CN105076129A - Insecticide microcapsules and preparation method thereof - Google Patents
Insecticide microcapsules and preparation method thereof Download PDFInfo
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- CN105076129A CN105076129A CN201410164225.0A CN201410164225A CN105076129A CN 105076129 A CN105076129 A CN 105076129A CN 201410164225 A CN201410164225 A CN 201410164225A CN 105076129 A CN105076129 A CN 105076129A
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- microcapsules
- expelling parasite
- phase transition
- liquid phase
- solid
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- 229910019142 PO4 Inorganic materials 0.000 description 1
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- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- DAKWPKUUDNSNPN-UHFFFAOYSA-N Trimethylolpropane triacrylate Chemical compound C=CC(=O)OCC(CC)(COC(=O)C=C)COC(=O)C=C DAKWPKUUDNSNPN-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
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- 125000000217 alkyl group Chemical group 0.000 description 1
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 1
- 229920003180 amino resin Polymers 0.000 description 1
- 150000008064 anhydrides Chemical group 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
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- 239000002585 base Substances 0.000 description 1
- 229940106691 bisphenol a Drugs 0.000 description 1
- NKKMVIVFRUYPLQ-UHFFFAOYSA-N but-2-enenitrile Chemical compound CC=CC#N NKKMVIVFRUYPLQ-UHFFFAOYSA-N 0.000 description 1
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- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 150000001244 carboxylic acid anhydrides Chemical group 0.000 description 1
- 125000003262 carboxylic acid ester group Chemical group [H]C([H])([*:2])OC(=O)C([H])([H])[*:1] 0.000 description 1
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- 238000001035 drying Methods 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000003822 epoxy resin Substances 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- FJOPOOBDMDAVIW-UHFFFAOYSA-N ethenyl acetate;hydrate Chemical compound O.CC(=O)OC=C FJOPOOBDMDAVIW-UHFFFAOYSA-N 0.000 description 1
- CYKDLUMZOVATFT-UHFFFAOYSA-N ethenyl acetate;prop-2-enoic acid Chemical compound OC(=O)C=C.CC(=O)OC=C CYKDLUMZOVATFT-UHFFFAOYSA-N 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 229940044949 eucalyptus oil Drugs 0.000 description 1
- 239000010642 eucalyptus oil Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 125000003976 glyceryl group Chemical group [H]C([*])([H])C(O[H])([H])C(O[H])([H])[H] 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 229940051250 hexylene glycol Drugs 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
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- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000001102 lavandula vera Substances 0.000 description 1
- 235000018219 lavender Nutrition 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- WBYWAXJHAXSJNI-UHFFFAOYSA-N methyl p-hydroxycinnamate Natural products OC(=O)C=CC1=CC=CC=C1 WBYWAXJHAXSJNI-UHFFFAOYSA-N 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- JRKICGRDRMAZLK-UHFFFAOYSA-L peroxydisulfate Chemical compound [O-]S(=O)(=O)OOS([O-])(=O)=O JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
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- 229920000515 polycarbonate Polymers 0.000 description 1
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- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical group CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 1
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- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 description 1
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Landscapes
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The present invention relates to insecticide microcapsules and a preparation method thereof, wherein the microcapsules comprise a capsule wall and a capsule core, and the capsule core comprises at least a solid-liquid phase transition material with a phase transition temperature of 10-50 DEG C and at least an insect repellent agent.
Description
Technical field
The present invention relates to a kind of expelling parasite microcapsules and preparation method thereof.Particularly, the present invention relates to a kind of expelling parasite microcapsules with peculiar release characteristics and long life and preparation method thereof.The invention still further relates to the expelling parasite application of expelling parasite additive and coating composition and this expelling parasite microcapsules comprising these expelling parasite microcapsules.
Background technology
The insect such as control insect, particularly mosquito, cockroach, ant, mite, is absolutely necessary for modern agriculture, food storing, health hygienic and field of textiles.At present, the pest repellant of safe and efficient microencapsulation form plays an important role in control insect.Usually, require that expelling parasite microcapsules have following character: can prevent and treat targeted insect, easily operate, stablize and there is certain holding time in the environment.But, usually there is pest repellant in practical application and run off from expelling parasite microcapsules in time thus the problem lost efficacy.In order to address this problem, usually need the place repetitive administration pest repellant to needing expelling parasite, this must cause the increase of the costs such as manpower and materials.
Known, phase change materials is a kind of material that phase in version can occur between solid, liquid, gas, and it has huge latent heat of phase change, can absorb, stores or discharge a large amount of heats under phase transition temperature.At present, great majority research is all that the latent heat of phase change had based on phase change materials self launches.Main application comprises the aspects such as intelligent automatic air-conditioning and construction thing, packaging material, pipe container, electrical and electronic component, warmth-retaining clothing, energy storage cooker.Up to now, also not about the research of phase change materials on the impact of the performance (such as physical property or hot property) of the material coexisted with it.
Current, still need a kind of expelling parasite microcapsules of improvement.
Summary of the invention
In the present invention, inventor have devised a kind of discharge controlled and can the holding time is longer in the environment expelling parasite microcapsules.
One aspect of the present invention provides a kind of expelling parasite microcapsules, and described microcapsules comprise cyst wall and capsule-core, and wherein said capsule-core comprises the solid-liquid phase transition material of at least one phase transition temperature within the scope of 10 to 50 DEG C and at least one insect repellent.In certain embodiments of the present invention, described solid-liquid phase transition material has the phase transition temperature within the scope of 10 to 30 DEG C.In other embodiments of the present invention, described solid-liquid phase transition material has the phase transition temperature within the scope of 30 to 50 DEG C.
Another aspect provides a kind of method for the preparation of expelling parasite microcapsules of the present invention, described method comprises: form cyst wall, and the solid-liquid phase transition material of described cyst wall encapsulating at least one phase transition temperature within the scope of 10 to 50 DEG C and at least one insect repellent are as capsule-core.In embodiments of the present invention, described cyst wall is formed by the emulsion polymerisation of the cohesion of macromolecular compound, the interfacial polycondensation of reactant mixture or ethylenically unsaturated monomer.
Of the present inventionly also will be supplied to a kind of expelling parasite additive on the other hand, it is dry powdered form or is form of suspension, and wherein, described expelling parasite additive package is containing expelling parasite microcapsules of the present invention.
Of the present inventionly also will be supplied to a kind of coating composition on the other hand, it comprises: the film-forming resin of film-forming amount; Supporting agent; Conventional additives; With expelling parasite microcapsules of the present invention or expelling parasite additive.
Of the present inventionly also will provide a kind of method for walking quickly and keeping away insect on the other hand, described method comprises: provide expelling parasite microcapsules of the present invention or expelling parasite additive; And by described expelling parasite microcapsules or expelling parasite additive application in the place needing expelling parasite.
