CN107439546A - A kind of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation and preparation method thereof - Google Patents

A kind of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation and preparation method thereof Download PDF

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Publication number
CN107439546A
CN107439546A CN201710733326.9A CN201710733326A CN107439546A CN 107439546 A CN107439546 A CN 107439546A CN 201710733326 A CN201710733326 A CN 201710733326A CN 107439546 A CN107439546 A CN 107439546A
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suspending agent
hydrophobic pesticidal
oil phase
preparation
hydrophobic
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刘昆
程文
王乐强
邓小楠
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Hefei University of Technology
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Hefei University of Technology
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/18Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
    • A01N37/26Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof containing the group; Thio analogues thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/02Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/26Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
    • A01N25/28Microcapsules or nanocapsules

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a kind of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation and preparation method thereof, and wherein mix preparation is the mixture of hydrophobic pesticidal microcapsule formulations and hydrophobic pesticidal suspending agent;The hydrophobic pesticidal microcapsule formulations are made up of microcapsule wall material and core, and the microcapsule wall material is polycaprolactone, and the core is hydrophobic pesticidal Acetochlor;The hydrophobic pesticidal suspending agent is Acetochlor suspending agent.The present invention is by the design to core wall material Solvent Anti-solvent system, and using coaxial needles capitiform into certain droplet, the mixing formulation of Acetochlor microcapsule formulations and suspending agent is prepared using the step of solvent extraction method one.Mixing dosage form product can not only improve the lasting effect of agricultural chemicals and utilization rate, prevent from abusing, and can reduce and eliminate pollution of the agricultural chemicals to environment.Present invention mixing dosage form product 48h internal stabilities are good, the sustained release phase reaches more than 25d, have good ecological benefits and economic value.

Description

A kind of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation and preparation method thereof
Technical field
The present invention relates to a kind of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation and preparation method thereof, belong to agricultural chemicals The technology field of improving dosage form.
Background technology
The missible oil formulation of hydrophobic pesticidal is that China is currently being widely used a kind of formulations of pesticide.But such formulations of pesticide Both sides wretched insufficiency often be present:(1) lasting effect is low, effective rate of utilization is relatively low, easily causes agricultural chemicals to be abused, to ecological ring Cause serious threat in border;(2) it is generally poisonous and harmful using organic solvent auxiliary material in production process, cause production process and finished product pair Environmental pollution is serious.Therefore, the rational modification of hydrophobic pesticidal missible oil formulation, that is, the less premise of its cost increase is being ensured Under, on the one hand increase operation rate and lasting effect, one side reduce pollution of the product to environment, there is important practical significance and answer With value.Currently used hydrophobic pesticidal missible oil, which improves formulation, to be included:(1) microcapsule formulations, (2) suspending agent formulation.Wherein, Microcapsule formulations can significantly improve the lasting effect and utilization rate of agricultural chemicals, but preparation process is complicated and the wave of pesticide original medicine be present Take, therefore cost is higher.Suspending agent formulation can eliminate in missible oil formulation the use of poisonous and harmful auxiliary material solvent and without agricultural chemicals The waste of active compound, but the lasting effect of agricultural chemicals can not be improved.
The content of the invention
In order to avoid above-mentioned the shortcomings of the prior art part, the present invention is intended to provide a kind of hydrophobic pesticidal microcapsules Agent and suspending agent mix preparation and preparation method thereof.Hydrophobic pesticidal mix preparation of the present invention can overcome existing hydrophobicity agriculture The problems such as utilization rate existing for medicine missible oil formulation is low, and environmental pollution is serious, there is the advantages of having good stability, the lasting period is long.
The present invention is according to drop engineering general principle, using coaxial syringe needle, using solvent extraction method, by core-wall The design of material-solvent-antisolvent system and the simplification to process, realize that one-step method prepares the microcapsules of hydrophobic pesticidal Acetochlor Agent and the mixing formulation of suspending agent.The raising agricultural chemicals utilization rate for mixing formulation while there are microcapsule formulations and lasting effect of the invention The use of the elimination organic solvent auxiliary material of advantage and suspending agent, reduce the advantages of environmental pollution.Meanwhile microcapsule formulations and suspension Agent and can enough overcomes the shortcomings that other side.In addition, the preparation method of the mixing formulation has simple and easy, it is excellent that running cost is low etc. Point.
