CN102091576A - Controlled-stirring-speed microcapsule preparation process - Google Patents
Controlled-stirring-speed microcapsule preparation process Download PDFInfo
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- CN102091576A CN102091576A CN2009102167215A CN200910216721A CN102091576A CN 102091576 A CN102091576 A CN 102091576A CN 2009102167215 A CN2009102167215 A CN 2009102167215A CN 200910216721 A CN200910216721 A CN 200910216721A CN 102091576 A CN102091576 A CN 102091576A
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Abstract
The invention discloses a controlled-stirring-speed microcapsule preparation process, which comprises the following steps: preparing wall material solution, emulsifying a core material, forming microcapsules, solidifying the microcapsules and drying the microcapsules. In the emulsifying process of the core material, the stirring speed is 700 to 900r/min, preferably 800r/min. In the invention, by controlling the stirring speed in the emulsifying process of the core material, the particle size percentage, embedding rate, mechanical strength and release rate of the microcapsules are improved, and consequently the overall performance of the microcapsules is improved.
Description
Technical field
The present invention relates to a kind of preparation technology, specifically be meant a kind of microcapsules preparation technology who controls mixing speed.
Background technology
The technical research of microcapsules probably starts from the thirties in last century, and being attended by the most momentous results is in the fifties.In the developing history process of microcapsules technology, the U.S. maintains the leading position to its research always, and Japan has also caught up with in 60～seventies gradually.China is starting late aspect the research microcapsules technology, but all has practical application and more deep research at aspects such as medicine, agricultural chemicals, cosmetics, food.The microcapsules particle diameter of initial preparation is called micron-sized microcapsules between 5～2000 microns.Along with the development of microcapsules technology, the particle diameter of the microcapsules of preparation can reach between 1～1000 nanometer less than 1 micron, often is called as Nano capsule.Along with the continuous progress of microcapsules technology, microcapsules will bring bigger benefit to the mankind.
Microcapsules are actually some little particles, and these little particles wrap the material that another kind is referred to as core by a kind of material that is referred to as the wall material and formed.On this basis, also have the microcapsules of some specific types, such as checking microcapsules, multiple wall microcapsules and occurring matrix type microcapsules etc.Enveloped is the two-phase of separating with cyst wall, and this is the feature of microcapsules.Microcapsules not only can the encapsulated solid powder, also can the enclosed liquid material.As adopting special preparation method, microcapsules can also be sealed gas.In addition.Hydrophobic material and water wetted material all can be encapsulated in the microcapsules.
The method that is used to prepare microcapsules is a lot, can divide diverse ways according to different standards, according to traditional sorting technique packing technology is divided into three kinds:
1, polymerisation method
During according to microencapsulation, the raw material difference of preparation shell material therefor, the difference of polymerization methods, the technology that the polymerisation legal system can be equipped with microcapsules is further divided into interfacial polymerization, situ aggregation method and suspension cross-linking method.Interfacial polymerization and situ aggregation method be with monomer as raw material, utilize synthesized polymer material to make the method for shell material.It is simple that these two kinds of methods have technology, and it is wide that shell material is selected, and can obtain to have the advantage of the shell material of multiple different performance.
(1) interfacial polymerization.Prepare in the technology of microcapsules at interfacial polymerization, capsule shell is that the polymerisation by two class monomers forms.The monomer of participating in polymerisation has two kinds at least, wherein must have two class monomers, and a class is oil-soluble monomer, and another kind of is water miscible monomer.They lay respectively at the inside and outside of core drop, and react on the surface of core drop, form thin polymer film.
(2) situ aggregation method.In position in the encapsulated process of polymerization, be not that reactive monomer is added to respectively in core drop and the suspension media, but monomer and initator all add decentralized photo or all add in the continuous phase, and promptly monomer component and catalyst are inside or the outsides that all is positioned at the core drop.In the microencapsulation system, monomer is soluble the single of microcapsules system in mutually, and polymer whole be insoluble in mutually, so polymerisation takes place on the surface of core drop.On the drop surface, polymerization single polymerization monomer produces low-molecular-weight relatively performed polymer, after this performed polymer size progressively increases, be deposited on the surface of core material, because constantly carrying out of crosslinked and polymerization, the final capsule shell that forms solid, the thin polymer film that is generated can cover all surfaces of core drop.
