Isolation of partially brominated diphenyl ether mixtures in crystalline form with higher melting range
AssigneeGreat Lakes Chemical Corporation
InventorsBhabatosh Bhattacharya, Wayne C. Muench
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Abstract
This invention relates to a process for isolation of partially brominated diphenyl ether mixtures ("Octabrom") having an average bromine content of 7.2-8.5. The process comprises: (i) adding a C.sub.1 -C.sub.4 alkanol to the Octabrom in solution in an organic solvent; (ii) maintaining the contact of the alkanol with Octabrom in the organic solvent for that period of time which is sufficient to allow the Octabrom to precipitate in crystalline form, making a slurry; and (iii) recovering the final Octabrom from the slurry.
Claims28
A method for the isolation of a solid partially brominated diphenyl ether product from a mixture of partially bromnated diphenyl ethers having an average of from about 7.2 to ab out 8.5 bromine atoms per molecule of diphenyl ether, the method comprising:
- a. providing a mixture of partially brominated diphenyl ethers, wherein said mixture has been removed form its bromination medium;
- b. dissolving the mixture in an organic solvent selected from the group consisting of benzene, toluene, and xylenes, or mixtures thereof, at a temperature sufficiently high for the partially brominated diphenyl ethers and solvent to form a solution,
- c. contacting the solution of step b with a C.sub.1 -C.sub.4 alkanol;
- d. maintaining the contact of step c, for a sufficient time to allow said diphenyl ether product to precipitate out;
- and
- e. recovering the precipitate.
A method for the isolation of a solid partially brominated diphenyl ether product from a mixture of partially brominated diphenyl ethers having an average of from about 7.2 to about 8.5 bromine atoms per molecule of diphenyl ether, the method comprising:
- a. providing a solution of the partially brominated diphenyl ethers in an organic solvent at a temperature sufficiently high for the partially brominated diphenyl esters to be dissolve din the organic solvent;
- b. contacting the solution of step a, with a C.sub.1 -C.sub.4 alkanol;
- c. maintaining the contact of step b, for a sufficient time to allow said diphenyl ether product to precipitate out;
- and
- d. recovering the precipitate;
- wherein the organic solvent is selected from the group consisting of benzene, toluene, and xylenes, or mixtures thereof.
A method for isolating a solid dipheny ether product having an average of from about 7.2 to about 8.5 bromine atoms per molecule of diphenyl ether from a mixture of partially brominated diphenyl ethers, wherein said mixture has been removed from its bromination medium, the method including contacting said mixture of partially brominated diphenyl ethers with a C.sub.1 -C.sub.4 alkanol to form a product mixture and recovering said product from said product mixture, wherein the improvement comprises:
- prior to said contacting of a C.sub.1 -C.sub.4 alkanol, providing a solution of said mixture of partially brominated diphenyl ethers in an organic solvent selected from the group consisting of benzene, toluene, and xylenes, or mixtures thereof, at a temperature sufficiently high for said mixture of partially brominated diphenyl ethers to be dissolved in said organic solvent.
A method for isolating a solid diphenyl ether product having an average of from about 7.2 to about 8.5 bromine atoms per molecule of diphenyl ether from a mixture of partially brominated diphenyl ethers, the method including contacting said mixture of partially brominated diphenyl ethers with a C.sub.1 -C.sub.4 alkanol to form a product mixture and recovering said product from said product mixture, wherein the improvement comprises:
- prior to said contacting of a C.sub.1 -C.sub.4 alkanol, providing a solution of said mixture of partially brominated diphenyl ethers in an organic solvent at a temperature sufficiently high for said mixture of partially brominated diphenyl ethers to be dissolved in said organic solvent, wherein the organic solvent is selected from the group consisting of benzene, toluene, and xylenes, or mixtures thereof.
A method for the isolation of a solid partially brominated diphenyl ether product from a mixture of partially brominated diphenyl ethers having an average of from about 7.2 to about 8.5 bromine atom per molecule of diphenyl ether, the method comprising:
- a. brominating diphenyl ether in liquid bromine in the presence of a bromination catalyst to afford a mixture of partially brominated diphenyl ethers;
- b. dissolving said mixture in an organic solvent selected from the group consisting of benzene, toluene, and xylenes, or mixtures thereof, at a temperature sufficiently high for the partially brominated diphenyl ethers to be dissolved in the organic solvent;
- c. contacting the solution of step (b) with a C.sub.1 -C.sub.4 alkanol;
- d. maintaining the contact of step (c) for a sufficient time to allow said diphenyl ether product to precipitate out;
- and
- e. recovering the precipitate.
Dependencies are inferred from the claim text.