CN105688767A - Preparation method of vanillin microcapsules - Google Patents
Preparation method of vanillin microcapsules Download PDFInfo
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- CN105688767A CN105688767A CN201610130064.2A CN201610130064A CN105688767A CN 105688767 A CN105688767 A CN 105688767A CN 201610130064 A CN201610130064 A CN 201610130064A CN 105688767 A CN105688767 A CN 105688767A
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- 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
- B01J13/04—Making microcapsules or microballoons by physical processes, e.g. drying, spraying
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Abstract
The invention discloses a preparation method of vanillin microcapsules. The method comprises steps as follows: chitosan is used as a wall material, acetic acid is added, and a chitosan-acetic acid solution is prepared; vanillin is used as a core material, and after ethanol is added for dissolution, an emulsifier is added for full dissolution; a pre-reaction emulsion is obtained through mixing, after high-speed shear homogenization, the pre-reaction emulsion passes through a formation limit type device under pressure, vanillin/chitosan micro emulsion droplets are prepared, a sodium lauryl sulfate aqueous solution is used as an emulsion droplet receiving solution, and the vanillin microcapsules are formed. Through representation, the vanillin microcapsules have good morphology and uniform particle distribution, microcapsules in different particle sizes can be prepared by changing the outlet size, and the pelletizing time for preparation of the vanillin microcapsules adopting a core-shell structure is shortened to a large extent. The obtained vanillin microcapsules in different particle sizes have great significance in matching with fabric in different pore diameters for textile aroma enhancement and in application of release effects caused by different particle sizes in fields of food, cosmetics, medicine and the like.
Description
Technical field
The present invention relates to perfume microcapsule technical field, specifically, the preparation method relating to a kind of vanillin microcapsule。
Background technology
Vanillin is a kind of solid spice with strong milk breath, at present at home and abroad food, medicine intermediate, and is widely used in daily cosmetics。But the defect that vanillin itself has: poorly water-soluble, and be exposed under air and light and easily lose its activity, its application in life is brought certain restriction and obstruction by high temperature resistance etc.。And vanillin many-side performance after vanillin micro encapsulation, will be greatly improved, largely increase its range of application。
By vanillin micro encapsulation, presently relevant research adopts the single wall material with certain inclusion effect that it is wrapped up mostly, such as Indulion cyclodextrin, chitosan, sodium alginate etc.。Wherein, relate to the research using chitosan to be wall material and frequently with aldehydes noxious substance it is solidified and could form shell-core structure after drying, consuming time long from emulsion to the formation shell-core structure time except aldehyde material is to the toxic effect of people in the method。
Summary of the invention
Present invention aim to overcome that the deficiency preparing vanillin microcapsule technology, it is provided that a kind of shortening balling-up time, and the vanillin microcapsule granule even particle size distribution obtained, pattern is good
The preparation method of vanillin microcapsule。
To achieve these goals, the present invention adopts the following technical scheme that
The preparation method of a kind of vanillin microcapsule, including with chitosan for wall material, adding acetic acid, prepare chitosan-acetic acid solution；With vanillin for core, after adding ethanol dissolving, add emulsifying agent and fully dissolve；Merge and obtain pre-reaction emulsion, after high speed shear homogenizing, pre-reaction emulsion is prepared vanillin/chitosan microemulsion by shaping restricted type device under elevated pressure and drip, accept liquid by lauryl sodium sulfate aqueous solution as emulsion droplet, form vanillin microcapsule。
As preferably, in the preparation method of above-mentioned vanillin microcapsule, described vanillin/chitosan microemulsion drips, and first adopts electric field dispersion, enters back in lauryl sodium sulfate aqueous solution。
