Recycle of discharged sodium borate fuel

• US 6,706,909 B1
• Filed: 05/12/2003
• Issued: 03/16/2004
• Est. Priority Date: 05/12/2003
• Status: Expired due to Fees

• Current Assignee: Millennium Cell Inc., US Borax Incorporated (Rio Tinto Limited)
• Original Assignee: Millennium Cell Inc., Us Borax
• Inventors: Wu, Ying, Snover, Jonathan
• Primary Examiner(s): McKane, Joseph K.
• Assistant Examiner(s): Shiao, Robert
• Application Number:
  US10/435,771
• Time in Patent Office: 309 Days
• Field of Search: 558/296
• US Class Current: 558/296
• CPC Class Codes: C07F 5/04 Esters of boric acids

Abstract

The present invention relates to an improvement in the recovery of boron values from a mixture of alkali metal borate and alkali metal hydroxide representing discharged fuel from a hydrogen generator apparatus. The mixture is reacted with carbon dioxide and a lower alcohol to form trialkyl borate, alkali bicarbonate and water. A porous water-absorbing material is added to the reaction mixture to absorb water as it forms thereby improving the yield of trialkyl borate. The trialkyl borate is converted to alkali borohydride that is used in the fuel.

Claims

1. A process for producing trialkyl borates of the formula B(OR)₃, wherein R is a straight- or branched-alkyl consisting of 1 to 6 carbon atoms, comprising reacting an alkali metal borate with carbon dioxide and a lower alcohol thereby producing trialkyl borate, alkali metal bicarbonate and water, said reaction being carried out in the presence of a porous particulate water-absorbing material to absorb said water as it forms.

2. The process in accordance with claim 1, wherein the alkali metal borate is a sodium borate represented by the formula Na₂O.xB₂O₃.yH₂O, wherein x is 1 to 5 and y is 0 to 10, and the lower alcohol is a straight- or branched-chain alkyl alcohol containing from 1 to 6 carbon atoms.

3. The process in accordance with claim 2, wherein said lower alcohol is a straight- or branched-chain alkyl alcohol containing from 1 to 4 carbon atoms.

4. The process in accordance with claim 3, wherein the lower alcohol is methanol or n-butanol.

5. The process in accordance with claim 1, wherein said water-absorbing material is a molecular sieve of Type 3A or 4A, or particulate alumina.

6. The process in accordance with claim 1, wherein said reaction is carried out in a continuous manner by passing the carbon dioxide and lower alcohol over a particulate mixture of alkali metal borate and said water-absorbing material.

7. The process in accordance with claim 1, wherein the trialkyl borate is isolated by distillation.

8. A process for producing trialkyl borates of the formula B(OR)₃, wherein R is a straight- or branched-alkyl consisting of 1 to 6 carbon atoms, from a solution of alkali metal borate and alkali metal hydroxide comprising:

a. drying said solution to form a particulate mixture of alkali metal borate and alkali metal hydroxide; and

b. reacting said particulate mixture with carbon dioxide and a lower alcohol thereby producing trialkyl borate, alkali metal bicarbonate and water, said reaction being carried out in the presence of a porous particulate water-absorbing material to absorb water as it forms.

9. The process in accordance with claim 8, wherein the alkali metal borate is a sodium borate represented by the formula Na₂O.xB₂O₃.yH₂O, wherein x is 1 to 5 and y is 0 to 10, the alkali metal hydroxide is sodium hydroxide, and the lower alcohol is a straight- or branched-chain alkyl alcohol containing from 1 to 6 carbons.

10. The process in accordance with claim 9, wherein said lower alcohol is a straight-or branched-chain alkyl alcohol containing from 1 to 4 carbon atoms.

11. The process in accordance with claim 10, wherein the lower alcohol is methanol or n-butanol.

12. The process in accordance with claim 8, wherein said reaction is carried out in a continuous manner by passing the carbon dioxide and lower alcohol over the particulate mixture of alkali metal borate and alkali metal borohydride and said water-absorbing material.

13. The process in accordance with claim 8, wherein said water-absorbing material is a molecular sieve of Type 3A or 4A, or particulate alumina.

14. The process in accordance with claim 8, wherein the trialkyl borate is isolated by distillation.

15. The process in accordance with claim 8, wherein the unreacted lower alcohol is recovered and reused in the process.

16. The process in accordance with claim 8, wherein the solution containing alkali metal borate and alkali metal hydroxide is discharged fuel from a hydrogen generator.

17. The process in accordance with claim 8, additionally including the step of converting the trialkyl borate to an alkali metal borohydride by reaction with an alkali metal hydride.

18. The process in accordance with claim 17, wherein the alkali metal is sodium.