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A kind of preparation method of thermosensitive fluorescent polymer

A fluorescent polymer and temperature-sensitive technology, applied in the preparation of microspheres, microcapsule preparations, etc., can solve the problems of easy demulsification into flocs, difficult removal of emulsifier residues, and difficulty in formulating small particle size emulsification systems. Achieve the effects of mild reaction conditions, high reaction yield and good monodispersity

Active Publication Date: 2016-04-06
XIAMEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the emulsion polymerization method is a mainstream method for preparing functional polymer nanospheres. By adjusting the amount of initiator, monomer amount, temperature, pH, stirring intensity, emulsifier type and amount, etc., different particle sizes and monodisperse particles can be prepared. However, there are problems such as the particle size of the microsphere is mostly larger than 200nm, the small particle size emulsification system is difficult to prepare, the emulsifier residue is difficult to remove, and the small particle size (<100nm) copolymer nanosphere technology is immature.
ZL200910234001.1 provides a method for preparing monodisperse polymer nanospheres, which combines soap-free emulsion polymerization and traditional emulsion polymerization techniques to prepare monodisperse homopolymer and copolymer nanospheres. The prepared homopolymer The particle size of the sphere is small (<100nm) and the particle size is uniform, but the emulsification system of the copolymer nanosphere (especially the copolymerization of lipophilic and hydrophilic monomers) is difficult to prepare, and it is easy to break into floc; CN103342768A discloses A method for preparing PMMA microspheres with a core-shell structure by soap-free emulsion polymerization. This method is simple and does not require an emulsifier, but the particle size of the microspheres is about 200nm, and small particle size (<100nm) nanospheres cannot be prepared.

Method used

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  • A kind of preparation method of thermosensitive fluorescent polymer
  • A kind of preparation method of thermosensitive fluorescent polymer
  • A kind of preparation method of thermosensitive fluorescent polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] (1) Synthesis of NMA monomer: Add 1.4319g (0.01moL) N-α-naphthylamine, 100mL benzene and 1.67mL (0.012moL) to a 250mL two-neck flask equipped with a dropping funnel, condenser, and magnetic stirrer Triethylamine, magnetically stirred in an ice bath until uniform to 0 °C. Continue stirring in the ice bath, and slowly add 1.16 mL (0.01 moL) of methacryloyl chloride dissolved in 15 mL of benzene into the above mixed solution with a dropping funnel. Heat the mixture to 40°C, react for 2 hours and cool to room temperature, filter to remove the formed triethylamine hydrochloride solid, collect the filtrate in a separatory funnel, and wash with distilled water, dilute hydrochloric acid, and dilute NaHCO successively 3 Wash each solution 3 times, add 5g of anhydrous magnesium sulfate, stir and dry, filter to obtain the product benzene solution, remove the solvent benzene by rotary evaporation to obtain a crude product, recrystallize in methanol 3 times to obtain 1.904g of white...

Embodiment 2

[0042] Steps (1) to (3) are the same as in Example 1.

[0043] Step (4) P(St-co-NMA) m -b-PPEGMA n Preparation of nanospheres: prepare 1mL2mg / mLP (St 83 -co-NMA 4 )-PPEGMA 18 / THF solution, slowly drop 50 μL of the above THF solution into 2 mL of deionized water stirred at high speed, stir at a constant speed with the open mouth open for 24 hours, and obtain P(St 83 -co-NMA 4 )-PPEGMA 18 Aqueous solution of nanoparticles. According to the DLS test, the particle size of nano-microspheres is 86nm at 25°C, and the particle size decreases continuously as the temperature rises gradually within the temperature range of 25-60°C.

Embodiment 3

[0045] Steps (1) to (3) are the same as in Example 1.

[0046] Step (4) P(St-co-NMA) m -b-PPEGMA n Preparation of nanospheres: prepare 1mL5mg / mLP (St 83 -co-NMA 4 )-PPEGMA 18 / 1,4-dioxane solution, slowly drop 50 μL of the above-mentioned dioxane solution into 2 mL of deionized water stirred at high speed, stir at a constant speed for 24 hours, and obtain P( St. 83 -co-NMA 4 )-PPEGMA 18 Aqueous solution of nanoparticles. The particle size of the nano-microspheres was 118nm at 25°C by DLS test, and the particle size decreased continuously when the temperature was gradually raised within the temperature range of 25-60°C.

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Abstract

The invention discloses a preparation method of a thermo-sensitive fluorescent polymer. The preparation method comprises the following steps: (1) synthesizing an NMA (N-alpha-naphthyl methacrylamide) monomer; (2) synthesizing a P(St-co-NMA)m (poly(styrene-co-NMA) macromolecular chain transfer agent; (3) synthesizing P(St-co-NMA)m-b-PENGMAn (P(St-co-NMA)m-b-poly(polyethylene glycol methacrylate)), namely the thermo-sensitive fluorescent polymer. According to the preparation method, the prepared nanoparticles simultaneously have thermosensitivity and fluorescence, and a series of fluorescent nanoparticles with different particle sizes can be prepared by changing external conditions.

Description

technical field [0001] The invention specifically relates to a preparation method of a temperature-sensitive fluorescent polymer. Background technique [0002] Environmentally responsive functional polymers have become a research hotspot in recent years. When the external environment (such as light, temperature, pH, ionic strength, electric field and magnetic field, etc.) changes, some physical or chemical properties of the polymer (morphology, Size, catalysis, recognition, etc.) will undergo corresponding reversible or irreversible changes, and has potential application value in the fields of controlled drug release, separation, microelectronics, optics, and catalysis. [0003] At present, the emulsion polymerization method is a mainstream method for preparing functional polymer nanospheres. By adjusting the amount of initiator, monomer amount, temperature, pH, stirring intensity, emulsifier type and amount, etc., different particle sizes and monodisperse particles can be p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F299/02C08F2/38C08F212/08C08F220/54C08J3/07B01J13/02
Inventor 戴李宗程玲罗伟昂宋存峰项佳懿许一婷何凯斌刘新瑜
Owner XIAMEN UNIV
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