As preferably, in the preparation method of above-mentioned vanillin microcapsule, described restricted type device refers to discharge tank, and the bottom of discharge tank is provided with the outlet of adjustable dimension。
As preferably, in the preparation method of above-mentioned vanillin microcapsule, the mass ratio of described wall material and core is 1:1 ~ 4:1, and wall material and core total mass concentration are 1.2%-3.0%。
As preferably, in the preparation method of above-mentioned vanillin microcapsule, described emulsifying agent is the mixture of span80 and tween80, and both mass ratioes are 5:2。
As preferably, in the preparation method of above-mentioned vanillin microcapsule, described pre-reaction emulsion high speed shear homogenizing time is 5min ~ 15min。
As preferably, in the preparation method of above-mentioned vanillin microcapsule, pre-reaction emulsion is regulated pH and 5.5 prepares vanillin/chitosan microemulsion drip by shaping restricted type device under elevated pressure again。
As preferably, in the preparation method of above-mentioned vanillin microcapsule, the wall material chitosan adopted is deacetylation >=95%, and viscosity is 100-200mpa.s, without the chitosan of degradation treatment；The grade of vanillin is AR, purity > 95%。
Compared with prior art, there is advantages that core innovative point of the present invention is in that to adopt a kind of nontoxic anionic as the conjugate with chitosan/vanillin microcapsule emulsion droplet, this material biological degradability > 90%, there is the foaming power of decontamination, emulsifying and excellence, as emulsifying agent, extinguishing chemical, foaming agent and textile auxiliary, also serve as the foaming agent of toothpaste and paste, powdery, shampoo。When the vanillin emulsion droplet formed is dropped in the aqueous solution of sodium lauryl sulphate at once to be formed the vanillin microcapsule of shell-core structure, substantially reducing balling-up time and the vanillin microcapsule granule even particle size distribution obtained, pattern is good。
Accompanying drawing illustrates:
Fig. 1 is restricted type apparatus structure schematic diagram；
Fig. 2 is microscope figure (left side) and the grain size distribution (right side) of embodiment 1 vanillin microcapsule；
Fig. 3 is the microscope figure of embodiment 2 vanillin microcapsule；
Fig. 4 is the microscope figure of embodiment 3 vanillin microcapsule；
Fig. 5 is the microscope figure of embodiment 4 vanillin microcapsule；
Fig. 6 is the microscope figure of embodiment 5 vanillin microcapsule；
Fig. 7 is the microscope figure of embodiment 6 vanillin microcapsule；
Fig. 8 is the microscope figure of embodiment 7 vanillin microcapsule。
Detailed description of the invention:
Below in conjunction with embodiment, the present invention is described further, but protection scope of the present invention is not limited to the scope that embodiment represents。
Embodiment 1:
Being 1.5% mass percent according to wall core total concentration, wall core mass ratio is 2:1, takes 7ml acetic acid and joins in 1g chitosan, adds 100ml distilled water simultaneously and is placed in water bath with thermostatic control magnetic agitation pot, stir 1h at 55 DEG C in chitosan-acetic acid solution。Take 0.5g vanillin, it is charged with 1g ethanol, dissolving, until vanillin, the mass ratio adding 1.0% emulsifying agent span80 and tween80(emulsifying agent span80 and tween80 after fully is 5:2), to be emulsified dose dissolves after fully with vanillin, sufficient chitosan-acetic acid solution is dissolved before adding, by system pH regulator to 5.5 after 5 minutes high speed shear homogenizing, take the sodium lauryl sulphate of 1.0% simultaneously and be dissolved in distilled water。The emulsion prepared is made to prepare vanillin/chitosan microemulsion and drip exporting (outlet size is 120 μm) by restricting type device, accept liquid by the lauryl sodium sulfate aqueous solution prepared as emulsion droplet, at once form vanillin microcapsule when the emulsion droplet formed divides to be spread to accept in liquid。Through follow-up dried, after vanillin microcapsule broken wall treatment, calculating vanillin embedding rate through gas chromatographic analysis is 60.96%。The structure of restricted type device is as it is shown in figure 1, include the outlet 2 of discharge tank 1 and adjustable dimension。1 is discharge tank；2 is the outlet of adjustable dimension；3 is extra electric field；4 for accepting liquid。