The mix preparation of hydrophobic pesticidal microcapsule formulations and suspending agent of the present invention, be hydrophobic pesticidal microcapsule formulations with it is hydrophobic The mixture of property agricultural chemicals suspension agent, it is also assumed that being hydrophobic pesticidal microcapsule formulations and suspension of the hydrophobic pesticidal in water Liquid.
The hydrophobic pesticidal microcapsule formulations are made up of microcapsule wall material and core, and the microcapsule wall material is polycaprolactone (PCL), the core is hydrophobic pesticidal Acetochlor (active ingredient is 92.2% acetochlor tc).
The total content of effective agricultural chemicals Acetochlor is 0.1-0.4wt% in mix preparation;Hydrophobic pesticidal is micro- in mix preparation The mass concentration of capsule is 0.25-0.45wt%, in hydrophobic pesticidal microcapsules effectively the content of agricultural chemicals Acetochlor for 5~ 25wt%.
The hydrophobic pesticidal suspending agent is Acetochlor suspending agent, mass concentration 0.08-0.20wt%;In addition institute State and also contain surfactant in hydrophobic pesticidal suspending agent, the mass concentration of surfactant is 0.5-1wt%.The surface Activating agent is neopelex (SDBS) or polyvinyl alcohol (PVA).
The Biodegradable high-molecular that the microcapsule wall material that the present invention uses is ratified for U.S.'s food with Bureau of Drugs Supervision (FDA)- Polycaprolactone, its molecular weight are Mw=1.4 × 105g/mol。
The preparation method of hydrophobic pesticidal microcapsule formulations of the present invention and suspending agent mix preparation, is prepared by solvent extraction method Obtain, comprise the following steps:
Step 1:Microcapsule wall material is dissolved in acquisition oil phase A in acetone, hydrophobic pesticidal is dissolved in acetone and obtains oil Phase B, surfactant is dissolved in deionized water and obtains aqueous phase C;Hydrophobic pesticidal in microcapsule wall material and oil phase B in oil phase A Mass fraction summation be 5%, the mass fraction of surfactant is 0.5-1% in aqueous phase C;
The microcapsule wall material is polycaprolactone, and the hydrophobic pesticidal is Acetochlor.
Step 2:Under conditions of constant temperature at the uniform velocity stirs, aqueous phase C constant temperature is at 25-40 DEG C, and mixing speed is in 500- 1000rpm;Oil phase A and oil phase B are separately added into the outer tube and inner tube of coaxial syringe needle with syringe pump, and formed in syringe needle end Drop;Oil phase A and oil phase B (being slowly added dropwise with the speed for being about 5 drop per second), oil phase A is added dropwise into aqueous phase C by coaxial needle tubing It is 1 with oil phase B gross mass and aqueous phase C mass ratio:5;
Step 3:Solvent acetone in oil phase A and oil phase B is soluble in water, triggers and is separated, is persistently stirred 2~4h of liquid Volatilized completely to acetone, the solidification of macromolecule wall material, obtain hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation.
The present invention selects appropriate low boiling point solvent according to hydrophobic pesticidal and parcel wall material and prepares respective solution.Profit The mixing of the pesticide solution and wall material solution and the formation of drop are realized with the flowing in coaxial syringe needle.Selected according to described solvent Anti-solvent, and drop is slowly dropped into the anti-solvent for adding surfactant and control temperature.Utilize solvent and anti-solvent Between the characteristic dissolved each other, by quick phase separation, i.e. solvent extraction method, realize the recrystallization and high score of pesticide original medicine Sub- wall material quickly prepares the microcapsule formulation of hydrophobic pesticidal to the cladding of hydrophobic pesticidal particle.The agricultural chemicals not being wrapped by Grain, disperse in the anti-solvent containing surfactant, form the suspending agent of hydrophobic pesticidal.Product of the present invention is hydrophobicity agriculture The mixture of medicine microcapsule formulations and its suspending agent.
