CN102010476B - Method for preparing monodisperse polymer microsphere by irradiation polymerization of ultraviolet light - Google Patents
Method for preparing monodisperse polymer microsphere by irradiation polymerization of ultraviolet light Download PDFInfo
- Publication number
- CN102010476B CN102010476B CN2010105283780A CN201010528378A CN102010476B CN 102010476 B CN102010476 B CN 102010476B CN 2010105283780 A CN2010105283780 A CN 2010105283780A CN 201010528378 A CN201010528378 A CN 201010528378A CN 102010476 B CN102010476 B CN 102010476B
- Authority
- CN
- China
- Prior art keywords
- water
- mixed solvent
- polymer
- polymer microsphere
- mono
- 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.)
- Active
Links
Images
Landscapes
- Polymerisation Methods In General (AREA)
Abstract
The invention relates to a method for preparing a monodisperse polymer microsphere by irradiation polymerization of ultraviolet light, belonging to the technical field of functional polymer microsphere preparation. In the method, an alkene monomer, a reactive macromolecule dispersion stabilizer and a photoinitiator are taken as raw materials, and polymerization is carried out on the raw materials in a mixed solvent of alcohol and water by the ultraviolet radiation to obtain the monodisperse polymer microsphere; the proportion of the raw materials is as follows: the dosage of the alkene monomer is 5-30g, the dosage of the reactive macromolecule dispersion stabilizer is 0.5-10g, the dosage of the photoinitiator is 0.2-1g and the dosage of the mixed solvent of alcohol and water is 100mL; and the reaction is initiated by the ultraviolet irradiation after the system is evenly mixed to obtain the monodisperse polymer microsphere. By using the method provided by the invention, the monodisperse polymer microsphere is obtained at normal temperature, the reaction energy consumption is low, the reaction speed can be regulated between dozens of minutes and dozens of hours, the diameter of particles of the polymer microsphere is controllable within the range of 100-800nm, and the surface of the microsphere has functional polymer chains.
Description
Technical field
The invention discloses the method that a kind of ultraviolet light irradiation polymerization prepares mono-disperse polymer microspheres, belong to functional polymer microsphere preparation technology field.
Background technology
Polymer microsphere has the advantages that specific surface area is big, particle diameter is controlled; And can carry out structure design according to the use needs; Through introducing the side chain of band functional group; Be used for load and prepare polymer microsphere or metal nanoparticle, have a wide range of applications in fields such as drug molecule load, microelectronics, support of the catalyst, light industries with biocompatibility.At present generally need to adopt higher temperature condition during the synthetic macromolecule microballoon, and long reaction time, be unfavorable for the saving of the energy.And adopt UV-light to cause, and reaction activity is lower, and polyreaction can be carried out at normal temperatures; The generation of radical and quencher can be through light unlatching and extinguish and control, speed of response is convenient to regulate very much; Do not need heating in the reaction process, conserve energy yet.
The diffuse-aggregate method that the present invention adopts UV-light to cause prepares polymer microsphere, and its preparation process is simple, and energy consumption of reaction is low, is suitable for the industrial production of mass-producing.
Summary of the invention
The objective of the invention is to disclose the method that a kind of ultraviolet light irradiation polymerization prepares mono-disperse polymer microspheres.
Technical scheme of the present invention: a kind of ultraviolet light irradiation polymerization prepares the method for mono-disperse polymer microspheres, is raw material with vinyl monomer, reactive polymer dispersion stabilizer and light trigger, in the mixed medium of alcohol and water, carries out polymerization by ultraviolet lighting and obtains.
Proportion of raw materials is following: the vinyl monomer consumption is 5-30g, and the reactive polymer amount of stabilizer is 0.5-10 g, and the light trigger consumption is 0.2-1 g, and alcohol is 100mL with the mixed solvent of water;
Reaction process: with the reactive polymer dispersion stabilizer be dissolved in the water, light trigger is dissolved in the alcoholic solvent, mixes the logical nitrogen of lucifuge 15 minutes again with vinyl monomer; Under nitrogen protection or air-proof condition, reaction is 0.5-24 hour under the irradiation of uv lamp; Products therefrom obtains mono-disperse polymer microspheres through centrifugal or filtering method.
