CN102091581A - Preparation process capable of improving embedding rate and release rate of microcapsules - Google Patents
Preparation process capable of improving embedding rate and release rate of microcapsules Download PDFInfo
- Publication number
- CN102091581A CN102091581A CN2009102167342A CN200910216734A CN102091581A CN 102091581 A CN102091581 A CN 102091581A CN 2009102167342 A CN2009102167342 A CN 2009102167342A CN 200910216734 A CN200910216734 A CN 200910216734A CN 102091581 A CN102091581 A CN 102091581A
- Authority
- CN
- China
- Prior art keywords
- microcapsules
- core
- wall material
- release rate
- rate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The invention discloses a preparation process capable of improving the embedding rate and release rate of microcapsules, 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 reaction temperature ranges from 40 to 60 DEG C, and the optimal emulsification reaction temperature is 50 DEG C. In the invention, by controlling the reaction temperature in the microcapsule forming process, the embedding rate and the 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 preparation technology who improves microcapsule embedded rate and release rate.
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.
Reaction temperature is very big to the microcapsules performance impact in the microcapsules forming process.Its reason is because wall material and core are the state of congealing at the normal temperature state, and viscosity is also bigger, and complex coacervation this moment takes place not too easily; If reaction temperature is too high, established emulsion may breakdown of emulsion, therefore, for emulsion reaction temperature among the microcapsules preparation technology reaction temperature that relatively is fit to should be arranged.
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 preparation technology who improves microcapsule embedded rate and release rate is provided, this preparation technology is by the reaction temperature in the control microcapsules forming process, thereby can improve microcapsule embedded rate and release rate, and then improve the overall performance of microcapsules.
Purpose of the present invention is achieved through the following technical solutions: a kind of preparation technology who improves microcapsule embedded rate and release rate, 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: take by weighing the wall material, after the distilled water immersion swelling, heating and stirring make its dissolving, are incubated standby then;
(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 promptly gets emulsion;
(c) microcapsules form: step (b) gained mixed liquor is carried out mechanical agitation under 40 ℃～60 ℃ condition, 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.
As preferred version of the present invention, reaction temperature is 50 ℃ in the described step (c).
In sum, the invention has the beneficial effects as follows: by the reaction temperature in the control microcapsules forming process, thereby can improve microcapsule embedded rate and release rate, and then improve 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 preparation technology who improves microcapsule embedded rate and release rate, 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: take by weighing the wall material, after the distilled water immersion swelling, heating and stirring make its dissolving, are incubated standby then;
(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 promptly gets emulsion;
(c) microcapsules form: step (b) gained mixed liquor is carried out mechanical agitation under 40 ℃～60 ℃ condition, 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.
Described wall material is gelatin and Arabic gum, and core is an atoleine.
Because reaction temperature is very big to the embedding rate and the release rate influence of microcapsules in the middle microcapsules forming process of step (c).Because wall material and core are the state of congealing at the normal temperature state, and viscosity is also bigger, complex coacervation this moment takes place not too easily; If reaction temperature is too high, established emulsion may breakdown of emulsion, therefore, for reaction temperature in the microcapsules forming process reaction temperature that relatively is fit to should be arranged.In order to obtain best emulsion reaction temperature, the present invention has carried out the influence experiment of differential responses temperature to microcapsules.
It is that 7 kinds of situations of 20 ℃, 30 ℃, 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃ are carried out the performance test of microcapsules that reaction temperature has been chosen in this experiment respectively, and the result is as shown in the table:
| Reaction temperature (℃) | 20 | 30 | 40 | 50 | 60 | 70 | 80 |
| Particle diameter percentage (%) | 80 | 81 | 81 | 82 | 81 | 80 | 80 |
| Embedding rate (%) | 74 | 76 | 79 | 87 | 78 | 73 | 75 |
| Release rate (%) | 69 | 67 | 68 | 66 | 70 | 69 | 71 |
As can be seen from the above table, along with the rising of reaction temperature, the particle diameter of microcapsules is constant substantially.This is because at emulsifying stage, and the size of core is definite substantially, so in the temperature of agglomeration phase, can not have influence on the particle diameter of capsule.
The embedding rate of microcapsules is 50 ℃ of maximums.When reason was low temperature, cohesion speed was slower, and the part core material particles is gathered into big drop, can not be coated fully, and when temperature was too high, the easy coalescence of part core became big drop, can not be coated.
Reaction temperature also has certain influence to the release rate of microcapsules, and in the time of 50 ℃, release rate is reduced to 66%, and strength ratio is bigger.
Take all factors into consideration, the range of reaction temperature in the microcapsules forming process should be controlled at 40 ℃～60 ℃, and optimal reaction temperature is 50 ℃.
As mentioned above, just can realize the present invention preferably.
