CN106035324A - Preparation method of microcapsule mosquito-repellent incense liquid containing meperfluthrin - Google Patents
Preparation method of microcapsule mosquito-repellent incense liquid containing meperfluthrin Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
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- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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Abstract
The invention provides a preparation method of a microcapsule mosquito-repellent incense liquid containing meperfluthrin. The method comprises the steps that a gelatin aqueous solution with the mass concentration ranging from 5% to 7% and an Arabic gum aqueous solution with the mass concentration ranging from 3% to 5% are prepared separately, and the two solutions are mixed; meperfluthrin, tert-butylhydroquinone and an extract of cycas revoluta Thunb. are added into the mixed solution obtained in the first step, stirring is conducted for 20 min to 40 min, meperfluthrin is mixedly dispersed in the mixed solution, and an emulsified solution is obtained; 70 ml-150 ml of deionized water is added into the emulsified solution obtained in the second step, stirring is conducted for 40 min to 60 min, and a diluted solution is obtained; the pH value of the diluted solution obtained in the third step is adjusted to range from 3.8 to 5.0, and a preformed solution is obtained; the temperature of the preformed solution obtained in the fourth step is decreased to 0 DEG C to 5 DEG C on the condition that the stirring speed ranges from 300 r/min to 500 r/min, heat preservation is conducted for 40 min to 60 min, and an agglomerated solution is obtained; 0.5-1 g of soluble starch, 1-2 g of 1-methyl itaconate and 2-5 g of cross-linking curing agent are added into the agglomerated solution, mixing is conducted to be uniform, and the microcapsule mosquito-repellent incense liquid is obtained. The mosquito-repellent incense liquid is lasting in effect and good in antifungal effect.
Description
Technical field
The present invention improves the preparation method of a kind of mosquito incense, a kind of microcapsule mosquito incense liquid containing fluorine chlorine ether chrysanthemum ester.
Background technology
Microcapsule technology is to utilize a class material to be coated with by another kind of material as filmogen, forms microencapsulation
A kind of technology.Capsule size, generally in nanometer to micron order, along with the development of nano fabrication technique, prepares nanoscale grain
The microcapsule in footpath is widely studied.Microcapsule is usually the nucleocapsid structure of monolayer, and the core that cyst membrane is coated with can also be in many
Core shape, is wrapped in the material within microcapsule and is referred to as the capsule heart, active substance, core etc., and the coating film outside microcapsule is referred to as wall
Material, cyst wall, housing etc..Material is carried out micro encapsulation and can improve the stability of material, control the rate of release of core, improve
It is wrapped by the physical property of material, it is simple to process etc..
Gelatin is that one is effectively protected colloid, can stop the gathering of crystal or ion, and have good biology
The compatibility, biodegradable and moulding property, be to prepare wall material raw material important in microcapsule.Prepare gelatin-microcapsule generally to select
Method have Simple coacervation, complex coacervation, freeze-drying, spray drying method etc..Carboxyl on gelatin side chain, amino and
Hydroxyl makes it have higher chemism, can be modified gelatin by various methods, obtains many and had both retained gelatin
Excellent properties, has again the new material of new features.Leng Yan state etc. utilizes acrylamide that gelatin carries out graft modification, with list
Microcapsule prepared by coacervation, research shows that the increase with grafted gelatin molecular weight, Microcapsules Size distribution broaden, along with connecing
The reduction of branch gelatine molecular weight, the particle diameter distribution of microcapsule is more concentrated, and tends to normal distribution.By other natural polymer
Sub-material is blended with gelatin, significantly improves its biocompatibility, controlled degradation, such as chitosan etc..
Existing technology is fast to fluorine chlorine ether chrysanthemum ester rate of release, and antibacterial repelling effect is the best, and the present invention improves it and resists
Bacterium repelling effect.
