CN103340196A - Leaf alcohol microcapsule and preparation method thereof - Google Patents
Leaf alcohol microcapsule and preparation method thereof Download PDFInfo
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- CN103340196A CN103340196A CN2013102980156A CN201310298015A CN103340196A CN 103340196 A CN103340196 A CN 103340196A CN 2013102980156 A CN2013102980156 A CN 2013102980156A CN 201310298015 A CN201310298015 A CN 201310298015A CN 103340196 A CN103340196 A CN 103340196A
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Abstract
The invention discloses a leaf alcohol microcapsule and a preparation method thereof, which belong to the field of botanical pesticide preparations. The microcapsule takes leaf alcohol as a core material and gelatin-arabic gum as a wall material; a ratio (W/W) of the core material to the wall material is 1 to 1; the volume ratio of gelatin liquid to arabic gum liquid is 1 to 1. The preparation method comprises the following steps of: adding the arabic gum liquid and the gelatin liquid into an emulsified core material, namely leaf alcohol emulsion; under continuous stirring, adjusting the pH value of a mixed suspension to produce agglomeration; and after the liquid is agglomerated, continuously stirring, adding deionized water to dilute the liquid, transferring the liquid to a hot water bath, adding a glutaraldehyde solution for solidification, then adjusting the pH value, filtering a product, washing the product by deionized water until the aldehyde flavor is eliminated, pumping the deionized water out, and drying the product to obtain microcapsule powder. The leaf alcohol microcapsule taking the gelatin-arabic gum as the wall material is extremely high in slow release performance, simple in technology, easy in operation and high in reproducibility, needs mild reaction conditions, has an environment protection effect, provides material basis and technical insurance to research on botanical pesticides, and has good application prospect.
Description
Technical field
The invention belongs to the botanical pesticide formulation art, especially relating to a kind of is the leaf-alcohol microcapsules and preparation method thereof of wall material with the gelatin-gum arabic.
Background technology
Being on the rise of problems such as the insect cause ferociously again sticks up because the traditional chemical agricultural chemicals is extensive use of, pest resistance to insecticide and residue of pesticide, people more and more pay attention to researching and developing biogenic pesticide (coming from plant, animal, microorganism etc.), especially be object with the natural plant product, the research of seeking novel insecticide active substance receives much attention.
There are some researches show, plant volatile to insect not only have poisoning, avoid keep away, effect that food refusal, inhibition are grown, but also have insect sex pheromone and attracting action.Because plant volatile is volatile; there is not specific protective device; be difficult to bring into play its usefulness; and controlled release formulation of capsule provides a formulation very easily for its application; microcapsules technology is for the physical property of improving enveloped matter, and the aspect tools such as release of improve Stability of Substance, controlling material as required have great advantage.
Leaf-alcohol is present in leaf, essential oil and the fruit of many plants, has fresh leafiness fragrance, be colourless oil liquid or little yellow liquid, extension is strong, have special herbal and leaf smell after the dilution, it is gentle to distinguish the flavor of, and Li Peng etc. discover that leaf-alcohol has attracting action to poplar caterpillar adult and two chrysomelid adult of spot firefly, a situation arises can to utilize leaf-alcohol that the attracting action of insect is observed and predicted insect, also can be used as a measure of the insect comprehensive regulation.But because the leaf-alcohol volatility is stronger, make its application be subjected to great restriction, a kind of it is coated on preparation method in the microcapsules if work out, making leaf-alcohol see through semi-enclosed cyst wall slowly discharges, can keep its inherent characteristic, the stability of main component can prolong its active action time again.
Summary of the invention
The object of the present invention is to provide a kind of stability that can keep the leaf-alcohol main component, prolong drug effect, reduce its volatility, have leaf-alcohol microcapsules of slow releasing function and preparation method thereof.
Leaf-alcohol microcapsules of the present invention are core with the leaf-alcohol, and gelatin-gum arabic is the wall material, and the core wall is 1:1 than (W/W), and the volume ratio of gelatin solution and Arabic glue is 1:1, and the mass concentration of Arabic glue and gelatin solution is 1.0～3.0%.