In the present invention, inventor creatively proposes, and also comprises the solid-liquid phase transition material of phase transition temperature within the scope of 10-50 DEG C in the capsule-core of expelling parasite microcapsules except pest repellant.This solid-liquid phase transition material and pest repellant as a mixture together be present in the capsule-core of expelling parasite microcapsules.Usually, be included in pest repellant in capsule-core and realize release by evaporating into gas molecule through the hole of cyst wall, or because the concentration difference existed between inside and outside microcapsules is by being diffused into outside to realize release.As everyone knows, material movement in a liquid or diffusion will be significantly higher than material movement in solids or diffusion.In expelling parasite microcapsules of the present invention, when the temperature of external environment is increased to the phase transition temperature greater than or equal to the solid-liquid phase transition material in capsule-core, can there is the transformation from solid phase to liquid phase in this phase change materials.The migration of pest repellant in the phase change materials under liquid phase state or diffusivity are comparatively strong, are thus easily discharged in external environment.And when the temperature of external environment is reduced to the phase transition temperature less than or equal to solid-liquid phase transition material, can there is the transformation from liquid phase to solid phase in this phase change materials.The migration of pest repellant in the phase change materials under solid state shape or diffusivity significantly reduce, and do not discharge or are seldom discharged in external environment.As a result, the release of the pest repellant in microcapsules can realize temperature and control by selecting the phase transition temperature of solid-liquid phase transition material.
Further, the phase transition temperature of this solid-liquid phase transition material is selected in the scope of 10-50 DEG C, thus the pest repellant be therewith present in capsule-core easily discharges in this temperature range, and usually do not discharge or seldom discharge at lower than the temperature of this temperature range.For pest repellant release, such temperature range is desirable, because the harmful insect of occurring in nature (particularly mosquito, cockroach, ant, mite) is mostly also in the survival of this temperature range or activity.As a result, the release of the pest repellant in expelling parasite microcapsules of the present invention is consistent with the mechanics of insect, thus improves expelling parasite actual effect, avoids unnecessary waste, and extends the service life of expelling parasite microcapsules.
In addition, expelling parasite microcapsules of the present invention can also be made in multiple easy, cheap mode, thus can meet the requirement in different application field.
The details of one or more embodiment of the present invention is illustrated in the following description.According to specification and claim, other features, objects and advantages of the present invention will become clear.
Embodiment
When using in this article, except as otherwise noted, " one ", " this ", " at least one " and " one or more " are used interchangeably.Therefore, the expelling parasite microcapsules such as comprising " one " pest repellant can be interpreted as representing in these expelling parasite microcapsules and comprise " one or more " pest repellant.
When composition is described to comprise or comprise specific components, the selectable components that the present invention does not relate to is not got rid of in expectation said composition, and estimate that said composition can be made up of involved component or form, or when method is described to comprise or comprise specific process step, do not get rid of the selective process step that the present invention does not relate in expectation the method, and estimate that the method can be made up of involved processing step or form.
In order to easy, only specifically disclose some number ranges herein.But any lower limit can be combined to form with any upper limit the scope clearly do not recorded; And lower limit can form with other lower values the scope clearly do not recorded arbitrarily, the same upper limit arbitrarily can be combined to form with other upper limit any the scope clearly do not recorded.In addition, although clearly do not record, each point between endpoints of ranges or single numerical value are included within the scope of this.Thus, each point or single numerical value as the lower limit of self or the upper limit and other point any or single combinations of values or can be combined to form with other lower limit or the upper limit scope clearly do not recorded.
When using for solid-liquid phase transition material, term " phase transition temperature " refers to, the temperature (being also referred to as Tp) when this solid-liquid phase transition material changes into liquid phase (i.e. liquid) from solid phase (i.e. solid) or when changing into solid phase (solid) from liquid phase (liquid).
In the present invention, " containing the oligomer of active hydrogen or polymer and polyisocyanates molar equivalent than " refer to, the mole of active hydrogen and the ratio of the mole of NCO in described polyisocyanates in the described oligomer containing active hydrogen or polymer.
In the present invention, " mass ratio of capsule-core and cyst wall " refers to the gross mass of solid-liquid phase transition material and the pest repellant encapsulated by cyst wall itself and the ratio of raw-material gross mass forming described cyst wall.
Term " preferably " and " preferably " refer to the embodiment of the present invention that can provide some benefit in some cases.But in identical or other situations, other embodiments also may be preferred.In addition, describing of one or more preferred embodiment does not mean that other embodiments are disabled, and is not intended to other embodiments to get rid of outside the scope of the invention.
expelling parasite microcapsules
According to an aspect of the present invention, provide a kind of expelling parasite microcapsules, described microcapsules comprise cyst wall and capsule-core, and wherein said capsule-core comprises the solid-liquid phase transition material of at least one phase transition temperature within the scope of 10 to 50 DEG C and at least one insect repellent.
In expelling parasite microcapsules of the present invention, capsule-core comprises the solid-liquid phase transition material of phase transition temperature in the scope of 10 to 50 DEG C.
This solid-liquid phase transition material and pest repellant as a mixture together be present in the capsule-core of expelling parasite microcapsules.When the temperature of external environment is increased to the phase transition temperature greater than or equal to the solid-liquid phase transition material in capsule-core, can there is the transformation from solid phase to liquid phase in this phase change materials.The migration of pest repellant in the phase change materials under liquid phase state or diffusivity are comparatively strong, are easily discharged in external environment.And when the temperature of external environment is reduced to the phase transition temperature less than or equal to solid-liquid phase transition material, can there is the transformation from liquid phase to solid phase in this phase change materials.The migration of pest repellant in the phase change materials under solid state shape or diffusivity significantly reduce, and do not discharge or are seldom discharged in external environment.As a result, the release of the pest repellant in microcapsules can realize temperature and control by selecting the phase transition temperature of solid-liquid phase transition material.
Further, the phase transition temperature of this solid-liquid phase transition material is selected in the scope of 10-50 DEG C, thus the pest repellant be therewith present in capsule-core easily discharges in this temperature range, but do not discharge or seldom discharge at lower than the temperature of this temperature range.For pest repellant release, such temperature range is desirable, because the harmful insect of occurring in nature (particularly mosquito, cockroach, ant, mite) also survival or activity in this temperature range mostly.Result, by mixing the solid liquid phase transition material of phase transition temperature within the scope of 10-50 DEG C in the capsule-core of expelling parasite microcapsules, make the release of pest repellant consistent with insect activity rule, thus improve the expelling parasite actual effect of expelling parasite microcapsules, avoid unnecessary release, and extend the service life of expelling parasite microcapsules.
