CN111001363B - Preparation method of high-mechanical-strength nano microcapsule with insect-trapping function - Google Patents
Preparation method of high-mechanical-strength nano microcapsule with insect-trapping function Download PDFInfo
- Publication number
- CN111001363B CN111001363B CN201911118411.XA CN201911118411A CN111001363B CN 111001363 B CN111001363 B CN 111001363B CN 201911118411 A CN201911118411 A CN 201911118411A CN 111001363 B CN111001363 B CN 111001363B
- Authority
- CN
- China
- Prior art keywords
- microcapsule
- poss
- vinyl
- mixture
- proportion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000003094 microcapsule Substances 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002418 insect attractant Substances 0.000 claims abstract description 27
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 22
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 7
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 7
- 239000003381 stabilizer Substances 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 29
- QMVPMAAFGQKVCJ-UHFFFAOYSA-N citronellol Chemical compound OCCC(C)CCC=C(C)C QMVPMAAFGQKVCJ-UHFFFAOYSA-N 0.000 claims description 10
- RUVINXPYWBROJD-ONEGZZNKSA-N trans-anethole Chemical compound COC1=CC=C(\C=C\C)C=C1 RUVINXPYWBROJD-ONEGZZNKSA-N 0.000 claims description 10
- 239000000975 dye Substances 0.000 claims description 9
- 238000006116 polymerization reaction Methods 0.000 claims description 9
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 8
- DCAYPVUWAIABOU-UHFFFAOYSA-N hexadecane Chemical compound CCCCCCCCCCCCCCCC DCAYPVUWAIABOU-UHFFFAOYSA-N 0.000 claims description 8
- -1 phenyl vinyl Chemical group 0.000 claims description 8
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 8
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 6
- XFCMNSHQOZQILR-UHFFFAOYSA-N 2-[2-(2-methylprop-2-enoyloxy)ethoxy]ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOCCOC(=O)C(C)=C XFCMNSHQOZQILR-UHFFFAOYSA-N 0.000 claims description 6
- QMVPMAAFGQKVCJ-SNVBAGLBSA-N (R)-(+)-citronellol Natural products OCC[C@H](C)CCC=C(C)C QMVPMAAFGQKVCJ-SNVBAGLBSA-N 0.000 claims description 5
- WTEVQBCEXWBHNA-UHFFFAOYSA-N Citral Natural products CC(C)=CCCC(C)=CC=O WTEVQBCEXWBHNA-UHFFFAOYSA-N 0.000 claims description 5
- 229940011037 anethole Drugs 0.000 claims description 5
- JGQFVRIQXUFPAH-UHFFFAOYSA-N beta-citronellol Natural products OCCC(C)CCCC(C)=C JGQFVRIQXUFPAH-UHFFFAOYSA-N 0.000 claims description 5
- 229940043350 citral Drugs 0.000 claims description 5
- 235000000484 citronellol Nutrition 0.000 claims description 5
- 239000010634 clove oil Substances 0.000 claims description 5
- WTEVQBCEXWBHNA-JXMROGBWSA-N geranial Chemical compound CC(C)=CCC\C(C)=C\C=O WTEVQBCEXWBHNA-JXMROGBWSA-N 0.000 claims description 5
- RUVINXPYWBROJD-UHFFFAOYSA-N para-methoxyphenyl Natural products COC1=CC=C(C=CC)C=C1 RUVINXPYWBROJD-UHFFFAOYSA-N 0.000 claims description 5
- HZUBBVGKQQJUME-UHFFFAOYSA-N 1,5-diamino-2-bromo-4,8-dihydroxyanthracene-9,10-dione Chemical compound O=C1C2=C(N)C(Br)=CC(O)=C2C(=O)C2=C1C(O)=CC=C2N HZUBBVGKQQJUME-UHFFFAOYSA-N 0.000 claims description 4
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 claims description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims description 4
- 235000005979 Citrus limon Nutrition 0.000 claims description 4
- 244000131522 Citrus pyriformis Species 0.000 claims description 4
- 235000000177 Indigofera tinctoria Nutrition 0.000 claims description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 4
- HVUMOYIDDBPOLL-XWVZOOPGSA-N Sorbitan monostearate Chemical compound CCCCCCCCCCCCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O HVUMOYIDDBPOLL-XWVZOOPGSA-N 0.000 claims description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 4
- TWFQJFPTTMIETC-UHFFFAOYSA-N dodecan-1-amine;hydron;chloride Chemical compound [Cl-].CCCCCCCCCCCC[NH3+] TWFQJFPTTMIETC-UHFFFAOYSA-N 0.000 claims description 4
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 4
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 4
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 4
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 4
- BXWNKGSJHAJOGX-UHFFFAOYSA-N hexadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCO BXWNKGSJHAJOGX-UHFFFAOYSA-N 0.000 claims description 4
- 229940097275 indigo Drugs 0.000 claims description 4
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 claims description 4
