CN104521955A - Pesticide microcapsule and preparation method thereof - Google Patents
Pesticide microcapsule and preparation method thereof Download PDFInfo
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- CN104521955A CN104521955A CN201410762586.5A CN201410762586A CN104521955A CN 104521955 A CN104521955 A CN 104521955A CN 201410762586 A CN201410762586 A CN 201410762586A CN 104521955 A CN104521955 A CN 104521955A
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Abstract
The invention relates to a pesticide microcapsule and a preparation method thereof. A pesticide/silicon dioxide microcapsule is prepared by an emulsion in-situ coating method, and then is subjected to surface functionalization, and then a pesticide/silicon dioxide/natural polymer double-walled pesticide microcapsule is prepared by crosslinking of a functional group and natural polymers. The pesticide microcapsule prepared by the invention has the advantages of high drug loading capacity and obvious sustained-release effect, the used wall material is harmless to the environment, and the release of the pesticide can be controlled by regulating and controlling the wall material.
Description
Technical field
The present invention relates to a kind of microcapsules and preparation method thereof, particularly a kind of agricultural chemicals double-coating microcapsules and preparation method thereof.
Background technology
The extermination of disease and insect pest is an important step in agricultural production, and applying pesticides is the main path of the agriculture field extermination of disease and insect pest, but traditional agricultural chemicals availability is low, and persticide residue is large, causes waste and environmental pollution.For effectively utilizing agricultural chemicals and reducing environmental pollution, sustained-release pesticides receives publicity, wherein microcapsule formulations, and cladded type slow release agent research is more.The natural polymer such as sodium alginate, shitosan is that carrier has the deficiencies such as intensity is low, drugloading rate is low, easy violent release.The acid monomer generated after the synthesis such as Lauxite, melamine resin macromolecule exists residual component difficult degradation, degraded or oligomer make soil pH value reduction cause the problems such as soil acidification.
In order to overcome the deficiency of above-mentioned microcapsule formulations, people propose to use sol-gel emulsion polymerization by drug encapsulation in silica shell.As Chinese patent ZL200610114438.8 discloses the microencapsulated water soluble drug of silica, Chinese patent application publication number CN103153050A discloses the metallized pesticide micro capsule of a kind of silica shell makes agricultural chemicals be able to controlled release, Chinese patent application publication number CN102515176A discloses a kind of Diplopore silica particles and uses thereof, United States Patent (USP) 8,889,044 discloses sol-gel process for being encapsulated in unmodified silica shell by agricultural chemicals.
Although these silica microcapsules provide slowly-releasing to a certain degree, because be all that individual layer is coated, slow release effect is limited, and the lasting period is short, and people wish that developed agricultural chemicals has certain lasting period, and clad again can not to environment.
Summary of the invention
The object of this invention is to provide a kind ofly have that drugloading rate is high, slow release effect is obvious, the lasting period is long, the pesticide micro capsule of wall material environmental sound and preparation method thereof.
Object of the present invention can be realized by following measure: the agricultural chemicals/silica microcapsules first by utilizing sol-gel process in-stiu coating to prepare with nucleocapsid structure, then coupling agent treatment is used, its surface band is made to have function base, recycling function base and natural polymer are cross-linked, prepare agricultural chemicals/silica/natural polymer double-coating pesticide micro capsule, hydrophobic pesticidal can be embedded in hollow interior, improve agricultural chemicals load capacity, and by regulating wall equipment structure and composition control farm chemical release, reach release/controlled release object.
Invention main points:
Pesticide slow-release microcapsules of the present invention, for having the core-shell particles of double shells, its kernel is pesticide activity component, and inner layer wall material is silica, and outer wall material is the natural polymer such as shitosan, feather keratin, and drugloading rate one quality counts 10 ~ 50%.
Preparation method of the present invention, specifically comprises the following steps:
A) be hydrolyzed in advance by siloxanes eka-silicon source material, obtain being hydrolyzed silicon source A, hydrolysising condition pH value is 8 ~ 12;
B) surfactant is soluble in water, form aqueous phase B, surfactant concentration is 1g/100mL ~ 5g/100 mL;
C) be dissolved in organic solvent by agricultural chemicals, form organic phase C, pesticide concentration is 50-1200mg/ mL;
D) under high velocity agitation, organic phase C is added aqueous phase B, the volume ratio of organic phase C and aqueous phase B is 1:50 ~ 1:10, continues stirring until Star City stable oil-in-water (O/W) type emulsion D;
E) in emulsion, add the silicon source A be hydrolyzed in advance, Keep agitation, aging, ageing time is 12 ~ 48 hours, silicon source material is fully hydrolyzed and polycondensation, forms coated with silica microcapsules E;
F) adding silane coupler to not being separated in microcapsules E system, stirring, reaction, temperature is 50 ~ 80 DEG C, and the reaction time is 1 ~ 6h.Centrifugal, dry, obtain function of surface microcapsules F;
G) natural polymer is water-soluble, form natural polymer solution, the concentration of natural polymer is 0.2 ~ 1.0w/v, function of surface microcapsules F is joined in Polymer Solution, the consumption of natural polymer is 3 ~ 20% of microcapsules F, adds thermal response, and reaction temperature is 30 ~ 80 DEG C, reaction time is that 6 ~ 24h. is centrifugal, and washing also drying obtains agricultural chemicals/silica/natural polymer core-shell particles microcapsules.
