CN102239829A - Dinotefuran aqueous suspension agent and its preparation method - Google Patents
Dinotefuran aqueous suspension agent and its preparation method Download PDFInfo
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Abstract
The invention discloses a dinotefuran aqueous suspension agent, which is made from the following components of: by weight, 5-40% of a dinotefuran original drug, 0-6% of an auxiliary suspension agent, 2-20% of a surfactant, 0-1% of a thickening agent, 0-1% of an antifoaming agent, 0-1% of an antiseptic, 0.5-5% of an antifreezing agent and 100% of water, wherein the auxiliary suspension agent is white carbon black, bentonite, magnesium aluminum silicate or kaolin; the surfactant is the random combination selected from five components consisting of NP, No. 500, polycarboxylate, TWEEN, 600P and Polyoxyethylene nonyl phenyl ether phosphate salt; the thickening agent is xanthan gum, carboxymethyl cellulose, polyacrylamide or polyvinyl alcohol; the antifoaming agent is an organic silicon antifoaming agent, tributyl phosphate or butanols; and the antifreezing agent is glycol, glycerin, urea, isopropanol or propylene glycol. The preparation provided by the invention accords with the high content and environmental-friendly preparation processing trend, is a biorational pesticide, and has an extensive application prospect.
Description
Technical field
The present invention relates to technical field of pesticide, be specifically related to a kind of MTI-446 aqueous suspension agent (SC) and preparation method thereof.
Background technology
MTI-446 (dinotefuran) is the third generation nicotinic insecticide of Mitsui chemical company exploitation.This medicament insecticidal spectrum is wide, has remarkable interior suction osmosis, and has promptly shown very high insecticidal activity at very low dosage.This medicine insecticidal spectrum is wide, can prevent various insects such as various Semipteras, Lepidoptera, diptera, orthoptera, Hymenoptera, beetle order.This medicament is fool proof to mammal, birds and aquatile, and crop is not had poisoning, can be used for numerous crops such as paddy rice, fruit tree, vegetables.
Modern agricultural chemicals changes very fast, just the direction towards environmental type develops, and suspending agent (SC) is exactly wherein a kind of, and agricultural chemicals suspension agent is that developing history is short in the pesticidal preparations, very fast a kind of formulation, many weed killer herbicides, insecticidal bactericide can both be processed into this formulation.Agricultural chemicals suspension agent is dispersion medium with water, insoluble or the former medicine of solid that is slightly soluble in water is through grinding, and by the effect of surfactant and other auxiliary agent, make it even dispersion, the more stable liquid-solid attitude system that form the tiny higher suspension of a kind of particle, can flow, compare with missible oil, can avoid using a large amount of organic solvents; Compare with wettable powder, then do not have the dust drift of dispersing; Toxicity and excitant to people and animals are all lower; And can alleviate poisoning to crop; Can be because of organic solvent does not burn in the storage transportation yet, safety is higher; The danger that user and entire environment are caused reduces to quite low degree.And, the agricultural chemicals suspension agent excellent performance, good dispersion, the suspensibility height, put forth effort with adhesion strength in the exhibition on plant corpus surface all more intense, resistance of rainwater washing against, drug effect is significantly and also relatively more lasting.At present domestic insecticides adjuvant also is not very flourishing, also has no small gap compared with developed countries, and the suspending agent that is made into existing auxiliary agent is in more or less the certain problem of existence aspect the physical stability.Serious lamination mainly on ageing stability, often occurs, even livering, knot occur admittedly, can't use and be recovered in processing.MTI-446 is made generally in 1% ~ 20% water-soluble granule, because of its solvability in water is bigger, so make difficulty of aqueous suspension agent, is prone to whole livering phenomenon, can't use.
Summary of the invention
Goal of the invention: at the deficiencies in the prior art, the purpose of this invention is to provide a kind of MTI-446 aqueous suspension agent,, can normally use so that it when making aqueous suspension agent, the livering phenomenon do not occur.Another object of the present invention provides the preparation method of above-mentioned MTI-446 aqueous suspension agent.