- 230000000977 initiatory effect Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 claims description 4
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims description 4
- 229920002379 silicone rubber Polymers 0.000 claims description 4
- 239000004945 silicone rubber Substances 0.000 claims description 4
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- HWSSEYVMGDIFMH-UHFFFAOYSA-N 2-[2-[2-(2-methylprop-2-enoyloxy)ethoxy]ethoxy]ethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCOCCOCCOC(=O)C(C)=C HWSSEYVMGDIFMH-UHFFFAOYSA-N 0.000 claims description 3
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 3
- 125000003700 epoxy group Chemical group 0.000 claims description 3
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 3
- AJIPIJNNOJSSQC-NYLIRDPKSA-N estetrol Chemical compound OC1=CC=C2[C@H]3CC[C@](C)([C@H]([C@H](O)[C@@H]4O)O)[C@@H]4[C@@H]3CCC2=C1 AJIPIJNNOJSSQC-NYLIRDPKSA-N 0.000 claims description 2
- 229950009589 estetrol Drugs 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 6
- 239000003999 initiator Substances 0.000 abstract description 6
- 239000011162 core material Substances 0.000 abstract description 5
- 239000011248 coating agent Substances 0.000 abstract description 4
- 238000000576 coating method Methods 0.000 abstract description 4
- 241000238631 Hexapoda Species 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000003292 glue Substances 0.000 abstract description 2
- 241001477931 Mythimna unipuncta Species 0.000 abstract 2
- 239000002994 raw material Substances 0.000 abstract 2
- 239000002131 composite material Substances 0.000 abstract 1
- 239000007970 homogeneous dispersion Substances 0.000 abstract 1
- 239000000178 monomer Substances 0.000 abstract 1
- 229920003023 plastic Polymers 0.000 abstract 1
- 239000004033 plastic Substances 0.000 abstract 1
- 230000000379 polymerizing effect Effects 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 20
- 239000000463 material Substances 0.000 description 7
- 241000607479 Yersinia pestis Species 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 238000000769 gas chromatography-flame ionisation detection Methods 0.000 description 5
- 238000000703 high-speed centrifugation Methods 0.000 description 5
- 238000004627 transmission electron microscopy Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 239000005667 attractant Substances 0.000 description 2
- 230000031902 chemoattractant activity Effects 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 238000002296 dynamic light scattering Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 235000003385 Diospyros ebenum Nutrition 0.000 description 1
- 241000792913 Ebenaceae Species 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 229910018557 Si O Inorganic materials 0.000 description 1
- 238000005411 Van der Waals force Methods 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 1
- 239000002195 soluble material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/14—Polymerisation; cross-linking
- B01J13/18—In situ polymerisation with all reactants being present in the same phase
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a preparation method of a high mechanical strength nano microcapsule with insect-attracting function, which takes water as a medium, traditional vinyl-containing micromolecules and vinyl-containing POSS molecules as monomers, an oily insect-attracting agent as a microcapsule core material, and then an auxiliary stabilizer, an emulsifier, a cross-linking agent and a dye are added, and after homogeneous dispersion, miniemulsion is initiated by an initiator to polymerize to generate an organic/inorganic composite microcapsule. The preparation method has the advantages of economic and easily-obtained raw materials and simpler process, and the target product can be directly obtained by directly polymerizing the raw materials through miniemulsion, thereby being beneficial to large-area popularization and application. Meanwhile, after the microcapsule is embedded in the oily insect attractant, the microcapsule can effectively play a role of slow release, thereby prolonging the service life. The microcapsule prepared by the invention can be uniformly mixed with the armyworm glue and the plastic plate to prepare the armyworm plate, the introduction of POSS groups ensures that the microcapsule is not easy to damage, and the operation of coating a layer of induced color on the microcapsule to attract insects can be saved.
