CN103493804B - Compound pesticide wetting agent and application of compound pesticide wetting agent in preparation of pesticide preparations - Google Patents
Compound pesticide wetting agent and application of compound pesticide wetting agent in preparation of pesticide preparations Download PDFInfo
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Abstract
The invention discloses a compound pesticide wetting agent and application of the compound pesticide wetting agent in the preparation of pesticide preparations. The compound pesticide wetting agent is characterized in that oxine-copper and tebuconazole are taken as pesticide active ingredients, properties such as the wetting efficiency, the medicine-holding quantity of leaves and the like are taken as evaluation indexes to screen the combinations of different varieties of wetting agents and the dose proportions of the wetting agents, and finally the compound wetting agent capable of effectively improving wetting and spreading capacities of the pesticide preparations and improving the effects for preventing and controlling crop diseases is obtained. The compound wetting agent consists of isomerous 1307 and a penetrating agent JFC and is capable of effectively improving properties such as the wetting efficiency, the medicine-holding quantity of leaves and the like of the pesticide preparations, and the prevention and cure efficiency of a pesticide suspension agent to crop diseases can be effectively improved. The invention further provides a oxine-copper.tebuconazole pesticide suspending agent, a oxine-copper pesticide suspending agent and preparation methods of the oxine-copper.tebuconazole pesticide suspending agent and the oxine-copper pesticide suspending agent and further discloses application of the oxine-copper.tebuconazole pesticide suspending agent and the oxine-copper pesticide suspending agent in the prevention and control of the bacteria or fungal diseases of crops.
Description
Technical field
The present invention relates to a kind of insecticides adjuvant, particularly relate to a kind of agricultural chemicals compound wetting agent, the invention further relates to this agricultural chemicals compound wetting agent prepare agricultural chemicals suspension agent, water-dispersible granules, can purposes in the preparation such as point Wettable Powder, belong to agricultural chemicals wetting agent field.
Background technology
Wetting agent be the basic formulation of agricultural chemicals as suspending agent, water-dispersible granules, can the necessary assistant component such as point Wettable Powder, be also the spray adjuvants component of pesticides application technology necessity.Agricultural chemicals wetting agent is by reducing surface tension, increases pastille liquid to the contact of the handling object surface of solids, changes drop contact angle from the teeth outwards and realizes wetting and permeability.Wetting agent kind is more, has natural wetting agent, as Tea Saponin, spent pulping liquor etc.; Chemical synthetic pesticide wetting agent variety protection is many, and mainly contain anion and the large class of nonionic two, conventional Nekal BX and K12 belong to anion surfactant, are current Application comparison one of kinds widely, significantly can reduce the surface tension of water.
Suspending agent (Suspens ion Concentrat ion, SC) being take water as medium, by some auxiliary agent, pulverized by sand milling, the former medicine of solid that is insoluble or that be slightly soluble in water is scattered in water equably, the stable liquid-solid state system that form the tiny higher suspension of a kind of particle, can flow.Have particle diameter little, good dispersion, good fluidity, suspensibility are high, biologically active is high, using dosage is little, resistance of rainwater washing against, residual low, to features such as people and animals' low toxicities.
Can jointly there is physical action with other auxiliary agent such as surfactant in suspending agent, thus by originally in water former medicine Granular composite that is insoluble or indissoluble enter in water, thus the suspension system defining stable chemical nature, be evenly distributed.The main component of suspending agent comprises former medicine, wetting agent, defoamer, dispersant, pH adjusting agent, thickener, antifreezing agent, water etc.The dispersion medium of suspending agent is water, therefore it has the features such as cheap, use safety, making is simple, storage is convenient, and can under any water temperature, condition of water quality, mix with water with arbitrary proportion. easy to use.Relative to the agricultural chemicals taking organic solvent as medium, it is safer to environment, poisoning is also lower etc.Suspending agent, as a novel agrochemical formulation, obviously can reduce the use of organic solvent in traditional agricultural chemicals, thus reduces environmental pollution, be worth promoting (Liu Bulin. formulations of pesticide process technology [M]. Beijing: Chemical Industry Press, 1998).
The composition of preparation also can have an impact to suspensibility, the composition of suspending agent comprises former medicine, water and auxiliary agent, the suspending agent stable in order to excellent, except fineness viscosity requires, also must select suitable auxiliary agent and active constituent content, auxiliary agent in suspending agent has multiple, mainly contain dispersant, wetting agent, thickener, antifreezing agent and defoamer etc., what wherein have the greatest impact is dispersant and wetting agent.In same form formula, different dispersants or wetting agent kind obviously can have influence on the performance of pesticide active ingredient.The kind of wetting agent and consumption are directly connected to the height of the wetting efficiency of pesticidal preparations and permeance property, liquid at the height of the liquid holdup of blade, and what finally have influence on pharmaceutical preparation prevents and treats efficiency.
Tebuconazole belongs to triazole type systemic fungicide, and have protection, treatment and eradicant action, fungicidal spectrum is wide, and the lasting period is normal, can prevent and treat plurality of plant diseases, as rust, powdery mildew, root rot, gray mold etc.Tebuconazole to be sprayed on crop and can be partially absorbed and mainly shift to top by plant is vegetative rapidly, not only there is bactericidal activity, also can promote plant growth, make it well developed root system, leaf look dark green, robust plant, effective tiller increase, thus can increase crop yield.