Summary of the invention
The present invention utilizes gelatin and arabic gum to wrap fluorine chlorine ether chrysanthemum ester, tert-butylhydroquinone, Cycas revoluta extract
Covering, soluble starch, 1-methyl itaconic ester, crosslinking and curing agent, to gelatin modified, increase the compactness of clad, reduce chlorine fluorine
Ethofenprox, the rate of release of tert-butylhydroquinone, persistent.
A kind of preparation method of the microcapsule mosquito incense liquid containing fluorine chlorine ether chrysanthemum ester, preparation process is as follows:
(1) respectively preparation mass concentration be 5%～7% aqueous gelatin solution and the arabic gum that mass concentration is 3%～5% water-soluble
Liquid each 150～250ml, and by two kinds of solution mixing；
(2) 4～8g fluorine chlorine ether chrysanthemum esters, tert-butylhydroquinone 1 ~ 4g, Cycas revoluta extract 1 ~ 3g are added what step (1) obtained
In mixed solution, low whipping speed 300～500r/min, whipping temp is 30～60 DEG C, and mixing time 20～40min, by chlorine
The mixing of fluorine ethofenprox is dispersed in above-mentioned mixed solution, obtains emulsion；
(3) adding deionized water 70～150ml in the emulsion that step (2) obtains, low whipping speed is 300～500r/min
Under the conditions of, mixing time 40～60min, obtain diluent；
(4) the pH value of the diluent obtained to step (3) is adjusted to 3.8～5.0 and obtains pre-polymerization liquid；
(5), under the conditions of low whipping speed is 300～500r/min, the temperature of the pre-polymerization liquid that step (4) obtains is made to be reduced to 0～5
DEG C, and it is incubated 40～60min, obtain coagulation liquid；
(6) in the coagulation liquid that step (5) obtains, with soluble starch 0.5 ~ 1g, 1-methyl itaconic ester 1 ~ 2g, crosslinking curing
Agent 2～5g, 20 DEG C of reaction 30min, add 4-bromine resorcinol 0.2g, Bis(pentaerythritol) 0.6g and titanium sulfate 0.1g, 30 DEG C are anti-
1.5h, mix homogeneously is answered to obtain microcapsule mosquito incense liquid.
The molecular weight of described gelatin is 10～150,000；Preparation Cycas revoluta extract: weigh Cycas revoluta powder 50～100g and be placed in
In container, add 500～1000ml tap waters and disecoctylmaleate sodium sulfonate 1 ~ 3g, water at 110～130 DEG C
Bath extraction 12～24h, obtains extract, and the filtrate that sucking filtration obtains is Cycas revoluta extract；Crosslinking and curing agent be aluminum sulfate, iron sulfate,
Aluminum chloride, the one of sodium alginate.
The present invention compares the advantage of original technology and is:
(1) select tert-butylhydroquinone, Cycas revoluta extract to strengthen fluorine chlorine ether chrysanthemum ester and mosquito is knocked down and kills the merit of activity
Effect, and have and drive fly, antibacterial effect；
(2) soluble starch, 1-methyl itaconic ester, the compactness of crosslinking and curing agent increase gelatin surface, slowly discharge；
(3) disecoctylmaleate sodium sulfonate promotes Cycas revoluta water to enter inside Cycas revoluta, extracts effective ingredient therein；
(4) aluminum sulfate, iron sulfate, aluminum chloride, sodium alginate environment-protecting asepsis, changes traditional big lacking of glutaraldehyde solidification toxicity
Fall into；
(5) dioctyl sodium sulfosuccinate has another name called disecoctylmaleate sodium sulfonate, fast penetrant T.
(6) Cycas revoluta powder is to be dried by Cycas revoluta, pulverizes, obtains Cycas revoluta powder.
(7) gelatine molecular weight is weight average molecular weight.
(8) being easiest to reunite for microcapsule, between the present invention, 4-bromine resorcinol, Bis(pentaerythritol) are at sulphuric acid
Titanium, increases the hydrophobicity of capsule surface, reduces the reunion between capsule.
