CN102091577A - Microcapsule preparation process capable of controlling core material to core wall ratio - Google Patents
Microcapsule preparation process capable of controlling core material to core wall ratio Download PDFInfo
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- CN102091577A CN102091577A CN2009102167234A CN200910216723A CN102091577A CN 102091577 A CN102091577 A CN 102091577A CN 2009102167234 A CN2009102167234 A CN 2009102167234A CN 200910216723 A CN200910216723 A CN 200910216723A CN 102091577 A CN102091577 A CN 102091577A
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Abstract
The invention discloses a microcapsule preparation process capable of controlling a core material to a core wall ratio, 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 core material to core wall ratio ranges from 2:1 to 5:1, and the core material with a core material to core wall ratio of 4:1 is preferred. In the invention, by controlling the core material to core wall ratio, the particle size percentage, embedding rate and releasing 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 core core wall ratio.
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.
The performance of the core core wall comparison microcapsules in microcapsules preparation technology has very big influence.For some occasions, as coating dyestuff, wish that core can be coated in the wall material for a long time, the compactness of microcapsules is had relatively high expectations, so just should reduce core wall rate of charge, core is as far as possible fully coated; And other occasions as coating medicine, essence, wish that then microcapsules have slow-release function, at this moment just should improve core wall rate of charge.In addition, the reduction of core wall ratio can improve the bearing capacity of microcapsules.Microcapsule degelling agent for atoleine, on the one hand, we wish that the core content in the capsule is big as much as possible, improve broken glue efficient, this just needs to improve core wall ratio, but excessive core wall ratio can make strength of microcapsules reduce and softgel shell compactness variation, and the core rate of release is too fast, can make the broken in advance glue of fracturing fluid; Therefore suitable core wall is compared to the atoleine microcapsule degelling agent and seems particularly important.
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 core core wall ratio is provided, this preparation technology is by control core core wall ratio, thereby improved particle diameter percentage, embedding rate 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 core core wall ratio, 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: take by weighing core wall ratio and be 2: 1～5: 1 core, drip emulsifying agent again, the vibration dissolving mixes with above-mentioned wall material solution, puts in the water bath with thermostatic control, and mechanical agitation emulsification 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, naturally cooling, when treating that temperature is 32～35 ℃, add ice cube, continuing to be stirred to temperature is below 10 ℃, stirs behind the adding curing agent again, transfer its pH to 9.0 with 20%NaOH solution again after the stirring, 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, the core wall of core was than 4: 1 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 control core core wall ratio, thereby improved particle diameter percentage, embedding rate 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 core core wall ratio, 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: take by weighing core wall ratio and be 2: 1～5: 1 core, drip emulsifying agent again, the vibration dissolving mixes with above-mentioned wall material solution, puts in the water bath with thermostatic control, and mechanical agitation emulsification 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, naturally cooling, when treating that temperature is 32～35 ℃, add ice cube, continuing to be stirred to temperature is below 10 ℃, stirs behind the adding curing agent again, transfer its pH to 9.0 with 20%NaOH solution again after the stirring, 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 the performance of the core wall of core comparison microcapsules has very big influence in the step (b).For some occasions, as coating dyestuff, wish that core can be coated in the wall material for a long time, the compactness of microcapsules is had relatively high expectations, so just should reduce core wall rate of charge, core is as far as possible fully coated; And other occasions as coating medicine, essence, wish that then microcapsules have slow-release function, at this moment just should improve core wall rate of charge.In addition, the reduction of core wall ratio can improve the bearing capacity of microcapsules.Microcapsule degelling agent for atoleine, on the one hand, we wish that the core content in the capsule is big as much as possible, improve broken glue efficient, this just needs to improve core wall ratio, but excessive core wall ratio can make strength of microcapsules reduce and softgel shell compactness variation, and the core rate of release is too fast, can make the broken in advance glue of fracturing fluid; Therefore suitable core wall is compared to the atoleine microcapsule degelling agent and seems particularly important.In order to obtain best core core wall ratio, the present invention has carried out the influence experiment of different core core wall comparison microcapsules.