Copper 8-hydroxyquinolinate belongs to organic chelated copper fungicide, there is extremely strong adhesion strength and resistance of rainwater washing against ability, have that safety is high, fungicidal spectrum light, lasting period are long, low cost and other advantages, to bacterial disease, there is special efficacy, for fungal disease, there is higher control efficiency.
After copper 8-hydroxyquinolinate and Tebuconazole are carried out compatibility, the two has certain synergistic function, can increasing action site; expanding prevention crop and object spectrum; the usage amount of pesticide active ingredient can be reduced simultaneously, effectively delay the drug-fast generation of damage by disease and insect, be conducive to preserving the ecological environment.
Publication No. is that the Chinese invention patent of CN101810181A discloses a kind of bactericidal pesticide composition and its production and use, the active ingredient of this bactericidal pesticide composition is made up of according to specific consumption proportion copper 8-hydroxyquinolinate and Tebuconazole, this bactericidal pesticide composition can prevent and treat various bacillary or fungal disease, but there is wetting and spreading ability, hold the defects such as dose is low on crop leaf in the agricultural chemicals suspension agent of this bactericidal pesticide composition, haves much room for improvement.
Summary of the invention
An object of the present invention is to provide a kind of wetting and spreading ability, the agricultural chemicals compound wetting agent of holding dose of raising liquid on crop leaf that effectively can improve pesticidal preparations.
Two of object of the present invention is applied to by described agricultural chemicals compound wetting agent to prepare pesticidal preparations.
Above-mentioned purpose of the present invention is achieved through the following technical solutions:
The present invention with Tebuconazole and copper 8-hydroxyquinolinate for active ingredient, with performances such as wetting efficiency, blade liquid holdups for evaluation index, carry out preferably to the combination of different wetting agent kind and consumption proportion thereof, determine better formula, the wetting efficiency of pesticidal preparations, the compound wetting agent of blade liquid holdup can be significantly improved to screen to obtain.
The present invention finally finds, the agricultural chemicals compound wetting agent be made up of isomery 1307 and penetrating agent JFC effectively can improve the wetability of pesticidal preparations, permeability and the liquid holdup at crop leaf thereof; In order to reach better wetting and osmotic effect, isomery 1307 is preferably 1-2:1-3 with the mass ratio of penetrating agent JFC, is particularly preferably 1:1.
Wetting agent is one of component important in suspending agent processing formula, is the key factor affecting preparation important technology index.The size that pesticide activity component drug effect plays, depend primarily on dilution the soaking and opening up situation on target of pesticidal preparations, dosage surface tension force is lower, and covering surfaces is long-pending larger.Expect agricultural chemicals suspension agent of good performance, select suitable wetting agent most important, on the one hand, because former medicine is various in style, its molecular structure, physicochemical property vary, and the wetting agent kind of selection is also different.On the other hand, according to different Target crops, select suitable wetting agent, make the surface tension of the liquid of recommended dose appropriateness be less than the critical surface tension of target plant, namely in liquid, the concentration of auxiliary agent meets or exceeds critical micelle concentration, and reaching increases agricultural chemicals and hold dose at plant surface, reduce agricultural chemicals to run off, thus minimizing pesticide dosage, reduce drug cost, alleviate the pollution of agricultural chemicals to environment.In suspending agent, various auxiliary agent all may impact the physical stability of preparation, and also interacts between auxiliary agent, only has selected auxiliary agent reasonable disposition in certain quality and quantitative range, mutual coordination, just can make preparation become a kind of stable suspended substance.The object that wetting agent uses, the first helps the air on displacement pesticide activity component particle surface, adds fast particle and enters wetting speed in water, particle is soaked rapidly.Its two be reduce viscosity, be convenient to better grinding.Usually select and low foamingly non-ly make wetting agent from surfactant, because produce the efficiency that foam may reduce product.The wetting agent often selected has lauryl sodium sulfate, alcohol ethoxylate, alkylphenol ethoxylate, octadecyl sodium sulfosuccinate.In same form formula, different wetting agent kinds obviously can have influence on the performance of pesticide active ingredient, as active ingredient and wetting agent mismatch 5 time, can cause suspending agent place for a long time layering, knot the end serious, particle becomes large, thus its suspensibility is declined, affect the absorption of blade face to medicament, this is particularly important to cauline leaf processing-type agricultural chemicals.
When different wetting agents is carried out composite, physicochemical property between various wetting agent differs greatly, also larger difference can be there is in the performance of composite for the different wetting agents compound wetting agent together obtained afterwards, some compound wetting agents can significantly improve the wetability of pesticidal preparations, permeability and even prevent and treat efficiency, some composite dispersing agents not only mismatch 5 each other, and also to have with the character of pesticide original medicine and conflict, compatibility was not at that time, not only can not improve the wetability of preparation or prevent and treat efficiency, instead the control efficiency of preparation can be reduced.