The present invention prepares above-mentioned leaf-alcohol microcapsules according to following steps:
(1) respectively wall material gelatin and gum Arabic being made mass concentration with deionized water is 1.0～3.0% glue, and gelatin solution is regulated pH to 7～8 with sodium hydroxide solution, and is standby.
(2) get leaf-alcohol and add the Tween-80 quick emulsification, the core leaf-alcohol emulsion that emulsification is good under continuous stirring condition, adds Arabic glue and gelatin solution respectively, mixed glue solution is stirred 10～30 min under 40～60 ℃, and suspendible is even.
(3) under constantly stirring, regulate suspension pH value to 2.8～4.5 and namely produce cohesion, with the situation of microscopic examination cohesion encystation.30～90min is continued to stir in the cohesion back, add 40～60 ℃ with suspension with the dilution of the deionized water of volume, remove hot bath, make the temperature of micro-capsule suspension be down to room temperature after, in the dislocation ice bath, after treating that temperature is down to below 5～10 ℃, add an amount of glutaraldehyde solution, the volume ratio of control suspension, deionized water, glutaraldehyde is 100:100:1.6, solidifies 0.5～1h, regulate pH value to 8～10 then, continue to stir 2.5～3.5h.
(4) step (3) gained solution is filtered, spend deionised water to there not being the aldehyde flavor, drain, put drying below 70 ℃, get microscapsule powder.
Described step (1) mesospore material is gelatin and gum Arabic, and gelatin concentration is 2.0%, gum Arabic 2.0%.
Emulsifier is Tween-80 in the described step (2), and content is 2% of suspension volume; Core is leaf-alcohol, and the core wall is 1:1 than (W/W); Stirring revolution is 550～880 r/min, preferred 660 r/min; Whipping temp is 45 ℃.
Stirring revolution in the described step (3) is 550～880 r/min, preferred 660 r/min; Condense pH value of solution=3.4 again; Multiple aggregation times 50 min.
The present invention has the following advantages:
(1) be that the leaf-alcohol microcapsules of wall material have good sustained release performance with the gelatin-gum arabic;
(2) cyst material of microcapsules is natural macromolecular material, cheap and environmental sound;
(3) surperficial smoother, spherical independent completion, the microcapsules particle diameter is evenly distributed;
(4) technology of the present invention is simple, and the reaction condition gentleness is easy to operate, favorable reproducibility, and environmental friendliness for the development of botanical pesticide provides material base and technical guarantee, has a good application prospect;
(5) leaf-alcohol microcapsules of the present invention can be as the attractant of desinsection (poplar caterpillar adult and two chrysomelid adult of spot firefly).
Description of drawings
Fig. 1 is the leaf-alcohol microcapsules sem photograph that the present invention prepares;
Fig. 2 is the leaf-alcohol microcapsules particle diameter distribution map that the present invention prepares;
Fig. 3 is the leaf-alcohol microcapsules infrared spectrogram that the present invention prepares;
Fig. 4 is the leaf-alcohol microcapsules releasing effect curve that the present invention prepares.
Embodiment
Below in conjunction with accompanying drawing technical scheme of the present invention is further described; but do not limit to so; every technical solution of the present invention is made amendment or is equal to replacement, and do not break away from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
The leaf-alcohol microcapsules of present embodiment are core with the leaf-alcohol, and gelatin-gum arabic is the wall material, and the core wall is 1:1 than (W/W).Its preparation method is as follows:
(1) preparation of glue: respectively wall material gelatin and gum Arabic being made mass concentration with deionized water is 2.0% glue, and gelatin solution is regulated pH to 7～8 with 20% sodium hydroxide solution, and is standby.