Said vinyl monomer is selected vinylbenzene, TEB 3K, methyl acrylate for use, or vinyl-acetic ester;
Said light trigger selects 2 for use, 2-dimethoxy-2 phenyl methyl phenyl ketone, UVNUL MS-40,1-hydroxy-cyclohexyl phenyl ketone, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone or 2-hydroxyl-aminomethyl phenyl propane-1-ketone;
Said reactive polymer dispersion stabilizer is selected methylacrylic acid list end-blocking polyoxyethylene glycol, vinylbenzene list end-blocking Vinylpyrrolidone polymer or vinylbenzene list end-blocking PNIPAM for use;
The mixed solvent of said alcohol and water is selected the mixed solvent of methanol, the mixed solvent of ethanol/water, the mixed solvent of propanol/water or the mixed solvent of isopropanol for use.
With the mono-disperse polymer microspheres of said method preparation, its surface has the functional polymer chain.
With the mono-disperse polymer microspheres of said method preparation, in ultraviolet light irradiation intensity 2.0 * 10
-2-4.0 mw/cm
2The time microspheres prepared be single dispersion for distributing.
Beneficial effect of the present invention: the present invention utilizes light trigger under the ultraviolet light irradiation condition, can be decomposed into the characteristics of radical; Under normal temperature, condition of normal pressure, carry out polyreaction; Reaction times can be as required regulated in dozens of minutes to tens hour, for preparing the mono-disperse polymer microspheres that the surface has the functional polymer chain a kind of energy-conservation, quick, simple, high-efficiency method is provided.
Description of drawings
The SEM photo of Fig. 1 polystyrene microsphere.
The SEM photo of Fig. 2 polystyrene microsphere.
The SEM photo of Fig. 3 poly (methyl methacrylate) micro-sphere.
Embodiment
Embodiment 1
Earlier with initiator 2; 2-dimethoxy-2 phenyl methyl phenyl ketone 0.3g is dissolved in the 70mL ethanol, and vinylbenzene list end-blocking PNIPAM 0.7g is dissolved in the water of 30mL, and both and monomer styrene 10g are mixed together; Place glass reactor, logical while stirring nitrogen sealed after 15 minutes; In uv irradiation intensity 5.2 * 10
-2Mw/cm
2Following irradiation reaction 24 hours; Products therefrom gets monodisperse polystyrene microsphere through centrifugal, dry, and particle diameter is 320 nm, and productive rate can reach 90%, and its particle diameter form is seen the SEM photo of Fig. 1.
Embodiment 2
With 2; 2-dimethoxy-2-phenyl methyl phenyl ketone 0.6g is dissolved in the 70mL ethanol, and vinylbenzene list end-blocking PNIPAM 2.0g is dissolved in the 30mL water, and both and monomer styrene 10g are mixed together; Insert in the glass reactor sealing in 15 minutes of logical while stirring nitrogen; At uv irradiation intensity 3.4 mw/cm
2Following irradiation reaction 30 minutes; Products therefrom gets monodisperse polystyrene microsphere through centrifugal, dry, and particle diameter is 428 nm, and productive rate can reach 85%, and its particle diameter form is seen the SEM photo of Fig. 2.
Embodiment 3
With 2; 2-dimethoxy-2 phenyl methyl phenyl ketone 0.5g is dissolved in the 70mL ethanol, and methylacrylic acid list end-blocking polyoxyethylene glycol 3.0g is dissolved in the 30mL water, and both and monomers methyl methacrylate 10g are mixed together; Insert in the glass reactor logical while stirring nitrogen 15 minutes; At uv irradiation intensity 3.4 mw/cm
2Under shone 30 minutes; Products therefrom is centrifugal, dry, obtains poly (methyl methacrylate) micro-sphere, productive rate 90%, the SEM photo of its particle diameter form such as Fig. 3.
Embodiment 4
UVNUL MS-40 0.2g and 1-hydroxycyclohexylphenylketone 0.4g are dissolved in the 80mL methyl alcohol; Methylacrylic acid list end-blocking polyoxyethylene glycol 5g is dissolved in the 20 mL water, both and TEB 3K 20g are mixed together; Insert in the glass reactor logical while stirring nitrogen 15 minutes; At uv irradiation intensity 3.4 mw/cm
2Under shone 30 minutes; Products therefrom is centrifugal, dry, obtains poly (methyl methacrylate) micro-sphere, productive rate 92%.