It is that 7 core assembly materials of 1: 1,2: 1,3: 1,4: 1,5: 1,6: 1 and 7: 1 carry out the performance test of microcapsules that core wall ratio has been chosen in this experiment respectively, and the result is as shown in the table:
| Core core wall ratio | 1∶1 | 2∶1 | 3∶1 | 4∶1 | 5∶1 | 6∶1 | 7∶1 |
| Particle diameter percentage (%) | 71 | 69 | 72 | 74 | 79 | 81 | 84 |
| Embedding rate (%) | 69 | 66 | 67 | 67 | 52 | 48 | 46 |
| Release rate (%) | 75 | 77 | 84 | 85 | 88 | 90 | 92 |
As can be seen from the above table, along with the increase of core core wall ratio, the target grain size percentage of gained microcapsules is increase tendency.Because along with the increase of core, under identical emulsification rotating speed and emulsification times, the suffered shearing force of core is not enough to it is dispersed into enough little particle, and the core drop can increase thereupon, so capsule particle must become big.But can find out also that from last table core wall ratio is that the target grain size percentage of 1: 1 gained microcapsules is 2: 1 greater than core wall ratio.The capsule-core consumption that reason is synthetic microcapsules more after a little while, the wall material increases the average covering amount of drop, it is big that particle diameter becomes.
Embedding rate changes not quite at the beginning along with the increase of core core wall ratio, illustrates that the core wall is increased to 4: 1 than from 1: 1 under other condition same cases, and the wall material is to the coating degree basically identical of core.Bigger 5: 1 place's embedding rate reduction amplitudes, reason is that core concentration is excessive, and emulsification is thorough inadequately, and some core easily is gathered into big drop, fails to be coated.
Along with the increase of core wall ratio, the release rate of capsule is increase tendency.Because the increase of core causes particle to increase on the one hand, the wall material amount that average packet overlays on particle surface reduces; On the other hand, core increases, identical emulsification condition, and core material particles is bigger, and the capsule intensity of formation must reduce, and under identical pressure, release rate will increase.
The intensity of considering microcapsules can improve by curing agent and later stage condition, and the core core wall ratio that we select to prepare microcapsules is 2: 1～5: 1, and preferentially to select core wall ratio for use be 4: 1 core.
As mentioned above, just can realize the present invention preferably.
Claims (4)
1. the microcapsules preparation technology of control core core wall ratio 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: take by weighing core wall ratio and be 2: 1～5: 1 core, drip emulsifying agent again, the vibration dissolving mixes with above-mentioned wall material solution, puts in the water bath with thermostatic control, and mechanical agitation emulsification 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, naturally cooling, when treating that temperature is 32～35 ℃, add ice cube, continuing to be stirred to temperature is below 10 ℃, stirs behind the adding curing agent again, transfer its pH to 9.0 with 20%NaOH solution again after the stirring, 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 core core wall ratio according to claim 1 is characterized in that, the core wall of core was than 4: 1 in the described step (b).
3. the microcapsules preparation technology of control core core wall ratio 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 core core wall ratio according to claim 1 is characterized in that the core in the described step (b) is an atoleine.
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| CN2009102167234A CN102091577A (en) | 2009-12-14 | 2009-12-14 | Microcapsule preparation process capable of controlling core material to core wall ratio |
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| CN2009102167234A CN102091577A (en) | 2009-12-14 | 2009-12-14 | Microcapsule preparation process capable of controlling core material to core wall ratio |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722252A (en) * | 2015-02-06 | 2015-06-24 | 宁波高新区零零七工业设计有限公司 | Preparation process for microcapsule |
| CN105161681A (en) * | 2015-08-10 | 2015-12-16 | 湘潭大学 | Microencapsulated carbon-coated carbon fluoride cathode material and preparation method thereof |
-
2009
- 2009-12-14 CN CN2009102167234A patent/CN102091577A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722252A (en) * | 2015-02-06 | 2015-06-24 | 宁波高新区零零七工业设计有限公司 | Preparation process for microcapsule |
| CN105161681A (en) * | 2015-08-10 | 2015-12-16 | 湘潭大学 | Microencapsulated carbon-coated carbon fluoride cathode material and preparation method thereof |
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Application publication date: 20110615 |