There is the wax coat that one deck is very thick on paddy rice surface, a lot of agricultural chemicals is difficult at rice leaf wet spreading, paddy pesticide availability is less than 40%, the retention volume of liquid on rice plant can be caused so few, the super-high-efficient wetting agent that interior absorption penetration is very strong must be selected to improve agricultural chemicals availability, if but surface tension is too low, liquid is difficult to stop on blade face.The object of adding appropriate wetting agent manages the liquid increased on rice plant to hold flow, reduces agricultural chemicals and run off, and for making liquid arrive disease plant base portion fast, suppresses germ to spread.Generally occur in the market increasing medicine liquid volume by strengthening water consumption, attempt to improve the liquid holdup of liquid on rice plant, the consequence done like this is the concentration diluting surfactant in liquid in fact, surfactant concentration in liquid is made not reach critical micelle concentration, the surface tension of liquid is greater than the critical surface tension of rice leaf, liquid can be reduced on the contrary on rice plant, hold flow, reduce pesticide control effect.Compound wetting agent of the present invention effectively can improve the liquid holdup of liquid on rice leaf, and that finally effectively improves pesticidal preparations prevents and treats efficiency.
Another object of the present invention using the present invention screen the compound wetting agent that obtains and to be applied to as insecticides adjuvant and to prepare pesticidal preparations; Described pesticidal preparations can be suspending agent, water-dispersible granules, can point Wettable Powder etc.; Wherein, the composition of described agricultural chemicals suspension agent comprises: pesticide active ingredient, dispersant, compound wetting agent, thickener, antifreezing agent, preservative; Wherein, pesticide active ingredient in described agricultural chemicals suspension agent can be have the bactericide of sterilization or disinsection efficiency, insecticide or various weed killer herbicide, these active ingredients are active ingredient that can be single, also can by the composite composition together of several active ingredient; Such as, can be the mixture that Tebuconazole and copper 8-hydroxyquinolinate form according to the mass ratio of 1:1-3.Wherein, calculate by mass percentage, the consumption of each composition can be: pesticide active ingredient 4-70%, dispersant 3-10%, compound wetting agent 1-6%, antifreezing agent 1-8%, preservative 0.1-2%, thickener 0.1-3%, and surplus is water.
The present invention screen to the different amounts of compound wetting agent in agricultural chemicals suspension agent showing tension force, liquid liquid holdup, hold the impact that the performances such as bubble amount have highly significant lastingly for suspending agent, in order to screen comparatively suitable consumption, the present invention with 36% copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent for experiment pesticidal preparations, take paddy rice as controlling object, the optimum amount of screening compound wetting agent.Experimental result finds, when interpolation compound wetting agent consumption is 1.5-4.5wt%, the surface tension of liquid is just in time close with the critical surface tension of rice leaf, the blade liquid holdup of paddy rice has remarkable lifting, wherein, when compound wetting agent consumption is 2.5wt%, the blade liquid holdup of paddy rice reaches and is up to 98.9%, exceeded this consumption, the blade liquid holdup of paddy rice increases not obvious even on a declining curve.Therefore, the addition of compound wetting agent of the present invention in agricultural chemicals suspension agent is preferably 1.5-4.0wt%, and more preferably 2.0-3.5wt%, most preferably is 2.0-2.5wt%.
The invention provides a kind of copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent, its constituent is: by mass percentage, and pesticide active ingredient 10-55%, dispersant 2-10%, compound wetting agent 1-6%, thickener 0.1-3%, antifreezing agent 1-8%, preservative 0.1-2%, surplus are water;
The consumption of each component is preferably: pesticide active ingredient 36%, dispersant 6%, compound wetting agent 1.5-4.0%, thickener 0.7%, antifreezing agent 5%, preservative 0.5%, and surplus is water;
Wherein, preferably, described pesticide active ingredient is made up of according to the mass ratio of 1:1-3 Tebuconazole and copper 8-hydroxyquinolinate; Preferred, described pesticide active ingredient is made up of according to the mass ratio of 1:2 Tebuconazole and copper 8-hydroxyquinolinate.
Present invention also offers a kind of copper 8-hydroxyquinolinate agricultural chemicals suspension agent, its constituent is: by mass percentage, and copper 8-hydroxyquinolinate 10-50%, dispersant 2-10%, compound wetting agent 1.5-4.0%, thickener 0.1-3%, antifreezing agent 1-8%, preservative 0.1-2%, surplus are water;
Preferably, each amounts of components is: copper 8-hydroxyquinolinate 33.5%, dispersant 6%, compound wetting agent 1.5-4.0%, thickener 0.7%, antifreezing agent 5%, preservative 0.5%, and surplus is water;
Described compound wetting agent is made up of isomery 1307 and penetrating agent JFC; In order to reach better control efficiency, isomery 1307 is preferably 1-2:1-3 with the mass ratio of penetrating agent JFC, is particularly preferably 1:1.
Described dispersant, thickener, antifreezing agent or preservative can be the components of some routines in agricultural chemicals suspension agent; Such as, described dispersant can be in naphthalenesulfonate formaldehyde condensation compound (NN0), alkylphenol polyoxyethylene (TX-10), alkyl phenol formaldehyde resin polyoxyethylene ether (Nongru-700 #), alkyl naphthalene sulfonic acid formaldehyde condensation products sodium salt (D425), detergent (LS), sodium lignin sulfonate (REAX85A, REAX83A), dispersing agent MF (Dispersant MF) or castor oil polyoxyethylene ether (BY130) any one or more than one by the composite dispersing agent of any mass ratio composition;
Described thickener can be in gelatin, sodium carboxymethylcellulose, hydroxyethylcellulose, modified starch, xanthans, bentonite, silica or Magnesiumaluminumsilicate any one or multiple;
Described preservative can be in Sodium Benzoate, sodium salicylate, KF88, propionic acid or sorbic acid and sodium salt thereof or other biological bactericide any one or multiple;
Described antifreezing agent can be in polyalcohols (as ethylene glycol, propane diols, glycerine), glycols (diethylene glycol (DEG), triethylene glycol) or polyethylene glycol any one or multiple.