Technical scheme: in order to realize the foregoing invention purpose, the technical solution used in the present invention is as follows:
A kind of MTI-446 aqueous suspension agent by weight percentage, comprises the former medicine 5 ~ 40% of MTI-446, suspension aid 0 ~ 6%, and surfactant 2 ~ 20%, thickener 0 ~ 1%, defoamer 0 ~ 1%, preservative 0 ~ 1%, antifreezing agent 0.5 ~ 5%, water complements to 100%.
The former medicine proportion of described MTI-446 is preferably 10 ~ 40% by weight percentage, and more preferably 15 ~ 35%.
Described suspension aid comprises white carbon, bentonite, Magnesiumaluminumsilicate and kaolin etc., and preferred weight percent is 0.5 ~ 4%, preferably uses white carbon, bentonite or Magnesiumaluminumsilicate.
Described surfactant is polyoxyethylene nonylphenol ether (NP), castor oil polyoxyethylene ether (BY), alkylbenzenesulfonate (500#), lignosulfonates (MF), naphthalene sulfonate (NNO), polycarboxylate, sorbitan fatty acid ester APEO (TWEEN), draws back powder (LX), lauryl sodium sulfate (K12), phenethyl phenol polyoxyethylene ether phosphate salt (600P), in polyoxyethylene nonylphenol ether phosphate ester salt (NPP) and the phenethyl phenol polyethenoxy ether sulphonate (600S) etc. 1 ~ 5 kind, be preferably 1 ~ 4 kind, more preferably 2 ~ 3 kinds; Be preferably polyoxyethylene nonylphenol ether (NP), alkylbenzenesulfonate (500#), polycarboxylate, sorbitan fatty acid ester APEO (TWEEN), phenethyl phenol polyoxyethylene ether phosphate salt (600P), polyoxyethylene nonylphenol ether phosphate ester salt (NPP).
Described thickener comprises xanthans, and carboxymethyl cellulose, polyacrylamide and polyvinyl alcohol etc. are preferably xanthans or carboxymethyl cellulose.
Described preservative comprises formaldehyde, benzoic acid, Ka Song and methenamine etc., is preferably formaldehyde, benzoic acid or card pine.
Described antifreezing agent comprises ethylene glycol, glycerine, urea, isopropyl alcohol and propane diols etc., is preferably ethylene glycol, glycerine and urea.
Described defoamer mainly is silicone defoaming agent, tributyl phosphate and butanols, is preferably silicone defoaming agent and tributyl phosphate.
A kind of method for preparing the MTI-446 aqueous suspension agent comprises:
(1) in shearing still, adds entry, shear down, progressively add surfactant and antifreezing agent, shear dissolving fully; Need the pre-heated surface activating agent in case of necessity, preheat temperature is 40 ℃ ~ 100 ℃;
(2) shear down, add former medicine in batches, after finishing, add the defoamer of half metering again; When the former medicine content of processing is lower than 10% or viscosity＜200mpa.s, can add thickener, thickener adds, and may increase milling time;
(3) enter the one-level sand mill after shearing evenly and the secondary sand mill carries out sand milling, reach designing requirement until dispersed former medicine particle diameter; The designing requirement particle diameter is generally 2 ~ 10 μ m;
(4) particle diameter is met the requirements of agricultural chemicals suspension agent and pump in the shearing still, under shear action, add auxiliary addition agents such as defoamer, thickener, preservative and suspension aid, viscosity reaches designing requirement; Designing requirement viscosity is generally 300 ~ 1000 mpa.s.
Specify: because of running water or underground water contain a large amount of electrolyte, can destroy the electric double layer of suspension system, the suggestion fresh water (FW) adopts deionized water; Agricultural chemicals needs to add after the auxiliary agent uniform dissolution in batches, otherwise can be not yet in effect wetting because of agricultural chemicals, may cause blending process viscosity to increase and can't suck sand mill; Different manufacturers such as thickener aluminium-magnesium silicate, xanthans, white carbon, even same producer different batches, quality fluctuation is bigger, addition needs according to actual conditions and viscosity needs, suitably adjust according to reference formulation, aluminium-magnesium silicate or white carbon addition are excessive, can cause the system livering, the virgin rubber addition is excessive altogether, system dispersive property variation.
