Method for starting up and shutting down a phosgene generator

Patent metadata

Field	Value
Publication number	US-9815703-B2
Application number	US-201515112261-A
Country	US
Kind code	B2
Filing date	Jan 16, 2015
Priority date	Jan 21, 2014
Publication date	Nov 14, 2017
Grant date	Nov 14, 2017

Abstract

The present invention relates to a method for operating a phosgene generator for producing phosgene by reacting carbon monoxide with chlorine in the gas phase on an activated carbon catalyst arranged in a reaction chamber, in which method, after a predefinable operating period, the phosgene production is at least temporarily interrupted by shutting down the phosgene generator over a shutdown period and, after a predefinable downtime, is resumed by starting up the phosgene generator over a start-up period, wherein the method is characterized in that the activated carbon catalyst, before the phosgene generator is started up, is freed of chlorine by adding carbon monoxide so that, during the start-up period, a maximum concentration of chlorine in the gas stream immediately downstream of the reaction chamber of 1000 ppmv is not exceeded. The invention also relates to the use of the phosgene thus obtained in the production of polycarbonate and isocyanates.

First claim

The invention claimed is:

1. A method of operating a phosgene generator for preparing phosgene by reacting carbon monoxide with chlorine in the gas phase over an activated carbon catalyst which is arranged in a reaction space, comprising at least temporarily interrupting the preparation of phosgene after a prescribeable period of operation by running down the phosgene generator over a running-down time and, after a prescribeable stoppage time, recommencing the preparation of phosgene by starting up the phosgene generator over a start-up time,
wherein
the activated carbon catalyst is freed of chlorine before starting up the phosgene generator by introducing carbon monoxide to such an extent that a maximum concentration of chlorine in the gas stream immediately downstream of the reaction space of 1000 ppmv is not exceeded during the start-up time.

2. The method of claim 1 , wherein a maximum concentration of chlorine in the gas stream immediately downstream of the reaction space of 100 ppmv is not exceeded.

3. The method of claim 1 , comprising reducing or directly interrupting the introduction of chlorine over the running-down time in order to adhere to the maximum concentration of chlorine during running-down of the phosgene generator, with the introduction of carbon monoxide being maintained until the concentration of chlorine has reached or gone below the maximum concentration.

4. The method of claim 3 , comprising maintaining the activated carbon catalyst at a temperature of from 60° C. to 140° C. during the running-down time.

5. The method of claim 1 , wherein the phosgene generator is in the stoppage time and, before it is started up, the introduction of carbon monoxide is commenced and comprising:
a) heating the activated carbon catalyst to a temperature of from 60° C. to 140° C. and/or
b) heating the carbon monoxide gas stream to a temperature of from 130° C. to 250° C., so that the chlorine still present on the activated carbon catalyst and/or in the reaction space from the previous production cycle reacts until the concentration thereof reaches or goes below the maximum concentration.

6. The method of claim 5 , wherein after the concentration of chlorine reaches or goes below the maximum concentration, the activated carbon catalyst is heated to a temperature of at least 140° C. before the introduction of chlorine is commenced.

7. The method of claim 1 , wherein the amount of carbon monoxide used for reaching or going below the maximum concentration of chlorine is at least 40 standard cubic meters per metric ton of activated carbon catalyst in the reaction space.

8. The method of claim 1 , wherein the commencement of the start-up of the phosgene generator is defined by the commencement of the introduction of chlorine.

9. The method of claim 1 , wherein the introduction of chlorine is increased to a desired end value over the start-up time, with the increase being carried out in steps.

10. The method of claim 1 , wherein the volume concentration of chlorine is determined UV-spectrometrically.

11. The method of claim 1 , wherein a molar excess of CO over chlorine of from 2 mol % to 20 mol % is set during the start-up time and the period of operation.

12. The method of claim 2 , wherein a maximum concentration of chlorine in the gas stream immediately downstream f the reaction space of 50 ppmv is not exceeded.

13. The method of claim 12 , wherein a maximum concentration of chlorine in the gas stream immediately downstream of the reaction space of 10 ppmv is not exceeded.

14. The method of claim 6 , wherein after the concentration of chlorine reaches or goes below the maximum concentration, the activated carbon catalyst is heated to a temperature of at least 180° C. before the introduction of chlorine is commenced.

15. The method of claim 7 , wherein the amount of carbon monoxide used for reaching or going below the maximum concentration of chlorine is at least 60 standard cubic meters per metric ton of activated carbon catalyst in the reaction space.

16. The method of claim 15 , wherein the amount of carbon monoxide used for reaching or going below the maximum concentration of chlorine is at least 80 standard cubic meters per metric ton of activated carbon in the reaction space.

17. The method of claim 9 , wherein the increase is carried out ire steps of 25%, 50%, 75% and then 100% of the desired end value.

18. The method of claim 9 , wherein the stepwise increase is d out at equal time intervals.

19. Polycarbonate prepared from phosgene obtained by the method of claim 1 .

20. Isocyanates prepared from phosgene obtained by the method of claim 1 .

Assignees

• Covestro Deutschland Ag

Inventors

• Knauf Thomas
• Rausch Andreas Karl
• Manzel Dirk
• Bjoerndahl Charles
• Ehlers Matthias
• Alvarez Herrero Carlos
• Munoz Velasco Francisco

Classifications

• C01B32/80 Primary

  Phosgene · CPC title

• C07C265/04

  of a saturated carbon skeleton · CPC title

• B01D2255/702

  Carbon · CPC title

• B01J21/18

  Carbon · CPC title

• C07C68/02

  from phosgene or haloformates · CPC title