CN103598178A - Preparation method of insect-protected starch slow release microspheres - Google Patents
Preparation method of insect-protected starch slow release microspheres Download PDFInfo
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- CN103598178A CN103598178A CN201310513460.XA CN201310513460A CN103598178A CN 103598178 A CN103598178 A CN 103598178A CN 201310513460 A CN201310513460 A CN 201310513460A CN 103598178 A CN103598178 A CN 103598178A
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Abstract
The invention relates to a preparation method of insect-protected starch slow release microspheres. The method comprises the following steps: processing soluble starch and a NaOH solution to prepare a homogeneous solution; adding Span-80 to cyclohexane, and carrying out heating stirring for full dissolving; adding epichlorohydrin to the homogeneous starch solution, and adding the obtained Span-80 solution to obtain starch microspheres; and adding the starch microspheres to a camphor essential oil solution, carrying out shaking and ultrasonic treatment for 2h, carrying out suction filtration, washing, and carrying out cold drying to obtain the insect-protected starch slow release microspheres. The insect-protected starch slow release microspheres have the following advantages: 1, the organic natural insect removing and inhibiting substance camphor essential oil is adsorbed in the starch microspheres, so the fragrance of camphor is slowly released, thereby long-term insect removal and bacterium inhibition effects are realized; 2, the adsorption performance is good; and 3, the camphor essential oil exists in the starch microspheres as a solid, so the deterioration is difficult.
Description
Technical field
The present invention relates to the preparation of a kind of insect protected, mothproof slow-release material, especially a kind of preparation method of insect protected starch sustained-release micro-spheres, for the insect protected of microenvironment, mothproofly have a better effects, can be used as insect protected, the mothproof reagent of certain space, relatively airtight environment.
Background technology
In recent years, synthesizing biological degradable macromolecular material comes into one's own day by day as the research of sustained-release preparation.Macromolecular material can be divided into non-biodegradation type and biodegradation type.Compare the release request of the more stable and applicable unstable material of Biodegradable system rate of release with nondegradable polymer release-control system.The advantages such as spherex has in numerous controlled release preparations that unique biological degradability, biocompatibility, degradation speed are adjustable, nontoxic, non-immunogenicity, stable storage, source are sufficient and cheap.Spherex becomes the focus and emphasis of people's research and development gradually.
Natural camphor essential oil is formed through steam distillation by the lignum cinnamomi camphorae matter part of Lauraceae, the pure and fresh nose that slightly rushes, the breath of band camphor, there is pain relieving, antibacterial, desinsection, repelling mosquitoes and preventing insects mosquito, sterilizing and itch-relieving, except the effect such as purifying air, be a kind of desirable antibacterial, pest repellant, for common insect, there is good dispel effect.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of insect protected starch sustained-release micro-spheres, organic natural insect-repelling antibacterial substance camphor essential oil is adsorbed in spherex, camphor fragrance slowly-releasing is discharged, reach long-term deinsectization, fungistatic effect.
The present invention solves the technical scheme that its technical problem adopts: adopt following steps:
1) the soluble starch 2-3 part of getting oven dry by mass fraction joins in the NaOH solution that 20 parts of concentration are 2mol/L, it is dissolved and form homogeneous phase solution;
2) by mass fraction, get 1-3 part sorbitol anhydride oleate, join in 100 parts of cyclohexanes, be heated to 50-70, ℃ stirring is also fully dissolved;
3) by mass fraction, get 1.8-2.3 part epoxychloropropane and add in step 1) gained solution, stir, reaction 5-7 hour;
4) by step 2) gained solution joins in the system of step 3), after question response finishes, standing, removes oil phase, washes away oil stain, then use absolute ethyl alcohol and acetone cyclic washing several times with ethyl acetate, dry, obtains spherex;
5) by mass fraction, getting percent by volume is natural camphor essential oil ethanolic solution 0.4-0.6 part of 80%, with absolute ethyl alcohol, is diluted to 10 parts, then in camphor spirit oil solution, adds the dry spherex of 0.1-0.3 part, concussion ultrasonic 2h;
6) suction filtration, and with absolute ethanol washing, cold wind dries up, and finally obtains insect protected starch sustained-release micro-spheres.