Use recommended formula and the more and sediment of wash rice water occurs when loose, can prepare qualified preparation by regulating thickener or dispersant proportioning.
Agricultural chemicals suspension agent is the heterogeneous complex system of a high degree of dispersion.Its composition, except that active ingredient and dispersion medium, also has more auxiliary agent, therefore, the various physical aspects of pesticide active ingredient itself, fusing point, volatility, solvability, distributivity and chemical property thereof comprise that the interaction of other composition in hydrolysis and photochemical stability, heat endurance, oxidation-reduction quality and compound and dispersion medium, surfactant and the preparation all can exert an influence to stability of formulation.And because it exists with the form of concentrated suspension liquid all the time, at lay up period, especially chemical instability may appear in long term storage, and more frequent what run into then is physical stability problem.This involves three aspects usually: (1) particle interphase interaction and cause the flocculation and clustering phenomena; (2) Ovshinsky (Ostwald) maturation; (3) layering and the particle deposition that causes because of action of gravity.Obviously, keep agricultural chemicals suspension agent physical stability storage period, just must control that suspension gather, sedimentation and crystal growth by prescription and processing technology.Just, it is coalescent that suspending agent is not merged between particle in storage process, and the granularity of dispersed particle and distribution thereof are remained unchanged; And dispersed phase particles can stably be suspended in the dispersion medium and not sedimentation.
Beneficial effect: compared with prior art, the outstanding advantage that MTI-446 aqueous suspension agent of the present invention has comprises:
The present invention selects a kind of suitable dispersant and wetting agent or multiple combination and suitable proportioning, is used for the MTI-446 aqueous suspension agent, solves preparation and the livering problem occurs after storing.Through long-term storage, easily flow, not stratified, do not lump, can be any with water, easy to use than being diluted to unit for uniform suspension.MTI-446 aqueous suspension agent of the present invention, be a kind of through the time stable MTI-446 aqueous suspension agent, for this agricultural chemicals increases a kind of formulation, widen suitable purposes.
The difficulty of processing MTI-446 SC maximum is that the former medicine of MTI-446 has certain solvability in water, have the Ostwald ripening phenomenon, and caking, livering phenomenon can appear in the heat storage, and stability does not pass a test.The present invention has solved the unsettled difficult problem of MTI-446 SC heat storage by the screening to surfactant.Said preparation meets the formulation processing trend of high-load and environmental protection, belongs to public nuisance-free agricultural chemicals, has broad application prospects.
Description of drawings
Fig. 1 is a MTI-446 aqueous suspension agent preparation technology flow chart.
Embodiment
The present invention is described further below in conjunction with specific embodiment.
Embodiment 1
The MTI-446 aqueous suspension agent, prescription (parts by weight) is: 10 parts of former medicines of MTI-446,4 parts of 600P, 1 part of NP, 1 part of Magnesiumaluminumsilicate, 0.2 part of thickener xanthans, 5 parts of ethylene glycol, 0.2 part of silicone defoaming agent, 0.2 part of benzoic acid, water are supplied 100 parts.
In shearing still, add entry, shear down, progressively add surfactant and antifreezing agent, shear dissolving fully; 40 ℃ ~ 100 ℃ of elder generation's temperature controls, the pre-heated surface activating agent; Shear down, branch 2 or the many batches of former medicines of adding MTI-446 after finishing, add the defoamer of half metering again; When the former medicine content of MTI-446 is lower than 10% or viscosity＜200mpa.s, can add thickener, may increase milling time; Enter the one-level sand mill after shearing evenly and the secondary sand mill carries out sand milling, reach 2 ~ 10 μ m of designing requirement until dispersed former medicine particle diameter; Particle diameter is met the requirements of agricultural chemicals suspension agent pump in the shearing still, under shear action, add auxiliary addition agents such as defoamer, thickener, preservative and suspension aid, viscosity reaches 300 ~ 1000 mpa.s of designing requirement; Discharging gets final product.
Embodiment 2
The MTI-446 aqueous suspension agent, prescription (parts by weight) is: 15 parts of former medicines of MTI-446,2 parts of 500#, 3 parts of LX, 5 parts of white carbons, 0.2 part of polyvinyl alcohol, 5 parts of urea, 0.2 part of silicone defoaming agent, 0.2 part of benzoic acid, water are supplied 100 parts.