Compared with prior art, the invention has the advantages that:
Hydrophobic pesticidal microcapsule formulations of the present invention compared with existing emulsifiable concentrates for agricultural chemicals formulation, have agriculture with suspending agent mix preparation Medicine lasting effect and utilization rate are higher, without using poisonous and hazardous organic solvent auxiliary material, prevent agricultural chemicals from abusing and reducing ambient wind The advantages such as danger;Compared with existing suspending agent formulation, there is higher agricultural chemicals lasting effect and utilization rate;Compared with microcapsule formulations, The hydrophobic pesticidal not being embedded be made suspending agent can make full use of pesticide original medicine thus product cost it is relatively low.
Preparation method of the present invention has simple to operate, it is easy to accomplish and cost it is cheap the advantages that.
Brief description of the drawings
Fig. 1 is the structural representation of the coaxial needle tubing used in preparation process of the present invention.
Fig. 2 be the embodiment of the present invention 1,2,3 under 298K, microcapsules 25d in deionized water release profiles.From Fig. 2 In as can be seen that embodiment 1 microcapsule product release it is most fast, the release of embodiment 3 is taken second place, and embodiment 2 discharge it is most slow. It can be found that aqueous phase speed of agitator improves the release of product can be caused to subtract by the contrast of the preparation condition of embodiment 1 and embodiment 2 It is slow.This is due to that polymer solution phase separation speed is slower when speed of agitator is relatively low, the relatively low reason of the coating gas porosity of formation. From embodiment 2 and embodiment 3 relatively, aqueous phase temperature, which improves, causes product release to be accelerated, and this is due to that higher temperature adds Fast polymer solution is separated, i.e. the solidification process of polymer wall material, forms the higher coating of gas porosity.In addition, releasing in 25d Put in experimentation, the cumulative release of all products is below 50%.
Fig. 3 be the embodiment of the present invention 1,4,5 under 298K, microcapsules 25d in deionized water release profiles.From Fig. 3 In as can be seen that the release of the microcapsule product of embodiment 1 is most fast, the slightly below embodiment 1 of embodiment 4, and embodiment 5 discharges It is most slow.Contrasted by the preparation condition of embodiment 1 and embodiment 4 it can be found that reducing surfactant SDBS dosage to product Release influence it is little.The contrast of embodiment 1 and embodiment 5 shows, production can be significantly slowed using PVA as surfactant Product are released.This is probably because PVA presence can slow down solidification, forms finer and close wall material coating.In addition, releasing in 25d Put in experimentation, the cumulative release of all products is below 50%.
Fig. 4 be the embodiment of the present invention 1,6,7 under 298K, microcapsules 25d in deionized water release profiles.From Fig. 4 In as can be seen that embodiment 7 microcapsule product release it is most fast, embodiment 1 is taken second place, and embodiment 6 discharge it is most slow.This and original Core in material is consistent with the ratio of wall material, i.e. core wall ratio is bigger, and the wall thickness of microcapsules is smaller, and release is faster;Anyway it is slower.Separately Outside, during 25d release experiment, the cumulative release of all products is below 50%.
Fig. 5 is that the embodiment of the present invention 1,2,3,4,5,6,7 stands the photograph after 6h (A), 12h (B), 24h (C) and 48h (D) Piece.From figure 5 it can be seen that the product of all preparations is being macroscopically stable in 48h, this is prepared by all products Being spray applied within 48h provides guarantee afterwards.
Embodiment
Explanation is further analyzed to technical solution of the present invention with reference to specific embodiment.
Embodiment 1:
The preparation method of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation is as follows in the present embodiment:
1st, accurate weighing polycaprolactone 0.125g and Acetochlor 0.125g are dissolved in 5g acetone respectively, obtain mass concentration and are 2.5% oil phase A and mass concentration is 2.5% oil phase B;50mL dissolvings 1wt% SDBS solution is prepared as aqueous phase C;
2nd, oil phase A and oil phase B are separately added into the outer tube and inner tube of coaxial syringe needle with syringe pump, and in syringe needle end shape Into drop;Oil phase A and oil phase B is added dropwise into aqueous phase C by coaxial needle tubing, drop rate is 6.5mL/min (5 drop about per second), During dropwise addition, 25 DEG C of aqueous phase C constant temperature is simultaneously stirred with 1000rpm speed.