Detailed description of the invention
Example one
(1) aqueous gelatin solution that mass concentration is 5% and the arabic gum each 150ml of aqueous solution that mass concentration is 3% are prepared respectively,
And by two kinds of solution mixing；The molecular weight of described gelatin is 100,000
(2) 4g fluorine chlorine ether chrysanthemum ester, tert-butylhydroquinone 1g, Cycas revoluta extract 1g are added the mixed solution that step (1) obtains
In, low whipping speed 300r/min, whipping temp is 30 DEG C, and mixing time 20min obtains emulsion；
(3) in the emulsion that step (2) obtains, deionized water 70ml is added, under the conditions of low whipping speed is 300r/min, 30 DEG C
Mixing time 40min, obtains diluent；
(4) pH value of the diluent obtained to step (3) is adjusted to 3.8 and obtains pre-polymerization liquid；
(5), under the conditions of low whipping speed is 300r/min, makes the temperature of the pre-polymerization liquid that step (4) obtains be reduced to 0 DEG C, and be incubated
40min, obtains coagulation liquid；
(6) in the coagulation liquid that step (5) obtains, soluble starch 0.5g, 1-methyl itaconic ester 1g, aluminum sulfate 2g are added, 20
DEG C reaction 30min, add 4-bromine resorcinol 0.2g, Bis(pentaerythritol) 0.6g and titanium sulfate 0.1g, 30 DEG C reaction 1.5h, mixing
Uniformly obtain microcapsule mosquito incense liquid.
Preparation Cycas revoluta extract: weigh Cycas revoluta powder 50g and be placed in container, adds 500ml tap water and maleic two
Acid di-sec-octyl sodium sulfonate 1g, water-bath extraction 12h at 110 DEG C, the filtrate that sucking filtration obtains is Cycas revoluta extract.
Example two
(1) aqueous gelatin solution that mass concentration is 7% and the arabic gum each 250ml of aqueous solution that mass concentration is 5% are prepared respectively,
And by two kinds of solution mixing；The molecular weight of described gelatin is 150,000
(2) 8g fluorine chlorine ether chrysanthemum ester, tert-butylhydroquinone 4g, Cycas revoluta extract 3g are added the mixed solution that step (1) obtains
In, low whipping speed 500r/min, whipping temp is 60 DEG C, and mixing time 40min obtains emulsion；
(3) in the emulsion that step (2) obtains, add deionized water 150ml, under the conditions of low whipping speed is 500r/min, stir
Mix time 60min, obtain diluent；
(4) the pH value of the diluent obtained to step (3) is adjusted to 5.0 and obtains pre-polymerization liquid；
(5), under the conditions of low whipping speed is 500r/min, makes the temperature of the pre-polymerization liquid that step (4) obtains be reduced to 5 DEG C, and protect
Temperature 60min, obtains coagulation liquid；
(6) in the coagulation liquid that step (5) obtains, soluble starch 1g, 1-methyl itaconic ester 2g, iron sulfate 5g are added, 20 DEG C
Reaction 30min, adds 4-bromine resorcinol 0.2g, Bis(pentaerythritol) 0.6g and titanium sulfate 0.1g, and 30 DEG C of reaction 1.5h, mixing is all
Even obtain microcapsule mosquito incense liquid.
Preparation Cycas revoluta extract: weigh Cycas revoluta powder 100g and be placed in container, adds 1000ml tap water and maleic
Diacid di-sec-octyl sodium sulfonate 3g, at 120 DEG C, water-bath extraction 24h, obtains extract, and the filtrate that sucking filtration obtains is Cycas revoluta extraction
Thing.
