CN103283720A - Preparation method of suspending agent - Google Patents
Preparation method of suspending agent Download PDFInfo
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- CN103283720A CN103283720A CN2013102694296A CN201310269429A CN103283720A CN 103283720 A CN103283720 A CN 103283720A CN 2013102694296 A CN2013102694296 A CN 2013102694296A CN 201310269429 A CN201310269429 A CN 201310269429A CN 103283720 A CN103283720 A CN 103283720A
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Abstract
The invention provides a preparation method of a suspending agent. The preparation method comprises the following steps of: (a) evenly mixing a crude pesticide contained in a pesticide composite, a first part by weight of anti-freezing agent auxiliary and water to obtain a mixture, wherein the auxiliary contains a first part by weight of anti-freezing agent, but does not contain a thickener; (b) sanding the mixture for at least two stages, and refluxing for re-sanding a part of the mixture discharged from each stage of sanding to obtain sanded slurry; (c) homogenizing the sanded slurry, a thickener and a second part by weight of anti-freezing agent to obtain the suspending agent. According to the method, the suspending agent is obtained by means of sanding the mixture for at least two stages, refluxing for re-sanding a part of the mixture discharged from each stage of sanding, and homogenizing the sanded slurry, the thickener and the remaining anti-freezing agent. According to the method, the rising of material temperature during sanding is avoided, the material structure is not damaged and the grain size of the obtained suspending agent is uniform, so that the storage stability and the played efficacy of the suspending agent are enhanced.
Description
Technical field
The present invention relates to the composition pesticide technical field, relate in particular to a kind of preparation method of suspending agent.
Background technology
Suspending agent is the pesticides new formulation of the development seventies in 20th century, and international code name is SC, is that pesticide original medicine, auxiliary agent and water mix, and utilizes wet method to carry out the flowable suspended substance of thickness that ultramicro grinding forms.Suspending agent be by the insoluble or former medicine of solid that is slightly soluble in water by some auxiliary agent, be scattered in the water the stable liquid-solid attitude system that form the tiny higher suspension of a kind of particle, can flow more equably by ultramicro grinding.Because but suspending agent does not have the dust from flying problem as wet-milling, and nonflammable explosive, particle diameter is little, the biologically active height, good drug efficacy, than great, packaging volume is little, with respect to other formulations of pesticide safety and environmental protections, therefore, SC has become the more kind of application in the water baseization pesticides new formulation.
At present the SC production technology is many sand mills series connection, material after the discharging of one-level sand mill all materials directly enter the secondary sand mill, material all enters three grades of sand mills or directly discharging after the discharging of secondary sand mill.Therefore prior art reaches required particle diameter in order to make material, can only reduce discharging speed fully grinds material, but so, discharging speed reduces and easily causes material livering in sand mill, owing to be subjected to the influence of sand mill quality, make material in the sand mill cavity, retain asynchronism(-nization) and cause the particle diameter distribution wide simultaneously.And the preparation of suspending agent use big molecule as thickener reducing the sedimentation of former medicine particle because its thickening characteristic causes the material temperature rise easily during sand milling, its structure may be destroyed in sand milling simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of suspending agent, method provided by the invention has been avoided the intensification of material when sand milling, has controlled the quality index of suspending agent well, the suspending agent uniform particle diameter that obtains.
The invention provides a kind of preparation method of suspending agent, may further comprise the steps:
A) pesticide original medicine that composition pesticide is comprised, auxiliary agent and water mix, and obtain mixed material after mixing, and described auxiliary agent comprises the antifreezing agent of first mass parts, and does not comprise thickener;
B) described mixed material is carried out two-stage sand milling at least, the part discharging of every grade of sand milling refluxes and carries out sand milling again, obtains the slurry behind the sand milling;
C) antifreezing agent with described sand milling discharging and thickener and second mass parts carries out homogeneous, obtains suspending agent.
Preferably, the progression of described sand milling is 2 grades～5 grades.
Preferably, the particle diameter D50 of described sand milling discharging disposed slurry is 0.1 μ m～30 μ m.