3rd, after being added dropwise, persistently it is stirred 2~4h of liquid and is volatilized completely to acetone, obtain hydrophobic pesticidal microcapsule formulations With suspending agent mix preparation.The Acetochlor effective content being made in product is 0.248%, and microcapsules bag medicine rate is 20.3%, is carried Medicine rate 16.9%.
Embodiment 2:
The preparation method of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation is as follows in the present embodiment:
1st, accurate weighing polycaprolactone 0.125g and Acetochlor 0.125g are dissolved in 5g acetone respectively, obtain mass concentration and are 2.5% oil phase A and mass concentration is 2.5% oil phase B;50mL dissolvings 1wt% SDBS solution is prepared as aqueous phase C;
2nd, oil phase A and oil phase B are separately added into the outer tube and inner tube of coaxial syringe needle with syringe pump, and in syringe needle end shape Into drop;Oil phase A and oil phase B is added dropwise into aqueous phase C by coaxial needle tubing, drop rate is 6.5mL/min (5 drop about per second), During dropwise addition, 25 DEG C of aqueous phase C constant temperature is simultaneously stirred with 500rpm speed.
3rd, after being added dropwise, persistently it is stirred 2~4h of liquid and is volatilized completely to acetone, obtain hydrophobic pesticidal microcapsule formulations With suspending agent mix preparation.The Acetochlor effective content being made in product is 0.248%, and microcapsules bag medicine rate is 24.5%, is carried Medicine rate 19.8%.
Embodiment 3:
The preparation method of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation is as follows in the present embodiment:
1st, accurate weighing polycaprolactone 0.125g and Acetochlor 0.125g are dissolved in 5g acetone respectively, obtain mass concentration and are 2.5% oil phase A and mass concentration is 2.5% oil phase B;50mL dissolvings 1wt% SDBS solution is prepared as aqueous phase C;
2nd, oil phase A and oil phase B are separately added into the outer tube and inner tube of coaxial syringe needle with syringe pump, and in syringe needle end shape Into drop;Oil phase A and oil phase B is added dropwise into aqueous phase C by coaxial needle tubing, drop rate is 6.5mL/min (5 drop about per second), During dropwise addition, 40 DEG C of aqueous phase C constant temperature is simultaneously stirred with 500rpm speed.
3rd, after being added dropwise, persistently it is stirred 2~4h of liquid and is volatilized completely to acetone, obtain hydrophobic pesticidal microcapsule formulations With suspending agent mix preparation.The Acetochlor effective content being made in product is 0.248%, and microcapsules bag medicine rate is 26.3%, is carried Medicine rate 20.9%.
For embodiment 1,2,3 under 298K, microcapsules in product 25d in deionized water release profiles are as shown in Figure 2. " collapse and the release " phenomenon triggered due to microcapsules rupture is not found in the release of microcapsules.
Embodiment 4:
The preparation method of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation is as follows in the present embodiment:
1st, accurate weighing polycaprolactone 0.125g and Acetochlor 0.125g are dissolved in 5g acetone respectively, obtain mass concentration and are 2.5% oil phase A and mass concentration is 2.5% oil phase B;50mL dissolvings 0.5wt% SDBS solution is prepared as aqueous phase C;
2nd, oil phase A and oil phase B are separately added into the outer tube and inner tube of coaxial syringe needle with syringe pump, and in syringe needle end shape Into drop;Oil phase A and oil phase B is added dropwise into aqueous phase C by coaxial needle tubing, drop rate is 6.5mL/min (5 drop about per second), During dropwise addition, 25 DEG C of aqueous phase C constant temperature is simultaneously stirred with 1000rpm speed.
3rd, after being added dropwise, persistently it is stirred 2~4h of liquid and is volatilized completely to acetone, obtain hydrophobic pesticidal microcapsule formulations With suspending agent mix preparation.The Acetochlor effective content being made in product is 0.248%, and microcapsules bag medicine rate is 34.3%, is carried Medicine rate 25.7%.