Described agricultural chemicals is more than one in diflubenzuron, Acetamiprid, chlopyrifos, Affirm (Merck Co.), Avermectin, Imidacloprid, ivermectin, High effect cypermethrin and pyrethroid.
Described natural polymer is the one of shitosan or feather keratin.
In step a, siloxanes eka-silicon source material is methyl silicate or ethyl orthosilicate.
In step a, siloxanes eka-silicon source Substance P hydrolysis catalyzer is ammoniacal liquor.
Surfactant in step b is softex kw or hexadecyltrimethylammonium chloride.
Organic solvent in step c is the one in ethyl acetate, butyl acetate, toluene, n-hexane, normal heptane, chloroform.
Silane coupler in step f is γ-glycidyl-oxypropyl trimethyl silane, isocyanatopropyl triethoxysilane.
Beneficial effect of the present invention:
Pesticide micro capsule of the present invention, adopt using to the nontoxic silica of soil and degradable and can as the natural polymer of Fertilizer application for double wall material, drugloading rate be high, has obvious pesticide slow-release/controlled-release effect, effectively can extend the lasting period of agricultural chemicals.Slow-release microcapsule of the present invention can provide desirable injurious insect control under lower frequency and/or rate of application.In addition, preparation method of the present invention is fairly simple, easy to implement.
Embodiment:
Embodiment 1
Be be hydrolyzed 1.5h in advance in the ammonia spirit of 9 at pH value by 4g silicon source material ethyl orthosilicate, obtain being hydrolyzed silicon source A; 2g softex kw is dissolved in 100mL deionized water, obtains aqueous phase B; 1g chlopyrifos is dissolved in 4mL ethyl acetate, obtains organic phase C; Under agitation, organic phase C is joined in aqueous phase B, continue stirring until and form stable O/w emulsion D; Drip in emulsion D and be hydrolyzed silicon source A, the aging 24h of stirring at room temperature in advance, obtain coated with silica pesticide micro capsule E; In system E, add 1mL γ-glycidyl-oxypropyl trimethyl silane, at 60 DEG C, react 4h, obtain epoxide modified coated with silica pesticide micro capsule F; 0.3% feather keratin solution 100mL is configured with ammonia spirit (PH10), add 3 g pesticide micro capsule F again, 6h is reacted at 60 DEG C, by solution centrifugal, respectively with deionized water, ethanol washing, drying obtains the coated pesticide micro capsule of double wall material, and load capacity is that 21.5%(load capacity refers to that pesticide quality accounts for the mass ratio of whole microcapsules).
Embodiment 2
Be be hydrolyzed 1.5h in advance in the ammonia spirit of 9 at pH value by 4g silicon source material ethyl orthosilicate, obtain being hydrolyzed silicon source A; 2g softex kw is dissolved in 100mL deionized water, obtains aqueous phase B; 2g chlopyrifos is dissolved in 4mL ethyl acetate, obtains organic phase C; Under agitation, organic phase C is joined in aqueous phase B, continue stirring until and form stable O/w emulsion D; Drip in emulsion D and be hydrolyzed silicon source A, the aging 24h of stirring at room temperature in advance, obtain coated with silica pesticide micro capsule E; In system E, add 1mL γ-glycidyl-oxypropyl trimethyl silane, at 60 DEG C, react 4h, obtain epoxide modified coated with silica pesticide micro capsule F; 0.3% feather keratin solution 100mL is configured with ammonia spirit (PH10), add 3 g pesticide micro capsule F, 6h is reacted at 60 DEG C, by solution centrifugal, respectively with deionized water, ethanol washing, drying obtains the coated chlorpyrifos microcapsule of double wall material, and load capacity is that 26.7%(load capacity refers to that pesticide quality accounts for the mass ratio of whole microcapsules).