(3) suspension cross-linking method.Above-mentioned interfacial polymerization and situ aggregation method all are to be raw material with the monomer, and form shell membrane through polymerisation.And the suspension cross-linking method is different with above-mentioned two kinds of methods, and it is to be raw material with the polymer, promptly earlier the linear polymer dissolving is formed solution, and then, when linear polymer suspended crosslinking curing, capsule shells is separated out and formed to polymer precipitation rapidly.
2, phase separation method
The basic principle that phase separation method prepares microcapsules is to utilize the physicochemical properties of polymer, and the character that promptly is separated is so be called physical-chemical process again.Difference according to the preparation medium can be divided into phase separation method: aqueous phase separation method and oil-phase separating method.In the aqueous phase separation method,, can be further divided into complex coacervation and single coacervation according to the quantity of the polymer that is separated.
3, physics and Mechanical Method
This Microencapsulation Method mainly is the physical change by the microcapsule shell material, adopts certain mechanical processing tools to carry out microencapsulation.Mainly contain solvent evaporation or solution extraction, fusing dispersion condensation method, spray drying process, fluidized bed process and some other mechanical means.
Emulsification stirring speed is very big to microcapsules grain diameter influence in microcapsules preparation technology.Because established polymer has rigid structure, the microcapsules particle diameter is when initial, and its liquid-drop diameter generally can not shrink, and therefore the control of microcapsules particle diameter just is converted into the control of gained liquid-drop diameter when disperseing.This moment, mechanical dispersion cut much ice, and mechanical dispersion is effective, and particle size distribution is narrow.Because it is bigger that the particle diameter of microcapsules requires, so the mixing speed of emulsifying stage should not be too fast, and speed also makes system produce a large amount of foams soon, and the intensity of capsule is reduced; If mixing speed is too little, core can not be emulsified, and product embedding rate and release performance will be subjected to very big influence, even can not form capsule.
Summary of the invention
Purpose of the present invention is in order to overcome the deficiencies in the prior art and defective, a kind of microcapsules preparation technology who controls mixing speed is provided, this preparation technology is by the mixing speed in the control core emulsion process, thereby improved particle diameter percentage, embedding rate, mechanical strength and the release rate of microcapsules, and then improved the overall performance of microcapsules.
Purpose of the present invention is achieved through the following technical solutions: the microcapsules preparation technology of control mixing speed, comprise that preparation, the emulsification of core, the microcapsules of wall material solution form, microcapsules solidify and dry five steps of microcapsules, wherein:
(a) preparation of wall material solution: the wall material is put into distilled water soak swelling, the insulation of heating back is standby;
(b) emulsification of core: choose core, drip emulsifying agent again, mix with above-mentioned wall material solution vibration dissolving back then, puts in the water bath with thermostatic control and stir, and mixing speed is 700r/min～900r/min, forms emulsion, promptly gets emulsion;
(c) microcapsules form: step (b) gained mixed liquor is carried out mechanical agitation, in the process that constantly stirs, slowly drip 10% acetum, microcapsules liquid forms;
(d) microcapsules solidify: the microcapsules liquid that forms in the step (c) is not stopped to stir, stir the back and add curing agent, transfer its pH to 9.0 with 20%NaOH solution again, continue to stir, system slowly is increased to 50 ℃ from gelling temperature, leave standstill and treat the microcapsules sedimentation;
(e) microcapsules drying: after the microcapsules sedimentation fully, the supernatant that inclines filters then or dries, and microcapsules wash with distilled water, drain, and place the insulating box drying, promptly get product.
As preferred version of the present invention, mixing speed is 800r/min in the described step (b).
Wall material in the described step (a) is gelatin and Arabic gum.
Core in the described step (b) is an atoleine.
In sum, the invention has the beneficial effects as follows: by the mixing speed in the control core emulsion process, thereby improved particle diameter percentage, embedding rate, mechanical strength and the release rate of microcapsules, and then improved the overall performance of microcapsules.