Claims (4)
1. a preparation technology who improves microcapsule embedded rate and release rate 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: take by weighing the wall material, after the distilled water immersion swelling, heating and stirring make its dissolving, are incubated standby then;
(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 promptly gets emulsion;
(c) microcapsules form: step (b) gained mixed liquor is carried out mechanical agitation under 40 ℃～60 ℃ condition, 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. a kind of preparation technology who improves microcapsule embedded rate and release rate according to claim 1 is characterized in that, reaction temperature is 50 ℃ in the described step (c).
3. a kind of preparation technology who improves microcapsule embedded rate and release rate according to claim 1 is characterized in that the wall material in the described step (a) is gelatin and Arabic gum.
4. a kind of preparation technology who improves microcapsule embedded rate and release rate according to claim 1 is characterized in that the core in the described step (b) is an atoleine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102167342A CN102091581A (en) | 2009-12-14 | 2009-12-14 | Preparation process capable of improving embedding rate and release rate of microcapsules |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009102167342A CN102091581A (en) | 2009-12-14 | 2009-12-14 | Preparation process capable of improving embedding rate and release rate of microcapsules |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102091581A true CN102091581A (en) | 2011-06-15 |
Family
ID=44124953
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009102167342A Pending CN102091581A (en) | 2009-12-14 | 2009-12-14 | Preparation process capable of improving embedding rate and release rate of microcapsules |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102091581A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104499378A (en) * | 2014-11-21 | 2015-04-08 | 东北林业大学 | Method for preparing environment-friendly waterproof fiberboard based on microcapsule |
| CN110583708A (en) * | 2019-09-05 | 2019-12-20 | 天津市城西广源电力工程有限公司 | Mosquito-repelling microcapsule and preparation method thereof |
-
2009
- 2009-12-14 CN CN2009102167342A patent/CN102091581A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104499378A (en) * | 2014-11-21 | 2015-04-08 | 东北林业大学 | Method for preparing environment-friendly waterproof fiberboard based on microcapsule |
| CN110583708A (en) * | 2019-09-05 | 2019-12-20 | 天津市城西广源电力工程有限公司 | Mosquito-repelling microcapsule and preparation method thereof |
| CN110583708B (en) * | 2019-09-05 | 2022-01-18 | 天津市城西广源电力工程有限公司 | Mosquito-repelling microcapsule and preparation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Fan et al. | Influence of operating conditions on the surface morphology of microcapsules prepared by in situ polymerization | |
| Pang et al. | Lignin-polyurea microcapsules with anti-photolysis and sustained-release performances synthesized via pickering emulsion template | |
| US8357318B2 (en) | Wax encapsulation | |
| CN102091579A (en) | Preparation process for gel breaker microcapsules | |
| CN107042082B (en) | Non-spherical microcapsule particle and preparation method thereof | |
| JPS6244970B2 (en) | ||
| Rochmadi et al. | Mechanism of microencapsulation with urea-formaldehyde polymer | |
| KR102668397B1 (en) | Fabrication of Gelatin-Gum arabic Capsules Using Fluidic Device | |
| CN105797660A (en) | Method for preparing capsules from oil-soluble etherified amino resin | |
| Pansuwan et al. | Innovative and high performance synthesis of microcapsules containing methyl anthranilate by microsuspension iodine transfer polymerization | |
| Rao et al. | Preparation and thermal properties of microencapsulated phase change material for enhancing fluid flow heat transfer | |
| CN113181846A (en) | Preparation method of pure lignin microcapsule based on Pickering emulsion solvent volatilization | |
| CN104830532A (en) | Preparation method of slow release microcapsule ginger oil essence | |
| Zhang et al. | Mechanism of the temperature-responsive material regulating porous morphology on epoxy phenolic novolac resin microcapsule surface | |
| CN102091576A (en) | Controlled-stirring-speed microcapsule preparation process | |
| CN103127031A (en) | Preparation method for oily and oil soluble drug nanocapsules | |
| CN100496698C (en) | Phase-variable microcapsule and its production | |
| CN102091581A (en) | Preparation process capable of improving embedding rate and release rate of microcapsules | |
| CN108355591A (en) | Dimethyl silicone polymer causes ethyl cellulose phase separation and prepares microcapsule method | |
| CN102091577A (en) | Microcapsule preparation process capable of controlling core material to core wall ratio | |
| CN102989389A (en) | Preparation technology of liquid microcapsule gel breaker by controlling ratio of core to wall | |
| CN102091580A (en) | Preparation process capable of obviously improving forming condition and performance of microcapsules | |
| CN107812500A (en) | A kind of magnetic polymer microsphere and preparation method thereof | |
| CN106902716B (en) | Preparation method of small-particle-size starch microspheres | |
| CN102091578A (en) | Microcapsule preparation process capable of controlling dosage of emulsifier |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20110615 |