Method and apparatus for producing decabromodiphenyl alkanes
View Patent ↗A method of producing decabromodiphenyl alkanes includes the steps of charging a reaction vessel with bromine and a bromination catalyst and introducing a diphenyl alkane into the vessel at a location above the level of the charge bromine and catalyst. A dip tube apparatus for introducing the diphenyl alkane includes an inner tube and an outer tube, each of which are disposed above the surface of the bromine reaction vessel. The inner tube is fitted with a plug having an opening. Diphenyl alkane flows through the inner tube, out the opening in the plug, and into the reactor. The outer tube is disposed around and along the inner tube. Reaction mass from the vessel is recirculated from the vessel, through the outer tube and back to the vessel so as to form a curtain of reaction mass around the stream of diphenyl alkane being simultaneously fed into the reaction vessel.
1. A method for preparing decabromodiphenyl alkanes comprising:
charging a reaction vessel with bromine and a bromination catalyst;
providing a dip tube apparatus having a first end and a second end located in the reaction vessel above the surface level of the bromine and the bromination catalyst;
introducing diphenyl alkane through the dip tube apparatus such that the diphenyl alkane flows from the first end, to the second end and enters the reaction vessel at a point above the surface level of bromine and bromination catalyst in the reaction vessel;
reacting the diphenyl alkane with the bromine and the bromination catalyst thereby forming a reaction mass; and
recirculating the reaction mass through the dip tube apparatus so as to form a curtain of recirculated reaction mass around the diphenyl alkane being introduced into the reaction vessel.
2. The method of claim 1 , wherein the dip tube apparatus includes an inner tube and an outer tube surrounding the inner tube.
3. The method of claim 2 , wherein the diphenyl alkane is introduced into the reaction vessel through the inner tube.
4. The method of claim 2 , wherein the reaction mass is recirculated through the outer tube.
5. The method of claim 2 , further including spacers positioning the inner tube within the outer tube.
6. The method of claim 1 , wherein the second end of the dip tube apparatus is located from about 1 inch to about 12 inches above the surface level of the bromine and bromination catalyst.
7. The method of claim 2 , wherein the distance between the curtain of recirculated reaction mass and the diphenyl alkane being introduced into the reaction vessel is at least about 0.5 inches.
8. The method of claim 2 , wherein the inner tube includes a first end and a second end located above the level of the bromine and bromination catalyst in the reaction vessel and the outer tube includes a first end and a second end, the second end of the outer tube being located farther above the surface level of the bromine and catalyst than the second end of the inner tube.
9. The method of claim 1 , wherein the reaction mass is recirculated at a rate of between about 45-250 gallons per minute.
10. The method of claim 1 , wherein the diphenyl alkane is fed to the reaction vessel at a rate of between about 4-8.5 pounds per minute.
11. The method of claim 1 , wherein the diphenyl alkane is fed to the reaction vessel at a velocity of about 9 meters per second to about 25 meters per second.
12. The method of claim 1 , wherein the diphenyl alkane is fed to the reaction vessel under a pressure of at least about 20 psig.
13. The method of claim 1 , wherein the diphenyl alkane is diphenylerhane.
14. The method of claim 1 , further including the step of purifying the decabromodiphenyl alkane by grinding it twice in an air mill utilizing heated air and then heat treating it.
15. The method of claim 14 , wherein the air is heated to an inlet temperature of about 250° C. to about 260° C.
16. The method of claim 15 , wherein the decabromodiphenyl alkane is heat treated at a temperature of about 240° C.
17. The method according to claim 16 , wherein the decabromodiphenyl alkane is heat treated for about 3 to about 4 hours.