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US 10,343,911 B2Granted
Method of producing soluble polyphosphides from red phosphorous using solution chemistry
AssigneeThe Florida State University Research Foundation, Inc.
InventorsMichael Shatruk, David Tyler McQuade, Alina Dragulescu-Andrasi, Levi Zane Miller, Chongin Pak
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Abstract
A method of producing soluble polyphosphides from red phosphorous using solution chemistry is presented. A reaction between an alkali metal alkoxy compound or alkali metal alkyl thiolate compound, such as potassium ethoxide, and shelf stable red phosphorus generated soluble polyphosphides in a variety of organic solvents with the 31P NMR spectrum being used to detect the species of polyphosphides produced.
Claims14
A method for producing polyphosphide anions soluble in organic solvents, comprising:
- providing red phosphorus or a composition of black phosphorus and red phosphorus wherein the red phosphorus has a grain size of about 1.4 mm to about 0.7 mm;
- providing an alkali metal alkoxy compound or alkali metal alkyl thiolate compound suspended in an organic solvent;
- wherein the alkali metal is sodium or potassium;
- allowing the red phosphorus and alkali metal or alkali metal compound to react, wherein the reaction uses reflux or an in-line packed column method;
- where the in-line packed column method comprises:
- providing a packing column;
- loading the packing column with the red phosphorus or composition of black phosphorus and red phosphorus in an inert environment;
- purging the packing column with an inert gas;
- setting a pressure regulator on the packing column to at least 1 bar;
- heating the packing column to a preselected temperature, where the preselected temperature is at least the boiling point of the alkali metal alkoxy compound or alkali metal alkyl thiolate wherein the temperature of the packing column or a reaction solution does not exceed the critical temperature of the organic solvent;
- suspending the alkali metal alkoxy compound or alkali metal alkyl thiolate compound in the organic solvent;
- flowing the organic solvent through the packing column;
- flowing the alkali metal alkoxy compound or alkali metal alkyl thiolate compound in the organic solvent through the packing column;
- and
- forming a compound containing the alkali metal and polyphosphide anions;
- wherein the reflux is performed for about 15 minutes to about 2 hours.
13 more elements
Dependencies are inferred from the claim text.