CN106589222A - Monodisperse high-molecular microspheres and preparation method thereof - Google Patents
Monodisperse high-molecular microspheres and preparation method thereof Download PDFInfo
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- CN106589222A CN106589222A CN201611103998.3A CN201611103998A CN106589222A CN 106589222 A CN106589222 A CN 106589222A CN 201611103998 A CN201611103998 A CN 201611103998A CN 106589222 A CN106589222 A CN 106589222A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/26—Esters containing oxygen in addition to the carboxy oxygen
- C08F220/32—Esters containing oxygen in addition to the carboxy oxygen containing epoxy radicals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/12—Polymerisation in non-solvents
- C08F2/16—Aqueous medium
- C08F2/20—Aqueous medium with the aid of macromolecular dispersing agents
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Abstract
The invention relates to monodisperse high-molecular microspheres and a preparation method thereof, and belongs to the technical field of high-molecular materials. With glycidyl methacrylate (GMA) as a main monomer, divinyl benzene (DVB) as a crosslinking agent and acrylonitrile (AN) as a third monomer, the monodisperse high-molecular microspheres having the particle size of 3-5 [mu]m are prepared through a high-molecular suspension polymerization reaction in the presence of a pore-forming agent.
Description
Technical field
The present invention relates to a kind of polymer microsphere and preparation method thereof, it is more particularly related to a kind of single dispersing
Polymer microsphere and preparation method thereof, belongs to technical field of polymer materials.
Background technology
Polymer microsphere is the quite varied functional material of a class application.Can be applicable to reagent for clinical diagnosis, medicament slow release
Carrier, activated protein and effective ingredient are isolated and purified.And mono dispersed micrograde polymer microsphere is due to its particle diameter distribution
It is very narrow to also act as chromatograph packing material, from the monodisperse polymer micro-sphere of this particle diameter, post pressure not only can be reduced, moreover it is possible to significantly
Raising post effect, polymer microballoon also have the advantages that it is corrosion-resistant, production it is easy.Therefore, monodisperse polymer micro-sphere is used as color
Spectrum filler represents the trend of chromatograph packing material development（Sui Xihua, yellow Tian Bao. Monodispersed cross linking polystyrene microsphers HPLC is fixed
The synthesis [J] of phase. synthesis chemistry, 1998,6 (3):302-306.）.
Existing polymer microsphere particle diameter distribution is not narrow enough.
The content of the invention
Present invention seek to address that in prior art polymer microsphere problem, there is provided a kind of mono-disperse polymer microspheres, should
Polymer microsphere has the advantages that particle diameter distribution is very narrow.
In order to realize foregoing invention purpose, its specific technical scheme is as follows：
A kind of mono-disperse polymer microspheres, it is characterised in that：Including following raw materials by weight：
Oil phase：
30 parts of divinylbenzene (DVB)
Glytidyl methacrylate（GMA）50 parts
Acrylonitrile（AN）20 parts
20 parts of isoamyl alcohol
20 parts of toluene
10 parts of diethylbenzene
3 parts of azodiisobutyronitrile (AIBN)；
Water phase：
5 parts of polyvinylpyrrolidone (PVPK)
Polyvinyl alcohol（PVA1788）5 parts
10 parts of gelatin
5 parts of NaCl
CaCO35 parts
500 parts of deionized water.
A kind of preparation method of mono-disperse polymer microspheres, it is characterised in that：Comprise the following steps that：
A, according to synthesis in water formula, accurately weigh NaCl, CaCO3, distilled water be put into reaction vessel, with 200 revs/min of rotating speed
Start stirring；Reaction vessel is positioned in water-bath and is heated to 65 DEG C, add polyvinyl alcohol, polyvinylpyrrolidone, gelatin,
This system is water phase.
B, accurately weigh divinylbenzene, glytidyl methacrylate, acrylonitrile, isoamyl alcohol, first according to recipe requirements
Benzene, diethylbenzene, azodiisobutyronitrile are sufficiently mixed uniformly in container, and this system is oil phase, is then put into aqueous phase reactions
In container, and it is warming up to 75 DEG C.
The speed stirred in C, holding reactor is 300 revs/min, oil phase is formed uniform bead and is dispersed in and matches somebody with somebody in advance
In the water phase for making；Temperature is risen to into 80 DEG C after bead sizing；
D, polymerization reaction system temperature is raised to 80 DEG C, is incubated 2-3 hour；Polymerization reaction system is warming up to into 85 DEG C, insulation
2-3 hour；Polymerization reaction system is warming up to into 90 DEG C, 2-3 hour is incubated；Reaction system is cooled to into 30-50 DEG C, is leached
Resin bead；
E, the porogen gone in resin by hydrodistillation distillation；Drip washing is carried out to resin using ethanol, the impurity of resin is removed
And the porogen of residual, air-dry and obtain microsphere.
The Advantageous Effects that the present invention brings：
The present invention is with glytidyl methacrylate（GMA）For principal monomer, divinylbenzene（DVB）For cross-linking agent, acrylonitrile
（AN）As Third monomer, particle diameter is prepared between 3-5 μm by polymer suspension polyreaction in the presence of porogen
Mono-disperse polymer microspheres.