Description
Technical Field
The invention relates to the field of nano material preparation, in particular to a preparation method of a high-mechanical-strength nano microcapsule with insect-trapping functionality.
Background
Food safety is always a topic closely concerned by common people and media, and the nation also provides great guarantee on the legislative level. The traditional method for killing pests and diseases mainly by pesticides is widely subject to the problem that the food safety is affected. Therefore, modern agriculture urgently needs to get rid of the traditional pest and disease damage expelling and killing mode, and a more environment-friendly method is adopted, such as a novel pest expelling and killing mode represented by a pest trapping plate, a pest trapping lamp and the like. The key core of this approach is to attract the original plant-destroying insects to the target site for killing. Therefore, the ingredients for attracting are critical, and generally speaking, the ingredients are mainly two parts, wherein the first part is the volatile oily attractant, and the other part is the specific attraction color. The oily insect attractant cannot meet the requirement of long-time use due to short exertion time, and the traditional solution is to prepare an attractant core or physically adsorb some materials, so that the problem of short volatilization time can be relieved to a certain extent, but the oily insect attractant needs to be repeatedly placed, and the release amount cannot be controlled. While the alluring color is basically achieved by painting a paint of a specific color on the base material, few materials integrate the two alluring factors.
The polymer microcapsule can effectively wrap the oily insect attractant to play a slow release role, and the release amount of the oily insect attractant can be regulated and controlled by controlling the crosslinking degree of the microcapsule. However, the conventional polymer microcapsules have a great disadvantage of insufficient strength, and are often damaged when applied to a coating or mixed with other materials to affect the use effect, so that it is necessary to enhance the overall strength of the polymer microcapsules.
Disclosure of Invention
Aiming at the technical defects, the invention aims to provide a preparation method of a high-mechanical-strength nano microcapsule with insect-trapping functionality, the prepared nano microcapsule combines an oily insect-trapping agent and trapping colors into a whole, the strength of the nano microcapsule is greatly enhanced, and the nano microcapsule plays a slow-release role in volatilization of the oily insect-trapping agent. The specific technical scheme of the invention is as follows:
a preparation method of high mechanical strength nano-microcapsule with insect-attracting function comprises the following steps: firstly, mixing and stirring 15-90mL of water, 1-10g of traditional vinyl-containing micromolecules, 1-10g of vinyl-containing POSS molecules, 0.1-5g of emulsifying agents, 0.1-5g of oily insect attractants, 0.1-5g of cross-linking agents, 0.1-3g of co-stabilizers and 0.01-1g of dyes at room temperature for 10min-1h, then treating for 1-10min at the low temperature of-10-5 ℃ through a cell crusher, adding 0.1-1g of potassium persulfate solution after the temperature is restored to the room temperature, and initiating polymerization for 5-24h at the temperature of 50-70 ℃ to finally obtain the nano microcapsule.
Wherein, the traditional vinyl-containing micromolecules are any one or a mixture of any several of ethyl methacrylate, lauryl methacrylate, butyl acrylate, styrene, acrylic acid and acrylonitrile in any proportion.
The POSS molecule containing vinyl is any one or a mixture of any several of octavinyl POSS, phenyl vinyl POSS, vinyl epoxy POSS, methyl propionyl isobutyl POSS and allyl POSS mixed in any proportion.