Preferably, the particle diameter D50 of described sand milling discharging disposed slurry is 1 μ m～20 μ m
Preferably, the capacity of returns of described every grade of sand milling is 9%～91%.
Preferably, the capacity of returns 44%～83% of described every grade of sand milling.
Preferably, the temperature of described sand milling is 5 ℃～45 ℃.
Preferably, the time of described homogeneous is 10min～120min.
Preferably, the mass content of active ingredient is 5%～80% in the composition pesticide.
Preferably, described step a) is specially:
The antifreezing agent of the former medicine of pesticide original medicine that composition pesticide is comprised, dispersant, wetting agent, first mass parts, defoamer, preservative, structure regulator and water mix, in employing homogenizer, dispersion machine or the colloid mill one or more are uniformly dispersed, and obtain mixed material.
The invention provides a kind of preparation method of suspending agent, may further comprise the steps: a) pesticide original medicine that composition pesticide is comprised, auxiliary agent and water mix, obtain mixed material after mixing, described auxiliary agent comprises the antifreezing agent of first mass parts, and does not comprise thickener; B) described mixed material is carried out two-stage sand milling at least, the part discharging of every grade of sand milling refluxes and carries out sand milling again, obtains the slurry behind the sand milling; C) antifreezing agent with described sand milling discharging and thickener and second mass parts carries out homogeneous, obtains suspending agent.The mixed material that method provided by the invention obtains after each component of composition pesticide is mixed carries out two-stage sand milling at least, in the process of carrying out sand milling, part backflow of slurry in the discharging that every grade of sand milling is obtained is carried out sand milling again, the rest parts slurry enters next stage sand grinding process or the qualified discharging of particle diameter, and after sand milling is finished, again the slurry that obtains and the antifreezing agent of thickener and second mass parts are carried out homogeneous, obtain suspending agent.Method provided by the invention is with the part discharging of the every grade of sand milling sand milling again that refluxes, and after finishing sand milling, add thickener again, thereby avoided in sand grinding process because the material that thickener causes intensification, just can not destroy the structure of pesticide original medicine yet, and the suspending agent even particle size that obtains of method provided by the invention, be conducive to improve the bin stability of suspending agent and the performance of drug effect.
In addition, method provided by the invention is convenient to control technological parameter and the condition of sand milling, and easy to operate, is convenient to quality index is controlled, and obtains suspending agent efficiently.
Embodiment
The invention provides a kind of preparation method of suspending agent, may further comprise the steps:
A) pesticide original medicine that composition pesticide is comprised, auxiliary agent and water mix, and obtain mixed material after mixing, and described auxiliary agent comprises the antifreezing agent of first mass parts, and does not comprise thickener;
B) described mixed material is carried out two-stage sand milling at least, the part discharging of every grade of sand milling refluxes and carries out sand milling again, obtains the slurry behind the sand milling;
C) antifreezing agent with described sand milling discharging and thickener and second mass parts carries out homogeneous, obtains suspending agent.
Method provided by the invention is carried out two-stage sand milling at least after other components except thickener in the composition pesticide are mixed, and the part backflow of slurry of every grade of sand milling discharging is carried out sand milling again, remaining slurry carries out next stage sand milling or the qualified discharging of particle diameter, finishes discharging until sand milling; Antifreezing agent with the slurry behind the sand milling that obtains and thickener and second mass parts carries out homogeneous then, obtains suspending agent.Method provided by the invention is mixed antifreezing agent at twice with pesticide original medicine, and behind sand milling, add thickener again, and in the process of sand milling, part backflow of slurry with every grade of sand milling discharging, thereby avoided the intensification of material in the sand grinding process, just can not destroy the structure of pesticide original medicine yet, just can not influence the performance of the suspending agent drug effect that obtains yet.And the suspending agent particle size that method provided by the invention obtains is even, the performance that is conducive to improve its bin stability and drug effect.