Inventing useful effect is: 1) take soluble starch as raw material, epoxychloropropane is crosslinking agent, adopts anti-phase outstanding newborn method synthetic starch microballoon, natural camphor essential oil is adsorbed in degradable starch microballoon again, is prepared into camphor sustained-release micro-spheres, method is simple, easy and simple to handle, pollution-free.Utilize the sustained-release micro-spheres that the inventive method makes to have larger specific surface area; being beneficial to fragrance discharges rapidly and uniformly; spherex can extend the emissioning time of fragrance; there is excellent slow release effect; can make camphor content in microenvironment maintain for a long time certain value, to reach good expelling parasite, antibacterial, the effect that purifies air, be beneficial to long-term the depositing of article; the field such as can be used for that ordinary clothing is deposited, historical relic's protection, book and file keeping are deposited, has the advantages such as anthelminthic effect is good, easy to use.2) prepared spherex uniform particle diameter, 10 microns of average grain diameters, specific surface area is large, and absorption property is good, and adsorbing capacity reaches 0.8g/g.3) camphor essential oil is present in spherex with solid-state form, not perishable.
Embodiment
Below the invention will be further described:
Embodiment 1: a kind of preparation method of insect protected starch sustained-release micro-spheres, comprises the following steps:
1) by mass fraction, get the soluble starch (C of oven dry
12h
22o
11, relative molecular weight 342.30) 2 parts join in the NaOH solution that 20 parts of concentration are 2mol/L, it is dissolved and forms homogeneous phase solution;
2) by mass fraction, get 1 part of sorbitol anhydride oleate (Span-80), join in 100 parts of cyclohexanes, be heated to 50 ℃, stir and fully dissolve;
3) by mass fraction, get 1.8 parts of epoxychloropropane, slowly add in step 1) gained solution, stir, react 5 hours;
4) by step 2) gained solution joins in the system of step 3), after question response finishes, standing, removes oil phase, washes away oil stain, then use absolute ethyl alcohol and acetone cyclic washing with ethyl acetate, dry, obtains spherex;
5) by mass fraction, getting percent by volume is 0.4 part of 80% natural camphor essential oil ethanolic solution, with absolute ethyl alcohol, is diluted to 10 parts, then in camphor spirit oil solution, adds 0.1 part of dry spherex, concussion ultrasonic 2h;
6) suction filtration, and with absolute ethanol washing, cold wind dries up, and finally obtains insect protected starch sustained-release micro-spheres.
Embodiment 2: a kind of preparation method of insect protected starch sustained-release micro-spheres, comprises the following steps:
1) by mass fraction, get the soluble starch (C of oven dry
12h
22o
11, relative molecular weight 342.30) 3 parts join in the NaOH solution that 20 parts of concentration are 2mol/L, it is dissolved and forms homogeneous phase solution;
2) by mass fraction, get 3 parts of sorbitol anhydride oleates (Span-80), join in 100 parts of cyclohexanes, be heated to 70 ℃, stir and fully dissolve;
3) by mass fraction, get 2.3 parts of epoxychloropropane, slowly add in step 1) gained solution, stir, react 7 hours;
4) by step 2) gained solution joins in the system of step 3), after question response finishes, standing, removes oil phase, washes away oil stain, then use absolute ethyl alcohol and acetone cyclic washing with ethyl acetate, dry, obtains spherex;
5) by mass fraction, getting percent by volume is 0.6 part of 80% natural camphor essential oil ethanolic solution, with absolute ethyl alcohol, is diluted to 10 parts, then in camphor spirit oil solution, adds 0.3 part of dry spherex, concussion ultrasonic 2h;
6) suction filtration, and with absolute ethanol washing, cold wind dries up, and finally obtains insect protected starch sustained-release micro-spheres.
