Initiated chemical vapor deposition of vinyl polymers for the encapsulation of particles
Described herein are all-dry encapsulation methods that enable well-defined polymers to be applied around particles. One aspect of the invention relates to a method of coating a particle, comprising the steps of: placing said particle in a vessel at a pressure; rotating said vessel at a rotating speed for a period of time; mixing together a first gaseous monomer at a first flow rate, and a gaseous initiator at a second flow rate, thereby forming a mixture; introducing said mixture into said vessel via a vapor feedline; heating said mixture, thereby forming a reactive mixture; contacting said particle with said reactive mixture; thereby forming a polymer coating on said particle. The methods may be modified forms of initiated chemical vapor deposition using a thermally-initiated radical polymerization to create conformal coatings around individual particles while avoiding agglomeration. Particle surfaces may be coated with a range of functional groups.
1. A method, comprising the steps of:
placing a plurality of individual particles in a vessel at a pressure; wherein said vessel comprises a vapor feedline for delivering vapors into said vessel through exit holes, and a filament in proximity to said exit holes; the individual particles consist of soda glass, silica, carbon, or a drug; and the diameters of said individual particles are about 5 μm to about 35 μm;
contacting said vessel with a water bath at a first temperature, wherein said first temperature is between about 0° C. and about 100° C.;
rotating said vessel at a rotating speed for a period of time;
mixing together a first gaseous monomer at a first flow rate, and a gaseous initiator at a second flow rate, thereby forming a mixture;
introducing said mixture into said vessel via said vapor feedline which comprises said filament at a second temperature, wherein said second temperature is between about 150° C. and 350° C.;
heating said mixture with said filament, thereby forming a reactive mixture;
contacting said plurality of individual particles with said reactive mixture; thereby forming a plurality of individual coated particles, wherein each individual coated particle consists of a substantially uniform polymer coating encapsulating one individual particle; the thickness of said substantially uniform polymer coating is about 3 μm to about 12 μm; each individual particle is non-agglomerated; and the plurality of individual coated particles is non-agglomerated.
2. The method of claim 1 , wherein the gaseous initiator is selected from the group consisting of compounds of formula I:
A-X—B I
wherein,
A is hydrogen, alkyl, cycloalkyl, aryl, heteroaryl, aralkyl or heteroaralkyl;
X is —O—O—or —N═N—; and
B is hydrogen, alkyl, cycloalkyl, aryl, heteroaryl, aralkyl or heteroaralkyl.
3. The method of claim 1 , wherein the gaseous initiator is selected from the group consisting of hydrogen peroxide, alkyl peroxides, aryl peroxides, hydroperoxides, halogens and azo compounds.
4. The method of claim 1 , wherein said first gaseous monomer is selected from the group consisting of
R is selected from the group consisting of hydrogen and alkyl;
R 1 is selected from the group consisting of hydrogen, alkyl, aralkyl, heteroaralkyl, and carboxyl;
R 2 is independently selected from the group consisting of hydrogen, alkyl, bromine, chlorine, hydroxyl, alkoxy, aryloxy, carboxyl, amino, acylamino, amido, carbamoyl, sulfhydryl, sulfonate, and sulfoxido;
X is selected from the group consisting of hydrogen, alkyl, cycloalkyl, heteocycloalkyl, aryl, heteroaryl, aralkyl, heteoaralkyl, and —(CH 2 ) n Y;
Y is selected from the group consisting of hydrogen, alkyl, cycloalkyl, heterocycloalkyl, aryl, heteroaryl, aralkyl, heteoaralkyl, nitro, halo, hydroxyl, alkoxy, aryloxy, carboxyl, heteroaryloxy, amino, acylamino, amido, carbamoyl, sulfhydryl, sulfonate, and sulfoxido;
and
n is 1-10 inclusive.
5. The method of claim 4 , wherein R is methyl.
6. The method of claim 4 , wherein X is hydrogen or —(CH 2 ) n Y.
7. The method of claim 4 , wherein Y is alkyl, cycloalkyl, heterocycloalkyl, aryl, nitro, halo, hydroxyl, alkoxy, aryloxy, amino, acylamino, amido, or carbamoyl.
8. The method of claim 4 , where n is 3-8 inclusive.
9. The method of claim 4 , wherein said first gaseous monomer is selected from the group consisting of
R is selected from the group consisting of hydrogen and methyl;
R 2 is independently selected from the group consisting of hydrogen, methyl, bromine and chlorine;
X is hydrogen or —(CH 2 ) 2 Y;
Y is selected from the group consisting of hydrogen, alkyl, cycloalkyl, heterocycloalkyl, aryl, heteroaryl, aralkyl, heteoaralkyl, nitro, halo, hydroxyl, alkoxy, aryloxy, carboxyl, heteroaryloxy, amino, acylamino, amido, carbamoyl, sulfhydryl, sulfonate, and sulfoxido;
and
n is 1-10 inclusive.
10. The method of claim 9 , wherein R is methyl.
11. The method of claim 9 , wherein Y is hydrogen or heterocycloalkyl.
12. The method of claim 9 , wherein Y is hydrogen.
13. The method of claim 9 , wherein Y is an oxirane.
14. The method of claim 9 , wherein n is 3-8 inclusive.
15. The method of claim 1 , wherein said individual particles consist of soda glass.
16. The method of claim 1 , wherein the average particle size of the plurality of individual coated particles is not more than 5% larger than the average particle size of the plurality of individual particles, apart from the particle size increase attributable to the coating itself.
17. The method of claim 1 , wherein said individual particles consist of silica.
18. The method of claim 1 , wherein said individual particles consist of carbon.
19. The method of claim 1 , wherein said individual particles consist of carbon in the form of graphite, a fullerene, a nanotube, or diamond.
20. The method of claim 1 , wherein said individual particles consist of a drug.