Method for purifying mixtures comprising 4,4′-methylenediphenyl diisocyanate

Patent metadata

Field	Value
Publication number	US-9505711-B2
Application number	US-201113296665-A
Country	US
Kind code	B2
Filing date	Nov 15, 2011
Priority date	Nov 17, 2010
Publication date	Nov 29, 2016
Grant date	Nov 29, 2016

Abstract

The invention relates to a method for purifying mixtures comprising 4,4′-methylenediphenyl diisocyanate, which comprises purifying by distillation a mixture I comprising 4,4′-methylenediphenyl diisocyanate having a hydrolyzable chlorine content as specified in ASTM D4663-10 of greater than 100 ppm by means of a column K 1 , wherein the gaseous stream comprising the mixture I is brought into contact in the column K 1 with at least one liquid compound A which has the same or higher boiling point than 4,4′-methylenediphenyl diisocyanate and which has a hydrolyzable chlorine content as specified in ASTM D4663-10 of a maximum of 100 ppm, and wherein the gaseous stream O obtained at the top of the column comprises 4,4′-methylenediphenyl diisocyanate has a hydrolyzable chlorine content as specified in ASTM D4663-10 of a maximum of 100 ppm.

First claim

The invention claimed is:

1. A method for purifying 4,4′-methylene diphenyl diisocyanate, the method comprising purifying a mixture by distillation through a distillation column, such that a first gaseous stream comprising the mixture contacts at least one liquid compound within the distillation column, to obtain a second gaseous stream at a top of the distillation column, which is removed to obtain purified 4,4′-methylene diphenyl diisocyanate,
wherein:
the mixture comprises 4,4′-methylenediphenyl diisocyanate having a hydrolyzable chlorine content of greater than 100 ppm as determined by ASTM D4663-10;
the second gaseous stream comprises the purified 4,4′-methylenediphenyl diisocyanate having a maximum hydrolyzable chlorine content of 100 ppm as determined by ASTM D4663-10;
wherein said distillation column comprises ordered packing elements and wherein said first gaseous stream is fed into said distillation column at a point below said ordered packing elements; and
said first gaseous stream is taken off as a side stream from a first column, and a product obtained from a bottom phase of said distillation column is recirculated to said first column.

2. The method according to claim 1 , wherein the at least one liquid compound is added above an uppermost separation element of the distillation column, such that the at least one liquid compound is predistributed to a plurality of delivery points to the distillation column.

3. The method according to claim 1 , wherein the at least one liquid compound is added to the distillation column through a liquid distributor.

4. The method according to claim 1 , wherein the mixture is fed into the distillation column in gaseous form.

5. The method according to claim 1 , wherein the second gaseous stream is cooled in at most 5 seconds to a temperature of 20° C. to 60° C. after its removal from the distillation column.

6. The method according to claim 1 , wherein the hydrolyzable chlorine content of the second gaseous stream and the at least one liquid compound is, in each case, a maximum of 50 ppm as determined by ASTM D4663-10.

7. The method according to claim 1 , wherein a maximum total chlorine content in the second gaseous stream is 100 ppm as determined by ASTM D4661-09.

8. The method according to claim 1 , wherein a maximum content of halogenated phenyl isocyanates in the second gaseous stream is 25 ppm.

9. The method according to claim 1 , wherein a maximum content of N,N-disubstituted carbamoyl chlorides in the second gaseous stream is 25 ppm.

10. The method according to claim 1 , wherein the hydrolyzable chlorine content in the second stream is at least 10 ppm less than in the mixture as determined by ASTM D4663-10.

11. The method according to claim 1 , wherein the mixture, before feeding into the distillation column, is taken off from a second said first column in which crude binuclear methylenediphenyl diisocyanate is completely or partially separated into its isomers.

12. The method according to claim 1 , wherein a pressure difference between the first gaseous stream and the second gaseous stream, in the distillation column, is 0.5 to 30 mbar.

13. The method according to claim 1 , wherein the distillation column is an ordered-packing column having a specific surface area of 100 to 1000 m 2 /m 3 .

14. The method according to claim 1 , wherein the distillation occurs such that a reflux ratio in the distillation column is ranges from 0.01 to 2.0.