Wherein the emulsifier is any one or a mixture of any several of span 60, tween 80, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and dodecyl ammonium chloride mixed in any proportion.
Wherein the oily insect attractant is any one or a mixture of any several of clove oil, anethole, estolol, citral and citronellol in any proportion.
Wherein the crosslinking agent is any one or a mixture of any several of divinylbenzene, ethylene glycol dimethacrylate, diethylene glycol dimethacrylate and triethylene glycol dimethacrylate which are mixed in any proportion.
Wherein the co-stabilizer is any one or a mixture of any several of hexadecane, hexadecanol, vinyl silicone rubber, dodecyl mercaptan and octadecyl acrylate in any proportion.
Wherein the dye is any one or a mixture of any several of reactive yellow X-RG, lemon yellow, indigo, disperse blue E-2RL and disperse brilliant blue E-4R mixed in any proportion
Compared with the prior art, the invention has the beneficial effects that: the microcapsule preparation method adopts a miniemulsion polymerization method, and the system medium is water, so the method is green and environment-friendly. After POSS groups are introduced into the microcapsules, the mechanical strength of the microcapsules can be greatly enhanced, and the problem that the microcapsules are damaged and fail in use is avoided. After a cross-linked network structure is formed in the system, the release of the oily insect attractant can be quantitatively controlled according to the control of the cross-linking degree. The dye material is innovatively and directly introduced into the microcapsule, and the POSS group is an inorganic core consisting of a silicon-oxygen framework alternately connected by Si-O, and is a nanostructure hybrid system of polyhedral oligomeric silsesquioxane. The dyes selected by the invention are all water-soluble materials, and can not be embedded into the core material of the oil-induced insect attractant in a POSS-based microcapsule system, the physical adsorption is formed only by the mutual attraction of intermolecular force (Van der Waals force) and the wall material, and the dyes can be re-dispersed and paved on plates when being used with the pest-sticking glue material, so that the step of brushing the luring color paint on the trap plate is saved.
Drawings
FIG. 1 is a graph of the dynamic light scattering particle size analyzer of the microcapsules of example 3 of the present invention.
Detailed Description
The following examples are further detailed, but the present invention is not limited thereto, and all similar structures and similar variations thereof using the present invention shall fall within the scope of the present invention.
The invention provides a preparation method of a high-mechanical-strength nano microcapsule with insect-attracting function, which comprises the following steps: firstly, mixing and stirring 15-90mL of water, 1-10g of traditional vinyl-containing micromolecules, 1-10g of vinyl-containing POSS molecules, 0.1-5g of emulsifying agents, 0.1-5g of oily insect attractants, 0.1-5g of cross-linking agents, 0.1-3g of co-stabilizers and 0.01-1g of dyes at room temperature for 10min-1h, then treating for 1-10min at the low temperature of-10-5 ℃ through a cell crusher, adding 0.1-1g of potassium persulfate solution after the temperature is restored to the room temperature, and initiating polymerization for 5-24h at the temperature of 50-70 ℃ to finally obtain the nano microcapsule.
The traditional vinyl-containing micromolecules are any one or a mixture of any several of ethyl methacrylate, lauryl methacrylate, butyl acrylate, styrene, acrylic acid and acrylonitrile in any proportion.
The POSS molecule containing vinyl is any one or a mixture of any several of octavinyl POSS, phenyl vinyl POSS, vinyl epoxy group POSS, methyl propionyl isobutyl POSS and allyl POSS in any proportion.
The emulsifier is any one or a mixture of any several of span 60, tween 80, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and dodecyl ammonium chloride mixed in any proportion.
The oily insect attractant is any one or a mixture of any several of clove oil, anethole, estetrol, citral and citronellol in any proportion.
The cross-linking agent is any one or a mixture of any several of divinylbenzene, ethylene glycol dimethacrylate, diethylene glycol dimethacrylate and triethylene glycol dimethacrylate mixed in any proportion.
The co-stabilizer is any one or a mixture of any several of hexadecane, hexadecanol, vinyl silicone rubber, dodecyl mercaptan and octadecyl acrylate in any proportion.