According to the application places of expelling parasite microcapsules, the solid-liquid phase transition material with different phase transition temperature range can be selected.Such as, in the region that ambient temperature is lower, such as frigid zone, selects the solid liquid phase transition material of phase transition temperature within the scope of 10 to 30 DEG C.In the region that ambient temperature is higher, such as the torrid zone or outdoor daylight direct projection region, select the solid liquid phase transition material of phase transition temperature within the scope of 30 to 50 DEG C.
According to the present invention, solid-liquid phase transition material can become liquid phase from solid transformation or become any material of solid phase from liquid-phase conversion under its phase transition temperature.In embodiments of the present invention, described solid-liquid phase transition material includes, but are not limited to inorganic crystal hydrate, the paraffin of C15-C24, fatty acid and fatty alcohol.As the exemplary embodiment of inorganic crystal hydrate, K can be used
2hPO
46H
2o (Tp=14 DEG C), Mn (NO
3)
26H
2o (Tp=25.5 DEG C), CaCl
212H
2o (Tp=29.8 DEG C), LiNO
32H
2o (Tp=30 DEG C), Na
2cO
310H
2o (Tp=32 DEG C), Na
2hPO
412H
2o (Tp=40 DEG C), KF2H
2o (Tp=42 DEG C), Na
2siO
34H
2o (Tp=48 DEG C) or MgSO
47H
2o (Tp=48.5 DEG C).As C
15-C
24the exemplary embodiment of paraffin, can C be used
15paraffin (Tp=10 DEG C), C
16paraffin (Tp=16.7 DEG C), C
17paraffin (Tp=21.7 DEG C), C
18paraffin (Tp=28 DEG C), C
19paraffin (Tp=32 DEG C), C
20paraffin (Tp=36.7 DEG C), C
21paraffin (Tp=40.2 DEG C), C
22paraffin (Tp=44 DEG C), C
23paraffin (Tp=47.5 DEG C) or C
24paraffin (Tp=50.6 DEG C).As the exemplary embodiment of fatty acid, acetic acid (Tp=16.7 DEG C), n-nonanoic acid (Tp=36 DEG C) or lauric acid (Tp=49 DEG C) can be used.As the exemplary embodiment of fatty alcohol, neopentyl glycol (Tp=44.1 DEG C) or lauryl alcohol (Tp=24 DEG C) can be used.
In a preferred embodiment of the invention, C is used
15-C
24paraffin is as solid-liquid phase transition material.According to the difference of its carbon number, C
15-C
24paraffin has different phase transition temperatures.By being combined by the paraffin of different chain length, the phase transition temperature wanted can be obtained.In addition, C15-24 paraffin also has low, the non-hygroscopic gas of toxicity, feature that burn into cost is not low.Therefore C15-24 paraffin is applicable to desirable solid-liquid phase transition material of the present invention.
In another preferred embodiment of the present invention, use lauryl alcohol as solid-liquid phase transition material.Consider the application places of expelling parasite microcapsules of the present invention, this lauryl alcohol with flowery odour is applicable to desirable solid-liquid phase transition material of the present invention.
In expelling parasite microcapsules of the present invention, insect repellent is present in capsule-core as anthelmintic activity composition.Term " insect repellent " refers to, can drive insect, suppress the reagent of insect activity or kill insects.In the present invention, this term can be used alternatingly with " pest repellant ".
According to the present invention, pest repellant comprises mosquito-repellent, cockroach repellant, ant repellant or lice class repellant.For the different objects that insect repellent is suitable for, those skilled in the art can select suitable pest repellant kind.
These insect repellents comprise vegetalitas repellant, organic synthesis repellant or its combination.Vegetalitas repellant can be obtained from insect-repellent plant by extraction known in the art or extraction process, and described insect-repellent plant includes, but not limited to cordate telosma, lavender, common nepenthes, geranium, daphne odera, Aztec marigold etc.Organic synthesis pest repellant comprises the repellant of the full stress-strain synthesis obtained by conventional organic synthesis technique, or by carrying out the repellant of half organic synthesis that modification or modification obtain to above-mentioned vegetalitas repellant.Such as, as the example of mosquito-repellent, Metadelphene, dimethyl phthalate, pyrethroid, natural chrysanthemum ester, lemon eucalyptus oil or its combination can be used.As the example of pyrethroid, phenothrin can be used.
In the capsule-core of expelling parasite microcapsules of the present invention, the mass ratio of described solid-liquid phase transition material and described insect repellent is between 1:5 to 5:1.In general, if the mass ratio of solid-liquid phase transition material and described insect repellent is too small, so solid-liquid phase transition material cannot play the effect of the release controlling insect repellent.If the mass ratio of solid-liquid phase transition material and described insect repellent is excessive, the waste of solid-liquid phase transition material can be caused, its maximizing the benefits cannot be realized.In a preferred embodiment of the invention, the mass ratio of solid-liquid phase transition material and insect repellent is in the scope of 1:3 to 3:1, and more preferably in the scope of 1:2 to 2:1, result can realize the maximizing the benefits of solid liquid phase transition material.
In expelling parasite microcapsules according to the present invention, described cyst wall is made up of any polymeric material with suitable mechanical strength.Preferably, cyst wall is made up of following material: xanthans, gelatin, gum Arabic, microcrystalline cellulose, polysiloxanes, polyurethane, polyureas, phenolic resins, melamine resin, polysulfones, poly-(methyl) acrylate, polystyrene, polyvinyl acetate or its combination.The composition of cyst wall can be selected in this area according to practical application area.
In certain embodiments of the present invention, cyst wall forms by comprising xanthans, gelatin, gum Arabic, microcrystalline cellulose or its natural polysaccharide combined.In other embodiments of the present invention, cyst wall is made up of polysiloxanes, polyurethane, polyureas, phenolic resins, melamine resin or polysulfones.In other embodiments of the present invention, cyst wall is made up of poly-(methyl) acrylate, polystyrene or polyvinyl acetate.
For expelling parasite microcapsules, " mass ratio of the capsule-core of microcapsules and the cyst wall of microcapsules " is by calculating as follows: all solid-liquid phase transition materials encapsulated by cyst wall and insect repellent itself with for the formation of the material of cyst wall or the mass ratio of material blends.In embodiments of the present invention, the mass ratio of described capsule-core and described cyst wall is between 1:5 to 5:1.In general, if the capsule-core of expelling parasite microcapsules and the mass ratio of cyst wall too small, then cyst wall can be caused blocked up, cause the pest repellant in capsule-core to be difficult to discharge.If the capsule-core of expelling parasite microcapsules and the mass ratio of cyst wall excessive, then cyst wall can be caused excessively thin, and cyst wall easily breaks, and causes the pest repellant in capsule-core to run off.In a preferred embodiment of the invention, the capsule-core of expelling parasite microcapsules and the mass ratio of cyst wall in the scope of 1:5 to 3:1, more preferably in the scope of 1:5 to 1:1.
the preparation of expelling parasite microcapsules
According to a further aspect in the invention, provide a kind of method for the preparation of expelling parasite microcapsules of the present invention, described method comprises: form cyst wall, and the solid-liquid phase transition material of described cyst wall encapsulating at least one phase transition temperature within the scope of 10 to 50 DEG C and at least one insect repellent are as capsule-core.