Present invention also offers a kind of method preparing copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent or copper 8-hydroxyquinolinate agricultural chemicals suspension agent, the method comprises: in sand mill, drop into pesticide active ingredient, dispersant, compound wetting agent, preservative, part thickener and water, grinding; When particle diameter D90 is when 2-15 μm (be preferably 5 μm), stop grinding, add after antifreezing agent stirs, then add remaining thickener and regulate viscosity, to obtain final product.
Copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent of the present invention or copper 8-hydroxyquinolinate agricultural chemicals suspension agent can prevent and treat various bacillary or fungal disease, be widely used in the disease control of vegetables, fruit tree, crop (comprising paddy rice, cotton, corn, soybean, tobacco etc.), especially for rice sheath blight disease, alternaria leaf spot of apple, there is significant preventive effect.
Embodiment
The present invention is further described below in conjunction with specific embodiment; these embodiments are only exemplary; what those skilled in the art should understand that is; can modify to the details of technical solution of the present invention and form lower without departing from the spirit and scope of the present invention or replace, but these amendments and replacement all fall within the scope of protection of the present invention.
Experiment material
Isomery 1307: purchased from Nanjing rising sun Fine Chemical Co., Ltd.
Penetrating agent JFC: purchased from Hangzhou Jiu Ling Chemical Co., Ltd..
The preparation of embodiment 136% copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent
Each component is taken: pesticide active ingredient 36%(copper 8-hydroxyquinolinate 24%, Tebuconazole 12%) according to following mass percent; Dispersant D4256%; Compound wetting agent (being made up of according to the mass ratio of 1:1 isomery 1307 and penetrating agent JFC) 2%; Antifreeze glycol 5%; Preservative sodium benzoate 0.5%; Aluminium-magnesium silicate 0.5%; Xanthans 0.2%, running water is supplied;
Pesticide active ingredient is dropped into, dispersant, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.1; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.148; Persistent foamability≤18ml; Pourability is qualified, cold and hot storage qualified stability.
The preparation of embodiment 236% copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent
Each component is taken: pesticide active ingredient 36%(copper 8-hydroxyquinolinate 24%, Tebuconazole 12%) according to following mass percent; Dispersant sodium lignin sulfonate REAX85A6%; Compound wetting agent (being made up of according to the mass ratio of 1:2 isomery 1307 and penetrating agent JFC) 2.5%; Antifreeze glycol 5%; Preservative KF88 0.5%; Aluminium-magnesium silicate 0.5%; Xanthans 0.2%, running water is supplied;
Pesticide active ingredient is dropped into, dispersant, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.2; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.145; Persistent foamability≤20ml; Pourability is qualified, cold and hot storage qualified stability.
The preparation of embodiment 336% copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent
Each component is taken: pesticide active ingredient 36%(copper 8-hydroxyquinolinate 24%, Tebuconazole 12%) according to following mass percent; Dispersant sodium lignin sulfonate REAX85A6%; Compound wetting agent (being made up of according to the mass ratio of 1:3 isomery 1307 and penetrating agent JFC) 2.5%; Antifreeze glycol 5%; Preservative sodium benzoate 0.5%; Aluminium-magnesium silicate 0.5%; Xanthans 0.2%, running water is supplied;
Pesticide active ingredient is dropped into, dispersant, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.4; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.148; Persistent foamability≤20ml; Pourability is qualified, cold and hot storage qualified stability.
The preparation of embodiment 436% copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent
Each component is taken: pesticide active ingredient 36%(copper 8-hydroxyquinolinate 24%, Tebuconazole 12%) according to following mass percent; Dispersant sodium lignin sulfonate REAX83A6%; Compound wetting agent (being made up of according to the mass ratio of 2:1 isomery 1307 and penetrating agent JFC) 2.0%; Antifreeze glycol 5%; Preservative sodium benzoate 0.5%; Aluminium-magnesium silicate 0.5%; Xanthans 0.2%; Running water is supplied;
Pesticide active ingredient is dropped into, dispersant, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.6; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.147; Persistent foamability≤21ml; Pourability is qualified, cold and hot storage qualified stability.
The preparation of embodiment 548% copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent
Each component is taken: pesticide active ingredient 48%(pesticide active ingredient is made up of according to the mass ratio of 3:1 copper 8-hydroxyquinolinate and Tebuconazole) according to following mass percent; Dispersant D4258%; Compound wetting agent (being made up of according to the mass ratio of 1:1 isomery 1307 and penetrating agent JFC) 2%; Antifreeze glycol 5%; Preservative sodium benzoate 0.5%; Aluminium-magnesium silicate 0.3%; Xanthans 0.1%, running water is supplied;
Pesticide active ingredient is dropped into, dispersant, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.5; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.156; Persistent foamability≤22ml; Pourability is qualified, cold and hot storage qualified stability.