The dye is any one or a mixture of any several of reactive yellow X-RG, lemon yellow, indigo, disperse blue E-2RL and disperse brilliant blue E-4R which are mixed in any proportion.
Example 1
50g of water, 5g of lauryl methacrylate, 1g of methylpropionyl isobutyl POSS, 0.1g of Tween 80, 0.2g of ebony alcohol, 0.1g of vinyl silicone rubber and 0.5g of active yellow X-RG are mixed and stirred at room temperature for 30min, then the mixture is treated by a cell crusher at the low temperature of-10 ℃ for 1min, the mixture is added with 0.1g of potassium persulfate aqueous solution containing an initiator after being recovered to the room temperature, the polymerization is initiated at the temperature of 60 ℃, and the nano microcapsule can be obtained after 8 h.
The microcapsule is spread on a 3cm multiplied by 3cm glass sheet, the oily insect attractant, namely the insect-attracting agent, namely the ethanol is also spread on the glass sheet, the glass sheet is placed outdoors, the microcapsule is taken back and placed into a glass bottle at intervals, the gas in the headspace with the same amount is taken after 24 hours, the concentration of the oily insect-attracting agent is detected by GC-FID, and the comparison shows that the microcapsule can maintain 67 percent of concentration after 15 days, and the concentration of the untreated oily insect-attracting agent is 0 percent. In addition, the microcapsules were not substantially damaged as observed by transmission electron microscopy after high-speed centrifugation, and represented excellent mechanical strength.
Example 2
70g of water, 8g of ethyl methacrylate, 3g of allyl POSS, 0.2g of dodecyl ammonium chloride, 1g of anethole, 0.2g of hexadecane and 0.6g of lemon yellow are mixed and stirred at room temperature for 40min, then the mixture is treated by a cell crusher at the low temperature of minus 5 ℃ for 3min, the mixture is recovered to the room temperature, then an aqueous solution containing 0.3g of initiator potassium persulfate is added to initiate polymerization at the temperature of 62 ℃, and the nano microcapsule can be obtained after 24 h.
The microcapsule is spread on a 3cm multiplied by 3cm glass sheet, the oily insect attractant anethole is also spread on the glass sheet in the same way, the glass sheet is placed outdoors, the microcapsule is taken back and placed into a glass bottle at intervals, the same amount of headspace gas is taken after 24 hours, the concentration of the oily insect attractant is detected by GC-FID, and the comparison shows that the microcapsule can maintain 32% concentration after 15 days, and the concentration of the untreated oily insect attractant is 0%. In addition, the microcapsules were not substantially damaged as observed by transmission electron microscopy after high-speed centrifugation, and represented excellent mechanical strength.
Example 3
Mixing and stirring 90g of water, 10g of butyl acrylate, 2g of vinyl epoxy group POSS, 0.3g of span 60, 2g of clove oil, 0.3g of hexadecanol and 0.7g of indigo at room temperature for 1 hour, treating for 5 minutes by a cell crusher at the low temperature of-2 ℃, returning to room temperature, adding an aqueous solution containing 0.5g of initiator potassium persulfate, and initiating polymerization at the temperature of 50 ℃ for 12 hours to obtain the nano microcapsule.
The microcapsule is spread on a 3cm multiplied by 3cm glass sheet, the same clove oil serving as the oily insect attractant is spread on the glass sheet, the glass sheet is placed outdoors, the microcapsule is taken back and placed into a glass bottle at intervals, the same amount of headspace gas is taken after 24 hours, the concentration of the oily insect attractant is detected by GC-FID, and comparison shows that the microcapsule can maintain 57% concentration after 15 days, and the concentration of the untreated oily insect attractant is 0%. In addition, the microcapsules were not substantially damaged as observed by transmission electron microscopy after high-speed centrifugation, and represented excellent mechanical strength.
As shown in FIG. 1, which is a dynamic light scattering particle size distribution Diagram (DLS) of the microcapsules prepared in example 3, the microcapsules had an average particle size of 61nm and exhibited a monodispersed distribution.