Gained vanillin microcapsule see Fig. 2 Stereo microscope figure (left side) and grain size distribution (right side), gained microemulsion system particle diameter volume distributed median scope is at about 209.73 μm。
Embodiment 2:
Being 1.5% mass percent according to wall core total concentration, wall core mass ratio is 3:1, takes 8ml acetic acid and joins in 1.13g chitosan, adds 100ml distilled water simultaneously and is placed in water bath with thermostatic control magnetic agitation pot, stir 1h at 55 DEG C in chitosan-acetic acid solution。Take 0.38g vanillin, it is charged with 0.76g ethanol, dissolving, until vanillin, the mass ratio adding 1.0% emulsifying agent span80 and tween80(emulsifying agent span80 and tween80 after fully is 5:2), to be emulsified dose dissolves after fully with vanillin, sufficient chitosan-acetic acid solution is dissolved before adding, by system pH regulator to 5.5 after 5 minutes high speed shear homogenizing, take 1.0% sodium lauryl sulphate simultaneously and be dissolved in distilled water。Make the emulsion prepared prepare vanillin/chitosan microemulsion by restricting type device outlet (outlet size is 100 μm) to drip, accept liquid by the lauryl sodium sulfate aqueous solution prepared as emulsion droplet, at once form vanillin microcapsule when the emulsion droplet formed divides to be spread to accept in liquid。Through follow-up dried, after vanillin microcapsule broken wall treatment, calculating vanillin embedding rate through gas chromatographic analysis is 50.93%。
Gained vanillin microcapsule is shown in microscope figure (3)。
Embodiment 3:
Being 1.5% mass percent according to wall core total concentration, wall core mass ratio is 2:1, takes 7ml acetic acid and joins in 1g chitosan, adds 100ml distilled water simultaneously and is placed in water bath with thermostatic control magnetic agitation pot, stir 1h at 55 DEG C in chitosan-acetic acid solution。Take 0.5g vanillin, it is charged with 1g ethanol, dissolving, until vanillin, the mass ratio adding 1.0% emulsifying agent span80 and tween80(emulsifying agent span80 and tween80 after fully is 5:2), to be emulsified dose dissolves after fully with vanillin, sufficient chitosan-acetic acid solution is dissolved before adding, by system pH regulator to 5.5 after 5 minutes high speed shear homogenizing, take 1.0% sodium lauryl sulphate simultaneously and be dissolved in distilled water。Make the emulsion prepared prepare vanillin/chitosan microemulsion by restricting type device outlet (outlet size is 150 μm) to drip, accept liquid by the lauryl sodium sulfate aqueous solution prepared as emulsion droplet, at once form vanillin microcapsule when the emulsion droplet formed divides to be spread to accept in liquid。Through follow-up dried, after vanillin microcapsule broken wall treatment, calculating vanillin embedding rate through gas chromatographic analysis is 59.73%。
Gained vanillin microcapsule is shown in microscope figure (4)。
Embodiment 4:
Being 1.5% according to wall core total concentration, wall core ratio is for 2:1, and taking 7ml acetic acid joins in 1g chitosan, adds 100ml distilled water simultaneously and is placed in water bath with thermostatic control magnetic agitation pot, stir 1h at 55 DEG C in chitosan-acetic acid solution。Take 0.5g vanillin, it is charged with 1g ethanol, dissolving, until vanillin, the mass ratio adding 1.0% emulsifying agent span80 and tween80(emulsifying agent span80 and tween80 after fully is 5:2), to be emulsified dose dissolves after fully with vanillin, sufficient chitosan-acetic acid solution is dissolved before adding, by system pH regulator to 5.5 after 5 minutes high speed shear homogenizing, take 1.0% sodium lauryl sulphate simultaneously and be dissolved in distilled water。Make the emulsion prepared prepare vanillin/chitosan microemulsion by shaping restricted type device outlet (outlet size is 300 μm) under pressure to drip, accept liquid by the lauryl sodium sulfate aqueous solution prepared as emulsion droplet, at once form vanillin microcapsule when the emulsion droplet formed divides to be spread to accept in liquid。Through follow-up dried, after vanillin microcapsule broken wall treatment, calculating vanillin embedding rate through gas chromatographic analysis is 52.22%。
