Preparation of mixed chlorohydrides of aluminum

Claim 2

IN A METHOD OF PREPARING LIQUID SOLUTIONS OF ALUMINUM COMPOUNDS CORRESPONDING TO THE FORMULA AIHXHAL3-X WHERE X IS 0 AND UP TO BUT NOT INCLUDING 3, THE STEPS WHICH COMPRISE REACTING AN ALKALI METAL HYDRIDE WITH ALHAL3, WHERE HAL IS HALOGEN SELECTED FROM THE GROUP CONSISTING OF CHLORINE, BROMINE AND IODINE, IN A MOLE RATIO OF ABOUT 1 TO 4 MOLES OF SAID ALKALI METAL HYDRIDE TO 1 MOLE OF SAID AIHAL3, IN A LIQUID MEDIUM COMPRISING A DIALKYL ETHER OF A GLYCOL SELECTED FROM THE GROUP CONSISTING OF ETHYLENE GLYCOL, PROPYLENE GLYCOL AND THEIR POLYGLYCOLS, SAID GLYCOL CONTAINING FROM 2 TO 8 CARBON ATOMS, THE ALKYLS OF SAID DIALKYL RADICAL CONTAINING FROM 1 TO 3 ATOMS, WHEREBY TO PRODUCE A FINAL CONCENTRATION BETWEEN ABOUT 0.1 AND 2 MOLES OF THE AIHXHAL3-X PER LITER IN SAID SOLUTIONS.

Claim 3

The method of claim 1, in which the liquid medium also includes a liquid aromatic hydrocarbon, the volume ratio of said dialkyl ether to said hydrocarbon being from 1 to 4 of said dialkyl ether to 1 of said hydrocarbon.

Claim 4

The method of claim 2, in which the alkali metal hydride is lithium hydride, and Hal is chlorine.

Claim 5

The method of claim 3, in which the liquid hydrocarbon is at least one member selected from the group consisting of benzene and toluene.

Claim 6

The method of claim 4, in which there is included in the reaction mixture an initiator in the form of at least one member selected from the group consisting of a preformed AlH3 and an alkali metal tetrahydridoaluminate, said initiator being utilized in amounts of about 0.5 to 5% by weight of the lithium hydride.

Claim 7

The method of claim 1, in which the alkyl groups of said dialkyl ether are methyl.

Claim 8

The method of claim 4, in which the alkyl groups of said dialkyl ether are methyl.

Claim 9

IN A METHOD OF PREPARING LIQUID AROMATIC HYDROCARBON SOLUTIONS OF MIXED CHLOROHYDRIDES OF ALUMINUM, THE STEPS WHICH COMPRISES: A. PROVIDING A SLURRY OF LIH IN A DIALKYL ETHER OF A MEMBER SELECTED FROM THE GROUP CONSISTING OF ETHYLENT GLYCOL, DIETHYLENE GLYCOL, TRIETHYLENE GLYCOL AND TETRAETHYLENE GLYCOL AND IN WHICH EACH ALKYL CONTAINS FROM 1 TO 2 CARBON ATOMS, B. PROVIDING A SOLUTION OF AICI3 IN AT LEAST ONE LIQUID AROMATIC HYDROCARBON SELECTED FROM THE GROUP CONSISTING OF BENZENE AND TOLUENE, SAID SOLUTION ALSO CONTAINING DIMETHYL ETHER, THE VOLUME RATIO OF SAID DIALKYL ETHER TO SAID HYDROCARBON BEING FROM 1 TO 4 OF SAID DIALKYL ETHER TO 1 OF SAID HYDROCARBON, C. THE INGREDIENTS BEING PROPORTIONED SO THAT THE MOLE TATIO OF LIH TO SICI3 IN THE (A) AND (B) COMPOSITION IS ABOUT 1 TO 4 OF LIH TO 1 OF AICI3, AND D. GRADUALLY ADDING THE (B) SOLUTION TO THE (A) SLURRY, WHEREBY TO PRODUCE A FINAL CONCENTRATION BETWEEN ABOUT 0.1 AND 2 MOLES PER LITER OF THE MIXED CHLOROHYDRIDES OF ALUMINUM IN SAID SOLUTIONS.

Claim 10

IN A METHOD OF PREPARING LIQUID AROMATIC HYDROCARBON SOLUTIONS OF MIXED CHLOROHYDRIDES OF ALUMINUM, THE STEPS WHICH COMPRISES: A. PROVIDING A SLURRY OF LIH IN A DIALKYL ETHER OF A MEMBER SELECTED FROM THE GROUP CONSISTING OF ETHYLENT GLYCOL, DIETHYLENE GLYCOL, TRIETHYLENE GLYCOL AND TETRAETHYLENE GLYCOL AND IN WHICH EACH ALKYL CONTAINS FROM 1 TO 2 CARBON ATOMS, B. PROVIDING A SOLUTION OF AICI3 IN AT LEAST ONE LIQUID AROMATIC HYDROCARBON SELECTED FROM THE GROUP CONSISTING OF BENZENE AND TOLUENE, SAID SOLUTION ALSO CONTAINING DIMETHYL ETHER, THE VOLUME RATIO OF SAID DIALKYL ETHER TO SAID HYDROCARBON BEING FROM 1 TO 4 OF SAID DIALKYL ETHER TO 1 OF SAID HYDROCARBON, C. THE INGREDIENTS BEING PROPORTIONED SO THAT THE MOLE TATIO OF LIH TO SICI3 IN THE (A) AND (B) COMPOSITION IS ABOUT 1 TO 4 OF LIH TO 1 OF AICI3, AND D. GRADUALLY ADDING THE (B) SOLUTION TO THE (A) SLURRY, WHEREBY TO PRODUCE A FINAL CONCENTRATION BETWEEN ABOUT 0.1 AND 2 MOLES PER LITER OF THE MIXED CHLOROHYDRIDES OF ALUMINUM IN SAID SOLUTIONS.

