METHOD FOR THE PRODUCTION OF ETHYLENEAMINES

• US 20200131111A1
• Filed: 05/24/2018
• Published: 04/30/2020
• Est. Priority Date: 06/09/2017
• Status: Active Grant

• Current Assignee: BASF SE
• Original Assignee: BASF SE
• Inventors: HEIDEMANN, Thomas, BECKER, Barbara, KOCH, Eva, MELDER, Johann-Peter, LUYKEN, Hermann
• Granted Patent: US 11,208,373 B2
• Time in Patent Office: Days
• CPC Class Codes: B01J 21/04 Alumina
• CPC Class Codes: B01J 21/066 Zirconium or hafnium; Oxides or hydroxides thereof
• CPC Class Codes: B01J 23/8913 Cobalt and noble metals
• CPC Class Codes: B01J 35/50 characterised by their shape or configuration
• CPC Class Codes: B01J 37/0203 the impregnation liquid containing organic compounds
• CPC Class Codes: B01J 37/0213 Preparation of the impregnating solution
• CPC Class Codes: B01J 37/0236 Drying, e.g. preparing a suspension, adding a soluble salt and drying
• CPC Class Codes: B01J 37/086 Decomposition of an organometallic compound, a metal complex or a metal salt of a carboxylic acid
• CPC Class Codes: B01J 37/088 Decomposition of a metal salt
• CPC Class Codes: C07C 209/16 with formation of amino groups bound to acyclic carbon atoms or to carbon atoms of rings other than six-membered aromatic rings
• CPC Class Codes: C07C 211/10 Diaminoethanes
• CPC Class Codes: C07C 213/02 by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
• CPC Class Codes: C07C 215/08 with only one hydroxy group and one amino group bound to the carbon skeleton

Abstract

The present invention relates to a process for preparing alkanolamines and/or ethyleneamines in the liquid phase, by reacting ethylene glycol and/or monoethanolamine with ammonia in the presence of an amination catalyst comprising Co, Ru and Sn.

Claims

1. A process for preparing alkanolamines and/or ethyleneamines in the liquid phase, by reacting ethylene glycol and/or monoethanolamine with ammonia in the presence of an amination catalyst comprising Co, Ru and Sn.

2. The process according to claim 1, wherein the amination catalyst is obtained by reducing a catalyst precursor.

3. The process according to claim 2, wherein the catalyst precursor comprises 0.01% to 20% by weight of catalytically active components of Ru, calculated as RuO;

and 1% to 50% by weight of catalytically active components of Co, calculated as CoO; and

0.1% to 5% by weight of catalytically active components of Sn, calculated as SnO.

4. The process according to claim 1, wherein the catalyst precursor comprises one or more added catalyst elements selected from the group consisting of Cu, Ni, Zr and Al.

5. The process according to claim 4, wherein the catalyst precursor comprises

(i) 0.2% to 5% by weight of catalytically active components of Sn, calculated as SnO,

(ii) 1% to 35% by weight of catalytically active components of Co, calculated as CoO,

(iii) 10% to 80% by weight of catalytically active components of Al and/or Zr, calculated as Al₂O₃ and ZrO₂ respectively;

(iv) 1% to 35% by weight of catalytically active components of Cu and/or 1% to 35% by weight of catalytically active components of Ni, calculated as CuO and NiO respectively; and

(v) 0.01% to 20% by weight of catalytically active components of Ru, calculated as RuO.

6. The process according claim 1, wherein the catalyst precursor comprises a support material.

7. The process according to claim 6, wherein the support material is aluminum oxide, zirconium oxide or mixtures thereof.

8. The process according to claim 7, wherein the median diameter d₅₀ of the support material particles is in the range from 1 to 500 μ

m.

9. The process according to claim 1, wherein the catalyst precursor is prepared by coprecipitation.

10. The process according to claim 1, wherein the catalyst precursor is prepared by precipitative application or impregnation.

11. The process according to claim 9, wherein the catalyst precursor is prepared by precipitative application or coprecipitation and is impregnated in a further step.

12. The process according to claim 11, wherein a catalyst precursor comprising only, with a portion of the active metals Ru, Co and Sn is prepared by coprecipitation or precipitative application and the missing active metals or the missing portion of the active metals are applied to the catalyst precursor in a subsequent impregnation step.

13. The process according to claim 12, wherein a catalyst precursor comprising the active metals Co and Sn is first prepared and is then contacted in a further impregnation step with the active metals Co and Ru.

14. The process according to claim 13, wherein a catalyst precursor is prepared by precipitative application of the soluble compounds of Co and Sn to a support material and the catalyst precursor thus obtained is contacted with a soluble compound of Ru and a soluble compound of Co in an impregnation step.

15. The process according to claim 14, wherein Sn nitrate and Co nitrate are precipitated onto a support material in the presence of complexing agents and the catalyst precursor thus obtained is contacted with a soluble compound of Ru and a soluble compound of Co in an impregnation step.

16. The process according to claim 1, wherein the catalyst precursor is reductively calcined.