The pesticide original medicine that the present invention comprises composition pesticide, auxiliary agent and water mix, and obtain mixed material after mixing, and described auxiliary agent comprises the antifreezing agent of first mass parts, and does not comprise thickener.The pesticide original medicine that the present invention preferably comprises composition pesticide, above-mentioned auxiliary agent and water mix, in employing homogenizer, dispersion machine and the colloid mill one or more are uniformly dispersed, obtain mixed material, as said components being disperseed in dispersant earlier, and then the material that obtains ground in colloid mill, obtain mixed material.The present invention does not have special restriction to the kind of described composition pesticide, method provided by the invention is applicable to the preparation of different types of agricultural chemicals suspension agent well known to those skilled in the art, this area can be according to the kind difference of the agricultural chemicals suspension agent for preparing, select the proportioning of suitable composition pesticide, can prepare atrazine 500g/L SC as method provided by the invention, piperazine humulone 48%SC, diuron 800g/L SC etc., those skilled in the art can be according to the kind difference of the suspending agent for preparing, and the component and the proportioning thereof that adopt its composition pesticide of knowing to comprise get final product.
In the present invention, described auxiliary agent comprises the antifreezing agent of first mass parts, and does not comprise thickener.When method provided by the invention is mixed in the component that composition pesticide is comprised, do not comprise thickener in the auxiliary agent that adopts, and only the antifreezing agent with first mass parts mixes with former medicine and water, and the antifreezing agent of remaining second mass parts mixes with slurry behind the sand milling with one of thickener in subsequent technique.The present invention is to the kind of described auxiliary agent, and the mass ratio of auxiliary agent and pesticide original medicine and water do not have special restriction, and those skilled in the art can select the proportioning between auxiliary agent well known to those skilled in the art and each component according to the kind difference of preparation suspending agent.
In the present invention, described auxiliary agent preferably includes antifreezing agent, defoamer, preservative and the structure regulator of dispersant, wetting agent, first mass parts.In the present invention, the purpose that wetting agent uses, the first help to get rid of the air on the former medicine ion surface, add fast particle and enter wetting speed in the water, make ion wetting rapidly; It two is to reduce viscosity, is convenient to better grinding.The present invention does not have special restriction to the kind of described wetting agent, adopt wetting agent well known to those skilled in the art to get final product, as adopting among lauryl sodium sulfate, alcohol ethoxylate, alkylphenol ethoxylate, octadecyl sodium sulfosuccinate and the wetting agent S one or more;
In the present invention, dispersant is flocculation and the cohesion that suppresses particle in the disperse phase, play a part stable suspersion agent formulation and promote dispersion liquid to enter to be diluted to unit for uniform suspension in the water, and be conducive to the user and spray application to target: the present invention does not have special restriction to the kind of described dispersant, adopt dispersant well known to those skilled in the art to get final product, as adopting in lignin sulfonic acid salt, naphthalene sulfonic acid-formaldehyde condensation product class, phosphoric acid ester and the polyethers dispersant one or more;
Contain a large amount of water in the pesticide suspension concentrate, form crystallization and reunion in production in the environment of low temperature, storage and the application process easily, influence properties of product.Antifreezing agent can improve the stability under the pesticide suspension concentrate low-temperature cold condition.The present invention does not have special restriction to the kind of described antifreezing agent, adopts antifreezing agent well known to those skilled in the art to get final product, as adopting the polyalcohols antifreezing agent, as ethylene glycol, propane diols, glycerine; Can also adopt the glycols antifreezing agent, as diethylene glycol (DEG), triethylene glycol, polyethylene glycol etc.;
The dispersion impeller that pesticide suspension concentrate rotates is at a high speed in process of production brought ambient air into dispersion easily, forms atomic little bubble, and this not only can influence viscosity, metering and the packing of product, and can reduce production efficiency.The a large amount of bubbles that produce in the process can be effectively eliminated in the adding of defoamer, enhance productivity.The present invention does not have special restriction to the kind of described defoamer, adopt defoamer well known to those skilled in the art to get final product, silicone based as adopting, polyethers, C8～C10 aliphatic alcohols and C10～C20 aliphatic carboxylic acid and lipid thereof, ester-ether type compound and cocoa butter EO-PO polymer etc.;
In the present invention, described preservative can adopt acetaldehyde, formaldehyde, Sodium Benzoate, polyformaldehyde, sodium citrate, sodium salicylate and sorbitol etc.;
In the present invention, form certain thixotroping structure in order to make pesticide suspension concentrate, need to add the certain structure conditioning agent.The particle that the use of structure regulator is not only in order to prevent from disperseing produces separation and precipitation or syneresis because of gravitate, but also in order to adjust the flowability of rheological characteristic and liquid.The present invention does not have special restriction to the kind of described structure regulator, adopts structure regulator well known to those skilled in the art to get final product, and can adopt the strong inorganic matter of hydrability, as aluminium-magnesium silicate, bentonite, attapulgite etc.; Also can adopt the high molecular polymer of good hydrophilic property such as carboxymethyl cellulose, xanthans, soluble starch etc.