(2) suspendible: getting the 2g leaf-alcohol, to add volumetric concentration be 50% Tween-80 4ml quick emulsification, the core leaf-alcohol emulsion that emulsification is good, be under the stirring condition of 660 r/min at revolution, add the Arabic glue of 50ml 2% and the gelatin solution of 50ml 2% respectively, under 45 ℃ mixed glue solution is stirred 15 min, suspendible is even.
(3) cohesion and solidify: be under the continuous stirring condition of 660 r/min at revolution, drip 10% acetic acid, regulate and namely produce cohesion, the situation of condensing encystation with microscopic examination about suspension pH value to 3.4.50min is continued to stir in the cohesion back, the deionized water 100ml dilution that adds 45 ℃, remove hot bath, after making the temperature of micro-capsule suspension be down to 25 ℃, in the dislocation ice bath, treat that temperature is down to below 10 ℃ after, add glutaraldehyde solution 1.6ml, solidify 0.5～1h, add 20% sodium hydroxide solution then to pH value about 9.0, continue to stir 3h.
(4) granulation, drying: step (3) gained solution is filtered, spend deionised water to there being the aldehyde flavor, drain, add appropriate amount of starch and make particle, put drying below 70 ℃, get microscapsule powder.
Leaf-alcohol essential oil microcapsules by the above-mentioned steps preparation mostly is regular sphere, surperficial smoother, and spherical independent completion, glutinous the company, embedding rate is 83.01 ± 2.67%, the microcapsules particle diameter concentrates on to be distributed in about 19 μ m (sees Fig. 1, Fig. 2).
As shown in Figure 3, in the curve of spectrum of gelatin-gum arabic drug-loading microcapsule, at 2966 cm
-1, 2914 cm
-1With 2853 cm
-1, 1671 cm
-1, 1441 cm
-1, 1376 cm
-1, 1002 cm
-1The characteristic spectrum that tangible core leaf-alcohol is arranged proves that synthetic gelatin-gum arabic microcapsules are coated with leaf-alcohol.
As can be seen from Figure 4, the rate of release of leaf-alcohol microcapsules will be starkly lower than the leaf-alcohol of not sealing.The former medicine of the leaf-alcohol of embedding not, the time that all is discharged in the medium is 4d, be that wall material prepared microcapsule is 11d by the time that bag filter all is discharged in the medium with the gelatin-gum arabic, illustrate that prepared is that the leaf-alcohol microcapsules of wall material have good sustained release performance with the gelatin-gum arabic.
In the present embodiment, the specific requirement of each raw material is as shown in table 1.
Table 1 experiment reagent
| Title | Specification | Sales company |
| Leaf-alcohol | Analyze pure | Analytic pure Aladdin |
| Gum Arabic tree powder | Viscosity cPa.s60.0～130.0 | Chemical Reagent Co., Ltd., Sinopharm Group |
| Gelatin | Type B | sigma |
Claims (10)
1. leaf-alcohol microcapsules, it is characterized in that described microcapsules are core with the leaf-alcohol, gelatin-gum arabic is the wall material, and the core wall is 1:1 than (W/W), the volume ratio of gelatin solution and Arabic glue is 1:1, and the mass concentration of Arabic glue and gelatin solution is 1.0～3.0%.
2. leaf-alcohol microcapsules according to claim 1 is characterized in that the mass concentration of described Arabic glue and gelatin solution is 2.0%.
3. the preparation method of the described leaf-alcohol microcapsules of claim 1 is characterized in that described method step is as follows:
(1) core leaf-alcohol emulsion that emulsification is good under continuous stirring condition, adds Arabic glue and gelatin solution respectively, mixed glue solution is stirred 10～30min under 40～60 ℃, and suspendible is even;
(2) under constantly stirring, regulate suspension pH value to 2.8～4.5 and namely produce cohesion, 30～90min is continued to stir in the cohesion back, add 40～60 ℃ with suspension with the dilution of the deionized water of volume, remove hot bath, after making the temperature of micro-capsule suspension be down to room temperature, in the dislocation ice bath, after treating that temperature is down to below 5～10 ℃, add an amount of glutaraldehyde solution, the volume ratio of control suspension, deionized water, glutaraldehyde is 100:100:1.6, solidifies 0.5～1h, regulate pH value to 8～10 then, continue to stir 2.5～3.5h;
(3) step (2) gained solution is filtered, spend deionised water to there not being the aldehyde flavor, drain, put drying below 70 ℃, get the described microscapsule powder of claim 1.
