CN111408325B - Preparation method of magnetic microcapsule - Google Patents
Preparation method of magnetic microcapsule Download PDFInfo
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- CN111408325B CN111408325B CN201910009744.2A CN201910009744A CN111408325B CN 111408325 B CN111408325 B CN 111408325B CN 201910009744 A CN201910009744 A CN 201910009744A CN 111408325 B CN111408325 B CN 111408325B
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- 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
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Abstract
The invention belongs to the technical field of microcapsule preparation, and particularly relates to a preparation method of a magnetic microcapsule. The invention comprises the steps of preparing emulsion, preparing magnetic microcapsules, testing the magnetic response of the magnetic microcapsules and the like. The method is simple, the prepared capsule has good magnetic effect performance, high reaction speed, easily obtained raw materials and uniformly dispersed nano particles.
Description
Technical Field
The utility model belongs to the technical field of microcapsule preparation, in particular to a preparation method of magnetic microcapsules.
Background
There are many methods for preparing magnetic microcapsules, and spray drying, complex coacervation and emulsion gel methods are commonly used. The microcapsule prepared by the complex coacervation method has the advantages of accurate and difficult PH control, and the microcapsule must be stirred all the time in the process, and the poor speed control is easy to adhere to the mass, thus causing the final capsule to have overlarge diameter and rough surface. And the nano materials are easy to agglomerate and are distributed unevenly. The smaller the material, the larger the specific surface area, the larger the surface energy of molecules among the materials, and particularly in aqueous solution, the more polar the material is and the more easily aggregated the material is.
The microcapsule prepared by the technology has the advantages of high reaction rate, no harm to the environment and the body of an operator, simple and quick preparation process, simple flow and easily obtained raw materials.
The research on the dispersion of the magnetic nanoparticles in the emulsion is an important problem nowadays, the technology introduces the magnetic nanoparticles in a blending mode in the process of preparing the magnetic microcapsules, and the magnetic nanoparticles are dispersed very uniformly.
Disclosure of Invention
In order to solve the problems of uneven distribution of nano particles and the like in the existing magnetic microcapsule preparation method, the invention provides a preparation method of a magnetic microcapsule, which is simple to operate and has good magnetic response performance.
The invention provides a preparation method of a magnetic microcapsule, which comprises the following steps and conditions:
the invention relates to abbreviated Chinese names: PVAc is polyvinyl acetate emulsion, PVA is polyvinyl alcohol, OP-10 is polyoxyethylene octyl phenol ether-10, SDS is sodium dodecyl sulfate, KPS is potassium persulfate, VAc is vinyl acetate, and DBP is dibutyl phthalate.
(1) Preparation method of PVAc emulsion
Under the condition of room temperature, 4g of PVA and 28g of deionized water are sequentially added into a four-port reactor, and heated and dissolved at 90 ℃ to prepare a needed PVA solution; 13mL of deionized water, 0.8mL of OP-10, 0.3g of SDS, 2mL of KPS solution with the mass volume concentration of 10mg/mL and 5.5mL of VAc are sequentially added into the obtained solution; subsequently, the mixture was heated in a water bath at 70 ℃ and stirred under reflux for 1 hour, and then 28mL of VAc and 7mL of KPS solution having a mass volume concentration of 10mg/mL were alternately added to the reaction mixture, and the dropwise addition was completed within 2 hours. After the dropwise addition, the temperature is raised to 90 ℃, the reaction is carried out until no reflux exists, and then the reaction product is cooled to 50 ℃. Adjusting the pH value to 5, adding 9.5g of DBP, and fully reacting for 30min to obtain PVAc emulsion.
(2)PVAc@Fe3O4Method for preparing emulsion
0.1g of Fe3O4Adding into 10mL of PVAc emulsion, stirring for 30min and mixing uniformly.
(3) Preparation of magnetic microcapsules
Putting NaCl crystal (diameter between 1mm and 30mm) into PVAc @ Fe3O4Standing for 2-10min, washing with water for 3min to dissolve NaCl to obtain magnetic microcapsule with thickness of 50-500um, inner diameter of 1-30mm, and outer diameter of 1.05-30.5 mm.