The present invention does not have special restriction to the mass ratio of described auxiliary agent and pesticide original medicine and water, and those skilled in the art can adopt the agricultural-chemical suspension agent prescription of knowing according to the kind of suspending agent.In the present invention, the mass content of active ingredient is preferably 5%～80% in the composition pesticide, and more preferably 30%～70%.
After obtaining mixed material, the present invention carries out the two-stage sand milling at least with described mixed material, and the part discharging of every grade of sand milling refluxes and carries out sand milling again, obtains the slurry behind the sand milling.The present invention carries out the two-stage sand milling at least with the mixed material that obtains, preferably carry out 2～5 grades of sand millings, more preferably carry out 3 grades of sand millings, and the part backflow of slurry that the discharging of every grade of sand milling obtains carried out sand milling again, preferably be back to sand milling at the corresponding levels and carry out sand milling again, the slurry of remainder enters next stage sand milling or the qualified discharging of particle diameter.In the present invention, the capacity of returns of every grade of sand milling is preferably 9%～91%, and more preferably 44%～83%, most preferably be 50～80%; The material that the present invention will enter next stage sand milling or the qualified discharging of particle diameter is designated as material A, the material of the part that refluxes is designated as material B, the mass ratio of described material A and material B is preferably 1:(0.1～10), 1:(0.8～5 more preferably), most preferably be 1:(1～4).In the present invention, the particle diameter D50 of the slurry that described sand milling discharging obtains is preferably 0.1 μ m～30 μ m, and more preferably 1 μ m～20 μ m most preferably are 1 μ m～5 μ m; In the present invention, the temperature of described sand milling is preferably 5 ℃～45 ℃, more preferably 10 ℃～40 ℃, most preferably is 15 ℃～35 ℃;
The present invention does not have special restriction to the method for described sand milling, adopts sand mill well known to those skilled in the art that the mixed material that obtains is carried out sand milling and gets final product.The present invention preferably adopts 2～5 sand mills, and described sand mill is connected, more preferably 3;
After finishing the sand milling to mixed material, the present invention after with described sand milling slurry and the antifreezing agent of thickener and remaining second mass parts carry out homogeneous, obtain suspending agent.The present invention joins the antifreezing agent of thickener and remaining second mass parts in the slurry behind the sand milling preferably under processing condition, after more preferably the antifreezing agent of thickener and second mass parts being mixed, joins in the slurry behind the sand milling again.In the present invention, the mass ratio of the antifreezing agent that described first quality is divided and the antifreezing agent of described second mass parts is preferably (2～5): 2, and 3:2 more preferably.
In the present invention, thickener can make suspending agent obtain suitable viscosity (250cp～1000cp), thus reduce the sedimentation of particle.The present invention does not have special restriction to kind and the consumption of described thickener, and the thickener that adopts suspending agent well known to those skilled in the art to adopt gets final product, as adopting organic thickening agent, as gum Arabic, xanthans, CMC polyvinyl alcohol, polyvinyl pyrrolidone etc.; Also can adopt inorganic thickening agent, as aluminium-magnesium silicate and bentonite; In the present invention, the time of described homogeneous is preferably 10 minutes～120 minutes, and more preferably 20 minutes～100 minutes, 30min～90min more preferably.