Embodiment 5:
The preparation method of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation is as follows in the present embodiment:
1st, accurate weighing polycaprolactone 0.125g and Acetochlor 0.125g are dissolved in 5g acetone respectively, obtain mass concentration and are 2.5% oil phase A and mass concentration is 2.5% oil phase B;Prepare 50mL dissolvings 1wt% polyvinyl alcohol (PVA) solution conduct Aqueous phase C;
2nd, oil phase A and oil phase B are separately added into the outer tube and inner tube of coaxial syringe needle with syringe pump, and in syringe needle end shape Into drop;Oil phase A and oil phase B is added dropwise into aqueous phase C by coaxial needle tubing, drop rate is 6.5mL/min (5 drop about per second), During dropwise addition, 25 DEG C of aqueous phase C constant temperature is simultaneously stirred with 1000rpm speed.
3rd, after being added dropwise, persistently it is stirred 2~4h of liquid and is volatilized completely to acetone, obtain hydrophobic pesticidal microcapsule formulations With suspending agent mix preparation.The Acetochlor effective content being made in product is 0.248%, and microcapsules bag medicine rate is 31.3%, is carried Medicine rate 24.0%.
Embodiment 1,4,5 is under 298K, microcapsules 25d in deionized water release profiles such as Fig. 3 in product.Microcapsules Release in do not find due to microcapsules rupture trigger " collapse and release " phenomenon.
Embodiment 6:
The preparation method of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation is as follows in the present embodiment:
1st, accurate weighing polycaprolactone 0.05g and Acetochlor 0.20g are dissolved in 5g acetone respectively, obtain mass concentration and are 1% oil phase A and mass concentration is 4% oil phase B;50mL dissolvings 1wt% SDBS solution is prepared as aqueous phase C;
2nd, oil phase A and oil phase B are separately added into the outer tube and inner tube of coaxial syringe needle with syringe pump, and in syringe needle end shape Into drop;Oil phase A and oil phase B is added dropwise into aqueous phase C by coaxial needle tubing, drop rate is 6.5mL/min (5 drop about per second), During dropwise addition, 25 DEG C of aqueous phase C constant temperature is simultaneously stirred with 1000rpm speed.
3rd, after being added dropwise, persistently it is stirred 2~4h of liquid and is volatilized completely to acetone, obtain hydrophobic pesticidal microcapsule formulations With suspending agent mix preparation.The Acetochlor effective content being made in product is 0.397%, and microcapsules bag medicine rate is 17.7%, is carried Medicine rate 18.0%.
Embodiment 7:
The preparation method of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation is as follows in the present embodiment:
1st, accurate weighing polycaprolactone 0.20g and Acetochlor 0.05g are dissolved in 5g acetone respectively, obtain mass concentration and are 4% oil phase A and mass concentration is 1% oil phase B;50mL dissolvings 1wt% SDBS solution is prepared as aqueous phase C;
2nd, oil phase A and oil phase B are separately added into the outer tube and inner tube of coaxial syringe needle with syringe pump, and in syringe needle end shape Into drop;Oil phase A and oil phase B is added dropwise into aqueous phase C by coaxial needle tubing, drop rate is 6.5mL/min (5 drop about per second), During dropwise addition, 25 DEG C of aqueous phase C constant temperature is simultaneously stirred with 1000rpm speed.
3rd, after being added dropwise, persistently it is stirred 2~4h of liquid and is volatilized completely to acetone, obtain hydrophobic pesticidal microcapsule formulations With suspending agent mix preparation.The Acetochlor effective content being made in product is 0.099%, and microcapsules bag medicine rate is 22.2%, is carried Medicine rate 8.5%.
Embodiment 1,6,7 is under 298K, microcapsules 25d in deionized water release profiles such as Fig. 4 in product.Microcapsules Release in do not find due to microcapsules rupture trigger " collapse and release " phenomenon.
Embodiment 1,2,3,4,5,6,7 stands photo such as Fig. 5 after 6h (A), 12h (B), 24h (C) and 48h (D).It can be seen that After preparation 6,12,24 and 48h mix preparations product can keep stable, microcapsule granule favorable dispersibility, not existing micro- glue Capsule particle coagulation and sedimentation phenomenon.Therefore after brand-new within 48h, Acetochlor mix preparation product can be used conveniently in sprinkling.