(4) Magnetic response of magnetic microcapsules
The prepared magnetic microcapsule is placed in a glass culture dish filled with water, and then the magnet is tightly attached to the outer surface of the bottom of the glass culture dish and continuously moves, so that the prepared magnetic microcapsule can be observed to move along with the movement of the magnet, and the prepared magnetic microcapsule is proved to have good magnetic response performance. Scanning electronic displayElemental distribution of the micromirror indicates magnetic Fe3O4The nanoparticles are uniformly dispersed in the microcapsules.
Advantageous effects
The process is simple, the prepared capsule has good magnetic response performance, high reaction rate, easily obtained raw materials and uniformly dispersed nano particles.
Detailed Description
Example 1
The invention provides a preparation method of a magnetic microcapsule, which comprises the following steps and conditions:
(1) preparation method of PVAc emulsion
Under the condition of room temperature, 4g of PVA and 28g of deionized water are sequentially added into a four-port reactor, and heated and dissolved at 90 ℃ to prepare a needed PVA solution; 13mL of deionized water, 0.8mL of OP-10, 0.3g of SDS, 2mL of KPS solution with the mass volume concentration of 10mg/mL and 5.5mL of VAc are sequentially added into the obtained solution; subsequently, the mixture was heated in a water bath at 70 ℃ and stirred under reflux for 1 hour, and then 28mL of VAc and 7mL of KPS solution having a mass volume concentration of 10mg/mL were alternately added to the reaction mixture, and the dropwise addition was completed within 2 hours. After the dropwise addition, the temperature is raised to 90 ℃, the reaction is carried out until no reflux exists, and then the reaction product is cooled to 50 ℃. Adjusting the pH value to 5, adding 9.5g of DBP, and fully reacting for 30min to obtain PVAc emulsion.
(2)PVAc@Fe3O4Method for preparing emulsion
0.1g of Fe3O4Adding into 10mL of PVAc emulsion, stirring for 30min and mixing uniformly.
(3) Preparation of magnetic microcapsules
Putting NaCl crystal (diameter is 1mm) into PVAc @ Fe3O4Standing the emulsion for 2min, then washing the emulsion for 3min to dissolve NaCl, and obtaining the magnetic microcapsule, wherein the thickness of the prepared magnetic microcapsule is 50um, the inner diameter of the magnetic microcapsule is 1mm, and the outer diameter of the magnetic microcapsule is 1.05 mm.
(4) Magnetic response of magnetic microcapsules
The prepared magnetic microcapsule is placed in a glass culture dish filled with water, and then the magnet is tightly attached to the outer surface of the bottom of the glass culture dish and continuously moves, so that the prepared magnetic microcapsule can be observedThe capsule moves along with the movement of the magnet, and the prepared magnetic microcapsule is proved to have good magnetic response performance. Elemental distribution of scanning electron microscopy indicates magnetic Fe3O4The nanoparticles are uniformly dispersed in the microcapsules.
Example 2
The invention provides a preparation method of a magnetic microcapsule, which comprises the following steps and conditions:
(1) preparation method of PVAc emulsion
Under the condition of room temperature, 4g of PVA and 28g of deionized water are sequentially added into a four-port reactor, and heated and dissolved at 90 ℃ to prepare a needed PVA solution; 13mL of deionized water, 0.8mL of OP-10, 0.3g of SDS, 2mL of KPS solution with the mass volume concentration of 10mg/mL and 5.5mL of VAc are sequentially added into the obtained solution; subsequently, the mixture was heated in a water bath at 70 ℃ and stirred under reflux for 1 hour, and then 28mL of VAc and 7mL of KPS solution having a mass volume concentration of 10mg/mL were alternately added to the reaction mixture, and the dropwise addition was completed within 2 hours. After the dropwise addition, the temperature is raised to 90 ℃, the reaction is carried out until no reflux exists, and then the reaction product is cooled to 50 ℃. Adjusting the pH value to 5, adding 9.5g of DBP, and fully reacting for 30min to obtain PVAc emulsion.
(2)PVAc@Fe3O4Method for preparing emulsion
0.1g of Fe3O4Adding into 10mL of PVAc emulsion, stirring for 30min and mixing uniformly.