Example three
(1) respectively preparation mass concentration be 6% aqueous gelatin solution and the arabic gum aqueous solution that mass concentration is 4% each
200ml, and by two kinds of solution mixing；The molecular weight of described gelatin is 120,000
(2) mixing 6g fluorine chlorine ether chrysanthemum ester, tert-butylhydroquinone 2.5g, Cycas revoluta extract 2g addition step (1) obtained is molten
In liquid, low whipping speed 400r/min, whipping temp is 45 DEG C, and mixing time 30min obtains emulsion；
(3) in the emulsion that step (2) obtains, add deionized water 110ml, under the conditions of low whipping speed is 400r/min, stir
Mix time 50min, obtain diluent；
(4) the pH value of the diluent obtained to step (3) adjusts 4.5 to obtain pre-polymerization liquid；
(5), under the conditions of low whipping speed is 400r/min, the temperature of the pre-polymerization liquid that step (4) obtains is made to be reduced to 2.5 DEG C, and
Insulation 50min, obtains coagulation liquid；
(6) in the coagulation liquid that step (5) obtains, soluble starch 0.75g, 1-methyl itaconic ester 1.5g, aluminum chloride are added
3.5g, 20 DEG C of reaction 30min, add 4-bromine resorcinol 0.2g, Bis(pentaerythritol) 0.6g and titanium sulfate 0.1g, 30 DEG C of reactions
1.5h, mix homogeneously obtains microcapsule mosquito incense liquid.
Preparation Cycas revoluta extract: weigh Cycas revoluta powder 75g and be placed in container, adds 750ml tap water and maleic two
Acid di-sec-octyl sodium sulfonate 2g, at 130 DEG C, water-bath extraction 18h, obtains extract, and the filtrate that sucking filtration obtains is Cycas revoluta extract.
Example four
(1) respectively preparation mass concentration be 5% aqueous gelatin solution and the arabic gum aqueous solution that mass concentration is 5% each
180ml, and by two kinds of solution mixing；
(2) 6g fluorine chlorine ether chrysanthemum ester, tert-butylhydroquinone 4g, Cycas revoluta extract 3g are added the mixed solution that step (1) obtains
In, low whipping speed 500r/min, whipping temp is 60 DEG C, and mixing time 40min obtains emulsion；
(3) in the emulsion that step (2) obtains, add deionized water 150ml, under the conditions of low whipping speed is 500r/min, stir
Mix time 60min, obtain diluent；
(4) the pH value of the diluent obtained to step (3) is adjusted to 5.0 and obtains pre-polymerization liquid；
(5), under the conditions of low whipping speed is 500r/min, makes the temperature of the pre-polymerization liquid that step (4) obtains be reduced to 5 DEG C, and protect
Temperature 60min, obtains coagulation liquid；
(6) in the coagulation liquid that step (5) obtains, soluble starch 1g, 1-methyl itaconic ester 2g, sodium alginate 2g are added, 20
DEG C reaction 30min, add 4-bromine resorcinol 0.2g, Bis(pentaerythritol) 0.6g and titanium sulfate 0.1g, 30 DEG C reaction 1.5h, mixing
Uniformly obtain microcapsule mosquito incense liquid.
Preparation Cycas revoluta extract: weigh Cycas revoluta powder 100g and be placed in container, adds 1000ml tap water and maleic
Diacid di-sec-octyl sodium sulfonate 3g, at 115 DEG C, water-bath extraction 24h, obtains extract, and the filtrate that sucking filtration obtains is Cycas revoluta extraction
Thing.