The invention provides a kind of preparation method of suspending agent, may further comprise the steps: a) pesticide original medicine that composition pesticide is comprised, auxiliary agent and water mix, obtain mixed material after mixing, described auxiliary agent comprises the antifreezing agent of first mass parts, and does not comprise thickener; B) described mixed material is carried out two-stage sand milling at least, the part discharging of every grade of sand milling refluxes and carries out sand milling again, obtains the slurry behind the sand milling; C) antifreezing agent with described sand milling discharging and thickener and second mass parts carries out homogeneous, obtains suspending agent.The mixed material that method provided by the invention obtains after each component of composition pesticide is mixed carries out two-stage sand milling at least, in the process of carrying out sand milling, part backflow of slurry in the discharging that every grade of sand milling is obtained is carried out sand milling again, the rest parts slurry enters next stage sand grinding process or the qualified discharging of particle diameter, and after sand milling is finished, again the slurry that obtains and the antifreezing agent of thickener and second mass parts are carried out homogeneous, obtain suspending agent.Method provided by the invention is with the part discharging of the every grade of sand milling sand milling again that refluxes, and after finishing sand milling, add thickener again, thereby avoided in sand grinding process because the material that thickener causes intensification, just can not destroy the structure of pesticide original medicine yet, and the suspending agent even particle size that obtains of method provided by the invention, be conducive to improve the bin stability of suspending agent and the performance of drug effect.
In addition, method provided by the invention is convenient to control technological parameter and the condition of sand milling, and easy to operate, is convenient to quality index is controlled, and obtains suspending agent efficiently.
In order to further specify the present invention, below in conjunction with embodiment the preparation method of suspending agent provided by the invention is described in detail, but they can not be interpreted as restriction to protection domain of the present invention.
Embodiment 1
In the 1500L charging tank, add the former medicine of 470kg97% atrazine, the fragrant polyoxyethylene ether phosphate 50kg of alkyl, ethylene glycol 30kg, aluminium-magnesium silicate 5kg, benzoic acid 2kg and 422kg water are uniformly dispersed with dispersion machine, through the colloid mill coarse crushing, obtain mixed material;
With the mixed material process two-stage sand milling that obtains, the capacity of returns of one-level sand milling is 40%～50% then, and the capacity of returns of secondary sand milling is 30～40%, and the sand milling temperature is between 20 ℃～30 ℃, and sand milling disposed slurry D50 controls between 1 μ m～2 μ m;
After sand milling is finished, the slurry that obtains is got to the discharge tank of 1500L, start homogeneous limit, homogenizer limit to wherein adding 1kg xanthans and 20kg ethylene glycol.Obtain atrazine 500g/L SC behind the homogeneous 30min.
Embodiment 2
In the 5000L charging tank, add the former medicine of 1500kg96% piperazine humulone, lignosulfonates 150kg, propane diols 90kg, aluminium-magnesium silicate 15kg, benzoic acid 3kg and 1179kg water are uniformly dispersed with dispersion machine, through the colloid mill coarse crushing, obtain mixed material;
Then with the mixed material that obtains through three grades of sand millings, one-level sand milling capacity of returns is 40%～50%, and secondary sand milling capacity of returns is that 30%～40%, three grades of sand milling capacities of returns are 30%～40%, the sand milling temperature is between 20 ℃～30 ℃, and sand milling disposed slurry D50 controls between 1.5 μ m～2.5 μ m;
After sand milling is finished, the slurry that obtains is got to the 5000L discharge tank, start homogeneous limit, homogenizer limit to wherein adding 3kg xanthans and 60kg propane diols, obtain piperazine humulone 480g/L SC behind the homogeneous 60min.
Embodiment 3
In the 5000L charging tank, add the former medicine of 1970kg96% diuron, acrylic acid copolymer-maleic anhydride 240kg, propane diols 90kg, aluminium-magnesium silicate 15kg, benzoic acid 3kg and 620kg water, be uniformly dispersed with dispersion machine, through the colloid mill coarse crushing, obtain mixed material;
Then with the mixed material that obtains through three grades of sand millings, one-level sand milling capacity of returns is 50%～60%, and secondary sand milling capacity of returns is that 40%～50%, three grades of sand milling capacities of returns are 50%～60%, the sand milling temperature is between 25 ℃～35 ℃, and sand milling disposed slurry D50 controls between 1 μ m～2.5 μ m;
After sand milling is finished, the slurry that obtains is got to the 5000L discharge tank, start homogeneous limit, homogenizer limit to wherein adding 2.4kg xanthans and 60kg propane diols, obtain diuron 800g/L SC behind the homogeneous 40min.