Embodiment 5
1-hydroxycyclohexylphenylketone 1.0g is dissolved in the 30mL ethanol, and vinylbenzene list end-blocking Vinylpyrrolidone polymer 10g is dissolved in the 70mL water, and both and TEB 3K 30g are mixed together, and inserts in the glass reactor, logical while stirring nitrogen 15 minutes; At uv irradiation intensity 3.4 mw/cm
2Under shone 30 minutes; Products therefrom is centrifugal, dry, obtains poly (methyl methacrylate) micro-sphere, productive rate 88%.
Embodiment 6
UVNUL MS-40 0.2g and 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone 0.4g are dissolved in the 50mL ethanol; Methylacrylic acid list end-blocking polyoxyethylene glycol 0.5g is dissolved in the 50 mL water; Both and vinyl-acetic ester 10g are mixed together; Insert in the glass reactor logical while stirring nitrogen 15 minutes; At uv irradiation intensity 3.4 mw/cm
2Under shone 30 minutes; Obtain the polyvinyl acetate ester microsphere of water-dispersion.
Claims (3)
1. a ultraviolet light irradiation polymerization prepares the method for mono-disperse polymer microspheres, it is characterized in that with vinyl monomer, reactive polymer dispersion stabilizer and light trigger be raw material, in the mixed medium of alcohol and water, carries out polymerization by ultraviolet lighting and obtains;
Proportion of raw materials is following: the vinyl monomer consumption is 5-30g, and the reactive polymer amount of stabilizer is 0.5-10 g, and the light trigger consumption is 0.2-1 g, and alcohol is 100mL with the mixed solvent of water;
Reaction process: the reactive polymer dispersion stabilizer is dissolved in the water, and light trigger is dissolved in the alcoholic solvent, and both mix with vinyl monomer again, the logical nitrogen of lucifuge 15 minutes; Under nitrogen protection or air-proof condition, reaction is 0.5-24 hour under the irradiation of uv lamp; Products therefrom obtains mono-disperse polymer microspheres through centrifugal or filtering method;
Said vinyl monomer is selected vinylbenzene, TEB 3K, methyl acrylate for use, or vinyl-acetic ester;
Said light trigger selects 2 for use, 2-dimethoxy-2 phenyl methyl phenyl ketone, UVNUL MS-40,1-hydroxy-cyclohexyl phenyl ketone, 2-methyl isophthalic acid-(4-methylthio group phenyl)-2-morpholinyl-1-acetone or 2-hydroxyl-aminomethyl phenyl propane-1-ketone;
Said reactive polymer dispersion stabilizer is selected methylacrylic acid list end-blocking polyoxyethylene glycol, vinylbenzene list end-blocking Vinylpyrrolidone polymer or vinylbenzene list end-blocking PNIPAM for use;
The mixed solvent of said alcohol and water is selected the mixed solvent of methanol, the mixed solvent of ethanol/water, the mixed solvent of propanol/water or the mixed solvent of isopropanol for use.
2. the preparation method of mono-disperse polymer microspheres according to claim 1 is characterized in that the polymer microsphere surface that makes has the functional polymer chain.
