Method for storing and/or transporting gallium chloride

Abstract

Method for storing and/or transporting GaCl.sub.3 involving the step of adding an aluminium compounds of the formula R.sub.3-xAlCl.sub.x, wherein R is a linear or branched alkyl group with 1-8 carbon atoms and x is 0 or 1, to said GaCl.sub.3 in an Al/Ga molar ratio of at least 0.2, thereby forming a liquid formulation, followed by introducing said liquid formulation in a container.

Claims

1. A method for storing and/or transporting GaCl.sub.3, comprising: adding an aluminum compound chosen from trimethylaluminum, triethylaluminum, tri(n-butyl) aluminum chloride, diethylaluminum chloride, and combinations thereof to said GaCl.sub.3 in a container in an Al/Ga molar ratio of from 0.33 to 1, thereby forming a non-corrosive liquid formulation that does not contain free HCl and that comprises at least one of GaMeCl.sub.2, GaEtCl.sub.2, AlEtCl.sub.2, dissolved GaCl.sub.3, Ga(n-Bu)Cl.sub.2, Al(n-Bu)Cl.sub.2, or combinations thereof; and storing and/or transporting the liquid formulation in the container.

2. The method of claim 1 wherein the aluminum compound is chosen from triethylaluminum, tri(n-butyl) aluminum chloride, diethylaluminum chloride, and combinations thereof.

3. The method of claim 1 wherein the aluminum compound is triethylaluminum and the Al/Ga molar ratio is 0.5.

4. The method of claim 3 wherein the liquid formulation comprises GaEtCl2 and AlEtCl2.

5. The method of claim 4 wherein the GaEtCl.sub.2 is present in an amount of 66 mol % and the AlEtCl.sub.2 is present in an amount of 33 mol %.

6. The method of claim 1 wherein the aluminum compound is triethylaluminum and the Al/Ga molar ratio is 0.33.

7. The method of claim 6 wherein the liquid formulation comprises GaEtCl2, AlEtCl2, and dissolved GaCl3.

8. The method of claim 7 wherein the GaEtC2 is present in an amount of 50 mol %, the AlEtCl2 is present in an amount of 25 mol %, and the dissolved GaCl3 is present in an amount of 25 mol %.

9. The method of claim 1 wherein the aluminum compound is tri(n-butyl) aluminum and the Al/Ga molar ratio is 0.33.

10. The method of claim 9 wherein the liquid formulation comprises Ga(n-Bu)Cl2, Al(n-Bu)Cl2, and dissolved GaCl3.

11. The method of claim 10 wherein the Ga(n-Bu)Cl2 is present in an amount of 50 mo1%, the Al(n-Bu)Cl2 is present in an amount of 25 mol %, and the dissolved GaCl3 is present in an amount of 25 mol %.

12. The method of claim 1 wherein the aluminum compound is diethylaluminum chloride and the Al/Ga molar ratio is 1.

13. The method of claim 12 wherein the liquid formulation comprises GaEtCl2 and AlEtCl2.

14. The method of claim 13 wherein the GaEtCl2 is present in an amount of 50 mol % and the AlEtCl2 is present in an amount of 50 mol %.

15. The method of claim 1 wherein the aluminum compound is triethylaluminum and the Al/Ga molar ratio is 0.5.

16. The method of claim 15 wherein the liquid formulation comprises GaEtCl2 and AlEtCl2.

17. The method of claim 16 wherein the GaEtCl2 is present in an amount of 66 mol % and the AlEtCl2 is present in an amount of 33 mol %.

18. A method of producing trialkyl gallium comprising the steps of: transporting the container comprising the liquid formulation of claim 1 to a reactor, introducing the liquid formulation into the reactor, and reacting the liquid formulation with a trialkyl aluminium compound AlR′3 to form trialkyl gallium GaR′3 and dialkyl aluminium chloride Al(R′)2Cl, wherein R′ is a linear or branched alkyl group with 1 to 8 carbon atoms.

19. A method of preparing trimethyl gallium comprising the steps of: transporting the container comprising the liquid formulation of claim 1 to a reactor, introducing the liquid formulation into the reactor, reacting the liquid formulation and a trialkyl aluminium compound A1R″3 to form a trialkyl gallium GaR″3 and dialkyl aluminium chloride Al(R″)2Cl, and subsequently reacting the trialkyl gallium GaR″3 with either trimethyl aluminium [Al(CH.sub.3).sub.3] or dimethylaluminium chloride [Al(CH.sub.3).sub.2Cl] to form the trimethyl gallium, wherein R″ is a linear or branched alkyl group with 2 to 8 carbon atoms.

