Process and supply unit for restabilizing free-radically polymerizable monomers

Patent metadata

Field	Value
Publication number	US-9957202-B2
Application number	US-201414261932-A
Country	US
Kind code	B2
Filing date	Apr 25, 2014
Priority date	Apr 26, 2013
Publication date	May 1, 2018
Grant date	May 1, 2018

Abstract

The present invention relates to a process for restabilizing free-radically polymerizable monomers. The process comprises the steps: (a) introduction of a solution of an inhibitor of the free-radical polymerization by means of an inert pressurized gas into a vessel ( 1 ) comprising the monomers via a line ( 10 ) which comprises an ascending region, and (b) mixing of the contents of the vessel and the inhibitor solution by blowing gas through the line ( 10 ). In step (a), the flow velocity of the pressurized gas is set so that plug flow or annular flow is obtained as flow regime of the inhibitor solution and in step (b) the superficial gas velocity is set to ≥0.1 mm/s. The present invention further relates to a supply unit ( 11 ) for carrying out the process.

First claim

The invention claimed is:

1. A process for stabilizing free-radically polymerizable monomers, comprising:
a) introducing a solution of an inhibitor of the free-radical polymerization by means of an inert pressurized gas into a vessel comprising the monomers via at least one line which comprises an ascending region and at its end means for introducing the inhibitor solution and for blowing gas into the vessel; and
b) mixing of the contents of the vessel and the inhibitor solution by blowing gas through the line,
wherein
the flow velocity of the pressurized gas in the introducing (a) is set so that plug flow or annular flow is obtained as flow regime of the inhibitor solution in the ascending region of the line and the superficial gas velocity in the vessel in the mixing (b) is set to from 0.1 to 20 mm/s, and
the flow velocity of the pressurized gas in the introducing (a) is set to from 6 to 12 m/s,
and wherein the supply unit comprises:
(a) a vessel for the inhibitor solution having an offtake tube extending into the inhibitor solution;
(b) at least one pressurized gas reservoir which is connected to the vessel for the inhibitor solution via a gas feed line;
(c) means for reducing the pressure on the pressurized gas reservoir;
(d) means in the gas feed line for setting the superficial gas velocity; and
(e) means for connecting the offtake line to the line to the vessel,
wherein the (d) means for setting the superficial gas velocity has a connecting piece comprising an orifice plate, where the superficial gas velocity in the vessel in the mixing (b) is set to from 0.1 to 20 mm/s by means of the orifice plate.

2. The process according to claim 1 , wherein the inhibitor solution and the gas stock are provided by at least one supply unit which comprises a vessel for the inhibitor solution and at least one pressurized gas reservoir.

3. The process according to claim 2 , wherein the supply unit is arranged at a distance from the vessel and is connected to the vessel via the line.

4. The process according to claim 1 , wherein the line runs from the supply unit to the vessel through the lid of the monomer vessel.

5. The process according to claim 1 , wherein a plurality of supply units are connected in series or in parallel to the line.

6. The process according to claim 1 , wherein the supply unit comprises one to six pressurized gas reservoirs.

7. The process according to claim 1 , wherein the supply unit is configured as a mobile unit.

8. The process according to claim 1 , wherein the vessel is an upright cylindrical vessel, wherein a ratio of height to diameter of the upright cylindrical vessel is from 0.1 to 8.

9. The process according to claim 8 , wherein in the introducing (a), the inhibitor solution is introduced in a region of the bottom of the vessel, wherein the region is located at a distance from the bottom of 1/100 to 1/10 of the vessel height and at a distance of 1/100 to 1/10 from the vessel wall.

Assignees

• Basf Se

Inventors

• Martin Friedrich-Georg
• Odenwald Oliver

Classifications

• B01J4/001

  Feed or outlet devices as such, e.g. feeding tubes · CPC title

• B01J2219/00272

  Addition of reaction inhibitor · CPC title

• C07B63/04 Primary

  Use of additives {(anti-oxidant compositions or compositions inhibiting chemical change in general C09K15/00)} · CPC title

• B01J19/002 Primary

  Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions · CPC title