4. the preparation method of leaf-alcohol microcapsules according to claim 3 is characterized in that the mass concentration of described Arabic glue and gelatin solution is 1.0～3.0%.
5. the preparation method of leaf-alcohol microcapsules according to claim 3 is characterized in that the mass concentration of described Arabic glue and gelatin solution is 2.0%.
6. according to the preparation method of claim 3,4 or 5 described leaf-alcohol microcapsules, it is characterized in that pH=7～8 of described gelatin solution.
7. the preparation method of leaf-alcohol microcapsules according to claim 3 is characterized in that the stirring revolution of described step (1), (2) is 550～880r/min.
8. the preparation method of leaf-alcohol microcapsules according to claim 3, the stirring revolution that it is characterized in that described step (1) is 660r/min, whipping temp is 45 ℃.
9. the preparation method of leaf-alcohol microcapsules according to claim 3 is characterized in that stirring revolution in the described step (2) is 660r/min; Condense pH value of solution=3.4 again; Multiple aggregation time 50min.
10. the preparation method of leaf-alcohol microcapsules according to claim 3 is characterized in that in the described step (1), adds 4ml, volumetric concentration in the 2g leaf-alcohol and is 50% Tween-80 and carry out emulsification.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2013102980156A CN103340196A (en) | 2013-07-16 | 2013-07-16 | Leaf alcohol microcapsule and preparation method thereof |
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| CN2013102980156A CN103340196A (en) | 2013-07-16 | 2013-07-16 | Leaf alcohol microcapsule and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107802617A (en) * | 2017-12-12 | 2018-03-16 | 天津北洋百川生物技术有限公司 | A kind of β polymalic acids/hydroxypropyl methylcellulose microcapsules and its preparation method and application |
| CN110368373A (en) * | 2019-07-15 | 2019-10-25 | 湘南学院 | A kind of micro-capsule and the preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4906488A (en) * | 1987-05-01 | 1990-03-06 | Arcade, Inc. | Modification of permeant |
| CN101161068A (en) * | 2007-11-16 | 2008-04-16 | 济南大学 | An environmental friendly controlled sustained-release insecticide and method for preparing the same |
| CN102068947A (en) * | 2010-12-28 | 2011-05-25 | 上海工程技术大学 | Preparation method of N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide microcapsules |
-
2013
- 2013-07-16 CN CN2013102980156A patent/CN103340196A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4906488A (en) * | 1987-05-01 | 1990-03-06 | Arcade, Inc. | Modification of permeant |
| CN101161068A (en) * | 2007-11-16 | 2008-04-16 | 济南大学 | An environmental friendly controlled sustained-release insecticide and method for preparing the same |
| CN102068947A (en) * | 2010-12-28 | 2011-05-25 | 上海工程技术大学 | Preparation method of N-ethyl-2-isopropyl-5-methylcyclohexanecarboxamide microcapsules |
Non-Patent Citations (2)
| Title |
|---|
| 王丹等: "Morphology and release profile of microcapsules encapsulated alpha-pinene by complex coacervation", 《ADVANCED MATERIALS RESEARCH》 * |
| 闵洁等: "叶醇微胶囊成壳过程的研究", 《印染助剂》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107802617A (en) * | 2017-12-12 | 2018-03-16 | 天津北洋百川生物技术有限公司 | A kind of β polymalic acids/hydroxypropyl methylcellulose microcapsules and its preparation method and application |
| CN110368373A (en) * | 2019-07-15 | 2019-10-25 | 湘南学院 | A kind of micro-capsule and the preparation method and application thereof |
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Application publication date: 20131009 |