# US 5,349,082 A · Toluene diisocyanate residue

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- Number: US 5,349,082 A
- Document ID: US5349082A
- Status: Granted
- Kind: A
- Application number: 08/033,935
- Filed: 1993-03-19
- Granted: 1994-09-20
- Earliest claimed: 1993-03-19
- Assignees: Miles Inc.
- Inventors: William E. Slack; Kenneth L. Dunlap; Larry W. Arndt; Louis Renbaum
- Web page: https://patentgrep.com/patent/US5349082A

## CPC

- C07C 263/20: Separation; Purification
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS

## Abstract

Disclosed herein is a process for recovering toluene diisocyanate (TDI) from a TDI residue solution, comprising mixing the residue solution with a polyisocyanate consisting essentially of methylenediphenyl diisocyanate (MDI) or MDI in combination with its higher ring oligomer, followed by heating the resulting mixture over a temperature range of 130.degree. to 250.degree. C. for a period of time sufficient to remove free TDI and thermally splittable TDI generated from equilibration of the TDI residue with MDI or the MDI oligomer by either a batch or continuous process.

## Claims

### Claim 1

A process for recovering toluene diisocyanate (TDI) from a TDI residue solution, comprising
(a) mixing the TDI residue solution with a polyisocyanate consisting essentially of methylenediphenyl diisocyanate (MDI) or MDI in combination with its higher ring oligomers,
(b) heating the resulting mixture over a temperature range from 130.degree. to 250.degree. C. at reduced pressure for a period of time sufficient to remove free TDI,
(c) recovering free TDI removed in (b),
(d) maintaining or increasing the temperature of the mixture of (b) for a period of time sufficient for equilibration of the TDI residue and MDI and any MDI oligomer to occur, and
(e) recovering TDI which is thermally split during (d) by either a batch or continuous process.

### Claim 2 (depends on 1)

The process of claim 1, wherein steps (b), (c), (d) and (e) are carried out over a temperature range of from 130.degree. to 250.degree. C. over a period of 1 to 180 minutes.

### Claim 3 (depends on 2)

The process of claim 2 in which step (d) is conducted at a temperature of from 160.degree. to 220.degree. C. over a period of from 2 to 120 minutes.

### Claim 4 (depends on 3)

The process of claim 3 wherein step (d) is conducted at a temperature of from 190.degree. to 210.degree. C. over a period of from 3 to 90 minutes.

### Claim 5

A continuous process for removing TDI monomer from a TDI residue solution comprising mixing the TDI residue solution with MDI or MDI with its higher ring oligomer, followed by removing free TDI monomer present in the TDI residue solution by passing the resulting mixture through an evaporation means at a reduced pressure, followed by heating at 160.degree. to 250.degree. C. for between 1 and 30 minutes, followed by again passing the mixture through an evaporation means at a reduced pressure to remove TDI monomer generated by the equilibration of TDI residue with MDI or the MDI oligomer, followed by optionally repeating the equilibration-evaporation steps at a reduced pressure until no thermally splittable TDI remains.