# US 6,297,409 B1 · Continuous process for the preparation of a high-purity hydrogenated ose by catalytic hydrogenation

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- Number: US 6,297,409 B1
- Document ID: US6297409B1
- Status: Granted
- Kind: B1
- Application number: 09/506,519
- Filed: 2000-02-17
- Granted: 2001-10-02
- Earliest claimed: 1999-02-17
- Assignees: Roquette Freres
- Inventors: Jean-Christophe Choque; Guy Fleche
- Web page: https://patentgrep.com/patent/US6297409B1

## CPC

- C07C 29/141: with hydrogen or hydrogen-containing gases
- C07C 29/145: with hydrogen or hydrogen-containing gases
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS

## Abstract

The invention relates to a continuous process for the preparation of a high-purity hydrogenated ose by catalytic hydrogenation of the corresponding ose in falling film reactors, wherein the hydrogenation is carried out in a series of fixed beds of ruthenium catalyst comprising: a) a first hydrogenation zone consisting of at least one fixed bed of ruthenium catalyst, and b) a second hydrogenation zone consisting of at least one fixed bed of ruthenium catalyst containing a promoter.

## Claims

### Claim 1

A continuous process for the preparation of a high-purity hydrogenated ose by hydrogenation of the corresponding ose in falling film reactors, comprising performing the hydrogenation in a series of fixed beds of ruthenium catalyst comprising:
a) a first hydrogenation zone consisting of at least one fixed bed of ruthenium catalyst, and
b) a second hydrogenation zone consisting of at least one fixed bed of ruthenium catalyst containing a promoter.

### Claim 2 (depends on 1)

The process of claim 1, wherein the promoter used with the ruthenium catalyst in the second hydrogenation zone is selected from the group consisting of titanium, molybdenum, platinum and chromium.

### Claim 3 (depends on 1)

The process of claim 1, wherein the promoter is platinum.

### Claim 4 (depends on 1)

The process of claim 1, wherein the ose is selected from the group consisting of erythrose, threose, glucose, mannose, galactose, ribose, arabinose, xylose, lyxose, and any isomer of anyone of said ose with a ketone group.

### Claim 5 (depends on 1)

The process of claim 1, wherein said ose is D-glucose.

### Claim 6 (depends on 1)

The process of claim 1, wherein the first hydrogenation zone is fed with an ose solution whose solids content is ranging between 20 and 50% by weight.

### Claim 7 (depends on 1)

The process of claim 1, wherein the first hydrogenation zone is fed with an ose solution whose solids content is ranging between 30 and 50% by weight.

### Claim 8 (depends on 1)

The process of claim 1, wherein, in each of the hydrogenation zones, the feed rate of the solution of ose to be hydrogenated is ranging between 0.3 and 2kg/l/h.

### Claim 9 (depends on 1)

The process of claim 1, wherein, in each of the hydrogenation zones, the feed rate of the solution of ose to be hydrogenated is ranging between 1 and 1.5 kg/l/h.

### Claim 10 (depends on 1)

The process of claim 1, wherein the surface flow velocity of the liquid passing through the beds of ruthenium catalyst arranged in series in the two hydrogenation zones is ranging between 0.02 and 0.2 cm/s.

### Claim 11 (depends on 1)

The process of claim 1, wherein the surface flow velocity of the liquid passing through the beds of ruthenium catalyst arranged in series in the two hydrogenation zones is of about 0.1 cm/s.

### Claim 12 (depends on 1)

The process of claim 1, wherein the temperature in the two hydrogenation zones is below 120° C., and wherein the hydrogen pressure in the two hydrogenation zones is at least 50 bar.

### Claim 13 (depends on 1)

The process of claim 1, wherein the temperature in the two hydrogenation zones is ranging between 80 and 105° C. and wherein the hydrogen pressure in the two hydrogenation zones is ranging between 80 and 150 bar.

### Claim 14 (depends on 1)

The process of claim 1, wherein the hydrogen flow rate is selected to provide an amount of hydrogen introduced of at least five times greater than the stoichiometry of the reaction.

### Claim 15 (depends on 1)

The process of claim 1, wherein the hydrogen flow rate is selected to provide an amount of hydrogen introduced of at least ten times greater than the stoichiometry of the reaction.

### Claim 16 (depends on 1)

The process of claim 1, wherein the hydrogenated ose is sorbitol.

### Claim 17 (depends on 1)

The process of claim 1, wherein the hydrogenated ose is sorbitol with a purity of at least 98.3% expressed as dry weight of obtained hydrogenated ose based on the total weight of hydrogenated, ose non-hydrogenated ose and co-products.

### Claim 18

The process of claim, wherein the hydrogenated ose is sorbitol with a purity of at least 98.5% by expressed as dry weight of obtained hydrogenated ose based on the total weight of hydrogenated, ose non-hydrogenated ose and co-products.