The preparation of embodiment 624% copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent
Each component is taken: pesticide active ingredient 24%(is made up of according to the mass ratio of 2:1 copper 8-hydroxyquinolinate and Tebuconazole) according to following mass percent; Dispersant sodium lignin sulfonate REAX83A6%; Compound wetting agent (being made up of according to the mass ratio of 2:1 isomery 1307 and penetrating agent JFC) 2.0%; Antifreezing agent glycerine 5%; Preservative KF88 0.5%; Aluminium-magnesium silicate 1.0%; Xanthans 0.2%; Running water is supplied;
Pesticide active ingredient is dropped into, dispersant, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 10 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.4; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.139; Persistent foamability≤21ml; Pourability is qualified, cold and hot storage qualified stability.
The preparation of embodiment 736% copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent
Each component is taken: pesticide active ingredient 36%(copper 8-hydroxyquinolinate 24%, Tebuconazole 12%) according to following mass percent; Dispersant sodium lignin sulfonate REAX85A10%; Compound wetting agent (being made up of according to the mass ratio of 1:3 isomery 1307 and penetrating agent JFC) 6%; Antifreeze glycol 8%; Preservative sodium benzoate 2%; Aluminium-magnesium silicate 0.6%; Xanthans 0.3%, running water is supplied;
Pesticide active ingredient is dropped into, dispersant, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.3; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.145; Persistent foamability≤22ml; Pourability is qualified, cold and hot storage qualified stability.
The preparation of embodiment 812% copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent
Each component is taken: pesticide active ingredient 12%(copper 8-hydroxyquinolinate 6%, Tebuconazole 6%) according to following mass percent; Dispersant sodium lignin sulfonate REAX85A2%; Compound wetting agent (being made up of according to the mass ratio of 1:3 isomery 1307 and penetrating agent JFC) 1%; Antifreeze glycol 3%; Preservative KF88 0.1%; Aluminium-magnesium silicate 2.5%; Xanthans 0.4%, running water is supplied;
Pesticide active ingredient is dropped into, dispersant, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 2 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.1; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.121; Persistent foamability≤22ml; Pourability is qualified, cold and hot storage qualified stability.
The preparation of embodiment 933.5% copper 8-hydroxyquinolinate agricultural chemicals suspension agent
Each component is taken: copper 8-hydroxyquinolinate 33.5% according to following mass percent; Dispersant D4256%; Compound wetting agent (being made up of according to the mass ratio of 1:1 isomery 1307 and penetrating agent JFC) 2%; Antifreeze glycol 5%; Preservative sodium benzoate 0.5%; Aluminium-magnesium silicate 0.5%; Xanthans 0.2%, running water is supplied;
Copper 8-hydroxyquinolinate is dropped into, dispersant D425, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.3; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.126; Persistent foamability≤18ml; Pourability is qualified, cold and hot storage qualified stability.
The preparation of embodiment 1033.5% copper 8-hydroxyquinolinate agricultural chemicals suspension agent
Each component is taken: copper 8-hydroxyquinolinate 33.5% according to following mass percent; Dispersant D4256%; Compound wetting agent (being made up of according to the mass ratio of 1:2 isomery 1307 and penetrating agent JFC) 2%; Antifreeze glycol 5%; Preservative sodium benzoate 0.5%; Aluminium-magnesium silicate 0.5%; Xanthans 0.2%, running water is supplied;
Copper 8-hydroxyquinolinate is dropped into, dispersant D425, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.3; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.129; Persistent foamability≤21ml; Pourability is qualified, cold and hot storage qualified stability.
The preparation of embodiment 1112% copper 8-hydroxyquinolinate agricultural chemicals suspension agent
Each component is taken: copper 8-hydroxyquinolinate 12% according to following mass percent; Dispersant D4256%; Compound wetting agent (being made up of according to the mass ratio of 1:1 isomery 1307 and penetrating agent JFC) 2%; Antifreeze glycol 5%; Preservative sodium benzoate 0.5%; Aluminium-magnesium silicate 1.0%; Xanthans 0.2%, running water is supplied;
Copper 8-hydroxyquinolinate is dropped into, dispersant D425, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.3; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.109; Persistent foamability≤18ml; Pourability is qualified, cold and hot storage qualified stability.
The preparation of embodiment 1248% copper 8-hydroxyquinolinate agricultural chemicals suspension agent
Each component is taken: pesticide active ingredient copper 8-hydroxyquinolinate 48% according to following mass percent; Dispersant D4256%; Compound wetting agent (being made up of according to the mass ratio of 1:2 isomery 1307 and penetrating agent JFC) 2%; Antifreeze glycol 5%; Preservative sodium benzoate 0.5%; Aluminium-magnesium silicate 0.3%; Xanthans 0.1%, running water is supplied;
Pesticide active ingredient is dropped into, dispersant, compound wetting agent, preservative, thickener aluminium-magnesium silicate and water, grinding in sand mill; When particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add thickener xanthans adjustment viscosity again, to obtain final product.