20. A method for storing and/or transporting GaCl.sub.3, consisting of: adding an aluminum compound chosen from trimethylaluminum, triethylaluminum, tri(n-butyl) aluminum chloride, diethylaluminum chloride, and combinations thereof to said GaCl.sub.3 in a container in an Al/Ga molar ratio of from 0.33 to 1, thereby forming a non-corrosive liquid formulation that does not contain free HCl and that comprises at least one of GaMeC.sub.2, GaEtCl.sub.2, AlEtCl2, dissolved GaCl.sub.3, Ga(n-Bu)Cl.sub.2, Al(n-Bu)Cl.sub.2, or combinations thereof; and storing and/or transporting the liquid formulation in the container.

Description

EXAMPLES

Example 1

(1) To gallium trichloride (3.49 gram, 0.020 mol) was slowly added—drop by drop—triethyl aluminum (1.14 gram, 0.010 mol). The molar ratio GaCl.sub.3:TEAL was 2:1 (the Al/Ga molar ratio was therefore 0.5).

(2) Reaction heat was produced. After the addition, the reaction mixture was cooled down to room temperature.

(3) A clear colorless liquid was obtained which contained—as analysed with 1H-NMR—66 mol % GaEtCl2 and 33 mol % AlEtCl.sub.2.

Example 2

(4) Example 1 was repeated, except that 5.29 gram (0.030 mol) gallium trichloride was used, resulting in a molar ratio GaCl.sub.3:TEAL of 3:1 (the Al/Ga molar ratio was therefore 0.33).

(5) A clear colorless liquid was obtained which contained 50 mol % GaEtCl.sub.2, 25 mol % AlEtCl.sub.2, and 25 mol % dissolved GaCl.sub.3.

Example 3

(6) Example 1 was repeated, except that 3.51 gram (0.020 mol) gallium trichloride and 1.99 gram (0.010 mol) tri(n-butyl) aluminum (TNBAL) was used, resulting in a molar ratio GaCl.sub.3:TNBAL of 3:1 (the Al/Ga molar ratio was therefore 0.33).

(7) A clear colorless liquid was obtained which contained 50 mol % Ga(n-Bu)Cl.sub.2, 25 mol % Al(n-Bu)Cl.sub.2, and 25 mol % dissolved GaCl.sub.3.

Example 4

(8) Example 1 was repeated, except that 3.53 gram (0.020 mol) gallium trichloride and 2.42 gram (0.020 mol) diethylaluminum chloride (DEAC) was used, resulting in a molar ratio GaCl3:DEAC of 1:1 (the Al/Ga molar ratio was therefore 1).

(9) A clear colorless liquid was obtained which contained 50 mol % GaEtCl.sub.2 and 50 mol % AlEtCl.sub.2.

Example 5

(10) Gallium chloride (17.60 gram, 0.10 mol) was added to a 50 ml two neck flask equipped with a distillation column, stirrer and thermocouple.

(11) Triethylaluminum (5.72 gram, 0.05 mol) was slowly added to the solid gallium chloride. A colorless liquid was obtained. After cooling down to room temperature, the reaction mixture remained a colorless liquid containing 66 mol % GaEtCl2 and 33 mol % AlEtCl2.

(12) Trimethylaluminium (18.1 gram, 0.25 mol) was slowly added to said colorless liquid.

(13) After the addition, the reaction mixture was gradually heated to 160° C. and the distillate was collected in a receiving flask. Trimethyl gallium was isolated in 85% yield (9.76 gram, 0.085 mol). This yield is comparable to a yield obtained by reacting trimethyl aluminium with solid gallium chloride.

(14) While at least one exemplary embodiment has been presented in the foregoing detailed description, it should be appreciated that a vast number of variations exist. It should also be appreciated that the exemplary embodiment or exemplary embodiments are only examples, and are not intended to limit the scope, applicability, or configuration of the various embodiments in any way. Rather, the foregoing detailed description will provide those skilled in the art with a convenient road map for implementing an exemplary embodiment as contemplated herein. It being understood that various changes may be made in the function and arrangement of elements described in an exemplary embodiment without departing from the scope of the various embodiments as set forth in the appended claims.