Example five
(1) respectively preparation mass concentration be 5% aqueous gelatin solution and the arabic gum aqueous solution that mass concentration is 5% each
180ml, and by two kinds of solution mixing；
(2) 6g fluorine chlorine ether chrysanthemum ester, tert-butylhydroquinone 4g, Cycas revoluta extract 3g are added the mixed solution that step (1) obtains
In, low whipping speed 500r/min, whipping temp is 60 DEG C, and mixing time 40min obtains emulsion；
(3) in the emulsion that step (2) obtains, add deionized water 150ml, under the conditions of low whipping speed is 500r/min, stir
Mix time 60min, obtain diluent；
(4) the pH value of the diluent obtained to step (3) is adjusted to 5.0 and obtains pre-polymerization liquid；
(5), under the conditions of low whipping speed is 500r/min, makes the temperature of the pre-polymerization liquid that step (4) obtains be reduced to 5 DEG C, and protect
Temperature 60min, obtains coagulation liquid；
(6) in the coagulation liquid that step (5) obtains, soluble starch 1g, 1-methyl itaconic ester 2g, aluminum sulfate 2g are added, 20 DEG C
Reaction 30min, adds 4-bromine resorcinol 0.2g, Bis(pentaerythritol) 0.6g and titanium sulfate 0.1g, and 30 DEG C of reaction 1.5h, mixing is all
Even obtain microcapsule mosquito incense liquid.
Preparation Cycas revoluta extract: weigh Cycas revoluta powder 100g and be placed in container, adds 1000ml tap water and maleic
Diacid di-sec-octyl sodium sulfonate 3g, at 125 DEG C, water-bath extraction 24h, obtains extract, and the filtrate that sucking filtration obtains is Cycas revoluta extraction
Thing.
The following is the experimental data of microcapsule mosquito incense liquid prepared by embodiment three.
By be dried under room temperature microcapsule mosquito incense product and be placed on 45 DEG C and wet with the fluorine chlorine ether chrysanthemum ester of its core equivalent
Degree be 70% constant temperature and humidity incubator in cultivate after a period of time and carry out antibiotic property experiment.
Table 1 microcapsule mosquito incense liquid is to the antibiotic rate (%) for examination strain
| Sample | Escherichia coli | Staphylococcus glucose bacterium | Aspergillus flavus |
| Fluorine chlorine ether chrysanthemum ester | 99 | 99 | 99 |
| Blank microcapsule | 0 | 0 | 0 |
| Microcapsule mosquito incense liquid | 99 | 99 | 99 |
2 30 days microcapsule mosquito incense liquid of table is to the antibiotic rate (%) for examination strain
| Sample | Escherichia coli | Staphylococcus glucose bacterium | Aspergillus flavus |
| Fluorine chlorine ether chrysanthemum ester | 0 | 0 | 0 |
| Blank microcapsule | 0 | 0 | 0 |
| Microcapsule mosquito incense liquid | 56 | 78 | 64 |
Finding out from table 2, under the same terms, fluorine chlorine ether chrysanthemum ester is being placed after 30 days almost without antibiotic property, and fluorine chlorine ether chrysanthemum ester is micro-
Capsule liquid still has stronger antibiotic property after placing 30 days, has reached the purpose that microcapsule slowly discharges, has made microcapsule have
Wider application prospect.
Repelling effect: respectively choose 10 people, blood group is consistent, is compared with market mosquito incense by microcapsule mosquito incense, discovery microcapsule
The vestige stung without mosquito with people morning next day of mosquito incense, market mosquito incense user has with 3 people next day the vestige having mosquito to sting.
The preferred embodiment of the present invention described in detail above.Should be appreciated that those of ordinary skill in the art without
Need creative work just can make many modifications and variations according to the design of the present invention.Therefore, all technology in the art
Personnel are available by logical analysis, reasoning, or a limited experiment the most on the basis of existing technology
Technical scheme, all should be in the protection domain being defined in the patent claims.