With above-mentioned prescription, be prepared according to the method for embodiment 1, get final product.
Embodiment 3
The MTI-446 aqueous suspension agent, prescription (parts by weight) is: 25 parts of former medicines of MTI-446,3 parts of 600P, 2 parts of polycarboxylates, 2 parts of bentonites, 0.2 part of thickener xanthans, 5 parts of antifreezing agent glycerine, 0.2 part of defoamer tributyl phosphate, 0.2 part of card pine, water is supplied 100 parts.
With above-mentioned prescription, be prepared according to the method for embodiment 1, get final product.
Embodiment 4
The MTI-446 aqueous suspension agent, prescription (parts by weight) is: 35 parts of former medicines of MTI-446,4 parts of polycarboxylates, 1 part of TWEEN, 1 part of Magnesiumaluminumsilicate, 0.2 part of thickener xanthans, 5 parts of antifreezing agent isopropyl alcohols, 0.2 part of silicone defoaming agent, 0.2 part of card pine, water is supplied 100 parts.
With above-mentioned prescription, be prepared according to the method for embodiment 1, get final product.
Embodiment 5
The MTI-446 aqueous suspension agent, prescription (parts by weight) is: 40 parts of former medicines of MTI-446,3 parts of 600,1 parts of NP, 1 part of Dispersant MF, 0.2 part of thickener polyvinyl alcohol, 5 parts of antifreeze glycols, 0.2 part of silicone defoaming agent, 0.2 part of benzoic acid, water are supplied 100 parts.
With above-mentioned prescription, be prepared according to the method for embodiment 1, get final product.
Embodiment 6
The MTI-446 aqueous suspension agent, prescription (parts by weight) is: 18 parts of former medicines of MTI-446,4 parts of NNO, 1 part of K12,1 part of Magnesiumaluminumsilicate, 0.2 part of thickener xanthans, 5 parts of antifreezing agent isopropyl alcohols, 0.2 part of silicone defoaming agent, 0.2 part of benzoic acid, water are supplied 100 parts.
By above-mentioned prescription, with the former medicine of MTI-446, surfactant, antifreezing agent, suspension aid, preservative, defoamer, add water to 90% of gross weight, carry out sand milling, make the granularity of preparation reach requirement.The good material of sand milling is added in the uncovered cup, carry out high shear, under agitation add thickener and remaining water, be trimmed to viscosity and reach designing requirement, get final product discharging.
Embodiment 7
The MTI-446 aqueous suspension agent, prescription (parts by weight) is: 22 parts of former medicines of MTI-446,4 parts of 600S, 1 part of BY, 0.2 part of thickener xanthans, 5 parts of antifreezing agent glycerine, 0.2 part of silicone defoaming agent, 0.2 part of benzoic acid, water are supplied 100 parts.
By above-mentioned prescription, with the former medicine of MTI-446, surfactant, antifreezing agent, suspension aid, preservative, defoamer, add water to 90% of gross weight, carry out sand milling, make the granularity of preparation reach requirement.The good material of sand milling is added in the uncovered cup, carry out high shear, under agitation add thickener and remaining water, be trimmed to viscosity and reach designing requirement, get final product discharging.
Embodiment 9
The MTI-446 aqueous suspension agent, prescription (parts by weight) is: 33 parts of former medicines of MTI-446,4 parts of 600,1 parts of AES, 1 part of Magnesiumaluminumsilicate, 0.2 part of thickener xanthans, 5 parts of antifreezing agent propane diols, 0.2 part of silicone defoaming agent, 0.2 part of formaldehyde, water are supplied 100 parts.
By above-mentioned prescription, with the former medicine of MTI-446, surfactant, antifreezing agent, suspension aid, preservative, defoamer, add water to 90% of gross weight, carry out sand milling, make the granularity of preparation reach requirement.The good material of sand milling is added in the uncovered cup, carry out high shear, under agitation add thickener and remaining water, be trimmed to viscosity and reach designing requirement, get final product discharging.