(3) Preparation of magnetic microcapsules
Putting NaCl crystal (diameter 15mm) into PVAc @ Fe3O4Standing for 5min in the emulsion, then washing with water for 3min to dissolve NaCl, and obtaining the magnetic microcapsule, wherein the thickness of the prepared magnetic microcapsule is 200um, the inner diameter of the magnetic microcapsule is 15mm, and the outer diameter of the magnetic microcapsule is 15.2 mm.
(4) Magnetic response of magnetic microcapsules
The prepared magnetic microcapsule is placed in a glass culture dish filled with water, and then the magnet is tightly attached to the outer surface of the bottom of the glass culture dish and continuously moves, so that the prepared magnetic microcapsule can be observed to move along with the movement of the magnet, and the prepared magnetic microcapsule is proved to have good magnetic response performance. Element distribution diagram of scanning electron microscopeMagnetic Fe3O4The nanoparticles are uniformly dispersed in the microcapsules.
Example 3
The invention provides a preparation method of a magnetic microcapsule, which comprises the following steps and conditions:
(1) preparation method of PVAc emulsion
Under the condition of room temperature, 4g of PVA and 28g of deionized water are sequentially added into a four-port reactor, and heated and dissolved at 90 ℃ to prepare a needed PVA solution; 13mL of deionized water, 0.8mL of OP-10, 0.3g of SDS, 2mL of KPS solution with the mass volume concentration of 10mg/mL and 5.5mL of VAc are sequentially added into the obtained solution; subsequently, the mixture was heated in a water bath at 70 ℃ and stirred under reflux for 1 hour, and then 28mL of VAc and 7mL of KPS solution having a mass volume concentration of 10mg/mL were alternately added to the reaction mixture, and the dropwise addition was completed within 2 hours. After the dropwise addition, the temperature is raised to 90 ℃, the reaction is carried out until no reflux exists, and then the reaction product is cooled to 50 ℃. Adjusting the pH value to 5, adding 9.5g of DBP, and fully reacting for 30min to obtain PVAc emulsion.
(2)PVAc@Fe3O4Method for preparing emulsion
0.1g of Fe3O4Adding into 10mL of PVAc emulsion, stirring for 30min and mixing uniformly.
(3) Preparation of magnetic microcapsules
Putting NaCl crystal (diameter 30mm) into PVAc @ Fe3O4Standing the emulsion for 10min, then washing the emulsion for 3min to dissolve NaCl, and obtaining the magnetic microcapsule, wherein the thickness of the prepared magnetic microcapsule is 500um, the inner diameter of the magnetic microcapsule is 30mm, and the outer diameter of the magnetic microcapsule is 30.5 mm.
(4) Magnetic response of magnetic microcapsules
The prepared magnetic microcapsule is placed in a glass culture dish filled with water, and then the magnet is tightly attached to the outer surface of the bottom of the glass culture dish and continuously moves, so that the prepared magnetic microcapsule can be observed to move along with the movement of the magnet, and the prepared magnetic microcapsule is proved to have good magnetic response performance. Elemental distribution of scanning electron microscopy indicates magnetic Fe3O4The nanoparticles are uniformly dispersed in the microcapsules.