The specific embodiment
Below in conjunction with embodiment, to the detailed description further of the present invention's do, but embodiments of the present invention are not limited thereto.
Embodiment:
The present invention relates to a kind of microcapsules preparation technology who controls mixing speed, comprise that preparation, the emulsification of core, the microcapsules of wall material solution form, microcapsules solidify and dry five steps of microcapsules, wherein:
(a) preparation of wall material solution: the wall material is put into distilled water soak swelling, the insulation of heating back is standby;
(b) emulsification of core: choose core, drip emulsifying agent again, mix with above-mentioned wall material solution vibration dissolving back then, puts in the water bath with thermostatic control and stir, and mixing speed is 700r/min～900r/min, forms emulsion, promptly gets emulsion;
(c) microcapsules form: step (b) gained mixed liquor is carried out mechanical agitation, in the process that constantly stirs, slowly drip 10% acetum, microcapsules liquid forms;
(d) microcapsules solidify: the microcapsules liquid that forms in the step (c) is not stopped to stir, stir the back and add curing agent, transfer its pH to 9.0 with 20%NaOH solution again, continue to stir, system slowly is increased to 50 ℃ from gelling temperature, leave standstill and treat the microcapsules sedimentation;
(e) microcapsules drying: after the microcapsules sedimentation fully, the supernatant that inclines filters then or dries, and microcapsules wash with distilled water, drain, and place the insulating box drying, promptly get product.
Wall material in the described step (a) is gelatin and Arabic gum.
Core in the described step (b) is an atoleine.
Because emulsification stirring speed is very big to microcapsules grain diameter influence in the step (b).Because established polymer has rigid structure, the microcapsules particle diameter is when initial, and its liquid-drop diameter generally can not shrink, and therefore the control of microcapsules particle diameter just is converted into the control of gained liquid-drop diameter when disperseing.This moment, mechanical dispersion cut much ice, and mechanical dispersion is effective, and particle size distribution is narrow.Because it is bigger that the particle diameter of microcapsules requires, so the mixing speed of emulsifying stage should not be too fast, and speed also makes system produce a large amount of foams soon, and the intensity of capsule is reduced; If mixing speed is too little, core can not be emulsified, and product embedding rate and release performance will be subjected to very big influence, even can not form capsule.In order to obtain best mixing speed, the present invention has carried out the influence experiment of different mixing speeds to microcapsules.
It is that 7 kinds of situations of 400r/min, 500r/min, 600r/min, 700r/min, 800r/min, 900r/min, 1000r/min are carried out the performance test of microcapsules that mixing speed has been chosen in this experiment respectively, and the result is as shown in the table:
| Emulsification rotating speed (r/min) | ?400 | 500 | 600 | 700 | 800 | 900 | 1000 |
| Particle diameter percentage (%) | ?72 | 74 | 75 | 78 | 80 | 76 | 72 |
| Embedding rate (%) | ?74 | 76 | 78 | 81 | 85 | 86 | 87 |
| Release rate (%) | ?92 | 90 | 89 | 88 | 87 | 86 | 85 |
As can be seen from the above table, at the emulsification rotating speed during at 800r/min, the microcapsules proportion maximum of target grain size.In emulsion process, the pressure that produces in sticky shearing power and the whipping process changes or relative viscosity changes the degree that is determining to smash drop, and along with emulsifying rate improves, shearing force also correspondingly increases, the degree of smashing of drop improves, and the microcapsule diameter of formation is also along with variation.
The embedding of microcapsules takes the lead in being increase tendency along with the increase of emulsifying rate, and when rotating speed increases to 800r/min, embedding rate tends towards stability.Reason may be emulsive rate when too low, and drop is gathered into bulk easily, is difficult to coat, and embedding rate is then low.When emulsive rate was big, core was emulsified into droplet, and the wall material can coat droplet well, and embedding rate remains unchanged substantially.
The release rate of microcapsules begins along with the emulsification rotating speed increases and reduces, and reason may be that emulsifying rate is little, and the drop of formation is big, and the wall material amount that single capsule is coated is big, and intensity also reduces.Release rate is minimum when 800r/min.When speed continues to increase, for a certain amount of core, improve emulsifying rate, the microcapsules number of formation is many, the cyst wall attenuation, intensity reduces, and release rate increases.
