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US 10,329,151 B2Granted
Method of converting red phosphorous to soluble polyphosphides using alkali metal compounds in a combination of tetrahydrofuran and dimethoxyethane
AssigneeThe Flrida 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 generating soluble polyphosphides using solution chemistry is presented. A reaction between potassium ethoxide in THF/DME 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 a combination of tetrahydrofuran and dimethoxyethane;
- 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;
- suspending the alkali metal alkoxy compound or alkali metal alkyl thiolate compound in the combination of tetrahydrofuran and dimethoxyethane;
- flowing the combination of tetrahydrofuran and dimethoxyethane through the packing column;
- flowing the alkali metal alkoxy compound or alkali metal alkyl thiolate compound in the combination of tetrahydrofuran and dimethoxyethane 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.