Claims (4)
1. the preparation method of the microcapsule mosquito incense liquid containing fluorine chlorine ether chrysanthemum ester, it is characterised in that preparation process is as follows:
(1) respectively preparation mass concentration be 5%～7% aqueous gelatin solution and the arabic gum that mass concentration is 3%～5% water-soluble
Liquid each 150～250ml, and by two kinds of solution mixing；
(2) 4～8g fluorine chlorine ether chrysanthemum esters, tert-butylhydroquinone 1 ~ 4g, Cycas revoluta extract 1 ~ 3g are added what step (1) obtained
In mixed solution, low whipping speed 300～500r/min, whipping temp is 30～60 DEG C, and mixing time 20～40min, by chlorine
The mixing of fluorine ethofenprox is dispersed in above-mentioned mixed solution, obtains emulsion；
(3) adding deionized water 70～150ml in the emulsion that step (2) obtains, low whipping speed is 300～500r/min
Under the conditions of, mixing time 40～60min, obtain diluent；
(4) the pH value of the diluent obtained to step (3) is adjusted to 3.8～5.0 and obtains pre-polymerization liquid；
(5), under the conditions of low whipping speed is 300～500r/min, the temperature of the pre-polymerization liquid that step (4) obtains is made to be reduced to 0～5
DEG C, and it is incubated 40～60min, obtain coagulation liquid；
(6) with soluble starch 0.5 ~ 1g, 1-methyl itaconic ester 1 ~ 2g, crosslinking curing in the coagulation liquid that step (5) obtains
Agent 2～5g, 20 DEG C of reaction 30min, add 4-bromine resorcinol 0.2g, Bis(pentaerythritol) 0.6g and titanium sulfate 0.1g, 30 DEG C are anti-
1.5h, mix homogeneously is answered to obtain microcapsule mosquito incense liquid.
2., according to the preparation method of a kind of microcapsule mosquito incense liquid containing fluorine chlorine ether chrysanthemum ester described in claim 1, its feature exists
In: the molecular weight of described gelatin is 10～150,000.
3. according to the preparation method of the mosquito incense liquid described in claim 1, it is characterised in that: preparation Cycas revoluta extract: weigh Cycas revoluta
Powder 50～100g is placed in container, adds 500～1000ml tap waters and disecoctylmaleate sodium sulfonate 1 ~ 3g,
At 110～130 DEG C, water-bath extraction 12～24h, obtains extract, and the filtrate that sucking filtration obtains is Cycas revoluta extract.
4. according to the preparation method of a kind of microcapsule mosquito incense liquid containing fluorine chlorine ether chrysanthemum ester described in claim 1, crosslinking curing
Agent is the one of aluminum sulfate, iron sulfate, aluminum chloride, sodium alginate.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114768697A (en) * | 2022-04-03 | 2022-07-22 | 湖州市食品药品检验研究院(湖州市药品和医疗器械不良反应监测中心、湖州市医疗器械监督检验中心、湖州市食品认证审评和粮油质量监测中心) | Preparation process and preparation device of cinnamon essential oil microcapsules |
| CN115633682A (en) * | 2022-09-27 | 2023-01-24 | 河北科技大学 | Mosquito-repelling microcapsule and preparation method thereof |
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| CN101554174A (en) * | 2009-05-14 | 2009-10-14 | 许春晖 | Novel insecticide for repelling and killing bugs |
| CN102232379A (en) * | 2010-05-06 | 2011-11-09 | 福建省金鹿日化股份有限公司 | Water-based electrothermal liquid mosquito-repellent incense and preparation method thereof |
| CN102579399A (en) * | 2012-03-20 | 2012-07-18 | 王全杰 | Preparation method of antibacterial Chinese mugwort oil microcapsules |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114768697A (en) * | 2022-04-03 | 2022-07-22 | 湖州市食品药品检验研究院(湖州市药品和医疗器械不良反应监测中心、湖州市医疗器械监督检验中心、湖州市食品认证审评和粮油质量监测中心) | Preparation process and preparation device of cinnamon essential oil microcapsules |
| CN115633682A (en) * | 2022-09-27 | 2023-01-24 | 河北科技大学 | Mosquito-repelling microcapsule and preparation method thereof |
| CN115633682B (en) * | 2022-09-27 | 2023-09-01 | 河北科技大学 | Mosquito-repellent microcapsule and preparation method thereof |
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