Product appearance is the green thick liquid that can flow, and product leading indicator content is qualified, pH=7.6; Fineness 100% is by 44 μm of wet screenings, and proportion is 1.167; Persistent foamability≤21ml; Pourability is qualified, cold and hot storage qualified stability.
The screening experiment of experimental example 1 compound wetting agent
One, for examination wetting agent kind
Isomery 1307, penetrating agent JFC, alkyl glycoside, bleeding agent SF and lauryl sodium sulfate;
Isomery 1307: Chinese is isomeric alcohol polyethenoxy ether 1307 is polymer of isomerous tridecanol and oxirane.Belong to isomery fatty alcohol polyethenoxy ether class type product, easily dispersion or water-soluble, has excellent wetability, permeability and emulsibility.Product is not containing APEO, and the isomery alcohol in isomery alcohol ether is not Guerbet alcohol, but contains the alkyl isomery alcohol of little side chain; It is the excellent substitute of polyoxyethylene nonylphenol ether, sodium phosphate trimer etc., and its performance is also more excellent compared with natural alcohol ether.Domestic have the enterprise such as Jiangyin Hua Yuan Chemical Co., Ltd., Nanjing rising sun Fine Chemical Co., Ltd to have production and sales.
Penetrating agent JFC: belong to non-ionic polyoxyethylene ether compound, micro-yellow or water white transparency oily thing liquid, penetration≤5 second as clear as crystal the solution of (0.1% aqueous solution) one-tenth soluble in water, heat-resisting, acid and alkali-resistance, resistance to slaine, chlorine-resistant, to various fiber without compatibility, textile industry is used as bleeding agent, can be used for the operations such as starching, destarch, kiering, bleaching, charing and chlorination, can be used as again dye bath and arrange the penetrant of bathing, and the bleeding agent of leather coating, also can be used as the concise of chemical & blended fabric, there is stronger washing ability.
Bleeding agent SF: belong to nonionic fatty alcohols polyoxyalkyl ether, penetration≤70 second (0.1% aqueous solution), has good infiltration, emulsification and washing function, can arbitrary proportion and the composite use of water, and its aqueous solution does not become sticky cream.
Alkyl glycoside is also known as APG, synthesized by renewable resources natural fat alcohol and glucose, be the comprehensive new non-ionic surfactants of a kind of performance, have the characteristic of conventional nonionic and anion surfactant concurrently, there is high surface, good ecological security and intermiscibility.APG surface tension is low, without cloud point, HLB value is adjustable, wetting power is strong, strong detergency, foaming abundancy fine and smooth, compatibility is strong, nontoxic, harmless, non-stimulated to skin, biological degradation is thorough rapidly, can be composite with any classes of surfactant, synergistic effect is obvious.There is stronger broad spectrum antibiotic activity, product thickening effect significantly, be easy to dilution, gel-free phenomenon, easy to use.And resistance to highly basic, resistance to strong acid, resistance to hard water, salt-resistance are strong.APG is not in Product Safety (containing harmful by-products dioxanes), and mildness and antibiotic property have advantage, and alternative existing petroleum base surfactant is become main flow surfactant.APG has well moistening and penetration property, do not pollute the features such as crops and soil and hygroscopicity are fabulous, and APG and Determination of Polyoxyethylene Non-ionic Surfactants do not have anti-phase cloud point unlike it, effectively can reduce medical liquid surface tension, delay the evaporation of liquid moisture, keep the hydration dissolved state of agricultural chemicals for a long time, contribute to improving plant leaf surface to the infiltration rate of agricultural chemicals and absorption ratio, suitable used as pesticides emulsifier, wetting powder, insecticide, plant growth regulator, adjustable soil temperature, to weed killer herbicide, insecticide and bactericide have significant synergistic effect.
Two, screening technique
(1) the formula composition screening experiment of compound wetting agent
1, experimental technique
According to for the different performance of examination wetting agent and effect, carry out suitable be combined into the method that 15 compound prescriptions and 6 alone formulas carry out repeated test and screen.
Each component is taken: pesticide active ingredient (copper 8-hydroxyquinolinate: Tebuconazole=2:1) content is 36% according to following mass percent; Dispersant total amount is the composition of 6%(dispersant); Wetting agent (composition of wetting agent and consumption are in table 1) total amount is 2%; Antifreezing agent (ethylene glycol) total amount is 5%; Preservative (Sodium Benzoate) total amount is 0.5%; Thickener: aluminium-magnesium silicate is 0.5%, xanthans is 0.2%; All the other consumption running water are supplied.
The preparation method of agricultural chemicals suspension agent is as follows: in sand mill, drop into pesticide active ingredient, dispersant, wetting agent, preservative, part thickener and water, grinding, when particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add remaining thickener adjustment viscosity again, to obtain final product.
Solution surface tension measures and adopts decylization method, test temperature (28 ± 1) DEG C, and experimental error scope is ± 0,05mN/m, measures 3 times, gets its mean value.
The mensuration of persistent foamability: add 180ml standard hard water in 250ml tool plug graduated cylinder, sample 1g, covers stopper, centered by bottom graduated cylinder, then at the uniform velocity put upside down up and down 30 times (each 2s), until particle is all scattered in water, be placed on experimental bench and leave standstill 1min, record foam volume.