Specific embodiment
Embodiment 1
A kind of mono-disperse polymer microspheres, including following raw materials by weight：
Oil phase：
30 parts of divinylbenzene (DVB)
Glytidyl methacrylate（GMA）50 parts
Acrylonitrile（AN）20 parts
20 parts of isoamyl alcohol
20 parts of toluene
10 parts of diethylbenzene
3 parts of azodiisobutyronitrile (AIBN)；
Water phase：
5 parts of polyvinylpyrrolidone (PVPK)
Polyvinyl alcohol（PVA1788）5 parts
10 parts of gelatin
5 parts of NaCl
CaCO35 parts
500 parts of deionized water.
Embodiment 2
A kind of preparation method of mono-disperse polymer microspheres, comprises the following steps that：
A, according to synthesis in water formula, accurately weigh NaCl, CaCO3, distilled water be put into reaction vessel, with 200 revs/min of rotating speed
Start stirring；Reaction vessel is positioned in water-bath and is heated to 65 DEG C, add polyvinyl alcohol, polyvinylpyrrolidone, gelatin,
This system is water phase.
B, accurately weigh divinylbenzene, glytidyl methacrylate, acrylonitrile, isoamyl alcohol, first according to recipe requirements
Benzene, diethylbenzene, azodiisobutyronitrile are sufficiently mixed uniformly in container, and this system is oil phase, is then put into aqueous phase reactions
In container, and it is warming up to 75 DEG C.
The speed stirred in C, holding reactor is 300 revs/min, oil phase is formed uniform bead and is dispersed in and matches somebody with somebody in advance
In the water phase for making；Temperature is risen to into 80 DEG C after bead sizing；
D, polymerization reaction system temperature is raised to 80 DEG C, is incubated 2 hours；Polymerization reaction system is warming up to into 85 DEG C, 2 are incubated
Hour；Polymerization reaction system is warming up to into 90 DEG C, 2 hours are incubated；Reaction system is cooled to into 30 DEG C, resin bead is leached；
E, the porogen gone in resin by hydrodistillation distillation；Drip washing is carried out to resin using ethanol, the impurity of resin is removed
And the porogen of residual, air-dry and obtain microsphere.
Embodiment 3
A kind of preparation method of mono-disperse polymer microspheres, comprises the following steps that：
A, according to synthesis in water formula, accurately weigh NaCl, CaCO3, distilled water be put into reaction vessel, with 200 revs/min of rotating speed
Start stirring；Reaction vessel is positioned in water-bath and is heated to 65 DEG C, add polyvinyl alcohol, polyvinylpyrrolidone, gelatin,
This system is water phase.
B, accurately weigh divinylbenzene, glytidyl methacrylate, acrylonitrile, isoamyl alcohol, first according to recipe requirements
Benzene, diethylbenzene, azodiisobutyronitrile are sufficiently mixed uniformly in container, and this system is oil phase, is then put into aqueous phase reactions
In container, and it is warming up to 75 DEG C.
The speed stirred in C, holding reactor is 300 revs/min, oil phase is formed uniform bead and is dispersed in and matches somebody with somebody in advance
In the water phase for making；Temperature is risen to into 80 DEG C after bead sizing；
D, polymerization reaction system temperature is raised to 80 DEG C, is incubated 3 hours；Polymerization reaction system is warming up to into 85 DEG C, 3 are incubated
Hour；Polymerization reaction system is warming up to into 90 DEG C, 3 hours are incubated；Reaction system is cooled to into 50 DEG C, resin bead is leached；
E, the porogen gone in resin by hydrodistillation distillation；Drip washing is carried out to resin using ethanol, the impurity of resin is removed
And the porogen of residual, air-dry and obtain microsphere.
Embodiment 4
A kind of preparation method of mono-disperse polymer microspheres, comprises the following steps that：
A, according to synthesis in water formula, accurately weigh NaCl, CaCO3, distilled water be put into reaction vessel, with 200 revs/min of rotating speed
Start stirring；Reaction vessel is positioned in water-bath and is heated to 65 DEG C, add polyvinyl alcohol, polyvinylpyrrolidone, gelatin,
This system is water phase.
B, accurately weigh divinylbenzene, glytidyl methacrylate, acrylonitrile, isoamyl alcohol, first according to recipe requirements
Benzene, diethylbenzene, azodiisobutyronitrile are sufficiently mixed uniformly in container, and this system is oil phase, is then put into aqueous phase reactions
In container, and it is warming up to 75 DEG C.
The speed stirred in C, holding reactor is 300 revs/min, oil phase is formed uniform bead and is dispersed in and matches somebody with somebody in advance
In the water phase for making；Temperature is risen to into 80 DEG C after bead sizing；
D, polymerization reaction system temperature is raised to 80 DEG C, is incubated 2.5 hours；Polymerization reaction system is warming up to into 85 DEG C, insulation
2.5 hours；Polymerization reaction system is warming up to into 90 DEG C, 2.5 hours are incubated；Reaction system is cooled to into 40 DEG C, tree is leached
Fat bead；
E, the porogen gone in resin by hydrodistillation distillation；Drip washing is carried out to resin using ethanol, the impurity of resin is removed
And the porogen of residual, air-dry and obtain microsphere.