Gained vanillin microcapsule is shown in microscope figure (5)。
Embodiment 5:
Being 1.5% according to wall core total concentration, wall core ratio is for 2:1, and taking 7ml acetic acid joins in 1g chitosan, adds 100ml distilled water simultaneously and is placed in water bath with thermostatic control magnetic agitation pot, stir 1h at 55 DEG C in chitosan-acetic acid solution。Take 0.5g vanillin, it is charged with 1g ethanol, dissolving, until vanillin, the mass ratio adding 1.0% emulsifying agent span80 and tween80(emulsifying agent span80 and tween80 after fully is 5:2), to be emulsified dose dissolves after fully with vanillin, sufficient chitosan-acetic acid solution is dissolved before adding, by system pH regulator to 5.5 after 5 minutes high speed shear homogenizing, take 1.0% sodium lauryl sulphate simultaneously and be dissolved in distilled water。Make the emulsion prepared prepare vanillin/chitosan microemulsion by shaping restricted type device outlet (outlet size is 450 μm) under pressure to drip, accept liquid by the lauryl sodium sulfate aqueous solution prepared as emulsion droplet, at once form vanillin microcapsule when the emulsion droplet formed divides to be spread to accept in liquid。Through follow-up dried, after vanillin microcapsule broken wall treatment, calculating vanillin embedding rate through gas chromatographic analysis is 49.93%。
Gained vanillin microcapsule is shown in microscope figure (6)。
Embodiment 6:
Being 1.5% according to wall core total concentration, wall core ratio is for 2:1, and taking 7ml acetic acid joins in 1g chitosan, adds 100ml distilled water simultaneously and is placed in water bath with thermostatic control magnetic agitation pot, stir 1h at 55 DEG C in chitosan-acetic acid solution。Take 0.5g vanillin, it is charged with 1g ethanol, dissolving, until vanillin, the mass ratio adding 1.0% emulsifying agent span80 and tween80(emulsifying agent span80 and tween80 after fully is 5:2), to be emulsified dose dissolves after fully with vanillin, sufficient chitosan-acetic acid solution is dissolved before adding, by system pH regulator to 5.5 after 5 minutes high speed shear homogenizing, take 1.0% sodium lauryl sulphate simultaneously and be dissolved in distilled water。Make the emulsion prepared prepare vanillin/chitosan microemulsion by shaping restricted type device outlet (being of a size of 750 μm) under pressure to drip, accept liquid by the lauryl sodium sulfate aqueous solution prepared as emulsion droplet, at once form vanillin microcapsule when the emulsion droplet formed divides to be spread to accept in liquid。Through follow-up dried, after vanillin microcapsule broken wall treatment, calculating vanillin embedding rate through gas chromatographic analysis is 45.48%。
Gained vanillin microcapsule is shown in microscope figure (7)。
Embodiment 7:
Being 1.5% according to wall core total concentration, wall core ratio is for 2:1, and taking 7ml acetic acid joins in 1g chitosan, adds 100ml distilled water simultaneously and is placed in water bath with thermostatic control magnetic agitation pot, stir 1h at 55 DEG C in chitosan-acetic acid solution。Take 0.5g vanillin, it is charged with 1g ethanol, dissolving, until vanillin, the mass ratio adding 1.0% emulsifying agent span80 and tween80(emulsifying agent span80 and tween80 after fully is 5:2), to be emulsified dose dissolves after fully with vanillin, sufficient chitosan-acetic acid solution is dissolved before adding, by system pH regulator to 5.5 after 5 minutes high speed shear homogenizing, take 1.0% sodium lauryl sulphate simultaneously and be dissolved in distilled water。Make the emulsion prepared prepare vanillin/chitosan microemulsion by shaping restricted type device outlet (being of a size of 1000 μm) under pressure to drip, accept liquid by the lauryl sodium sulfate aqueous solution prepared as emulsion droplet, at once form vanillin microcapsule when the emulsion droplet formed divides to be spread to accept in liquid。Through follow-up dried, after vanillin microcapsule broken wall treatment, calculating vanillin embedding rate through gas chromatographic analysis is 44.10%。
Gained vanillin microcapsule is shown in microscope figure (8)。
