Method for preparing monodisperse polymer nano-microspheres

A nano-microsphere and monodispersity technology, which is applied in the field of preparing monodisperse polymer nano-microspheres, can solve the problems of difficulty in ensuring the size and monodispersity of polymer microspheres, prolonging the nucleation time, and homogeneous nucleation. The size of the microspheres is easy to control, the product repeatability is good, and the effect of increasing the nucleation density

Inactive Publication Date: 2012-05-30
NANJING TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method is also not suitable for the preparation of microspheres <100nm
[0004] Although traditional emulsion polymerization is often used to prepare nanospheres, the process involved in the preparation of monodisperse microspheres by this method is complex and difficult to control
On the one hand, reducing the amount of emulsifier can shorten the nucleation time, but it may induce homogeneous nucleation, resulting in a bimodal particle size distribution of the generated polymer microspheres
If the amount of emulsifier is increased, homogeneous nucleation can be avoided, but the nucleation time is prolonged, resulting in a broadening of the microsphere size distribution
Microemulsion polymerization is also a common method for preparing nano-microspheres, but this method consumes a large amount of surfactant and brings great trouble to the cleaning of polymer microspheres
Although miniemulsion polymerization can prepare nanoscale polymer microspheres, it often requires efficient emulsification and homogenization equipment, and the process is difficult to control, and it is difficult to ensure the monodispersity of polymer microspheres.

Method used

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  • Method for preparing monodisperse polymer nano-microspheres
  • Method for preparing monodisperse polymer nano-microspheres
  • Method for preparing monodisperse polymer nano-microspheres

Examples

Experimental program
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Effect test

Embodiment 1

[0026] In a 250mL three-necked flask equipped with a condenser, add 96mL of deionized water and 0.17g of sodium lauryl sulfate to form a transparent solution. During stirring, 2.5 mL of styrene was added. Nitrogen was passed for 15 minutes, and the reaction system was heated to raise the temperature to 70°C. Then add 4 mL of an aqueous solution containing 0.13 g of potassium persulfate, stir at 200 rpm, and react for 4 hours to obtain monodisperse polystyrene microspheres with a diameter of 77 nm and a PDI of 1.005. Its typical scanning electron microscope pictures are as follows: figure 1 As shown, the average diameter of the microspheres is 77 nm, and the PDI is 1.005.

Embodiment 2

[0028] In a 250mL three-necked flask equipped with a condenser, add 96mL of deionized water and 0.09g of sodium dodecylsulfonate to form a transparent solution. During stirring, 10 mL of methyl methacrylate was added. Nitrogen was passed for 15 minutes, and the reaction system was heated to raise the temperature to 80°C. Then add 4 mL of an aqueous solution containing 0.09 g of potassium persulfate, stir at a speed of 300 rpm, and react for 3 hours to obtain monodisperse polymethyl methacrylate microspheres with an average diameter of 59 nm and a PDI of 1.01. Its typical scanning electron microscope pictures are as follows: figure 2 As shown, the average diameter of the microspheres is 59 nm, and the PDI is 1.01.

Embodiment 3

[0030] In a 250mL three-necked flask equipped with a condenser, add 71mL of deionized water, 32mL of absolute ethanol, and 0.45g of dodecyltrimethylammonium bromide to form a transparent solution. During stirring, 2.5 mL of divinylbenzene was added. Nitrogen was passed for 15 minutes, and the reaction system was heated to raise the temperature to 60°C. Then add 4 mL of an aqueous solution containing 0.13 g of ammonium persulfate, stir at 400 rpm, and react for 2 hours to obtain monodisperse polydivinylbenzene microspheres with a diameter of 61 nm and a PDI of 1.01.

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Abstract

The invention relates to a method for preparing high-monodispersity polymer nano-microspheres. By adopting innovative measures of adding surfactant in a concentration lower than critical micelle concentration to a polymerization reaction system, stabilizing primary particles generated by homogeneous nucleation in an early stage of polymerization, introducing an appropriate amount of polar solventto improve the critical micelle concentration of the surfactant in a dispersion medium and increase the solubility of monomers in the dispersion medium, and the like, the method effectively increasesthe stability of the primary particles generated by homogeneous nucleation in the early stage of polymerization, shortens polymerization time, and finally obtains polymer microspheres which have particle size less than 100 nm and are highly uniform in size distribution. The method is different from soap-free emulsion polymerization and conventional emulsion polymerization methods, simple in preparation process and easy to control, and the obtained polymer nano-microspheres are excellent in monodispersity. The products of each batch are good in reproducibility, so the method is easy to realizeindustrialization.

Description

technical field [0001] The invention relates to a method for preparing monodisperse polymer nanospheres, in particular to a simple and efficient method for preparing highly monodisperse polymer nanospheres, which can be widely used in biological sciences, medical diagnosis and treatment, electronics and Optoelectronics science, standard metrology, chromatographic analysis and other fields. Background technique [0002] Monodisperse polymer nanospheres refer to polymer microspheres with the same particle shape, diameter <100nm, and uniform size distribution. In recent years, due to the wide application of polymer microspheres in biological science, medical diagnosis and treatment, electronic and optoelectronic device technology, more and more people pay more and more attention, and the preparation methods involved are also various. [0003] Soap-free emulsion polymerization is a very effective method for preparing monodisperse polymer microspheres. However, since no surf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J13/14
Inventor 曾燕伟胡振兴
Owner NANJING TECH UNIV
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