Example 4
80g of water, 6g of styrene, 4g of phenyl vinyl POSS, 1g of sodium dodecyl sulfate, 0.5g of citronellol, 1g of dodecyl mercaptan and 0.5g of disperse brilliant blue E-4R are mixed and stirred for 20min at room temperature, then the mixture is treated for 6min at the low temperature of-1 ℃ by a cell crusher, the mixture is restored to the room temperature, then 0.2g of potassium persulfate aqueous solution containing an initiator is added to initiate polymerization at the temperature of 58 ℃, and the nano microcapsule can be obtained after 6 h.
The microcapsule is spread on a 3cm multiplied by 3cm glass sheet, the oily insect attractant citronellol is also spread on the glass sheet in the same way, the glass sheet is placed outdoors, the oily insect attractant is taken back and placed into a glass bottle at intervals, the same amount of headspace gas is taken after 24 hours, the concentration of the oily insect attractant is detected by GC-FID, and the comparison shows that the microcapsule can maintain 51 percent concentration after 15 days, and the untreated oily insect attractant has 0 percent concentration. In addition, the microcapsules were not substantially damaged as observed by transmission electron microscopy after high-speed centrifugation, and represented excellent mechanical strength.
Example 5
Firstly, 65g of water, 9g of acrylonitrile, 6g of POSS containing octavinyl, 0.5g of sodium dodecyl benzene sulfonate, 3g of citral, 0.5g of octadecyl acrylate and 0.1g of disperse blue E-2RL are mixed and stirred for 50min at room temperature, then the mixture is treated for 7min by a cell crusher at the low temperature of-2 ℃, and after the mixture is recovered to the room temperature, an aqueous solution containing 0.6g of initiator potassium persulfate is added to initiate polymerization at the temperature of 70 ℃, and the nano microcapsule can be obtained after 10 h.
The microcapsule is spread on a 3cm multiplied by 3cm glass sheet, the oily insect attractant citral is also spread on the glass sheet in the same way, the glass sheet is placed outdoors, the microcapsule is taken back and placed into a glass bottle at intervals, the same amount of headspace gas is taken after 24 hours, the concentration of the oily insect attractant is detected by GC-FID, and the comparison shows that the microcapsule can maintain 35% concentration after 15 days, and the concentration of the untreated oily insect attractant is 0%. In addition, the microcapsules were not substantially damaged as observed by transmission electron microscopy after high-speed centrifugation, and represented excellent mechanical strength.
| Examples | 1 | 2 | 3 | 4 | 5 |
| Coating ratio (%) | 47.2 | 92.1 | 59.8 | 71.3 | 87.4 |
The table above shows the coating ratios (%) of examples 1 to 5.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (7)
1. A preparation method of high mechanical strength nano microcapsule with insect-attracting function is characterized in that: the method comprises the following steps: firstly, mixing and stirring 15-90mL of water, 1-10g of traditional vinyl-containing micromolecules, 1-10g of vinyl-containing POSS molecules, 0.1-5g of emulsifying agents, 0.1-5g of oily insect attractants, 0.1-5g of cross-linking agents, 0.1-3g of co-stabilizers and 0.01-1g of water-based dyes for 10min-1h at room temperature, then treating for 1-10min by a cell crusher at the low temperature of-10-5 ℃, returning to room temperature, adding 0.1-1g of potassium persulfate solution, initiating polymerization for 5-24h at 50-70 ℃ to finally obtain the nano microcapsule, the traditional vinyl-containing micromolecules are any one or a mixture of any several of ethyl methacrylate, lauryl methacrylate, butyl acrylate, styrene, acrylic acid and acrylonitrile in any proportion.
2. The method of claim 1, wherein: the POSS molecule containing vinyl is any one or a mixture of any several of octavinyl POSS, phenyl vinyl POSS, vinyl epoxy group POSS, methyl propionyl isobutyl POSS and allyl POSS in any proportion.