The DSAl00 type optical method droplet morphology analytical system that wetting efficiency utilizes Switzerland Kruss company designs to produce measures contact angle and shows, the angle specifically referring to drop and sprawl between surface, when contact angle equals 0 °, show the minimum amount on the moistening blade face of the complete energy of the surface area of selected wetting agent on unit blade face.
2, experimental result
Experimental result is in table 1.
Table 1 wetting agent difference composition affects experimental result to performances such as preparation wetting efficiencies
Wetting efficiency refers to the efficiency of surfactant wetting surface, represent 100% wettability treatment blade face necessary minimum surface activating agent equilibrium concentration in a liquid, generally represent with %W/V (mass/volume), equilibrium concentration value is lower, represent that wetting efficiency is higher, wettability is better.
Isomery 1307, penetrating agent JFC, alkyl glycoside, bleeding agent SF and lauryl sodium sulfate are formed 50 kinds of compound wetting agents according to different mass ratios by this experiment between two, investigated the wetting efficiency of these compound wetting agents on rice crop surface, lasting foam number respectively and be mixed with product surface tension.
From experimental result, the compound wetting agent be made up of isomery 1307 and penetrating agent JFC wetting efficiency, lasting foam number and be mixed with product the performance such as surface tension on significantly to be better than other compound wetting agent, wherein, isomery 1307 and penetrating agent JFC are according to 1-2:1-3, when especially forming according to the mass ratio of 1:1, its wetting efficiency will be far superior to other compound wetting agent, and difference is extremely remarkable.
(2) the optimum consumption screening experiment of compound wetting agent in pesticidal preparations
1, compound wetting agent: be made up of according to the mass ratio of 1:1 isomery 1307 and penetrating agent JFC;
2, experimental technique
In order to filter out the Optimum of wetting agent in pesticidal preparations, flow is held with the liquid increased on rice plant, this experimental design 10 groups of experiments, often group experiment adopts different wetting agent consumptions to prepare 36% copper 8-hydroxyquinolinate/tebuconazole suspension concentrates, often group is except the consumption difference of wetting agent, all the other are all identical, specific as follows:
1st group of experiment: take each component according to following mass percent: pesticide active ingredient (copper 8-hydroxyquinolinate: Tebuconazole=2:1) content is 36%; Dispersant sodium lignin sulfonate total amount is 6%; Compound wetting agent total amount is 0.5%; Antifreezing agent (ethylene glycol) total amount is 5%; Preservative (Sodium Benzoate) total amount is 0.5%; Thickener: aluminium-magnesium silicate is 0.5%, xanthans is 0.2%; All the other consumption running water are supplied.
The preparation method of agricultural chemicals suspension agent is as follows: in sand mill, drop into pesticide active ingredient, dispersant, wetting agent, preservative, part thickener and water, grinding, when particle diameter D90 is at 5 μm, stop grinding, add after antifreezing agent stirs and add remaining thickener adjustment viscosity again, to obtain final product.
2nd group of experiment: compound wetting agent total amount is 1.0%, all the other are all tested with the 1st group identical (consumption of running water is done to adjust accordingly).
3rd group of experiment: compound wetting agent total amount is 1.5%, all the other are all tested with the 1st group identical (consumption of running water is done to adjust accordingly).
4th group of experiment: compound wetting agent total amount is 2.0%, all the other are all tested with the 1st group identical (consumption of running water is done to adjust accordingly).
5th group of experiment: compound wetting agent total amount is 2.5%, all the other are all tested with the 1st group identical (consumption of running water is done to adjust accordingly).
6th group of experiment: compound wetting agent total amount is 3.0%, all the other are all tested with the 1st group identical (consumption of running water is done to adjust accordingly).
7th group of experiment: compound wetting agent total amount is 3.5%, all the other are all tested with the 1st group identical (consumption of running water is done to adjust accordingly).
8th group of experiment: compound wetting agent total amount is 4.0%, all the other are all tested with the 1st group identical (consumption of running water is done to adjust accordingly).
9th group of experiment: compound wetting agent total amount is 4.5%, all the other are all tested with the 1st group identical (consumption of running water is done to adjust accordingly).
10th group of experiment: compound wetting agent total amount is 5.0%, all the other are all tested with the 1st group identical (consumption of running water is done to adjust accordingly).
Be subject with paddy rice, the surface tension of 10 kinds of agricultural chemicals suspension agents prepared by mensuration, hold bubble amount and blade liquid holdup lastingly.
Liquid holdup measuring method on rice leaf is taken out after soaking 10S after being weighed by fresh rice leaf in the surfactant solution of variable concentrations, weigh again when blade does not drip, in triplicate, calculating mean value, then measure leaf area with area measurement instrument, the liquid holdup of unit of account area lobes tentatively judges infiltration and the wettability of liquid.
Solution surface tension measures and adopts decylization method, test temperature (28 ± 1) DEG C, and experimental error scope is ± 0,05mN/m, measures 3 times, gets its mean value.
The mensuration of persistent foamability: add 180ml standard hard water in 250ml tool plug graduated cylinder, sample 1g, covers stopper, centered by bottom graduated cylinder, then at the uniform velocity put upside down up and down 30 times (each 2s), until particle is all scattered in water, be placed on experimental bench and leave standstill 1min, record foam volume.
3, experimental result
Experimental result is in table 2.