3. the preparation method of mono-disperse polymer microspheres according to claim 1 is characterized in that ultraviolet light irradiation intensity is 2.0 * 10
-2-4.0 mw/cm
2The time microspheres prepared be single dispersion for distributing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105283780A CN102010476B (en) | 2010-11-02 | 2010-11-02 | Method for preparing monodisperse polymer microsphere by irradiation polymerization of ultraviolet light |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010105283780A CN102010476B (en) | 2010-11-02 | 2010-11-02 | Method for preparing monodisperse polymer microsphere by irradiation polymerization of ultraviolet light |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102010476A CN102010476A (en) | 2011-04-13 |
| CN102010476B true CN102010476B (en) | 2012-07-11 |
Family
ID=43840821
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010105283780A Active CN102010476B (en) | 2010-11-02 | 2010-11-02 | Method for preparing monodisperse polymer microsphere by irradiation polymerization of ultraviolet light |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102010476B (en) |
Families Citing this family (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304198B (en) * | 2011-06-01 | 2013-06-26 | 华南师范大学 | Method for preparing surface functionalized polymer microspheres |
| CN102731701A (en) * | 2012-04-23 | 2012-10-17 | 苏州异导光电材料科技有限公司 | Method for preparing mono-disperse polymer functional microspheres with photochemical method |
| CN102718894B (en) * | 2012-06-29 | 2015-09-23 | 河北智生环保科技有限公司 | A kind of low-temperature synthetic method of monodisperse polymer micro-sphere |
| CN103665226B (en) * | 2012-09-20 | 2015-12-02 | 大连理工常熟研究院有限公司 | A kind of light-initiated in-situ emulsion polymerization prepares the method for polymer microsphere |
| CN103192074B (en) * | 2013-04-10 | 2015-04-22 | 苏州宇希新材料科技有限公司 | Highly dispersed sliver powder and conductive silver paste for film batteries |
| CN103265657A (en) * | 2013-05-27 | 2013-08-28 | 德州学院 | Method for preparing monodisperse polymer microspheres by photo-initiation precipitation polymerization |
| CN105399879B (en) * | 2015-11-19 | 2018-02-13 | 苏州大学 | A kind of preparation method of water-soluble Properties of Polystyrene Nano Particles |
| CN106893014A (en) * | 2015-12-21 | 2017-06-27 | 上海东升新材料有限公司 | A kind of preparation method of polyvinyl acetate particle and products thereof |
| CN105968243B (en) * | 2016-06-05 | 2018-09-18 | 王金明 | A kind of preparation method of polyisoprene catalyst |
| CN106349421B (en) * | 2016-08-26 | 2018-06-26 | 广州天赐高新材料股份有限公司 | A kind of polymer microsphere and preparation method thereof |
| CN106432564B (en) * | 2016-09-13 | 2019-03-12 | 中国科学院过程工程研究所 | A method of preparing functionalization monodisperse polymer micro-sphere |
| CN107129551A (en) * | 2017-05-05 | 2017-09-05 | 佛山市飞时达新材料科技有限公司 | A kind of preparation method based on the polystyrene microsphere that 2,3 pentanediones are light trigger |
| CN108341966B (en) * | 2018-03-09 | 2020-10-27 | 北京化工大学 | Preparation method of functionalized polymer microspheres |
| CN109293996A (en) * | 2018-09-05 | 2019-02-01 | 安徽新翔包装材料有限公司 | A kind of degradable environment protection paper-plastic bag and preparation method thereof |
| CN109293997A (en) * | 2018-09-05 | 2019-02-01 | 安徽新翔包装材料有限公司 | A kind of waterproof degradation environment protection bag |
| CN109337128A (en) * | 2018-09-05 | 2019-02-15 | 安徽新翔包装材料有限公司 | A kind of decomposable environmentally-friendly plastic packaging bag of high tenacity |
| CN109385057A (en) * | 2018-09-05 | 2019-02-26 | 安徽新翔包装材料有限公司 | A kind of enviroment protective degradable wrapping paper |
| CN110511307A (en) * | 2019-07-17 | 2019-11-29 | 山东科技大学 | A kind of method of energy-efficient synthesizing submicron PMMA microsphere |
| CN110498870B (en) * | 2019-07-17 | 2021-11-26 | 山东科技大学 | Method for preparing PMMA microspheres by using natural materials |
| CN112316922B (en) * | 2020-10-19 | 2023-12-12 | 南通大学 | Preservative adsorption microsphere as well as preparation method and application thereof |
| CN112646067B (en) * | 2020-12-10 | 2021-09-28 | 中山大学 | Method for synthesizing monodisperse polymer microspheres in pure water medium |
| CN117624427B (en) * | 2024-01-25 | 2024-04-23 | 山东省科学院激光研究所 | Laser gain medium, preparation method thereof and yellow-green laser |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1278534A (en) * | 2000-06-13 | 2001-01-03 | 复旦大学 | Polymer microball with fluorescent mark and its preparation |
