IP Library Granted Patent US 7,108,770
Granted Patent B2
US 7,108,770 · App. 10/687,157 · Granted Sep 19, 2006

Process for the purification of toluene diisocyanate incorporating a dividing-wall distillation column for the final purification

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Quick Facts
Patent No.
US 7,108,770
App. No.
10/687,157
Granted
Sep 19, 2006
Kind
B2
Abstract

Toluene diisocyanate is recovered from a crude distillation feed containing less than 2% by weight of phosgene by (a) fractionating the crude distillation feed containing less than 2% by weight of phosgene to remove the solvent and optionally the reaction residues to produce a crude toluene diisocyanate feed containing less than 20% by weight of solvent and (b) separating the crude toluene diisocyanate feed containing less than 20% by weight of solvent in a divided-wall distillation column into four product fractions P1–P4. P1 is a vapor phase low-boiler and solvent-enriched gas stream, P2 is a low-boiler and solvent-enriched product, P3 is a high boiler-enriched bottoms product containing toluene diisocyanate and P4 is a toluene diisocyanate product stream lean in low-boilers, high-boilers and reaction residues.

Claims (16)

1. A process for the purification of toluene diisocyanate from a crude distillation feed comprising less than 2% by weight of phosgene comprising

a) fractionating the crude distillation feed comprising less than 2% by weight of phosgene to remove solvent and, optionally, reaction residue to produce a crude toluene diisocyanate feed comprising less than 20% by weight of solvent and

b) separating the crude toluene diisocyanate feed comprising less than 20% by weight of solvent in a divided-wall distillation column into four product fractions P1–P4 comprising: P1, a vapor phase low-boiler and solvent-enriched gas stream, P2, a low-boiler and solvent-enriched product, P3, a high-boiler-enriched bottoms product comprising toluene diisocyanate and P4, a toluene diisocyanate product stream lean in low-boiler, high-boiler and reaction residue.

2. The process of claim 1 in which the product fraction P1 comprises 20–99% by weight of the solvent, the low-boiler and toluene diisocyanate.

3. The process of claim 1 in which the product fraction P2 comprises the solvent the low boiler and toluene diisocyanate.

4. The process of claim 1 in which the product fraction P3 comprises toluene diisocyanate and 0.5–15% by weight of the high boiler.

5. The process of claim 1 in which the product fraction P4 has a toluene concentration of at least 99.5% by weight and comprises less than 200 ppm by weight of the solvent and/or chlorinated aromatic hydrocarbon, less than 100 ppm by weight hydrolyzable chlorine and less than 40 ppm by weight acid.

6. A process for the production of toluene diisocyanate comprising:

a) reacting toluene diamine with phosgene to produce a crude distillation feed,

b) separating any unreacted phosgene present in an amount greater than or equal to 2% by weight from the crude distillation feed to obtain a crude distillation feed comprising less than 2% by weight of phosgene,

c) fractionating the crude distillation feed comprising less than 2% by weight of phosgene to remove solvent and optionally the reaction residue to produce a crude toluene diisocyanate feed comprising less than 20% by weight of the solvent and

d) separating the crude toluene diisocyanate feed comprising less than 20% by weight of the solvent in a divided-wall distillation column into four product fractions P1–P4 comprising: P1, a vapor phase low-boiler and solvent-enriched gas stream, P2, a low-boiler and solvent-enriched product, P3, a high boiler enriched bottoms product comprising toluene diisocyanate and P4, a toluene diisocyanate product stream lean in low-boiler, high-boiler and reaction residue.

7. The process of claim 6 in which the product fraction P1 comprises 20–99% by weight of the solvent the low-boiler and toluene diisocyanate.

8. The process of claim 6 in which the product fraction P2 comprises the solvent, the low boiler and toluene diisocyanate.

9. The process of claim 6 in which the product fraction P3 comprises toluene diisocyanate and 0.5–15% by weight of the high-boiler.

10. The process of claim 6 in which the product fraction P4 has a toluene diisocyanate concentration of at least 99.5% by weight and comprises less than 200 ppm by weight of the solvent and/or chlorinated aromatic hydrocarbons, less than 100 ppm by weight hydrolyzable chlorine and less than 40 ppm by weight acid.

Assignments (4)
CHANGE OF NAME Recorded Apr 6, 2016
From: BAYER MATERIALSCIENCE AG
To: COVESTRO DEUTSCHLAND AG
Reel/Frame 038365/0392 →
CHANGE OF NAME Recorded Mar 22, 2016
From: BAYER MATERIALSCIENCE AG
To: COVESTRO DEUTSCHLAND AG
Reel/Frame 038399/0358 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 9, 2016
From: BAYER AG
To: BAYER MATERIALSCIENCE AG
Reel/Frame 038044/0799 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Feb 13, 2004
From: GRUN, MARCUS PAUL; BRADY, BILL JR.; KEGGENHOFF, BERTHOLD; VERKERK, KAI; SCHAL, HANS-PETER
To: BAYER AKTIENGESELLSCHAFT
Reel/Frame 014979/0685 →