Embodiment 3
Be be hydrolyzed 1.5h in advance in the ammonia spirit of 9 at pH value by 4g silicon source material ethyl orthosilicate, obtain being hydrolyzed silicon source A; 2g softex kw is dissolved in 100mL deionized water, obtains aqueous phase B; 1.5g chlopyrifos is dissolved in 4mL ethyl acetate, obtains organic phase C; Under agitation, organic phase C is joined in aqueous phase B, continue stirring until and form stable O/w emulsion D; Drip in emulsion D and be hydrolyzed silicon source A, the aging 24h of stirring at room temperature in advance, obtain coated with silica pesticide micro capsule E; In system E, add 1mL γ-glycidyl-oxypropyl trimethyl silane, at 60 DEG C, react 4h, obtain epoxide modified coated with silica pesticide micro capsule F; 0.3% feather keratin solution 100mL is configured with ammonia spirit (PH10), add 3 g pesticide micro capsule F again, 6h is reacted at 60 DEG C, by solution centrifugal, respectively with deionized water, ethanol washing, drying, obtains the coated chlorpyrifos microcapsule of double wall material, and load capacity is that 23.8%(load capacity refers to that pesticide quality accounts for the mass ratio of whole microcapsules).
Embodiment 4
Be be hydrolyzed 1.5h in advance in the ammonia spirit of 10 at pH value by 4g silicon source material ethyl orthosilicate, obtain being hydrolyzed silicon source A; 2g softex kw is dissolved in 100mL deionized water, obtains aqueous phase B; 1g Avermectin is dissolved in 4mL toluene, obtains organic phase C; Under agitation, organic phase C is joined in aqueous phase B, continue stirring until and form stable O/w emulsion D; Drip in emulsion D and be hydrolyzed silicon source A, the aging 24h of stirring at room temperature in advance, obtain coated with silica pesticide micro capsule E; In system E, add 1mL γ-glycidyl-oxypropyl trimethyl silane, at 60 DEG C, react 4h, obtain epoxide modified coated with silica pesticide micro capsule F; 0.3% feather keratin solution 100mL is configured with ammonia spirit (PH10), add 3 g pesticide micro capsule F, 6h is reacted at 60 DEG C, by solution centrifugal, respectively with deionized water, ethanol washing, drying obtains the coated avermectin microcapsule of double wall material, and load capacity is that 17.3%(load capacity refers to that pesticide quality accounts for the mass ratio of whole microcapsules).
Embodiment 5
Be be hydrolyzed 1.5h in advance in the ammonia spirit of 10 at pH value by 4g silicon source material ethyl orthosilicate, obtain being hydrolyzed silicon source A; 2g softex kw is dissolved in 100mL deionized water, obtains aqueous phase B; 2g Avermectin is dissolved in 4mL toluene, obtains organic phase C; Under agitation, organic phase C is joined in aqueous phase B, continue stirring until and form stable O/w emulsion D; Drip in emulsion D and be hydrolyzed silicon source A, the aging 24h of stirring at room temperature in advance, obtain coated with silica pesticide micro capsule E; In system E, add 1mL γ-glycidyl-oxypropyl trimethyl silane, 60 DEG C, reaction 4h, obtains epoxide modified coated with silica pesticide micro capsule F; 0.2% chitosan solution 100mL is configured with acetum (PH5), add 3 g pesticide micro capsule F again, 6h is reacted at 60 DEG C, by solution centrifugal, respectively with deionized water, ethanol washing, drying, obtains the coated avermectin microcapsule of double wall material, and load capacity is that 19.8%(load capacity refers to that pesticide quality accounts for the mass ratio of whole microcapsules).
Embodiment 6
Be be hydrolyzed 1.5h in advance in the ammonia spirit of 9 at pH value by 4g silicon source material ethyl orthosilicate, obtain being hydrolyzed silicon source A; 2g softex kw is dissolved in 100mL deionized water, obtains aqueous phase B; 1g Imidacloprid is dissolved in 4mL chloroform, obtains organic phase C; Under agitation, organic phase C is joined in aqueous phase B, continue stirring until and form stable O/w emulsion D; Drip in emulsion D and be hydrolyzed silicon source A, the aging 24h of stirring at room temperature in advance, obtain coated with silica pesticide micro capsule E; In system E, add 1mL γ-glycidyl-oxypropyl trimethyl silane, at 60 DEG C, react 4h, obtain epoxide modified coated with silica pesticide micro capsule F; 0.3% feather keratin solution 100mL is configured with ammonia spirit (PH10), add 2.5g pesticide micro capsule F, 6h is reacted at 60 DEG C, by solution centrifugal, respectively with deionized water, ethanol washing, drying obtains the coated Imidacloprid microcapsules of double wall material, and load capacity is that 16.8%(load capacity refers to that pesticide quality accounts for the mass ratio of whole microcapsules).