Claims (1)
1. The preparation method of the magnetic microcapsule is characterized by comprising the following steps and conditions:
(1) preparation method of PVAc emulsion
Under the condition of room temperature, 4g of PVA and 28g of deionized water are sequentially added into a four-port reactor, and heated and dissolved at 90 ℃ to prepare a needed PVA solution; 13mL of deionized water, 0.8mL of OP-10, 0.3g of SDS, 2mL of KPS solution with the mass volume concentration of 10mg/mL and 5.5mL of VAc are sequentially added into the obtained solution; then heating the mixture in water bath at 70 ℃, refluxing and stirring for 1h, and then alternately adding 28mL of VAc and 7mL of KPS solution with the mass volume concentration of 10mg/mL into the reaction solution, wherein the dropwise addition is finished within 2 h; after the dropwise addition is finished, the temperature is raised to 90 ℃, the reaction is carried out until no reflux exists, and then the reaction product is cooled to 50 ℃; adjusting the pH value to 5, adding 9.5g of DBP, and fully reacting for 30min to obtain PVAc emulsion;
(2)PVAc@Fe3O4method for preparing emulsion
0.1g of Fe3O4Adding the mixture into 10mL of PVAc emulsion, stirring for 30min and uniformly mixing;
(3) preparation of magnetic microcapsules
Putting NaCl crystals with the diameter of 1-30mm into PVAc @ Fe3O4Standing for 2-10min in the emulsion, and then washing with water for 3min to dissolve NaCl to obtain magnetic microcapsule with thickness of 50-500um, inner diameter of 1-30mm and outer diameter of 1.05-30.5 mm;
(4) magnetic response of magnetic microcapsules
The prepared magnetic microcapsule is placed in a glass culture dish filled with water, then the magnet is tightly attached to the outer surface of the bottom of the glass culture dish and continuously moves, the prepared magnetic microcapsule can be observed to move along with the movement of the magnet, the prepared magnetic microcapsule is proved to have good magnetic response performance, and the element distribution diagram of a scanning electron microscope shows that the magnetic Fe is3O4The nano particles are uniformly dispersed in the microcapsule;
wherein, PVAc is polyvinyl acetate emulsion, PVA is polyvinyl alcohol, OP-10 is polyoxyethylene octyl phenol ether-10, SDS is sodium dodecyl sulfate, KPS is potassium persulfate, VAc is vinyl acetate, and DBP is dibutyl phthalate.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57140641A (en) * | 1981-02-20 | 1982-08-31 | Tanabe Seiyaku Co Ltd | Microcapsule and preparation thereof |
| US4879175A (en) * | 1985-12-11 | 1989-11-07 | Minnesota Mining And Manufacturing Company | Device for exposing colorant to be transferred |
| JP2006061826A (en) * | 2004-08-26 | 2006-03-09 | Pilot Corporation | Production method of microcapsule, microcapsule, and magnetic display medium using it |
| US9828452B1 (en) * | 2004-11-11 | 2017-11-28 | Instituto Alberto Luiz Coimbra De Pós-Graduação E Pesquisa De Engenharia—Coppe | Process for the synthesis of poly (vinyl alcohol) and/or poly (vinyl acetate) with spherical morphology and shell-and-nucleus structure and its use in vascular embolization |
| CN107435039A (en) * | 2017-06-13 | 2017-12-05 | 安徽安龙基因医学检验所有限公司 | A kind of preparation method and storage method of the immunomagnetic beads for sorting leucocyte |
| CN107490681A (en) * | 2017-09-29 | 2017-12-19 | 安徽安龙基因科技有限公司 | A kind of preparation method of EpCAM antibody immune magnetic beads |
-
2019
- 2019-01-07 CN CN201910009744.2A patent/CN111408325B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57140641A (en) * | 1981-02-20 | 1982-08-31 | Tanabe Seiyaku Co Ltd | Microcapsule and preparation thereof |
| US4879175A (en) * | 1985-12-11 | 1989-11-07 | Minnesota Mining And Manufacturing Company | Device for exposing colorant to be transferred |
| JP2006061826A (en) * | 2004-08-26 | 2006-03-09 | Pilot Corporation | Production method of microcapsule, microcapsule, and magnetic display medium using it |
| US9828452B1 (en) * | 2004-11-11 | 2017-11-28 | Instituto Alberto Luiz Coimbra De Pós-Graduação E Pesquisa De Engenharia—Coppe | Process for the synthesis of poly (vinyl alcohol) and/or poly (vinyl acetate) with spherical morphology and shell-and-nucleus structure and its use in vascular embolization |
| CN107435039A (en) * | 2017-06-13 | 2017-12-05 | 安徽安龙基因医学检验所有限公司 | A kind of preparation method and storage method of the immunomagnetic beads for sorting leucocyte |
| CN107490681A (en) * | 2017-09-29 | 2017-12-19 | 安徽安龙基因科技有限公司 | A kind of preparation method of EpCAM antibody immune magnetic beads |
Non-Patent Citations (1)
| Title |
|---|
| Preparation and UV-protective Property of PVAc/ZnO and PVAc/TiO2 Microcapsules/poly(lactic acid) Nanocomposites;Bin Zhang，Jian Han;《Fibers and Polymers》;20161130;第17卷(第11期);第1849-1857页 * |
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