsion, 20% Fluosulfonamide oxalether cream.As can be seen from Table 2, the soybean yields after embodiment 1 to 5 chemicals treatment is higher than contrast agents, and higher than artificial weeding, volume increase obviously.
The fomesafen soluble powder adopting above-mentioned test method obtained to embodiment 6 to 8 provided by the invention carries out field control effectiveness test discovery, the preventive effect of the fomesafen soluble powder that embodiment 6 to 8 provided by the invention is obtained and the fomesafen soluble powder that the embodiment of the present invention 1 to 5 provides is close, compared with control group, preventive effect has significant difference; Investigation result display is carried out to the Quality and yield of soybean, the effect of increasing production of the fomesafen soluble powder that embodiment 6 to 8 provided by the invention is obtained and the fomesafen soluble powder that the embodiment of the present invention 1 to 5 provides is close, soybean yields after embodiment 6 to 8 chemicals treatment is higher than contrast agents, higher than artificial weeding, volume increase obviously.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be considered as protection scope of the present invention.
Claims (8)
1. a fomesafen soluble powder, is characterized in that, is made up of the raw material of following weight portion:
Fomesafen solid salt 32 ~ 99 weight portion
Auxiliary agent 0.2 ~ 30 weight portion
Soluble filler 0.8 ~ 66 weight portion;
The preparation method of described fomesafen solid salt is after fomesafen adds alkali salify, crystallization, filtration, after drying and get final product;
Described crystallization comprises the first crystallization and the second crystallization;
The temperature of described first crystallization is 10 ~ 25 DEG C, and the time of described first crystallization is 4 ~ 8h;
The temperature of described second crystallization is-5 ~ 0 DEG C, and the time of described second crystallization is 2 ~ 6h;
Described drying comprises first dry, the second dry and the 3rd drying;
The temperature of described first drying is 20 ~ 30 DEG C, and the time of described first drying is 2 ~ 4h;
The temperature of described second drying is 40 ~ 50 DEG C, and the time of described second drying is 1 ~ 2h;
The temperature of described 3rd drying is 80 ~ 100 DEG C, and the time of described 3rd drying is 1 ~ 2h.
2. fomesafen soluble powder according to claim 1, is characterized in that, is made up of the raw material of following weight portion:
Fomesafen solid salt 75 ~ 99 weight portion
Auxiliary agent 0.2 ~ 10 weight portion
Soluble filler 0.8 ~ 23 weight portion.
3. fomesafen soluble powder according to claim 1 and 2, is characterized in that, described fomesafen solid salt is fomesafen sodium or fomesafen potassium.
4. fomesafen soluble powder according to claim 1 and 2, is characterized in that, the purity of described fomesafen solid salt is at least 99%.
5. fomesafen soluble powder according to claim 1 and 2, is characterized in that, described auxiliary agent is nonionic surface active agent and/or ionic surfactant.
6. fomesafen soluble powder according to claim 5, it is characterized in that, described nonionic surface active agent is a kind of or both the above mixtures in alkylaryl polyoxyethylene ether, aliphatic alcohol polyethenoxy base ether or polyoxyethylene carboxylate.
7. fomesafen soluble powder according to claim 5, it is characterized in that, described ionic surfactant is anionic surfactant, described anionic surfactant is alkylbenzenesulfonate, alpha-alkene sulfonate, alkylsulfonate, alpha-sulfo monocarboxylate, fatty acid sulfoalkyl ester, sulphosuccinates, alkyl glyceryl ether sulfonate, alkylnaphthalene sulfonate, lignosulfonates, alkyl phosphoric acid list dibasic acid esters salt, fatty alcohol-polyoxyethylene ether phosphate mono-ester/diester salt, a kind of or both above mixtures in fatty alcohol sulfate salt or secondary alkyl sulphate salt.
8. fomesafen soluble powder according to claim 1 and 2, it is characterized in that, described soluble filler is sodium sulphate, sodium bicarbonate, natrium carbonicum calcinatum, Anhydrous potassium carbonate, saleratus, ammonium sulfate, sodium chloride, potassium chloride, soluble starch, pull open a kind of in powder or urea or both above mixtures.
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| CN106386794A (en) * | 2016-08-31 | 2017-02-15 | 江苏长青生物科技有限公司 | High-content fomesafen aqueous solution and preparation method thereof |
| CN107593733A (en) * | 2017-10-01 | 2018-01-19 | 江苏长青生物科技有限公司 | A kind of fomesafen aqua synergistic formula composition |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101715765A (en) * | 2009-11-30 | 2010-06-02 | 青岛易百农化科技有限公司 | Fomesafen soluble solid medicament form |
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| NZ231897A (en) * | 1988-12-30 | 1992-09-25 | Monsanto Co | Dry water-soluble granular composition comprising glyphosate and a liquid surfactant |
| CN1276711C (en) * | 2003-05-16 | 2006-09-27 | 山东滨州农药厂 | Herbicide composition containing bentazone, fomesafen and quizalofop-P-fefuryl |
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| CN101715765A (en) * | 2009-11-30 | 2010-06-02 | 青岛易百农化科技有限公司 | Fomesafen soluble solid medicament form |
Non-Patent Citations (1)
| Title |
|---|
| 刘步林.可溶性粉剂.《农药剂型加工技术》.化学工业出版社,1998,第198页. * |
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