Take all factors into consideration above-mentioned factor, the mixing speed among the present invention in the core emulsion process is 700r/min～900r/min, and preferentially selects 800r/min for use, and this condition prepared microcapsule target grain size percentage maximum has higher embedding rate and mechanical strength.
Claims (4)
1. the microcapsules preparation technology of control mixing speed is characterized in that, comprises that preparation, the emulsification of core, the microcapsules of wall material solution form, microcapsules solidify and dry five steps of microcapsules, wherein:
(a) preparation of wall material solution: the wall material is put into distilled water soak swelling, the insulation of heating back is standby;
(b) emulsification of core: choose core, drip emulsifying agent again, mix with above-mentioned wall material solution vibration dissolving back then, puts in the water bath with thermostatic control and stir, and mixing speed is 700r/min～900r/min, forms emulsion, promptly gets emulsion;
(c) microcapsules form: step (b) gained mixed liquor is carried out mechanical agitation, in the process that constantly stirs, slowly drip 10% acetum, microcapsules liquid forms;
(d) microcapsules solidify: the microcapsules liquid that forms in the step (c) is not stopped to stir, stir the back and add curing agent, transfer its pH to 9.0 with 20%NaOH solution again, continue to stir, system slowly is increased to 50 ℃ from gelling temperature, leave standstill and treat the microcapsules sedimentation;
(e) microcapsules drying: after the microcapsules sedimentation fully, the supernatant that inclines filters then or dries, and microcapsules wash with distilled water, drain, and place the insulating box drying, promptly get product.
2. the microcapsules preparation technology of control mixing speed according to claim 1 is characterized in that, mixing speed is 800r/min in the described step (b).
3. the microcapsules preparation technology of control mixing speed according to claim 1 is characterized in that, the wall material in the described step (a) is gelatin and Arabic gum.
4. the microcapsules preparation technology of control mixing speed according to claim 1 is characterized in that, the core in the described step (b) is an atoleine.
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| CN2009102167215A CN102091576A (en) | 2009-12-14 | 2009-12-14 | Controlled-stirring-speed microcapsule preparation process |
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| CN2009102167215A CN102091576A (en) | 2009-12-14 | 2009-12-14 | Controlled-stirring-speed microcapsule preparation process |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105161681A (en) * | 2015-08-10 | 2015-12-16 | 湘潭大学 | Microencapsulated carbon-coated carbon fluoride cathode material and preparation method thereof |
| CN105688767A (en) * | 2016-03-08 | 2016-06-22 | 中山大学惠州研究院 | Preparation method of vanillin microcapsules |
| CN106054304A (en) * | 2016-08-19 | 2016-10-26 | 京东方科技集团股份有限公司 | Polarizing plate, manufacturing method thereof and corresponding device |
| CN109046194A (en) * | 2018-08-21 | 2018-12-21 | 武汉佰玛生物科技有限公司 | A kind of method that limonene emulsification prepares chitosan microball |
-
2009
- 2009-12-14 CN CN2009102167215A patent/CN102091576A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105161681A (en) * | 2015-08-10 | 2015-12-16 | 湘潭大学 | Microencapsulated carbon-coated carbon fluoride cathode material and preparation method thereof |
| CN105688767A (en) * | 2016-03-08 | 2016-06-22 | 中山大学惠州研究院 | Preparation method of vanillin microcapsules |
| CN105688767B (en) * | 2016-03-08 | 2018-04-06 | 中山大学惠州研究院 | A kind of preparation method of vanillic aldehyde microcapsules |
| CN106054304A (en) * | 2016-08-19 | 2016-10-26 | 京东方科技集团股份有限公司 | Polarizing plate, manufacturing method thereof and corresponding device |
| CN109046194A (en) * | 2018-08-21 | 2018-12-21 | 武汉佰玛生物科技有限公司 | A kind of method that limonene emulsification prepares chitosan microball |
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Application publication date: 20110615 |