Embodiment 10
After finishing the prescription of embodiment 1 ~ 9, respectively to fineness, suspensibility, the viscosity of finished product, heat storage stability, cold storage stability are tested again, pass through the ageing stability that reaches 2 years again and deposit, and determine that above prescription meets the requirement of table 1 fully.
Table 1 MTI-446 aqueous suspension agent quality index
| ? | Project | Quality index | Remarks |
| 1 | Outward appearance (25 ℃) | The milky viscous mobile liquid | ? |
| 2 | Pourability (residual)≤% | 5 | ? |
| 3 | Particle diameter (μ m) | 2~10 | ? |
| 4 | Viscosity (mpa.s) | 300~1000 | ? |
| 5 | PH value | 5～7 | ? |
| 6 | Emulsion foaming characteristic (diluting 200 times) 1min≤ | 25ml | ? |
| 7 | Refrigeration (0 ± 1 ℃ of 7d) | Not stratified, non-crystallizable | ? |
| 8 | Heat storage (54 ± 1 ℃ of 14d) bleed≤ | 5 | ? |
| 9 | Former medicine resolution ratio≤% | 5 | Heat storage back is detected |
| 10 | Suspensibility 〉=% | 90 | ? |
Claims (9)
1. a MTI-446 aqueous suspension agent is characterized in that, by weight percentage, comprises following each component: the former medicine 5 ~ 40% of MTI-446, suspension aid 0 ~ 6%, surfactant 2 ~ 20%, thickener 0 ~ 1%, defoamer 0 ~ 1%, preservative 0 ~ 1%, antifreezing agent 0.5 ~ 5%, water complements to 100%; Described suspension aid is white carbon, bentonite, Magnesiumaluminumsilicate or kaolin; Described surfactant is polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, alkylbenzenesulfonate, lignosulfonates, naphthalene sulfonate, polycarboxylate, sorbitan fatty acid ester APEO, draws back powder, lauryl sodium sulfate, phenethyl phenol polyoxyethylene ether phosphate salt, any mixing of 1 ~ 5 kind in polyoxyethylene nonylphenol ether phosphate ester salt and the phenethyl phenol polyethenoxy ether sulphonate; Described thickener is an xanthans, carboxymethyl cellulose, polyacrylamide or polyvinyl alcohol; Described defoamer is silicone defoaming agent, tributyl phosphate or butanols; Described preservative is formaldehyde, benzoic acid, Ka Song or methenamine; Described antifreezing agent is ethylene glycol, glycerine, urea, isopropyl alcohol or propane diols.
2. MTI-446 aqueous suspension agent according to claim 1 is characterized in that: the percentage by weight of the shared total aqueous suspension agent of the former medicine of described MTI-446 is 10 ~ 40%.
3. MTI-446 aqueous suspension agent according to claim 1 and 2 is characterized in that: the percentage by weight of the shared total aqueous suspension agent of the former medicine of described MTI-446 is 15 ~ 35%.
4. MTI-446 aqueous suspension agent according to claim 1 is characterized in that: the percentage by weight of the shared total aqueous suspension agent of described suspension aid is 0.5 ~ 4%.
5. MTI-446 aqueous suspension agent according to claim 1 is characterized in that: described surfactant is that 1 ~ 4 kind in polyoxyethylene nonylphenol ether, alkylbenzenesulfonate, polycarboxylate, sorbitan fatty acid ester APEO, phenethyl phenol polyoxyethylene ether phosphate salt and the polyoxyethylene nonylphenol ether phosphate ester salt mixes arbitrarily.
6. a method for preparing the described MTI-446 aqueous suspension agent of claim 1 is characterized in that, comprising:
(1) in shearing still, adds entry, shear down, progressively add surfactant and antifreezing agent, shear dissolving fully;
(2) shear down, add former medicine in batches, after finishing, add the defoamer of half metering again;
(3) after shearing evenly, change the one-level sand mill over to and the secondary sand mill carries out sand milling, reach designing requirement until dispersed former medicine particle diameter;
(4) particle diameter is met the requirements of agricultural chemicals suspension agent and pump in the shearing still, under shear action, add defoamer, thickener, preservative and suspension aid, be trimmed to viscosity and reach designing requirement, get final product discharging.
