CN102399340B - Preparation method of carboxylated polystyrene microball - Google Patents
Preparation method of carboxylated polystyrene microball Download PDFInfo
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- CN102399340B CN102399340B CN 201010278715 CN201010278715A CN102399340B CN 102399340 B CN102399340 B CN 102399340B CN 201010278715 CN201010278715 CN 201010278715 CN 201010278715 A CN201010278715 A CN 201010278715A CN 102399340 B CN102399340 B CN 102399340B
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Abstract
The invention relates to a preparation method of a carboxylated polystyrene microball. The preparation method concretely comprises the following steps: 1, cleaning styrene with a sodium hydroxide solution, and then cleaning styrene with pure water; 2, adding sodium bicarbonate, water and an olefin acid to cleaned styrene to form a mixed solution, and accessing nitrogen to the mixed solution for 10-20min with stirring and cooling; 3, heating the mixed solution to 65-80DEG C in a water bath, adding potassium peroxydisulfate, and reacting for 4-6h; 4, heating the mixed solution to 81-90DEG C in the water bath, and reacting for 2-4h; and 5, cleaning the mixed solution with pure water. The carboxyl distribution proportion on the surface of the carboxylated polystyrene microball prepared with the preparation method of the invention is high.
Description
Technical field
The invention belongs to biological detection and use the microballoon field, relate to a kind of preparation method of carboxylic polystyrene microsphere.
Background technology
Carboxylic polystyrene microsphere is mainly used in crosslinked biomacromolecule and carries out Biological Detection.At present, when preparing carboxylic polystyrene microsphere, all adopt and add acrylic acid mode to polystyrene microsphere surface introducing carboxyl with polymerization.But the most of carboxyl of the carboxylic polystyrene microsphere that adopts this method to prepare is embedded in microballoon inside, and the carboxyl distribution proportion on polystyrene microsphere surface is not high, is generally 0.25mmol/g.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of carboxylic polystyrene microsphere, the distribution proportion height of its surperficial carboxyl of carboxylic polystyrene microsphere of making of method thus.
To achieve these goals, the technical scheme that the present invention proposes is: the preparation method of carboxylic polystyrene microsphere, and step comprises: (1) is cleaned vinylbenzene with sodium hydroxide solution, clean with pure water again; (2) add sodium bicarbonate, water and olefin(e) acid in the vinylbenzene after cleaning, form mixed solution, then under stirring, cooling off, logical nitrogen is 10～20 minutes in mixed solution; (3) heating in water bath mixed solution to 65～80 ℃ then add Potassium Persulphate, react 4～6 hours; (4) reacted 2～4 hours heating in water bath mixed solution to 81～90 ℃; (5) pure water cleans mixed solution.
Olefin(e) acid is hexenoic acid or undecylenic acid in the described step (2).Cinnamic content is 80～95% in the described step (2); The content of olefin(e) acid is 4～20% in the described step (2).
In the technical scheme of the present invention, vinylbenzene being cleaned with sodium hydroxide solution earlier, clean with pure water, is the impurity that may exist in the vinylbenzene in order to remove.Olefin(e) acid is hexenoic acid or undecylenic acid, hexenoic acid or undecylenic acid are difficult for being converted into corresponding salt in mixed solution, cause the mixed solution oil soluble to reduce, olefin(e) acid can not enter polymerization in the spheroid, thereby the carboxyl of being introduced by them is improved in the ratio of polystyrene microsphere surface arrangement.Cinnamic content is 80～95% in the mixed solution, the content of olefin(e) acid is 4～20%, the content that the experimental results show that olefin(e) acid transformation efficiency that vinylbenzene changes polystyrene in 4～20% scope the time is directly proportional with the add-on of olefin(e) acid, and the adding of alkaline sodium bicarbonate can make the corresponding increase of transformation efficiency.But the content of olefin(e) acid is higher than at 20% o'clock, and transformation efficiency increase degree diminishes.Under stirring, cooling off, logical nitrogen 10～20 minutes is in order to eliminate the influence of oxygen for polyreaction.Heating in water bath mixed solution to 65～80 ℃ then add Potassium Persulphate, react 4～6 hours; Potassium Persulphate is an initiator of polyreaction, keeps reaction conditions at 65～80 ℃, and reaction helped the carrying out of polyreaction in 4～6 hours.Reacted 2～4 hours heating in water bath mixed solution to 81～90 ℃, and particle diameter that can microballoon is homogeneous more.Obtain carboxylated polystyrene microsphere this moment.Clean mixed solution with pure water at last, flush away impurity is to prevent the microballoon sedimentation.
