# US 5,349,094 A · Process for the production of oligoglycerol mixtures of increased diglycerol content

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- Number: US 5,349,094 A
- Document ID: US5349094A
- Status: Granted
- Kind: A
- Application number: 07/898,061
- Filed: 1992-06-12
- Granted: 1994-09-20
- Earliest claimed: 1992-06-12
- Assignees: Henkel Kommanditgesellschaft auf Aktien
- Inventors: Eugene G. Harris; Udo Hees; Reinhard Bunte; Johannes W. Hachgenei; Peter Kuhm
- Web page: https://patentgrep.com/patent/US5349094A

## CPC

- C07C 41/09: by dehydration of compounds containing hydroxy groups
- C08G 65/34: from hydroxy compounds or their metallic derivatives {(C08G65/26 takes precedence)}
- C07C: ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C08G: MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS

## Abstract

Oligoglycerol mixtures having a high diglycerol content are prepared by a process in which glycerol is condensed in the presence of zeolites corresponding to formula (I) M.sub.2/z O * Al.sub.2 O.sub.3 * x SIO.sub.2 * y H.sub.2 O (I) in which M is an alkali metal or alkaline earth metal having a valency of z, x is a number of 1.8 to 12 and y is a number of 0 to 8. The water of condensation which is formed during the reaction, is continuously removed from the reaction mixture and the reaction is terminated when the quantity of water theoretically necessary for the formation of diglycerol has been separated.

## Claims

### Claim 1

A process for the production of oligoglycerol mixtures of increased diglycerol content which comprises condensing glycerol in the presence of zeolites having the formula (I)
M.sub.2/z O * Al.sub.2 O.sub.3 * x SiO.sub.2 * y H.sub.2 O (I)
in which M is an alkali metal or alkaline earth metal having a valency of z, x is a number of 1.8 to 12 and y is a number of 0 to 8, removing continuously the water of condensation, which is formed during the reaction, from the reaction mixture and terminating the reaction when the quantity of water theoretically necessary for the formation of diglycerol has been separated.

### Claim 2 (depends on 1)

A process as claimed in claim 1, wherein the zeolites are selected from the group consisting of zeolite X, zeolite Y, zeolite L, Zeolite A and mordenite are used.

### Claim 3 (depends on 1)

A process as claimed in claim 1 wherein the zeolites are used in quantities of 1 to 10% by weight, based on the glycerol.

### Claim 4 (depends on 2)

The process as claimed in claim 2 wherein the zeolites are used in quantities of 1 to 10% by weight, based on the glycerol.

### Claim 5 (depends on 1)

A process as claimed in claim 1 wherein the condensation is carried out at temperature of 200.degree. to 260.degree. C.

### Claim 6 (depends on 2)

The process as claimed in claim 2 wherein the condensation is carried out at temperature of 200.degree. to 260.degree. C.

### Claim 7 (depends on 1)

A process as claimed in claim 1 wherein the zeolites are separated from the oligoglycerol mixture after the reaction.

### Claim 8 (depends on 1)

A process according to claim 1 wherein M is sodium.

### Claim 9 (depends on 1)

A process according to claim 1 wherein the zeolite is selected from
Na.sub.86 [(AlO.sub.2).sub.86 (SiO.sub.2).sub.106 ]* 264 H.sub.2 O
Na.sub.56 [(AlO.sub.2).sub.56 (SIO.sub.2).sub.136 ]* 325 H.sub.2 O
or Na.sub.8.7 [(AlO.sub.2).sub.8.7 (SiO.sub.2).sub.39.3 ]* 24 H.sub.2 O.

### Claim 10 (depends on 2)

The process as claimed in claim 2 wherein the zeolite is select from
Na.sub.86 [(AlO.sub.2).sub.86 (SiO.sub.2).sub.106 ]* 264 H.sub.2 O
Na.sub.56 [(AlO.sub.2).sub.56 (SIO.sub.2).sub.136 ]* 325 H.sub.2 O
or Na.sub.8.7 [(AlO.sub.2).sub.8.7 (SiO.sub.2).sub.39.3 ]* 24 H.sub.2 O.