Table 2 wetting agent different amounts is on the impact of 36% copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent properties
Show by experiment, the critical surface tension of rice leaf positive and negative is between 29.9-32.8mN/m.The surface tension of clear water is about 72mN/m, is far longer than the critical surface tension of rice leaf, the surface tension that compound wetting agent can reduce water is added in formula, before compound concentration of wetting agent reaches critical micelle concentration, although the surface tension of liquid is less than the critical surface tension of rice leaf, but the hold flow of its liquid on rice leaf increases limited, only have after in liquid, concentration of wetting agent reaches critical micelle concentration, liquid just increases fast at the flow of holding of rice leaf, explanation only has concentration of wetting agent in liquid reach or exceed critical micelle concentration, simultaneously the surface tension of liquid is close to the critical surface tension of rice leaf, just can roll up liquid and hold flow on rice leaf.
From the data of table 2, wetting agent adopts different additions in agricultural chemicals suspension agent, the surface tension of preparation, blade liquid holdup, hold the yet and then change thereupon of the indexs such as bubble amount lastingly, but when its consumption is to certain consumption, it not too obvious that surface tension and liquid holdup change.When interpolation compound wetting agent consumption is 1.5-4.5wt%, the surface tension of liquid is just in time close with the critical surface tension of rice leaf, the blade liquid holdup of paddy rice has remarkable lifting, wherein, when compound wetting agent consumption is 2.5wt%, the blade liquid holdup of paddy rice reaches and is up to 98.9%, has exceeded this consumption, and the blade liquid holdup of paddy rice increases not obvious even on a declining curve.Therefore, the addition of compound wetting agent of the present invention in agricultural chemicals suspension agent is preferably 1.5-4.0wt%, and more preferably 2.0-3.5wt%, most preferably is 2.0-2.5wt%.
Claims (12)
1. an agricultural chemicals compound wetting agent, is characterized in that: be made up of according to the mass ratio of 1:1 isomery 1307 and penetrating agent JFC.
2. agricultural chemicals compound wetting agent according to claim 1 prepare agricultural chemicals suspension agent, pesticide water dispersive granule or agricultural chemicals can purposes in point Wettable Powder.
3. an agricultural chemicals suspension agent, comprising: pesticide active ingredient, dispersant, compound wetting agent, thickener, antifreezing agent, preservative and water; It is characterized in that: described compound wetting agent is compound wetting agent according to claim 1.
4. according to agricultural chemicals suspension agent according to claim 3, it is characterized in that, by mass percentage, the consumption of each component is: pesticide active ingredient 4-70%, dispersant 3-10%, compound wetting agent 1-6%, antifreezing agent 1-8%, preservative 0.1-2%, thickener 0.1-3%, surplus is water.
5. a copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent, its constituent is: by mass percentage, and pesticide active ingredient 10-50%, dispersant 2-10%, compound wetting agent 1.5-4.0%, thickener 0.1-3%, antifreezing agent 1-8%, preservative 0.1-2%, surplus are water; Described pesticide active ingredient is made up of copper 8-hydroxyquinolinate and Tebuconazole; It is characterized in that: described compound wetting agent is agricultural chemicals compound wetting agent according to claim 1.
6. according to copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent according to claim 5, it is characterized in that: by mass percentage, pesticide active ingredient 36%, dispersant 6%, compound wetting agent 1.5-4.0%, thickener 0.7%, antifreezing agent 5%, preservative 0.5%, surplus are water; Described pesticide active ingredient is made up of according to the mass ratio of 1:1-3 Tebuconazole and copper 8-hydroxyquinolinate.
7. according to copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent according to claim 6, it is characterized in that: the consumption of compound wetting agent is 2.0-3.5wt%.
8. according to copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent according to claim 7, it is characterized in that: the consumption of compound wetting agent is 2.0-2.5wt%.
9. prepare a method for the copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent of claim 6-8 described in any one, it is characterized in that, the method comprises: in sand mill, drop into pesticide active ingredient, dispersant, compound wetting agent, preservative, part thickener and water, grinding; When particle diameter D90 is at 2-15 μm, stop grinding, add after antifreezing agent stirs and add remaining thickener adjustment viscosity again, to obtain final product.
10. a copper 8-hydroxyquinolinate agricultural chemicals suspension agent, its constituent is: by mass percentage, and copper 8-hydroxyquinolinate 10-50%, dispersant 2-10%, compound wetting agent 1.5-4.0%, thickener 0.1-3%, antifreezing agent 1-8%, preservative 0.1-2%, surplus are water; It is characterized in that: described compound wetting agent is agricultural chemicals compound wetting agent according to claim 1.
11., according to copper 8-hydroxyquinolinate agricultural chemicals suspension agent according to claim 10, is characterized in that, each Ingredient Amount is: copper 8-hydroxyquinolinate 33.5%, dispersant 6%, compound wetting agent 1.5-4.0%, thickener 0.7%, antifreezing agent 5%, preservative 0.5%.
Copper 8-hydroxyquinolinate Tebuconazole agricultural chemicals suspension agent described in any one of agricultural chemicals suspension agent described in 12. claim 3-4,5-8 or the claim 10-11 application of copper 8-hydroxyquinolinate agricultural chemicals suspension agent in control vegetative bacteria or fungal disease described in any one.
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