Lithium-porous metal oxide compositions and lithium reagent-porous metal compositions

Abstract

The invention relates to lithium metal/porous metal oxide compositions. These lithium metal compositions are prepared by mixing liquid lithium metal with a porous metal oxide in an inert atmosphere under exothermic conditions sufficient to absorb the liquid lithium metal into the porous metal oxide pores. The lithium metal/porous metal oxide compositions of the invention are preferably loaded with lithium metal up to about 40% by weight, with about 20% to 40% by weight being the most preferred loading. The invention also relates to lithium reagent-porous metal oxide compositions having RLi absorbed into a porous oxide. In formula RLi, R is an alkyl group, an alkenyl group, an alkynyl group, an aryl group, an alkaryl group, or an NR 1 R 2 group; R 1 is an alkyl group, an alkenyl group, an alkynyl group, an aryl group, an alkaryl group; and R 2 is hydrogen, an alkyl group, an alkenyl group, an alkynyl group, an aryl group, and an alkaryl group. The preparation and use of these compositions are also described.

1 . A lithium metal/porous metal oxide composition prepared by a process comprising:
 mixing liquid lithium metal with a porous metal oxide in an inert atmosphere under exothermic conditions sufficient to absorb the liquid lithium metal into the porous metal oxide pores.   
     
     
         2 . The lithium metal/porous metal oxide composition of  claim 1 , wherein the lithium metal is loaded up to about 40% by weight, the pores of the porous metal oxide have an average pore size of 30 Å to 500 Å, and the porous metal oxide is selected from porous alumina, porous titanium oxide, porous calcium oxide, porous zirconia, porous iron oxide, porous Co 3 O 4 , porous metal phosphate, porous hybrid phosphosilicate, porous aluminates, porous vanadates, and molybdates. 
     
     
         3 . The lithium metal/porous metal oxide composition of  claim 2 , wherein the lithium metal is loaded to about 20% to 40% by weight. 
     
     
         4 . The lithium metal/porous metal oxide composition of  claim 2 , wherein the porous metal oxide is alumina. 
     
     
         5 . The lithium metal/porous metal oxide composition of  claim 2 , wherein the pores of the porous metal oxide have an average pore size of 60 Å to 190 Å. 
     
     
         6 . A method for preparing a lithium reagent-porous metal oxide composition comprising the steps of:
 mixing liquid lithium metal with a porous metal oxide in an inert atmosphere under exothermic conditions sufficient to absorb the liquid lithium metal into the porous metal oxide, and   reacting the resulting lithium metal/porous metal oxide composition with a compound RX at a temperature of about −80° C. to 0° C.,   wherein R is an alkyl group, an alkenyl group, an alkynyl group, an aryl group, an alkaryl group, or an NR 1 R 2  group;   R 1  is an alkyl group, an alkenyl group, an alkynyl group, an aryl group, an alkaryl group or an Si(R 3 ) 3  group;   R 2  is hydrogen, an alkyl group, an alkenyl group, an alkynyl group, an aryl group, an alkaryl group, or an Si(R 3 ) 3  group;   R 3  is an alkyl group, an alkenyl group, an alkynyl group, an aryl group, or an alkaryl group; and   X is a halogen.   
     
     
         7 . The method for preparing a lithium reagent-porous metal oxide composition of  claim 6 , wherein the lithium metal is loaded up to about 40% by weight, the pores of the porous metal oxide have an average pore size of 30 Å to 500 Å, and the porous metal oxide is selected from porous alumina, porous titanium oxide, porous calcium oxide, porous zirconia, porous iron oxide, porous Co 3 O 4 , porous metal phosphate, porous hybrid phosphosilicate, porous aluminates, porous vanadates, and molybdates. 
     
     
         8 . The method for preparing a lithium reagent-porous metal oxide composition of  claim 6 , wherein the lithium metal is loaded to about 20% to 40% by weight. 
     
     
         9 . The method for preparing a lithium reagent-porous metal oxide composition of  claim 6 , wherein the porous metal oxide is alumina. 
     
     
         10 . The method for preparing a lithium reagent-porous metal oxide composition of  claim 6 , wherein the pores of the porous metal oxide have an average pore size of 60 Å to 190 Å. 
     
     
         11 . A method for preparing an organolithium-porous metal oxide composition comprising the step of:
 mixing lithium metal, a porous metal oxide, and an alkyl halide solution in the presence of a solvent under conditions sufficient to absorb the lithium into the pores of the porous metal oxide, and   evaporating any excess solvent.   
     
     
         12 . The method for preparing an organolithium-porous metal oxide composition of  claim 11 , wherein the lithium metal is loaded up to about 40% by weight, the pores of the porous metal oxide have an average pore size of 30 Å to 500 Å, and the porous metal oxide is selected from porous alumina, porous titanium oxide, porous calcium oxide, porous zirconia, porous iron oxide, porous Co 3 O 4 , porous metal phosphate, porous hybrid phospho silicate, porous aluminates, porous vanadates, and molybdates. 
     
     
         13 . The method for preparing an organolithium-porous metal oxide composition of  claim 11 , wherein the lithium metal is loaded to about 20% to 40% by weight. 
     
     
         14 . The method for preparing an organolithium-porous metal oxide composition of  claim 11 , wherein the porous metal oxide is alumina. 
     
     
         15 . The method for preparing an organolithium-porous metal oxide composition of  claim 11 , wherein the pores of the porous metal oxide have an average pore size of 60 Å to 190 Å. 
     
     
         16 . A method of absorbing an organolithium species into the pores of a porous material, comprising:
 contacting the organolithium species with the porous material under cold conditions, wherein the porous material is selected from the group consisting of porous silica gel and a porous metal oxide,   distilling any excess solvent, and   drying the resulting organolithium material.