In the preparation of expelling parasite microcapsules of the present invention, the formation of described cyst wall comprises the cohesion of macromolecular compound, the interfacial polycondensation of reactant mixture or the emulsion polymerisation of ethylenically unsaturated monomer.
the cohesion of macromolecular compound
Form cyst wall by the cohesion of macromolecular compound to be realized by method known in following polymer arts, the method comprises: under the existence of emulsifier, to the dispersion of materials of capsule-core be formed in the aqueous solution of macromolecular compound, optionally carry out appropriately crosslinked by crosslinking agent to described macromolecular compound, carry out post processing subsequently, such as filter, wash, dry etc.
In the preparation of expelling parasite microcapsules of the present invention, described cohesion adopts following macromolecular compound to implement, and described macromolecular compound comprises the natural polysaccharide be selected from by xanthans, gelatin, gum Arabic, microcrystalline cellulose or combinations thereof.In order to strengthen the intensity of cyst wall, optionally in coacervated system, adding any known crosslinking agent being suitable for crosslinked natural polysaccharide, including, but not limited to aziridine, formaldehyde or its any combination.In a particular embodiment, use the formalin of 37% as crosslinking agent.
In an embodiment of the invention, the preparation of expelling parasite microcapsules adopts coacervation to be implemented by following: under the existence of any suitable emulsifier such as lauryl sodium sulfate SDS, the pest repellant and solid-liquid phase transition material that form capsule-core are dispersed in the aqueous solution of macromolecular compound such as gelatin and/or gum Arabic, optional employing pH adjusting agent regulates the pH value of coacervated system, then adding crosslinking agent such as formalin carries out appropriately crosslinked, thus forms expelling parasite microcapsules of the present invention.
Formed in the technical process of cyst wall in the cohesion by HMW, the consumption of emulsifier, pH adjusting agent and consumption thereof, crosslinking agent and the reaction condition of such as reaction temperature, mixing speed empirically can be determined by those skilled in the art.
the interfacial polycondensation of reactant mixture
Form cyst wall by the interfacial polycondensation of reactant mixture to be realized by the method that following polymer arts is known, the method comprises: under the existence of catalyzer and optional chain extender, and the aqueous phase that the oil phase formed core materials and oil-soluble monomer or monomer mixture and water-soluble monomer or monomer mixture are formed carries out interfacial condensation.
In the preparation of expelling parasite microcapsules of the present invention, described interfacial polycondensation can adopt following reactant mixture to implement, and described reactant mixture at least comprises: containing the oligomer of active hydrogen or polymer and active hydrogen reaction compound.
According to the present invention, " oligomer or polymer containing active hydrogen " refers to that itself is containing can providing any oligomer of the functional group of active hydrogen or polymer and/or can changing into any oligomer or polymer that can provide the functional group of active hydrogen containing in the process being formed cyst wall by polycondensation.It is known that active hydrogen has reactivity with the active hydrogen reaction functional group of such as isocyanate groups, it can be derived from-COOH ,-OH ,-SH, secondary amino group and primary amino functionalities.In addition, some functional groups, such as ester group (especially carboxylic acid ester groups), thioether group or anhydride group (especially carboxylic acid anhydride group) can such as become can provide the functional group of active hydrogen by hydrolysis.In order to realize interfacial polycondensation, containing the oligomer of active hydrogen or polymer preferably water miscible.
Contain the oligomer of active hydrogen and/or the example of polymer as suitable, PPG, PEPA, polycarbonate polyol, polyolefin polyhydric alcohol and combination thereof can be used.Preferably, be water soluble polyether polyols containing the oligomer of active hydrogen and/or polymer.As the example of PPG, can such as use the PTMEG with following formula structure:
Wherein R is the alkyl group of hydrogen or the optional replacement with 6 carbon atoms at the most, and n is the integer of 2-6, and m is the integer of 10 to 120.Its instantiation comprises polyethylene glycol, poly-(ethylene glycol and 1,2-propylene glycol) copolymer, polytetramethylene glycol.Particularly preferably there is the polyethylene glycol of 200 to 1000g/mol, preferably 300 to 800g/mol, more preferably 350 to 600g/mol molecular weight.
According to the present invention, " active hydrogen reaction compound " refers to, can react thus form any compound of covalently bound key with active hydrogen.In the present invention, use polyisocyanates as active hydrogen reaction compound.As the example of suitable polyisocyanate compound, hexamethylene diisocyanate can be used, ten dimethylene diisocyanates, cyclohexane-1, 4-vulcabond, 4, 4 '-two cyclohexyl methane diisocyanate, pentamethylene-1, 3-vulcabond, PPDI, Toluene-2,4-diisocyanate, 4-vulcabond, naphthalene-1, 4-vulcabond, biphenyl-4, 4 '-vulcabond, benzene-1, 2, 4-triisocyanate, dimethylbenzene-l, 4-vulcabond, dimethylbenzene-l, 3-vulcabond, methyl diphenylene diisocyanate, butane-1, 2, 3-triisocyanate, poly methylene poly phenyl poly isocyanate, its polyurethane-type prepolymer, one or more or its any combination in its polyester based prepolymers or its polyether based prepolymers.
In an embodiment of the invention, the preparation of expelling parasite microcapsules adopts interfacial polymerization to be implemented by following: under the existence of suitable emulsifier, oil phase is formed by forming the pest repellant of capsule-core and solid-liquid phase transition material and at least one active hydrogen reaction compound, then prepare containing the oligomer of active hydrogen or the aqueous phase of polymer, finally under the existence of suitable catalyzer and chain extender, make above-mentioned oil phase and aqueous phase carry out interfacial condensation reaction, thus form expelling parasite microcapsules of the present invention.
In order to obtain suitable cyst wall intensity, than preferably change in the scope of 0.9:1 to 1.1:1 with the molar equivalent of polyisocyanates containing the oligomer of active hydrogen or polymer.In the specific embodiment of the present invention, containing the molar equivalent of the oligomer of active hydrogen or polymer and polyisocyanates than changing in the scope of 0.98:1 to 1.02:1.
