Polyamines and process for preparation thereof

Patent metadata

Field	Value
Publication number	US-8987518-B2
Application number	US-201414190784-A
Country	US
Kind code	B2
Filing date	Feb 26, 2014
Priority date	Feb 28, 2013
Publication date	Mar 24, 2015
Grant date	Mar 24, 2015

Abstract

The present invention relates to polyamines and to a process for preparing polyamines.

First claim

The invention claimed is:

1. A process for preparing a polyamine in a reactor by conversion of a diamine present in a liquid phase in the presence of a catalyst present in a solid phase, at a temperature of from 50 to 200° C. and a pressure of from 1 to 400 bar,
the process comprising:
supplying a gas to the reactor, wherein an amount of gas supplied is from 1 to 1000 liters of gas per liter of free reactor volume per hour; and
introducing the gas into the liquid phase and removing the gas from the reactor together with ammonia which is formed in the conversion.

2. The process according to claim 1 , wherein the gas is an inert gas.

3. The process according to claim 1 , wherein the gas comprises hydrogen.

4. The process according to claim 1 , wherein the gas comprises exclusively hydrogen.

5. The process according to claim 1 , wherein the gas supplied is dispersed in the liquid phase.

6. The process according to claim 5 , wherein a temperature in the reactor is 165° C. or less.

7. The process according to claim 1 , wherein the conversion of the diamines is performed continuously.

8. The process according to claim 7 , wherein a catalyst hourly space velocity in continuous mode is from 0.1 to 1.5 kg of diamine per liter of catalyst per hour, or a residence time in batchwise mode is from 0.5 to 3 hours.

9. The process according to claim 1 , wherein the gas is removed from the reactor separately from the liquid phase.

10. The process according to claim 9 , wherein ammonia is condensed out of the gas stream, to obtain a gas stream essentially free of ammonia, and a liquid stream comprising ammonia, and the gas removed from ammonia is optionally recycled into the reactor.

11. The process according to claim 1 , wherein entrained diamines and oligomers of the diamine are removed from the gas stream prior to removal of the ammonia.

12. The process according to claim 2 , wherein entrained diamines and oligomers of the diamine are removed from the gas stream by flash evaporation.

13. The process according to claim 1 , wherein the gas is removed from the reactor together with at least a portion of the liquid phase.

14. The process according to claim 5 , further comprising decompressing the liquid phase, which is removed into a column, such that gas and ammonia are drawn off at a top of the column and the polyamine is drawn off at a bottom of the column.

15. The process according to claim 14 , wherein the gas drawn off at the top is partially condensed so as to obtain a gas comprising essentially no ammonia, and an ammonia-containing liquid phase.

16. The process according to claim 14 , wherein diamines and oligomers of the diamine are removed from a side draw of the column and are optionally recycled into the reactor.

17. The process according to claim 14 , wherein the bottoms from the column are introduced into a second column and diamines and oligomers of the diamine are removed at a top of the second column and the polyamine is drawn off at a bottom of the second column.

18. The process according to claim 7 , wherein a side draw product comprising oligomers of the diamine is removed from a second column and may be recycled into the process.

19. The process according to claim 1 , wherein gas recycled into the reactor, diamines, or both, or oligomers of the diamine recycled into the reactor comprise essentially no ammonia.

20. A polyamine obtained by the process according to claim 1 by conversion of a diamine, which has:
a) a degree of branching of from 0 to 0.5;
b) a mean degree of polymerization Pn of 5 or more;
c) a polydispersity of from 1.5 to 10;
d) a metal content of less than 10 ppm;
e) a phosphorus content of less than 10 ppm;
f) a color number of less than 80 Hazen;
g) an OH number of less than 5 mg KOH/g;
h) a chloride content of less than 500 ppm; and
i) a proportion of deaminated polymers of less than 3% by weight.

21. A process for promoting adhesion, comprising contacting an adhesive comprising the polyamine according to claim 20 to a substrate in need thereof.

22. The process according to claim 1 , wherein the conversion of the diamines is performed batchwise.

Assignees

• Basf Se

Inventors

• Altenhoff Ansgar Gereon
• Mueller Christoph
• Mueller Christian
• Kunst Andreas
• Reissner Thomas
• Dahmen Kirsten

Classifications

• C09J179/02 Primary

  Polyamines · CPC title

• C08G73/0206 Primary

  Polyalkylene(poly)amines · CPC title