15. The method according to claim 1 , wherein said at least one liquid compound comprises at least 98 wt. % 4,4′-methylenediphenyl diisocyanate.

16. The method according to claim 1 , wherein said at least one liquid compound comprises at least 98.5 wt. % 4,4′-methylenediphenyl diisocyanate.

17. The method according to claim 1 , wherein said at least one liquid compound comprises at least 97 wt. % 4,4′-methylenediphenyl diisocyanate, and has a maximum hydrolyzable chlorine content of 100 ppm as determined by ASTM D4663-10.

18. The method according to claim 1 , wherein said at least one liquid compound is added above an uppermost separation element of the distillation column from an external device for storing.

19. The method according to claim 1 , wherein said at least one liquid compound is recirculated from a storage tank for storing the purified 4,4′-methylenediphenyl diisocyanate, such that a ratio of an amount of recirculated 4,4′-methylenediphenyl diisocyanate to an amount of 4,4′-methylenediphenyl diisocyanate newly fed to the storage tank ranges from 0.05 to 0.4.

20. A method for purifying 4,4′-methylene diphenyl diisocyanate, the method comprising purifying a mixture by distillation through a distillation column, such that a first gaseous stream comprising the mixture contacts at least one liquid compound within the distillation column, to obtain a second gaseous stream at a top of the distillation column, which is removed to obtain purified 4,4′-methylene diphenyl diisocyanate,
wherein:
the mixture comprises 4,4′-methylenediphenyl diisocyanate having a hydrolyzable chlorine content of greater than 100 ppm as determined by ASTM D4663-10;
the second gaseous stream comprises the purified 4,4′-methylenediphenyl diisocyanate having a maximum hydrolyzable chlorine content of 100 ppm as determined by ASTM D4663-10; and
wherein said distillation column comprises ordered packing elements and wherein said first gaseous stream is fed into said distillation column at a point below said ordered packing elements; and
said first gaseous stream is taken off as a side stream from a first column, and a product obtained from a bottom phase of said distillation column is recirculated to said first column,
wherein said at least one liquid compound comprises at least 97 wt. % 4,4′-methylenediphenyl diisocyanate, and has a maximum hydrolyzable chlorine content of 100 ppm as determined by ASTM D4663-10;
said at least one liquid compound is added above an uppermost separation element of the distillation column from an external device for storing; and
said at least one liquid compound is recirculated from a storage tank for storing the purified 4,4′-methylenediphenyl diisocyanate, such that a ratio of an amount of recirculated 4,4′-methylenediphenyl diisocyanate to an amount of 4,4′-methylenediphenyl diisocyanate newly fed to the storage tank ranges from 0.05 to 0.4.

21. The method according to claim 1 , wherein said at least one liquid compound is recirculated from a storage tank for storing the purified 4,4′-methylenediphenyl diisocyanate, such that a ratio of an amount of recirculated 4,4′-methylenediphenyl diisocyanate to an amount of 4,4′-methylenediphenyl diisocyanate newly fed to the storage tank ranges from 0.05 to 0.4 and
wherein a ratio of said at least one liquid compound to said first gaseous stream SAT [w/w] is 0.01 to 2.0.

22. A method for purifying 4,4′-methylene diphenyl diisocyanate, the method comprising purifying a mixture by distillation through a distillation column, such that a first gaseous stream comprising the mixture contacts at least one liquid compound within the distillation column, to obtain a second gaseous stream at a top of the distillation column, which is removed to obtain purified 4,4′-methylene diphenyl diisocyanate,
wherein:
the mixture comprises 4,4′-methylenediphenyl diisocyanate having a hydrolyzable chlorine content of greater than 100 ppm as determined by ASTM D4663-10;
the second gaseous stream comprises the purified 4,4′-methylenediphenyl diisocyanate havi

Assignees

• Bock Michael
• Jacobs Johannes
• Thiele Kai
• Merten Anne-Kathrin
• Basf Se

Inventors

• Bock Michael
• Jacobs Johannes
• Thiele Kai
• Merten Anne-Kathrin

Classifications

• C07C263/20 Primary

  Separation; Purification · CPC title

• C07C265/14

  containing at least two isocyanate groups bound to the same carbon skeleton · CPC title