Embodiment 7
Be be hydrolyzed 1.5h in advance in the ammonia spirit of 9 at pH value by 4g silicon source material ethyl orthosilicate, obtain being hydrolyzed silicon source A; 2g softex kw is dissolved in 100mL deionized water, obtains aqueous phase B; 2g Imidacloprid is dissolved in 4mL chloroform, obtains organic phase C; Under agitation, organic phase C is joined in aqueous phase B, continue stirring until and form stable O/w emulsion D; Drip in emulsion D and be hydrolyzed silicon source A, the aging 24h of stirring at room temperature in advance, obtain coated with silica pesticide micro capsule E; In system E, add 1mL γ-glycidyl-oxypropyl trimethyl silane, at 60 DEG C, react 4h, obtain epoxide modified coated with silica pesticide micro capsule F; 0.2% chitosan solution 100mL is configured with acetum (PH5), add 3g pesticide micro capsule F again, 6h is reacted at 60 DEG C, by solution centrifugal, respectively with deionized water, ethanol washing, drying obtains the coated Imidacloprid microcapsules of double wall material, and load capacity is that 20.3%(load capacity refers to that pesticide quality accounts for the mass ratio of whole microcapsules).
Embodiment 8
Be be hydrolyzed 1.5h in advance in the ammonia spirit of 9 at pH value by 4g silicon source material ethyl orthosilicate, obtain being hydrolyzed silicon source A; 2g hexadecyltrimethylammonium chloride is dissolved in 100mL deionized water, obtains aqueous phase B; 1g Acetamiprid is dissolved in 4mL chloroform, obtains organic phase C; Under agitation, organic phase C is joined in aqueous phase B, continue stirring until and form stable O/w emulsion D; Drip in emulsion D and be hydrolyzed silicon source A, the aging 24h of stirring at room temperature in advance, obtain coated with silica pesticide micro capsule E; In system E, add 1mL γ-glycidyl-oxypropyl trimethyl silane, at 40 DEG C, react 12h, obtain epoxide modified coated with silica pesticide micro capsule F; 0.2% chitosan solution 100mL is configured with acetum (PH5), add 3g pesticide micro capsule F again, 8h is reacted at 50 DEG C, by solution centrifugal, respectively with deionized water, ethanol washing, drying obtains the coated acetamiprid microcapsule of double wall material, and load capacity is that 16.3%(load capacity refers to that pesticide quality accounts for the mass ratio of whole microcapsules).
Embodiment 9
Be be hydrolyzed 1.5h in advance in the ammonia spirit of 9 at pH value by 4g silicon source material ethyl orthosilicate, obtain being hydrolyzed silicon source A; 2g hexadecyltrimethylammonium chloride is dissolved in 100mL deionized water, obtains aqueous phase B; 2g Acetamiprid is dissolved in 5mL chloroform, obtains organic phase C; Under agitation, organic phase C is joined in aqueous phase B, continue stirring until and form stable O/w emulsion D; Drip in emulsion D and be hydrolyzed silicon source A, the aging 24h of stirring at room temperature in advance, obtain coated with silica pesticide micro capsule E; In system E, add 1mL γ-glycidyl-oxypropyl trimethyl silane, at 40 DEG C, react 12h, obtain epoxide modified coated with silica pesticide micro capsule F; 0.3% feather keratin solution 100mL is configured with ammonia spirit (PH8), add 3g pesticide micro capsule F again, 8h is reacted at 50 DEG C, by solution centrifugal, respectively with deionized water, ethanol washing, drying obtains the coated acetamiprid microcapsule of double wall material, and load capacity is that 21.4%(load capacity refers to that pesticide quality accounts for the mass ratio of whole microcapsules).
Claims (9)
1. microcapsules, it comprises core, and this core comprises the active component being encapsulated in capsule material, it is characterized in that, described capsule material is silica and the natural polymer double wall material of loose structure, and drugloading rate is 10-50% in mass; Specifically comprise the following steps:
A) siloxanes eka-silicon source material is hydrolyzed in advance, obtains being hydrolyzed silicon source A;
B) surfactant is soluble in water, form aqueous phase B;
C) agricultural chemicals is dissolved in organic solvent, forms organic phase C;
D) under high velocity agitation, organic phase C is added aqueous phase B, the volume ratio of organic phase C and aqueous phase B is 1:50 ~ 1:10, continues stirring until and forms stable oil-in-water (O/W) type emulsion D;
E) in emulsion, the silicon source A be hydrolyzed is in advance added, Keep agitation, aging, silicon source material is fully hydrolyzed and polycondensation, forms coated with silica microcapsules E;
F) adding silane coupler to not being separated in microcapsules E system, stirring, reaction, centrifugal, drying obtains function of surface microcapsules F;
G) natural polymer is water-soluble, form natural polymer solution, join in Polymer Solution, add thermal response by function of surface microcapsules F, centrifugal, washing also drying obtains natural polymer/silica/agricultural chemicals core-shell particles microcapsules.