Embodiment 4
In the 1500L charging tank, add the former medicine of 323kg96% thiophene worm piperazine, acrylic acid copolymer-maleic anhydride 50kg, propane diols 30kg, aluminium-magnesium silicate 5kg, benzoic acid 1kg and 569kg water, be uniformly dispersed with dispersion machine, through the colloid mill coarse crushing, obtain mixed material;
Then with the mixed material that obtains through three grades of sand millings, one-level sand milling capacity of returns is 30%～50%, and secondary sand milling capacity of returns is that 30%～50%, three grades of sand milling capacities of returns are 40%～60%, the sand milling temperature is between 25 ℃～35 ℃, and sand milling disposed slurry D50 controls between 2 μ m～3 μ m;
After sand milling is finished, the slurry that obtains is got to the 1500L discharge tank, start homogeneous limit, homogenizer limit to wherein adding 2kg xanthans and 20kg propane diols, homogeneous 30min obtains thiophene worm piperazine 350g/L SC.
Embodiment 5
In the 1500L charging tank, add the former medicine of 508kg97% Imidacloprid, acrylic acid copolymer-maleic anhydride 50kg, propane diols 30kg, aluminium-magnesium silicate 5kg, benzoic acid 1kg and 374kg water, be uniformly dispersed with dispersion machine, through the colloid mill coarse crushing, obtain mixed material;
Then with the mixed material that obtains through three grades of sand millings, one-level sand milling capacity of returns is 30%～40%, and secondary sand milling capacity of returns is that 30%～40%, three grades of sand milling capacities of returns are 40%～50%, the sand milling temperature is between 25 ℃～35 ℃, and sand milling disposed slurry D50 controls between 1.5 μ m～3.0 μ m;
After sand milling is finished, the slurry that obtains is got to the 1500L discharge tank, start homogeneous limit, homogenizer limit to wherein adding 0.8kg xanthans and 20kg propane diols, obtain Imidacloprid 600g/L SC behind the homogeneous 40min.
Embodiment 6
In the 5000L charging tank, add the former medicine of 2250kg96% tpn, polyvinyl alcohol APEO 240kg, propane diols 30kg, aluminium-magnesium silicate 15kg, benzoic acid 3kg and 1399kg water, be uniformly dispersed with dispersion machine, mix through homogenizer, obtain mixed material;
Then with the mixed material process level Four sand milling that obtains, one-level sand milling capacity of returns is 50%～60%, secondary sand milling capacity of returns is 5%～60%, three grades of sand milling capacities of returns are 50%～60%, level Four sand milling capacity of returns is 50%～60%, the sand milling temperature is between 25 ℃～35 ℃, and sand milling disposed slurry D50 controls between 0.8 μ m～2.0 μ m;
After sand milling is finished, the slurry that obtains is got to the 5000L discharge tank, start homogeneous limit, homogenizer limit to wherein adding 3.2kg xanthans and 60kg propane diols, obtain tpn 720g/L SC behind the homogeneous 60min.
Embodiment 7
In the 1500L charging tank, add the former medicine of 4.1kg98% paclobutrazol, NN010kg, ethylene glycol 30kg, aluminium-magnesium silicate 20kg, paraformaldehyde 1kg and 403kg water, be uniformly dispersed with dispersion machine, through the colloid mill coarse crushing, obtain mixed material;
With the mixed material process two-stage sand milling that obtains, one-level sand milling capacity of returns is 10%～20% then, and secondary sand milling capacity of returns is 30%～40%, and the sand milling temperature is between 20 ℃～35 ℃, and sand milling disposed slurry D50 controls between 0.8 μ m～1.5 μ m;
After sand milling is finished, the slurry that obtains is got to the 1500L discharge tank, start homogeneous limit, homogenizer limit to wherein adding 2kg xanthans, 30kg ethylene glycol and 500kg water, obtain paclobutrazol 4g/L SC behind the homogeneous 30min.