3. The method of claim 1, wherein: the emulsifier is any one or a mixture of any several of span 60, tween 80, sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and dodecyl ammonium chloride mixed in any proportion.
4. The method of claim 1, wherein: the oily insect attractant is any one or a mixture of any several of clove oil, anethole, estetrol, citral and citronellol in any proportion.
5. The method of claim 1, wherein: the cross-linking agent is any one or a mixture of any several of divinylbenzene, ethylene glycol dimethacrylate, diethylene glycol dimethacrylate and triethylene glycol dimethacrylate mixed in any proportion.
6. The method of claim 1, wherein: the co-stabilizer is any one or a mixture of any several of hexadecane, hexadecanol, vinyl silicone rubber, dodecyl mercaptan and octadecyl acrylate in any proportion.
7. The method of claim 1, wherein: the water-based dye is any one or a mixture of any several of reactive yellow X-RG, lemon yellow, indigo, disperse blue E-2RL and disperse brilliant blue E-4R which are mixed in any proportion.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911118411.XA CN111001363B (en) | 2019-11-15 | 2019-11-15 | Preparation method of high-mechanical-strength nano microcapsule with insect-trapping function |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911118411.XA CN111001363B (en) | 2019-11-15 | 2019-11-15 | Preparation method of high-mechanical-strength nano microcapsule with insect-trapping function |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111001363A CN111001363A (en) | 2020-04-14 |
| CN111001363B true CN111001363B (en) | 2021-11-02 |
Family
ID=70113723
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911118411.XA Active CN111001363B (en) | 2019-11-15 | 2019-11-15 | Preparation method of high-mechanical-strength nano microcapsule with insect-trapping function |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111001363B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111978906B (en) * | 2020-08-07 | 2022-07-29 | 浙江优力新材料有限公司 | MS sealant with insect expelling and ultraviolet aging resisting functions and preparation method thereof |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4874611A (en) * | 1985-06-20 | 1989-10-17 | The Dow Chemical Company | Microencapsulated ant bait |
| CN102108106A (en) * | 2011-01-05 | 2011-06-29 | 常州大学 | Method for preparing microcapsule through miniemulsion polymerization by utilizing siloxane copolymer as auxiliary stabilizing agent |
| CN102186462A (en) * | 2008-10-20 | 2011-09-14 | 微胶囊科技公司 | Microcapsules having an envelope composed essentially of silsesquioxane homopolymers or copolymers |
| WO2012004461A1 (en) * | 2009-05-26 | 2012-01-12 | Biosynthis | Silicone microcapsules having a cationic function |
| CN102675667A (en) * | 2012-05-23 | 2012-09-19 | 哈尔滨工业大学 | Preparation method of self-repairing POSS/microcapsule composite film |
| CN102726383A (en) * | 2012-07-05 | 2012-10-17 | 常州美胜生物材料有限公司 | Slow release type insect pest attractant microcapsule and preparation method thereof |
| CN103160077A (en) * | 2013-02-01 | 2013-06-19 | 厦门大学 | Self-lubrication-type wear-resistant epoxy resin containing POSS and preparation method thereof |
| CN104313719A (en) * | 2014-11-04 | 2015-01-28 | 常熟市新达纬编厂 | Uvioresistant fiber |
| CN105432610A (en) * | 2015-12-16 | 2016-03-30 | 中国林业科学研究院森林生态环境与保护研究所 | Dendrolimus punctatus (walker) sex pheromone microcapsule and preparation method thereof |
-
2019
- 2019-11-15 CN CN201911118411.XA patent/CN111001363B/en active Active
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4874611A (en) * | 1985-06-20 | 1989-10-17 | The Dow Chemical Company | Microencapsulated ant bait |
| CN102186462A (en) * | 2008-10-20 | 2011-09-14 | 微胶囊科技公司 | Microcapsules having an envelope composed essentially of silsesquioxane homopolymers or copolymers |
