Method for preparing sodium chloro-aluminate

Patent metadata

Field	Value
Publication number	US-9567232-B1
Application number	US-201514831357-A
Country	US
Kind code	B1
Filing date	Aug 20, 2015
Priority date	Aug 20, 2015
Publication date	Feb 14, 2017
Grant date	Feb 14, 2017

Abstract

Different methods for the preparation of high purity NaAlCl 4 are disclosed. The methods includes charging a feed having an intimate mixture of aluminum chloride, sodium chloride, and aluminum metal, to a reactor at an initial temperature less than about 80° C., carrying out a solid state reaction to form a solid NaAlCl 4 at an intermediate temperature less than about 145° C., melting the formed solid NaAlCl 4 at an elevated temperature greater than about 150° C. to produce molten phase NaAlCl 4 , holding the reactor at a raised temperature greater than about 165° C. to substantially complete formation of colorless NaAlCl 4 and filtering the reactor contents at a final temperature greater than about 165° C.

First claim

The invention claimed is:

1. A method for the preparation of high purity NaAlCl 4 , comprising:
charging a feed comprising an intimate mixture of aluminum chloride, sodium chloride, and aluminum metal to a reactor at an initial temperature less than about 80 degree Celsius;
carrying out a solid state reaction at an intermediate temperature less than about 145 degree Celsius, to form solid NaAlCl 4 ;
melting the solid NaAlCl 4 at an elevated temperature greater than about 150 degree Celsius, to produce molten phase NaAlCl 4 ;
holding the reactor at a raised temperature greater than about 165 degree Celsius, to substantially complete formation of colorless NaAlCl 4 ; and
filtering reactor contents at a final temperature greater than about 165 degree Celsius, to remove residual reactants and by-products.

2. The method of claim 1 , further comprising introducing excess sodium chloride in the feed in an amount greater than about 0.5%, compared to a stoichiometric level of sodium chloride required for a complete chemical reaction producing NaAlCl 4 .

3. The method of claim 1 , wherein an average surface area of the aluminum metal is greater than about 0.05 m 2 per 1 kg of NaAlCl 4 .

4. The method of claim 3 , further comprising restricting a total residual moisture in the intimate mixture to less than about 1500 ppm.

5. The method of claim 1 , wherein the solid state reaction at the intermediate temperature is carried out until at least about 50% of NaAlCl 4 is formed.

6. The method of claim 1 , further comprising determining completion of colorless NaAlCl 4 formation by measuring an evolution of hydrogen, hydrogen chloride, or a combination of hydrogen and hydrogen chloride from the reactor.

7. The method of claim 6 , further comprising removing at least 50% of the total hydrogen chloride evolved, during the solid state reaction.

8. The method of claim 6 , further comprising monitoring the level of hydrogen chloride in the final reaction mixture by measuring the evolution of hydrogen in the reactor and the pH change in the scrubber.

9. The method of claim 1 , further comprising applying an external temperature to the reactor wherein the external temperature applied in melting the NaAlCl 4 is maintained at less than about 145 degree Celsius.

10. The method of claim 1 , wherein the reactor is held at the raised temperature at least for about 2 hours.

11. The method of claim 1 , wherein the reactor contents are filtered at a pressure greater than about 0.8 bar-gauge and at a temperature greater than about 180 degree Celsius.

12. The method of claim 1 , further comprising an inert gas head-space purging with a rate such that an average purge gas residence time is between about 0.05 hours to about 0.4 hours to effectively remove hydrogen chloride and hydrogen without causing reactant loss.

13. The method of claim 1 , wherein a yield of the high purity NaAlCl 4 is more than about 97% of the theoretically estimated value.

14. The method of claim 1 , wherein a yellowness index of the high purity NaAlCl 4 produced is less than about 0.2.

15. The method of claim 1 , wherein the high purity NaAlCl 4 is produced within 6 hours from melting of the solid NaAlCl 4 .

16. The method of claim 1 , further comprising producing the high purity NaAlCl 4 in a semi-continuous mode.

17. The method of claim 16 , further comprising retaining at least about 15 vol % of liquid from a previous production during charging for a subsequent production.

18. A method for the preparation of high purity NaAlCl 4 , comprising:
charging a feed comprising an intimate mixture of aluminum chloride, sodium chloride, and a high surface area aluminum metal to a reactor at an initial temperature less than about 50 degree Celsius;
carrying out a solid state reaction at an intermediate temperature less than about 145 degree Celsius, to form solid NaAlCl 4 ;
melting the solid NaAlCl 4 at a raised temperature greater than about 150 degree Celsius to produce molten phase NaAlCl 4 ;
holding the reactor at a raised temperature greater than about 165 degree Celsius, to substantially complete formation of colorless NaAlCl 4 ; and
filtering reactor contents at a final temperature greater than about 180 degree Celsius and a pressure greater than about 0.8 bar-gauge to remove residual reactants and by-products, wherein
the sodium chloride in the feed is in excess in an amount greater than about 1%, compared to a stoichiometric level of sodium chloride required for a complete chemical reaction producing NaAlCl 4 ; and
wherein an average surface area of the aluminum metal flakes in the feed is greater than about 0.05 m 2 /kg of produced NaAlCl 4 .

19. A method for the preparation of high purity NaAlCl 4 in a semi-continuous mode, comprising:
charging a feed comprising an intimate mixture of aluminum chloride, sodium chloride, and aluminum metal to a reactor at an initial temperature less than about 80 degree Celsius;
carrying out a solid state reaction at an intermediate temperature less than about 145 degree Celsius, to form solid NaAlCl 4 ;
melting the solid NaAlCl 4 at an elevated temperature greater than about 150 degree Celsius, to produce molten phase NaAlCl 4 ;
holding the reactor at a raised temperature greater than about 165 degree Celsius, to substantially complete formation of colorless NaAlCl 4 ;
filtering reactor contents at a final temperature greater than about 180 degree Celsius and a pressure greater than about 0.8 bar-gauge, retaining at least about 15 volume percent of the contents in the reactor;
initiating the charging of a subsequent feed comprising an intimate mixture of aluminum chloride, sodium chloride, and aluminum metal to the reactor at a temperature greater than about 165 degree Celsius;
continuing the charging in a controlled rate to keep a reaction temperature of the subsequent feed in a range from about 156 degree Celsius to about 190 degree Celsius, to avoid freezing reactor contents and to minimize reactant losses;
holding the reactor at a raised temperature greater than about 165 degree Celsius, to substantially complete formation of colorless NaAlCl 4 ; and
repeating the filtering, charging and holding steps to semi-continuously form the high purity NaAlCl 4 .

20. The method of claim 19 , further comprising introducing excess sodium chloride in the feed in an amount greater than about 1%, compared to a stoichiometric level of sodium chloride required for a complete chemical reaction producing NaAlCl 4 .

Assignees

• Gen Electric

Inventors

• Stella Albert Santo
• Kniajanski Sergei
• Buckley Paul William
• Miebach Barbara Ellen
• Shanklin Elliott West
• Howson Paul Edward
• Woodruff David Winfield

Classifications

• C01F7/78 Primary

  Compounds containing aluminium, with or without oxygen or hydrogen, and containing two or more other elements (aluminates C01F7/02; compounds containing aluminium, fluorine and alkali or alkaline earth metals C01F7/54; nitrates containing other cations besides aluminium C01F7/66; sulfides, sulfites or sulfates containing other cations besides aluminium C01F7/70 - C01F7/74) · CPC title

• C01F7/002 Primary

  Chemistry & Metallurgy · mapped topic