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US 10,329,152 B2Granted
Method of synthesizing soluble polyphosphides from red phosphorous
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 synthesizing soluble polyphosphides using shelf-stable reagents and common organic solvents is presented. A reaction between an alkali metal alkoxy compound or alkali metal alkyl thiolate compound 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.
Claims13
A method for producing polyphosphide anions soluble in organic solvents, comprising:
- providing red phosphorus or a composition of black phosphorus and red phosphorus;
- 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 and 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;
- forming a compound containing the alkali metal and polyphosphide anions;
- evaporating the organic solvent off the compound containing the alkali metal and polyphosphide anions;
- redissolving the compound containing the alkali metal and polyphosphide anions in ethanol;
- and
- separating the black phosphorus from the polyphosphide anions.
15 more elements
Dependencies are inferred from the claim text.