Claim 11

In a method of preparing liquid solutions of mixed chlorohydrides of aluminum, the steps which comprise: a. providing a sLurry of LiH in a dialkyl ether of a member selected from the group consisting of ethylene glycol, diethylene glycol, triethylene glycol and tetraethylene glycol and in which each alkyl contains from 1 to 2 carbon atoms, b. providing a solution of AlCl3 and NaCl or LiCl in a substantially 1:1 molar ratio in a dialkyl ether of a glycol selected from the group consisting of ethylene glycol, propylene glycol and their polyglycols, said glycol containing from 2 to 8 carbon atoms, the alkyls of said dialkyl radical containing from 1 to 3 carbon atoms, c. The ingredients being proportioned so that the mole ratio of LiH to AlCl3 in the (a) and (b) compositions is about 1 to 4 of LiH to 1 of AlCl3, and d. gradually adding the (b) solution to the (a) slurry, whereby to produce a final concentration between about 0.1 and 2 moles per liter of the mixed chlorohydrides of aluminum in said solutions.

Claim 12

In a method of preparing liquid solutions of mixed chlorohydrides of aluminum, the steps which comprise: a. providing a sLurry of LiH in a dialkyl ether of a member selected from the group consisting of ethylene glycol, diethylene glycol, triethylene glycol and tetraethylene glycol and in which each alkyl contains from 1 to 2 carbon atoms, b. providing a solution of AlCl3 and NaCl or LiCl in a substantially 1:1 molar ratio in a dialkyl ether of a glycol selected from the group consisting of ethylene glycol, propylene glycol and their polyglycols, said glycol containing from 2 to 8 carbon atoms, the alkyls of said dialkyl radical containing from 1 to 3 carbon atoms, c. The ingredients being proportioned so that the mole ratio of LiH to AlCl3 in the (a) and (b) compositions is about 1 to 4 of LiH to 1 of AlCl3, and d. gradually adding the (b) solution to the (a) slurry, whereby to produce a final concentration between about 0.1 and 2 moles per liter of the mixed chlorohydrides of aluminum in said solutions.

Claim 13

The method of claim 8, in which said (a) slurry also contains an initiator in the form of at least one member selected from the group consisting of a preformed AlH3 and an alkali metal tetrahydridoaluminate, said initiator being utilized in amounts of about 0.5 to 5% by weight of the LiH.

Claim 14

The method of claim 8, in which during step (d) at least a part of the dimethyl ether is allowed to evaporate from the reaction mixture.

Claim 15

The method of claim 9, in which said (a) slurry also contains an initiator in the form of at least one member selected from the group consisting of a preformed AlH3 and an alkali metal tetrahydridoaluminate, said initiator being utilized in amounts of about 0.5 to 5% by weight of the LiH.

Claim 16

The method of claim 6, in which the alkyl groups of said dialkyl ether are methyl.

Claim 17

A solution of a halohydride of aluminum in a liquid aromatic hydrocarbon solvent and a dialkyl ether of a glycol selected from the group consisting of ethylene glycol, propylene glycol and their polyglycols, said glycol containing from 2 to 8 carbon atoms, the alkyls of said dialkyl radical containing from 1 to 3 carbon atoms, said solution containing from about 0.1 to 2 moles of said halohydride of aluminum per liter, said halohydride corresponding to the formula AlHnClm where the sum of n and m is 3, and also halo of said halohydride being selected from the group consisting of chlorine, bromine, and iodine.

Claim 18

A solution of a halohydride of aluminum in a liquid aromatic hydrocarbon solvent and a dialkyl ether of a glycol selected from the group consisting of ethylene glycol, propylene glycol and their polyglycols, said glycol containing from 2 to 8 carbon atoms, the alkyls of said dialkyl radical containing from 1 to 3 carbon atoms, said solution containing from about 0.1 to 2 moles of said halohydride of aluminum per liter, said halohydride corresponding to the formula AlHnClm where the sum of n and m is 3, and also halo of said halohydride being selected from the group consisting of chlorine, bromine, and iodine.

Claim 19

A solution according to claim 14, in which the alkyl groups of said dialkyl ether are methyl groups.

Claim 20

A solution according to claim 15, in which the aromatic hydrocarbon solvent is a member selected from the group consisting of benzene and toluene.