Embodiment 8
In the 5000L charging tank, add 1310kg98% carbendazim active compound, polyvinyl alcohol APEO 150kg, propane diols 90kg, aluminium-magnesium silicate 15kg, benzoic acid 3kg and 1347kg water, be uniformly dispersed with dispersion machine, mix through homogenizer, obtain mixed material;
With the mixed material process secondary sand milling that obtains, one-level sand milling capacity of returns is 50%～60% then, and secondary sand milling capacity of returns is 50%～60%, and the sand milling temperature is between 20 ℃～30 ℃, and sand milling disposed slurry D50 controls between 1.2 μ m～2.0 μ m;
After sand milling is finished, the slurry that obtains is got to the 5000L discharge tank, start homogeneous limit, homogenizer limit to wherein adding 4.5kg xanthans and 60kg propane diols, obtain carbendazim 500g/L SC behind the homogeneous 30min.
The present invention detects the carbendazim 500g/L SC that obtains, and the result is as shown in table 1, the testing result that table 1 obtains for the embodiment of the invention 8.
The testing result that table 1 embodiment of the invention 8 obtains.
As can be seen from Table 1, the suspending agent that method provided by the invention obtains has higher suspensibility, and even particle size can be all by 400 order wet screenings, and have higher bin stability.
Comparative example
In the 5000L charging tank, add 1310kg98% carbendazim active compound, polyvinyl alcohol APEO 150kg, propane diols 90kg, aluminium-magnesium silicate 15kg, benzoic acid 3kg and 1347kg water, be uniformly dispersed with dispersion machine, mix through homogenizer, obtain mixed material; Adding residue 60kg propane diols and 4.5kg xanthans again mixes through homogenizer.
With the mixed material process secondary sand milling that obtains, one-level sand milling and secondary sand milling do not reflux then, and the sand milling temperature is between 20 ℃～30 ℃, and sand milling disposed slurry D50 controls between 1.2 μ m～2.0 μ m; Obtain carbendazim 500g/L SC.
The present invention detects the carbendazim 500g/L SC that obtains, and the result is as shown in table 2, the testing result that table 2 obtains for comparative example of the present invention.
The testing result that table 2 comparative example of the present invention obtains
Contrast technology of the present invention (embodiment 8) and can find that with traditional handicraft (comparative example) this technology has improved for the uniformity of material particles sand milling, do not have the following bulky grain of 400 orders.Traditional handicraft 400 order wet screening percent of pass stop up mister head easily less than 100%.Traditional handicraft is because oarse-grained existence causes suspensibility low slightly simultaneously, and heat storage back bulky grain sedimentation causes the partial material sedimentation knot end.
As seen from the above embodiment, the invention provides a kind of preparation method of suspending agent, may further comprise the steps: a) pesticide original medicine that composition pesticide is comprised, auxiliary agent and water mix, and obtain mixed material after mixing, described auxiliary agent comprises the antifreezing agent of first mass parts, and does not comprise thickener; B) described mixed material is carried out two-stage sand milling at least, the part discharging of every grade of sand milling refluxes and carries out sand milling again, obtains the slurry behind the sand milling; C) antifreezing agent with described sand milling discharging and thickener and second mass parts carries out homogeneous, obtains suspending agent.The mixed material that method provided by the invention obtains after each component of composition pesticide is mixed carries out two-stage sand milling at least, in the process of carrying out sand milling, part backflow of slurry in the discharging that every grade of sand milling is obtained is carried out sand milling again, the rest parts slurry enters next stage sand grinding process or the qualified discharging of particle diameter, and after sand milling is finished, again the slurry that obtains and the antifreezing agent of thickener and second mass parts are carried out homogeneous, obtain suspending agent.Method provided by the invention is with the part discharging of the every grade of sand milling sand milling again that refluxes, and after finishing sand milling, add thickener again, thereby avoided in sand grinding process because the material that thickener causes intensification, just can not destroy the structure of pesticide original medicine yet, and the suspending agent even particle size that obtains of method provided by the invention, be conducive to improve the bin stability of suspending agent and the performance of drug effect.