Formed in the technical process of cyst wall at the interfacial polycondensation by reactant mixture, the reaction condition of emulsifier, chain extender, catalyzer and their consumption and such as reaction temperature, mixing speed empirically can be determined by those skilled in the art.In the specific embodiment of the present invention, use ethylenediamine as the example of chain extender, use dibutyltin dilaurate as the example of catalyzer.
the emulsion polymerisation of ethylenically unsaturated monomer
Form cyst wall by the emulsion polymerisation of ethylenically unsaturated monomer can adopt method known in following polymer arts to realize, the method comprises, and under the existence of emulsifier, the material and ethylenically unsaturated monomer that form capsule-core is carried out emulsification; And under the existence of initator, make described ethylenically unsaturated monomer carry out emulsion polymerisation.Said method can use the emulsion polymerization technique of any conventional, such as single-order polymerization technique, multistage polymerization technique, continuous processing etc.
According to the present invention, described emulsion polymerisation adopts following ethylenically unsaturated monomer to implement, and described ethylenically unsaturated monomer comprises esters of acrylic acid, vinylacetate, phenylethylene, vinyl cyanide and combination thereof.
In embodiments of the present invention, the preparation of expelling parasite microcapsules adopts emulsion polymerisation to be implemented by following: under the effect of suitable emulsifier, the pest repellant of formation capsule-core and solid-liquid phase transition material and ethylenically unsaturated monomer or monomer mixture is made to be dispersed into emulsion in water, then the emulsion drop prepared is added in the polymer reactor containing initator and is polymerized, thus form expelling parasite microcapsules of the present invention.
According to the present invention, the cyst wall of expelling parasite microcapsules is formed by following polymerize monomer mixtures, and described monomer mixture comprises, relative to the gross weight of described monomer mixture, the hard ethylenically unsaturated monomer of 60 to 90 % by weight, the homopolymers of described hard ethylenically unsaturated monomer has the Tg higher than 25 DEG C; The soft ethylenically unsaturated monomer of 4 to 30 % by weight, the homopolymers of described soft ethylenically unsaturated monomer has the Tg being less than 15 DEG C; The multifunctional ethylenically unsaturated monomer of 1 to 20 % by weight; With 0 to 10 % by weight the ethylenically unsaturated monomer with acid functional group.
i) hard ethylenically unsaturated monomer
In the preparation of expelling parasite microcapsules of the present invention, any hard ethylenically unsaturated monomer can be used.In the present invention, " hard ethylenically unsaturated monomer " refers to, its homopolymers has the ethylenically unsaturated monomer higher than the Tg of 25 DEG C.In embodiments of the present invention, described hard ethylenically unsaturated monomer is selected from by phenylethylene, (methyl) esters of acrylic acid, (methyl) vinyl cyanide and the group that forms thereof.In a preferred embodiment of the invention, described hard ethylenically unsaturated monomer is selected from the group be made up of styrene, methyl methacrylate and combination thereof.
In expelling parasite microcapsules of the present invention, cyst wall comprises, relative to the gross weight of the monomer mixture of the described cyst wall of formation, and the hard ethylenically unsaturated monomer of 60 to 90 % by weight, preferably 65 to 90 % by weight, more preferably 70 to 85 % by weight.
ii) soft ethylenically unsaturated monomer
In the preparation of expelling parasite microcapsules of the present invention, any soft ethylenically unsaturated monomer can be used.In the present invention, " soft ethylenically unsaturated monomer " refers to, its homopolymers has the ethylenically unsaturated monomer of the Tg being less than 15 DEG C.In embodiments of the present invention, described soft ethylenically unsaturated monomer is selected from by (methyl) acrylic acid C3-C12 Arrcostab, vinylacetate class and the group that forms thereof.In a preferred embodiment of the invention, described soft ethylenically unsaturated monomer is selected from the group be made up of butyl acrylate, 2-EHA, ethyl acrylate, vinylacetate and combination thereof.
In expelling parasite microcapsules of the present invention, cyst wall comprises, relative to the gross weight of the monomer mixture of the described cyst wall of formation, and the soft ethylenically unsaturated monomer of 4 to 30 % by weight, preferably 5 to 25 % by weight, more preferably 10 to 20 % by weight.
iii) multifunctional ethylenically unsaturated monomer
In the preparation of expelling parasite microcapsules of the present invention, any multifunctional ethylenically unsaturated monomer can be used.In the present invention, " multifunctional ethylenically unsaturated monomer " refers to, has two or more, preferably three, even four olefinic unsaturated functional groups play the monomer of crosslinked action.In embodiments of the present invention, described multifunctional ethylenically unsaturated monomer is selected from by tripropylene glycol two (methyl) acrylate, dipropylene glycol two (methyl) acrylate, 1, 6-hexylene glycol two (methyl) acrylate, hexylene glycol two (methyl) acrylate of ethoxylation, 1, 4-butanediol two (methyl) acrylate, neopentyl glycol two (methyl) acrylate, propenoxylated neopentyl glycol two (methyl) acrylate, bisphenol-A two (methyl) acrylate of 4-ethoxylation, trimethylolpropane tris (methyl) acrylate, trimethylolpropane tris (methyl) acrylate of ethoxylation, propenoxylated glyceryl three (methyl) acrylate, pentaerythrite three (methyl) acrylate, the group of two-trimethylolpropane four (methyl) acrylate and combination composition thereof.In a preferred embodiment of the invention, described multifunctional ethylenically unsaturated monomer is selected from pentaerythritol triacrylate, trimethylolpropane triacrylate or its combination.
In the preparation of expelling parasite microcapsules of the present invention, the consumption of multifunctional ethylenically unsaturated monomer can make a significant impact the rate of release of pest repellant.Generally speaking, the consumption of multifunctional ethylenically unsaturated monomer is higher, and the crosslink density of cyst wall is larger, and result causes the rate of release of pest repellant slower.In contrast, the consumption of multifunctional ethylenically unsaturated monomer is lower, and the crosslink density of cyst wall is less, and result pest repellant can discharge fast.In the present invention, according to the rate of release expected, the consumption of multifunctional ethylenically unsaturated monomer is selected.In embodiments of the present invention, cyst wall comprises, relative to the gross weight of the monomer mixture of the described cyst wall of formation, and the multifunctional ethylenically unsaturated monomer of 1 to 20 % by weight, preferably 1 to 10 % by weight, more preferably 2 to 8 % by weight.
iv) there is the ethylenically unsaturated monomer of acid functional group
In the preparation of expelling parasite microcapsules of the present invention, can optionally use the ethylenically unsaturated monomer with acid functional group.This emulsion polymerisation existing for ethylenically unsaturated monomer with the ethylenically unsaturated monomer of acid functional group provides latex stability extraly.
