Process for workup of a crude ester comprising esterification catalyst hydrolysis product in suspended particulate form

Patent metadata

Field	Value
Publication number	US-9932292-B2
Application number	US-201515500197-A
Country	US
Kind code	B2
Filing date	Jul 29, 2015
Priority date	Aug 1, 2014
Publication date	Apr 3, 2018
Grant date	Apr 3, 2018

Abstract

In a process for workup of a crude ester comprising esterification catalyst hydrolysis product in suspended particulate form, a) the crude ester is admixed in an emulsifying tank with 1% to 10% by weight of water and the water is emulsified in the crude ester to obtain a suspoemulsion, b) the suspoemulsion from the emulsifying tank is transferred to an agglomerating tank containing an initial charge of water-undersaturated crude ester, such that a water content below the solubility limit of water in the crude ester is established in the mixture of the suspoemulsion and the initial charge of crude ester, as a result of which the suspended particulate esterification catalyst hydrolysis products form stable agglomerates, and c) the agglomerates formed are filtered off.

First claim

The invention claimed is:

1. A process for workup of a crude ester product that includes an esterification catalyst hydrolysis product in suspended particulate form, the process comprising
a) admixing the crude ester product in a tank with 1% to 10% by weight of water, based on the crude ester, and emulsifying the aqueous crude ester product to obtain a suspoemulsion, wherein the emulsifying of the aqueous crude ester product in step a) is achieved with at least one mixer at a Reynolds number of greater than 10 4 with a volume-specific power input in the range from 0.4 to 2.54 kW/m 3 ,
b) transferring the suspoemulsion from the tank to an agglomerating tank containing an initial charge of water-undersaturated crude ester, wherein the water content is below the solubility limit of water in the combined mixture of the suspoemulsion and the initial charge of the water-undersaturated crude ester, upon which the suspended particulate esterification catalyst hydrolysis product forms stable agglomerates, and
c) separating the agglomerates from the combined crude ester suspoemulsion product.

2. The process according to claim 1 , wherein the crude ester has an acid number of less than 0.1 mg KOH/g crude ester.

3. The process according to claim 1 , wherein the emulsifying the aqueous crude ester product in step a) with at least one stirrer at a circumferential speed in the range from 2.8 to 6.2 m/s.

4. The process according to claim 1 , wherein the suspoemulsion obtained in step a) comprises distributed water droplets having a mean particle size of more than 10 μm to less than 2000 μm.

5. The process according to claim 1 , wherein the tank has a height/diameter ratio H/D within a range from 1 to 6.

6. The process according to claim 1 , wherein the water content in the agglomerating tank is maintained below the solubility limit of water in step b) by continually distilling off water.

7. The process according to claim 1 , wherein the suspoemulsion is mixed in in the agglomerating tank with at least one mixer at a volume-specific power input of less than 0.2 kW/m 3 .

8. The process according to claim 1 , wherein the the combined crude ester suspoemulsion product from step c) is subjected to a stripping treatment.

9. The process according to claim 1 , wherein the suspended particulate esterification catalyst hydrolysis product is an esterification product of an esterification reaction catalyzed by a metallic esterification catalyst with an aqueous base from which a portion of water was removed from the esterification product/base mixture.

10. The process according to claim 9 , wherein the aqueous base is added to the esterification product at a temperature T of more than 100° C. under a pressure p equal to or greater than the vapor pressure of water at the temperature T.

11. The process according to claim 9 , wherein the water is from the esterification product/base mixture by decompressing the esterification product/base mixture.

12. A process for workup of a crude ester product, the process comprising
a) admixing the crude ester product in an emulsification tank with 1% to 10% by weight of water, based on the crude ester product, and emulsifying the aqueous crude ester product to obtain a suspoemulsion, the emulsification conducted with a volume-specific power input in a range from 0.6 to 2.0 kW/m 3 ,
wherein the crude ester is an esterification product of an esterification reaction catalyzed by a metallic esterification catalyst with an aqueous base from which a portion of water was removed from the esterification product/base mixture,

b) transferring the suspoemulsion from the emulsification tank to an agglomerating tank that contains an initial charge of water-undersaturated crude ester product to provide a mixture of the suspoemulsion and the initial charge of the water-undersaturated crude ester, wherein the water content in the mixture is maintained below the solubility limit of water of the crude ester product with a continuous removal of water from the agglomerating tank, and upon which the suspended particulate esterification catalyst hydrolysis product forms stable agglomerates, and
c) separating the agglomerates from the mixture of crude ester suspoemulsion product.

13. The process according to claim 12 , wherein the mixture in the agglomerating tank is stirred with a mixer at a volume-specific power input of less than 0.2 kW/m 3 .

14. The process according to claim 12 , wherein the crude ester product has an alcohol content of 1 to 6 wt %, based on the crude ester product, and suspoemulsion of step a) comprises distributed water droplets having a mean particle size of more than 200 μm to less than 2000 μm.

Assignees

• Basf Se

Inventors

• Makarczyk Piotr
• Breitscheidel Boris
• Rössler-Feigel Beatrice
• MÜHLHEIMS Kerstin

Classifications

• C07C67/56 Primary

  by solid-liquid treatment; by chemisorption · CPC title

• C07C69/80

  Phthalic acid esters · CPC title

• C07C67/62 Primary

  Use of additives, e.g. for stabilisation · CPC title

• C07C67/54

  by distillation · CPC title