Method of making dye-doped polystyre microparticles

Patent metadata

Field	Value
Publication number	US-9957336-B2
Application number	US-201514706585-A
Country	US
Kind code	B2
Filing date	May 7, 2015
Priority date	May 8, 2014
Publication date	May 1, 2018
Grant date	May 1, 2018

Abstract

Various embodiments provide dye-doped polystyrene microspheres generated using dispersion polymerization. Polystyrene microspheres may be doped with fluorescent dyes, such as xanthene derivatives including kiton red 620 (KR620), using dispersion polymerization. Certain functionalities, such as sodium styrene sulfonate, may be used to shift the equilibrium distribution of dye molecules to favor incorporation of the dye into the particles. Polyelectrolyte materials, such as poly(diallyldimethyl ammonium chloride), PolyDADMAC, may be used to electrostatically trap and bind dye molecules within the particles. A buffer may be used to stabilize the pH change of the solution during dye-doped polystyrene microsphere generation and the buffer may be selected depending on the pKa of the dye being incorporated. The various embodiments may provide dye-doped polystyrene microspheres, such as KR620-doped polystyrene microspheres that are non-toxic and non-carcinogenic. These non-toxic and non-carcinogenic dye-doped polystyrene microspheres may be suitable for use in wind tunnel testing.

First claim

What is claimed is:

1. A method of making a dye-doped polystyrene microsphere, comprising:
providing a first amount of a styrene monomer;
providing a second amount of a radical initiator;
providing a third amount of a fluorescent dye;
providing a fourth amount of a functionalized monomer selected to impart a charge on the styrene monomer;
providing a fifth amount of a polyelectrolyte material of opposite charge to the functionalized monomer; and
reacting the first amount of a styrene monomer, the second amount of a radical initiator, the third amount of a fluorescent dye, the fourth amount of a functionalized monomer, and the fifth amount of a polyelectrolyte material together in an inert atmosphere to generate the dye-doped polystyrene microsphere having a mean diameter from about 0.5 μm to about 1.5 μm.

2. The method of claim 1 , further comprising providing a sixth amount of a buffer material, wherein reacting the first amount of a styrene monomer, the second amount of a radical initiator, the third amount of a fluorescent dye, the fourth amount of a functionalized monomer, and the fifth amount of a polyelectrolyte, material together in an inert atmosphere to generate the dye-doped polystyrene microsphere comprises reacting the first amount of a styrene monomer, the second amount of a radical initiator, the third amount of a fluorescent dye, the fourth amount of a functionalized monomer, the fifth amount of a polyelectrolyte material, and the sixth amount of the buffer material together in an inert atmosphere to generate the dye-doped polystyrene microsphere.

3. The method of claim 2 , wherein the radical initiator is potassium persulfate.

4. The method of claim 3 , wherein the fluorescent dye has a positive charge or a negative charge.

5. The method of claim 4 , wherein the fluorescent dye is kiton red 620 (KR620).

6. The method of claim 2 , wherein the functionalized monomer is a functionalized styrene monomer or a functionalized acrylate monomer.

7. The method of claim 6 , wherein the functionalized monomer is sodium styrene sulfonate.

8. The method of claim. 2 , wherein the polyelectrolyte material is poly(diallyldimethyl ammonium chloride) (polyD).

9. The method of claim 2 , wherein the buffer material is sodium bicarbonate.

10. The method of claim 9 , wherein:
the radical initiator is potassium persulfate;
the fluorescent dye is kiton red 620 (KR620);
the functionalized monomer is sodium styrene sulfonate;
the polyelectrolyte material is poly(diallyldimethyl ammonium chloride) (polyD);
the first amount of the styrene monomer is 33 mL;
the third amount of the KR620 is 5 milligrams to 50 milligrams; and
the second amount of the potassium persulfate is 0,2059 grams.

11. The method of claim 9 , wherein:
the radical initiator is potassium persulfate;
the fluorescent dye is kiton red 620 (KR620);
the functionalized monomer is sodium styrene sulfonate;
the polyelectrolyte material is poly (diallyldimethyl ammonium chloride) (polyD);
the first amount of the styrene monomer is 187 grams;
the fourth amount of the sodium styrene sulfonate is 20 grams;
the fifth amount of the polyD is 0.8 grams;
the sixth amount of the sodium bicarbonate is 12 grams;
the third amount of the KR620 is 0.4 grams; and
the second amount of the potassium persulfate is 1.6 grams.

12. The method of claim 9 , further comprising providing a seventh amount of a cross linking agent, wherein reacting the first amount of a styrene monomer, the second amount of a potassium persulfate, the third amount of a xanthene dye, the fourth amount of a functionalized monomer, the fifth amount of a polyelectrolyte material, and the sixth amount of the buffer material together in an inert atmosphere to generate the dye-doped polystyrene microsphere comprises reacting the first amount of a styrene monomer, the second amount of a potassium persulfate, the third amount of a xanthene dye, the fourth amount of a functionalized monomer, the fifth amount of a polyelectrolyte material, the sixth amount of the buffer material, and the seventh amount of the cross linking agent together in an inert atmosphere to generate the dye-doped polystyrene microsphere.

13. The method of claim 12 , wherein the cross linking agent is divinylbenzene.

14. The method of claim 1 , where the dye-doped polystyrene microsphere has a mean diameter of about 1 μm.

Assignees

• The United States Of America Represented By The Administrator Of The Nat Aeronautics And Space Admin
• Nasa

Inventors

• Wohl Jr Christopher J
• Tiemsin Pacita I
• Danehy Paul M
• Danley Jason E

Classifications

• C08F212/30 Primary

  Sulfur · CPC title

• G01M9/04

  Details · CPC title

• C09D11/50

  Sympathetic, colour changing or similar inks · CPC title

• C09K11/025

  non-luminescent particle coatings or suspension media · CPC title

• C09D11/328

  characterised by dyes · CPC title