In embodiments of the present invention, the ethylenically unsaturated monomer with acid functional group comprises the ethylenically unsaturated monomer with carboxylic acid functional, the ethylenically unsaturated monomer with phosphonic functional groups, has the ethylenically unsaturated monomer of sulfonic acid functional group.In a preferred embodiment of the invention, as the example of ethylenically unsaturated monomer with acid functional group, the ethylenically unsaturated monomer with carboxylic acid functional can be used.The example of above-mentioned carboxylic acid functionalized ethylenically unsaturated monomer comprises the group of acrylic acid, methacrylic acid, β-acryloxy propionic, ethylacrylic acid, α-chloroacrylic acid, crotonic acid, atropic acid, cinnamic acid, chloro-cinnamic acid, itaconic acid, maleic acid and combination composition thereof.Preferably, acrylic acid is used as an example.
In embodiments of the present invention, cyst wall comprises, relative to the gross weight of the monomer mixture of the described cyst wall of formation, and the ethylenically unsaturated monomer with acid functional group of 0 to 10 % by weight, preferably 0 to 5 % by weight, more preferably 0 to 2 % by weight.The ethylenically unsaturated monomer with acid functional group of lower consumption is favourable for the stable expelling parasite microcapsules of acquisition.Therefore, the consumption of the above-mentioned ethylenically unsaturated monomer with carboxylic acid functional, relative to the gross weight of the monomer mixture of the described cyst wall of formation, preferably in the scope of 0 to 1 weight.
The dispersion of above-mentioned ethylenically unsaturated monomer or monomer mixture can complete under the assistance of any known emulsifier.The example of available emulsifier comprises anion surfactant well known in the art, non-ionic surface active agent or its combination.Also the stable reagent of other types can be used, such as protective colloid.Preferably, the combination of anion surfactant and non-ionic surface active agent is used.Anion surfactant comprises aliphatic carboxylate, aliphatic sulfonate, aliphatic sulphate and aliphatic phosphate.Preferably, use alkali metal, such as Na, K or Li, or alkali salt, such as Ca or Ba.In a particular embodiment, use and comprise aliphatic sulfonate, preferably use dodecyl sodium sulfonate alkali metal salt, more preferably comprise dodecyl sodium sulfate (SDS).Non-ionic surface active agent comprises alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether.Preferably, alkylphenol polyoxyethylene is used.In a particular embodiment, OPEO (OP-10) is used.
Any known radical initiator initiated polymerization can be used.The example of available initator comprises, and thermolysis produces the initator of free radical at the polymerization temperature.Example comprises water-soluble and water-insoluble initator.The example producing the initator of free radical comprises persulfuric acid salt, such as ammonium persulfate or persulfuric acid alkali metal (comprising potassium, sodium or lithium); Peroxide, such as cumene hydroperoxide, TBHP, di-tert-butyl peroxide, dicapryl peroxide, crosses pentanoic acid tert-butyl ester, crosses different nonanoic acid tert-butyl ester, crosses octanoic acid ter-butyl ester, crosses neodecanoic acid tertiary butyl ester, peroxide two carbonic acid two (2-ethylhexyl) ester, peroxide two carbonic acid two (isotridecyl) ester; Azo-compound, such as azo two (isobutyronitrile) and azo two (4-cyanopentanoic acid); With the redox system of routine.Preferably, water soluble starter persulfate is used.More specifically, use ammonium persulfate as radical initiator.
In the preparation process of expelling parasite microcapsules of the present invention, the reaction condition of emulsifier and consumption and such as reaction temperature, mixing speed etc. empirically can be determined by those skilled in the art.Preferably, the pre-emulsification technology of monomer mixture carries out under the mixing speed of 2000rpm or higher, preferably carries out under the mixing speed of 4000rpm or higher.
expelling parasite additive
Another aspect provides a kind of expelling parasite additive, it is dry powdered form or is form of suspension, and wherein said expelling parasite additive package is containing expelling parasite microcapsules of the present invention.
According to the present invention, prepared expelling parasite microcapsules are form of suspension.The expelling parasite microcapsules of form of suspension can be used as it is, or the process means of this area routine can be adopted to form dried powder.Such as, the formation of dried powder can be realized by spraying dry, freeze drying or heating, drying etc.
coating composition
Another aspect provides a kind of coating composition, this coating composition comprises: the film-forming resin of film-forming amount; Supporting agent; Conventional additives; With expelling parasite microcapsules of the present invention or expelling parasite additive.
As use alpha nerein, " film-forming resin " refers to and usually play filming function and the resin be bonded together by all components in paint field.
When described coating composition is water-based paint compositions, the film-forming resin applied comprises organosilicon water-based latex, cinnamic acrylic ester water-based latex, pure acrylate water-based latex, organic-silicon-modified acrylic ester aquosity latex, vinylacetate water-based latex, vinyl acetate-acrylate water-based latex, ethylene-vinyl acetate water-based latex, vinylacetate-ethylene water-based latex, vinyl acetate-acrylate-tertiary carbonic ester (such as tertiary ethylene carbonate VeoVa10) water-based latex, fluorocarbon polymer water-based latex or its combination.Above-mentioned water-based latex can adopt suitable emulsion polymerisation process preparation well known to those of ordinary skill in the art.Or, as the instantiation of water-based latex, any commercially available product suitably can be used, such as cinnamic acrylic ester water-based latex, such as, purchased from RS998A, RS968 or RS936W of the rich Industrial Co., Ltd. of Ahmedabad.
When described coating composition is solvent-borne coating composition, the film-forming resin applied comprises, but be not limited to, abietic resin, alkyd resins, phenolic resins, amino resins, mylar, acrylic resin, epoxy resin, polyurethane resin, carbamide resin, vistanex, nitrocellulose resin, organic siliconresin or the film-forming resin being usually used in solvent-borne coating composition well known by persons skilled in the art.
Above-mentioned film-forming resin can adopt suitable preparation method's preparation well known to those of ordinary skill in the art.Or, any commercially available product suitably can be used, the alkyd resins of the trade mark CY468, CY472, CY474, CY499 of such as Dutch DSM N. V..
As those skilled in the art can easy understand, coating composition comprises the film-forming resin of film-forming amount.Preferably, the content of described film-forming resin in coating composition of the present invention, relative to the gross weight of coating composition, in the scope of about 5 to 45 % by weight.Preferably, film-forming resin content in the coating composition, based on the gross weight of described coating composition, be at least about 10 % by weight, more preferably at least about 15 % by weight, even more preferably at least about 20 % by weight.And preferably, the content of film-forming resin in coating composition of the present invention, based on the gross weight of described coating composition, at the most about 40 % by weight, be preferably at the most about 35 % by weight or be more preferably at the most about 30 % by weight.