Claims (8)
1. a preparation method for vanillin microcapsule, including with chitosan for wall material, adding acetic acid, prepare chitosan-acetic acid solution；With vanillin for core, after adding ethanol dissolving, add emulsifying agent and fully dissolve；Merge and obtain pre-reaction emulsion, after high speed shear homogenizing, pre-reaction emulsion is prepared vanillin/chitosan microemulsion by shaping restricted type device under elevated pressure and drip, accept liquid by lauryl sodium sulfate aqueous solution as emulsion droplet, form vanillin microcapsule。
2. the preparation method of vanillin microcapsule as claimed in claim 1, it is characterised in that described vanillin/chitosan microemulsion drips, first adopts electric field dispersion, enters back in lauryl sodium sulfate aqueous solution。
3. the preparation method of vanillin microcapsule as claimed in claim 1, it is characterised in that described restricted type device refers to discharge tank, and the bottom of discharge tank is provided with the outlet of adjustable dimension。
4. the preparation method of vanillin microcapsule as claimed in claim 1, it is characterised in that the mass ratio of described wall material and core is 1:1 ~ 4:1, and wall material and core total mass concentration are 1.2%-3.0%。
5. the preparation method of vanillin microcapsule as claimed in claim 1, it is characterised in that described emulsifying agent is the mixture of span80 and tween80, and both mass ratioes are 5:2。
6. the preparation method of vanillin microcapsule as claimed in claim 1, it is characterised in that described pre-reaction emulsion high speed shear homogenizing time is 5min ~ 15min。
7. the preparation method of vanillin microcapsule as claimed in claim 1, it is characterised in that pre-reaction emulsion is regulated pH and 5.5 prepares vanillin/chitosan microemulsion by shaping restricted type device under elevated pressure again and drip。
8. the preparation method of vanillin microcapsule as claimed in claim 1, it is characterised in that the wall material chitosan adopted is deacetylation >=95%, and viscosity is 100-200mpa.s, without the chitosan of degradation treatment；The grade of vanillin is AR, purity > 95%。
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Cited By (6)
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| CN106179144A (en) * | 2016-07-11 | 2016-12-07 | 中山大学惠州研究院 | A kind of controlled method preparing vanillin microcapsule emulsion |
| CN106955651A (en) * | 2017-03-10 | 2017-07-18 | 佛山市禅香新材料有限公司 | A kind of microfluidic control for vanillic aldehyde microcapsules drop method |
| CN107021821A (en) * | 2017-04-27 | 2017-08-08 | 陕西科技大学 | Micro- fertilizer of a kind of antifreeze multielement slow-release of humic acid capsule structure nutrition and preparation method thereof |
| CN107558260A (en) * | 2017-09-01 | 2018-01-09 | 南通香佳纺织科技有限公司 | A kind of rose scent microcapsules printing assistant and preparation method thereof |
| CN111604081A (en) * | 2020-06-22 | 2020-09-01 | 中山大学 | Method for quasi-continuous synthesis of monatomic catalyst |
| CN113698509A (en) * | 2021-04-01 | 2021-11-26 | 重庆科技学院 | Method for preparing ethyl vanillin carboxymethyl chitosan embedded paclitaxel nanoparticles |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106179144A (en) * | 2016-07-11 | 2016-12-07 | 中山大学惠州研究院 | A kind of controlled method preparing vanillin microcapsule emulsion |
| CN106955651A (en) * | 2017-03-10 | 2017-07-18 | 佛山市禅香新材料有限公司 | A kind of microfluidic control for vanillic aldehyde microcapsules drop method |
| CN107021821A (en) * | 2017-04-27 | 2017-08-08 | 陕西科技大学 | Micro- fertilizer of a kind of antifreeze multielement slow-release of humic acid capsule structure nutrition and preparation method thereof |
| CN107558260A (en) * | 2017-09-01 | 2018-01-09 | 南通香佳纺织科技有限公司 | A kind of rose scent microcapsules printing assistant and preparation method thereof |
| CN111604081A (en) * | 2020-06-22 | 2020-09-01 | 中山大学 | Method for quasi-continuous synthesis of monatomic catalyst |
| CN111604081B (en) * | 2020-06-22 | 2021-06-25 | 中山大学 | Method for quasi-continuous synthesis of monatomic catalyst |
| CN113698509A (en) * | 2021-04-01 | 2021-11-26 | 重庆科技学院 | Method for preparing ethyl vanillin carboxymethyl chitosan embedded paclitaxel nanoparticles |
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