| WO2012004461A1 (en) * | 2009-05-26 | 2012-01-12 | Biosynthis | Silicone microcapsules having a cationic function |
| CN102108106A (en) * | 2011-01-05 | 2011-06-29 | 常州大学 | Method for preparing microcapsule through miniemulsion polymerization by utilizing siloxane copolymer as auxiliary stabilizing agent |
| CN102675667A (en) * | 2012-05-23 | 2012-09-19 | 哈尔滨工业大学 | Preparation method of self-repairing POSS/microcapsule composite film |
| CN102726383A (en) * | 2012-07-05 | 2012-10-17 | 常州美胜生物材料有限公司 | Slow release type insect pest attractant microcapsule and preparation method thereof |
| CN103160077A (en) * | 2013-02-01 | 2013-06-19 | 厦门大学 | Self-lubrication-type wear-resistant epoxy resin containing POSS and preparation method thereof |
| CN104313719A (en) * | 2014-11-04 | 2015-01-28 | 常熟市新达纬编厂 | Uvioresistant fiber |
| CN105432610A (en) * | 2015-12-16 | 2016-03-30 | 中国林业科学研究院森林生态环境与保护研究所 | Dendrolimus punctatus (walker) sex pheromone microcapsule and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111001363A (en) | 2020-04-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111001363B (en) | Preparation method of high-mechanical-strength nano microcapsule with insect-trapping function | |
| ES2148659T3 (en) | PREPARATION PROCESS OF MULTICOLORED AQUEOUS PAINT. | |
| DE2320068A1 (en) | STABILIZED LATEX AND METHOD FOR MANUFACTURING IT | |
| DE102009001776A1 (en) | Composition comprising as aqueous dispersion preferably benzophenone-containing (meth) acrylate polymers mixed with these different (meth) acrylate polymers and the use of the composition | |
| DE60033436D1 (en) | METHOD FOR PRODUCING ENLARGED LATEX PARTICLES | |
| EP1891140A1 (en) | Method for producing an aqueous polymer dispersion | |
| DE60010938D1 (en) | FINE-PIECE LATEX AND ITS PRODUCTION BY A VACCINE CRYSTAL PROCESS | |
| EP1883656A1 (en) | Method for the production of an aqueous polymer dispersion | |
| EP0320865B1 (en) | Process for the preparation of aqueous polymer dispersions | |
| CN108395504B (en) | Method for preparing double-response polymer Janus microspheres by soap-free emulsion polymerization | |
| DE2009066A1 (en) | Process for the production of block copolymers | |
| EP1869094A1 (en) | Method for producing an aqueous polymer dispersion | |
| DE2251063C3 (en) | Process for sealing contact points between surfaces | |
| CN108570123A (en) | A kind of acrylic acid ester emulsion and preparation method thereof for plastic basis material | |
| US20070071684A1 (en) | Process for the preparation of surface coatings and films | |
| EP1846464A1 (en) | Method for the production of an aqueous polymer dispersion | |
| KR101492843B1 (en) | Ink-jet ink for color filter and method for preparing the same and method for preparation of color filter | |
| KR970706312A (en) | Copolymer latex and process for its production (COPOLYMER LATEX AND PROCESS FOR PRODUCING THE SAME) | |
| Chemtob et al. | 1, 4-polybutadiene-based particles prepared by aqueous suspension ring-opening metathesis polymerization | |
| DE1720897C3 (en) | Process for the polymerisation of ethylenically unsaturated monomers in an aqueous emulsion | |
| CN107698702B (en) | Method for preparing fluorine-containing hollow microspheres by using single nano particle to stabilize multiple Pickering emulsions | |
| EP0308864A2 (en) | Process for preparing uniformly sized, fine particles of polymer | |
| JPH08319303A (en) | Aqueous polymer dispersion, thickening agent for aqueous system, oil-in-water emulsion and production of aqueous polymer dispersion | |
| CN112029040A (en) | Preparation method of acrylate core-shell structure emulsion for insect-trapping board glue | |
| DE60118731T2 (en) | STABILIZATION OF LIGHT-SENSITIVE SUBSTANCES |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |