Method for vacuum purification

Patent metadata

Field	Value
Publication number	US-9937438-B2
Application number	US-201414911036-A
Country	US
Kind code	B2
Filing date	Jul 11, 2014
Priority date	Aug 13, 2013
Publication date	Apr 10, 2018
Grant date	Apr 10, 2018

Abstract

The present invention relates to a process for the vacuum purification of chemical compounds and to an apparatus for carrying out this process.

First claim

The invention claimed is:

1. Process for the purification of chemical substances which are solid at room temperature (sublimation material), where the substance is heated in vacuo, converted into the gas phase and subsequently condensed, characterised in that the vessel containing the sublimation material and the condensation unit rotate, and in that the process is carried out in an apparatus which has, between the rotating part and the static part, a rotation coupling which is selected from a rotary feedthrough with ferrofluidic seal or a double- or triple-acting mechanical face seal.

2. Process according to claim 1 , characterised in that the sublimation material is converted into the gas phase from the solid state or from the melt and in that the condensation takes place into the solid phase or into the liquid phase.

3. Process according to claim 1 , characterised in that it is carried out at a pressure of 10 −3 to 10 −7 mbar, preferably 10 −4 to 10 −6 mbar.

4. Process according to claim 1 , characterised in that the sublimation material has a molecular weight in the range from 300 to 5000 g/mol, preferably from 400 to 2500 g/mol, particularly preferably in the range from 450 to 1.500 g/mol.

5. Process according to claim 1 , characterised in that the process is carried out using a carrier gas in a pressure range from 10 −1 to 10 −4 mbar.

6. Process according to claim 1 , characterised in that the process is carried out semi-continuously.

7. Process according to claim 1 , characterised in that the rotational speed is in the range from 0.5 to 100 min −1 , preferably in the range from 1 to 20 min −1 , particularly preferably in the range from 1.5 to 10 min −1 .

8. Process according to claim 1 , characterised in that the sublimation material is converted into the gas phase at a temperature in the range from 200° C. to 500° C., preferably in the range from 250° C. to 450° C., particularly preferably in the range from 250° C. to 400° C.

Assignees

• Merck Patent Gmbh

Inventors

• Stoessel Philipp
• Fuchs Juergen

Classifications

• B01D3/085

  using a rotary evaporator · CPC title

• C07B63/00

  Purification; Separation (separation of optically-active compounds C07B57/00); Stabilisation; Use of additives · CPC title

• B01D7/00 Primary

  Sublimation (B01D8/00 takes precedence; freeze-drying F26) · CPC title