Claims (2)
1. a kind of mono-disperse polymer microspheres, it is characterised in that：Including following raw materials by weight：
Oil phase：
30 parts of divinylbenzene (DVB)
Glytidyl methacrylate（GMA）50 parts
Acrylonitrile（AN）20 parts
20 parts of isoamyl alcohol
20 parts of toluene
10 parts of diethylbenzene
3 parts of azodiisobutyronitrile (AIBN)；
Water phase：
5 parts of polyvinylpyrrolidone (PVPK)
Polyvinyl alcohol（PVA1788）5 parts
10 parts of gelatin
5 parts of NaCl
CaCO35 parts
500 parts of deionized water.
2. the preparation method of a kind of mono-disperse polymer microspheres according to claim 1, it is characterised in that：Including following work
Skill step：
A, according to synthesis in water formula, accurately weigh NaCl, CaCO3, distilled water be put into reaction vessel, with 200 revs/min of rotating speed
Start stirring；Reaction vessel is positioned in water-bath and is heated to 65 DEG C, add polyvinyl alcohol, polyvinylpyrrolidone, gelatin,
This system is water phase；
B, accurately weigh according to recipe requirements divinylbenzene, glytidyl methacrylate, acrylonitrile, isoamyl alcohol, toluene, two
Ethylbenzene, azodiisobutyronitrile are sufficiently mixed uniformly in container, and this system is oil phase, is then put into aqueous phase reactions container
It is interior, and it is warming up to 75 DEG C；
C, keep the speed stirred in reactor to be 300 revs/min, oil phase is formed uniform bead and is dispersed in and prepare in advance
Water phase in；Temperature is risen to into 80 DEG C after bead sizing；
D, polymerization reaction system temperature is raised to 80 DEG C, is incubated 2-3 hour；Polymerization reaction system is warming up to into 85 DEG C, insulation
2-3 hour；Polymerization reaction system is warming up to into 90 DEG C, 2-3 hour is incubated；Reaction system is cooled to into 30-50 DEG C, is leached
Resin bead；
E, the porogen gone in resin by hydrodistillation distillation；Drip washing is carried out to resin using ethanol, the impurity of resin is removed
And the porogen of residual, air-dry and obtain microsphere.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611103998.3A CN106589222A (en) | 2016-12-05 | 2016-12-05 | Monodisperse high-molecular microspheres and preparation method thereof |
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| CN201611103998.3A CN106589222A (en) | 2016-12-05 | 2016-12-05 | Monodisperse high-molecular microspheres and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116037221A (en) * | 2023-02-07 | 2023-05-02 | 蚌埠市天星树脂有限责任公司 | Preparation process of cation exchange resin for treating wastewater and waste gas |
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| CN1362973A (en) * | 1999-04-09 | 2002-08-07 | 迪纳尔帕蒂克勒斯有限公司 | Process for the preparation of monodisperse polymer particles |
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| CN101481431A (en) * | 2008-01-09 | 2009-07-15 | 罗门哈斯公司 | Method for producing polymer beads of uniform size |
| CN101531734A (en) * | 2008-03-14 | 2009-09-16 | 北京化工大学 | Preparation and application of composite TiO*copolymer microspheres |
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| CN105289760A (en) * | 2015-10-23 | 2016-02-03 | 蓝星（成都）新材料有限公司 | Amphoteric ion exchange resin |
| CN105777968A (en) * | 2016-03-25 | 2016-07-20 | 华南理工大学 | Preparation method for monodisperse cap-shaped non-spherical emulsion particles |
-
2016
- 2016-12-05 CN CN201611103998.3A patent/CN106589222A/en active Pending
Patent Citations (10)
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| CN1362973A (en) * | 1999-04-09 | 2002-08-07 | 迪纳尔帕蒂克勒斯有限公司 | Process for the preparation of monodisperse polymer particles |
| CN1938091A (en) * | 2004-02-06 | 2007-03-28 | 兰爱克谢斯德国有限责任公司 | Method for the production of monodispersed pearl polymers containing acrylic |
| CN101148486A (en) * | 2007-10-25 | 2008-03-26 | 刘文韬 | Micro/nano level mesoporous structure substance with biological affinity and forming method thereof |
| CN101481431A (en) * | 2008-01-09 | 2009-07-15 | 罗门哈斯公司 | Method for producing polymer beads of uniform size |
| CN101531734A (en) * | 2008-03-14 | 2009-09-16 | 北京化工大学 | Preparation and application of composite TiO*copolymer microspheres |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116037221A (en) * | 2023-02-07 | 2023-05-02 | 蚌埠市天星树脂有限责任公司 | Preparation process of cation exchange resin for treating wastewater and waste gas |
| CN116037221B (en) * | 2023-02-07 | 2023-08-18 | 蚌埠市天星树脂有限责任公司 | Preparation process of cation exchange resin for treating wastewater and waste gas |
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Application publication date: 20170426 |