Method for producing ruthenium/iron/carbon carrier catalysts

Patent metadata

Field	Value
Publication number	US-10562009-B2
Application number	US-201615765821-A
Country	US
Kind code	B2
Filing date	Oct 4, 2016
Priority date	Oct 5, 2015
Publication date	Feb 18, 2020
Grant date	Feb 18, 2020

Abstract

The present invention relates to a process for producing iron-doped ruthenium-carbon support catalysts and also their use for the selective liquid-phase hydrogenation of carbonyl compounds to the corresponding alcohols, in particular for the hydrogenation of citral to geraniol or nerol or of citronellal to citronellal.

First claim

The invention claimed is:

1. A process for producing a ruthenium-iron-carbon support catalyst comprising from 0.1 to 5% by weight of iron in addition to from 0.1 to 10% by weight of ruthenium on a carbon support by
a) introducing a support into water
b) simultaneously adding the catalytically active components ruthenium and iron in the form of solutions of their metal salts
c) coprecipitating the catalytically active components on the support by addition of a base
d) separating the catalyst from the aqueous phase of the support suspension
e) drying the catalyst
f) reducing the catalyst in a stream of hydrogen at from 100 to less than 400° C. in a reduction reactor
g) removing the catalyst from the reduction reactor under liquids having a flashpoint of greater than 80° C.
or
passivating the catalyst by passing a diluted oxygen stream over it
or
passivating the catalyst by passing a diluted oxygen stream over it and removal of the catalyst from the reduction reactor under liquids having a flashpoint of greater than 80° C.

2. The process according to claim 1 , wherein the catalyst produced is a suspended catalyst.

3. The process according to claim 1 , wherein the catalyst produced is a fixed-bed catalyst.

4. The process according to claim 1 , wherein steps (b) and (c) are carried out at a temperature of from 50 to 95° C.

5. The process according to claim 1 , wherein steps (b) and (c) are carried out either simultaneously or successively.

6. The process according to claim 1 , wherein the catalytically active components are used in the form of their chlorides, nitrates, nitrosyl nitrates, acetates, oxides, hydroxides or acetylacetonates.

7. The process according to claim 1 , wherein the carbon support is pretreated by oxidation by means of HNO 3 , oxygen, hydrogen peroxide or hydrochloric acid.

8. The process according to claim 1 , wherein Na 2 CO 3 , NaHCO 3 , (NH 4 ) 2 CO 3 , NH 3 , urea, NaOH, KOH or LiOH is used as base for precipitation of the catalytically active components onto the support.

9. The process according to claim 1 , wherein NaOH is used for precipitation of the catalytically active components.

10. A process comprising selective liquid-phase hydrogenating carbonyl compounds of the general formula I

where
R 1 , R 2 are, independently of one another, identical or different and are each hydrogen or a saturated or a monounsaturated or polyunsaturated straight-chain or branched, optionally substituted, C 1 -C 20 -alkyl radical, an optionally substituted aryl radical or an optionally substituted heterocyclic group,
to the corresponding alcohols of the general formula II

where R 1 , R 2 are as defined above;
where the hydrogenation occurs over a catalyst produced by the process according to claim 1 .

11. The process according to claim 10 , wherein the carbonyl compound is an alpha,beta-unsaturated carbonyl compound.

12. The process according to claim 10 , wherein the carbonyl compound is citral.

13. The process according to claim 10 , wherein the carbonyl compound is citronellal.

14. The process according to claim 10 as suspended catalyst or fixed-bed catalyst.

15. The process according to claim 1 , wherein the reduction in step f) is carried out at from 120 to 300° C.

16. The process according to claim 1 , wherein the reduction in step f) is carried out at from 150 to 250° C.

17. The process according to claim 1 , wherein the reduction in step f) is carried out at from 180 to 220° C.

Assignees

• Basf Se

Inventors

• Schaack Bernd Bastian
• Wanisch Helmut
• Wucher Barbara
• Huber Sabine

Classifications

• B01J37/035

  Precipitation on carriers · CPC title

• B01J33/00

  Protection of catalysts, e.g. by coating · CPC title

• B01J37/0018

  Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat) · CPC title

• B01J21/18 Primary

  Carbon · CPC title

• C07C29/141 Primary

  with hydrogen or hydrogen-containing gases · CPC title