Method for removing HCN from crude dinitro toluene

Patent metadata

Field	Value
Publication number	US-9428441-B2
Application number	US-201414916210-A
Country	US
Kind code	B2
Filing date	Sep 1, 2014
Priority date	Sep 5, 2013
Publication date	Aug 30, 2016
Grant date	Aug 30, 2016

Abstract

A process for the preparation of dintrotoluene which comprises (a) nitrating toluene with a nitrating acid, wherein said nitrating acid is a mixture of nitric acid and sulfuric acid, in one or more nitration steps, and separating the nitrating acid from the process stream thus formed, wherein a crude mixture comprising dinitrotoluene and a fraction of said nitrating acid dissolved therein is obtained, said crude mixture further comprising at least 50 ppm of HCN, and (b) washing the crude dinitrotoluene containing mixture in one or more washing steps, wherein, before the first washing step is carried out, the crude mixture is distilled and/or stripped to remove HCN therefrom, wherein a crude dinitrotoluene containing mixture which is essentially free of HCN is obtained.

First claim

The invention claimed is:

1. A process for the preparation of dinitrotoluene which comprises
(a) nitrating toluene with a nitrating acid, wherein said nitrating acid is a mixture of nitric acid and sulfuric acid, in one or more nitration steps, and separating the nitrating acid from the process stream thus formed, wherein a crude mixture comprising dinitrotoluene and a fraction of said nitrating acid dissolved therein is obtained, said crude mixture further comprising at least 50 ppm of HCN, and
(b) washing the crude dinitrotoluene containing mixture in one or more washing steps,
wherein, before the first washing step is carried out, the crude mixture is distilled and/or stripped in a flash evaporator, stripping or distillation column to remove HCN therefrom, wherein a crude dinitrotoluene containing mixture which is essentially free of HCN is obtained, and the gaseous phase obtained from the top of the flash evaporator, stripping or distillation column is partially condensed in order to recover a condensate containing nitric acid, sulfuric acid and dinitrotoluene while keeping as least 50% of the HCN in the gaseous phase.

2. The process of claim 1 , wherein the crude dinitrotoluene containing mixture is distilled in a column having up to 10 theoretical plates.

3. The process of claim 2 , wherein the crude dinitrotoluene containing mixture is distilled in a column having 2 to 4 theoretical plates.

4. The process of claim 1 , wherein the crude dinitrotoluene containing mixture is distilled in a flash evaporator.

5. The process according to claim 1 , wherein the distillation is carried out as a vacuum distillation at a pressure of from 10 to 200 mbar.

6. The process according to claim 1 , wherein the distillation is combined with a stripping operation using a stripping gas.

7. The process according to claim 6 , wherein the stripping operation is carried out using air or nitrogen as a stripping gas.

8. The process according to claim 1 , wherein the gaseous phase obtained in the distillation and/or stripping is partially condensed in a multistep condenser.

9. The process of claim 8 , wherein the liquid condensate phase comprising dinitrotoluene, nitric acid and sulfuric acid is at least in part recycled to one or more of the nitration steps (a).

10. The process of claim 1 , wherein at least 90% of the HCN present in the crude dinitrotoluene containing mixture are removed by the distillation and/or stripping before the first washing step.

11. The process of claim 1 , wherein the crude dinitrololuene containing mixture after the distillation and/or stripping, but before the first washing step has been carried out, contains at most 15 ppm of HCN.

Assignees

• Basf Se

Inventors

• Dai Yuan Shen
• Spuhl Katharina
• Hempel Renate

Classifications

• C07C205/06

  having nitro groups bound to carbon atoms of six-membered aromatic rings · CPC title

• C07C201/08

  by substitution of hydrogen atoms by nitro groups · CPC title

• C07C201/16 Primary

  Separation; Purification; Stabilisation; Use of additives · CPC title