| EP1742979A1 (en) * | 2004-04-23 | 2007-01-17 | Eugenia Kumacheva | Method of producing polymeric particles with selected size, shape, morphology and composition |
-
2010
- 2010-11-02 CN CN2010105283780A patent/CN102010476B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1278534A (en) * | 2000-06-13 | 2001-01-03 | 复旦大学 | Polymer microball with fluorescent mark and its preparation |
| EP1742979A1 (en) * | 2004-04-23 | 2007-01-17 | Eugenia Kumacheva | Method of producing polymeric particles with selected size, shape, morphology and composition |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102010476A (en) | 2011-04-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102010476B (en) | Method for preparing monodisperse polymer microsphere by irradiation polymerization of ultraviolet light | |
| CN105646789B (en) | A kind of preparation method of nanoscale fluorescent polymer rare earth coordination thing microballoon | |
| CN102786615B (en) | Method for preparing grapheme-polyvinyl chloride nano composite resin through in situ suspension polymerization | |
| CN102492068B (en) | Quantum dots modified by macromolecular monomer, preparation method for quantum dots and application of quantum dots | |
| CN106977635B (en) | A kind of light-initiated active free radical polymerization method | |
| CN102492073A (en) | Quantum dot-based multifunctional magnetic fluorescent microsphere and its preparation method | |
| CN102718894B (en) | A kind of low-temperature synthetic method of monodisperse polymer micro-sphere | |
| CN102504077A (en) | Preparation method of quantum dot polymer microspheres | |
| CN106590310A (en) | Uvioresistant paint with self-repairing function and preparation method and application thereof | |
| CN102153715A (en) | Room temperature self-repair thermoplastic polymer material | |
| CN102807338A (en) | The method for preparing macroscopic body of porous carbon nano tube by gelcasting | |
| JP2008535963A5 (en) | ||
| CN104086683B (en) | A kind of preparation method of steady persistence high-molecular luminous material | |
| CN101602827A (en) | A kind of preparation method of high oil-absorbing resin | |
| CN101709103B (en) | Method for preparing photoresponse hydrogel containing azo monomer by utilizing light sources with different wavelengths | |
| CN102731701A (en) | Method for preparing mono-disperse polymer functional microspheres with photochemical method | |
| CN102181001B (en) | Controllable/active free radical polymerization method | |
| CN102351765A (en) | High efficiency RAFT chain transfer agent S,S'-bis(alpha, alpha'-methyl-alpha''-acetate)trithiocarbonate and its preparation method | |
| CN103254373B (en) | Preparation method of stable segmented copolymer PAPMA (Polymethyl Acrylate P-acetamide Phenyl Ester)-b-PNIPAM (Polyisopropyl Acrylamide) based Au nanometer particle | |
| CN103656668A (en) | Bortezomib sustained-release preparation and preparation method thereof | |
| CN108003270A (en) | A kind of water-absorbing resin for reducing residual acrylic acid and preparation method thereof | |
| CN102167754B (en) | Active free radical polymerization method taking bithiaxanthene diol and derivatives thereof as initiator | |
| CN104926974A (en) | Method for preparing styrene-acrylate copolymer | |
| CN103911079B (en) | A kind of transparent esters of acrylic acid sizing agent of normal temp solidified high stvength | |
| CN102382267B (en) | Method for preparing interpenetrating network intelligent hydrogel by adopting frontal polymerization |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| ASS | Succession or assignment of patent right |
Free format text: FORMER OWNER: GUANGZHOU WUXING MATERIAL TECHNOLOGY CO., LTD. Effective date: 20140709 Owner name: GUANGZHOU WUXING MATERIAL TECHNOLOGY CO., LTD. Free format text: FORMER OWNER: JIANGNAN UNIVERSITY Effective date: 20140709 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| COR | Change of bibliographic data |
Free format text: CORRECT: ADDRESS; FROM: 214122 WUXI, JIANGSU PROVINCE TO: 511400 GUANGZHOU, GUANGDONG PROVINCE |
|
| TR01 | Transfer of patent right |
Effective date of registration: 20140709 Address after: 511400, Panyu District 730, Yingbin Road, Guangdong, Guangzhou Province, building 416, energy saving science and Technology Park Patentee after: Guangzhou Wuxing Material Technology Co., Ltd. Address before: College of chemistry and material engineering Jiangnan University No. 1800 214122 Jiangsu city of Wuxi province Wuxi City Binhu Lihu Avenue Patentee before: Jiangnan University Patentee before: Guangzhou Wuxing Material Technology Co., Ltd. |