Extra supporting agent can be added, with the viscosity of adjusting coating composition during the preparation of described coating composition.When described coating composition is water-based paint compositions, described supporting agent comprise water, with the miscible supporting agent of water such as alcohols or its combine.When described coating composition is solvent-borne coating composition, described supporting agent comprises esters solvent, alcohols solvent, ether solvent, ketones solvent, varsol or its arbitrary composition.
The addition of supporting agent can regulate according to required viscosity and processing request.The addition of supporting agent, relative to the gross weight of described coating composition, in the scope of about 15 to 40 % by weight, preferably in the scope of 15 to 35 % by weight.
Coating composition of the present invention also comprises conventional additives, and these additives can not adversely affect coating composition or solidified coating therefrom.Suitable additive comprises the processing characteristics or manufacturing property, the aesthetic feeling of enhancing composition, the specific function character improving coating composition or hardening composition therefrom or characteristic (such as to the adhesiveness of base material) that such as can improve composition or those reagent reduced costs.The additive that can comprise is such as filler, lubricant, coalescents, wetting agent, plasticizer, crosslinking agent, defoamer, colouring agent, wax, antioxidant, flow control agent, thixotropic agent, dispersant, adhesion promoter, UV stabilizing agent, thickener, defoamer, pH adjusting agent, solvent or its combination.The content of each optional member is enough to play it and is intended to achieve the goal, but preferably, such content can not adversely affect coating composition or solidified coating therefrom.In a preferred embodiment, coating composition of the present invention can also comprise thickener, dispersant, defoamer, wetting agent, pH adjusting agent, filler, coalescents, mould inhibitor, preservative or its any combination as conventional additives.According to the present invention, the total amount of conventional additives is 0.1 % by weight to about 79 % by weight relative to the gross weight of described coating composition.
Coating composition of the present invention also comprises expelling parasite microcapsules of the present invention or expelling parasite additive, and the consumption of these reagent can be determined as required, usually accounts for the 5-15 % by weight of described coating composition gross weight.
In the embodiment of a water-based paint compositions of the present invention, described water-based paint compositions comprises, based on the gross weight of described water-based paint compositions,
The water of 15 to 40 % by weight;
The described film-forming resin of 5 to 45 % by weight;
The conventional additives of 0.1 to 79 % by weight; With
The expelling parasite microcapsules of the present invention of 5 to 15 % by weight or expelling parasite additive.
In the embodiment of a solvent-borne coating composition of the present invention, described solvent-borne coating composition comprises, based on the gross weight of described solvent-borne coating composition,
The supporting agent of 15 to 40 % by weight;
The described film-forming resin of 5 to 45 % by weight;
The conventional additives of 0.1 to 79 % by weight; With
The expelling parasite microcapsules of the present invention of 5 to 15 % by weight or expelling parasite additive.
the application of expelling parasite microcapsules
According to a further aspect in the invention, provide a kind of method for walking quickly and keeping away insect, described method comprises: provide expelling parasite microcapsules of the present invention or expelling parasite additive; And by described expelling parasite microcapsules or expelling parasite additive application in the place needing expelling parasite.These need the place of expelling parasite comprise metope, door-plate, ceiling, floor, furniture, cabinet, fabric and other need the place of expelling parasite.In embodiments of the present invention, expelling parasite microcapsules of the present invention or expelling parasite additive are added in the coating composition for metope.
Embodiment
Following embodiment more particularly describes content disclosed by the invention, and these embodiments are only for illustrative explanation, because carrying out various modifications and variations in the scope of the disclosure of invention is obvious for a person skilled in the art.Unless otherwise stated, all parts reported in following examples, percentage and ratio are all based on weighing scale, and all reagent used in embodiment are all commercially available and can directly use and without the need to further process.
Embodiment 1: synthesize expelling parasite microcapsules by the cohesion of macromolecular compound
In the four-hole boiling flask being provided with agitator, thermometer and addition funnel, add 4.0g emulsifier sodium lauryl sulfate (SDS) solution in the aqueous gelatin solution of 100g3%, then under the mixing speed of 8000rpm, 2g pest repellant phenothrin and 2g phase change materials lauryl alcohol are distributed to wherein, stir 5 minutes, thus form dispersion emulsion.Dispersion emulsion be heated to about 40 DEG C and keep at such a temperature.Then, add the Arabic gum aqueous solution of 100g3%, and fully mix.Then the acetic acid solution of 10% is dripped, until pH is down to 3.8-4.3.Stir after 40 minutes under about 1000rpm, mixture is cooled to lower than 10 DEG C, and in reactant mixture, add the sodium hydrate aqueous solution of 5%, until pH rises to 9.0.Add the formalin of 37% of 5mL, then the temperature of reactant mixture is increased to 50 DEG C, and keep 20 minutes at such a temperature, thus define product.Products therefrom is filtered, washs, dry post processing, thus obtain 9.5g expelling parasite microcapsules of the present invention.
Embodiment 2: synthesize expelling parasite microcapsules by the interfacial polycondensation of reactant mixture
In the there-necked flask being provided with mechanical agitation and addition funnel, add 1g pest repellant phenothrin and 0.5g phase change materials lauryl alcohol and 1.2g cyclohexane.After abundant dissolving, add the emulsifier of TDI and 5.0g of 2.0g wherein, and stir, thus form oil phase.In another flask, add in 4.6gPEG400 and 100mL deionized water.After abundant dissolving, define aqueous phase.By gained aqueous phase and oil phase mixing, and adopt high speed dispersor to disperse to be no less than 5 minutes under the speed of 8000rpm, thus form dispersion emulsion.
In the four mouthfuls of reaction bulbs being provided with agitator, thermometer, thermostat and addition funnel, under the mixing speed of 1000rpm, in gained dispersion emulsion, add the dibutyltin dilaurate catalyzer of 0.04g.Reactant mixture is reacted 2 hours under room temperature (23 DEG C ± 2 DEG C), then adds the diethylamine of 0.40g, thus define the end product of form of suspension.
Embodiment 3: synthesize expelling parasite microcapsules by the emulsion polymerisation of ethylenically unsaturated monomer
In the four-hole boiling flask being provided with agitating device and addition funnel, add pest repellant phenothrin and phase change materials lauryl alcohol that 125g styrene, 25g butyl acrylate, 10g pentaerythritol triacrylate and 60g mass ratio are 1:1.Then, add 5g dodecyl sodium sulfate (SDS) and 2.5g OPEO (OP-10) solution in 150g water wherein, and mix.Under 5000rpm, stir 1h, thus form pre-emulsion.