7. the method for preparing the MTI-446 aqueous suspension agent according to claim 6 is characterized in that: in the step (1), and described water level deionized water.
8. the method for preparing the MTI-446 aqueous suspension agent according to claim 6 is characterized in that: in the step (1), dispersant and wetting agent are carried out the preheating preliminary treatment, preheat temperature is 40 ℃ ~ 100 ℃.
9. the method for preparing the MTI-446 aqueous suspension agent according to claim 6 is characterized in that: in the step (2), when former medicine content is lower than 10% or viscosity＜200mpa.s, add thickener.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103283720A (en) * | 2013-06-26 | 2013-09-11 | 山东潍坊润丰化工有限公司 | Preparation method of suspending agent |
| CN104663701A (en) * | 2015-01-23 | 2015-06-03 | 河北威远生化农药有限公司 | Dinotefuran synergistic suspending agent and preparation method thereof |
| CN106577722A (en) * | 2015-10-14 | 2017-04-26 | 上海师范大学 | Dinotefuran suspending agent and preparation method thereof |
| CN107788005A (en) * | 2017-10-31 | 2018-03-13 | 南京扬子鸿利源化学品有限责任公司 | A kind of new dinotefuran aqueous suspension agent and preparation method thereof |
| CN108586070A (en) * | 2018-06-28 | 2018-09-28 | 安徽瑞然生物药肥科技有限公司 | insecticide fertilizer and preparation method thereof |
| CN108902150A (en) * | 2018-05-28 | 2018-11-30 | 徐建自 | A kind of Synergistic bactericidal composition and its suspending agent containing cyprodinil and fludioxonil |
| CN109221225A (en) * | 2018-09-28 | 2019-01-18 | 绩溪农华生物科技有限公司 | A kind of dinotefuran synergy suspending agent and preparation method thereof |
| CN115067325A (en) * | 2022-06-14 | 2022-09-20 | 江苏剑牌农化股份有限公司 | Preparation method of anhydrous dinotefuran suspending agent |
| CN115104620A (en) * | 2021-08-13 | 2022-09-27 | 山东恒利达生物科技有限公司 | Furan nicotine insecticidal composition and application thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103283720A (en) * | 2013-06-26 | 2013-09-11 | 山东潍坊润丰化工有限公司 | Preparation method of suspending agent |
| CN103283720B (en) * | 2013-06-26 | 2014-08-27 | 山东潍坊润丰化工股份有限公司 | Preparation method of suspending agent |
| CN104663701A (en) * | 2015-01-23 | 2015-06-03 | 河北威远生化农药有限公司 | Dinotefuran synergistic suspending agent and preparation method thereof |
| CN106577722A (en) * | 2015-10-14 | 2017-04-26 | 上海师范大学 | Dinotefuran suspending agent and preparation method thereof |
| CN107788005A (en) * | 2017-10-31 | 2018-03-13 | 南京扬子鸿利源化学品有限责任公司 | A kind of new dinotefuran aqueous suspension agent and preparation method thereof |
| CN108902150A (en) * | 2018-05-28 | 2018-11-30 | 徐建自 | A kind of Synergistic bactericidal composition and its suspending agent containing cyprodinil and fludioxonil |
| CN108586070A (en) * | 2018-06-28 | 2018-09-28 | 安徽瑞然生物药肥科技有限公司 | insecticide fertilizer and preparation method thereof |
| CN109221225A (en) * | 2018-09-28 | 2019-01-18 | 绩溪农华生物科技有限公司 | A kind of dinotefuran synergy suspending agent and preparation method thereof |
| CN115104620A (en) * | 2021-08-13 | 2022-09-27 | 山东恒利达生物科技有限公司 | Furan nicotine insecticidal composition and application thereof |
| CN115104620B (en) * | 2021-08-13 | 2023-08-11 | 山东恒利达生物科技有限公司 | Furannicotine insecticidal composition and application thereof |
| CN115067325A (en) * | 2022-06-14 | 2022-09-20 | 江苏剑牌农化股份有限公司 | Preparation method of anhydrous dinotefuran suspending agent |
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Application publication date: 20111116 |