Embodiment 3: a kind of preparation method of insect protected starch sustained-release micro-spheres, comprises the following steps:
1) by mass fraction, get the soluble starch (C of oven dry
12h
22o
11, relative molecular weight 342.30) 2.5 parts join in the NaOH solution that 20 parts of concentration are 2mol/L, it is dissolved and forms homogeneous phase solution;
2) by mass fraction, get 2 parts of sorbitol anhydride oleates (Span-80), join in 100 parts of cyclohexanes, be heated to 60 ℃, stir and fully dissolve;
3) by mass fraction, get 2.1 parts of epoxychloropropane, slowly add in step 1) gained solution, stir, react 6 hours;
4) by step 2) gained solution joins in the system of step 3), after question response finishes, standing, removes oil phase, washes away oil stain, then use absolute ethyl alcohol and acetone cyclic washing with ethyl acetate, dry, obtains spherex;
5) by mass fraction, getting percent by volume is 0.5 part of 80% natural camphor essential oil ethanolic solution, with absolute ethyl alcohol, is diluted to 10 parts, then in camphor spirit oil solution, adds 0.2 part of dry spherex, concussion ultrasonic 2h;
6) suction filtration, and with absolute ethanol washing, cold wind dries up, and finally obtains insect protected starch sustained-release micro-spheres.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (1)
1. a preparation method for insect protected starch sustained-release micro-spheres, is characterized in that adopting following steps:
1) the soluble starch 2-3 part of getting oven dry by mass fraction joins in the NaOH solution that 20 parts of concentration are 2mol/L, it is dissolved and form homogeneous phase solution;
2) by mass fraction, get 1-3 part sorbitol anhydride oleate, join in 100 parts of cyclohexanes, be heated to 50-70, ℃ stirring is also fully dissolved;
3) by mass fraction, get 1.8-2.3 part epoxychloropropane and add in step 1) gained solution, stir, reaction 5-7 hour;
4) by step 2) gained solution joins in the system of step 3), after question response finishes, standing, removes oil phase, washes away oil stain, then use absolute ethyl alcohol and acetone cyclic washing several times with ethyl acetate, dry, obtains spherex;
5) by mass fraction, getting percent by volume is natural camphor essential oil ethanolic solution 0.4-0.6 part of 80%, with absolute ethyl alcohol, is diluted to 10 parts, then in camphor spirit oil solution, adds the dry spherex of 0.1-0.3 part, concussion ultrasonic 2h;
6) suction filtration, and with absolute ethanol washing, cold wind dries up, and finally obtains insect protected starch sustained-release micro-spheres.
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| CN201310513460.XA CN103598178A (en) | 2013-10-25 | 2013-10-25 | Preparation method of insect-protected starch slow release microspheres |
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| CN201310513460.XA CN103598178A (en) | 2013-10-25 | 2013-10-25 | Preparation method of insect-protected starch slow release microspheres |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104130066A (en) * | 2014-08-06 | 2014-11-05 | 成都新柯力化工科技有限公司 | Starch microsphere slow-release fertilizer and preparation method and application thereof |
| CN109608698A (en) * | 2018-12-24 | 2019-04-12 | 宁波酷尔塑料科技有限公司 | Preparation method, composite material and preparation method and the application of modified pest repellant |
| CN110665049A (en) * | 2019-10-25 | 2020-01-10 | 石家庄亿生堂医用品有限公司 | Method for preparing hemostatic starch microspheres by ultrasonic |
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| CN1805784A (en) * | 2003-05-11 | 2006-07-19 | 内盖夫研发局属本古里昂大学 | Encapsulated essential oils |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104130066A (en) * | 2014-08-06 | 2014-11-05 | 成都新柯力化工科技有限公司 | Starch microsphere slow-release fertilizer and preparation method and application thereof |
| CN104130066B (en) * | 2014-08-06 | 2016-03-02 | 成都新柯力化工科技有限公司 | A kind of spherex slow release fertilizer and its preparation method and application |
| CN109608698A (en) * | 2018-12-24 | 2019-04-12 | 宁波酷尔塑料科技有限公司 | Preparation method, composite material and preparation method and the application of modified pest repellant |
| CN110665049A (en) * | 2019-10-25 | 2020-01-10 | 石家庄亿生堂医用品有限公司 | Method for preparing hemostatic starch microspheres by ultrasonic |
| CN110665049B (en) * | 2019-10-25 | 2022-02-01 | 石家庄亿生堂医用品有限公司 | Method for preparing hemostatic starch microspheres by ultrasonic |
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Application publication date: 20140226 |