2. microcapsules as claimed in claim 1, it is characterized in that, described active component is agricultural chemicals.
3. microcapsules as claimed in claim 1, it is characterized in that, described natural polymer wall material is the one of shitosan or feather keratin.
4. as claimed in claim 2 microcapsules, is characterized in that, described agricultural chemicals is more than one in diflubenzuron, Acetamiprid, chlopyrifos, Affirm (Merck Co.), Avermectin, Imidacloprid, ivermectin, High effect cypermethrin and pyrethroid.
5. microcapsules as claimed in claim 1, it is characterized in that, its preparation method comprises the following steps:
A) siloxanes eka-silicon source material is hydrolyzed in advance, obtains being hydrolyzed silicon source A;
B) surfactant is soluble in water, form aqueous phase B;
C) agricultural chemicals is dissolved in organic solvent, forms organic phase C;
D) under high velocity agitation, organic phase C is added aqueous phase B, the volume ratio of organic phase C and aqueous phase B is 1:50 ~ 1:10, continues stirring until Star City stable oil-in-water (O/W) type emulsion D;
E) in emulsion, the silicon source A be hydrolyzed is in advance added, Keep agitation, aging, silicon source material is fully hydrolyzed and polycondensation, forms coated with silica microcapsules E;
F) adding silane coupler to not being separated in microcapsules E system, stirring, reaction, centrifugal, drying obtains function of surface microcapsules F;
G) natural polymer is water-soluble, form natural polymer solution, join in Polymer Solution by function of surface microcapsules F, heating, reaction, centrifugal, washing also drying obtains natural polymer/silica/agricultural chemicals core-shell particles microcapsules;
In step a, siloxanes eka-silicon source material is methyl silicate or ethyl orthosilicate;
In step a, siloxanes eka-silicon source Substance P hydrolysis catalyzer is ammoniacal liquor;
Surfactant in step b is softex kw or hexadecyltrimethylammonium chloride;
Organic solvent in step c is the one in ethyl acetate, butyl acetate, toluene, n-hexane, normal heptane, chloroform;
Silane coupler in step f is γ-glycidyl-oxypropyl trimethyl silane, isocyanatopropyl triethoxysilane;
Microcapsules as claimed in claim 5, is characterized in that, the pH value of solution A hydrolysis is 8 ~ 12;
Microcapsules as claimed in claim 5, is characterized in that, the concentration of solution B surfactant is 0.5g/100mL ~ 5g/100 mL;
Microcapsules as claimed in claim 5, is characterized in that, solution C Pesticides concentration is 50-1200mg/mL.
Microcapsules as claimed in claim 5, is characterized in that, in step e, ageing time is 16 ~ 48h, and temperature is room temperature.
6. microcapsules as claimed in claim 5, it is characterized in that, in step f, silane coupler consumption is 5 ~ 20% of siloxanes eka-silicon source material.
7. microcapsules as claimed in claim 5, it is characterized in that, in step f, reaction temperature is 50 ~ 80 DEG C, and the reaction time is 1 ~ 6h.
8. microcapsules as claimed in claim 5, it is characterized in that, in step g, the concentration of natural polymer is 0.2 ~ 1.0w/v, and the consumption of natural polymer is 3 ~ 20% of microcapsules F.
9. microcapsules as claimed in claim 5, it is characterized in that, in step g, reaction temperature is 30 ~ 80 DEG C, and the reaction time is 6 ~ 24h.
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| CN105831113A (en) * | 2016-03-30 | 2016-08-10 | 华中农业大学 | Nanosilica-grafted organic functional polymer organic phosphorous insecticide sustained-release agent and preparation method thereof |
| CN105850993A (en) * | 2016-03-30 | 2016-08-17 | 华中农业大学 | Nano-sized silicon dioxide grafted organic functional polymer bisamide pesticide slow-release agent and preparation method thereof |
| CN105850992A (en) * | 2016-03-30 | 2016-08-17 | 华中农业大学 | Nano silicon dioxide grafted organic functional polymer macrolide insecticide slow-release agent and preparation method thereof |
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