Be provided with in four mouthfuls of reaction bulbs of agitator, thermometer, condenser and addition funnel at another, add 300g deionized water, 1gSDS, 0.5gOP-10,0.2g ammonium persulfate.While stirring, mixture is heated to 80 DEG C, then drips pre-emulsion, drip and complete in 2h.After dropping terminates, 0.5h at temperature being continued remain on 80 DEG C, thus define the expelling parasite microcapsules of emulsion form.
embodiment 4: water-based paint compositions
Expelling parasite microcapsules of the present invention and water, conventional film-forming resins and conventional additives (are comprised cellulose, defoamer, dispersant, wetting agent, pH adjusting agent, TiO
2, filler, coalescents, mould inhibitor and preservative) mix, thus form coating composition of the present invention.Shown in the table 1 composed as follows of coating composition.
Table 1: the component composition of water-based paint compositions and consumption thereof
| Raw material | Consumption | Source |
| Water | 15～40％ | |
| Cellulose | 0.03～0.5％ | Be purchased |
| Defoamer | 0.05～0.5％ | Be purchased |
| Dispersant | 0.05～0.5％ | Be purchased |
| Wetting agent | 0.05～0.5％ | Be purchased |
| PH adjusting agent | 0.05～0.5％ | Be purchased |
| TiO2 | 5～30％ | Be purchased |
| Filler | 10～60％ | Be purchased |
| Conventional film-forming resins | 5～30％ | Be purchased |
| Expelling parasite microcapsules of the present invention | 5～15％ | Self-control |
| Coalescents | 1～10％ | Be purchased |
| Mould inhibitor | 0.05～0.2％ | Be purchased |
| Preservative | 0.05～0.2％ | Be purchased |
Aforementioned coating composition, as wall surface coating, shows effective anthelminthic effect.
Claims (21)
1. expelling parasite microcapsules, described microcapsules comprise cyst wall and capsule-core, and wherein said capsule-core comprises the solid-liquid phase transition material of at least one phase transition temperature within the scope of 10 to 50 DEG C and at least one insect repellent.
2. expelling parasite microcapsules as claimed in claim 1, wherein, described solid-liquid phase transition material has the phase transition temperature within the scope of 10 to 30 DEG C.
3. expelling parasite microcapsules as claimed in claim 1, wherein, described solid-liquid phase transition material has the phase transition temperature within the scope of 30 to 50 DEG C.
4. expelling parasite microcapsules as claimed in claim 1, wherein, described solid-liquid phase transition material is selected from the group be made up of the paraffin of inorganic crystal hydrate, C15-C24, fatty acid and fatty alcohol.
5. as the expelling parasite microcapsules in Claims 1-4 as described in any one, wherein, described insect repellent is mosquito-repellent, cockroach repellant, ant repellant or lice class repellant.
6. expelling parasite microcapsules as claimed in claim 5, wherein, described repellant comprises vegetalitas repellant, organic synthesis repellant or its combination.
7. expelling parasite microcapsules as claimed in claim 1, wherein, described cyst wall is selected from by the group of xanthans, gelatin, gum Arabic, microcrystalline cellulose, polysiloxanes, polyurethane, polyureas, phenolic resins, melamine resin, polysulfones, poly-(methyl) acrylate, polystyrene, polyvinyl acetate, polyacrylonitrile or combinations thereof.
8. expelling parasite microcapsules as claimed in claim 1, wherein, the mass ratio of described solid-liquid phase transition material and described insect repellent is in the scope of 1:5 to 5:1.
9. expelling parasite microcapsules as claimed in claim 1, wherein, the mass ratio of the capsule-core of described microcapsules and the cyst wall of described microcapsules is in the scope of 1:5 to 5:1.
10., for the preparation of a method for the expelling parasite microcapsules in claim 1-9 described in any one, described method comprises:
Form cyst wall, the solid-liquid phase transition material of described cyst wall encapsulating at least one phase transition temperature within the scope of 10 to 50 DEG C and at least one insect repellent are as capsule-core.
11. methods as claimed in claim 10, wherein, the formation of described cyst wall comprises the cohesion of macromolecular compound, the interfacial polycondensation of reactant mixture or the emulsion polymerisation of ethylenically unsaturated monomer.
12. methods as claimed in claim 11, wherein, described cohesion adopts following macromolecular compound to implement, and described macromolecular compound comprises the natural polysaccharide be selected from by the group of xanthans, gelatin, gum Arabic, microcrystalline cellulose or combinations thereof.
13. methods as claimed in claim 11, wherein, described interfacial polycondensation adopts following reactant mixture to implement, and described reactant mixture at least comprises: containing the oligomer of active hydrogen or polymer and active hydrogen reaction compound.
14. methods as claimed in claim 13, wherein, described interfacial condensation comprises, under the existence of catalyzer and optional chain extender, the described oligomer containing active hydrogen or polymer and polyisocyanates are reacted, wherein, the described oligomer containing active hydrogen or polymer compare in the scope of 0.9:1 to 1.1:1 with the molar equivalent of described polyisocyanates.
15. methods as claimed in claim 14, wherein, described active hydrogen is derived from-COOH ,-OH ,-SH, secondary amino group or primary amino functionalities.
16. methods as claimed in claim 14, wherein, the described oligomer containing active hydrogen or polymer are water miscible.
17. methods as claimed in claim 14, wherein, described polyisocyanates comprises hexamethylene diisocyanate, ten dimethylene diisocyanates, cyclohexane-1, 4-vulcabond, 4, 4 '-two cyclohexyl methane diisocyanate, pentamethylene-1, 3-vulcabond, PPDI, Toluene-2,4-diisocyanate, 4-vulcabond, naphthalene-1, 4-vulcabond, biphenyl-4, 4 '-vulcabond, benzene-1, 2, 4-triisocyanate, dimethylbenzene-l, 4-vulcabond, dimethylbenzene-l, 3-vulcabond, methyl diphenylene diisocyanate, butane-1, 2, 3-triisocyanate, poly methylene poly phenyl poly isocyanate, its polyurethane-type prepolymer, one or more or its any combination in its polyester based prepolymers or its polyether based prepolymers.
18. methods as claimed in claim 11, wherein, described emulsion polymerisation adopts following ethylenically unsaturated monomer to implement, and described ethylenically unsaturated monomer comprises esters of acrylic acid, vinylacetate, phenylethylene, vinyl cyanide or its combination.
19. 1 kinds of expelling parasite additives, it is dry powdered form or is form of suspension, and wherein, described expelling parasite additive package is containing the expelling parasite microcapsules in claim 1 to 9 described in any one.
20. 1 kinds of coating compositions, comprise: the film-forming resin of film-forming amount; Supporting agent; Conventional additives; With the expelling parasite microcapsules in claim 1 to 9 described in any one or expelling parasite additive according to claim 19.
21. 1 kinds for walking quickly and keeping away the method for insect, described method comprises:
Expelling parasite microcapsules in claim 1 to 9 described in any one or expelling parasite additive according to claim 19 are provided; And
By described expelling parasite microcapsules or expelling parasite additive application in the place needing expelling parasite.
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