Advantage of the present invention is to introduce carboxyl by hexenoic acid or undecylenic acid at microsphere surface, has improved the distribution proportion of carboxyl on the polystyrene microsphere surface.
Embodiment
The preparation method of the carboxylic polystyrene microsphere of embodiment, step comprises: (1) is cleaned vinylbenzene 3 times with sodium hydroxide solution, cleans with pure water again; (2) add sodium bicarbonate, water and undecylenic acid in the vinylbenzene after cleaning, form mixed solution, then under stirring, cooling off, logical nitrogen is 15 minutes in mixed solution; (3) heating in water bath mixed solution to 75 ℃ then adds Potassium Persulphate, reacts 5 hours; (4) heating in water bath mixed solution to 82 ℃ reacted 3 hours, obtained carboxylated polystyrene microsphere this moment; (5) pure water cleans mixed solution 2 times, flush away impurity.Cinnamic content is 85% in the described step (2), and the content of undecylenic acid is 14%.With this method gained carboxylic polystyrene microsphere particle diameter is 150nm, and the distribution proportion of carboxyl on the polystyrene microsphere surface is 0.5mmol/g, apparently higher than the carboxyl of the existing method preparation distribution proportion on the polystyrene microsphere surface.
Claims (3)
1. the preparation method of carboxylic polystyrene microsphere, it is characterized in that step comprises: (1) is cleaned vinylbenzene with sodium hydroxide solution, clean with pure water again; (2) add sodium bicarbonate, water and hexenoic acid or undecylenic acid in the vinylbenzene after cleaning, form mixed solution, then under stirring, cooling off, logical nitrogen is 10～20 minutes in mixed solution; (3) heating in water bath mixed solution to 65～80 ℃ then add Potassium Persulphate, react 4～6 hours; (4) reacted 2～4 hours heating in water bath mixed solution to 81～90 ℃; (5) pure water cleans mixed solution.
2. the preparation method of carboxylic polystyrene microsphere according to claim 1 is characterized in that cinnamic content is 80～95% in the described step (2).
3. the preparation method of carboxylic polystyrene microsphere according to claim 1 and 2 is characterized in that the content of middle hexenoic acid of described step (2) or undecylenic acid is 4～20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 201010278715 CN102399340B (en) | 2010-09-13 | 2010-09-13 | Preparation method of carboxylated polystyrene microball |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010278715 CN102399340B (en) | 2010-09-13 | 2010-09-13 | Preparation method of carboxylated polystyrene microball |
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| Publication Number | Publication Date |
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| CN102399340A CN102399340A (en) | 2012-04-04 |
| CN102399340B true CN102399340B (en) | 2013-07-31 |
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| CN 201010278715 Expired - Fee Related CN102399340B (en) | 2010-09-13 | 2010-09-13 | Preparation method of carboxylated polystyrene microball |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106674403A (en) * | 2017-01-03 | 2017-05-17 | 宏葵生物（中国）有限公司 | Preparation method of polystyrene microspheres for enhancing immunoturbidimetry and application thereof |
| CN116875973B (en) * | 2023-09-07 | 2023-11-21 | 南通海星电子股份有限公司 | Preparation method of sintered foil for electrolytic capacitor |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5283079A (en) * | 1987-10-26 | 1994-02-01 | Baxter Diagnostics Inc. | Process to make magnetically responsive fluorescent polymer particles |
| CN101392172A (en) * | 2008-11-01 | 2009-03-25 | 厦门大学 | Carboxylic fluorescent encoding microsphere and synthetic method thereof |
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2010
- 2010-09-13 CN CN 201010278715 patent/CN102399340B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5283079A (en) * | 1987-10-26 | 1994-02-01 | Baxter Diagnostics Inc. | Process to make magnetically responsive fluorescent polymer particles |
| CN101392172A (en) * | 2008-11-01 | 2009-03-25 | 厦门大学 | Carboxylic fluorescent encoding microsphere and synthetic method thereof |
Non-Patent Citations (2)
| Title |
|---|
| "液相芯片中羧基功能性聚苯乙烯微球的制备、表征及其在生物检测中的应用";许艳军;《工程科技I辑》;20090831;B016-76(正文第43页3.2.2.5节，第51-54页第3.3.5节) * |
| 许艳军."液相芯片中羧基功能性聚苯乙烯微球的制备、表征及其在生物检测中的应用".《工程科技I辑》.2009,B016-76. |
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