In addition, method provided by the invention is convenient to control technological parameter and the condition of sand milling, and easy to operate, is convenient to quality index is controlled, and obtains suspending agent efficiently.
The above only is preferred embodiment of the present invention; should be pointed out that for those skilled in the art, under the prerequisite that does not break away from the principle 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 (10)
1. the preparation method of a suspending agent may further comprise the steps:
A) pesticide original medicine that composition pesticide is comprised, auxiliary agent and water mix, and obtain mixed material after mixing, and described auxiliary agent comprises the antifreezing agent of first mass parts, and does not comprise thickener;
B) described mixed material is carried out two-stage sand milling at least, the part discharging of every grade of sand milling refluxes and carries out sand milling again, obtains the slurry behind the sand milling;
C) antifreezing agent with described sand milling discharging and thickener and second mass parts carries out homogeneous, obtains suspending agent.
2. method according to claim 1 is characterized in that, the progression of described sand milling is 2 grades～5 grades.
3. preparation method according to claim 1 is characterized in that, the particle diameter D50 of described sand milling discharging disposed slurry is 0.1 μ m～30 μ m.
4. preparation method according to claim 1 is characterized in that, the particle diameter D50 of described sand milling discharging disposed slurry is 1 μ m～20 μ m.
5. preparation method according to claim 1 is characterized in that, the capacity of returns of described every grade of sand milling is 9%～91%.
6. according to claim 1 or 4 any described preparation methods, it is characterized in that the capacity of returns 44%～83% of described every grade of sand milling.
7. preparation method according to claim 1 is characterized in that, the temperature of described sand milling is 5 ℃～45 ℃.
8. preparation method according to claim 1 is characterized in that, the time of described homogeneous is 10min～120min.
9. preparation method according to claim 1 is characterized in that, the mass content of active ingredient is 5%～80% in the composition pesticide.
10. preparation method according to claim 1 is characterized in that, described step a) is specially:
The antifreezing agent of the former medicine of pesticide original medicine that composition pesticide is comprised, dispersant, wetting agent, first mass parts, defoamer, preservative, structure regulator and water mix, in employing homogenizer, dispersion machine or the colloid mill one or more are uniformly dispersed, and obtain mixed material.
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| CN201310269429.6A CN103283720B (en) | 2013-06-26 | 2013-06-26 | Preparation method of suspending agent |
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| CN105028509A (en) * | 2015-07-23 | 2015-11-11 | 安徽省圣丹生物化工有限公司 | Preparation method of efficient herbicide |
| CN105494400A (en) * | 2016-02-04 | 2016-04-20 | 南宫市荣威生物药业有限公司 | Atrazine-containing weeding suspending agent and preparation method thereof |
| CN109845766A (en) * | 2019-03-18 | 2019-06-07 | 海南博士威农用化学有限公司 | The suspending agent and preparation method and application for preventing and treating Tirathaba Rufivena On Areca Palms and Brontispa longissima |
| CN109953030A (en) * | 2017-12-25 | 2019-07-02 | 江苏托球农化股份有限公司 | A kind of Paclobutrazol suspension concentrate and preparation method thereof |
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| CN105028509A (en) * | 2015-07-23 | 2015-11-11 | 安徽省圣丹生物化工有限公司 | Preparation method of efficient herbicide |
| CN105494400A (en) * | 2016-02-04 | 2016-04-20 | 南宫市荣威生物药业有限公司 | Atrazine-containing weeding suspending agent and preparation method thereof |
| CN109953030A (en) * | 2017-12-25 | 2019-07-02 | 江苏托球农化股份有限公司 | A kind of Paclobutrazol suspension concentrate and preparation method thereof |
| CN109845766A (en) * | 2019-03-18 | 2019-06-07 | 海南博士威农用化学有限公司 | The suspending agent and preparation method and application for preventing and treating Tirathaba Rufivena On Areca Palms and Brontispa longissima |
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| CN103283720B (en) | 2014-08-27 |
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