Claims (10)

1. a kind of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation, it is characterised in that:
The mix preparation is the mixture of hydrophobic pesticidal microcapsule formulations and hydrophobic pesticidal suspending agent;
The hydrophobic pesticidal microcapsule formulations are made up of microcapsule wall material and core, and the microcapsule wall material is polycaprolactone, institute It is hydrophobic pesticidal Acetochlor to state core;
The hydrophobic pesticidal suspending agent is Acetochlor suspending agent.
2. mix preparation according to claim 1, it is characterised in that:
The total content of effective agricultural chemicals Acetochlor is 0.1-0.4wt% in mix preparation;
The mass concentration of hydrophobic pesticidal microcapsules is 0.25-0.45wt% in mix preparation, is had in hydrophobic pesticidal microcapsules The content for imitating agricultural chemicals Acetochlor is 5~25wt%.
3. mix preparation according to claim 1, it is characterised in that:
The mass concentration of Acetochlor is 0.08-0.20wt% in the hydrophobic pesticidal suspending agent.
4. mix preparation according to claim 1, it is characterised in that:
Also contain surfactant in the hydrophobic pesticidal suspending agent, the mass concentration of surfactant is 0.5-1wt%.
5. mix preparation according to claim 4, it is characterised in that:
The surfactant is neopelex or polyvinyl alcohol.
6. mix preparation according to claim 1, it is characterised in that:
The molecular weight of polycaprolactone is Mw=1.4 × 105g/mol。
7. the preparation method of the hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation described in a kind of claim 1, its feature It is to comprise the following steps:
Step 1:Microcapsule wall material is dissolved in acquisition oil phase A in acetone, hydrophobic pesticidal is dissolved in acquisition oil phase B in acetone, Surfactant is dissolved in deionized water and obtains aqueous phase C;
Step 2:Under conditions of constant temperature at the uniform velocity stirs, aqueous phase C constant temperature is at 25-40 DEG C, and mixing speed is in 500-1000rpm;With Oil phase A and oil phase B are separately added into the outer tube and inner tube of coaxial syringe needle by syringe pump, and form drop in syringe needle end, are passed through Oil phase A and oil phase B is added dropwise into aqueous phase C for coaxial needle tubing;
Step 3:After being added dropwise to complete, persistently it is stirred 2~4h of liquid and is volatilized completely to acetone, obtain hydrophobic pesticidal microcapsule formulations With suspending agent mix preparation.
8. preparation method according to claim 7, it is characterised in that:
In step 1, the mass fraction summation of hydrophobic pesticidal is 5% in microcapsule wall material and oil phase B in oil phase A, table in aqueous phase C The mass fraction of face activating agent is 0.5-1%.
9. preparation method according to claim 7, it is characterised in that:
In step 2, oil phase A and oil phase B gross mass are 1 with aqueous phase C mass ratio:5.
10. preparation method according to claim 7, it is characterised in that:
In step 2, rate of addition is per second 5 drops.
CN201710733326.9A 2017-08-24 2017-08-24 A kind of hydrophobic pesticidal microcapsule formulations and suspending agent mix preparation and preparation method thereof Pending CN107439546A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992013448A1 (en) * 1991-02-06 1992-08-20 Zeneca Inc. Microcapsules and microencapsulation process
CN106259315A (en) * 2016-08-08 2017-01-04 安徽国星生物化学有限公司 A kind of hydrophobic pesticidal preparation containing microcapsule and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1992013448A1 (en) * 1991-02-06 1992-08-20 Zeneca Inc. Microcapsules and microencapsulation process
CN106259315A (en) * 2016-08-08 2017-01-04 安徽国星生物化学有限公司 A kind of hydrophobic pesticidal preparation containing microcapsule and preparation method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
王乐强: "药物与农药的溶剂蒸发法和溶剂提取法剂型改进与表征", 《中国优秀硕士学位论文全文数据库 工程科技I辑》 *
王乐强等: "乙草胺乳油的溶剂提取法改进", 《农药》 *

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